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_4316224
_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            'C62.75 H80.5 B1.25 F30 O P6.25 Ru1.25'
_chemical_formula_weight         1754.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                   29.3244(2)
_cell_length_b                   29.3244(2)
_cell_length_c                   17.9383(2)
_cell_measurement_reflns_used    90964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4510
_cell_measurement_theta_min      2.7458
_cell_volume                     15425.5(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            253414
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
;
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         17670
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1192P)^2^+21.6357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                12713
_reflns_number_total             17670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100438d_si_001_9.cif
_cod_data_source_block           p10mkw1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C62.75 H80.50 B1.25 F30 O P6.25 Ru1.25'
_cod_database_code               4316224