# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb85
_database_code_depnum_ccdc_archive 'CCDC 1409124'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-praseodymium(iii) 
;
_chemical_formula_moiety         'C6 H6 F18 N3 O15 Pr1 S6'
_chemical_formula_sum            'C6 H6 F18 N3 O15 Pr S6'
_chemical_formula_weight         1035.41
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pr O8 H16 C6 F18 S6 O12 N3'
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'
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'
Pr Pr -0.2180 2.8214 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'
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'

_cell_length_a                   18.53745(8)
_cell_length_b                   18.53745(8)
_cell_length_c                   18.53745(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6370.16(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    26264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0702
_cell_measurement_theta_min      3.1019
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87643
_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    2.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35367
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.11
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -13.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701 -102.0000   70.0000 72

#__ type_ start__ end____ width___ exp.time_
  2 omega    7.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -99.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
  3 omega    4.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000 -180.0000 62

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000 -120.0000 47

#__ type_ start__ end____ width___ exp.time_
  5 omega  -49.00   -4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -38.0000  120.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0320897000
_diffrn_orient_matrix_UB_12      0.0208049000
_diffrn_orient_matrix_UB_13      -0.0020764000
_diffrn_orient_matrix_UB_21      0.0173262000
_diffrn_orient_matrix_UB_22      -0.0285897000
_diffrn_orient_matrix_UB_23      -0.0185704000
_diffrn_orient_matrix_UB_31      -0.0116988000
_diffrn_orient_matrix_UB_32      0.0146301000
_diffrn_orient_matrix_UB_33      -0.0333462000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                5127
_reflns_number_total             5355
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.791
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00033(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5355
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.185
_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)+(0.0241P)²+60.4562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1244
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Pr1 Pr 0.48395(2) 0.98395(2) 0.51605(2) 0.01573(14) Uani 1 d . . 3 S T P
O1 O 0.4712(3) 1.1026(3) 0.4592(3) 0.0263(12) Uani 1 d . . 1 . . .
C2 C 0.4122(7) 0.7252(5) 0.4737(6) 0.053(3) Uani 1 d . . 1 . . .
F3 F 0.4295(7) 0.7420(4) 0.4074(4) 0.104(4) Uani 1 d . . 1 . . .
F4 F 0.4345(4) 0.6570(3) 0.4880(5) 0.068(2) Uani 1 d . . 1 . . .
F5 F 0.3437(4) 0.7313(4) 0.4824(5) 0.068(2) Uani 1 d . . 1 . . .
S6 S 0.45703(13) 0.78550(11) 0.53725(13) 0.0323(5) Uani 1 d . . 1 . . .
O7 O 0.4367(3) 0.8570(3) 0.5125(3) 0.0256(11) Uani 1 d . . 1 . . .
O8 O 0.4308(6) 0.7635(5) 0.6039(4) 0.064(2) Uani 1 d . . 1 . . .
N9 N 0.5372(5) 0.7669(5) 0.5191(10) 0.088(5) Uani 1 d . . 1 . . .
S10 S 0.60172(12) 0.81836(12) 0.51681(15) 0.0364(5) Uani 1 d . . 1 . . .
O11 O 0.6432(6) 0.8019(5) 0.4550(5) 0.072(3) Uani 1 d . . 1 . . .
O12 O 0.5843(3) 0.8926(3) 0.5270(4) 0.0314(14) Uani 1 d . . 1 . . .
C13 C 0.6595(8) 0.7953(7) 0.5949(7) 0.058(3) Uani 1 d . . 1 . . .
F14 F 0.6746(5) 0.7258(5) 0.5925(6) 0.099(3) Uani 1 d . . 1 . . .
F15 F 0.7177(5) 0.8337(5) 0.5927(6) 0.095(3) Uani 1 d . . 1 . . .
F16 F 0.6207(7) 0.8090(6) 0.6545(5) 0.122(5) Uani 1 d . . 1 . . .
Pr2 Pr 0.23033(2) 0.73033(2) 0.76967(2) 0.01816(15) Uani 1 d . . 3 S T P
O17 O 0.3547(3) 0.7250(3) 0.7273(3) 0.0304(12) Uani 1 d . . 1 . . .
C18 C 0.3239(5) 0.5513(5) 0.6061(4) 0.0286(17) Uani 1 d . . 1 . . .
F19 F 0.3078(4) 0.5834(4) 0.5445(3) 0.0503(16) Uani 1 d . . 1 . . .
F20 F 0.3790(3) 0.5859(3) 0.6382(3) 0.0400(13) Uani 1 d . . 1 . . .
F21 F 0.3433(3) 0.4843(3) 0.5931(3) 0.0347(11) Uani 1 d . . 1 . . .
S22 S 0.24318(10) 0.55380(10) 0.66397(10) 0.0217(4) Uani 1 d . . 1 . . .
O23 O 0.2318(3) 0.6292(3) 0.6766(3) 0.0257(11) Uani 1 d . . 1 . . .
O24 O 0.1892(3) 0.5165(4) 0.6240(3) 0.0312(13) Uani 1 d . . 1 . . .
N25 N 0.2712(4) 0.5103(4) 0.7317(4) 0.0274(13) Uani 1 d . . 1 . . .
S26 S 0.25490(10) 0.53084(10) 0.81173(10) 0.0225(4) Uani 1 d . . 1 . . .
O27 O 0.2415(3) 0.6069(3) 0.8235(3) 0.0245(11) Uani 1 d . . 1 . . .
O28 O 0.3050(3) 0.4972(3) 0.8585(3) 0.0275(13) Uani 1 d . . 1 . . .
C29 C 0.1686(5) 0.4877(5) 0.8299(5) 0.0314(18) Uani 1 d . . 1 . . .
F30 F 0.1194(3) 0.5117(3) 0.7829(3) 0.0355(11) Uani 1 d . . 1 . . .
F31 F 0.1459(3) 0.5042(4) 0.8964(3) 0.0486(16) Uani 1 d . . 1 . . .
F32 F 0.1738(3) 0.4171(3) 0.8244(4) 0.0438(14) Uani 1 d . . 1 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O1 2.451(5) 9_466 ?
Pr1 O1 2.451(5) 8_656 ?
Pr1 O1 2.451(5) . ?
Pr1 O7 2.512(5) 9_466 ?
Pr1 O7 2.512(5) . ?
Pr1 O7 2.512(5) 8_656 ?
Pr1 O12 2.524(6) 9_466 ?
Pr1 O12 2.524(6) . ?
Pr1 O12 2.524(6) 8_656 ?
C2 F3 1.308(12) . ?
C2 F4 1.357(13) . ?
C2 F5 1.285(14) . ?
C2 S6 1.824(12) . ?
S6 O7 1.452(6) . ?
S6 O8 1.389(8) . ?
S6 N9 1.562(10) . ?
N9 S10 1.531(10) . ?
S10 O11 1.413(9) . ?
S10 O12 1.426(6) . ?
S10 C13 1.851(12) . ?
C13 F14 1.319(14) . ?
C13 F15 1.293(16) . ?
C13 F16 1.342(16) . ?
Pr2 O17 2.438(6) . ?
Pr2 O17 2.438(6) 8_656 ?
Pr2 O17 2.438(6) 9_466 ?
Pr2 O23 2.548(5) 8_656 ?
Pr2 O23 2.548(5) . ?
Pr2 O23 2.548(5) 9_466 ?
Pr2 O27 2.504(5) 8_656 ?
Pr2 O27 2.504(5) . ?
Pr2 O27 2.504(5) 9_466 ?
C18 F19 1.322(10) . ?
C18 F20 1.345(10) . ?
C18 F21 1.314(10) . ?
C18 S22 1.841(9) . ?
S22 O23 1.433(6) . ?
S22 O24 1.423(6) . ?
S22 N25 1.581(7) . ?
N25 S26 1.561(7) . ?
S26 O27 1.449(5) . ?
S26 O28 1.416(5) . ?
S26 C29 1.820(9) . ?
C29 F30 1.337(10) . ?
C29 F31 1.338(11) . ?
C29 F32 1.315(10) . ?

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
_geom_angle_publ_flag
O1 Pr1 O1 75.0(2) 9_466 8_656 ?
O1 Pr1 O1 75.0(2) 9_466 . ?
O1 Pr1 O1 75.0(2) 8_656 . ?
O1 Pr1 O7 92.10(19) 9_466 8_656 ?
O1 Pr1 O7 142.8(2) . . ?
O1 Pr1 O7 135.93(18) . 8_656 ?
O1 Pr1 O7 142.8(2) 8_656 8_656 ?
O1 Pr1 O7 142.8(2) 9_466 9_466 ?
O1 Pr1 O7 92.10(19) 8_656 . ?
O1 Pr1 O7 135.93(18) 8_656 9_466 ?
O1 Pr1 O7 92.1(2) . 9_466 ?
O1 Pr1 O7 135.93(18) 9_466 . ?
O1 Pr1 O12 135.05(19) 9_466 9_466 ?
O1 Pr1 O12 135.05(19) 8_656 8_656 ?
O1 Pr1 O12 67.63(19) 9_466 . ?
O1 Pr1 O12 67.63(19) 8_656 9_466 ?
O1 Pr1 O12 67.63(19) . 8_656 ?
O1 Pr1 O12 72.0(2) . 9_466 ?
O1 Pr1 O12 72.0(2) 8_656 . ?
O1 Pr1 O12 72.0(2) 9_466 8_656 ?
O1 Pr1 O12 135.05(19) . . ?
O7 Pr1 O7 72.9(2) 9_466 8_656 ?
O7 Pr1 O7 72.9(2) 9_466 . ?
O7 Pr1 O7 72.9(2) 8_656 . ?
O7 Pr1 O12 68.30(19) 9_466 9_466 ?
O7 Pr1 O12 68.30(19) . . ?
O7 Pr1 O12 132.85(19) 9_466 . ?
O7 Pr1 O12 70.8(2) . 9_466 ?
O7 Pr1 O12 70.8(2) 9_466 8_656 ?
O7 Pr1 O12 70.8(2) 8_656 . ?
O7 Pr1 O12 68.30(19) 8_656 8_656 ?
O7 Pr1 O12 132.85(19) . 8_656 ?
O7 Pr1 O12 132.85(19) 8_656 9_466 ?
O12 Pr1 O12 119.993(4) 9_466 . ?
O12 Pr1 O12 119.993(4) 9_466 8_656 ?
O12 Pr1 O12 119.994(3) 8_656 . ?
F3 C2 F4 109.3(9) . . ?
F3 C2 S6 110.4(7) . . ?
F4 C2 S6 107.8(9) . . ?
F5 C2 F3 109.9(13) . . ?
F5 C2 F4 111.0(8) . . ?
F5 C2 S6 108.4(7) . . ?
O7 S6 C2 103.7(5) . . ?
O7 S6 N9 112.3(5) . . ?
O8 S6 C2 103.6(5) . . ?
O8 S6 O7 117.2(5) . . ?
O8 S6 N9 117.4(8) . . ?
N9 S6 C2 99.1(7) . . ?
S6 O7 Pr1 139.2(4) . . ?
S10 N9 S6 127.7(7) . . ?
N9 S10 C13 106.7(8) . . ?
O11 S10 N9 108.2(8) . . ?
O11 S10 O12 116.0(5) . . ?
O11 S10 C13 105.7(6) . . ?
O12 S10 N9 114.9(5) . . ?
O12 S10 C13 104.5(5) . . ?
S10 O12 Pr1 143.5(4) . . ?
F14 C13 S10 108.7(11) . . ?
F14 C13 F16 109.0(11) . . ?
F15 C13 S10 109.4(9) . . ?
F15 C13 F14 111.0(11) . . ?
F15 C13 F16 111.7(14) . . ?
F16 C13 S10 106.9(9) . . ?
O17 Pr2 O17 75.3(2) . 8_656 ?
O17 Pr2 O17 75.3(2) . 9_466 ?
O17 Pr2 O17 75.3(2) 8_656 9_466 ?
O17 Pr2 O23 136.1(2) 8_656 . ?
O17 Pr2 O23 136.1(2) 9_466 8_656 ?
O17 Pr2 O23 66.23(19) . 8_656 ?
O17 Pr2 O23 66.23(18) 9_466 . ?
O17 Pr2 O23 136.1(2) . 9_466 ?
O17 Pr2 O23 75.0(2) 8_656 8_656 ?
O17 Pr2 O23 75.0(2) 9_466 9_466 ?
O17 Pr2 O23 75.0(2) . . ?
O17 Pr2 O23 66.23(19) 8_656 9_466 ?
O17 Pr2 O27 132.41(18) 9_466 . ?
O17 Pr2 O27 90.8(2) . . ?
O17 Pr2 O27 145.21(19) 8_656 . ?
O17 Pr2 O27 145.21(19) . 9_466 ?
O17 Pr2 O27 90.8(2) 8_656 8_656 ?
O17 Pr2 O27 132.41(18) 8_656 9_466 ?
O17 Pr2 O27 90.8(2) 9_466 9_466 ?
O17 Pr2 O27 132.41(18) . 8_656 ?
O17 Pr2 O27 145.21(19) 9_466 8_656 ?
O23 Pr2 O23 119.923(13) . 8_656 ?
O23 Pr2 O23 119.925(13) . 9_466 ?
O23 Pr2 O23 119.924(13) 8_656 9_466 ?
O27 Pr2 O23 133.11(19) 8_656 . ?
O27 Pr2 O23 66.22(18) 9_466 9_466 ?
O27 Pr2 O23 66.22(18) 8_656 8_656 ?
O27 Pr2 O23 70.17(19) 9_466 . ?
O27 Pr2 O23 70.17(19) 8_656 9_466 ?
O27 Pr2 O23 70.17(19) . 8_656 ?
O27 Pr2 O23 133.10(19) 9_466 8_656 ?
O27 Pr2 O23 66.23(18) . . ?
O27 Pr2 O23 133.11(19) . 9_466 ?
O27 Pr2 O27 75.2(2) 9_466 8_656 ?
O27 Pr2 O27 75.2(2) . 8_656 ?
O27 Pr2 O27 75.2(2) . 9_466 ?
F19 C18 F20 109.8(7) . . ?
F19 C18 S22 108.0(6) . . ?
F20 C18 S22 110.3(6) . . ?
F21 C18 F19 109.2(7) . . ?
F21 C18 F20 108.9(7) . . ?
F21 C18 S22 110.7(6) . . ?
O23 S22 C18 103.9(4) . . ?
O23 S22 N25 114.6(3) . . ?
O24 S22 C18 104.8(4) . . ?
O24 S22 O23 117.1(4) . . ?
O24 S22 N25 113.4(4) . . ?
N25 S22 C18 100.5(4) . . ?
S22 O23 Pr2 146.1(3) . . ?
S26 N25 S22 124.5(4) . . ?
N25 S26 C29 103.8(4) . . ?
O27 S26 N25 114.5(4) . . ?
O27 S26 C29 104.4(4) . . ?
O28 S26 N25 110.3(4) . . ?
O28 S26 O27 116.7(3) . . ?
O28 S26 C29 105.7(4) . . ?
S26 O27 Pr2 147.5(3) . . ?
F30 C29 S26 109.4(6) . . ?
F30 C29 F31 108.0(8) . . ?
F31 C29 S26 110.2(6) . . ?
F32 C29 S26 111.0(6) . . ?
F32 C29 F30 109.4(7) . . ?
F32 C29 F31 108.8(8) . . ?


_olex2_date_sample_data_collection 2012-09-27
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb96-b-sample
_database_code_depnum_ccdc_archive 'CCDC 1409125'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-lanthanum(iii)hemi(pentahydrate)
_chemical_formula_moiety         'C6 H6 F18 La1 N3 O15 S6, 2.5(H2 O)'
_chemical_formula_sum            'C6 H11 F18 La N3 O17.50 S6'
_chemical_formula_weight         1078.45
_chemical_melting_point          ?
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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
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'

_cell_length_a                   15.5598(15)
_cell_length_b                   15.5598(15)
_cell_length_c                   8.2562(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1731.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0182
_cell_measurement_theta_min      2.8878
_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_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_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_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -91.00  -59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3076  178.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
  2 omega  -93.00  -65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3076 -178.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
  3 omega  -28.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1826    0.0000  -60.0000 104

#__ type_ start__ end____ width___ exp.time_
  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_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                2570
_reflns_number_total             2737
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         4.106
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.252
_refine_ls_extinction_coef       ?
_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_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0950
_refine_ls_restrained_S_all      1.187
_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
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
;
_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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) . ?

