#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/18/7221800.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7221800
loop_
_publ_author_name
'Vander Hoogerstraete, Tom'
'Brooks, Neil R.'
'Onghena, Bieke'
'Van Meervelt, Luc'
'Binnemans, Koen'
_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       'ω 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/[σ²(Fo²)+(0.0407P)²+51.1317P] where P=(Fo²+2Fc²)/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
#BEGIN Tags that were not found in dictionaries:
_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'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 '-x, -y, -z'
5 'y, -x+y, -z'
6 'x-y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
La1 La 0.6667 0.3333 0.42369(10) 0.0184(3) Uani 1 d . . 3 S T P
S10 S 0.92882(19) 0.5465(2) 0.3260(3) 0.0248(6) Uani 1 d . . 1 . . .
S6 S 0.7914(2) 0.5158(2) 0.0826(3) 0.0253(6) Uani 1 d . . 1 . . .
O8 O 0.7118(5) 0.4629(6) 0.1996(8) 0.0251(15) Uani 1 d . . 1 . . .
F14 F 0.8595(7) 0.6514(7) 0.4582(9) 0.051(2) Uani 1 d . . 1 . . .
O1 O 0.6845(5) 0.4536(6) 0.6403(7) 0.0235(15) Uani 1 d . . 1 . . .
O11 O 0.8511(5) 0.4630(6) 0.4119(8) 0.0234(15) Uani 1 d . . 1 . . .
O7 O 0.7833(7) 0.4679(7) -0.0700(9) 0.0354(19) Uani 1 d . . 1 . . .
F4 F 0.7920(8) 0.6786(7) 0.1592(10) 0.060(2) Uani 1 d . . 1 . . .
F15 F 1.0108(7) 0.7367(6) 0.3707(11) 0.057(2) Uani 1 d . . 1 . . .
F3 F 0.8516(8) 0.6808(7) -0.0760(11) 0.066(3) Uani 1 d . . 1 . . .
O12 O 1.0243(6) 0.5548(7) 0.3216(9) 0.0339(19) Uani 1 d . . 1 . . .
N9 N 0.8988(7) 0.5621(8) 0.1522(10) 0.030(2) Uani 1 d . . 1 . . .
F5 F 0.6946(7) 0.5949(8) -0.0339(12) 0.062(3) Uani 1 d . . 1 . . .
F16 F 0.9811(9) 0.6505(7) 0.5869(10) 0.067(3) Uani 1 d . . 1 . . .
C13 C 0.9450(11) 0.6536(10) 0.4450(14) 0.040(3) Uani 1 d . . 1 . . .
C2 C 0.7818(10) 0.6256(11) 0.0317(14) 0.040(3) Uani 1 d . . 1 . . .
O17 O 1.006(2) 0.9701(17) 0.328(2) 0.043(6) Uiso 0.43(3) d A -1 1 . U .
O18 O 0.881(4) 0.877(4) 0.339(6) 0.056(9) Uiso 0.23(3) d B -2 1 . U .
O19 O 0.922(5) 0.916(5) 0.233(8) 0.052(9) Uiso 0.18(3) d C -3 1 . U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 -1 0 0.0600 1.9998 -1.0000 -0.0000 0.0238 -0.0636 0.0611
-2 1 0 0.0600 -1.9998 1.0000 0.0000 -0.0238 0.0636 -0.0611
0 0 1 0.1820 -0.0000 -0.0001 1.0000 -0.0043 -0.0602 -0.0609
0 0 -1 0.1820 0.0000 0.0001 -1.0000 0.0043 0.0602 0.0609
0 -1 0 0.0639 -0.0000 -0.9998 -0.0000 0.0508 0.0080 -0.0114
0 1 0 0.0639 0.0000 0.9998 0.0000 -0.0508 -0.0080 0.0114
1 1 0 0.0532 0.9999 0.9997 0.0000 -0.0643 -0.0438 0.0477
-1 -1 0 0.0532 -0.9999 -0.9997 -0.0000 0.0643 0.0438 -0.0477
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O8 La1 O8 73.6(3) 3_665 .
