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_7131727
_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 2bc 2'
_space_group_name_H-M_alt        'P 2 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-03-16
_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                   7.9087(2)
_cell_length_b                   8.9042(3)
_cell_length_c                   24.2405(8)
_cell_measurement_reflns_used    3869
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      3.6220
_cell_volume                     1707.03(9)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_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    -89.00  29.00   0.50    0.50    --    0.00 -38.00  60.00  236
  2  \w     84.00 181.00   0.50    0.50    --   98.80  45.00-180.00  194
  3  \w     10.00  43.00   0.50    0.50    --   98.80 -82.00-120.00   66
  4  \w     79.00 116.00   0.50    0.50    --   98.80  45.00  60.00   74
  5  \w    156.00 181.00   0.50    0.50    --   98.80  45.00  60.00   50
  6  \w     76.00 188.00   0.50    0.50    --   98.80  45.00 150.00  224
  7  \w     48.00 100.00   0.50    0.50    --   98.80 -61.00-120.00  104
  8  \w     46.00 129.00   0.50    0.50    --   98.80 -82.00-120.00  166
  9  \w     69.00 136.00   0.50    0.50    --   98.80 -82.00 -60.00  134
 10  \w      9.00  42.00   0.50    0.50    --   98.80 -61.00-120.00   66
;
_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      -0.0517166000
_diffrn_orient_matrix_UB_12      0.0258416000
_diffrn_orient_matrix_UB_13      -0.1093793000
_diffrn_orient_matrix_UB_21      0.0365941000
_diffrn_orient_matrix_UB_22      0.0576008000
_diffrn_orient_matrix_UB_23      -0.1452909000
_diffrn_orient_matrix_UB_31      0.0048666000
_diffrn_orient_matrix_UB_32      -0.1611744000
_diffrn_orient_matrix_UB_33      -0.0696384000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.784
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17019
_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    2.938
_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         2.925
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.406
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1044P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                2961
_reflns_number_total             3291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02098c2.cif
_cod_data_source_block           hy_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7131726--7131728.cif.'
_cod_database_code               7131727
_shelx_shelxl_version_number     2016/4
_reflns_odcompleteness_completeness 99.61
_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:
 C5(H5), C9(H9)
2.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c), N3(H3a,H3b,H3c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              35095
_shelx_hkl_checksum              45816
_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 3.040
_oxdiff_exptl_absorpt_empirical_full_min 0.332