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_4071957
_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         'C29 H40 Si2 Zr'
_chemical_formula_structural     '[Zr(C5H4-CMe2-C13H8)(CH2SiMe3)2]'
_chemical_formula_sum            'C29 H40 Si2 Zr'
_chemical_formula_weight         536.01
_chemical_name_common            'Compound 1'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.3040(9)
_cell_length_b                   16.6904(3)
_cell_length_c                   8.9689(2)
_cell_measurement_reflns_used    14413
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      3.70
_cell_volume                     5584.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(1)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14413
_diffrn_reflns_theta_full        22.20
_diffrn_reflns_theta_max         22.20
_diffrn_reflns_theta_min         3.70
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 SORTAV (Blessing, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0642
_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^)+22.2495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2160
_reflns_number_total             3415
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800486p_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P ccn'
_cod_database_code               4071957