#------------------------------------------------------------------------------
#$Date: 2016-02-04 02:21:29 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175564 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/46/4344673.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4344673
loop_
_publ_author_name
'Mäkelä, Toni'
'Minkkinen, Miia-Elina'
'Rissanen, Kari'
_publ_section_title
;
 Ion Pair Binding in the Solid-State with Ditopic Crown Ether Uranyl
 Salophen Receptors.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1339
_journal_page_last               1346
_journal_paper_doi               10.1021/acs.inorgchem.5b02780
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C30 H34 F N2 O10 Rb S0.5 U, 0.15(C2 H3 O S), 0.85(C2 H6 O S)'
_chemical_formula_sum            'C32 H39.55 F N2 O11 Rb S1.5 U'
_chemical_formula_weight         1018.79
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4206(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3212(2)
_cell_length_b                   16.7621(2)
_cell_length_c                   15.8630(2)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.5528
_cell_measurement_theta_min      2.8911
_cell_volume                     3718.84(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   -8.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921   77.0000  -30.0000 99

  2 omega  -50.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921  -37.0000   60.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0451464000
_diffrn_orient_matrix_UB_12      -0.0054447000
_diffrn_orient_matrix_UB_13      -0.0107852000
_diffrn_orient_matrix_UB_21      -0.0197154000
_diffrn_orient_matrix_UB_22      -0.0301388000
_diffrn_orient_matrix_UB_23      -0.0299124000
_diffrn_orient_matrix_UB_31      -0.0120320000
_diffrn_orient_matrix_UB_32      0.0292026000
_diffrn_orient_matrix_UB_33      -0.0329434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_laue_measured_fraction_full 0.966
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12315
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.812
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             1982
_exptl_crystal_recrystallization_method 'Evaporation of acetone/DMSO'
_exptl_crystal_size_max          0.3398
_exptl_crystal_size_mid          0.2722
_exptl_crystal_size_min          0.1235
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0324P)²+17.9014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5854
_reflns_number_total             6497
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02780_si_006.cif
_cod_data_source_block           R1_RbF
_cod_original_cell_volume        3718.84(9)
_cod_original_formula_sum        'C32 H39.55 F N2 O11 Rb S1.50 U'
_cod_database_code               4344673
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C32 H40 N2 O11 U1 Rb1 F1 S2'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-C29A = S1B-C29B = S1A-C30A = S1B-C30B
 1.86 with sigma of 0.01
 S1B-O10B = S1A-O10A = O10C-S1C = S1D-O10D
 1.68 with sigma of 0.01
 C32C-S1C = C31C-S1C = S1D-C32D = C31D-S1D
 1.86 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(S1B) = Uanis(S1A)
Uanis(O10B) = Uanis(S1B)
Uanis(O10A) = Uanis(S1A)
Uanis(C29B) = Uanis(S1B)
Uanis(C29A) = Uanis(S1A)
Uanis(S1B) = Uanis(C30B)
Uanis(C30A) = Uanis(S1A)
Uanis(C31D) = Uanis(S1D)
Uanis(O10D) = Uanis(S1D)
Uanis(C32D) = Uanis(S1D)
Uanis(C27B) = Uanis(C27A)
Uanis(S1C) = Uanis(O10C)
Uanis(C31C) = Uanis(S1C)
Uanis(S1C) = Uanis(C32C)
Uanis(C32D) = Uanis(C32C)
4. Others
 Fixed Sof: S1A(0.25) S1B(0.25) O8A(0.7) O8B(0.3) O10A(0.5) O10B(0.5)
 H26A(0.7) H26B(0.7) H26C(0.3) H26D(0.3) C27A(0.7) H27A(0.7) H27B(0.7)
 C27B(0.3) H27C(0.3) H27D(0.3) H28A(0.7) H28B(0.7) H28C(0.3) H28D(0.3)
 C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C29B(0.5) H29D(0.5) H29E(0.5)
 H29F(0.5) C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C30B(0.5) H30D(0.5)
 H30E(0.5) H30F(0.5) S1D(0.15) O10D(0.15) C31D(0.15) H31D(0.15) H31E(0.15)
 H31F(0.15) C32D(0.15) S1C(0.85) O10C(0.85) C31C(0.85) H31A(0.85) H31B(0.85)
 H31C(0.85) C32C(0.85) H32A(0.85) H32B(0.85) H32C(0.85)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C26(H26C,H26D), C27A(H27A,H27B), C27B(H27C,H27D),
 C28(H28A,H28B), C28(H28C,H28D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C20(H20)
5.c Idealised Me refined as rotating group:
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C31D(H31D,H31E,H31F), C31C(H31A,H31B,H31C), C32C(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.12954(2) 0.22889(2) 0.14534(2) 0.01739(7) Uani 1 1 d . . . .
