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_7055593
_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         'F5 Ti, F5 Xe'
_chemical_formula_sum            'F10 Ti Xe'
_chemical_formula_weight         369.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.139(2)
_cell_length_b                   8.5173(9)
_cell_length_c                   18.1876(16)
_cell_measurement_reflns_used    1973
_cell_measurement_temperature    149.97(15)
_cell_measurement_theta_max      27.5280
_cell_measurement_theta_min      4.1680
_cell_volume                     2809.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.97(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3213
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w    -62.00  17.00   1.00  800.00    --    9.00 -57.00-150.00   79
  2  \w     11.00  50.00   1.00  800.00    --    9.00  57.00  30.00   39
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120372000
_diffrn_orient_matrix_UB_12      0.0525936000
_diffrn_orient_matrix_UB_13      0.0277077000
_diffrn_orient_matrix_UB_21      0.0342788000
_diffrn_orient_matrix_UB_22      0.0085104000
_diffrn_orient_matrix_UB_23      -0.0184050000
_diffrn_orient_matrix_UB_31      -0.0144251000
_diffrn_orient_matrix_UB_32      0.0640050000
_diffrn_orient_matrix_UB_33      -0.0203815000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7823
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.895
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.101
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    3.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.028
_refine_diff_density_max         7.688
_refine_diff_density_min         -3.278
_refine_diff_density_rms         0.475
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+323.2242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2076
_reflns_number_total             3029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00955g2.cif
_cod_data_source_block           xef5ttif5
_cod_depositor_comments
'Adding full bibliography for 7055592--7055594.cif.'
_cod_original_cell_volume        2810.0(5)
_cod_database_code               7055593
_reflns_odcompleteness_completeness 96.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              72326
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.738