# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2023
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_Npe-TCNQ
_database_code_depnum_ccdc_archive 'CCDC 2286627'
loop_
_audit_author_name
_audit_author_address
'Joseph E. Reynolds III'
;Sandia National laboratory
United States of America
;
_audit_update_record
;
2023-08-03 deposited with the CCDC. 2023-09-26 downloaded from the CCDC.
;
_audit_creation_date 2022-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic 3TCNQ2NPE
_chemical_formula_moiety 'C17 H13 N, 1.5(C12 H4 N4)'
_chemical_formula_sum 'C35 H19 N7'
_chemical_formula_weight 537.57
_chemical_melting_point ?
_chemical_oxdiff_formula N4C18H18
_chemical_oxdiff_usercomment 'Solvent MeCN. 1:1 NVP:TCNQ'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.8862(4)
_cell_length_b 11.8127(5)
_cell_length_c 12.3102(5)
_cell_angle_alpha 93.827(3)
_cell_angle_beta 93.940(3)
_cell_angle_gamma 111.868(4)
_cell_volume 1324.40(9)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9179
_cell_measurement_temperature 102(3)
_cell_measurement_theta_max 72.7970
_cell_measurement_theta_min 3.5720
_shelx_estimated_absorpt_T_max 0.972
_shelx_estimated_absorpt_T_min 0.769
_exptl_absorpt_coefficient_mu 0.660
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.628
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear dark blue'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary blue
_exptl_crystal_density_diffrn 1.348
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 556
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 4 5 0.0682
-6 3 3 0.2140
-6 0 -1 0.1597
-3 -3 -5 0.1035
-6 1 0 0.1633
4 -5 -6 0.1346
6 -2 0 0.2000
0 5 -6 0.0197
0 -5 6 0.0214
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method '1:1 (DMF/MeCN)'
_exptl_crystal_size_max 0.421
_exptl_crystal_size_mid 0.186
_exptl_crystal_size_min 0.044
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9140 3.9586 4.6439 -0.5221 0.7533 0.4000
-6.1293 3.3378 2.7052 -0.2046 0.3045 -0.9303
-5.8139 -0.0079 -0.9175 0.1778 -0.2496 -0.9519
-2.6530 -3.0482 -4.7727 0.5621 -0.6596 -0.4990
-6.1226 0.7714 -0.2092 0.1080 -0.1334 -0.9852
3.7482 -4.5790 -5.5566 0.5595 -0.6489 0.5156
6.3939 -2.4375 -0.0922 -0.1033 -0.0949 0.9901
-0.3466 4.8916 -6.4030 0.8754 0.4777 0.0739
0.2698 -4.8636 6.4102 -0.8749 -0.4766 -0.0858
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0235
_diffrn_reflns_av_unetI/netI 0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 14402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.000
_diffrn_reflns_theta_min 3.617
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 102(3)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -117.00 -18.00 1.00 2.50 -- -42.59 -38.00 90.00 99
2 \w -87.00 -6.00 1.00 2.50 -- -42.59 125.00-120.00 81
3 \w -123.00 -2.00 1.00 2.50 -- -42.59 -19.00 150.00 121
4 \w 27.00 99.00 1.00 2.50 -- 42.59-125.00 60.00 72
5 \w 27.00 99.00 1.00 2.50 -- 42.59-125.00 0.00 72
6 \w 31.00 130.00 1.00 7.50 -- 104.03 -45.00-150.00 99
7 \w 78.00 177.00 1.00 7.50 -- 104.03 45.00-120.00 99
8 \w 103.00 178.00 1.00 7.50 -- 104.03 77.00 -90.00 75
9 \w 31.00 112.00 1.00 7.50 -- 104.03-125.00 -30.00 81
10 \w 22.00 106.00 1.00 7.50 -- 104.03 -95.00 60.00 84
11 \w 78.00 177.00 1.00 7.50 -- 104.03 45.00 -30.00 99
12 \w 78.00 177.00 1.00 7.50 -- 104.03 45.00-180.00 99
13 \w 22.00 106.00 1.00 7.50 -- 104.03 -95.00 120.00 84
14 \w 22.00 106.00 1.00 7.50 -- 104.03 -95.00 0.00 84
15 \w 28.00 137.00 1.00 7.50 -- 104.03 -77.00-180.00 109
16 \w 28.00 132.00 1.00 7.50 -- 104.03 -30.00 -60.00 104
17 \w -116.00 -14.00 1.00 2.50 -- -42.59 -57.00 60.00 102
18 \w -116.00 -14.00 1.00 2.50 -- -42.59 -57.00 -30.00 102
19 \w 14.00 116.00 1.00 2.50 -- 42.59 57.00 -60.00 102
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0112428000
_diffrn_orient_matrix_UB_12 0.0175216000
_diffrn_orient_matrix_UB_13 -0.1227225000
_diffrn_orient_matrix_UB_21 0.0382017000
_diffrn_orient_matrix_UB_22 0.1380527000
_diffrn_orient_matrix_UB_23 0.0287893000
_diffrn_orient_matrix_UB_31 0.1640097000
_diffrn_orient_matrix_UB_32 0.0240970000
_diffrn_orient_matrix_UB_33 -0.0020083000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4451
_reflns_number_total 5154
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_refine_diff_density_max 0.274
_refine_diff_density_min -0.195
_refine_diff_density_rms 0.043
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 379
_refine_ls_number_reflns 5154
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0431
_refine_ls_R_factor_gt 0.0372
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1021
_refine_ls_wR_factor_ref 0.1073
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25), C26(H26),
C34(H34), C35(H35)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.17548(11) 0.28132(9) 0.51408(8) 0.0242(2) Uani 1 1 d . . . . .
C1 C 0.11944(13) 0.36792(11) 0.50650(10) 0.0257(3) Uani 1 1 d . . . . .
H1 H 0.034055 0.358667 0.541900 0.031 Uiso 1 1 calc R U . . .
C2 C 0.17803(13) 0.47030(11) 0.45028(10) 0.0248(2) Uani 1 1 d . . . . .
H2 H 0.131912 0.527785 0.446903 0.030 Uiso 1 1 calc R U . . .
C3 C 0.30503(12) 0.48883(10) 0.39859(9) 0.0214(2) Uani 1 1 d . . . . .
C4 C 0.36365(12) 0.39816(10) 0.40551(9) 0.0233(2) Uani 1 1 d . . . . .
H4 H 0.449089 0.404840 0.371155 0.028 Uiso 1 1 calc R U . . .
C5 C 0.29623(12) 0.29879(10) 0.46275(9) 0.0230(2) Uani 1 1 d . . . . .
H5 H 0.338279 0.238556 0.466013 0.028 Uiso 1 1 calc R U . . .
C6 C 0.36807(12) 0.59846(10) 0.34144(9) 0.0233(2) Uani 1 1 d . . . . .
H6 H 0.311646 0.647548 0.331841 0.028 Uiso 1 1 calc R U . . .
C7 C 0.49860(12) 0.63543(10) 0.30153(9) 0.0209(2) Uani 1 1 d . . . . .
H7 H 0.556571 0.588129 0.314112 0.025 Uiso 1 1 calc R U . . .
C8 C 0.56051(12) 0.74260(10) 0.23997(9) 0.0201(2) Uani 1 1 d . . . . .
C9 C 0.49245(13) 0.82551(10) 0.23026(9) 0.0235(2) Uani 1 1 d . . . . .
H9 H 0.411472 0.817679 0.270660 0.028 Uiso 1 1 calc R U . . .
C10 C 0.53999(13) 0.92080(10) 0.16229(10) 0.0249(2) Uani 1 1 d . . . . .
H10 H 0.491486 0.976511 0.157705 0.030 Uiso 1 1 calc R U . . .
C11 C 0.65578(13) 0.93381(10) 0.10267(9) 0.0238(2) Uani 1 1 d . . . . .
H11 H 0.684685 0.996401 0.054619 0.029 Uiso 1 1 calc R U . . .
C12 C 0.73256(12) 0.85467(10) 0.11219(9) 0.0207(2) Uani 1 1 d . . . . .
C13 C 0.85430(13) 0.86905(10) 0.05228(9) 0.0245(2) Uani 1 1 d . . . . .
H13 H 0.882111 0.931018 0.003559 0.029 Uiso 1 1 calc R U . . .
C14 C 0.93277(13) 0.79556(11) 0.06306(10) 0.0265(3) Uani 1 1 d . . . . .
H14 H 1.013853 0.806153 0.022041 0.032 Uiso 1 1 calc R U . . .
C15 C 0.89173(13) 0.70391(10) 0.13583(9) 0.0241(2) Uani 1 1 d . . . . .
H15 H 0.947368 0.654118 0.144970 0.029 Uiso 1 1 calc R U . . .
C16 C 0.77289(12) 0.68563(10) 0.19350(9) 0.0213(2) Uani 1 1 d . . . . .
H16 H 0.746817 0.622579 0.241222 0.026 Uiso 1 1 calc R U . . .
C17 C 0.68776(12) 0.75917(9) 0.18335(9) 0.0191(2) Uani 1 1 d . . . . .
N2 N 0.36223(12) 0.13406(10) 0.18972(9) 0.0302(2) Uani 1 1 d . . . . .
N3 N 0.16050(11) -0.18151(9) 0.36785(8) 0.0267(2) Uani 1 1 d . . . . .
N4 N -0.51495(12) 0.10923(10) 0.45992(9) 0.0330(3) Uani 1 1 d . . . . .
N5 N -0.28285(12) 0.40113(9) 0.27771(9) 0.0305(2) Uani 1 1 d . . . . .
C18 C 0.26447(13) 0.07817(11) 0.23461(9) 0.0226(2) Uani 1 1 d . . . . .
C19 C 0.14831(12) -0.09675(10) 0.33519(9) 0.0212(2) Uani 1 1 d . . . . .
C20 C 0.14174(12) 0.01107(10) 0.29172(9) 0.0200(2) Uani 1 1 d . . . . .
C21 C 0.03000(12) 0.05244(10) 0.30371(8) 0.0190(2) Uani 1 1 d . . . . .
