B(C6F5)3as C6F5Transfer Agent in Zirconium Chemistry: Borole Sandwich and Borole-Bridged Triple-Decker Complexes
Woodman, Timothy J.; Thornton-Pett, Mark; Hughes, David L.; Bochmann, Manfred; Organometallics 20 (2001) 4080–; doi:10.1021/om010348i

data_4077357
_publ_section_title
;
 B(C6F5)3as C6F5Transfer Agent in Zirconium Chemistry:&#x00A0; Borole
 Sandwich and Borole-Bridged Triple-Decker Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4080
_journal_paper_doi               10.1021/om010348i
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C37 H43 B F10 N2 Si2 Zr'
_chemical_formula_weight         863.94
_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                79.6120(10)
_cell_angle_beta                 86.3340(10)
_cell_angle_gamma                75.1260(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3671(2)
_cell_length_b                   15.9864(3)
_cell_length_c                   25.3180(5)
_cell_measurement_temperature    150(2)
_cell_volume                     4372.97(14)
_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    'ORTEP3 for Windows (Farrugia, 1997)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42596
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.9493
_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            'pale green'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         16775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+4.1386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                11825
_reflns_number_total             16775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010348i.cif
_cod_data_source_block           tjw2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077357