Silyl Hydrides of Tantalum Supported by Cyclopentadienyl-imido Ligand Sets: Syntheses, X-ray, NMR, and DFT Studies
Ignatov, Stanislav K.; Rees, Nicholas H.; Merkoulov, Alexei A.; Dubberley, Stuart R.; Razuvaev, Alexei G.; Mountford, Philip; Nikonov, Georgii I.; Organometallics 27 (2008) 5968–; doi:10.1021/om800553y

data_4072053
_publ_section_title
;
 Silyl Hydrides of Tantalum Supported by Cyclopentadienyl-imido Ligand
 Sets: Syntheses, X-ray, NMR, and DFT Studies
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5968
_journal_paper_doi               10.1021/om800553y
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C17 H27 Cl2 N1 P1 Si1 Ta1 '
_chemical_formula_sum            'C17 H27 Cl2 N P Si Ta'
_chemical_formula_weight         556.31
_chemical_name_systematic
;                                                                               
 Ta(C5H5)(N-2,6-C6H3Me2)(SiCl2Me)(H)(PMe3)                                                                         
;
_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
_audit_creation_date             03-07-07
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 106.379(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3952(3)
_cell_length_b                   14.8865(4)
_cell_length_c                   13.2074(5)
_cell_measurement_reflns_used    4078
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2149.51(12)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8483
_diffrn_reflns_theta_full        22.094
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         3.174
_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    5.491
_exptl_absorpt_correction_T_max  0.27
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' brown-red '
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    none
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1088.000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         4.45
_refine_diff_density_min         -2.45
_refine_ls_extinction_coef       155.6(212)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.1289
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2326
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.0087
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 5.03 -4.14 1.73 1.13 -0.896 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0798
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0798
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2326
_reflns_number_total             4781
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om800553y_si_001.cif
_cod_data_source_block           aam1b
_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.

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

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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C17 H27 Cl2 N1 P1 Si1 Ta1 '
_cod_database_code               4072053