C22 C -0.09200(12) -0.00973(10) 0.36492(9) 0.0189(2) Uani 1 1 d . . . . .
H22 H -0.099194 -0.083821 0.394407 0.023 Uiso 1 1 calc R U . . .
C23 C -0.19546(12) 0.03712(10) 0.38023(8) 0.0190(2) Uani 1 1 d . . . . .
H23 H -0.274325 -0.004066 0.421154 0.023 Uiso 1 1 calc R U . . .
C24 C -0.18804(12) 0.14935(10) 0.33515(8) 0.0186(2) Uani 1 1 d . . . . .
C25 C -0.06912(12) 0.20837(10) 0.27054(9) 0.0200(2) Uani 1 1 d . . . . .
H25 H -0.063831 0.280694 0.238521 0.024 Uiso 1 1 calc R U . . .
C26 C 0.03365(12) 0.16189(10) 0.25548(9) 0.0203(2) Uani 1 1 d . . . . .
H26 H 0.110446 0.201556 0.212279 0.024 Uiso 1 1 calc R U . . .
C27 C -0.29025(12) 0.20007(10) 0.35240(9) 0.0200(2) Uani 1 1 d . . . . .
C28 C -0.41285(13) 0.14682(10) 0.41351(9) 0.0232(2) Uani 1 1 d . . . . .
C29 C -0.28395(12) 0.31196(10) 0.30923(9) 0.0223(2) Uani 1 1 d . . . . .
N6 N 0.06213(11) 0.46879(10) 0.14545(9) 0.0310(2) Uani 1 1 d . . . . .
N7 N 0.25844(12) 0.77467(9) -0.04490(9) 0.0301(2) Uani 1 1 d . . . . .
C30 C 0.15714(13) 0.51934(10) 0.09602(9) 0.0230(2) Uani 1 1 d . . . . .
C31 C 0.26624(12) 0.68883(10) -0.01156(9) 0.0218(2) Uani 1 1 d . . . . .
C32 C 0.27434(12) 0.58219(10) 0.03292(9) 0.0201(2) Uani 1 1 d . . . . .
C33 C 0.38631(12) 0.54224(9) 0.01707(8) 0.0186(2) Uani 1 1 d . . . . .
C34 C 0.50019(12) 0.60442(10) -0.05069(9) 0.0199(2) Uani 1 1 d . . . . .
H34 H 0.498944 0.674544 -0.083626 0.024 Uiso 1 1 calc R U . . .
C35 C 0.39249(12) 0.43670(9) 0.06712(9) 0.0198(2) Uani 1 1 d . . . . .
H35 H 0.319180 0.395668 0.112512 0.024 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0248(5) 0.0242(5) 0.0242(5) 0.0043(4) 0.0019(4) 0.0099(4)
C1 0.0248(6) 0.0267(6) 0.0279(6) 0.0049(5) 0.0073(5) 0.0114(5)
C2 0.0245(6) 0.0242(6) 0.0296(6) 0.0048(5) 0.0061(5) 0.0126(5)
C3 0.0196(5) 0.0225(5) 0.0218(5) 0.0017(4) 0.0006(4) 0.0079(4)
C4 0.0203(6) 0.0237(6) 0.0266(6) 0.0024(4) 0.0027(4) 0.0092(5)
C5 0.0221(6) 0.0220(6) 0.0261(5) 0.0022(4) 0.0001(4) 0.0100(5)
C6 0.0235(6) 0.0229(6) 0.0253(5) 0.0038(4) 0.0023(4) 0.0107(5)
C7 0.0220(6) 0.0200(5) 0.0214(5) 0.0018(4) 0.0008(4) 0.0090(4)
C8 0.0206(5) 0.0178(5) 0.0215(5) 0.0002(4) -0.0007(4) 0.0075(4)
C9 0.0217(6) 0.0211(5) 0.0282(6) 0.0010(4) 0.0020(4) 0.0091(4)
C10 0.0265(6) 0.0191(5) 0.0317(6) 0.0010(4) -0.0017(5) 0.0127(5)
C11 0.0278(6) 0.0169(5) 0.0256(5) 0.0035(4) -0.0018(4) 0.0078(4)
C12 0.0215(5) 0.0166(5) 0.0219(5) 0.0009(4) -0.0011(4) 0.0054(4)
C13 0.0242(6) 0.0214(5) 0.0246(5) 0.0036(4) 0.0018(4) 0.0046(4)
C14 0.0219(6) 0.0280(6) 0.0280(6) -0.0004(5) 0.0044(5) 0.0078(5)
C15 0.0232(6) 0.0234(6) 0.0275(6) -0.0002(4) 0.0003(4) 0.0116(5)
C16 0.0228(6) 0.0183(5) 0.0231(5) 0.0016(4) -0.0004(4) 0.0087(4)
C17 0.0204(5) 0.0158(5) 0.0197(5) 0.0005(4) -0.0005(4) 0.0058(4)
N2 0.0279(5) 0.0349(6) 0.0343(6) 0.0121(4) 0.0104(4) 0.0168(5)
N3 0.0237(5) 0.0270(5) 0.0340(5) 0.0078(4) 0.0061(4) 0.0135(4)
N4 0.0308(6) 0.0353(6) 0.0447(6) 0.0194(5) 0.0161(5) 0.0214(5)
N5 0.0360(6) 0.0253(5) 0.0354(6) 0.0082(4) 0.0052(5) 0.0166(4)
C18 0.0231(6) 0.0267(6) 0.0229(5) 0.0048(4) 0.0033(4) 0.0144(5)
C19 0.0166(5) 0.0261(6) 0.0228(5) 0.0021(4) 0.0040(4) 0.0099(4)
C20 0.0196(5) 0.0215(5) 0.0198(5) 0.0022(4) 0.0013(4) 0.0089(4)
C21 0.0185(5) 0.0202(5) 0.0176(5) 0.0009(4) 0.0000(4) 0.0071(4)
C22 0.0196(5) 0.0174(5) 0.0198(5) 0.0037(4) 0.0007(4) 0.0072(4)
C23 0.0187(5) 0.0191(5) 0.0188(5) 0.0036(4) 0.0019(4) 0.0066(4)
C24 0.0186(5) 0.0194(5) 0.0178(5) 0.0018(4) -0.0008(4) 0.0078(4)
C25 0.0200(5) 0.0201(5) 0.0206(5) 0.0053(4) 0.0022(4) 0.0077(4)
C26 0.0189(5) 0.0213(5) 0.0210(5) 0.0060(4) 0.0037(4) 0.0072(4)
C27 0.0202(5) 0.0207(5) 0.0207(5) 0.0042(4) 0.0027(4) 0.0091(4)
C28 0.0247(6) 0.0239(6) 0.0279(6) 0.0083(5) 0.0046(5) 0.0157(5)
C29 0.0214(6) 0.0236(6) 0.0248(5) 0.0033(4) 0.0038(4) 0.0116(5)
N6 0.0263(5) 0.0315(6) 0.0395(6) 0.0123(5) 0.0082(5) 0.0134(5)
N7 0.0300(5) 0.0242(5) 0.0392(6) 0.0068(4) -0.0002(4) 0.0139(4)
C30 0.0219(6) 0.0218(5) 0.0278(6) 0.0040(4) 0.0001(5) 0.0112(5)
C31 0.0183(5) 0.0215(6) 0.0262(5) 0.0020(4) 0.0000(4) 0.0087(4)
C32 0.0202(5) 0.0177(5) 0.0226(5) 0.0025(4) 0.0000(4) 0.0078(4)
C33 0.0192(5) 0.0161(5) 0.0196(5) 0.0006(4) -0.0016(4) 0.0063(4)
C34 0.0215(6) 0.0165(5) 0.0210(5) 0.0037(4) -0.0003(4) 0.0067(4)
C35 0.0197(5) 0.0175(5) 0.0212(5) 0.0038(4) 0.0009(4) 0.0060(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.3380(15) . ?
N1 C5 1.3433(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.3865(16) . ?
C2 H2 0.9500 . ?
C2 C3 1.3974(15) . ?
C3 C4 1.3994(15) . ?
C3 C6 1.4632(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.3823(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.3391(16) . ?
C7 H7 0.9500 . ?
C7 C8 1.4719(15) . ?
C8 C9 1.3862(15) . ?
C8 C17 1.4360(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.4049(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.3683(16) . ?
C11 H11 0.9500 . ?
C11 C12 1.4123(15) . ?
C12 C13 1.4170(16) . ?
C12 C17 1.4315(15) . ?
C13 H13 0.9500 . ?
C13 C14 1.3697(17) . ?
C14 H14 0.9500 . ?
C14 C15 1.4111(17) . ?
C15 H15 0.9500 . ?
C15 C16 1.3701(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.4224(15) . ?
N2 C18 1.1498(16) . ?
N3 C19 1.1470(15) . ?
N4 C28 1.1496(15) . ?
N5 C29 1.1431(15) . ?
C18 C20 1.4388(15) . ?
C19 C20 1.4354(15) . ?
C20 C21 1.3769(15) . ?
C21 C22 1.4494(15) . ?
C21 C26 1.4477(14) . ?
C22 H22 0.9500 . ?
C22 C23 1.3499(15) . ?
C23 H23 0.9500 . ?
C23 C24 1.4499(14) . ?
C24 C25 1.4467(14) . ?
C24 C27 1.3743(15) . ?
C25 H25 0.9500 . ?
C25 C26 1.3402(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.4322(15) . ?
C27 C29 1.4389(15) . ?
N6 C30 1.1482(16) . ?
N7 C31 1.1454(15) . ?
C30 C32 1.4342(15) . ?
C31 C32 1.4333(15) . ?
C32 C33 1.3758(15) . ?
C33 C34 1.4483(15) . ?
C33 C35 1.4463(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.3428(15) 2_665 ?
C35 H35 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C5 115.57(10) . . ?
N1 C1 H1 117.9 . . ?
N1 C1 C2 124.17(11) . . ?
C2 C1 H1 117.9 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 119.91(11) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 116.21(10) . . ?
C2 C3 C6 119.62(10) . . ?
