#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:36:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179253 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/73/4317314.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_4317314
loop_
_publ_author_name
'Massimo Cametti'
'Laura Ilander'
'Arto Valkonen'
'Martin Nieger'
'Maija Nissinen'
'Elisa Nauha'
'Kari Rissanen'
_publ_section_title
;
 Non-Centrosymmetric Tetrameric Assemblies of Tetramethylammonium Halides
 with Uranyl Salophen Complexes in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11473
_journal_page_last               11484
_journal_paper_doi               10.1021/ic101547r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C32 H24 F N2 O6 S U, C4 H12 N'
_chemical_formula_sum            'C36 H36 F N3 O6 S U'
_chemical_formula_weight         895.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.9641(4)
_cell_length_b                   18.9641(4)
_cell_length_c                   19.0964(3)
_cell_measurement_reflns_used    41110
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     6867.8(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker, 2004)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL-97; MERCURY (Macrae, et al., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX-II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.843
_exptl_absorpt_correction_T_max  0.620104
_exptl_absorpt_correction_T_min  0.524198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0323
_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)+(0.0000P)²+20.6765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                5467
_reflns_number_total             6065
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic101547r_si_006.cif
_cod_data_source_block           7(TMA)F
_cod_database_code               4317314
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.347363(12) 0.394065(12) 0.690509(11) 0.02259(6) Uani 1 1 d . . .
S3 S 0.30326(9) 0.67010(9) 0.80769(11) 0.0372(4) Uani 1 1 d . . .
F1 F 0.3906(2) 0.3159(2) 0.61970(18) 0.0339(9) Uani 1 1 d . . .
O1 O 0.3979(2) 0.4598(2) 0.6453(2) 0.0273(11) Uani 1 1 d . . .
O2 O 0.2916(2) 0.3349(2) 0.7387(2) 0.0321(11) Uani 1 1 d . . .
O9 O 0.2633(2) 0.3995(2) 0.6053(2) 0.0308(11) Uani 1 1 d . . .
O14 O 0.2026(3) 0.3022(3) 0.5293(2) 0.0439(13) Uani 1 1 d . . .
O25 O 0.4405(2) 0.3557(2) 0.7563(2) 0.0302(11) Uani 1 1 d . . .
O30 O 0.5204(3) 0.2458(2) 0.7845(3) 0.0416(13) Uani 1 1 d . . .
N6 N 0.2530(3) 0.4912(3) 0.7162(3) 0.0279(13) Uani 1 1 d . . .
N22 N 0.3683(2) 0.4730(2) 0.8041(3) 0.0246(11) Uani 1 1 d . . .
C1 C 0.3365(3) 0.5409(3) 0.7995(3) 0.0270(15) Uani 1 1 d . . .
C2 C 0.3566(4) 0.6017(4) 0.8314(3) 0.0322(17) Uani 1 1 d . . .
H2 H 0.3953 0.6056 0.8628 0.039 Uiso 1 1 calc R . .
C4 C 0.2536(4) 0.6171(4) 0.7540(4) 0.0339(17) Uani 1 1 d . . .
H4 H 0.2144 0.6330 0.7273 0.041 Uiso 1 1 calc R . .
C5 C 0.2777(3) 0.5497(4) 0.7545(3) 0.0275(15) Uani 1 1 d . . .
C7 C 0.1865(3) 0.4880(4) 0.7002(4) 0.0323(16) Uani 1 1 d . . .
H7 H 0.1565 0.5237 0.7182 0.039 Uiso 1 1 calc R . .
C8 C 0.1547(4) 0.4340(4) 0.6569(4) 0.0328(17) Uani 1 1 d . . .
C9 C 0.1953(4) 0.3923(4) 0.6126(3) 0.0317(16) Uani 1 1 d . . .
C10 C 0.1596(4) 0.3403(4) 0.5714(4) 0.0397(18) Uani 1 1 d . . .
C11 C 0.0869(4) 0.3322(5) 0.5780(4) 0.048(2) Uani 1 1 d . . .
H11 H 0.0635 0.2962 0.5523 0.058 Uiso 1 1 calc R . .
C12 C 0.0485(4) 0.3755(5) 0.6213(5) 0.053(2) Uani 1 1 d . . .
H12 H -0.0012 0.3700 0.6244 0.064 Uiso 1 1 calc R . .
C13 C 0.0814(4) 0.4259(5) 0.6597(4) 0.044(2) Uani 1 1 d . . .
