Synthesis and Properties of Heterocyclic Substituted 1,2-Enedithiolates of Nickel, Palladium, and Platinum
Sharada P. Kaiwar; John K. Hsu; Louise M. Liable-Sands; Arnold L. Rheingold; Robert S. Pilato; Inorganic Chemistry 36 (1997) 4234–4240; doi:10.1021/ic970194s

data_4324020
_publ_contact_author
;
     Dr. R. S. Pilato
     Department of Chemistry and Biochemistry
     University of Maryland
     College Park, MD 20742
;
_publ_contact_author_email       Robert_S_Pilato@umail.umd.edu
_publ_contact_author_fax         '+301 314 9656'
_publ_contact_author_phone       '+301 405 1903'
_publ_section_title
;
 Synthesis and Properties of Heterocyclic Substituted 1,2-Enedithiolates
 of Nickel, Palladium, and Platinum
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4234
_journal_page_last               4240
_journal_paper_doi               10.1021/ic970194s
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C32 H28 N2 Ni P2 S2'
_chemical_formula_weight         625.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.3750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2522(2)
_cell_length_b                   17.1482(3)
_cell_length_c                   15.0820(3)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3166.05(10)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      218(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       phi,omega
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.1302
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11556
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.869
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.978
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_obs          0.0563
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1542
_refine_ls_wR_factor_obs         0.1184
_reflns_number_observed          3840
_reflns_number_total             6718
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970194s.cif
_cod_data_source_block           piln
_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^)+(0.0300P)^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^)+(0.0300P)^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_database_code               4324020