C4 C3 C6 124.17(10) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.46(10) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 124.66(10) . . ?
N1 C5 H5 117.7 . . ?
C4 C5 H5 117.7 . . ?
C3 C6 H6 117.2 . . ?
C7 C6 C3 125.51(10) . . ?
C7 C6 H6 117.2 . . ?
C6 C7 H7 117.0 . . ?
C6 C7 C8 125.99(10) . . ?
C8 C7 H7 117.0 . . ?
C9 C8 C7 120.72(10) . . ?
C9 C8 C17 118.71(10) . . ?
C17 C8 C7 120.47(9) . . ?
C8 C9 H9 119.1 . . ?
C8 C9 C10 121.78(10) . . ?
C10 C9 H9 119.1 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.35(10) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.35(10) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C13 120.67(10) . . ?
C11 C12 C17 119.88(11) . . ?
C13 C12 C17 119.45(10) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 C12 121.45(11) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.20(11) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.02(11) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.3 . . ?
C15 C16 C17 121.32(10) . . ?
C17 C16 H16 119.3 . . ?
C12 C17 C8 118.74(10) . . ?
C16 C17 C8 123.75(10) . . ?
C16 C17 C12 117.51(10) . . ?
N2 C18 C20 178.55(12) . . ?
N3 C19 C20 176.44(11) . . ?
C19 C20 C18 115.22(9) . . ?
C21 C20 C18 120.38(10) . . ?
C21 C20 C19 124.38(10) . . ?
C20 C21 C22 121.88(10) . . ?
C20 C21 C26 119.81(10) . . ?
C26 C21 C22 118.30(9) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.33(10) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.99(10) . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 118.39(9) . . ?
C27 C24 C23 121.76(10) . . ?
C27 C24 C25 119.85(9) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.56(10) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 H26 119.3 . . ?
C25 C26 C21 121.33(10) . . ?
C25 C26 H26 119.3 . . ?
C24 C27 C28 123.63(10) . . ?
C24 C27 C29 122.57(10) . . ?
C28 C27 C29 113.80(9) . . ?
N4 C28 C27 175.58(11) . . ?
N5 C29 C27 177.29(12) . . ?
N6 C30 C32 179.17(12) . . ?
N7 C31 C32 178.37(12) . . ?
C31 C32 C30 115.29(9) . . ?
C33 C32 C30 121.85(10) . . ?
C33 C32 C31 122.86(10) . . ?
C32 C33 C34 120.77(10) . . ?
C32 C33 C35 120.76(10) . . ?
C35 C33 C34 118.47(10) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.24(10) 2_665 . ?
C35 C34 H34 119.9 2_665 . ?
C33 C35 H35 119.4 . . ?
C34 C35 C33 121.29(10) 2_665 . ?
C34 C35 H35 119.4 2_665 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -1.12(19) . . . . ?
C1 N1 C5 C4 0.54(17) . . . . ?
C1 C2 C3 C4 1.48(17) . . . . ?
C1 C2 C3 C6 -178.66(11) . . . . ?
C2 C3 C4 C5 -0.91(16) . . . . ?
C2 C3 C6 C7 170.55(11) . . . . ?
C3 C4 C5 N1 -0.10(18) . . . . ?
C3 C6 C7 C8 177.30(10) . . . . ?
C4 C3 C6 C7 -9.60(19) . . . . ?
C5 N1 C1 C2 0.08(17) . . . . ?
C6 C3 C4 C5 179.23(11) . . . . ?
C6 C7 C8 C9 8.48(18) . . . . ?
C6 C7 C8 C17 -167.77(11) . . . . ?
C7 C8 C9 C10 -172.92(10) . . . . ?
C7 C8 C17 C12 171.41(10) . . . . ?
C7 C8 C17 C16 -8.47(16) . . . . ?
C8 C9 C10 C11 0.39(18) . . . . ?
C9 C8 C17 C12 -4.92(15) . . . . ?
C9 C8 C17 C16 175.21(10) . . . . ?
C9 C10 C11 C12 -2.59(17) . . . . ?
C10 C11 C12 C13 -178.80(11) . . . . ?
C10 C11 C12 C17 0.92(17) . . . . ?
C11 C12 C13 C14 177.97(11) . . . . ?
C11 C12 C17 C8 2.84(16) . . . . ?
C11 C12 C17 C16 -177.28(10) . . . . ?
C12 C13 C14 C15 -0.28(17) . . . . ?
C13 C12 C17 C8 -177.44(9) . . . . ?
C13 C12 C17 C16 2.45(16) . . . . ?
C13 C14 C15 C16 1.61(17) . . . . ?
C14 C15 C16 C17 -0.84(17) . . . . ?
C15 C16 C17 C8 178.69(10) . . . . ?
C15 C16 C17 C12 -1.19(16) . . . . ?
C17 C8 C9 C10 3.39(16) . . . . ?
C17 C12 C13 C14 -1.76(17) . . . . ?
C18 C20 C21 C22 -177.19(10) . . . . ?
C18 C20 C21 C26 2.03(16) . . . . ?
C19 C20 C21 C22 1.39(17) . . . . ?
C19 C20 C21 C26 -179.39(10) . . . . ?
C20 C21 C22 C23 176.29(10) . . . . ?
C20 C21 C26 C25 -176.35(10) . . . . ?
C21 C22 C23 C24 0.66(16) . . . . ?
C22 C21 C26 C25 2.89(16) . . . . ?
C22 C23 C24 C25 1.73(15) . . . . ?
C22 C23 C24 C27 -178.23(10) . . . . ?
C23 C24 C25 C26 -1.80(15) . . . . ?
C23 C24 C27 C28 -1.21(17) . . . . ?
C23 C24 C27 C29 179.40(10) . . . . ?
C24 C25 C26 C21 -0.53(16) . . . . ?
C25 C24 C27 C28 178.83(10) . . . . ?
C25 C24 C27 C29 -0.57(17) . . . . ?
C26 C21 C22 C23 -2.94(15) . . . . ?
C27 C24 C25 C26 178.17(11) . . . . ?
C30 C32 C33 C34 177.46(10) . . . . ?
C30 C32 C33 C35 -2.14(16) . . . . ?
C31 C32 C33 C34 -2.74(17) . . . . ?
C31 C32 C33 C35 177.65(10) . . . . ?
C32 C33 C34 C35 -178.83(10) . . . 2_665 ?
C32 C33 C35 C34 178.82(10) . . . 2_665 ?
C34 C33 C35 C34 -0.79(17) . . . 2_665 ?
C35 C33 C34 C35 0.78(17) . . . 2_665 ?
_shelx_res_file
;
TITL CY_B8b in P-1 #2
cy_b8b.res
created by SHELXL-2018/3 at 10:31:54 on 28-Jun-2022
REM reset to P-1 #2
CELL 1.54184 9.886245 11.812746 12.310211 93.8271 93.9401 111.868
ZERR 2 0.000359 0.00046 0.000452 0.0031 0.003 0.0035
LATT 1
SFAC C H N
UNIT 70 38 14
L.S. 10
PLAN 5
SIZE 0.044 0.186 0.421
TEMP -171
CONF
BOND
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.065000 0.166600
FVAR 2.90920
N1 3 0.175485 0.281318 0.514085 11.00000 0.02482 0.02425 =
0.02424 0.00434 0.00186 0.00988
C1 1 0.119437 0.367919 0.506504 11.00000 0.02478 0.02672 =
0.02790 0.00493 0.00733 0.01136
AFIX 43
H1 2 0.034055 0.358667 0.541900 11.00000 -1.20000
AFIX 0
C2 1 0.178034 0.470304 0.450280 11.00000 0.02448 0.02417 =
0.02959 0.00482 0.00607 0.01257
AFIX 43
H2 2 0.131912 0.527785 0.446903 11.00000 -1.20000
AFIX 0
C3 1 0.305026 0.488833 0.398585 11.00000 0.01957 0.02251 =
0.02181 0.00171 0.00055 0.00794
C4 1 0.363648 0.398157 0.405512 11.00000 0.02026 0.02375 =
0.02658 0.00242 0.00269 0.00918
AFIX 43
H4 2 0.449089 0.404840 0.371155 11.00000 -1.20000
AFIX 0
C5 1 0.296228 0.298786 0.462749 11.00000 0.02206 0.02197 =
0.02615 0.00224 0.00007 0.00999
AFIX 43
H5 2 0.338279 0.238556 0.466013 11.00000 -1.20000
AFIX 0
C6 1 0.368071 0.598457 0.341441 11.00000 0.02352 0.02289 =
0.02532 0.00379 0.00235 0.01070
AFIX 43
H6 2 0.311646 0.647548 0.331841 11.00000 -1.20000
AFIX 0
C7 1 0.498600 0.635426 0.301532 11.00000 0.02201 0.02003 =
0.02143 0.00179 0.00083 0.00897
AFIX 43
H7 2 0.556571 0.588129 0.314112 11.00000 -1.20000
AFIX 0
C8 1 0.560505 0.742602 0.239969 11.00000 0.02061 0.01776 =
0.02147 0.00017 -0.00072 0.00754
C9 1 0.492451 0.825510 0.230261 11.00000 0.02173 0.02109 =
0.02823 0.00099 0.00195 0.00908
AFIX 43
H9 2 0.411472 0.817679 0.270660 11.00000 -1.20000
AFIX 0
C10 1 0.539992 0.920804 0.162294 11.00000 0.02648 0.01912 =
0.03172 0.00101 -0.00169 0.01271
AFIX 43
H10 2 0.491486 0.976511 0.157705 11.00000 -1.20000
AFIX 0
C11 1 0.655782 0.933808 0.102672 11.00000 0.02776 0.01692 =
0.02556 0.00351 -0.00180 0.00779
AFIX 43
H11 2 0.684685 0.996401 0.054619 11.00000 -1.20000
AFIX 0
C12 1 0.732558 0.854672 0.112187 11.00000 0.02147 0.01662 =
0.02190 0.00085 -0.00112 0.00539
C13 1 0.854303 0.869046 0.052276 11.00000 0.02421 0.02138 =
0.02457 0.00355 0.00179 0.00462
AFIX 43
H13 2 0.882111 0.931018 0.003559 11.00000 -1.20000
AFIX 0
C14 1 0.932771 0.795555 0.063059 11.00000 0.02192 0.02796 =
0.02803 -0.00036 0.00443 0.00785
AFIX 43
H14 2 1.013853 0.806153 0.022041 11.00000 -1.20000
AFIX 0
C15 1 0.891732 0.703911 0.135827 11.00000 0.02316 0.02336 =
0.02746 -0.00016 0.00028 0.01158
AFIX 43
H15 2 0.947368 0.654118 0.144970 11.00000 -1.20000
AFIX 0
C16 1 0.772885 0.685630 0.193499 11.00000 0.02279 0.01830 =
0.02310 0.00156 -0.00039 0.00869
AFIX 43
H16 2 0.746817 0.622579 0.241222 11.00000 -1.20000
AFIX 0
C17 1 0.687758 0.759168 0.183346 11.00000 0.02044 0.01579 =
0.01972 0.00054 -0.00053 0.00584
N2 3 0.362233 0.134059 0.189718 11.00000 0.02791 0.03492 =
0.03429 0.01205 0.01039 0.01679
N3 3 0.160505 -0.181510 0.367847 11.00000 0.02367 0.02699 =
