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_4081854
_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_formula_moiety         'C32 H12 B F24, C39 H45 Ni P2 Ru S2'
_chemical_formula_sum            'C71 H57 B F24 Ni P2 Ru S2'
_chemical_formula_weight         1662.82
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                102.3660(10)
_cell_angle_beta                 103.8520(10)
_cell_angle_gamma                92.9970(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3813(15)
_cell_length_b                   16.484(2)
_cell_length_c                   18.511(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.24
_cell_volume                     3561.6(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 V2008/2, TWINABS V2008/2 
(Bruker, 2005 & 2008) 
;
_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      188(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm83tas2
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39382
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9007
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_id                bm83tas2
_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, 4, 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         13125
_refine_ls_number_restraints     2736
_refine_ls_restrained_S_all      1.482
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+3.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                10648
_reflns_number_total             13125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4006824_si_002.cif
_cod_data_source_block           bm83tas2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_H-M      'P-1   '
_cod_database_code               4081854