#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:52:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179310 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/07/4320780.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_4320780
loop_
_publ_author_name
'Leonor Maria'
'Ângela Domingos'
'Isabel Santos'
_publ_section_title
;
 Unique Uranium(III) Cations Anchored by Polydentate Sulfur-Based Ligands:
 Synthesis and Structure of [U{H(R)B(timMe)2}2(THF)3][BPh4] (R = H, Ph)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6863
_journal_page_last               6864
_journal_paper_doi               10.1021/ic0106827
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     '[U{H(u-H)B(MeC3H2N2S)2}2(THF)3][BPh4].OC4H8'
_chemical_formula_sum            'C56 H76 B3 N8 O4 S4 U'
_chemical_formula_weight         1323.95
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                113.09(3)
_cell_angle_beta                 106.39(3)
_cell_angle_gamma                97.91(2)
_cell_formula_units_Z            2
_cell_length_a                   12.818(4)
_cell_length_b                   16.290(3)
_cell_length_c                   18.355(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      7.7
_cell_volume                     3246(2)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MOLEN(Fair,1990)
_computing_molecular_graphics    ORTEP(Johnson,1976)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4-Enraf-Nonius
_diffrn_measurement_method       ω/2\qscans
_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  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9727
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        13.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.8086
_exptl_absorpt_correction_type   'empirical via\y-scan North et al(1968)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.221
_refine_diff_density_min         -3.609
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         7951
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.330
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_obs          0.1092
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1668P)²+2.4067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3690
_refine_ls_wR_factor_obs         0.2489
_reflns_number_observed          5431
_reflns_number_total             9297
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0106827_2.cif
_cod_data_source_block           uh2btim
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1668P)^2^+2.4067P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1668P)^2^+2.4067P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3245.7(21)
_cod_database_code               4320780
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 0.21457(7) 0.21523(6) 0.43042(5) 0.0424(3) Uani 1 d . .
S1 S 0.2819(5) 0.1680(4) 0.5725(3) 0.0528(15) Uani 1 d . .
S2 S 0.3315(5) 0.0810(4) 0.3561(4) 0.063(2) Uani 1 d . .
S3 S 0.2890(5) 0.4013(4) 0.5740(4) 0.055(2) Uani 1 d . .
S4 S 0.0263(5) 0.2790(5) 0.3613(4) 0.063(2) Uani 1 d . .
O1 O 0.3239(13) 0.3208(11) 0.3896(9) 0.061(4) Uani 1 d . .
O2 O 0.0664(12) 0.0673(10) 0.3909(10) 0.058(4) Uani 1 d . .
O3 O 0.1309(14) 0.1356(12) 0.2624(9) 0.070(5) Uani 1 d . .
N11 N 0.5015(15) 0.2794(12) 0.6311(11) 0.045(4) Uani 1 d . .
N12 N 0.4400(17) 0.2810(13) 0.7307(11) 0.055(5) Uani 1 d . .
N21 N 0.5249(15) 0.1664(13) 0.4993(12) 0.056(5) Uani 1 d . .
N22 N 0.5148(18) 0.0292(14) 0.4109(14) 0.072(6) Uani 1 d . .
N31 N 0.1321(17) 0.3505(13) 0.6334(10) 0.047(5) Uani 1 d . .
N32 N 0.2874(18) 0.4524(13) 0.7330(11) 0.063(6) Uani 1 d . .
N41 N -0.0274(16) 0.3330(12) 0.5058(11) 0.057(5) Uani 1 d . .
N42 N -0.1059(17) 0.3833(14) 0.4186(14) 0.066(6) Uani 1 d . .
C11 C 0.4087(19) 0.2429(15) 0.6454(12) 0.049(6) Uani 1 d . .
C12 C 0.5864(20) 0.3340(18) 0.7080(16) 0.067(7) Uani 1 d . .
H12 H 0.6586(20) 0.3658(18) 0.7172(16) 0.080 Uiso 1 calc R .
C13 C 0.5465(21) 0.3335(18) 0.7684(15) 0.063(7) Uani 1 d . .
H13 H 0.5871(21) 0.3648(18) 0.8269(15) 0.076 Uiso 1 calc R .
