Dichloromethane Alkylates a Trithiolato-Ruthenium Complex to Yield a Methylene-Bridged Thioether Core. Synthesis and Structural Comparison to the Thiolato-Ruthenium Precursor
Craig A. Grapperhaus; Selma Poturovic; Mark S. Mashuta; Inorganic Chemistry 41 (2002) 4309–4311; doi:10.1021/ic025735e

data_4318425
_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        'Craig A. Grapperhaus'
_publ_contact_author_phone       502-852-5932
_publ_section_title
;
 Dichloromethane Alkylates a Trithiolato-Ruthenium Complex to Yield a
 Methylene-Bridged Thioether Core. Synthesis and Structural Comparison to
 the Thiolato-Ruthenium Precursor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4309
_journal_page_last               4311
_journal_paper_doi               10.1021/ic025735e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
;
C55 H44 P3 Ru S3, 2(Cl0.5), 3(C0.33 H0.66 Cl0.66),
3(C0.5 H1.5 O0.5 H0.5), 3(H O0.5)
;
_chemical_formula_sum            'C57.5 H54 Cl3 O3 P3 Ru S3'
_chemical_formula_weight         1052.56
_chemical_name_common            '[Ru((DPPBT)~2~CH~2~)(DPPBT)]Cl'
_chemical_name_systematic
; 
 [(bis-(2-diphenylphosphinothiaphenolato)methane)
 (2-diphenylphosphinothiaphenolato)ruthenium(II)]chloride
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   21.5147(7)
_cell_length_b                   21.5147(7)
_cell_length_c                   61.015(4)
_cell_measurement_reflns_used    7951
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.73
_cell_volume                     24459(2)
_computing_cell_refinement       'SAINT 6.2 (Bruker, 1994)'
_computing_data_collection       'SMART 5.624 (Bruker, 1994)'
_computing_data_reduction        'SAINT 6.2 (Bruker, 1994)'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.057
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            72654
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M.; SADABS (1996).

;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             9756
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         12974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.076
_refine_ls_R_factor_gt           0.051
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
  calc w=1/[\s^2^(Fo^2^)+(0.04000P)^2^+21.044P]
  where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.141
_refine_ls_wR_factor_ref         0.152
_reflns_number_gt                9707
_reflns_number_total             12974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025735e_s2_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
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_sg_symbol_H-M      'R -3'
_cod_database_code               4318425