#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:04:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180410 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/79/7207987.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_7207987
loop_
_publ_author_name
'Hou, Qin'
'Bai, Fu-Quan'
'Jia, Ming-Jun'
'Jin, Juan'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 New organically templated chained and layered iodoplumbates
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              4000
_journal_paper_doi               10.1039/c2ce25102g
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C8 H22 I6 N2 O Pb2'
_chemical_formula_weight         1338.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.165(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9629(3)
_cell_length_b                   14.8833(6)
_cell_length_c                   21.0907(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2485.09(18)
_computing_cell_refinement       Bruker
_computing_data_collection       Bruker
_computing_data_reduction        Bruker
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  siements
_diffrn_measurement_method       Omega
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17700
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    20.982
_exptl_absorpt_correction_T_max  0.123
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.886
_refine_diff_density_min         -3.065
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         6130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0447
_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)+(0.0534P)²+20.4927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                3829
_reflns_number_total             6130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25102g.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7207987
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 0.25297(6) 0.92686(4) 0.03558(3) 0.03897(15) Uani 1 1 d .
Pb2 Pb 0.24367(7) 1.21168(4) -0.08533(3) 0.04066(15) Uani 1 1 d .
I1 I 0.07994(14) 0.73410(7) 0.02046(6) 0.0625(3) Uani 1 1 d .
I2 I 0.44264(13) 0.85808(8) 0.16392(5) 0.0546(3) Uani 1 1 d .
I3 I -0.04785(11) 1.00782(7) 0.10409(4) 0.0446(2) Uani 1 1 d .
I4 I 0.43108(11) 1.12193(6) 0.04790(4) 0.0411(2) Uani 1 1 d .
I5 I 0.08251(18) 1.29859(10) -0.21189(6) 0.0807(4) Uani 1 1 d .
I6 I 0.40084(12) 1.38195(6) -0.03098(5) 0.0474(3) Uani 1 1 d .
N1 N -0.2239(15) 1.4601(9) -0.1816(5) 0.049(3) Uani 1 1 d .
N2 N 0.0441(15) 1.5884(8) -0.1377(5) 0.045(3) Uani 1 1 d .
C1 C -0.018(2) 1.5215(11) -0.0963(7) 0.055(4) Uani 1 1 d .
H1A H -0.0059 1.5441 -0.0529 0.066 Uiso 1 1 calc R
H1B H 0.0509 1.4679 -0.0972 0.066 Uiso 1 1 calc R
C2 C -0.2061(19) 1.4958(11) -0.1153(6) 0.049(4) Uani 1 1 d .
H2A H -0.2411 1.4507 -0.0863 0.059 Uiso 1 1 calc R
H2B H -0.2774 1.5483 -0.1129 0.059 Uiso 1 1 calc R
C3 C -0.1658(19) 1.5307(11) -0.2242(7) 0.050(4) Uani 1 1 d .
H3A H -0.1804 1.5092 -0.2678 0.061 Uiso 1 1 calc R
H3B H -0.2354 1.5838 -0.2218 0.061 Uiso 1 1 calc R
C4 C 0.0104(18) 1.5548(11) -0.2073(7) 0.053(4) Uani 1 1 d .
H4A H 0.0415 1.6015 -0.2359 0.063 Uiso 1 1 calc R
H4B H 0.0809 1.5029 -0.2128 0.063 Uiso 1 1 calc R
C5 C -0.4024(19) 1.4292(12) -0.1996(8) 0.062(5) Uani 1 1 d .
H5A H -0.4338 1.3885 -0.1670 0.074 Uiso 1 1 calc R
H5B H -0.4768 1.4809 -0.2002 0.074 Uiso 1 1 calc R
C6 C -0.429(2) 1.3847(14) -0.2606(9) 0.079(6) Uani 1 1 d .
H6A H -0.5458 1.3672 -0.2688 0.119 Uiso 1 1 calc R
H6B H -0.3590 1.3323 -0.2602 0.119 Uiso 1 1 calc R
H6C H -0.4014 1.4249 -0.2935 0.119 Uiso 1 1 calc R
C7 C 0.2283(19) 1.6075(12) -0.1187(9) 0.062(5) Uani 1 1 d .
