#------------------------------------------------------------------------------
#$Date: 2021-08-19 01:12:36 +0300 (Thu, 19 Aug 2021) $
#$Revision: 268126 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564375.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_1564375
loop_
_publ_author_name
'Keener, Megan'
'Scopelliti, Rosario'
'Mazzanti, Marinella'
_publ_section_title
;
 Nitride Protonation and NH3 Binding versus N--H Bond Cleavage in Uranium
 Nitrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03957A
_journal_year                    2021
_chemical_formula_moiety         'C32 H68 N3 O8 U2, 3(C24 H20 B)'
_chemical_formula_sum            'C104 H128 B3 N3 O8 U2'
_chemical_formula_weight         2056.58
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-04-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.7065(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.5736(3)
_cell_length_b                   13.29349(9)
_cell_length_c                   24.4177(2)
_cell_measurement_reflns_used    63894
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.8200
_cell_measurement_theta_min      3.6290
_cell_volume                     9194.29(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -61.00   1.00    5.00    --  -41.04-150.00 158.00   52
  2  ω    -68.00 -43.00   1.00    5.00    --  -41.04 122.00  41.00   25
  3  ω    -85.00 -60.00   1.00    5.00    --  -41.04 150.00-156.00   25
  4  ω     36.00  61.00   1.00    5.00    --   41.04-122.00 -39.00   25
  5  ω     76.00 101.00   1.00    5.00    --   41.04-150.00 158.00   25
  6  ω     60.00  85.00   1.00   20.00    --  112.00-150.00 158.00   25
  7  ω     50.00  75.00   1.00   20.00    --  112.00-122.00 -39.00   25
  8  ω     92.00 125.00   1.00   20.00    --  112.00 150.00-156.00   33
  9  ω    109.00 153.00   1.00   20.00    --  112.00 122.00  41.00   44
 10  ω   -109.00 -14.00   1.00    5.00    --  -41.04 -57.00  60.00   95
 11  ω   -109.00 -17.00   1.00    5.00    --  -41.04 -38.00 150.00   92
 12  ω    -87.00  -8.00   1.00    5.00    --  -41.04 125.00 -60.00   79
 13  ω    -28.00  62.00   1.00    5.00    --   41.04 -38.00  90.00   90
 14  ω     11.00  74.00   1.00    5.00    --   41.04 -99.00-120.00   63
 15  ω    109.00 135.00   1.00   20.00    --  112.00  30.00  90.00   26
 16  ω     37.00  98.00   1.00   20.00    --  112.00-111.00-120.00   61
 17  ω     86.00 175.00   1.00   20.00    --  112.00  45.00  30.00   89
 18  ω    106.00 136.00   1.00   20.00    --  112.00 -45.00 120.00   30
 19  ω    116.00 176.00   1.00   20.00    --  112.00 111.00  30.00   60
 20  ω     66.00 109.00   1.00   20.00    --  112.00-111.00  60.00   43
 21  ω     37.00 105.00   1.00   20.00    --  112.00-111.00-150.00   68
 22  ω     56.00  81.00   1.00   20.00    --  112.00 -77.00 150.00   25
 23  ω     87.00 112.00   1.00   20.00    --  112.00 -77.00 150.00   25
 24  ω     54.00  90.00   1.00   20.00    --  112.00 -45.00 120.00   36
 25  ω     87.00 151.00   1.00   20.00    --  112.00  30.00-180.00   64
 26  ω     40.00 108.00   1.00   20.00    --  112.00-111.00 150.00   68
 27  ω    133.00 174.00   1.00   20.00    --  112.00 111.00-180.00   41
 28  ω     36.00  85.00   1.00   20.00    --  112.00 -94.00  60.00   49
 29  ω    106.00 178.00   1.00   20.00    --  112.00  77.00-150.00   72
 30  ω     80.00 122.00   1.00   20.00    --  112.00 178.00-150.00   42
 31  ω     86.00 114.00   1.00   20.00    --  112.00  45.00   0.00   28
 32  ω    123.00 178.00   1.00   20.00    --  112.00  45.00   0.00   55
 33  ω     36.00 109.00   1.00   20.00    --  112.00-111.00 -30.00   73
 34  ω     81.00 107.00   1.00   20.00    --  112.00 -94.00 -30.00   26
 35  ω     68.00 109.00   1.00   20.00    --  112.00-111.00 -90.00   41
 36  ω    105.00 146.00   1.00   20.00    --  112.00  77.00 -60.00   41
 37  ω     62.00 109.00   1.00   20.00    --  112.00-111.00 120.00   47
 38  ω     52.00  81.00   1.00   20.00    --  112.00 -94.00  30.00   29
 39  ω     79.00 137.00   1.00   20.00    --  112.00 -61.00 -90.00   58
 40  ω    110.00 173.00   1.00   20.00    --  112.00 111.00 -90.00   63
 41  ω     90.00 174.00   1.00   20.00    --  112.00  61.00  90.00   84
 42  ω     47.00  72.00   1.00   20.00    --  112.00 -61.00-150.00   25
 43  ω    106.00 140.00   1.00   20.00    --  112.00 -61.00-150.00   34
 44  ω     61.00  86.00   1.00   20.00    --  112.00-111.00-180.00   25
 45  ω    124.00 153.00   1.00   20.00    --  112.00  61.00 -30.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0541305000
_diffrn_orient_matrix_UB_12      0.0046252000
_diffrn_orient_matrix_UB_13      0.0244882000
_diffrn_orient_matrix_UB_21      0.0005895000
_diffrn_orient_matrix_UB_22      0.0999581000
_diffrn_orient_matrix_UB_23      -0.0317010000
_diffrn_orient_matrix_UB_31      -0.0053277000
_diffrn_orient_matrix_UB_32      0.0584105000
_diffrn_orient_matrix_UB_33      0.0522870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            115292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.142
_diffrn_reflns_theta_min         3.120
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.289
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plate
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.967
_refine_diff_density_min         -2.698
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         19118
_refine_ls_number_restraints     1969
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0281
_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)+(0.0328P)²+17.0380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18009
_reflns_number_total             19118
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc03957a2.cif
_cod_data_source_block           mk-218
_cod_original_cell_volume        9194.26(14)
_cod_database_code               1564375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C104 H128 B3 N3 O8 U2'
_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.
;
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.183
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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, All N(H,H) groups
2. Restrained distances
 C30-C29 \\sim C33-C29 \\sim C31-C30 \\sim C34-C33 \\sim C32-C31 \\sim C35-C34
\\sim C45-C44 \\sim C49-C48
 \\sim C46-C45 \\sim C50-C49 \\sim C47-C46 \\sim C50-C47 \\sim C16-C12 \\sim
C13-C12 \\sim C14-C13 \\sim C17-
 C16 \\sim C15-C14 \\sim C18-C17 \\sim C8-C7 \\sim C8-C11 \\sim C9-C10 \\sim
C6-C5 \\sim C11-C10 \\sim C7-C6 ~
 C22-C21 \\sim C24-C23 \\sim C21-C20 \\sim C23-C20 \\sim C20-C19 \\sim C37-C36
\\sim C41-C40 \\sim C38-C37
 \\sim C42-C41 \\sim C43-C42 \\sim C39-C38
 with sigma of 0.02
 O6-C29 \\sim O6-C32 \\sim O6-C35 \\sim O8-C47 \\sim O8-C48 \\sim O8-C44 \\sim
O3-C15 \\sim O3-C18 \\sim O3-
 C12 \\sim O2-C9 \\sim O2-C5 \\sim O2-C8 \\sim O4-C22 \\sim O4-C24 \\sim O4-C19
\\sim O7-C40 \\sim O7-C36 \\sim O7-
 C39 \\sim O7-C43
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H12C)=Sof(H12D)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(H47C)=Sof(H47D)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=1-FVAR(2)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H47A)=Sof(H47B)=FVAR(2)
 Sof(H29C)=Sof(H29D)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=1-FVAR(3)
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(3)
 Sof(H20C)=Sof(H20D)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 1-FVAR(4)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 FVAR(4)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=1-FVAR(5)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(5)
 Sof(H8BC)=Sof(H8BD)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=1-FVAR(6)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(H8AA)=Sof(H8AB)=FVAR(6)
 Fixed X: U1(0.20508) U2(0.32015)
 Fixed Y: U1(0.53156) U2(0.54191)
 Fixed Z: U1(0.735129) U2(0.758301)
5.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), C1(H1A,H1B), C2(H2C,H2D), C3(H3C,H3D), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8AA,H8AB), C8(H8BC,H8BD), C9(H9A,
 H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C12(H12C,H12D), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C20(H20C,H20D), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C29(H29C,H29D),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C47(H47C,H47D),
  C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
5.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C94(H94), C95(H95),
 C96(H96), C97(H97), C98(H98), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104), C106(H106), C107(H107), C108(H108), C109(H109), C110(H110),
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122)
;
_olex2_date_sample_data_collection 2021-04-23
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.769
_oxdiff_exptl_absorpt_empirical_full_min 0.634
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 0.205080 0.531560 0.735129 0.02059(3) Uani 1 1 d . . . . .
U2 U 0.320150 0.541910 0.758301 0.02732(4) Uani 1 1 d . . . . .
O1 O 0.14297(9) 0.64944(19) 0.68994(10) 0.0314(5) Uani 1 1 d . . . . .
O2 O 0.16602(12) 0.4418(2) 0.64420(11) 0.0464(7) Uani 1 1 d D . . . .
O3 O 0.16667(8) 0.38565(18) 0.76447(10) 0.0295(5) Uani 1 1 d D . . . .
O4 O 0.17582(9) 0.59010(18) 0.81560(10) 0.0314(5) Uani 1 1 d D . . . .
O5 O 0.33863(10) 0.4541(2) 0.67633(11) 0.0359(5) Uani 1 1 d . . . . .
O6 O 0.37628(10) 0.6711(2) 0.74465(13) 0.0477(7) Uani 1 1 d D . . . .
O7 O 0.35201(12) 0.5788(3) 0.86297(12) 0.0498(7) Uani 1 1 d D . . . .
O8 O 0.37939(10) 0.4035(2) 0.79816(11) 0.0414(6) Uani 1 1 d D . . . .
N1 N 0.26731(10) 0.4535(2) 0.76744(12) 0.0253(5) Uani 1 1 d . . . . .
N2 N 0.26361(12) 0.6624(2) 0.77606(14) 0.0361(6) Uani 1 1 d . . . . .
