Addition of [(eta(5)-C(5)Me(5))IrH(4)] to a zwitterionic silylene: stepwise formation of iridium(V)-silyl and iridium(III)-silylene complexes.
Jungton, Ann-Katrin; Meltzer, Antje; Präsang, Carsten; Braun, Thomas; Driess, Matthias; Penner, Anna; Dalton transactions (Cambridge, England : 2003) 39 (2010) 5436–5438; doi:10.1039/c0dt00236d

data_7026146
_publ_section_title
;
 Addition of [(eta(5)-C(5)Me(5))IrH(4)] to a zwitterionic silylene:
 stepwise formation of iridium(V)-silyl and iridium(III)-silylene
 complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5436
_journal_page_last               5438
_journal_paper_doi               10.1039/c0dt00236d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C39 H59 Ir N2 Si'
_chemical_formula_sum            'C39 H59 Ir N2 Si'
_chemical_formula_weight         776.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1058(4)
_cell_length_b                   11.9735(3)
_cell_length_c                   16.7760(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      1.94
_cell_volume                     3636.87(16)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,360 exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42435
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    3.732
_exptl_absorpt_correction_T_max  0.7545
_exptl_absorpt_correction_T_min  0.5223
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After
that a numerical absorption correction basing on a Gaussian algorithsm
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    none
_exptl_crystal_description       lattice
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.150
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         11005
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0219P)^2^+1.3260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                9327
_reflns_number_total             11005
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c0dt00236d.txt
_cod_data_source_block           c:\anna\akju22a
_cod_database_code               7026146