#------------------------------------------------------------------------------
#$Date: 2015-12-09 14:58:19 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171069 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/18/7221806.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_7221806
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_absolute_configuration ad
_chemical_formula_moiety         'C6 H6 Ce1 F18 N3 O15 S6'
_chemical_formula_sum            'C6 H6 Ce F18 N3 O15 S6'
_chemical_formula_weight         1034.62
_chemical_name_systematic
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-cerium(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                   18.51715(13)
_cell_length_b                   18.51715(13)
_cell_length_c                   18.51715(13)
_cell_measurement_reflns_used    5496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5090
_cell_measurement_theta_min      3.4670
_cell_volume                     6349.25(8)
_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 0.862
_diffrn_measurement_details
;
  1 omega  -57.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   19.0000 -180.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0145512000
_diffrn_orient_matrix_UB_12      0.0338456000
_diffrn_orient_matrix_UB_13      0.0105851000
_diffrn_orient_matrix_UB_21      -0.0054935000
_diffrn_orient_matrix_UB_22      -0.0091318000
_diffrn_orient_matrix_UB_23      0.0367771000
_diffrn_orient_matrix_UB_31      0.0349927000
_diffrn_orient_matrix_UB_32      -0.0154914000
_diffrn_orient_matrix_UB_33      0.0013867000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9870
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86310
_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    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0241P)²+14.5785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                4510
_reflns_number_total             4839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01270h2.cif
_cod_data_source_block           nrb171
_cod_depositor_comments
'Adding full bibliography for 7221799--7221808.cif.'
_cod_original_cell_volume        6349.25(7)
_cod_database_code               7221806
_chemical_oxdiff_formula         'Ce C6 F18 S6 O12 N3 O8 H16'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 O1-H1A = O1-H1B
 0.84 with sigma of 0.01
 H1A-H1B
 1.35 with sigma of 0.02
 O17-H17A = O17-H17B
 0.84 with sigma of 0.01
 H17A-H17B
 1.35 with sigma of 0.02
;
_olex2_date_sample_data_collection 2013-06-28
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'z, x, y'
3 'y, z, x'
4 '-y+1/2, -z, x+1/2'
5 'z+1/2, -x+1/2, -y'
6 '-y, z+1/2, -x+1/2'
7 '-z+1/2, -x, y+1/2'
8 '-z, x+1/2, -y+1/2'
9 'y+1/2, -z+1/2, -x'
10 '-x+1/2, -y, z+1/2'
11 'x+1/2, -y+1/2, -z'
12 '-x, y+1/2, -z+1/2'
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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ce1 Ce 0.484058(12) 0.984058(12) 0.515942(12) 0.01630(9) Uani 1 d 3 S T P
O1 O 0.47178(19) 1.10332(17) 0.45942(17) 0.0261(7) Uani 1 d 1 D . .
C2 C 0.4125(4) 0.7252(3) 0.4729(3) 0.059(2) Uani 1 d 1 . . .
F3 F 0.4279(4) 0.7423(2) 0.4071(2) 0.107(2) Uani 1 d 1 . . .
F4 F 0.4337(3) 0.65661(18) 0.4868(3) 0.0784(14) Uani 1 d 1 . . .
F5 F 0.3422(2) 0.7309(2) 0.4836(2) 0.0670(11) Uani 1 d 1 . . .
S6 S 0.45746(7) 0.78496(7) 0.53621(8) 0.0355(3) Uani 1 d 1 . . .
O7 O 0.43668(17) 0.85654(16) 0.51309(18) 0.0255(7) Uani 1 d 1 . . .
O8 O 0.4341(3) 0.7623(3) 0.6043(2) 0.0614(13) Uani 1 d 1 . . .
N9 N 0.5378(3) 0.7660(3) 0.5170(5) 0.090(3) Uani 1 d 1 . . .
S10 S 0.60206(7) 0.81788(7) 0.51618(9) 0.0402(3) Uani 1 d 1 . . .
O11 O 0.6461(3) 0.8021(3) 0.4557(3) 0.0787(18) Uani 1 d 1 . . .
