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_4077353
_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
;
 [Nb(NBu-t){MeC(2-NC5H4)(CH2NSiMe3)2}Cl(py)] + LiCH(SiMe3)2
;
_chemical_formula_moiety         ' C26 H57 N4 Nb Si4 '
_chemical_formula_sum            'C26 H57 N4 Nb Si4'
_chemical_formula_weight         631.03
_chemical_melting_point          ?
_chemical_name_systematic
;
 [Nb(NBu-t){MeC(2-NC5H4)(CH2NSiMe3)2}{CH(SiMe3)2}]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                92.37(5)
_cell_angle_beta                 93.16(5)
_cell_angle_gamma                92.05(4)
_cell_formula_units_Z            4.00
_cell_length_a                   11.296(6)
_cell_length_b                   17.556(7)
_cell_length_c                   18.07(1)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    170
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     3572(3)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;SHELXTL/PC (Sheldrick, 1994) 
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      170
_diffrn_measurement_device       'Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
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_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        9.69
_diffrn_standards_interval_time  '60 minutes'
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_exptl_absorpt_coefficient_mu    4.26
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_exptl_absorpt_correction_T_min  0.71
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_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
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'Larson 1970 Crystallographic Computing eq 22'
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_refine_ls_number_reflns         11933
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0531
_refine_ls_shift/esd_max         0.064
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0615
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
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_reflns_limit_k_min              -21
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_observed          11933
_reflns_number_total             14493
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            om0103153.cif
_cod_data_source_block           COMPOUND_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 'none' 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_primary' value 'direct methods' was changed to
'direct'.

'_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 
;
_cod_original_cell_volume        3572.9(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C26 H57 N4 Nb Si4 '
_cod_database_code               4077353