H2A H 0.260344 0.719801 0.754965 0.043 Uiso 1 1 calc R U . . .
H2B H 0.267353 0.675767 0.813651 0.043 Uiso 1 1 calc R U . . .
N3 N 0.25426(11) 0.5864(3) 0.67537(13) 0.0343(6) Uani 1 1 d . . . . .
H3A H 0.251698 0.547767 0.643876 0.041 Uiso 1 1 calc R U . . .
H3B H 0.252079 0.653152 0.666636 0.041 Uiso 1 1 calc R U . . .
C1 C 0.14739(15) 0.7423(3) 0.65857(19) 0.0425(9) Uani 1 1 d . . . . .
H1A H 0.168454 0.731470 0.634091 0.051 Uiso 1 1 calc R U . . .
H1B H 0.160028 0.798158 0.685385 0.051 Uiso 1 1 calc R U . . .
C2 C 0.09764(15) 0.7644(3) 0.62278(19) 0.0420(8) Uani 1 1 d . . . . .
H2C H 0.088867 0.723527 0.587388 0.050 Uiso 1 1 calc R U . . .
H2D H 0.093424 0.836570 0.612611 0.050 Uiso 1 1 calc R U . . .
C3 C 0.06915(14) 0.7340(3) 0.66333(17) 0.0393(8) Uani 1 1 d . . . . .
H3C H 0.071742 0.784963 0.693640 0.047 Uiso 1 1 calc R U . . .
H3D H 0.035438 0.723636 0.642478 0.047 Uiso 1 1 calc R U . . .
C4 C 0.09265(13) 0.6366(3) 0.68767(17) 0.0367(7) Uani 1 1 d . . . . .
H4A H 0.089416 0.624634 0.726387 0.044 Uiso 1 1 calc R U . . .
H4B H 0.078500 0.579205 0.662782 0.044 Uiso 1 1 calc R U . . .
C5 C 0.1399(5) 0.4891(9) 0.5894(4) 0.048(3) Uani 0.519(17) 1 d D . P A 1
H5A H 0.157555 0.546664 0.579906 0.057 Uiso 0.519(17) 1 calc R U P A 1
H5B H 0.108217 0.512109 0.590044 0.057 Uiso 0.519(17) 1 calc R U P A 1
C6 C 0.1367(4) 0.4035(8) 0.5484(3) 0.053(2) Uani 0.519(17) 1 d D . P A 1
H6A H 0.167707 0.387546 0.542614 0.063 Uiso 0.519(17) 1 calc R U P A 1
H6B H 0.113338 0.416784 0.510954 0.063 Uiso 0.519(17) 1 calc R U P A 1
C7 C 0.1203(6) 0.3218(13) 0.5815(5) 0.069(3) Uani 0.519(17) 1 d D . P A 1
H7A H 0.089076 0.336663 0.587060 0.083 Uiso 0.519(17) 1 calc R U P A 1
H7B H 0.119823 0.254454 0.563975 0.083 Uiso 0.519(17) 1 calc R U P A 1
C8 C 0.15993(18) 0.3337(3) 0.63529(19) 0.0497(9) Uani 1 1 d D . . . .
H8AA H 0.151952 0.301600 0.667917 0.060 Uiso 0.519(17) 1 calc R U P A 1
H8AB H 0.189182 0.302632 0.631083 0.060 Uiso 0.519(17) 1 calc R U P A 1
H8BC H 0.147846 0.301667 0.664903 0.060 Uiso 0.481(17) 1 calc R U P A 2
H8BD H 0.189705 0.300500 0.634473 0.060 Uiso 0.481(17) 1 calc R U P A 2
C9 C 0.1558(4) 0.4920(10) 0.5870(4) 0.047(3) Uani 0.481(17) 1 d D . P A 2
H9A H 0.181865 0.482035 0.569590 0.057 Uiso 0.481(17) 1 calc R U P A 2
H9B H 0.150011 0.564971 0.589687 0.057 Uiso 0.481(17) 1 calc R U P A 2
C10 C 0.1117(5) 0.4374(11) 0.5540(4) 0.069(3) Uani 0.481(17) 1 d D . P A 2
H10A H 0.107194 0.439973 0.512285 0.083 Uiso 0.481(17) 1 calc R U P A 2
H10B H 0.083227 0.464052 0.562643 0.083 Uiso 0.481(17) 1 calc R U P A 2
C11 C 0.1241(10) 0.3320(15) 0.5780(8) 0.109(9) Uani 0.481(17) 1 d D . P A 2
H11A H 0.095148 0.298231 0.581243 0.131 Uiso 0.481(17) 1 calc R U P A 2
H11B H 0.136576 0.292410 0.551178 0.131 Uiso 0.481(17) 1 calc R U P A 2
C12 C 0.11508(13) 0.3769(3) 0.75214(19) 0.0403(8) Uani 1 1 d D . . . .
H12A H 0.098989 0.394225 0.711812 0.048 Uiso 0.778(16) 1 calc R U P B 1
H12B H 0.103172 0.421330 0.777431 0.048 Uiso 0.778(16) 1 calc R U P B 1
H12C H 0.100030 0.382768 0.710450 0.048 Uiso 0.222(16) 1 calc R U P B 2
H12D H 0.103037 0.431947 0.771374 0.048 Uiso 0.222(16) 1 calc R U P B 2
C13 C 0.1075(3) 0.2667(5) 0.7640(6) 0.0473(18) Uani 0.778(16) 1 d D . P B 1
H13A H 0.105851 0.224235 0.730126 0.057 Uiso 0.778(16) 1 calc R U P B 1
H13B H 0.078460 0.257169 0.775740 0.057 Uiso 0.778(16) 1 calc R U P B 1
C14 C 0.1520(2) 0.2433(5) 0.8133(4) 0.050(2) Uani 0.778(16) 1 d D . P B 1
H14A H 0.149881 0.272286 0.849807 0.061 Uiso 0.778(16) 1 calc R U P B 1
H14B H 0.157607 0.170009 0.817911 0.061 Uiso 0.778(16) 1 calc R U P B 1
C15 C 0.1898(3) 0.2949(6) 0.7926(5) 0.043(2) Uani 0.778(16) 1 d D . P B 1
H15A H 0.217547 0.311813 0.825047 0.051 Uiso 0.778(16) 1 calc R U P B 1
H15B H 0.200013 0.251606 0.765382 0.051 Uiso 0.778(16) 1 calc R U P B 1
C16 C 0.1028(10) 0.2771(18) 0.773(2) 0.056(9) Uani 0.222(16) 1 d D . P B 2
H16A H 0.075547 0.245505 0.744793 0.067 Uiso 0.222(16) 1 calc R U P B 2
H16B H 0.095813 0.283645 0.810110 0.067 Uiso 0.222(16) 1 calc R U P B 2
C17 C 0.1478(6) 0.2189(12) 0.7789(11) 0.036(4) Uani 0.222(16) 1 d D . P B 2
H17A H 0.151355 0.163355 0.806767 0.044 Uiso 0.222(16) 1 calc R U P B 2
H17B H 0.148849 0.191049 0.741623 0.044 Uiso 0.222(16) 1 calc R U P B 2
C18 C 0.1853(8) 0.2978(15) 0.8000(13) 0.028(3) Uani 0.222(16) 1 d D . P B 2
H18A H 0.189895 0.312651 0.840984 0.034 Uiso 0.222(16) 1 calc R U P B 2
H18B H 0.215799 0.275953 0.794720 0.034 Uiso 0.222(16) 1 calc R U P B 2
C19 C 0.16622(16) 0.6956(3) 0.82558(17) 0.0427(8) Uani 1 1 d D . . . .
H19A H 0.131975 0.706950 0.818915 0.051 Uiso 1 1 calc R U . . .
H19B H 0.177732 0.740635 0.800194 0.051 Uiso 1 1 calc R U . . .
C20 C 0.1928(2) 0.7133(4) 0.88713(18) 0.0548(11) Uani 1 1 d D . . . .
H20A H 0.179001 0.769667 0.903474 0.066 Uiso 0.916(12) 1 calc R U P C 1
H20B H 0.226555 0.727328 0.891786 0.066 Uiso 0.916(12) 1 calc R U P C 1
H20C H 0.170393 0.730872 0.908967 0.066 Uiso 0.084(12) 1 calc R U P C 2
H20D H 0.214966 0.770181 0.890078 0.066 Uiso 0.084(12) 1 calc R U P C 2
C21 C 0.1863(3) 0.6144(4) 0.9141(2) 0.072(2) Uani 0.916(12) 1 d D . P C 1
H21A H 0.156306 0.613939 0.924516 0.087 Uiso 0.916(12) 1 calc R U P C 1
H21B H 0.212707 0.601992 0.949006 0.087 Uiso 0.916(12) 1 calc R U P C 1
C22 C 0.1855(3) 0.5350(4) 0.86888(19) 0.0495(16) Uani 0.916(12) 1 d D . P C 1
H22A H 0.216256 0.500080 0.877224 0.059 Uiso 0.916(12) 1 calc R U P C 1
H22B H 0.160465 0.484649 0.867253 0.059 Uiso 0.916(12) 1 calc R U P C 1
C23 C 0.2197(16) 0.620(2) 0.9118(17) 0.040(6) Uani 0.084(12) 1 d D . P C 2
H23A H 0.223687 0.611094 0.953184 0.048 Uiso 0.084(12) 1 calc R U P C 2
H23B H 0.250343 0.613279 0.903297 0.048 Uiso 0.084(12) 1 calc R U P C 2
C24 C 0.181(2) 0.555(4) 0.8742(9) 0.033(4) Uani 0.084(12) 1 d D . P C 2
H24A H 0.189979 0.483201 0.878259 0.040 Uiso 0.084(12) 1 calc R U P C 2
H24B H 0.151137 0.564038 0.884259 0.040 Uiso 0.084(12) 1 calc R U P C 2
C25 C 0.34006(15) 0.4955(3) 0.62167(16) 0.0402(8) Uani 1 1 d . . . . .
H25A H 0.372320 0.490583 0.617533 0.048 Uiso 1 1 calc R U . . .
H25B H 0.330361 0.567035 0.618468 0.048 Uiso 1 1 calc R U . . .
C26 C 0.30557(17) 0.4326(3) 0.57611(17) 0.0452(9) Uani 1 1 d . . . . .
H26A H 0.321435 0.403798 0.549074 0.054 Uiso 1 1 calc R U . . .
