#------------------------------------------------------------------------------
#$Date: 2022-04-21 00:53:58 +0300 (Thu, 21 Apr 2022) $
#$Revision: 274602 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/99/7129997.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_7129997
loop_
_publ_author_name
'Fertig, Alex A.'
'Cooney, Shannon E.'
'Meyer, Rachel L.'
'Brennessel, William W.'
'Matson, Ellen'
_publ_section_title
;
 Mechanistic Insight into Rapid Oxygen-Atom Transfer from a
 Calix-Functionalized Polyoxovanadate
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01228F
_journal_year                    2022
_chemical_formula_moiety         'C52 H76 O19 V6, 5(C2 H3 N)'
_chemical_formula_sum            'C62 H91 N5 O19 V6'
_chemical_formula_weight         1516.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2022-01-28 deposited with the CCDC.	2022-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.8300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2605(2)
_cell_length_b                   17.61780(10)
_cell_length_c                   20.1094(2)
_cell_measurement_reflns_used    31409
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.4470
_cell_measurement_theta_min      3.3250
_cell_volume                     7281.34(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00  22.00   0.50    0.48    --  -49.75  96.00-167.00  202
  2  ω    -30.00  22.00   0.50    0.48    --  -49.75  38.00 -60.00  104
  3  ω    -42.00 -12.00   0.50    1.94    --  -84.25  45.00  60.00   60
  4  ω    -83.00 -12.00   0.50    1.94    --  -84.25  96.00-167.00  142
  5  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00 -90.00   56
  6  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00-150.00   56
  7  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00-180.00   56
  8  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00 -90.00  150
  9  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00-120.00  106
 10  ω     34.00 127.00   0.50    1.94    --  105.75 -77.00-120.00  186
 11  ω     98.00 164.00   0.50    1.94    --  105.75  15.00   0.00  132
 12  ω     97.00 178.00   0.50    1.94    --  105.75  45.00  60.00  162
 13  ω     98.00 164.00   0.50    1.94    --  105.75  15.00 -30.00  132
 14  ω    103.00 178.00   0.50    1.94    --  105.75  96.00-167.00  150
 15  ω     92.00 178.00   0.50    1.94    --  105.75 125.00 -30.00  172
 16  ω     98.00 139.00   0.50    1.94    --  105.75  15.00 120.00   82
 17  ω     34.00 109.00   0.50    1.94    --  105.75 -96.00  83.00  150
 18  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00  90.00  106
 19  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00 120.00  150
 20  ω     34.00 127.00   0.50    1.94    --  105.75 -77.00 120.00  186
 21  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00 120.00  106
 22  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00   0.00  150
 23  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00 -30.00  106
 24  ω    -10.00  80.00   0.50    0.48    --   49.75 -96.00  83.00  180
 25  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00 120.00   56
 26  ω   -121.00 -70.00   0.50    0.48    --  -49.75-125.00-120.00  102
 27  ω   -156.00 -81.00   0.50    1.94    --  -84.25 -96.00  83.00  150
;
_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      0.0121332000
_diffrn_orient_matrix_UB_12      0.0608240000
_diffrn_orient_matrix_UB_13      -0.0503689000
_diffrn_orient_matrix_UB_21      -0.0256262000
_diffrn_orient_matrix_UB_22      -0.0547193000
_diffrn_orient_matrix_UB_23      -0.0606273000
_diffrn_orient_matrix_UB_31      -0.0693942000
_diffrn_orient_matrix_UB_32      0.0308415000
_diffrn_orient_matrix_UB_33      -0.0083901000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46057
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.870
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       needle
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7666
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0428
_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)+(0.0855P)²+8.4034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7171
_reflns_number_total             7666
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01228f2.cif
_cod_data_source_block           matrm24
_cod_database_code               7129997
_shelx_shelxl_version_number     2018/3
_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   0.569
_shelx_estimated_absorpt_t_min   0.255
_reflns_odcompleteness_completeness 99.75
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C15 \\sim C4-C15'
 with sigma of 0.02
 C15-C16 \\sim C15-C17 \\sim C15-C18 \\sim C15'-C16' \\sim C15'-C17' \\sim
C15'-C18'
 with sigma of 0.02
 C16-C17 \\sim C17-C18 \\sim C18-C16 \\sim C16'-C17' \\sim C17'-C18' \\sim
C18'-C16'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C15')
Uanis(C16) = Uanis(C16')
Uanis(C17) = Uanis(C17')
Uanis(C18) = Uanis(C18')
4. Others
 Sof(C15')=Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17')=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
 Fixed Sof: H32A(0.5) H32B(0.5) H32C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16'(H16D,H16E,H16F),
 C17'(H17D,H17E,H17F), C18'(H18D,H18E,H18F), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C)
;
_olex2_submission_original_sample_id matrm24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.143
_oxdiff_exptl_absorpt_empirical_full_min 0.643
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
V1 V 0.750000 0.64727(2) 0.500000 0.01273(11) Uani 1 2 d S T P . .
