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_4103404
_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         'C44 H60 Hf2 N2 O6 Si2, C7 H8'
_chemical_formula_sum            'C51 H68 Hf2 N2 O6 Si2'
_chemical_formula_weight         1218.23
_chemical_name_systematic
; 
 ? 
;
_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                93.492(2)
_cell_angle_beta                 93.530(2)
_cell_angle_gamma                108.196(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0535(4)
_cell_length_b                   12.2029(5)
_cell_length_c                   19.7494(8)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.32
_cell_volume                     2744.54(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56011
_diffrn_reflns_theta_full        28.55
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.868
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_correction_T_min  0.5117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         13606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                10470
_reflns_number_total             13606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106848y_si_001_2.cif
_cod_data_source_block           djk17
_cod_original_cell_volume        2744.54(18)
_cod_database_code               4103404