#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:23:47 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179576 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/41/4504104.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_4504104
loop_
_publ_author_name
'Wang, Xiao-Feng'
'Lv, Yang'
'Okamura, Taka-aki'
'Kawaguchi, Hiroyuki'
'Wu, Gang'
'Sun, Wei-Yin'
'Ueyama, Norikazu'
_publ_section_title
;
 Structure Variation of Mercury(II) Halide Complexes with Different
 Imidazole-Containing Ligands
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1125
_journal_paper_doi               10.1021/cg060814c
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'C36 H38 I6 Hg3 N14 O2 '
_chemical_formula_sum            'C36 H38 Hg3 I6 N14 O2'
_chemical_formula_weight         2061.97
_chemical_name_systematic
; 
[Hg3I6(F1)2]-2DMF 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_date             'Fri Apr 23 22:10:14 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.50(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.676(17)
_cell_length_b                   15.860(11)
_cell_length_c                   18.097(12)
_cell_measurement_reflns_used    15765
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5305(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26329
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    12.198
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.868
_refine_diff_density_min         -3.587
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0090P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0397
_reflns_number_gt                3450
_reflns_number_total             6097
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg060814csi20070307_054928.cif
_cod_data_source_block           4
_cod_original_cell_volume        5304(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4504104
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
Hg1 Hg 0.0000 0.932793(19) 0.2500 0.03372(9) Uani 1 2 d S
Hg2 Hg 0.616050(13) 0.786964(13) 0.483884(15) 0.03649(7) Uani 1 1 d .
I1 I -0.05264(2) 0.98874(3) 0.34474(3) 0.05037(13) Uani 1 1 d .
I2 I 0.61571(3) 0.91137(2) 0.38573(3) 0.05398(14) Uani 1 1 d .
I3 I 0.65621(3) 0.76876(3) 0.65144(3) 0.05541(13) Uani 1 1 d .
O1 O 0.2957(3) 0.9103(3) 0.3945(3) 0.0676(15) Uani 1 1 d .
N1 N 0.3527(3) 0.9751(3) 0.3362(3) 0.0448(14) Uani 1 1 d .
N11 N 0.1617(2) 0.7178(3) 0.3870(2) 0.0235(10) Uani 1 1 d .
N12 N 0.0767(2) 0.8163(3) 0.3337(3) 0.0289(11) Uani 1 1 d .
N31 N 0.3896(2) 0.7050(2) 0.3968(3) 0.0278(11) Uani 1 1 d .
N32 N 0.4932(2) 0.7490(3) 0.4151(3) 0.0334(12) Uani 1 1 d .
N51 N 0.3212(2) 0.4769(2) 0.5187(3) 0.0274(11) Uani 1 1 d .
N52 N 0.3492(3) 0.3429(3) 0.5416(3) 0.0380(13) Uani 1 1 d .
C1 C 0.2274(3) 0.6757(3) 0.4116(3) 0.0228(13) Uani 1 1 d .
C2 C 0.2759(3) 0.7107(3) 0.3922(3) 0.0231(12) Uani 1 1 d .
H1 H 0.2660 0.7635 0.3633 0.028 Uiso 1 1 calc R
C3 C 0.3391(3) 0.6676(3) 0.4156(3) 0.0265(13) Uani 1 1 d .
C4 C 0.3553(3) 0.5914(3) 0.4577(3) 0.0280(13) Uani 1 1 d .
H2 H 0.3987 0.5625 0.4729 0.034 Uiso 1 1 calc R
C5 C 0.3067(3) 0.5579(3) 0.4774(3) 0.0253(13) Uani 1 1 d .
C6 C 0.2432(3) 0.5998(3) 0.4558(3) 0.0254(13) Uani 1 1 d .
H3 H 0.2110 0.5768 0.4711 0.030 Uiso 1 1 calc R
C11 C 0.1412(3) 0.7965(3) 0.3507(3) 0.0313(14) Uani 1 1 d .
H4 H 0.1705 0.8323 0.3394 0.038 Uiso 1 1 calc R
C12 C 0.0533(3) 0.7475(4) 0.3592(3) 0.0373(15) Uani 1 1 d .
