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_4134816
_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                 104.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.433(7)
_cell_length_b                   8.3738(17)
_cell_length_c                   8.3760(17)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.52
_cell_volume                     2270.8(9)
_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(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.881
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5494
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.191
_diffrn_reflns_theta_min         2.512
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.119
_exptl_absorpt_correction_T_max  0.1101
_exptl_absorpt_correction_T_min  0.0107
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.3535
_exptl_crystal_size_mid          0.0908
_exptl_crystal_size_min          0.0903
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.326
_refine_ls_abs_structure_details
;
 Flack x determined using 303 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.651
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1143P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                1517
_reflns_number_total             3739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01625_si_005.cif
_cod_data_source_block           cc
_cod_original_cell_volume        2270.8(8)
_cod_database_code               4134816
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.47(14)
 0.53(14)
2. 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
3. Restrained distances
 N2-C2
 1.5 with sigma of 0.02
 N1-C1
 1.5 with sigma of 0.02
 C4-C5 = C5-C6
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C6-C5
 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
 C1-N1
 1.5 with sigma of 0.02
 C6-C5 = C5-C4
 1.5 with sigma of 0.02
 C5-C4 = C4-C3
 1.5 with sigma of 0.02
 C4-C3 = C3-C2
 1.5 with sigma of 0.02
 C3-C2 = C2-N2
 1.5 with sigma of 0.02
 C2-N2 = N2-C6
 1.5 with sigma of 0.02
 N2-C6 = C6-C5
 1.5 with sigma of 0.02
 C5-C4 = C4-C7
 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
 C4-C6
 2.442 with sigma of 0.04
 N2-C6
 2.442 with sigma of 0.04
 N2-C3
 2.442 with sigma of 0.04
 C2-C4
 2.442 with sigma of 0.04
 C3-C5
 2.442 with sigma of 0.04
 C6-C4
 2.558 with sigma of 0.04
 C5-C3
 2.558 with sigma of 0.04
 C4-C2
 2.544 with sigma of 0.04
 C3-N2
 2.516 with sigma of 0.04
 C2-C6
 2.53 with sigma of 0.04
 N2-C5
 2.516 with sigma of 0.04
 C5-C7
 2.598 with sigma of 0.04
 C3-C7
 2.442 with sigma of 0.04
 C4-N3
 2.598 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uiso(N2) = Uiso(C6) = Uiso(C5) = Uiso(C4) = Uiso(C7) = Uiso(C3) = Uiso(C2) =
Uiso(N3)
Uiso(C1) = Uiso(N1)
Uiso(N2) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(C7) =
Uiso(N3)
Uiso(C6) = Uiso(C5) = Uiso(C4) = Uiso(C3) = Uiso(C2) = Uiso(N2) = Uiso(C7) =
Uiso(N3)
5.a Ternary CH refined with riding coordinates:
 C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C7(H7A,H7B), C3(H3D,H3E), C5(H5A,H5B), C6(H6A,H6B), C2(H2C,H2D)
5.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_shelx_res_checksum              13768
_shelx_hkl_checksum              77660
_olex2_submission_special_instructions 'No special instructions were received'