#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/36/4323637.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_4323637
loop_
_publ_author_name
'Jorge A. R. Navarro'
'M. Angustias Romero'
'Juan M. Salas'
'Miguel Quirós'
'Edward R. T. Tiekink'
_publ_contact_author
;
 Dr ERT Tiekink,
 Department of Chemistry,
 The University of Adelaide,
 AUSTRALIA 5005
;
_publ_contact_author_email       ' etiekink@chemistry.adelaide.edu.au '
_publ_contact_author_fax         ' 61 8 83034358 '
_publ_contact_author_phone       ' 61 8 83035943 '
_publ_section_title
;
 First Example of Equatorial-Equatorial Disposition of End-to-End
 Thiocyanate Bridges in a Polynuclear Copper(II) Complex and Its Relation
 to the Very Efficient Transmission of the Magnetic Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4988
_journal_page_last               4991
_journal_paper_doi               10.1021/ic970083t
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'C8 H8 Cu N6 O2 S2 '
_chemical_formula_sum            'C8 H8 Cu N6 O2 S2'
_chemical_formula_weight         347.86
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Thu Jul  4 17:53:03 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                89.45(2)
_cell_angle_beta                 77.44(2)
_cell_angle_gamma                69.75(2)
_cell_formula_units_Z            2
_cell_length_a                   8.408(2)
_cell_length_b                   10.581(3)
_cell_length_c                   7.927(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      7.8
_cell_volume                     644.1(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.10183
_diffrn_orient_matrix_UB_12      -0.03098
_diffrn_orient_matrix_UB_13      -0.02788
_diffrn_orient_matrix_UB_21      0.04721
_diffrn_orient_matrix_UB_22      -0.05976
_diffrn_orient_matrix_UB_23      0.10969
_diffrn_orient_matrix_UB_31      -0.06600
_diffrn_orient_matrix_UB_32      0.07531
_diffrn_orient_matrix_UB_33      0.06310
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.53
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3167
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        4.28
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_description       plate
_exptl_crystal_F_000             350.00
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.621
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2143
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0326
_refine_ls_shift/esd_max         0.0033
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0360
_reflns_number_observed          2143
_reflns_number_total             2968
_reflns_observed_criterion       3.00
_cod_data_source_file            ic970083t.cif
_cod_data_source_block           '[IC970083T]'
_cod_original_cell_volume        644.2(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C8 H8 Cu N6 O2 S2 '
_cod_database_code               4323637
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Cu -0.31551(5) -0.38744(4) 0.25347(5) 0.0320(1) Uij ? ?
S(1) -0.8088(1) -0.48447(9) 0.5256(1) 0.0365(2) Uij ? ?
S(2) 0.2285(1) -0.36913(10) -0.0214(1) 0.0444(3) Uij ? ?
O(1) -0.4322(3) -0.1679(2) 0.4302(3) 0.0450(7) Uij ? ?
O(7) -0.7472(4) -0.0015(3) -0.2599(3) 0.0548(8) Uij ? ?
N(1) -0.4575(4) -0.2187(3) -0.2059(3) 0.0394(8) Uij ? ?
N(3) -0.4141(3) -0.2710(3) 0.0625(3) 0.0302(7) Uij ? ?
N(4) -0.6614(3) -0.0854(3) 0.2189(3) 0.0348(8) Uij ? ?
N(8) -0.5841(4) -0.1281(3) -0.0815(3) 0.0334(7) Uij ? ?
N(11) -0.5418(3) -0.3997(3) 0.3496(4) 0.0395(8) Uij ? ?
N(12) -0.0908(4) -0.3739(3) 0.1636(4) 0.0393(8) Uij ? ?
C(2) -0.3606(5) -0.3002(3) -0.1131(4) 0.0387(9) Uij ? ?
C(3a) -0.5554(4) -0.1622(3) 0.0769(4) 0.0297(8) Uij ? ?
C(5') -0.9099(5) 0.1098(4) 0.3657(5) 0.054(1) Uij ? ?
C(5) -0.8025(4) 0.0247(3) 0.2027(5) 0.0390(10) Uij ? ?
C(6) -0.8369(4) 0.0539(3) 0.0440(5) 0.042(1) Uij ? ?
C(7) -0.7297(5) -0.0209(3) -0.1123(5) 0.041(1) Uij ? ?
C(11) -0.6513(4) -0.4353(3) 0.4216(4) 0.0304(8) Uij ? ?
C(12) 0.0416(4) -0.3713(3) 0.0883(4) 0.0320(9) Uij ? ?
