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_4075739
_publ_section_title
;
 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
;
_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
;
major component: C25H32Si2Zr
 minor component: C24H29ClSi2Zr
;
_chemical_formula_sum            'C24.68 H31.05 Cl0.32 Si2 Zr'
_chemical_formula_weight         486.39
_chemical_name_common            3
_chemical_name_systematic
; 
 ? 
;
_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                 110.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.403(3)
_cell_length_b                   12.499(3)
_cell_length_c                   13.997(3)
_cell_measurement_temperature    140(1)
_cell_volume                     2362.4(10)
_computing_cell_refinement       'DENZO (Otwinowski and Minor, 1985)'
_computing_data_collection       'MSC R-Axis-II control software'
_computing_data_reduction
; 
DENZO, Scalepack (Otwinowski and Minor, 1985) 
;
_computing_molecular_graphics    'XP (SHELXTL, v.5, 1994)'
_computing_publication_material  'XL (SHELXTL 1997)'
_computing_structure_refinement  'XL (SHELXTL 1997)'
_computing_structure_solution    'XS (SHELXTL 1997)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8151
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                4027
_reflns_number_total             4297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049248dsi20050124_124227.cif
_cod_data_source_block           f3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.2183P] 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^)+(0.0336P)^2^+1.2183P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2362.3(8)
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               4075739