H13 H 0.0543 0.4561 0.6888 0.052 Uiso 1 1 calc R . .
C15 C 0.1804(5) 0.2346(4) 0.5048(4) 0.053(2) Uani 1 1 d . . .
H15A H 0.1462 0.2397 0.4659 0.064 Uiso 1 1 calc R . .
H15B H 0.1579 0.2075 0.5430 0.064 Uiso 1 1 calc R . .
C16 C 0.2460(5) 0.1982(4) 0.4799(4) 0.047(2) Uani 1 1 d . . .
C17 C 0.3040(5) 0.1979(4) 0.5225(4) 0.051(2) Uani 1 1 d . . .
H17 H 0.3020 0.2190 0.5675 0.061 Uiso 1 1 calc R . .
C18 C 0.3652(6) 0.1667(5) 0.4995(5) 0.069(3) Uani 1 1 d . . .
H18 H 0.4053 0.1663 0.5294 0.082 Uiso 1 1 calc R . .
C19 C 0.3700(5) 0.1352(4) 0.4323(5) 0.068(3) Uani 1 1 d . . .
H19 H 0.4128 0.1154 0.4154 0.082 Uiso 1 1 calc R . .
C20 C 0.3091(5) 0.1349(4) 0.3929(5) 0.052(2) Uani 1 1 d . . .
H20 H 0.3097 0.1119 0.3487 0.062 Uiso 1 1 calc R . .
C21 C 0.2480(5) 0.1660(4) 0.4143(4) 0.045(2) Uani 1 1 d . . .
H21 H 0.2075 0.1658 0.3850 0.054 Uiso 1 1 calc R . .
C23 C 0.4025(3) 0.4576(4) 0.8598(3) 0.0271(16) Uani 1 1 d . . .
H23 H 0.4011 0.4919 0.8960 0.032 Uiso 1 1 calc R . .
C24 C 0.4427(3) 0.3948(4) 0.8745(3) 0.0281(16) Uani 1 1 d . . .
C25 C 0.4602(3) 0.3466(3) 0.8205(4) 0.0313(16) Uani 1 1 d . . .
C26 C 0.5040(4) 0.2873(4) 0.8395(4) 0.0339(17) Uani 1 1 d . . .
C27 C 0.5254(4) 0.2781(4) 0.9084(4) 0.042(2) Uani 1 1 d . . .
H27 H 0.5533 0.2382 0.9202 0.050 Uiso 1 1 calc R . .
C28 C 0.5072(4) 0.3253(4) 0.9599(4) 0.0404(19) Uani 1 1 d . . .
H28 H 0.5226 0.3180 1.0067 0.049 Uiso 1 1 calc R . .
C29 C 0.4665(4) 0.3830(4) 0.9435(4) 0.0371(18) Uani 1 1 d . . .
H29 H 0.4543 0.4156 0.9792 0.045 Uiso 1 1 calc R . .
C31 C 0.5646(6) 0.1858(4) 0.7991(6) 0.0781(14) Uani 1 1 d . . .
H31A H 0.5403 0.1526 0.8308 0.094 Uiso 1 1 calc R . .
H31B H 0.6092 0.2011 0.8215 0.094 Uiso 1 1 calc R . .
C32 C 0.5792(6) 0.1518(5) 0.7307(6) 0.0781(14) Uani 1 1 d . . .
C33 C 0.5225(6) 0.1249(4) 0.6900(7) 0.0781(14) Uani 1 1 d . . .
H33 H 0.4755 0.1298 0.7066 0.094 Uiso 1 1 calc R . .
C34 C 0.5345(6) 0.0913(5) 0.6257(6) 0.0781(14) Uani 1 1 d . . .
H34 H 0.4976 0.0723 0.5979 0.094 Uiso 1 1 calc R . .
C35 C 0.6089(6) 0.0879(5) 0.6048(6) 0.0781(14) Uani 1 1 d . . .
H35 H 0.6204 0.0651 0.5620 0.094 Uiso 1 1 calc R . .
C36 C 0.6621(6) 0.1155(5) 0.6436(6) 0.0781(14) Uani 1 1 d . . .
H36 H 0.7093 0.1129 0.6270 0.094 Uiso 1 1 calc R . .
C37 C 0.6484(6) 0.1468(4) 0.7054(5) 0.0781(14) Uani 1 1 d . . .
