#------------------------------------------------------------------------------
#$Date: 2022-04-21 00:53:58 +0300 (Thu, 21 Apr 2022) $
#$Revision: 274602 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/99/7129996.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_7129996
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
'C60 H87 O19 P V6, 0.584(C4 H10 O), 0.208(C4 H6 N2)'
_chemical_formula_sum            'C63.17 H94.09 N0.42 O19.59 P V6'
_chemical_formula_weight         1509.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-03-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-01-28 deposited with the CCDC.	2022-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5148(4)
_cell_length_b                   20.0029(3)
_cell_length_c                   15.83572(19)
_cell_measurement_reflns_used    22024
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0600
_cell_measurement_theta_min      3.3990
_cell_volume                     7131.80(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_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      100.00(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 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -22.00   0.50    3.10    --  -47.20 -83.00 -93.00  196
  2  ω     93.00 178.00   0.50   12.38    --  107.75  58.00 -88.00  170
  3  ω     82.00 178.00   0.50   12.38    --  107.75  83.00  28.00  192
  4  ω     82.00 178.00   0.50   12.38    --  107.75  83.00 136.00  192
  5  ω   -120.00 -34.00   0.50    3.10    --  -47.20 -38.00-180.00  172
  6  ω    -30.00  26.00   0.50    3.10    --  -47.20  38.00  30.00  112
  7  ω    -27.00   5.00   0.50    3.10    --   47.20 -19.00 120.00   64
  8  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00  60.00  104
  9  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00 -30.00  104
 10  ω     35.00 109.00   0.50   12.38    --  107.75 -94.00-150.00  148
 11  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00 150.00  104
 12  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00   0.00  104
 13  ω     94.00 164.00   0.50   12.38    --  107.75  15.00  90.00  140
 14  ω     94.00 164.00   0.50   12.38    --  107.75  15.00-120.00  140
 15  ω     32.00  57.00   0.50    3.10    --   47.20  57.00  30.00   50
;
_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      0.0505007000
_diffrn_orient_matrix_UB_12      0.0491935000
_diffrn_orient_matrix_UB_13      -0.0210196000
_diffrn_orient_matrix_UB_21      -0.0320459000
_diffrn_orient_matrix_UB_22      0.0194643000
_diffrn_orient_matrix_UB_23      -0.0823268000
_diffrn_orient_matrix_UB_31      -0.0332470000
_diffrn_orient_matrix_UB_32      0.0559663000
_diffrn_orient_matrix_UB_33      0.0473732000
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.779
_diffrn_reflns_theta_min         3.412
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       needle
_exptl_crystal_F_000             3143
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0587
_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)+(0.0504P)²+21.0480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7056
_reflns_number_total             7723
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01228f2.cif
_cod_data_source_block           matrm28
_cod_original_cell_volume        7131.78(17)
_cod_database_code               7129996
_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   0.789
_shelx_estimated_absorpt_t_min   0.259
_reflns_odcompleteness_completeness 99.85
_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
 C10-C20 \\sim C10-C20'
 with sigma of 0.01
 C20-C21 \\sim C20-C22 \\sim C20-C23 \\sim C20'-C21' \\sim C20'-C22' \\sim
C20'-C23'
 with sigma of 0.01
 C21-C22 \\sim C22-C23 \\sim C23-C21 \\sim C21'-C22' \\sim C22'-C23' \\sim
C23'-C21'
 with sigma of 0.02
 P1-C35 \\sim P1-C36
 with sigma of 0.01
3. Restrained planarity
 C29, C31, C33, C30, C32, C34
 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
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C40 \\sim C42: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 2A
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) = Uanis(C20')
5. Rigid body (RIGU) restrains
 C37, C38, O13, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C29, C34, C33, C32, C31, C30} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C29, C30, C31, C32, C33, C34}
{C40, C39, O13, C38, C37} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C37, C38, O13, C39, C40}
7. Others
 Sof(C20')=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22')=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(N1)=Sof(C41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=0.5*(1-FVAR(3))
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(O13)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=0.5*FVAR(3)
 Fixed Sof: H25A(0.5) H25B(0.5) H25C(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 P1(0.5) C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C38(H38A,H38B), C39(H39A,H39B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34)
8.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C21'(H21D,H21E,H21F),
 C22'(H22D,H22E,H22F), C23'(H23D,H23E,H23F), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C)
;
_olex2_submission_original_sample_id matrm28
_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 2.191
_oxdiff_exptl_absorpt_empirical_full_min 0.533
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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 0.31175(3) 0.750000 0.42801(4) 0.01885(16) Uani 1 2 d S T P . .
