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_1570002
_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         'C78 H56 N4 O9 S4 Zn2, 3(C4 H9 N O), 5(H2 O)'
_chemical_formula_sum            'C90 H93 N7 O17 S4 Zn2'
_chemical_formula_weight         1803.69
_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             2022-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                78.006(4)
_cell_angle_beta                 76.999(4)
_cell_angle_gamma                83.799(4)
_cell_formula_units_Z            2
_cell_length_a                   11.873(2)
_cell_length_b                   17.012(3)
_cell_length_c                   22.921(4)
_cell_measurement_reflns_used    6082
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.21
_cell_volume                     4403.4(13)
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27985
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.226
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1209 before and 0.0887 after correction.
 The Ratio of minimum to maximum transmission is 0.57.

Final HKLF 4 output contains 76867 reflections, Rint = 0.0916
 (10398 with I > 3sig(I), Rint = 0.0582)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       prism
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         27985
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0758P)^2^+13.0180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18444
_reflns_number_total             27985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5044.cif
_cod_data_source_block           dte-15
_cod_original_cell_volume        4403.4(14)
_cod_database_code               1570002
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8738(6)
 0.1262(6)
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. Rigid body (RIGU) restrains
 O12A, N7A, C87A, C89A, H89d, H89e, H89f, C90, H90a, H90b, H90c, C90A, H90d,
 H90e, H90f
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, N7, C87, C88, H88a, H88b, H88c, C88A, H88d, H88e, H88f, C89, H89a, H89b,
 H89c
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O12A)=Sof(N7A)=Sof(C87A)=Sof(C89A)=Sof(H89d)=Sof(H89e)=Sof(H89f)=Sof(C90)=
 Sof(H90a)=Sof(H90b)=Sof(H90c)=Sof(C90A)=Sof(H90d)=Sof(H90e)=Sof(H90f)=1-FVAR(1)
 Sof(O12)=Sof(N7)=Sof(C87)=Sof(C88)=Sof(H88a)=Sof(H88b)=Sof(H88c)=Sof(C88A)=
 Sof(H88d)=Sof(H88e)=Sof(H88f)=Sof(C89)=Sof(H89a)=Sof(H89b)=Sof(H89c)=FVAR(1)
5.a Free rotating group:
 O13(H13a,H13b), O14(H14a,H14b), O15(H15a,H15b), O16(H16a,H16b), O17(H17a,H17b)
5.b Rotating group:
 O9(H9a,H9b)
5.c 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), 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), C70(H70), C76(H76)
5.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C29(H29a,H29b,H29c), C46(H46a,H46b,H46c), C63(H63a,H63b,
 H63c), C80(H80a,H80b,H80c), C81(H81a,H81b,H81c), C82(H82a,H82b,H82c), C84(H84a,
 H84b,H84c), C85(H85a,H85b,H85c), C86(H86a,H86b,H86c), C88(H88a,H88b,H88c),
 C88A(H88d,H88e,H88f), C89(H89a,H89b,H89c), C89A(H89d,H89e,H89f), C90(H90a,H90b,
 H90c), C90A(H90d,H90e,H90f)
;
_shelx_res_checksum              83136
_shelx_hkl_checksum              50442
_shelx_fab_checksum              26180
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'