O12 O 0.58401(18) 0.89169(18) 0.52775(19) 0.0329(8) Uani 1 d 1 . . .
C13 C 0.6584(5) 0.7942(4) 0.5950(5) 0.068(2) Uani 1 d 1 . . .
F14 F 0.6733(3) 0.7256(3) 0.5932(3) 0.1020(19) Uani 1 d 1 . . .
F15 F 0.7164(3) 0.8327(3) 0.5950(4) 0.1034(19) Uani 1 d 1 . . .
F16 F 0.6190(4) 0.8063(4) 0.6541(3) 0.136(3) Uani 1 d 1 . . .
Ce2 Ce 0.230988(13) 0.730988(13) 0.769012(13) 0.01877(9) Uani 1 d 3 S T P
O17 O 0.35641(16) 0.7266(2) 0.72629(19) 0.0295(7) Uani 1 d 1 D . .
C18 C 0.3246(3) 0.5508(3) 0.6061(3) 0.0288(10) Uani 1 d 1 . . .
F19 F 0.30813(19) 0.58222(19) 0.54467(17) 0.0476(8) Uani 1 d 1 . . .
F20 F 0.37878(16) 0.58484(18) 0.63749(18) 0.0416(8) Uani 1 d 1 . . .
F21 F 0.34351(16) 0.48322(17) 0.59357(16) 0.0367(7) Uani 1 d 1 . . .
S22 S 0.24389(6) 0.55357(6) 0.66378(6) 0.0221(2) Uani 1 d 1 . . .
O23 O 0.23188(18) 0.62930(16) 0.67638(16) 0.0248(6) Uani 1 d 1 . . .
O24 O 0.19004(18) 0.51605(19) 0.62364(18) 0.0309(7) Uani 1 d 1 . . .
N25 N 0.2714(2) 0.5109(2) 0.7309(2) 0.0250(7) Uani 1 d 1 . . .
S26 S 0.25558(6) 0.53099(6) 0.81123(6) 0.0227(2) Uani 1 d 1 . . .
O27 O 0.24171(17) 0.60701(16) 0.82373(16) 0.0239(7) Uani 1 d 1 . . .
O28 O 0.30605(18) 0.49697(17) 0.85824(17) 0.0293(8) Uani 1 d 1 . . .
C29 C 0.1686(3) 0.4876(3) 0.8301(3) 0.0316(10) Uani 1 d 1 . . .
F30 F 0.11971(14) 0.51137(16) 0.78307(17) 0.0361(7) Uani 1 d 1 . . .
F31 F 0.14710(18) 0.5039(2) 0.89610(17) 0.0492(9) Uani 1 d 1 . . .
F32 F 0.17431(18) 0.41721(16) 0.8235(2) 0.0457(8) Uani 1 d 1 . . .
H1A H 0.473(3) 1.111(3) 0.4145(7) 0.034(15) Uiso 1 d 1 D . .
H1B H 0.444(3) 1.135(3) 0.477(2) 0.06(2) Uiso 1 d 1 D . .
H17A H 0.387(2) 0.708(3) 0.754(2) 0.037(16) Uiso 1 d 1 D . .
H17B H 0.380(2) 0.743(3) 0.691(2) 0.06(2) Uiso 1 d 1 D . .
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'
Ce Ce -0.2486 2.6331 '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'
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_
_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
O1 Ce1 O1 74.88(13) 8_656 9_466
O1 Ce1 O1 74.88(12) 8_656 .
O1 Ce1 O1 74.88(12) 9_466 .
O1 Ce1 O7 143.33(11) 9_466 9_466
O1 Ce1 O7 143.33(11) 8_656 8_656
O1 Ce1 O7 92.45(11) 9_466 8_656
O1 Ce1 O7 92.45(11) 8_656 .
O1 Ce1 O7 135.63(11) 8_656 9_466
O1 Ce1 O7 143.33(11) . .
O1 Ce1 O7 135.63(10) . 8_656
O1 Ce1 O7 92.45(11) . 9_466
O1 Ce1 O7 135.63(10) 9_466 .
