Zirconium, Hafnium, and Tantalum Amide Silyl Complexes: Their Preparation and Conversion to Metallaheterocyclic Complexes via γ-Hydrogen Abstraction by Silyl Ligands
Xianghua Yu; Siwei Bi; Ilia A. Guzei; Zhenyang Lin; Zi-Ling Xue; Inorganic Chemistry 43 (2004) 7111–7119; doi:10.1021/ic049023v

data_4311877
_publ_section_title
;
 Zirconium, Hafnium, and Tantalum Amide Silyl Complexes: Their Preparation
 and Conversion to Metallaheterocyclic Complexes via \g-Hydrogen
 Abstraction by Silyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7111
_journal_page_last               7119
_journal_paper_doi               10.1021/ic049023v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C28 H55 N4 Si3 Ta'
_chemical_formula_weight         712.98
_chemical_name_systematic
; 
tantalum amide silyl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.894(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.771(3)
_cell_length_b                   33.042(8)
_cell_length_c                   12.751(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3376.6(17)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       multi-scan
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35528
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  0.4301
_exptl_absorpt_correction_T_min  0.2576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.522
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+3.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                7438
_reflns_number_total             8104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049023vrom20040721_122003.cif
_cod_data_source_block           tguzei
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3376.6(15)
_cod_database_code               4311877