H37 H 0.6862 0.1658 0.7322 0.094 Uiso 1 1 calc R . .
N38 N 0.5802(2) 0.3429(3) 0.5818(2) 0.0221(12) Uani 1 1 d . . .
C39 C 0.5748(4) 0.3547(4) 0.6587(3) 0.0345(18) Uani 1 1 d . . .
H39A H 0.5891 0.4031 0.6696 0.052 Uiso 1 1 calc R . .
H39B H 0.6059 0.3215 0.6832 0.052 Uiso 1 1 calc R . .
H39C H 0.5260 0.3472 0.6738 0.052 Uiso 1 1 calc R . .
C40 C 0.5300(3) 0.3913(4) 0.5461(4) 0.0329(17) Uani 1 1 d . . .
H40A H 0.5432 0.4402 0.5561 0.049 Uiso 1 1 calc R . .
H40B H 0.4822 0.3824 0.5633 0.049 Uiso 1 1 calc R . .
H40C H 0.5317 0.3831 0.4955 0.049 Uiso 1 1 calc R . .
C41 C 0.5586(5) 0.2695(4) 0.5654(4) 0.047(2) Uani 1 1 d . . .
H41A H 0.5105 0.2615 0.5824 0.071 Uiso 1 1 calc R . .
H41B H 0.5909 0.2365 0.5884 0.071 Uiso 1 1 calc R . .
H41C H 0.5602 0.2622 0.5147 0.071 Uiso 1 1 calc R . .
C42 C 0.6531(4) 0.3568(4) 0.5566(4) 0.0413(19) Uani 1 1 d . . .
H42A H 0.6663 0.4055 0.5680 0.062 Uiso 1 1 calc R . .
H42B H 0.6552 0.3500 0.5058 0.062 Uiso 1 1 calc R . .
H42C H 0.6859 0.3243 0.5796 0.062 Uiso 1 1 calc R . .
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'
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'
F F 0.0171 0.0103 '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_
_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 U1 O2 174.6(2) . . ?
O1 U1 F1 88.45(17) . . ?
O2 U1 F1 96.61(18) . . ?
O1 U1 O9 89.93(18) . . ?
O2 U1 O9 88.96(18) . . ?
F1 U1 O9 81.40(15) . . ?
O1 U1 O25 94.16(18) . . ?
O2 U1 O25 88.57(18) . . ?
F1 U1 O25 80.36(15) . . ?
O9 U1 O25 161.18(15) . . ?
O1 U1 N6 88.08(18) . . ?
O2 U1 N6 86.60(18) . . ?
F1 U1 N6 149.08(15) . . ?
O9 U1 N6 67.89(16) . . ?
O25 U1 N6 130.54(15) . . ?
O1 U1 N22 85.50(17) . . ?
O2 U1 N22 91.26(18) . . ?
F1 U1 N22 146.64(14) . . ?
O9 U1 N22 131.27(15) . . ?
O25 U1 N22 67.45(15) . . ?
N6 U1 N22 63.49(15) . . ?
C2 S3 C4 92.2(3) . . ?
C9 O9 U1 127.5(4) . . ?
C10 O14 C15 119.8(6) . . ?
C25 O25 U1 141.9(4) . . ?
C26 O30 C31 116.5(6) . . ?
C7 N6 C5 118.8(6) . . ?
C7 N6 U1 126.0(4) . . ?
C5 N6 U1 115.2(4) . . ?
C23 N22 C1 118.1(6) . . ?
C23 N22 U1 128.7(4) . . ?
C1 N22 U1 113.2(4) . . ?
C2 C1 C5 113.1(6) . . ?
C2 C1 N22 128.3(6) . . ?
C5 C1 N22 118.5(6) . . ?
C1 C2 S3 111.1(5) . . ?
C1 C2 H2 124.5 . . ?
S3 C2 H2 124.5 . . ?
C5 C4 S3 111.3(5) . . ?
C5 C4 H4 124.4 . . ?
S3 C4 H4 124.4 . . ?
C4 C5 N6 128.8(6) . . ?
C4 C5 C1 112.3(6) . . ?
N6 C5 C1 118.8(6) . . ?
N6 C7 C8 124.9(6) . . ?
N6 C7 H7 117.6 . . ?
C8 C7 H7 117.6 . . ?
C9 C8 C13 120.8(7) . . ?
C9 C8 C7 121.3(6) . . ?
C13 C8 C7 118.0(7) . . ?
