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_7026195
_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         'C51 H82 Cl2 Ir2 N2 P2 Si'
_chemical_formula_sum            'C51 H86 Cl2 Ir2 N2 P2 Si'
_chemical_formula_weight         1272.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   'no H-Atom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.567(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6736(9)
_cell_length_b                   10.0455(7)
_cell_length_c                   19.8282(14)
_cell_measurement_reflns_used    12190
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.08
_cell_volume                     2770.6(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1045
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24195
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    5.007
_exptl_absorpt_correction_T_max  0.6089
_exptl_absorpt_correction_T_min  0.5622
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.447
_refine_diff_density_min         -3.511
_refine_diff_density_rms         0.502
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         12190
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0769P)^2^+123.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2353
_reflns_number_gt                9069
_reflns_number_total             12190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00264j.txt
_cod_data_source_block           (PcyN-P,N)2Ir2H2(m-Cl)(m-H)(m-SiClMes)-(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7026195