#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:12:27 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179831 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/27/7012729.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7012729
loop_
_publ_author_name
'Lancaster, Simon J.'
'Hughes, David L.'
_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/[σ²(Fo²)+(0.0459P)²+0.2987P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.11896(4) 0.77186(3) 0.34134(3) 0.02889(12) Uani 1 1 d . . .
C11 C 0.3711(2) 0.81621(15) 0.28048(15) 0.0272(4) Uani 1 1 d . . .
C12 C 0.2987(2) 0.90407(16) 0.29697(17) 0.0334(5) Uani 1 1 d . . .
H12 H 0.2661 0.9300 0.2457 0.040 Uiso 1 1 calc R . .
C13 C 0.2853(3) 0.94468(17) 0.40382(18) 0.0391(5) Uani 1 1 d . . .
H13 H 0.2460 1.0031 0.4351 0.047 Uiso 1 1 calc R . .
C14 C 0.3420(3) 0.88101(18) 0.45456(17) 0.0377(5) Uani 1 1 d . . .
H14 H 0.3448 0.8888 0.5249 0.045 Uiso 1 1 calc R . .
C15 C 0.3940(2) 0.80298(17) 0.37891(15) 0.0307(4) Uani 1 1 d . . .
H15 H 0.4368 0.7507 0.3920 0.037 Uiso 1 1 calc R . .
B B 0.4390(3) 0.75389(17) 0.17590(17) 0.0257(4) Uani 1 1 d . . .
N21 N 0.45377(18) 0.64148(13) 0.19041(12) 0.0253(3) Uani 1 1 d . . .
C22 C 0.3227(2) 0.56638(15) 0.19342(15) 0.0276(4) Uani 1 1 d . . .
H22 H 0.2243 0.5783 0.1820 0.033 Uiso 1 1 calc R . .
C23 C 0.3311(3) 0.47337(16) 0.21275(16) 0.0331(5) Uani 1 1 d . . .
H23 H 0.2395 0.4232 0.2135 0.040 Uiso 1 1 calc R . .
C24 C 0.4772(3) 0.45488(17) 0.23120(16) 0.0354(5) Uani 1 1 d . . .
H24 H 0.4849 0.3918 0.2429 0.042 Uiso 1 1 calc R . .
C25 C 0.6111(3) 0.53259(18) 0.23179(17) 0.0358(5) Uani 1 1 d . . .
H25 H 0.7105 0.5234 0.2461 0.043 Uiso 1 1 calc R . .
C26 C 0.5954(2) 0.62391(16) 0.21096(16) 0.0307(4) Uani 1 1 d . . .
H26 H 0.6860 0.6754 0.2111 0.037 Uiso 1 1 calc R . .
C31 C 0.6180(2) 0.82040(15) 0.16690(15) 0.0270(4) Uani 1 1 d . . .
C32 C 0.6838(2) 0.78618(16) 0.07517(15) 0.0299(4) Uani 1 1 d . . .
F32 F 0.60780(14) 0.69229(10) 0.00098(9) 0.0382(3) Uani 1 1 d . . .
C33 C 0.8254(2) 0.83975(18) 0.05541(16) 0.0329(5) Uani 1 1 d . . .
F33 F 0.88034(15) 0.80174(12) -0.03550(10) 0.0468(3) Uani 1 1 d . . .
C34 C 0.9134(2) 0.93180(18) 0.12977(18) 0.0353(5) Uani 1 1 d . . .
F34 F 1.05388(15) 0.98499(12) 0.11262(11) 0.0494(4) Uani 1 1 d . . .
C35 C 0.8566(3) 0.96894(17) 0.22204(17) 0.0355(5) Uani 1 1 d . . .
F35 F 0.94068(16) 1.05879(11) 0.29594(11) 0.0524(4) Uani 1 1 d . . .
C36 C 0.7119(2) 0.91335(16) 0.23865(15) 0.0307(4) Uani 1 1 d . . .
