Synthesis of Cyclopentadienyl-, Indenyl-, and Fluorenylbis(pentafluorophenyl)boranes as Ligands in Titanium and Zirconium Half-Sandwich Complexes. The Crystal Structures of C13H9B(C6F5)2·t-BuNH2, C13H8SiMe3B(C6F5)2, and {η5-C5H4B(C6F5)2}TiCl3
Duchateau, Robbert; Lancaster, Simon J.; Thornton-Pett, Mark; Bochmann, Manfred; Organometallics 16 (1997) 4995–; doi:10.1021/om970433j

data_4078338
_publ_section_title
;
 Synthesis of Cyclopentadienyl-, Indenyl-, and
 Fluorenylbis(pentafluorophenyl)boranes as Ligands in Titanium and
 Zirconium Half-Sandwich Complexes. The Crystal Structures of
 C13H9B(C6F5)2&#x00B7;t-BuNH2, C13H8SiMe3B(C6F5)2, and
 {\h5-C5H4B(C6F5)2}TiCl3
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              4995
_journal_paper_doi               10.1021/om970433j
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C31.5 H21 B F10 Si'
_chemical_formula_weight         628.38
_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_date             96-10-03
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                96.057(10)
_cell_angle_beta                 98.008(10)
_cell_angle_gamma                98.856(9)
_cell_formula_units_Z            2
_cell_length_a                   7.8748(8)
_cell_length_b                   8.6936(9)
_cell_length_c                   20.896(2)
_cell_measurement_reflns_used    73
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      39.1
_cell_measurement_theta_min      30.2
_cell_volume                     1387.9(2)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
   Scan width (omega) = 1.55 - 1.80, scan ratio 2theta:omega = 1.00
   I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0101
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4402
_diffrn_reflns_theta_max         64.50
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        9.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  0.5814
_exptl_absorpt_correction_T_min  0.4858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.40  

    H   K   L   2Theta   Chi   Imin/Imax
    0  -1   1    10.7    87.1    0.892
    0   1  -1    10.7   -87.1    0.883
    0  -2   3    23.1    82.0    0.863
    0   2  -3    23.1   -82.0    0.851
    0  -3   3    32.5    87.1    0.906
    0   3  -3    32.5   -87.1    0.922
    0   4  -4    43.9   -87.1    0.887
    0  -4   4    43.9    87.1    0.828
   -1   6  -6    68.0   -81.3    0.954
    1  -6   6    68.0    81.3    0.788
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       prism
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1448
_refine_ls_wR_factor_obs         0.1425
_reflns_number_observed          4186
_reflns_number_total             4402
_reflns_observed_criterion       >2sigma(I)
_cod_duplicate_entry             4078337
_cod_data_source_file            om4995.cif
_cod_data_source_block           MB11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.6793P] 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^)+(0.0515P)^2^+2.6793P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C31.50 H21 B F10 Si'
_cod_database_code               4078338
_audit_contact_author            'J. Richter'