#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:32:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/70/4317074.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_4317074
loop_
_publ_author_name
'Javier Sánchez-Nieves'
'Luis M. Frutos'
'Pascual Royo'
'Obis Castaño'
'Eberhardt Herdtweck'
'Marta E. G. Mosquera'
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl für Anorganische Chemie,
       Technische Universität München,
       Lichtenbergstrasse 4,
       D-85747 Garching bei München,
       Germany.

       Departamento de Química Inorgánica
       Facultad de Farmacia
       Universidad de Alcalá
       Campus Universitario
       28871 Alcalá de Henares
       Spain
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Dr. Eberhardt Herdtweck
       Dr. Marta E. G. Mosquera
;
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
 Trapping Unstable Terminal M-O Multiple Bonds of Monocyclopentadienyl
 Niobium and Tantalum Complexes with Lewis Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10642
_journal_page_last               10648
_journal_paper_doi               10.1021/ic1016609
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C28 H15 Al Cl2 F15 O Ta'
_chemical_formula_weight         931.23
_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                90.945(9)
_cell_angle_beta                 110.889(7)
_cell_angle_gamma                104.017(8)
_cell_formula_units_Z            2
_cell_length_a                   10.7086(10)
_cell_length_b                   11.2122(10)
_cell_length_c                   14.0319(14)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.566
_cell_measurement_theta_min      4.244
_cell_volume                     1517.3(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34266
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.944
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.382
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0122(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0216P)²+1.0156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                6182
_reflns_number_total             6811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016609_si_001_1.cif
_cod_data_source_block           3a
_cod_original_cell_volume        1517.3(2)
_cod_database_code               4317074
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
Ta1 Ta 0.141154(13) 0.331105(12) 0.625060(9) 0.01528(7) Uani 1 1 d . . .
Al1 Al 0.08126(11) 0.16669(11) 0.82668(8) 0.0188(2) Uani 1 1 d . . .
O1 O 0.1338(3) 0.2468(2) 0.73146(18) 0.0209(6) Uani 1 1 d . . .
Cl1 Cl 0.10415(11) 0.51575(9) 0.66047(8) 0.0322(2) Uani 1 1 d . . .
Cl2 Cl -0.05562(9) 0.22715(10) 0.49272(7) 0.0259(2) Uani 1 1 d . . .
C1 C 0.3618(4) 0.2951(4) 0.6604(3) 0.0193(8) Uani 1 1 d . . .
C2 C 0.2781(4) 0.2443(4) 0.5568(3) 0.0199(8) Uani 1 1 d . . .
C3 C 0.2529(4) 0.3449(4) 0.4973(3) 0.0224(8) Uani 1 1 d . . .
C4 C 0.3163(4) 0.4563(4) 0.5639(3) 0.0242(8) Uani 1 1 d . . .
C5 C 0.3813(4) 0.4261(4) 0.6653(3) 0.0221(8) Uani 1 1 d . . .
C6 C 0.2677(4) 0.0316(4) 0.9734(3) 0.0257(8) Uani 1 1 d . . .
C7 C 0.3413(4) -0.0557(5) 1.0011(3) 0.0326(10) Uani 1 1 d . . .
C8 C 0.3452(4) -0.1339(4) 0.9264(4) 0.0339(10) Uani 1 1 d . . .
C9 C 0.2744(4) -0.1240(4) 0.8242(3) 0.0321(10) Uani 1 1 d . . .
C10 C 0.1986(4) -0.0373(4) 0.8012(3) 0.0274(9) Uani 1 1 d . . .
C11 C 0.4236(4) 0.2258(4) 0.7480(3) 0.0244(8) Uani 1 1 d . . .
H11A H 0.4715 0.2820 0.8099 0.037 Uiso 1 1 calc R . .
H11B H 0.4876 0.1884 0.7337 0.037 Uiso 1 1 calc R . .
H11C H 0.3511 0.1626 0.7566 0.037 Uiso 1 1 calc R . .
C12 C 0.2296(4) 0.1097(4) 0.5149(3) 0.0302(10) Uani 1 1 d . . .
H12A H 0.2597 0.0607 0.5698 0.045 Uiso 1 1 calc R . .
H12B H 0.2681 0.0973 0.4645 0.045 Uiso 1 1 calc R . .
H12C H 0.1303 0.0853 0.4837 0.045 Uiso 1 1 calc R . .
C13 C 0.1800(5) 0.3320(5) 0.3823(3) 0.0322(10) Uani 1 1 d . . .
