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_1569991
_publ_section_title
;
 Development of a scalar-based geometric parameterization approach for the
 crystal structure landscape of dithienylethene-based crystalline solids.
;
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252523008060
_journal_volume                  10
_journal_year                    2023
_chemical_formula_moiety         '4(C34 H27.5 N2 S2), 7(C7 H5 O4)'
_chemical_formula_sum            'C185 H145 N8 O28 S8'
_chemical_formula_weight         3184.56
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                71.454(6)
_cell_angle_beta                 88.132(6)
_cell_angle_gamma                78.607(6)
_cell_formula_units_Z            1
_cell_length_a                   10.602(2)
_cell_length_b                   16.714(4)
_cell_length_c                   24.181(5)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    90.00
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.17
_cell_volume                     3980.2(15)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.00
_diffrn_measured_fraction_theta_full 0.999
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.311
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1544 before and 0.0733 after correction.
The Ratio of minimum to maximum transmission is 0.7627.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             1663
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1176
_refine_ls_number_reflns         13567
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0813P)^2^+15.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9836
_reflns_number_total             13567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5044.cif
_cod_data_source_block           dte-4
_cod_original_cell_volume        3980.4(14)
_cod_database_code               1569991
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C96-C95
 1.4 with sigma of 0.02
 C96-O16
 1.35 with sigma of 0.02
 O11-H11 = O12-H12 = O8-H8 = O7-H7B = O4-H4C = O3-H3C = O16-H16A
 0.84 with sigma of 0.02
 N4-H4B = N3-H3B = N2-H2 = N1-H1
 0.88 with sigma of 0.02
 C94-C93 = C92-O15
 1.37 with sigma of 0.02
 C96-C91
 1.43 with sigma of 0.02
 O15-H15A
 0.84 with sigma of 0.02
 C95-C94 = C92-C91
 1.39 with sigma of 0.02
 C93-C92
 1.41 with sigma of 0.02
 C91-C90
 1.45 with sigma of 0.02
 C90-O14
 1.27 with sigma of 0.02
 C90-O13
 1.31 with sigma of 0.02
 C91-O13
 2.36 with sigma of 0.04
 C95-C93
 2.43 with sigma of 0.04
 C93-O15
 2.37 with sigma of 0.04
 C96-C92
 2.41 with sigma of 0.04
 C93-C91
 2.45 with sigma of 0.04
 C96-C90 = C92-C90
 2.49 with sigma of 0.04
 C94-C92 = C91-O14
 2.38 with sigma of 0.04
 C96-C94
 2.39 with sigma of 0.04
3. Restrained planarity
 O13, O14, O15, O16, C90, C91, C92, C93, C94, C95, C96
 with sigma of 0.1
4. Rigid bond restraints
 C2, C3, C4, C5, C6, C7, C2A, C3A, C4A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C2A \\sim C3A \\sim C4A
\\sim C5A \\sim C6A \\sim C7A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
6. Rigid body (RIGU) restrains
 O13, O14, O15, O16, C90, C91, C92, C93, C94, C95, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7)=FVAR(1)
 Fixed Sof: H67(0.5) H15A(0.5) H16A(0.5) O13(0.5) O14(0.5) O15(0.5) H1(0.5)
 O16(0.5) C90(0.5) C91(0.5) C92(0.5) C93(0.5) H93(0.5) C94(0.5) H94(0.5)
 C95(0.5) H95(0.5) C96(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 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), C3(H3),
 C4(H4), C5(H5), C6(H6), C7(H7), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
 C7A(H7A), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C48(H48),
  C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C60(H60), C65(H65), C66(H66), C67(H67), C68(H68), C72(H72), C73(H73),
  C74(H74), C79(H79), C80(H80), C81(H81), C86(H86), C87(H87), C88(H88),
 C93(H93), C94(H94), C95(H95)
8.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C29(H29A,H29B,H29C), C46(H46A,H46B,H46C), C63(H63A,H63B,
 H63C)
;
_shelx_res_checksum              75099
_shelx_hkl_checksum              76169
_shelx_fab_checksum              7330
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'