0.03399 0.00775 0.00609 0.01351
N4 3 -0.514954 0.109234 0.459918 11.00000 0.03079 0.03530 =
0.04468 0.01938 0.01612 0.02140
N5 3 -0.282849 0.401125 0.277707 11.00000 0.03604 0.02534 =
0.03545 0.00822 0.00516 0.01657
C18 1 0.264475 0.078170 0.234610 11.00000 0.02307 0.02672 =
0.02294 0.00478 0.00326 0.01439
C19 1 0.148313 -0.096751 0.335185 11.00000 0.01661 0.02606 =
0.02277 0.00213 0.00396 0.00987
C20 1 0.141743 0.011071 0.291724 11.00000 0.01955 0.02153 =
0.01978 0.00220 0.00131 0.00890
C21 1 0.030001 0.052444 0.303711 11.00000 0.01852 0.02018 =
0.01765 0.00091 0.00002 0.00713
C22 1 -0.092003 -0.009728 0.364917 11.00000 0.01964 0.01744 =
0.01982 0.00365 0.00071 0.00723
AFIX 43
H22 2 -0.099194 -0.083821 0.394407 11.00000 -1.20000
AFIX 0
C23 1 -0.195463 0.037119 0.380228 11.00000 0.01871 0.01910 =
0.01881 0.00363 0.00189 0.00656
AFIX 43
H23 2 -0.274325 -0.004066 0.421154 11.00000 -1.20000
AFIX 0
C24 1 -0.188039 0.149346 0.335153 11.00000 0.01861 0.01937 =
0.01778 0.00181 -0.00083 0.00778
C25 1 -0.069118 0.208372 0.270542 11.00000 0.02003 0.02007 =
0.02064 0.00530 0.00219 0.00773
AFIX 43
H25 2 -0.063831 0.280694 0.238521 11.00000 -1.20000
AFIX 0
C26 1 0.033652 0.161889 0.255478 11.00000 0.01890 0.02130 =
0.02101 0.00598 0.00366 0.00719
AFIX 43
H26 2 0.110446 0.201556 0.212279 11.00000 -1.20000
AFIX 0
C27 1 -0.290250 0.200070 0.352404 11.00000 0.02023 0.02074 =
0.02066 0.00416 0.00265 0.00907
C28 1 -0.412852 0.146819 0.413511 11.00000 0.02472 0.02391 =
0.02791 0.00827 0.00458 0.01571
C29 1 -0.283950 0.311962 0.309232 11.00000 0.02143 0.02365 =
0.02477 0.00327 0.00378 0.01163
N6 3 0.062133 0.468792 0.145454 11.00000 0.02631 0.03147 =
0.03953 0.01226 0.00821 0.01342
N7 3 0.258436 0.774667 -0.044901 11.00000 0.02998 0.02421 =
0.03920 0.00682 -0.00025 0.01387
C30 1 0.157145 0.519338 0.096025 11.00000 0.02186 0.02175 =
0.02782 0.00399 0.00012 0.01118
C31 1 0.266243 0.688832 -0.011563 11.00000 0.01828 0.02151 =
0.02624 0.00197 0.00005 0.00873
C32 1 0.274341 0.582194 0.032924 11.00000 0.02024 0.01769 =
0.02262 0.00251 0.00004 0.00780
C33 1 0.386308 0.542240 0.017069 11.00000 0.01919 0.01609 =
0.01961 0.00058 -0.00162 0.00631
C34 1 0.500186 0.604417 -0.050689 11.00000 0.02152 0.01650 =
0.02101 0.00370 -0.00035 0.00666
AFIX 43
H34 2 0.498944 0.674544 -0.083626 11.00000 -1.20000
AFIX 0
C35 1 0.392486 0.436700 0.067122 11.00000 0.01975 0.01754 =
0.02121 0.00382 0.00091 0.00604
AFIX 43
H35 2 0.319180 0.395668 0.112512 11.00000 -1.20000
AFIX 0
HKLF 4
REM CY_B8b in P-1 #2
REM wR2 = 0.1073, GooF = S = 1.031, Restrained GooF = 1.031 for all data
REM R1 = 0.0372 for 4451 Fo > 4sig(Fo) and 0.0431 for all 5154 data
REM 379 parameters refined using 0 restraints
END
WGHT 0.0650 0.1666
REM Highest difference peak 0.274, deepest hole -0.195, 1-sigma level 0.043
Q1 1 0.7161 0.8175 0.1472 11.00000 0.05 0.27
Q2 1 0.3842 0.4885 0.0439 11.00000 0.05 0.23
Q3 1 -0.1874 0.0902 0.3552 11.00000 0.05 0.21
Q4 1 -0.1276 0.1776 0.3004 11.00000 0.05 0.20
Q5 1 0.4536 0.5771 -0.0177 11.00000 0.05 0.20
;
_shelx_res_checksum 74300
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.885
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Npe-TCNB
_database_code_depnum_ccdc_archive 'CCDC 2286628'
loop_
_audit_author_name
_audit_author_address
'Joseph E. Reynolds III '
;Sandia National laboratory
United States of America
;
_audit_update_record
;
2023-08-03 deposited with the CCDC. 2023-09-26 downloaded from the CCDC.
;
_audit_creation_date 2022-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C10 H2 N4, C17 H13 N'
_chemical_formula_sum 'C27 H15 N5'
_chemical_formula_weight 409.44
_chemical_melting_point ?
_chemical_oxdiff_formula N5C26H15
_chemical_oxdiff_usercomment '1:1 acetonitrile:DMF'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 6.7312(3)
_cell_length_b 36.6599(13)
_cell_length_c 9.5150(4)
_cell_angle_alpha 90
_cell_angle_beta 106.283(4)
_cell_angle_gamma 90
_cell_volume 2253.79(17)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2625
_cell_measurement_temperature 99.95(10)
_cell_measurement_theta_max 68.1260
_cell_measurement_theta_min 4.7860
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.586
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.87727
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier .
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.207
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 848
_exptl_crystal_preparation 'cryoloop with paratone oil'
_exptl_crystal_recrystallization_method 'slow evaporation / 1:1 DMF:MeCN'
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.077
_exptl_crystal_size_min 0.037
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0264
_diffrn_reflns_av_unetI/netI 0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 39
_diffrn_reflns_limit_k_min -44
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 8966
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 72.129
_diffrn_reflns_theta_min 4.825
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 99.95(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -55.00 32.00 1.00 22.50 -- -42.47 38.00 0.00 87
2 \w -76.00 26.00 1.00 22.50 -- -42.47 19.00 -90.00 102
3 \w 73.00 174.00 1.00 65.00 -- 102.45 61.00 -60.00 101
4 \w 123.00 155.00 1.00 65.00 -- 102.45 125.00 -60.00 32
5 \w 101.00 132.00 1.00 65.00 -- 102.45 -61.00-150.00 31
6 \w 30.00 77.00 1.00 65.00 -- 102.45 -61.00-150.00 47
7 \w 74.00 160.00 1.00 65.00 -- 102.45 61.00 30.00 86
8 \w 112.00 143.00 1.00 65.00 -- 102.45 77.00 -30.00 31
9 \w 98.00 135.00 1.00 65.00 -- 102.45 125.00 -30.00 37
10 \w 138.00 164.00 1.00 65.00 -- 102.45 125.00 -30.00 26
11 \w 132.00 178.00 1.00 65.00 -- 102.45 77.00 120.00 46
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1730409000
_diffrn_orient_matrix_UB_12 0.0287689000
_diffrn_orient_matrix_UB_13 -0.0304468000
_diffrn_orient_matrix_UB_21 0.0994812000
_diffrn_orient_matrix_UB_22 0.0173632000
_diffrn_orient_matrix_UB_23 0.1505777000
_diffrn_orient_matrix_UB_31 0.1297588000
_diffrn_orient_matrix_UB_32 0.0251040000
_diffrn_orient_matrix_UB_33 -0.0690603000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3702
_reflns_number_total 4325
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_refine_diff_density_max 0.940
_refine_diff_density_min -0.336
_refine_diff_density_rms 0.086
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 353
_refine_ls_number_reflns 4325
_refine_ls_number_restraints 102
_refine_ls_R_factor_all 0.1331
_refine_ls_R_factor_gt 0.1237
_refine_ls_restrained_S_all 1.074
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+8.6783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3330
_refine_ls_wR_factor_ref 0.3397
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim N1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C3 \\sim C6 \\sim C3A \\sim C6A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C4 \\sim C5 \\sim C1A \\sim C2A \\sim C4A \\sim C5A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
Sof(H7B)=Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=
Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
Sof(H7A)=Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=
Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
C22(H22), C27(H27), C7(H7B), C7(H7A), C9(H9), C10(H10), C11(H11), C13(H13),
C14(H14), C15(H15), C16(H16), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C1A(H1A),
C2A(H2A), C4A(H4A), C5A(H5A), C6A(H6A)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N -0.1655(7) 0.38942(11) 0.6917(4) 0.0414(10) Uani 1 1 d . . . . .