O9 C9 C8 123.7(6) . . ?
O9 C9 C10 118.7(7) . . ?
C8 C9 C10 117.6(7) . . ?
O14 C10 C11 126.2(7) . . ?
O14 C10 C9 114.1(6) . . ?
C11 C10 C9 119.6(8) . . ?
C12 C11 C10 120.9(8) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 120.2(8) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C8 120.8(8) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
O14 C15 C16 105.9(6) . . ?
O14 C15 H15A 110.6 . . ?
C16 C15 H15A 110.6 . . ?
O14 C15 H15B 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.7 . . ?
C17 C16 C21 120.7(9) . . ?
C17 C16 C15 118.7(8) . . ?
C21 C16 C15 120.5(8) . . ?
C16 C17 C18 119.5(9) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 121.6(9) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C20 C19 C18 116.2(10) . . ?
C20 C19 H19 121.9 . . ?
C18 C19 H19 121.9 . . ?
C21 C20 C19 123.2(9) . . ?
C21 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
C20 C21 C16 118.8(8) . . ?
C20 C21 H21 120.6 . . ?
C16 C21 H21 120.6 . . ?
N22 C23 C24 128.1(6) . . ?
N22 C23 H23 115.9 . . ?
C24 C23 H23 115.9 . . ?
C29 C24 C25 120.2(6) . . ?
C29 C24 C23 118.8(6) . . ?
C25 C24 C23 121.0(6) . . ?
O25 C25 C24 122.4(6) . . ?
O25 C25 C26 120.6(6) . . ?
C24 C25 C26 116.9(6) . . ?
O30 C26 C27 126.6(6) . . ?
O30 C26 C25 113.0(6) . . ?
C27 C26 C25 120.4(7) . . ?
C28 C27 C26 121.5(7) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 119.7(7) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C24 121.2(7) . . ?
C28 C29 H29 119.4 . . ?
C24 C29 H29 119.4 . . ?
O30 C31 C32 106.5(8) . . ?
O30 C31 H31A 110.4 . . ?
C32 C31 H31A 110.4 . . ?
O30 C31 H31B 110.4 . . ?
C32 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
C37 C32 C33 119.7(10) . . ?
C37 C32 C31 120.5(12) . . ?
C33 C32 C31 119.8(10) . . ?
C34 C33 C32 121.2(10) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 114.5(12) . . ?
C33 C34 H34 122.7 . . ?
C35 C34 H34 122.7 . . ?
C36 C35 C34 123.4(11) . . ?
C36 C35 H35 118.3 . . ?
C34 C35 H35 118.3 . . ?
C37 C36 C35 120.4(11) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C32 120.8(12) . . ?
C36 C37 H37 119.6 . . ?
C32 C37 H37 119.6 . . ?
C41 N38 C42 110.9(6) . . ?
C41 N38 C40 107.8(5) . . ?
C42 N38 C40 109.7(5) . . ?
C41 N38 C39 109.2(5) . . ?
C42 N38 C39 110.8(5) . . ?
C40 N38 C39 108.3(5) . . ?
N38 C39 H39A 109.5 . . ?
N38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N38 C40 H40A 109.5 . . ?
N38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N38 C41 H41A 109.5 . . ?
N38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N38 C42 H42A 109.5 . . ?
N38 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N38 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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
U1 O1 1.794(4) . ?
U1 O2 1.796(5) . ?
U1 F1 2.168(3) . ?
U1 O9 2.281(4) . ?
U1 O25 2.286(5) . ?
U1 N6 2.614(5) . ?
U1 N22 2.664(5) . ?
S3 C2 1.706(7) . ?
S3 C4 1.717(8) . ?
O9 C9 1.303(8) . ?
O14 C10 1.354(9) . ?
O14 C15 1.427(9) . ?
O25 C25 1.294(8) . ?
O30 C26 1.350(8) . ?
O30 C31 1.440(9) . ?
N6 C7 1.299(8) . ?
N6 C5 1.410(8) . ?
N22 C23 1.279(8) . ?
N22 C1 1.426(8) . ?
C1 C2 1.359(9) . ?
C1 C5 1.417(9) . ?
C2 H2 0.9500 . ?
C4 C5 1.357(9) . ?
C4 H4 0.9500 . ?
C7 C8 1.447(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.389(10) . ?
C8 C13 1.401(10) . ?
C9 C10 1.434(10) . ?
C10 C11 1.393(11) . ?
