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_1568483
_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         '0.25(Cu4 I32 Sb4), 0.5(H2 O), 2(C6 H16 N2)'
_chemical_formula_sum            'C12 H33 Cu I8 N4 O0.5 Sb'
_chemical_formula_weight         1441.91
_chemical_name_systematic        CDACuSbI
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-20 deposited with the CCDC.	2023-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.809(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.934(5)
_cell_length_b                   19.721(6)
_cell_length_c                   18.703(6)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.41
_cell_volume                     6245(3)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0850
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45741
_diffrn_reflns_theta_full        25.58
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.50
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.465
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.6758.
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    3.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5128
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.051
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         11566
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                6901
_reflns_number_total             11566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nr06996b2.cif
_cod_data_source_block           cdacusbi
_cod_depositor_comments
'Adding full bibliography for 1568483--1568484.cif.'
_cod_original_cell_volume        6246(3)
_cod_original_formula_sum        'C12 H33 Cu I8 N4 O0.50 Sb'
_cod_database_code               1568483
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O1(H1D,H1E)
3.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C23(H23)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6D,H6E), C8(H8A,H8B), C10(H10A,H10B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C24(H24A,H24B)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E), N4(H4A,H4B,H4C), N5(H5A,
 H5B,H5C), N6(H6A,H6B,H6C), N7(H7A,H7B,H7C), N8(H8C,H8D,H8E)
;
_olex2_submission_special_instructions 'No special instructions were received'