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
_geom_angle_publ_flag
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_
_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


_olex2_date_sample_data_collection 2012-10-29
_olex2_submission_special_instructions 'No special instructions were received'

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9750(17)
2 0.0250(17)

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb117
_database_code_depnum_ccdc_archive 'CCDC 1409126'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-neodinium(iii)
;
_chemical_formula_moiety         'C6 H6 F18 N3 Nd1 O15 S6'
_chemical_formula_sum            'C6 H6 F18 N3 Nd O15 S6'
_chemical_formula_weight         1038.74
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nd C6 F18 S6 O12 N3 O3 H6'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'
5 'z, x, y'
6 'y, z, x'
7 '-z+1/2, -x, y+1/2'
8 '-y, z+1/2, -x+1/2'
9 'z+1/2, -x+1/2, -y'
10 '-y+1/2, -z, x+1/2'
11 '-z, x+1/2, -y+1/2'
12 'y+1/2, -z+1/2, -x'

_cell_length_a                   18.4695(2)
_cell_length_b                   18.4695(2)
_cell_length_c                   18.4695(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6300.34(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8790
_cell_measurement_theta_min      3.1060
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    2.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17704
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         3.12
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9631
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.50   -5.50   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1510  132.0000  -15.0000 74

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.50  -17.50   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1510  132.0000  165.0000 62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0291617000
_diffrn_orient_matrix_UB_12      -0.0044835000
_diffrn_orient_matrix_UB_13      0.0246124000
_diffrn_orient_matrix_UB_21      -0.0244500000
_diffrn_orient_matrix_UB_22      -0.0028796000
_diffrn_orient_matrix_UB_23      -0.0294454000
_diffrn_orient_matrix_UB_31      0.0053503000
_diffrn_orient_matrix_UB_32      -0.0380281000
_diffrn_orient_matrix_UB_33      -0.0006341000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                4451
_reflns_number_total             4849
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(13)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.076
_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)+(0.0659P)²+1.7225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1099
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Nd1 Nd 0.484015(15) 0.984015(15) 0.515985(15) 0.01503(12) Uani 1 d . . 3 S T P
O1 O 0.4721(3) 1.1020(2) 0.4600(2) 0.0247(9) Uani 1 d . . 1 D . .
C2 C 0.4142(5) 0.7253(4) 0.4737(4) 0.045(2) Uani 1 d . . 1 . . .
F3 F 0.4320(5) 0.7419(3) 0.4078(3) 0.101(3) Uani 1 d . . 1 . . .
F4 F 0.4342(3) 0.6571(2) 0.4882(3) 0.0626(15) Uani 1 d . . 1 . . .
F5 F 0.3434(3) 0.7310(3) 0.4814(3) 0.0637(15) Uani 1 d . . 1 . . .
S6 S 0.45652(9) 0.78633(9) 0.53788(9) 0.0293(4) Uani 1 d . . 1 . . .
O7 O 0.4378(2) 0.8579(2) 0.5126(3) 0.0245(9) Uani 1 d . . 1 . . .
O8 O 0.4289(4) 0.7644(3) 0.6057(3) 0.0571(17) Uani 1 d . . 1 . . .
N9 N 0.5379(4) 0.7677(4) 0.5244(7) 0.089(4) Uani 1 d . . 1 . . .
S10 S 0.60141(9) 0.81871(9) 0.51719(11) 0.0317(4) Uani 1 d . . 1 . . .
O11 O 0.6436(4) 0.8021(4) 0.4557(4) 0.069(2) Uani 1 d . . 1 . . .
O12 O 0.5843(2) 0.8939(2) 0.5276(2) 0.0283(10) Uani 1 d . . 1 . . .
C13 C 0.6595(5) 0.7967(5) 0.5949(5) 0.056(2) Uani 1 d . . 1 . . .
F14 F 0.6758(3) 0.7272(3) 0.5931(4) 0.0783(19) Uani 1 d . . 1 . . .
F15 F 0.7186(3) 0.8346(3) 0.5902(4) 0.087(2) Uani 1 d . . 1 . . .
F16 F 0.6242(5) 0.8100(5) 0.6547(4) 0.120(3) Uani 1 d . . 1 . . .
Nd2 Nd 0.229748(16) 0.729748(16) 0.770252(16) 0.01698(13) Uani 1 d . . 3 S T P
O17 O 0.3535(2) 0.7245(2) 0.7279(2) 0.0264(9) Uani 1 d . . 1 D . .
C18 C 0.3233(4) 0.5516(4) 0.6066(4) 0.0278(13) Uani 1 d . . 1 . . .
F19 F 0.3082(3) 0.5841(3) 0.5450(2) 0.0449(11) Uani 1 d . . 1 . . .
F20 F 0.3785(2) 0.5862(2) 0.6385(2) 0.0386(10) Uani 1 d . . 1 . . .
F21 F 0.3431(2) 0.4841(2) 0.5938(2) 0.0331(9) Uani 1 d . . 1 . . .
S22 S 0.24296(8) 0.55393(8) 0.66430(8) 0.0204(3) Uani 1 d . . 1 . . .
O23 O 0.2305(2) 0.6299(2) 0.6772(2) 0.0240(9) Uani 1 d . . 1 . . .
O24 O 0.1893(2) 0.5160(3) 0.6237(3) 0.0296(10) Uani 1 d . . 1 . . .
N25 N 0.2703(3) 0.5107(3) 0.7316(3) 0.0251(10) Uani 1 d . . 1 . . .
S26 S 0.25463(8) 0.53087(7) 0.81195(8) 0.0206(3) Uani 1 d . . 1 . . .
O27 O 0.2408(2) 0.6070(2) 0.8240(2) 0.0205(8) Uani 1 d . . 1 . . .
O28 O 0.3049(2) 0.4972(2) 0.8591(2) 0.0278(10) Uani 1 d . . 1 . . .
C29 C 0.1675(4) 0.4878(4) 0.8305(3) 0.0300(14) Uani 1 d . . 1 . . .
F30 F 0.1182(2) 0.5108(2) 0.7834(2) 0.0336(9) Uani 1 d . . 1 . . .
F31 F 0.1456(2) 0.5040(3) 0.8970(2) 0.0447(11) Uani 1 d . . 1 . . .
F32 F 0.1732(2) 0.4166(2) 0.8247(3) 0.0428(11) Uani 1 d . . 1 . . .
H17A H 0.383(3) 0.704(5) 0.755(3) 0.07(3) Uiso 1 d . . 1 D . .
H17B H 0.375(3) 0.734(4) 0.689(2) 0.05(3) Uiso 1 d . . 1 D . .
H1A H 0.480(5) 1.110(4) 0.4158(14) 0.06(3) Uiso 1 d . . 1 D . .
H1B H 0.441(4) 1.132(4) 0.474(4) 0.06(3) Uiso 1 d . . 1 D . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O1 2.421(4) 12_466 ?
Nd1 O1 2.421(4) 11_656 ?
Nd1 O1 2.421(4) . ?
Nd1 O7 2.482(4) . ?
Nd1 O7 2.482(4) 11_656 ?
Nd1 O7 2.482(4) 12_466 ?
Nd1 O12 2.499(4) . ?
Nd1 O12 2.499(4) 11_656 ?
Nd1 O12 2.499(4) 12_466 ?
C2 F3 1.297(9) . ?
C2 F4 1.341(10) . ?
C2 F5 1.320(11) . ?
C2 S6 1.813(8) . ?
S6 O7 1.444(4) . ?
S6 O8 1.412(5) . ?
S6 N9 1.562(8) . ?
N9 S10 1.509(7) . ?
S10 O11 1.411(6) . ?
S10 O12 1.438(5) . ?
S10 C13 1.838(10) . ?
C13 F14 1.320(10) . ?
C13 F15 1.299(11) . ?
C13 F16 1.306(11) . ?
Nd2 O17 2.417(4) 11_656 ?
Nd2 O17 2.417(4) . ?
Nd2 O17 2.417(4) 12_466 ?
Nd2 O23 2.521(4) 12_466 ?
Nd2 O23 2.521(4) 11_656 ?
Nd2 O23 2.521(4) . ?
Nd2 O27 2.483(4) 11_656 ?
Nd2 O27 2.483(4) 12_466 ?
Nd2 O27 2.483(4) . ?
C18 F19 1.316(8) . ?
C18 F20 1.340(7) . ?
C18 F21 1.320(7) . ?
C18 S22 1.828(7) . ?
S22 O23 1.441(4) . ?
S22 O24 1.426(4) . ?
S22 N25 1.560(5) . ?
N25 S26 1.557(5) . ?
S26 O27 1.447(4) . ?
S26 O28 1.416(4) . ?
S26 C29 1.828(7) . ?
C29 F30 1.328(7) . ?
C29 F31 1.327(8) . ?
C29 F32 1.325(8) . ?

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
_geom_angle_publ_flag
O1 Nd1 O1 74.69(17) 12_466 11_656 ?
O1 Nd1 O1 74.69(17) 12_466 . ?
O1 Nd1 O1 74.69(17) 11_656 . ?
O1 Nd1 O7 143.36(15) 12_466 12_466 ?
O1 Nd1 O7 135.48(14) . 11_656 ?
O1 Nd1 O7 92.27(15) . 12_466 ?
O1 Nd1 O7 135.48(14) 11_656 12_466 ?
O1 Nd1 O7 135.48(14) 12_466 . ?
O1 Nd1 O7 143.36(15) 11_656 11_656 ?
O1 Nd1 O7 92.27(15) 11_656 . ?
O1 Nd1 O7 143.36(15) . . ?
O1 Nd1 O7 92.27(15) 12_466 11_656 ?
O1 Nd1 O12 67.04(15) 12_466 . ?
O1 Nd1 O12 67.04(15) 11_656 12_466 ?
O1 Nd1 O12 134.65(15) 11_656 11_656 ?
O1 Nd1 O12 72.55(15) 11_656 . ?
O1 Nd1 O12 72.55(15) . 12_466 ?
O1 Nd1 O12 134.65(15) . . ?
O1 Nd1 O12 67.04(15) . 11_656 ?
O1 Nd1 O12 134.65(15) 12_466 12_466 ?
O1 Nd1 O12 72.55(15) 12_466 11_656 ?
O7 Nd1 O7 73.07(16) . 12_466 ?
O7 Nd1 O7 73.07(16) . 11_656 ?
O7 Nd1 O7 73.07(16) 12_466 11_656 ?
O7 Nd1 O12 68.44(14) . . ?
O7 Nd1 O12 70.84(14) 11_656 . ?
O7 Nd1 O12 70.85(14) 12_466 11_656 ?
O7 Nd1 O12 133.06(14) 12_466 . ?
O7 Nd1 O12 70.85(14) . 12_466 ?
O7 Nd1 O12 68.44(14) 11_656 11_656 ?
O7 Nd1 O12 68.44(14) 12_466 12_466 ?
O7 Nd1 O12 133.06(14) 11_656 12_466 ?
O7 Nd1 O12 133.06(14) . 11_656 ?
O12 Nd1 O12 119.996(3) . 11_656 ?
O12 Nd1 O12 119.997(2) . 12_466 ?
O12 Nd1 O12 119.997(2) 12_466 11_656 ?
F3 C2 F4 109.8(7) . . ?
F3 C2 F5 109.5(9) . . ?
F3 C2 S6 110.9(5) . . ?
F4 C2 S6 109.6(6) . . ?
F5 C2 F4 109.1(6) . . ?
F5 C2 S6 107.9(5) . . ?
O7 S6 C2 104.7(4) . . ?
O7 S6 N9 112.4(4) . . ?
O8 S6 C2 104.2(4) . . ?
O8 S6 O7 117.5(3) . . ?
O8 S6 N9 115.3(6) . . ?
N9 S6 C2 100.0(5) . . ?
S6 O7 Nd1 140.2(3) . . ?
S10 N9 S6 128.7(5) . . ?
N9 S10 C13 104.3(6) . . ?
O11 S10 N9 111.3(6) . . ?
O11 S10 O12 116.1(4) . . ?
O11 S10 C13 105.0(4) . . ?
O12 S10 N9 114.9(4) . . ?
O12 S10 C13 103.7(4) . . ?
S10 O12 Nd1 142.6(3) . . ?
F14 C13 S10 109.2(7) . . ?
F15 C13 S10 108.6(6) . . ?
F15 C13 F14 109.3(7) . . ?
F15 C13 F16 112.0(10) . . ?
F16 C13 S10 109.2(7) . . ?
F16 C13 F14 108.6(8) . . ?
O17 Nd2 O17 75.20(17) . 11_656 ?
O17 Nd2 O17 75.20(17) . 12_466 ?
O17 Nd2 O17 75.20(17) 11_656 12_466 ?
O17 Nd2 O23 135.82(15) 11_656 . ?
O17 Nd2 O23 135.82(15) 12_466 11_656 ?
O17 Nd2 O23 75.21(15) 11_656 11_656 ?
O17 Nd2 O23 65.98(14) 12_466 . ?
O17 Nd2 O23 65.98(14) 11_656 12_466 ?
O17 Nd2 O23 65.98(14) . 11_656 ?
O17 Nd2 O23 75.21(15) 12_466 12_466 ?
O17 Nd2 O23 75.21(15) . . ?
O17 Nd2 O23 135.82(15) . 12_466 ?
O17 Nd2 O27 132.60(14) 12_466 . ?
O17 Nd2 O27 132.60(14) . 11_656 ?
O17 Nd2 O27 145.11(14) 12_466 11_656 ?
O17 Nd2 O27 145.11(14) . 12_466 ?
O17 Nd2 O27 90.87(14) 11_656 11_656 ?
O17 Nd2 O27 132.60(14) 11_656 12_466 ?
O17 Nd2 O27 90.87(14) . . ?
O17 Nd2 O27 90.87(15) 12_466 12_466 ?
O17 Nd2 O27 145.11(14) 11_656 . ?
O23 Nd2 O23 119.934(9) 11_656 12_466 ?
O23 Nd2 O23 119.935(9) . 12_466 ?
O23 Nd2 O23 119.933(9) . 11_656 ?
O27 Nd2 O23 69.91(14) 11_656 12_466 ?
O27 Nd2 O23 133.21(14) . 12_466 ?
O27 Nd2 O23 66.67(13) 12_466 12_466 ?
O27 Nd2 O23 66.67(13) 11_656 11_656 ?
O27 Nd2 O23 66.67(13) . . ?
O27 Nd2 O23 69.90(14) . 11_656 ?
O27 Nd2 O23 69.91(14) 12_466 . ?
O27 Nd2 O23 133.21(14) 11_656 . ?
O27 Nd2 O23 133.21(14) 12_466 11_656 ?
O27 Nd2 O27 75.11(15) 12_466 . ?
O27 Nd2 O27 75.11(15) 11_656 . ?
O27 Nd2 O27 75.11(15) 12_466 11_656 ?
F19 C18 F20 108.8(6) . . ?
F19 C18 F21 109.6(5) . . ?
F19 C18 S22 108.7(5) . . ?
F20 C18 S22 110.4(4) . . ?
F21 C18 F20 108.5(5) . . ?
F21 C18 S22 110.6(5) . . ?
O23 S22 C18 104.5(3) . . ?
O23 S22 N25 114.7(3) . . ?
O24 S22 C18 104.2(3) . . ?
O24 S22 O23 117.0(3) . . ?
O24 S22 N25 113.1(3) . . ?
N25 S22 C18 101.0(3) . . ?
S22 O23 Nd2 145.7(2) . . ?
S26 N25 S22 125.2(3) . . ?
N25 S26 C29 103.8(3) . . ?
O27 S26 N25 114.3(3) . . ?
O27 S26 C29 103.8(3) . . ?
O28 S26 N25 111.1(3) . . ?
O28 S26 O27 116.6(3) . . ?
O28 S26 C29 105.7(3) . . ?
S26 O27 Nd2 147.2(2) . . ?
F30 C29 S26 110.0(4) . . ?
F31 C29 S26 110.1(5) . . ?
F31 C29 F30 109.0(6) . . ?
F32 C29 S26 110.3(5) . . ?
F32 C29 F30 108.6(5) . . ?
F32 C29 F31 108.8(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
O17 H17A O11 0.840(10) 1.94(2) 2.771(7) 169(9) 5
O17 H17B O8 0.837(10) 1.918(16) 2.752(7) 174(9) .
O1 H1A O24 0.842(10) 1.959(18) 2.795(6) 172(9) 8_655
O1 H1B O28 0.838(10) 1.985(16) 2.819(6) 173(9) 9_466


_olex2_date_sample_data_collection 2012-12-12
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb147
_database_code_depnum_ccdc_archive 'CCDC 1409127'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Heptaaqua-scandium(iii) tris(bis(trifluoromethylsulfonyl)imide) hydrate
;
_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_melting_point          ?
_chemical_oxdiff_formula         'Sc C6 F18 S6 O12 N3 O6 H12'
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'
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'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8946(4)
_cell_length_b                   19.9678(10)
_cell_length_c                   18.7790(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.166(5)
_cell_angle_gamma                90.00
_cell_volume                     3301.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8560
_cell_measurement_theta_min      3.2410
_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_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ? 
;
_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_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -59.00   43.75   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   19.0000   90.0000 137

#__ type_ start__ end____ width___ exp.time_
  2 omega  -33.00    3.75   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000    0.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   29.00   0.7500   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000 -180.0000 56