C14 C 0.3662(26) 0.2621(24) 0.7752(17) 0.108(12) Uani 1 d . .
H14A H 0.2930(26) 0.2221(24) 0.7339(17) 0.162 Uiso 1 calc R .
H14B H 0.3579(26) 0.3196(24) 0.8124(17) 0.162 Uiso 1 calc R .
H14C H 0.3999(26) 0.2324(24) 0.8080(17) 0.162 Uiso 1 calc R .
C21 C 0.4591(18) 0.0937(18) 0.4262(16) 0.051(6) Uani 1 d . .
C22 C 0.6218(23) 0.1456(23) 0.5318(19) 0.085(9) Uani 1 d . .
H22 H 0.6813(23) 0.1831(23) 0.5836(19) 0.102 Uiso 1 calc R .
C23 C 0.6142(29) 0.0587(26) 0.4732(22) 0.102(11) Uani 1 d . .
H23 H 0.6686(29) 0.0267(26) 0.4767(22) 0.122 Uiso 1 calc R .
C24 C 0.4768(25) -0.0642(16) 0.3336(18) 0.080(8) Uani 1 d . .
H24A H 0.4025(25) -0.0727(16) 0.2958(18) 0.120 Uiso 1 calc R .
H24B H 0.4746(25) -0.1125(16) 0.3511(18) 0.120 Uiso 1 calc R .
H24C H 0.5290(25) -0.0668(16) 0.3047(18) 0.120 Uiso 1 calc R .
C31 C 0.2349(20) 0.3999(14) 0.6472(11) 0.045(6) Uani 1 d . .
C32 C 0.2110(34) 0.4323(26) 0.7717(20) 0.105(12) Uani 1 d . .
H32 H 0.2246(34) 0.4572(26) 0.8297(20) 0.126 Uiso 1 calc R .
C33 C 0.1194(26) 0.3730(19) 0.7103(16) 0.072(8) Uani 1 d . .
H33 H 0.0546(26) 0.3489(19) 0.7170(16) 0.086 Uiso 1 calc R .
C34 C 0.4043(29) 0.5184(22) 0.7751(17) 0.107(11) Uani 1 d . .
H34A H 0.4242(29) 0.5479(22) 0.8357(17) 0.160 Uiso 1 calc R .
H34B H 0.4061(29) 0.5648(22) 0.7552(17) 0.160 Uiso 1 calc R .
H34C H 0.4575(29) 0.4847(22) 0.7612(17) 0.160 Uiso 1 calc R .
C41 C -0.0333(19) 0.3356(15) 0.4312(16) 0.057(6) Uani 1 d . .
C42 C -0.0997(23) 0.3814(23) 0.5329(20) 0.095(11) Uani 1 d . .
H42 H -0.1130(23) 0.3899(23) 0.5823(20) 0.114 Uiso 1 calc R .
C43 C -0.1475(24) 0.4138(20) 0.4822(20) 0.098(11) Uani 1 d . .
H43 H -0.1982(24) 0.4495(20) 0.4878(20) 0.117 Uiso 1 calc R .
C44 C -0.1423(23) 0.4030(22) 0.3477(21) 0.098(10) Uani 1 d . .
H44A H -0.1953(23) 0.4390(22) 0.3546(21) 0.148 Uiso 1 calc R .
H44B H -0.1781(23) 0.3457(22) 0.2961(21) 0.148 Uiso 1 calc R .
H44C H -0.0780(23) 0.4375(22) 0.3447(21) 0.148 Uiso 1 calc R .
C111 C 0.4237(29) 0.3101(26) 0.3664(25) 0.117(12) Uani 1 d . .
H11A H 0.4880(29) 0.3200(26) 0.4151(25) 0.141 Uiso 1 calc R .
H11B H 0.4082(29) 0.2482(26) 0.3211(25) 0.141 Uiso 1 calc R .
C112 C 0.4471(40) 0.3795(28) 0.3380(29) 0.139(16) Uani 1 d . .
H11C H 0.5271(40) 0.4127(28) 0.3664(29) 0.167 Uiso 1 calc R .
H11D H 0.4313(40) 0.3482(28) 0.2773(29) 0.167 Uiso 1 calc R .