V2 V 0.65120(2) 0.77055(2) 0.41457(2) 0.01695(11) Uani 1 1 d . . . . .
V3 V 0.69276(2) 0.77126(2) 0.58561(2) 0.01711(11) Uani 1 1 d . . . . .
V4 V 0.750000 0.89776(3) 0.500000 0.01972(12) Uani 1 2 d S T P . .
O1 O 0.750000 0.55602(11) 0.500000 0.0177(4) Uani 1 2 d S T P . .
O2 O 0.58434(8) 0.76665(8) 0.35674(8) 0.0265(3) Uani 1 1 d . . . . .
O3 O 0.65279(8) 0.77214(8) 0.64239(8) 0.0259(3) Uani 1 1 d . . . . .
O4 O 0.750000 0.98772(12) 0.500000 0.0285(5) Uani 1 2 d S T P . .
O5 O 0.66910(6) 0.65761(7) 0.43091(7) 0.0146(3) Uani 1 1 d . . . . .
O6 O 0.70421(6) 0.65819(7) 0.57095(7) 0.0149(3) Uani 1 1 d . . . . .
O7 O 0.61993(7) 0.77045(7) 0.49997(8) 0.0199(3) Uani 1 1 d . . . . .
O8 O 0.78448(7) 0.77267(7) 0.64265(7) 0.0195(3) Uani 1 1 d . . . . .
O9 O 0.67048(7) 0.88248(8) 0.42953(7) 0.0218(3) Uani 1 1 d . . . . .
O10 O 0.70201(7) 0.88251(8) 0.56771(7) 0.0221(3) Uani 1 1 d . . . . .
O11 O 0.750000 0.76807(9) 0.500000 0.0164(4) Uani 1 2 d S T P . .
C1 C 0.63724(8) 0.59128(10) 0.40415(9) 0.0157(3) Uani 1 1 d . . . . .
C2 C 0.65282(8) 0.55751(10) 0.34731(9) 0.0173(3) Uani 1 1 d . . . . .
C3 C 0.62398(9) 0.48827(11) 0.32419(10) 0.0195(4) Uani 1 1 d . . . . .
H3 H 0.633504 0.465476 0.286202 0.023 Uiso 1 1 calc R U . . .
C4 C 0.58112(9) 0.45177(11) 0.35617(11) 0.0215(4) Uani 1 1 d D . . . .
C5 C 0.56822(9) 0.48691(11) 0.41323(11) 0.0211(4) Uani 1 1 d . . . . .
H5 H 0.540185 0.463196 0.435419 0.025 Uiso 1 1 calc R U . . .
C6 C 0.59581(8) 0.55649(10) 0.43843(10) 0.0173(4) Uani 1 1 d . . . . .
C7 C 0.68620(9) 0.59298(10) 0.60038(10) 0.0164(3) Uani 1 1 d . . . . .
C8 C 0.62706(9) 0.55823(10) 0.56856(10) 0.0179(4) Uani 1 1 d . . . . .
C9 C 0.61143(9) 0.49073(11) 0.59728(10) 0.0204(4) Uani 1 1 d . . . . .
H9 H 0.572054 0.467181 0.576948 0.024 Uiso 1 1 calc R U . . .
C10 C 0.65255(10) 0.45731(11) 0.65519(11) 0.0219(4) Uani 1 1 d . . . . .
