Isolation and crystal structure of a novel dinuclear nickel(II) O-bound sulfinate from the oxidation of 2,2′-bipyridine-1,2-benzenedithiolatonickel(II)
Matthew Cocker, T.; Bachman, Robert E.; Chemical Communications  (1999) 875–; doi:10.1039/a900673g

data_7110471
_publ_section_title
;
 Isolation and crystal structure of a novel dinuclear nickel(II) O-bound
 sulfinate from the oxidation of
 2,2&#x2032;-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       '\w 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/[\s^2^(Fo^2^)+(0.0307P)^2^+2.4213P] where P=(Fo^2^+2Fc^2^)/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