C113 C 0.3873(36) 0.4406(26) 0.3527(29) 0.124(14) Uani 1 d . .
H11E H 0.3454(36) 0.4421(26) 0.3004(29) 0.149 Uiso 1 calc R .
H11F H 0.4364(36) 0.5025(26) 0.3935(29) 0.149 Uiso 1 calc R .
C114 C 0.3083(32) 0.4065(21) 0.3878(23) 0.107(11) Uani 1 d . .
H11G H 0.3229(32) 0.4533(21) 0.4450(23) 0.128 Uiso 1 calc R .
H11H H 0.2306(32) 0.3959(21) 0.3527(23) 0.128 Uiso 1 calc R .
C221 C -0.0508(25) 0.0597(22) 0.3761(22) 0.107(12) Uani 1 d . .
H22A H -0.0785(25) 0.0917(22) 0.3432(22) 0.129 Uiso 1 calc R .
H22B H -0.0616(25) 0.0875(22) 0.4298(22) 0.129 Uiso 1 calc R .
C222 C -0.1124(27) -0.0394(23) 0.3291(23) 0.110(12) Uani 1 d . .
H22C H -0.1718(27) -0.0527(23) 0.3493(23) 0.132 Uiso 1 calc R .
H22D H -0.1465(27) -0.0578(23) 0.2687(23) 0.132 Uiso 1 calc R .
C223 C -0.0302(32) -0.0883(26) 0.3445(28) 0.127(14) Uani 1 d . .
H22E H -0.0350(32) -0.1372(26) 0.2910(28) 0.152 Uiso 1 calc R .
H22F H -0.0443(32) -0.1165(26) 0.3799(28) 0.152 Uiso 1 calc R .
C224 C 0.0839(29) -0.0205(19) 0.3883(17) 0.092(10) Uani 1 d . .
H22G H 0.1186(29) -0.0134(19) 0.4455(17) 0.110 Uiso 1 calc R .
H22H H 0.1327(29) -0.0411(19) 0.3571(17) 0.110 Uiso 1 calc R .
C331 C 0.1603(38) 0.1705(30) 0.2105(28) 0.143(15) Uani 1 d U .
H33A H 0.2379(38) 0.1716(30) 0.2155(28) 0.172 Uiso 1 calc R .
H33B H 0.1541(38) 0.2334(30) 0.2277(28) 0.172 Uiso 1 calc R .
C332 C 0.0837(51) 0.1106(40) 0.1233(38) 0.206(24) Uani 1 d U .
H33C H 0.0277(51) 0.1399(40) 0.1050(38) 0.247 Uiso 1 calc R .
H33D H 0.1250(51) 0.0965(40) 0.0851(38) 0.247 Uiso 1 calc R .
C333 C 0.0317(46) 0.0295(37) 0.1241(32) 0.175(19) Uani 1 d U .
H33E H 0.0733(46) -0.0162(37) 0.1099(32) 0.210 Uiso 1 calc R .
H33F H -0.0453(46) 0.0028(37) 0.0827(32) 0.210 Uiso 1 calc R .
C334 C 0.0315(41) 0.0561(33) 0.2129(30) 0.162(17) Uani 1 d U .
H33G H -0.0366(41) 0.0729(33) 0.2182(30) 0.194 Uiso 1 calc R .
H33H H 0.0395(41) 0.0065(33) 0.2289(30) 0.194 Uiso 1 calc R .
B1 B 0.5052(24) 0.2635(23) 0.5435(17) 0.065(8) Uani 1 d D .
H1A H 0.5686(24) 0.3140(23) 0.5509(17) 0.078 Uiso 1 calc RD .
H1B H 0.4314(24) 0.2659(23) 0.5068(17) 0.078 Uiso 1 calc RD .
B2 B 0.0387(24) 0.2805(21) 0.5520(20) 0.062(8) Uani 1 d D .
H2A H -0.0153(24) 0.2415(21) 0.5646(20) 0.075 Uiso 1 calc RD .
H2B H 0.0714(24) 0.2378(21) 0.5136(20) 0.075 Uiso 1 calc RD .
C300 C 0.2245(20) 0.4524(16) 0.0028(12) 0.051(6) Uani 1 d . .
