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_4320032
_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_formula_sum            'C24 H43 Cl N5 Si2 Ta'
_chemical_formula_weight         674.21
_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   'constrained to idealised positions'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Fourier difference methods'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.560(5)
_cell_length_b                   16.571(4)
_cell_length_c                   22.319(6)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      26
_cell_volume                     5755(3)
_computing_cell_refinement       'STADI4 v1.07'
_computing_data_collection       'STADI4 v1.07 (Stoe, 1997)'
_computing_data_reduction        'XRED v1.09 (Stoe, 1996)'
_computing_molecular_graphics    'SHELXTL v5.03 (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Stoe stadi-4'
_diffrn_measurement_method       'omega theta'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5600
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%
;
random variation; +/-2.5 for crystal 1, +/-2.2 for crystal 2
;
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.017
_exptl_absorpt_correction_T_max  '0.366 for crystal 1, 0.499 for crystal 2'
_exptl_absorpt_correction_T_min  '0.257 for crystal 1, 0.319 for crystal 2'
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          '0.45 crystal 1, 0.25 crystal 2'
_exptl_crystal_size_mid          '0.41 crystal 1, 0.25 crystal 2'
_exptl_crystal_size_min          '0.20 crystal 1, 0.20 crystal 2'
_refine_diff_density_max         1.461
_refine_diff_density_min         -2.578
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+73.9272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                4419
_reflns_number_total             5600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0102541_4.cif
_cod_data_source_block           COMPOUND_3
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+73.9272P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+73.9272P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4320032