#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:47:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179764 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006053.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_7006053
loop_
_publ_author_name
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 Reactivity of niobium(v) and tantalum(v) halides with carbonyl
 compounds: synthesis of simple coordination adducts, C-H bond
 activation, C=O protonation, and halide transfer.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4343
_journal_page_last               4351
_journal_paper_doi               10.1039/b708531a
_journal_year                    2007
_chemical_formula_sum            'C18 H27 F7 O6 Ta2'
_chemical_formula_weight         834.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.3387(15)
_cell_length_b                   11.3387(15)
_cell_length_c                   32.002(8)
_cell_measurement_reflns_used    5290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2445
_cell_measurement_theta_min      2.4335
_cell_volume                     3563.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            12926
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    9.292
_exptl_absorpt_correction_T_max  0.4018
_exptl_absorpt_correction_T_min  0.2856
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.907
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0533P)²+13.5225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                1535
_reflns_number_total             1887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708531a.txt
_cod_data_source_block           r-3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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_sg_symbol_H-M      R-3
_cod_database_code               7006053
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.3333 0.6667 0.035149(10) 0.01503(13) Uani 1 3 d S . .
F1 F 0.3333 0.6667 -0.02449(15) 0.0178(10) Uani 1 3 d S . .
C1 C 0.3321(5) 1.0425(6) 0.02250(18) 0.0228(11) Uani 1 1 d . . .
H1A H 0.3251 1.0274 -0.0078 0.034 Uiso 1 1 calc R . .
H1B H 0.3963 1.1387 0.0283 0.034 Uiso 1 1 calc R . .
H1C H 0.2424 1.0179 0.0338 0.034 Uiso 1 1 calc R . .
C2 C 0.3817(5) 0.9565(5) 0.04243(16) 0.0168(10) Uani 1 1 d . . .
C3 C 0.4519(5) 0.9897(5) 0.08061(16) 0.0188(11) Uani 1 1 d . . .
C4 C 0.5042(5) 0.9083(5) 0.09466(16) 0.0159(10) Uani 1 1 d . . .
C5 C 0.6045(6) 0.9507(6) 0.13009(18) 0.0245(12) Uani 1 1 d . . .
H5A H 0.5561 0.9338 0.1567 0.037 Uiso 1 1 calc R . .
H5B H 0.6713 1.0479 0.1276 0.037 Uiso 1 1 calc R . .
H5C H 0.6515 0.8979 0.1290 0.037 Uiso 1 1 calc R . .
C6 C 0.4767(6) 1.1160(5) 0.10390(18) 0.0244(12) Uani 1 1 d . . .
H6A H 0.5202 1.1206 0.1308 0.037 Uiso 1 1 calc R . .
H6B H 0.3896 1.1125 0.1087 0.037 Uiso 1 1 calc R . .
H6C H 0.5363 1.1969 0.0873 0.037 Uiso 1 1 calc R . .
O1 O 0.3554(4) 0.8487(4) 0.02067(11) 0.0167(7) Uani 1 1 d . . .
O2 O 0.4755(4) 0.7934(4) 0.07799(11) 0.0187(8) Uani 1 1 d . . .
Ta2 Ta 0.0000 1.0000 0.102974(11) 0.01805(14) Uani 1 3 d S . .
F2 F 0.0175(4) 0.8724(3) 0.06901(11) 0.0304(8) Uani 1 1 d . . .
F3 F 0.1444(3) 1.0163(4) 0.13681(11) 0.0312(8) 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'
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
F1 Ta1 O1 76.64(10) . . ?
F1 Ta1 O1 76.64(10) . 2_665 ?
O1 Ta1 O1 114.83(8) . 2_665 ?
F1 Ta1 O1 76.64(10) . 3_565 ?
O1 Ta1 O1 114.83(8) . 3_565 ?
O1 Ta1 O1 114.83(8) 2_665 3_565 ?
F1 Ta1 O2 131.82(10) . 2_665 ?
O1 Ta1 O2 78.41(14) . 2_665 ?
O1 Ta1 O2 77.53(14) 2_665 2_665 ?
O1 Ta1 O2 151.53(15) 3_565 2_665 ?
F1 Ta1 O2 131.82(10) . . ?
O1 Ta1 O2 77.53(14) . . ?
O1 Ta1 O2 151.53(15) 2_665 . ?
O1 Ta1 O2 78.41(14) 3_565 . ?
O2 Ta1 O2 80.39(15) 2_665 . ?
F1 Ta1 O2 131.82(10) . 3_565 ?
