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_4302273
_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         'C37 H55 Cl N3 O2 Ta, 0.75(C4 H10 O)'
_chemical_formula_sum            'C40 H62.5 Cl N3 O2.75 Ta'
_chemical_formula_weight         845.83
_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                 101.802(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7164(6)
_cell_length_b                   18.3370(7)
_cell_length_c                   31.2188(13)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.81
_cell_measurement_theta_min      2.63
_cell_volume                     8246.4(6)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 25 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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            492193
_diffrn_reflns_theta_full        47.98
_diffrn_reflns_theta_max         47.98
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  0.4493
_exptl_absorpt_correction_T_min  0.3540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3484
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         10.132
_refine_diff_density_min         -8.855
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.760
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     905
_refine_ls_number_reflns         75746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.760
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.004
_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          0.1059
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                50883
_reflns_number_total             75746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802234x_si_002_4.cif
_cod_data_source_block           complex3
_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_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      'P 21/n'
_cod_original_formula_sum        'C40 H62.50 Cl N3 O2.75 Ta'
_cod_database_code               4302273