Amine, Amido, and Imido Complexes of Tantalum Supported by a Pyridine-Linked Bis(phenolate) Pincer Ligand: Ta‒N π-Bonding Influences Pincer Ligand Geometry
Tonks, Ian A.; Henling, Larry M.; Day, Michael W.; Bercaw, John E.; Inorganic Chemistry 48 (2009) 5096–5105; doi:10.1021/ic802234x

data_4302276
_publ_section_title
;
 Amine, Amido, and Imido Complexes of Tantalum Supported by a Pyridine-Linked
 Bis(phenolate) Pincer Ligand: Ta--N \p-Bonding Influences Pincer Ligand
 Geometry
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5096
_journal_page_last               5105
_journal_paper_doi               10.1021/ic802234x
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C36 H52 Cl N2 O2 Ta, C4 H10 O'
_chemical_formula_sum            'C40 H62 Cl N2 O3 Ta'
_chemical_formula_weight         835.32
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.510(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.432(2)
_cell_length_b                   13.7447(7)
_cell_length_c                   12.4876(6)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.32
_cell_volume                     8004.6(7)
_computing_cell_refinement       'Bruker SAINT-Plus v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.34A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 11 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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63460
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    2.850
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_correction_T_min  0.5729
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Flake
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
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_refine_diff_density_max         2.305
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.678
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_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          0.0563
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                6077
_reflns_number_total             8588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802234x_si_002_7.cif
_cod_data_source_block           complex6
_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.

'_refine_ls_hydrogen_treatment' value 'Mixed' changed to
'mixed' 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_enum 1527 2010-12-29 10:47:43Z saulius 

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_cell_volume        8004.5(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302276