Synthesis, Ion Aggregation, Alkyl Bonding Modes, and Dynamics of 14-Electron Metallocenium Ion Pairs [(SBI)MCH2SiMe3+···X-] (M = Zr, Hf): Inner-Sphere (X = MeB(C6F5)3) versus Outer-Sphere (X = B(C6F5)4) Structures and the Implications for “Continuous” or “Intermittent” Alkene Polymerization Mechanisms
Song, Fuquan; Lancaster, Simon J.; Cannon, Roderick D.; Schormann, Mark; Humphrey, Simon M.; Zuccaccia, Cristiano; Macchioni, Alceo; Bochmann, Manfred; Organometallics 24 (2005) 1315–; doi:10.1021/om049248d

data_4075740
_publ_section_title
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 Synthesis, Ion Aggregation, Alkyl Bonding Modes, and Dynamics of
 14-Electron Metallocenium Ion Pairs
 [(SBI)MCH2SiMe3+&#x00B7;&#x00B7;&#x00B7;X-] (M = Zr, Hf):&#x00A0;
 Inner-Sphere (X = MeB(C6F5)3) versus Outer-Sphere (X = B(C6F5)4)
 Structures and the Implications for &#x201C;Continuous&#x201D; or
 &#x201C;Intermittent&#x201D; Alkene Polymerization Mechanisms
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_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1315
_journal_paper_doi               10.1021/om049248d
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         C25H32HfSi2
_chemical_formula_sum            'C25 H32 Hf Si2'
_chemical_formula_weight         567.18
_chemical_name_common            6
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2146(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3497(2)
_cell_length_b                   12.5146(2)
_cell_length_c                   13.9676(2)
_cell_measurement_temperature    180(2)
_cell_volume                     2353.81(6)
_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    SHELXP-97
_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(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21487
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  0.7416
_exptl_absorpt_correction_T_min  0.4214
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.766
_refine_diff_density_min         -2.787
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.3370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                5415
_reflns_number_total             6285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049248dsi20050124_124227.cif
_cod_data_source_block           f6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.3370P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.3370P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4075740