Cyclometalated Tantalum Diphenolate Pincer Complexes: Intramolecular C−H/M−CH3σ-Bond Metathesis May Be Faster than O−H/M−CH3Protonolysis
Agapie, Theodor; Bercaw, John E.; Organometallics 26 (2007) 2957–; doi:10.1021/om700284c

data_4073345
_publ_section_title
;
 Cyclometalated Tantalum Diphenolate Pincer Complexes:&#x00A0;
 Intramolecular C&#x2212;H/M&#x2212;CH3\s-Bond Metathesis May Be Faster
 than O&#x2212;H/M&#x2212;CH3Protonolysis
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2957
_journal_paper_doi               10.1021/om700284c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '2(C35 H47 Cl2 O2 Ta), C6 H6'
_chemical_formula_sum            'C76 H100 Cl4 O4 Ta2'
_chemical_formula_weight         1581.26
_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                88.7480(10)
_cell_angle_beta                 88.5720(10)
_cell_angle_gamma                89.2020(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2683(7)
_cell_length_b                   17.5151(11)
_cell_length_c                   18.2677(12)
_cell_measurement_reflns_used    23349
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.54
_cell_measurement_theta_min      2.16
_cell_volume                     3603.1(4)
_computing_cell_refinement       'Bruker SAINT v6.45A'
_computing_data_collection       'Bruker SMART v5.630'
_computing_data_reduction        'Bruker SAINT v6.45A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF v6.12'
_computing_structure_refinement  'Bruker XL v6.12'
_computing_structure_solution    'Bruker XS v6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.774
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 6 \f settings'
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62765
_diffrn_reflns_theta_full        33.65
_diffrn_reflns_theta_max         33.65
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  0.8298
_exptl_absorpt_correction_T_min  0.4442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         8.416
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.622
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     801
_refine_ls_number_reflns         22143
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.626
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                15102
_reflns_number_total             22143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700284c-file004.cif
_cod_data_source_block           ta19
_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 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073345