The crystal structure of 3-butyl-1-methyl-1H-imidazol-3-ium catena-poly[tris(μ2-bromido-κ 2 Br:Br)lead(II)], C8H15Br3N2Pb
Zhang, Hui; Yu, Shan Shan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 757–759; doi:10.1515/ncrs-2019-0093

data_8105841
_publ_section_title
;
 The crystal structure of 3-butyl-1-methyl-1H-imidazol-3-ium
 catena-poly[tris(\m2-bromido-\k 2 Br:Br)lead(II)], C8H15Br3N2Pb
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              757
_journal_page_last               759
_journal_paper_doi               10.1515/ncrs-2019-0093
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'Br3 Pb, C8 H15 N2'
_chemical_formula_sum            'C8 H15 Br3 N2 Pb'
_chemical_formula_weight         586.14
_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     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7781(9)
_cell_length_b                   9.7129(15)
_cell_length_c                   19.158(2)
_cell_measurement_reflns_used    3570
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8520
_cell_measurement_theta_min      2.3410
_cell_volume                     1447.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f(Rigaku OD,2015)[1]'
_computing_data_collection       'CrysAlisPro 1.171.38.43f(Rigaku OD,2015)[1]'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f(Rigaku OD,2015)[1]'
_computing_molecular_graphics    'Diamond 4.0   [4]'
_computing_publication_material  'ShelXL (Sheldrick, 2015)    [3]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)   [3]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)      [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -55.00  40.00   1.00    4.00    --   11.74 -57.00  60.00   95
  2  \w    -14.00  77.00   1.00    4.00    --   11.74  77.00 -30.00   91
  3  \w    -12.00  85.00   1.00    4.00    --   11.74  57.00-150.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0389791000
_diffrn_orient_matrix_UB_12      0.0484763000
_diffrn_orient_matrix_UB_13      0.0226030000
_diffrn_orient_matrix_UB_21      0.0341193000
_diffrn_orient_matrix_UB_22      0.0544355000
_diffrn_orient_matrix_UB_23      -0.0204217000
_diffrn_orient_matrix_UB_31      -0.0752453000
_diffrn_orient_matrix_UB_32      -0.0006057000
_diffrn_orient_matrix_UB_33      -0.0210129000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9348
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.126
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (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    2.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.463
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.239
_refine_ls_abs_structure_details
;
 Flack x determined using 834 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0304P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2311
_reflns_number_total             2555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0093_suppl.cif
_cod_data_source_block           3_1223
_cod_database_code               8105841
_shelx_estimated_absorpt_t_max   0.241
_shelx_estimated_absorpt_t_min   0.199
_reflns_odcompleteness_completeness 99.94
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              18925
_shelx_hkl_checksum              31036
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.598