H5 H 0.0077 0.7432 0.3545 0.045 Uiso 1 1 calc R
C13 C 0.1045(3) 0.6879(3) 0.3916(4) 0.0395(16) Uani 1 1 d .
H6 H 0.1016 0.6346 0.4136 0.047 Uiso 1 1 calc R
C31 C 0.4621(3) 0.7083(3) 0.4495(4) 0.0336(14) Uani 1 1 d .
H7 H 0.4878 0.6837 0.5056 0.040 Uiso 1 1 calc R
C32 C 0.4376(3) 0.7726(3) 0.3341(4) 0.0393(15) Uani 1 1 d .
H8 H 0.4437 0.8027 0.2930 0.047 Uiso 1 1 calc R
C33 C 0.3729(3) 0.7470(3) 0.3212(3) 0.0362(15) Uani 1 1 d .
H9 H 0.3264 0.7559 0.2713 0.043 Uiso 1 1 calc R
C51 C 0.3440(3) 0.4094(3) 0.4946(4) 0.0345(15) Uani 1 1 d .
H10 H 0.3548 0.4095 0.4501 0.041 Uiso 1 1 calc R
C52 C 0.3289(3) 0.3698(4) 0.5977(4) 0.0436(17) Uani 1 1 d .
H11 H 0.3276 0.3354 0.6398 0.052 Uiso 1 1 calc R
C53 C 0.3112(3) 0.4518(4) 0.5845(3) 0.0386(16) Uani 1 1 d .
H12 H 0.2950 0.4856 0.6145 0.046 Uiso 1 1 calc R
C101 C 0.3515(5) 0.9389(4) 0.3986(5) 0.067(2) Uani 1 1 d .
H13 H 0.3961 0.9331 0.4521 0.081 Uiso 1 1 calc R
C102 C 0.2869(4) 0.9854(5) 0.2524(5) 0.090(3) Uani 1 1 d .
H14 H 0.2456 0.9653 0.2554 0.108 Uiso 1 1 calc R
H15 H 0.2906 0.9527 0.2089 0.108 Uiso 1 1 calc R
H16 H 0.2802 1.0452 0.2362 0.108 Uiso 1 1 calc R
C103 C 0.4183(4) 1.0043(4) 0.3418(5) 0.081(2) Uani 1 1 d .
H17 H 0.4598 0.9922 0.3998 0.098 Uiso 1 1 calc R
H18 H 0.4150 1.0652 0.3313 0.098 Uiso 1 1 calc R
H19 H 0.4244 0.9752 0.2983 0.098 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
Hg Hg -2.3894 9.2266 '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'
O O 0.0106 0.0060 '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'
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'
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
N12 Hg1 N12 80.3(2) 2 .
N12 Hg1 I1 105.82(11) 2 .
N12 Hg1 I1 103.73(10) . .
N12 Hg1 I1 103.73(10) 2 2
N12 Hg1 I1 105.82(11) . 2
I1 Hg1 I1 141.02(4) . 2
N52 Hg2 N32 93.61(16) 5_666 .
N52 Hg2 I2 114.52(12) 5_666 .
N32 Hg2 I2 103.28(11) . .
N52 Hg2 I3 100.41(11) 5_666 .
N32 Hg2 I3 100.27(11) . .
I2 Hg2 I3 135.95(3) . .
C101 N1 C103 123.6(7) . .
C101 N1 C102 120.8(6) . .
C103 N1 C102 115.5(5) . .
C13 N11 C11 105.5(4) . .
C13 N11 C1 127.6(4) . .
C11 N11 C1 126.9(4) . .
C11 N12 C12 105.4(4) . .
C11 N12 Hg1 129.4(4) . .
C12 N12 Hg1 124.1(4) . .
C31 N31 C33 106.5(4) . .
C31 N31 C3 127.0(5) . .
C33 N31 C3 126.4(5) . .
C31 N32 C32 105.0(5) . .
C31 N32 Hg2 126.8(4) . .
C32 N32 Hg2 127.8(4) . .
C51 N51 C53 107.5(4) . .
