#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/04/7110471.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110471
loop_
_publ_author_name
'Matthew Cocker, T.'
'Bachman, Robert E.'
_publ_section_title
;
 Isolation and crystal structure of a novel dinuclear nickel(II) O-bound
 sulfinate from the oxidation of
 2,2′-bipyridine-1,2-benzenedithiolatonickel(II)
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              875
_journal_paper_doi               10.1039/a900673g
_journal_year                    1999
_chemical_formula_sum            'C27.5 H20 N4.5 Ni O6.5 S2'
_chemical_formula_weight         640.31
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.0170(10)
_cell_angle_beta                 101.8868(3)
_cell_angle_gamma                110.0760(10)
_cell_formula_units_Z            2
_cell_length_a                   9.31350(10)
_cell_length_b                   12.5526(2)
_cell_length_c                   12.7451(2)
_cell_measurement_reflns_used    5387
_cell_measurement_temperature    173(2)
_cell_volume                     1344.26(4)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14865
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             657
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6302
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0307P)²+2.4213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                4041
_reflns_number_total             6302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900673gsup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1344.26(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C27.50 H20 N4.50 Ni O6.50 S2'
_cod_database_code               7110471
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
Ni1 Ni 0.83181(7) 0.16391(5) 0.79732(4) 0.01960(15) Uani 1 1 d .
S1 S 1.00110(16) 0.28935(10) 0.60544(9) 0.0309(3) Uani 1 1 d .
S2 S 1.20668(13) 0.30038(9) 0.87085(8) 0.0209(2) Uani 1 1 d .
O1 O 0.9081(4) 0.2076(2) 0.6614(2) 0.0256(7) Uani 1 1 d .
O2 O 1.0513(4) 0.2640(2) 0.8978(2) 0.0229(7) Uani 1 1 d .
O3 O 1.1068(5) 0.2453(3) 0.5623(3) 0.0532(11) Uani 1 1 d .
O4 O 0.9063(5) 0.3255(3) 0.5259(3) 0.0645(14) Uani 1 1 d .
O5 O 1.2188(4) 0.2137(2) 0.7940(2) 0.0255(7) Uani 1 1 d .
O6 O 1.3330(4) 0.3426(3) 0.9704(2) 0.0275(7) Uani 1 1 d .
N1 N 0.7689(4) 0.0996(3) 0.9316(3) 0.0204(8) Uani 1 1 d .
N11 N 0.8811(4) 0.0155(3) 0.7829(3) 0.0224(8) Uani 1 1 d .
N21 N 0.6021(4) 0.0860(3) 0.7003(3) 0.0214(8) Uani 1 1 d .
N31 N 0.7563(4) 0.2998(3) 0.8082(3) 0.0232(8) Uani 1 1 d .
C2 C 0.7786(5) -0.0046(4) 0.9399(3) 0.0225(9) Uani 1 1 d .
C3 C 0.7381(6) -0.0591(4) 1.0240(4) 0.0304(11) Uani 1 1 d .
H3A H 0.7431 -0.1331 1.0274 0.036 Uiso 1 1 calc R
C4 C 0.6904(6) -0.0066(4) 1.1032(4) 0.0322(11) Uani 1 1 d .
H4A H 0.6643 -0.0427 1.1622 0.039 Uiso 1 1 calc R
C5 C 0.6813(6) 0.0992(4) 1.0949(4) 0.0313(11) Uani 1 1 d .
H5A H 0.6480 0.1373 1.1479 0.038 Uiso 1 1 calc R
C6 C 0.7214(6) 0.1495(4) 1.0079(3) 0.0280(11) Uani 1 1 d .
H6A H 0.7147 0.2227 1.0025 0.034 Uiso 1 1 calc R
C12 C 0.8389(5) -0.0528(4) 0.8549(3) 0.0230(9) Uani 1 1 d .
C13 C 0.8515(6) -0.1602(4) 0.8489(4) 0.0310(11) Uani 1 1 d .
H13A H 0.8223 -0.2066 0.9011 0.037 Uiso 1 1 calc R
C14 C 0.9066(6) -0.1982(4) 0.7665(4) 0.0366(12) Uani 1 1 d .
H14A H 0.9144 -0.2720 0.7604 0.044 Uiso 1 1 calc R
C15 C 0.9509(6) -0.1286(4) 0.6924(4) 0.0356(12) Uani 1 1 d .
