#------------------------------------------------------------------------------
#$Date: 2023-01-06 11:35:32 +0200 (Fri, 06 Jan 2023) $
#$Revision: 280168 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/77/1567756.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_1567756
loop_
_publ_author_name
'Cooney, Shannon E.'
'Fertig, Alex A.'
'Buisch, Madeleine R.'
'Brennessel, William W.'
'Matson, Ellen M.'
_publ_section_title
;
 Coordination-induced bond weakening of water at the surface of an
 oxygen-deficient polyoxovanadate cluster.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              12726
_journal_page_last               12737
_journal_paper_doi               10.1039/d2sc04843d
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety
'C53.046 H80.523 N0.523 O18.477 V6, 3.477(C4 H8 O)'
_chemical_formula_sum            'C66.95 H108.34 N0.52 O21.95 V6'
_chemical_formula_weight         1577.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-06-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-24 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4807(2)
_cell_length_b                   27.8595(5)
_cell_length_c                   18.7836(2)
_cell_measurement_reflns_used    17304
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      78.7590
_cell_measurement_theta_min      3.4540
_cell_volume                     7577.77(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  27.00   0.50    3.37    --  -47.29  23.00  77.00   94
  2  ω   -122.00 -35.00   0.50    3.37    --  -47.29 -23.00 -87.00  174
  3  ω    -80.00 -19.00   0.50   13.49    --  -91.75 101.00-123.00  122
  4  ω    -98.00 -21.00   0.50   13.49    --  -91.75 141.00 -58.00  154
  5  ω    101.00 178.00   0.50   13.49    --  113.25  23.00  77.00  154
  6  ω     43.00 123.00   0.50   13.49    --  113.25-141.00-115.00  160
  7  ω   -119.00 -73.00   0.50    3.37    --  -47.29-125.00-120.00   92
  8  ω    -16.00  28.00   0.50    3.37    --  -47.29  19.00-150.00   88
  9  ω    -27.00  30.00   0.50    3.37    --   47.29 -19.00-180.00  114
 10  ω    101.00 178.00   0.50   13.49    --  113.25  45.00  30.00  154
 11  ω     42.00 111.00   0.50   13.49    --  113.25-125.00 -30.00  138
 12  ω     42.00 106.00   0.50   13.49    --  113.25 -94.00  60.00  128
 13  ω     42.00 111.00   0.50   13.49    --  113.25-125.00 150.00  138
 14  ω     42.00  79.00   0.50   13.49    --  113.25 -61.00-180.00   74
 15  ω     32.00  95.00   0.50    3.37    --   47.29  57.00 120.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0052944000
_diffrn_orient_matrix_UB_12      -0.0525993000
_diffrn_orient_matrix_UB_13      -0.0250601000
_diffrn_orient_matrix_UB_21      0.1061115000
_diffrn_orient_matrix_UB_22      -0.0034426000
_diffrn_orient_matrix_UB_23      0.0024668000
_diffrn_orient_matrix_UB_31      -0.0048748000
_diffrn_orient_matrix_UB_32      -0.0167682000
_diffrn_orient_matrix_UB_33      0.0780533000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48002
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.488
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             3309
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8377
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1040P)²+5.1446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5983
_reflns_number_total             8377
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc04843d2.cif
_cod_data_source_block           matsec01
_cod_depositor_comments          'Adding full bibliography for 1567756.cif.'
_cod_original_cell_volume        7577.78(19)
_cod_database_code               1567756
_shelx_shelxl_version_number     2019/2
_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   0.461
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{N1, O1}
3. Restrained distances
 C24-C25 \\sim C24-C26 \\sim C24-C27
 with sigma of 0.01
 C25-C26 \\sim C26-C27 \\sim C27-C25
 with sigma of 0.02
 C28-C29 \\sim C28-C30 \\sim C28-C31 \\sim C28'-C29' \\sim C28'-C30' \\sim
C28'-C31'
 with sigma of 0.01
 C29-C30 \\sim C30-C31 \\sim C31-C29 \\sim C29'-C30' \\sim C30'-C31' \\sim
C31'-C29'
 with sigma of 0.02
 C32-C33 \\sim C32-C34 \\sim C32-C35
 with sigma of 0.01
 C33-C34 \\sim C34-C35 \\sim C35-C33
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(N1) = Uanis(O1)
5. Rigid body (RIGU) restrains
 C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28', C29', C30', C31'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O15, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16, C40, C41, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O15', C36', C37', C38', C39'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17', C44', C45', C46', C47'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O15, C36, C37, C38, C39} sigma for 1-2: 0.02, 1-3: 0.04
{O16, C43, C42, C41, C40} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O16, C40, C41, C42, C43}
{O15, C39, C38, C37, C36} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15, C36, C37, C38, C39}
{O15', C39', C38', C37', C36'} sigma for 1-2: 0.02, 1-3: 0.04
{O15, C36, C37, C38, C39} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15', C36', C37', C38', C39'}
{O15, C36, C37, C38, C39} sigma for 1-2: 0.02, 1-3: 0.04
{O17, C47, C46, C45, C44} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17, C44, C45, C46, C47}
{O17', C47', C46', C45', C44'} sigma for 1-2: 0.02, 1-3: 0.04
{O15, C36, C37, C38, C39} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17', C44', C45', C46', C47'}
7. Others
 Sof(C28')=Sof(C29')=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30')=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=Sof(C31')=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(O15')=Sof(C36')=Sof(H36C)=Sof(H36D)=Sof(C37')=Sof(H37C)=Sof(H37D)=
 Sof(C38')=Sof(H38C)=Sof(H38D)=Sof(C39')=Sof(H39C)=Sof(H39D)=1-FVAR(2)
 Sof(O15)=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(2)
 Sof(O1)=Sof(H1A)=Sof(H1B)=Sof(O16)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 0.5*(1-FVAR(4))
 Sof(N1)=Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=0.5*FVAR(4)
 Sof(O17')=Sof(C44')=Sof(H44C)=Sof(H44D)=Sof(C45')=Sof(H45C)=Sof(H45D)=
 Sof(C46')=Sof(H46C)=Sof(H46D)=Sof(C47')=Sof(H47C)=Sof(H47D)=0.5*(1-FVAR(5))
 Sof(O17)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=0.5*FVAR(5)
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C24(0.5)
 C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
8.a Riding coordinates:
 C2(H2A,H2B,H2C), O1(H1A,H1B)
8.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C22(H22A,
 H22B), C23(H23A,H23B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C36'(H36C,H36D), C37'(H37C,H37D), C38'(H38C,H38D), C39'(H39C,
 H39D), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C44'(H44C,H44D), C45'(H45C,H45D), C46'(H46C,H46D), C47'(H47C,H47D)
8.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C)
8.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C16(H16), C20(H20)
8.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C29'(H29D,H29E,H29F), C30'(H30D,H30E,H30F), C31'(H31D,H31E,H31F),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_olex2_submission_original_sample_id matsec01
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.785
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, 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_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
V1 V 0.54110(6) 0.40703(3) 0.250000 0.0513(2) Uani 1 2 d S T P . .
V2 V 0.39533(7) 0.32228(4) 0.250000 0.0765(3) Uani 1 2 d S T P . .