C51 N51 C5 124.2(4) . .
C53 N51 C5 128.2(4) . .
C51 N52 C52 105.9(4) . .
C51 N52 Hg2 120.6(4) . 5_666
C52 N52 Hg2 133.5(4) . 5_666
C6 C1 C2 120.2(5) . .
C6 C1 N11 119.7(5) . .
C2 C1 N11 120.1(4) . .
C3 C2 C1 119.0(5) . .
C3 C2 H1 120.5 . .
C1 C2 H1 120.5 . .
C4 C3 C2 121.9(5) . .
C4 C3 N31 119.4(5) . .
C2 C3 N31 118.7(5) . .
C3 C4 C5 118.3(5) . .
C3 C4 H2 120.8 . .
C5 C4 H2 120.8 . .
C4 C5 C6 121.3(5) . .
C4 C5 N51 119.3(5) . .
C6 C5 N51 119.4(5) . .
C1 C6 C5 119.2(5) . .
C1 C6 H3 120.4 . .
C5 C6 H3 120.4 . .
N12 C11 N11 111.8(5) . .
N12 C11 H4 124.1 . .
N11 C11 H4 124.1 . .
C13 C12 N12 109.9(5) . .
C13 C12 H5 125.0 . .
N12 C12 H5 125.0 . .
C12 C13 N11 107.3(5) . .
C12 C13 H6 126.3 . .
N11 C13 H6 126.3 . .
N32 C31 N31 112.7(5) . .
N32 C31 H7 123.7 . .
N31 C31 H7 123.7 . .
C33 C32 N32 110.7(5) . .
C33 C32 H8 124.7 . .
N32 C32 H8 124.7 . .
C32 C33 N31 105.1(5) . .
C32 C33 H9 127.5 . .
N31 C33 H9 127.5 . .
N52 C51 N51 110.5(4) . .
N52 C51 H10 124.8 . .
N51 C51 H10 124.8 . .
C53 C52 N52 110.2(5) . .
C53 C52 H11 124.9 . .
N52 C52 H11 124.9 . .
C52 C53 N51 105.9(5) . .
C52 C53 H12 127.1 . .
N51 C53 H12 127.1 . .
O1 C101 N1 124.9(8) . .
O1 C101 H13 117.5 . .
N1 C101 H13 117.5 . .
N1 C102 H14 109.5 . .
N1 C102 H15 109.5 . .
H14 C102 H15 109.5 . .
N1 C102 H16 109.5 . .
H14 C102 H16 109.5 . .
H15 C102 H16 109.5 . .
N1 C103 H17 109.5 . .
N1 C103 H18 109.5 . .
H17 C103 H18 109.5 . .
N1 C103 H19 109.5 . .
H17 C103 H19 109.5 . .
H18 C103 H19 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 N12 2.417(4) 2
Hg1 N12 2.417(4) .
Hg1 I1 2.6596(13) .
Hg1 I1 2.6597(13) 2
Hg2 N52 2.319(4) 5_666
Hg2 N32 2.353(5) .
Hg2 I2 2.6523(13) .
Hg2 I3 2.698(2) .
O1 C101 1.257(8) .
N1 C101 1.280(7) .
N1 C103 1.447(7) .
N1 C102 1.448(8) .
N11 C13 1.370(6) .
N11 C11 1.372(6) .
N11 C1 1.418(6) .
N12 C11 1.302(6) .
N12 C12 1.380(6) .
N31 C31 1.348(6) .
N31 C33 1.389(6) .
N31 C3 1.434(6) .
N32 C31 1.301(6) .
N32 C32 1.377(6) .
N51 C51 1.343(6) .
N51 C53 1.377(6) .
N51 C5 1.436(6) .
N52 C51 1.322(6) .
N52 C52 1.369(6) .
N52 Hg2 2.319(4) 5_666
C1 C6 1.384(6) .
C1 C2 1.388(6) .
C2 C3 1.384(7) .
C2 H1 0.9500 .
C3 C4 1.372(6) .
C4 C5 1.382(6) .
C4 H2 0.9500 .
C5 C6 1.388(6) .
C6 H3 0.9500 .
