#------------------------------------------------------------------------------
#$Date: 2019-11-23 19:27:40 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234856 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/95/4349525.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_4349525
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            'C6 H7 Br3 N Pb'
_chemical_formula_weight         540.05
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.093(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.3566(7)
_cell_length_b                   21.531(3)
_cell_length_c                   11.0429(17)
_cell_measurement_reflns_used    5984
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.64
_cell_volume                     1035.7(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11594
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    27.805
_exptl_absorpt_correction_T_max  0.1250
_exptl_absorpt_correction_T_min  0.0255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.403
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0273
_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)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                2090
_reflns_number_total             2383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00292g2.cif
_cod_data_source_block           02_a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4349525
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.67980(4) 0.399085(9) 0.520678(18) 0.03185(9) Uani 1 1 d .
N1 N 0.8477(9) 0.3531(2) 0.9849(4) 0.0284(10) Uani 1 1 d .
C1 C 0.9757(16) 0.2900(3) 0.9740(6) 0.0449(15) Uani 1 1 d .
H1 H 0.8262 0.2633 0.9359 0.067 Uiso 1 1 calc R
H00C H 1.0272 0.2742 1.0532 0.067 Uiso 1 1 calc R
H00D H 1.1569 0.2913 0.9260 0.067 Uiso 1 1 calc R
Br1 Br 0.21649(13) 0.35404(3) 0.35269(5) 0.03735(15) Uani 1 1 d .
Br2 Br 0.49648(15) 0.30619(3) 0.68950(6) 0.04431(17) Uani 1 1 d .
C2 C 0.6718(13) 0.3677(3) 1.0799(5) 0.0344(12) Uani 1 1 d .
H2 H 0.6424 0.3385 1.1407 0.041 Uiso 1 1 calc R
C5 C 0.7613(11) 0.4528(2) 0.9012(4) 0.0268(10) Uani 1 1 d .
H5 H 0.7962 0.4812 0.8394 0.032 Uiso 1 1 calc R
C4 C 0.5761(11) 0.4692(2) 0.9971(4) 0.0235(10) Uani 1 1 d .
Br3 Br 0.24634(12) 0.48040(2) 0.64798(5) 0.03275(14) Uani 1 1 d .
C3 C 0.5365(13) 0.4245(3) 1.0882(5) 0.0331(12) Uani 1 1 d .
H3 H 0.4170 0.4338 1.1547 0.040 Uiso 1 1 calc R
C6 C 0.8927(13) 0.3952(2) 0.8969(5) 0.0309(12) Uani 1 1 d .
H6 H 1.0156 0.3849 0.8320 0.037 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.03250(14) 0.03055(13) 0.03285(14) -0.00400(8) 0.00940(9) -0.00526(8)
N1 0.035(2) 0.025(2) 0.025(2) -0.0002(17) 0.0004(19) 0.0017(17)
C1 0.058(4) 0.031(3) 0.046(4) 0.008(3) 0.009(3) 0.011(3)
Br1 0.0452(3) 0.0378(3) 0.0295(3) -0.0040(2) 0.0094(2) -0.0046(2)
Br2 0.0615(4) 0.0358(3) 0.0358(3) 0.0034(2) 0.0056(3) -0.0087(3)
C2 0.049(3) 0.029(3) 0.025(3) 0.008(2) 0.008(2) 0.001(2)
C5 0.032(3) 0.033(3) 0.016(2) 0.004(2) 0.0034(19) -0.001(2)
C4 0.030(2) 0.026(3) 0.015(2) 0.0009(18) -0.0010(19) -0.002(2)
Br3 0.0396(3) 0.0334(3) 0.0255(3) -0.0003(2) 0.0081(2) 0.0006(2)
C3 0.049(3) 0.027(3) 0.024(3) 0.001(2) 0.007(2) 0.000(2)
C6 0.037(3) 0.034(3) 0.022(3) 0.002(2) 0.006(2) 0.001(2)
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
Br2 Pb1 Br1 89.05(2) . .
Br2 Pb1 Br3 85.13(2) . .
Br1 Pb1 Br3 93.416(19) . .
Br2 Pb1 Br1 112.74(2) . 1_655
Br1 Pb1 Br1 92.050(19) . 1_655
Br3 Pb1 Br1 161.395(17) . 1_655
Br2 Pb1 Br3 167.224(18) . 3_666
Br1 Pb1 Br3 88.588(18) . 3_666
Br3 Pb1 Br3 82.479(18) . 3_666
Br1 Pb1 Br3 79.891(17) 1_655 3_666
C6 N1 C2 119.9(4) . .
C6 N1 C1 120.1(5) . .
C2 N1 C1 119.9(5) . .
N1 C1 H1 109.5 . .
N1 C1 H00C 109.5 . .
H1 C1 H00C 109.5 . .
N1 C1 H00D 109.5 . .
H1 C1 H00D 109.5 . .
H00C C1 H00D 109.5 . .
Pb1 Br1 Pb1 92.049(19) . 1_455
N1 C2 C3 121.0(5) . .
N1 C2 H2 119.5 . .
C3 C2 H2 119.5 . .
C6 C5 C4 120.4(5) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C5 C4 C3 116.9(5) . .
C5 C4 C4 121.8(5) . 3_667
C3 C4 C4 121.3(5) . 3_667
Pb1 Br3 Pb1 97.521(18) . 3_666
C2 C3 C4 120.5(5) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
N1 C6 C5 121.3(5) . .
N1 C6 H6 119.4 . .
C5 C6 H6 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br2 2.8585(7) .
Pb1 Br1 2.8832(7) .
Pb1 Br3 2.9511(6) .
Pb1 Br1 3.1645(7) 1_655
Pb1 Br3 3.2140(7) 3_666
N1 C6 1.345(7) .
N1 C2 1.348(7) .
N1 C1 1.476(7) .
C1 H1 0.9600 .
C1 H00C 0.9600 .
C1 H00D 0.9600 .
Br1 Pb1 3.1645(7) 1_455
C2 C3 1.362(8) .
C2 H2 0.9300 .
C5 C6 1.368(7) .
C5 C4 1.389(7) .
C5 H5 0.9300 .
C4 C3 1.406(7) .
C4 C4 1.484(10) 3_667
Br3 Pb1 3.2139(7) 3_666
C3 H3 0.9300 .
C6 H6 0.9300 .
