B(C6F5)3 as a C6F5 transfer reagent in zirconium chemistry: facile formation of the borole-bridged triple-decker complex [Zr2Cp″2(C6F5)2{μ-η5∶η5-C4H4BCH2-η3,κF-CHCHCHB(C6F5)3}]
Woodman, Timothy J.; Bochmann, Manfred; Thornton-Pett, Mark; Chemical Communications  (2001) 329–; doi:10.1039/b009016f

data_7114754
_publ_section_title
;
 B(C6F5)3 as a C6F5 transfer reagent in zirconium chemistry: facile
 formation of the borole-bridged triple-decker complex
 [Zr2Cp&#x2033;2(C6F5)2{\m-\h5&#x2236;\h5-C4H4BCH2-\h3,\kF-CHCHCHB(C6F5)3}]
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              329
_journal_paper_doi               10.1039/b009016f
_journal_year                    2001
_chemical_formula_sum            'C68 H71 B2 F25 O2 Si4 Zr2'
_chemical_formula_weight         1711.67
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.858(2)
_cell_angle_beta                 106.311(2)
_cell_angle_gamma                102.906(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2618(3)
_cell_length_b                   13.6828(3)
_cell_length_c                   22.1150(6)
_cell_measurement_temperature    150(2)
_cell_volume                     3682.30(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28520
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.9517
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         12129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+11.3877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                8712
_reflns_number_total             12129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009016f.txt
_cod_data_source_block           tjw901a
_cod_original_cell_volume        3682.30(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114754