H26B H 0.278571 0.474078 0.554374 0.054 Uiso 1 1 calc R U . . .
C27 C 0.28892(16) 0.3492(3) 0.60866(17) 0.0442(8) Uani 1 1 d . . . . .
H27A H 0.257114 0.364044 0.612324 0.053 Uiso 1 1 calc R U . . .
H27B H 0.288174 0.283471 0.589386 0.053 Uiso 1 1 calc R U . . .
C28 C 0.32524(18) 0.3499(3) 0.66584(17) 0.0462(9) Uani 1 1 d . . . . .
H28A H 0.311831 0.323634 0.695785 0.055 Uiso 1 1 calc R U . . .
H28B H 0.352823 0.308208 0.665138 0.055 Uiso 1 1 calc R U . . .
C29 C 0.36759(16) 0.7581(3) 0.7074(2) 0.0485(10) Uani 1 1 d D . . . .
H29A H 0.364040 0.819841 0.728476 0.058 Uiso 0.671(17) 1 calc R U P D 1
H29B H 0.339002 0.748770 0.674725 0.058 Uiso 0.671(17) 1 calc R U P D 1
H29C H 0.368884 0.820074 0.730301 0.058 Uiso 0.329(17) 1 calc R U P D 2
H29D H 0.335803 0.753280 0.679727 0.058 Uiso 0.329(17) 1 calc R U P D 2
C30 C 0.4123(4) 0.7622(16) 0.6876(7) 0.064(4) Uani 0.671(17) 1 d D . P D 1
H30A H 0.404885 0.743025 0.646804 0.077 Uiso 0.671(17) 1 calc R U P D 1
H30B H 0.425516 0.831189 0.692124 0.077 Uiso 0.671(17) 1 calc R U P D 1
C31 C 0.4475(4) 0.6893(11) 0.7242(6) 0.070(4) Uani 0.671(17) 1 d D . P D 1
H31A H 0.448401 0.625049 0.704038 0.084 Uiso 0.671(17) 1 calc R U P D 1
H31B H 0.479669 0.718432 0.736988 0.084 Uiso 0.671(17) 1 calc R U P D 1
C32 C 0.4269(2) 0.6767(7) 0.7722(3) 0.0468(18) Uani 0.671(17) 1 d D . P D 1
H32A H 0.438561 0.614244 0.793763 0.056 Uiso 0.671(17) 1 calc R U P D 1
H32B H 0.434737 0.734648 0.798696 0.056 Uiso 0.671(17) 1 calc R U P D 1
C33 C 0.4045(8) 0.762(3) 0.6762(12) 0.052(4) Uani 0.329(17) 1 d D . P D 2
H33A H 0.410993 0.832151 0.666821 0.062 Uiso 0.329(17) 1 calc R U P D 2
H33B H 0.395363 0.721490 0.640736 0.062 Uiso 0.329(17) 1 calc R U P D 2
C34 C 0.4458(8) 0.7168(16) 0.7206(12) 0.052(4) Uani 0.329(17) 1 d D . P D 2
H34A H 0.460432 0.766459 0.750680 0.062 Uiso 0.329(17) 1 calc R U P D 2
H34B H 0.470016 0.692284 0.703010 0.062 Uiso 0.329(17) 1 calc R U P D 2
C35 C 0.4242(5) 0.6295(13) 0.7452(10) 0.057(5) Uani 0.329(17) 1 d D . P D 2
H35A H 0.421002 0.568758 0.720976 0.069 Uiso 0.329(17) 1 calc R U P D 2
H35B H 0.443386 0.612968 0.784577 0.069 Uiso 0.329(17) 1 calc R U P D 2
C36 C 0.3257(3) 0.5483(7) 0.9051(3) 0.060(2) Uani 0.733(14) 1 d D . P E 1
H36A H 0.296619 0.588592 0.899766 0.072 Uiso 0.733(14) 1 calc R U P E 1
H36B H 0.317355 0.476004 0.901445 0.072 Uiso 0.733(14) 1 calc R U P E 1
C37 C 0.3609(5) 0.5704(11) 0.9617(4) 0.063(3) Uani 0.733(14) 1 d D . P E 1
H37A H 0.345009 0.583138 0.991611 0.075 Uiso 0.733(14) 1 calc R U P E 1
H37B H 0.383538 0.514197 0.974050 0.075 Uiso 0.733(14) 1 calc R U P E 1
C38 C 0.3850(8) 0.6630(11) 0.9494(5) 0.080(4) Uani 0.733(14) 1 d D . P E 1
H38A H 0.415756 0.673702 0.978474 0.096 Uiso 0.733(14) 1 calc R U P E 1
H38B H 0.365048 0.723426 0.947286 0.096 Uiso 0.733(14) 1 calc R U P E 1
C39 C 0.3914(3) 0.6374(9) 0.8917(4) 0.069(3) Uani 0.733(14) 1 d D . P E 1
H39A H 0.392775 0.699465 0.869903 0.082 Uiso 0.733(14) 1 calc R U P E 1
H39B H 0.420937 0.599015 0.896457 0.082 Uiso 0.733(14) 1 calc R U P E 1
C40 C 0.3609(10) 0.5127(12) 0.9113(6) 0.063(6) Uani 0.267(14) 1 d D . P E 2
H40A H 0.391177 0.476955 0.916532 0.075 Uiso 0.267(14) 1 calc R U P E 2
H40B H 0.335356 0.462008 0.905301 0.075 Uiso 0.267(14) 1 calc R U P E 2
C41 C 0.363(2) 0.575(3) 0.9635(13) 0.085(13) Uani 0.267(14) 1 d D . P E 2
H41A H 0.332491 0.572233 0.973088 0.102 Uiso 0.267(14) 1 calc R U P E 2
H41B H 0.388541 0.552549 0.996884 0.102 Uiso 0.267(14) 1 calc R U P E 2
C42 C 0.372(2) 0.680(3) 0.9457(14) 0.079(13) Uani 0.267(14) 1 d D . P E 2
H42A H 0.401724 0.706029 0.971915 0.094 Uiso 0.267(14) 1 calc R U P E 2
H42B H 0.345934 0.725042 0.947378 0.094 Uiso 0.267(14) 1 calc R U P E 2
C43 C 0.3759(9) 0.6758(13) 0.8857(10) 0.057(5) Uani 0.267(14) 1 d D . P E 2
H43A H 0.359672 0.733685 0.862862 0.069 Uiso 0.267(14) 1 calc R U P E 2
H43B H 0.409373 0.675342 0.885505 0.069 Uiso 0.267(14) 1 calc R U P E 2
C44 C 0.3714(4) 0.3386(6) 0.8428(4) 0.0538(19) Uani 0.690(13) 1 d D . P F 1
H44A H 0.337265 0.325628 0.835958 0.065 Uiso 0.690(13) 1 calc R U P F 1
H44B H 0.383938 0.370296 0.880875 0.065 Uiso 0.690(13) 1 calc R U P F 1
C45 C 0.3974(2) 0.2417(5) 0.8396(3) 0.0452(17) Uani 0.690(13) 1 d D . P F 1
H45A H 0.375362 0.184023 0.831179 0.054 Uiso 0.690(13) 1 calc R U P F 1
H45B H 0.422094 0.228797 0.876037 0.054 Uiso 0.690(13) 1 calc R U P F 1
C46 C 0.4194(3) 0.2582(6) 0.7913(3) 0.0529(19) Uani 0.690(13) 1 d D . P F 1
H46A H 0.399642 0.227532 0.755434 0.064 Uiso 0.690(13) 1 calc R U P F 1
H46B H 0.451343 0.228077 0.800795 0.064 Uiso 0.690(13) 1 calc R U P F 1
C47 C 0.42205(16) 0.3755(4) 0.7848(2) 0.0544(10) Uani 1 1 d D . . . .
H47A H 0.450446 0.404375 0.812336 0.065 Uiso 0.690(13) 1 calc R U P F 1
H47B H 0.421242 0.395250 0.745432 0.065 Uiso 0.690(13) 1 calc R U P F 1
H47C H 0.448369 0.406472 0.814631 0.065 Uiso 0.310(13) 1 calc R U P F 2
H47D H 0.421023 0.409838 0.748480 0.065 Uiso 0.310(13) 1 calc R U P F 2
C48 C 0.3795(6) 0.3117(10) 0.8319(8) 0.044(3) Uani 0.310(13) 1 d D . P F 2
H48A H 0.347011 0.294515 0.832055 0.053 Uiso 0.310(13) 1 calc R U P F 2
H48B H 0.399090 0.321649 0.871826 0.053 Uiso 0.310(13) 1 calc R U P F 2
C49 C 0.3997(5) 0.2297(12) 0.8041(10) 0.052(4) Uani 0.310(13) 1 d D . P F 2
H49A H 0.374227 0.197463 0.773667 0.063 Uiso 0.310(13) 1 calc R U P F 2
H49B H 0.414401 0.177777 0.832715 0.063 Uiso 0.310(13) 1 calc R U P F 2
C50 C 0.4360(6) 0.2731(10) 0.7788(9) 0.060(3) Uani 0.310(13) 1 d D . P F 2
H50A H 0.468741 0.258392 0.801776 0.072 Uiso 0.310(13) 1 calc R U P F 2
H50B H 0.431136 0.253141 0.738458 0.072 Uiso 0.310(13) 1 calc R U P F 2
C51 C -0.11475(11) 0.4883(2) 0.64741(13) 0.0229(5) Uani 1 1 d . . . . .
C52 C -0.12871(13) 0.4619(3) 0.69582(14) 0.0277(6) Uani 1 1 d . . . . .
H52 H -0.105041 0.444588 0.729975 0.033 Uiso 1 1 calc R U . . .
C53 C -0.17583(14) 0.4599(3) 0.69588(17) 0.0352(7) Uani 1 1 d . . . . .
H53 H -0.183503 0.441895 0.729793 0.042 Uiso 1 1 calc R U . . .
C54 C -0.21153(13) 0.4839(3) 0.64708(16) 0.0351(7) Uani 1 1 d . . . . .
H54 H -0.243644 0.482696 0.647097 0.042 Uiso 1 1 calc R U . . .
C55 C -0.19934(12) 0.5099(3) 0.59786(15) 0.0322(7) Uani 1 1 d . . . . .
H55 H -0.223244 0.526312 0.563752 0.039 Uiso 1 1 calc R U . . .