C11 C12 1.373(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.356(12) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.500(12) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.367(12) . ?
C16 C21 1.395(10) . ?
C17 C18 1.375(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.419(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(11) . ?
C19 H19 0.9500 . ?
C20 C21 1.363(12) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C23 C24 1.443(10) . ?
C23 H23 0.9500 . ?
C24 C29 1.411(9) . ?
C24 C25 1.417(9) . ?
C25 C26 1.444(9) . ?
C26 C27 1.386(10) . ?
C27 C28 1.374(10) . ?
C27 H27 0.9500 . ?
C28 C29 1.376(10) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C31 C32 1.482(14) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.402(13) . ?
C32 C33 1.423(16) . ?
C33 C34 1.401(15) . ?
C33 H33 0.9500 . ?
C34 C35 1.467(14) . ?
C34 H34 0.9500 . ?
C35 C36 1.356(15) . ?
C35 H35 0.9500 . ?
C36 C37 1.347(13) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
N38 C41 1.483(9) . ?
N38 C42 1.487(8) . ?
N38 C40 1.488(8) . ?
N38 C39 1.489(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 U1 O9 C9 -145.5(5) . . . . ?
O2 U1 O9 C9 29.2(6) . . . . ?
F1 U1 O9 C9 126.1(6) . . . . ?
O25 U1 O9 C9 111.7(7) . . . . ?
N6 U1 O9 C9 -57.5(5) . . . . ?
N22 U1 O9 C9 -61.5(6) . . . . ?
O1 U1 O25 C25 123.2(7) . . . . ?
O2 U1 O25 C25 -52.1(7) . . . . ?
F1 U1 O25 C25 -149.1(7) . . . . ?
O9 U1 O25 C25 -134.7(7) . . . . ?
N6 U1 O25 C25 32.2(8) . . . . ?
N22 U1 O25 C25 39.8(7) . . . . ?
O1 U1 N6 C7 124.4(5) . . . . ?
O2 U1 N6 C7 -56.5(5) . . . . ?
F1 U1 N6 C7 40.6(6) . . . . ?
O9 U1 N6 C7 33.7(5) . . . . ?
O25 U1 N6 C7 -141.7(5) . . . . ?
N22 U1 N6 C7 -149.7(5) . . . . ?
O1 U1 N6 C5 -59.3(4) . . . . ?
O2 U1 N6 C5 119.7(4) . . . . ?
F1 U1 N6 C5 -143.1(4) . . . . ?
O9 U1 N6 C5 -150.0(4) . . . . ?
O25 U1 N6 C5 34.5(5) . . . . ?
N22 U1 N6 C5 26.6(4) . . . . ?
O1 U1 N22 C23 -115.6(5) . . . . ?
O2 U1 N22 C23 68.7(5) . . . . ?
F1 U1 N22 C23 -35.4(7) . . . . ?
O9 U1 N22 C23 158.4(5) . . . . ?
O25 U1 N22 C23 -19.2(5) . . . . ?
N6 U1 N22 C23 154.3(6) . . . . ?
O1 U1 N22 C1 64.1(4) . . . . ?
O2 U1 N22 C1 -111.6(4) . . . . ?
F1 U1 N22 C1 144.4(4) . . . . ?
O9 U1 N22 C1 -21.9(5) . . . . ?
O25 U1 N22 C1 160.5(4) . . . . ?
N6 U1 N22 C1 -26.0(4) . . . . ?
C23 N22 C1 C2 27.3(10) . . . . ?
U1 N22 C1 C2 -152.4(6) . . . . ?
C23 N22 C1 C5 -155.3(6) . . . . ?
U1 N22 C1 C5 24.9(7) . . . . ?
C5 C1 C2 S3 0.7(7) . . . . ?
N22 C1 C2 S3 178.2(5) . . . . ?
C4 S3 C2 C1 -0.3(5) . . . . ?
C2 S3 C4 C5 -0.2(5) . . . . ?
S3 C4 C5 N6 -177.9(5) . . . . ?
S3 C4 C5 C1 0.6(7) . . . . ?
C7 N6 C5 C4 -31.0(10) . . . . ?
U1 N6 C5 C4 152.5(6) . . . . ?
C7 N6 C5 C1 150.6(6) . . . . ?
U1 N6 C5 C1 -25.9(7) . . . . ?
C2 C1 C5 C4 -0.9(8) . . . . ?
