Largest perfluorometallate [Ti10F45]5−oligomer and polymeric ([Ti3F13]−)∞and ([TiF5]−)∞anions prepared as [XeF5]+salts
Mazej, Zoran; Goreshnik, Evgeny A.; New J. Chem. 40 (2016) 7320–; doi:10.1039/C6NJ00955G

data_7055594
_publ_section_title
;
 Largest perfluorometallate [Ti10F45]5&#x2212;oligomer and polymeric
 ([Ti3F13]&#x2212;)\\infty and ([TiF5]&#x2212;)\\infty anions prepared as
 [XeF5]+salts
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7320
_journal_paper_doi               10.1039/C6NJ00955G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'F26 Ti6, 2(F5 Xe)'
_chemical_formula_sum            'F36 Ti6 Xe2'
_chemical_formula_weight         1233.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2014-04-09
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                89.601(5)
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_cell_length_c                   13.4581(7)
_cell_measurement_reflns_used    4483
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.27a (release 02-12-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.27a (release 02-12-2013 CrysAlis171 .NET)
(compiled Dec  2 2013,13:24:55)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.27a (release 02-12-2013 CrysAlis171 .NET)
(compiled Dec  2 2013,13:24:55)
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_computing_molecular_graphics
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Crystal Impact GbR, Bonn, Germany (2004-2005) DIAMOND v3.1.
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
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 SHELXL-2014/7 (Sheldrick, 2014)
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SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6426
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_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.8132
_diffrn_measurement_details
;
  1 omega  -58.00   34.00   1.0000  109.9000
omega____ theta____ kappa____ phi______ frames
    -       11.3380  -57.0000 -180.0000 92

  2 omega  -15.00   77.00   1.0000  109.9000
omega____ theta____ kappa____ phi______ frames
    -       11.3380   77.0000   90.0000 92

  3 omega  -17.00   82.00   1.0000  109.9000
omega____ theta____ kappa____ phi______ frames
    -       11.3380   57.0000  -30.0000 99
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0273985000
_diffrn_orient_matrix_UB_12      0.0447131000
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_diffrn_orient_matrix_UB_21      0.0743565000
_diffrn_orient_matrix_UB_22      -0.0310823000
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_diffrn_orient_matrix_UB_31      -0.0022866000
_diffrn_orient_matrix_UB_32      0.0372861000
_diffrn_orient_matrix_UB_33      -0.0428102000
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
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_diffrn_reflns_number            9831
_diffrn_reflns_theta_full        25.000000
_diffrn_reflns_theta_max         29.75
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.471
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.27a (release 02-12-2013 CrysAlis171 .NET)
(compiled Dec  2 2013,13:24:55)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.0857
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.4274
_exptl_crystal_size_mid          0.1085
_exptl_crystal_size_min          0.031
_refine_diff_density_max         4.392
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.330
_refine_ls_d_res_low             5.643995
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
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_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4404
_reflns_number_total             6162
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6nj00955g3.cif
_cod_data_source_block           XeF5Ti3F13
_cod_depositor_comments
'Adding full bibliography for 7055592--7055594.cif.'
_cod_original_cell_volume        1327.82(14)
_cod_database_code               7055594
_shelx_res_checksum              3810