#------------------------------------------------------------------------------
#$Date: 2017-03-31 08:31:57 +0300 (Fri, 31 Mar 2017) $
#$Revision: 194638 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/79/7227959.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_7227959
loop_
_publ_author_name
'Wang, Rong-Yan'
'Zhang, Xiao'
'Huo, Qi-Sheng'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 New discrete iodometallates with in situ generated triimidazole
 derivatives as countercations (Mn+ = Ag+, Pb2+, Bi3+)
;
_journal_issue                   31
_journal_name_full               'RSC Adv.'
_journal_page_first              19073
_journal_paper_doi               10.1039/C6RA27510A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C36 H46 I12 N12 O2 Pb3'
_chemical_formula_weight         2823.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.496(3)
_cell_length_b                   20.569(4)
_cell_length_c                   12.634(3)
_cell_measurement_reflns_used    22282
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.21
_cell_volume                     3196.4(13)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_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  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30245
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.716
_exptl_absorpt_correction_T_max  0.254
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0492
_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)+(0.0160P)²+10.7798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                5113
_reflns_number_total             7292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra27510a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        3196.3(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7227959
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.19558(3) 0.102288(18) 0.32159(3) 0.03711(10) Uani 1 1 d .
Pb2 Pb 0.0000 0.0000 0.5000 0.04275(15) Uani 1 2 d S
I1 I 0.26427(7) 0.03539(3) 0.12896(6) 0.0544(2) Uani 1 1 d .
I2 I 0.42976(6) 0.17308(3) 0.36829(5) 0.04693(18) Uani 1 1 d .
I3 I 0.09445(6) 0.22146(3) 0.18501(5) 0.04551(18) Uani 1 1 d .
I4 I -0.04129(6) 0.03437(4) 0.24807(5) 0.05243(19) Uani 1 1 d .
I5 I -0.24239(6) 0.03756(4) 0.52845(6) 0.05007(18) Uani 1 1 d .
I6 I 0.09225(8) 0.14542(4) 0.55035(6) 0.0619(2) Uani 1 1 d .
N1 N 0.3139(6) 0.2765(4) 0.8941(6) 0.0375(19) Uani 1 1 d .
N2 N 0.5687(7) -0.0392(4) 1.2926(6) 0.0413(19) Uani 1 1 d .
N3 N 0.9514(6) 0.1388(4) 0.8819(6) 0.0370(18) Uani 1 1 d .
N4 N 0.4322(6) 0.2105(3) 0.9806(5) 0.0314(17) Uani 1 1 d .
N5 N 0.6132(6) 0.0249(3) 1.1723(5) 0.0311(17) Uani 1 1 d .
N6 N 0.7903(6) 0.1428(3) 0.9195(6) 0.0308(16) Uani 1 1 d .
C1 C 0.2858(9) 0.2649(5) 0.9921(8) 0.043(3) Uani 1 1 d .
H1A H 0.2265 0.2826 1.0171 0.052 Uiso 1 1 calc R
C2 C 0.3581(8) 0.2238(5) 1.0455(8) 0.048(3) Uani 1 1 d .
H2A H 0.3583 0.2072 1.1141 0.057 Uiso 1 1 calc R
C3 C 0.4032(8) 0.2433(5) 0.8883(7) 0.038(2) Uani 1 1 d .
H3A H 0.4396 0.2428 0.8302 0.045 Uiso 1 1 calc R
C4 C 0.6360(9) -0.0735(5) 1.2390(8) 0.050(3) Uani 1 1 d .
H4A H 0.6577 -0.1165 1.2515 0.060 Uiso 1 1 calc R
C5 C 0.6648(9) -0.0337(4) 1.1651(8) 0.043(3) Uani 1 1 d .
H5A H 0.7112 -0.0437 1.1174 0.052 Uiso 1 1 calc R
C6 C 0.5553(8) 0.0203(5) 1.2522(7) 0.040(2) Uani 1 1 d .
H6A H 0.5133 0.0530 1.2750 0.049 Uiso 1 1 calc R
C7 C 0.7805(9) 0.1435(4) 0.8079(7) 0.041(2) Uani 1 1 d .
H7A H 0.7164 0.1455 0.7579 0.050 Uiso 1 1 calc R
C8 C 0.8820(9) 0.1410(5) 0.7871(8) 0.042(2) Uani 1 1 d .
H8A H 0.9013 0.1408 0.7193 0.050 Uiso 1 1 calc R
C9 C 0.8958(7) 0.1385(4) 0.9604(7) 0.034(2) Uani 1 1 d .
H9A H 0.9253 0.1358 1.0332 0.041 Uiso 1 1 calc R
C10 C 0.7028(7) 0.0878(4) 1.0515(6) 0.030(2) Uani 1 1 d .
H10A H 0.7626 0.0603 1.0665 0.036 Uiso 1 1 calc R
C11 C 0.7008(8) 0.1375(4) 0.9772(7) 0.034(2) Uani 1 1 d .
C12 C 0.6133(8) 0.1789(4) 0.9524(7) 0.033(2) Uani 1 1 d .
H12A H 0.6129 0.2122 0.9025 0.040 Uiso 1 1 calc R
C13 C 0.5251(7) 0.1690(4) 1.0049(6) 0.029(2) Uani 1 1 d .
C14 C 0.5224(8) 0.1199(4) 1.0794(7) 0.034(2) Uani 1 1 d .
H14A H 0.4623 0.1137 1.1125 0.040 Uiso 1 1 calc R
C15 C 0.6157(8) 0.0796(4) 1.1027(6) 0.030(2) Uani 1 1 d .