V2 V 0.42573(3) 0.67081(3) 0.37107(3) 0.02664(15) Uani 1 1 d . . . . .
V3 V 0.30771(3) 0.66697(3) 0.25234(3) 0.02693(15) Uani 1 1 d . . . . .
V4 V 0.42878(4) 0.750000 0.19256(5) 0.02466(18) Uani 1 2 d S T P . .
O1 O 0.27070(14) 0.750000 0.5118(2) 0.0244(6) Uani 1 2 d S T P . .
O2 O 0.46845(13) 0.60630(17) 0.42077(17) 0.0480(7) Uani 1 1 d . . . . .
O3 O 0.26561(13) 0.61122(14) 0.21374(16) 0.0419(7) Uani 1 1 d . . . . .
O4 O 0.47106(16) 0.750000 0.1119(2) 0.0317(8) Uani 1 2 d S T P . .
O5 O 0.36679(9) 0.68300(10) 0.46807(12) 0.0194(4) Uani 1 1 d . . . . .
O6 O 0.26814(10) 0.68184(11) 0.36895(13) 0.0233(4) Uani 1 1 d . . . . .
O7 O 0.36741(11) 0.61185(11) 0.31471(14) 0.0278(5) Uani 1 1 d . . . . .
O8 O 0.26674(15) 0.750000 0.2134(2) 0.0314(8) Uani 1 2 d S T P . .
O9 O 0.46961(14) 0.750000 0.41289(19) 0.0262(7) Uani 1 2 d S T P . .
O10 O 0.46875(11) 0.68035(12) 0.26393(14) 0.0305(5) Uani 1 1 d . . . . .
O11 O 0.36832(12) 0.68010(13) 0.16256(15) 0.0357(6) Uani 1 1 d . . . . .
O12 O 0.36661(14) 0.750000 0.31977(18) 0.0210(6) Uani 1 2 d S T P . .
C1 C 0.35928(14) 0.65573(14) 0.54744(18) 0.0194(6) Uani 1 1 d . . . . .
C2 C 0.38630(13) 0.68628(15) 0.61708(18) 0.0196(6) Uani 1 1 d . . . . .
C3 C 0.37723(14) 0.65696(15) 0.69632(18) 0.0216(6) Uani 1 1 d . . . . .
H3 H 0.395698 0.676629 0.744200 0.026 Uiso 1 1 calc R U . . .
C4 C 0.34244(14) 0.60043(15) 0.70800(19) 0.0227(6) Uani 1 1 d . . . . .
C5 C 0.31513(15) 0.57332(15) 0.6366(2) 0.0241(6) Uani 1 1 d . . . . .
H5 H 0.290730 0.534928 0.643247 0.029 Uiso 1 1 calc R U . . .
C6 C 0.32216(15) 0.60020(14) 0.55646(19) 0.0223(6) Uani 1 1 d . . . . .
C7 C 0.21949(14) 0.65538(16) 0.41071(19) 0.0248(6) Uani 1 1 d . . . . .
C8 C 0.22819(15) 0.60345(17) 0.4680(2) 0.0268(7) Uani 1 1 d . . . . .
C9 C 0.17985(17) 0.58374(19) 0.5171(2) 0.0339(8) Uani 1 1 d . . . . .
H9 H 0.184949 0.548228 0.556300 0.041 Uiso 1 1 calc R U . . .
C10 C 0.12443(17) 0.6142(2) 0.5109(2) 0.0372(9) Uani 1 1 d D . . . .
C11 C 0.11800(16) 0.6651(2) 0.4519(2) 0.0364(8) Uani 1 1 d . . . . .
H11 H 0.080106 0.685349 0.445195 0.044 Uiso 1 1 calc R U . . .
C12 C 0.16504(15) 0.68781(19) 0.4020(2) 0.0298(7) Uani 1 1 d . . . . .
C13 C 0.4227(2) 0.750000 0.6080(3) 0.0211(8) Uani 1 2 d S T P . .
H13A H 0.442111 0.750000 0.551862 0.025 Uiso 1 2 calc R U P . .
H13B H 0.454418 0.750000 0.651287 0.025 Uiso 1 2 calc R U P . .
