Deprotonation Reactions of Zirconium and Hafnium Amide Complexes H2N-M[N(SiMe3)2]3 and Subsequent Silyl Migration from Amide -N(SiMe3)2 to Imide NH Ligands
Xianghua Yu; Zi-Ling Xue; Inorganic Chemistry 44 (2005) 1505–1510; doi:10.1021/ic0485413

data_4308687
_publ_contact_author_name        'Zi-Ling Xue'
_publ_section_title
;
Deprotonation Reactions of Zirconium and Hafnium Amide Complexes
H2N-M[N(SiMe3)2]3 and Subsequent Silyl Migration from Amide -N(SiMe3)2 to
Imide NH Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1505
_journal_page_last               1510
_journal_paper_doi               10.1021/ic0485413
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C26 H71 Hf Li N4 O2 Si6'
_chemical_formula_weight         825.84
_chemical_name_common            Hafnium
_chemical_name_systematic
; 
Hafnium Trimethylsilylamide lithium THF
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.946(5)
_cell_length_b                   19.674(7)
_cell_length_c                   33.694(12)
_cell_measurement_temperature    173(2)
_cell_volume                     8582(5)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            94047
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  0.5836
_exptl_absorpt_correction_T_min  0.5065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         20753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          5.337
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+40.8098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                18476
_reflns_number_total             20753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485413rom20041019_121835.cif
_cod_data_source_block           hfor
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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        8581(5)
_cod_database_code               4308687