Synthesis of η(2)-cyclooctene iridium and rhodium complexes supported by a novel P,N-chelate ligand and their reactivity toward hydrosilanes: facile Cl migration from metal to silicon via silylene complex intermediates and formation of a base-stabilised silylene complex.
Hashimoto, Hisako; Suzuki, Toshinori; Tobita, Hiromi; Dalton transactions (Cambridge, England : 2003) 39 (2010) 9386–9400; doi:10.1039/c0dt00264j

data_7026199
_publ_section_title
;
 Synthesis of \h(2)-cyclooctene iridium and rhodium complexes supported by
 a novel P,N-chelate ligand and their reactivity toward hydrosilanes:
 facile Cl migration from metal to silicon via silylene complex
 intermediates and formation of a base-stabilised silylene complex.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9386
_journal_page_last               9400
_journal_paper_doi               10.1039/c0dt00264j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C31 H62 Cl N P Rh Si4, C7 H8'
_chemical_formula_sum            'C38 H70 Cl N P Rh Si4'
_chemical_formula_weight         822.64
_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                70.960(4)
_cell_angle_beta                 77.3979(19)
_cell_angle_gamma                71.675(3)
_cell_formula_units_Z            2
_cell_length_a                   9.53940(10)
_cell_length_b                   13.1147(2)
_cell_length_c                   19.6455(5)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.11
_cell_volume                     2187.12(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19687
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9014
_exptl_absorpt_correction_T_min  0.8854
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0554P)^2^+4.7362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                7779
_reflns_number_total             9660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00264j.txt
_cod_data_source_block
(PcyN-P,N)RhH[SiMe2C(SiMe3)2SiClMe-Si,Si]-(10)-?C7H8
_cod_original_cell_volume        2187.11(7)
_cod_database_code               7026199