#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:26:59 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179579 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/44/4504448.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_4504448
loop_
_publ_author_name
'Wang, Jing'
'Zhang, Yue-Hua'
'Li, Hao-Xiang'
'Lin, Zhuo-Jia'
'Tong, Ming-Liang'
_publ_section_title
;
 Construction of Pyridinethiolate-Bridged 2D and 3D Coordination Networks
 of d10Metal Halides via Solvothermalin SituDisulfide Cleavage Reactions
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2352
_journal_paper_doi               10.1021/cg070622x
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C5 H5 Cu4 I4 N S'
_chemical_formula_weight         872.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.947(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.106(2)
_cell_length_b                   4.1222(4)
_cell_length_c                   15.5059(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1399.4(2)
_computing_cell_refinement
;
SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 1997.
;
_computing_data_collection
;
SMART for Windows NT, Bruker AXS Inc., 1998.
;
_computing_data_reduction
;
SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 1997.
;
_computing_molecular_graphics
;
XP-Interactive Molecular Graphics, Ver. 6.10, Bruker AXS Inc., 2000.
;
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2998
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.936
_exptl_absorpt_correction_T_max  0.5222
_exptl_absorpt_correction_T_min  0.1179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.894
_refine_diff_density_min         -4.249
_refine_diff_density_rms         0.578
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1501
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0708
_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)+(0.1278P)²+137.6907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.1969
_reflns_number_gt                1412
_reflns_number_total             1501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg070622x-file003.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4504448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
I1 I 0.26234(5) 0.0000 0.37475(8) 0.0131(4) Uani 1 2 d S
I2 I 0.09102(8) 0.0000 0.48049(12) 0.0426(6) Uani 1 2 d S
I3 I 0.09529(6) -1.0000 0.03099(9) 0.0204(4) Uani 1 2 d S
I4 I 0.26440(5) -0.5000 0.13044(8) 0.0148(4) Uani 1 2 d S
Cu1 Cu 0.20757(13) 0.0000 0.5173(2) 0.0313(7) Uani 1 2 d S
Cu2 Cu 0.14339(12) 0.0000 0.3352(2) 0.0274(7) Uani 1 2 d S
Cu3 Cu 0.14243(13) -0.5000 0.12612(18) 0.0271(7) Uani 1 2 d S
Cu4 Cu 0.21359(15) -1.0000 0.0355(2) 0.0365(8) Uani 1 2 d S
S1 S 0.11608(19) -0.5000 0.2636(3) 0.0117(9) Uani 1 2 d S
N1 N -0.0040(10) -0.5000 0.1792(15) 0.039(5) Uani 1 2 d SU
H1 H 0.0100 -0.5000 0.1302 0.047 Uiso 1 2 calc SR
C1 C 0.0361(8) -0.5000 0.2547(13) 0.014(4) Uani 1 2 d SU
C2 C 0.0121(10) -0.5000 0.3300(15) 0.027(5) Uani 1 2 d SU
H2 H 0.0382 -0.5000 0.3824 0.033 Uiso 1 2 calc SR
C3 C -0.0515(13) -0.5000 0.3317(19) 0.042(6) Uani 1 2 d SU
H3 H -0.0661 -0.5000 0.3852 0.050 Uiso 1 2 calc SR
C4 C -0.0890(11) -0.5000 0.2633(16) 0.032(5) Uani 1 2 d SU
H4 H -0.1308 -0.5000 0.2662 0.038 Uiso 1 2 calc SR
C5 C -0.0666(12) -0.5000 0.1795(19) 0.039(6) Uani 1 2 d SU
H5 H -0.0934 -0.5000 0.1277 0.047 Uiso 1 2 calc SR
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
Cu2 I1 Cu1 68.71(10) . .
Cu2 I1 Cu1 107.52(8) . 7_556
Cu1 I1 Cu1 65.40(8) . 7_556
Cu2 I1 Cu1 107.52(8) . 7_546
Cu1 I1 Cu1 65.40(8) . 7_546
Cu1 I1 Cu1 100.50(11) 7_556 7_546
Cu1 I2 Cu2 69.38(10) . .
