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_4078339
_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            'C17 H4 B Cl3 F10 Ti'
_chemical_formula_weight         563.26
_chemical_name_systematic
; 
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             97-04-01
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.342(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1617(6)
_cell_length_b                   19.0088(11)
_cell_length_c                   10.3960(8)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      15.2
_cell_volume                     1945.5(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) = 1.85 - 2.00, 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6612
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.8666
_exptl_absorpt_correction_T_min  0.7261
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.09  

    H   K   L   2Theta   Chi   Imin/Imax
    2   2   0     9.3    82.2    0.845
   -2  -2   0     9.3   -82.2    0.843
   -2  -3   0    10.5   -81.5    0.878
    2   3   0    10.5    81.5    0.889
    3   3   0    14.0    82.2    0.851
   -3  -3   0    14.0   -82.2    0.862
   -3  -5  -1    17.7   -80.8    0.868
    3   5   1    17.7    80.8    0.858
    4   4   0    18.7    82.2    0.868
   -4  -4   0    18.7   -82.2    0.877
    4   5   0    19.8    83.7    0.884
   -4  -5   0    19.8   -83.7    0.894
   -4  -5  -1    21.1   -85.4    0.873
    4   5   1    21.1    85.4    0.862
   -5  -6   0    24.6   -83.8    0.873
    5   6   0    24.6    83.8    0.875
   -5  -7   0    25.8   -82.7    0.896
    5   7   0    25.8    82.7    0.873
    5   7   1    26.9    86.6    0.886
   -5  -7  -1    26.9   -86.6    0.881
    6   5   1    28.5    80.3    0.862
   -6  -5  -1    28.5   -80.3    0.880
   -6  -8  -1    31.7   -88.3    0.863
    6   8   1    31.7    88.3    0.893
   -6  -8  -2    33.3   -82.4    0.845
    6   8   2    33.3    82.4    0.873
   -7  -6  -1    33.3   -81.1    0.856
    7   6   1    33.3    81.1    0.853
   -7  -9  -1    36.5   -89.4    0.877
    7   9   1    36.5    89.4    0.883
   -7 -10  -1    37.7   -86.6    0.888
    7  10   1    37.7    86.6    0.878
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       cube
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_obs          0.0258
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.6255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0668
_refine_ls_wR_factor_obs         0.0617
_reflns_number_observed          3003
_reflns_number_total             3419
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om4995.cif
_cod_data_source_block           MB18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.6255P] 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^)+(0.0246P)^2^+1.6255P] 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/n
_cod_database_code               4078339
_audit_contact_author            'J. Richter'