Asymmetric Oxygenation of a Ruthenium Dithiolate Mimics the Mixed Sulfenato/Sulfinato Donor Sets of Nitrile Hydratase and Thiocyanate Hydrolase
César A. Masitas; Mark S. Mashuta; Craig A. Grapperhaus; Inorganic Chemistry 49 (2010) 5344–5346; doi:10.1021/ic100414c

data_4315775
_publ_contact_author_email       grapperhaus@louisville.edu
_publ_contact_author_fax         '(502)852-8149 '
_publ_contact_author_phone       '(502)852-5932 '
_publ_section_title
;
 Asymmetric Oxygenation of a Ruthenium Dithiolate Mimics the Mixed
 Sulfenato/Sulfinato Donor Sets of Nitrile Hydratase and Thiocyanate
 Hydrolase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5344
_journal_page_last               5346
_journal_paper_doi               10.1021/ic100414c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C32 H43 N2 P Ru S3'
_chemical_formula_sum            'C32 H43 N2 P Ru S3'
_chemical_formula_weight         683.90
_chemical_name_common
; 
 (N,N'-bis-(2'-methyl-2'-mercaptopropyl)-1-thia-4,7-diazacyclononane)
 (triphenylphosphine)ruthenium(II)
;
_chemical_name_systematic
; 
 (N,N'-bis-(2'-methyl-2'-mercaptopropyl)-1-thia-4,7-diazacyclononane)
 (triphenylphosphine)ruthenium(II)
;
_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-97
_audit_update_record
;
  Jan_22_2009 text and data added by Mark S. Mashuta
  Jan_24_2009 text and data added by Mark S. Mashuta
  Feb_22_2010 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.848(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.085(4)
_cell_length_b                   16.885(6)
_cell_length_c                   16.110(6)
_cell_measurement_reflns_used    6525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.35
_cell_volume                     2999.6(19)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2002)'
_computing_data_collection       'SMART 5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2002)'
_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-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22663
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.9454
_exptl_absorpt_correction_T_min  0.8745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, (1996).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block_cut
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+1.3979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                5554
_reflns_number_total             6966
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100414c_si_002_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 the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 
;
_cod_original_cell_volume        2999.7(19)
_cod_database_code               4315775