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_4133151
_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), C6 H14 N'
_chemical_formula_sum            'C6 H14 Br3 N Pb'
_chemical_formula_weight         547.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.9990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   7.9457(4)
_cell_length_b                   16.1647(9)
_cell_length_c                   37.860(2)
_cell_measurement_reflns_used    9195
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.74
_cell_volume                     4862.7(4)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      249.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            44028
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         1.076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.690
_exptl_absorpt_correction_T_max  0.36942
_exptl_absorpt_correction_T_min  0.02950
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.989
_exptl_crystal_description       needle
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.656
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.159
_refine_diff_density_min         -2.275
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details
;
 Flack x determined using 4123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.486(14)
_refine_ls_extinction_coef       0.000097(13)
_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   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         21686
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+21.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                10912
_reflns_number_total             21686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08691_si_006.cif
_cod_data_source_block           hexPbBr3
_cod_original_cell_volume        4862.7(5)
_cod_database_code               4133151
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.335
_shelx_estimated_absorpt_t_min   0.023
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C2-C3
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 N2-C7
 1.5 with sigma of 0.02
 C7-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-N2
 1.5 with sigma of 0.02
 N3-C13
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C14-C15
 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
 N3-C18
 1.5 with sigma of 0.02
 N4-C19
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 C20-C21
 1.5 with sigma of 0.02
 C20-C21
 1.5 with sigma of 0.02
 C21-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-N4
 1.5 with sigma of 0.02
 N7-C37
 1.5 with sigma of 0.02
 C37-C38
 1.5 with sigma of 0.02
 C38-C39
 1.5 with sigma of 0.02
 C39-C40
 1.5 with sigma of 0.02
 C40-C41
 1.5 with sigma of 0.02
 C41-C42
 1.5 with sigma of 0.02
 C42-N7
 1.5 with sigma of 0.02
 N8-C43
 1.5 with sigma of 0.02
 C43-C44
 1.5 with sigma of 0.02
 C44-C45
 1.5 with sigma of 0.02
 C45-C46
 1.5 with sigma of 0.02
 C46-C47
 1.5 with sigma of 0.02
 C47-C48
 1.5 with sigma of 0.02
 C48-N8
 1.5 with sigma of 0.02
 N9-C55
 1.5 with sigma of 0.02
 C55-C56
 1.5 with sigma of 0.02
 C58-C59
 1.5 with sigma of 0.02
 C59-C60
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(N1) = Uiso(N2) = Uiso(N3) = Uiso(N4) = Uiso(N7) = Uiso(N8) = Uiso(C2) =
Uiso(C3) = Uiso(C4) = Uiso(C7) = Uiso(C8) = Uiso(C9) = Uiso(C10) = Uiso(C11) =
Uiso(C12) = Uiso(C13) = Uiso(C14) = Uiso(C15) = Uiso(C16) = Uiso(C17) =
Uiso(C18) = Uiso(C19) = Uiso(C20) = Uiso(C21) = Uiso(C22) = Uiso(C23) =
Uiso(C24) = Uiso(C37) = Uiso(C38) = Uiso(C39) = Uiso(C40) = Uiso(C41) =
Uiso(C42) = Uiso(C43) = Uiso(C44) = Uiso(C45) = Uiso(C46) = Uiso(C47) =
Uiso(C48)
Uiso(N9) = Uiso(C55) = Uiso(C56) = Uiso(C58) = Uiso(C59) = Uiso(C60)
Uiso(N10) = Uiso(C49) = Uiso(C50) = Uiso(C51) = Uiso(C52) = Uiso(C53) =
Uiso(C54)
Uiso(N9) = Uiso(C55) = Uiso(C56) = Uiso(C58) = Uiso(C59) = Uiso(C60)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), N2(H2C,H2D), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 N3(H3C,H3D), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), N4(H4C,H4D), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), N7(H7C,H7D),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C42(H42A,H42B), N8(H8C,H8D), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), N9(H9C,H9D), N10(H10C,H10D),
 C49(H49A,H49B), C60(H60A,H60B), C55(H55A,H55B), C54(H54A,H54B), C53(H53A,H53B),
  C52(H52A,H52B), C59(H59A,H59B), C56(H56A,H56B), C58(H58A,H58B), C50(H50A,
 H50B), C51(H51A,H51B), C64(H64A,H64B), C0AA(H0AA,H0AB), C63(H63A,H63B),
 C62(H62A,H62B)
;
_olex2_submission_special_instructions 'No special instructions were received'