Organic Cation Alloying on Intralayer A and Interlayer A' sites in 2D Hybrid Dion-Jacobson Lead Bromide Perovskites (A')(A)Pb<sub>2</sub>Br<sub>7</sub>.
Mao, Lingling; Guo, Peijun; Kepenekian, Mikaël; Spanopoulos, Ioannis; He, Yihui; Katan, Claudine; Even, Jacky; Schaller, Richard D.; Seshadri, Ram; Stoumpos, Constantinos C.; Kanatzidis, Mercouri G.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01625

data_4134817
_publ_section_title
;
 Organic Cation Alloying on Intralayer A and Interlayer A' sites in 2D
 Hybrid Dion-Jacobson Lead Bromide Perovskites
 (A')(A)Pb<sub>2</sub>Br<sub>7</sub>.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01625
_journal_year                    2020
_chemical_formula_moiety         'Br7 Pb2, C N, C6 H16 N2'
_chemical_formula_sum            'C7 H0.5 Br7 N3 Pb2'
_chemical_formula_weight         1100.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.921(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.193(2)
_cell_length_b                   8.3678(11)
_cell_length_c                   8.3469(10)
_cell_measurement_reflns_used    6327
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.809
_cell_measurement_theta_min      2.515
_cell_volume                     1131.0(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.01
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13102
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.981
_diffrn_reflns_theta_min         1.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.221
_exptl_absorpt_correction_T_max  0.4811
_exptl_absorpt_correction_T_min  0.1123
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1216 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.2334. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             945
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.966
_refine_diff_density_min         -3.172
_refine_diff_density_rms         0.314
_refine_ls_abs_structure_details
;
 Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0960P)^2^+12.6989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                3611
_reflns_number_total             5029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01625_si_009.cif
_cod_data_source_block           pc
_cod_original_cell_volume        1131.0(3)
_cod_original_formula_sum        'C7 H0.50 Br7 N3 Pb2'
_cod_database_code               4134817
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.126
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C1-N1
 1.5 with sigma of 0.02
 N2-C2 = C2-C3
 1.5 with sigma of 0.02
 C2-C3 = C3-C4
 1.5 with sigma of 0.02
 C3-C4 = C4-C5
 1.5 with sigma of 0.02
 C4-C5 = C5-C6
 1.5 with sigma of 0.02
 C5-C6 = C6-N2
 1.5 with sigma of 0.02
 C6-N2 = N2-C2
 1.5 with sigma of 0.02
 C3-C4 = C4-C7
 1.5 with sigma of 0.02
 C4-C7 = C7-N3
 1.5 with sigma of 0.02
 N2-C3
 2.516 with sigma of 0.04
 C2-C4
 2.544 with sigma of 0.04
 C3-C5
 2.544 with sigma of 0.04
 C4-C6
 2.558 with sigma of 0.04
 C5-N2
 2.516 with sigma of 0.04
 C6-C2
 2.544 with sigma of 0.04
 C3-C7
 2.442 with sigma of 0.04
 C4-N3
 2.598 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(C1) = Uiso(N1)
Uiso(N2) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(C7) =
Uiso(N3)
4.a Ternary CH refined with riding coordinates:
 C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C2(H2D,H2C), C3(H3E,H3D), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
4.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C)
;
_shelx_res_checksum              6675
_shelx_hkl_checksum              26106
_olex2_submission_special_instructions 'No special instructions were received'