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_4133150
_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         'Br10 Pb3, 2(C5 H14 N2)'
_chemical_formula_sum            'C10 H28 Br10 N4 Pb3'
_chemical_formula_weight         1625.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 97.92(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.062(9)
_cell_length_b                   9.5432(19)
_cell_length_c                   15.205(3)
_cell_measurement_reflns_used    10628
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.82
_cell_volume                     6476(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    '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 0.996
_diffrn_measured_fraction_theta_max 0.991
_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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24781
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.205
_diffrn_reflns_theta_min         1.825
_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    27.906
_exptl_absorpt_correction_T_max  0.3658
_exptl_absorpt_correction_T_min  0.0420
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    3.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             5696
_exptl_crystal_size_max          0.1626
_exptl_crystal_size_mid          0.0824
_exptl_crystal_size_min          0.0236
_refine_diff_density_max         5.254
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       0.000109(12)
_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   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         8706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                5009
_reflns_number_total             8706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08691_si_008.cif
_cod_data_source_block           mpz2Pb3Br10
_cod_database_code               4133150
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 N1(H), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(HA,HB), C4(HC,HD), N5(H5A,H5B), N6(HE,HF), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C12(HJ,HK), C13(H13A,H13B), C14(HL,HM)
2.c Idealised Me refined as rotating group:
 C11(HG,HH,HI), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'