#__ type_ start__ end____ width___ exp.time_
  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       'ω 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_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                6547
_reflns_number_total             7599
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       ?
_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_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.046
_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)+(0.0287P)²+2.4643P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0736
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_refinement_flags_posn
Sc1 Sc 0.63704(4) 0.236723(18) 0.236024(18) 0.00881(8) Uani 1 d . . .
O1 O 0.50954(17) 0.16097(8) 0.17012(8) 0.0161(3) Uani 1 d . . .
H1A H 0.514(3) 0.1586(15) 0.1290(17) 0.038(9) Uiso 1 d . . .
H1B H 0.470(3) 0.1271(16) 0.1837(16) 0.041(9) Uiso 1 d . . .
O2 O 0.82569(17) 0.17121(8) 0.23700(9) 0.0160(3) Uani 1 d . . .
H2A H 0.898(3) 0.1765(15) 0.2207(16) 0.036(9) Uiso 1 d . . .
H2B H 0.816(3) 0.1324(16) 0.2423(16) 0.040(9) Uiso 1 d . . .
O3 O 0.57328(17) 0.16342(8) 0.31253(8) 0.0141(3) Uani 1 d . . .
H3A H 0.588(3) 0.1680(16) 0.3534(18) 0.044(9) Uiso 1 d . . .
H3B H 0.519(4) 0.1303(17) 0.3013(18) 0.054(10) Uiso 1 d . . .
O4 O 0.63795(18) 0.28921(8) 0.33484(8) 0.0131(3) Uani 1 d . . .
H4A H 0.713(3) 0.3088(14) 0.3567(15) 0.034(8) Uiso 1 d . . .
H4B H 0.577(3) 0.2873(14) 0.3568(14) 0.027(8) Uiso 1 d . . .
O5 O 0.42475(16) 0.28593(8) 0.22078(8) 0.0133(3) Uani 1 d . . .
H5A H 0.403(3) 0.3185(15) 0.2423(16) 0.035(8) Uiso 1 d . . .
H5B H 0.355(3) 0.2778(15) 0.1868(17) 0.042(9) Uiso 1 d . . .
O6 O 0.83881(16) 0.30096(7) 0.24182(8) 0.0119(3) Uani 1 d . . .
H6A H 0.838(3) 0.3407(17) 0.2315(17) 0.045(9) Uiso 1 d . . .
H6B H 0.915(3) 0.2956(14) 0.2697(15) 0.032(8) Uiso 1 d . . .
O7 O 0.63850(18) 0.27335(8) 0.12614(8) 0.0154(3) Uani 1 d . . .
H7A H 0.708(3) 0.2707(14) 0.1063(15) 0.035(8) Uiso 1 d . . .
H7B H 0.571(3) 0.2913(15) 0.1031(16) 0.036(8) Uiso 1 d . . .
C8 C 0.6622(3) 0.48940(13) 0.11604(13) 0.0298(5) Uani 1 d . . .
F9 F 0.65867(17) 0.43232(8) 0.08132(8) 0.0391(4) Uani 1 d . . .
F10 F 0.7550(2) 0.53074(9) 0.08831(9) 0.0546(5) Uani 1 d . . .
F11 F 0.5243(2) 0.51514(10) 0.10777(9) 0.0549(5) Uani 1 d . . .
S12 S 0.73635(6) 0.47838(2) 0.21147(3) 0.01570(11) Uani 1 d . . .
O13 O 0.87282(16) 0.43971(7) 0.21176(9) 0.0216(3) Uani 1 d . . .
O14 O 0.75537(18) 0.54497(7) 0.23967(9) 0.0249(4) Uani 1 d . . .
N15 N 0.61645(19) 0.43351(8) 0.24249(9) 0.0155(4) Uani 1 d . . .
S16 S 0.48089(5) 0.46162(2) 0.27977(3) 0.01389(10) Uani 1 d . . .
O17 O 0.38244(16) 0.40632(7) 0.28837(8) 0.0191(3) Uani 1 d . . .
O18 O 0.41523(17) 0.52323(8) 0.25157(8) 0.0209(3) Uani 1 d . . .
C19 C 0.5662(2) 0.48260(10) 0.37232(11) 0.0163(4) Uani 1 d . . .
F20 F 0.65128(15) 0.43287(7) 0.40195(7) 0.0277(3) Uani 1 d . . .
F21 F 0.65187(14) 0.53690(6) 0.37375(7) 0.0237(3) Uani 1 d . . .
F22 F 0.45555(14) 0.49328(7) 0.41099(7) 0.0241(3) Uani 1 d . . .
C23 C 0.0902(2) 0.43790(11) 0.42703(11) 0.0174(4) Uani 1 d . . .
F24 F 0.20183(14) 0.46027(7) 0.47517(7) 0.0252(3) Uani 1 d . . .
F25 F -0.02569(14) 0.48037(6) 0.42252(7) 0.0252(3) Uani 1 d . . .
F26 F 0.13751(15) 0.43525(7) 0.36312(7) 0.0249(3) Uani 1 d . . .
S27 S 0.02784(5) 0.35462(3) 0.45169(3) 0.01318(10) Uani 1 d . . .
O28 O -0.00304(16) 0.36226(8) 0.52394(8) 0.0205(3) Uani 1 d . . .
O29 O -0.09706(15) 0.34012(8) 0.39660(8) 0.0182(3) Uani 1 d . . .
N30 N 0.17191(18) 0.30946(9) 0.45202(9) 0.0151(4) Uani 1 d . . .
S31 S 0.21273(5) 0.26951(2) 0.38516(3) 0.01231(10) Uani 1 d . . .
O32 O 0.37417(15) 0.26394(8) 0.39115(8) 0.0180(3) Uani 1 d . . .
O33 O 0.12986(15) 0.28710(7) 0.31616(7) 0.0164(3) Uani 1 d . . .
C34 C 0.1482(3) 0.18477(11) 0.40166(12) 0.0218(5) Uani 1 d . . .
F35 F -0.00197(15) 0.18409(7) 0.39912(8) 0.0333(3) Uani 1 d . . .
F36 F 0.18435(19) 0.14425(7) 0.35083(8) 0.0385(4) Uani 1 d . . .
F37 F 0.21071(17) 0.16202(7) 0.46529(8) 0.0332(3) Uani 1 d . . .
C38 C 0.1420(3) 0.40630(11) 0.07938(11) 0.0208(5) Uani 1 d . . .
F39 F -0.00692(16) 0.40151(8) 0.07158(9) 0.0413(4) Uani 1 d . . .
F40 F 0.1792(2) 0.46011(7) 0.04604(9) 0.0436(4) Uani 1 d . . .
F41 F 0.19285(19) 0.41301(8) 0.14878(7) 0.0394(4) Uani 1 d . . .
S42 S 0.22555(5) 0.33146(2) 0.04309(3) 0.01299(10) Uani 1 d . . .
O43 O 0.14170(16) 0.32235(7) -0.02723(7) 0.0177(3) Uani 1 d . . .
O44 O 0.38509(16) 0.34501(8) 0.05062(8) 0.0197(3) Uani 1 d . . .
N45 N 0.20448(18) 0.27520(8) 0.10089(9) 0.0132(3) Uani 1 d . . .
S46 S 0.05929(5) 0.22955(3) 0.10147(2) 0.01207(10) Uani 1 d . . .
O47 O 0.07023(15) 0.20065(7) 0.17212(7) 0.0163(3) Uani 1 d . . .
O48 O -0.08179(15) 0.25841(8) 0.06990(7) 0.0171(3) Uani 1 d . . .
C49 C 0.0946(2) 0.15839(10) 0.04399(11) 0.0146(4) Uani 1 d . . .
F50 F 0.19970(13) 0.11860(6) 0.07887(7) 0.0189(3) Uani 1 d . . .
F51 F -0.03215(13) 0.12399(6) 0.02631(7) 0.0218(3) Uani 1 d . . .
F52 F 0.14319(14) 0.17965(6) -0.01559(6) 0.0210(3) Uani 1 d . . .
O53 O 0.40039(19) 0.06027(8) 0.25006(9) 0.0206(3) Uani 1 d . . .
H53A H 0.313(3) 0.0544(15) 0.2486(16) 0.039(9) Uiso 1 d . . .
H53B H 0.439(3) 0.0240(16) 0.2518(16) 0.040(9) Uiso 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 O1 2.1695(15) . ?
Sc1 O2 2.1257(15) . ?
Sc1 O3 2.1816(15) . ?
Sc1 O4 2.1302(15) . ?
Sc1 O5 2.1118(15) . ?
Sc1 O6 2.1959(14) . ?
Sc1 O7 2.1909(15) . ?
C8 F9 1.311(3) . ?
C8 F10 1.325(3) . ?
C8 F11 1.319(3) . ?
C8 S12 1.833(3) . ?
S12 O13 1.4379(15) . ?
S12 O14 1.4324(15) . ?
S12 N15 1.5670(17) . ?
N15 S16 1.5808(17) . ?
S16 O17 1.4326(15) . ?
S16 O18 1.4308(15) . ?
S16 C19 1.843(2) . ?
C19 F20 1.322(2) . ?
C19 F21 1.323(2) . ?
C19 F22 1.321(2) . ?
C23 F24 1.322(2) . ?
C23 F25 1.328(2) . ?
C23 F26 1.328(2) . ?
C23 S27 1.833(2) . ?
S27 O28 1.4301(14) . ?
S27 O29 1.4360(14) . ?
S27 N30 1.5662(17) . ?
N30 S31 1.5729(17) . ?
S31 O32 1.4287(14) . ?
S31 O33 1.4402(14) . ?
S31 C34 1.827(2) . ?
C34 F35 1.330(3) . ?
C34 F36 1.325(3) . ?
C34 F37 1.325(3) . ?
C38 F39 1.316(3) . ?
C38 F40 1.309(3) . ?
C38 F41 1.324(2) . ?
C38 S42 1.842(2) . ?
S42 O43 1.4330(14) . ?
S42 O44 1.4317(15) . ?
S42 N45 1.5915(17) . ?
N45 S46 1.5819(17) . ?
S46 O47 1.4374(14) . ?
S46 O48 1.4307(14) . ?
S46 C49 1.838(2) . ?
C49 F50 1.327(2) . ?
C49 F51 1.322(2) . ?
C49 F52 1.325(2) . ?

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
_geom_angle_publ_flag
O1 Sc1 O3 75.18(6) . . ?
O1 Sc1 O6 142.45(6) . . ?
O1 Sc1 O7 76.58(6) . . ?
O2 Sc1 O1 85.64(6) . . ?
O2 Sc1 O3 81.96(6) . . ?
O2 Sc1 O4 112.95(6) . . ?
O2 Sc1 O6 73.77(6) . . ?
O2 Sc1 O7 95.93(6) . . ?
O3 Sc1 O6 130.26(6) . . ?
O3 Sc1 O7 151.77(6) . . ?
O4 Sc1 O1 140.98(6) . . ?
O4 Sc1 O3 74.07(6) . . ?
O4 Sc1 O6 76.56(6) . . ?
O4 Sc1 O7 131.03(6) . . ?
O5 Sc1 O1 82.08(6) . . ?
O5 Sc1 O2 167.71(6) . . ?
O5 Sc1 O3 95.18(6) . . ?
O5 Sc1 O4 77.40(6) . . ?
O5 Sc1 O6 116.34(6) . . ?
O5 Sc1 O7 80.90(6) . . ?
O7 Sc1 O6 74.79(6) . . ?
F9 C8 F10 108.6(2) . . ?
F9 C8 F11 108.9(2) . . ?
F9 C8 S12 111.21(17) . . ?
F10 C8 S12 107.55(18) . . ?
F11 C8 F10 109.4(2) . . ?
F11 C8 S12 111.17(16) . . ?
O13 S12 C8 104.73(10) . . ?
O13 S12 N15 108.07(9) . . ?
O14 S12 C8 104.90(11) . . ?
O14 S12 O13 116.22(10) . . ?
O14 S12 N15 116.38(9) . . ?
N15 S12 C8 105.24(11) . . ?
S12 N15 S16 124.31(11) . . ?
N15 S16 C19 105.10(9) . . ?
O17 S16 N15 107.05(9) . . ?
O17 S16 C19 104.20(9) . . ?
O18 S16 N15 116.00(9) . . ?
O18 S16 O17 118.72(9) . . ?
O18 S16 C19 104.20(9) . . ?
F20 C19 S16 111.13(14) . . ?
F20 C19 F21 108.28(17) . . ?
F21 C19 S16 111.35(14) . . ?
F22 C19 S16 108.41(14) . . ?
F22 C19 F20 108.45(17) . . ?
F22 C19 F21 109.17(17) . . ?
F24 C23 F25 109.18(17) . . ?
F24 C23 F26 109.13(16) . . ?
F24 C23 S27 111.01(14) . . ?
F25 C23 S27 109.60(14) . . ?
F26 C23 F25 108.09(17) . . ?
F26 C23 S27 109.77(14) . . ?
O28 S27 C23 104.40(10) . . ?
O28 S27 O29 118.15(9) . . ?
O28 S27 N30 108.96(9) . . ?
O29 S27 C23 103.40(9) . . ?
O29 S27 N30 115.82(9) . . ?
N30 S27 C23 104.28(9) . . ?
S27 N30 S31 124.77(11) . . ?
N30 S31 C34 102.75(10) . . ?
O32 S31 N30 108.66(9) . . ?
O32 S31 O33 118.03(9) . . ?
O32 S31 C34 104.52(10) . . ?
O33 S31 N30 116.61(9) . . ?
O33 S31 C34 104.21(10) . . ?
F35 C34 S31 109.96(16) . . ?
F36 C34 S31 109.23(15) . . ?
F36 C34 F35 108.24(18) . . ?
F37 C34 S31 111.66(15) . . ?
F37 C34 F35 108.61(18) . . ?
F37 C34 F36 109.08(19) . . ?
F39 C38 F41 108.32(19) . . ?
F39 C38 S42 110.64(15) . . ?
F40 C38 F39 108.97(19) . . ?
F40 C38 F41 108.27(19) . . ?
F40 C38 S42 110.27(15) . . ?
F41 C38 S42 110.31(15) . . ?
O43 S42 C38 105.03(9) . . ?
O43 S42 N45 116.27(9) . . ?
O44 S42 C38 104.85(10) . . ?
O44 S42 O43 119.59(9) . . ?
O44 S42 N45 106.09(9) . . ?
N45 S42 C38 103.16(9) . . ?
S46 N45 S42 125.93(10) . . ?
N45 S46 C49 103.50(9) . . ?
O47 S46 N45 106.83(8) . . ?
O47 S46 C49 103.70(9) . . ?
O48 S46 N45 115.72(9) . . ?
O48 S46 O47 118.99(8) . . ?
O48 S46 C49 106.31(9) . . ?
F50 C49 S46 109.89(13) . . ?
F51 C49 S46 109.78(13) . . ?
F51 C49 F50 109.20(16) . . ?
F51 C49 F52 108.86(16) . . ?
F52 C49 S46 110.59(14) . . ?
F52 C49 F50 108.49(16) . . ?

