White-Light Emission and Structural Distortion in New Corrugated Two-Dimensional Lead Bromide Perovskites.
Mao, Lingling; Wu, Yilei; Stoumpos, Constantinos C.; Wasielewski, Michael R.; Kanatzidis, Mercouri G.; Journal of the American Chemical Society 139 (2017) 5210–5215; doi:10.1021/jacs.7b01312

data_4131240
_publ_section_title
;
 White-Light Emission and Structural Distortion in New Corrugated
 Two-Dimensional Lead Bromide Perovskites.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5210
_journal_page_last               5215
_journal_paper_doi               10.1021/jacs.7b01312
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '0.13(Br32 Pb8), C6 H18 N2'
_chemical_formula_sum            'C6 H18 Br4 N2 Pb'
_chemical_formula_weight         645.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   41.685(8)
_cell_length_b                   23.962(5)
_cell_length_c                   12.000(2)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      3.21
_cell_volume                     11986(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      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 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.1389
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45002
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.186
_diffrn_reflns_theta_min         2.590
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.896
_exptl_absorpt_correction_T_max  0.4095
_exptl_absorpt_correction_T_min  0.0943
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.860
_exptl_crystal_description       plate
_exptl_crystal_F_000             9280
_exptl_crystal_size_max          0.1271
_exptl_crystal_size_mid          0.0319
_exptl_crystal_size_min          0.0212
_refine_diff_density_max         2.142
_refine_diff_density_min         -2.210
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Flack x determined using 1751 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.000049(3)
_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   0.831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         13741
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    0.726
_reflns_Friedel_fraction_max     0.688
_reflns_number_gt                6799
_reflns_number_total             13741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01312_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        11987(4)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               4131240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 N6-C18
 1.5 with sigma of 0.02
 N6-C17
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2)
Uanis(C2) = Uanis(C3)
Uanis(C3) = Uanis(C4)
Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) =
Uanis(C11) = Uanis(C12) = Uanis(C19)
4.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), N3(H3C,H3D,H3E), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), N5(H5D,H5E,H5F), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), N7(H7C,H7D,H7E), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'