Cu4 I3 Cu3 70.78(8) . .
Cu4 I3 Cu3 70.78(8) . 1_545
Cu3 I3 Cu3 101.49(10) . 1_545
Cu4 I4 Cu4 65.92(9) 7_535 .
Cu4 I4 Cu4 65.92(9) 7_535 1_565
Cu4 I4 Cu4 100.17(11) . 1_565
Cu4 I4 Cu3 106.88(10) 7_535 .
Cu4 I4 Cu3 69.18(8) . .
Cu4 I4 Cu3 69.18(8) 1_565 .
I2 Cu1 I1 111.98(12) . .
I2 Cu1 I1 107.11(9) . 7_556
I1 Cu1 I1 114.60(8) . 7_556
I2 Cu1 I1 107.11(9) . 7_546
I1 Cu1 I1 114.60(8) . 7_546
I1 Cu1 I1 100.50(11) 7_556 7_546
I2 Cu1 Cu1 128.20(11) . 7_556
I1 Cu1 Cu1 57.61(10) . 7_556
I1 Cu1 Cu1 57.00(7) 7_556 7_556
I1 Cu1 Cu1 123.60(16) 7_546 7_556
I2 Cu1 Cu1 128.20(11) . 7_546
I1 Cu1 Cu1 57.61(10) . 7_546
I1 Cu1 Cu1 123.60(16) 7_556 7_546
I1 Cu1 Cu1 57.00(7) 7_546 7_546
Cu1 Cu1 Cu1 91.13(17) 7_556 7_546
I2 Cu1 Cu2 57.06(9) . .
I1 Cu1 Cu2 54.91(8) . .
I1 Cu1 Cu2 129.53(5) 7_556 .
I1 Cu1 Cu2 129.53(5) 7_546 .
Cu1 Cu1 Cu2 93.49(14) 7_556 .
Cu1 Cu1 Cu2 93.49(14) 7_546 .
S1 Cu2 S1 120.1(2) . 1_565
S1 Cu2 I1 106.94(12) . .
S1 Cu2 I1 106.94(12) 1_565 .
S1 Cu2 I2 106.39(13) . .
S1 Cu2 I2 106.39(13) 1_565 .
I1 Cu2 I2 109.94(11) . .
S1 Cu2 Cu1 119.95(11) . .
S1 Cu2 Cu1 119.95(11) 1_565 .
I1 Cu2 Cu1 56.38(9) . .
I2 Cu2 Cu1 53.56(9) . .
S1 Cu3 I3 112.71(10) . .
S1 Cu3 I3 112.71(10) . 1_565
I3 Cu3 I3 101.49(10) . 1_565
S1 Cu3 I4 111.15(15) . .
I3 Cu3 I4 109.17(8) . .
I3 Cu3 I4 109.17(8) 1_565 .
S1 Cu3 Cu4 130.06(10) . 1_565
I3 Cu3 Cu4 117.07(12) . 1_565
I3 Cu3 Cu4 53.77(6) 1_565 1_565
I4 Cu3 Cu4 55.40(7) . 1_565
S1 Cu3 Cu4 130.06(10) . .
I3 Cu3 Cu4 53.77(6) . .
I3 Cu3 Cu4 117.07(12) 1_565 .
I4 Cu3 Cu4 55.40(7) . .
Cu4 Cu3 Cu4 84.98(12) 1_565 .
I3 Cu4 I4 106.78(12) . 7_535
I3 Cu4 I4 110.87(10) . .
I4 Cu4 I4 114.08(9) 7_535 .
