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_4071959
_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         'C22 H21 Cl Zr'
_chemical_formula_structural     '[Zr(C5H4-CMe2-C13H8)MeCl]'
_chemical_formula_sum            'C22 H21 Cl Zr'
_chemical_formula_weight         412.06
_chemical_name_common            'Compound 5'
_chemical_name_systematic
;
Chloro{[2-(\h^5^-cyclopentadienyl)-2-(\h^5^-fluorenyl)propane]}\
methylzirconium(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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.353(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2398(6)
_cell_length_b                   10.7676(6)
_cell_length_c                   18.156(3)
_cell_measurement_reflns_used    13612
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      4.41
_cell_volume                     1764.5(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    'DIRDIF99-2 (Beurskens <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_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            13612
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.664
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         13635
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1513P)^2^+5.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2724
_refine_ls_wR_factor_ref         0.2934
_reflns_number_gt                9290
_reflns_number_total             13635
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om800486p_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071959