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_4311878
_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 H82 N6 Si8 Zr2'
_chemical_formula_weight         910.13
_chemical_name_common            Zirconium
_chemical_name_systematic
; 
Zirconium Cyclic Amide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.425(10)
_cell_angle_beta                 99.529(10)
_cell_angle_gamma                105.110(10)
_cell_formula_units_Z            2
_cell_length_a                   10.172(6)
_cell_length_b                   14.421(9)
_cell_length_c                   18.947(12)
_cell_measurement_temperature    173(2)
_cell_volume                     2503(3)
_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 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27249
_diffrn_reflns_theta_full        28.61
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.9001
_exptl_absorpt_correction_T_min  0.8682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         11837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.096
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.6347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                8430
_reflns_number_total             11837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049023vrom20040721_122018.cif
_cod_data_source_block           yc
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4311878