F36 F 0.66482(15) 0.95636(10) 0.33132(9) 0.0420(3) Uani 1 1 d . . .
C41 C 0.3306(2) 0.74078(15) 0.06732(15) 0.0264(4) Uani 1 1 d . . .
C42 C 0.3296(2) 0.83318(16) 0.04290(16) 0.0312(4) Uani 1 1 d . . .
F42 F 0.41663(15) 0.93034(9) 0.10753(9) 0.0369(3) Uani 1 1 d . . .
C43 C 0.2487(3) 0.83635(19) -0.04560(17) 0.0373(5) Uani 1 1 d . . .
F43 F 0.25663(18) 0.93035(12) -0.06244(11) 0.0509(4) Uani 1 1 d . . .
C44 C 0.1601(3) 0.7421(2) -0.11605(16) 0.0387(5) Uani 1 1 d . . .
F44 F 0.07663(17) 0.74246(13) -0.20212(11) 0.0540(4) Uani 1 1 d . . .
C45 C 0.1558(2) 0.64762(18) -0.09717(16) 0.0345(5) Uani 1 1 d . . .
F45 F 0.06795(16) 0.55418(11) -0.16585(10) 0.0458(3) Uani 1 1 d . . .
C46 C 0.2415(2) 0.64710(16) -0.00916(15) 0.0288(4) Uani 1 1 d . . .
F46 F 0.23561(15) 0.54919(9) -0.00159(9) 0.0388(3) Uani 1 1 d . . .
Cl5 Cl 0.00142(6) 0.70293(4) 0.17631(4) 0.03317(14) Uani 1 1 d . . .
Cl6 Cl -0.06319(7) 0.84491(5) 0.42225(5) 0.04463(16) Uani 1 1 d . . .
Cl7 Cl 0.09866(6) 0.62635(4) 0.39153(4) 0.03775(15) Uani 1 1 d . . .
C81 C 0.6583(4) 0.6951(2) 0.6074(2) 0.0597(8) Uani 1 1 d . . .
C82 C 0.4992(5) 0.6702(3) 0.5701(2) 0.0694(9) Uani 1 1 d . . .
H82 H 0.4598 0.6168 0.5069 0.083 Uiso 1 1 calc R . .
C83 C 0.3994(4) 0.7235(3) 0.6253(3) 0.0686(9) Uani 1 1 d . . .
H83 H 0.2933 0.7056 0.5993 0.082 Uiso 1 1 calc R . .
C84 C 0.4558(3) 0.8033(2) 0.7192(2) 0.0558(7) Uani 1 1 d . . .
H84 H 0.3883 0.8397 0.7562 0.067 Uiso 1 1 calc R . .
C85 C 0.6118(3) 0.8285(2) 0.7573(2) 0.0551(7) Uani 1 1 d . . .
H85 H 0.6502 0.8816 0.8209 0.066 Uiso 1 1 calc R . .
C86 C 0.7123(3) 0.7750(2) 0.7017(2) 0.0556(7) Uani 1 1 d . . .
H86 H 0.8181 0.7932 0.7282 0.067 Uiso 1 1 calc R . .
C87 C 0.7710(6) 0.6365(3) 0.5497(3) 0.1068(16) Uani 1 1 d . . .
H87A H 0.7298 0.6051 0.4775 0.160 Uiso 1 1 calc R . .
H87B H 0.7829 0.5812 0.5778 0.160 Uiso 1 1 calc R . .
H87C H 0.8715 0.6862 0.5573 0.160 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl6 Ti Cl7 102.32(3) . . ?
Cl6 Ti Cl5 101.51(3) . . ?
Cl7 Ti Cl5 103.11(3) . . ?
Cl6 Ti C14 99.03(6) . . ?
Cl7 Ti C14 97.73(7) . . ?
Cl5 Ti C14 146.70(6) . . ?
Cl6 Ti C13 85.69(6) . . ?
Cl7 Ti C13 132.63(7) . . ?
Cl5 Ti C13 121.13(6) . . ?
