#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:50:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179080 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/42/4304268.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_4304268
loop_
_publ_author_name
'Grigory B. Nikiforov'
'Herbert W. Roesky'
'Peter G. Jones'
'Jörg Magull'
'Arne Ringe'
'Rainer B. Oswald'
_publ_contact_author_address
;Institut fuer Anorganische Chemie
Universitaet Goettingen
Tammannstr. 4
37077 Goettingen
Germany
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         '0049 /551 /39-3373'
_publ_contact_author_name        'Herbert W. Roesky'
_publ_contact_author_phone       '0049/ 551/ 39-3001'
_publ_section_title
;
Preparation of Ti(IV) Fluoride N-Heterocyclic Carbene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2171
_journal_page_last               2179
_journal_paper_doi               10.1021/ic701751r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H48 Cl4 F6 N6 Ti2'
_chemical_formula_weight         772.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                112.235(4)
_cell_angle_beta                 105.096(4)
_cell_angle_gamma                94.226(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7060(6)
_cell_length_b                   9.4675(6)
_cell_length_c                   11.9152(8)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.99
_cell_measurement_theta_min      2.37
_cell_volume                     861.24(11)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX2 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0216
_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            26753
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.9214
_exptl_absorpt_correction_T_min  0.8015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         6530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0264
_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)+(0.0347P)²+0.2790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                5766
_reflns_number_total             6530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701751r-file004.cif
_cod_data_source_block           nitinet
_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        861.24(10)
_cod_database_code               4304268
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 0.365858(19) 0.561243(18) 0.414139(14) 0.00996(4) Uani 1 1 d . . .
C1 C 0.26088(11) 0.76527(10) 0.50982(8) 0.01224(15) Uani 1 1 d . . .
C2 C 0.23583(12) 0.98645(11) 0.66407(9) 0.01507(16) Uani 1 1 d . . .
C3 C 0.08508(12) 0.89773(11) 0.59946(9) 0.01440(16) Uani 1 1 d . . .
C4 C 0.51541(12) 0.96205(12) 0.65105(10) 0.01805(17) Uani 1 1 d . . .
H4A H 0.5669 0.8852 0.5996 0.022 Uiso 1 1 calc R . .
H4B H 0.5608 0.9809 0.7410 0.022 Uiso 1 1 calc R . .
H4C H 0.5356 1.0595 0.6415 0.022 Uiso 1 1 calc R . .
C5 C 0.29272(14) 1.14385(12) 0.77115(10) 0.0217(2) Uani 1 1 d . . .
H5A H 0.2014 1.1794 0.8002 0.026 Uiso 1 1 calc R . .
H5B H 0.3373 1.2166 0.7419 0.026 Uiso 1 1 calc R . .
H5C H 0.3769 1.1391 0.8418 0.026 Uiso 1 1 calc R . .
C6 C -0.07407(13) 0.92337(12) 0.62000(11) 0.01967(18) Uani 1 1 d . . .
H6A H -0.0561 1.0076 0.7041 0.024 Uiso 1 1 calc R . .
H6B H -0.1322 0.8278 0.6156 0.024 Uiso 1 1 calc R . .
H6C H -0.1386 0.9516 0.5538 0.024 Uiso 1 1 calc R . .
C7 C -0.03278(11) 0.64576(12) 0.40513(9) 0.01613(16) Uani 1 1 d . . .
H7A H -0.0178 0.6222 0.3216 0.019 Uiso 1 1 calc R . .
H7B H -0.1341 0.6841 0.4064 0.019 Uiso 1 1 calc R . .
H7C H -0.0375 0.5513 0.4207 0.019 Uiso 1 1 calc R . .
C8 C 0.26676(12) 0.57760(11) 0.16077(9) 0.01531(16) Uani 1 1 d . . .
H8A H 0.2454 0.4985 0.0727 0.018 Uiso 1 1 calc R . .
H8B H 0.3815 0.6309 0.1929 0.018 Uiso 1 1 calc R . .
C9 C 0.15764(14) 0.69552(13) 0.15903(10) 0.02068(19) Uani 1 1 d . . .
H9A H 0.0439 0.6422 0.1235 0.025 Uiso 1 1 calc R . .
H9B H 0.1810 0.7470 0.1062 0.025 Uiso 1 1 calc R . .
H9C H 0.1777 0.7733 0.2463 0.025 Uiso 1 1 calc R . .
C10 C 0.10533(12) 0.36499(11) 0.17205(9) 0.01687(17) Uani 1 1 d . . .
H10A H 0.0198 0.3873 0.1114 0.020 Uiso 1 1 calc R . .
H10B H 0.0575 0.3459 0.2330 0.020 Uiso 1 1 calc R . .
C11 C 0.16332(15) 0.21994(13) 0.09907(12) 0.0267(2) Uani 1 1 d . . .
H11A H 0.2184 0.2414 0.0436 0.032 Uiso 1 1 calc R . .
