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_4134820
_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, C6 H16 N2, C H6 N'
_chemical_formula_sum            'C7 H22 Br7 N3 Pb2'
_chemical_formula_weight         1122.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 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                 104.599(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.2368(17)
_cell_length_b                   8.3841(5)
_cell_length_c                   8.3801(4)
_cell_measurement_reflns_used    7585
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.53
_cell_volume                     2259.8(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      293.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18020
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.251
_exptl_absorpt_correction_T_max  0.6161
_exptl_absorpt_correction_T_min  0.1159
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1162 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.1881.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.031
_refine_diff_density_max         2.007
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.270
_refine_ls_abs_structure_details
;
 Flack x determined using 1462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.55(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.467
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.953
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                3457
_reflns_number_total             5412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01625_si_007.cif
_cod_data_source_block           cc
_cod_database_code               4134820
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.485
_shelx_estimated_absorpt_t_min   0.173
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N0AA-C1AA = C1AA-C3
 1.5 with sigma of 0.02
 C1AA-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-N0AA
 1.5 with sigma of 0.02
 C6-N0AA = N0AA-C1AA
 1.5 with sigma of 0.02
 C3-C4 = C4-C7
 1.5 with sigma of 0.02
 C4-C7 = C7-N1AA
 1.5 with sigma of 0.02
 C1-N1
 1.5 with sigma of 0.02
 N0AA-C3
 2.53 with sigma of 0.04
 C1AA-C4
 2.544 with sigma of 0.04
 C3-C5
 2.558 with sigma of 0.04
 C4-C6
 2.516 with sigma of 0.04
 C5-N0AA
 2.558 with sigma of 0.04
 C6-C1AA
 2.53 with sigma of 0.04
 C3-C7
 2.442 with sigma of 0.04
 C4-N1AA
 2.598 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N0AA) = Uiso(C1AA) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(C7)
= Uiso(N1AA)
Uiso(N1) = Uiso(C1)
4.a Ternary CH refined with riding coordinates:
 C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 N0AA(H0AA,H0AB), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C1AA(H1AD,H1AE),
 C6(H6A,H6B)
4.c Idealised Me refined as rotating group:
 N1AA(H1AA,H1AB,H1AC), C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_shelx_res_checksum              94090
_shelx_hkl_checksum              8388
_olex2_submission_special_instructions 'No special instructions were received'