V3 V 0.39609(5) 0.40675(2) 0.37674(3) 0.0657(2) Uani 1 1 d . . . . .
V4 V 0.39724(5) 0.48353(3) 0.250000 0.0546(2) Uani 1 2 d S T P . .
V5 V 0.23594(7) 0.40697(4) 0.250000 0.0818(3) Uani 1 2 d S T P . .
O2 O 0.3993(3) 0.26460(15) 0.250000 0.0997(15) Uani 1 2 d S T P A .
O3 O 0.3982(2) 0.40745(10) 0.46132(15) 0.0836(8) Uani 1 1 d . . . . .
O4 O 0.3996(3) 0.55719(14) 0.250000 0.0653(9) Uani 1 2 d S T P A .
H4 H 0.415(4) 0.570(2) 0.291(3) 0.112(18) Uiso 1 1 d . . . . .
O5 O 0.1241(3) 0.4078(2) 0.250000 0.1125(18) Uani 1 2 d S T P A .
O6 O 0.5331(3) 0.33740(11) 0.250000 0.0619(8) Uani 1 2 d S T P A .
O7 O 0.53419(16) 0.40723(8) 0.35372(11) 0.0555(5) Uani 1 1 d . . . . .
O8 O 0.5363(2) 0.47703(10) 0.250000 0.0474(6) Uani 1 2 d S T P A .
O9 O 0.39635(19) 0.33659(10) 0.35473(15) 0.0777(7) Uani 1 1 d . . . . .
O10 O 0.39734(15) 0.47751(9) 0.35417(11) 0.0588(5) Uani 1 1 d . . . . .
O11 O 0.2603(3) 0.33655(16) 0.250000 0.0939(13) Uani 1 2 d S T P A .
O12 O 0.2612(2) 0.40710(11) 0.35525(16) 0.0838(8) Uani 1 1 d . . . . .
O13 O 0.2626(2) 0.47755(14) 0.250000 0.0721(9) Uani 1 2 d S T P A .
O14 O 0.3990(2) 0.40780(12) 0.250000 0.0591(8) Uani 1 2 d S T P A .
N1 N 0.6876(3) 0.40660(12) 0.250000 0.0580(8) Uani 0.523(11) 2 d S TU P A 1
C1 C 0.7674(8) 0.4071(4) 0.250000 0.067(3) Uani 0.523(11) 2 d S TU P A 1
C2 C 0.8650(11) 0.4097(7) 0.250000 0.115(6) Uani 0.523(11) 2 d S TU P A 1
H2A H 0.888015 0.397278 0.205730 0.173 Uiso 0.261(5) 1 d R U P A -1
H2B H 0.884705 0.442308 0.255660 0.173 Uiso 0.261(5) 1 d R U P A -1
H2C H 0.888505 0.390668 0.288610 0.173 Uiso 0.261(5) 1 d R U P A -1
O1 O 0.6876(3) 0.40660(12) 0.250000 0.0580(8) Uani 0.477(11) 2 d S TU P A 2
H1A H 0.710975 0.404058 0.299000 0.087 Uiso 0.239(5) 1 d R U P A -2
H1B H 0.711225 0.437038 0.229260 0.087 Uiso 0.239(5) 1 d R U P A -2
O16 O 0.8557(9) 0.4110(5) 0.1970(8) 0.092(4) Uani 0.239(5) 1 d D U P A -2
C40 C 0.8987(17) 0.3697(6) 0.2262(9) 0.101(7) Uani 0.239(5) 1 d D . P A -2
H40A H 0.954260 0.361031 0.198382 0.121 Uiso 0.239(5) 1 calc R U P A -2
H40B H 0.855565 0.342152 0.226094 0.121 Uiso 0.239(5) 1 calc R U P A -2
C41 C 0.9235(16) 0.3827(6) 0.2982(10) 0.097(5) Uani 0.239(5) 1 d D . P A -2
H41A H 0.985739 0.370357 0.310318 0.116 Uiso 0.239(5) 1 calc R U P A -2
H41B H 0.878369 0.369553 0.332684 0.116 Uiso 0.239(5) 1 calc R U P A -2
C42 C 0.9222(17) 0.4381(6) 0.2989(10) 0.098(6) Uani 0.239(5) 1 d D . P A -2
H42A H 0.873954 0.450324 0.331493 0.118 Uiso 0.239(5) 1 calc R U P A -2
H42B H 0.982841 0.451113 0.313793 0.118 Uiso 0.239(5) 1 calc R U P A -2
C43 C 0.9018(19) 0.4510(6) 0.2254(10) 0.107(7) Uani 0.239(5) 1 d D . P A -2
H43A H 0.862011 0.479901 0.223505 0.129 Uiso 0.239(5) 1 calc R U P A -2
H43B H 0.959403 0.457561 0.198746 0.129 Uiso 0.239(5) 1 calc R U P A -2
C3 C 0.3446(4) 0.30582(16) 0.4014(3) 0.0937(14) Uani 1 1 d . . . . .
H3A H 0.350015 0.272510 0.385159 0.141 Uiso 1 1 calc R U . . .
H3B H 0.368914 0.308538 0.449898 0.141 Uiso 1 1 calc R U . . .
H3C H 0.279473 0.315434 0.400910 0.141 Uiso 1 1 calc R U . . .
C4 C 0.3561(3) 0.51001(15) 0.4027(2) 0.0781(11) Uani 1 1 d . . . . .
H4A H 0.366069 0.498683 0.451449 0.117 Uiso 1 1 calc R U . . .
H4B H 0.383994 0.541818 0.396907 0.117 Uiso 1 1 calc R U . . .
H4C H 0.289651 0.512008 0.393161 0.117 Uiso 1 1 calc R U . . .
C5 C 0.1897(5) 0.3025(3) 0.250000 0.122(3) Uani 1 2 d S T P . .
H5A H 0.163835 0.299781 0.298045 0.183 Uiso 0.5 1 calc R U P A -1
H5B H 0.214462 0.271376 0.235112 0.183 Uiso 0.5 1 calc R U P A -1
H5C H 0.141104 0.312535 0.216843 0.183 Uiso 0.5 1 calc R U P A -1
C6 C 0.1928(4) 0.4114(2) 0.4050(3) 0.128(2) Uani 1 1 d . . . . .
H6A H 0.218942 0.406828 0.452637 0.192 Uiso 1 1 calc R U . . .
H6B H 0.145386 0.386954 0.396296 0.192 Uiso 1 1 calc R U . . .
H6C H 0.165026 0.443365 0.401702 0.192 Uiso 1 1 calc R U . . .
C7 C 0.1952(4) 0.5130(3) 0.250000 0.102(2) Uani 1 2 d S T P . .
H7A H 0.171529 0.517339 0.201535 0.154 Uiso 0.5 1 calc R U P A -1
H7B H 0.221874 0.543223 0.266946 0.154 Uiso 0.5 1 calc R U P A -1
H7C H 0.144460 0.503423 0.281518 0.154 Uiso 0.5 1 calc R U P A -1
C8 C 0.6126(4) 0.30980(17) 0.250000 0.0667(13) Uani 1 2 d S T P . .
C9 C 0.6535(3) 0.29845(13) 0.3146(2) 0.0725(10) Uani 1 1 d . . . . .
