#------------------------------------------------------------------------------
#$Date: 2022-08-27 04:56:34 +0300 (Sat, 27 Aug 2022) $
#$Revision: 277420 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/53/7245385.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_7245385
loop_
_publ_author_name
'Takeyama, Tomoyuki'
'Takao, Koichiro'
_publ_section_title
;
 Effects of coordinating heteroatoms on molecular structure, thermodynamic
 stability and redox behavior of uranyl(vi) complexes with pentadentate
 Schiff-base ligands
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              24260
_journal_page_last               24268
_journal_paper_doi               10.1039/D2RA04639C
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C28 H38 N2 O6 S U, C H2 Cl2'
_chemical_formula_sum            'C29 H40 Cl2 N2 O6 S U'
_chemical_formula_weight         853.62
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.602(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3889(14)
_cell_length_b                   18.8968(9)
_cell_length_c                   10.3557(6)
_cell_measurement_reflns_used    6606
_cell_measurement_temperature    113
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      1.7350
_cell_volume                     3171.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -20.50   0.50   90.00    --   20.00  54.00 -30.00  105
  2  ω      4.00 106.50   0.50   90.00    --   20.00  54.00 -30.00  205
  3  ω    -69.00  -0.50   0.50   90.00    --   20.00  54.00-150.00  137
  4  ω     17.00  70.50   0.50   90.00    --   20.00  54.00-150.00  107
  5  ω    -36.00   3.50   0.50   90.00    --   20.00  54.00-180.00   79
  6  ω     34.00  67.50   0.50   90.00    --   20.00  54.00-180.00   67
  7  ω    -71.00 -40.50   0.50   90.00    --   20.00  54.00  30.00   61
  8  ω    -74.00  48.50   0.50   90.00    --   20.00  54.00 -90.00  245
  9  ω    -67.00  77.50   0.50   90.00    --   20.00  54.00  -8.79  289
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0342679000
_diffrn_orient_matrix_UB_12      0.0233618000
_diffrn_orient_matrix_UB_13      -0.0061311000
_diffrn_orient_matrix_UB_21      0.0272471000
_diffrn_orient_matrix_UB_22      0.0293672000
_diffrn_orient_matrix_UB_23      0.0087938000
_diffrn_orient_matrix_UB_31      -0.0000539000
_diffrn_orient_matrix_UB_32      0.0017107000
_diffrn_orient_matrix_UB_33      -0.0683707000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1154
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35851
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.890
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.661
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.053
_refine_diff_density_max         4.306
_refine_diff_density_min         -4.642
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         9534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0662
_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)+(0.0940P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5994
_reflns_number_total             9534
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra04639c2.cif
_cod_data_source_block           210120_uo2meosalidien_s
_cod_database_code               7245385
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H34N3O6S1U1
_chemical_oxdiff_usercomment     210120_UO2MeOsalidien_S
_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 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) =
Uanis(C18)
Uanis(Cl1A) = Uanis(Cl1B) = Uanis(Cl2A) = Uanis(Cl2B)
Uanis(O1) = Uanis(O2)
3. Others
 Fixed Sof: Cl2B(0.8) Cl1A(0.8) H29A(0.8) H29B(0.8) H29C(0.2) H29D(0.2)
 Cl1B(0.2) Cl2A(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C29(H29A,H29B),
 C29(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C16(H16), C7(H7), C3(H3), C12(H12), C14(H14)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.441
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.71479(2) 0.33713(2) 0.42130(3) 0.02304(10) Uani 1 1 d . . . . .
S1 S 0.61346(14) 0.20706(10) 0.4348(2) 0.0301(4) Uani 1 1 d . . . . .
Cl2B Cl 0.6322(4) 0.7069(3) -0.0150(5) 0.1110(16) Uani 0.8 1 d . . P A 1
O1 O 0.7378(4) 0.3247(3) 0.5929(5) 0.0274(9) Uani 1 1 d . . . . .
Cl1A Cl 0.7325(4) 0.6911(3) 0.2406(5) 0.1110(16) Uani 0.8 1 d . . P A 2
O2 O 0.6872(4) 0.3412(3) 0.2488(5) 0.0274(9) Uani 1 1 d . . . . .
