#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310692.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_4310692
loop_
_publ_author_name
'Fouad Bentiss'
'Michel Lagrenée'
'Olivier Mentré'
'Pierre Conflant'
'Hervé Vezin'
'Jean Pierre Wignacourt'
'Elizabeth M. Holt'
_publ_contact_author_address
;                                        Department of Chemistry
                                          Oklahoma State University
                                          Stillwater, Oklahoma 74078
;
_publ_contact_author_email       betsy@biochem.okstate.edu
_publ_contact_author_fax         '405 744 6007'
_publ_contact_author_name        'Dr Elizabeth M. Holt'
_publ_contact_author_phone       '405 744 5949'
_publ_section_title
;
 Intermolecular Magnetic Couplings in the Dinuclear Copper(II) Complex
 μ-Chloro-μ-[2,5-bis(2-pyridyl)-1,3,4-thiadiazole] Aqua Chlorocopper(II)
 Dichlorocopper(II): Synthesis, Crystal Structure, and EPR and Magnetic
 Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1865
_journal_page_last               1873
_journal_paper_doi               10.1021/ic030128s
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 H10 Cl4 Cu2 N4 O S'
_chemical_formula_sum            'C12 H10 Cl4 Cu2 N4 O S'
_chemical_formula_weight         527.18
_chemical_name_common
;
mu-chloro-mu-[2,5-di(2-pyridyl)-1,3,4-thiadiazole] 
aquachlorocopper(II) dichlorocopper(II)
;
_chemical_name_systematic
;
mu-chloro-mu-[2,5-di(2-pyridyl)-1,3,4-thiadiazole] 
aquachlorocopper(II) dichlorocopper(II)
;
_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
_cell_angle_alpha                79.054(5)
_cell_angle_beta                 82.478(6)
_cell_angle_gamma                67.099(5)
_cell_formula_units_Z            2
_cell_length_a                   9.296(3)
_cell_length_b                   9.933(3)
_cell_length_c                   10.412(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.2
_cell_measurement_theta_min      7.0
_cell_volume                     867.8(5)
_computing_cell_refinement       'XSCANS (Siemens, 1991)'
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        'XSCANS (Siemens, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD Brucker Smart'
_diffrn_measurement_method       θ/2θ
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3984
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    3.194
_exptl_absorpt_correction_T_max  23.29
_exptl_absorpt_correction_T_min  2.60
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XEMP,  Siemens (1991)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0968P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                2203
_reflns_number_total             2473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030128s.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4310692
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.63728(6) 0.90808(5) 0.35145(5) 0.0306(2) Uani 1 1 d . . .
Cu2 Cu 0.28419(6) 1.24271(5) 0.23629(5) 0.0297(2) Uani 1 1 d . . .
Cl1 Cl 0.20310(13) 1.47714(12) 0.26190(11) 0.0395(3) Uani 1 1 d . . .
Cl2 Cl 0.42561(13) 1.24007(12) 0.01078(10) 0.0384(3) Uani 1 1 d . . .
Cl3 Cl 0.51053(12) 1.16195(12) 0.35589(10) 0.0350(3) Uani 1 1 d . . .
Cl4 Cl 0.85221(13) 0.89020(13) 0.43418(12) 0.0429(3) Uani 1 1 d . . .
O1 O 0.7044(4) 0.9431(4) 0.1229(3) 0.0430(8) Uani 1 1 d . . .
H1A H 0.7531 0.8625 0.0989 0.064 Uiso 1 1 calc R . .
S1 S 0.24155(12) 0.81043(12) 0.25353(11) 0.0335(3) Uani 1 1 d . . .
C2 C 0.4211(5) 0.7879(5) 0.3000(4) 0.0259(9) Uani 1 1 d . . .
N3 N 0.4374(4) 0.9118(4) 0.2998(3) 0.0268(8) Uani 1 1 d . . .
N4 N 0.3120(4) 1.0313(4) 0.2588(3) 0.0285(8) Uani 1 1 d . . .
C5 C 0.1989(5) 0.9977(4) 0.2300(4) 0.0265(9) Uani 1 1 d . . .
C6 C 0.5582(5) 0.6530(5) 0.3389(4) 0.0269(9) Uani 1 1 d . . .
N7 N 0.6777(4) 0.6854(4) 0.3665(3) 0.0298(8) Uani 1 1 d . . .
C8 C 0.8081(5) 0.5747(5) 0.4048(4) 0.0353(10) Uani 1 1 d . . .
H8A H 0.8916 0.5958 0.4233 0.042 Uiso 1 1 calc R . .
C9 C 0.8229(5) 0.4285(5) 0.4180(4) 0.0354(10) Uani 1 1 d . . .
H9A H 0.9142 0.3528 0.4477 0.042 Uiso 1 1 calc R . .
C10 C 0.7024(5) 0.3964(5) 0.3870(4) 0.0344(10) Uani 1 1 d . . .
H10A H 0.7120 0.2987 0.3929 0.041 Uiso 1 1 calc R . .
C11 C 0.5660(5) 0.5112(5) 0.3469(4) 0.0326(10) Uani 1 1 d . . .
H11A H 0.4820 0.4926 0.3259 0.039 Uiso 1 1 calc R . .
C12 C 0.0612(5) 1.1212(5) 0.1787(4) 0.0290(9) Uani 1 1 d . . .
