Understanding the Cubic Phase Stabilization and Crystallization Kinetics in Mixed Cations and Halides Perovskite Single Crystals.
Xie, Li-Qiang; Chen, Liang; Nan, Zi-Ang; Lin, Hai-Xin; Wang, Tan; Zhan, Dong-Ping; Yan, Jia-Wei; Mao, Bing-Wei; Tian, Zhong-Qun; Journal of the American Chemical Society 139 (2017) 3320–3323; doi:10.1021/jacs.6b12432

data_4125879
_publ_section_title
;
 Understanding the Cubic Phase Stabilization and Crystallization Kinetics
 in Mixed Cations and Halides Perovskite Single Crystals.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3320
_journal_page_last               3323
_journal_paper_doi               10.1021/jacs.6b12432
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'4(Br0.11 I0.64 Pb0.25), 6(C0.1 N0.25), 0.03(C12), 0.03(N12)'
_chemical_formula_sum            'C H5.15 Br0.45 I2.55 N1.85 Pb'
_chemical_formula_weight         611.00
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.2242(6)
_cell_length_b                   6.2242(6)
_cell_length_c                   6.2242(6)
_cell_measurement_reflns_used    540
_cell_measurement_temperature    170(6)
_cell_measurement_theta_max      28.1580
_cell_measurement_theta_min      4.6240
_cell_volume                     241.13(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(6)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -40.00   23.00   1.0000    4.7600
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   77.0000  -90.0000 63

  2 omega  -54.00   52.00   1.0000    4.7600
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   77.0000   30.0000 106

  3 omega    6.00   39.00   1.0000    4.7600
omega____ theta____ kappa____ phi______ frames
    -       22.0372   77.0000  120.0000 33
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1033988000
_diffrn_orient_matrix_UB_12      -0.0281264000
_diffrn_orient_matrix_UB_13      -0.0383103000
_diffrn_orient_matrix_UB_21      -0.0040581000
_diffrn_orient_matrix_UB_22      0.0868967000
_diffrn_orient_matrix_UB_23      -0.0738563000
_diffrn_orient_matrix_UB_31      0.0473222000
_diffrn_orient_matrix_UB_32      0.0683649000
_diffrn_orient_matrix_UB_33      0.0779382000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            877
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.439
_exptl_absorpt_correction_type   none
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    4.208
_exptl_crystal_description
;
;
_exptl_crystal_F_000             258
_refine_diff_density_max         2.145
_refine_diff_density_min         -3.325
_refine_diff_density_rms         0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         89
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0760P)^2^+1.2030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                89
_reflns_number_total             89
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12432_si_002.cif
_cod_data_source_block           e1515
_cod_original_cell_volume        241.13(7)
_cod_database_code               4125879
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Br02, I02}
{C2, N2}
2. Restrained distances
 C1_$1-N4_$2
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br02) = Uanis(I02)
Uiso(C2) = Uiso(N2)
4. Others
 Fixed Sof: Br02(0.00938) I02(0.05313) C1(0.01302) N4(0.03125) C2(0.00781)
 N2(0.00781)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'