Rb1 Rb 0.14191(4) -0.20602(3) 0.48471(3) 0.02946(13) Uani 1 1 d . . . .
S1A S 0.2026(7) -0.4322(5) 0.4646(6) 0.0665(14) Uani 0.25 1 d D P A 2
S1B S 0.2571(7) -0.4344(5) 0.4921(6) 0.0665(14) Uani 0.25 1 d D P B 1
F1 F 0.0537(2) 0.28877(19) 0.02597(18) 0.0281(7) Uani 1 1 d . . . .
O1 O 0.2011(3) 0.3148(2) 0.1809(2) 0.0264(8) Uani 1 1 d . . . .
O2 O 0.0603(3) 0.1404(2) 0.1167(2) 0.0256(8) Uani 1 1 d . . . .
O3 O 0.2309(3) 0.1967(3) 0.0574(2) 0.0288(9) Uani 1 1 d . . . .
O4 O 0.0038(3) 0.2865(2) 0.1888(2) 0.0229(8) Uani 1 1 d . . . .
O5 O 0.2747(3) -0.0990(2) 0.4079(3) 0.0313(9) Uani 1 1 d . . . .
O6 O 0.3583(3) -0.1828(2) 0.5629(2) 0.0328(9) Uani 1 1 d . . . .
O7 O 0.2304(3) -0.2394(3) 0.6683(3) 0.0521(13) Uani 1 1 d . . . .
O8A O 0.0993(5) -0.1014(4) 0.6274(4) 0.0294(16) Uani 0.7 1 d . P C 1
O8B O 0.1565(15) -0.1030(9) 0.6534(10) 0.040(4) Uani 0.3 1 d . P C 2
O9 O 0.1743(3) -0.0229(2) 0.5045(2) 0.0350(10) Uani 1 1 d . . . .
O10A O 0.2523(10) -0.3514(7) 0.4718(12) 0.0665(14) Uani 0.5 1 d D P A 2
O10B O 0.2248(10) -0.3551(7) 0.4515(11) 0.0665(14) Uani 0.5 1 d D P B 1
N1 N 0.2684(3) 0.1357(3) 0.2249(3) 0.0193(9) Uani 1 1 d . . . .
N2 N 0.1432(3) 0.2054(2) 0.3074(3) 0.0167(9) Uani 1 1 d . . . .
C1 C 0.3509(4) 0.1237(3) 0.2075(3) 0.0214(11) Uani 1 1 d . . . .
H1 H 0.3936 0.0928 0.2466 0.026 Uiso 1 1 calc R . . .
C2 C 0.3842(4) 0.1532(3) 0.1333(3) 0.0213(11) Uani 1 1 d . . . .
C3 C 0.4814(4) 0.1430(4) 0.1322(4) 0.0309(13) Uani 1 1 d . . . .
H3 H 0.5211 0.1175 0.1785 0.037 Uiso 1 1 calc R . . .
C4 C 0.5193(4) 0.1693(4) 0.0652(4) 0.0346(14) Uani 1 1 d . . . .
H4 H 0.5843 0.1642 0.0669 0.041 Uiso 1 1 calc R . . .
C5 C 0.4589(4) 0.2038(4) -0.0054(4) 0.0341(14) Uani 1 1 d . . . .
H5 H 0.4837 0.2211 -0.0519 0.041 Uiso 1 1 calc R . . .
C6 C 0.3631(4) 0.2129(4) -0.0079(4) 0.0314(13) Uani 1 1 d . . . .
H6 H 0.3239 0.2356 -0.0564 0.038 Uiso 1 1 calc R . . .
C7 C 0.3228(4) 0.1885(3) 0.0614(3) 0.0216(11) Uani 1 1 d . . . .
C8 C 0.1196(4) 0.2574(3) 0.3588(3) 0.0206(11) Uani 1 1 d . . . .
H8 H 0.1381 0.2471 0.4176 0.025 Uiso 1 1 calc R . . .
C9 C 0.0670(4) 0.3301(3) 0.3335(3) 0.0237(11) Uani 1 1 d . . . .
C10 C 0.0675(5) 0.3888(4) 0.3962(4) 0.0362(15) Uani 1 1 d . . . .
H10 H 0.1017 0.3802 0.4523 0.043 Uiso 1 1 calc R . . .
C11 C 0.0184(5) 0.4589(4) 0.3764(4) 0.0455(18) Uani 1 1 d . . . .
H11 H 0.0216 0.4984 0.4180 0.055 Uiso 1 1 calc R . . .
