Regulating the crystal and electronic structures and optical properties of hybrid bromoplumbates with alkylated N, S- or P-containing aromatic cations
Gao, Cheng-Cheng; Tang, Xue-Na; Miao, Jing-Ling; Li, Yu; Li, Cuncheng; Liu, Guang-Ning; CrystEngComm 25 (2023) 6556–6567; doi:10.1039/D3CE00931A

data_7247629
_publ_section_title
;
 Regulating the crystal and electronic structures and optical properties
 of hybrid bromoplumbates with alkylated N, S- or P-containing aromatic
 cations
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6556
_journal_page_last               6567
_journal_paper_doi               10.1039/D3CE00931A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Br3 Pb, C8 H8 N S'
_chemical_formula_sum            'C8 H8 Br3 N Pb S'
_chemical_formula_weight         597.13
_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     direct
_audit_creation_date             2023-09-20
_audit_creation_method
;
FinalCif V106 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7383(4)
_cell_length_b                   11.5787(7)
_cell_length_c                   14.7269(12)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5100
_cell_measurement_theta_min      3.2240
_cell_volume                     1319.52(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     35.00  88.00   1.00   20.00    --   15.86 178.00  90.00   53
  2  \w     41.00  88.00   1.00   20.00    --   15.86 178.00 -90.00   47
  3  \w     35.00  80.00   1.00   20.00    --   15.86 178.00-180.00   45
  4  \w    -24.00  13.00   1.00   20.00    --  -16.95 -99.00 -90.00   37
  5  \w     15.00  55.00   1.00   20.00    --   15.70 -99.00  30.00   40
  6  \w    -11.00  42.00   1.00   20.00    --   15.70  77.00-180.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0766429000
_diffrn_orient_matrix_UB_12      -0.0300414000
_diffrn_orient_matrix_UB_13      0.0119650000
_diffrn_orient_matrix_UB_21      0.0443052000
_diffrn_orient_matrix_UB_22      0.0267179000
_diffrn_orient_matrix_UB_23      -0.0366035000
_diffrn_orient_matrix_UB_31      0.0239828000
_diffrn_orient_matrix_UB_32      0.0462200000
_diffrn_orient_matrix_UB_33      0.0288766000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6548
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.338
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    21.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.006
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.290
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.280
_refine_ls_abs_structure_details
;
 Flack x determined using 468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0394P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1541
_reflns_number_total             2397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00931a2.cif
_cod_data_source_block           cmp1
_cod_depositor_comments
'Adding full bibliography for 7247629--7247634.cif.'
_cod_database_code               7247629
_chemical_oxdiff_formula         'C H N S Br Pb'
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 6.163
_oxdiff_exptl_absorpt_empirical_full_min 0.451
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32