C301 C 0.3267(21) 0.4664(16) -0.0017(13) 0.055(6) Uani 1 d . .
H30A H 0.3641(21) 0.4208(16) -0.0048(13) 0.066 Uiso 1 calc R .
C302 C 0.3804(23) 0.5481(21) -0.0018(13) 0.070(8) Uani 1 d . .
H30B H 0.4505(23) 0.5541(21) -0.0076(13) 0.083 Uiso 1 calc R .
C303 C 0.3309(31) 0.6174(20) 0.0064(17) 0.085(9) Uani 1 d . .
H30C H 0.3673(31) 0.6731(20) 0.0099(17) 0.102 Uiso 1 calc R .
C304 C 0.2286(33) 0.6029(27) 0.0094(29) 0.133(16) Uani 1 d . .
H30D H 0.1904(33) 0.6477(27) 0.0100(29) 0.160 Uiso 1 calc R .
C305 C 0.1760(28) 0.5256(22) 0.0116(28) 0.121(14) Uani 1 d . .
H30E H 0.1070(28) 0.5218(22) 0.0192(28) 0.146 Uiso 1 calc R .
C306 C 0.2331(19) 0.2896(14) 0.0022(13) 0.046(5) Uani 1 d . .
C307 C 0.3003(26) 0.2905(21) 0.0758(19) 0.091(9) Uani 1 d . .
H30F H 0.2969(26) 0.3281(21) 0.1279(19) 0.109 Uiso 1 calc R .
C308 C 0.3796(31) 0.2299(31) 0.0712(27) 0.149(17) Uani 1 d . .
H30G H 0.4301(31) 0.2343(31) 0.1211(27) 0.179 Uiso 1 calc R .
C309 C 0.3773(32) 0.1686(24) -0.0062(24) 0.113(13) Uani 1 d . .
H30H H 0.4207(32) 0.1268(24) -0.0105(24) 0.136 Uiso 1 calc R .
C310 C 0.3134(34) 0.1711(26) -0.0719(20) 0.118(14) Uani 1 d . .
H30I H 0.3099(34) 0.1285(26) -0.1248(20) 0.142 Uiso 1 calc R .
C311 C 0.2490(23) 0.2325(19) -0.0702(17) 0.078(8) Uani 1 d . .
H30J H 0.2145(23) 0.2357(19) -0.1205(17) 0.093 Uiso 1 calc R .
C312 C 0.1176(19) 0.3878(15) 0.0853(12) 0.050(6) Uani 1 d . .
C313 C 0.0283(32) 0.3436(30) 0.0898(22) 0.160(22) Uani 1 d . .
H31A H -0.0243(32) 0.2943(30) 0.0399(22) 0.192 Uiso 1 calc R .
C314 C 0.0061(44) 0.3661(35) 0.1662(29) 0.207(30) Uani 1 d . .
H31B H -0.0533(44) 0.3267(35) 0.1666(29) 0.249 Uiso 1 calc R .
C315 C 0.0684(36) 0.4414(27) 0.2353(16) 0.107(12) Uani 1 d . .
H31C H 0.0547(36) 0.4593(27) 0.2856(16) 0.128 Uiso 1 calc R .
C316 C 0.1457(39) 0.4864(26) 0.2290(25) 0.168(26) Uani 1 d . .
H31D H 0.1894(39) 0.5427(26) 0.2761(25) 0.202 Uiso 1 calc R .
C317 C 0.1740(37) 0.4620(28) 0.1595(24) 0.202(31) Uani 1 d . .
H31E H 0.2387(37) 0.5005(28) 0.1642(24) 0.243 Uiso 1 calc R .
C318 C 0.0391(20) 0.3059(14) -0.0852(12) 0.045(6) Uani 1 d . .
C319 C -0.0025(31) 0.3466(30) -0.1352(23) 0.123(13) Uani 1 d . .
H32A H 0.0351(31) 0.4060(30) -0.1234(23) 0.148 Uiso 1 calc R .
C320 C -0.1136(33) 0.2902(45) -0.2116(24) 0.155(23) Uani 1 d . .
H32B H -0.1479(33) 0.3166(45) -0.2452(24) 0.186 Uiso 1 calc R .
C321 C -0.1605(37) 0.2041(23) -0.2295(32) 0.155(25) Uani 1 d . .
