#------------------------------------------------------------------------------
#$Date: 2022-09-22 12:45:20 +0300 (Thu, 22 Sep 2022) $
#$Revision: 278084 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/58/8105841.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8105841
loop_
_publ_author_name
'Zhang, Hui'
'Yu, Shan Shan'
_publ_section_title
;
 The crystal structure of 3-butyl-1-methyl-1H-imidazol-3-ium
 catena-poly[tris(μ2-bromido-κ 2 Br:Br)lead(II)], C8H15Br3N2Pb
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für 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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -55.00  40.00   1.00    4.00    --   11.74 -57.00  60.00   95
  2  ω    -14.00  77.00   1.00    4.00    --   11.74  77.00 -30.00   91
  3  ω    -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       'ω 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/[σ²(Fo²)+(0.0304P)²] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0093_suppl.cif
_cod_data_source_block           3_1223
_cod_database_code               8105841
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.33382(5) 0.24408(6) 0.50211(2) 0.01423(17) Uani 1 1 d . . . . .
Br1 Br 0.54694(15) 0.45583(17) 0.43895(8) 0.0187(4) Uani 1 1 d . . . . .
Br2 Br 0.09795(17) 0.45597(16) 0.55817(8) 0.0182(3) Uani 1 1 d . . . . .
Br3 Br 0.09135(16) 0.22871(16) 0.37833(7) 0.0185(3) Uani 1 1 d . . . . .
N1 N 0.6359(12) 0.7536(15) 0.5853(5) 0.020(3) Uani 1 1 d . . . . .
N2 N 0.4319(13) 0.7094(13) 0.6591(6) 0.018(3) Uani 1 1 d . . . . .
C1 C 0.5374(16) 0.6547(17) 0.6133(7) 0.020(3) Uani 1 1 d . U . . .
H1 H 0.542903 0.561707 0.602002 0.024 Uiso 1 1 calc R . . . .
C2 C 0.5882(18) 0.8742(17) 0.6157(8) 0.026(4) Uani 1 1 d . . . . .
H2 H 0.634296 0.960579 0.606330 0.032 Uiso 1 1 calc R . . . .
C3 C 0.4625(19) 0.8463(17) 0.6617(8) 0.026(4) Uani 1 1 d . . . . .
H3 H 0.406692 0.909744 0.690163 0.032 Uiso 1 1 calc R . . . .
C4 C 0.3096(17) 0.6299(17) 0.7024(7) 0.022(4) Uani 1 1 d . . . . .
H4A H 0.358477 0.615889 0.748453 0.026 Uiso 1 1 calc R . . . .
H4B H 0.291242 0.540174 0.681432 0.026 Uiso 1 1 calc R . . . .
C5 C 0.1382(17) 0.7040(18) 0.7092(8) 0.030(4) Uani 1 1 d . . . . .
H5A H 0.154443 0.788331 0.735542 0.035 Uiso 1 1 calc R . . . .
H5B H 0.096720 0.728650 0.663143 0.035 Uiso 1 1 calc R . . . .
C6 C 0.0050(19) 0.6155(17) 0.7455(8) 0.028(4) Uani 1 1 d . . . . .
H6A H 0.053202 0.580519 0.788673 0.033 Uiso 1 1 calc R . . . .
H6B H -0.021973 0.537256 0.716004 0.033 Uiso 1 1 calc R . . . .
C7 C -0.1607(18) 0.694(2) 0.7618(8) 0.040(5) Uani 1 1 d . . . . .
H7A H -0.207158 0.731123 0.719464 0.060 Uiso 1 1 calc GR . . . .
H7B H -0.136433 0.766876 0.793916 0.060 Uiso 1 1 calc GR . . . .
H7C H -0.242668 0.631652 0.782273 0.060 Uiso 1 1 calc GR . . . .
C8 C 0.7672(17) 0.7352(18) 0.5319(7) 0.027(4) Uani 1 1 d . . . . .
H8A H 0.726309 0.771364 0.488349 0.041 Uiso 1 1 calc GR . . . .
H8B H 0.792143 0.638949 0.526751 0.041 Uiso 1 1 calc GR . . . .
H8C H 0.869838 0.783220 0.545482 0.041 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br1 Pb1 Br1 169.98(4) . 4_456
Br1 Pb1 Br2 90.72(4) . .
Br1 Pb1 Br2 84.79(4) . 4_556
Br1 Pb1 Br3 93.67(4) . .
Br1 Pb1 Br3 82.93(4) . 4_556
Br2 Pb1 Br1 81.96(4) . 4_456
Br2 Pb1 Br1 102.63(4) 4_556 4_456
Br2 Pb1 Br2 175.37(4) . 4_556
Br2 Pb1 Br3 94.26(4) . 4_556
Br2 Pb1 Br3 86.13(4) . .
Br3 Pb1 Br1 104.35(4) 4_556 4_456
Br3 Pb1 Br1 79.07(4) . 4_456
Br3 Pb1 Br2 84.11(4) 4_556 4_556
Br3 Pb1 Br2 95.24(4) . 4_556
Br3 Pb1 Br3 176.58(3) . 4_556
Pb1 Br1 Pb1 79.60(4) . 4_556
Pb1 Br2 Pb1 80.64(4) . 4_456
Pb1 Br3 Pb1 79.47(3) . 4_456
C1 N1 C2 106.9(12) . .
C1 N1 C8 126.4(15) . .
C2 N1 C8 126.7(14) . .
C1 N2 C3 108.2(13) . .
C1 N2 C4 124.4(13) . .
C3 N2 C4 127.3(13) . .
N1 C1 H1 125.2 . .
N2 C1 N1 109.6(14) . .
N2 C1 H1 125.2 . .
N1 C2 H2 126.1 . .
C3 C2 N1 107.8(14) . .
C3 C2 H2 126.1 . .
N2 C3 H3 126.2 . .
C2 C3 N2 107.6(14) . .
C2 C3 H3 126.2 . .
N2 C4 H4A 109.4 . .
N2 C4 H4B 109.4 . .
N2 C4 C5 111.4(13) . .
H4A C4 H4B 108.0 . .
C5 C4 H4A 109.4 . .
C5 C4 H4B 109.4 . .
C4 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
H5A C5 H5B 107.9 . .
C6 C5 C4 111.7(14) . .
C6 C5 H5A 109.3 . .
C6 C5 H5B 109.3 . .
C5 C6 H6A 109.0 . .
C5 C6 H6B 109.0 . .
C5 C6 C7 112.9(14) . .
H6A C6 H6B 107.8 . .
C7 C6 H6A 109.0 . .
C7 C6 H6B 109.0 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
N1 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br1 2.9055(16) .
Pb1 Br1 3.1662(15) 4_456
Pb1 Br2 3.0544(15) 4_556
Pb1 Br2 2.9589(16) .
Pb1 Br3 3.0334(13) .
Pb1 Br3 3.0543(14) 4_556
N1 C1 1.340(19) .
N1 C2 1.360(19) .
N1 C8 1.457(15) .
N2 C1 1.314(18) .
N2 C3 1.35(2) .
N2 C4 1.479(18) .
C1 H1 0.9300 .
C2 H2 0.9300 .
C2 C3 1.34(2) .
C3 H3 0.9300 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.52(2) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C6 1.51(2) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.53(2) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
