#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:27:40 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/95/4349528.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_4349528
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 Br10 N4 Pb3'
_chemical_formula_weight         1793.17
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_H-M   'C 1 2/m 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                90.00
_cell_angle_beta                 110.850(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.748(3)
_cell_length_b                   9.5035(16)
_cell_length_c                   12.453(2)
_cell_measurement_reflns_used    1493
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.32
_cell_volume                     2073.5(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5952
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    21.805
_exptl_absorpt_correction_T_max  0.3187
_exptl_absorpt_correction_T_min  0.0818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.415
_refine_diff_density_min         -2.821
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0485P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                1713
_reflns_number_total             2243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00292g2.cif
_cod_data_source_block           02_a
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4349528
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.7622(8) 0.5000 0.0308(11) 0.053(4) Uani 1 2 d S
H1A H 0.7607 0.5951 0.0040 0.079 Uiso 0.50 1 calc PR
H1B H 0.7129 0.4575 -0.0044 0.079 Uiso 0.50 1 calc PR
H1C H 0.7994 0.4474 0.0108 0.079 Uiso 0.50 1 calc PR
Pb1 Pb 0.54176(3) 0.5000 0.69566(4) 0.0358(2) Uani 1 2 d S
Br1 Br 0.69934(8) 0.5000 0.72047(13) 0.0446(4) Uani 1 2 d S
C8 C 0.9163(11) 0.5000 0.8802(12) 0.065(5) Uani 1 2 d S
H8A H 0.9115 0.5932 0.9066 0.097 Uiso 0.50 1 calc PR
H8B H 0.9687 0.4705 0.9123 0.097 Uiso 0.50 1 calc PR
H8C H 0.8850 0.4363 0.9039 0.097 Uiso 0.50 1 calc PR
C7 C 0.8789(7) 0.3811(12) 0.6967(9) 0.052(3) Uani 1 1 d .
H7 H 0.8856 0.2970 0.7373 0.062 Uiso 1 1 calc R
C6 C 0.8567(6) 0.3766(11) 0.5810(9) 0.046(3) Uani 1 1 d .
H6 H 0.8494 0.2902 0.5435 0.055 Uiso 1 1 calc R
N1 N 0.7831(6) 0.5000 0.1571(9) 0.036(3) Uani 1 2 d S
Br2 Br 0.5000 0.29150(16) 0.5000 0.0512(4) Uani 1 2 d S
C2 C 0.7924(6) 0.3773(11) 0.2146(9) 0.046(3) Uani 1 1 d .
H2 H 0.7852 0.2928 0.1744 0.055 Uiso 1 1 calc R
Pb2 Pb 0.5000 0.5000 1.0000 0.0416(2) Uani 1 4 d S
N2 N 0.8914(6) 0.5000 0.7535(9) 0.037(3) Uani 1 2 d S
Br3 Br 0.57649(7) 0.71818(12) 0.89773(10) 0.0536(3) Uani 1 1 d .
C3 C 0.8118(6) 0.3756(11) 0.3296(9) 0.045(3) Uani 1 1 d .
H3 H 0.8174 0.2900 0.3679 0.054 Uiso 1 1 calc R
Br4 Br 0.61282(9) 0.5000 1.24508(19) 0.0718(6) Uani 1 2 d S
C4 C 0.8237(7) 0.5000 0.3911(10) 0.029(3) Uani 1 2 d S
C5 C 0.8448(7) 0.5000 0.5179(11) 0.032(3) Uani 1 2 d S
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
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Br1 Pb1 Br2 92.77(3) . .
Br1 Pb1 Br2 92.77(3) . 5_666
Br2 Pb1 Br2 82.02(5) . 5_666
Br1 Pb1 Br3 90.10(3) . 6_565
Br2 Pb1 Br3 97.67(4) . 6_565
Br2 Pb1 Br3 177.12(3) 5_666 6_565
Br1 Pb1 Br3 90.11(3) . .
Br2 Pb1 Br3 177.12(3) . .