H32C H -0.2199(37) 0.1662(23) -0.2812(32) 0.186 Uiso 1 calc R .
C322 C -0.1253(28) 0.1718(31) -0.1768(23) 0.138(16) Uani 1 d . .
H32D H -0.1652(28) 0.1146(31) -0.1852(23) 0.166 Uiso 1 calc R .
C323 C -0.0276(27) 0.2239(34) -0.1077(24) 0.151(19) Uani 1 d . .
H32E H -0.0046(27) 0.1976(34) -0.0713(24) 0.181 Uiso 1 calc R .
B3 B 0.1560(21) 0.3594(20) 0.0016(18) 0.053(7) Uani 1 d . .
O1S O 0.6147(43) 0.2142(36) 0.2706(37) 0.263(21) Uiso 1 d . .
C1S C 0.6422(56) 0.1793(49) 0.3317(44) 0.213(25) Uiso 1 d . .
C2S C 0.6898(58) 0.1018(49) 0.2979(48) 0.222(27) Uiso 1 d . .
C3S C 0.7194(73) 0.1160(60) 0.2317(59) 0.279(36) Uiso 1 d . .
C4S C 0.6435(68) 0.1694(57) 0.1905(54) 0.258(32) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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 151.3(5) . . ?
O1 U1 O3 74.6(5) . . ?
O2 U1 O3 76.7(5) . . ?
O1 U1 S4 83.2(3) . . ?
O2 U1 S4 87.0(4) . . ?
O3 U1 S4 67.0(4) . . ?
O1 U1 S3 74.0(4) . . ?
O2 U1 S3 131.5(4) . . ?
O3 U1 S3 139.1(4) . . ?
S4 U1 S3 83.6(2) . . ?
O1 U1 S2 85.7(4) . . ?
O2 U1 S2 82.3(4) . . ?
O3 U1 S2 67.7(4) . . ?
S4 U1 S2 134.7(2) . . ?
S3 U1 S2 134.3(2) . . ?
O1 U1 S1 131.7(3) . . ?
O2 U1 S1 72.7(4) . . ?
O3 U1 S1 140.7(4) . . ?
S4 U1 S1 133.8(2) . . ?
S3 U1 S1 80.2(2) . . ?
S2 U1 S1 84.1(2) . . ?
O1 U1 B1 71.8(6) . . ?
O2 U1 B1 123.6(6) . . ?
O3 U1 B1 120.9(6) . . ?
S4 U1 B1 149.0(6) . . ?
S3 U1 B1 72.2(5) . . ?
S2 U1 B1 62.6(5) . . ?
S1 U1 B1 61.7(5) . . ?
O1 U1 B2 125.1(6) . . ?
O2 U1 B2 72.3(6) . . ?
O3 U1 B2 121.6(6) . . ?
S4 U1 B2 63.1(4) . . ?
S3 U1 B2 61.0(5) . . ?
S2 U1 B2 148.7(5) . . ?
S1 U1 B2 71.2(4) . . ?
B1 U1 B2 117.5(6) . . ?
C11 S1 U1 109.0(8) . . ?
C21 S2 U1 113.6(9) . . ?
C31 S3 U1 110.0(8) . . ?
C41 S4 U1 115.3(8) . . ?
C114 O1 C111 104.0(23) . . ?
C114 O1 U1 129.4(17) . . ?
C111 O1 U1 126.6(16) . . ?
C221 O2 C224 106.6(23) . . ?
C221 O2 U1 124.6(17) . . ?
C224 O2 U1 128.5(16) . . ?
C331 O3 C334 110.7(28) . . ?
C331 O3 U1 126.5(21) . . ?
C334 O3 U1 121.9(21) . . ?
C12 N11 C11 108.0(19) . . ?
C12 N11 B1 126.2(21) . . ?
C11 N11 B1 125.8(18) . . ?
C13 N12 C11 110.4(21) . . ?
C13 N12 C14 125.4(20) . . ?
C11 N12 C14 124.0(21) . . ?
C21 N21 C22 108.5(21) . . ?
C21 N21 B1 128.9(18) . . ?
C22 N21 B1 122.6(22) . . ?