O8 La1 O8 73.6(3) 3_665 2_655
O8 La1 O8 73.6(3) 2_655 .
O1 La1 O8 92.5(2) 3_665 3_665
O1 La1 O8 147.2(2) . 3_665
O1 La1 O8 131.6(2) . 2_655
O1 La1 O8 92.5(2) . .
O1 La1 O8 147.2(2) 2_655 .
O1 La1 O8 131.6(2) 3_665 .
O1 La1 O8 147.2(2) 3_665 2_655
O1 La1 O8 92.5(2) 2_655 2_655
O1 La1 O8 131.6(2) 2_655 3_665
O1 La1 O1 74.5(3) 3_665 2_655
O1 La1 O1 74.5(3) 3_665 .
O1 La1 O1 74.5(3) 2_655 .
O1 La1 O11 65.7(2) 3_665 .
O1 La1 O11 77.0(2) 2_655 2_655
O1 La1 O11 77.0(2) . .
O1 La1 O11 135.8(2) 2_655 .
O1 La1 O11 77.0(2) 3_665 3_665
O1 La1 O11 135.8(2) 3_665 2_655
O1 La1 O11 65.7(2) 2_655 3_665
O1 La1 O11 65.7(2) . 2_655
O1 La1 O11 135.8(2) . 3_665
O11 La1 O8 70.2(2) . 3_665
O11 La1 O8 131.5(2) 2_655 3_665
O11 La1 O8 66.0(2) 2_655 2_655
O11 La1 O8 66.0(2) . .
O11 La1 O8 70.2(2) 2_655 .
O11 La1 O8 70.2(2) 3_665 2_655
O11 La1 O8 131.5(2) . 2_655
O11 La1 O8 66.0(2) 3_665 3_665
O11 La1 O8 131.5(2) 3_665 .
O11 La1 O11 119.86(2) . 2_655
O11 La1 O11 119.86(2) 3_665 2_655
O11 La1 O11 119.86(2) 3_665 .
O11 S10 N9 114.2(5) . .
O11 S10 C13 103.1(5) . .
O12 S10 O11 117.4(5) . .
O12 S10 N9 109.9(5) . .
O12 S10 C13 105.5(6) . .
N9 S10 C13 105.4(6) . .
O8 S6 N9 115.3(4) . .
O8 S6 C2 103.6(5) . .
O7 S6 O8 117.3(5) . .
O7 S6 N9 110.9(5) . .
O7 S6 C2 104.8(5) . .
N9 S6 C2 102.8(6) . .
S6 O8 La1 138.1(4) . .
S10 O11 La1 146.6(4) . .
S6 N9 S10 126.8(6) . .
F14 C13 S10 110.0(9) . .
F14 C13 F15 109.8(11) . .
F15 C13 S10 108.9(9) . .
F16 C13 S10 108.1(10) . .
F16 C13 F14 111.8(11) . .
F16 C13 F15 108.2(11) . .
F4 C2 S6 111.4(8) . .
F4 C2 F3 109.4(12) . .
F4 C2 F5 110.0(12) . .
F3 C2 S6 109.4(9) . .
F5 C2 S6 107.8(10) . .
F5 C2 F3 108.7(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O8 2.562(7) 2_655
La1 O8 2.563(7) .
La1 O8 2.562(7) 3_665
La1 O1 2.501(7) 2_655
La1 O1 2.501(7) 3_665
La1 O1 2.501(7) .
La1 O11 2.555(7) .
La1 O11 2.555(7) 3_665
La1 O11 2.555(7) 2_655
S10 O11 1.443(7) .
S10 O12 1.426(8) .
S10 N9 1.565(9) .
S10 C13 1.840(13) .
S6 O8 1.458(7) .
S6 O7 1.438(8) .
S6 N9 1.562(9) .
S6 C2 1.836(14) .
F14 C13 1.318(17) .
F4 C2 1.298(16) .
F15 C13 1.331(15) .
F3 C2 1.332(15) .
F5 C2 1.309(16) .
F16 C13 1.311(14) .
#BEGIN Loops that were not found in dictionaries:
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9750(17)
2 0.0250(17)
#END Loops that were not found in dictionaries
