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_4078804
_publ_section_title
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 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            'C30 H49 Ir N Si Ta'
_chemical_formula_weight         824.94
_chemical_name_systematic
; 
 ? 
;
_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                 107.6480(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0774(4)
_cell_length_b                   21.5886(5)
_cell_length_c                   20.0210(6)
_cell_measurement_reflns_used    58896
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     6210.1(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58896
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    7.859
_exptl_absorpt_correction_T_max  0.6754
_exptl_absorpt_correction_T_min  0.4275
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (T.Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         14190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+5.9757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                11848
_reflns_number_total             14572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300429u_si_002.cif
_cod_data_source_block           4c
_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 2.4.2 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      P21/n
_cod_database_code               4078804