C12 C -0.0356(5) 0.4703(4) 0.2943(4) 0.0437(17) Uani 1 1 d . . . .
H12 H -0.0692 0.5177 0.2807 0.052 Uiso 1 1 calc R . . .
C13 C -0.0402(4) 0.4123(4) 0.2323(4) 0.0353(14) Uani 1 1 d . . . .
H13 H -0.0785 0.4206 0.1778 0.042 Uiso 1 1 calc R . . .
C14 C 0.0111(4) 0.3417(3) 0.2494(3) 0.0229(11) Uani 1 1 d . . . .
C15 C 0.2474(4) 0.0949(3) 0.2975(3) 0.0180(10) Uani 1 1 d . . . .
C16 C 0.1843(4) 0.1319(3) 0.3416(3) 0.0177(10) Uani 1 1 d . . . .
C17 C 0.1607(4) 0.0949(3) 0.4129(3) 0.0210(11) Uani 1 1 d . . . .
H17 H 0.1212 0.1207 0.4437 0.025 Uiso 1 1 calc R . . .
C18 C 0.1960(4) 0.0200(3) 0.4380(3) 0.0250(12) Uani 1 1 d . . . .
C19 C 0.2537(4) -0.0192(3) 0.3905(3) 0.0228(11) Uani 1 1 d . . . .
C20 C 0.2805(4) 0.0185(3) 0.3219(3) 0.0235(11) Uani 1 1 d . . . .
H20 H 0.3209 -0.0073 0.2920 0.028 Uiso 1 1 calc R . . .
C21 C 0.3747(4) -0.1182(4) 0.4344(4) 0.0383(15) Uani 1 1 d . . . .
H21A H 0.4121 -0.0793 0.4106 0.046 Uiso 1 1 calc R . . .
H21B H 0.3864 -0.1703 0.4121 0.046 Uiso 1 1 calc R . . .
C22 C 0.4050(4) -0.1185(4) 0.5294(4) 0.0381(15) Uani 1 1 d . . . .
H22A H 0.4738 -0.1250 0.5463 0.046 Uiso 1 1 calc R . . .
H22B H 0.3882 -0.0682 0.5525 0.046 Uiso 1 1 calc R . . .
C23 C 0.3847(4) -0.1881(4) 0.6534(4) 0.0372(15) Uani 1 1 d . . . .
H23A H 0.3702 -0.1384 0.6792 0.045 Uiso 1 1 calc R . . .
H23B H 0.4528 -0.1978 0.6712 0.045 Uiso 1 1 calc R . . .
C24 C 0.3301(5) -0.2555(5) 0.6829(4) 0.0465(17) Uani 1 1 d . . . .
H24A H 0.3401 -0.3038 0.6524 0.056 Uiso 1 1 calc R . . .
H24B H 0.3546 -0.2647 0.7441 0.056 Uiso 1 1 calc R . . .
C25 C 0.2033(6) -0.1940(6) 0.7359(5) 0.069(3) Uani 1 1 d . . . .
H25A H 0.2516 -0.1540 0.7572 0.083 Uiso 1 1 calc R . . .
H25B H 0.1984 -0.2290 0.7835 0.083 Uiso 1 1 calc R . . .
C26 C 0.1101(6) -0.1548(5) 0.7021(5) 0.0507(19) Uani 1 1 d . . . .
H26A H 0.0625 -0.1966 0.6874 0.061 Uiso 0.7 1 calc R P C 1
H26B H 0.0940 -0.1245 0.7491 0.061 Uiso 0.7 1 calc R P C 1
H26C H 0.0629 -0.1895 0.6671 0.061 Uiso 0.3 1 calc R P C 2
H26D H 0.0839 -0.1279 0.7460 0.061 Uiso 0.3 1 calc R P C 2
C27A C 0.1516(7) -0.0267(5) 0.6492(5) 0.0291(19) Uani 0.7 1 d . P C 1
H27A H 0.2194 -0.0366 0.6698 0.035 Uiso 0.7 1 calc R P C 1
H27B H 0.1279 0.0022 0.6933 0.035 Uiso 0.7 1 calc R P C 1
C27B C 0.1088(18) -0.0431(16) 0.6276(14) 0.0291(19) Uani 0.3 1 d . P C 2
H27C H 0.1021 -0.0143 0.6790 0.035 Uiso 0.3 1 calc R P C 2
H27D H 0.0455 -0.0623 0.6008 0.035 Uiso 0.3 1 calc R P C 2
C28 C 0.1335(4) 0.0187(3) 0.5669(3) 0.0286(13) Uani 1 1 d . . . .
