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_7055592
_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_absolute_configuration unk
_chemical_formula_moiety         'F45 Ti10, 5(F5 Xe)'
_chemical_formula_sum            'F70 Ti10 Xe5'
_chemical_formula_weight         2465.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_audit_creation_date             2015-07-17
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8980(4)
_cell_length_b                   16.7388(4)
_cell_length_c                   17.3542(4)
_cell_measurement_reflns_used    6155
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.4910
_cell_measurement_theta_min      4.2720
_cell_volume                     5489.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
Crystal Impact GbR, Bonn, Germany (2004-2005) DIAMOND v3.1.
;
_computing_publication_material
;
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
;
 SHELXL-2014/7 (Sheldrick, 2014)
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6426
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9732
_diffrn_measured_fraction_theta_max 0.7236
_diffrn_measurement_details
;
  1 omega   -6.00   70.00   1.0000   14.9750
omega____ theta____ kappa____ phi______ frames
    -        9.0022   57.0000   90.0000 76

  2 omega  -47.00   16.00   1.0000   14.9750
omega____ theta____ kappa____ phi______ frames
    -        9.0022  -57.0000  -90.0000 63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0346905000
_diffrn_orient_matrix_UB_12      0.0123536000
_diffrn_orient_matrix_UB_13      -0.0100552000
_diffrn_orient_matrix_UB_21      0.0142427000
_diffrn_orient_matrix_UB_22      -0.0270451000
_diffrn_orient_matrix_UB_23      0.0273732000
_diffrn_orient_matrix_UB_31      0.0014612000
_diffrn_orient_matrix_UB_32      -0.0301714000
_diffrn_orient_matrix_UB_33      -0.0286644000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9865
_diffrn_reflns_theta_full        25.000000
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.651
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    2.9595
_exptl_crystal_description       block
_exptl_crystal_F_000             4479.8
_exptl_crystal_size_max          0.5668
_exptl_crystal_size_mid          0.3907
_exptl_crystal_size_min          0.3511
_refine_diff_density_max         2.306
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 1995 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.039(9)
_refine_ls_d_res_high            0.734698
_refine_ls_d_res_low             5.895666
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0436P)^2^+31.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.610
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              20
_reflns_limit_l_min              -22
_reflns_number_gt                5148
_reflns_number_total             5429
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6nj00955g4.cif
_cod_data_source_block           (XeF5)5Ti10F45_capp2
_cod_depositor_comments
'Adding full bibliography for 7055592--7055594.cif.'
_cod_database_code               7055592
_chemical_oxdiff_formula         'Xe5 Ti10 F70'
_reflns_odcompleteness_completeness 97.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32