Inner- and Outer-Sphere Roles of Ruthenium Phosphido Complexes in the Hydrophosphination of Alkenes
Belli, Roman G.; Burton, Krista M. E.; Rufh, Stephanie A.; McDonald, Robert; Rosenberg, Lisa; Organometallics 34 (2015) 5637–; doi:10.1021/acs.organomet.5b00835

data_4088071
_publ_section_title
;
 Inner- and Outer-Sphere Roles of Ruthenium Phosphido Complexes in the
 Hydrophosphination of Alkenes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5637
_journal_paper_doi               10.1021/acs.organomet.5b00835
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H42 N P2 Ru, C24 B F20, 2.5(C6 H6)'
_chemical_formula_sum            'C91 H57 B F20 N P2 Ru'
_chemical_formula_weight         1718.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                104.6950(4)
_cell_angle_beta                 107.8349(4)
_cell_angle_gamma                108.4208(4)
_cell_formula_units_Z            2
_cell_length_a                   16.0400(6)
_cell_length_b                   16.8124(6)
_cell_length_c                   16.8412(6)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.30
_cell_volume                     3780.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.437
_diffrn_reflns_theta_min         1.385
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9187
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         18521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+1.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15091
_reflns_number_total             18521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00835_si_001.cif
_cod_data_source_block           6
_cod_database_code               4088071
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              81835
_shelx_hkl_checksum              43802