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_4088072
_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         'C46 H38 N P2 Ru, C24 B F20'
_chemical_formula_sum            'C70 H38 B F20 N P2 Ru'
_chemical_formula_weight         1446.83
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.0631(5)
_cell_angle_beta                 105.0829(5)
_cell_angle_gamma                94.3895(5)
_cell_formula_units_Z            2
_cell_length_a                   13.0253(5)
_cell_length_b                   13.4007(5)
_cell_length_c                   18.4817(7)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.26
_cell_volume                     3041.5(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    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.380
_diffrn_reflns_theta_min         1.165
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9823
_exptl_absorpt_correction_T_min  0.9063
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         14662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0408P)^2^+1.1250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12370
_reflns_number_total             14662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00835_si_001.cif
_cod_data_source_block           7
_cod_database_code               4088072
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              16908
_shelx_hkl_checksum              10035