H13A H 0.1764 0.4121 0.3603 0.048 Uiso 1 1 calc R . .
H13B H 0.0875 0.2797 0.3634 0.048 Uiso 1 1 calc R . .
H13C H 0.2298 0.2959 0.3502 0.048 Uiso 1 1 calc R . .
C14 C 0.3230(5) 0.5848(4) 0.5330(4) 0.0360(10) Uani 1 1 d . . .
H14A H 0.3689 0.6439 0.5932 0.054 Uiso 1 1 calc R . .
H14B H 0.2307 0.5925 0.4980 0.054 Uiso 1 1 calc R . .
H14C H 0.3737 0.6000 0.4882 0.054 Uiso 1 1 calc R . .
C15 C 0.4675(4) 0.5176(4) 0.7595(3) 0.0323(10) Uani 1 1 d . . .
H15A H 0.4643 0.5998 0.7428 0.048 Uiso 1 1 calc R . .
H15B H 0.5617 0.5126 0.7831 0.048 Uiso 1 1 calc R . .
H15C H 0.4312 0.4987 0.8126 0.048 Uiso 1 1 calc R . .
C16 C 0.1934(4) 0.0450(4) 0.8729(3) 0.0224(8) Uani 1 1 d . . .
C21 C 0.1095(4) 0.2943(4) 0.9378(3) 0.0206(8) Uani 1 1 d . . .
C22 C 0.0330(4) 0.2688(4) 1.0001(3) 0.0233(8) Uani 1 1 d . . .
C23 C 0.0442(4) 0.3505(4) 1.0792(3) 0.0289(9) Uani 1 1 d . . .
C24 C 0.1373(5) 0.4651(4) 1.0981(3) 0.0314(10) Uani 1 1 d . . .
C25 C 0.2147(5) 0.4967(4) 1.0387(3) 0.0348(10) Uani 1 1 d . . .
C26 C 0.2004(4) 0.4108(4) 0.9609(3) 0.0310(9) Uani 1 1 d . . .
C31 C -0.1212(4) 0.0866(3) 0.7531(3) 0.0179(7) Uani 1 1 d . . .
C32 C -0.1878(4) -0.0325(4) 0.7586(3) 0.0188(7) Uani 1 1 d . . .
C33 C -0.3290(4) -0.0842(4) 0.7133(3) 0.0215(8) Uani 1 1 d . . .
C34 C -0.4110(4) -0.0131(4) 0.6566(3) 0.0240(9) Uani 1 1 d . . .
C35 C -0.3500(4) 0.1070(4) 0.6470(3) 0.0225(8) Uani 1 1 d . . .
C36 C -0.2084(4) 0.1536(4) 0.6953(3) 0.0207(8) Uani 1 1 d . . .
F6 F 0.2702(3) 0.1073(3) 1.05106(17) 0.0397(7) Uani 1 1 d . . .
F7 F 0.4096(3) -0.0659(3) 1.1006(2) 0.0498(8) Uani 1 1 d . . .
F8 F 0.4203(3) -0.2158(3) 0.9502(2) 0.0518(8) Uani 1 1 d . . .
F9 F 0.2782(3) -0.1984(3) 0.7496(2) 0.0517(8) Uani 1 1 d . . .
F10 F 0.1262(3) -0.0323(3) 0.69994(17) 0.0371(7) Uani 1 1 d . . .
F22 F -0.0581(3) 0.1569(3) 0.98382(19) 0.0387(6) Uani 1 1 d . . .
F23 F -0.0320(3) 0.3210(3) 1.13728(19) 0.0472(8) Uani 1 1 d . . .
F24 F 0.1512(3) 0.5468(3) 1.1756(2) 0.0531(9) Uani 1 1 d . . .
F26 F 0.2831(3) 0.4454(3) 0.9067(2) 0.0523(8) Uani 1 1 d . . .
F32 F -0.1130(2) -0.1088(2) 0.81296(17) 0.0272(5) Uani 1 1 d . . .
F33 F -0.3884(2) -0.2016(2) 0.72138(19) 0.0329(6) Uani 1 1 d . . .
F34 F -0.5487(2) -0.0595(3) 0.6116(2) 0.0365(6) Uani 1 1 d . . .
F35 F -0.4295(2) 0.1780(3) 0.59105(18) 0.0339(6) Uani 1 1 d . . .