O4 O 0.8406(3) 0.3708(3) 0.3889(5) 0.0268(12) Uani 1 1 d . . . . .
O5 O 0.5032(4) 0.5379(3) 0.8552(6) 0.0392(15) Uani 1 1 d . . . . .
N2 N 0.7977(4) 0.2257(3) 0.3951(6) 0.0246(14) Uani 1 1 d . . . . .
O3 O 0.6808(3) 0.4476(3) 0.4711(5) 0.0274(12) Uani 1 1 d . . . . .
O6 O 1.0361(4) 0.2965(3) 0.0214(6) 0.0373(14) Uani 1 1 d . . . . .
C21 C 0.7555(6) 0.5906(4) 0.5255(9) 0.040(2) Uani 1 1 d . . . . .
H21A H 0.740981 0.556663 0.454282 0.061 Uiso 1 1 calc R U . . .
H21B H 0.810397 0.610176 0.521187 0.061 Uiso 1 1 calc R U . . .
H21C H 0.714855 0.629028 0.517182 0.061 Uiso 1 1 calc R U . . .
C17 C 0.9165(5) 0.4048(4) 0.2164(8) 0.0283(7) Uani 1 1 d . . . . .
C5 C 0.5131(5) 0.4579(4) 0.6729(8) 0.0267(16) Uani 1 1 d . . . . .
H5 H 0.460009 0.438395 0.675942 0.032 Uiso 1 1 calc R U . . .
N1 N 0.5589(4) 0.3462(3) 0.4074(7) 0.0269(14) Uani 1 1 d . . . . .
C4 C 0.5451(5) 0.5088(4) 0.7608(8) 0.0307(18) Uani 1 1 d . . . . .
C16 C 0.9672(5) 0.3826(4) 0.1292(8) 0.0283(7) Uani 1 1 d . . . . .
H16 H 0.991069 0.417037 0.079550 0.034 Uiso 1 1 calc R U . . .
C15 C 0.9851(5) 0.3084(4) 0.1109(8) 0.0283(7) Uani 1 1 d . . . . .
C26 C 0.7999(5) 0.4935(4) 0.1934(8) 0.0345(19) Uani 1 1 d . . . . .
H26A H 0.781087 0.477463 0.103861 0.052 Uiso 1 1 calc R U . . .
H26B H 0.786260 0.543633 0.201194 0.052 Uiso 1 1 calc R U . . .
H26C H 0.772560 0.465652 0.254286 0.052 Uiso 1 1 calc R U . . .
C6 C 0.5613(5) 0.4351(4) 0.5767(7) 0.0254(16) Uani 1 1 d . . . . .
C1 C 0.6387(5) 0.4660(4) 0.5677(7) 0.0233(15) Uani 1 1 d . . . . .
C11 C 0.7701(5) 0.1588(4) 0.4466(8) 0.0279(17) Uani 1 1 d . . . . .
H11A H 0.771817 0.162684 0.542316 0.033 Uiso 1 1 calc R U . . .
H11B H 0.807797 0.120135 0.429328 0.033 Uiso 1 1 calc R U . . .
C2 C 0.6704(5) 0.5194(4) 0.6600(8) 0.0293(17) Uani 1 1 d . . . . .
C7 C 0.5228(5) 0.3848(4) 0.4832(8) 0.0295(18) Uani 1 1 d . . . . .
H7 H 0.464668 0.379632 0.476791 0.035 Uiso 1 1 calc R U . . .
C3 C 0.6221(5) 0.5376(4) 0.7540(8) 0.0315(19) Uani 1 1 d . . . . .
H3 H 0.642976 0.571882 0.817512 0.038 Uiso 1 1 calc R U . . .
C20 C 0.8253(6) 0.4977(5) 0.6766(9) 0.038(2) Uani 1 1 d . . . . .
H20A H 0.812913 0.460172 0.611345 0.058 Uiso 1 1 calc R U . . .
H20B H 0.830012 0.477321 0.764343 0.058 Uiso 1 1 calc R U . . .
H20C H 0.877487 0.520609 0.665475 0.058 Uiso 1 1 calc R U . . .
C24 C 0.8946(5) 0.4835(4) 0.2262(8) 0.0274(16) Uani 1 1 d . . . . .
C18 C 0.8825(5) 0.3526(4) 0.2930(8) 0.0283(7) Uani 1 1 d . . . . .
