Bis[<i>N</i>,<i>N</i>'-bis(trimethylsilyl)benzamidinato]diethylhafnium(IV)
Fischer, Reinald; Walther, Dirk; Imhof, Wolfgang; Acta Crystallographica Section E 62 (2006) m568–m570; doi:10.1107/S1600536806005721

data_2208398
_publ_section_title
;
 Bis[<i>N</i>,<i>N</i>'-bis(trimethylsilyl)benzamidinato]diethylhafnium(IV)
;
_journal_coeditor_code           OM2003
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m568
_journal_page_last               m570
_journal_paper_doi               10.1107/S1600536806005721
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Hf (C2 H5)2 (C13 H23 N2 Si2)2]'
_chemical_formula_moiety         'C30 H56 Hf N4 Si4'
_chemical_formula_sum            'C30 H56 Hf N4 Si4'
_chemical_formula_weight         763.64
_chemical_name_systematic
;
Bis[N,N'-bis(trimethylsilyl)benzamidinato]diethylhafnium(IV)
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.205(2)
_cell_length_b                   20.790(4)
_cell_length_c                   17.234(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      20.06
_cell_measurement_theta_min      18.47
_cell_volume                     4292.6(14)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'MolEN (Enraf--Nonius, 1990)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2-\q
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7584
_diffrn_reflns_theta_full        24.64
_diffrn_reflns_theta_max         24.64
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_time  600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.779
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+17.7042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                5285
_reflns_number_total             7229
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2003.cif
_cod_data_source_block           I
_cod_original_cell_volume        4292.6(13)
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208398
_cod_database_fobs_code          2208398