C14 C 0.28861(16) 0.57106(16) 0.4812(2) 0.0268(7) Uani 1 1 d . . . . .
H14A H 0.312794 0.577140 0.429517 0.032 Uiso 1 1 calc R U . . .
H14B H 0.283134 0.522454 0.489994 0.032 Uiso 1 1 calc R U . . .
C15 C 0.1573(2) 0.750000 0.3484(3) 0.0304(10) Uani 1 2 d S T P . .
H15A H 0.186957 0.750000 0.302301 0.036 Uiso 1 2 calc R U P . .
H15B H 0.117212 0.750001 0.322695 0.036 Uiso 1 2 calc R U P . .
C16 C 0.33465(16) 0.56632(17) 0.79448(19) 0.0277(7) Uani 1 1 d . . . . .
C17 C 0.3738(3) 0.5034(3) 0.7962(3) 0.0598(14) Uani 1 1 d . . . . .
H17A H 0.370229 0.481630 0.851391 0.090 Uiso 1 1 calc R U . . .
H17B H 0.415302 0.516072 0.786481 0.090 Uiso 1 1 calc R U . . .
H17C H 0.360869 0.472525 0.751875 0.090 Uiso 1 1 calc R U . . .
C18 C 0.3522(2) 0.6124(2) 0.8670(2) 0.0476(11) Uani 1 1 d . . . . .
H18A H 0.327869 0.653059 0.865048 0.071 Uiso 1 1 calc R U . . .
H18B H 0.394202 0.624435 0.861704 0.071 Uiso 1 1 calc R U . . .
H18C H 0.345681 0.589456 0.920879 0.071 Uiso 1 1 calc R U . . .
C19 C 0.27058(19) 0.5456(2) 0.8081(2) 0.0412(9) Uani 1 1 d . . . . .
H19A H 0.266106 0.526835 0.864953 0.062 Uiso 1 1 calc R U . . .
H19B H 0.259506 0.511854 0.766126 0.062 Uiso 1 1 calc R U . . .
H19C H 0.244708 0.584718 0.802172 0.062 Uiso 1 1 calc R U . . .
C20 C 0.0773(2) 0.5871(3) 0.5733(3) 0.0350(16) Uani 0.640(6) 1 d D U P A 1
C21 C 0.0957(3) 0.6050(3) 0.6635(3) 0.0465(17) Uani 0.640(6) 1 d D . P A 1
H21A H 0.100471 0.653575 0.668200 0.070 Uiso 0.640(6) 1 calc R U P A 1
H21B H 0.133380 0.583002 0.676960 0.070 Uiso 0.640(6) 1 calc R U P A 1
H21C H 0.064979 0.589966 0.702994 0.070 Uiso 0.640(6) 1 calc R U P A 1
C22 C 0.0685(3) 0.5116(3) 0.5651(4) 0.0407(16) Uani 0.640(6) 1 d D U P A 1
H22A H 0.035467 0.497464 0.601300 0.061 Uiso 0.640(6) 1 calc R U P A 1
H22B H 0.104858 0.488509 0.582552 0.061 Uiso 0.640(6) 1 calc R U P A 1
H22C H 0.059463 0.500371 0.506245 0.061 Uiso 0.640(6) 1 calc R U P A 1
C23 C 0.0188(3) 0.6218(4) 0.5519(5) 0.051(2) Uani 0.640(6) 1 d D U P A 1
H23A H -0.013032 0.603479 0.587206 0.077 Uiso 0.640(6) 1 calc R U P A 1
H23B H 0.009261 0.614403 0.492244 0.077 Uiso 0.640(6) 1 calc R U P A 1
H23C H 0.022557 0.669918 0.562517 0.077 Uiso 0.640(6) 1 calc R U P A 1
C20' C 0.0641(4) 0.6075(5) 0.5585(6) 0.0350(16) Uani 0.360(6) 1 d D U P A 2
C21' C 0.0118(5) 0.5899(6) 0.5004(7) 0.047(3) Uani 0.360(6) 1 d D U P A 2
H21D H 0.022315 0.551280 0.465412 0.070 Uiso 0.360(6) 1 calc R U P A 2
H21E H 0.002683 0.628165 0.464008 0.070 Uiso 0.360(6) 1 calc R U P A 2
H21F H -0.023116 0.579002 0.534796 0.070 Uiso 0.360(6) 1 calc R U P A 2
C22' C 0.0456(6) 0.6686(5) 0.6111(8) 0.057(4) Uani 0.360(6) 1 d D . P A 2
H22D H 0.013168 0.656097 0.649152 0.085 Uiso 0.360(6) 1 calc R U P A 2
H22E H 0.032335 0.704372 0.573311 0.085 Uiso 0.360(6) 1 calc R U P A 2
H22F H 0.079643 0.684161 0.644284 0.085 Uiso 0.360(6) 1 calc R U P A 2
C23' C 0.0744(5) 0.5484(5) 0.6178(7) 0.045(3) Uani 0.360(6) 1 d D U P A 2
H23D H 0.107078 0.558887 0.656588 0.067 Uiso 0.360(6) 1 calc R U P A 2
H23E H 0.084686 0.508640 0.584679 0.067 Uiso 0.360(6) 1 calc R U P A 2
H23F H 0.038220 0.539665 0.650349 0.067 Uiso 0.360(6) 1 calc R U P A 2
C24 C 0.38258(19) 0.54780(18) 0.2829(3) 0.0385(9) Uani 1 1 d . . . . .