C11 C 0.71189(9) 0.49353(11) 0.68389(10) 0.0209(4) Uani 1 1 d . . . . .
H11 H 0.740237 0.471974 0.722261 0.025 Uiso 1 1 calc R U . . .
C12 C 0.73014(9) 0.56047(10) 0.65730(9) 0.0175(4) Uani 1 1 d . . . . .
C13 C 0.58257(8) 0.59049(11) 0.50302(10) 0.0182(4) Uani 1 1 d . . . . .
H13A H 0.537670 0.580693 0.503018 0.022 Uiso 1 1 calc R U . . .
H13B H 0.588455 0.645058 0.502429 0.022 Uiso 1 1 calc R U . . .
C14 C 0.79781(9) 0.59306(11) 0.68622(9) 0.0177(4) Uani 1 1 d . . . . .
H14A H 0.811171 0.584127 0.735432 0.021 Uiso 1 1 calc R U . . .
H14B H 0.796677 0.647484 0.678712 0.021 Uiso 1 1 calc R U . . .
C19 C 0.63584(11) 0.38356(12) 0.68758(12) 0.0283(4) Uani 1 1 d . . . . .
C20 C 0.57024(12) 0.35076(14) 0.64801(15) 0.0392(6) Uani 1 1 d . . . . .
H20A H 0.571189 0.340729 0.601350 0.059 Uiso 1 1 calc R U . . .
H20B H 0.536335 0.386604 0.648426 0.059 Uiso 1 1 calc R U . . .
H20C H 0.562075 0.304389 0.669431 0.059 Uiso 1 1 calc R U . . .
C21 C 0.63317(14) 0.40065(15) 0.76178(14) 0.0412(6) Uani 1 1 d . . . . .
H21A H 0.600165 0.437970 0.761328 0.062 Uiso 1 1 calc R U . . .
H21B H 0.674588 0.419693 0.787431 0.062 Uiso 1 1 calc R U . . .
H21C H 0.623091 0.354937 0.782912 0.062 Uiso 1 1 calc R U . . .
C22 C 0.68864(12) 0.32431(13) 0.68850(15) 0.0377(5) Uani 1 1 d . . . . .
H22A H 0.729728 0.342867 0.715474 0.056 Uiso 1 1 calc R U . . .
H22B H 0.691414 0.314847 0.642326 0.056 Uiso 1 1 calc R U . . .
H22C H 0.677918 0.278028 0.708291 0.056 Uiso 1 1 calc R U . . .
C23 C 0.55869(10) 0.80227(14) 0.50121(13) 0.0309(5) Uani 1 1 d . . . . .
H23A H 0.528679 0.796198 0.456896 0.046 Uiso 1 1 calc R U . . .
H23B H 0.563988 0.855301 0.512212 0.046 Uiso 1 1 calc R U . . .
H23C H 0.542103 0.776783 0.535360 0.046 Uiso 1 1 calc R U . . .
C24 C 0.80164(11) 0.81714(12) 0.70441(11) 0.0277(4) Uani 1 1 d . . . . .
H24A H 0.767438 0.814132 0.727563 0.042 Uiso 1 1 calc R U . . .
H24B H 0.807692 0.869076 0.692984 0.042 Uiso 1 1 calc R U . . .
H24C H 0.841273 0.797989 0.734021 0.042 Uiso 1 1 calc R U . . .
C25 C 0.62164(12) 0.94006(13) 0.41216(15) 0.0374(6) Uani 1 1 d . . . . .
H25A H 0.640061 0.985120 0.398017 0.056 Uiso 1 1 calc R U . . .
H25B H 0.605580 0.951229 0.451566 0.056 Uiso 1 1 calc R U . . .
H25C H 0.586482 0.922495 0.375246 0.056 Uiso 1 1 calc R U . . .
C26 C 0.68541(15) 0.94246(13) 0.60759(13) 0.0398(6) Uani 1 1 d . . . . .
H26A H 0.723384 0.957795 0.642199 0.060 Uiso 1 1 calc R U . . .
H26B H 0.652668 0.925194 0.629233 0.060 Uiso 1 1 calc R U . . .