O1 Ce1 O12 67.79(11) 8_656 9_466
O1 Ce1 O12 72.73(11) . 9_466
O1 Ce1 O12 135.48(11) 8_656 8_656
O1 Ce1 O12 72.73(11) 9_466 8_656
O1 Ce1 O12 67.79(11) 9_466 .
O1 Ce1 O12 72.73(11) 8_656 .
O1 Ce1 O12 135.48(11) . .
O1 Ce1 O12 67.79(11) . 8_656
O1 Ce1 O12 135.48(11) 9_466 9_466
O7 Ce1 O7 72.58(12) . 9_466
O7 Ce1 O7 72.58(12) . 8_656
O7 Ce1 O7 72.58(12) 9_466 8_656
O7 Ce1 O12 132.05(11) 8_656 9_466
O7 Ce1 O12 67.84(11) 9_466 9_466
O7 Ce1 O12 132.05(11) 9_466 .
O7 Ce1 O12 132.05(11) . 8_656
O7 Ce1 O12 70.62(11) . 9_466
O7 Ce1 O12 67.84(11) 8_656 8_656
O7 Ce1 O12 70.62(11) 8_656 .
O7 Ce1 O12 67.84(11) . .
O7 Ce1 O12 70.62(11) 9_466 8_656
O12 Ce1 O12 119.969(5) 9_466 .
O12 Ce1 O12 119.968(4) 9_466 8_656
O12 Ce1 O12 119.968(4) 8_656 .
F3 C2 F4 110.3(5) . .
F3 C2 F5 109.8(7) . .
F3 C2 S6 111.0(4) . .
F4 C2 S6 108.5(6) . .
F5 C2 F4 109.4(5) . .
F5 C2 S6 107.8(4) . .
O7 S6 C2 104.3(3) . .
O7 S6 N9 113.0(3) . .
O8 S6 C2 104.9(3) . .
O8 S6 O7 117.4(3) . .
O8 S6 N9 115.5(4) . .
N9 S6 C2 98.7(4) . .
S6 O7 Ce1 139.5(2) . .
S10 N9 S6 126.8(4) . .
N9 S10 C13 106.4(4) . .
O11 S10 N9 109.0(4) . .
O11 S10 O12 116.9(3) . .
O11 S10 C13 104.5(4) . .
O12 S10 N9 114.8(3) . .
O12 S10 C13 104.0(3) . .
S10 O12 Ce1 143.9(2) . .
F14 C13 S10 109.4(7) . .
F14 C13 F16 107.5(7) . .
F15 C13 S10 109.9(5) . .
F15 C13 F14 111.3(6) . .
F15 C13 F16 111.3(9) . .
F16 C13 S10 107.4(5) . .
O17 Ce2 O17 74.74(13) 8_656 9_466
O17 Ce2 O17 74.75(13) 8_656 .
O17 Ce2 O17 74.75(13) 9_466 .
O17 Ce2 O23 75.67(11) . .
O17 Ce2 O23 75.67(11) 9_466 9_466
O17 Ce2 O23 136.01(11) 9_466 8_656
O17 Ce2 O23 66.50(11) 8_656 9_466
O17 Ce2 O23 66.50(11) 9_466 .
O17 Ce2 O23 136.01(11) 8_656 .
O17 Ce2 O23 66.50(11) . 8_656
O17 Ce2 O23 75.67(11) 8_656 8_656
O17 Ce2 O23 136.01(11) . 9_466
O17 Ce2 O27 91.43(11) . .
O17 Ce2 O27 91.43(11) 9_466 9_466
O17 Ce2 O27 91.43(11) 8_656 8_656
O17 Ce2 O27 145.50(11) 8_656 .
O17 Ce2 O27 145.50(11) . 9_466
O17 Ce2 O27 132.64(10) 9_466 .
O17 Ce2 O27 132.63(10) . 8_656
O17 Ce2 O27 145.50(11) 9_466 8_656
O17 Ce2 O27 132.64(10) 8_656 9_466
O23 Ce2 O23 119.883(9) . 8_656
O23 Ce2 O23 119.885(9) . 9_466
O23 Ce2 O23 119.884(9) 8_656 9_466
O27 Ce2 O23 69.83(11) 9_466 .