H28A H 0.0652 0.0249 0.5454 0.034 Uiso 0.7 1 calc R P C 1
H28B H 0.1617 0.0714 0.5768 0.034 Uiso 0.7 1 calc R P C 1
H28C H 0.0766 0.0473 0.5386 0.034 Uiso 0.3 1 calc R P C 2
H28D H 0.1790 0.0567 0.5984 0.034 Uiso 0.3 1 calc R P C 2
C29A C 0.3073(10) -0.4916(10) 0.4562(13) 0.0665(14) Uani 0.5 1 d D P A 2
H29A H 0.3296 -0.4755 0.4058 0.100 Uiso 0.5 1 calc GR P A 2
H29B H 0.2902 -0.5470 0.4516 0.100 Uiso 0.5 1 calc GR P A 2
H29C H 0.3570 -0.4833 0.5066 0.100 Uiso 0.5 1 calc GR P A 2
C29B C 0.2771(13) -0.4994(10) 0.4080(10) 0.0665(14) Uani 0.5 1 d D P B 1
H29D H 0.2394 -0.5469 0.4072 0.100 Uiso 0.5 1 calc GR P B 1
H29E H 0.3436 -0.5135 0.4183 0.100 Uiso 0.5 1 calc GR P B 1
H29F H 0.2591 -0.4727 0.3534 0.100 Uiso 0.5 1 calc GR P B 1
C30A C 0.2393(13) -0.4646(11) 0.5749(8) 0.0665(14) Uani 0.5 1 d D P A 2
H30A H 0.3071 -0.4735 0.5884 0.100 Uiso 0.5 1 calc GR P A 2
H30B H 0.2070 -0.5133 0.5827 0.100 Uiso 0.5 1 calc GR P A 2
H30C H 0.2235 -0.4243 0.6125 0.100 Uiso 0.5 1 calc GR P A 2
C30B C 0.1901(12) -0.4472(11) 0.5742(10) 0.0665(14) Uani 0.5 1 d D P B 1
H30D H 0.2313 -0.4392 0.6299 0.100 Uiso 0.5 1 calc GR P B 1
H30E H 0.1642 -0.5002 0.5709 0.100 Uiso 0.5 1 calc GR P B 1
H30F H 0.1390 -0.4090 0.5659 0.100 Uiso 0.5 1 calc GR P B 1
S1D S 0.5434(12) -0.1123(12) 0.2515(13) 0.082(3) Uani 0.15 1 d D P D 3
O10D O 0.532(3) -0.0169(16) 0.284(3) 0.082(3) Uani 0.15 1 d D P D 3
C31D C 0.604(7) -0.117(7) 0.367(2) 0.082(3) Uani 0.15 1 d D P D 3
H31D H 0.6715 -0.1258 0.3719 0.123 Uiso 0.15 1 calc GR P D 3
H31E H 0.5780 -0.1596 0.3948 0.123 Uiso 0.15 1 calc GR P D 3
H31F H 0.5952 -0.0673 0.3947 0.123 Uiso 0.15 1 calc GR P D 3
C32D C 0.636(3) -0.058(3) 0.208(4) 0.082(3) Uani 0.15 1 d D P D 3
S1C S 0.5900(2) -0.05579(18) 0.29490(19) 0.0713(7) Uani 0.85 1 d D P E 1
O10C O 0.4903(5) -0.0225(4) 0.2876(5) 0.0713(7) Uani 0.85 1 d D P E 1
C31C C 0.6127(12) -0.1194(9) 0.3877(7) 0.0713(7) Uani 0.85 1 d D P E 1
H31A H 0.6222 -0.0874 0.4391 0.107 Uiso 0.85 1 calc GR P E 1
H31B H 0.6690 -0.1506 0.3881 0.107 Uiso 0.85 1 calc GR P E 1
H31C H 0.5591 -0.1543 0.3858 0.107 Uiso 0.85 1 calc GR P E 1
C32C C 0.5855(8) -0.1284(7) 0.2119(7) 0.082(3) Uani 0.85 1 d D P E 1
H32A H 0.5559 -0.1761 0.2270 0.123 Uiso 0.85 1 calc GR P E 1
H32B H 0.6493 -0.1403 0.2057 0.123 Uiso 0.85 1 calc GR P E 1
H32C H 0.5490 -0.1078 0.1585 0.123 Uiso 0.85 1 calc GR P E 1
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'
Rb Rb -0.9393 2.9676 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 22 -7 0.0887 -1.0000 22.0000 -7.0000 -0.0894 -0.4340 0.8851
0 -21 -10 0.1074 0.0000 -21.0000 -10.0000 0.2222 0.9320 -0.2838
2 0 21 0.1009 2.0000 0.0000 21.0000 -0.1362 -0.6676 -0.7159
20 -2 0 0.0586 20.0000 -2.0000 -0.0000 0.9138 -0.3340 -0.2990
-20 1 1 0.0624 -20.0000 1.0000 1.0000 -0.9192 0.3343 0.2369
-2 16 -15 0.1131 -2.0000 16.0000 -15.0000 -0.0156 0.0059 0.9855
20 2 -4 0.0672 20.0000 2.0000 -4.0000 0.9352 -0.3349 -0.0505
-19 -8 9 0.0912 -19.0000 -8.0000 9.0000 -0.9113 0.3465 -0.3015
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
F1 U1 Rb1 38.48(8) . 2
F1 U1 O3 81.03(12) . .