H15A H 0.9889 -0.1538 0.6346 0.043 Uiso 1 1 calc R
C16 C 0.9385(6) -0.0215(4) 0.7043(3) 0.0278(10) Uani 1 1 d .
H16A H 0.9718 0.0276 0.6550 0.033 Uiso 1 1 calc R
C22 C 0.5212(5) 0.1560(4) 0.6864(3) 0.0236(10) Uani 1 1 d .
C23 C 0.3652(6) 0.1161(4) 0.6231(3) 0.0295(11) Uani 1 1 d .
H23A H 0.3096 0.1668 0.6149 0.035 Uiso 1 1 calc R
C24 C 0.2935(6) 0.0014(4) 0.5727(4) 0.0327(11) Uani 1 1 d .
H24A H 0.1875 -0.0279 0.5289 0.039 Uiso 1 1 calc R
C25 C 0.3766(6) -0.0707(4) 0.5864(3) 0.0300(11) Uani 1 1 d .
H25A H 0.3290 -0.1499 0.5522 0.036 Uiso 1 1 calc R
C26 C 0.5296(6) -0.0256(4) 0.6504(3) 0.0272(10) Uani 1 1 d .
H26A H 0.5866 -0.0753 0.6599 0.033 Uiso 1 1 calc R
C32 C 0.6086(5) 0.2773(4) 0.7462(3) 0.0236(10) Uani 1 1 d .
C33 C 0.5452(6) 0.3624(4) 0.7423(4) 0.0313(11) Uani 1 1 d .
H33A H 0.4411 0.3453 0.6991 0.038 Uiso 1 1 calc R
C34 C 0.6354(6) 0.4724(4) 0.8022(4) 0.0376(12) Uani 1 1 d .
H34A H 0.5940 0.5318 0.8003 0.045 Uiso 1 1 calc R
C35 C 0.7857(6) 0.4950(4) 0.8643(4) 0.0331(11) Uani 1 1 d .
H35A H 0.8492 0.5700 0.9062 0.040 Uiso 1 1 calc R
C36 C 0.8425(6) 0.4072(4) 0.8649(3) 0.0286(10) Uani 1 1 d .
H36A H 0.9469 0.4233 0.9071 0.034 Uiso 1 1 calc R
C41 C 1.1264(5) 0.4180(4) 0.7034(3) 0.0247(10) Uani 1 1 d .
C42 C 1.2176(5) 0.4227(3) 0.8081(3) 0.0197(9) Uani 1 1 d .
C43 C 1.3244(5) 0.5288(4) 0.8695(3) 0.0238(10) Uani 1 1 d .
H43A H 1.3846 0.5324 0.9406 0.029 Uiso 1 1 calc R
C44 C 1.3445(6) 0.6293(4) 0.8289(4) 0.0302(11) Uani 1 1 d .
H44A H 1.4219 0.7006 0.8705 0.036 Uiso 1 1 calc R
C45 C 1.2526(6) 0.6261(4) 0.7284(4) 0.0349(12) Uani 1 1 d .
H45A H 1.2637 0.6954 0.7013 0.042 Uiso 1 1 calc R
C46 C 1.1439(6) 0.5211(4) 0.6668(4) 0.0335(12) Uani 1 1 d .
H46A H 1.0796 0.5196 0.5978 0.040 Uiso 1 1 calc R
O1S O 0.5382(13) 0.7221(9) 0.5737(8) 0.085(3) Uiso 0.50 1 d P
N1S N 0.4733(12) 0.5397(8) 0.5060(8) 0.088(3) Uiso 0.50 1 d PD
C1S C 0.587(2) 0.6415(14) 0.5539(17) 0.046(6) Uiso 0.25 1 d PD
C2S C 0.307(3) 0.508(2) 0.4584(19) 0.052(6) Uiso 0.25 1 d P
C3S C 0.4733(12) 0.5397(8) 0.5060(8) 0.088(3) Uiso 0.25 1 d P
C1S' C 0.440(3) 0.6346(17) 0.523(2) 0.064(7) Uiso 0.25 1 d PD
C2S' C 0.649(2) 0.5609(16) 0.5391(13) 0.089(5) Uiso 0.50 1 d P
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
O2 Ni1 N31 91.76(13) . .