N3 N -0.1692(5) 0.28007(10) 0.6873(4) 0.0291(8) Uani 1 1 d . . . . .
N4 N -0.4799(5) 0.28317(10) -0.0677(4) 0.0277(8) Uani 1 1 d . . . . .
N5 N -0.4820(8) 0.39285(11) -0.0541(4) 0.0460(11) Uani 1 1 d . . . . .
C18 C -0.2127(7) 0.37335(11) 0.5830(5) 0.0302(9) Uani 1 1 d . . . . .
C19 C -0.2154(6) 0.29570(10) 0.5783(4) 0.0212(8) Uani 1 1 d . . . . .
C20 C -0.2705(6) 0.35381(11) 0.4466(4) 0.0236(8) Uani 1 1 d . . . . .
C21 C -0.2719(5) 0.31581(10) 0.4430(4) 0.0193(8) Uani 1 1 d . . . . .
C22 C -0.3270(5) 0.29740(10) 0.3104(4) 0.0194(8) Uani 1 1 d . . . . .
H22 H -0.328818 0.272035 0.308761 0.023 Uiso 1 1 calc R U . . .
C23 C -0.3793(5) 0.31691(11) 0.1802(4) 0.0207(8) Uani 1 1 d . . . . .
C24 C -0.4354(6) 0.29811(11) 0.0428(4) 0.0213(8) Uani 1 1 d . . . . .
C25 C -0.4372(7) 0.37595(12) 0.0508(4) 0.0314(10) Uani 1 1 d . . . . .
C26 C -0.3787(6) 0.35522(11) 0.1842(4) 0.0233(8) Uani 1 1 d . . . . .
C27 C -0.3236(7) 0.37386(11) 0.3164(4) 0.0275(9) Uani 1 1 d . . . . .
H27 H -0.322065 0.399228 0.318375 0.033 Uiso 1 1 calc R U . . .
C7 C 0.2421(9) 0.40796(14) 0.4804(5) 0.0441(12) Uani 1 1 d . . . . .
H7B H 0.246187 0.422521 0.401188 0.053 Uiso 0.386(8) 1 calc R U P A 2
H7A H 0.169668 0.422119 0.401523 0.053 Uiso 0.614(8) 1 calc R U P A 1
C8 C 0.2322(6) 0.36895(12) 0.4587(4) 0.0281(9) Uani 1 1 d . . . . .
C9 C 0.2838(6) 0.34596(14) 0.5803(5) 0.0335(10) Uani 1 1 d . . . . .
H9 H 0.323030 0.356064 0.673640 0.040 Uiso 1 1 calc R U . . .
C10 C 0.2779(6) 0.30816(13) 0.5647(5) 0.0313(10) Uani 1 1 d . . . . .
H10 H 0.313504 0.293450 0.647685 0.038 Uiso 1 1 calc R U . . .
C11 C 0.2208(6) 0.29253(12) 0.4300(5) 0.0285(9) Uani 1 1 d . . . . .
H11 H 0.215370 0.267254 0.421307 0.034 Uiso 1 1 calc R U . . .
C12 C 0.1697(6) 0.31445(11) 0.3034(4) 0.0241(8) Uani 1 1 d . . . . .
C13 C 0.1117(6) 0.29794(13) 0.1631(5) 0.0315(10) Uani 1 1 d . . . . .
H13 H 0.108054 0.272644 0.155652 0.038 Uiso 1 1 calc R U . . .
C14 C 0.0613(7) 0.31844(15) 0.0394(5) 0.0371(11) Uani 1 1 d . . . . .
H14 H 0.023848 0.307224 -0.051907 0.045 Uiso 1 1 calc R U . . .
C15 C 0.0658(7) 0.35632(15) 0.0497(5) 0.0372(11) Uani 1 1 d . . . . .
H15 H 0.031103 0.370177 -0.035600 0.045 Uiso 1 1 calc R U . . .
C16 C 0.1207(7) 0.37378(13) 0.1836(4) 0.0316(10) Uani 1 1 d . . . . .
H16 H 0.122149 0.399125 0.187545 0.038 Uiso 1 1 calc R U . . .
C17 C 0.1750(6) 0.35323(12) 0.3153(4) 0.0247(9) Uani 1 1 d . . . . .
N1 N 0.369(2) 0.5411(3) 0.6736(13) 0.073(3) Uani 0.614(8) 1 d . U P A 1
C1 C 0.455(3) 0.5176(3) 0.7748(14) 0.090(4) Uani 0.614(8) 1 d . U P A 1
H1 H 0.525760 0.526408 0.866838 0.108 Uiso 0.614(8) 1 calc R U P A 1
C2 C 0.446(3) 0.4801(3) 0.7532(13) 0.089(4) Uani 0.614(8) 1 d . U P A 1
H2 H 0.507311 0.464851 0.831509 0.107 Uiso 0.614(8) 1 calc R U P A 1
C3 C 0.3468(19) 0.4644(3) 0.6169(11) 0.047(2) Uani 0.614(8) 1 d . U P A 1
C4 C 0.235(4) 0.4911(8) 0.519(4) 0.069(4) Uani 0.614(8) 1 d . U P A 1
H4 H 0.154982 0.483965 0.426876 0.083 Uiso 0.614(8) 1 calc R U P A 1
C5 C 0.243(3) 0.5265(5) 0.556(2) 0.068(4) Uani 0.614(8) 1 d . U P A 1
H5 H 0.150416 0.542043 0.493069 0.082 Uiso 0.614(8) 1 calc R U P A 1
C6 C 0.3409(19) 0.4254(3) 0.5976(12) 0.050(2) Uani 0.614(8) 1 d . U P A 1
H6 H 0.414821 0.411488 0.676654 0.059 Uiso 0.614(8) 1 calc R U P A 1
N1A N 0.235(3) 0.5407(4) 0.692(2) 0.074(4) Uani 0.386(8) 1 d . U P A 2
C1A C 0.217(4) 0.5150(4) 0.788(2) 0.090(4) Uani 0.386(8) 1 d . U P A 2
H1A H 0.189547 0.522230 0.874810 0.108 Uiso 0.386(8) 1 calc R U P A 2
C2A C 0.236(4) 0.4779(5) 0.763(2) 0.088(4) Uani 0.386(8) 1 d . U P A 2
H2A H 0.242069 0.461730 0.838820 0.106 Uiso 0.386(8) 1 calc R U P A 2
C3A C 0.248(3) 0.4644(4) 0.6358(17) 0.044(3) Uani 0.386(8) 1 d . U P A 2
C4A C 0.293(6) 0.4887(14) 0.516(6) 0.069(5) Uani 0.386(8) 1 d . U P A 2
H4A H 0.302441 0.478378 0.428504 0.083 Uiso 0.386(8) 1 calc R U P A 2
C5A C 0.318(5) 0.5252(9) 0.538(4) 0.072(5) Uani 0.386(8) 1 d . U P A 2
H5A H 0.372856 0.540470 0.480246 0.087 Uiso 0.386(8) 1 calc R U P A 2
C6A C 0.246(3) 0.4249(5) 0.6080(19) 0.043(3) Uani 0.386(8) 1 d . U P A 2
H6A H 0.247707 0.409861 0.686882 0.051 Uiso 0.386(8) 1 calc R U P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N2 0.057(3) 0.035(2) 0.028(2) -0.0068(16) 0.0041(18) 0.0042(18)
N3 0.0319(19) 0.0301(19) 0.0223(17) 0.0009(14) 0.0028(14) 0.0005(14)
N4 0.0285(17) 0.0341(19) 0.0206(17) -0.0014(14) 0.0070(13) -0.0006(14)
N5 0.069(3) 0.038(2) 0.028(2) 0.0092(17) 0.0075(19) 0.008(2)
C18 0.039(2) 0.024(2) 0.024(2) 0.0019(17) 0.0048(17) 0.0030(17)
C19 0.0217(18) 0.0221(18) 0.0207(19) -0.0002(15) 0.0075(14) -0.0009(15)
C20 0.026(2) 0.027(2) 0.0170(18) -0.0015(15) 0.0044(15) 0.0006(15)
C21 0.0140(16) 0.0260(19) 0.0180(18) 0.0000(14) 0.0046(13) -0.0001(14)
C22 0.0186(17) 0.0199(18) 0.0204(18) -0.0008(14) 0.0066(14) -0.0012(14)
C23 0.0161(17) 0.027(2) 0.0185(18) -0.0014(15) 0.0041(14) 0.0008(14)
C24 0.0169(17) 0.0282(19) 0.0186(18) 0.0010(15) 0.0049(14) -0.0001(14)
C25 0.046(3) 0.026(2) 0.021(2) 0.0002(17) 0.0083(18) 0.0032(18)
C26 0.026(2) 0.027(2) 0.0163(18) 0.0015(15) 0.0043(15) 0.0029(15)
C27 0.039(2) 0.0219(19) 0.0205(19) 0.0024(15) 0.0063(17) 0.0022(17)
C7 0.061(3) 0.035(3) 0.034(2) 0.003(2) 0.009(2) 0.001(2)
C8 0.025(2) 0.033(2) 0.026(2) -0.0039(17) 0.0062(16) -0.0014(16)
C9 0.023(2) 0.057(3) 0.0190(19) -0.0045(18) 0.0042(16) -0.0016(19)
C10 0.021(2) 0.045(3) 0.027(2) 0.0103(18) 0.0053(16) -0.0003(18)
C11 0.0194(19) 0.032(2) 0.036(2) 0.0069(17) 0.0104(16) 0.0037(16)
C12 0.0155(17) 0.032(2) 0.026(2) 0.0019(16) 0.0075(15) -0.0018(15)
C13 0.0196(19) 0.039(2) 0.037(2) -0.0114(19) 0.0103(17) -0.0058(17)
C14 0.023(2) 0.064(3) 0.024(2) -0.011(2) 0.0069(17) -0.008(2)
C15 0.029(2) 0.064(3) 0.019(2) 0.005(2) 0.0067(17) 0.002(2)
C16 0.037(2) 0.036(2) 0.022(2) 0.0044(17) 0.0083(17) 0.0016(18)
C17 0.0226(19) 0.033(2) 0.0169(18) -0.0011(15) 0.0026(15) 0.0010(16)
N1 0.098(8) 0.034(4) 0.083(6) -0.003(4) 0.017(6) -0.002(6)
C1 0.162(10) 0.041(5) 0.059(5) 0.001(4) 0.016(6) -0.007(6)
C2 0.163(10) 0.037(4) 0.057(5) -0.005(4) 0.011(6) -0.009(6)
C3 0.065(6) 0.041(4) 0.038(4) -0.001(3) 0.018(4) 0.009(5)
C4 0.086(13) 0.039(5) 0.078(5) 0.003(4) 0.017(8) 0.012(8)
C5 0.087(12) 0.042(4) 0.076(6) -0.002(4) 0.023(7) 0.016(7)
C6 0.065(6) 0.041(4) 0.040(4) 0.001(3) 0.011(5) 0.004(5)
N1A 0.089(10) 0.039(6) 0.080(8) 0.005(6) -0.001(9) -0.008(8)
C1A 0.162(11) 0.033(6) 0.057(7) -0.006(5) 0.004(8) 0.001(7)
C2A 0.160(11) 0.036(6) 0.052(6) -0.012(5) 0.003(8) 0.005(7)
C3A 0.058(7) 0.038(5) 0.040(5) 0.003(4) 0.022(5) 0.005(6)
C4A 0.091(14) 0.038(6) 0.078(6) -0.001(5) 0.020(9) 0.014(9)
C5A 0.091(14) 0.041(6) 0.080(7) -0.003(6) 0.017(9) 0.012(9)
C6A 0.059(7) 0.038(5) 0.034(5) -0.001(4) 0.017(6) 0.005(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C18 1.155(6) . ?
