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_7012730
_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         'C32 H19 B Cl3 F10 N3 Zr, 1.5(C D Cl3)'
_chemical_formula_structural     '[Zr(py)2Cl3{C5H4B(py)(C6F5)2}].1.5(CDCl3)'
_chemical_formula_sum            'C33.5 H19 B Cl7.5 D1.5 F10 N3 Zr'
_chemical_formula_weight         1024.4
_chemical_name_common            'complex 15'
_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                67.46(1)
_cell_angle_beta                 76.82(1)
_cell_angle_gamma                84.93(1)
_cell_formula_units_Z            4
_cell_length_a                   11.201(1)
_cell_length_b                   18.241(1)
_cell_length_c                   21.174(3)
_cell_measurement_temperature    140(1)
_cell_volume                     3890.5(8)
_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  'SHELXL (Sheldrick, 1997)'
_computing_structure_refinement  'XL, SHELXL (Sheldrick, 1997)'
_computing_structure_solution    'XS (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22856
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            'clear, colourless'
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         13163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+2.2116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                11449
_reflns_number_total             13163
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b300552f.txt
_cod_data_source_block           simonl4
_cod_original_cell_volume        3890.5(7)
_cod_original_formula_sum        'C33.50 H19 D1.5 B Cl7.50 F10 N3 Zr'
_cod_database_code               7012730