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_4310914
_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 O2 S2'
_chemical_formula_sum            'C12 H26 N2 Ni O2 S2'
_chemical_formula_weight         353.18
_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             'Jan 21, 2002'
_audit_creation_method           SHELXL-97
_audit_update_record
;
  Jan_21_2002 text and data added by Mark S. Mashuta
  Oct_7_2003 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6040(13)
_cell_length_b                   12.515(3)
_cell_length_c                   20.482(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     1677.8(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7686
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        'not applied (less than 0.5)'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0073(4)
_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   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+1.3644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                2999
_reflns_number_total             3846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035205ysi20031021_120352_2.cif
_cod_data_source_block           2
_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               4310914