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_4079182
_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            'C76 H104 Hf4 N4 O6'
_chemical_formula_weight         1883.59
_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                73.565(5)
_cell_angle_beta                 73.880(5)
_cell_angle_gamma                80.049(5)
_cell_formula_units_Z            1
_cell_length_a                   10.709(5)
_cell_length_b                   12.121(5)
_cell_length_c                   15.003(5)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.74
_cell_volume                     1785.0(13)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20133
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    5.849
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.482
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.3027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                6531
_reflns_number_total             8170
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3005542_si_003.cif
_cod_data_source_block           sps38
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079182