F1 U1 O4 77.97(12) . .
F1 U1 N1 149.60(12) . .
F1 U1 N2 147.69(12) . .
O1 U1 Rb1 111.00(12) . 2
O1 U1 F1 92.71(14) . .
O1 U1 O2 176.30(16) . .
O1 U1 O3 89.24(16) . .
O1 U1 O4 89.97(15) . .
O1 U1 N1 90.23(15) . .
O1 U1 N2 83.82(15) . .
O2 U1 Rb1 71.41(12) . 2
O2 U1 F1 90.87(14) . .
O2 U1 O3 92.26(16) . .
O2 U1 O4 89.83(15) . .
O2 U1 N1 87.17(15) . .
O2 U1 N2 92.65(15) . .
O3 U1 Rb1 114.24(9) . 2
O3 U1 N1 68.75(13) . .
O3 U1 N2 130.84(13) . .
O4 U1 Rb1 47.10(9) . 2
O4 U1 O3 158.93(13) . .
O4 U1 N1 132.31(13) . .
O4 U1 N2 69.94(13) . .
N1 U1 Rb1 158.32(9) . 2
N2 U1 Rb1 113.64(9) . 2
N2 U1 N1 62.70(13) . .
F1 Rb1 O4 57.46(9) 2_545 2_545
F1 Rb1 O5 134.63(10) 2_545 .
F1 Rb1 O6 159.59(10) 2_545 .
F1 Rb1 O7 105.47(11) 2_545 .
F1 Rb1 O8A 72.56(14) 2_545 .
F1 Rb1 O8B 87.2(4) 2_545 .
F1 Rb1 O9 99.44(11) 2_545 .
F1 Rb1 O10A 121.5(2) 2_545 .
F1 Rb1 O10B 114.5(3) 2_545 .
F1 Rb1 C26 74.76(14) 2_545 .
F1 Rb1 C27B 78.3(4) 2_545 .
O4 Rb1 O6 142.08(10) 2_545 .
O4 Rb1 O8B 133.6(4) 2_545 .
O4 Rb1 O9 100.83(10) 2_545 .
O4 Rb1 C26 130.65(14) 2_545 .
O4 Rb1 C27B 115.6(4) 2_545 .
O5 Rb1 O4 91.59(10) . 2_545
O5 Rb1 O6 55.38(10) . .
O5 Rb1 O8B 94.8(3) . .
O5 Rb1 O9 50.79(10) . .
O5 Rb1 C26 116.79(14) . .
O5 Rb1 C27B 89.0(4) . .
O6 Rb1 O8B 73.4(4) . .
O6 Rb1 O9 73.84(11) . .
O6 Rb1 C26 84.84(14) . .
O6 Rb1 C27B 84.8(4) . .
O7 Rb1 O4 159.04(12) . 2_545
O7 Rb1 O5 109.33(12) . .
O7 Rb1 O6 56.81(12) . .
O7 Rb1 O8A 59.17(18) . .
O7 Rb1 O8B 48.3(3) . .
O7 Rb1 O9 93.67(13) . .
O7 Rb1 C26 40.22(16) . .
O7 Rb1 C27B 67.4(4) . .
O8A Rb1 O4 119.04(15) . 2_545
O8A Rb1 O5 101.60(14) . .
O8A Rb1 O6 88.43(15) . .
O8A Rb1 O9 53.32(15) . .
O8A Rb1 C26 22.73(18) . .
O8B Rb1 C26 22.3(3) . .
O8B Rb1 C27B 19.2(5) . .
O9 Rb1 O8B 52.6(3) . .
O9 Rb1 C26 73.79(13) . .
O9 Rb1 C27B 40.0(4) . .
O10A Rb1 O4 100.1(3) . 2_545
O10A Rb1 O5 93.9(3) . .
O10A Rb1 O6 68.0(2) . .
O10A Rb1 O7 77.8(4) . .
