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_4074621
_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         'C31 H35 B F3 Ir N6 O2'
_chemical_formula_sum            'C31 H35 B F3 Ir N6 O2'
_chemical_formula_weight         783.66
_chemical_name_common            'compound 5'
_chemical_name_systematic
; 
(Tp^Me2^)Ir(CF~3~COO)(Ph)(=C(Me)Ph)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.392(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.4856(13)
_cell_length_b                   19.3601(14)
_cell_length_c                   20.1012(15)
_cell_measurement_reflns_used    6974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      2.34
_cell_volume                     6418.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61470
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.215
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS V2.10'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         18442
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0358P)^2^+8.9717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                14785
_reflns_number_total             18492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050634k_si.cif
_cod_data_source_block           compd5
_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_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074621