H7A H 0.2458 1.6164 -0.0729 0.074 Uiso 1 1 calc R
H7B H 0.2937 1.5554 -0.1288 0.074 Uiso 1 1 calc R
C8 C 0.292(2) 1.6864(14) -0.1502(9) 0.078(6) Uani 1 1 d .
H8A H 0.4111 1.6928 -0.1375 0.118 Uiso 1 1 calc R
H8D H 0.2343 1.7392 -0.1379 0.118 Uiso 1 1 calc R
H8B H 0.2732 1.6790 -0.1956 0.118 Uiso 1 1 calc R
OW1 O 0.1878(18) 0.2706(10) 0.1405(7) 0.094(4) Uiso 1 1 d .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
I2 Pb1 I3 92.77(3) . .
I2 Pb1 I1 87.44(4) . .
I3 Pb1 I1 92.76(3) . .
I2 Pb1 I4 93.30(3) . .
I3 Pb1 I4 88.19(3) . .
I1 Pb1 I4 178.77(3) . .
I2 Pb1 I4 93.71(3) . 3_675
I3 Pb1 I4 169.76(3) . 3_675
I1 Pb1 I4 95.44(3) . 3_675
I4 Pb1 I4 83.54(3) . 3_675
I2 Pb1 I3 177.73(3) . 3_575
I3 Pb1 I3 88.26(3) . 3_575
I1 Pb1 I3 90.49(3) . 3_575
I4 Pb1 I3 88.76(3) . 3_575
I4 Pb1 I3 85.56(3) 3_675 3_575
I6 Pb2 I5 95.35(4) . .
I6 Pb2 I1 86.83(3) . 3_575
I5 Pb2 I1 89.13(4) . 3_575
I6 Pb2 I2 98.63(3) . 3_675
I5 Pb2 I2 87.98(3) . 3_675
I1 Pb2 I2 174.03(3) 3_575 3_675
I6 Pb2 I4 83.41(3) . .
I5 Pb2 I4 177.59(4) . .
I1 Pb2 I4 92.85(3) 3_575 .
I2 Pb2 I4 90.16(3) 3_675 .
Pb2 I1 Pb1 95.23(3) 3_575 .
Pb1 I2 Pb2 89.40(3) . 3_675
Pb1 I3 Pb1 91.74(3) . 3_575
Pb1 I4 Pb1 96.46(3) . 3_675
Pb1 I4 Pb2 98.05(3) . .
Pb1 I4 Pb2 86.34(3) 3_675 .
C3 N1 C2 108.0(12) . .
C3 N1 C5 114.2(12) . .
C2 N1 C5 109.8(12) . .
C1 N2 C7 110.9(12) . .
C1 N2 C4 108.3(12) . .
C7 N2 C4 112.2(11) . .
N2 C1 C2 113.4(12) . .
N1 C2 C1 108.7(12) . .
C4 C3 N1 112.4(13) . .
C3 C4 N2 112.1(12) . .
C6 C5 N1 114.3(14) . .
C8 C7 N2 114.0(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.1268(11) .
Pb1 I3 3.1656(10) .
Pb1 I1 3.1836(12) .
Pb1 I4 3.2294(10) .
Pb1 I4 3.3028(10) 3_675
Pb1 I3 3.3551(11) 3_575
Pb2 I6 2.9991(11) .
Pb2 I5 3.1159(14) .
Pb2 I1 3.1497(12) 3_575
Pb2 I2 3.3096(12) 3_675
Pb2 I4 3.3177(11) .
I1 Pb2 3.1497(12) 3_575
I2 Pb2 3.3096(12) 3_675
I3 Pb1 3.3551(11) 3_575
I4 Pb1 3.3028(10) 3_675
N1 C3 1.487(18) .
N1 C2 1.489(17) .
N1 C5 1.503(19) .
N2 C1 1.446(18) .
N2 C7 1.505(19) .
N2 C4 1.547(18) .
C1 C2 1.56(2) .
C3 C4 1.455(19) .
C5 C6 1.44(2) .
C7 C8 1.47(2) .
