The synthesis of half-sandwich bis(pentafluorophenyl)boryl-substituted cyclopentadienyl zirconium, niobium and tantalum complexes and the isolation and molecular structure of a zwitterionic niobocene
Lancaster, Simon J.; Hughes, David L.; Dalton Transactions  (2003) 1779–; doi:10.1039/b300552f

data_7012729
_publ_section_title
;
 The synthesis of half-sandwich bis(pentafluorophenyl)boryl-substituted
 cyclopentadienyl zirconium, niobium and tantalum complexes and the
 isolation and molecular structure of a zwitterionic niobocene
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1779
_journal_paper_doi               10.1039/b300552f
_journal_year                    2003
_chemical_formula_moiety         'C22 H9 B Cl3 F10 N Ti, C7 H8'
_chemical_formula_structural     '[TiCl3{C5H4B(Py)(C6F5)2}].tol'
_chemical_formula_sum            'C29 H17 B Cl3 F10 N Ti'
_chemical_formula_weight         734.50
_chemical_name_common            'complex 14'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                107.44(1)
_cell_angle_beta                 92.97(1)
_cell_angle_gamma                103.27(1)
_cell_formula_units_Z            2
_cell_length_a                   8.799(1)
_cell_length_b                   13.523(1)
_cell_length_c                   13.626(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1492.8(4)
_computing_cell_refinement       'DENZO (Otwinowski and Minor, 1985)'
_computing_data_collection       'MSC R-Axis-II control software'
_computing_data_reduction
'DENZO, SCALEPACK (Otwinowski and Minor, 1985)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'XL (Sheldrick, 1993)'
_computing_structure_refinement  'XL (Sheldrick, 1993)'
_computing_structure_solution    'XS (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device       'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8342
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'diamond-shaped prisms'
_exptl_crystal_F_000             732
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.2987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                4224
_reflns_number_total             4926
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b300552f.txt
_cod_data_source_block           simonl2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7012729