H26C H 0.668983 0.984799 0.578219 0.060 Uiso 1 1 calc R U . . .
C15 C 0.54919(17) 0.37654(19) 0.3275(2) 0.0299(5) Uani 0.875(3) 1 d D . P A 1
C16 C 0.50403(17) 0.3926(2) 0.25656(19) 0.0543(9) Uani 0.875(3) 1 d D . P A 1
H16A H 0.485073 0.345959 0.236232 0.081 Uiso 0.875(3) 1 calc R U P A 1
H16B H 0.528487 0.415369 0.227713 0.081 Uiso 0.875(3) 1 calc R U P A 1
H16C H 0.470162 0.426713 0.261177 0.081 Uiso 0.875(3) 1 calc R U P A 1
C17 C 0.60149(14) 0.31979(15) 0.32099(19) 0.0405(7) Uani 0.875(3) 1 d D . P A 1
H17A H 0.581457 0.272233 0.304445 0.061 Uiso 0.875(3) 1 calc R U P A 1
H17B H 0.631390 0.312456 0.365192 0.061 Uiso 0.875(3) 1 calc R U P A 1
H17C H 0.624524 0.338976 0.289251 0.061 Uiso 0.875(3) 1 calc R U P A 1
C18 C 0.50941(17) 0.34184(18) 0.3733(2) 0.0508(9) Uani 0.875(3) 1 d D . P A 1
H18A H 0.492062 0.293821 0.354704 0.076 Uiso 0.875(3) 1 calc R U P A 1
H18B H 0.474335 0.375384 0.375263 0.076 Uiso 0.875(3) 1 calc R U P A 1
H18C H 0.536870 0.334536 0.418865 0.076 Uiso 0.875(3) 1 calc R U P A 1
C15' C 0.5496(10) 0.3752(10) 0.3287(11) 0.0299(5) Uani 0.125(3) 1 d D . P A 2
C16' C 0.5667(11) 0.3155(12) 0.3862(11) 0.0543(9) Uani 0.125(3) 1 d D . P A 2
H16D H 0.612300 0.304129 0.396349 0.081 Uiso 0.125(3) 1 calc R U P A 2
H16E H 0.542054 0.270099 0.371489 0.081 Uiso 0.125(3) 1 calc R U P A 2
H16F H 0.556297 0.334911 0.426737 0.081 Uiso 0.125(3) 1 calc R U P A 2
C17' C 0.4750(8) 0.3815(10) 0.3076(12) 0.0405(7) Uani 0.125(3) 1 d D . P A 2
H17D H 0.456976 0.338049 0.280615 0.061 Uiso 0.125(3) 1 calc R U P A 2
H17E H 0.462504 0.426786 0.280857 0.061 Uiso 0.125(3) 1 calc R U P A 2
H17F H 0.458996 0.383724 0.348034 0.061 Uiso 0.125(3) 1 calc R U P A 2
C18' C 0.5694(11) 0.3419(12) 0.2664(12) 0.0508(9) Uani 0.125(3) 1 d D . P A 2
H18D H 0.553140 0.291022 0.258262 0.076 Uiso 0.125(3) 1 calc R U P A 2
H18E H 0.616011 0.341406 0.275463 0.076 Uiso 0.125(3) 1 calc R U P A 2
H18F H 0.551519 0.372502 0.226536 0.076 Uiso 0.125(3) 1 calc R U P A 2
N1 N 0.3387(2) 0.89635(16) 0.32609(16) 0.0717(9) Uani 1 1 d . . . . .
N2 N 0.4804(3) 0.5805(4) 0.1037(2) 0.156(3) Uani 1 1 d . . . . .
N3 N 0.750000 0.2455(3) 0.500000 0.119(3) Uani 1 2 d S T P . .
C27 C 0.35682(19) 0.87370(19) 0.3802(2) 0.0622(9) Uani 1 1 d . . . . .
C28 C 0.3754(3) 0.8454(3) 0.4524(2) 0.0927(15) Uani 1 1 d . . . . .
H28A H 0.403329 0.881656 0.481232 0.139 Uiso 1 1 calc R U . . .