C16 C 0.2566(10) 0.3187(5) 0.8087(8) 0.055(3) Uani 1 1 d .
H16A H 0.1952 0.3384 0.8324 0.083 Uiso 1 1 calc R
H16B H 0.2320 0.2933 0.7453 0.083 Uiso 1 1 calc R
H16C H 0.3050 0.3521 0.7926 0.083 Uiso 1 1 calc R
C17 C 0.5149(10) -0.0642(6) 1.3804(8) 0.063(3) Uani 1 1 d .
H17A H 0.4756 -0.0296 1.4073 0.095 Uiso 1 1 calc R
H17B H 0.5690 -0.0808 1.4376 0.095 Uiso 1 1 calc R
H17C H 0.4654 -0.0984 1.3531 0.095 Uiso 1 1 calc R
C18 C 1.0704(9) 0.1403(6) 0.8937(9) 0.058(3) Uani 1 1 d .
H18A H 1.1022 0.1375 0.9685 0.087 Uiso 1 1 calc R
H18B H 1.0925 0.1802 0.8645 0.087 Uiso 1 1 calc R
H18C H 1.0945 0.1042 0.8558 0.087 Uiso 1 1 calc R
OW1 O 0.3331(12) 0.2190(7) 0.6346(12) 0.158(5) Uani 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
I1 Pb1 I3 93.24(3) . .
I1 Pb1 I2 88.61(3) . .
I3 Pb1 I2 90.70(3) . .
I1 Pb1 I4 87.04(3) . .
I3 Pb1 I4 85.44(3) . .
I2 Pb1 I4 174.01(2) . .
I5 Pb2 I5 180.0 . 3_556
I5 Pb2 I4 86.08(3) . 3_556
I5 Pb2 I4 93.92(3) 3_556 3_556
I5 Pb2 I4 93.92(3) . .
I5 Pb2 I4 86.08(3) 3_556 .
I4 Pb2 I4 180.0 3_556 .
I5 Pb2 I6 93.79(2) . .
I5 Pb2 I6 86.21(2) 3_556 .
I4 Pb2 I6 91.11(2) 3_556 .
I4 Pb2 I6 88.89(2) . .
I5 Pb2 I6 86.21(2) . 3_556
I5 Pb2 I6 93.79(2) 3_556 3_556
I4 Pb2 I6 88.89(2) 3_556 3_556
I4 Pb2 I6 91.11(2) . 3_556
I6 Pb2 I6 180.0 . 3_556
Pb2 I4 Pb1 80.37(3) . .
C3 N1 C1 108.3(8) . .
C3 N1 C16 124.9(8) . .
C1 N1 C16 126.8(8) . .
C6 N2 C4 109.4(8) . .
C6 N2 C17 124.4(9) . .
C4 N2 C17 126.2(9) . .
C9 N3 C8 109.3(8) . .
C9 N3 C18 126.0(9) . .
C8 N3 C18 124.7(8) . .
C3 N4 C2 108.3(8) . .
C3 N4 C13 124.9(7) . .
C2 N4 C13 126.8(7) . .
C6 N5 C5 108.0(7) . .
C6 N5 C15 126.0(8) . .
C5 N5 C15 125.9(7) . .
C9 N6 C7 107.3(8) . .
C9 N6 C11 127.0(8) . .
C7 N6 C11 125.1(8) . .
C2 C1 N1 108.1(9) . .
C1 C2 N4 107.0(8) . .
N1 C3 N4 108.3(7) . .
C5 C4 N2 107.2(9) . .
C4 C5 N5 107.6(8) . .
N2 C6 N5 107.8(9) . .
C8 C7 N6 106.3(9) . .
C7 C8 N3 107.9(8) . .
N3 C9 N6 109.1(8) . .
C15 C10 C11 119.4(8) . .
C12 C11 C10 121.9(8) . .
C12 C11 N6 119.6(8) . .
C10 C11 N6 118.3(8) . .
C11 C12 C13 117.6(8) . .
C14 C13 C12 123.0(8) . .
C14 C13 N4 117.7(8) . .
C12 C13 N4 119.3(7) . .
C13 C14 C15 116.7(8) . .
C10 C15 C14 121.4(8) . .
C10 C15 N5 119.4(8) . .
C14 C15 N5 118.8(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.0481(9) .
Pb1 I3 3.1327(10) .
Pb1 I2 3.2282(10) .
Pb1 I4 3.2565(11) .
Pb2 I5 3.2068(9) .
Pb2 I5 3.2068(9) 3_556
Pb2 I4 3.2121(9) 3_556
Pb2 I4 3.2121(9) .
Pb2 I6 3.2282(10) .
Pb2 I6 3.2282(10) 3_556
N1 C3 1.321(11) .
N1 C1 1.366(11) .
N1 C16 1.470(11) .
N2 C6 1.326(12) .
N2 C4 1.365(12) .
N2 C17 1.487(11) .
N3 C9 1.307(10) .
N3 C8 1.350(12) .
N3 C18 1.469(13) .
N4 C3 1.340(11) .
N4 C2 1.369(11) .
N4 C13 1.429(10) .
N5 C6 1.345(11) .
N5 C5 1.376(11) .
N5 C15 1.431(10) .
N6 C9 1.332(11) .
N6 C7 1.393(11) .
N6 C11 1.443(11) .
C1 C2 1.331(13) .
C4 C5 1.339(13) .
C7 C8 1.341(14) .
C10 C15 1.372(12) .
C10 C11 1.385(12) .
C11 C12 1.377(13) .
C12 C13 1.397(12) .
C13 C14 1.386(11) .
C14 C15 1.419(12) .