C19 C 0.7559(5) 0.5526(4) 0.6586(8) 0.0308(18) Uani 1 1 d . . . . .
C25 C 0.9248(6) 0.5117(5) 0.3607(8) 0.0358(19) Uani 1 1 d . . . . .
H25A H 0.900280 0.484161 0.425384 0.054 Uiso 1 1 calc R U . . .
H25B H 0.908718 0.561445 0.365587 0.054 Uiso 1 1 calc R U . . .
H25C H 0.985050 0.507774 0.378895 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6825(5) 0.1414(4) 0.3827(8) 0.0295(18) Uani 1 1 d . . . . .
H10A H 0.666861 0.093539 0.409134 0.035 Uiso 1 1 calc R U . . .
H10B H 0.679028 0.142274 0.286401 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5050(6) 0.3028(5) 0.3121(9) 0.040(2) Uani 1 1 d . . . . .
H8A H 0.491744 0.329328 0.229190 0.047 Uiso 1 1 calc R U . . .
H8B H 0.452701 0.293042 0.345733 0.047 Uiso 1 1 calc R U . . .
C23 C 0.4216(6) 0.5139(6) 0.8577(9) 0.048(3) Uani 1 1 d . . . . .
H23A H 0.388516 0.521516 0.771880 0.072 Uiso 1 1 calc R U . . .
H23B H 0.397351 0.540261 0.924040 0.072 Uiso 1 1 calc R U . . .
H23C H 0.422555 0.463336 0.878798 0.072 Uiso 1 1 calc R U . . .
C12 C 0.8580(5) 0.2227(4) 0.3312(8) 0.0283(7) Uani 1 1 d . . . . .
H12 H 0.881224 0.177035 0.324149 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5474(6) 0.2319(4) 0.2862(8) 0.0329(19) Uani 1 1 d . . . . .
H9A H 0.580356 0.237616 0.214214 0.039 Uiso 1 1 calc R U . . .
H9B H 0.505325 0.194821 0.261160 0.039 Uiso 1 1 calc R U . . .
C14 C 0.9481(5) 0.2602(4) 0.1792(8) 0.0283(7) Uani 1 1 d . . . . .
H14 H 0.957913 0.211319 0.166643 0.034 Uiso 1 1 calc R U . . .
C22 C 0.7768(7) 0.6078(5) 0.7676(10) 0.050(3) Uani 1 1 d . . . . .
H22A H 0.832666 0.625912 0.766292 0.076 Uiso 1 1 calc R U . . .
H22B H 0.773785 0.585684 0.852374 0.076 Uiso 1 1 calc R U . . .
H22C H 0.737201 0.646910 0.753590 0.076 Uiso 1 1 calc R U . . .
C13 C 0.8964(5) 0.2801(4) 0.2670(8) 0.0283(7) Uani 1 1 d . . . . .
C27 C 0.9349(6) 0.5282(4) 0.1279(8) 0.0342(19) Uani 1 1 d . . . . .
H27A H 0.994598 0.530555 0.156166 0.051 Uiso 1 1 calc R U . . .
H27B H 0.911781 0.576164 0.123867 0.051 Uiso 1 1 calc R U . . .
H27C H 0.923743 0.506363 0.041212 0.051 Uiso 1 1 calc R U . . .
C28 C 1.0625(6) 0.2256(5) 0.0103(9) 0.043(2) Uani 1 1 d . . . . .
H28A H 1.095243 0.222137 -0.061288 0.065 Uiso 1 1 calc R U . . .
H28B H 1.014271 0.194574 -0.007668 0.065 Uiso 1 1 calc R U . . .
H28C H 1.096347 0.211168 0.092198 0.065 Uiso 1 1 calc R U . . .
C29 C 0.7287(10) 0.6964(10) 0.0758(14) 0.108(6) Uani 1 1 d . . . . .
