Reactions of Decamethylhafnocene with 1,3-Butadiynes: Formation of Hafnacyclocumulenes and C−H Activation at Pentamethylcyclopentadienyl Ligands
Beweries, Torsten; Burlakov, Vladimir V.; Peitz, Stephan; Bach, Marc A.; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Rosenthal, Uwe; Organometallics 26 (2007) 6827–; doi:10.1021/om700911a

data_4074076
_publ_section_title
;
 Reactions of Decamethylhafnocene with 1,3-Butadiynes: Formation of
 Hafnacyclocumulenes and C&#x2212;H Activation at
 Pentamethylcyclopentadienyl Ligands
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6827
_journal_paper_doi               10.1021/om700911a
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C42 H66 Hf N2'
_chemical_formula_weight         777.46
_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                64.457(4)
_cell_angle_beta                 80.109(4)
_cell_angle_gamma                66.716(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4937(6)
_cell_length_b                   13.1411(6)
_cell_length_c                   15.2373(8)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    200(2)
_cell_volume                     1907.38(19)
_computing_data_collection       STOE-X-AREA
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE-IPDS II'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27242
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_T_max  0.5892
_exptl_absorpt_correction_T_min  0.4178
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0409
_reflns_number_gt                6861
_reflns_number_total             7508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700911a-file003.cif
_cod_data_source_block           ks634
_cod_original_cell_volume        1907.38(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074076