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_1573946
_publ_section_title
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 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         'Cl6 Sb, 3(C11 H13 N2)'
_chemical_formula_sum            'C33 H39 Cl6 N6 Sb'
_chemical_formula_weight         854.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-05-26 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.792(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7360(6)
_cell_length_b                   26.6108(15)
_cell_length_c                   14.4804(10)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      54.906
_cell_measurement_theta_min      2.889
_cell_volume                     3749.8(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28199
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        52.999
_diffrn_reflns_theta_max         52.999
_diffrn_reflns_theta_min         2.656
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.774
_exptl_absorpt_correction_T_max  0.0911
_exptl_absorpt_correction_T_min  0.0185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1320 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.2031.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       PRSIM
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.422
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.369(15)
_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     764
_refine_ls_number_reflns         12777
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1091P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                10228
_reflns_number_total             12777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh01427h3.cif
_cod_data_source_block           b23072805a0770_0m
_cod_depositor_comments
'Adding full bibliography for 1573946--1573947.cif.'
_cod_database_code               1573946
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.551
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.631(15)
 0.369(15)
2. 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
3. Restrained distances
 C27-C26 = C5-C4 = C16-C15
 1.513 with sigma of 0.002
 C16-C15 \\sim C5-C4 \\sim C27-C26 \\sim C49-C48
 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C15(H15A,H15B), C26(H26A,H26B), C37(H37A,H37B), C48(H48A,H48B),
 C59(H59A,H59B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C9(H9), C8(H8), C7(H7), C6(H6), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C17(H17), C18(H18), C23(H23),
  C24(H24), C25(H25), C32(H32), C31(H31), C30(H30), C29(H29), C28(H28),
 C34(H34), C35(H35), C36(H36), C43(H43), C42(H42), C41(H41), C40(H40), C39(H39),
  C45(H45), C46(H46), C47(H47), C54(H54), C53(H53), C52(H52), C51(H51),
 C50(H50), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64),
  C65(H65)
4.c Fitted hexagon refined as free rotating group:
 C5(C10,C9,C8,C7,C6), C19(C20,C21,C16,C17,C18), C27(C32,C31,C30,C29,C28),
 C38(C43,C42,C41,C40,C39), C49(C54,C53,C52,C51,C50), C60(C61,C62,C63,C64,C65)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C44(H44A,H44B,
 H44C), C55(H55A,H55B,H55C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              14143
_olex2_submission_special_instructions 'No special instructions were received'