Synthesis and Reactivity of Tantalum Complexes Supported by Bidentate X2and Tridentate LX2Ligands with Two Phenolates Linked to Pyridine, Thiophene, Furan, and Benzene Connectors: Mechanistic Studies of the Formation of a Tantalum Benzylidene and Insertion Chemistry for Tantalum−Carbon Bonds
Agapie, Theodor; Day, Michael W.; Bercaw, John E.; Organometallics 27 (2008) 6123–; doi:10.1021/om8002653

data_4071605
_publ_section_title
;
 Synthesis and Reactivity of Tantalum Complexes Supported by Bidentate
 X2and Tridentate LX2Ligands with Two Phenolates Linked to Pyridine,
 Thiophene, Furan, and Benzene Connectors: Mechanistic Studies of the
 Formation of a Tantalum Benzylidene and Insertion Chemistry for
 Tantalum&#x2212;Carbon Bonds
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6123
_journal_paper_doi               10.1021/om8002653
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C49 H59 O3 Ta, C5 H12'
_chemical_formula_sum            'C54 H71 O3 Ta'
_chemical_formula_weight         949.06
_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                74.600(2)
_cell_angle_beta                 89.357(2)
_cell_angle_gamma                73.670(2)
_cell_formula_units_Z            4
_cell_length_a                   16.4299(8)
_cell_length_b                   17.0630(9)
_cell_length_c                   18.7829(9)
_cell_measurement_reflns_used    5821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.26
_cell_volume                     4860.3(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 4 \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  0.1412
_diffrn_reflns_av_sigmaI/netI    0.1515
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24079
_diffrn_reflns_theta_full        20.07
_diffrn_reflns_theta_max         20.07
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  0.9095
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_type   Gausian
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0528
_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          0.0956
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                5642
_reflns_number_total             9156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8002653_si_014.cif
_cod_data_source_block           ta33
_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               4071605