New Cationic and Zwitterionic Cp*M(κ2-P,S) Complexes (M = Rh, Ir): Divergent Reactivity Pathways Arising from Alternative Modes of Ancillary Ligand Participation in Substrate Activation
Kevin D. Hesp; Robert McDonald; Michael J. Ferguson; Mark Stradiotto; Journal of the American Chemical Society 130 (2008) 16394–16406; doi:10.1021/ja8062277

data_4108765
_publ_section_title
;
 New Cationic and Zwitterionic Cp*M(\k2-P,S) Complexes (M = Rh, Ir):
 Divergent Reactivity Pathways Arising from Alternative Modes of Ancillary
 Ligand Participation in Substrate Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16394
_journal_page_last               16406
_journal_paper_doi               10.1021/ja8062277
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C26 H35 Ir O P S, C F3 O3 S'
_chemical_formula_sum            'C27 H35 F3 Ir O4 P S2'
_chemical_formula_weight         767.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.643(2)
_cell_angle_beta                 75.359(2)
_cell_angle_gamma                80.987(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1759(8)
_cell_length_b                   10.9655(8)
_cell_length_c                   15.4658(9)
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.74
_cell_volume                     1474.66(19)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12226
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.773
_exptl_absorpt_correction_T_max  0.7165
_exptl_absorpt_correction_T_min  0.2878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.286
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         12226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                11389
_reflns_number_total             12226
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja8062277_si_001_4.cif
_cod_data_source_block           dal0804
_cod_database_code               4108765