C56 C -0.15192(12) 0.5118(3) 0.59879(14) 0.0267(6) Uani 1 1 d . . . . .
H56 H -0.144464 0.530030 0.564764 0.032 Uiso 1 1 calc R U . . .
C57 C -0.04875(11) 0.3792(2) 0.61852(13) 0.0222(5) Uani 1 1 d . . . . .
C58 C -0.08353(13) 0.3254(3) 0.57862(15) 0.0323(7) Uani 1 1 d . . . . .
H58 H -0.115195 0.348766 0.569044 0.039 Uiso 1 1 calc R U . . .
C59 C -0.07358(14) 0.2384(3) 0.55217(17) 0.0376(8) Uani 1 1 d . . . . .
H59 H -0.098212 0.204717 0.524582 0.045 Uiso 1 1 calc R U . . .
C60 C -0.02840(14) 0.2012(3) 0.56585(15) 0.0336(7) Uani 1 1 d . . . . .
H60 H -0.021609 0.141632 0.548256 0.040 Uiso 1 1 calc R U . . .
C61 C 0.00684(13) 0.2515(3) 0.60533(15) 0.0326(7) Uani 1 1 d . . . . .
H61 H 0.038237 0.226469 0.615252 0.039 Uiso 1 1 calc R U . . .
C62 C -0.00320(12) 0.3388(3) 0.63086(14) 0.0276(6) Uani 1 1 d . . . . .
H62 H 0.021875 0.372552 0.657779 0.033 Uiso 1 1 calc R U . . .
C63 C -0.02404(11) 0.4987(2) 0.71156(13) 0.0212(5) Uani 1 1 d . . . . .
C64 C -0.01341(12) 0.4163(2) 0.74930(13) 0.0257(6) Uani 1 1 d . . . . .
H64 H -0.025578 0.352077 0.735492 0.031 Uiso 1 1 calc R U . . .
C65 C 0.01401(12) 0.4245(3) 0.80574(14) 0.0292(6) Uani 1 1 d . . . . .
H65 H 0.019998 0.366678 0.829621 0.035 Uiso 1 1 calc R U . . .
C66 C 0.03273(12) 0.5170(3) 0.82739(14) 0.0290(6) Uani 1 1 d . . . . .
H66 H 0.051735 0.523099 0.865895 0.035 Uiso 1 1 calc R U . . .
C67 C 0.02314(12) 0.6002(3) 0.79178(14) 0.0276(6) Uani 1 1 d . . . . .
H67 H 0.035605 0.664080 0.805915 0.033 Uiso 1 1 calc R U . . .
C68 C -0.00473(11) 0.5907(2) 0.73523(13) 0.0234(5) Uani 1 1 d . . . . .
H68 H -0.010878 0.649027 0.711769 0.028 Uiso 1 1 calc R U . . .
C69 C -0.04951(11) 0.5778(2) 0.60502(12) 0.0221(5) Uani 1 1 d . . . . .
C70 C -0.07077(12) 0.6726(2) 0.60307(13) 0.0258(6) Uani 1 1 d . . . . .
H70 H -0.091697 0.683338 0.625622 0.031 Uiso 1 1 calc R U . . .
C71 C -0.06267(13) 0.7517(3) 0.56965(14) 0.0292(6) Uani 1 1 d . . . . .
H71 H -0.077918 0.814535 0.569833 0.035 Uiso 1 1 calc R U . . .
C72 C -0.03235(14) 0.7389(3) 0.53609(15) 0.0334(7) Uani 1 1 d . . . . .
H72 H -0.026624 0.792458 0.513217 0.040 Uiso 1 1 calc R U . . .
C73 C -0.01048(15) 0.6459(3) 0.53657(15) 0.0360(7) Uani 1 1 d . . . . .
H73 H 0.010405 0.635792 0.513908 0.043 Uiso 1 1 calc R U . . .
C74 C -0.01916(13) 0.5678(3) 0.57018(14) 0.0289(6) Uani 1 1 d . . . . .
H74 H -0.003954 0.504979 0.569602 0.035 Uiso 1 1 calc R U . . .
B1 B -0.05916(13) 0.4864(3) 0.64596(15) 0.0223(5) Uani 1 1 d . . . . .
C75 C 0.16443(12) 0.9984(2) 0.59104(14) 0.0282(6) Uani 1 1 d . . . . .
C76 C 0.15212(14) 1.0191(3) 0.64124(16) 0.0338(7) Uani 1 1 d . . . . .
H76 H 0.176590 1.024910 0.676177 0.041 Uiso 1 1 calc R U . . .
C77 C 0.10531(15) 1.0315(3) 0.6420(2) 0.0414(8) Uani 1 1 d . . . . .
H77 H 0.098585 1.045265 0.677070 0.050 Uiso 1 1 calc R U . . .
C78 C 0.06889(15) 1.0237(3) 0.5920(2) 0.0420(8) Uani 1 1 d . . . . .
H78 H 0.037024 1.031284 0.592324 0.050 Uiso 1 1 calc R U . . .
C79 C 0.07959(14) 1.0045(3) 0.54131(18) 0.0385(7) Uani 1 1 d . . . . .
H79 H 0.054957 1.000139 0.506438 0.046 Uiso 1 1 calc R U . . .
C80 C 0.12629(13) 0.9916(3) 0.54135(16) 0.0332(7) Uani 1 1 d . . . . .
H80 H 0.132615 0.977576 0.506115 0.040 Uiso 1 1 calc R U . . .
C81 C 0.22771(13) 1.0743(3) 0.54216(14) 0.0295(6) Uani 1 1 d . . . . .
C82 C 0.19603(17) 1.1523(4) 0.5209(2) 0.0590(13) Uani 1 1 d . . . . .
H82 H 0.168863 1.157855 0.534081 0.071 Uiso 1 1 calc R U . . .
C83 C 0.20231(19) 1.2229(5) 0.4812(2) 0.0686(15) Uani 1 1 d . . . . .
H83 H 0.179054 1.273173 0.467098 0.082 Uiso 1 1 calc R U . . .
C84 C 0.24154(18) 1.2199(4) 0.46245(18) 0.0496(9) Uani 1 1 d . . . . .
H84 H 0.246009 1.267772 0.435566 0.059 Uiso 1 1 calc R U . . .
C85 C 0.2741(2) 1.1467(4) 0.4833(2) 0.0557(11) Uani 1 1 d . . . . .
H85 H 0.302011 1.144065 0.471399 0.067 Uiso 1 1 calc R U . . .
C86 C 0.26706(17) 1.0755(3) 0.5219(2) 0.0500(10) Uani 1 1 d . . . . .
H86 H 0.290400 1.025015 0.535037 0.060 Uiso 1 1 calc R U . . .
C87 C 0.25343(12) 1.0137(3) 0.65392(14) 0.0295(6) Uani 1 1 d . . . . .
C88 C 0.26257(15) 1.1117(3) 0.67538(16) 0.0401(8) Uani 1 1 d . . . . .
H88 H 0.253483 1.166570 0.649621 0.048 Uiso 1 1 calc R U . . .
C89 C 0.28441(18) 1.1321(4) 0.73283(18) 0.0486(9) Uani 1 1 d . . . . .
H89 H 0.288767 1.199761 0.745809 0.058 Uiso 1 1 calc R U . . .
C90 C 0.29992(16) 1.0532(4) 0.77140(17) 0.0455(8) Uani 1 1 d . . . . .
H90 H 0.315825 1.066584 0.810402 0.055 Uiso 1 1 calc R U . . .
C91 C 0.29185(16) 0.9562(3) 0.75215(17) 0.0428(8) Uani 1 1 d . . . . .
H91 H 0.301797 0.901765 0.778019 0.051 Uiso 1 1 calc R U . . .
C92 C 0.26905(14) 0.9372(3) 0.69461(15) 0.0363(7) Uani 1 1 d . . . . .
H92 H 0.263838 0.869233 0.682395 0.044 Uiso 1 1 calc R U . . .
C93 C 0.23320(13) 0.8772(3) 0.57028(13) 0.0303(6) Uani 1 1 d . . . . .
C94 C 0.20023(15) 0.8018(3) 0.54831(14) 0.0347(7) Uani 1 1 d . . . . .
H94 H 0.168225 0.812958 0.547056 0.042 Uiso 1 1 calc R U . . .
C95 C 0.21248(18) 0.7098(3) 0.52791(16) 0.0443(8) Uani 1 1 d . . . . .
H95 H 0.188939 0.660244 0.513373 0.053 Uiso 1 1 calc R U . . .
C96 C 0.2587(2) 0.6914(3) 0.52899(17) 0.0509(9) Uani 1 1 d . . . . .
H96 H 0.266840 0.631035 0.513298 0.061 Uiso 1 1 calc R U . . .
C97 C 0.29299(19) 0.7621(3) 0.55322(18) 0.0486(9) Uani 1 1 d . . . . .
H97 H 0.325111 0.749195 0.555688 0.058 Uiso 1 1 calc R U . . .
C98 C 0.28030(15) 0.8521(3) 0.57396(16) 0.0383(7) Uani 1 1 d . . . . .
H98 H 0.304477 0.898822 0.591381 0.046 Uiso 1 1 calc R U . . .
B2 B 0.21968(14) 0.9902(3) 0.58910(16) 0.0280(6) Uani 1 1 d . . . . .
C99 C 0.41360(12) 0.3755(3) 0.51643(14) 0.0297(6) Uani 1 1 d . . . . .
C100 C 0.37512(13) 0.3412(3) 0.47148(15) 0.0350(7) Uani 1 1 d . . . . .
H100 H 0.373322 0.271585 0.462217 0.042 Uiso 1 1 calc R U . . .
C101 C 0.33989(14) 0.4043(4) 0.44028(16) 0.0409(7) Uani 1 1 d . . . . .
H101 H 0.314565 0.377682 0.410481 0.049 Uiso 1 1 calc R U . . .
C102 C 0.34146(15) 0.5065(4) 0.45242(18) 0.0444(8) Uani 1 1 d . . . . .
H102 H 0.317237 0.550013 0.431245 0.053 Uiso 1 1 calc R U . . .
C103 C 0.37880(15) 0.5441(3) 0.49581(19) 0.0417(8) Uani 1 1 d . . . . .
H103 H 0.380478 0.613997 0.504379 0.050 Uiso 1 1 calc R U . . .
C104 C 0.41389(14) 0.4792(3) 0.52685(17) 0.0339(7) Uani 1 1 d . . . . .
