Ligand Mobility and Solution Structures of the Metallocenium Ion Pairs [Me2C(Cp)(fluorenyl)MCH2SiMe3+···X−] (M = Zr, Hf; X = MeB(C6F5)3, B(C6F5)4)
Alonso-Moreno, Carlos; Lancaster, Simon J.; Wright, Joseph A.; Hughes, David L.; Zuccaccia, Cristiano; Correa, Andrea; Macchioni, Alceo; Cavallo, Luigi; Bochmann, Manfred; Organometallics 27 (2008) 5474–; doi:10.1021/om800486p

data_4071958
_publ_section_title
;
 Ligand Mobility and Solution Structures of the Metallocenium Ion Pairs
 [Me2C(Cp)(fluorenyl)MCH2SiMe3+&#x00B7;&#x00B7;&#x00B7;X&#x2212;] (M = Zr,
 Hf; X = MeB(C6F5)3, B(C6F5)4)
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5474
_journal_paper_doi               10.1021/om800486p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C23 H24 Hf'
_chemical_formula_structural     '[Hf(C5H4-CMe2-C13H8)Me2]'
_chemical_formula_sum            'C23 H24 Hf'
_chemical_formula_weight         478.91
_chemical_name_common            'Compound 4'
_chemical_name_systematic
;
{[2-(\h^5^-Cyclopentadienyl)-2-(\h^5^-fluorenyl)propane]}\
dimethylhafnium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.011(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3987(9)
_cell_length_b                   10.7366(10)
_cell_length_c                   18.2206(15)
_cell_measurement_reflns_used    26136
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      3.50
_cell_volume                     1798.4(3)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
 SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
 and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24638
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.801
_exptl_absorpt_correction_T_max  0.312
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         5.955
_refine_diff_density_min         -2.485
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+37.4586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                3402
_reflns_number_total             4114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800486p_si_002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071958