Diastereoselective Synthesis of Arene Ruthenium(II) Complexes Containing Chiral Phosphetane-Based Tethers†,1
Pinto, Patrícia; Götz, Andreas W.; Marconi, Guido; Hess, Bernd A.; Marinetti, Angela; Heinemann, Frank W.; Zenneck, Ulrich; Organometallics 25 (2006) 2607–; doi:10.1021/om050461z

data_4074608
_publ_section_title
;
 Diastereoselective Synthesis of Arene Ruthenium(II) Complexes Containing
 Chiral Phosphetane-Based Tethers&#x2020;,1
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2607
_journal_paper_doi               10.1021/om050461z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C26 H40 Cl F6 N P2 Ru, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C26.5 H41 Cl2 F6 N P2 Ru'
_chemical_formula_weight         721.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 97.201(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.012(2)
_cell_length_b                   10.631(1)
_cell_length_c                   31.003(3)
_cell_measurement_reflns_used    293
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     6216.8(11)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
'\f- and \w-scans with 0.80 \% and 12 sec per frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            41871
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 4839 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         11249
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                8733
_reflns_number_total             11249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050461zsi20050607_112635.cif
_cod_data_source_block           pp0304
_cod_original_cell_volume        6216.8(9)
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C26.50 H41 Cl2 F6 N P2 Ru'
_cod_database_code               4074608