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_4071095
_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         'C21 H21 Cl2 O2 P Ru'
_chemical_formula_sum            'C21 H21 Cl2 O2 P Ru'
_chemical_formula_weight         508.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.709(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7487(3)
_cell_length_b                   9.9464(7)
_cell_length_c                   10.4269(6)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     1010.59(10)
_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 40 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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30994
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 2463 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5214
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                4541
_reflns_number_total             5214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701257m-file002.cif
_cod_data_source_block           iw0309a
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4071095