Diastereoselective Routes to [Amino{σ(P):η6-(ansa-phosphinite)benzene}chlororuthenium(II)] PF6Salts: Kinetic versus Thermodynamic Preferences
Weber, Immo; Heinemann, Frank W.; Bauer, Walter; Superchi, Stefano; Zahl, Achim; Richter, Daniela; Zenneck, Ulrich; Organometallics 27 (2008) 4116–; doi:10.1021/om701257m

data_4071097
_publ_section_title
;
 Diastereoselective Routes to
 [Amino{\s(P):\h6-(ansa-phosphinite)benzene}chlororuthenium(II)] PF6Salts:
 Kinetic versus Thermodynamic Preferences
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4116
_journal_paper_doi               10.1021/om701257m
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
 C27 H27 Cl F N O2 P Ru, F6 P, 0.5(C H4 O)
;
_chemical_formula_sum            'C27.5 H29 Cl F7 N O2.5 P2 Ru'
_chemical_formula_weight         744.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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
_cell_angle_alpha                76.588(5)
_cell_angle_beta                 89.832(5)
_cell_angle_gamma                60.962(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9667(9)
_cell_length_b                   10.9759(7)
_cell_length_c                   14.2777(7)
_cell_measurement_reflns_used    320
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     1449.39(19)
_computing_cell_refinement       'EVALCCD (Bruker-Nonius, 2002)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Bruker-Nonius, 2002)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \w-rotations with 2.0 \% and 24 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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43503
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 5835 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   -0.012(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         12743
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                10553
_reflns_number_total             12743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701257m-file004.cif
_cod_data_source_block           iw0404
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C27.50 H29 Cl F7 N O2.50 P2 Ru'
_cod_database_code               4071097