#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:05:59 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229773 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/57/7045732.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_7045732
loop_
_publ_author_name
'Xiao, Hong'
'Zhou, Jian'
'Liu, Xing'
_publ_section_title
;
 Two new 3-D cadmium bromoplumbates: the only example of heterometallic
 bromoplumbate based on crown
 [Cd(Pb₄O₄)Br₂] clusters.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4833
_journal_page_last               4839
_journal_paper_doi               10.1039/c8dt00428e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C8 H16 Br6 Cd O8 Pb6'
_chemical_formula_sum            'C8 H16 Br6 Cd O8 Pb6'
_chemical_formula_weight         2075.22
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
;
2018-01-28 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.965(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4173(9)
_cell_length_b                   13.6560(11)
_cell_length_c                   21.909(2)
_cell_measurement_reflns_used    28432
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.65
_cell_volume                     2783.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28432
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    45.552
_exptl_absorpt_correction_T_max  0.6386
_exptl_absorpt_correction_T_min  0.1920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.290
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.459
_refine_ls_extinction_coef       0.000109(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0588
_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)+(0.0443P)²+390.5807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                2888
_reflns_number_total             3305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00428e2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7045731--7045732.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7045732
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 -0.07939(6) 0.35447(4) 0.54485(3) 0.02133(17) Uani 1 1 d .
Pb2 Pb 0.65093(7) 0.49802(5) 0.64317(3) 0.02789(19) Uani 1 1 d .
Pb3 Pb 0.76548(6) 0.50271(4) 0.83909(3) 0.02305(17) Uani 1 1 d .
Cd1 Cd 0.5000 0.34034(12) 0.7500 0.0204(3) Uani 1 2 d S
Br1 Br 0.5000 0.59647(16) 0.7500 0.0254(5) Uani 1 2 d S
Br2 Br -0.08209(19) 0.56410(12) 0.56675(8) 0.0288(4) Uani 1 1 d .
Br3 Br -0.38245(18) 0.39193(12) 0.45332(8) 0.0279(4) Uani 1 1 d .
Br4 Br 0.5000 0.13905(12) 0.7500 0.0135(4) Uani 1 2 d S
O1 O 0.2896(12) 0.4086(9) 0.7630(5) 0.024(2) Uani 1 1 d .
O2 O 0.2332(14) 0.3606(9) 0.8824(6) 0.034(3) Uani 1 1 d .
O3 O 0.1390(12) 0.3632(9) 0.6145(6) 0.030(3) Uani 1 1 d .
O4 O 0.4357(11) 0.4022(8) 0.6497(5) 0.022(2) Uani 1 1 d .
C1 C 0.178(2) 0.3426(17) 0.7717(9) 0.040(5) Uani 1 1 d .
H1A H 0.1675 0.2940 0.7390 0.048 Uiso 1 1 calc R
H1B H 0.0886 0.3781 0.7693 0.048 Uiso 1 1 calc R
C2 C 0.211(2) 0.2921(13) 0.8331(9) 0.037(4) Uani 1 1 d .
H2A H 0.1308 0.2496 0.8384 0.044 Uiso 1 1 calc R
H2B H 0.2956 0.2518 0.8341 0.044 Uiso 1 1 calc R
C3 C 0.3861(19) 0.3355(13) 0.5994(8) 0.027(3) Uani 1 1 d .
H3A H 0.4568 0.2842 0.5983 0.032 Uiso 1 1 calc R
H3B H 0.3759 0.3707 0.5605 0.032 Uiso 1 1 calc R
C4 C 0.2442(18) 0.2905(12) 0.6071(9) 0.028(4) Uani 1 1 d .
H4A H 0.2096 0.2509 0.5711 0.034 Uiso 1 1 calc R
H4B H 0.2576 0.2479 0.6429 0.034 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'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 '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
O2 Pb1 O3 97.4(5) 2_556 .
O2 Pb1 Br2 80.1(3) 2_556 .
O3 Pb1 Br2 82.7(3) . .
O2 Pb2 O1 74.5(4) 2_656 2_656
O2 Pb2 O4 90.4(4) 2_656 .
O1 Pb2 O4 76.1(4) 2_656 .
O2 Pb2 Br1 143.5(3) 2_656 .
O1 Pb2 Br1 70.0(3) 2_656 .
O4 Pb2 Br1 73.5(3) . .
O3 Pb3 O4 74.8(4) 2_656 2_656
O3 Pb3 O1 89.0(4) 2_656 2_656
O4 Pb3 O1 75.2(4) 2_656 2_656
O3 Pb3 Br1 145.7(3) 2_656 .