C11 H4 0.9500 .
C12 C13 1.337(7) .
C12 H5 0.9500 .
C13 H6 0.9500 .
C31 H7 0.9500 .
C32 C33 1.357(7) .
C32 H8 0.9500 .
C33 H9 0.9500 .
C51 H10 0.9500 .
C52 C53 1.341(7) .
C52 H11 0.9500 .
C53 H12 0.9500 .
C101 H13 0.9500 .
C102 H14 0.9800 .
C102 H15 0.9800 .
C102 H16 0.9800 .
C103 H17 0.9800 .
C103 H18 0.9800 .
C103 H19 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N12 Hg1 N12 C11 119.2(5) 2
I1 Hg1 N12 C11 -136.7(4) .
I1 Hg1 N12 C11 17.6(5) 2
N12 Hg1 N12 C12 -47.3(3) 2
I1 Hg1 N12 C12 56.7(4) .
I1 Hg1 N12 C12 -149.0(3) 2
N52 Hg2 N32 C31 84.2(4) 5_666
I2 Hg2 N32 C31 -159.5(4) .
I3 Hg2 N32 C31 -17.0(4) .
N52 Hg2 N32 C32 -103.6(4) 5_666
I2 Hg2 N32 C32 12.6(4) .
I3 Hg2 N32 C32 155.1(4) .
C13 N11 C1 C6 -9.1(8) .
C11 N11 C1 C6 173.2(4) .
C13 N11 C1 C2 171.5(5) .
C11 N11 C1 C2 -6.2(7) .
C6 C1 C2 C3 1.7(7) .
N11 C1 C2 C3 -178.9(4) .
C1 C2 C3 C4 -0.3(8) .
C1 C2 C3 N31 -178.8(4) .
C31 N31 C3 C4 -41.9(7) .
C33 N31 C3 C4 140.0(5) .
C31 N31 C3 C2 136.7(5) .
C33 N31 C3 C2 -41.4(7) .
C2 C3 C4 C5 -0.5(8) .
N31 C3 C4 C5 178.1(4) .
C3 C4 C5 C6 -0.2(7) .
C3 C4 C5 N51 177.8(4) .
C51 N51 C5 C4 -44.9(7) .
C53 N51 C5 C4 139.1(5) .
C51 N51 C5 C6 133.2(5) .
C53 N51 C5 C6 -42.9(8) .
C2 C1 C6 C5 -2.4(7) .
N11 C1 C6 C5 178.2(4) .
C4 C5 C6 C1 1.7(8) .
N51 C5 C6 C1 -176.3(4) .
C12 N12 C11 N11 -0.5(6) .
Hg1 N12 C11 N11 -169.0(3) .
C13 N11 C11 N12 0.4(6) .
C1 N11 C11 N12 178.5(4) .
C11 N12 C12 C13 0.4(6) .
Hg1 N12 C12 C13 169.7(4) .
N12 C12 C13 N11 -0.2(6) .
C11 N11 C13 C12 -0.1(6) .
C1 N11 C13 C12 -178.2(4) .
C32 N32 C31 N31 -1.0(6) .
Hg2 N32 C31 N31 172.5(3) .
C33 N31 C31 N32 0.6(6) .
C3 N31 C31 N32 -177.8(4) .
C31 N32 C32 C33 1.2(6) .
Hg2 N32 C32 C33 -172.3(3) .
N32 C32 C33 N31 -0.8(6) .
C31 N31 C33 C32 0.2(6) .
C3 N31 C33 C32 178.6(5) .
C52 N52 C51 N51 -0.1(7) .
Hg2 N52 C51 N51 178.2(3) 5_666
C53 N51 C51 N52 -0.2(6) .
C5 N51 C51 N52 -176.9(5) .
C51 N52 C52 C53 0.3(7) .
Hg2 N52 C52 C53 -177.7(4) 5_666
N52 C52 C53 N51 -0.4(7) .
C51 N51 C53 C52 0.4(6) .
C5 N51 C53 C52 176.9(5) .
C103 N1 C101 O1 -177.4(6) .
C102 N1 C101 O1 -0.7(10) .
