Di- and Tetrametallic Hafnocene Oxamidides Prepared from CO-Induced N2Bond Cleavage and Thermal Rearrangement to Hafnocene Cyanide Derivatives
Semproni, Scott P.; Margulieux, Grant W.; Chirik, Paul J.; Organometallics 31 (2012) 6278–; doi:10.1021/om3005542

data_4079183
_publ_section_title
;
 Di- and Tetrametallic Hafnocene Oxamidides Prepared from CO-Induced
 N2Bond Cleavage and Thermal Rearrangement to Hafnocene Cyanide
 Derivatives
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6278
_journal_paper_doi               10.1021/om3005542
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C46 H72 Hf2 N2 O2 Si2'
_chemical_formula_weight         1098.22
_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                87.330(5)
_cell_angle_beta                 69.543(5)
_cell_angle_gamma                87.477(5)
_cell_formula_units_Z            1
_cell_length_a                   9.588(5)
_cell_length_b                   10.972(5)
_cell_length_c                   11.333(5)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.27
_cell_volume                     1115.3(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12691
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    4.743
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0130
_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^)+(0.0177P)^2^+0.3567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0309
_refine_ls_wR_factor_ref         0.0313
_reflns_number_gt                4736
_reflns_number_total             4955
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3005542_si_003.cif
_cod_data_source_block           sps47
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079183