Regulating structural asymmetry <i>via</i> fluorination engineering in hybrid lead bromide perovskites.
Ru, Hua-Yang; Wang, Zhao-Yang; Liu, Hua-Li; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 59 (2023) 8111–8114; doi:10.1039/d3cc02098c

data_7131728
_publ_section_title
;
 Regulating structural asymmetry <i>via</i> fluorination engineering in
 hybrid lead bromide perovskites.
;
_journal_issue                   52
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8111
_journal_page_last               8114
_journal_paper_doi               10.1039/d3cc02098c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Br4 Pb, 2(C3 H7 F3 N)'
_chemical_formula_sum            'C6 H14 Br4 F6 N2 Pb'
_chemical_formula_weight         755.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-18 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2480(2)
_cell_length_b                   8.90729(7)
_cell_length_c                   7.91028(7)
_cell_measurement_reflns_used    10803
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.6090
_cell_measurement_theta_min      5.2620
_cell_volume                     1708.49(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     41.00  88.00   0.50    0.50    --    0.00  57.00   0.00   94
  2  \w    -21.00  30.00   0.50    0.50    --    0.00 -77.00   0.00  102
  3  \w    -37.00   7.00   0.50    0.50    --    0.00  82.00  60.00   88
  4  \w    -28.00   1.00   0.50    0.50    --    0.00  57.00   0.00   58
  5  \w     18.00  89.00   0.50    0.50    --    0.00  82.00  60.00  142
  6  \w    -89.00 -45.00   0.50    0.50    --    0.00 -77.00   0.00   88
  7  \w     13.00 159.00   0.50    0.50    --   98.80 -15.00 -60.00  292
  8  \w     16.00 126.00   0.50    0.50    --   98.80 -82.00 120.00  220
  9  \w     45.00  72.00   0.50    0.50    --   98.80 -15.00  90.00   54
 10  \w     61.00 134.00   0.50    0.50    --   98.80 -82.00-120.00  146
 11  \w     38.00 176.00   0.50    0.50    --   98.80  15.00   0.00  276
 12  \w     52.00 101.00   0.50    0.50    --   98.80 -82.00  30.00   98
 13  \w     16.00 135.00   0.50    0.50    --   98.80 -82.00 -90.00  238
 14  \w     19.00 136.00   0.50    0.50    --   98.80 -82.00 -60.00  234
 15  \w     66.00 100.00   0.50    0.50    --   98.80 -82.00  90.00   68
 16  \w    148.00 188.00   0.50    0.50    --   98.80  45.00  90.00   80
 17  \w     80.00 117.00   0.50    0.50    --   98.80  45.00  90.00   74
 18  \w     94.00 120.00   0.50    0.50    --   98.80 -82.00-180.00   52
 19  \w     18.00 127.00   0.50    0.50    --   98.80 -61.00 120.00  218
 20  \w     22.00  47.00   0.50    0.50    --   98.80 -82.00   0.00   50
 21  \w     96.00 126.00   0.50    0.50    --   98.80 -82.00   0.00   60
 22  \w     98.00 145.00   0.50    0.50    --   98.80 -15.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111210000
_diffrn_orient_matrix_UB_12      0.0008773000
_diffrn_orient_matrix_UB_13      -0.1916901000
_diffrn_orient_matrix_UB_21      0.0625243000
_diffrn_orient_matrix_UB_22      -0.0053244000
_diffrn_orient_matrix_UB_23      -0.0340609000
_diffrn_orient_matrix_UB_31      -0.0019807000
_diffrn_orient_matrix_UB_32      -0.1729181000
_diffrn_orient_matrix_UB_33      0.0000107000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15698
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.741
_diffrn_reflns_theta_min         5.290
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.935
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.425
_refine_diff_density_min         -4.435
_refine_diff_density_rms         0.437
_refine_ls_abs_structure_details
;
 Flack x determined using 1281 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1558P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                3223
_reflns_number_total             3382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02098c2.cif
_cod_data_source_block           hy_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7131726--7131728.cif.'
_cod_original_cell_volume        1708.49(3)
_cod_database_code               7131728
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.460
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C1AA(H1AA)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), N9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              9198
_shelx_hkl_checksum              14006
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.146
_oxdiff_exptl_absorpt_empirical_full_min 0.476