N22 C1 C5 C4 -178.6(6) . . . . ?
C2 C1 C5 N6 177.8(5) . . . . ?
N22 C1 C5 N6 0.1(9) . . . . ?
C5 N6 C7 C8 175.2(6) . . . . ?
U1 N6 C7 C8 -8.7(9) . . . . ?
N6 C7 C8 C9 -18.6(10) . . . . ?
N6 C7 C8 C13 162.8(6) . . . . ?
U1 O9 C9 C8 57.1(8) . . . . ?
U1 O9 C9 C10 -125.1(6) . . . . ?
C13 C8 C9 O9 176.7(6) . . . . ?
C7 C8 C9 O9 -1.9(10) . . . . ?
C13 C8 C9 C10 -1.1(10) . . . . ?
C7 C8 C9 C10 -179.8(6) . . . . ?
C15 O14 C10 C11 -20.8(11) . . . . ?
C15 O14 C10 C9 158.0(6) . . . . ?
O9 C9 C10 O14 1.6(9) . . . . ?
C8 C9 C10 O14 179.6(6) . . . . ?
O9 C9 C10 C11 -179.5(6) . . . . ?
C8 C9 C10 C11 -1.5(10) . . . . ?
O14 C10 C11 C12 -178.3(7) . . . . ?
C9 C10 C11 C12 2.9(11) . . . . ?
C10 C11 C12 C13 -1.6(12) . . . . ?
C11 C12 C13 C8 -1.1(12) . . . . ?
C9 C8 C13 C12 2.5(11) . . . . ?
C7 C8 C13 C12 -178.8(7) . . . . ?
C10 O14 C15 C16 -162.8(6) . . . . ?
O14 C15 C16 C17 48.4(8) . . . . ?
O14 C15 C16 C21 -130.7(7) . . . . ?
C21 C16 C17 C18 1.3(11) . . . . ?
C15 C16 C17 C18 -177.8(7) . . . . ?
C16 C17 C18 C19 0.5(13) . . . . ?
C17 C18 C19 C20 -2.8(13) . . . . ?
C18 C19 C20 C21 3.4(13) . . . . ?
C19 C20 C21 C16 -1.8(12) . . . . ?
C17 C16 C21 C20 -0.7(11) . . . . ?
C15 C16 C21 C20 178.4(7) . . . . ?
C1 N22 C23 C24 -175.4(6) . . . . ?
U1 N22 C23 C24 4.3(10) . . . . ?
N22 C23 C24 C29 -169.4(7) . . . . ?
N22 C23 C24 C25 12.5(11) . . . . ?
U1 O25 C25 C24 -38.6(11) . . . . ?
U1 O25 C25 C26 144.0(5) . . . . ?
C29 C24 C25 O25 -178.9(6) . . . . ?
C23 C24 C25 O25 -0.9(10) . . . . ?
C29 C24 C25 C26 -1.4(9) . . . . ?
C23 C24 C25 C26 176.6(6) . . . . ?
C31 O30 C26 C27 -0.1(11) . . . . ?
C31 O30 C26 C25 179.4(6) . . . . ?
O25 C25 C26 O30 0.1(9) . . . . ?
C24 C25 C26 O30 -177.5(6) . . . . ?
O25 C25 C26 C27 179.6(6) . . . . ?
C24 C25 C26 C27 2.0(10) . . . . ?
O30 C26 C27 C28 177.9(7) . . . . ?
C25 C26 C27 C28 -1.5(11) . . . . ?
C26 C27 C28 C29 0.3(11) . . . . ?
C27 C28 C29 C24 0.3(11) . . . . ?
C25 C24 C29 C28 0.3(10) . . . . ?
C23 C24 C29 C28 -177.7(6) . . . . ?
C26 O30 C31 C32 -176.1(7) . . . . ?
O30 C31 C32 C37 118.0(9) . . . . ?
O30 C31 C32 C33 -60.9(10) . . . . ?
C37 C32 C33 C34 2.1(13) . . . . ?
C31 C32 C33 C34 -178.9(7) . . . . ?
C32 C33 C34 C35 -0.9(12) . . . . ?
C33 C34 C35 C36 -0.9(13) . . . . ?
C34 C35 C36 C37 1.6(14) . . . . ?
C35 C36 C37 C32 -0.4(13) . . . . ?
C33 C32 C37 C36 -1.5(13) . . . . ?
C31 C32 C37 C36 179.6(8) . . . . ?
