Crystal structures of hydrated rare-earth bis(trifluoromethylsulfonyl)imide salts
Vander Hoogerstraete, Tom; Brooks, Neil R.; Onghena, Bieke; Van Meervelt, Luc; Binnemans, Koen; CrystEngComm 17 (2015) 7142–; doi:10.1039/C5CE01270H

data_7221802
_publ_section_title
;
 Crystal structures of hydrated rare-earth
 bis(trifluoromethylsulfonyl)imide salts
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7142
_journal_paper_doi               10.1039/C5CE01270H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'H14 O7 Sc, 3(C2 F6 N O4 S2), H2 O'
_chemical_formula_sum            'C6 H16 F18 N3 O20 S6 Sc'
_chemical_formula_weight         1029.54
_chemical_name_systematic
;
Heptaaqua-scandium(iii) tris(bis(trifluoromethylsulfonyl)imide) hydrate
;
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_audit_update_record
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.166(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8946(4)
_cell_length_b                   19.9678(10)
_cell_length_c                   18.7790(8)
_cell_measurement_reflns_used    8048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8560
_cell_measurement_theta_min      3.2410
_cell_volume                     3301.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details
;
  1 omega  -59.00   43.75   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   19.0000   90.0000 137

  2 omega  -33.00    3.75   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000    0.0000 49

  3 omega  -13.00   29.00   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000 -180.0000 56

  4 omega    2.00   81.50   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000  120.0000 106
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0585817000
_diffrn_orient_matrix_UB_12      0.0187608000
_diffrn_orient_matrix_UB_13      -0.0125756000
_diffrn_orient_matrix_UB_21      -0.0378904000
_diffrn_orient_matrix_UB_22      -0.0029760000
_diffrn_orient_matrix_UB_23      -0.0357984000
_diffrn_orient_matrix_UB_31      -0.0403932000
_diffrn_orient_matrix_UB_32      0.0299723000
_diffrn_orient_matrix_UB_33      0.0043107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17794
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.70
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0318
_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/[\s^2^(Fo^2^)+(0.0287P)^2^+2.4643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                6547
_reflns_number_total             7599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01270h2.cif
_cod_data_source_block           nrb147
_cod_depositor_comments
'Adding full bibliography for 7221799--7221808.cif.'
_cod_database_code               7221802
_chemical_oxdiff_formula         'Sc C6 F18 S6 O12 N3 O6 H12'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2013-04-12
_olex2_submission_special_instructions 'No special instructions were received'