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 O28 0.78(3) 2.00(3) 2.770(2) 169(3) 4_665
O1 H1B O53 0.82(3) 1.98(3) 2.767(2) 159(3) .
O2 H2A O47 0.76(3) 1.95(3) 2.704(2) 172(3) 1_655
O2 H2B O14 0.79(3) 1.90(3) 2.675(2) 166(3) 2_645
O3 H3A O43 0.77(3) 2.23(3) 2.998(2) 177(3) 4_666
O3 H3B O53 0.83(3) 1.92(4) 2.733(2) 165(3) .
O4 H4A O29 0.83(3) 1.86(3) 2.675(2) 168(3) 1_655
O4 H4B O32 0.73(3) 2.05(3) 2.753(2) 162(3) .
O5 H5A O17 0.80(3) 1.98(3) 2.769(2) 169(3) .
O5 H5B N45 0.84(3) 1.94(3) 2.775(2) 169(3) .
O6 H6A O13 0.82(3) 2.04(3) 2.852(2) 170(3) .
O6 H6B O33 0.80(3) 1.99(3) 2.775(2) 165(3) 1_655
O7 H7A O48 0.77(3) 2.09(3) 2.853(2) 170(3) 1_655
O7 H7B O44 0.78(3) 2.10(3) 2.869(2) 174(3) .
O53 H53A O18 0.78(3) 2.12(3) 2.899(2) 171(3) 2_545
O53 H53B O13 0.80(3) 2.40(3) 3.157(2) 157(3) 2_645


_olex2_date_sample_data_collection 2013-04-12
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb153
_database_code_depnum_ccdc_archive 'CCDC 1409128'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
pentaaqua-tris(bis(trifluoromethylsulfonyl)imide-O)-samarium(iii) 
;
_chemical_formula_moiety         'C6 H10 F18 N3 O17 S6 Sm'
_chemical_formula_sum            'C6 H10 F18 N3 O17 S6 Sm'
_chemical_formula_weight         1080.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Sm C6 F18 S6 O12 N3 O6 H12'
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'
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9489(3)
_cell_length_b                   18.4605(5)
_cell_length_c                   12.9858(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.507(2)
_cell_angle_gamma                90.00
_cell_volume                     3094.56(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9940
_cell_measurement_theta_min      3.3400
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73121
_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    2.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16706
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.07
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -8.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
  2 omega  -38.00    5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000 -180.0000 43

#__ type_ start__ end____ width___ exp.time_
  3 omega  -88.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -19.0000   30.0000 106

#__ type_ start__ end____ width___ exp.time_
  4 omega  -44.00  -15.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000    0.0000 29

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   21.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000   90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0502693000
_diffrn_orient_matrix_UB_12      0.0147776000
_diffrn_orient_matrix_UB_13      0.0103987000
_diffrn_orient_matrix_UB_21      -0.0216020000
_diffrn_orient_matrix_UB_22      0.0352220000
_diffrn_orient_matrix_UB_23      0.0021820000
_diffrn_orient_matrix_UB_31      -0.0044731000
_diffrn_orient_matrix_UB_32      -0.0042402000
_diffrn_orient_matrix_UB_33      0.0537875000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_number_gt                6389
_reflns_number_total             7124
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.037
_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)+(0.0198P)²+1.5285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0527
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
 O2-H2A = O2-H2B
 0.84 with sigma of 0.01
 H2A-H2B
 1.35 with sigma of 0.02
 O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 H3A-H3B
 1.35 with sigma of 0.02
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
 H4A-H4B
 1.35 with sigma of 0.02
 O5-H5A = O5-H5B
 0.84 with sigma of 0.01
 H5A-H5B
 1.35 with sigma of 0.02
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_refinement_flags_posn
Sm1 Sm 0.650491(8) 0.246116(6) 0.709535(8) 0.00763(4) Uani 1 d . . .
O1 O 0.82617(13) 0.26707(10) 0.67034(13) 0.0162(4) Uani 1 d . . D
H1A H 0.850(2) 0.2695(17) 0.6118(12) 0.038(10) Uiso 1 d . . D
H1B H 0.863(2) 0.2948(16) 0.7078(19) 0.051(11) Uiso 1 d . . D
O2 O 0.65319(14) 0.11747(9) 0.71796(14) 0.0200(4) Uani 1 d . . D
H2A H 0.6088(16) 0.0896(13) 0.691(2) 0.041(10) Uiso 1 d . . D
H2B H 0.7061(14) 0.0933(14) 0.735(2) 0.041(10) Uiso 1 d . . D
O3 O 0.66333(14) 0.21278(10) 0.53311(12) 0.0177(4) Uani 1 d . . D
H3A H 0.671(3) 0.2431(12) 0.4868(17) 0.033(10) Uiso 1 d . . D
H3B H 0.629(2) 0.1775(12) 0.509(2) 0.052(11) Uiso 1 d . . D
O4 O 0.48246(12) 0.20773(10) 0.63800(13) 0.0168(4) Uani 1 d . . D
H4A H 0.459(2) 0.2225(19) 0.5803(13) 0.053(11) Uiso 1 d . . D
H4B H 0.4327(15) 0.2014(17) 0.6740(17) 0.036(9) Uiso 1 d . . D
O5 O 0.59645(15) 0.34915(10) 0.61282(13) 0.0206(4) Uani 1 d . . D
H5A H 0.593(3) 0.3903(9) 0.640(2) 0.057(12) Uiso 1 d . . D
H5B H 0.570(3) 0.3522(18) 0.5521(11) 0.060(12) Uiso 1 d . . D
C6 C 0.7792(2) 0.13459(14) 1.02939(18) 0.0199(5) Uani 1 d . . .
F7 F 0.76123(13) 0.18899(9) 1.09176(11) 0.0292(4) Uani 1 d . . .
F8 F 0.69050(12) 0.10193(9) 1.00052(12) 0.0304(4) Uani 1 d . . .
F9 F 0.84206(12) 0.08749(9) 1.07895(11) 0.0275(4) Uani 1 d . . .
S10 S 0.83925(4) 0.16946(3) 0.91587(4) 0.01127(11) Uani 1 d . . .
O11 O 0.75693(12) 0.21242(9) 0.86500(11) 0.0137(3) Uani 1 d . . .
O12 O 0.92960(12) 0.20821(9) 0.95643(12) 0.0160(3) Uani 1 d . . .
N13 N 0.85544(15) 0.10123(11) 0.84761(14) 0.0140(4) Uani 1 d . . .
S14 S 0.96230(4) 0.05789(3) 0.84810(4) 0.01142(11) Uani 1 d . . .
O15 O 0.93984(13) -0.01536(9) 0.81885(12) 0.0164(4) Uani 1 d . . .
O16 O 1.03453(12) 0.07225(9) 0.93444(12) 0.0145(3) Uani 1 d . . .
C17 C 1.0188(2) 0.09654(14) 0.73459(18) 0.0192(5) Uani 1 d . . .
F18 F 0.95787(13) 0.08288(9) 0.65029(10) 0.0296(4) Uani 1 d . . .
F19 F 1.11045(12) 0.06672(9) 0.72593(12) 0.0310(4) Uani 1 d . . .
F20 F 1.02970(12) 0.16724(8) 0.74573(11) 0.0250(3) Uani 1 d . . .
C21 C 0.75808(19) 0.40916(15) 0.98736(19) 0.0204(5) Uani 1 d . . .
F22 F 0.76773(12) 0.34282(9) 1.02533(11) 0.0276(4) Uani 1 d . . .
F23 F 0.83044(13) 0.45071(10) 1.03524(11) 0.0352(4) Uani 1 d . . .
F24 F 0.66600(12) 0.43480(9) 1.00390(11) 0.0299(4) Uani 1 d . . .
S25 S 0.77495(4) 0.40979(3) 0.84812(4) 0.01137(11) Uani 1 d . . .
O26 O 0.70132(12) 0.35640(9) 0.80664(11) 0.0122(3) Uani 1 d . . .
O27 O 0.75846(13) 0.48275(9) 0.81692(13) 0.0201(4) Uani 1 d . . .
N28 N 0.88628(14) 0.37774(11) 0.83850(15) 0.0144(4) Uani 1 d . . .
S29 S 0.98989(4) 0.42371(3) 0.85703(4) 0.01292(12) Uani 1 d . . .
O30 O 0.98107(13) 0.49935(9) 0.83653(14) 0.0211(4) Uani 1 d . . .
O31 O 1.04891(13) 0.40134(9) 0.94941(13) 0.0208(4) Uani 1 d . . .
C32 C 1.0609(2) 0.38558(15) 0.7530(2) 0.0237(6) Uani 1 d . . .
F33 F 1.01338(14) 0.39896(12) 0.66187(12) 0.0466(5) Uani 1 d . . .
F34 F 1.07114(14) 0.31461(9) 0.76448(15) 0.0443(5) Uani 1 d . . .
F35 F 1.15431(11) 0.41486(9) 0.75715(13) 0.0317(4) Uani 1 d . . .
C36 C 0.41265(19) 0.35582(14) 0.88636(18) 0.0190(5) Uani 1 d . . .
F37 F 0.35063(13) 0.34156(10) 0.80280(12) 0.0371(4) Uani 1 d . . .
F38 F 0.35638(12) 0.38198(9) 0.95795(11) 0.0285(4) Uani 1 d . . .
F39 F 0.48140(13) 0.40429(9) 0.86327(14) 0.0386(4) Uani 1 d . . .
S40 S 0.47861(4) 0.27216(3) 0.93173(4) 0.01193(12) Uani 1 d . . .
O41 O 0.52997(13) 0.24875(9) 0.84191(12) 0.0150(4) Uani 1 d . . .
O42 O 0.54039(12) 0.28979(10) 1.02280(12) 0.0167(4) Uani 1 d . . .
N43 N 0.38722(15) 0.22128(12) 0.95927(14) 0.0152(4) Uani 1 d . . .
S44 S 0.31794(4) 0.17207(3) 0.88051(4) 0.01534(13) Uani 1 d . . .
O45 O 0.34055(14) 0.17500(12) 0.77503(13) 0.0309(5) Uani 1 d . . .
O46 O 0.21233(13) 0.17903(10) 0.90289(13) 0.0234(4) Uani 1 d . . .
C47 C 0.3553(3) 0.08121(17) 0.9259(3) 0.0382(8) Uani 1 d . . .
F48 F 0.45480(17) 0.07124(12) 0.91899(19) 0.0682(7) Uani 1 d . . .
F49 F 0.30233(18) 0.03365(10) 0.86694(16) 0.0564(6) Uani 1 d . . .
F50 F 0.33393(18) 0.07250(10) 1.02290(14) 0.0570(6) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.4012(16) . ?
Sm1 O2 2.3776(18) . ?
Sm1 O3 2.3906(16) . ?
Sm1 O4 2.4045(16) . ?
Sm1 O5 2.3552(17) . ?
Sm1 O11 2.4341(15) . ?
Sm1 O26 2.4572(15) . ?
Sm1 O41 2.4113(16) . ?
C6 F7 1.322(3) . ?
C6 F8 1.325(3) . ?
C6 F9 1.323(3) . ?
C6 S10 1.837(2) . ?
S10 O11 1.4461(16) . ?
S10 O12 1.4356(16) . ?
S10 N13 1.564(2) . ?
N13 S14 1.598(2) . ?
S14 O15 1.4283(17) . ?
S14 O16 1.4273(16) . ?
S14 C17 1.840(2) . ?
C17 F18 1.322(3) . ?
C17 F19 1.321(3) . ?
C17 F20 1.320(3) . ?
C21 F22 1.322(3) . ?
C21 F23 1.327(3) . ?
C21 F24 1.316(3) . ?
C21 S25 1.838(2) . ?
S25 O26 1.4456(16) . ?
S25 O27 1.4179(17) . ?
S25 N28 1.5723(19) . ?
N28 S29 1.5897(19) . ?
S29 O30 1.4245(17) . ?
S29 O31 1.4317(17) . ?
S29 C32 1.833(3) . ?
C32 F33 1.314(3) . ?
C32 F34 1.324(3) . ?
C32 F35 1.322(3) . ?
C36 F37 1.325(3) . ?
C36 F38 1.317(3) . ?
C36 F39 1.313(3) . ?
C36 S40 1.839(3) . ?
S40 O41 1.4531(17) . ?
S40 O42 1.4127(16) . ?
S40 N43 1.574(2) . ?
N43 S44 1.591(2) . ?
S44 O45 1.4241(17) . ?
S44 O46 1.4259(17) . ?
S44 C47 1.830(3) . ?
C47 F48 1.312(4) . ?
C47 F49 1.321(3) . ?
C47 F50 1.320(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
_geom_angle_publ_flag
O1 Sm1 O4 144.02(6) . . ?
O1 Sm1 O11 74.51(6) . . ?
O1 Sm1 O26 75.84(6) . . ?
O1 Sm1 O41 145.58(6) . . ?
O2 Sm1 O1 99.20(6) . . ?
O2 Sm1 O3 77.59(6) . . ?
O2 Sm1 O4 74.51(6) . . ?
O2 Sm1 O11 72.62(6) . . ?
O2 Sm1 O26 143.29(6) . . ?
O2 Sm1 O41 89.73(6) . . ?
O3 Sm1 O1 72.54(6) . . ?
O3 Sm1 O4 71.51(6) . . ?
O3 Sm1 O11 130.66(6) . . ?
O3 Sm1 O26 132.00(6) . . ?
O3 Sm1 O41 141.82(6) . . ?
O4 Sm1 O11 132.95(6) . . ?
O4 Sm1 O26 129.81(6) . . ?
O4 Sm1 O41 70.41(6) . . ?
O5 Sm1 O1 90.21(7) . . ?
O5 Sm1 O2 146.50(6) . . ?
O5 Sm1 O3 74.75(6) . . ?
O5 Sm1 O4 79.05(6) . . ?
O5 Sm1 O11 140.70(6) . . ?
O5 Sm1 O26 70.18(6) . . ?
O5 Sm1 O41 100.49(6) . . ?
O11 Sm1 O26 71.02(5) . . ?
O41 Sm1 O11 76.70(5) . . ?
O41 Sm1 O26 77.27(5) . . ?
F7 C6 F8 109.2(2) . . ?
F7 C6 F9 109.4(2) . . ?
F7 C6 S10 109.36(18) . . ?
F8 C6 S10 110.17(16) . . ?
F9 C6 F8 109.0(2) . . ?
F9 C6 S10 109.72(17) . . ?
O11 S10 C6 102.43(11) . . ?
O11 S10 N13 108.04(10) . . ?
O12 S10 C6 105.34(11) . . ?
O12 S10 O11 116.39(10) . . ?
O12 S10 N13 117.88(10) . . ?
N13 S10 C6 104.88(11) . . ?
S10 O11 Sm1 150.23(10) . . ?
S10 N13 S14 123.75(12) . . ?
N13 S14 C17 101.61(11) . . ?
O15 S14 N13 108.34(10) . . ?
O15 S14 C17 103.85(11) . . ?
O16 S14 N13 115.09(10) . . ?
O16 S14 O15 119.46(10) . . ?
O16 S14 C17 106.26(11) . . ?
F18 C17 S14 109.91(17) . . ?
F19 C17 S14 108.84(17) . . ?
F19 C17 F18 109.4(2) . . ?
F20 C17 S14 109.97(17) . . ?
F20 C17 F18 109.3(2) . . ?
F20 C17 F19 109.4(2) . . ?
F22 C21 F23 108.5(2) . . ?
F22 C21 S25 110.94(17) . . ?
F23 C21 S25 108.85(17) . . ?
F24 C21 F22 109.4(2) . . ?
F24 C21 F23 109.3(2) . . ?
F24 C21 S25 109.72(17) . . ?
O26 S25 C21 103.67(10) . . ?
O26 S25 N28 107.21(10) . . ?
O27 S25 C21 105.08(12) . . ?
O27 S25 O26 117.45(10) . . ?
O27 S25 N28 116.95(11) . . ?
N28 S25 C21 104.85(11) . . ?
S25 O26 Sm1 153.94(10) . . ?
S25 N28 S29 123.73(13) . . ?
N28 S29 C32 98.62(11) . . ?
O30 S29 N28 116.15(10) . . ?
O30 S29 O31 117.97(11) . . ?
O30 S29 C32 106.04(12) . . ?
O31 S29 N28 111.19(11) . . ?
O31 S29 C32 103.94(12) . . ?
F33 C32 S29 111.40(19) . . ?
F33 C32 F34 108.8(2) . . ?
F33 C32 F35 108.8(2) . . ?
F34 C32 S29 110.42(18) . . ?
F35 C32 S29 108.88(18) . . ?
F35 C32 F34 108.5(2) . . ?
F37 C36 S40 109.38(18) . . ?
F38 C36 F37 108.5(2) . . ?
F38 C36 S40 110.52(17) . . ?
F39 C36 F37 109.1(2) . . ?
F39 C36 F38 109.5(2) . . ?
F39 C36 S40 109.83(17) . . ?
O41 S40 C36 102.88(10) . . ?
O41 S40 N43 113.87(10) . . ?
O42 S40 C36 107.03(11) . . ?
O42 S40 O41 118.40(10) . . ?
O42 S40 N43 109.49(10) . . ?
N43 S40 C36 103.62(11) . . ?
S40 O41 Sm1 160.21(10) . . ?
S40 N43 S44 126.21(12) . . ?
N43 S44 C47 101.22(13) . . ?
O45 S44 N43 116.64(11) . . ?
O45 S44 O46 117.74(11) . . ?
O45 S44 C47 106.00(15) . . ?
O46 S44 N43 108.60(10) . . ?
O46 S44 C47 104.49(14) . . ?
F48 C47 S44 110.0(2) . . ?
F48 C47 F49 109.6(3) . . ?
F48 C47 F50 109.2(3) . . ?
F49 C47 S44 108.1(2) . . ?
F50 C47 S44 110.4(2) . . ?
F50 C47 F49 109.5(3) . . ?

