Group 5 Imido Complexes Derived from Diamido-Pyridine Ligands
Stephen M. Pugh; Alexander J. Blake; Lutz H. Gade; Philip Mountford; Inorganic Chemistry 40 (2001) 3992–4001; doi:10.1021/ic0102541

data_4320030
_publ_contact_author
;
Dr P. Mountford
Inorganic Chemistry Laboratory
South Parks Road
Oxford
OX1 3QR
UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 Group 5 Imido Complexes Derived from Diamido-Pyridine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3992
_journal_page_last               4001
_journal_paper_doi               10.1021/ic0102541
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source
;
[V(N-2,6-C6H3Pri2)Cl3(thf)] + MeC(2-C5H4N)(CH2NHSiMe2Bu-t)2 + NEt3
;
_chemical_formula_moiety         ' C27 H46 Cl2 N4 Si1 V1 '
_chemical_formula_sum            'C27 H46 Cl2 N4 Si V'
_chemical_formula_weight         576.63
_chemical_name_systematic
;
[V(N-2,6-C6H3Pri2){MeC(2-C5H4N)(CH2NH2)(CH2NHSiMe2Bu-t)}Cl2]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   'geometric and difference maps'
_atom_sites_solution_primary     SIR92
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.90(2)
_cell_length_b                   16.834(9)
_cell_length_c                   24.025(13)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      10.0
_cell_volume                     6026(9)
_computing_cell_refinement       'STADI4 (Stoe & Cie 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie 1995a)'
_computing_data_reduction
;
X-RED (Stoe & Cie, 1995b)
CRYSTALS (Watkin et al, 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_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(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.92 - 1.87, scan ratio 2theta:omega = 1.00
 I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_sigmaI/netI    0.2090
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4406
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.27
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'triangluar plate'
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.29
_refine_diff_density_min         -1.00
_refine_ls_abs_structure_Flack   'not required'
_refine_ls_extinction_coef       'not required'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.944
_refine_ls_hydrogen_treatment
;
Hydrogen atoms were refined in a riding model for C-H atoms (placed
in calculated positions). Fractional coordinates for the N-H atoms
(located from difference maps) were refined subject to similarity
restraints on N-H bond lengths. The N-H and C-H U[iso] values were
estimated as 1.3 times the Uequiv of the supporting N or C atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.151
_refine_ls_R_factor_obs          0.099
_refine_ls_shift/esd_max         0.089
_refine_ls_structure_factor_coef F**2
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_all         0.161
_refine_ls_wR_factor_obs         0.125
_reflns_d_resolution_high        0.929
_reflns_d_resolution_low         8.011
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_observed          2202
_reflns_number_total             3933
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic0102541_2.cif
_cod_data_source_block           COMPOUND_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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:
data name '_contact_author_fax' replaced with
'_publ_contact_author_fax' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        6026.3(9)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        ' C27 H46 Cl2 N4 Si1 V1 '
_cod_database_code               4320030