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_4078336
_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            'C29 H20 B F10 N'
_chemical_formula_weight         583.27
_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             96-09-12
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.908(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.677(2)
_cell_length_b                   9.7230(12)
_cell_length_c                   19.898(2)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      39.8
_cell_measurement_theta_min      30.2
_cell_volume                     2503.3(6)
_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      200(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
  Scan width (omega) = 1.45 - 1.70, 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    0.0082
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3872
_diffrn_reflns_theta_max         64.51
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.6999
_exptl_absorpt_correction_T_min  0.4306
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.25  

    H   K   L   2Theta   Chi   Imin/Imax
   -3   0  -3    28.7   -86.9    0.838
    3   0   3    28.7    86.9    0.840
    4   0   4    38.5    86.9    0.806
   -4   0  -4    38.5   -86.9    0.850
   -4   0  -6    46.4   -83.9    0.890
    4   0   6    46.4    83.9    0.809
    6   0   6    59.3    86.9    0.743
   -6   0  -6    59.3   -86.9    0.928
    9   0   9    95.9    86.9    0.608
   -9   0  -9    95.9   -86.9    0.937
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00004(10)
_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   1.135
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_obs          0.0434
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+3.9857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1164
_refine_ls_wR_factor_obs         0.1155
_reflns_number_observed          3774
_reflns_number_total             3872
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om4995.cif
_cod_data_source_block           MB12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+3.9857P] 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^)+(0.0364P)^2^+3.9857P] 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        2503.4(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4078336
_audit_contact_author            'J. Richter'