Two-dimensional lead-free iodide-based hybrid double perovskites: crystal growth, thin-film preparation and photocurrent responses
Bi, Le-Yu; Hu, Yue-Qiao; Li, Mu-Qing; Hu, Tian-Li; Zhang, Hao-Lan; Yin, Xing-Tian; Que, Wen-Xiu; Lassoued, Mohamed Saber; Zheng, Yan-Zhen; Journal of Materials Chemistry A 7 (2019) 19662–; doi:10.1039/C9TA04325J

data_7237670
_publ_section_title
;
 Two-dimensional lead-free iodide-based hybrid double perovskites: crystal
 growth, thin-film preparation and photocurrent responses
;
_journal_issue                   34
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              19662
_journal_paper_doi               10.1039/C9TA04325J
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '0.25(Bi4 Cu4 I32), 2(C6 H16 N2), 0.5(H2 O)'
_chemical_formula_sum            'C12 H33 Bi Cu I8 N4 O0.5'
_chemical_formula_weight         1529.14
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-03-01 deposited with the CCDC.	2019-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.297(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.062(6)
_cell_length_b                   19.825(7)
_cell_length_c                   18.808(7)
_cell_measurement_reflns_used    7546
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.311
_cell_measurement_theta_min      2.388
_cell_volume                     6362(4)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56482
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.587
_diffrn_reflns_theta_min         1.492
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    13.968
_exptl_absorpt_correction_T_max  0.4401
_exptl_absorpt_correction_T_min  0.2902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0891 before and 0.0463 after correction. 
The Ratio of minimum to maximum transmission is 0.6594. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_description       bulk
_exptl_crystal_F_000             5384
_exptl_crystal_size_max          2.2
_exptl_crystal_size_mid          1.8
_exptl_crystal_size_min          1.6
_refine_diff_density_max         3.184
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         13153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+51.6670P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9613
_reflns_number_total             13153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ta04325j3.cif
_cod_data_source_block           mo_bly_1_20180627_0m
_cod_original_formula_sum        'C12 H33 Bi Cu I8 N4 O0.50'
_cod_database_code               7237670
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.330
_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. Others
 Fixed Sof: I5(0.9) I0AA(0.1)
3.a Free rotating group:
 O1(H1D,H1E)
3.b Ternary CH refined with riding coordinates:
 C22(H22), C13(H13), C19(H19), C1(H1), C11(H11), C7(H7), C4(H4), C16(H16)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B), C18(H18A,H18B), C12(H12A,H12B), C20(H20A,H20B),
 C14(H14A,H14B), C2(H2D,H2E), C21(H21A,H21B), C5(H5D,H5E), C9(H9A,H9B),
 C15(H15A,H15B), C8(H8A,H8B), C17(H17A,H17B), C6(H6D,H6E), C24(H24A,H24B),
 C23(H23A,H23B)
3.d Idealised Me refined as rotating group:
 N7(H7A,H7B,H7C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C), N3(H3C,H3D,H3E), N2(H2A,
 H2B,H2C), N6(H6A,H6B,H6C), N1(H1A,H1B,H1C), N8(H8C,H8D,H8E)
;
_shelx_res_checksum              24578
_olex2_submission_special_instructions 'No special instructions were received'