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_4133146
_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         'Br5 Pb, Br4 Pb, Br, 3(C6 H16 N2)'
_chemical_formula_sum            'C18 H48 Br10 N6 Pb2'
_chemical_formula_weight         1562.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                73.597(3)
_cell_angle_beta                 84.960(3)
_cell_angle_gamma                88.793(3)
_cell_formula_units_Z            2
_cell_length_a                   6.2455(4)
_cell_length_b                   16.8901(10)
_cell_length_c                   20.1013(11)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.44
_cell_volume                     2026.2(2)
_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      249.96
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31554
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         1.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.177
_exptl_absorpt_correction_T_max  0.6710
_exptl_absorpt_correction_T_min  0.1228
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1282 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.1830.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.639
_refine_diff_density_min         -1.844
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         10015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+4.4410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8432
_reflns_number_total             10015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08691_si_002.cif
_cod_data_source_block           2,6-dmpzPb2Br10
_cod_database_code               4133146
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.134
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), N3(H3C,H3D), N4(H4C,H4D),
 C9(H9A,H9B), C10(H10A,H10B), N5(H5A,H5B), N6(H6D,H6E), C15(H15A,H15B),
 C16(H16A,H16B)
2.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'