H24A H 0.408704 0.552826 0.233832 0.058 Uiso 1 1 calc R U . . .
H24B H 0.346374 0.524083 0.266101 0.058 Uiso 1 1 calc R U . . .
H24C H 0.403144 0.522220 0.326868 0.058 Uiso 1 1 calc R U . . .
C25 C 0.2299(3) 0.750000 0.1412(3) 0.0451(14) Uani 1 2 d S T P . .
H25A H 0.195057 0.721775 0.151589 0.068 Uiso 0.5 1 calc R U P B -1
H25B H 0.252079 0.732447 0.092782 0.068 Uiso 0.5 1 calc R U P B -1
H25C H 0.216922 0.795778 0.129040 0.068 Uiso 0.5 1 calc R U P B -1
C26 C 0.5326(2) 0.750000 0.4185(4) 0.0411(13) Uani 1 2 d S T P . .
H26A H 0.545109 0.779974 0.464056 0.062 Uiso 0.5 1 calc R U P C -1
H26B H 0.549452 0.765450 0.364869 0.062 Uiso 0.5 1 calc R U P C -1
H26C H 0.546586 0.704576 0.430319 0.062 Uiso 0.5 1 calc R U P C -1
C27 C 0.5126(2) 0.6380(3) 0.2332(3) 0.0604(15) Uani 1 1 d . . . . .
H27A H 0.523260 0.605348 0.276808 0.091 Uiso 1 1 calc R U . . .
H27B H 0.547796 0.664291 0.218050 0.091 Uiso 1 1 calc R U . . .
H27C H 0.497840 0.614535 0.183149 0.091 Uiso 1 1 calc R U . . .
C28 C 0.3616(3) 0.6582(3) 0.0814(3) 0.0688(17) Uani 1 1 d . . . . .
H28A H 0.333358 0.620883 0.080316 0.103 Uiso 1 1 calc R U . . .
H28B H 0.400010 0.643233 0.059445 0.103 Uiso 1 1 calc R U . . .
H28C H 0.346432 0.694765 0.046287 0.103 Uiso 1 1 calc R U . . .
