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_7131726
_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         'Br5 Pb, 3(C3 H10 N)'
_chemical_formula_sum            'C9 H30 Br5 N3 Pb'
_chemical_formula_weight         787.10
_chemical_name_systematic        (C3H10N)3PbBr5
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-03-18
_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                   8.6172(3)
_cell_length_b                   11.8062(5)
_cell_length_c                   21.5472(9)
_cell_measurement_reflns_used    4980
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.7000
_cell_measurement_theta_min      2.7730
_cell_volume                     2192.13(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_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     17.00  97.00   0.50    0.80    --    7.30  82.00-120.00  160
  2  \w    -12.00  84.00   0.50    0.80    --    7.30  57.00-150.00  192
  3  \w    -27.00  -2.00   0.50    0.80    --    7.30  82.00-120.00   50
;
_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      0.0020363000
_diffrn_orient_matrix_UB_12      0.0471881000
_diffrn_orient_matrix_UB_13      0.0203705000
_diffrn_orient_matrix_UB_21      -0.0236409000
_diffrn_orient_matrix_UB_22      -0.0352364000
_diffrn_orient_matrix_UB_23      0.0249087000
_diffrn_orient_matrix_UB_31      0.0788415000
_diffrn_orient_matrix_UB_32      -0.0117814000
_diffrn_orient_matrix_UB_33      0.0069543000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12421
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.874
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17576
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.349
_refine_diff_density_min         -2.151
_refine_diff_density_rms         0.553
_refine_ls_abs_structure_details
;
 Flack x determined using 1567 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0640P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.772
_reflns_number_gt                4294
_reflns_number_total             4853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02098c2.cif
_cod_data_source_block           hy
_cod_depositor_comments
'Adding full bibliography for 7131726--7131728.cif.'
_cod_database_code               7131726
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.633
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N3-C9A = N3-C9B = N2-C5 = N1-C2
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H8BD(0.5) H8BE(0.5) H8BF(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
 H3BD(0.5) H3BE(0.5) H3BF(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) H7AA(0.5)
 H7AB(0.5) H7AC(0.5) H7BE(0.5) H7BF(0.5) H7BD(0.5) C9B(0.5) H9B(0.5) C9A(0.5)
 H9A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C9B(H9B), C9A(H9A)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8BD,H8BE,H8BF), C8(H8AA,H8AB,H8AC), N1(H1A,H1B,H1C),
 C4(H4A,H4B,H4C), C1(H1D,H1E,H1F), N3(H3BD,H3BE,H3BF), N3(H3AA,H3AB,H3AC),
 C7(H7AA,H7AB,H7AC), C7(H7BE,H7BF,H7BD), C6(H6A,H6B,H6C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              76195
_shelx_hkl_checksum              53986
_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 3.663
_oxdiff_exptl_absorpt_empirical_full_min 0.684