C10 C 0.7356(3) 0.27160(14) 0.3128(2) 0.0842(12) Uani 1 1 d . . . . .
H10 H 0.762993 0.262116 0.356562 0.101 Uiso 1 1 calc R U . . .
C11 C 0.7778(5) 0.2585(2) 0.250000 0.0840(17) Uani 1 2 d S T P . .
C12 C 0.6155(2) 0.40727(12) 0.39210(17) 0.0577(8) Uani 1 1 d . . . . .
C13 C 0.6579(2) 0.45091(12) 0.40799(15) 0.0560(7) Uani 1 1 d . . . . .
C14 C 0.7429(3) 0.44947(14) 0.44351(17) 0.0645(9) Uani 1 1 d . . . . .
H14 H 0.772823 0.478860 0.454669 0.077 Uiso 1 1 calc R U . . .
C15 C 0.7848(3) 0.40679(15) 0.4630(2) 0.0737(10) Uani 1 1 d . . . . .
C16 C 0.7403(3) 0.36447(15) 0.44496(19) 0.0771(11) Uani 1 1 d . . . . .
H16 H 0.768151 0.334859 0.457895 0.093 Uiso 1 1 calc R U . . .
C17 C 0.6570(3) 0.36350(13) 0.40898(17) 0.0643(9) Uani 1 1 d . . . . .
C18 C 0.6148(3) 0.50484(16) 0.250000 0.0492(9) Uani 1 2 d S T P . .
C19 C 0.6544(2) 0.51731(11) 0.31479(15) 0.0520(7) Uani 1 1 d . . . . .
C20 C 0.7322(3) 0.54679(13) 0.31338(18) 0.0641(9) Uani 1 1 d . . . . .
H20 H 0.759238 0.556417 0.357197 0.077 Uiso 1 1 calc R U . . .
C21 C 0.7716(4) 0.5626(2) 0.250000 0.0689(13) Uani 1 2 d S T P D .
C22 C 0.6140(3) 0.31547(14) 0.3850(2) 0.0751(11) Uani 1 1 d . . . . .
H22A H 0.625569 0.290812 0.421881 0.090 Uiso 1 1 calc R U . . .
H22B H 0.546366 0.319427 0.380226 0.090 Uiso 1 1 calc R U . . .
C23 C 0.6164(2) 0.49844(12) 0.38532(16) 0.0551(7) Uani 1 1 d . . . . .
H23A H 0.628401 0.522542 0.422940 0.066 Uiso 1 1 calc R U . . .
H23B H 0.548683 0.494662 0.381025 0.066 Uiso 1 1 calc R U . . .
C24 C 0.8674(6) 0.2280(3) 0.2531(11) 0.128(3) Uani 0.5 1 d D . P B -1
C25 C 0.8371(8) 0.1763(3) 0.2364(14) 0.151(7) Uani 0.5 1 d D . P B -1
H25A H 0.783892 0.167834 0.266105 0.227 Uiso 0.5 1 calc R U P B -1
H25B H 0.888200 0.154231 0.246472 0.227 Uiso 0.5 1 calc R U P B -1
H25C H 0.820011 0.173874 0.186085 0.227 Uiso 0.5 1 calc R U P B -1
C26 C 0.9157(18) 0.2291(8) 0.3260(11) 0.163(7) Uani 0.5 1 d D U P B -1
H26A H 0.935022 0.262039 0.336785 0.244 Uiso 0.5 1 calc R U P B -1
H26B H 0.872820 0.217922 0.362817 0.244 Uiso 0.5 1 calc R U P B -1
H26C H 0.969969 0.208138 0.324882 0.244 Uiso 0.5 1 calc R U P B -1
C27 C 0.9346(17) 0.2453(8) 0.1951(10) 0.151(7) Uani 0.5 1 d D U P B -1
H27A H 0.904395 0.243491 0.148495 0.227 Uiso 0.5 1 calc R U P B -1
H27B H 0.989720 0.224850 0.195052 0.227 Uiso 0.5 1 calc R U P B -1
H27C H 0.952659 0.278568 0.204777 0.227 Uiso 0.5 1 calc R U P B -1
C28 C 0.8734(7) 0.4050(3) 0.5040(4) 0.098(3) Uani 0.635(10) 1 d D U P C 1
C29 C 0.8534(6) 0.3840(4) 0.5769(5) 0.126(4) Uani 0.635(10) 1 d D . P C 1
H29A H 0.910772 0.382489 0.604563 0.189 Uiso 0.635(10) 1 calc R U P C 1
H29B H 0.828151 0.351537 0.571483 0.189 Uiso 0.635(10) 1 calc R U P C 1
H29C H 0.808556 0.404248 0.601790 0.189 Uiso 0.635(10) 1 calc R U P C 1
C30 C 0.9431(7) 0.3736(4) 0.4649(7) 0.134(4) Uani 0.635(10) 1 d D U P C 1
H30A H 0.917203 0.341440 0.458219 0.200 Uiso 0.635(10) 1 calc R U P C 1
H30B H 0.999971 0.371422 0.493001 0.200 Uiso 0.635(10) 1 calc R U P C 1
H30C H 0.956938 0.387832 0.418397 0.200 Uiso 0.635(10) 1 calc R U P C 1
C31 C 0.9158(7) 0.4544(3) 0.5147(7) 0.125(4) Uani 0.635(10) 1 d D . P C 1
H31A H 0.930591 0.468512 0.468279 0.188 Uiso 0.635(10) 1 calc R U P C 1
H31B H 0.972343 0.451478 0.543008 0.188 Uiso 0.635(10) 1 calc R U P C 1
H31C H 0.871725 0.475133 0.539713 0.188 Uiso 0.635(10) 1 calc R U P C 1
C28' C 0.8831(12) 0.4079(5) 0.5025(7) 0.107(5) Uani 0.365(10) 1 d D U P C 2
C29' C 0.9507(12) 0.4390(7) 0.4610(10) 0.144(7) Uani 0.365(10) 1 d D . P C 2
H29D H 0.954986 0.427302 0.411945 0.215 Uiso 0.365(10) 1 calc R U P C 2
H29E H 1.011726 0.437361 0.483518 0.215 Uiso 0.365(10) 1 calc R U P C 2
H29F H 0.929014 0.472296 0.460979 0.215 Uiso 0.365(10) 1 calc R U P C 2
C30' C 0.8686(11) 0.4300(7) 0.5755(7) 0.125(7) Uani 0.365(10) 1 d D . P C 2
H30D H 0.854144 0.464162 0.570284 0.187 Uiso 0.365(10) 1 calc R U P C 2
H30E H 0.925022 0.426338 0.603837 0.187 Uiso 0.365(10) 1 calc R U P C 2
H30F H 0.817347 0.413723 0.599566 0.187 Uiso 0.365(10) 1 calc R U P C 2
C31' C 0.9234(14) 0.3578(5) 0.5115(11) 0.138(7) Uani 0.365(10) 1 d D U P C 2
H31D H 0.878133 0.337121 0.535130 0.207 Uiso 0.365(10) 1 calc R U P C 2
H31E H 0.979578 0.359632 0.540409 0.207 Uiso 0.365(10) 1 calc R U P C 2
H31F H 0.938423 0.344531 0.464577 0.207 Uiso 0.365(10) 1 calc R U P C 2
C32 C 0.8528(5) 0.5979(3) 0.250000 0.098(2) Uani 1 2 d DS T P . .
