The First Systematic Synthesis of Heterobimetallic Dithiolene-Bridged Complexes. Synthesis and Characterization of Metal Complexes of 4-(1',2'-Ethylenedithiolate)-1,3-dithiole-2-one and Dimeric Metal Complexes of 1,2,3,4-Butadienetetrathiolate
Christopher E. Keefer; Suzanne T. Purrington; Robert D. Bereman; Paul D. Boyle; Inorganic Chemistry 38 (1999) 5437–5442; doi:10.1021/ic990841a

data_4322408
_publ_contact_author
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Professor Robert D. Bereman
Department of Chemistry
Box 8204
North Carolina State University
Raleigh, NC 27695-8204
USA
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_publ_contact_author_email       R_Bereman@ncsu.edu
_publ_contact_author_fax         1(919)5155079
_publ_contact_author_phone       1(919)5151963
_publ_section_title
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 The First Systematic Synthesis of Heterobimetallic Dithiolene-Bridged
 Complexes. Synthesis and Characterization of Metal Complexes of
 4-(1',2'-Ethylenedithiolate)-1,3-dithiole-2-one and Dimeric Metal
 Complexes of 1,2,3,4-Butadienetetrathiolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5437
_journal_page_last               5442
_journal_paper_doi               10.1021/ic990841a
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C26 H40 N Ni O2 S8'
_chemical_formula_weight         713.78
_chemical_name_systematic
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 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.8160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3508(2)
_cell_length_b                   26.4703(7)
_cell_length_c                   15.2778(3)
_cell_measurement_reflns_used    5638
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.59
_cell_volume                     3327.69(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measurement_device       'Siemens SMART-CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30337
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  1.065
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_obs          0.0834
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+8.2985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2167
_refine_ls_wR_factor_obs         0.1948
_reflns_number_observed          4013
_reflns_number_total             5685
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990841a_1.cif
_cod_data_source_block           4
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+8.2985P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+8.2985P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322408