C14 Ti C13 35.24(9) . . ?
Cl6 Ti C12 108.73(5) . . ?
Cl7 Ti C12 143.10(6) . . ?
Cl5 Ti C12 89.92(6) . . ?
C14 Ti C12 58.58(8) . . ?
C13 Ti C12 35.21(7) . . ?
Cl6 Ti C15 134.09(5) . . ?
Cl7 Ti C15 86.38(6) . . ?
Cl5 Ti C15 120.49(5) . . ?
C14 Ti C15 35.16(7) . . ?
C13 Ti C15 58.07(8) . . ?
C12 Ti C15 57.71(8) . . ?
Cl6 Ti C11 142.70(5) . . ?
Cl7 Ti C11 109.55(5) . . ?
Cl5 Ti C11 89.85(5) . . ?
C14 Ti C11 58.52(7) . . ?
C13 Ti C11 58.53(7) . . ?
C12 Ti C11 35.10(7) . . ?
C15 Ti C11 34.44(7) . . ?
C15 C11 C12 105.49(17) . . ?
C15 C11 B 125.24(18) . . ?
C12 C11 B 128.71(18) . . ?
C15 C11 Ti 70.53(11) . . ?
C12 C11 Ti 69.78(11) . . ?
B C11 Ti 130.59(13) . . ?
C13 C12 C11 108.9(2) . . ?
C13 C12 Ti 71.76(12) . . ?
C11 C12 Ti 75.12(11) . . ?
C13 C12 H12 125.5 . . ?
C11 C12 H12 125.5 . . ?
Ti C12 H12 119.4 . . ?
C14 C13 C12 108.02(18) . . ?
C14 C13 Ti 72.09(12) . . ?
C12 C13 Ti 73.02(12) . . ?
C14 C13 H13 126.0 . . ?
C12 C13 H13 126.0 . . ?
Ti C13 H13 120.7 . . ?
C13 C14 C15 107.44(19) . . ?
C13 C14 Ti 72.66(13) . . ?
C15 C14 Ti 73.80(12) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 H14 126.3 . . ?
Ti C14 H14 119.2 . . ?
C14 C15 C11 110.0(2) . . ?
C14 C15 Ti 71.04(12) . . ?
C11 C15 Ti 75.03(11) . . ?
C14 C15 H15 125.0 . . ?
C11 C15 H15 125.0 . . ?
Ti C15 H15 120.6 . . ?
N21 B C11 105.56(15) . . ?
N21 B C31 107.05(15) . . ?
C11 B C31 111.85(15) . . ?
N21 B C41 114.56(15) . . ?
C11 B C41 112.78(16) . . ?
C31 B C41 105.03(15) . . ?
C26 N21 C22 117.66(17) . . ?
C26 N21 B 121.54(16) . . ?
C22 N21 B 120.42(16) . . ?
N21 C22 C23 122.12(19) . . ?
N21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C22 C23 C24 119.7(2) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 118.5(2) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C26 C25 C24 119.3(2) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
N21 C26 C25 122.72(19) . . ?
N21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C36 C31 C32 113.47(17) . . ?
C36 C31 B 127.45(16) . . ?
C32 C31 B 118.95(17) . . ?
F32 C32 C33 116.49(17) . . ?
F32 C32 C31 119.28(17) . . ?
C33 C32 C31 124.19(19) . . ?
F33 C33 C32 120.6(2) . . ?
F33 C33 C34 119.79(18) . . ?
C32 C33 C34 119.62(18) . . ?
F34 C34 C35 120.2(2) . . ?
F34 C34 C33 120.67(19) . . ?
C35 C34 C33 119.11(19) . . ?
F35 C35 C34 120.15(19) . . ?
F35 C35 C36 120.25(19) . . ?
C34 C35 C36 119.6(2) . . ?
F36 C36 C31 120.55(17) . . ?
F36 C36 C35 115.47(18) . . ?
C31 C36 C35 123.98(18) . . ?
C42 C41 C46 112.85(18) . . ?