H104 H 0.439172 0.506570 0.556442 0.041 Uiso 1 1 calc R U . . .
C105 C 0.49602(13) 0.3595(3) 0.60007(14) 0.0296(6) Uani 1 1 d . . . . .
C106 C 0.48518(15) 0.3925(3) 0.64949(16) 0.0403(8) Uani 1 1 d . . . . .
H106 H 0.454993 0.377076 0.653719 0.048 Uiso 1 1 calc R U . . .
C107 C 0.51676(18) 0.4466(3) 0.69236(18) 0.0473(9) Uani 1 1 d . . . . .
H107 H 0.507776 0.468128 0.724840 0.057 Uiso 1 1 calc R U . . .
C108 C 0.56116(19) 0.4695(3) 0.68811(19) 0.0497(10) Uani 1 1 d . . . . .
H108 H 0.582938 0.506064 0.717574 0.060 Uiso 1 1 calc R U . . .
C109 C 0.57341(17) 0.4383(4) 0.64033(19) 0.0508(10) Uani 1 1 d . . . . .
H109 H 0.603714 0.453837 0.636522 0.061 Uiso 1 1 calc R U . . .
C110 C 0.54130(14) 0.3840(3) 0.59778(16) 0.0393(8) Uani 1 1 d . . . . .
H110 H 0.550672 0.362485 0.565573 0.047 Uiso 1 1 calc R U . . .
C111 C 0.47797(12) 0.2520(3) 0.50112(14) 0.0280(6) Uani 1 1 d . . . . .
C112 C 0.49650(14) 0.3166(3) 0.46723(15) 0.0342(7) Uani 1 1 d . . . . .
H112 H 0.495152 0.387213 0.472679 0.041 Uiso 1 1 calc R U . . .
C113 C 0.51669(14) 0.2810(3) 0.42606(16) 0.0369(7) Uani 1 1 d . . . . .
H113 H 0.529532 0.327046 0.404761 0.044 Uiso 1 1 calc R U . . .
C114 C 0.51810(15) 0.1785(3) 0.41606(16) 0.0394(8) Uani 1 1 d . . . . .
H114 H 0.532568 0.153799 0.388679 0.047 Uiso 1 1 calc R U . . .
C115 C 0.49827(16) 0.1131(3) 0.44632(17) 0.0422(9) Uani 1 1 d . . . . .
H115 H 0.497800 0.042986 0.438744 0.051 Uiso 1 1 calc R U . . .
C116 C 0.47885(15) 0.1498(3) 0.48811(16) 0.0353(7) Uani 1 1 d . . . . .
H116 H 0.465612 0.103212 0.508670 0.042 Uiso 1 1 calc R U . . .
C117 C 0.43636(13) 0.2087(3) 0.58425(14) 0.0297(6) Uani 1 1 d . . . . .
C118 C 0.46826(14) 0.1388(3) 0.61766(16) 0.0363(7) Uani 1 1 d . . . . .
H118 H 0.500345 0.141954 0.617642 0.044 Uiso 1 1 calc R U . . .
C119 C 0.45531(16) 0.0657(3) 0.65055(17) 0.0409(8) Uani 1 1 d . . . . .
H119 H 0.478218 0.019905 0.672127 0.049 Uiso 1 1 calc R U . . .
C120 C 0.40897(17) 0.0594(3) 0.65202(18) 0.0427(8) Uani 1 1 d . . . . .
H120 H 0.399953 0.010336 0.675155 0.051 Uiso 1 1 calc R U . . .
C121 C 0.37611(17) 0.1252(3) 0.6195(2) 0.0475(10) Uani 1 1 d . . . . .
H121 H 0.344108 0.121213 0.619814 0.057 Uiso 1 1 calc R U . . .
C122 C 0.38987(15) 0.1981(3) 0.58586(18) 0.0398(8) Uani 1 1 d . . . . .
H122 H 0.366519 0.241943 0.563251 0.048 Uiso 1 1 calc R U . . .
B3 B 0.45580(14) 0.2983(3) 0.55028(16) 0.0290(6) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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
1 0 0 0.0369
-1 0 0 0.0210
-2 -1 -1 0.0659
-2 -1 1 0.0646
-1 -2 -1 0.0769
1 0 -2 0.0971
1 -1 -2 0.0779
-1 -2 1 0.0783
-1 2 2 0.0622
1 2 -1 0.0705
-1 -2 2 0.0779
1 -2 -2 0.0707
2 -1 -1 0.0647
18 3 -3 0.0535
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 U2 131.47(6) . . ?
O1 U1 O2 78.91(10) . . ?
O1 U1 O3 106.84(8) . . ?
O1 U1 O4 76.55(8) . . ?
O1 U1 N2 94.62(10) . . ?
O1 U1 N3 92.19(9) . . ?
O2 U1 U2 111.40(8) . . ?
O3 U1 U2 121.69(5) . . ?
O3 U1 O2 75.34(9) . . ?
O3 U1 O4 73.84(8) . . ?
O4 U1 U2 115.38(6) . . ?
O4 U1 O2 132.51(10) . . ?
N1 U1 U2 35.84(8) . . ?
N1 U1 O1 167.21(10) . . ?
N1 U1 O2 103.54(11) . . ?
N1 U1 O3 85.86(9) . . ?
N1 U1 O4 109.26(10) . . ?
N1 U1 N2 75.72(11) . . ?
N1 U1 N3 76.13(11) . . ?
N2 U1 U2 47.67(7) . . ?
N2 U1 O2 142.55(11) . . ?
N2 U1 O3 140.52(10) . . ?
N2 U1 O4 79.72(9) . . ?
N3 U1 U2 47.74(7) . . ?
N3 U1 O2 79.31(11) . . ?
N3 U1 O3 144.36(10) . . ?
N3 U1 O4 141.09(10) . . ?
N3 U1 N2 63.98(11) . . ?
O5 U2 U1 107.17(7) . . ?
O5 U2 O8 71.54(9) . . ?
O6 U2 U1 134.94(7) . . ?
O6 U2 O5 84.67(10) . . ?
O6 U2 O7 86.07(10) . . ?
O6 U2 O8 98.00(10) . . ?
O7 U2 U1 104.53(8) . . ?
O7 U2 O5 143.18(10) . . ?
O7 U2 O8 74.61(10) . . ?
O8 U2 U1 127.06(7) . . ?
N1 U2 U1 36.75(8) . . ?
N1 U2 O5 99.82(10) . . ?
N1 U2 O6 171.42(11) . . ?
N1 U2 O7 94.43(11) . . ?
N1 U2 O8 90.38(10) . . ?
N1 U2 N2 76.75(11) . . ?
N1 U2 N3 76.96(11) . . ?
N2 U2 U1 47.98(7) . . ?
N2 U2 O5 139.80(10) . . ?
N2 U2 O6 95.09(11) . . ?
N2 U2 O7 76.49(11) . . ?
N2 U2 O8 147.24(10) . . ?
N2 U2 N3 64.21(11) . . ?
N3 U2 U1 47.83(7) . . ?
N3 U2 O5 75.91(10) . . ?
N3 U2 O6 97.24(10) . . ?
N3 U2 O7 140.71(11) . . ?
N3 U2 O8 142.39(10) . . ?
C1 O1 U1 127.4(2) . . ?
C1 O1 C4 108.3(3) . . ?
C4 O1 U1 124.3(2) . . ?
C5 O2 U1 126.1(5) . . ?
C8 O2 U1 127.7(2) . . ?
C8 O2 C5 105.9(5) . . ?
C8 O2 C9 108.5(6) . . ?
C9 O2 U1 122.3(5) . . ?
C12 O3 U1 122.8(2) . . ?
C15 O3 U1 126.7(3) . . ?
C15 O3 C12 110.4(3) . . ?
C18 O3 U1 132.5(9) . . ?
C18 O3 C12 104.5(9) . . ?
C19 O4 U1 124.0(2) . . ?
C19 O4 C24 96(2) . . ?
C22 O4 U1 121.9(3) . . ?
C22 O4 C19 109.4(3) . . ?
C24 O4 U1 135(3) . . ?
C25 O5 U2 128.8(2) . . ?
C28 O5 U2 118.5(2) . . ?
C28 O5 C25 106.2(3) . . ?
C29 O6 U2 129.3(3) . . ?
C29 O6 C32 102.9(4) . . ?
C29 O6 C35 107.1(6) . . ?
C32 O6 U2 127.8(3) . . ?
C35 O6 U2 114.0(6) . . ?
C36 O7 U2 121.7(3) . . ?
C39 O7 U2 129.2(4) . . ?
C39 O7 C36 108.8(5) . . ?
C40 O7 U2 130.2(7) . . ?
C40 O7 C43 105.5(12) . . ?
C43 O7 U2 123.0(10) . . ?
C44 O8 U2 118.2(4) . . ?
C47 O8 U2 130.9(2) . . ?
C47 O8 C44 110.9(5) . . ?
C47 O8 C48 92.9(7) . . ?
C48 O8 U2 135.0(7) . . ?
U2 N1 U1 107.41(12) . . ?
U2 N2 U1 84.36(9) . . ?
U2 N3 U1 84.43(9) . . ?
O1 C1 C2 104.3(3) . . ?
C1 C2 C3 101.6(3) . . ?
C4 C3 C2 101.8(3) . . ?
O1 C4 C3 105.0(3) . . ?
O2 C5 C6 101.4(8) . . ?
C5 C6 C7 99.0(10) . . ?
C8 C7 C6 95.8(8) . . ?
O2 C8 C7 105.5(7) . . ?
O2 C8 C11 100.3(8) . . ?
O2 C9 C10 101.2(8) . . ?
C9 C10 C11 99.3(12) . . ?
C8 C11 C10 112.0(11) . . ?
O3 C12 C13 103.7(4) . . ?
O3 C12 C16 109.8(10) . . ?
C12 C13 C14 101.8(6) . . ?
C15 C14 C13 101.2(6) . . ?
O3 C15 C14 103.9(5) . . ?
C12 C16 C17 101.0(13) . . ?
C18 C17 C16 103(2) . . ?
O3 C18 C17 103.7(13) . . ?
O4 C19 C20 104.2(3) . . ?
C19 C20 C21 101.8(4) . . ?
C19 C20 C23 109.6(16) . . ?
C20 C21 C22 105.3(4) . . ?
O4 C22 C21 105.1(4) . . ?
