Synthesis and Oxygenation of a Nickel(II) and Zinc(II) Dithiolate: An Experimental and Theoretical Comparison
Craig A. Grapperhaus; Christopher S. Mullins; Pawel M. Kozlowski; Mark S. Mashuta; Inorganic Chemistry 43 (2004) 2859–2866; doi:10.1021/ic035205y

data_4310913
_publ_contact_author_address
' Department of Chemistry, University of Louisville, Louisville, KY 40292, USA'
_publ_contact_author_email       craig.grapperhaus@louisville.edu
_publ_contact_author_fax         502-852-8149
_publ_contact_author_name        'Grapperhaus, Craig A.'
_publ_contact_author_phone       502-852-5932
_publ_section_title
;
 Synthesis and Oxygenation of a Nickel(II) and Zinc(II) Dithiolate: An
 Experimental and Theoretical Comparison
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2859
_journal_page_last               2866
_journal_paper_doi               10.1021/ic035205y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 H26 N2 Ni S2'
_chemical_formula_sum            'C12 H26 N2 Ni S2'
_chemical_formula_weight         321.18
_chemical_name_common            '[(bmmp-TASN)Ni]'
_chemical_name_systematic
; 
 [(bmmp-TASN)Ni] 
;
_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_date             'November 25, 2001'
_audit_creation_method           SHELXL-97
_audit_update_record
;
  December_21_2001 text and data added by Mark S. Mashuta
  Oct_6_2003 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.562(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1621(10)
_cell_length_b                   20.7343(10)
_cell_length_c                   12.3340(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     1558.3(3)
_computing_cell_refinement       'Enraf-Nonius Diffractometer Control'
_computing_data_collection       'Enraf-Nonius Diffractometer Control'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'data from \w/2\q_scans'
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_source         'normal focus Philips Mo tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2873
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        'not applied (less than 0.5)'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0069(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+1.1806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                2395
_reflns_number_total             2742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035205ysi20031021_120352_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4310913