Regulating intermolecular interactions for stable multifunctional organic-inorganic metal halide hybrid glasses.
Jiang, Chunyan; Yan, Jing; Qiu, Jianrong; Wu, Mingmei; Xu, Beibei; Materials horizons 12 (2025) 3515–3524; doi:10.1039/d4mh01427h

data_1573947
_publ_section_title
;
 Regulating intermolecular interactions for stable multifunctional
 organic-inorganic metal halide hybrid glasses.
;
_journal_issue                   10
_journal_name_full               'Materials horizons'
_journal_page_first              3515
_journal_page_last               3524
_journal_paper_doi               10.1039/d4mh01427h
_journal_volume                  12
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(Cl5 Sb), 4(C11 H13 N2)'
_chemical_formula_sum            'C44 H52 Cl10 N8 Sb2'
_chemical_formula_weight         1290.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-26 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.5697(15)
_cell_length_b                   17.5697(15)
_cell_length_c                   8.7813(10)
_cell_measurement_reflns_used    5152
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      58.574
_cell_measurement_theta_min      3.094
_cell_volume                     2710.7(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11536
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.200
_diffrn_reflns_theta_min         3.095
_exptl_absorpt_coefficient_mu    8.631
_exptl_absorpt_correction_T_max  0.0717
_exptl_absorpt_correction_T_min  0.0095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1706 before and 0.0684 after correction. The Ratio of minimum to maximum transmission is 0.1325. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0853P)^2^+7.3943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                1948
_reflns_number_total             2974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh01427h3.cif
_cod_data_source_block           b23072408a0770_0m
_cod_depositor_comments
'Adding full bibliography for 1573946--1573947.cif.'
_cod_original_cell_volume        2710.7(6)
_cod_database_code               1573947
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.479
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl2(0.75) Cl3(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C2(H2), C7(H7), C6(H6), C10(H10), C9(H9), C8(H8)
3.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C10,C9,C8)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              79026
_olex2_submission_special_instructions 'No special instructions were received'