N13 N 0.0758(4) 1.2528(4) 0.1735(3) 0.0282(8) Uani 1 1 d . . .
C14 C -0.0393(5) 1.3744(5) 0.1235(4) 0.0342(10) Uani 1 1 d . . .
H14A H -0.0309 1.4654 0.1192 0.041 Uiso 1 1 calc R . .
C15 C -0.1708(5) 1.3712(5) 0.0776(4) 0.0393(11) Uani 1 1 d . . .
H15A H -0.2479 1.4581 0.0416 0.047 Uiso 1 1 calc R . .
C16 C -0.1858(5) 1.2381(5) 0.0860(4) 0.0399(11) Uani 1 1 d . . .
H16A H -0.2741 1.2339 0.0568 0.048 Uiso 1 1 calc R . .
C17 C -0.0683(5) 1.1092(5) 0.1383(4) 0.0332(10) Uani 1 1 d . . .
H17A H -0.0767 1.0177 0.1458 0.040 Uiso 1 1 calc R . .
H1B H 0.628(7) 1.023(7) 0.091(6) 0.08(2) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
N3 Cu1 N7 77.34(13) . . yes
N3 Cu1 Cl4 172.59(11) . . yes
N7 Cu1 Cl4 99.43(10) . . yes
N3 Cu1 Cl3 87.13(10) . . yes
N7 Cu1 Cl3 161.55(10) . . yes
Cl4 Cu1 Cl3 94.77(5) . . yes
N3 Cu1 O1 85.45(13) . . yes
N7 Cu1 O1 95.70(12) . . yes
Cl4 Cu1 O1 101.58(9) . . yes
Cl3 Cu1 O1 92.90(9) . . yes
N4 Cu2 N13 77.26(13) . . yes
N4 Cu2 Cl1 162.86(10) . . yes
N13 Cu2 Cl1 96.89(10) . . yes
N4 Cu2 Cl3 86.40(10) . . yes
N13 Cu2 Cl3 160.51(10) . . yes
Cl1 Cu2 Cl3 95.70(4) . . yes
N4 Cu2 Cl2 93.84(10) . . yes
N13 Cu2 Cl2 95.44(9) . . yes
Cl1 Cu2 Cl2 102.80(4) . . yes
Cl3 Cu2 Cl2 96.21(5) . . yes
Cu1 Cl3 Cu2 106.81(4) . . yes
C2 S1 C5 87.1(2) . . yes
N3 C2 C6 115.4(4) . . yes
N3 C2 S1 113.4(3) . . yes
C6 C2 S1 131.1(3) . . yes
C2 N3 N4 113.2(3) . . yes
C2 N3 Cu1 119.3(3) . . yes
N4 N3 Cu1 127.5(3) . . yes
C5 N4 N3 113.1(3) . . yes
C5 N4 Cu2 118.8(3) . . yes
N3 N4 Cu2 128.1(3) . . yes
N4 C5 C12 116.4(4) . . yes
N4 C5 S1 113.1(3) . . yes
C12 C5 S1 130.4(3) . . yes
N7 C6 C11 123.0(4) . . yes
N7 C6 C2 111.8(4) . . yes
C11 C6 C2 125.2(4) . . yes
C8 N7 C6 118.4(4) . . yes
C8 N7 Cu1 125.3(3) . . yes
C6 N7 Cu1 116.2(3) . . yes
N7 C8 C9 121.7(4) . . yes
C10 C9 C8 119.6(4) . . yes
C9 C10 C11 119.1(4) . . yes
C6 C11 C10 118.2(4) . . yes
N13 C12 C17 122.9(4) . . yes
N13 C12 C5 111.5(3) . . yes
C17 C12 C5 125.6(4) . . yes
C14 N13 C12 117.6(4) . . yes
C14 N13 Cu2 126.3(3) . . yes
C12 N13 Cu2 116.0(3) . . yes
N13 C14 C15 122.9(4) . . yes
C16 C15 C14 118.9(4) . . yes
C15 C16 C17 119.7(4) . . yes
C12 C17 C16 117.9(4) . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 1.985(3) . yes
Cu1 N7 2.073(4) . yes
Cu1 Cl4 2.2095(13) . yes
Cu1 Cl3 2.3383(13) . yes
Cu1 O1 2.375(3) . yes
Cu2 N4 1.985(3) . yes
Cu2 N13 2.085(3) . yes
Cu2 Cl1 2.2088(14) . yes
Cu2 Cl3 2.3695(13) . yes
Cu2 Cl2 2.5358(13) . yes
S1 C2 1.718(4) . yes
S1 C5 1.719(4) . yes
C2 N3 1.297(5) . yes
C2 C6 1.478(6) . yes
N3 N4 1.346(5) . yes
N4 C5 1.304(5) . yes
C5 C12 1.462(6) . yes
C6 N7 1.348(5) . yes
C6 C11 1.368(6) . yes
N7 C8 1.326(5) . yes
C8 C9 1.386(6) . yes
C9 C10 1.369(6) . yes
C10 C11 1.384(6) . yes
C12 N13 1.356(5) . yes
C12 C17 1.380(6) . yes
N13 C14 1.332(5) . yes
C14 C15 1.383(6) . yes
C15 C16 1.367(7) . yes
C16 C17 1.390(6) . yes
