Synthesis and Properties of a Rhodium Complex Having a Novel β-Ketophosphenato Ligand, a Heavier Congener of a β-Ketoiminato Ligand#
Sasamori, Takahiro; Matsumoto, Teruyuki; Takeda, Nobuhiro; Tokitoh, Norihiro; Organometallics 26 (2007) 3621–; doi:10.1021/om700412g

data_4073511
_publ_section_title
;
 Synthesis and Properties of a Rhodium Complex Having a Novel
 \b-Ketophosphenato Ligand, a Heavier Congener of a \b-Ketoiminato Ligand#
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3621
_journal_paper_doi               10.1021/om700412g
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C39 H76 O P Rh Si6'
_chemical_formula_sum            'C39 H76 O P Rh Si6'
_chemical_formula_weight         863.42
_chemical_name_common            2b
_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                102.3125(13)
_cell_angle_beta                 90.6913(8)
_cell_angle_gamma                104.4184(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0909(2)
_cell_length_b                   11.1677(2)
_cell_length_c                   22.2560(4)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      1.88
_cell_volume                     2367.57(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25098
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.9189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         8695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+3.2521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                7958
_reflns_number_total             8695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700412g-file002.cif
_cod_data_source_block           rhcod
_cod_original_sg_symbol_Hall     '    -P 1'
_cod_database_code               4073511