N3 C19 1.149(5) . ?
N4 C24 1.148(5) . ?
N5 C25 1.141(6) . ?
C18 C20 1.437(5) . ?
C19 C21 1.439(5) . ?
C20 C21 1.393(5) . ?
C20 C27 1.398(5) . ?
C21 C22 1.387(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.388(5) . ?
C23 C24 1.432(5) . ?
C23 C26 1.405(5) . ?
C25 C26 1.437(5) . ?
C26 C27 1.388(5) . ?
C27 H27 0.9300 . ?
C7 H7B 0.9300 . ?
C7 H7A 0.9300 . ?
C7 C8 1.444(6) . ?
C7 C6 1.296(12) . ?
C7 C6A 1.358(17) . ?
C8 C9 1.394(6) . ?
C8 C17 1.431(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.393(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.358(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.408(6) . ?
C12 C13 1.417(6) . ?
C12 C17 1.426(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.357(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.381(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.419(5) . ?
N1 C1 1.300(16) . ?
N1 C5 1.31(2) . ?
C1 H1 0.9300 . ?
C1 C2 1.390(15) . ?
C2 H2 0.9300 . ?
C2 C3 1.404(15) . ?
C3 C4 1.41(3) . ?
C3 C6 1.440(14) . ?
C4 H4 0.9300 . ?
C4 C5 1.34(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N1A C1A 1.34(3) . ?
N1A C5A 1.80(4) . ?
C1A H1A 0.9300 . ?
C1A C2A 1.40(2) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.33(2) . ?
C3A C4A 1.55(6) . ?
C3A C6A 1.47(2) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.36(4) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C18 C20 179.1(5) . . ?
N3 C19 C21 179.0(4) . . ?
C21 C20 C18 121.2(3) . . ?
C21 C20 C27 120.4(3) . . ?
C27 C20 C18 118.4(4) . . ?
C20 C21 C19 119.5(3) . . ?
C22 C21 C19 120.0(3) . . ?
C22 C21 C20 120.5(3) . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.8(3) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 C26 119.6(3) . . ?
C26 C23 C24 120.2(3) . . ?
N4 C24 C23 179.7(5) . . ?
N5 C25 C26 179.0(5) . . ?
C23 C26 C25 120.5(3) . . ?
C27 C26 C23 121.0(3) . . ?
C27 C26 C25 118.5(4) . . ?
C20 C27 H27 120.6 . . ?
C26 C27 C20 118.8(4) . . ?
C26 C27 H27 120.6 . . ?
C8 C7 H7B 117.6 . . ?
C8 C7 H7A 116.4 . . ?
C6 C7 H7A 116.4 . . ?
C6 C7 C8 127.2(7) . . ?
C6A C7 H7B 117.6 . . ?
C6A C7 C8 124.8(9) . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 C17 119.0(4) . . ?
C17 C8 C7 121.6(4) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.4(4) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 C17 120.4(4) . . ?
C13 C12 C17 119.7(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.5(4) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.3(4) . . ?
C17 C16 H16 119.8 . . ?
C12 C17 C8 118.1(4) . . ?
C16 C17 C8 124.2(4) . . ?
C16 C17 C12 117.7(4) . . ?
C1 N1 C5 113.9(12) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.7(12) . . ?
C2 C1 H1 118.2 . . ?
C1 C2 H2 119.0 . . ?
C1 C2 C3 122.1(11) . . ?
C3 C2 H2 119.0 . . ?
C2 C3 C4 110.6(17) . . ?
C2 C3 C6 120.8(9) . . ?
C4 C3 C6 127.8(17) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121(2) . . ?
C5 C4 H4 119.3 . . ?
N1 C5 C4 125.9(16) . . ?
N1 C5 H5 117.0 . . ?
C4 C5 H5 117.0 . . ?
C7 C6 C3 126.1(9) . . ?
C7 C6 H6 116.9 . . ?
C3 C6 H6 116.9 . . ?
C1A N1A C5A 116.3(18) . . ?
N1A C1A H1A 118.9 . . ?
N1A C1A C2A 122(2) . . ?
C2A C1A H1A 118.9 . . ?
C1A C2A H2A 118.1 . . ?
C3A C2A C1A 123.8(19) . . ?
C3A C2A H2A 118.1 . . ?
C2A C3A C4A 122(2) . . ?
C2A C3A C6A 122.2(15) . . ?
C6A C3A C4A 115(2) . . ?
C3A C4A H4A 120.2 . . ?
C5A C4A C3A 120(4) . . ?
C5A C4A H4A 120.2 . . ?
N1A C5A H5A 123.7 . . ?
C4A C5A N1A 113(3) . . ?
C4A C5A H5A 123.7 . . ?
C7 C6A C3A 127.6(14) . . ?
C7 C6A H6A 116.2 . . ?
C3A C6A H6A 116.2 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C20 C21 C19 0.3(6) . . . . ?
C18 C20 C21 C22 -179.6(4) . . . . ?
C18 C20 C27 C26 179.7(4) . . . . ?
C19 C21 C22 C23 -179.3(3) . . . . ?
C20 C21 C22 C23 0.6(5) . . . . ?
C21 C20 C27 C26 0.4(6) . . . . ?
C21 C22 C23 C24 179.7(3) . . . . ?
C21 C22 C23 C26 -0.9(5) . . . . ?
C22 C23 C26 C25 -178.5(4) . . . . ?
C22 C23 C26 C27 0.9(6) . . . . ?
C23 C26 C27 C20 -0.7(6) . . . . ?
C24 C23 C26 C25 1.0(6) . . . . ?
C24 C23 C26 C27 -179.6(4) . . . . ?
C25 C26 C27 C20 178.7(4) . . . . ?
C27 C20 C21 C19 179.6(4) . . . . ?
C27 C20 C21 C22 -0.3(6) . . . . ?
C7 C8 C9 C10 -179.6(4) . . . . ?
C7 C8 C17 C12 179.8(4) . . . . ?
C7 C8 C17 C16 -1.0(7) . . . . ?
C8 C7 C6 C3 -179.4(9) . . . . ?
C8 C7 C6A C3A -177.4(13) . . . . ?
C8 C9 C10 C11 -0.2(6) . . . . ?
C9 C8 C17 C12 1.2(6) . . . . ?
C9 C8 C17 C16 -179.6(4) . . . . ?
C9 C10 C11 C12 1.0(6) . . . . ?
C10 C11 C12 C13 179.6(4) . . . . ?
C10 C11 C12 C17 -0.8(6) . . . . ?
C11 C12 C13 C14 179.8(4) . . . . ?
C11 C12 C17 C8 -0.4(6) . . . . ?
C11 C12 C17 C16 -179.6(4) . . . . ?
C12 C13 C14 C15 -0.2(6) . . . . ?
C13 C12 C17 C8 179.3(4) . . . . ?
C13 C12 C17 C16 0.0(6) . . . . ?
C13 C14 C15 C16 0.0(7) . . . . ?
C14 C15 C16 C17 0.2(7) . . . . ?
C15 C16 C17 C8 -179.5(4) . . . . ?
C15 C16 C17 C12 -0.2(6) . . . . ?
C17 C8 C9 C10 -0.9(6) . . . . ?
C17 C12 C13 C14 0.1(6) . . . . ?
N1 C1 C2 C3 2(3) . . . . ?
C1 N1 C5 C4 -17(2) . . . . ?
C1 C2 C3 C4 -9(2) . . . . ?
C1 C2 C3 C6 179.7(15) . . . . ?
C2 C3 C4 C5 4(3) . . . . ?
C2 C3 C6 C7 174.8(13) . . . . ?
C3 C4 C5 N1 9(3) . . . . ?
C4 C3 C6 C7 6(2) . . . . ?
C5 N1 C1 C2 11(3) . . . . ?
C6 C7 C8 C9 18.3(10) . . . . ?
C6 C7 C8 C17 -160.2(8) . . . . ?
C6 C3 C4 C5 174.4(14) . . . . ?
N1A C1A C2A C3A -9(4) . . . . ?
C1A N1A C5A C4A 18(3) . . . . ?
C1A C2A C3A C4A 15(4) . . . . ?