C23 N22 C21 110.4(23) . . ?
C23 N22 C24 122.2(22) . . ?
C21 N22 C24 127.4(22) . . ?
C31 N31 C33 109.1(20) . . ?
C31 N31 B2 130.6(19) . . ?
C33 N31 B2 120.4(23) . . ?
C31 N32 C32 107.6(23) . . ?
C31 N32 C34 123.6(23) . . ?
C32 N32 C34 128.8(24) . . ?
C41 N41 C42 105.3(22) . . ?
C41 N41 B2 130.2(19) . . ?
C42 N41 B2 124.4(23) . . ?
C41 N42 C43 112.7(23) . . ?
C41 N42 C44 126.8(22) . . ?
C43 N42 C44 120.5(21) . . ?
N12 C11 N11 105.3(19) . . ?
N12 C11 S1 126.5(20) . . ?
N11 C11 S1 128.1(15) . . ?
C13 C12 N11 107.4(22) . . ?
N12 C13 C12 108.7(21) . . ?
N21 C21 N22 107.6(19) . . ?
N21 C21 S2 129.4(18) . . ?
N22 C21 S2 122.8(21) . . ?
C23 C22 N21 106.6(27) . . ?
N22 C23 C22 106.9(24) . . ?
N31 C31 N32 106.8(19) . . ?
N31 C31 S3 127.6(15) . . ?
N32 C31 S3 125.5(20) . . ?
C33 C32 N32 106.6(24) . . ?
C32 C33 N31 109.9(27) . . ?
N42 C41 N41 105.8(19) . . ?
N42 C41 S4 125.6(20) . . ?
N41 C41 S4 128.2(16) . . ?
C43 C42 N41 112.6(27) . . ?
C42 C43 N42 103.5(22) . . ?
C112 C111 O1 106.2(28) . . ?
C113 C112 C111 114.0(35) . . ?
C112 C113 C114 104.5(30) . . ?
O1 C114 C113 110.2(27) . . ?
O2 C221 C222 107.6(27) . . ?
C223 C222 C221 106.2(28) . . ?
C222 C223 C224 108.1(28) . . ?
O2 C224 C223 106.0(24) . . ?
O3 C331 C332 108.0(38) . . ?
C333 C332 C331 105.1(50) . . ?
C332 C333 C334 107.6(50) . . ?
O3 C334 C333 100.4(35) . . ?
N11 B1 N21 109.2(21) . . ?
N11 B1 U1 99.2(14) . . ?
N21 B1 U1 100.9(14) . . ?
N31 B2 N41 109.3(19) . . ?
N31 B2 U1 96.4(14) . . ?
N41 B2 U1 99.2(15) . . ?
C301 C300 C305 115.7(25) . . ?
C301 C300 B3 125.2(20) . . ?
C305 C300 B3 119.1(22) . . ?
C300 C301 C302 122.2(23) . . ?
C303 C302 C301 120.6(26) . . ?
C304 C303 C302 117.1(29) . . ?
C303 C304 C305 123.3(30) . . ?
C304 C305 C300 120.8(29) . . ?
C311 C306 C307 114.1(22) . . ?
C311 C306 B3 122.2(21) . . ?
C307 C306 B3 123.1(21) . . ?
C306 C307 C308 119.5(28) . . ?
C309 C308 C307 120.1(29) . . ?
C310 C309 C308 117.2(28) . . ?
C309 C310 C311 124.6(29) . . ?
C306 C311 C310 123.6(25) . . ?
C313 C312 C317 108.6(25) . . ?
C313 C312 B3 127.1(23) . . ?
C317 C312 B3 124.2(24) . . ?
C312 C313 C314 124.3(32) . . ?
C315 C314 C313 120.4(33) . . ?
C316 C315 C314 114.8(33) . . ?
C315 C316 C317 125.6(33) . . ?
C312 C317 C316 125.7(29) . . ?
C323 C318 C319 113.8(29) . . ?
C323 C318 B3 123.1(24) . . ?
C319 C318 B3 122.9(25) . . ?
C318 C319 C320 117.2(35) . . ?
C321 C320 C319 119.6(37) . . ?
C322 C321 C320 120.9(41) . . ?
C321 C322 C323 118.0(43) . . ?
