Synthesis and Characterization of Square Planar Nickel(II)-Arylthiolate Complexes with the Biphenyl-2,2'-dithiolate Ligand
Edurne Erkizia; Rebecca R. Conry; Inorganic Chemistry 39 (2000) 1674–1679; doi:10.1021/ic990931f

data_4320862
_publ_contact_author_address
;   University of Nevada, Reno
    Department of Chemistry 216
    Reno, Nevada  89557   USA
;
_publ_contact_author_email       conry@chem.unr.edu
_publ_contact_author_name        'Rebecca R. Conry'
_publ_section_title
;
 Synthesis and Characterization of Square Planar Nickel(II)-Arylthiolate
 Complexes with the Biphenyl-2,2'-dithiolate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1674
_journal_page_last               1679
_journal_paper_doi               10.1021/ic990931f
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C60 H71 N3 Ni2 S7'
_chemical_formula_weight         1176.04
_chemical_name_common            'complex 1'
_chemical_name_systematic
;  bis(tetraethylammonium)[(tris-2,2'dithiolatobiphenyl)dinickel(II)],
acetonitrile solvate, 0.5 biphenyldisulfide clathrate
;
_chemical_temperature_decomposition 449(2)
_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 generated with manual editing'
_cell_angle_alpha                69.263(10)
_cell_angle_beta                 69.267(8)
_cell_angle_gamma                83.117(10)
_cell_formula_units_Z            2
_cell_length_a                   13.806(2)
_cell_length_b                   14.267(2)
_cell_length_c                   16.873(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      1.97
_cell_volume                     2906.8(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.1715
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7622
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        33
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   'semi-empirical from psi-scans'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         6592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.179
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_obs          0.0752
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2011
_refine_ls_wR_factor_obs         0.1468
_reflns_number_observed          3041
_reflns_number_total             6593
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990931f_1.cif
_cod_data_source_block           complex1.IC990931F
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.0000P] 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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2906.9(7)
_cod_database_code               4320862