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_4079185
_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            'C44 H62 Hf2 N4 O4'
_chemical_formula_weight         1067.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000
_cell_angle_beta                 106.585(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   20.209(5)
_cell_length_b                   12.339(5)
_cell_length_c                   17.859(5)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.44
_cell_volume                     4268(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16648
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                4091
_reflns_number_total             4862
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3005542_si_003.cif
_cod_data_source_block           sps60
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4079185