O1 Ta1 O2 151.53(15) . 3_565 ?
O1 Ta1 O2 78.41(14) 2_665 3_565 ?
O1 Ta1 O2 77.53(14) 3_565 3_565 ?
O2 Ta1 O2 80.39(15) 2_665 3_565 ?
O2 Ta1 O2 80.39(15) . 3_565 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.3(5) . . ?
O1 C2 C1 113.6(4) . . ?
C3 C2 C1 123.1(5) . . ?
C4 C3 C2 118.3(5) . . ?
C4 C3 C6 121.9(5) . . ?
C2 C3 C6 119.7(5) . . ?
O2 C4 C3 123.9(5) . . ?
O2 C4 C5 113.7(4) . . ?
C3 C4 C5 122.3(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 O1 Ta1 133.9(3) . . ?
C4 O2 Ta1 134.0(3) . . ?
F3 Ta2 F3 90.53(15) . 2_675 ?
F3 Ta2 F3 90.53(15) . 3_465 ?
F3 Ta2 F3 90.53(15) 2_675 3_465 ?
F3 Ta2 F2 179.63(15) . 3_465 ?
F3 Ta2 F2 89.77(15) 2_675 3_465 ?
F3 Ta2 F2 89.25(15) 3_465 3_465 ?
F3 Ta2 F2 89.25(15) . . ?
F3 Ta2 F2 179.63(16) 2_675 . ?
F3 Ta2 F2 89.77(15) 3_465 . ?
F2 Ta2 F2 90.45(15) 3_465 . ?
F3 Ta2 F2 89.77(15) . 2_675 ?
F3 Ta2 F2 89.25(15) 2_675 2_675 ?
F3 Ta2 F2 179.63(15) 3_465 2_675 ?
F2 Ta2 F2 90.45(15) 3_465 2_675 ?
F2 Ta2 F2 90.45(15) . 2_675 ?
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 F1 1.909(5) . ?
Ta1 O1 2.005(3) . ?
Ta1 O1 2.005(3) 2_665 ?
Ta1 O1 2.005(3) 3_565 ?
Ta1 O2 2.056(4) 2_665 ?
Ta1 O2 2.056(4) . ?
Ta1 O2 2.056(4) 3_565 ?
C1 C2 1.490(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O1 1.305(6) . ?
C2 C3 1.403(7) . ?
C3 C4 1.398(7) . ?
C3 C6 1.511(7) . ?
C4 O2 1.290(6) . ?
C4 C5 1.504(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Ta2 F3 1.893(3) . ?
Ta2 F3 1.893(3) 2_675 ?
Ta2 F3 1.893(3) 3_465 ?
Ta2 F2 1.897(3) 3_465 ?
Ta2 F2 1.897(3) . ?
Ta2 F2 1.897(3) 2_675 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 4.4(7) . . . . ?
C1 C2 C3 C4 -174.5(5) . . . . ?
O1 C2 C3 C6 -179.4(5) . . . . ?
C1 C2 C3 C6 1.7(7) . . . . ?
C2 C3 C4 O2 -10.5(7) . . . . ?
C6 C3 C4 O2 173.4(5) . . . . ?
C2 C3 C4 C5 167.1(5) . . . . ?
C6 C3 C4 C5 -9.0(8) . . . . ?
C3 C2 O1 Ta1 25.5(7) . . . . ?
C1 C2 O1 Ta1 -155.5(4) . . . . ?
F1 Ta1 O1 C2 -171.6(4) . . . . ?
O1 Ta1 O1 C2 120.2(5) 2_665 . . . ?
O1 Ta1 O1 C2 -103.4(5) 3_565 . . . ?
O2 Ta1 O1 C2 49.9(4) 2_665 . . . ?
O2 Ta1 O1 C2 -32.6(4) . . . . ?
O2 Ta1 O1 C2 7.3(6) 3_565 . . . ?
C3 C4 O2 Ta1 -11.6(8) . . . . ?
C5 C4 O2 Ta1 170.6(3) . . . . ?
F1 Ta1 O2 C4 84.7(5) . . . . ?
O1 Ta1 O2 C4 25.7(4) . . . . ?
O1 Ta1 O2 C4 -93.9(5) 2_665 . . . ?
O1 Ta1 O2 C4 144.7(5) 3_565 . . . ?
O2 Ta1 O2 C4 -54.5(5) 2_665 . . . ?
O2 Ta1 O2 C4 -136.2(4) 3_565 . . . ?