C33 C 0.9329(7) 0.5758(5) 0.2912(7) 0.155(5) Uani 0.5 1 d D . P D -1
H33A H 0.910792 0.564379 0.337534 0.232 Uiso 0.5 1 calc R U P D -1
H33B H 0.981067 0.600056 0.298502 0.232 Uiso 0.5 1 calc R U P D -1
H33C H 0.958423 0.548807 0.264206 0.232 Uiso 0.5 1 calc R U P D -1
C34 C 0.8218(9) 0.6448(4) 0.2848(6) 0.156(5) Uani 0.5 1 d D . P D -1
H34A H 0.870964 0.668828 0.280322 0.234 Uiso 0.5 1 calc R U P D -1
H34B H 0.808733 0.639168 0.335294 0.234 Uiso 0.5 1 calc R U P D -1
H34C H 0.765924 0.656547 0.261097 0.234 Uiso 0.5 1 calc R U P D -1
C35 C 0.8854(7) 0.6098(4) 0.1742(5) 0.114(4) Uani 0.5 1 d D . P D -1
H35A H 0.901865 0.580029 0.149426 0.171 Uiso 0.5 1 calc R U P D -1
H35B H 0.939558 0.630839 0.176543 0.171 Uiso 0.5 1 calc R U P D -1
H35C H 0.835685 0.626028 0.148340 0.171 Uiso 0.5 1 calc R U P D -1
O15 O 0.4635(7) 0.6173(4) 0.3488(6) 0.119(3) Uani 0.601(8) 1 d D U P E 1
C36 C 0.4171(8) 0.6434(5) 0.4025(6) 0.141(4) Uani 0.601(8) 1 d D U P E 1
H36A H 0.398152 0.621624 0.441592 0.169 Uiso 0.601(8) 1 calc R U P E 1
H36B H 0.361238 0.658933 0.382844 0.169 Uiso 0.601(8) 1 calc R U P E 1
C37 C 0.4805(9) 0.6789(4) 0.4286(6) 0.129(3) Uani 0.601(8) 1 d D U P E 1
H37A H 0.493250 0.673502 0.479730 0.154 Uiso 0.601(8) 1 calc R U P E 1
H37B H 0.453718 0.711411 0.422968 0.154 Uiso 0.601(8) 1 calc R U P E 1
C38 C 0.5689(9) 0.6749(4) 0.3860(8) 0.137(4) Uani 0.601(8) 1 d D U P E 1
H38A H 0.580101 0.704413 0.358004 0.165 Uiso 0.601(8) 1 calc R U P E 1
H38B H 0.622463 0.669194 0.417694 0.165 Uiso 0.601(8) 1 calc R U P E 1
C39 C 0.5538(8) 0.6348(5) 0.3404(8) 0.170(5) Uani 0.601(8) 1 d D U P E 1
H39A H 0.563596 0.644587 0.290285 0.204 Uiso 0.601(8) 1 calc R U P E 1
H39B H 0.598696 0.609146 0.351830 0.204 Uiso 0.601(8) 1 calc R U P E 1
O15' O 0.4238(11) 0.6212(5) 0.3492(10) 0.117(4) Uani 0.399(8) 1 d D U P E 2
C36' C 0.4077(12) 0.6702(5) 0.3406(12) 0.143(7) Uani 0.399(8) 1 d D . P E 2
H36C H 0.345551 0.678717 0.358561 0.172 Uiso 0.399(8) 1 calc R U P E 2
H36D H 0.411348 0.679074 0.289656 0.172 Uiso 0.399(8) 1 calc R U P E 2
C37' C 0.4773(13) 0.6951(5) 0.3804(12) 0.136(5) Uani 0.399(8) 1 d D U P E 2
H37C H 0.453025 0.706049 0.426930 0.163 Uiso 0.399(8) 1 calc R U P E 2
H37D H 0.500723 0.723230 0.353689 0.163 Uiso 0.399(8) 1 calc R U P E 2
C38' C 0.5546(12) 0.6568(6) 0.3905(17) 0.153(5) Uani 0.399(8) 1 d D U P E 2
H38C H 0.595463 0.654538 0.348405 0.184 Uiso 0.399(8) 1 calc R U P E 2
H38D H 0.592012 0.662856 0.433660 0.184 Uiso 0.399(8) 1 calc R U P E 2
C39' C 0.4970(13) 0.6150(5) 0.3981(10) 0.129(5) Uani 0.399(8) 1 d D U P E 2
H39C H 0.532342 0.585473 0.386978 0.155 Uiso 0.399(8) 1 calc R U P E 2
H39D H 0.473012 0.612513 0.447304 0.155 Uiso 0.399(8) 1 calc R U P E 2
O17 O 0.164(2) 0.2903(11) 0.5261(18) 0.203(10) Uani 0.283(12) 1 d D U P F -1
C44 C 0.114(3) 0.2630(16) 0.5752(16) 0.207(11) Uani 0.283(12) 1 d D U P F -1
H44A H 0.082096 0.284321 0.609570 0.248 Uiso 0.283(12) 1 calc R U P F -1
H44B H 0.155650 0.241411 0.601934 0.248 Uiso 0.283(12) 1 calc R U P F -1
C45 C 0.047(3) 0.2355(19) 0.535(2) 0.274(12) Uani 0.283(12) 1 d D U P F -1
H45A H -0.014082 0.251019 0.535263 0.329 Uiso 0.283(12) 1 calc R U P F -1
H45B H 0.041622 0.202388 0.553948 0.329 Uiso 0.283(12) 1 calc R U P F -1
C46 C 0.092(4) 0.2360(17) 0.460(2) 0.245(18) Uani 0.283(12) 1 d D . P F -1
H46A H 0.145619 0.214261 0.456033 0.294 Uiso 0.283(12) 1 calc R U P F -1
H46B H 0.046471 0.228253 0.421732 0.294 Uiso 0.283(12) 1 calc R U P F -1
C47 C 0.118(2) 0.2862(15) 0.4592(18) 0.206(12) Uani 0.283(12) 1 d D . P F -1
H47A H 0.160129 0.293604 0.419119 0.247 Uiso 0.283(12) 1 calc R U P F -1
H47B H 0.063460 0.307474 0.456778 0.247 Uiso 0.283(12) 1 calc R U P F -1
O17' O 0.206(2) 0.2598(17) 0.492(3) 0.24(2) Uani 0.217(12) 1 d D . P F -2
C44' C 0.141(4) 0.265(3) 0.548(4) 0.206(10) Uani 0.217(12) 1 d D U P F -2
H44C H 0.122977 0.299263 0.552468 0.247 Uiso 0.217(12) 1 calc R U P F -2
H44D H 0.168185 0.254248 0.593263 0.247 Uiso 0.217(12) 1 calc R U P F -2
C45' C 0.063(3) 0.236(3) 0.528(3) 0.273(13) Uani 0.217(12) 1 d D U P F -2
H45C H 0.017382 0.254501 0.500266 0.328 Uiso 0.217(12) 1 calc R U P F -2
H45D H 0.032392 0.222457 0.570957 0.328 Uiso 0.217(12) 1 calc R U P F -2
C46' C 0.109(4) 0.1961(18) 0.483(3) 0.27(2) Uani 0.217(12) 1 d D . P F -2
H46C H 0.138688 0.171276 0.512804 0.324 Uiso 0.217(12) 1 calc R U P F -2
H46D H 0.064314 0.180628 0.450141 0.324 Uiso 0.217(12) 1 calc R U P F -2
C47' C 0.176(4) 0.2239(19) 0.444(2) 0.199(16) Uani 0.217(12) 1 d D . P F -2
H47C H 0.228946 0.203513 0.429734 0.239 Uiso 0.217(12) 1 calc R U P F -2
H47D H 0.148336 0.238410 0.401452 0.239 Uiso 0.217(12) 1 calc R U P F -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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'
V V 0.0687 2.1097 '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
O6 V1 O7 89.99(7) . . ?