O27 Ce2 O23 132.46(10) . 9_466
O27 Ce2 O23 69.83(11) . 8_656
O27 Ce2 O23 69.83(11) 8_656 9_466
O27 Ce2 O23 132.46(10) 8_656 .
O27 Ce2 O23 132.46(10) 9_466 8_656
O27 Ce2 O23 66.20(10) 9_466 9_466
O27 Ce2 O23 66.20(10) 8_656 8_656
O27 Ce2 O23 66.20(10) . .
O27 Ce2 O27 74.73(11) 9_466 8_656
O27 Ce2 O27 74.73(11) . 8_656
O27 Ce2 O27 74.73(11) . 9_466
F19 C18 F20 110.3(4) . .
F19 C18 F21 109.2(4) . .
F19 C18 S22 107.6(3) . .
F20 C18 F21 109.2(4) . .
F20 C18 S22 110.5(3) . .
F21 C18 S22 110.1(3) . .
O23 S22 C18 104.3(2) . .
O23 S22 N25 114.6(2) . .
O24 S22 C18 104.6(2) . .
O24 S22 O23 116.8(2) . .
O24 S22 N25 113.4(2) . .
N25 S22 C18 100.5(2) . .
S22 O23 Ce2 146.16(19) . .
S22 N25 S26 125.3(2) . .
N25 S26 C29 104.0(2) . .
O27 S26 N25 114.63(19) . .
O27 S26 C29 103.9(2) . .
O28 S26 N25 110.72(19) . .
O28 S26 O27 116.62(19) . .
O28 S26 C29 105.4(2) . .
S26 O27 Ce2 146.65(19) . .
F30 C29 S26 109.2(3) . .
F31 C29 S26 109.9(4) . .
F31 C29 F30 108.9(4) . .
F32 C29 S26 110.3(3) . .
F32 C29 F30 108.8(4) . .
F32 C29 F31 109.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O1 2.454(3) 8_656
Ce1 O1 2.454(3) 9_466
Ce1 O1 2.454(3) .
Ce1 O7 2.519(3) .
Ce1 O7 2.520(3) 8_656
Ce1 O7 2.520(3) 9_466
Ce1 O12 2.529(3) 9_466
Ce1 O12 2.530(3) .
Ce1 O12 2.529(3) 8_656
C2 F3 1.291(7) .
C2 F4 1.354(8) .
C2 F5 1.322(8) .
C2 S6 1.814(7) .
S6 O7 1.445(3) .
S6 O8 1.398(4) .
S6 N9 1.570(6) .
N9 S10 1.529(6) .
S10 O11 1.416(5) .
S10 O12 1.423(4) .
S10 C13 1.846(8) .
C13 F14 1.301(8) .
C13 F15 1.288(9) .
C13 F16 1.334(9) .
Ce2 O17 2.455(3) 8_656
Ce2 O17 2.455(3) 9_466
Ce2 O17 2.455(3) .
Ce2 O23 2.547(3) 8_656
Ce2 O23 2.547(3) .
Ce2 O23 2.547(3) 9_466
Ce2 O27 2.517(3) 9_466
Ce2 O27 2.517(3) .
Ce2 O27 2.517(3) 8_656
C18 F19 1.314(6) .
C18 F20 1.319(5) .
C18 F21 1.321(5) .
C18 S22 1.837(5) .
S22 O23 1.439(3) .
S22 O24 1.425(3) .
S22 N25 1.558(4) .
N25 S26 1.562(4) .
S26 O27 1.450(3) .
S26 O28 1.424(3) .
S26 C29 1.833(5) .
C29 F30 1.331(5) .
C29 F31 1.321(6) .
C29 F32 1.313(6) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O24 0.843(10) 1.962(12) 2.802(5) 175(5) 6_655
O1 H1B O28 0.835(10) 2.00(2) 2.809(4) 164(6) 5_466
O17 H17A O11 0.840(10) 1.929(17) 2.752(5) 166(5) 2
O17 H17B O8 0.841(10) 1.929(17) 2.758(5) 169(6) .
