Chiral Dicationic Bis(aqua) Complexes [Ru(OH2)2(PNNP)]2+: The Effect of Double Chloride Abstraction on Asymmetric Cyclopropanation
Bonaccorsi, Cristina; Santoro, Francesco; Gischig, Sebastian; Mezzetti, Antonio; Organometallics 25 (2006) 2002–; doi:10.1021/om0510627

data_4074962
_publ_section_title
;
 Chiral Dicationic Bis(aqua) Complexes [Ru(OH2)2(PNNP)]2+:&#x00A0; The
 Effect of Double Chloride Abstraction on Asymmetric Cyclopropanation
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_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2002
_journal_paper_doi               10.1021/om0510627
_journal_volume                  25
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_sum            'C52.5 H37 Cl F36 N2 O2 P2 Ru Sb2'
_chemical_formula_weight         1853.80
_chemical_name_common            '[Ru(PNNP)(OH2)2](SbF6)2'
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3100(15)
_cell_length_b                   22.511(2)
_cell_length_c                   47.384(6)
_cell_measurement_reflns_used    8200
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.222
_cell_volume                     13131(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER APEX'
_diffrn_measurement_method       '\w scans'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            39875
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  0.8618
_exptl_absorpt_correction_T_min  0.7577
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs vers. 2.03'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             7192
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.764
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         13418
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+5.2495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                11736
_reflns_number_total             13418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0510627si20051212_011841.cif
_cod_data_source_block           '[Ru(PNNP)(OH2)2](SbF6)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_formula_sum        'C52.50 H37 Cl F36 N2 O2 P2 Ru Sb2'
_cod_database_code               4074962