O2 Ni1 O1 90.97(12) . .
N31 Ni1 O1 90.79(13) . .
O2 Ni1 N11 94.03(13) . .
N31 Ni1 N11 173.54(15) . .
O1 Ni1 N11 91.98(13) . .
O2 Ni1 N21 170.95(13) . .
N31 Ni1 N21 79.19(14) . .
O1 Ni1 N21 89.49(13) . .
N11 Ni1 N21 94.99(14) . .
O2 Ni1 N1 88.43(12) . .
N31 Ni1 N1 98.19(13) . .
O1 Ni1 N1 171.01(13) . .
N11 Ni1 N1 79.12(14) . .
N21 Ni1 N1 92.52(14) . .
O4 S1 O3 113.2(3) . .
O4 S1 O1 112.7(2) . .
O3 S1 O1 111.0(2) . .
O4 S1 C41 105.3(2) . .
O3 S1 C41 105.8(2) . .
O1 S1 C41 108.36(18) . .
O5 S2 O6 114.49(19) . .
O5 S2 O2 113.02(18) . .
O6 S2 O2 109.70(17) . .
O5 S2 C42 108.00(18) . .
O6 S2 C42 105.99(19) . .
O2 S2 C42 104.94(18) . .
S1 O1 Ni1 151.98(19) . .
S2 O2 Ni1 128.38(16) . .
C6 N1 C2 118.4(4) . .
C6 N1 Ni1 127.0(3) . .
C2 N1 Ni1 114.6(3) . .
C16 N11 C12 118.6(4) . .
C16 N11 Ni1 125.8(3) . .
C12 N11 Ni1 115.4(3) . .
C22 N21 C26 118.4(4) . .
C22 N21 Ni1 115.4(3) . .
C26 N21 Ni1 126.2(3) . .
C36 N31 C32 118.7(4) . .
C36 N31 Ni1 126.0(3) . .
C32 N31 Ni1 115.1(3) . .
N1 C2 C3 121.2(4) . .
N1 C2 C12 115.5(4) . .
C3 C2 C12 123.3(4) . .
C4 C3 C2 120.1(4) . .
C5 C4 C3 118.6(4) . .
C4 C5 C6 119.0(4) . .
N1 C6 C5 122.7(4) . .
N11 C12 C13 121.8(4) . .
N11 C12 C2 115.1(4) . .
C13 C12 C2 123.1(4) . .
C14 C13 C12 119.0(4) . .
C13 C14 C15 119.7(4) . .
C14 C15 C16 118.4(4) . .
N11 C16 C15 122.5(4) . .
N21 C22 C23 122.0(4) . .
N21 C22 C32 115.0(4) . .
C23 C22 C32 123.0(4) . .
C24 C23 C22 118.5(4) . .
C23 C24 C25 119.6(4) . .
C26 C25 C24 118.7(4) . .
N21 C26 C25 122.7(4) . .
N31 C32 C33 121.2(4) . .
N31 C32 C22 115.2(4) . .
C33 C32 C22 123.6(4) . .
C34 C33 C32 119.2(4) . .
C35 C34 C33 119.4(4) . .
C34 C35 C36 118.9(5) . .
N31 C36 C35 122.6(5) . .
C46 C41 C42 118.3(4) . .
C46 C41 S1 115.4(3) . .
C42 C41 S1 126.0(3) . .
C43 C42 C41 119.3(4) . .
C43 C42 S2 115.9(3) . .
C41 C42 S2 124.8(3) . .
C44 C43 C42 121.1(4) . .
C45 C44 C43 120.0(4) . .
C44 C45 C46 119.5(4) . .
C45 C46 C41 121.6(4) . .
C1S' O1S C1S 65.1(14) . .
C3S N1S N1S 0.0(10) 2_666 2_666
C3S N1S C1S 112.4(16) 2_666 .
N1S N1S C1S 112.4(16) 2_666 .
C3S N1S C1S' 171(2) 2_666 .
N1S N1S C1S' 171(2) 2_666 .
C1S N1S C1S' 59.0(16) . .
C3S N1S C2S' 71.2(11) 2_666 2_666
N1S N1S C2S' 71.2(11) 2_666 2_666
C1S N1S C2S' 175.9(15) . 2_666
C1S' N1S C2S' 117.4(18) . 2_666
C3S N1S C2S 116.2(15) 2_666 .
