Two-dimensional semiconducting Cu(I)/Sb(III) bimetallic hybrid iodides with a double perovskite structure and photocurrent response.
Li, Qian-Wen; Bi, Le-Yu; Lassoued, Mohamed Saber; Luo, Qian-Cheng; Yan, Rong; Ding, Xin-Kai; Gou, Gao-Yang; Zheng, Yan-Zhen; Nanoscale 15 (2023) 5265–5273; doi:10.1039/d2nr06996b

data_1568484
_publ_section_title
;
 Two-dimensional semiconducting Cu(I)/Sb(III) bimetallic hybrid iodides
 with a double perovskite structure and photocurrent response.
;
_journal_issue                   11
_journal_name_full               Nanoscale
_journal_page_first              5265
_journal_page_last               5273
_journal_paper_doi               10.1039/d2nr06996b
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'Cu I8 Sb, H2 O, 4(C6 H14 N)'
_chemical_formula_sum            'C24 H58 Cu I8 N4 O Sb'
_chemical_formula_weight         1619.23
_chemical_name_systematic        (CA)4CuSbI8H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-01-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-20 deposited with the CCDC.	2023-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.362(10)
_cell_length_b                   8.491(2)
_cell_length_c                   19.599(6)
_cell_measurement_reflns_used    2478
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.63
_cell_volume                     4402(2)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         1.539
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.729
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.7160.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.836
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0525P)^2^+70.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2592
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr06996b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1568483--1568484.cif.'
_cod_database_code               1568484
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.284
_shelx_estimated_absorpt_t_min   0.134
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C2-C8
 1.53 with sigma of 0.02
 C3-C1
 1.53 with sigma of 0.02
 C1-C3
 1.53 with sigma of 0.02
 C3-C12
 1.53 with sigma of 0.02
 C12-C5
 1.53 with sigma of 0.02
 C6-C5
 1.53 with sigma of 0.02
 C10-C6
 1.53 with sigma of 0.02
 C1-C10
 1.53 with sigma of 0.02
 C2-C11
 1.53 with sigma of 0.02
 C11-C7
 1.53 with sigma of 0.02
 C7-C4
 1.53 with sigma of 0.02
 C4-C9
 1.53 with sigma of 0.02
 C9-C8
 1.53 with sigma of 0.02
 C8-C2
 1.53 with sigma of 0.02
 C8-C2 \\sim C2-C11 \\sim C9-C8 \\sim C9-C4 \\sim C7-C4 \\sim C7-C11 \\sim
C10-C1 \\sim C3-C1 \\sim C3-C12 ~
 C5-C12 \\sim C6-C5 \\sim C6-C10
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Cu1(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              55753
_olex2_submission_special_instructions 'No special instructions were received'