C1A C2A C3A C6A -173(2) . . . . ?
C2A C3A C4A C5A -1(4) . . . . ?
C2A C3A C6A C7 175(2) . . . . ?
C3A C4A C5A N1A -14(3) . . . . ?
C4A C3A C6A C7 -13(3) . . . . ?
C5A N1A C1A C2A -7(3) . . . . ?
C6A C7 C8 C9 -17.9(12) . . . . ?
C6A C7 C8 C17 163.5(10) . . . . ?
C6A C3A C4A C5A -173(2) . . . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 62.2 27.4 ?
2 0.000 0.500 1.000 62.2 27.4 ?
_smtbx_masks_void_probe_radius 1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_file
;
TITL cy_d1_a.res in P2(1)/c
cy_d1.res
created by SHELXL-2018/3 at 10:51:45 on 28-Jun-2022
REM Old TITL CY_D1 in P21/m #11
REM SHELXT solution in P2(1)/c: R1 0.266, Rweak 0.039, Alpha 0.147
REM 4.369 for 89 systematic absences, Orientation as input
REM Formula found by SHELXT: C23 N7
CELL 1.54184 6.7312 36.6599 9.515 90 106.283 90
ZERR 4 0.0003 0.0013 0.0004 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N
UNIT 108 60 20
SIMU 0.01 0.02 2 N1 N1a
SIMU 0.01 0.02 2 C3 C6 C3a C6a
SIMU 0.01 0.02 2 C1 C2 C4 C5 C1a C2a C4a C5a
L.S. 10
PLAN 5
CONF
BOND
list 4
MORE -1
BOND $H
ABIN
fmap 2
acta
OMIT -1 1 2
OMIT 0 1 8
OMIT -2 3 2
OMIT 0 1 1
REM
REM
REM
WGHT 0.131600 8.678301
FVAR 0.34192 0.61367
N2 3 -0.165539 0.389417 0.691749 11.00000 0.05662 0.03518 =
0.02778 -0.00675 0.00414 0.00415
N3 3 -0.169231 0.280072 0.687315 11.00000 0.03192 0.03007 =
0.02235 0.00085 0.00277 0.00051
N4 3 -0.479866 0.283169 -0.067667 11.00000 0.02849 0.03408 =
0.02056 -0.00140 0.00700 -0.00065
N5 3 -0.482019 0.392848 -0.054127 11.00000 0.06872 0.03763 =
0.02808 0.00918 0.00749 0.00826
C18 1 -0.212740 0.373346 0.583041 11.00000 0.03926 0.02441 =
0.02437 0.00192 0.00483 0.00301
C19 1 -0.215434 0.295698 0.578283 11.00000 0.02174 0.02209 =
0.02075 -0.00019 0.00751 -0.00085
C20 1 -0.270526 0.353812 0.446632 11.00000 0.02572 0.02703 =
0.01696 -0.00148 0.00440 0.00061
C21 1 -0.271906 0.315813 0.443048 11.00000 0.01404 0.02599 =
0.01803 0.00002 0.00461 -0.00010
C22 1 -0.326962 0.297399 0.310437 11.00000 0.01862 0.01994 =
0.02037 -0.00077 0.00664 -0.00120
AFIX 43
H22 2 -0.328818 0.272035 0.308761 11.00000 -1.20000
AFIX 0
C23 1 -0.379284 0.316911 0.180232 11.00000 0.01613 0.02714 =
0.01845 -0.00142 0.00415 0.00077
C24 1 -0.435375 0.298112 0.042804 11.00000 0.01695 0.02820 =
0.01865 0.00104 0.00492 -0.00005
C25 1 -0.437209 0.375949 0.050751 11.00000 0.04611 0.02647 =
0.02082 0.00017 0.00826 0.00324
C26 1 -0.378675 0.355217 0.184168 11.00000 0.02592 0.02652 =
0.01634 0.00153 0.00429 0.00287
C27 1 -0.323616 0.373865 0.316414 11.00000 0.03877 0.02192 =
0.02050 0.00237 0.00631 0.00221
AFIX 43
H27 2 -0.322065 0.399228 0.318375 11.00000 -1.20000
AFIX 0
C7 1 0.242118 0.407963 0.480376 11.00000 0.06056 0.03511 =
0.03405 0.00281 0.00892 0.00137
PART 2
AFIX 43
H7B 2 0.246187 0.422521 0.401188 -21.00000 -1.20000
AFIX 43
PART 1
H7A 2 0.169668 0.422119 0.401523 21.00000 -1.20000
AFIX 0
PART 0
C8 1 0.232189 0.368954 0.458733 11.00000 0.02549 0.03259 =
0.02559 -0.00395 0.00618 -0.00143
C9 1 0.283818 0.345958 0.580258 11.00000 0.02333 0.05711 =
0.01900 -0.00454 0.00417 -0.00158
AFIX 43
H9 2 0.323030 0.356064 0.673640 11.00000 -1.20000
AFIX 0
C10 1 0.277903 0.308158 0.564745 11.00000 0.02128 0.04460 =
0.02720 0.01028 0.00533 -0.00030
AFIX 43
H10 2 0.313504 0.293450 0.647685 11.00000 -1.20000
AFIX 0
C11 1 0.220792 0.292527 0.430007 11.00000 0.01940 0.03172 =
0.03602 0.00694 0.01045 0.00373
AFIX 43
H11 2 0.215370 0.267254 0.421307 11.00000 -1.20000
AFIX 0
C12 1 0.169729 0.314447 0.303360 11.00000 0.01554 0.03209 =
0.02568 0.00185 0.00748 -0.00179
C13 1 0.111676 0.297944 0.163073 11.00000 0.01955 0.03937 =
0.03700 -0.01142 0.01026 -0.00584
AFIX 43
H13 2 0.108054 0.272644 0.155652 11.00000 -1.20000
AFIX 0
C14 1 0.061294 0.318444 0.039413 11.00000 0.02335 0.06371 =
0.02432 -0.01115 0.00688 -0.00850
AFIX 43
H14 2 0.023848 0.307224 -0.051907 11.00000 -1.20000
AFIX 0
C15 1 0.065834 0.356315 0.049677 11.00000 0.02870 0.06420 =
0.01884 0.00481 0.00674 0.00226
AFIX 43
H15 2 0.031103 0.370177 -0.035600 11.00000 -1.20000
AFIX 0
C16 1 0.120739 0.373776 0.183608 11.00000 0.03721 0.03572 =
0.02200 0.00437 0.00833 0.00161
AFIX 43
H16 2 0.122149 0.399125 0.187545 11.00000 -1.20000
AFIX 0
C17 1 0.175031 0.353234 0.315292 11.00000 0.02259 0.03288 =
0.01695 -0.00109 0.00257 0.00097
PART 1
N1 3 0.369018 0.541105 0.673621 21.00000 0.09797 0.03362 =
0.08306 -0.00324 0.01707 -0.00179
C1 1 0.454610 0.517611 0.774815 21.00000 0.16180 0.04120 =
0.05851 0.00058 0.01580 -0.00743
AFIX 43
H1 2 0.525760 0.526408 0.866838 21.00000 -1.20000
AFIX 0
C2 1 0.445764 0.480068 0.753203 21.00000 0.16251 0.03650 =
0.05703 -0.00488 0.01136 -0.00913
AFIX 43
H2 2 0.507311 0.464851 0.831509 21.00000 -1.20000
AFIX 0
C3 1 0.346840 0.464410 0.616883 21.00000 0.06478 0.04061 =
0.03846 -0.00073 0.01788 0.00882
C4 1 0.235411 0.491083 0.519106 21.00000 0.08638 0.03919 =
0.07822 0.00343 0.01660 0.01238
AFIX 43
H4 2 0.154982 0.483965 0.426876 21.00000 -1.20000
AFIX 0
C5 1 0.242911 0.526467 0.556215 21.00000 0.08718 0.04175 =
0.07644 -0.00158 0.02310 0.01633
AFIX 43
H5 2 0.150416 0.542043 0.493069 21.00000 -1.20000
AFIX 0
C6 1 0.340890 0.425436 0.597610 21.00000 0.06540 0.04107 =
0.04016 0.00116 0.01144 0.00402
AFIX 43
H6 2 0.414821 0.411488 0.676654 21.00000 -1.20000
AFIX 0
PART 2
N1A 3 0.235241 0.540664 0.692339 -21.00000 0.08895 0.03934 =
0.08001 0.00468 -0.00102 -0.00833
C1A 1 0.216592 0.515041 0.788257 -21.00000 0.16230 0.03336 =
0.05688 -0.00635 0.00373 0.00118
AFIX 43
H1A 2 0.189547 0.522230 0.874810 -21.00000 -1.20000
AFIX 0
C2A 1 0.236412 0.477926 0.762567 -21.00000 0.16039 0.03625 =
0.05194 -0.01242 0.00322 0.00465
AFIX 43
H2A 2 0.242069 0.461730 0.838820 -21.00000 -1.20000
AFIX 0
C3A 1 0.247642 0.464413 0.635846 -21.00000 0.05806 0.03786 =
0.03998 0.00302 0.02224 0.00476
C4A 1 0.292835 0.488692 0.515658 -21.00000 0.09052 0.03802 =
0.07771 -0.00143 0.02034 0.01437
AFIX 43
H4A 2 0.302441 0.478378 0.428504 -21.00000 -1.20000
AFIX 0
C5A 1 0.318426 0.525163 0.538070 -21.00000 0.09102 0.04137 =
0.08027 -0.00315 0.01736 0.01156
AFIX 43
H5A 2 0.372856 0.540470 0.480246 -21.00000 -1.20000
AFIX 0
C6A 1 0.245949 0.424948 0.607965 -21.00000 0.05908 0.03766 =
0.03395 -0.00054 0.01716 0.00539
AFIX 43
H6A 2 0.247707 0.409861 0.686882 -21.00000 -1.20000
AFIX 0
HKLF 4
REM cy_d1_a.res in P2(1)/c
REM wR2 = 0.3397, GooF = S = 1.085, Restrained GooF = 1.074 for all data
REM R1 = 0.1237 for 3702 Fo > 4sig(Fo) and 0.1331 for all 4325 data