H29A H 0.761372 0.740562 0.089508 0.130 Uiso 0.8 1 calc R U P A 1
H29B H 0.761588 0.657331 0.045916 0.130 Uiso 0.8 1 calc R U P A 1
H29C H 0.741332 0.744856 0.048321 0.130 Uiso 0.2 1 calc R U P A 2
H29D H 0.767517 0.662610 0.044252 0.130 Uiso 0.2 1 calc R U P A 2
Cl1B Cl 0.6678(19) 0.6704(11) 0.2254(19) 0.1110(16) Uani 0.2 1 d . . P A 1
Cl2A Cl 0.632(2) 0.6749(12) 0.023(2) 0.1110(16) Uani 0.2 1 d . . P A 2
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'
Cl Cl 0.1484 0.1585 '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'
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
5 3 -14 0.2612
-14 -21 -1 0.0382
-3 -1 15 0.3652
22 1 2 0.0354
3 26 0 0.1116
-23 -2 0 0.0046
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 S1 83.17(18) . . ?
O1 U1 O2 174.4(2) . . ?
O1 U1 O4 97.2(2) . . ?
O1 U1 N2 87.7(2) . . ?
O1 U1 O3 85.1(2) . . ?
O1 U1 N1 97.3(2) . . ?
O2 U1 S1 91.32(18) . . ?
O2 U1 O4 86.5(2) . . ?
O2 U1 N2 89.4(2) . . ?
O2 U1 O3 99.0(2) . . ?
O2 U1 N1 80.7(2) . . ?
O4 U1 S1 140.88(15) . . ?
O4 U1 N2 72.5(2) . . ?
O4 U1 O3 92.1(2) . . ?
O4 U1 N1 156.3(2) . . ?
N2 U1 S1 68.42(16) . . ?
N2 U1 N1 126.7(2) . . ?
O3 U1 S1 126.70(15) . . ?
O3 U1 N2 162.1(2) . . ?
O3 U1 N1 70.6(2) . . ?
N1 U1 S1 59.73(14) . . ?
C10 S1 U1 100.0(3) . . ?
C9 S1 U1 90.8(3) . . ?
C9 S1 C10 104.2(4) . . ?
C18 O4 U1 129.0(5) . . ?
C4 O5 C23 116.9(7) . . ?
C11 N2 U1 118.4(5) . . ?
C12 N2 U1 124.2(5) . . ?
C12 N2 C11 117.1(7) . . ?
C1 O3 U1 125.9(5) . . ?
C15 O6 C28 116.1(7) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
C16 C17 C24 120.4(7) . . ?
C16 C17 C18 118.4(7) . . ?
C18 C17 C24 121.1(7) . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.5(8) . . ?
C6 C5 H5 120.7 . . ?
C7 N1 U1 123.8(5) . . ?
C7 N1 C8 116.3(7) . . ?
C8 N1 U1 119.8(5) . . ?
C5 C4 O5 124.3(8) . . ?
C5 C4 C3 120.2(8) . . ?
C3 C4 O5 115.4(7) . . ?
C17 C16 H16 118.9 . . ?
C17 C16 C15 122.2(7) . . ?
C15 C16 H16 118.9 . . ?
O6 C15 C16 114.1(7) . . ?
C14 C15 O6 128.0(8) . . ?
C14 C15 C16 117.8(8) . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
C5 C6 C7 116.0(7) . . ?
C1 C6 C5 121.2(7) . . ?
C1 C6 C7 122.5(7) . . ?
O3 C1 C6 120.6(7) . . ?
O3 C1 C2 120.2(7) . . ?
C6 C1 C2 119.1(7) . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C10 110.4(6) . . ?
H11A C11 H11B 108.1 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C1 C2 C19 121.4(7) . . ?
C3 C2 C1 117.0(8) . . ?
C3 C2 C19 121.5(7) . . ?
N1 C7 C6 126.5(8) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
C4 C3 C2 123.9(8) . . ?
C4 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
C17 C24 C26 109.8(6) . . ?
C17 C24 C27 111.1(7) . . ?
C25 C24 C17 110.8(7) . . ?
C25 C24 C26 109.9(7) . . ?
C25 C24 C27 107.6(7) . . ?
C27 C24 C26 107.5(6) . . ?
O4 C18 C17 121.5(7) . . ?
O4 C18 C13 120.3(7) . . ?
C13 C18 C17 118.2(8) . . ?
C2 C19 C21 108.3(7) . . ?
C2 C19 C22 111.9(8) . . ?
C20 C19 C21 109.0(7) . . ?
C20 C19 C2 112.6(7) . . ?
