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_7221804
_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_absolute_configuration ad
_chemical_formula_moiety         'C6 H6 F18 Gd1 N3 O15 S6'
_chemical_formula_sum            'C6 H6 F18 Gd N3 O15 S6'
_chemical_formula_weight         1051.75
_chemical_name_systematic
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-gadolinium(iii) 
;
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3973(2)
_cell_length_b                   18.3973(2)
_cell_length_c                   18.3973(2)
_cell_measurement_reflns_used    24463
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1040
_cell_measurement_theta_min      3.1330
_cell_volume                     6226.76(12)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -89.00  -63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000   90.0000 26

  2 omega  -45.00   -9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000  -90.0000 36

  3 omega  -47.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000 -120.0000 99

  4 omega  -42.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000   90.0000 50

  5 omega  -41.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -57.0000    0.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0365377000
_diffrn_orient_matrix_UB_12      0.0068689000
_diffrn_orient_matrix_UB_13      -0.0102006000
_diffrn_orient_matrix_UB_21      0.0042986000
_diffrn_orient_matrix_UB_22      0.0370792000
_diffrn_orient_matrix_UB_23      0.0096620000
_diffrn_orient_matrix_UB_31      0.0115897000
_diffrn_orient_matrix_UB_32      0.0079910000
_diffrn_orient_matrix_UB_33      -0.0358924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35933
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58907
_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    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5163
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+5.7232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0403
_reflns_number_gt                5004
_reflns_number_total             5163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01270h2.cif
_cod_data_source_block           nrb167
_cod_depositor_comments
'Adding full bibliography for 7221799--7221808.cif.'
_cod_original_cell_volume        6226.75(12)
_cod_database_code               7221804
_chemical_oxdiff_formula         'Gd C6 F18 S6 O12 N3 O8 H16'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 O17-H17A = O17-H17B
 0.84 with sigma of 0.01
 H17A-H17B
 1.35 with sigma of 0.02
 O1-H1A = O1-H1B
 0.84 with sigma of 0.01
 H1A-H1B
 1.35 with sigma of 0.02
;
_olex2_date_sample_data_collection 2013-06-20
_olex2_submission_special_instructions 'No special instructions were received'