#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:04:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180410 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/79/7207988.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_7207988
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            'C10 H26 I6 N2 O Pb2'
_chemical_formula_weight         1366.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                108.705(4)
_cell_angle_beta                 95.269(4)
_cell_angle_gamma                92.523(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8807(5)
_cell_length_b                   11.6550(7)
_cell_length_c                   14.2611(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1387.99(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10170
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    18.787
_exptl_absorpt_correction_T_max  0.153
_exptl_absorpt_correction_T_min  0.133
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         6823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0476
_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)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                3734
_reflns_number_total             6823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25102g.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7207988
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 0.47098(5) 0.53293(5) 0.17563(4) 0.04283(14) Uani 1 1 d .
Pb2 Pb 0.05530(5) 0.69009(5) 0.12376(4) 0.04581(15) Uani 1 1 d .
I1 I 0.52021(11) 0.39520(10) 0.32364(8) 0.0674(3) Uani 1 1 d .
I2 I 0.78192(9) 0.70327(10) 0.25254(8) 0.0670(3) Uani 1 1 d .
I3 I 0.36089(9) 0.67084(8) 0.00132(7) 0.0509(2) Uani 1 1 d .
I4 I 0.14556(10) 0.37642(9) 0.09391(8) 0.0636(3) Uani 1 1 d .
I5 I 0.29792(9) 0.73084(8) 0.31848(7) 0.0479(2) Uani 1 1 d .
I6 I 0.06224(10) 0.95233(9) 0.14103(8) 0.0649(3) Uani 1 1 d .
OW1 O -0.1088(14) 0.3102(12) 0.2622(11) 0.119(4) Uiso 1 1 d .
N1 N 0.0379(13) 0.3765(10) 0.4489(9) 0.064(4) Uani 1 1 d .
N2 N 0.4711(10) 0.0210(9) -0.0944(7) 0.042(3) Uani 1 1 d .
C1 C -0.046(2) 0.4093(18) 0.5352(15) 0.112(7) Uani 1 1 d .
H1A H -0.1123 0.3393 0.5322 0.134 Uiso 1 1 calc R
H1B H 0.0251 0.4280 0.5948 0.134 Uiso 1 1 calc R
C2 C 0.1362(17) 0.4897(16) 0.4559(15) 0.096(6) Uani 1 1 d .
H2A H 0.2119 0.5090 0.5133 0.115 Uiso 1 1 calc R
H2B H 0.1886 0.4744 0.3968 0.115 Uiso 1 1 calc R
C3 C 0.148(2) 0.280(2) 0.4481(15) 0.110(7) Uani 1 1 d .
H3A H 0.2083 0.2686 0.3928 0.132 Uiso 1 1 calc R
H3B H 0.2159 0.3055 0.5095 0.132 Uiso 1 1 calc R
C4 C 0.060(2) 0.1664(17) 0.4378(16) 0.114(7) Uani 1 1 d .
H4A H -0.0072 0.1415 0.3761 0.136 Uiso 1 1 calc R
H4B H -0.0016 0.1792 0.4925 0.136 Uiso 1 1 calc R
C5 C 0.167(2) 0.0649(19) 0.4380(16) 0.149(10) Uani 1 1 d .
H5A H 0.1080 -0.0084 0.4323 0.224 Uiso 1 1 calc R
H5B H 0.2339 0.0897 0.4991 0.224 Uiso 1 1 calc R
H5C H 0.2260 0.0507 0.3827 0.224 Uiso 1 1 calc R
C6 C 0.5606(13) -0.0842(13) -0.0864(10) 0.054(4) Uani 1 1 d .
H6A H 0.6351 -0.1009 -0.1338 0.065 Uiso 1 1 calc R
H6B H 0.4934 -0.1568 -0.1000 0.065 Uiso 1 1 calc R
C7 C 0.3613(14) 0.0456(14) -0.0197(10) 0.058(4) Uani 1 1 d .
H7A H 0.2945 -0.0269 -0.0318 0.070 Uiso 1 1 calc R
H7B H 0.2996 0.1094 -0.0274 0.070 Uiso 1 1 calc R
C8 C 0.3855(16) -0.0129(14) -0.1987(10) 0.065(4) Uani 1 1 d .
