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_7221800
_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         'C6 H6 F18 La1 N3 O15 S6, 2.5(H2 O)'
_chemical_formula_sum            'C6 H11 F18 La N3 O17.5 S6'
_chemical_formula_weight         1078.45
_chemical_name_systematic
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-lanthanum(iii)hemi(pentahydrate)
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.5598(15)
_cell_length_b                   15.5598(15)
_cell_length_c                   8.2562(9)
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0182
_cell_measurement_theta_min      2.8878
_cell_volume                     1731.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
  1 omega  -91.00  -59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3076  178.0000  -90.0000 32

  2 omega  -93.00  -65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3076 -178.0000   30.0000 28

  3 omega  -28.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1826    0.0000  -60.0000 104

  4 omega  -22.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1826   19.0000  120.0000 91
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0134937000
_diffrn_orient_matrix_UB_12      -0.0507745000
_diffrn_orient_matrix_UB_13      -0.0043458000
_diffrn_orient_matrix_UB_21      -0.0357753000
_diffrn_orient_matrix_UB_22      -0.0079922000
_diffrn_orient_matrix_UB_23      -0.0601693000
_diffrn_orient_matrix_UB_31      0.0362829000
_diffrn_orient_matrix_UB_32      0.0114345000
_diffrn_orient_matrix_UB_33      -0.0609305000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8585
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    2.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.106
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2737
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0950
_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^)+(0.0407P)^2^+51.1317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                2570
_reflns_number_total             2737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01270h2.cif
_cod_data_source_block           nrb96-b-sample
_cod_depositor_comments
'Adding full bibliography for 7221799--7221808.cif.'
_cod_original_formula_sum        'C6 H11 F18 La N3 O17.50 S6'
_cod_database_code               7221800
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9750(17) 0.0250(17)
2. Uiso/Uaniso restraints and constraints
O18 \\sim O17 \\sim O19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
;
_olex2_date_sample_data_collection 2012-10-29
_olex2_submission_special_instructions 'No special instructions were received'