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_4079188
_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            'C149.03 H188 F4 Hf8 I4 N3.03 O7.03'
_chemical_formula_weight         4145.54
_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                78.706(2)
_cell_angle_beta                 86.968(3)
_cell_angle_gamma                88.166(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3702(10)
_cell_length_b                   16.9273(19)
_cell_length_c                   23.057(3)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.72
_cell_volume                     3580.4(7)
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53565
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    6.693
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1983
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.051
_refine_diff_density_max         3.639
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         16432
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0252P)^2^+40.1795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                14721
_reflns_number_total             16432
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3005542_si_003.cif
_cod_data_source_block           sps77
_cod_original_cell_volume        3580.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079188