C20 C23 C24 90(3) . . ?
O4 C24 C23 105(3) . . ?
O5 C25 C26 105.8(3) . . ?
C25 C26 C27 105.5(3) . . ?
C28 C27 C26 103.3(4) . . ?
O5 C28 C27 104.9(3) . . ?
O6 C29 C30 102.3(6) . . ?
O6 C29 C33 108.9(10) . . ?
C31 C30 C29 107.5(8) . . ?
C32 C31 C30 99.8(8) . . ?
O6 C32 C31 104.1(7) . . ?
C29 C33 C34 100.2(14) . . ?
C33 C34 C35 104.0(17) . . ?
O6 C35 C34 102.4(12) . . ?
C37 C36 O7 102.6(6) . . ?
C38 C37 C36 102.7(10) . . ?
C37 C38 C39 101.3(9) . . ?
O7 C39 C38 106.4(8) . . ?
O7 C40 C41 108.1(19) . . ?
C42 C41 C40 103(2) . . ?
C41 C42 C43 109(2) . . ?
O7 C43 C42 103.3(19) . . ?
O8 C44 C45 105.6(5) . . ?
C44 C45 C46 104.8(5) . . ?
C45 C46 C47 105.5(5) . . ?
O8 C47 C46 99.3(5) . . ?
O8 C47 C50 124.1(8) . . ?
O8 C48 C49 106.7(11) . . ?
C48 C49 C50 109.4(13) . . ?
C47 C50 C49 93.6(11) . . ?
C52 C51 B1 123.3(3) . . ?
C56 C51 C52 114.9(3) . . ?
C56 C51 B1 121.8(3) . . ?
C53 C52 C51 122.8(3) . . ?
C54 C53 C52 120.7(3) . . ?
C53 C54 C55 118.5(3) . . ?
C54 C55 C56 119.9(3) . . ?
C55 C56 C51 123.3(3) . . ?
C58 C57 C62 115.1(3) . . ?
C58 C57 B1 122.9(3) . . ?
C62 C57 B1 121.8(3) . . ?
C57 C58 C59 122.5(3) . . ?
C60 C59 C58 120.3(4) . . ?
C59 C60 C61 119.0(3) . . ?
C60 C61 C62 120.3(3) . . ?
C61 C62 C57 122.7(3) . . ?
C64 C63 B1 121.3(3) . . ?
C68 C63 C64 114.9(3) . . ?
C68 C63 B1 123.7(3) . . ?
C65 C64 C63 123.1(3) . . ?
C64 C65 C66 120.2(3) . . ?
C67 C66 C65 118.7(3) . . ?
C66 C67 C68 120.3(3) . . ?
C67 C68 C63 122.8(3) . . ?
C70 C69 C74 114.9(3) . . ?
C70 C69 B1 121.9(3) . . ?
C74 C69 B1 123.2(3) . . ?
C71 C70 C69 123.1(3) . . ?
C72 C71 C70 120.1(3) . . ?
C71 C72 C73 118.7(3) . . ?
C74 C73 C72 120.2(3) . . ?
C73 C74 C69 122.8(3) . . ?
C57 B1 C51 109.0(3) . . ?
C57 B1 C63 110.1(3) . . ?
C57 B1 C69 107.9(2) . . ?
C63 B1 C51 109.3(2) . . ?
C63 B1 C69 110.2(3) . . ?
C69 B1 C51 110.3(3) . . ?
C76 C75 B2 123.0(3) . . ?
C80 C75 C76 115.0(3) . . ?
C80 C75 B2 121.8(3) . . ?
C77 C76 C75 122.8(4) . . ?
C78 C77 C76 120.1(4) . . ?
C77 C78 C79 118.9(4) . . ?
C78 C79 C80 120.2(4) . . ?
C79 C80 C75 123.0(4) . . ?
C82 C81 B2 122.8(3) . . ?
C86 C81 C82 113.7(4) . . ?
C86 C81 B2 123.5(3) . . ?
C81 C82 C83 123.2(5) . . ?
C84 C83 C82 120.5(5) . . ?
C85 C84 C83 118.3(4) . . ?
C84 C85 C86 120.7(5) . . ?
C81 C86 C85 123.6(5) . . ?
C88 C87 C92 114.8(3) . . ?
C88 C87 B2 122.4(3) . . ?
C92 C87 B2 122.0(3) . . ?
C89 C88 C87 122.8(4) . . ?
C88 C89 C90 120.0(4) . . ?
C91 C90 C89 119.0(4) . . ?
C90 C91 C92 120.1(4) . . ?
C91 C92 C87 123.1(4) . . ?
C94 C93 C98 115.1(3) . . ?
C94 C93 B2 124.2(3) . . ?
C98 C93 B2 120.7(3) . . ?
C93 C94 C95 122.6(4) . . ?
C96 C95 C94 120.1(4) . . ?
C95 C96 C97 119.2(4) . . ?
C96 C97 C98 119.8(4) . . ?
C97 C98 C93 123.0(4) . . ?
C75 B2 C81 108.3(3) . . ?
C75 B2 C93 112.8(3) . . ?
C87 B2 C75 107.0(3) . . ?
C87 B2 C81 111.6(3) . . ?
C87 B2 C93 108.2(3) . . ?
C93 B2 C81 109.0(3) . . ?
C100 C99 B3 121.0(3) . . ?
C104 C99 C100 114.9(3) . . ?
C104 C99 B3 124.0(3) . . ?
C101 C100 C99 122.9(4) . . ?
C100 C101 C102 120.2(4) . . ?
C103 C102 C101 119.2(4) . . ?
C102 C103 C104 119.8(4) . . ?
C103 C104 C99 123.0(4) . . ?
C106 C105 B3 119.5(3) . . ?
C110 C105 C106 114.9(4) . . ?
C110 C105 B3 125.6(3) . . ?
C107 C106 C105 122.7(4) . . ?
C108 C107 C106 120.4(4) . . ?
C107 C108 C109 118.9(4) . . ?
C108 C109 C110 119.9(4) . . ?
C109 C110 C105 123.3(4) . . ?
C112 C111 B3 120.3(3) . . ?
C116 C111 C112 115.1(3) . . ?
C116 C111 B3 124.6(3) . . ?
C113 C112 C111 122.5(4) . . ?
C114 C113 C112 120.2(4) . . ?
C115 C114 C113 119.1(3) . . ?
C114 C115 C116 120.0(4) . . ?
C115 C116 C111 123.0(3) . . ?
C118 C117 B3 119.8(3) . . ?
C122 C117 C118 114.8(3) . . ?
C122 C117 B3 125.3(3) . . ?
C119 C118 C117 123.4(4) . . ?
C118 C119 C120 120.0(4) . . ?
C121 C120 C119 119.1(4) . . ?
C120 C121 C122 120.0(4) . . ?
C117 C122 C121 122.7(4) . . ?
C99 B3 C105 110.2(3) . . ?
C99 B3 C111 105.8(3) . . ?
C99 B3 C117 112.4(3) . . ?
C111 B3 C105 111.6(3) . . ?
C111 B3 C117 111.5(3) . . ?
C117 B3 C105 105.5(3) . . ?
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 U2 3.28827(3) . ?
U1 O1 2.425(2) . ?
U1 O2 2.493(3) . ?
U1 O3 2.456(2) . ?
U1 O4 2.488(2) . ?
U1 N1 2.062(3) . ?
U1 N2 2.455(3) . ?
U1 N3 2.449(3) . ?
U2 O5 2.509(2) . ?
U2 O6 2.477(3) . ?
U2 O7 2.505(3) . ?
U2 O8 2.534(3) . ?
U2 N1 2.018(3) . ?
U2 N2 2.443(3) . ?
U2 N3 2.445(3) . ?
O1 C1 1.478(4) . ?
O1 C4 1.483(4) . ?
O2 C5 1.480(9) . ?
O2 C8 1.457(5) . ?
O2 C9 1.499(9) . ?
O3 C12 1.472(4) . ?
O3 C15 1.457(6) . ?
O3 C18 1.465(14) . ?
O4 C19 1.465(4) . ?
O4 C22 1.448(5) . ?
O4 C24 1.469(15) . ?
O5 C25 1.456(4) . ?
O5 C28 1.444(5) . ?
O6 C29 1.447(5) . ?
O6 C32 1.456(6) . ?
O6 C35 1.518(11) . ?
O7 C36 1.513(7) . ?
O7 C39 1.408(7) . ?
O7 C40 1.435(12) . ?
O7 C43 1.498(13) . ?
O8 C44 1.462(7) . ?
O8 C47 1.440(5) . ?
O8 C48 1.470(11) . ?
C1 C2 1.509(6) . ?
C2 C3 1.527(6) . ?
C3 C4 1.508(5) . ?
C5 C6 1.501(11) . ?
C6 C7 1.516(12) . ?
C7 C8 1.497(11) . ?
C8 C11 1.493(12) . ?
C9 C10 1.508(12) . ?
C10 C11 1.523(13) . ?
C12 C13 1.522(7) . ?
C12 C16 1.502(14) . ?
C13 C14 1.537(10) . ?
C14 C15 1.516(9) . ?
C16 C17 1.512(14) . ?
C17 C18 1.506(14) . ?
C19 C20 1.501(5) . ?
C20 C21 1.508(7) . ?
C20 C23 1.505(14) . ?
C21 C22 1.522(7) . ?
C23 C24 1.513(15) . ?
C25 C26 1.525(6) . ?
C26 C27 1.525(6) . ?
C27 C28 1.497(6) . ?
C29 C30 1.535(9) . ?
C29 C33 1.501(13) . ?
C30 C31 1.512(10) . ?
C31 C32 1.478(10) . ?
C33 C34 1.508(13) . ?
C34 C35 1.528(13) . ?
C36 C37 1.500(11) . ?
C37 C38 1.496(10) . ?
C38 C39 1.512(9) . ?
C40 C41 1.509(14) . ?
C41 C42 1.502(14) . ?
C42 C43 1.504(14) . ?
C44 C45 1.514(8) . ?
C45 C46 1.516(8) . ?
C46 C47 1.572(8) . ?
C47 C50 1.441(12) . ?
C48 C49 1.496(12) . ?
C49 C50 1.498(13) . ?
C51 C52 1.404(4) . ?
C51 C56 1.402(4) . ?
C51 B1 1.655(5) . ?
C52 C53 1.394(5) . ?
C53 C54 1.383(5) . ?
