Vinylidene Compounds from the Reactions of Me3SiC⋮CSiMe3with TpMe2Ir Precursors. Protonation to Alkylidene and Iridabenzene Structures
Ilg, Kerstin; Paneque, Margarita; Poveda, Manuel L.; Rendón, Nuria; Santos, Laura L.; Carmona, Ernesto; Mereiter, Kurt; Organometallics 25 (2006) 2230–; doi:10.1021/om050634k

data_4074622
_publ_section_title
;
 Vinylidene Compounds from the Reactions of Me3SiC&#x22EE;CSiMe3with
 TpMe2Ir Precursors. Protonation to Alkylidene and Iridabenzene Structures
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2230
_journal_paper_doi               10.1021/om050634k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C23 H34 B Ir N6, 0.5(C4 H10 O)'
_chemical_formula_sum            'C25 H39 B Ir N6 O0.5'
_chemical_formula_weight         634.63
_chemical_name_common            'compound 6 x 1/2Et~2~O'
_chemical_name_systematic
; 
(Tp^Me2^)IrH(CHC(Me)C(Me)CHC(Me)).1/2Et~2~O
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 129.232(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.009(2)
_cell_length_b                   7.9680(5)
_cell_length_c                   25.7960(17)
_cell_measurement_reflns_used    7279
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.66
_cell_volume                     5573.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            41322
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.816
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.366
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         8030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+35.6936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                6812
_reflns_number_total             8030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050634k_si.cif
_cod_data_source_block           compd6.1/2Et2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5573.9(6)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4074622