O6 V1 O7 89.99(7) . 6_556 ?
O6 V1 O8 174.52(15) . . ?
O6 V1 O14 87.18(14) . . ?
O6 V1 N1 93.09(14) . . ?
O6 V1 O1 93.09(14) . . ?
O7 V1 O7 174.11(15) . 6_556 ?
O7 V1 O8 89.73(7) 6_556 . ?
O7 V1 O8 89.73(7) . . ?
O7 V1 O14 87.06(7) . . ?
O7 V1 O14 87.06(7) 6_556 . ?
O7 V1 N1 92.94(7) . . ?
O7 V1 N1 92.94(7) 6_556 . ?
O7 V1 O1 92.94(7) 6_556 . ?
O7 V1 O1 92.94(7) . . ?
O8 V1 O14 87.34(13) . . ?
O8 V1 N1 92.39(13) . . ?
O8 V1 O1 92.39(13) . . ?
O14 V1 N1 179.73(13) . . ?
O14 V1 O1 179.73(13) . . ?
O2 V2 O6 99.9(2) . . ?
O2 V2 O9 101.44(8) . . ?
O2 V2 O9 101.44(8) . 6_556 ?
O2 V2 O11 103.5(2) . . ?
O2 V2 O14 176.7(2) . . ?
O6 V2 O14 76.80(12) . . ?
O9 V2 O6 87.23(8) 6_556 . ?
O9 V2 O6 87.23(8) . . ?
O9 V2 O9 157.07(16) 6_556 . ?
O9 V2 O14 78.53(8) 6_556 . ?
O9 V2 O14 78.54(8) . . ?
O11 V2 O6 156.59(17) . . ?
O11 V2 O9 88.15(9) . 6_556 ?
O11 V2 O9 88.15(9) . . ?
O11 V2 O14 79.79(15) . . ?
O3 V3 O7 101.11(13) . . ?
O3 V3 O9 102.64(13) . . ?
O3 V3 O10 101.43(12) . . ?
O3 V3 O12 102.75(14) . . ?
O3 V3 O14 177.48(14) . . ?
O7 V3 O14 76.79(10) . . ?
O9 V3 O7 87.76(10) . . ?
O9 V3 O10 155.92(11) . . ?
O9 V3 O14 78.76(11) . . ?
O10 V3 O7 86.59(9) . . ?
O10 V3 O14 77.15(10) . . ?
O12 V3 O7 156.12(11) . . ?
O12 V3 O9 87.98(12) . . ?
O12 V3 O10 87.79(11) . . ?
O12 V3 O14 79.34(12) . . ?
O4 V4 O14 178.37(15) . . ?
O8 V4 O4 94.20(14) . . ?
O8 V4 O14 84.17(12) . . ?
O10 V4 O4 94.91(7) 6_556 . ?
O10 V4 O4 94.90(7) . . ?
O10 V4 O8 89.52(7) 6_556 . ?
O10 V4 O8 89.52(7) . . ?
O10 V4 O10 170.19(15) . 6_556 ?
O10 V4 O14 85.09(7) 6_556 . ?
O10 V4 O14 85.09(7) . . ?
O13 V4 O4 95.83(16) . . ?
O13 V4 O8 169.97(15) . . ?
O13 V4 O10 89.62(7) . 6_556 ?
O13 V4 O10 89.62(7) . . ?
O13 V4 O14 85.80(15) . . ?
O5 V5 O11 101.0(2) . . ?
O5 V5 O12 100.47(9) . 6_556 ?
O5 V5 O12 100.47(9) . . ?
O5 V5 O13 100.3(2) . . ?
O5 V5 O14 178.7(2) . . ?
O11 V5 O12 88.26(9) . . ?
O11 V5 O12 88.25(9) . 6_556 ?
O11 V5 O13 158.69(18) . . ?
O11 V5 O14 80.36(15) . . ?
O12 V5 O12 159.06(17) 6_556 . ?
O12 V5 O14 79.53(8) 6_556 . ?
O12 V5 O14 79.53(8) . . ?
O13 V5 O12 87.90(9) . 6_556 ?
O13 V5 O12 87.89(9) . . ?
O13 V5 O14 78.33(13) . . ?
V4 O4 H4 114(4) . . ?
V4 O4 H4 114(4) . 6_556 ?
H4 O4 H4 123(7) . 6_556 ?
V1 O6 V2 105.34(17) . . ?
C8 O6 V1 120.3(3) . . ?
C8 O6 V2 134.3(3) . . ?
V1 O7 V3 105.14(11) . . ?
C12 O7 V1 118.5(2) . . ?
C12 O7 V3 136.32(19) . . ?
V1 O8 V4 97.21(12) . . ?
C18 O8 V1 122.2(3) . . ?
C18 O8 V4 140.6(3) . . ?
V3 O9 V2 113.40(13) . . ?
C3 O9 V2 118.4(3) . . ?
C3 O9 V3 117.2(3) . . ?
V4 O10 V3 107.04(11) . . ?
C4 O10 V3 119.1(2) . . ?
C4 O10 V4 125.9(2) . . ?
V5 O11 V2 111.69(19) . . ?
C5 O11 V2 125.7(5) . . ?
C5 O11 V5 122.6(5) . . ?
V3 O12 V5 112.14(13) . . ?
C6 O12 V3 124.9(4) . . ?
C6 O12 V5 122.7(4) . . ?
V4 O13 V5 106.00(18) . . ?
C7 O13 V4 129.8(4) . . ?
C7 O13 V5 124.2(4) . . ?
V1 O14 V2 90.68(13) . . ?
V1 O14 V3 91.01(8) . 6_556 ?
V1 O14 V3 91.00(8) . . ?
V1 O14 V4 91.29(12) . . ?
V1 O14 V5 178.84(17) . . ?
V3 O14 V2 89.27(8) . . ?
V3 O14 V2 89.28(8) 6_556 . ?
V3 O14 V3 177.54(16) . 6_556 ?
V4 O14 V2 178.03(17) . . ?
V4 O14 V3 90.69(8) . . ?
V4 O14 V3 90.69(8) . 6_556 ?
V4 O14 V5 89.88(13) . . ?
V5 O14 V2 88.16(11) . . ?
V5 O14 V3 88.98(8) . . ?
V5 O14 V3 88.98(8) . 6_556 ?