I3 Cu4 I4 110.87(10) . 1_545
I4 Cu4 I4 114.08(9) 7_535 1_545
I4 Cu4 I4 100.17(11) . 1_545
I3 Cu4 Cu4 126.36(12) . 7_535
I4 Cu4 Cu4 57.10(12) 7_535 7_535
I4 Cu4 Cu4 56.98(7) . 7_535
I4 Cu4 Cu4 122.49(17) 1_545 7_535
I3 Cu4 Cu4 126.36(12) . 7_525
I4 Cu4 Cu4 57.10(12) 7_535 7_525
I4 Cu4 Cu4 122.49(17) . 7_525
I4 Cu4 Cu4 56.98(7) 1_545 7_525
Cu4 Cu4 Cu4 89.72(19) 7_535 7_525
I3 Cu4 Cu3 55.46(8) . .
I4 Cu4 Cu3 127.95(9) 7_535 .
I4 Cu4 Cu3 55.42(6) . .
I4 Cu4 Cu3 117.94(13) 1_545 .
Cu4 Cu4 Cu3 92.45(6) 7_535 .
Cu4 Cu4 Cu3 174.74(19) 7_525 .
I3 Cu4 Cu3 55.46(8) . 1_545
I4 Cu4 Cu3 127.95(9) 7_535 1_545
I4 Cu4 Cu3 117.94(13) . 1_545
I4 Cu4 Cu3 55.42(6) 1_545 1_545
Cu4 Cu4 Cu3 174.74(19) 7_535 1_545
Cu4 Cu4 Cu3 92.45(6) 7_525 1_545
Cu3 Cu4 Cu3 84.98(12) . 1_545
C1 S1 Cu3 108.1(7) . .
C1 S1 Cu2 103.0(3) . .
Cu3 S1 Cu2 110.76(13) . .
C1 S1 Cu2 103.0(3) . 1_545
Cu3 S1 Cu2 110.76(13) . 1_545
Cu2 S1 Cu2 120.1(2) . 1_545
C1 N1 C5 122(2) . .
C1 N1 H1 119.1 . .
C5 N1 H1 119.1 . .
C2 C1 N1 117.0(19) . .
C2 C1 S1 116.5(16) . .
N1 C1 S1 126.5(16) . .
C1 C2 C3 122(2) . .
C1 C2 H2 119.0 . .
C3 C2 H2 119.0 . .
C4 C3 C2 122(3) . .
C4 C3 H3 119.0 . .
C2 C3 H3 119.0 . .
C3 C4 C5 119(2) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N1 C5 C4 118(2) . .
N1 C5 H5 121.1 . .
C4 C5 H5 121.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu2 2.616(3) .
I1 Cu1 2.662(3) .
I1 Cu1 2.681(2) 7_556
I1 Cu1 2.681(2) 7_546
I2 Cu1 2.560(3) .
I2 Cu2 2.671(4) .
I3 Cu4 2.607(3) .
I3 Cu3 2.662(2) .
I3 Cu3 2.662(2) 1_545
I4 Cu4 2.683(4) 7_535
I4 Cu4 2.687(2) .
I4 Cu4 2.687(2) 1_565
I4 Cu3 2.688(3) .
Cu1 I1 2.681(2) 7_556
Cu1 I1 2.681(2) 7_546
Cu1 Cu1 2.886(4) 7_556
Cu1 Cu1 2.886(4) 7_546
Cu1 Cu2 2.979(4) .
Cu2 S1 2.379(3) .
Cu2 S1 2.379(3) 1_565
Cu3 S1 2.286(5) .
Cu3 I3 2.662(2) 1_565
Cu3 Cu4 3.051(3) 1_565
Cu3 Cu4 3.051(3) .
Cu4 I4 2.683(4) 7_535
Cu4 I4 2.687(2) 1_545
Cu4 Cu4 2.922(5) 7_535
Cu4 Cu4 2.922(5) 7_525
Cu4 Cu3 3.051(3) 1_545
S1 C1 1.754(19) .
S1 Cu2 2.379(3) 1_545
N1 C1 1.37(3) .
N1 C5 1.38(3) .
N1 H1 0.8600 .
C1 C2 1.35(3) .
C2 C3 1.41(3) .
C2 H2 0.9300 .
C3 C4 1.25(4) .
C3 H3 0.9300 .
C4 C5 1.45(3) .
C4 H4 0.9300 .
C5 H5 0.9300 .