REM 353 parameters refined using 102 restraints
END
WGHT 0.1316 8.6800
REM Highest difference peak 0.940, deepest hole -0.336, 1-sigma level 0.086
Q1 1 0.1043 0.4136 0.1516 11.00000 0.05 0.94
Q2 1 -0.0457 0.5342 0.8163 11.00000 0.05 0.65
Q3 1 0.1107 0.5253 0.9387 11.00000 0.05 0.63
Q4 1 0.6606 0.5203 0.8811 11.00000 0.05 0.60
Q5 1 0.0384 0.5126 0.8568 11.00000 0.05 0.54
;
_shelx_res_checksum 25644
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2 6 4 0.4498 0.0001
2 6 5 1.2220 0.0030
2 6 6 2.3162 0.0004
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2 7 6 -2.1321 -0.0074
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2 8 2 -3.7625 -0.0043
2 8 3 -1.1944 0.0069
2 8 4 0.4114 0.0045
2 8 5 0.8689 0.0061
2 8 6 1.7366 0.0046
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2 10 3 -1.0986 0.0003
2 10 4 0.9521 0.0053
2 10 5 0.4394 0.0024
2 10 6 1.3752 0.0061
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2 11 0 -2.8716 -0.0005
2 11 1 1.9229 0.0015
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2 12 3 -0.4852 -0.0057
2 12 4 1.4619 0.0020
2 12 5 0.2491 -0.0019
2 12 6 1.1436 0.0038
2 12 7 1.4317 0.0001
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2 12 9 -0.2973 0.0009
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2 14 3 0.6788 -0.0061
2 14 4 1.3044 -0.0027
2 14 5 0.3572 -0.0025
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2 16 5 0.5092 -0.0001
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2 18 0 -0.3814 -0.0006
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2 21 6 0.9241 0.0010
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2 22 0 1.0905 0.0000
2 22 1 2.5594 -0.0010
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2 23 3 1.9576 -0.0021
2 23 4 -0.9288 0.0013
2 23 5 1.5602 -0.0030
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2 24 3 1.7345 -0.0010
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2 25 4 -0.9301 0.0028
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3 1 8 -0.0885 -0.0170
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3 2 8 -0.1704 0.0083
3 2 9 0.1963 0.0140
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3 3 1 1.4980 -0.0119
3 3 2 2.4774 0.0039
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3 3 4 0.5619 0.0110
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3 3 7 0.2945 -0.0047
3 3 8 -0.1905 -0.0105
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3 5 3 -0.8534 0.0050
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6 2 2 -1.1003 0.0075
6 2 3 -0.6098 -0.0056
6 2 4 0.0012 -0.0028
6 2 5 0.1177 0.0012
6 3 0 0.9242 -0.0046
6 3 1 1.0209 -0.0018
6 3 2 1.1680 0.0047
6 3 3 0.6571 -0.0003
6 3 4 0.3367 0.0016
6 3 5 -0.2820 0.0066
6 4 0 -0.3765 -0.0080
6 4 1 -1.2917 0.0033
6 4 2 -1.2567 0.0024
6 4 3 -1.0319 -0.0058
6 4 4 -0.0016 -0.0055
6 4 5 0.1504 0.0012
6 5 0 0.8295 -0.0094
6 5 1 1.2976 0.0011
6 5 2 1.4362 0.0038
6 5 3 0.7445 0.0015
6 5 4 0.5404 0.0005
6 5 5 -0.2792 0.0058
6 6 0 -0.5793 -0.0035
6 6 1 -1.1479 0.0038
6 6 2 -1.4337 -0.0004
6 6 3 -1.2266 -0.0032
6 6 4 -0.0757 -0.0024
6 6 5 0.0480 0.0022
6 7 0 0.3336 -0.0082
6 7 1 1.4481 0.0017
6 7 2 1.3672 0.0018
6 7 3 0.8602 -0.0007
6 7 4 0.7454 -0.0026
6 7 5 -0.2067 0.0001
6 8 0 -0.5471 0.0009
6 8 1 -0.8161 0.0018
6 8 2 -1.4641 0.0000
6 8 3 -1.3026 0.0012
6 8 4 -0.2043 0.0034
6 8 5 -0.1732 0.0039
6 9 0 -0.0432 -0.0025
6 9 1 1.2587 0.0007
6 9 2 1.2655 -0.0005
6 9 3 0.8872 -0.0044
6 9 4 0.9525 -0.0055
6 9 5 -0.0954 -0.0048
6 10 0 -0.1878 0.0028
6 10 1 -0.7211 -0.0006
6 10 2 -1.1925 0.0018
6 10 3 -1.3744 0.0044
6 10 4 -0.3011 0.0068
6 10 5 -0.4228 0.0044
6 11 0 0.0431 0.0026
6 11 1 0.6934 -0.0003
6 11 2 1.3235 -0.0018
6 11 3 0.7283 -0.0061
6 11 4 1.1016 -0.0054
6 12 0 0.3561 0.0018
6 12 1 -0.9577 -0.0013
6 12 2 -0.6473 0.0025
6 12 3 -1.4287 0.0039
6 12 4 -0.3144 0.0056
6 13 0 0.4809 0.0031
6 13 1 -0.0085 0.0001
6 13 2 1.4480 -0.0016
6 13 3 0.4370 -0.0044
6 13 4 1.0924 -0.0014
6 14 0 0.7645 -0.0007
6 14 1 -1.2352 0.0002
6 14 2 -0.0811 0.0010
6 14 3 -1.3401 -0.0001
6 14 4 -0.2938 0.0018
6 15 0 0.8529 -0.0003
6 15 1 -0.4739 0.0016
6 15 2 1.3788 -0.0001
6 15 3 0.1968 -0.0010
6 15 4 0.8710 0.0042
6 16 0 0.7842 -0.0026
6 16 1 -1.1780 0.0021
6 16 2 0.2140 -0.0012
6 16 3 -1.0187 -0.0049
6 16 4 -0.3265 -0.0008
6 17 0 0.8245 -0.0038
6 17 1 -0.4953 0.0027
6 17 2 0.9652 0.0017
6 17 3 0.1458 0.0013
6 17 4 0.5062 0.0078
6 18 0 0.4561 -0.0023
6 18 1 -0.6750 0.0025
6 18 2 0.1599 -0.0025
6 18 3 -0.5381 -0.0071
6 19 0 0.4011 -0.0042
6 19 1 -0.2057 0.0021
6 19 2 0.3322 0.0027
6 19 3 0.2384 0.0018
6 20 0 0.0883 -0.0003
6 20 1 0.0275 0.0011
6 20 2 -0.0518 -0.0023
6 20 3 -0.1105 -0.0059
6 21 0 -0.1242 -0.0018
6 21 1 0.0561 0.0006
6 21 2 -0.2059 0.0026
6 21 3 0.3025 0.0016
6 22 0 -0.0198 0.0015
6 22 1 0.5329 -0.0007
6 22 2 -0.1601 -0.0015
6 23 0 -0.4246 0.0007
6 23 1 0.0603 -0.0003
6 23 2 -0.3910 0.0017
6 24 0 0.1640 0.0013
6 24 1 0.5926 -0.0015
6 24 2 -0.0770 -0.0013
6 25 0 -0.3624 0.0014
6 25 1 -0.1366 0.0002
6 26 0 0.4137 -0.0007
6 26 1 0.2587 -0.0012
6 27 0 -0.0425 0.0006
6 27 1 -0.3073 0.0013
6 28 0 0.4925 -0.0025
6 28 1 -0.1912 -0.0003
6 29 0 0.2912 -0.0003
7 0 0 -0.8054 0.0044
7 0 2 0.2839 -0.0027
7 1 0 0.2525 -0.0023
7 1 1 0.1727 -0.0031
7 1 2 0.2400 0.0029
7 2 0 -0.7083 0.0027
7 2 1 -0.5235 -0.0001
7 2 2 0.3370 -0.0038
7 3 0 0.6060 -0.0046
7 3 1 0.0883 -0.0019
7 3 2 0.6367 0.0037
7 4 0 -0.5055 0.0016
7 4 1 -0.8128 -0.0007
7 4 2 0.4093 -0.0026
7 5 0 0.6284 -0.0049
7 5 1 0.0533 -0.0015
7 5 2 0.8252 0.0035
7 6 0 -0.3593 0.0017
7 6 1 -0.7967 -0.0013
7 6 2 0.3411 0.0007
7 7 0 0.4089 -0.0021
7 7 1 0.1661 -0.0022
7 7 2 0.7873 0.0019
7 8 0 -0.3202 0.0022
7 8 1 -0.6093 -0.0018
7 8 2 0.0864 0.0039
7 9 0 0.2263 0.0021
7 9 1 0.3556 -0.0030
7 9 2 0.6197 -0.0004
7 10 0 -0.2795 0.0023
7 10 1 -0.4783 -0.0018
7 10 2 -0.2254 0.0051
7 11 0 0.3121 0.0043
7 11 1 0.4443 -0.0028
7 11 2 0.4673 -0.0016
7 12 0 -0.1135 0.0012
7 12 1 -0.5397 -0.0012
7 12 2 -0.4154 0.0037
7 13 0 0.6505 0.0031
7 13 1 0.3363 -0.0011
7 13 2 0.4178 -0.0006
7 14 0 0.1589 -0.0009
7 14 1 -0.7266 -0.0006
7 14 2 -0.4227 0.0009
7 15 0 0.9834 -0.0002
7 15 1 0.1163 0.0014
7 15 2 0.4390 0.0021
7 16 0 0.3870 -0.0030
7 16 1 -0.8268 -0.0005
7 17 0 1.0157 -0.0028
7 17 1 -0.0433 0.0032
7 18 0 0.4452 -0.0037
7 18 1 -0.6677 -0.0009
7 19 0 0.6555 -0.0029
7 20 0 0.3486 -0.0028
0 0 0 0.0 0.0
;
_shelx_fab_checksum 21743
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.399
_oxdiff_exptl_absorpt_empirical_full_min 0.802