O4 Pb3 Br1 74.6(3) 2_656 .
O1 Pb3 Br1 68.6(2) 2_656 .
O1 Cd1 O1 131.0(6) 2_656 .
O1 Cd1 O4 82.3(4) 2_656 2_656
O1 Cd1 O4 80.6(4) . 2_656
O1 Cd1 O4 80.6(4) 2_656 .
O1 Cd1 O4 82.3(4) . .
O4 Cd1 O4 137.8(5) 2_656 .
O1 Cd1 Br4 114.5(3) 2_656 .
O1 Cd1 Br4 114.5(3) . .
O4 Cd1 Br4 111.1(3) 2_656 .
O4 Cd1 Br4 111.1(3) . .
Pb3 Br1 Pb3 132.68(8) 2_656 .
Pb3 Br1 Pb2 77.29(3) 2_656 .
Pb3 Br1 Pb2 83.36(3) . .
Pb3 Br1 Pb2 83.36(3) 2_656 2_656
Pb3 Br1 Pb2 77.29(3) . 2_656
Pb2 Br1 Pb2 130.58(8) . 2_656
C1 O1 Cd1 116.0(12) . .
C1 O1 Pb2 106.8(10) . 2_656
Cd1 O1 Pb2 103.2(4) . 2_656
C1 O1 Pb3 112.6(10) . 2_656
Cd1 O1 Pb3 99.2(4) . 2_656
Pb2 O1 Pb3 119.0(5) 2_656 2_656
C2 O2 Pb2 112.1(10) . 2_656
C2 O2 Pb1 117.6(10) . 2_556
Pb2 O2 Pb1 124.9(5) 2_656 2_556
C4 O3 Pb3 113.5(9) . 2_656
C4 O3 Pb1 116.1(10) . .
Pb3 O3 Pb1 125.0(5) 2_656 .
C3 O4 Cd1 119.4(10) . .
C3 O4 Pb3 105.8(9) . 2_656
Cd1 O4 Pb3 101.8(4) . 2_656
C3 O4 Pb2 117.8(9) . .
Cd1 O4 Pb2 98.8(4) . .
Pb3 O4 Pb2 112.2(4) 2_656 .
O1 C1 C2 111.4(15) . .
O1 C1 H1A 109.4 . .
C2 C1 H1A 109.4 . .
O1 C1 H1B 109.4 . .
C2 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
O2 C2 C1 111.4(16) . .
O2 C2 H2A 109.3 . .
C1 C2 H2A 109.3 . .
O2 C2 H2B 109.3 . .
C1 C2 H2B 109.3 . .
H2A C2 H2B 108.0 . .
O4 C3 C4 111.1(14) . .
O4 C3 H3A 109.4 . .
C4 C3 H3A 109.4 . .
O4 C3 H3B 109.4 . .
C4 C3 H3B 109.4 . .
H3A C3 H3B 108.0 . .
O3 C4 C3 111.9(14) . .
O3 C4 H4A 109.2 . .
C3 C4 H4A 109.2 . .
O3 C4 H4B 109.2 . .
C3 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.316(11) 2_556
Pb1 O3 2.365(11) .
Pb1 Br2 2.9034(17) .
Pb2 O2 2.285(11) 2_656
Pb2 O1 2.382(12) 2_656
Pb2 O4 2.435(11) .
Pb2 Br1 3.2159(12) .
Pb3 O3 2.277(12) 2_656
Pb3 O4 2.384(10) 2_656
Pb3 O1 2.561(11) 2_656
Pb3 Br1 3.1904(11) .
Cd1 O1 2.248(11) 2_656
Cd1 O1 2.248(11) .
Cd1 O4 2.345(11) 2_656
Cd1 O4 2.345(11) .
Cd1 Br4 2.749(2) .
Br1 Pb3 3.1904(11) 2_656
Br1 Pb2 3.2159(12) 2_656
O1 C1 1.42(2) .
O1 Pb2 2.382(12) 2_656
O1 Pb3 2.561(11) 2_656
O2 C2 1.42(2) .
O2 Pb2 2.285(11) 2_656
O2 Pb1 2.316(11) 2_556
O3 C4 1.430(19) .
O3 Pb3 2.277(12) 2_656
O4 C3 1.448(19) .
O4 Pb3 2.384(10) 2_656
C1 C2 1.50(3) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.50(2) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