C54 C55 1.394(5) . ?
C55 C56 1.396(5) . ?
C57 C58 1.394(5) . ?
C57 C62 1.400(4) . ?
C57 B1 1.641(4) . ?
C58 C59 1.396(5) . ?
C59 C60 1.373(6) . ?
C60 C61 1.373(5) . ?
C61 C62 1.390(5) . ?
C63 C64 1.407(4) . ?
C63 C68 1.402(4) . ?
C63 B1 1.648(4) . ?
C64 C65 1.388(5) . ?
C65 C66 1.390(5) . ?
C66 C67 1.385(5) . ?
C67 C68 1.396(4) . ?
C69 C70 1.403(4) . ?
C69 C74 1.409(4) . ?
C69 B1 1.650(4) . ?
C70 C71 1.394(5) . ?
C71 C72 1.388(5) . ?
C72 C73 1.393(5) . ?
C73 C74 1.393(5) . ?
C75 C76 1.402(5) . ?
C75 C80 1.402(5) . ?
C75 B2 1.652(5) . ?
C76 C77 1.400(6) . ?
C77 C78 1.381(6) . ?
C78 C79 1.387(6) . ?
C79 C80 1.391(6) . ?
C81 C82 1.393(6) . ?
C81 C86 1.390(5) . ?
C81 B2 1.666(5) . ?
C82 C83 1.400(6) . ?
C83 C84 1.364(7) . ?
C84 C85 1.362(7) . ?
C85 C86 1.393(6) . ?
C87 C88 1.401(5) . ?
C87 C92 1.404(5) . ?
C87 B2 1.640(5) . ?
C88 C89 1.392(5) . ?
C89 C90 1.396(7) . ?
C90 C91 1.370(6) . ?
C91 C92 1.396(5) . ?
C93 C94 1.393(5) . ?
C93 C98 1.409(5) . ?
C93 B2 1.654(5) . ?
C94 C95 1.406(5) . ?
C95 C96 1.381(7) . ?
C96 C97 1.384(7) . ?
C97 C98 1.393(6) . ?
C99 C100 1.411(5) . ?
C99 C104 1.401(5) . ?
C99 B3 1.643(5) . ?
C100 C101 1.383(6) . ?
C101 C102 1.388(7) . ?
C102 C103 1.386(6) . ?
C103 C104 1.394(5) . ?
C105 C106 1.405(5) . ?
C105 C110 1.394(5) . ?
C105 B3 1.650(5) . ?
C106 C107 1.387(6) . ?
C107 C108 1.380(7) . ?
C108 C109 1.381(6) . ?
C109 C110 1.391(6) . ?
C111 C112 1.409(5) . ?
C111 C116 1.396(5) . ?
C111 B3 1.644(5) . ?
C112 C113 1.391(5) . ?
C113 C114 1.387(6) . ?
C114 C115 1.377(6) . ?
C115 C116 1.395(5) . ?
C117 C118 1.406(5) . ?
C117 C122 1.394(5) . ?
C117 B3 1.647(5) . ?
C118 C119 1.383(5) . ?
C119 C120 1.384(6) . ?
C120 C121 1.377(6) . ?
C121 C122 1.404(5) . ?
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 O1 C1 C2 160.3(2) . . . . ?
U1 O1 C4 C3 172.2(2) . . . . ?
U1 O2 C5 C6 165.1(6) . . . . ?
U1 O2 C8 C7 159.5(8) . . . . ?
U1 O2 C8 C11 165.8(14) . . . . ?
U1 O2 C9 C10 -149.0(9) . . . . ?
U1 O3 C12 C13 166.0(5) . . . . ?
U1 O3 C12 C16 177(2) . . . . ?
U1 O3 C15 C14 166.7(5) . . . . ?
U1 O3 C18 C17 -154.4(12) . . . . ?
U1 O4 C19 C20 -128.6(3) . . . . ?
U1 O4 C22 C21 150.8(5) . . . . ?
U1 O4 C24 C23 98(4) . . . . ?
U2 O5 C25 C26 -123.4(3) . . . . ?
U2 O5 C28 C27 115.2(3) . . . . ?
U2 O6 C29 C30 -143.1(9) . . . . ?
U2 O6 C29 C33 -133.2(16) . . . . ?
U2 O6 C32 C31 129.0(8) . . . . ?
U2 O6 C35 C34 165.5(13) . . . . ?
U2 O7 C36 C37 171.4(7) . . . . ?
U2 O7 C39 C38 161.3(8) . . . . ?
U2 O7 C40 C41 -160(2) . . . . ?
U2 O7 C43 C42 159(3) . . . . ?
U2 O8 C44 C45 156.1(5) . . . . ?
U2 O8 C47 C46 -144.2(4) . . . . ?
U2 O8 C47 C50 -138.0(11) . . . . ?
U2 O8 C48 C49 134.3(10) . . . . ?
O1 C1 C2 C3 37.5(4) . . . . ?
O2 C5 C6 C7 47.5(13) . . . . ?
O2 C8 C11 C10 2(3) . . . . ?
O2 C9 C10 C11 -38.1(19) . . . . ?
O3 C12 C13 C14 33.3(8) . . . . ?
O3 C12 C16 C17 -18(4) . . . . ?
O4 C19 C20 C21 -37.0(5) . . . . ?
O4 C19 C20 C23 3(2) . . . . ?
O5 C25 C26 C27 -5.1(4) . . . . ?
O6 C29 C30 C31 -11.0(15) . . . . ?
O6 C29 C33 C34 -32(2) . . . . ?
O7 C36 C37 C38 35.7(12) . . . . ?
O7 C40 C41 C42 -20(5) . . . . ?
O8 C44 C45 C46 -0.1(9) . . . . ?
O8 C47 C50 C49 -12.4(17) . . . . ?
O8 C48 C49 C50 33(2) . . . . ?
C1 O1 C4 C3 -9.9(4) . . . . ?
C1 C2 C3 C4 -43.2(4) . . . . ?
C2 C3 C4 O1 32.9(4) . . . . ?
C4 O1 C1 C2 -17.5(4) . . . . ?
C5 O2 C8 C7 -14.8(10) . . . . ?
C5 C6 C7 C8 -54.9(14) . . . . ?
C6 C7 C8 O2 43.1(13) . . . . ?
C8 O2 C5 C6 -20.5(11) . . . . ?
C8 O2 C9 C10 44.2(13) . . . . ?
C9 O2 C8 C11 -28.2(15) . . . . ?
C9 C10 C11 C8 23(3) . . . . ?
C12 O3 C15 C14 -16.7(10) . . . . ?
C12 O3 C18 C17 31(2) . . . . ?
C12 C13 C14 C15 -43.2(10) . . . . ?
C12 C16 C17 C18 37(4) . . . . ?
C13 C14 C15 O3 36.8(11) . . . . ?
C15 O3 C12 C13 -10.7(8) . . . . ?
C16 C17 C18 O3 -43(3) . . . . ?
C18 O3 C12 C16 -8(3) . . . . ?
C19 O4 C22 C21 -5.6(7) . . . . ?
C19 O4 C24 C23 -57(4) . . . . ?
C19 C20 C21 C22 33.8(8) . . . . ?
C19 C20 C23 C24 -33(3) . . . . ?
C20 C21 C22 O4 -18.0(9) . . . . ?
C20 C23 C24 O4 55(4) . . . . ?
C22 O4 C19 C20 27.2(5) . . . . ?
C24 O4 C19 C20 30(2) . . . . ?
C25 O5 C28 C27 -38.8(4) . . . . ?
C25 C26 C27 C28 -17.5(4) . . . . ?
C26 C27 C28 O5 34.3(4) . . . . ?
C28 O5 C25 C26 27.0(4) . . . . ?
C29 O6 C32 C31 -50.3(10) . . . . ?
C29 O6 C35 C34 16.0(19) . . . . ?
C29 C30 C31 C32 -17.8(17) . . . . ?
C29 C33 C34 C35 41(3) . . . . ?
C30 C31 C32 O6 40.8(15) . . . . ?
C32 O6 C29 C30 36.2(10) . . . . ?
C33 C34 C35 O6 -36(2) . . . . ?
C35 O6 C29 C33 10.1(18) . . . . ?
C36 O7 C39 C38 -11.5(11) . . . . ?
C36 C37 C38 C39 -42.4(15) . . . . ?
C37 C38 C39 O7 33.6(15) . . . . ?
C39 O7 C36 C37 -15.1(10) . . . . ?
C40 O7 C43 C42 -32(3) . . . . ?
C40 C41 C42 C43 -1(6) . . . . ?
C41 C42 C43 O7 20(5) . . . . ?
C43 O7 C40 C41 33(3) . . . . ?
C44 O8 C47 C46 36.5(6) . . . . ?
C44 C45 C46 C47 21.7(9) . . . . ?
C45 C46 C47 O8 -34.8(6) . . . . ?
C47 O8 C44 C45 -24.4(8) . . . . ?
C47 O8 C48 C49 -33.7(13) . . . . ?
C48 O8 C47 C50 30.8(13) . . . . ?
C48 C49 C50 C47 -12.8(18) . . . . ?
C51 C52 C53 C54 0.4(6) . . . . ?
C52 C51 C56 C55 0.2(5) . . . . ?
C52 C51 B1 C57 96.0(3) . . . . ?
C52 C51 B1 C63 -24.4(4) . . . . ?
C52 C51 B1 C69 -145.7(3) . . . . ?
C52 C53 C54 C55 0.1(6) . . . . ?
C53 C54 C55 C56 -0.4(6) . . . . ?
C54 C55 C56 C51 0.2(6) . . . . ?
C56 C51 C52 C53 -0.5(5) . . . . ?
C56 C51 B1 C57 -80.7(4) . . . . ?
C56 C51 B1 C63 159.0(3) . . . . ?
C56 C51 B1 C69 37.6(4) . . . . ?
C57 C58 C59 C60 1.4(6) . . . . ?
C58 C57 C62 C61 0.0(5) . . . . ?
C58 C57 B1 C51 29.2(4) . . . . ?
C58 C57 B1 C63 149.1(3) . . . . ?
C58 C57 B1 C69 -90.6(4) . . . . ?
C58 C59 C60 C61 -0.7(6) . . . . ?
C59 C60 C61 C62 -0.2(5) . . . . ?
C60 C61 C62 C57 0.6(5) . . . . ?
C62 C57 C58 C59 -0.9(5) . . . . ?
