Structural Diversity in White-Light-Emitting Hybrid Lead Bromide Perovskites.
Mao, Lingling; Guo, Peijun; Kepenekian, Mikaël; Hadar, Ido; Katan, Claudine; Even, Jacky; Schaller, Richard D.; Stoumpos, Constantinos C.; Kanatzidis, Mercouri G.; Journal of the American Chemical Society 140 (2018) 13078–13088; doi:10.1021/jacs.8b08691

data_4133149
_publ_section_title
;
 Structural Diversity in White-Light-Emitting Hybrid Lead Bromide
 Perovskites.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13078
_journal_page_last               13088
_journal_paper_doi               10.1021/jacs.8b08691
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.5(Br6 Pb2), C7 H16 N'
_chemical_formula_sum            'C7 H16 Br3 N Pb'
_chemical_formula_weight         561.13
_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             2018-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.550(3)
_cell_length_b                   39.660(8)
_cell_length_c                   7.9623(16)
_cell_measurement_reflns_used    5874
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      1.96
_cell_volume                     5226.2(18)
_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_type            STOE
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15674
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         1.972
_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
_exptl_absorpt_coefficient_mu    22.045
_exptl_absorpt_correction_T_max  0.6029
_exptl_absorpt_correction_T_min  0.3884
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_description       needle
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.0293
_exptl_crystal_size_mid          0.0194
_exptl_crystal_size_min          0.0143
_refine_diff_density_max         3.313
_refine_diff_density_min         -2.538
_refine_diff_density_rms         0.530
_refine_ls_abs_structure_details
;
 Flack x determined using 1481 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.00070(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         8230
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1588
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.3147
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.855
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                4094
_reflns_number_total             8230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08691_si_005.cif
_cod_data_source_block           hepPbBr3
_cod_original_cell_volume        5226.3(18)
_cod_database_code               4133149
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.43(6) 0.57(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Restrained distances
 N1-C1
 1.5 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C2-C0AA
 1.5 with sigma of 0.02
 C0AA-C4
 1.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C6-C7
 1.5 with sigma of 0.02
 C7-N1
 1.5 with sigma of 0.02
 N2-C8
 1.5 with sigma of 0.02
 C8-C9
 1.5 with sigma of 0.02
 C9-C10
 1.5 with sigma of 0.02
 C10-C11
 1.5 with sigma of 0.02
 C11-C12
 1.5 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C14-N2
 1.5 with sigma of 0.02
 C3-C15
 1.5 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 C16-C17
 1.5 with sigma of 0.02
 C17-C18
 1.5 with sigma of 0.02
 C18-C19
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 N21-C3 = N21-C20
 1.5 with sigma of 0.02
 N21-C3
 1.5 with sigma of 0.02
 N4-C22
 1.5 with sigma of 0.02
 C22-C23
 1.5 with sigma of 0.02
 C23-C24
 1.5 with sigma of 0.02
 C24-C25
 1.5 with sigma of 0.02
 C25-C26
 1.5 with sigma of 0.02
 C26-C27
 1.5 with sigma of 0.02
 C27-C28
 1.5 with sigma of 0.02
 C28-N4
 1.5 with sigma of 0.02
 C25-C27
 2.3 with sigma of 0.02
 C25-C27
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(N1) = Uiso(C1) = Uiso(C2) = Uiso(C0AA) = Uiso(C4) = Uiso(C5) = Uiso(C6) =
Uiso(C7)
Uiso(N2) = Uiso(C8) = Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(C13)
= Uiso(C14)
Uiso(C3) = Uiso(C15) = Uiso(C16) = Uiso(C17) = Uiso(C18) = Uiso(C19) = Uiso(C20)
Uiso(N4) = Uiso(C22) = Uiso(C23) = Uiso(C24) = Uiso(C25) = Uiso(C26) =
Uiso(C27) = Uiso(C28)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4C,H4D), C8(H8A,H8B), N21(H21A,H21B), N2(H2C,H2D), C3(H3A,
 H3B), C7(H7A,H7B), C27(H27A,H27B), C10(H10A,H10B), C4(H4A,H4B), C25(H25A,H25B),
  C20(H20A,H20B), C24(H24A,H24B), C19(H19A,H19B), C5(H5A,H5B), C11(H11A,H11B),
 C2(H2A,H2B), C6(H6A,H6B), C14(H14A,H14B), C13(H13A,H13B), C15(H15A,H15B),
 C22(H22A,H22B), C9(H9A,H9B), C12(H12A,H12B), C28(H28A,H28B), C18(H18A,H18B),
 C1(H1C,H1D), C0AA(H0AA,H0AB), C26(H26A,H26B), C17(H17A,H17B), C23(H23A,H23B),
 C16(H16A,H16B)
;
_olex2_submission_special_instructions 'No special instructions were received'