C1 N1 V1 178.9(6) . . ?
N1 C1 C2 177.9(13) . . ?
C43 O16 C40 106.7(15) . . ?
O16 C40 H40A 110.6 . . ?
O16 C40 H40B 110.6 . . ?
O16 C40 C41 105.6(14) . . ?
H40A C40 H40B 108.7 . . ?
C41 C40 H40A 110.6 . . ?
C41 C40 H40B 110.6 . . ?
C40 C41 H41A 110.8 . . ?
C40 C41 H41B 110.8 . . ?
C40 C41 C42 104.7(12) . . ?
H41A C41 H41B 108.9 . . ?
C42 C41 H41A 110.8 . . ?
C42 C41 H41B 110.8 . . ?
C41 C42 H42A 111.0 . . ?
C41 C42 H42B 111.0 . . ?
H42A C42 H42B 109.0 . . ?
C43 C42 C41 104.0(12) . . ?
C43 C42 H42A 111.0 . . ?
C43 C42 H42B 111.0 . . ?
O16 C43 C42 105.1(14) . . ?
O16 C43 H43A 110.7 . . ?
O16 C43 H43B 110.7 . . ?
C42 C43 H43A 110.7 . . ?
C42 C43 H43B 110.7 . . ?
H43A C43 H43B 108.8 . . ?
O9 C3 H3A 109.5 . . ?
O9 C3 H3B 109.5 . . ?
O9 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O10 C4 H4A 109.5 . . ?
O10 C4 H4B 109.5 . . ?
O10 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O11 C5 H5A 109.5 . . ?
O11 C5 H5B 109.5 . . ?
O11 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O12 C6 H6A 109.5 . . ?
O12 C6 H6B 109.5 . . ?
O12 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O13 C7 H7A 109.5 . . ?
O13 C7 H7B 109.5 . . ?
O13 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O6 C8 C9 118.8(3) . . ?
O6 C8 C9 118.8(3) . 6_556 ?
C9 C8 C9 122.1(5) 6_556 . ?
C8 C9 C10 117.5(4) . . ?
C8 C9 C22 122.0(4) . . ?
C10 C9 C22 120.5(4) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.5(4) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C10 117.7(6) 6_556 . ?
C10 C11 C24 123.3(8) 6_556 . ?
C10 C11 C24 118.9(8) . . ?
O7 C12 C13 119.2(3) . . ?
O7 C12 C17 119.0(3) . . ?
C13 C12 C17 121.5(3) . . ?
C12 C13 C14 117.7(3) . . ?
C12 C13 C23 121.8(3) . . ?
C14 C13 C23 120.5(3) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 C13 122.4(4) . . ?
C15 C14 H14 118.8 . . ?
C14 C15 C16 117.6(4) . . ?
C14 C15 C28 122.7(5) . . ?
C14 C15 C28' 119.6(6) . . ?
C16 C15 C28 119.7(5) . . ?
C16 C15 C28' 122.8(6) . . ?
C15 C16 H16 118.6 . . ?
C17 C16 C15 122.8(4) . . ?
C17 C16 H16 118.6 . . ?
C12 C17 C22 121.1(3) . . ?
C16 C17 C12 118.0(4) . . ?
C16 C17 C22 120.8(3) . . ?
O8 C18 C19 118.8(2) . . ?
O8 C18 C19 118.8(2) . 6_556 ?
C19 C18 C19 122.3(4) . 6_556 ?
C18 C19 C20 117.6(3) . . ?
C18 C19 C23 121.7(3) . . ?
C20 C19 C23 120.7(3) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 C19 122.3(3) . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C20 117.6(5) 6_556 . ?
C20 C21 C32 121.2(2) . . ?
C20 C21 C32 121.2(2) 6_556 . ?
C9 C22 C17 111.9(3) . . ?
C9 C22 H22A 109.2 . . ?
C9 C22 H22B 109.2 . . ?
C17 C22 H22A 109.2 . . ?
C17 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C13 C23 C19 113.7(3) . . ?
C13 C23 H23A 108.8 . . ?
C13 C23 H23B 108.8 . . ?
C19 C23 H23A 108.8 . . ?
C19 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C25 C24 C11 105.5(7) . . ?
C25 C24 C26 109.3(8) . . ?
C25 C24 C27 109.2(8) . . ?
C26 C24 C11 113.7(16) . . ?
C26 C24 C27 109.6(8) . . ?
C27 C24 C11 109.3(15) . . ?
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 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
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 . . ?
C15 C28 C29 108.3(7) . . ?
C15 C28 C30 109.8(7) . . ?
C15 C28 C31 112.6(6) . . ?
C29 C28 C30 109.8(7) . . ?
C29 C28 C31 107.9(7) . . ?
C31 C28 C30 108.4(7) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29' C28' C15 110.1(11) . . ?
C30' C28' C15 107.7(10) . . ?
C30' C28' C29' 108.7(10) . . ?
C30' C28' C31' 109.0(9) . . ?
C31' C28' C15 112.0(11) . . ?
C31' C28' C29' 109.3(10) . . ?
C28' C29' H29D 109.5 . . ?
C28' C29' H29E 109.5 . . ?
C28' C29' H29F 109.5 . . ?
H29D C29' H29E 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C28' C30' H30D 109.5 . . ?
C28' C30' H30E 109.5 . . ?
C28' C30' H30F 109.5 . . ?
H30D C30' H30E 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C28' C31' H31D 109.5 . . ?
C28' C31' H31E 109.5 . . ?
C28' C31' H31F 109.5 . . ?
H31D C31' H31E 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
C21 C32 C35 111.9(4) . . ?
C33 C32 C21 108.9(6) . . ?
C33 C32 C34 110.6(7) . . ?
C33 C32 C35 108.9(7) . . ?
C34 C32 C21 108.9(6) . . ?
C34 C32 C35 107.6(7) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C39 O15 C36 110.1(8) . . ?
O15 C36 H36A 110.3 . . ?
O15 C36 H36B 110.3 . . ?
O15 C36 C37 107.1(8) . . ?
H36A C36 H36B 108.6 . . ?
C37 C36 H36A 110.3 . . ?
C37 C36 H36B 110.3 . . ?
C36 C37 H37A 110.1 . . ?
C36 C37 H37B 110.1 . . ?
C36 C37 C38 108.0(8) . . ?
H37A C37 H37B 108.4 . . ?
C38 C37 H37A 110.1 . . ?
C38 C37 H37B 110.1 . . ?
C37 C38 H38A 110.9 . . ?
C37 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
C39 C38 C37 104.3(8) . . ?
C39 C38 H38A 110.9 . . ?
C39 C38 H38B 110.9 . . ?
O15 C39 C38 110.4(9) . . ?
O15 C39 H39A 109.6 . . ?
O15 C39 H39B 109.6 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
C36' O15' C39' 108.6(11) . . ?
O15' C36' H36C 110.3 . . ?
O15' C36' H36D 110.3 . . ?
O15' C36' C37' 107.3(11) . . ?
H36C C36' H36D 108.5 . . ?
C37' C36' H36C 110.3 . . ?
C37' C36' H36D 110.3 . . ?
C36' C37' H37C 111.0 . . ?
C36' C37' H37D 111.0 . . ?
C36' C37' C38' 103.7(11) . . ?