F36 F -0.1550(2) 0.2732(2) 0.68520(17) 0.0266(5) Uani 1 1 d . . .
F25 F 0.3036(4) 0.6086(3) 1.0575(2) 0.0579(9) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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'
Al Al 0.0645 0.0514 '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'
Ta Ta -0.7052 6.5227 '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
O1 Ta1 Cl1 104.91(8) . . ?
O1 Ta1 Cl2 103.28(9) . . ?
Cl1 Ta1 Cl2 105.32(4) . . ?
O1 Ta1 C1 86.74(12) . . ?
Cl1 Ta1 C1 125.14(10) . . ?
Cl2 Ta1 C1 124.14(9) . . ?
O1 Ta1 C2 104.99(12) . . ?
Cl1 Ta1 C2 141.60(11) . . ?
Cl2 Ta1 C2 90.59(9) . . ?
C1 Ta1 C2 34.94(11) . . ?
O1 Ta1 C5 105.29(13) . . ?
Cl1 Ta1 C5 91.32(10) . . ?
Cl2 Ta1 C5 141.75(9) . . ?
C1 Ta1 C5 34.97(13) . . ?
C2 Ta1 C5 57.76(13) . . ?
O1 Ta1 C3 139.17(11) . . ?
Cl1 Ta1 C3 111.15(10) . . ?
Cl2 Ta1 C3 85.32(9) . . ?
C1 Ta1 C3 57.07(12) . . ?
C2 Ta1 C3 34.34(13) . . ?
C5 Ta1 C3 56.46(12) . . ?
O1 Ta1 C4 139.27(12) . . ?
Cl1 Ta1 C4 84.97(9) . . ?
Cl2 Ta1 C4 112.11(9) . . ?
C1 Ta1 C4 57.07(13) . . ?
C2 Ta1 C4 56.63(13) . . ?
C5 Ta1 C4 34.16(12) . . ?
C3 Ta1 C4 33.13(13) . . ?
O1 Al1 C21 107.05(16) . . ?
O1 Al1 C16 107.65(15) . . ?
C21 Al1 C16 113.94(15) . . ?
O1 Al1 C31 104.19(14) . . ?
C21 Al1 C31 110.15(15) . . ?
C16 Al1 C31 113.17(17) . . ?
Ta1 O1 Al1 165.08(15) . . ?
C2 C1 C5 107.4(3) . . ?
C2 C1 C11 126.9(3) . . ?
C5 C1 C11 125.7(3) . . ?
C2 C1 Ta1 72.93(18) . . ?
C5 C1 Ta1 73.01(19) . . ?
C11 C1 Ta1 121.4(3) . . ?
C1 C2 C3 108.0(3) . . ?
C1 C2 C12 126.6(3) . . ?
C3 C2 C12 125.3(3) . . ?
C1 C2 Ta1 72.13(18) . . ?
C3 C2 Ta1 76.3(2) . . ?
C12 C2 Ta1 119.8(3) . . ?
C4 C3 C2 108.2(3) . . ?
C4 C3 C13 126.8(4) . . ?
C2 C3 C13 124.9(4) . . ?
C4 C3 Ta1 73.6(2) . . ?
C2 C3 Ta1 69.3(2) . . ?
C13 C3 Ta1 126.1(3) . . ?
C3 C4 C5 108.0(4) . . ?
C3 C4 C14 126.1(4) . . ?
C5 C4 C14 125.7(4) . . ?
C3 C4 Ta1 73.3(2) . . ?
C5 C4 Ta1 69.4(2) . . ?
C14 C4 Ta1 126.1(3) . . ?
C4 C5 C1 108.3(3) . . ?
C4 C5 C15 125.9(4) . . ?
C1 C5 C15 125.6(4) . . ?
C4 C5 Ta1 76.5(2) . . ?
C1 C5 Ta1 72.0(2) . . ?
C15 C5 Ta1 121.9(3) . . ?
F6 C6 C7 116.6(3) . . ?
F6 C6 C16 119.6(3) . . ?
C7 C6 C16 123.7(4) . . ?
F7 C7 C8 119.4(4) . . ?
F7 C7 C6 121.0(4) . . ?
C8 C7 C6 119.7(4) . . ?
F8 C8 C7 121.3(4) . . ?
F8 C8 C9 119.3(4) . . ?
C7 C8 C9 119.4(4) . . ?
F9 C9 C10 121.3(4) . . ?
F9 C9 C8 120.4(4) . . ?
C10 C9 C8 118.3(4) . . ?