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 N43 0.841(10) 2.084(11) 2.920(2) 172(3) 4_665
O1 H1B N28 0.834(10) 2.287(17) 3.047(3) 152(3) .
O2 H2A O30 0.829(10) 2.047(14) 2.843(2) 161(3) 2_646
O2 H2B N13 0.834(10) 2.333(19) 3.015(3) 139(3) .
O2 H2B O27 0.834(10) 2.21(2) 2.789(2) 127(2) 2_646
O3 H3A O46 0.833(10) 1.905(11) 2.724(3) 167(3) 4_665
O3 H3B O31 0.833(10) 1.918(10) 2.750(2) 178(3) 4_565
O4 H4A O12 0.830(10) 2.068(15) 2.861(2) 160(3) 4_565
O4 H4B O45 0.833(10) 1.906(11) 2.724(2) 167(3) .
O5 H5A O15 0.840(10) 1.881(13) 2.707(2) 168(3) 2_656
O5 H5B O12 0.835(10) 2.40(3) 3.037(2) 134(3) 4_565
O5 H5B O16 0.835(10) 2.09(2) 2.797(2) 142(3) 4_565


_olex2_date_sample_data_collection 2013-05-06
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb167
_database_code_depnum_ccdc_archive 'CCDC 1409129'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-gadolinium(iii) 
;
_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_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Gd C6 F18 S6 O12 N3 O8 H16'
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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'
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'

_cell_length_a                   18.3973(2)
_cell_length_b                   18.3973(2)
_cell_length_c                   18.3973(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6226.75(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24463
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1040
_cell_measurement_theta_min      3.1330
_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_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ? 
;
_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_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -89.00  -63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -45.00   -9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000  -90.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000 -120.0000 99

#__ type_ start__ end____ width___ exp.time_
  4 omega  -42.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000   90.0000 50

#__ type_ start__ end____ width___ exp.time_
  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       'ω 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_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                5004
_reflns_number_total             5163
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_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_coef       ?
_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_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0184
_refine_ls_restrained_S_all      1.060
_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/[σ²(Fo²)+(0.0160P)²+5.7232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0403
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Gd1 Gd 0.765914(6) 0.734086(6) 0.265914(6) 0.01243(4) Uani 1 d . . 3 S T P
O1 O 0.77888(11) 0.78961(9) 0.15077(10) 0.0204(4) Uani 1 d . . 1 D . .
H1A H 0.773(2) 0.8348(7) 0.1445(19) 0.045(11) Uiso 1 d . . 1 D . .
H1B H 0.8055(17) 0.7767(17) 0.1164(14) 0.045(11) Uiso 1 d . . 1 D . .
C2 C 0.8332(2) 0.77584(17) 0.52383(17) 0.0382(7) Uani 1 d . . 1 . . .
F3 F 0.90431(13) 0.77345(14) 0.51766(12) 0.0611(7) Uani 1 d . . 1 . . .
F4 F 0.8101(2) 0.84094(11) 0.50764(12) 0.0844(10) Uani 1 d . . 1 . . .
F5 F 0.81442(13) 0.75982(13) 0.59174(9) 0.0526(6) Uani 1 d . . 1 . . .
S6 S 0.79445(4) 0.70967(4) 0.46177(3) 0.02260(13) Uani 1 d . . 1 . . .
O7 O 0.81158(9) 0.73811(10) 0.39040(9) 0.0195(4) Uani 1 d . . 1 . . .
O8 O 0.82723(16) 0.64333(11) 0.48194(13) 0.0459(6) Uani 1 d . . 1 . . .
N9 N 0.71330(15) 0.7134(3) 0.48144(16) 0.0784(15) Uani 1 d . . 1 . . .
S10 S 0.64920(4) 0.73080(4) 0.43009(3) 0.02507(14) Uani 1 d . . 1 . . .
O11 O 0.66584(10) 0.72143(10) 0.35450(10) 0.0228(4) Uani 1 d . . 1 . . .
O12 O 0.61161(17) 0.79469(15) 0.44997(15) 0.0568(8) Uani 1 d . . 1 . . .
C13 C 0.5864(2) 0.6562(2) 0.45092(19) 0.0431(9) Uani 1 d . . 1 . . .
F14 F 0.61559(18) 0.59379(13) 0.43358(18) 0.0879(10) Uani 1 d . . 1 . . .
F15 F 0.52710(12) 0.66564(16) 0.41185(12) 0.0641(7) Uani 1 d . . 1 . . .
F16 F 0.57012(13) 0.65685(15) 0.52044(12) 0.0645(7) Uani 1 d . . 1 . . .
Gd2 Gd 0.478508(6) 0.521492(6) 0.021492(6) 0.01379(4) Uani 1 d . . 3 S T P
O17 O 0.47166(11) 0.40039(9) -0.02116(10) 0.0217(4) Uani 1 d . . 1 D . .
H17A H 0.4866(16) 0.3819(15) -0.0597(10) 0.026(8) Uiso 1 d . . 1 D . .
H17B H 0.4523(19) 0.3682(14) 0.0041(15) 0.050(12) Uiso 1 d . . 1 D . .
C18 C 0.41575(15) 0.58109(15) 0.26224(16) 0.0256(6) Uani 1 d . . 1 . . .
F19 F 0.36685(8) 0.53305(10) 0.23893(9) 0.0299(4) Uani 1 d . . 1 . . .
F20 F 0.42191(10) 0.57515(11) 0.33310(9) 0.0369(4) Uani 1 d . . 1 . . .
F21 F 0.39339(10) 0.64689(10) 0.24545(11) 0.0404(5) Uani 1 d . . 1 . . .
S22 S 0.50332(3) 0.56237(3) 0.21841(3) 0.01784(12) Uani 1 d . . 1 . . .
O23 O 0.48932(10) 0.57430(9) 0.14191(9) 0.0190(4) Uani 1 d . . 1 . . .
O24 O 0.55384(10) 0.61029(10) 0.25254(10) 0.0241(4) Uani 1 d . . 1 . . .
N25 N 0.51940(11) 0.48176(11) 0.23929(11) 0.0207(4) Uani 1 d . . 1 . . .
S26 S 0.49204(3) 0.41416(3) 0.19547(3) 0.01694(12) Uani 1 d . . 1 . . .
O27 O 0.47849(11) 0.42800(9) 0.11954(9) 0.0199(4) Uani 1 d . . 1 . . .
O28 O 0.43898(10) 0.37260(10) 0.23371(11) 0.0254(4) Uani 1 d . . 1 . . .
C29 C 0.57381(15) 0.35708(15) 0.19684(15) 0.0233(5) Uani 1 d . . 1 . . .
F30 F 0.62801(9) 0.38913(11) 0.16273(10) 0.0351(4) Uani 1 d . . 1 . . .
F31 F 0.55790(11) 0.29538(10) 0.16410(12) 0.0431(5) Uani 1 d . . 1 . . .
F32 F 0.59361(9) 0.34316(9) 0.26410(10) 0.0313(4) Uani 1 d . . 1 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.3637(18) 5_566 ?
Gd1 O1 2.3637(18) 4_664 ?
Gd1 O1 2.3637(18) . ?
Gd1 O7 2.4404(17) 4_664 ?
Gd1 O7 2.4405(17) . ?
Gd1 O7 2.4404(17) 5_566 ?
Gd1 O11 2.4697(18) . ?
Gd1 O11 2.4697(17) 4_664 ?
Gd1 O11 2.4697(18) 5_566 ?
C2 F3 1.315(4) . ?
C2 F4 1.305(4) . ?
C2 F5 1.329(4) . ?
C2 S6 1.815(3) . ?
S6 O7 1.4482(18) . ?
S6 O8 1.411(2) . ?
S6 N9 1.538(3) . ?
N9 S10 1.544(3) . ?
S10 O11 1.4343(19) . ?
S10 O12 1.412(3) . ?
S10 C13 1.836(4) . ?
C13 F14 1.307(5) . ?
C13 F15 1.317(4) . ?
C13 F16 1.314(4) . ?
Gd2 O17 2.3654(17) . ?
Gd2 O17 2.3654(17) 6_655 ?
Gd2 O17 2.3654(17) 7_564 ?
Gd2 O23 2.4272(17) 6_655 ?
Gd2 O23 2.4272(17) 7_564 ?
Gd2 O23 2.4273(17) . ?
Gd2 O27 2.4924(17) 6_655 ?
Gd2 O27 2.4924(17) 7_564 ?
Gd2 O27 2.4924(17) . ?
C18 F19 1.332(3) . ?
C18 F20 1.313(3) . ?
C18 F21 1.315(3) . ?
C18 S22 1.834(3) . ?
S22 O23 1.4473(18) . ?
S22 O24 1.4268(18) . ?
S22 N25 1.560(2) . ?
N25 S26 1.565(2) . ?
S26 O27 1.4417(17) . ?
S26 O28 1.4257(19) . ?
S26 C29 1.835(3) . ?
C29 F30 1.317(3) . ?
C29 F31 1.318(3) . ?
C29 F32 1.315(3) . ?

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
_geom_angle_publ_flag
O1 Gd1 O1 75.33(7) 5_566 4_664 ?
O1 Gd1 O1 75.33(7) 5_566 . ?
O1 Gd1 O1 75.33(7) 4_664 . ?
O1 Gd1 O7 142.48(6) 5_566 5_566 ?
O1 Gd1 O7 142.48(6) . . ?
O1 Gd1 O7 91.54(6) . 5_566 ?
O1 Gd1 O7 135.81(6) 4_664 5_566 ?
O1 Gd1 O7 91.54(6) 5_566 4_664 ?
O1 Gd1 O7 91.54(6) 4_664 . ?
O1 Gd1 O7 142.48(6) 4_664 4_664 ?
O1 Gd1 O7 135.81(6) . 4_664 ?
O1 Gd1 O7 135.81(6) 5_566 . ?
O1 Gd1 O11 66.90(6) 5_566 . ?
O1 Gd1 O11 66.90(6) 4_664 5_566 ?
O1 Gd1 O11 72.29(6) 5_566 4_664 ?
O1 Gd1 O11 72.29(6) 4_664 . ?
O1 Gd1 O11 72.29(6) . 5_566 ?
O1 Gd1 O11 135.01(6) . . ?
O1 Gd1 O11 66.90(6) . 4_664 ?
O1 Gd1 O11 135.01(6) 5_566 5_566 ?
O1 Gd1 O11 135.01(6) 4_664 4_664 ?
O7 Gd1 O7 73.50(7) 4_664 5_566 ?
O7 Gd1 O7 73.49(7) 4_664 . ?
O7 Gd1 O7 73.49(7) 5_566 . ?
O7 Gd1 O11 68.92(6) . . ?
O7 Gd1 O11 133.40(6) . 4_664 ?
O7 Gd1 O11 68.92(6) 4_664 4_664 ?
O7 Gd1 O11 133.40(6) 5_566 . ?
O7 Gd1 O11 133.40(6) 4_664 5_566 ?
O7 Gd1 O11 70.23(6) 5_566 4_664 ?
O7 Gd1 O11 68.92(6) 5_566 5_566 ?
O7 Gd1 O11 70.23(6) . 5_566 ?
O7 Gd1 O11 70.23(6) 4_664 . ?
O11 Gd1 O11 119.998(1) . 4_664 ?
O11 Gd1 O11 119.997(1) . 5_566 ?
O11 Gd1 O11 119.997(1) 5_566 4_664 ?
F3 C2 F5 109.4(3) . . ?
F3 C2 S6 108.3(2) . . ?
F4 C2 F3 109.6(3) . . ?
F4 C2 F5 109.5(3) . . ?
F4 C2 S6 110.1(2) . . ?
F5 C2 S6 109.9(2) . . ?
O7 S6 C2 104.05(14) . . ?
O7 S6 N9 114.10(14) . . ?
O8 S6 C2 104.31(15) . . ?
O8 S6 O7 117.26(14) . . ?
O8 S6 N9 113.1(2) . . ?
N9 S6 C2 101.7(2) . . ?
S6 O7 Gd1 139.91(11) . . ?
S6 N9 S10 127.35(19) . . ?
N9 S10 C13 101.4(2) . . ?
O11 S10 N9 113.91(15) . . ?
O11 S10 C13 104.30(15) . . ?
O12 S10 N9 112.8(2) . . ?
O12 S10 O11 117.11(14) . . ?
O12 S10 C13 105.08(17) . . ?
S10 O11 Gd1 141.96(12) . . ?
F14 C13 S10 110.3(3) . . ?
F14 C13 F15 108.9(4) . . ?
F14 C13 F16 109.9(3) . . ?
F15 C13 S10 107.9(2) . . ?
F16 C13 S10 109.8(3) . . ?
F16 C13 F15 110.0(3) . . ?
O17 Gd2 O17 75.84(7) . 7_564 ?
O17 Gd2 O17 75.84(7) . 6_655 ?
O17 Gd2 O17 75.84(7) 6_655 7_564 ?
O17 Gd2 O23 144.21(6) . 6_655 ?
O17 Gd2 O23 133.17(6) 6_655 6_655 ?
O17 Gd2 O23 144.21(6) 7_564 . ?
O17 Gd2 O23 90.40(6) 7_564 6_655 ?
O17 Gd2 O23 90.40(6) . 7_564 ?
O17 Gd2 O23 90.40(6) 6_655 . ?
O17 Gd2 O23 144.21(6) 6_655 7_564 ?
O17 Gd2 O23 133.17(6) 7_564 7_564 ?
O17 Gd2 O23 133.17(6) . . ?
O17 Gd2 O27 135.92(6) 6_655 7_564 ?
O17 Gd2 O27 74.49(7) 7_564 6_655 ?
O17 Gd2 O27 74.49(7) 6_655 . ?
O17 Gd2 O27 65.80(6) 7_564 7_564 ?
O17 Gd2 O27 65.80(6) . . ?
O17 Gd2 O27 135.92(6) . 6_655 ?
O17 Gd2 O27 74.49(7) . 7_564 ?
O17 Gd2 O27 65.80(6) 6_655 6_655 ?
O17 Gd2 O27 135.92(6) 7_564 . ?
O23 Gd2 O23 75.07(7) 6_655 . ?
O23 Gd2 O23 75.07(7) 7_564 6_655 ?
O23 Gd2 O23 75.06(7) 7_564 . ?
O23 Gd2 O27 67.40(6) 6_655 6_655 ?
O23 Gd2 O27 69.74(6) 6_655 7_564 ?
O23 Gd2 O27 133.56(6) 6_655 . ?
O23 Gd2 O27 69.74(6) . 6_655 ?
O23 Gd2 O27 69.74(6) 7_564 . ?
O23 Gd2 O27 67.40(6) . . ?
O23 Gd2 O27 133.56(6) 7_564 6_655 ?
O23 Gd2 O27 133.56(6) . 7_564 ?
O23 Gd2 O27 67.40(6) 7_564 7_564 ?
O27 Gd2 O27 119.962(3) 7_564 . ?
O27 Gd2 O27 119.962(3) 7_564 6_655 ?
O27 Gd2 O27 119.963(3) 6_655 . ?
F19 C18 S22 109.09(18) . . ?
F20 C18 F19 108.8(2) . . ?
F20 C18 F21 109.7(2) . . ?
F20 C18 S22 110.2(2) . . ?
F21 C18 F19 108.9(2) . . ?
F21 C18 S22 110.1(2) . . ?
O23 S22 C18 104.05(12) . . ?
O23 S22 N25 114.67(11) . . ?
O24 S22 C18 105.23(12) . . ?
O24 S22 O23 116.75(11) . . ?
O24 S22 N25 110.81(11) . . ?
N25 S22 C18 103.70(13) . . ?
S22 O23 Gd2 147.28(11) . . ?
S22 N25 S26 124.57(14) . . ?
N25 S26 C29 100.60(12) . . ?
O27 S26 N25 114.48(11) . . ?
O27 S26 C29 104.84(12) . . ?
O28 S26 N25 113.09(12) . . ?
O28 S26 O27 117.03(12) . . ?
O28 S26 C29 104.34(12) . . ?
S26 O27 Gd2 145.40(11) . . ?
F30 C29 S26 110.97(19) . . ?
F30 C29 F31 109.6(2) . . ?
F31 C29 S26 107.73(19) . . ?
F32 C29 S26 110.57(19) . . ?
F32 C29 F30 109.0(2) . . ?
F32 C29 F31 108.9(2) . . ?