H28B H 0.397784 0.797826 0.454210 0.139 Uiso 1 1 calc R U . . .
H28C H 0.336871 0.838377 0.468378 0.139 Uiso 1 1 calc R U . . .
C29 C 0.5054(2) 0.6098(2) 0.1537(2) 0.0676(10) Uani 1 1 d . . . . .
C30 C 0.53822(12) 0.64442(17) 0.21542(16) 0.0463(7) Uani 1 1 d . . . . .
H30A H 0.575403 0.671326 0.208769 0.069 Uiso 1 1 calc R U . . .
H30B H 0.552248 0.606360 0.250229 0.069 Uiso 1 1 calc R U . . .
H30C H 0.509530 0.679351 0.229614 0.069 Uiso 1 1 calc R U . . .
C31 C 0.750000 0.3118(3) 0.500000 0.0840(18) Uani 1 2 d S T P . .
C32 C 0.750000 0.3928(3) 0.500000 0.0815(18) Uani 1 2 d S T P . .
H32A H 0.757491 0.411007 0.457674 0.122 Uiso 0.5 1 calc R U P B -1
H32B H 0.783838 0.411007 0.537963 0.122 Uiso 0.5 1 calc R U P B -1
H32C H 0.708672 0.411007 0.504363 0.122 Uiso 0.5 1 calc R U P B -1
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
O1 V1 O5 95.43(4) . . ?
O1 V1 O5 95.43(4) . 2_656 ?
O1 V1 O6 95.71(4) . 2_656 ?
O1 V1 O6 95.71(4) . . ?
O1 V1 O11 180.0 . . ?
O5 V1 O5 169.14(8) . 2_656 ?
O5 V1 O6 89.06(6) . 2_656 ?
O5 V1 O6 89.86(6) 2_656 2_656 ?
O5 V1 O6 89.86(6) . . ?
O5 V1 O6 89.06(6) 2_656 . ?
O5 V1 O11 84.57(4) 2_656 . ?
O5 V1 O11 84.57(4) . . ?
O6 V1 O6 168.57(8) . 2_656 ?
O6 V1 O11 84.29(4) . . ?
O6 V1 O11 84.29(4) 2_656 . ?
O2 V2 O5 99.83(6) . . ?
O2 V2 O7 101.36(8) . . ?
O2 V2 O8 101.23(8) . 2_656 ?
O2 V2 O9 105.08(7) . . ?
O2 V2 O11 176.46(7) . . ?
O5 V2 O11 76.63(6) . . ?
O7 V2 O5 87.13(5) . . ?
O7 V2 O8 157.41(6) . 2_656 ?
O7 V2 O9 88.41(6) . . ?
O7 V2 O11 78.64(4) . . ?
O8 V2 O5 89.09(5) 2_656 . ?
O8 V2 O9 85.70(6) 2_656 . ?
O8 V2 O11 78.82(4) 2_656 . ?
O9 V2 O5 155.09(6) . . ?
O9 V2 O11 78.46(6) . . ?
O3 V3 O6 102.66(6) . . ?
O3 V3 O7 100.39(8) . . ?
O3 V3 O8 102.17(8) . . ?
O3 V3 O10 102.36(7) . . ?
O3 V3 O11 178.64(7) . . ?
O6 V3 O11 76.53(6) . . ?
O7 V3 O6 87.90(5) . . ?
O7 V3 O10 86.70(6) . . ?
O7 V3 O11 78.51(4) . . ?
O8 V3 O6 87.70(5) . . ?
O8 V3 O7 157.43(6) . . ?
O8 V3 O10 87.99(6) . . ?
O8 V3 O11 78.93(4) . . ?
O10 V3 O6 154.96(6) . . ?
O10 V3 O11 78.43(6) . . ?
O4 V4 O9 98.03(4) . . ?
O4 V4 O9 98.03(4) . 2_656 ?
O4 V4 O10 98.05(4) . 2_656 ?
O4 V4 O10 98.05(4) . . ?
O4 V4 O11 180.0 . . ?
O9 V4 O9 163.94(8) 2_656 . ?
O9 V4 O11 81.97(4) 2_656 . ?
O9 V4 O11 81.97(4) . . ?
