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_7012727
_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         'C25 H17 B Cl3 F10 Nb Si, 1.5(C7 H8)'
_chemical_formula_structural
'[NbCl2{C5H4B(Cl)(C6F5)2}(C5H4SiMe3)].1.5(toluene)'
_chemical_formula_sum            'C35.5 H29 B Cl3 F10 Nb Si'
_chemical_formula_weight         883.75
_chemical_name_common            'complex 9'
_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                116.58(3)
_cell_angle_beta                 99.60(2)
_cell_angle_gamma                96.390(10)
_cell_formula_units_Z            2
_cell_length_a                   9.601(2)
_cell_length_b                   14.492(4)
_cell_length_c                   15.252(8)
_cell_measurement_temperature    140(1)
_cell_volume                     1829.2(13)
_computing_cell_refinement       'DENZO/CELL (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  'SHELXL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10730
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'diamond-shaped plate'
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                5315
_reflns_number_total             6318
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b300552f.txt
_cod_data_source_block           simonl6a
_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_original_cell_volume        1829.2(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012727