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 O28 0.846(10) 1.947(11) 2.791(3) 177(3) 8_655
O1 H1B O24 0.834(10) 2.003(14) 2.818(3) 165(4) 4_664
O17 H17A O8 0.833(10) 1.928(11) 2.755(3) 173(3) 8_645
O17 H17B O12 0.832(10) 1.982(13) 2.801(3) 168(4) 12_645


_olex2_date_sample_data_collection 2013-06-20
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb169
_database_code_depnum_ccdc_archive 'CCDC 1409130'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
pentaaqua-tris(bis(trifluoromethylsulfonyl)imide-O)-dysprosium(iii) 
;
_chemical_formula_moiety         'C6 H10 Dy F18 N3 O17 S6'
_chemical_formula_sum            'C6 H10 Dy F18 N3 O17 S6'
_chemical_formula_weight         1093.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Dy C6 F18 S6 O12 N3 O8 H16'
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'
Dy Dy -0.1892 4.4098 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.8735(6)
_cell_length_b                   18.3588(9)
_cell_length_c                   12.9082(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.119(4)
_cell_angle_gamma                90.00
_cell_volume                     3042.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2470
_cell_measurement_theta_min      3.3410
_exptl_absorpt_coefficient_mu    3.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87248
_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    2.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14116
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         3.10
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   43.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701 -178.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -57.0000  -60.0000 62

#__ type_ start__ end____ width___ exp.time_
  3 omega  -51.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -19.0000  -30.0000 110

#__ type_ start__ end____ width___ exp.time_
  4 omega   69.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701 -178.0000   90.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0113818000
_diffrn_orient_matrix_UB_12      0.0130681000
_diffrn_orient_matrix_UB_13      -0.0512694000
_diffrn_orient_matrix_UB_21      -0.0482077000
_diffrn_orient_matrix_UB_22      0.0138948000
_diffrn_orient_matrix_UB_23      0.0144631000
_diffrn_orient_matrix_UB_31      0.0243682000
_diffrn_orient_matrix_UB_32      0.0336459000
_diffrn_orient_matrix_UB_33      0.0140218000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_number_gt                6221
_reflns_number_total             6929
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.040
_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/[σ²(Fo²)+(0.0190P)²+1.4123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0510
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
 O2-H2A = O2-H2B
 0.84 with sigma of 0.01
 H2A-H2B
 1.35 with sigma of 0.02
 O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 H3A-H3B
 1.35 with sigma of 0.02
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
 H4A-H4B
 1.35 with sigma of 0.02
 O5-H5A = O5-H5B
 0.84 with sigma of 0.01
 H5A-H5B
 1.35 with sigma of 0.02
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_refinement_flags_posn
Dy1 Dy 0.650707(8) 0.245379(6) 0.710131(8) 0.00698(4) Uani 1 d . . .
O1 O 0.82320(14) 0.26644(11) 0.67156(14) 0.0146(4) Uani 1 d . . D
H1A H 0.849(2) 0.2661(18) 0.6140(12) 0.037(10) Uiso 1 d . . D
H1B H 0.864(2) 0.2902(17) 0.7121(19) 0.046(11) Uiso 1 d . . D
O2 O 0.65488(14) 0.11921(10) 0.71999(14) 0.0161(4) Uani 1 d . . D
H2A H 0.6110(17) 0.0904(12) 0.692(2) 0.035(10) Uiso 1 d . . D
H2B H 0.7055(14) 0.0942(13) 0.743(2) 0.025(9) Uiso 1 d . . D
O3 O 0.66497(14) 0.21136(11) 0.53677(13) 0.0158(4) Uani 1 d . . D
H3A H 0.678(2) 0.2432(11) 0.4941(17) 0.021(9) Uiso 1 d . . D
H3B H 0.630(3) 0.1776(13) 0.509(2) 0.064(14) Uiso 1 d . . D
O4 O 0.48599(13) 0.20580(11) 0.64000(14) 0.0146(4) Uani 1 d . . D
H4A H 0.460(2) 0.2220(18) 0.5830(14) 0.042(11) Uiso 1 d . . D
H4B H 0.4362(15) 0.2022(17) 0.6783(17) 0.032(9) Uiso 1 d . . D
O5 O 0.59506(15) 0.34613(10) 0.61591(14) 0.0183(4) Uani 1 d . . D
H5A H 0.592(2) 0.3882(8) 0.640(2) 0.036(10) Uiso 1 d . . D
H5B H 0.568(3) 0.3453(18) 0.5552(13) 0.062(13) Uiso 1 d . . D
C6 C 0.7780(2) 0.13615(15) 1.0300(2) 0.0179(6) Uani 1 d . . .
F7 F 0.76004(13) 0.19130(9) 1.09295(12) 0.0267(4) Uani 1 d . . .
F8 F 0.68905(12) 0.10359(9) 1.00145(13) 0.0276(4) Uani 1 d . . .
F9 F 0.84124(12) 0.08904(9) 1.08045(12) 0.0246(4) Uani 1 d . . .
S10 S 0.83858(4) 0.17098(3) 0.91610(4) 0.01002(12) Uani 1 d . . .
O11 O 0.75602(13) 0.21397(9) 0.86416(13) 0.0123(4) Uani 1 d . . .
O12 O 0.92936(13) 0.21023(10) 0.95658(13) 0.0143(4) Uani 1 d . . .
N13 N 0.85529(15) 0.10181(11) 0.84836(16) 0.0126(4) Uani 1 d . . .
S14 S 0.96284(5) 0.05816(3) 0.84970(4) 0.01029(12) Uani 1 d . . .
O15 O 0.94052(13) -0.01582(9) 0.82169(13) 0.0152(4) Uani 1 d . . .
O16 O 1.03492(13) 0.07328(9) 0.93659(13) 0.0135(4) Uani 1 d . . .
C17 C 1.0197(2) 0.09630(15) 0.7356(2) 0.0177(6) Uani 1 d . . .
F18 F 0.95866(13) 0.08176(9) 0.65046(11) 0.0266(4) Uani 1 d . . .
F19 F 1.11223(12) 0.06609(10) 0.72692(13) 0.0286(4) Uani 1 d . . .
F20 F 1.03042(12) 0.16755(8) 0.74520(12) 0.0228(4) Uani 1 d . . .
C21 C 0.7578(2) 0.41000(16) 0.9867(2) 0.0185(6) Uani 1 d . . .
F22 F 0.76867(12) 0.34360(9) 1.02605(11) 0.0239(4) Uani 1 d . . .
F23 F 0.83007(12) 0.45297(10) 1.03307(12) 0.0313(4) Uani 1 d . . .
F24 F 0.66481(12) 0.43539(9) 1.00353(12) 0.0266(4) Uani 1 d . . .
S25 S 0.77352(4) 0.40954(3) 0.84613(5) 0.01012(12) Uani 1 d . . .
O26 O 0.69936(12) 0.35541(9) 0.80543(12) 0.0114(3) Uani 1 d . . .
O27 O 0.75665(13) 0.48289(10) 0.81449(14) 0.0176(4) Uani 1 d . . .
N28 N 0.88529(15) 0.37724(11) 0.83601(16) 0.0127(4) Uani 1 d . . .
S29 S 0.98949(5) 0.42383(3) 0.85569(5) 0.01135(12) Uani 1 d . . .
O30 O 0.98060(13) 0.49999(10) 0.83399(15) 0.0189(4) Uani 1 d . . .
O31 O 1.04730(13) 0.40201(10) 0.94964(14) 0.0187(4) Uani 1 d . . .
C32 C 1.0626(2) 0.38495(16) 0.7527(2) 0.0223(6) Uani 1 d . . .
F33 F 1.01546(14) 0.39758(13) 0.66042(13) 0.0436(5) Uani 1 d . . .
F34 F 1.07364(14) 0.31391(9) 0.76565(17) 0.0424(5) Uani 1 d . . .
F35 F 1.15585(11) 0.41529(10) 0.75702(14) 0.0294(4) Uani 1 d . . .
C36 C 0.4140(2) 0.35649(15) 0.8852(2) 0.0167(5) Uani 1 d . . .
F37 F 0.35123(13) 0.34163(11) 0.80173(13) 0.0335(5) Uani 1 d . . .
F38 F 0.35730(12) 0.38263(9) 0.95759(12) 0.0256(4) Uani 1 d . . .
F39 F 0.48225(13) 0.40579(9) 0.86186(15) 0.0344(4) Uani 1 d . . .
S40 S 0.48106(5) 0.27255(4) 0.93087(4) 0.01049(12) Uani 1 d . . .
O41 O 0.53167(13) 0.24855(9) 0.84024(13) 0.0132(4) Uani 1 d . . .
O42 O 0.54397(13) 0.29065(10) 1.02188(13) 0.0155(4) Uani 1 d . . .
N43 N 0.38941(15) 0.22134(12) 0.96006(15) 0.0137(4) Uani 1 d . . .
S44 S 0.31868(5) 0.17217(4) 0.88186(5) 0.01351(13) Uani 1 d . . .
O45 O 0.34149(14) 0.17357(13) 0.77578(14) 0.0271(5) Uani 1 d . . .
O46 O 0.21268(13) 0.18035(11) 0.90431(14) 0.0213(4) Uani 1 d . . .
C47 C 0.3543(3) 0.08084(17) 0.9285(3) 0.0331(8) Uani 1 d . . .
F48 F 0.45429(16) 0.06940(12) 0.92138(19) 0.0602(7) Uani 1 d . . .
F49 F 0.30045(17) 0.03288(10) 0.86995(17) 0.0521(6) Uani 1 d . . .
F50 F 0.33266(17) 0.07291(11) 1.02631(15) 0.0506(6) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.3425(18) . ?
Dy1 O2 2.3202(18) . ?
Dy1 O3 2.3431(17) . ?
Dy1 O4 2.3597(17) . ?
Dy1 O5 2.2997(18) . ?
Dy1 O11 2.3950(16) . ?
Dy1 O26 2.4240(16) . ?
Dy1 O41 2.3542(17) . ?
C6 F7 1.329(3) . ?
C6 F8 1.321(3) . ?
C6 F9 1.326(3) . ?
C6 S10 1.828(3) . ?
S10 O11 1.4491(17) . ?
S10 O12 1.4388(17) . ?
S10 N13 1.565(2) . ?
N13 S14 1.599(2) . ?
S14 O15 1.4294(18) . ?
S14 O16 1.4306(17) . ?
S14 C17 1.830(3) . ?
C17 F18 1.332(3) . ?
C17 F19 1.326(3) . ?
C17 F20 1.320(3) . ?
C21 F22 1.324(3) . ?
C21 F23 1.329(3) . ?
C21 F24 1.318(3) . ?
C21 S25 1.840(3) . ?
S25 O26 1.4501(17) . ?
S25 O27 1.4194(18) . ?
S25 N28 1.570(2) . ?
N28 S29 1.596(2) . ?
S29 O30 1.4290(18) . ?
S29 O31 1.4337(18) . ?
S29 C32 1.828(3) . ?
C32 F33 1.318(3) . ?
C32 F34 1.321(3) . ?
C32 F35 1.321(3) . ?
C36 F37 1.327(3) . ?
C36 F38 1.317(3) . ?
C36 F39 1.312(3) . ?
C36 S40 1.843(3) . ?
S40 O41 1.4480(18) . ?
S40 O42 1.4177(17) . ?
S40 N43 1.575(2) . ?
N43 S44 1.591(2) . ?
S44 O45 1.4211(19) . ?
S44 O46 1.4232(18) . ?
S44 C47 1.829(3) . ?
C47 F48 1.314(4) . ?
C47 F49 1.324(3) . ?
C47 F50 1.320(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
_geom_angle_publ_flag
O1 Dy1 O3 72.57(6) . . ?
O1 Dy1 O4 143.97(6) . . ?
O1 Dy1 O11 74.18(6) . . ?
O1 Dy1 O26 75.88(6) . . ?
O1 Dy1 O41 145.40(6) . . ?
O2 Dy1 O1 99.08(7) . . ?
O2 Dy1 O3 77.48(7) . . ?
O2 Dy1 O4 74.35(6) . . ?
O2 Dy1 O11 72.82(6) . . ?
O2 Dy1 O26 143.13(6) . . ?
O2 Dy1 O41 89.96(6) . . ?
O3 Dy1 O4 71.42(6) . . ?
O3 Dy1 O11 130.55(6) . . ?
O3 Dy1 O26 132.20(6) . . ?
O3 Dy1 O41 141.96(6) . . ?
O4 Dy1 O11 133.14(6) . . ?
O4 Dy1 O26 130.07(6) . . ?
O5 Dy1 O1 91.08(7) . . ?
O5 Dy1 O2 146.83(6) . . ?
O5 Dy1 O3 75.65(7) . . ?
O5 Dy1 O4 78.91(7) . . ?
O5 Dy1 O11 140.26(6) . . ?
O5 Dy1 O26 69.97(6) . . ?
O5 Dy1 O41 99.41(7) . . ?
O11 Dy1 O26 70.68(6) . . ?
O41 Dy1 O4 70.62(6) . . ?
O41 Dy1 O11 76.85(6) . . ?
O41 Dy1 O26 77.00(6) . . ?
F7 C6 S10 109.16(18) . . ?
F8 C6 F7 109.3(2) . . ?
F8 C6 F9 109.3(2) . . ?
F8 C6 S10 110.19(17) . . ?
F9 C6 F7 108.9(2) . . ?
F9 C6 S10 109.93(18) . . ?
O11 S10 C6 102.80(11) . . ?
O11 S10 N13 108.00(10) . . ?
O12 S10 C6 105.38(11) . . ?
O12 S10 O11 116.41(10) . . ?
O12 S10 N13 117.94(11) . . ?
N13 S10 C6 104.43(12) . . ?
S10 O11 Dy1 150.21(11) . . ?
S10 N13 S14 123.66(13) . . ?
N13 S14 C17 101.29(12) . . ?
O15 S14 N13 108.38(11) . . ?
O15 S14 O16 119.34(10) . . ?
O15 S14 C17 104.18(12) . . ?
O16 S14 N13 115.06(11) . . ?
O16 S14 C17 106.39(11) . . ?
F18 C17 S14 109.94(18) . . ?
F19 C17 S14 108.78(18) . . ?
F19 C17 F18 109.1(2) . . ?
F20 C17 S14 110.43(18) . . ?
F20 C17 F18 109.1(2) . . ?
F20 C17 F19 109.5(2) . . ?
F22 C21 F23 108.8(2) . . ?
F22 C21 S25 110.98(18) . . ?
F23 C21 S25 108.91(18) . . ?
F24 C21 F22 109.5(2) . . ?
F24 C21 F23 109.3(2) . . ?
F24 C21 S25 109.25(18) . . ?
O26 S25 C21 104.14(11) . . ?
O26 S25 N28 107.12(11) . . ?
O27 S25 C21 104.72(12) . . ?
O27 S25 O26 117.56(10) . . ?
O27 S25 N28 117.16(11) . . ?
N28 S25 C21 104.48(12) . . ?
S25 O26 Dy1 153.42(10) . . ?
S25 N28 S29 123.31(14) . . ?
N28 S29 C32 98.39(12) . . ?
O30 S29 N28 116.02(11) . . ?
O30 S29 O31 117.94(11) . . ?
O30 S29 C32 106.12(13) . . ?
O31 S29 N28 111.36(11) . . ?
O31 S29 C32 104.05(12) . . ?
F33 C32 S29 111.15(19) . . ?
F33 C32 F34 109.0(3) . . ?
F33 C32 F35 108.8(2) . . ?
F34 C32 S29 110.5(2) . . ?
F35 C32 S29 108.60(19) . . ?
F35 C32 F34 108.8(2) . . ?
F37 C36 S40 109.38(19) . . ?
F38 C36 F37 108.4(2) . . ?
F38 C36 S40 110.37(18) . . ?
F39 C36 F37 109.6(2) . . ?
F39 C36 F38 109.0(2) . . ?
F39 C36 S40 110.11(18) . . ?
O41 S40 C36 102.91(11) . . ?
O41 S40 N43 113.57(11) . . ?
O42 S40 C36 107.22(12) . . ?
O42 S40 O41 118.51(11) . . ?
O42 S40 N43 109.56(11) . . ?
N43 S40 C36 103.52(12) . . ?
S40 O41 Dy1 159.66(11) . . ?
S40 N43 S44 126.24(13) . . ?
N43 S44 C47 101.11(13) . . ?
O45 S44 N43 116.92(11) . . ?
O45 S44 O46 117.50(12) . . ?
O45 S44 C47 105.64(15) . . ?
O46 S44 N43 108.93(11) . . ?
O46 S44 C47 104.54(14) . . ?
F48 C47 S44 110.3(2) . . ?
F48 C47 F49 109.2(3) . . ?
F48 C47 F50 108.9(3) . . ?
F49 C47 S44 108.2(2) . . ?
F50 C47 S44 110.5(2) . . ?
F50 C47 F49 109.6(3) . . ?

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 N43 0.835(10) 2.103(12) 2.927(3) 169(3) 4_665
O1 H1B N28 0.837(10) 2.263(19) 3.006(3) 148(3) .
O2 H2A O30 0.836(10) 2.051(14) 2.854(3) 161(3) 2_646
O2 H2B N13 0.833(10) 2.285(17) 2.982(3) 141(2) .
O2 H2B O27 0.833(10) 2.24(2) 2.798(3) 125(2) 2_646
O3 H3A O46 0.829(10) 1.894(10) 2.721(3) 176(3) 4_665
O3 H3B O31 0.832(10) 1.934(10) 2.765(3) 178(3) 4_565
O4 H4A O12 0.839(10) 2.069(14) 2.875(2) 161(3) 4_565
O4 H4B O45 0.840(10) 1.888(12) 2.711(3) 166(3) .
O5 H5A O15 0.835(10) 1.884(12) 2.708(3) 169(3) 2_656
O5 H5B O12 0.836(10) 2.35(2) 3.037(3) 140(3) 4_565
O5 H5B O16 0.836(10) 2.16(3) 2.809(2) 134(3) 4_565


_olex2_date_sample_data_collection 2013-06-26
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb171
_database_code_depnum_ccdc_archive 'CCDC 1409131'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
Triaqua-tris(bis(trifluoromethylsulfonyl)imide-O,O')-cerium(iii)
;
_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_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ce C6 F18 S6 O12 N3 O8 H16'
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'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'
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'

_cell_length_a                   18.51715(13)
_cell_length_b                   18.51715(13)
_cell_length_c                   18.51715(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6349.25(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5090
_cell_measurement_theta_min      3.4670
_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_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_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_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      
;
#__ type_ start__ end____ width___ exp.time_
  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_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                4510
_reflns_number_total             4839
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_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_coef       ?
_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_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.023
_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
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
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 . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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) .