H11B H 0.0700 0.1344 0.0470 0.032 Uiso 1 1 calc R . .
H11C H 0.2388 0.1907 0.1597 0.032 Uiso 1 1 calc R . .
F1 F 0.49462(7) 0.39296(7) 0.39819(5) 0.01385(11) Uani 1 1 d . . .
F2 F 0.52274(7) 0.69350(7) 0.40513(6) 0.01523(11) Uani 1 1 d . . .
F3 F 0.21189(7) 0.44305(7) 0.43886(6) 0.01668(11) Uani 1 1 d . . .
N1 N 0.34110(10) 0.90335(9) 0.60799(8) 0.01334(14) Uani 1 1 d . . .
N2 N 0.10311(10) 0.76466(9) 0.50455(7) 0.01241(13) Uani 1 1 d . . .
N3 N 0.23939(10) 0.50043(9) 0.24202(7) 0.01239(13) Uani 1 1 d . . .
C99 C 0.65463(17) 0.27490(16) 0.17838(12) 0.0299(2) Uani 1 1 d . . .
H99A H 0.5531 0.2388 0.1907 0.036 Uiso 1 1 calc R . .
H99B H 0.7402 0.3199 0.2623 0.036 Uiso 1 1 calc R . .
Cl1 Cl 0.71134(4) 0.11536(3) 0.07204(3) 0.02903(7) Uani 1 1 d . . .
Cl2 Cl 0.62533(4) 0.41899(4) 0.11909(3) 0.03200(7) 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'
N N 0.0061 0.0033 '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'
Ti Ti 0.2776 0.4457 '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'
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
F3 Ti F2 174.45(3) . . ?
F3 Ti N3 91.11(3) . . ?
F2 Ti N3 93.27(3) . . ?
F3 Ti F1 88.37(3) . . ?
F2 Ti F1 94.11(3) . . ?
N3 Ti F1 101.34(3) . . ?
F3 Ti F1 85.93(3) . 2_666 ?
F2 Ti F1 89.96(3) . 2_666 ?
N3 Ti F1 174.74(3) . 2_666 ?
F1 Ti F1 74.26(3) . 2_666 ?
F3 Ti C1 86.50(3) . . ?
F2 Ti C1 89.37(3) . . ?
N3 Ti C1 100.06(3) . . ?
F1 Ti C1 158.08(3) . . ?
F1 Ti C1 84.11(3) 2_666 . ?
F3 Ti Ti 86.39(2) . 2_666 ?
F2 Ti Ti 92.48(2) . 2_666 ?
N3 Ti Ti 139.59(3) . 2_666 ?
F1 Ti Ti 38.322(16) . 2_666 ?
F1 Ti Ti 35.942(15) 2_666 2_666 ?
C1 Ti Ti 119.98(2) . 2_666 ?
N2 C1 N1 103.93(8) . . ?
N2 C1 Ti 126.55(7) . . ?
N1 C1 Ti 127.75(6) . . ?
C3 C2 N1 106.41(8) . . ?
C3 C2 C5 131.30(9) . . ?
N1 C2 C5 122.26(9) . . ?
C2 C3 N2 106.28(8) . . ?
C2 C3 C6 130.68(9) . . ?
N2 C3 C6 123.02(9) . . ?
N3 C8 C9 111.47(8) . . ?
N3 C10 C11 111.35(8) . . ?
Ti F1 Ti 105.74(3) . 2_666 ?
C1 N1 C2 111.64(8) . . ?
C1 N1 C4 125.66(8) . . ?
C2 N1 C4 122.70(8) . . ?
C1 N2 C3 111.73(8) . . ?
C1 N2 C7 124.33(8) . . ?
C3 N2 C7 123.75(8) . . ?
C8 N3 C10 111.84(8) . . ?
C8 N3 Ti 124.55(6) . . ?
C10 N3 Ti 123.56(6) . . ?
Cl2 C99 Cl1 110.92(7) . . ?
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 F3 1.8357(6) . ?
Ti F2 1.8361(6) . ?
Ti N3 1.8938(8) . ?
Ti F1 1.9940(6) . ?
Ti F1 2.1066(6) 2_666 ?
Ti C1 2.2367(9) . ?
Ti Ti 3.2699(4) 2_666 ?
C1 N2 1.3580(12) . ?
C1 N1 1.3592(12) . ?
C2 C3 1.3574(14) . ?
C2 N1 1.3902(12) . ?
C2 C5 1.4889(14) . ?
C3 N2 1.3907(12) . ?
C3 C6 1.4899(14) . ?
C4 N1 1.4593(13) . ?
C7 N2 1.4610(13) . ?
C8 N3 1.4689(12) . ?
C8 C9 1.5208(14) . ?
C10 N3 1.4714(13) . ?
C10 C11 1.5245(15) . ?
F1 Ti 2.1066(6) 2_666 ?
C99 Cl2 1.7640(13) . ?
C99 Cl1 1.7657(13) . ?