H8A H 0.3239 -0.0885 -0.2124 0.078 Uiso 1 1 calc R
H8B H 0.3179 0.0496 -0.2005 0.078 Uiso 1 1 calc R
C9 C 0.4884(17) -0.0272(16) -0.2779(11) 0.079(5) Uani 1 1 d .
H9A H 0.5558 -0.0900 -0.2764 0.095 Uiso 1 1 calc R
H9B H 0.5502 0.0483 -0.2643 0.095 Uiso 1 1 calc R
C10 C 0.397(2) -0.0618(18) -0.3851(12) 0.108(7) Uani 1 1 d .
H10A H 0.4674 -0.0701 -0.4339 0.162 Uiso 1 1 calc R
H10B H 0.3319 0.0009 -0.3872 0.162 Uiso 1 1 calc R
H10C H 0.3377 -0.1374 -0.3994 0.162 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'
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
I1 Pb1 I5 93.16(3) . .
I1 Pb1 I2 95.07(3) . .
I5 Pb1 I2 90.27(3) . .
I1 Pb1 I4 88.40(3) . .
I5 Pb1 I4 87.40(3) . .
I2 Pb1 I4 175.92(3) . .
I1 Pb1 I3 93.29(3) . 2_665
I5 Pb1 I3 173.16(3) . 2_665
I2 Pb1 I3 91.43(3) . 2_665
I4 Pb1 I3 90.51(3) . 2_665
I6 Pb2 I2 94.08(3) . 1_455
I6 Pb2 I5 95.01(3) . .
I2 Pb2 I5 91.02(3) 1_455 .
I6 Pb2 I4 89.06(3) . 2_565
I2 Pb2 I4 97.45(3) 1_455 2_565
I5 Pb2 I4 170.32(3) . 2_565
I6 Pb2 I3 87.90(3) . .
I2 Pb2 I3 175.56(3) 1_455 .
I5 Pb2 I3 84.83(2) . .
I4 Pb2 I3 86.55(3) 2_565 .
Pb2 I2 Pb1 123.74(4) 1_655 .
Pb2 I3 Pb1 140.13(3) . 2_665
Pb1 I4 Pb2 129.79(3) . 2_565
Pb1 I5 Pb2 85.02(3) . .
C1 N1 C3 113.9(13) . .
C1 N1 C2 106.3(13) . .
C3 N1 C2 105.3(12) . .
C7 N2 C6 108.9(9) . .
C7 N2 C8 109.4(9) . .
C6 N2 C8 109.4(10) . .
C2 C1 N1 114.9(14) 2_566 .
C1 C2 N1 110.9(12) 2_566 .
C4 C3 N1 108.4(15) . .
C3 C4 C5 110.6(18) . .
N2 C6 C7 106.5(11) . 2_655
N2 C7 C6 112.2(10) . 2_655
C9 C8 N2 112.9(11) . .
C8 C9 C10 112.0(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.0479(10) .
Pb1 I5 3.1154(10) .
Pb1 I2 3.2146(11) .
Pb1 I4 3.2545(10) .
Pb1 I3 3.3761(10) 2_665
Pb2 I6 2.9839(11) .
Pb2 I2 3.1562(10) 1_455
Pb2 I5 3.2472(11) .
Pb2 I4 3.2767(11) 2_565
Pb2 I3 3.3372(9) .
I2 Pb2 3.1562(10) 1_655
I3 Pb1 3.3761(10) 2_665
I4 Pb2 3.2767(11) 2_565
N1 C1 1.453(18) .
N1 C3 1.52(2) .
N1 C2 1.520(17) .
N2 C7 1.479(14) .
N2 C6 1.519(15) .
N2 C8 1.527(16) .
C1 C2 1.43(2) 2_566
C2 C1 1.43(2) 2_566
C3 C4 1.47(2) .
C4 C5 1.55(2) .
C6 C7 1.523(17) 2_655
C7 C6 1.523(17) 2_655
C8 C9 1.490(18) .
C9 C10 1.583(19) .