Br2 Pb1 Br3 97.67(4) 5_666 .
Br3 Pb1 Br3 82.50(5) 6_565 .
Br1 Pb1 Br4 161.90(5) . 5_667
Br2 Pb1 Br4 100.84(3) . 5_667
Br2 Pb1 Br4 100.84(3) 5_666 5_667
Br3 Pb1 Br4 76.39(4) 6_565 5_667
Br3 Pb1 Br4 76.39(4) . 5_667
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C7 C6 122.1(11) . .
N2 C7 H7 119.0 . .
C6 C7 H7 119.0 . .
C7 C6 C5 120.3(11) . .
C7 C6 H6 119.8 . .
C5 C6 H6 119.8 . .
C2 N1 C2 119.9(12) 6_565 .
C2 N1 C1 120.0(6) 6_565 .
C2 N1 C1 120.0(6) . .
Pb1 Br2 Pb1 97.98(5) . 5_666
N1 C2 C3 120.7(11) . .
N1 C2 H2 119.6 . .
C3 C2 H2 119.6 . .
Br4 Pb2 Br4 180.0 . 5_667
Br4 Pb2 Br3 80.95(4) . 5_667
Br4 Pb2 Br3 99.05(4) 5_667 5_667
Br4 Pb2 Br3 99.05(4) . .
Br4 Pb2 Br3 80.95(4) 5_667 .
Br3 Pb2 Br3 180.00(4) 5_667 .
Br4 Pb2 Br3 99.05(4) . 6_565
Br4 Pb2 Br3 80.95(4) 5_667 6_565
Br3 Pb2 Br3 94.20(4) 5_667 6_565
Br3 Pb2 Br3 85.80(4) . 6_565
Br4 Pb2 Br3 80.95(4) . 2_657
Br4 Pb2 Br3 99.05(4) 5_667 2_657
Br3 Pb2 Br3 85.80(4) 5_667 2_657
Br3 Pb2 Br3 94.20(4) . 2_657
Br3 Pb2 Br3 180.0 6_565 2_657
C7 N2 C7 119.4(13) 6_565 .
C7 N2 C8 120.3(6) 6_565 .
C7 N2 C8 120.3(6) . .
Pb2 Br3 Pb1 83.77(3) . .
C2 C3 C4 120.6(10) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
Pb2 Br4 Pb1 82.47(4) . 5_667
C3 C4 C3 117.4(12) 6_565 .
C3 C4 C5 121.2(6) 6_565 .
C3 C4 C5 121.2(6) . .
C6 C5 C6 115.8(12) . 6_565
C6 C5 C4 122.1(6) . .
C6 C5 C4 122.1(6) 6_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.479(16) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
Pb1 Br1 2.8591(15) .
Pb1 Br2 3.0197(12) .
Pb1 Br2 3.0197(12) 5_666
Pb1 Br3 3.1446(12) 6_565
Pb1 Br3 3.1447(12) .
Pb1 Br4 3.2352(19) 5_667
C8 N2 1.477(17) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C7 N2 1.310(12) .
C7 C6 1.350(14) .
C7 H7 0.9300 .
C6 C5 1.385(12) .
C6 H6 0.9300 .
N1 C2 1.347(11) 6_565
N1 C2 1.347(11) .
Br2 Pb1 3.0197(11) 5_666
C2 C3 1.346(14) .
C2 H2 0.9300 .
Pb2 Br4 3.032(2) .
Pb2 Br4 3.032(2) 5_667
Pb2 Br3 3.0460(11) 5_667
Pb2 Br3 3.0460(11) .
Pb2 Br3 3.0460(11) 6_565
Pb2 Br3 3.0461(11) 2_657
N2 C7 1.310(12) 6_565
C3 C4 1.384(11) .
C3 H3 0.9300 .
Br4 Pb1 3.2352(19) 5_667
C4 C3 1.384(11) 6_565
C4 C5 1.484(17) .
C5 C6 1.385(12) 6_565