O10 V4 O9 88.65(6) 2_656 2_656 ?
O10 V4 O9 89.11(6) 2_656 . ?
O10 V4 O9 89.11(6) . 2_656 ?
O10 V4 O9 88.65(6) . . ?
O10 V4 O10 163.89(8) . 2_656 ?
O10 V4 O11 81.95(4) 2_656 . ?
O10 V4 O11 81.95(4) . . ?
V1 O5 V2 107.73(6) . . ?
C1 O5 V1 117.24(11) . . ?
C1 O5 V2 135.02(11) . . ?
V1 O6 V3 107.80(6) . . ?
C7 O6 V1 118.55(11) . . ?
C7 O6 V3 133.65(11) . . ?
V2 O7 V3 112.73(7) . . ?
C23 O7 V2 121.52(13) . . ?
C23 O7 V3 119.48(13) . . ?
V3 O8 V2 112.39(7) . 2_656 ?
C24 O8 V2 116.65(12) . 2_656 ?
C24 O8 V3 119.97(13) . . ?
V4 O9 V2 110.62(7) . . ?
C25 O9 V2 123.31(14) . . ?
C25 O9 V4 121.76(14) . . ?
V4 O10 V3 110.96(7) . . ?
C26 O10 V3 124.90(13) . . ?
C26 O10 V4 123.33(14) . . ?
V1 O11 V2 91.06(4) . . ?
V1 O11 V2 91.06(4) . 2_656 ?
V1 O11 V3 91.37(4) . . ?
V1 O11 V3 91.37(4) . 2_656 ?
V1 O11 V4 180.0 . . ?
V2 O11 V2 177.87(8) . 2_656 ?
V2 O11 V3 89.863(12) . 2_656 ?
V2 O11 V3 89.860(12) 2_656 . ?
V2 O11 V3 90.088(12) 2_656 2_656 ?
V2 O11 V3 90.088(12) . . ?
V3 O11 V3 177.26(8) . 2_656 ?
V4 O11 V2 88.94(4) . . ?
V4 O11 V2 88.94(4) . 2_656 ?
V4 O11 V3 88.63(4) . . ?
V4 O11 V3 88.63(4) . 2_656 ?
O5 C1 C2 118.67(16) . . ?
O5 C1 C6 119.11(16) . . ?
C6 C1 C2 121.91(17) . . ?
C1 C2 C14 121.40(16) . 2_656 ?
C3 C2 C1 117.98(17) . . ?
C3 C2 C14 120.56(16) . 2_656 ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.19(18) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C15 120.2(2) . . ?
C3 C4 C15' 120.7(8) . . ?
C5 C4 C3 117.62(18) . . ?
C5 C4 C15 122.2(2) . . ?
C5 C4 C15' 121.6(8) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.43(18) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C5 117.84(17) . . ?
C1 C6 C13 121.91(16) . . ?
C5 C6 C13 120.20(17) . . ?
O6 C7 C8 118.73(16) . . ?
O6 C7 C12 119.13(16) . . ?
C8 C7 C12 121.90(17) . . ?
C7 C8 C9 117.67(17) . . ?
C7 C8 C13 121.32(16) . . ?
C9 C8 C13 120.95(17) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 C8 122.63(18) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C11 117.25(18) . . ?
C9 C10 C19 123.20(18) . . ?
C11 C10 C19 119.54(18) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.61(18) . . ?
C12 C11 H11 118.7 . . ?
C7 C12 C14 121.74(16) . . ?
C11 C12 C7 117.87(17) . . ?
C11 C12 C14 120.22(17) . . ?
C6 C13 C8 112.49(15) . . ?
C6 C13 H13A 109.1 . . ?
C6 C13 H13B 109.1 . . ?
C8 C13 H13A 109.1 . . ?
C8 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C2 C14 H14A 109.3 2_656 . ?
C2 C14 H14B 109.3 2_656 . ?
C12 C14 C2 111.60(15) . 2_656 ?
C12 C14 H14A 109.3 . . ?
C12 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C10 C19 C21 108.43(18) . . ?
C20 C19 C10 112.21(18) . . ?
C20 C19 C21 108.9(2) . . ?
