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_4133145
_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         '0.33(Br12 Pb3), C6 H16 N2'
_chemical_formula_sum            'C6 H16 Br4 N2 Pb'
_chemical_formula_weight         643.04
_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             2018-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.77(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.536(2)
_cell_length_b                   12.415(2)
_cell_length_c                   16.430(3)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.73
_cell_volume                     2134.1(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.1307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.206
_diffrn_reflns_theta_min         2.733
_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    23.11
_exptl_absorpt_correction_T_max  0.3758
_exptl_absorpt_correction_T_min  0.0732
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.983
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.0911
_exptl_crystal_size_mid          0.0549
_exptl_crystal_size_min          0.0196
_refine_diff_density_max         1.694
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.282
_refine_ls_abs_structure_details
;
 Flack x determined using 1594 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_coef       0.00279(18)
_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   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         10816
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0870P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                4864
_reflns_number_total             10816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08691_si_004.cif
_cod_data_source_block           epzPbBr4
_cod_original_cell_volume        2134.2(8)
_cod_database_code               4133145
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(5) 0.52(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1-C2
 1.5 with sigma of 0.02
 C2-N1
 1.5 with sigma of 0.02
 N1-C3
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 C4-N2
 1.5 with sigma of 0.02
 N2-C5
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C6-N1
 1.5 with sigma of 0.02
 C7-C8
 1.5 with sigma of 0.02
 C8-N3
 1.5 with sigma of 0.02
 N3-C9
 1.5 with sigma of 0.02
 N3-C12
 1.5 with sigma of 0.02
 C9-C10
 1.5 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C10-N4
 1.5 with sigma of 0.02
 C11-N4
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C14-N5
 1.5 with sigma of 0.02
 N5-C18
 1.5 with sigma of 0.02
 N5-C15
 1.5 with sigma of 0.02
 C17-C18
 1.5 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 N6-C17
 1.5 with sigma of 0.02
 N6-C16
 1.5 with sigma of 0.02
 C8-C9
 2.2 with sigma of 0.02
 C8-C9
 2.5 with sigma of 0.02
 C7-C8
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C1) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) = Uiso(N1) =
Uiso(N2)
Uiso(C7) = Uiso(C8) = Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(N3) =
Uiso(N4)
Uiso(C13) = Uiso(C14) = Uiso(N5) = Uiso(C15) = Uiso(C16) = Uiso(N6) = Uiso(C17)
= Uiso(C18)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N5(H5), N3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), N2(H2A,H2B), C6(H6A,H6B), C16(H16A,H16B), C4(H4A,H4B),
 C17(H17A,H17B), N6(H6C,H6D), C3(H3A,H3B), C15(H15A,H15B), C2(H2C,H2D), C5(H5A,
 H5B), C14(H14A,H14B), C12(H12A,H12B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), N4(H4C,H4D), C8(H8A,H8B)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'