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_4302271
_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         'C51 H61 N4 O2 Ta, 1.5(C6 H6)'
_chemical_formula_sum            'C60 H70 N4 O2 Ta'
_chemical_formula_weight         1060.15
_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                 105.9790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.7250(8)
_cell_length_b                   17.8546(5)
_cell_length_c                   23.6141(7)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.03
_cell_measurement_theta_min      2.45
_cell_volume                     10427.1(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 16 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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            233565
_diffrn_reflns_theta_full        43.26
_diffrn_reflns_theta_max         43.26
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.7382
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
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_refine_diff_density_min         -2.632
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
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_refine_ls_number_reflns         38134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.009
_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          0.0520
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                25419
_reflns_number_total             38134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802234x_si_002_2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
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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_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_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302271