N1S N1S C2S 116.2(15) 2_666 .
C1S N1S C2S 131.2(16) . .
C1S' N1S C2S 72.3(17) . .
C2S' N1S C2S 45.5(11) 2_666 .
C3S N1S C2S' 56.8(9) 2_666 .
N1S N1S C2S' 56.8(9) 2_666 .
C1S N1S C2S' 55.6(12) . .
C1S' N1S C2S' 114.5(17) . .
C2S' N1S C2S' 128.1(10) 2_666 .
C2S N1S C2S' 170.4(14) . .
O1S C1S C1S' 54.1(13) . .
O1S C1S N1S 114.6(17) . .
C1S' C1S N1S 60.8(10) . .
O1S C1S C2S' 175.5(18) . .
C1S' C1S C2S' 130.2(15) . .
N1S C1S C2S' 69.6(12) . .
C2S' C2S N1S 62.9(16) 2_666 .
C2S' C2S C1S' 114(2) 2_666 .
N1S C2S C1S' 51.1(10) . .
O1S C1S' C1S 60.9(17) . .
O1S C1S' N1S 121(2) . .
C1S C1S' N1S 60.2(9) . .
O1S C1S' C2S 177(2) . .
C1S C1S' C2S 116.7(13) . .
N1S C1S' C2S 56.6(13) . .
C2S C2S' C1S 169(2) 2_666 .
C2S C2S' C3S 71.6(17) 2_666 2_666
C1S C2S' C3S 106.7(15) . 2_666
C2S C2S' N1S 71.6(17) 2_666 2_666
C1S C2S' N1S 106.7(15) . 2_666
C3S C2S' N1S 0.0(9) 2_666 2_666
C2S C2S' N1S 123(2) 2_666 .
C1S C2S' N1S 54.8(8) . .
C3S C2S' N1S 51.9(10) 2_666 .
N1S C2S' N1S 51.9(10) 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.054(3) .
Ni1 N31 2.059(4) .
Ni1 O1 2.060(3) .
Ni1 N11 2.066(4) .
Ni1 N21 2.069(4) .
Ni1 N1 2.075(3) .
S1 O4 1.420(4) .
S1 O3 1.452(4) .
S1 O1 1.452(3) .
S1 C41 1.792(4) .
S2 O5 1.436(3) .
S2 O6 1.446(3) .
S2 O2 1.485(3) .
S2 C42 1.786(4) .
N1 C6 1.332(5) .
N1 C2 1.355(5) .
N11 C16 1.341(5) .
N11 C12 1.346(5) .
N21 C22 1.343(5) .
N21 C26 1.345(5) .
N31 C36 1.340(5) .
N31 C32 1.355(5) .
C2 C3 1.380(6) .
C2 C12 1.483(6) .
C3 C4 1.377(6) .
C4 C5 1.373(6) .
C5 C6 1.386(6) .
C12 C13 1.389(6) .
C13 C14 1.371(6) .
C14 C15 1.383(7) .
C15 C16 1.384(6) .
C22 C23 1.395(6) .
C22 C32 1.487(6) .
C23 C24 1.379(6) .
C24 C25 1.381(7) .
C25 C26 1.374(6) .
C32 C33 1.387(6) .
C33 C34 1.384(7) .
C34 C35 1.374(7) .
C35 C36 1.377(6) .
C41 C46 1.391(6) .
C41 C42 1.410(6) .
C42 C43 1.388(6) .
C43 C44 1.380(6) .
C44 C45 1.375(6) .
C45 C46 1.384(6) .
O1S C1S' 1.17(3) .
O1S C1S 1.27(2) .
N1S C3S 1.267(17) 2_666
N1S N1S 1.267(17) 2_666
N1S C1S 1.330(10) .
N1S C1S' 1.338(10) .
N1S C2S' 1.347(18) 2_666
N1S C2S 1.44(3) .
N1S C2S' 1.52(2) .
C1S C1S' 1.31(3) .
C1S C2S' 1.34(3) .
C2S C2S' 1.08(3) 2_666
C2S C1S' 1.64(4) .
C2S' C2S 1.08(3) 2_666
C2S' C3S 1.347(18) 2_666
C2S' N1S 1.347(18) 2_666