P1 P 0.49695(9) 0.54365(10) 0.47101(12) 0.0360(4) Uani 0.5 1 d D . P D -1
C29 C 0.5691(4) 0.5776(4) 0.5058(5) 0.055(2) Uani 0.5 1 d D . P D -1
C30 C 0.5730(5) 0.6145(5) 0.5808(6) 0.071(3) Uani 0.5 1 d D . P D -1
H30 H 0.540159 0.616049 0.618454 0.085 Uiso 0.5 1 calc R U P D -1
C31 C 0.6215(6) 0.6468(5) 0.5989(8) 0.081(4) Uani 0.5 1 d D . P D -1
H31 H 0.623393 0.671615 0.649902 0.097 Uiso 0.5 1 calc R U P D -1
C32 C 0.6704(5) 0.6460(5) 0.5459(7) 0.063(3) Uani 0.5 1 d D . P D -1
H32 H 0.705363 0.669930 0.560384 0.075 Uiso 0.5 1 calc R U P D -1
C33 C 0.6676(5) 0.6101(5) 0.4725(8) 0.074(3) Uani 0.5 1 d D . P D -1
H33 H 0.700753 0.608922 0.435448 0.089 Uiso 0.5 1 calc R U P D -1
C34 C 0.6187(5) 0.5772(5) 0.4533(7) 0.068(3) Uani 0.5 1 d D . P D -1
H34 H 0.617319 0.552478 0.402147 0.082 Uiso 0.5 1 calc R U P D -1
C35 C 0.5134(5) 0.4702(5) 0.4082(6) 0.053(2) Uani 0.5 1 d D . P D -1
H35A H 0.476382 0.446618 0.394959 0.080 Uiso 0.5 1 calc R U P D -1
H35B H 0.539766 0.440447 0.440026 0.080 Uiso 0.5 1 calc R U P D -1
H35C H 0.532933 0.483749 0.355606 0.080 Uiso 0.5 1 calc R U P D -1
C36 C 0.4535(5) 0.5158(7) 0.5593(7) 0.072(4) Uani 0.5 1 d D . P D -1
H36A H 0.436593 0.554639 0.588458 0.108 Uiso 0.5 1 calc R U P D -1
H36B H 0.478871 0.490811 0.598426 0.108 Uiso 0.5 1 calc R U P D -1
H36C H 0.421350 0.486892 0.539263 0.108 Uiso 0.5 1 calc R U P D -1
C37 C 0.6419(12) 0.8669(16) 0.5428(17) 0.092(8) Uani 0.292(6) 1 d D U P E -1
H37A H 0.683289 0.873875 0.525651 0.137 Uiso 0.292(6) 1 calc R U P E -1
H37B H 0.620875 0.909780 0.542423 0.137 Uiso 0.292(6) 1 calc R U P E -1
H37C H 0.622666 0.836048 0.503279 0.137 Uiso 0.292(6) 1 calc R U P E -1
C38 C 0.6403(9) 0.8380(12) 0.6296(15) 0.073(6) Uani 0.292(6) 1 d D . P E -1
H38A H 0.633313 0.875714 0.668787 0.088 Uiso 0.292(6) 1 calc R U P E -1
H38B H 0.604562 0.809259 0.632377 0.088 Uiso 0.292(6) 1 calc R U P E -1
O13 O 0.6889(5) 0.7992(6) 0.6650(7) 0.054(3) Uani 0.292(6) 1 d D . P E -1
C39 C 0.6859(12) 0.7839(11) 0.7538(12) 0.089(7) Uani 0.292(6) 1 d D . P E -1
H39A H 0.646054 0.765364 0.765947 0.107 Uiso 0.292(6) 1 calc R U P E -1
H39B H 0.689559 0.826312 0.785630 0.107 Uiso 0.292(6) 1 calc R U P E -1
C40 C 0.7312(11) 0.7361(11) 0.7875(12) 0.058(5) Uani 0.292(6) 1 d D U P E -1
H40A H 0.738483 0.700846 0.745745 0.088 Uiso 0.292(6) 1 calc R U P E -1
H40B H 0.716582 0.716066 0.839945 0.088 Uiso 0.292(6) 1 calc R U P E -1
H40C H 0.768360 0.760100 0.798719 0.088 Uiso 0.292(6) 1 calc R U P E -1
N1 N 0.7410(13) 0.750000 0.6534(12) 0.108(8) Uani 0.416(11) 2 d S TU P E 2
C41 C 0.7367(11) 0.750000 0.7215(13) 0.065(5) Uani 0.416(11) 2 d S TU P E 2
C42 C 0.7315(15) 0.750000 0.8174(14) 0.052(5) Uani 0.416(11) 2 d S TU P E 2
H42A H 0.736309 0.795712 0.838625 0.077 Uiso 0.208(6) 1 calc R U P E 2
H42B H 0.762556 0.721395 0.841502 0.077 Uiso 0.208(6) 1 calc R U P E 2
H42C H 0.692422 0.732893 0.833815 0.077 Uiso 0.208(6) 1 calc R U P E 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'
P P 0.2955 0.4335 '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 95.56(10) . . ?
O1 V1 O5 95.56(10) . 7_575 ?
O1 V1 O6 96.17(10) . 7_575 ?
O1 V1 O6 96.17(10) . . ?
O1 V1 O12 179.06(14) . . ?
O5 V1 O5 87.82(13) . 7_575 ?
O5 V1 O12 83.77(9) 7_575 . ?
O5 V1 O12 83.77(9) . . ?
O6 V1 O5 89.74(9) . . ?
O6 V1 O5 168.20(10) 7_575 . ?
