#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:27:40 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/95/4349527.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_4349527
loop_
_publ_author_name
'Liu, Guangfeng'
'Liu, Jie'
'Tao, Xutang'
'Li, Dong-sheng'
'Zhang, Qichun'
_publ_section_title
;
 Surfactants as additives make the structures of organic--inorganic hybrid
 bromoplumbates diverse
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1388
_journal_paper_doi               10.1039/C6QI00292G
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C24 H28 Br18 N4 Pb7'
_chemical_formula_weight         3261.21
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           Triclinic'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                116.0700(10)
_cell_angle_beta                 110.7090(10)
_cell_angle_gamma                90.9180(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7421(6)
_cell_length_b                   12.9277(8)
_cell_length_c                   13.2958(8)
_cell_measurement_reflns_used    5452
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.28
_cell_volume                     1377.36(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15048
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    34.390
_exptl_absorpt_correction_T_max  0.5463
_exptl_absorpt_correction_T_min  0.0604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.191
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0066P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                4642
_reflns_number_total             5612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00292g2.cif
_cod_data_source_block           02_a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4349527
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.5000 1.0000 1.0000 0.03267(13) Uani 1 2 d S
C1 C 0.5629(12) 0.3576(9) 0.3030(10) 0.050(3) Uani 1 1 d .
H1A H 0.6400 0.3405 0.2724 0.074 Uiso 1 1 calc R
H1B H 0.5018 0.2853 0.2797 0.074 Uiso 1 1 calc R
H1C H 0.6079 0.4030 0.3905 0.074 Uiso 1 1 calc R
Br1 Br 0.19323(12) 0.87972(9) 0.79920(9) 0.0448(3) Uani 1 1 d .
Pb2 Pb 0.59227(3) 0.88588(3) 0.58425(3) 0.02744(10) Uani 1 1 d .
C2 C 0.5252(11) 0.4836(8) 0.2081(8) 0.037(2) Uani 1 1 d .
H2 H 0.6216 0.4807 0.2106 0.044 Uiso 1 1 calc R
Br2 Br 0.67174(12) 0.94968(10) 0.84030(9) 0.0462(3) Uani 1 1 d .
Pb3 Pb 0.76344(4) 0.94046(3) 0.32303(3) 0.03482(11) Uani 1 1 d .
C3 C 0.4398(10) 0.5489(8) 0.1592(8) 0.033(2) Uani 1 1 d .
H3 H 0.4796 0.5893 0.1294 0.040 Uiso 1 1 calc R
Br3 Br 0.27455(10) 0.78464(9) 0.50503(10) 0.0435(3) Uani 1 1 d .
Pb4 Pb 0.98851(4) 0.69541(3) 0.52401(3) 0.03664(11) Uani 1 1 d .
C4 C 0.2960(9) 0.5537(8) 0.1548(8) 0.031(2) Uani 1 1 d .
Br4 Br 0.89617(10) 0.97623(9) 0.59577(9) 0.0400(2) Uani 1 1 d .
C12 C -0.0374(12) 0.8478(10) -0.0146(11) 0.057(3) Uani 1 1 d .
H12A H -0.1344 0.8415 -0.0123 0.086 Uiso 1 1 calc R
H12B H -0.0489 0.8255 -0.0967 0.086 Uiso 1 1 calc R
H12C H 0.0173 0.9275 0.0386 0.086 Uiso 1 1 calc R
Br5 Br 0.47969(9) 0.86632(7) 0.33008(8) 0.0293(2) Uani 1 1 d .
C5 C 0.2459(11) 0.4938(9) 0.2020(9) 0.042(2) Uani 1 1 d .
H5 H 0.1503 0.4964 0.2016 0.051 Uiso 1 1 calc R
Br6 Br 0.68743(10) 0.65969(8) 0.52682(9) 0.0382(2) Uani 1 1 d .
C6 C 0.3282(11) 0.4314(9) 0.2491(9) 0.044(3) Uani 1 1 d .
H6 H 0.2894 0.3921 0.2804 0.053 Uiso 1 1 calc R
Br7 Br 0.59130(11) 0.79511(8) 0.04647(9) 0.0401(2) Uani 1 1 d .
C7 C 0.2067(9) 0.6260(8) 0.1081(8) 0.031(2) Uani 1 1 d .
Br8 Br 0.82620(10) 0.70979(8) 0.28509(9) 0.0352(2) Uani 1 1 d .
C8 C 0.2305(11) 0.6510(9) 0.0246(9) 0.039(2) Uani 1 1 d .
