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_7247633
_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         'Br8 Pb3, 2(C10 H12 N S)'
_chemical_formula_sum            'C20 H24 Br8 N2 Pb3 S2'
_chemical_formula_weight         1617.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 91.913(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8791(4)
_cell_length_b                   21.8322(14)
_cell_length_c                   17.9977(10)
_cell_measurement_reflns_used    2929
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8660
_cell_measurement_theta_min      3.0050
_cell_volume                     3486.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 (G. Sheldrick)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -53.00   35.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -37.0000  -30.0000 88

  2 omega   -3.00   85.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   37.0000  150.0000 88

  3 omega  -25.00   22.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -99.0000  120.0000 47

  4 omega   35.00   88.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000 -120.0000 53

  5 omega  -85.00  -49.00   1.0000   28.6000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -77.0000  -30.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0750795000
_diffrn_orient_matrix_UB_12      0.0062571000
_diffrn_orient_matrix_UB_13      -0.0099777000
_diffrn_orient_matrix_UB_21      0.0081234000
_diffrn_orient_matrix_UB_22      -0.0307687000
_diffrn_orient_matrix_UB_23      -0.0118533000
_diffrn_orient_matrix_UB_31      -0.0262791000
_diffrn_orient_matrix_UB_32      0.0083367000
_diffrn_orient_matrix_UB_33      -0.0362487000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.1725
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19454
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    3.081
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.591
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6330
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0274P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3025
_reflns_number_total             6330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00931a2.cif
_cod_data_source_block           cmp3
_cod_depositor_comments
'Adding full bibliography for 7247629--7247634.cif.'
_cod_database_code               7247633
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32