Early‒Late Heterobimetallic Complexes with a Ta‒Ir Multiple Bond: Bimetallic Oxidative Additions of C‒H, N‒H, and O‒H Bonds
Oishi, Masataka; Kino, Masashi; Saso, Masayuki; Oshima, Masato; Suzuki, Hiroharu; Organometallics 31 (2012) 4658–; doi:10.1021/om300429u

data_4078806
_publ_section_title
;
 Early--Late Heterobimetallic Complexes with a Ta--Ir Multiple Bond:
 Bimetallic Oxidative Additions of C--H, N--H, and O--H Bonds
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4658
_journal_paper_doi               10.1021/om300429u
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C28 H52 Ir O Si Ta'
_chemical_formula_weight         805.94
_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                86.9420(18)
_cell_angle_beta                 86.5780(16)
_cell_angle_gamma                87.1730(16)
_cell_formula_units_Z            2
_cell_length_a                   10.5120(5)
_cell_length_b                   11.1074(6)
_cell_length_c                   13.3546(8)
_cell_measurement_reflns_used    14395
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.06
_cell_volume                     1552.63(15)
_computing_cell_refinement       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_collection       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_reduction        'PROCESS-AUTO (T.Higashi, 1998)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       'oscillation photograph'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode ultraX18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14395
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    7.857
_exptl_absorpt_correction_T_max  0.5331
_exptl_absorpt_correction_T_min  0.2716
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (T.Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.723
_refine_diff_density_min         -8.255
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0767P)^2^+31.8871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                4921
_reflns_number_total             7057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300429u_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078806