F10 C10 C16 118.2(3) . . ?
F10 C10 C9 117.1(3) . . ?
C16 C10 C9 124.7(4) . . ?
C10 C16 C6 114.1(3) . . ?
C10 C16 Al1 119.7(3) . . ?
C6 C16 Al1 126.1(3) . . ?
C26 C21 C22 114.3(3) . . ?
C26 C21 Al1 126.2(3) . . ?
C22 C21 Al1 119.6(3) . . ?
F22 C22 C23 117.0(4) . . ?
F22 C22 C21 118.6(3) . . ?
C23 C22 C21 124.4(4) . . ?
F23 C23 C24 119.9(4) . . ?
F23 C23 C22 121.9(4) . . ?
C24 C23 C22 118.2(4) . . ?
F24 C24 C25 120.1(4) . . ?
F24 C24 C23 119.5(4) . . ?
C25 C24 C23 120.4(4) . . ?
F25 C25 C24 119.6(4) . . ?
F25 C25 C26 121.4(5) . . ?
C24 C25 C26 119.0(4) . . ?
F26 C26 C21 119.7(4) . . ?
F26 C26 C25 116.6(4) . . ?
C21 C26 C25 123.7(4) . . ?
C32 C31 C36 114.0(3) . . ?
C32 C31 Al1 125.3(3) . . ?
C36 C31 Al1 120.6(3) . . ?
F32 C32 C31 119.8(3) . . ?
F32 C32 C33 115.4(4) . . ?
C31 C32 C33 124.8(3) . . ?
F33 C33 C32 122.1(3) . . ?
F33 C33 C34 119.2(3) . . ?
C32 C33 C34 118.7(4) . . ?
F34 C34 C35 120.1(3) . . ?
F34 C34 C33 120.6(4) . . ?
C35 C34 C33 119.3(4) . . ?
F35 C35 C36 120.9(4) . . ?
F35 C35 C34 119.9(3) . . ?
C36 C35 C34 119.2(3) . . ?
F36 C36 C35 116.4(3) . . ?
F36 C36 C31 119.6(3) . . ?
C35 C36 C31 124.0(4) . . ?
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
Ta1 O1 1.795(3) . ?
Ta1 Cl1 2.2790(9) . ?
Ta1 Cl2 2.2794(9) . ?
Ta1 C1 2.372(3) . ?
Ta1 C2 2.382(3) . ?
Ta1 C5 2.385(4) . ?
Ta1 C3 2.474(4) . ?
Ta1 C4 2.477(4) . ?
Al1 O1 1.800(3) . ?
Al1 C21 1.988(4) . ?
Al1 C16 1.998(4) . ?
Al1 C31 2.001(4) . ?
C1 C2 1.427(5) . ?
C1 C5 1.429(5) . ?
C1 C11 1.501(5) . ?
C2 C3 1.436(5) . ?
C2 C12 1.505(5) . ?
C3 C4 1.411(5) . ?
C3 C13 1.507(5) . ?
C4 C5 1.431(5) . ?
C4 C14 1.504(6) . ?
C5 C15 1.510(5) . ?
C6 F6 1.359(5) . ?
C6 C7 1.378(6) . ?
C6 C16 1.382(5) . ?
C7 F7 1.346(5) . ?
C7 C8 1.374(6) . ?
C8 F8 1.333(5) . ?
C8 C9 1.384(6) . ?
C9 F9 1.346(5) . ?
C9 C10 1.383(6) . ?
C10 F10 1.365(4) . ?
C10 C16 1.379(5) . ?
C21 C26 1.379(6) . ?
C21 C22 1.386(6) . ?
C22 F22 1.348(5) . ?
C22 C23 1.380(5) . ?
C23 F23 1.338(5) . ?
C23 C24 1.377(7) . ?
C24 F24 1.353(4) . ?
C24 C25 1.366(7) . ?
C25 F25 1.335(5) . ?
C25 C26 1.385(6) . ?
C26 F26 1.356(5) . ?
C31 C32 1.371(6) . ?
C31 C36 1.384(5) . ?
C32 F32 1.368(4) . ?
C32 C33 1.380(5) . ?
C33 F33 1.342(5) . ?
C33 C34 1.379(5) . ?
C34 F34 1.341(4) . ?
C34 C35 1.379(6) . ?
C35 F35 1.359(4) . ?
C35 C36 1.379(5) . ?
C36 F36 1.356(5) . ?
