Centimeter-Sized 2D Perovskitoid Single Crystals for Efficient X-ray Photoresponsivity
Ma, Chuang; Gao, Lili; Xu, Zhuo; Li, Xiaotong; Song, Xin; Liu, Yucheng; Yang, Tinghuan; Li, Haojin; Du, Yachao; Zhao, Guangtao; Liu, Xinmei; Kanatzidis, Mercouri G.; Liu, Shengzhong Frank; Zhao, Kui; Chemistry of Materials 34 (2022) 1699–1709; doi:10.1021/acs.chemmater.1c03832

data_4004069
_publ_section_title
;
 Centimeter-Sized 2D Perovskitoid Single Crystals for Efficient X-ray
 Photoresponsivity
;
_journal_issue                   4
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1699
_journal_page_last               1709
_journal_paper_doi               10.1021/acs.chemmater.1c03832
_journal_volume                  34
_journal_year                    2022
_chemical_formula_moiety         'Br4 Pb, C6 H9 N3'
_chemical_formula_sum            'C6 H9 Br4 N3 Pb'
_chemical_formula_weight         649.99
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3428(9)
_cell_length_b                   9.0610(5)
_cell_length_c                   18.5386(10)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      53.88
_cell_measurement_theta_min      4.24
_cell_volume                     2687.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      189.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9316
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.915
_diffrn_reflns_theta_min         4.238
_exptl_absorpt_coefficient_mu    26.614
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    3.213
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.833
_refine_diff_density_min         -4.735
_refine_diff_density_rms         0.866
_refine_ls_extinction_coef       0.00078(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2448
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0893P)^2^+22.5943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2292
_reflns_number_total             2448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c03832_si_003.cif
_cod_data_source_block           s_a
_cod_database_code               4004069
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.100
_shelx_estimated_absorpt_t_min   0.076
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 N1, N2, N3, C1, C2, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C4(H4), C5(H5), C7(H7)
4.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_shelx_res_checksum              84674
_shelx_hkl_checksum              98023
_olex2_submission_special_instructions 'No special instructions were received'