O10A Rb1 O8B 125.1(5) . .
O10A Rb1 O9 139.1(2) . .
O10A Rb1 C26 115.9(4) . .
O10A Rb1 C27B 144.0(5) . .
O10B Rb1 O4 91.6(3) . 2_545
O10B Rb1 O5 97.0(3) . .
O10B Rb1 O6 76.4(3) . .
O10B Rb1 O7 84.8(3) . .
O10B Rb1 O8A 143.2(4) . .
O10B Rb1 O9 145.2(3) . .
O10B Rb1 C26 121.1(4) . .
C27B Rb1 C26 35.2(4) . .
O10A S1A Rb1 40.7(7) . .
O10A S1A C29A 96.4(10) . .
O10A S1A C30A 99.3(10) . .
C29A S1A Rb1 137.1(7) . .
C30A S1A Rb1 103.7(7) . .
C30A S1A C29A 80.5(9) . .
O10B S1B C29B 107.6(11) . .
O10B S1B C30B 104.7(11) . .
C30B S1B C29B 131.8(10) . .
U1 F1 Rb1 111.75(12) . 2
C7 O3 U1 139.4(3) . .
U1 O4 Rb1 100.07(12) . 2
C14 O4 U1 124.9(3) . .
C14 O4 Rb1 123.7(3) . 2
C19 O5 Rb1 121.3(3) . .
C19 O5 C21 115.7(5) . .
C21 O5 Rb1 114.7(3) . .
C22 O6 Rb1 116.9(3) . .
C23 O6 Rb1 115.2(3) . .
C23 O6 C22 112.5(5) . .
C24 O7 Rb1 113.4(4) . .
C24 O7 C25 113.7(6) . .
C25 O7 Rb1 120.5(4) . .
C26 O8A Rb1 104.4(5) . .
C27A O8A Rb1 119.9(5) . .
C27A O8A C26 111.8(7) . .
C26 O8B Rb1 100.0(9) . .
C27B O8B Rb1 103.5(14) . .
C27B O8B C26 113(2) . .
C18 O9 Rb1 119.7(3) . .
C18 O9 C28 118.1(4) . .
C28 O9 Rb1 118.4(3) . .
S1A O10A Rb1 119.5(8) . .
S1B O10B Rb1 142.5(12) . .
C1 N1 U1 128.8(3) . .
C1 N1 C15 117.5(4) . .
C15 N1 U1 113.8(3) . .
C8 N2 U1 123.8(3) . .
C8 N2 C16 119.3(4) . .
C16 N2 U1 116.8(3) . .
N1 C1 C2 126.8(5) . .
C3 C2 C1 118.0(5) . .
C3 C2 C7 119.1(5) . .
C7 C2 C1 122.9(5) . .
C4 C3 C2 122.0(5) . .
C3 C4 C5 118.7(5) . .
C6 C5 C4 121.0(5) . .
C5 C6 C7 121.3(5) . .
O3 C7 C2 121.8(5) . .
O3 C7 C6 120.5(5) . .
C6 C7 C2 117.7(5) . .
N2 C8 C9 126.1(5) . .
C10 C9 C8 118.4(5) . .
C10 C9 C14 119.3(5) . .
C14 C9 C8 122.2(5) . .
C11 C10 C9 121.1(5) . .
C10 C11 C12 119.5(6) . .
C13 C12 C11 120.6(6) . .
C12 C13 C14 121.4(5) . .
O4 C14 C9 122.0(5) . .
O4 C14 C13 119.9(5) . .
C13 C14 C9 118.0(5) . .
C16 C15 N1 117.5(4) . .
C20 C15 N1 123.2(5) . .
C20 C15 C16 119.1(5) . .
C15 C16 N2 116.9(4) . .
C17 C16 N2 122.9(5) . .
C17 C16 C15 120.2(4) . .
C18 C17 C16 120.1(5) . .
O9 C18 C17 124.8(5) . .
O9 C18 C19 115.4(5) . .
C17 C18 C19 119.7(5) . .
O5 C19 C18 118.3(5) . .
C20 C19 O5 120.9(5) . .
C20 C19 C18 120.4(5) . .
C19 C20 C15 120.3(5) . .
O5 C21 C22 110.7(5) . .
O6 C22 C21 108.9(5) . .
O6 C23 C24 108.7(5) . .
O7 C24 C23 112.1(6) . .
O7 C25 C26 109.4(6) . .
O8A C26 Rb1 52.9(4) . .
O8A C26 C25 119.6(6) . .
O8B C26 Rb1 57.6(7) . .
O8B C26 C25 88.7(10) . .
C25 C26 Rb1 87.3(4) . .
