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_4073513
_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         'C76 H164 Li2 O4 P2 Si14, C6 H14'
_chemical_formula_sum            'C41 H89 Li O2 P Si7'
_chemical_formula_weight         848.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1418(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.4620(4)
_cell_length_b                   12.3405(2)
_cell_length_c                   36.7695(6)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.85
_cell_volume                     11040.3(3)
_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 7.31
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            92054
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.9136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         19339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0832P)^2^+14.9147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                13671
_reflns_number_total             19339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700412g-file004.cif
_cod_data_source_block           tmsli
_cod_original_sg_symbol_Hall     '    -P 2yab'
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4073513