Synthesis and Isolation of Di-n-butylhafnocene and Its Application as a Versatile Starting Material for the Synthesis of New Hafnacycles
Burlakov, Vladimir V.; Beweries, Torsten; Bogdanov, Vyacheslav S.; Arndt, Perdita; Baumann, Wolfgang; Petrovskii, Pavel V.; Spannenberg, Anke; Lyssenko, Konstantin A.; Shur, Vladimir B.; Rosenthal, Uwe; Organometallics 28 (2009) 2864–; doi:10.1021/om900122w

data_4069287
_publ_section_title
;
 Synthesis and Isolation of Di-n-butylhafnocene and Its Application as a
 Versatile Starting Material for the Synthesis of New Hafnacycles
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2864
_journal_paper_doi               10.1021/om900122w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C64 H52 Hf2'
_chemical_formula_weight         1178.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.212(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8491(2)
_cell_length_b                   26.7157(5)
_cell_length_c                   11.3534(3)
_cell_measurement_reflns_used    30747
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.52
_cell_volume                     2326.87(10)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27477
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.501
_exptl_absorpt_correction_T_max  0.7049
_exptl_absorpt_correction_T_min  0.4833
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (STOE & CIE, 2005)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0173
_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^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0388
_reflns_number_gt                4270
_reflns_number_total             4912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900122w_si_005.cif
_cod_data_source_block           ks924
_cod_original_cell_volume        2326.88(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069287