Organo Ruthenium–Nickel Dithiolates with Redox-Responsive Nickel Sites
Chambers, Geoffrey M.; Angamuthu, Raja; Gray, Danielle L.; Rauchfuss, Thomas B.; Organometallics 32 (2013) 6324–; doi:10.1021/om4006824

data_4081852
_publ_contact_author
; 
Thomas B. Rauchfuss
University of Illinois
A328 CLSL, Box 12-6
600 South Mathews Avenue
Urbana, IL 61801
USA
;
_publ_section_title
;
 Organo Ruthenium--Nickel Dithiolates with Redox-Responsive Nickel Sites
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6324
_journal_paper_doi               10.1021/om4006824
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H44 Ni P2 Ru S2 '
_chemical_formula_sum            'C39 H44 Ni P2 Ru S2'
_chemical_formula_weight         798.58
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8534(2)
_cell_length_b                   13.3759(3)
_cell_length_c                   14.4473(4)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.58
_cell_measurement_theta_min      3.30
_cell_volume                     1803.13(7)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  bc25tas
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17673
_diffrn_reflns_theta_full        67.94
_diffrn_reflns_theta_max         67.94
_diffrn_reflns_theta_min         4.62
_exptl_absorpt_coefficient_mu    6.155
_exptl_absorpt_correction_T_max  0.6118
_exptl_absorpt_correction_T_min  0.2138
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_id                bc25tas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -2 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack (1983),  2408 Friedels'
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0233P)^2^+0.5692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                5497
_reflns_number_total             5566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4006824_si_002.cif
_cod_data_source_block           bc25tas
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     'P -2yac '
_cod_original_sg_symbol_H-M      'Pn   '
_cod_database_code               4081852