C62 C57 B1 C51 -155.3(3) . . . . ?
C62 C57 B1 C63 -35.4(4) . . . . ?
C62 C57 B1 C69 84.9(3) . . . . ?
C63 C64 C65 C66 -0.5(5) . . . . ?
C64 C63 C68 C67 0.3(5) . . . . ?
C64 C63 B1 C51 80.2(3) . . . . ?
C64 C63 B1 C57 -39.5(4) . . . . ?
C64 C63 B1 C69 -158.4(3) . . . . ?
C64 C65 C66 C67 0.5(5) . . . . ?
C65 C66 C67 C68 -0.1(5) . . . . ?
C66 C67 C68 C63 -0.3(5) . . . . ?
C68 C63 C64 C65 0.1(5) . . . . ?
C68 C63 B1 C51 -96.1(3) . . . . ?
C68 C63 B1 C57 144.1(3) . . . . ?
C68 C63 B1 C69 25.3(4) . . . . ?
C69 C70 C71 C72 0.1(5) . . . . ?
C70 C69 C74 C73 0.4(5) . . . . ?
C70 C69 B1 C51 37.1(4) . . . . ?
C70 C69 B1 C57 156.1(3) . . . . ?
C70 C69 B1 C63 -83.7(4) . . . . ?
C70 C71 C72 C73 0.1(5) . . . . ?
C71 C72 C73 C74 0.1(6) . . . . ?
C72 C73 C74 C69 -0.4(6) . . . . ?
C74 C69 C70 C71 -0.3(5) . . . . ?
C74 C69 B1 C51 -143.8(3) . . . . ?
C74 C69 B1 C57 -24.8(4) . . . . ?
C74 C69 B1 C63 95.4(3) . . . . ?
B1 C51 C52 C53 -177.4(3) . . . . ?
B1 C51 C56 C55 177.1(3) . . . . ?
B1 C57 C58 C59 174.8(3) . . . . ?
B1 C57 C62 C61 -175.9(3) . . . . ?
B1 C63 C64 C65 -176.6(3) . . . . ?
B1 C63 C68 C67 176.9(3) . . . . ?
B1 C69 C70 C71 178.9(3) . . . . ?
B1 C69 C74 C73 -178.7(3) . . . . ?
C75 C76 C77 C78 -0.1(6) . . . . ?
C76 C75 C80 C79 0.1(5) . . . . ?
C76 C75 B2 C81 -122.1(3) . . . . ?
C76 C75 B2 C87 -1.7(4) . . . . ?
C76 C75 B2 C93 117.2(4) . . . . ?
C76 C77 C78 C79 -0.7(6) . . . . ?
C77 C78 C79 C80 1.2(6) . . . . ?
C78 C79 C80 C75 -0.9(6) . . . . ?
C80 C75 C76 C77 0.4(5) . . . . ?
C80 C75 B2 C81 53.6(4) . . . . ?
C80 C75 B2 C87 174.0(3) . . . . ?
C80 C75 B2 C93 -67.1(4) . . . . ?
C81 C82 C83 C84 -2.2(10) . . . . ?
C82 C81 C86 C85 -0.9(7) . . . . ?
C82 C81 B2 C75 14.5(5) . . . . ?
C82 C81 B2 C87 -103.0(5) . . . . ?
C82 C81 B2 C93 137.6(4) . . . . ?
C82 C83 C84 C85 0.2(9) . . . . ?
C83 C84 C85 C86 1.2(8) . . . . ?
C84 C85 C86 C81 -0.9(8) . . . . ?
C86 C81 C82 C83 2.4(8) . . . . ?
C86 C81 B2 C75 -167.6(4) . . . . ?
C86 C81 B2 C87 74.9(5) . . . . ?
C86 C81 B2 C93 -44.5(5) . . . . ?
C87 C88 C89 C90 2.6(7) . . . . ?
C88 C87 C92 C91 0.2(6) . . . . ?
C88 C87 B2 C75 -79.8(4) . . . . ?
C88 C87 B2 C81 38.4(5) . . . . ?
C88 C87 B2 C93 158.3(3) . . . . ?
C88 C89 C90 C91 -2.2(7) . . . . ?
C89 C90 C91 C92 0.9(7) . . . . ?
C90 C91 C92 C87 0.1(6) . . . . ?
C92 C87 C88 C89 -1.5(6) . . . . ?
C92 C87 B2 C75 90.0(4) . . . . ?
C92 C87 B2 C81 -151.8(3) . . . . ?
C92 C87 B2 C93 -31.9(4) . . . . ?
C93 C94 C95 C96 -0.2(5) . . . . ?
C94 C93 C98 C97 4.8(5) . . . . ?
C94 C93 B2 C75 11.1(4) . . . . ?
C94 C93 B2 C81 -109.2(4) . . . . ?
C94 C93 B2 C87 129.2(3) . . . . ?
C94 C95 C96 C97 3.6(6) . . . . ?
C95 C96 C97 C98 -2.6(6) . . . . ?
C96 C97 C98 C93 -1.7(6) . . . . ?
C98 C93 C94 C95 -3.8(5) . . . . ?
C98 C93 B2 C75 -171.2(3) . . . . ?
C98 C93 B2 C81 68.6(4) . . . . ?
C98 C93 B2 C87 -53.0(4) . . . . ?
B2 C75 C76 C77 176.3(3) . . . . ?
B2 C75 C80 C79 -175.9(3) . . . . ?
B2 C81 C82 C83 -179.5(5) . . . . ?
B2 C81 C86 C85 -179.0(4) . . . . ?
B2 C87 C88 C89 169.0(4) . . . . ?
B2 C87 C92 C91 -170.3(4) . . . . ?
B2 C93 C94 C95 174.0(3) . . . . ?
B2 C93 C98 C97 -173.1(3) . . . . ?
C99 C100 C101 C102 0.3(5) . . . . ?
C100 C99 C104 C103 0.6(5) . . . . ?
C100 C99 B3 C105 179.5(3) . . . . ?
C100 C99 B3 C111 58.8(4) . . . . ?
C100 C99 B3 C117 -63.1(4) . . . . ?
C100 C101 C102 C103 0.4(6) . . . . ?
C101 C102 C103 C104 -0.5(6) . . . . ?
C102 C103 C104 C99 0.0(6) . . . . ?
C104 C99 C100 C101 -0.7(5) . . . . ?
C104 C99 B3 C105 3.4(4) . . . . ?
C104 C99 B3 C111 -117.3(3) . . . . ?
C104 C99 B3 C117 120.8(4) . . . . ?
C105 C106 C107 C108 -0.8(7) . . . . ?
C106 C105 C110 C109 -1.1(6) . . . . ?
C106 C105 B3 C99 71.4(4) . . . . ?
C106 C105 B3 C111 -171.4(3) . . . . ?
C106 C105 B3 C117 -50.1(4) . . . . ?
C106 C107 C108 C109 0.5(8) . . . . ?
C107 C108 C109 C110 -0.6(8) . . . . ?
C108 C109 C110 C105 0.9(8) . . . . ?
C110 C105 C106 C107 1.0(6) . . . . ?
C110 C105 B3 C99 -107.7(4) . . . . ?
C110 C105 B3 C111 9.4(5) . . . . ?
C110 C105 B3 C117 130.7(4) . . . . ?
C111 C112 C113 C114 1.6(6) . . . . ?
C112 C111 C116 C115 2.5(6) . . . . ?
C112 C111 B3 C99 57.5(4) . . . . ?
C112 C111 B3 C105 -62.3(4) . . . . ?
C112 C111 B3 C117 180.0(3) . . . . ?
C112 C113 C114 C115 1.6(7) . . . . ?
C113 C114 C115 C116 -2.7(7) . . . . ?
C114 C115 C116 C111 0.5(7) . . . . ?
C116 C111 C112 C113 -3.6(6) . . . . ?
C116 C111 B3 C99 -120.3(4) . . . . ?
C116 C111 B3 C105 119.9(4) . . . . ?
C116 C111 B3 C117 2.1(5) . . . . ?
C117 C118 C119 C120 -0.5(6) . . . . ?
C118 C117 C122 C121 1.8(6) . . . . ?
C118 C117 B3 C99 -177.0(3) . . . . ?
C118 C117 B3 C105 -56.9(4) . . . . ?
C118 C117 B3 C111 64.4(4) . . . . ?
C118 C119 C120 C121 1.4(7) . . . . ?
C119 C120 C121 C122 -0.6(7) . . . . ?
C120 C121 C122 C117 -1.0(7) . . . . ?
C122 C117 C118 C119 -1.0(6) . . . . ?
C122 C117 B3 C99 -1.0(5) . . . . ?
C122 C117 B3 C105 119.1(4) . . . . ?
C122 C117 B3 C111 -119.5(4) . . . . ?
B3 C99 C100 C101 -177.2(3) . . . . ?
B3 C99 C104 C103 176.9(3) . . . . ?
B3 C105 C106 C107 -178.2(4) . . . . ?
B3 C105 C110 C109 178.1(4) . . . . ?
B3 C111 C112 C113 178.4(4) . . . . ?
B3 C111 C116 C115 -179.6(4) . . . . ?
B3 C117 C118 C119 175.4(4) . . . . ?
B3 C117 C122 C121 -174.4(4) . . . . ?
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
1.0000 -0.0000 -0.0000 0.0541 0.0006 -0.0053
-1.0000 0.0000 0.0000 -0.0541 -0.0006 0.0053
-2.0001 -1.0000 -0.9999 -0.1374 -0.0694 -0.1000
-2.0001 -1.0000 1.0000 -0.0884 -0.1328 0.0045
-1.0002 -2.0000 -0.9999 -0.0879 -0.1688 -0.1638
1.0000 -0.0000 -2.0000 0.0052 0.0640 -0.1099
0.9999 -1.0000 -2.0000 0.0005 -0.0360 -0.1683
-1.0001 -2.0000 1.0001 -0.0389 -0.2322 -0.0592
-0.9998 2.0000 1.9999 0.0041 0.1359 0.2267
1.0001 2.0000 -1.0001 0.0389 0.2322 0.0592
-1.0001 -2.0000 2.0000 -0.0144 -0.2639 -0.0069
0.9998 -2.0000 -1.9999 -0.0041 -0.1359 -0.2267
1.9999 -1.0000 -1.0000 0.0791 -0.0671 -0.1214
18.0003 3.0000 -3.0002 0.9148 0.4056 -0.0775