O8A C27A C28 104.3(7) . .
O8B C27B Rb1 57.3(13) . .
O8B C27B C28 126(2) . .
C28 C27B Rb1 92.2(10) . .
O9 C28 C27A 109.8(5) . .
O9 C28 C27B 107.0(10) . .
O10D S1D C31D 78(4) . .
O10D S1D C32D 77(3) . .
C31D S1D C32D 100(4) . .
O10C S1C C31C 106.5(7) . .
O10C S1C C32C 108.1(5) . .
C32C S1C C31C 99.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 Rb1 4.1363(6) 2
U1 F1 2.211(3) .
U1 O1 1.787(4) .
U1 O2 1.788(4) .
U1 O3 2.284(4) .
U1 O4 2.277(4) .
U1 N1 2.628(4) .
U1 N2 2.566(4) .
Rb1 F1 2.771(3) 2_545
Rb1 O4 3.077(3) 2_545
Rb1 O5 3.052(4) .
Rb1 O6 3.105(4) .
Rb1 O7 2.968(5) .
Rb1 O8A 3.027(7) .
Rb1 O8B 3.153(17) .
Rb1 O9 3.109(4) .
Rb1 O10A 2.936(15) .
Rb1 O10B 2.863(15) .
Rb1 C26 3.676(7) .
Rb1 C27B 3.64(2) .
S1A O10A 1.524(9) .
S1A C29A 1.828(9) .
S1A C30A 1.799(9) .
S1B O10B 1.507(9) .
S1B C29B 1.794(9) .
S1B C30B 1.788(9) .
F1 Rb1 2.771(3) 2
O3 C7 1.311(6) .
O4 Rb1 3.077(3) 2
O4 C14 1.322(6) .
O5 C19 1.385(6) .
O5 C21 1.440(7) .
O6 C22 1.431(7) .
O6 C23 1.406(7) .
O7 C24 1.422(8) .
O7 C25 1.435(10) .
O8A C26 1.466(9) .
O8A C27A 1.462(11) .
O8B C26 1.418(16) .
O8B C27B 1.23(3) .
O9 C18 1.367(6) .
O9 C28 1.435(6) .
N1 C1 1.285(7) .
N1 C15 1.427(6) .
N2 C8 1.287(7) .
N2 C16 1.422(6) .
C1 C2 1.447(7) .
C2 C3 1.406(7) .
C2 C7 1.412(7) .
C3 C4 1.367(8) .
C4 C5 1.385(9) .
C5 C6 1.374(8) .
C6 C7 1.407(8) .
C8 C9 1.444(7) .
C9 C10 1.398(8) .
C9 C14 1.414(7) .
C10 C11 1.369(9) .
C11 C12 1.377(9) .
C12 C13 1.373(9) .
C13 C14 1.389(8) .
C15 C16 1.401(7) .
C15 C20 1.391(7) .
C16 C17 1.395(7) .
C17 C18 1.379(7) .
C18 C19 1.396(8) .
C19 C20 1.382(7) .
C21 C22 1.476(9) .
C23 C24 1.505(10) .
C25 C26 1.481(11) .
C27A C28 1.484(10) .
C27B C28 1.51(3) .
S1D O10D 1.698(10) .
S1D C31D 1.857(10) .
S1D C32D 1.861(10) .
S1C O10C 1.514(6) .
S1C C31C 1.790(8) .
S1C C32C 1.783(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
U1 O3 C7 C2 39.6(8) .
U1 O3 C7 C6 -142.3(5) .
U1 O4 C14 C9 -54.7(6) .
U1 O4 C14 C13 127.9(5) .
U1 N1 C1 C2 -6.6(8) .
U1 N1 C15 C16 -28.7(5) .
U1 N1 C15 C20 146.4(4) .
U1 N2 C8 C9 11.6(7) .
U1 N2 C16 C15 25.6(5) .
U1 N2 C16 C17 -151.2(4) .
Rb1 O4 C14 C9 169.1(4) 2
Rb1 O4 C14 C13 -8.3(7) 2
Rb1 O5 C19 C18 25.8(6) .
Rb1 O5 C19 C20 -147.5(4) .
Rb1 O5 C21 C22 -55.1(6) .
Rb1 O6 C22 C21 -44.4(6) .
Rb1 O6 C23 C24 40.9(6) .
Rb1 O7 C24 C23 57.6(7) .
Rb1 O7 C25 C26 19.1(9) .
Rb1 O8A C26 O8B 85.8(14) .
Rb1 O8A C26 C25 60.2(8) .
Rb1 O8A C27A C28 56.9(8) .
Rb1 O8B C26 O8A -70.4(13) .