C42 C41 B 117.75(17) . . ?
C46 C41 B 129.33(17) . . ?
F42 C42 C43 115.02(18) . . ?
F42 C42 C41 119.76(18) . . ?
C43 C42 C41 125.2(2) . . ?
F43 C43 C44 120.4(2) . . ?
F43 C43 C42 120.5(2) . . ?
C44 C43 C42 119.1(2) . . ?
F44 C44 C45 120.4(2) . . ?
F44 C44 C43 120.7(2) . . ?
C45 C44 C43 118.9(2) . . ?
F45 C45 C44 119.44(19) . . ?
F45 C45 C46 120.1(2) . . ?
C44 C45 C46 120.5(2) . . ?
F46 C46 C45 115.30(18) . . ?
F46 C46 C41 121.30(18) . . ?
C45 C46 C41 123.39(19) . . ?
C86 C81 C82 117.8(3) . . ?
C86 C81 C87 119.8(3) . . ?
C82 C81 C87 122.4(3) . . ?
C83 C82 C81 121.0(3) . . ?
C83 C82 H82 119.5 . . ?
C81 C82 H82 119.5 . . ?
C82 C83 C84 120.3(3) . . ?
C82 C83 H83 119.8 . . ?
C84 C83 H83 119.8 . . ?
C85 C84 C83 119.5(3) . . ?
C85 C84 H84 120.3 . . ?
C83 C84 H84 120.3 . . ?
C84 C85 C86 120.2(3) . . ?
C84 C85 H85 119.9 . . ?
C86 C85 H85 119.9 . . ?
C85 C86 C81 121.3(3) . . ?
C85 C86 H86 119.4 . . ?
C81 C86 H86 119.4 . . ?
C81 C87 H87A 109.5 . . ?
C81 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C81 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti Cl6 2.2399(7) . ?
Ti Cl7 2.2426(7) . ?
Ti Cl5 2.2483(8) . ?
Ti C14 2.324(2) . ?
Ti C13 2.332(2) . ?
Ti C12 2.348(2) . ?
Ti C15 2.360(2) . ?
Ti C11 2.4182(19) . ?
C11 C15 1.415(3) . ?
C11 C12 1.439(3) . ?
C11 B 1.642(3) . ?
C12 C13 1.416(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.415(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
B N21 1.623(3) . ?
B C31 1.656(3) . ?
B C41 1.658(3) . ?
N21 C26 1.352(3) . ?
N21 C22 1.362(2) . ?
C22 C23 1.377(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.389(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C31 C36 1.386(3) . ?
C31 C32 1.401(3) . ?
C32 F32 1.361(2) . ?
C32 C33 1.373(3) . ?
C33 F33 1.352(2) . ?
C33 C34 1.377(3) . ?
C34 F34 1.350(2) . ?
C34 C35 1.373(3) . ?
C35 F35 1.347(2) . ?
C35 C36 1.389(3) . ?
C36 F36 1.353(2) . ?
C41 C42 1.388(3) . ?
C41 C46 1.405(3) . ?
C42 F42 1.365(2) . ?
C42 C43 1.385(3) . ?
C43 F43 1.345(3) . ?
C43 C44 1.374(3) . ?
C44 F44 1.353(3) . ?
C44 C45 1.370(3) . ?
C45 F45 1.356(2) . ?
C45 C46 1.386(3) . ?
C46 F46 1.348(2) . ?
C81 C86 1.383(4) . ?
C81 C82 1.393(5) . ?
C81 C87 1.515(4) . ?
C82 C83 1.375(5) . ?
C82 H82 0.9300 . ?
C83 C84 1.382(5) . ?
C83 H83 0.9300 . ?
C84 C85 1.370(4) . ?
C84 H84 0.9300 . ?
C85 C86 1.383(4) . ?
C85 H85 0.9300 . ?
C86 H86 0.9300 . ?
C87 H87A 0.9600 . ?
C87 H87B 0.9600 . ?
C87 H87C 0.9600 . ?