H8 H 0.3012 0.6194 -0.0057 0.047 Uiso 1 1 calc R
N13 N 0.4690(8) 0.4252(7) 0.2513(7) 0.0376(19) Uani 1 1 d .
Br9 Br 0.96025(11) 0.45560(8) 0.33573(9) 0.0417(2) Uani 1 1 d .
C9 C 0.1494(11) 0.7230(9) -0.0149(9) 0.043(3) Uani 1 1 d .
H9 H 0.1672 0.7399 -0.0708 0.051 Uiso 1 1 calc R
N14 N 0.0464(8) 0.7683(7) 0.0265(7) 0.039(2) Uani 1 1 d .
C11 C 0.0981(10) 0.6734(9) 0.1484(9) 0.043(3) Uani 1 1 d .
H11 H 0.0786 0.6575 0.2044 0.052 Uiso 1 1 calc R
C10 C 0.0198(11) 0.7427(9) 0.1073(9) 0.045(3) Uani 1 1 d .
H10 H -0.0533 0.7732 0.1350 0.054 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 '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'
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 179.999(1) . 2_677
Br1 Pb1 Br2 97.54(3) . .
Br1 Pb1 Br2 82.46(3) 2_677 .
Br1 Pb1 Br2 82.46(3) . 2_677
Br1 Pb1 Br2 97.54(3) 2_677 2_677
Br2 Pb1 Br2 180.0 . 2_677
Br1 Pb1 Br7 99.32(3) . 1_556
Br1 Pb1 Br7 80.68(3) 2_677 1_556
Br2 Pb1 Br7 90.08(3) . 1_556
Br2 Pb1 Br7 89.92(3) 2_677 1_556
Br1 Pb1 Br7 80.68(3) . 2_676
Br1 Pb1 Br7 99.33(3) 2_677 2_676
Br2 Pb1 Br7 89.92(3) . 2_676
Br2 Pb1 Br7 90.08(3) 2_677 2_676
Br7 Pb1 Br7 180.00(4) 1_556 2_676
N13 C1 H1A 109.5 . .
N13 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N13 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Pb1 Br1 Pb4 149.58(4) . 1_455
Br2 Pb2 Br6 93.51(3) . .
Br2 Pb2 Br3 94.31(3) . .
Br6 Pb2 Br3 94.27(3) . .
Br2 Pb2 Br5 167.63(3) . .
Br6 Pb2 Br5 98.74(3) . .
Br3 Pb2 Br5 83.12(3) . .
Br2 Pb2 Br5 81.85(3) . 2_676
Br6 Pb2 Br5 174.11(3) . 2_676
Br3 Pb2 Br5 89.71(3) . 2_676
Br5 Pb2 Br5 86.02(2) . 2_676
Br2 Pb2 Br4 100.77(3) . .
Br6 Pb2 Br4 85.76(3) . .
Br3 Pb2 Br4 164.89(3) . .
Br5 Pb2 Br4 81.95(3) . .
Br5 Pb2 Br4 91.52(3) 2_676 .
N13 C2 C3 120.3(9) . .
N13 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
Pb2 Br2 Pb1 134.64(4) . .
Br8 Pb3 Br5 87.37(3) . .
Br8 Pb3 Br7 79.43(3) . .
Br5 Pb3 Br7 83.82(3) . .
Br8 Pb3 Br4 87.27(3) . 2_776
Br5 Pb3 Br4 160.16(3) . 2_776
Br7 Pb3 Br4 113.88(3) . 2_776
Br8 Pb3 Br4 77.97(3) . .
Br5 Pb3 Br4 81.65(2) . .
Br7 Pb3 Br4 153.57(3) . .
Br4 Pb3 Br4 78.55(3) 2_776 .
C4 C3 C2 120.3(9) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
Pb2 Br3 Pb4 158.17(4) . 1_455
Br9 Pb4 Br6 96.91(3) . .
Br9 Pb4 Br8 77.94(3) . .
Br6 Pb4 Br8 86.84(3) . .
Br9 Pb4 Br3 91.25(3) . 1_655
Br6 Pb4 Br3 165.02(3) . 1_655
Br8 Pb4 Br3 82.60(3) . 1_655
Br9 Pb4 Br1 141.19(3) . 1_655
Br6 Pb4 Br1 103.55(3) . 1_655
Br8 Pb4 Br1 135.12(3) . 1_655
Br3 Pb4 Br1 77.08(3) 1_655 1_655
Br9 Pb4 Br9 75.87(3) . 2_766
Br6 Pb4 Br9 79.30(3) . 2_766
Br8 Pb4 Br9 148.50(3) . 2_766
Br3 Pb4 Br9 115.00(3) 1_655 2_766
Br1 Pb4 Br9 76.03(3) 1_655 2_766
C5 C4 C3 116.6(9) . .