C318 C323 C322 129.5(42) . . ?
C306 B3 C300 110.8(18) . . ?
C306 B3 C318 109.3(19) . . ?
C300 B3 C318 109.4(19) . . ?
C306 B3 C312 109.3(18) . . ?
C300 B3 C312 110.4(19) . . ?
C318 B3 C312 107.6(17) . . ?
C1S O1S C4S 117.5(61) . . ?
O1S C1S C2S 107.6(60) . . ?
C3S C2S C1S 102.7(67) . . ?
C2S C3S C4S 114.2(75) . . ?
O1S C4S C3S 91.5(62) . . ?
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 2.53(2) . ?
U1 O2 2.556(15) . ?
U1 O3 2.638(14) . ?
U1 S4 2.917(5) . ?
U1 S3 2.926(6) . ?
U1 S2 2.933(6) . ?
U1 S1 2.936(5) . ?
U1 B1 3.52(3) . ?
U1 B2 3.58(3) . ?
S1 C11 1.69(2) . ?
S2 C21 1.70(2) . ?
S3 C31 1.68(2) . ?
S4 C41 1.70(2) . ?
O1 C114 1.45(3) . ?
O1 C111 1.47(3) . ?
O2 C221 1.43(3) . ?
O2 C224 1.46(3) . ?
O3 C331 1.39(4) . ?
O3 C334 1.45(4) . ?
N11 C12 1.36(3) . ?
N11 C11 1.39(3) . ?
N11 B1 1.54(3) . ?
N12 C13 1.33(3) . ?
N12 C11 1.35(3) . ?
N12 C14 1.49(4) . ?
N21 C21 1.32(3) . ?
N21 C22 1.37(3) . ?
N21 B1 1.56(3) . ?
N22 C23 1.32(4) . ?
N22 C21 1.33(3) . ?
N22 C24 1.51(3) . ?
N31 C31 1.34(3) . ?
N31 C33 1.38(3) . ?
N31 B2 1.50(3) . ?
N32 C31 1.36(2) . ?
N32 C32 1.43(4) . ?
N32 C34 1.50(4) . ?
N41 C41 1.37(3) . ?
N41 C42 1.37(3) . ?
N41 B2 1.59(3) . ?
N42 C41 1.32(3) . ?
N42 C43 1.37(3) . ?
N42 C44 1.43(3) . ?
C12 C13 1.35(3) . ?
C22 C23 1.37(4) . ?
C32 C33 1.29(4) . ?
C42 C43 1.29(4) . ?
C111 C112 1.45(4) . ?
C112 C113 1.33(5) . ?
C113 C114 1.50(4) . ?
C221 C222 1.46(4) . ?
C222 C223 1.44(4) . ?
C223 C224 1.48(4) . ?
C331 C332 1.45(6) . ?
C332 C333 1.40(6) . ?
C333 C334 1.51(6) . ?
C300 C301 1.33(3) . ?
C300 C305 1.39(3) . ?
C300 B3 1.63(4) . ?
C301 C302 1.41(3) . ?
C302 C303 1.35(4) . ?
C303 C304 1.32(4) . ?
C304 C305 1.37(4) . ?
C306 C311 1.38(3) . ?
C306 C307 1.38(3) . ?
C306 B3 1.61(3) . ?
C307 C308 1.51(4) . ?
C308 C309 1.37(5) . ?
C309 C310 1.27(4) . ?
C310 C311 1.38(4) . ?
C312 C313 1.31(3) . ?
C312 C317 1.32(3) . ?
C312 B3 1.66(3) . ?
C313 C314 1.43(5) . ?
C314 C315 1.30(5) . ?
C315 C316 1.21(4) . ?
C316 C317 1.35(4) . ?
C318 C323 1.32(4) . ?
C318 C319 1.37(4) . ?
C318 B3 1.66(3) . ?
C319 C320 1.53(5) . ?
C320 C321 1.32(6) . ?
C321 C322 1.28(5) . ?
C322 C323 1.37(4) . ?
O1S C1S 1.43(7) . ?
O1S C4S 1.54(8) . ?
C1S C2S 1.47(8) . ?
C2S C3S 1.46(9) . ?
C3S C4S 1.62(10) . ?