_olex2_date_sample_data_collection 2013-06-28
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb175
_database_code_depnum_ccdc_archive 'CCDC 1409132'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
pentaaqua-tris(bis(trifluoromethylsulfonyl)imide-O)-terbium(iii) 
;
_chemical_formula_moiety         'C6 H10 F18 N3 O17 S6 Tb'
_chemical_formula_sum            'C6 H10 F18 N3 O17 S6 Tb'
_chemical_formula_weight         1089.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Tb C6 F18 S6 O12 N3 O8 H16'
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'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9085(3)
_cell_length_b                   18.3690(4)
_cell_length_c                   12.9307(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.275(2)
_cell_angle_gamma                90.00
_cell_volume                     3057.56(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9620
_cell_measurement_theta_min      3.3560
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74452
_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    2.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14352
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.09
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -93.00  -66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8388 -178.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega   48.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7138  178.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega  -46.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7138    0.0000 -120.0000 129

#__ type_ start__ end____ width___ exp.time_
  4 omega  -26.00   -1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7138  -19.0000 -150.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0318214000
_diffrn_orient_matrix_UB_12      0.0035713000
_diffrn_orient_matrix_UB_13      -0.0469278000
_diffrn_orient_matrix_UB_21      -0.0273384000
_diffrn_orient_matrix_UB_22      -0.0320129000
_diffrn_orient_matrix_UB_23      0.0120688000
_diffrn_orient_matrix_UB_31      -0.0357622000
_diffrn_orient_matrix_UB_32      0.0212666000
_diffrn_orient_matrix_UB_33      0.0260476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_number_gt                6201
_reflns_number_total             6942
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6942
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0200
_refine_ls_restrained_S_all      1.017
_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)+(0.0166P)²+2.1535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0454
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
 O2-H2A = O2-H2B
 0.84 with sigma of 0.01
 H2A-H2B
 1.35 with sigma of 0.02
 O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 H3A-H3B
 1.35 with sigma of 0.02
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
 H4A-H4B
 1.35 with sigma of 0.02
 O5-H5A = O5-H5B
 0.84 with sigma of 0.01
 H5A-H5B
 1.35 with sigma of 0.02
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_refinement_flags_posn
Tb1 Tb 0.650962(8) 0.245625(5) 0.710038(8) 0.00696(4) Uani 1 d . . .
O1 O 0.82420(13) 0.26655(10) 0.67118(13) 0.0149(3) Uani 1 d . . D
H1A H 0.849(2) 0.2702(17) 0.6133(12) 0.044(10) Uiso 1 d . . D
H1B H 0.8623(19) 0.2920(14) 0.7118(17) 0.035(9) Uiso 1 d . . D
O2 O 0.65397(14) 0.11887(9) 0.71976(14) 0.0178(4) Uani 1 d . . D
H2A H 0.6114(15) 0.0888(11) 0.694(2) 0.025(8) Uiso 1 d . . D
H2B H 0.7057(14) 0.0949(13) 0.743(2) 0.036(9) Uiso 1 d . . D
O3 O 0.66510(13) 0.21179(10) 0.53620(13) 0.0156(4) Uani 1 d . . D
H3A H 0.676(3) 0.2412(12) 0.4894(17) 0.041(10) Uiso 1 d . . D
H3B H 0.632(2) 0.1763(11) 0.511(2) 0.036(9) Uiso 1 d . . D
O4 O 0.48526(12) 0.20708(10) 0.63951(13) 0.0149(3) Uani 1 d . . D
H4A H 0.4645(19) 0.2194(16) 0.5799(10) 0.028(8) Uiso 1 d . . D
H4B H 0.4342(14) 0.2000(15) 0.6740(17) 0.025(8) Uiso 1 d . . D
O5 O 0.59632(14) 0.34721(9) 0.61431(14) 0.0185(4) Uani 1 d . . D
H5A H 0.592(2) 0.3889(9) 0.639(2) 0.043(10) Uiso 1 d . . D
H5B H 0.570(2) 0.3478(17) 0.5534(11) 0.051(11) Uiso 1 d . . D
C6 C 0.77882(19) 0.13571(14) 1.02966(19) 0.0182(5) Uani 1 d . . .
F7 F 0.76062(12) 0.19077(8) 1.09251(11) 0.0278(4) Uani 1 d . . .
F8 F 0.68940(11) 0.10339(9) 1.00136(12) 0.0277(4) Uani 1 d . . .
F9 F 0.84178(12) 0.08879(8) 1.08017(11) 0.0248(3) Uani 1 d . . .
S10 S 0.83903(4) 0.17068(3) 0.91590(4) 0.00996(11) Uani 1 d . . .
O11 O 0.75648(12) 0.21347(8) 0.86416(12) 0.0125(3) Uani 1 d . . .
O12 O 0.92965(12) 0.20957(9) 0.95653(12) 0.0146(3) Uani 1 d . . .
N13 N 0.85538(14) 0.10167(10) 0.84819(15) 0.0129(4) Uani 1 d . . .
S14 S 0.96288(4) 0.05801(3) 0.84912(4) 0.01054(11) Uani 1 d . . .
O15 O 0.94029(12) -0.01577(8) 0.82085(13) 0.0158(3) Uani 1 d . . .
O16 O 1.03503(12) 0.07305(9) 0.93577(12) 0.0143(3) Uani 1 d . . .
C17 C 1.01981(19) 0.09623(13) 0.73488(19) 0.0177(5) Uani 1 d . . .
F18 F 0.95872(12) 0.08199(9) 0.65028(11) 0.0276(4) Uani 1 d . . .
F19 F 1.11190(12) 0.06621(9) 0.72641(12) 0.0294(4) Uani 1 d . . .
F20 F 1.03065(12) 0.16738(8) 0.74521(11) 0.0237(3) Uani 1 d . . .
C21 C 0.75828(19) 0.40976(14) 0.98693(19) 0.0189(5) Uani 1 d . . .
F22 F 0.76862(12) 0.34341(8) 1.02586(11) 0.0251(3) Uani 1 d . . .
F23 F 0.83050(12) 0.45228(9) 1.03340(12) 0.0317(4) Uani 1 d . . .
F24 F 0.66526(11) 0.43540(9) 1.00345(12) 0.0264(4) Uani 1 d . . .
S25 S 0.77416(4) 0.40955(3) 0.84669(4) 0.01021(11) Uani 1 d . . .
O26 O 0.70012(11) 0.35568(8) 0.80561(12) 0.0113(3) Uani 1 d . . .
O27 O 0.75729(12) 0.48292(9) 0.81501(14) 0.0187(4) Uani 1 d . . .
N28 N 0.88575(14) 0.37730(10) 0.83633(15) 0.0131(4) Uani 1 d . . .
S29 S 0.99008(4) 0.42370(3) 0.85592(4) 0.01168(11) Uani 1 d . . .
O30 O 0.98108(12) 0.49972(9) 0.83454(14) 0.0191(4) Uani 1 d . . .
O31 O 1.04856(13) 0.40199(9) 0.94953(13) 0.0199(4) Uani 1 d . . .
C32 C 1.06285(19) 0.38498(15) 0.7532(2) 0.0217(6) Uani 1 d . . .
F33 F 1.01544(13) 0.39774(12) 0.66096(13) 0.0452(5) Uani 1 d . . .
F34 F 1.07383(14) 0.31387(9) 0.76569(16) 0.0433(5) Uani 1 d . . .
F35 F 1.15603(11) 0.41506(9) 0.75723(13) 0.0298(4) Uani 1 d . . .
C36 C 0.41391(18) 0.35575(13) 0.88569(19) 0.0169(5) Uani 1 d . . .
F37 F 0.35163(13) 0.34148(10) 0.80205(12) 0.0346(4) Uani 1 d . . .
F38 F 0.35706(12) 0.38232(8) 0.95759(12) 0.0270(4) Uani 1 d . . .
F39 F 0.48262(12) 0.40526(9) 0.86212(15) 0.0361(4) Uani 1 d . . .
S40 S 0.48074(4) 0.27237(3) 0.93113(4) 0.01073(11) Uani 1 d . . .
O41 O 0.53185(12) 0.24850(8) 0.84085(12) 0.0140(3) Uani 1 d . . .
O42 O 0.54345(12) 0.29043(9) 1.02221(12) 0.0154(3) Uani 1 d . . .
N43 N 0.38902(15) 0.22124(11) 0.95994(15) 0.0145(4) Uani 1 d . . .
S44 S 0.31871(4) 0.17198(3) 0.88158(4) 0.01363(12) Uani 1 d . . .
O45 O 0.34149(13) 0.17375(11) 0.77555(13) 0.0272(5) Uani 1 d . . .
O46 O 0.21269(12) 0.18023(10) 0.90396(14) 0.0211(4) Uani 1 d . . .
C47 C 0.3546(2) 0.08072(15) 0.9284(3) 0.0349(7) Uani 1 d . . .
F48 F 0.45458(15) 0.06972(11) 0.92081(19) 0.0613(6) Uani 1 d . . .
F49 F 0.30048(16) 0.03305(9) 0.86948(16) 0.0514(5) Uani 1 d . . .
F50 F 0.33303(17) 0.07271(10) 1.02562(15) 0.0514(5) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.3598(16) . ?
Tb1 O2 2.3319(16) . ?
Tb1 O3 2.3524(16) . ?
Tb1 O4 2.3701(16) . ?
Tb1 O5 2.3198(16) . ?
Tb1 O11 2.4023(16) . ?
Tb1 O26 2.4289(15) . ?
Tb1 O41 2.3697(15) . ?
C6 F7 1.329(3) . ?
C6 F8 1.325(3) . ?
C6 F9 1.323(3) . ?
C6 S10 1.831(2) . ?
S10 O11 1.4472(16) . ?
S10 O12 1.4364(16) . ?
S10 N13 1.5639(19) . ?
N13 S14 1.6020(19) . ?
S14 O15 1.4280(16) . ?
S14 O16 1.4296(17) . ?
S14 C17 1.838(2) . ?
C17 F18 1.326(3) . ?
C17 F19 1.322(3) . ?
C17 F20 1.320(3) . ?
C21 F22 1.322(3) . ?
C21 F23 1.325(3) . ?
C21 F24 1.322(3) . ?
C21 S25 1.840(3) . ?
S25 O26 1.4489(16) . ?
S25 O27 1.4206(17) . ?
S25 N28 1.5725(19) . ?
N28 S29 1.5979(19) . ?
S29 O30 1.4265(17) . ?
S29 O31 1.4344(18) . ?
S29 C32 1.827(3) . ?
C32 F33 1.320(3) . ?
C32 F34 1.322(3) . ?
C32 F35 1.321(3) . ?
C36 F37 1.325(3) . ?
C36 F38 1.320(3) . ?
C36 F39 1.322(3) . ?
C36 S40 1.833(3) . ?
S40 O41 1.4510(16) . ?
S40 O42 1.4178(17) . ?
S40 N43 1.578(2) . ?
N43 S44 1.591(2) . ?
S44 O45 1.4239(17) . ?
S44 O46 1.4277(16) . ?
S44 C47 1.830(3) . ?
C47 F48 1.318(4) . ?
C47 F49 1.324(3) . ?
C47 F50 1.316(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
_geom_angle_publ_flag
O1 Tb1 O4 144.01(6) . . ?
O1 Tb1 O11 74.28(6) . . ?
O1 Tb1 O26 75.93(5) . . ?
O1 Tb1 O41 145.48(6) . . ?
O2 Tb1 O1 99.32(6) . . ?
O2 Tb1 O3 77.61(6) . . ?
O2 Tb1 O4 74.54(6) . . ?
O2 Tb1 O11 72.76(6) . . ?
O2 Tb1 O26 143.22(6) . . ?
O2 Tb1 O41 89.59(6) . . ?
O3 Tb1 O1 72.38(6) . . ?
O3 Tb1 O4 71.67(6) . . ?
O3 Tb1 O11 130.41(6) . . ?
O3 Tb1 O26 132.08(6) . . ?
O3 Tb1 O41 142.06(6) . . ?
O4 Tb1 O11 133.27(6) . . ?
O4 Tb1 O26 129.68(5) . . ?
O5 Tb1 O1 90.61(6) . . ?
O5 Tb1 O2 146.62(6) . . ?
O5 Tb1 O3 75.22(6) . . ?
O5 Tb1 O4 78.77(6) . . ?
O5 Tb1 O11 140.48(6) . . ?
O5 Tb1 O26 70.09(6) . . ?
O5 Tb1 O41 100.10(6) . . ?
O11 Tb1 O26 70.86(5) . . ?
O41 Tb1 O4 70.51(6) . . ?
O41 Tb1 O11 76.78(5) . . ?
O41 Tb1 O26 77.12(5) . . ?
F7 C6 S10 109.23(17) . . ?
F8 C6 F7 108.64(19) . . ?
F8 C6 S10 110.40(17) . . ?
F9 C6 F7 108.9(2) . . ?
F9 C6 F8 109.6(2) . . ?
F9 C6 S10 110.08(16) . . ?
O11 S10 C6 102.71(10) . . ?
O11 S10 N13 107.87(10) . . ?
O12 S10 C6 105.28(11) . . ?
O12 S10 O11 116.78(10) . . ?
O12 S10 N13 117.88(10) . . ?
N13 S10 C6 104.39(11) . . ?
S10 O11 Tb1 150.39(10) . . ?
S10 N13 S14 123.69(12) . . ?
N13 S14 C17 101.58(11) . . ?
O15 S14 N13 108.24(10) . . ?
O15 S14 O16 119.52(10) . . ?
O15 S14 C17 104.07(11) . . ?
O16 S14 N13 114.99(10) . . ?
O16 S14 C17 106.26(11) . . ?
F18 C17 S14 109.81(16) . . ?
F19 C17 S14 108.85(17) . . ?
F19 C17 F18 109.4(2) . . ?
F20 C17 S14 110.04(16) . . ?
F20 C17 F18 109.3(2) . . ?
F20 C17 F19 109.4(2) . . ?
F22 C21 F23 108.8(2) . . ?
F22 C21 F24 109.5(2) . . ?
F22 C21 S25 110.98(16) . . ?
F23 C21 S25 108.77(16) . . ?
F24 C21 F23 109.5(2) . . ?
F24 C21 S25 109.22(18) . . ?
O26 S25 C21 104.11(10) . . ?
O26 S25 N28 107.15(10) . . ?
O27 S25 C21 104.85(11) . . ?
O27 S25 O26 117.36(10) . . ?
O27 S25 N28 117.03(10) . . ?
N28 S25 C21 104.76(11) . . ?
S25 O26 Tb1 153.53(9) . . ?
S25 N28 S29 123.51(12) . . ?
N28 S29 C32 98.62(11) . . ?
O30 S29 N28 115.84(10) . . ?
O30 S29 O31 117.77(11) . . ?
O30 S29 C32 106.20(12) . . ?
O31 S29 N28 111.70(10) . . ?
O31 S29 C32 103.79(11) . . ?
F33 C32 S29 111.03(18) . . ?
F33 C32 F34 108.9(2) . . ?
F33 C32 F35 108.7(2) . . ?
F34 C32 S29 110.61(18) . . ?
F35 C32 S29 108.93(18) . . ?
F35 C32 F34 108.6(2) . . ?
F37 C36 S40 109.80(17) . . ?
F38 C36 F37 108.22(19) . . ?
F38 C36 F39 109.0(2) . . ?
F38 C36 S40 110.86(17) . . ?
F39 C36 F37 108.9(2) . . ?
F39 C36 S40 109.94(16) . . ?
O41 S40 C36 103.06(10) . . ?
O41 S40 N43 113.85(10) . . ?
O42 S40 C36 107.26(11) . . ?
O42 S40 O41 118.25(10) . . ?
O42 S40 N43 109.59(10) . . ?
N43 S40 C36 103.28(11) . . ?
S40 O41 Tb1 159.91(10) . . ?
S40 N43 S44 126.20(12) . . ?
N43 S44 C47 101.09(13) . . ?
O45 S44 N43 116.83(10) . . ?
O45 S44 O46 117.55(11) . . ?
O45 S44 C47 105.89(14) . . ?
O46 S44 N43 108.69(10) . . ?
O46 S44 C47 104.64(13) . . ?
F48 C47 S44 109.9(2) . . ?
F48 C47 F49 109.5(3) . . ?
F49 C47 S44 107.8(2) . . ?
F50 C47 S44 110.6(2) . . ?
F50 C47 F48 109.4(3) . . ?
F50 C47 F49 109.6(3) . . ?