C5 C4 C7 122.3(8) . .
C3 C4 C7 121.0(8) . .
Pb2 Br4 Pb3 163.05(4) . 2_776
Pb2 Br4 Pb3 95.11(3) . .
Pb3 Br4 Pb3 101.45(3) 2_776 .
N14 C12 H12A 109.5 . .
N14 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N14 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Pb3 Br5 Pb2 101.19(3) . .
Pb3 Br5 Pb2 93.72(3) . 2_676
Pb2 Br5 Pb2 93.98(2) . 2_676
C6 C5 C4 122.9(9) . .
C6 C5 H5 118.5 . .
C4 C5 H5 118.5 . .
Pb2 Br6 Pb4 106.20(3) . .
C5 C6 N13 120.3(9) . .
C5 C6 H6 119.9 . .
N13 C6 H6 119.9 . .
Pb1 Br7 Pb3 96.64(3) 1_554 .
C8 C7 C11 117.5(9) . .
C8 C7 C4 121.1(8) . .
C11 C7 C4 121.5(8) . .
Pb3 Br8 Pb4 114.31(3) . .
C7 C8 C9 120.4(9) . .
C7 C8 H8 119.8 . .
C9 C8 H8 119.8 . .
C2 N13 C6 119.5(9) . .
C2 N13 C1 118.8(8) . .
C6 N13 C1 121.6(8) . .
Pb4 Br9 Pb4 104.13(3) . 2_766
N14 C9 C8 120.8(9) . .
N14 C9 H9 119.6 . .
C8 C9 H9 119.6 . .
C9 N14 C10 119.5(9) . .
C9 N14 C12 120.2(9) . .
C10 N14 C12 120.3(9) . .
C10 C11 C7 120.8(10) . .
C10 C11 H11 119.6 . .
C7 C11 H11 119.6 . .
N14 C10 C11 121.0(9) . .
N14 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br1 3.0061(10) .
Pb1 Br1 3.0061(10) 2_677
Pb1 Br2 3.0107(10) .
Pb1 Br2 3.0107(10) 2_677
Pb1 Br7 3.0519(10) 1_556
Pb1 Br7 3.0520(10) 2_676
C1 N13 1.478(12) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
Br1 Pb4 3.1728(10) 1_455
Pb2 Br2 2.9185(10) .
Pb2 Br6 2.9356(10) .
Pb2 Br3 2.9591(10) .
Pb2 Br5 3.0505(10) .
Pb2 Br5 3.0791(9) 2_676
Pb2 Br4 3.0926(10) .
C2 N13 1.338(12) .
C2 C3 1.396(13) .
C2 H2 0.9300 .
Pb3 Br8 2.9113(10) .
Pb3 Br5 2.9574(9) .
Pb3 Br7 3.0543(10) .
Pb3 Br4 3.1070(9) 2_776
Pb3 Br4 3.1978(11) .
C3 C4 1.384(11) .
C3 H3 0.9300 .
Br3 Pb4 3.1319(10) 1_455
Pb4 Br9 2.9356(10) .
Pb4 Br6 2.9779(10) .
Pb4 Br8 3.0986(11) .
Pb4 Br3 3.1320(10) 1_655
Pb4 Br1 3.1728(10) 1_655
Pb4 Br9 3.1798(11) 2_766
C4 C5 1.366(13) .
C4 C7 1.474(13) .
Br4 Pb3 3.1070(9) 2_776
C12 N14 1.493(13) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
Br5 Pb2 3.0791(9) 2_676
C5 C6 1.339(14) .
C5 H5 0.9300 .
C6 N13 1.366(12) .
C6 H6 0.9300 .
Br7 Pb1 3.0520(10) 1_554
C7 C8 1.373(12) .
C7 C11 1.384(11) .
C8 C9 1.388(13) .
C8 H8 0.9300 .
Br9 Pb4 3.1798(11) 2_766
C9 N14 1.333(11) .
C9 H9 0.9300 .
N14 C10 1.354(12) .
C11 C10 1.358(14) .
C11 H11 0.9300 .
C10 H10 0.9300 .
