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_1570005
_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
'C48 H34 N2 O4 S2 Zn, 2(H2 O), [+ solvents]0.167[]'
_chemical_formula_sum            'C48 H38 N2 O6 S2 Zn'
_chemical_formula_weight         868.29
_space_group_crystal_system      hexagonal
_space_group_IT_number           181
_space_group_name_Hall           'P 64 2 (0 0 2)'
_space_group_name_H-M_alt        'P 64 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-04-14
_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                120
_cell_formula_units_Z            6
_cell_length_a                   15.4656(4)
_cell_length_b                   15.4656(4)
_cell_length_c                   45.0635(14)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    90.00
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      2.36
_cell_volume                     9334.5(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            222145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         1.586
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2117 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.9078.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.927
_exptl_crystal_description       prism
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.269(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         9557
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+1.9226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7354
_reflns_number_total             9557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5044.cif
_cod_data_source_block           dte-18
_cod_original_cell_volume        9334.5(5)
_cod_original_sg_symbol_Hall     'P 64 2c (0 0 -1)'
_cod_database_code               1570005
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.731(16)
 0.269(16)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(O3) \\sim Ueq, : with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Sof(O3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(O3)=Sof(H3A)=Sof(H3B)=FVAR(1)
5.a Free rotating group:
 O3(H3A,H3B), O3A(H3AA,H3AB)
5.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), C19(H19), C20(H20), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              70224
_shelx_hkl_checksum              89399
_shelx_fab_checksum              95720
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'