Amide-silyl ligand exchanges and equilibria among group 4 amide and silyl complexes.
Cai, Hu; Yu, Xianghua; Chen, Shujian; Qiu, He; Guzei, Ilia A.; Xue, Zi-Ling; Inorganic chemistry 46 (2007) 8071–8078; doi:10.1021/ic7010293

data_4339766
_publ_section_title
;
 Amide-silyl ligand exchanges and equilibria among group 4 amide and silyl
 complexes.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8071
_journal_page_last               8078
_journal_paper_doi               10.1021/ic7010293
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C15 H45 Hf N3 Si4'
_chemical_formula_weight         558.38
_chemical_name_common            Hafnium
_chemical_name_systematic
; 
Hafnium tris(amid) Trimethylsilyl silide
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.483(5)
_cell_length_b                   15.483(5)
_cell_length_c                   19.378(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4023(2)
_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 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11001
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    4.072
_exptl_absorpt_correction_T_max  0.5803
_exptl_absorpt_correction_T_min  0.2616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker 2003'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.792
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.217
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.89(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2027
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+62.8777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1655
_reflns_number_gt                1820
_reflns_number_total             2027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7010293-file004.cif
_cod_data_source_block           roh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               4339766