Formation of Stabletrans-Dihydride Ruthenium(II) and 16-Electron Ruthenium(0) Complexes Based on Phosphinite PONOP Pincer Ligands. Reactivity toward Water and Electrophiles
Salem, Hiyam; Shimon, Linda J. W.; Diskin-Posner, Yael; Leitus, Gregory; Ben-David, Yehoshoa; Milstein, David; Organometallics 28 (2009) 4791–; doi:10.1021/om9004077

data_4069775
_publ_section_title
;
 Formation of Stabletrans-Dihydride Ruthenium(II) and 16-Electron
 Ruthenium(0) Complexes Based on Phosphinite PONOP Pincer Ligands.
 Reactivity toward Water and Electrophiles
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4791
_journal_paper_doi               10.1021/om9004077
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'C91 H156 Cl N4 O15 P8 Ru4, 4(C23 H39 N O4 P2 Ru)'
_chemical_formula_sum            'C183 H312 Cl N8 O31 P16 Ru8'
_chemical_formula_weight         4459.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.076(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.2782(4)
_cell_length_b                   14.5962(5)
_cell_length_c                   26.5498(8)
_cell_measurement_reflns_used    69538
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.326
_cell_volume                     5145.6(3)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Apex2 CCD'
_diffrn_measurement_method       'phi and omega 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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            69538
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.8010
_exptl_absorpt_correction_T_min  0.6983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2323
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         17123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+5.1224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                14614
_reflns_number_total             17123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9004077_si_001.cif
_cod_data_source_block           complex15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4069775