Reactivity, Structures, and NMR Spectroscopy of Half-Sandwich Pentamethylcyclopentadienyl Rhodium Amido Complexes Relevant to Transfer Hydrogenation
Blacker, A. John; Duckett, Simon B.; Grace, Jake; Perutz, Robin N.; Whitwood, Adrian C.; Organometallics 28 (2009) 1435–; doi:10.1021/om8009969

data_4068645
_publ_section_title
;
 Reactivity, Structures, and NMR Spectroscopy of Half-Sandwich
 Pentamethylcyclopentadienyl Rhodium Amido Complexes Relevant to Transfer
 Hydrogenation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1435
_journal_paper_doi               10.1021/om8009969
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C30 H35 F N2 O3 Rh S, 0.5(C7 H7), C F3 O3 S'
_chemical_formula_sum            'C34.5 H38.5 F4 N2 O6 Rh S2'
_chemical_formula_weight         820.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                107.266(7)
_cell_angle_beta                 113.603(7)
_cell_angle_gamma                97.270(7)
_cell_formula_units_Z            2
_cell_length_a                   12.286(5)
_cell_length_b                   12.454(5)
_cell_length_c                   13.377(5)
_cell_measurement_reflns_used    5934
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.72
_cell_volume                     1719.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23383
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.78
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             841
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0422P)^2^+1.5765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                7779
_reflns_number_total             8538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009969_si_001.cif
_cod_data_source_block           rnp0609m
_cod_original_formula_sum        'C34.50 H38.50 F4 N2 O6 Rh S2'
_cod_database_code               4068645