Pincer Phosphine Complexes of Ruthenium: Formation of Ru(P-O-P)(PPh3)HCl (P-O-P = xantphos, DPEphos, (Ph2PCH2CH2)2O) and Ru(dppf)(PPh3)HCl and Characterization of Cationic Dioxygen, Dihydrogen, Dinitrogen, and Arene Coordinated Phosphine Products
Araminta E. W. Ledger; Aitor Moreno; Charles E. Ellul; Mary F. Mahon; Paul S. Pregosin; Michael K. Whittlesey; Jonathan M. J. Williams; Inorganic Chemistry 49 (2010) 7244–7256; doi:10.1021/ic100438d

data_4316220
_publ_section_title
;
 Pincer Phosphine Complexes of Ruthenium: Formation of Ru(P-O-P)(PPh3)HCl
 (P-O-P = xantphos, DPEphos, (Ph2PCH2CH2)2O) and Ru(dppf)(PPh3)HCl and
 Characterization of Cationic Dioxygen, Dihydrogen, Dinitrogen, and Arene
 Coordinated Phosphine Products
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7244
_journal_page_last               7256
_journal_paper_doi               10.1021/ic100438d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C89.5 H61 B Cl F24 O3 P3 Ru'
_chemical_formula_weight         1880.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 97.14
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2770(1)
_cell_length_b                   40.2040(4)
_cell_length_c                   17.2050(2)
_cell_measurement_reflns_used    122700
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     9112.61(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski, Minor 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            126839
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3796
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         15997
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0963
_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^)+(0.1162P)^2^+23.7270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2347
_refine_ls_wR_factor_ref         0.2625
_reflns_number_gt                10693
_reflns_number_total             15997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100438d_si_001_5.cif
_cod_data_source_block           k09mkw11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        9112.55(16)
_cod_original_formula_sum        'C89.50 H61 B Cl F24 O3 P3 Ru'
_cod_database_code               4316220