C22 C19 C10 109.51(17) . . ?
C22 C19 C20 108.5(2) . . ?
C22 C19 C21 109.3(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O7 C23 H23A 109.5 . . ?
O7 C23 H23B 109.5 . . ?
O7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O8 C24 H24A 109.5 . . ?
O8 C24 H24B 109.5 . . ?
O8 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O9 C25 H25A 109.5 . . ?
O9 C25 H25B 109.5 . . ?
O9 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C26 H26A 109.5 . . ?
O10 C26 H26B 109.5 . . ?
O10 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C16 C15 C4 107.6(3) . . ?
C16 C15 C18 108.9(3) . . ?
C17 C15 C4 109.7(2) . . ?
C17 C15 C16 109.8(3) . . ?
C17 C15 C18 108.5(3) . . ?
C18 C15 C4 112.3(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16' C15' C4 109.4(15) . . ?
C16' C15' C17' 106.6(14) . . ?
C16' C15' C18' 106.9(15) . . ?
C17' C15' C4 111.0(14) . . ?
C18' C15' C4 116.2(15) . . ?
C18' C15' C17' 106.3(14) . . ?
C15' C16' H16D 109.5 . . ?
C15' C16' H16E 109.5 . . ?
C15' C16' H16F 109.5 . . ?
H16D C16' H16E 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
C15' C17' H17D 109.5 . . ?
C15' C17' H17E 109.5 . . ?
C15' C17' H17F 109.5 . . ?
H17D C17' H17E 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
C15' C18' H18D 109.5 . . ?
C15' C18' H18E 109.5 . . ?
C15' C18' H18F 109.5 . . ?
H18D C18' H18E 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
N1 C27 C28 175.3(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C29 C30 178.0(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 C32 180.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.608(2) . ?
V1 O5 1.9232(12) 2_656 ?
V1 O5 1.9231(12) . ?
V1 O6 1.9318(13) 2_656 ?
V1 O6 1.9317(13) . ?
V1 O11 2.1282(17) . ?
V2 O2 1.5911(16) . ?
V2 O5 2.0367(13) . ?
V2 O7 1.9939(15) . ?
V2 O8 2.0002(15) 2_656 ?
V2 O9 2.0210(14) . ?
V2 O11 2.3490(3) . ?
V3 O3 1.5883(16) . ?
V3 O6 2.0375(13) . ?
V3 O7 1.9996(15) . ?
V3 O8 1.9935(15) . ?
V3 O10 2.0115(14) . ?
V3 O11 2.3496(3) . ?
V4 O4 1.585(2) . ?
V4 O9 1.9268(15) . ?
V4 O9 1.9268(15) 2_656 ?
V4 O10 1.9179(14) . ?
V4 O10 1.9179(14) 2_656 ?
V4 O11 2.2848(17) . ?
O5 C1 1.388(2) . ?
O6 C7 1.390(2) . ?
O7 C23 1.424(2) . ?
O8 C24 1.434(2) . ?
O9 C25 1.429(2) . ?
O10 C26 1.424(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.392(3) . ?
C2 C3 1.391(3) . ?
C2 C14 1.520(2) 2_656 ?
C3 H3 0.9300 . ?
C3 C4 1.399(3) . ?
C4 C5 1.392(3) . ?
C4 C15 1.533(4) . ?
C4 C15' 1.543(16) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(3) . ?
C6 C13 1.521(3) . ?
C7 C8 1.398(3) . ?
C7 C12 1.401(3) . ?
C8 C9 1.399(3) . ?
C8 C13 1.522(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.395(3) . ?
C10 C11 1.400(3) . ?
C10 C19 1.535(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.390(3) . ?
C12 C14 1.520(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C19 C20 1.531(3) . ?
C19 C21 1.537(3) . ?
C19 C22 1.530(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C15 C16 1.528(5) . ?
C15 C17 1.525(4) . ?
C15 C18 1.529(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C15' C16' 1.537(15) . ?
C15' C17' 1.537(15) . ?
C15' C18' 1.537(14) . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
C17' H17D 0.9600 . ?
C17' H17E 0.9600 . ?
