Functionalization of Hafnium Oxamidide Complexes Prepared from CO-Induced N2 Cleavage
Donald J. Knobloch; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 132 (2010) 15340–15350; doi:10.1021/ja106848y

data_4103405
_publ_section_title
;
 Functionalization of Hafnium Oxamidide Complexes Prepared from CO-Induced
 N2 Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15340
_journal_page_last               15350
_journal_paper_doi               10.1021/ja106848y
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'(C21 H30 Hf I N O Si)0.92, (C20 H30 Hf I2 Si)0.08'
_chemical_formula_sum            'C20.92 H30 Hf I1.08 N0.92 O0.92 Si'
_chemical_formula_weight         652.73
_chemical_name_systematic
; 
 ? 
;
_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                 109.1670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5359(5)
_cell_length_b                   24.7208(11)
_cell_length_c                   10.0763(5)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.85
_cell_measurement_theta_min      2.29
_cell_volume                     2243.66(19)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16473
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.198
_exptl_absorpt_correction_T_max  0.3703
_exptl_absorpt_correction_T_min  0.1906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         6804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+3.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                6241
_reflns_number_total             6804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106848y_si_001_3.cif
_cod_data_source_block           djk16
_cod_database_code               4103405