C20 C19 C22 106.9(7) . . ?
C22 C19 C21 108.0(7) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
S1 C10 H10A 110.1 . . ?
S1 C10 H10B 110.1 . . ?
C11 C10 S1 108.2(5) . . ?
C11 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N1 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
N1 C8 C9 111.0(7) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C12 H12 115.7 . . ?
N2 C12 C13 128.7(8) . . ?
C13 C12 H12 115.7 . . ?
S1 C9 H9A 110.2 . . ?
S1 C9 H9B 110.2 . . ?
C8 C9 S1 107.7(6) . . ?
C8 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C15 C14 H14 119.1 . . ?
C15 C14 C13 121.8(8) . . ?
C13 C14 H14 119.1 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C13 C12 122.4(8) . . ?
C14 C13 C18 121.2(8) . . ?
C14 C13 C12 116.4(7) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl2B C29 H29A 114.3 . . ?
Cl2B C29 H29B 114.3 . . ?
Cl2B C29 Cl1B 85.9(11) . . ?
Cl1A C29 H29C 111.4 . . ?
Cl1A C29 H29D 111.4 . . ?
H29A C29 H29B 111.5 . . ?
H29C C29 H29D 109.3 . . ?
Cl1B C29 H29A 114.3 . . ?
Cl1B C29 H29B 114.3 . . ?
Cl2A C29 Cl1A 101.8(14) . . ?
Cl2A C29 H29C 111.4 . . ?
Cl2A C29 H29D 111.4 . . ?
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 S1 2.981(2) . ?
U1 O1 1.776(5) . ?
U1 O2 1.778(5) . ?
U1 O4 2.231(5) . ?
U1 N2 2.543(6) . ?
U1 O3 2.241(5) . ?
U1 N1 2.543(7) . ?
S1 C10 1.815(9) . ?
S1 C9 1.806(8) . ?
Cl2B C29 1.728(16) . ?
Cl1A C29 1.702(15) . ?
O4 C18 1.333(10) . ?
O5 C4 1.390(10) . ?
O5 C23 1.416(12) . ?
N2 C11 1.469(9) . ?
N2 C12 1.270(10) . ?
O3 C1 1.343(9) . ?
O6 C15 1.356(10) . ?
O6 C28 1.417(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C19 1.553(12) . ?
C17 C16 1.381(11) . ?
C17 C24 1.537(11) . ?
C17 C18 1.429(11) . ?
C5 H5 0.9500 . ?
C5 C4 1.373(11) . ?
C5 C6 1.427(11) . ?
N1 C7 1.279(10) . ?
N1 C8 1.470(10) . ?
C4 C3 1.385(12) . ?
C16 H16 0.9500 . ?
C16 C15 1.451(11) . ?
C15 C14 1.351(11) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C24 1.550(11) . ?
C6 C1 1.412(11) . ?
C6 C7 1.435(11) . ?
C1 C2 1.434(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.524(12) . ?
C2 C3 1.387(12) . ?
C2 C19 1.536(12) . ?
C7 H7 0.9500 . ?
C3 H3 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.530(11) . ?
C24 C25 1.505(11) . ?
C24 C27 1.545(11) . ?
C18 C13 1.422(10) . ?
C19 C22 1.537(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.551(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.464(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C14 H14 0.9500 . ?
C14 C13 1.384(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 H29C 0.9900 . ?
C29 H29D 0.9900 . ?
C29 Cl1B 2.02(3) . ?
C29 Cl2A 1.65(4) . ?
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
U1 S1 C10 C11 41.0(6) . . . . ?
U1 S1 C9 C8 -62.4(6) . . . . ?
U1 O4 C18 C17 126.8(7) . . . . ?
U1 O4 C18 C13 -55.0(10) . . . . ?
U1 N2 C11 C10 59.0(7) . . . . ?
U1 N2 C12 C13 4.1(12) . . . . ?
U1 O3 C1 C6 -53.9(9) . . . . ?
U1 O3 C1 C2 128.6(6) . . . . ?
U1 N1 C7 C6 7.8(11) . . . . ?
U1 N1 C8 C9 30.5(9) . . . . ?
O4 C18 C13 C12 7.6(12) . . . . ?
O4 C18 C13 C14 -171.9(7) . . . . ?