H(1o) -0.4482 -0.1915 0.5567 0.0573 Uij ? ?
H(2) -0.2573 -0.3764 -0.1653 0.0464 Uij ? ?
H(2o) -0.3653 -0.1286 0.4188 0.0573 Uij ? ?
H(4) -0.6345 -0.1074 0.3270 0.0573 Uij ? ?
H(5a) -0.8384 0.1470 0.4155 0.0646 Uij ? ?
H(5b) -1.0069 0.1828 0.3393 0.0646 Uij ? ?
H(5c) -0.9539 0.0545 0.4480 0.0646 Uij ? ?
H(6) -0.9403 0.1299 0.0373 0.0502 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 16 0.003 0.002 'International Tables'
H 0 16 0.000 0.000 'International Tables'
Cu 0 2 0.320 1.265 'International Tables'
N 0 12 0.006 0.003 'International Tables'
O 0 4 0.011 0.006 'International Tables'
S 0 4 0.125 0.123 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-3 0 2
-2 0 0
-2 -1 0
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S(1) Cu O(1) 94.33(6) ? ? ? yes
S(1) Cu N(3) 176.93(8) ? ? ? yes
S(1) Cu N(11) 92.43(8) ? ? ? yes
S(1) Cu N(12) 86.67(9) ? ? ? yes
O(1) Cu N(3) 84.22(9) ? ? ? yes
O(1) Cu N(11) 85.0(1) ? ? ? yes
O(1) Cu N(12) 94.0(1) ? ? ? yes
N(3) Cu N(11) 90.1(1) ? ? ? yes
N(3) Cu N(12) 90.7(1) ? ? ? yes
N(11) Cu N(12) 178.6(1) ? ? ? yes
Cu S(1) C(11) 102.6(1) ? ? ? yes
N(8) N(1) C(2) 102.1(3) ? ? ? yes
Cu N(3) C(2) 127.4(2) ? ? ? yes
Cu N(3) C(3a) 129.7(2) ? ? ? yes
C(2) N(3) C(3a) 102.3(3) ? ? ? yes
C(3a) N(4) C(5) 119.6(3) ? ? ? yes
N(1) N(8) C(3a) 109.5(3) ? ? ? yes
N(1) N(8) C(7) 125.5(3) ? ? ? yes
C(3a) N(8) C(7) 124.9(3) ? ? ? yes
Cu N(11) C(11) 163.1(3) ? ? ? yes
Cu N(12) C(12) 170.7(3) ? ? ? yes
N(1) C(2) N(3) 115.8(3) ? ? ? yes
N(3) C(3a) N(4) 129.7(3) ? ? ? yes
N(3) C(3a) N(8) 110.3(3) ? ? ? yes
N(4) C(3a) N(8) 120.0(3) ? ? ? yes
N(4) C(5) C(5') 116.7(3) ? ? ? yes
N(4) C(5) C(6) 120.2(3) ? ? ? yes
C(5') C(5) C(6) 123.1(3) ? ? ? yes
C(5) C(6) C(7) 123.5(3) ? ? ? yes
O(7) C(7) N(8) 119.9(3) ? ? ? yes
O(7) C(7) C(6) 128.5(3) ? ? ? yes
N(8) C(7) C(6) 111.6(3) ? ? ? yes
S(1) C(11) N(11) 179.4(3) ? ? ? yes
S(2) C(12) N(12) 178.9(3) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu S(1) 2.4019(9) ? ? yes
Cu O(1) 2.491(2) ? ? yes
Cu N(3) 2.073(2) ? ? yes
Cu N(11) 1.938(3) ? ? yes
Cu N(12) 1.923(3) ? ? yes
S(1) C(11) 1.643(3) ? ? yes
S(2) C(12) 1.630(3) ? ? yes
O(7) C(7) 1.218(4) ? ? yes
N(1) N(8) 1.371(4) ? ? yes
N(1) C(2) 1.308(4) ? ? yes
N(3) C(2) 1.369(4) ? ? yes
N(3) C(3a) 1.322(4) ? ? yes
N(4) C(3a) 1.342(4) ? ? yes
N(4) C(5) 1.375(4) ? ? yes
N(8) C(3a) 1.352(4) ? ? yes
N(8) C(7) 1.417(4) ? ? yes
N(11) C(11) 1.150(4) ? ? yes
N(12) C(12) 1.152(4) ? ? yes
C(5') C(5) 1.500(5) ? ? yes
C(5) C(6) 1.360(5) ? ? yes
C(6) C(7) 1.419(5) ? ? yes
