Syntheses of RuHCl(CO)(PAr3)3 and RuH2(CO)(PAr3)3 Containing Various Triarylphosphines and Their Use for Arylation of Sterically Congested Aromatic C–H Bonds
Ogiwara, Yohei; Miyake, Masashi; Kochi, Takuya; Kakiuchi, Fumitoshi; Organometallics 36 (2017) 159–; doi:10.1021/acs.organomet.6b00540

data_4086879
_publ_section_title
;
 Syntheses of RuHCl(CO)(PAr3)3 and RuH2(CO)(PAr3)3 Containing Various
 Triarylphosphines and Their Use for Arylation of Sterically Congested
 Aromatic C--H Bonds
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              159
_journal_paper_doi               10.1021/acs.organomet.6b00540
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C65 H68 O1.5 P3 Ru'
_chemical_formula_weight         1067.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.5734(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.406(2)
_cell_length_b                   13.9274(6)
_cell_length_c                   20.4289(8)
_cell_measurement_reflns_used    26196
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.03
_cell_volume                     11636.3(9)
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43666
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.741
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10218
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+47.7311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7427
_reflns_number_total             10218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00540_si_002.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 4086879--4086881.cif.'
_cod_original_cell_volume        11636.2(9)
_cod_original_formula_sum        'C65 H68 O1.50 P3 Ru'
_cod_database_code               4086879
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-3
_shelx_res_checksum              22391
_shelx_hkl_checksum              76902