O5 C4 C3 C2 -174.9(7) . . . . ?
N2 C11 C10 S1 -66.9(8) . . . . ?
N2 C12 C13 C18 15.0(13) . . . . ?
N2 C12 C13 C14 -165.5(8) . . . . ?
O3 C1 C2 C3 177.6(7) . . . . ?
O3 C1 C2 C19 -5.0(11) . . . . ?
O6 C15 C14 C13 -179.2(8) . . . . ?
C17 C16 C15 O6 -179.9(7) . . . . ?
C17 C16 C15 C14 2.3(12) . . . . ?
C17 C18 C13 C12 -174.1(7) . . . . ?
C17 C18 C13 C14 6.3(12) . . . . ?
C5 C4 C3 C2 1.4(12) . . . . ?
C5 C6 C1 O3 -175.3(7) . . . . ?
C5 C6 C1 C2 2.3(11) . . . . ?
C5 C6 C7 N1 -164.0(8) . . . . ?
N1 C8 C9 S1 31.4(9) . . . . ?
C4 C5 C6 C1 -2.8(11) . . . . ?
C4 C5 C6 C7 -176.7(7) . . . . ?
C16 C17 C24 C26 119.8(8) . . . . ?
C16 C17 C24 C25 -118.7(8) . . . . ?
C16 C17 C24 C27 0.9(11) . . . . ?
C16 C17 C18 O4 172.5(7) . . . . ?
C16 C17 C18 C13 -5.7(11) . . . . ?
C16 C15 C14 C13 -1.8(12) . . . . ?
C15 C14 C13 C18 -2.6(13) . . . . ?
C15 C14 C13 C12 177.9(7) . . . . ?
C6 C5 C4 O5 176.9(7) . . . . ?
C6 C5 C4 C3 1.0(11) . . . . ?
C6 C1 C2 C3 0.0(11) . . . . ?
C6 C1 C2 C19 177.3(7) . . . . ?
C1 C6 C7 N1 22.2(12) . . . . ?
C1 C2 C3 C4 -1.9(12) . . . . ?
C1 C2 C19 C21 61.8(9) . . . . ?
C1 C2 C19 C20 -58.8(10) . . . . ?
C1 C2 C19 C22 -179.3(7) . . . . ?
C11 N2 C12 C13 178.4(8) . . . . ?
C7 N1 C8 C9 -146.8(8) . . . . ?
C7 C6 C1 O3 -1.8(11) . . . . ?
C7 C6 C1 C2 175.8(7) . . . . ?
C3 C2 C19 C21 -121.0(8) . . . . ?
C3 C2 C19 C20 118.4(8) . . . . ?
C3 C2 C19 C22 -2.1(11) . . . . ?
C24 C17 C16 C15 -176.0(7) . . . . ?
C24 C17 C18 O4 -9.9(12) . . . . ?
C24 C17 C18 C13 171.8(7) . . . . ?
C18 C17 C16 C15 1.6(12) . . . . ?
C18 C17 C24 C26 -57.7(10) . . . . ?
C18 C17 C24 C25 63.9(10) . . . . ?
C18 C17 C24 C27 -176.5(7) . . . . ?
C19 C2 C3 C4 -179.2(7) . . . . ?
C10 S1 C9 C8 -162.9(6) . . . . ?
C8 N1 C7 C6 -175.1(7) . . . . ?
C23 O5 C4 C5 -1.3(11) . . . . ?
C23 O5 C4 C3 174.8(7) . . . . ?
C12 N2 C11 C10 -115.6(8) . . . . ?
C9 S1 C10 C11 134.3(6) . . . . ?
C28 O6 C15 C16 173.4(7) . . . . ?
C28 O6 C15 C14 -9.0(12) . . . . ?
loop_
_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
4.8912 3.3785 -14.4642 0.0000 0.1053 0.9944
-13.9521 -20.7523 -1.0928 -0.0000 -0.9992 0.0400
-3.3074 -1.0191 14.6027 0.0000 0.0084 -1.0000
22.1590 1.4621 1.9108 -0.7369 0.6635 -0.1293
3.3613 26.3294 0.0556 0.4996 0.8653 0.0411
-22.7936 -1.6301 -0.0228 0.7431 -0.6691 -0.0000