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 N43 0.837(10) 2.093(10) 2.924(2) 172(3) 4_665
O1 H1B N28 0.836(10) 2.251(16) 3.013(3) 152(3) .
O2 H2A O30 0.833(10) 2.042(12) 2.853(2) 164(3) 2_646
O2 H2B N13 0.837(10) 2.281(17) 2.996(3) 144(2) .
O2 H2B O27 0.837(10) 2.25(2) 2.798(2) 123(2) 2_646
O3 H3A O46 0.831(10) 1.899(11) 2.719(2) 169(3) 4_665
O3 H3B O31 0.828(10) 1.936(10) 2.763(2) 176(3) 4_565
O4 H4A O12 0.829(10) 2.083(15) 2.864(2) 157(3) 4_565
O4 H4B O45 0.833(9) 1.903(11) 2.720(2) 166(3) .
O5 H5A O15 0.833(10) 1.882(12) 2.706(2) 169(3) 2_656
O5 H5B O12 0.834(10) 2.37(2) 3.037(2) 137(3) 4_565
O5 H5B O16 0.834(10) 2.13(2) 2.798(2) 137(3) 4_565


_olex2_date_sample_data_collection 2013-07-09
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nrb176
_database_code_depnum_ccdc_archive 'CCDC 1409133'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;
_audit_creation_date             2015-06-19
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5047)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
pentaaqua-tris(bis(trifluoromethylsulfonyl)imide-O)-erbium(iii) 
;
_chemical_formula_moiety         'C6 H10 Er F18 N3 O17 S6'
_chemical_formula_sum            'C6 H10 Er F18 N3 O17 S6'
_chemical_formula_weight         1097.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Er C6 F18 S6 O12 N3 O5 H10'
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'
Er Er -0.2586 4.9576 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.8788(4)
_cell_length_b                   18.2797(7)
_cell_length_c                   12.8814(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.524(3)
_cell_angle_gamma                90.00
_cell_volume                     3023.10(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9470
_cell_measurement_theta_min      3.3610
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84822
_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    2.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14426
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.74
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00   53.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000   60.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -28.00   27.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -57.0000 -180.0000 55

#__ type_ start__ end____ width___ exp.time_
  3 omega   15.00   89.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000  120.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0504347000
_diffrn_orient_matrix_UB_12      -0.0125693000
_diffrn_orient_matrix_UB_13      0.0100775000
_diffrn_orient_matrix_UB_21      -0.0118076000
_diffrn_orient_matrix_UB_22      -0.0059996000
_diffrn_orient_matrix_UB_23      -0.0540237000
_diffrn_orient_matrix_UB_31      0.0193802000
_diffrn_orient_matrix_UB_32      -0.0361736000
_diffrn_orient_matrix_UB_33      0.0054812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_number_gt                6279
_reflns_number_total             6912
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_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)'
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0173
_refine_ls_restrained_S_all      1.023
_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)+(0.0167P)²+1.9627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0411
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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
 O2-H2A = O2-H2B
 0.84 with sigma of 0.01
 H2A-H2B
 1.35 with sigma of 0.02
 O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 H3A-H3B
 1.35 with sigma of 0.02
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
 H4A-H4B
 1.35 with sigma of 0.02
 O5-H5A = O5-H5B
 0.84 with sigma of 0.01
 H5A-H5B
 1.35 with sigma of 0.02
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_refinement_flags_posn
Er1 Er 0.651335(6) 0.245206(5) 0.710173(6) 0.00641(3) Uani 1 d . . .
O1 O 0.82269(11) 0.26586(9) 0.67218(12) 0.0133(3) Uani 1 d . . D
H1A H 0.848(2) 0.2662(16) 0.6145(11) 0.038(9) Uiso 1 d . . D
H1B H 0.8592(18) 0.2909(14) 0.7144(16) 0.038(9) Uiso 1 d . . D
O2 O 0.65509(11) 0.11989(8) 0.71970(12) 0.0154(3) Uani 1 d . . D
H2A H 0.6131(15) 0.0898(11) 0.692(2) 0.030(8) Uiso 1 d . . D
H2B H 0.7085(13) 0.0966(13) 0.740(2) 0.043(9) Uiso 1 d . . D
O3 O 0.66643(11) 0.21135(9) 0.53846(11) 0.0142(3) Uani 1 d . . D
H3A H 0.679(2) 0.2422(11) 0.4940(16) 0.023(8) Uiso 1 d . . D
H3B H 0.634(2) 0.1755(10) 0.513(2) 0.043(9) Uiso 1 d . . D
O4 O 0.48762(11) 0.20624(9) 0.64013(11) 0.0136(3) Uani 1 d . . D
H4A H 0.4643(19) 0.2206(16) 0.5817(11) 0.036(8) Uiso 1 d . . D
H4B H 0.4374(14) 0.1994(16) 0.6761(16) 0.032(8) Uiso 1 d . . D
O5 O 0.59551(13) 0.34546(9) 0.61615(12) 0.0174(3) Uani 1 d . . D
H5A H 0.593(2) 0.3873(8) 0.641(2) 0.040(9) Uiso 1 d . . D
H5B H 0.572(2) 0.3477(17) 0.5542(10) 0.058(11) Uiso 1 d . . D
C6 C 0.77788(17) 0.13639(13) 1.03025(17) 0.0167(4) Uani 1 d . . .
F7 F 0.75987(11) 0.19175(8) 1.09306(10) 0.0252(3) Uani 1 d . . .
F8 F 0.68841(10) 0.10389(8) 1.00149(11) 0.0262(3) Uani 1 d . . .
F9 F 0.84120(10) 0.08941(8) 1.08080(10) 0.0233(3) Uani 1 d . . .
S10 S 0.83864(4) 0.17128(3) 0.91562(4) 0.00911(10) Uani 1 d . . .
O11 O 0.75586(10) 0.21413(8) 0.86335(11) 0.0115(3) Uani 1 d . . .
O12 O 0.92942(11) 0.21067(8) 0.95620(11) 0.0127(3) Uani 1 d . . .
N13 N 0.85551(12) 0.10194(10) 0.84808(13) 0.0119(4) Uani 1 d . . .
S14 S 0.96327(4) 0.05799(3) 0.84982(4) 0.00940(10) Uani 1 d . . .
O15 O 0.94084(11) -0.01611(8) 0.82224(12) 0.0144(3) Uani 1 d . . .
O16 O 1.03546(10) 0.07369(8) 0.93688(11) 0.0130(3) Uani 1 d . . .
C17 C 1.02058(16) 0.09586(13) 0.73492(16) 0.0160(4) Uani 1 d . . .
F18 F 0.95986(11) 0.08098(8) 0.64999(10) 0.0258(3) Uani 1 d . . .
F19 F 1.11327(10) 0.06546(8) 0.72690(11) 0.0273(3) Uani 1 d . . .
F20 F 1.03128(10) 0.16722(7) 0.74456(10) 0.0223(3) Uani 1 d . . .
C21 C 0.75777(16) 0.40995(13) 0.98682(17) 0.0168(5) Uani 1 d . . .
F22 F 0.76913(10) 0.34396(8) 1.02674(10) 0.0229(3) Uani 1 d . . .
F23 F 0.83039(10) 0.45361(9) 1.03212(11) 0.0297(4) Uani 1 d . . .
F24 F 0.66464(10) 0.43583(8) 1.00333(11) 0.0251(3) Uani 1 d . . .
S25 S 0.77342(4) 0.40918(3) 0.84557(4) 0.00902(10) Uani 1 d . . .
O26 O 0.69928(10) 0.35464(8) 0.80508(11) 0.0101(3) Uani 1 d . . .
O27 O 0.75645(11) 0.48271(8) 0.81285(13) 0.0170(3) Uani 1 d . . .
N28 N 0.88552(12) 0.37670(9) 0.83537(14) 0.0113(3) Uani 1 d . . .
S29 S 0.98998(4) 0.42353(3) 0.85548(4) 0.01039(10) Uani 1 d . . .
O30 O 0.98090(11) 0.49966(8) 0.83371(13) 0.0178(3) Uani 1 d . . .
O31 O 1.04762(11) 0.40169(9) 0.94992(12) 0.0174(3) Uani 1 d . . .
C32 C 1.06386(17) 0.38433(13) 0.75244(19) 0.0203(5) Uani 1 d . . .
F33 F 1.01672(11) 0.39655(11) 0.65994(11) 0.0419(5) Uani 1 d . . .
F34 F 1.07539(12) 0.31324(8) 0.76610(15) 0.0412(4) Uani 1 d . . .
F35 F 1.15708(9) 0.41494(8) 0.75710(12) 0.0277(3) Uani 1 d . . .
C36 C 0.41480(16) 0.35635(13) 0.88444(17) 0.0159(4) Uani 1 d . . .
F37 F 0.35264(11) 0.34132(9) 0.80088(11) 0.0326(4) Uani 1 d . . .
F38 F 0.35776(10) 0.38231(8) 0.95720(11) 0.0247(3) Uani 1 d . . .
F39 F 0.48315(11) 0.40602(8) 0.86116(13) 0.0326(4) Uani 1 d . . .
S40 S 0.48263(4) 0.27255(3) 0.93042(4) 0.00938(10) Uani 1 d . . .
O41 O 0.53312(11) 0.24834(8) 0.83953(11) 0.0124(3) Uani 1 d . . .
O42 O 0.54589(11) 0.29097(9) 1.02147(11) 0.0142(3) Uani 1 d . . .
N43 N 0.39095(13) 0.22117(11) 0.95987(13) 0.0129(4) Uani 1 d . . .
S44 S 0.31954(4) 0.17188(3) 0.88187(4) 0.01221(10) Uani 1 d . . .
O45 O 0.34259(12) 0.17300(11) 0.77555(12) 0.0255(4) Uani 1 d . . .
O46 O 0.21333(11) 0.18099(9) 0.90457(12) 0.0199(3) Uani 1 d . . .
C47 C 0.3545(2) 0.08050(14) 0.9295(2) 0.0324(6) Uani 1 d . . .
F48 F 0.45478(13) 0.06841(10) 0.92232(17) 0.0569(6) Uani 1 d . . .
F49 F 0.29992(14) 0.03220(9) 0.87080(15) 0.0498(5) Uani 1 d . . .
F50 F 0.33281(15) 0.07276(9) 1.02757(13) 0.0482(5) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.3286(14) . ?
Er1 O2 2.2943(15) . ?
Er1 O3 2.3198(14) . ?
Er1 O4 2.3381(14) . ?
Er1 O5 2.2814(15) . ?
Er1 O11 2.3684(13) . ?
Er1 O26 2.3997(14) . ?
Er1 O41 2.3447(14) . ?
C6 F7 1.327(3) . ?
C6 F8 1.323(2) . ?
C6 F9 1.320(2) . ?
C6 S10 1.839(2) . ?
S10 O11 1.4458(14) . ?
S10 O12 1.4361(14) . ?
S10 N13 1.5623(18) . ?
N13 S14 1.6023(17) . ?
S14 O15 1.4242(15) . ?
S14 O16 1.4282(14) . ?
S14 C17 1.840(2) . ?
C17 F18 1.322(2) . ?
C17 F19 1.328(3) . ?
C17 F20 1.317(3) . ?
C21 F22 1.315(3) . ?
C21 F23 1.329(2) . ?
C21 F24 1.322(2) . ?
C21 S25 1.846(2) . ?
S25 O26 1.4488(14) . ?
S25 O27 1.4204(15) . ?
S25 N28 1.5760(17) . ?
N28 S29 1.5984(17) . ?
S29 O30 1.4226(15) . ?
S29 O31 1.4310(15) . ?
S29 C32 1.838(2) . ?
C32 F33 1.313(3) . ?
C32 F34 1.318(3) . ?
C32 F35 1.322(2) . ?
C36 F37 1.319(2) . ?
C36 F38 1.324(2) . ?
C36 F39 1.316(3) . ?
C36 S40 1.838(2) . ?
S40 O41 1.4524(15) . ?
S40 O42 1.4150(14) . ?
S40 N43 1.5783(18) . ?
N43 S44 1.5878(18) . ?
S44 O45 1.4242(16) . ?
S44 O46 1.4308(15) . ?
S44 C47 1.824(3) . ?
C47 F48 1.320(3) . ?
C47 F49 1.328(3) . ?
C47 F50 1.323(3) . ?

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
_geom_angle_publ_flag
O1 Er1 O4 144.00(5) . . ?
O1 Er1 O11 74.23(5) . . ?
O1 Er1 O26 76.23(5) . . ?
O1 Er1 O41 145.55(5) . . ?
O2 Er1 O1 99.02(5) . . ?
O2 Er1 O3 77.39(6) . . ?
O2 Er1 O4 74.40(5) . . ?
O2 Er1 O11 73.01(5) . . ?
O2 Er1 O26 143.28(5) . . ?
O2 Er1 O41 89.92(5) . . ?
O3 Er1 O1 71.99(5) . . ?
O3 Er1 O4 72.04(5) . . ?
O3 Er1 O11 130.21(5) . . ?
O3 Er1 O26 132.12(5) . . ?
O3 Er1 O41 142.38(5) . . ?
O4 Er1 O11 133.19(5) . . ?
O4 Er1 O26 129.68(5) . . ?
O4 Er1 O41 70.45(5) . . ?
O5 Er1 O1 91.28(6) . . ?
O5 Er1 O2 146.60(6) . . ?
O5 Er1 O3 75.80(6) . . ?
O5 Er1 O4 78.64(6) . . ?
O5 Er1 O11 140.31(5) . . ?
O5 Er1 O26 70.03(5) . . ?
O5 Er1 O41 99.35(6) . . ?
O11 Er1 O26 70.67(5) . . ?
O41 Er1 O11 76.82(5) . . ?
O41 Er1 O26 76.88(5) . . ?
F7 C6 S10 109.32(15) . . ?
F8 C6 F7 108.83(18) . . ?
F8 C6 S10 110.32(15) . . ?
F9 C6 F7 109.03(18) . . ?
F9 C6 F8 109.67(19) . . ?
F9 C6 S10 109.64(14) . . ?
O11 S10 C6 102.53(9) . . ?
O11 S10 N13 108.06(9) . . ?
O12 S10 C6 105.51(9) . . ?
O12 S10 O11 116.56(9) . . ?
O12 S10 N13 117.68(9) . . ?
N13 S10 C6 104.62(10) . . ?
S10 O11 Er1 150.20(9) . . ?
S10 N13 S14 123.87(11) . . ?
N13 S14 C17 101.65(10) . . ?
O15 S14 N13 108.35(9) . . ?
O15 S14 O16 119.58(9) . . ?
O15 S14 C17 104.09(10) . . ?
O16 S14 N13 114.82(9) . . ?
O16 S14 C17 106.17(9) . . ?
F18 C17 S14 109.85(14) . . ?
F18 C17 F19 109.03(18) . . ?
F19 C17 S14 108.97(15) . . ?
F20 C17 S14 110.03(15) . . ?
F20 C17 F18 109.43(18) . . ?
F20 C17 F19 109.51(18) . . ?
F22 C21 F23 109.06(18) . . ?
F22 C21 F24 109.87(18) . . ?
F22 C21 S25 111.15(15) . . ?
F23 C21 S25 108.03(15) . . ?
F24 C21 F23 109.29(18) . . ?
F24 C21 S25 109.40(15) . . ?
O26 S25 C21 103.88(9) . . ?
O26 S25 N28 107.02(9) . . ?
O27 S25 C21 105.01(10) . . ?
O27 S25 O26 117.56(9) . . ?
O27 S25 N28 116.89(9) . . ?
N28 S25 C21 104.89(10) . . ?
S25 O26 Er1 153.23(9) . . ?
S25 N28 S29 123.34(11) . . ?
N28 S29 C32 98.70(10) . . ?
O30 S29 N28 115.91(9) . . ?
O30 S29 O31 118.01(10) . . ?
O30 S29 C32 106.15(11) . . ?
O31 S29 N28 111.22(9) . . ?
O31 S29 C32 103.98(10) . . ?
F33 C32 S29 111.12(16) . . ?
F33 C32 F34 109.1(2) . . ?
F33 C32 F35 108.8(2) . . ?
F34 C32 S29 110.31(16) . . ?
F34 C32 F35 108.60(19) . . ?
F35 C32 S29 108.80(16) . . ?
F37 C36 F38 108.52(17) . . ?
F37 C36 S40 109.38(16) . . ?
F38 C36 S40 110.29(15) . . ?
F39 C36 F37 109.38(19) . . ?
F39 C36 F38 109.43(19) . . ?
F39 C36 S40 109.82(14) . . ?
O41 S40 C36 103.05(9) . . ?
O41 S40 N43 113.80(9) . . ?
O42 S40 C36 107.26(10) . . ?
O42 S40 O41 118.40(9) . . ?
O42 S40 N43 109.58(9) . . ?
N43 S40 C36 103.16(10) . . ?
S40 O41 Er1 159.62(9) . . ?
S40 N43 S44 126.33(11) . . ?
N43 S44 C47 101.02(11) . . ?
O45 S44 N43 116.50(9) . . ?
O45 S44 O46 118.03(10) . . ?
O45 S44 C47 105.79(13) . . ?
O46 S44 N43 108.66(9) . . ?
O46 S44 C47 104.63(12) . . ?
F48 C47 S44 110.3(2) . . ?
F48 C47 F49 109.0(2) . . ?
F48 C47 F50 109.3(2) . . ?
F49 C47 S44 108.14(18) . . ?
F50 C47 S44 110.74(19) . . ?
F50 C47 F49 109.3(2) . . ?

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 N43 0.833(10) 2.123(11) 2.947(2) 170(3) 4_665
O1 H1B N28 0.829(10) 2.218(15) 2.985(2) 154(3) .
O2 H2A O30 0.830(10) 2.057(13) 2.860(2) 163(3) 2_646
O2 H2B N13 0.833(10) 2.263(17) 2.972(2) 143(2) .
O2 H2B O27 0.833(10) 2.25(2) 2.800(2) 124(2) 2_646
O3 H3A O46 0.828(10) 1.891(10) 2.716(2) 174(3) 4_665
O3 H3B O31 0.827(10) 1.939(10) 2.763(2) 174(3) 4_565
O4 H4A O12 0.831(10) 2.068(14) 2.864(2) 160(3) 4_565
O4 H4B O45 0.834(9) 1.901(10) 2.723(2) 169(2) .
O5 H5A O15 0.831(10) 1.888(12) 2.704(2) 167(3) 2_656
O5 H5B O12 0.832(10) 2.40(2) 3.030(2) 134(3) 4_565
O5 H5B O16 0.832(10) 2.11(2) 2.799(2) 140(3) 4_565


_olex2_date_sample_data_collection 2013-07-09
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
