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_1569997
_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         'C68 H56 Cd N4 O2 S4, 2(N O3)'
_chemical_formula_sum            'C68 H56 Cd N6 O8 S4'
_chemical_formula_weight         1325.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8116(12)
_cell_length_b                   21.432(3)
_cell_length_c                   69.162(8)
_cell_measurement_reflns_used    9035
_cell_measurement_temperature    90.00
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.24
_cell_volume                     14544(3)
_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    'SHELXS  (Sheldrick, 2008)'
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       92
_diffrn_reflns_limit_l_min       -92
_diffrn_reflns_number            66341
_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         28.331
_diffrn_reflns_theta_min         1.990
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1205 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.9130.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       prism
_exptl_crystal_F_000             5456
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0927
_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^)+(0.0494P)^2^+496.5558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4453
_reflns_number_total             4548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5044.cif
_cod_data_source_block           dte-10
_cod_original_cell_volume        14543(3)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1569997
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.937
_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, All O(H,H) groups
2. Restrained distances
 N2-O2 = N2-O4
 1.25 with sigma of 0.02
 N2-O3
 1.24 with sigma of 0.02
 N2-O2 \\sim N2-O3 \\sim N2-O4
 with sigma of 0.02
 O2-O3 \\sim O3-O4 \\sim O4-O2
 with sigma of 0.04
 Cd1-H1A \\sim Cd1-H1B
 with sigma of 0.02
3. Restrained planarity
 O2, O3, O4, N2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O4 \\sim N2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O2, O3, O4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) O2(0.5) O3(0.5) O4(0.5) N2(0.5)
7.a Free rotating group:
 O1(H1A,H1B)
7.b 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)
7.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              11797
_shelx_hkl_checksum              41334
_shelx_fab_checksum              19755
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'