Development of a scalar-based geometric parameterization approach for the crystal structure landscape of dithienylethene-based crystalline solids.
Mitchell, Travis B.; Zhang, Xiaotong; Jerozal, Ronald T.; Chen, Yu Sheng; Wang, SuYin; Benedict, Jason B.; IUCrJ 10 (2023) –; doi:10.1107/S2052252523008060

data_1569999
_publ_section_title
;
 Development of a scalar-based geometric parameterization approach for the
 crystal structure landscape of dithienylethene-based crystalline solids.
;
_journal_coeditor_code           YC5044
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252523008060
_journal_volume                  10
_journal_year                    2023
_chemical_formula_moiety         '2(Br), C68 H52 Cu N4 S4, 2(C3 H7 N O)'
_chemical_formula_sum            'C74 H66 Br2 Cu N6 O2 S4'
_chemical_formula_weight         1422.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                105.0120(10)
_cell_angle_beta                 98.4520(10)
_cell_angle_gamma                99.1780(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5108(3)
_cell_length_b                   11.4444(3)
_cell_length_c                   16.0164(4)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    90.00
_cell_measurement_theta_max      32.64
_cell_measurement_theta_min      2.21
_cell_volume                     1629.52(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44606
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.203
_diffrn_reflns_theta_min         1.343
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0610 before and 0.0371 after correction.
The Ratio of minimum to maximum transmission is 0.9672.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             731
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         12487
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+1.0289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10164
_reflns_number_total             12487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5044.cif
_cod_data_source_block           dte-12
_cod_database_code               1569999
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-O1
 1.22 with sigma of 0.02
 C35-N3
 1.36 with sigma of 0.02
 N3-C36
 1.45 with sigma of 0.02
 N3-C37
 1.46 with sigma of 0.02
 C35A-O1A
 1.22 with sigma of 0.02
 C35A-N3A
 1.36 with sigma of 0.02
 N3A-C37A
 1.45 with sigma of 0.02
 N3A-C36A
 1.46 with sigma of 0.02
 C35-C36
 2.46 with sigma of 0.04
 C35A-C37A
 2.46 with sigma of 0.04
 C35-C37
 2.45 with sigma of 0.04
 C35A-C36A
 2.45 with sigma of 0.04
 N3-C36 \\sim N3-C37
 with sigma of 0.02
 N3A-C37A \\sim N3A-C36A
 with sigma of 0.02
3. Restrained planarity
 O1, N3, C35, C36, C37
 with sigma of 0.1
 O1A, N3A, C35A, C36A, C37A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim N3 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1A \\sim N3A \\sim C35A \\sim C36A \\sim C37A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O1, N3, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, N3A, C35A, C36A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O1A(0.5) N3A(0.5) C35A(0.5) H35A(0.5) C36A(0.5) H36d(0.5)
 H36f(0.5) H36e(0.5) C37A(0.5) H37d(0.5) H37e(0.5) H37f(0.5) O1(0.5) N3(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36a(0.5) H36b(0.5) H36c(0.5) C37(0.5) H37a(0.5)
 H37b(0.5) H37c(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C31(H31),
  C32(H32), C33(H33), C34(H34), C35A(H35A), C35(H35)
7.b Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C29(H29a,H29b,H29c), C36A(H36d,H36f,H36e), C37A(H37d,
 H37e,H37f), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c)
;
_shelx_res_checksum              81126
_shelx_hkl_checksum              25349
_olex2_submission_special_instructions 'No special instructions were received'