Rb1 O8B C26 C25 87.6(7) .
Rb1 O8B C27B C28 -66(2) .
Rb1 O9 C18 C17 140.3(5) .
Rb1 O9 C18 C19 -35.5(6) .
Rb1 O9 C28 C27A 45.1(6) .
Rb1 O9 C28 C27B 17.1(11) .
Rb1 C27B C28 O9 -12.7(8) .
Rb1 C27B C28 C27A -113(2) .
O5 C19 C20 C15 170.8(5) .
O5 C21 C22 O6 66.5(6) .
O6 C23 C24 O7 -67.2(7) .
O7 C25 C26 Rb1 -13.2(6) .
O7 C25 C26 O8A -57.0(10) .
O7 C25 C26 O8B -70.8(10) .
O8A C27A C28 O9 -64.0(8) .
O8A C27A C28 C27B 25(2) .
O8B C27B C28 O9 38(3) .
O8B C27B C28 C27A -63(3) .
O9 C18 C19 O5 6.8(7) .
O9 C18 C19 C20 -179.8(5) .
N1 C1 C2 C3 171.1(5) .
N1 C1 C2 C7 -11.5(8) .
N1 C15 C16 N2 3.0(6) .
N1 C15 C16 C17 179.9(4) .
N1 C15 C20 C19 -176.9(5) .
N2 C8 C9 C10 -164.6(6) .
N2 C8 C9 C14 19.2(9) .
N2 C16 C17 C18 173.8(5) .
C1 N1 C15 C16 150.5(5) .
C1 N1 C15 C20 -34.5(7) .
C1 C2 C3 C4 -179.6(5) .
C1 C2 C7 O3 -0.1(8) .
C1 C2 C7 C6 -178.2(5) .
C2 C3 C4 C5 -3.0(9) .
C3 C2 C7 O3 177.3(5) .
C3 C2 C7 C6 -0.8(8) .
C3 C4 C5 C6 1.1(9) .
C4 C5 C6 C7 0.8(9) .
C5 C6 C7 O3 -179.1(5) .
C5 C6 C7 C2 -0.9(8) .
C7 C2 C3 C4 2.8(9) .
C8 N2 C16 C15 -151.0(5) .
C8 N2 C16 C17 32.2(7) .
C8 C9 C10 C11 -179.5(6) .
C8 C9 C14 O4 -0.2(8) .
C8 C9 C14 C13 177.3(5) .
C9 C10 C11 C12 2.8(11) .
C10 C9 C14 O4 -176.3(5) .
C10 C9 C14 C13 1.1(8) .
C10 C11 C12 C13 -0.3(12) .
C11 C12 C13 C14 -1.8(11) .
C12 C13 C14 O4 178.9(6) .
C12 C13 C14 C9 1.4(9) .
C14 C9 C10 C11 -3.2(10) .
C15 N1 C1 C2 174.3(5) .
C15 C16 C17 C18 -2.9(8) .
C16 N2 C8 C9 -172.0(5) .
C16 C15 C20 C19 -1.9(8) .
C16 C17 C18 O9 -177.1(5) .
C16 C17 C18 C19 -1.5(8) .
C17 C18 C19 O5 -169.2(5) .
C17 C18 C19 C20 4.2(8) .
C18 O9 C28 C27A -156.8(6) .
C18 O9 C28 C27B 175.1(11) .
C18 C19 C20 C15 -2.5(8) .
C19 O5 C21 C22 93.9(6) .
C20 C15 C16 N2 -172.3(4) .
C20 C15 C16 C17 4.6(7) .
C21 O5 C19 C18 -121.0(6) .
C21 O5 C19 C20 65.6(7) .
C22 O6 C23 C24 178.4(5) .
C23 O6 C22 C21 179.0(5) .
C24 O7 C25 C26 158.8(6) .
C25 O7 C24 C23 -85.0(7) .
C26 O8A C27A C28 179.5(6) .
C26 O8B C27B Rb1 -107.2(18) .
C26 O8B C27B C28 -173.3(15) .
C27A O8A C26 Rb1 -131.0(7) .
C27A O8A C26 O8B -45.3(14) .
C27A O8A C26 C25 -70.9(10) .
C27B O8B C26 Rb1 109(2) .
C27B O8B C26 O8A 39.0(16) .
C27B O8B C26 C25 -163.1(19) .
C28 O9 C18 C17 -17.5(8) .
C28 O9 C18 C19 166.7(5) .
C29A S1A O10A Rb1 178.5(9) .
C29B S1B O10B Rb1 167.4(11) .
C30A S1A O10A Rb1 -100.2(10) .
C30B S1B O10B Rb1 23.8(17) .