H37C C37' H37D 109.0 . . ?
C38' C37' H37C 111.0 . . ?
C38' C37' H37D 111.0 . . ?
C37' C38' H38C 112.0 . . ?
C37' C38' H38D 112.0 . . ?
H38C C38' H38D 109.7 . . ?
C39' C38' C37' 98.7(12) . . ?
C39' C38' H38C 112.0 . . ?
C39' C38' H38D 112.0 . . ?
O15' C39' C38' 105.7(13) . . ?
O15' C39' H39C 110.6 . . ?
O15' C39' H39D 110.6 . . ?
C38' C39' H39C 110.6 . . ?
C38' C39' H39D 110.6 . . ?
H39C C39' H39D 108.7 . . ?
C44 O17 C47 107.1(17) . . ?
O17 C44 H44A 110.3 . . ?
O17 C44 H44B 110.3 . . ?
O17 C44 C45 107.0(16) . . ?
H44A C44 H44B 108.6 . . ?
C45 C44 H44A 110.3 . . ?
C45 C44 H44B 110.3 . . ?
C44 C45 H45A 111.5 . . ?
C44 C45 H45B 111.5 . . ?
C44 C45 C46 101.3(16) . . ?
H45A C45 H45B 109.3 . . ?
C46 C45 H45A 111.5 . . ?
C46 C45 H45B 111.5 . . ?
C45 C46 H46A 112.4 . . ?
C45 C46 H46B 112.4 . . ?
H46A C46 H46B 109.9 . . ?
C47 C46 C45 97.0(18) . . ?
C47 C46 H46A 112.4 . . ?
C47 C46 H46B 112.4 . . ?
O17 C47 C46 101.3(19) . . ?
O17 C47 H47A 111.5 . . ?
O17 C47 H47B 111.5 . . ?
C46 C47 H47A 111.5 . . ?
C46 C47 H47B 111.5 . . ?
H47A C47 H47B 109.3 . . ?
C44' O17' C47' 110.3(18) . . ?
O17' C44' H44C 110.5 . . ?
O17' C44' H44D 110.5 . . ?
O17' C44' C45' 106.0(19) . . ?
H44C C44' H44D 108.7 . . ?
C45' C44' H44C 110.5 . . ?
C45' C44' H44D 110.5 . . ?
C44' C45' H45C 111.4 . . ?
C44' C45' H45D 111.4 . . ?
C44' C45' C46' 101.7(19) . . ?
H45C C45' H45D 109.3 . . ?
C46' C45' H45C 111.4 . . ?
C46' C45' H45D 111.4 . . ?
C45' C46' H46C 111.7 . . ?
C45' C46' H46D 111.7 . . ?
H46C C46' H46D 109.5 . . ?
C47' C46' C45' 100.4(18) . . ?
C47' C46' H46C 111.7 . . ?
C47' C46' H46D 111.7 . . ?
O17' C47' C46' 105.7(19) . . ?
O17' C47' H47C 110.6 . . ?
O17' C47' H47D 110.6 . . ?
C46' C47' H47C 110.6 . . ?
C46' C47' H47D 110.6 . . ?
H47C C47' H47D 108.7 . . ?
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
V1 O6 1.943(3) . ?
V1 O7 1.951(2) 6_556 ?
V1 O7 1.951(2) . ?
V1 O8 1.951(3) . ?
V1 O14 2.058(3) . ?
V1 N1 2.122(4) . ?
V1 O1 2.122(4) . ?
V2 O2 1.608(4) . ?
V2 O6 2.039(4) . ?
V2 O9 2.007(3) . ?
V2 O9 2.007(3) 6_556 ?
V2 O11 1.995(5) . ?
V2 O14 2.383(3) . ?
V3 O3 1.589(3) . ?
V3 O7 2.046(2) . ?
V3 O9 1.998(3) . ?
V3 O10 2.016(2) . ?
V3 O12 1.995(3) . ?
V3 O14 2.3811(6) . ?
V4 O4 2.052(4) . ?
V4 O8 2.021(3) . ?
V4 O10 1.964(2) 6_556 ?
V4 O10 1.964(2) . ?
V4 O13 1.957(4) . ?
V4 O14 2.110(3) . ?
V5 O5 1.620(5) . ?
V5 O11 1.993(5) . ?
V5 O12 2.010(3) . ?
V5 O12 2.010(3) 6_556 ?
V5 O13 2.004(4) . ?
V5 O14 2.361(3) . ?
O4 H4 0.88(5) . ?
O4 H4 0.88(5) 6_556 ?
O6 C8 1.384(6) . ?
O7 C12 1.380(4) . ?
O8 C18 1.377(5) . ?
O9 C3 1.437(4) . ?
O10 C4 1.416(4) . ?
O11 C5 1.394(7) . ?
O12 C6 1.366(6) . ?
O13 C7 1.389(7) . ?
N1 C1 1.155(12) . ?
C1 C2 1.42(2) . ?
O16 C40 1.418(14) . ?
O16 C43 1.406(14) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.446(15) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.545(19) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.456(15) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.387(5) 6_556 ?
C8 C9 1.388(5) . ?
C9 C10 1.404(6) . ?
C9 C22 1.516(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(5) . ?
C11 C24 1.551(10) . ?
C12 C13 1.394(5) . ?
C12 C17 1.396(5) . ?
C13 C14 1.400(5) . ?
C13 C23 1.515(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(5) . ?
C15 C16 1.385(6) . ?
C15 C28 1.498(11) . ?
C15 C28' 1.606(18) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(6) . ?
C17 C22 1.543(5) . ?
C18 C19 1.389(3) . ?
C18 C19 1.389(3) 6_556 ?
C19 C20 1.394(5) . ?
C19 C23 1.528(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(4) . ?
C21 C32 1.533(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.537(9) . ?
C24 C26 1.538(9) . ?
C24 C27 1.540(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.518(7) . ?
C28 C30 1.524(8) . ?
C28 C31 1.521(8) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C28' C29' 1.523(9) . ?
C28' C30' 1.517(8) . ?
C28' C31' 1.520(8) . ?
C29' H29D 0.9800 . ?
C29' H29E 0.9800 . ?
C29' H29F 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C31' H31D 0.9800 . ?
C31' H31E 0.9800 . ?
C31' H31F 0.9800 . ?
C32 C33 1.525(9) . ?
C32 C34 1.528(9) . ?
C32 C35 1.535(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O15 C36 1.414(10) . ?
O15 C39 1.405(11) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.437(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.514(14) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.424(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O15' C36' 1.396(13) . ?
O15' C39' 1.414(13) . ?
C36' H36C 0.9900 . ?
C36' H36D 0.9900 . ?
C36' C37' 1.434(14) . ?
C37' H37C 0.9900 . ?
C37' H37D 0.9900 . ?
C37' C38' 1.558(17) . ?
C38' H38C 0.9900 . ?
C38' H38D 0.9900 . ?
C38' C39' 1.439(15) . ?
C39' H39C 0.9900 . ?
C39' H39D 0.9900 . ?
O17 C44 1.398(16) . ?
O17 C47 1.427(16) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.443(17) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.56(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.451(17) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
O17' C44' 1.404(16) . ?
O17' C47' 1.410(16) . ?
