Group 5 Imido Complexes Supported by Diamido−pyridine Ligands: Aryloxide, Amide, Benzamidinate, Alkyl, and Cyclopentadienyl Derivatives
Pugh, Stephen M.; Trösch, Dominique J. M.; Skinner, Michael E. G.; Gade, Lutz H.; Mountford, Philip; Organometallics 20 (2001) 3531–; doi:10.1021/om0103153

data_4077352
_publ_section_title
;
 Group 5 Imido Complexes Supported by Diamido&#x2212;pyridine
 Ligands:&#x00A0; Aryloxide, Amide, Benzamidinate, Alkyl, and
 Cyclopentadienyl Derivatives
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3531
_journal_paper_doi               10.1021/om0103153
_journal_volume                  20
_journal_year                    2001
_chemical_compound_source
;
 [Ta(N-2,6-C6H3-i-Pr2){MeC(2-NC5H4)(CH2NSiMe3)2}Cl(py)] 
 + Li[O-2,6-C6H3-i-Pr2]
;
_chemical_formula_moiety         ' C39 H63 N4 O1 Si2 Ta1 '
_chemical_formula_sum            'C39 H63 N4 O Si2 Ta'
_chemical_formula_weight         841.08
_chemical_name_systematic
;
 [Ta(N-2,6-C6H3-i-Pr2){MeC(2-NC5H4)(CH2NSiMe3)2}(O-2,6-C6H3-i-Pr2)]
;
_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     SHELXS86
_cell_angle_alpha                96.504(2)
_cell_angle_beta                 98.040(1)
_cell_angle_gamma                92.121(2)
_cell_formula_units_Z            2.00
_cell_length_a                   11.5100(3)
_cell_length_b                   11.9300(2)
_cell_length_c                   14.9600(4)
_cell_measurement_reflns_used    12281
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     2018.02(8)
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection       'DIP2000 software 'Xpress (MAC Science, 1989)''
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type  'Enraf-nonius DIP2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12281
_diffrn_reflns_theta_max         26.59
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    2.78
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.95
_refine_diff_density_min         -1.27
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       43.3(64)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0539
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7025
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0264
_refine_ls_shift/esd_max         0.0038
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0295
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          7025
_reflns_number_total             7866
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            om0103153.cif
_cod_data_source_block           COMPOUND_6
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2018.0
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C39 H63 N4 O1 Si2 Ta1 '
_cod_database_code               4077352