Structural Origins of Broadband Emission from Layered Pb‒Br Hybrid Perovskites
Smith, Matthew D.; Jaffe, Adam; Dohner, Emma R.; Lindenberg, Aaron; Karunadasa, Hemamala I.; Chem. Sci.  (2017) –; doi:10.1039/C7SC01590A

data_1545806
_publ_section_title
;
 Structural Origins of Broadband Emission from Layered Pb--Br Hybrid
 Perovskites
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01590A
_journal_year                    2017
_chemical_formula_moiety         '(Br4 Pb1), C8 H22 N2'
_chemical_formula_sum            'C8 H22 Br4 N2 Pb'
_chemical_formula_weight         673.10
_chemical_name_systematic        'octanediammonium tetrabromoplumbate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.340(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.807(3)
_cell_length_b                   7.9891(14)
_cell_length_c                   8.2769(14)
_cell_measurement_reflns_used    6235
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.970
_cell_volume                     884.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.970
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.551
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1278 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.4872.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Slow cooling from concentrated hydrobromic acid'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2706
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0393P)^2^+0.4830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2216
_reflns_number_total             2706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01590a2.cif
_cod_data_source_block           p21c_2
_cod_database_code               1545806
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H,H,H,H) groups
2. Restrained distances
 C1A-C2
 1.54 with sigma of 0.01
 C4A-C3 \\sim C3-C4
 with sigma of 0.02
 C4-C4_$1 \\sim C4A-C4A_$1
 with sigma of 0.02
 C1-N1 \\sim N1-C1A
 with sigma of 0.02
 C1-C2 \\sim C2-C1A
 with sigma of 0.01
3. Rigid bond restraints
 N1, C1, C2, C3, C4, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C1A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C4A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H2BC)=Sof(H2BD)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H2AA)=Sof(H2AB)=
 FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3AA,H3AB), C3(H3BC,H3BD),
 C4(H4A,H4B), C4A(H4AA,H4AB), C1A(H1AD,H1AE)
6.b Me refined with riding coordinates:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_shelx_res_checksum              29552
_olex2_submission_special_instructions 'No special instructions were received'