C44' H44C 0.9900 . ?
C44' H44D 0.9900 . ?
C44' C45' 1.443(17) . ?
C45' H45C 0.9900 . ?
C45' H45D 0.9900 . ?
C45' C46' 1.56(2) . ?
C46' H46C 0.9900 . ?
C46' H46D 0.9900 . ?
C46' C47' 1.436(17) . ?
C47' H47C 0.9900 . ?
C47' H47D 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4 O15 0.88(5) 1.84(5) 2.665(9) 154(5) . yes
O4 H4 O15' 0.88(5) 1.80(5) 2.601(15) 150(5) . yes
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
V1 O6 C8 C9 -86.9(4) . . . 6_556 ?
V1 O6 C8 C9 86.9(4) . . . . ?
V1 O7 C12 C13 87.0(3) . . . . ?
V1 O7 C12 C17 -87.8(3) . . . . ?
V1 O8 C18 C19 88.3(4) . . . 6_556 ?
V1 O8 C18 C19 -88.3(4) . . . . ?
V2 O6 C8 C9 93.1(4) . . . 6_556 ?
V2 O6 C8 C9 -93.1(4) . . . . ?
V3 O7 C12 C13 -93.6(3) . . . . ?
V3 O7 C12 C17 91.6(4) . . . . ?
V4 O8 C18 C19 91.7(4) . . . . ?
V4 O8 C18 C19 -91.7(4) . . . 6_556 ?
O6 C8 C9 C10 -178.2(4) . . . . ?
O6 C8 C9 C22 -0.2(7) . . . . ?
O7 C12 C13 C14 -176.5(3) . . . . ?
O7 C12 C13 C23 1.0(5) . . . . ?
O7 C12 C17 C16 177.5(3) . . . . ?
O7 C12 C17 C22 0.5(5) . . . . ?
O8 C18 C19 C20 -178.0(3) . . . . ?
O8 C18 C19 C23 3.8(6) . . . . ?
O16 C40 C41 C42 -19(3) . . . . ?
C40 O16 C43 C42 -38(3) . . . . ?
C40 C41 C42 C43 -3(3) . . . . ?
C41 C42 C43 O16 24(3) . . . . ?
C43 O16 C40 C41 36(2) . . . . ?
C8 C9 C10 C11 3.1(7) . . . . ?
C8 C9 C22 C17 -92.3(5) . . . . ?
C9 C8 C9 C10 -4.7(8) 6_556 . . . ?
C9 C8 C9 C22 173.3(3) 6_556 . . . ?
C9 C10 C11 C10 -1.6(9) . . . 6_556 ?
C9 C10 C11 C24 -178.9(5) . . . . ?
C10 C9 C22 C17 85.6(4) . . . . ?
C10 C11 C24 C25 101.4(11) . . . . ?
C10 C11 C24 C25 -75.7(12) 6_556 . . . ?
C10 C11 C24 C26 -18.3(13) . . . . ?
C10 C11 C24 C26 164.5(10) 6_556 . . . ?
C10 C11 C24 C27 -141.2(10) . . . . ?
C10 C11 C24 C27 41.7(11) 6_556 . . . ?
C12 C13 C14 C15 -0.1(5) . . . . ?
C12 C13 C23 C19 -94.5(4) . . . . ?
C12 C17 C22 C9 93.2(4) . . . . ?
C13 C12 C17 C16 2.8(5) . . . . ?
C13 C12 C17 C22 -174.2(3) . . . . ?
C13 C14 C15 C16 1.1(6) . . . . ?
C13 C14 C15 C28 -177.0(5) . . . . ?
C13 C14 C15 C28' 179.1(6) . . . . ?
C14 C13 C23 C19 82.9(4) . . . . ?
C14 C15 C16 C17 0.0(6) . . . . ?
C14 C15 C28 C29 113.4(7) . . . . ?
C14 C15 C28 C30 -126.7(7) . . . . ?
C14 C15 C28 C31 -5.9(9) . . . . ?
C14 C15 C28' C29' -51.1(11) . . . . ?
C14 C15 C28' C30' 67.2(11) . . . . ?
C14 C15 C28' C31' -173.0(9) . . . . ?
C15 C16 C17 C12 -1.8(6) . . . . ?
C15 C16 C17 C22 175.2(4) . . . . ?
C16 C15 C28 C29 -64.6(8) . . . . ?
C16 C15 C28 C30 55.3(8) . . . . ?
C16 C15 C28 C31 176.1(7) . . . . ?
C16 C15 C28' C29' 126.8(10) . . . . ?
C16 C15 C28' C30' -114.9(10) . . . . ?
C16 C15 C28' C31' 4.9(12) . . . . ?
C16 C17 C22 C9 -83.7(4) . . . . ?
C17 C12 C13 C14 -1.8(5) . . . . ?
C17 C12 C13 C23 175.7(3) . . . . ?
C18 C19 C20 C21 -1.7(6) . . . . ?
C18 C19 C23 C13 88.5(4) . . . . ?
C19 C18 C19 C20 5.5(7) 6_556 . . . ?
C19 C18 C19 C23 -172.7(3) 6_556 . . . ?
C19 C20 C21 C20 -1.8(8) . . . 6_556 ?
C19 C20 C21 C32 175.5(5) . . . . ?
C20 C19 C23 C13 -89.6(4) . . . . ?
C20 C21 C32 C33 -123.9(7) 6_556 . . . ?
C20 C21 C32 C33 58.9(8) . . . . ?
C20 C21 C32 C34 115.5(7) 6_556 . . . ?
C20 C21 C32 C34 -61.7(8) . . . . ?
C20 C21 C32 C35 -3.4(9) 6_556 . . . ?
C20 C21 C32 C35 179.4(6) . . . . ?
C22 C9 C10 C11 -174.9(5) . . . . ?
C23 C13 C14 C15 -177.7(3) . . . . ?
C23 C19 C20 C21 176.5(4) . . . . ?
C28 C15 C16 C17 178.1(5) . . . . ?
C28' C15 C16 C17 -178.0(6) . . . . ?
O15 C36 C37 C38 2.0(17) . . . . ?
C36 O15 C39 C38 -3(2) . . . . ?
C36 C37 C38 C39 -3.6(17) . . . . ?
C37 C38 C39 O15 3.9(18) . . . . ?
C39 O15 C36 C37 0.5(19) . . . . ?
O15' C36' C37' C38' 19(2) . . . . ?
C36' O15' C39' C38' -29(3) . . . . ?
C36' C37' C38' C39' -35(2) . . . . ?
C37' C38' C39' O15' 39(3) . . . . ?
C39' O15' C36' C37' 5(3) . . . . ?
O17 C44 C45 C46 21(5) . . . . ?
C44 O17 C47 C46 -40(4) . . . . ?
C44 C45 C46 C47 -43(4) . . . . ?
C45 C46 C47 O17 49(4) . . . . ?
C47 O17 C44 C45 10(5) . . . . ?
O17' C44' C45' C46' 29(7) . . . . ?
C44' O17' C47' C46' -19(8) . . . . ?
C44' C45' C46' C47' -39(5) . . . . ?
C45' C46' C47' O17' 35(6) . . . . ?
C47' O17' C44' C45' -8(9) . . . . ?