C17' H17F 0.9600 . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
N1 C27 1.130(5) . ?
N2 C29 1.134(5) . ?
N3 C31 1.168(9) . ?
C27 C28 1.491(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.398(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.428(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
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 O5 C1 C2 -88.16(17) . . . . ?
V1 O5 C1 C6 85.58(17) . . . . ?
V1 O6 C7 C8 -86.49(17) . . . . ?
V1 O6 C7 C12 88.01(18) . . . . ?
V2 O5 C1 C2 91.59(19) . . . . ?
V2 O5 C1 C6 -94.7(2) . . . . ?
V3 O6 C7 C8 93.3(2) . . . . ?
V3 O6 C7 C12 -92.25(19) . . . . ?
O5 C1 C2 C3 175.46(16) . . . . ?
O5 C1 C2 C14 -1.6(3) . . . 2_656 ?
O5 C1 C6 C5 -175.32(16) . . . . ?
O5 C1 C6 C13 2.2(3) . . . . ?
O6 C7 C8 C9 177.04(16) . . . . ?
O6 C7 C8 C13 -0.1(3) . . . . ?
O6 C7 C12 C11 -177.38(16) . . . . ?
O6 C7 C12 C14 -2.1(3) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C1 C6 C13 C8 -94.3(2) . . . . ?
C2 C1 C6 C5 -1.8(3) . . . . ?
C2 C1 C6 C13 175.71(16) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C2 C3 C4 C15 178.4(2) . . . . ?
C2 C3 C4 C15' 179.5(10) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C3 C4 C15 C16 -65.7(3) . . . . ?
C3 C4 C15 C17 53.7(4) . . . . ?
C3 C4 C15 C18 174.4(3) . . . . ?
C3 C4 C15' C16' 122.5(12) . . . . ?
C3 C4 C15' C17' -120.2(13) . . . . ?
C3 C4 C15' C18' 1.4(19) . . . . ?
C4 C5 C6 C1 0.5(3) . . . . ?
C4 C5 C6 C13 -177.06(17) . . . . ?
C5 C4 C15 C16 113.1(3) . . . . ?
C5 C4 C15 C17 -127.5(3) . . . . ?
C5 C4 C15 C18 -6.8(4) . . . . ?
C5 C4 C15' C16' -57.5(16) . . . . ?
C5 C4 C15' C17' 59.8(17) . . . . ?
C5 C4 C15' C18' -178.6(13) . . . . ?
C5 C6 C13 C8 83.1(2) . . . . ?
C6 C1 C2 C3 1.9(3) . . . . ?
C6 C1 C2 C14 -175.15(16) . . . 2_656 ?
C7 C8 C9 C10 -0.6(3) . . . . ?
C7 C8 C13 C6 91.7(2) . . . . ?
C7 C12 C14 C2 -90.3(2) . . . 2_656 ?
C8 C7 C12 C11 -3.1(3) . . . . ?
C8 C7 C12 C14 172.21(17) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C8 C9 C10 C19 179.56(18) . . . . ?
C9 C8 C13 C6 -85.4(2) . . . . ?
C9 C10 C11 C12 0.6(3) . . . . ?
C9 C10 C19 C20 1.4(3) . . . . ?
C9 C10 C19 C21 -118.9(2) . . . . ?
C9 C10 C19 C22 121.9(2) . . . . ?
C10 C11 C12 C7 1.4(3) . . . . ?
C10 C11 C12 C14 -174.00(17) . . . . ?
C11 C10 C19 C20 -178.1(2) . . . . ?
C11 C10 C19 C21 61.7(3) . . . . ?
C11 C10 C19 C22 -57.6(3) . . . . ?
C11 C12 C14 C2 84.9(2) . . . 2_656 ?
C12 C7 C8 C9 2.7(3) . . . . ?
C12 C7 C8 C13 -174.48(16) . . . . ?
C13 C8 C9 C10 176.58(17) . . . . ?
C14 C2 C3 C4 176.37(17) 2_656 . . . ?
C19 C10 C11 C12 -179.92(18) . . . . ?
C15 C4 C5 C6 -178.2(2) . . . . ?
C15' C4 C5 C6 -179.4(10) . . . . ?