O6 V1 O5 168.20(10) . 7_575 ?
O6 V1 O5 89.73(9) 7_575 7_575 ?
O6 V1 O6 90.31(14) 7_575 . ?
O6 V1 O12 84.49(9) 7_575 . ?
O6 V1 O12 84.49(9) . . ?
O2 V2 O5 95.99(11) . . ?
O2 V2 O7 97.20(13) . . ?
O2 V2 O9 99.28(13) . . ?
O2 V2 O10 100.65(11) . . ?
O2 V2 O12 174.46(12) . . ?
O5 V2 O12 78.52(10) . . ?
O7 V2 O5 88.81(9) . . ?
O7 V2 O9 163.50(10) . . ?
O7 V2 O12 82.09(9) . . ?
O9 V2 O5 88.69(11) . . ?
O9 V2 O12 81.43(9) . . ?
O10 V2 O5 163.35(9) . . ?
O10 V2 O7 89.74(10) . . ?
O10 V2 O9 88.00(12) . . ?
O10 V2 O12 84.85(10) . . ?
O3 V3 O6 100.81(12) . . ?
O3 V3 O7 101.79(14) . . ?
O3 V3 O8 100.94(14) . . ?
O3 V3 O11 103.15(12) . . ?
O3 V3 O12 175.69(12) . . ?
O6 V3 O12 74.89(10) . . ?
O7 V3 O6 85.87(9) . . ?
O7 V3 O12 77.79(8) . . ?
O8 V3 O6 87.53(12) . . ?
O8 V3 O7 157.14(11) . . ?
O8 V3 O12 79.36(10) . . ?
O11 V3 O6 156.01(10) . . ?
O11 V3 O7 87.97(11) . . ?
O11 V3 O8 89.23(13) . . ?
O11 V3 O12 81.15(10) . . ?
O4 V4 O10 100.58(12) . . ?
O4 V4 O10 100.58(12) . 7_575 ?
O4 V4 O11 102.43(12) . 7_575 ?
O4 V4 O11 102.43(12) . . ?
O4 V4 O12 178.10(16) . . ?
O10 V4 O10 87.92(15) 7_575 . ?
O10 V4 O11 87.35(11) 7_575 7_575 ?
O10 V4 O11 156.98(10) . 7_575 ?
O10 V4 O11 87.35(11) . . ?
O10 V4 O11 156.98(10) 7_575 . ?
O10 V4 O12 78.08(8) 7_575 . ?
O10 V4 O12 78.08(8) . . ?
O11 V4 O11 88.24(17) 7_575 . ?
O11 V4 O12 78.90(9) 7_575 . ?
O11 V4 O12 78.90(9) . . ?
P1 O2 V2 170.8(2) . . ?
V1 O5 V2 104.61(9) . . ?
C1 O5 V1 119.63(18) . . ?
C1 O5 V2 135.75(18) . . ?
V1 O6 V3 108.40(10) . . ?
C7 O6 V1 116.27(18) . . ?
C7 O6 V3 135.32(19) . . ?
V2 O7 V3 109.90(11) . . ?
C24 O7 V2 122.6(2) . . ?
C24 O7 V3 119.0(2) . . ?
V3 O8 V3 112.52(16) . 7_575 ?
C25 O8 V3 121.39(11) . . ?
C25 O8 V3 121.39(11) . 7_575 ?
V2 O9 V2 106.20(15) . 7_575 ?
C26 O9 V2 121.24(14) . 7_575 ?
C26 O9 V2 121.24(14) . . ?
V2 O10 V4 109.45(11) . . ?
C27 O10 V2 126.5(2) . . ?
C27 O10 V4 123.0(2) . . ?
V3 O11 V4 112.83(11) . . ?
C28 O11 V3 123.6(3) . . ?
C28 O11 V4 121.4(3) . . ?
V1 O12 V2 93.07(9) . . ?
V1 O12 V2 93.07(9) . 7_575 ?
V1 O12 V3 92.19(10) . 7_575 ?
V1 O12 V3 92.19(10) . . ?
V1 O12 V4 179.02(15) . . ?
V2 O12 V2 90.90(11) . 7_575 ?
V2 O12 V3 174.60(15) . 7_575 ?
V2 O12 V3 90.02(2) 7_575 7_575 ?
V2 O12 V3 174.60(15) 7_575 . ?
V2 O12 V3 90.02(2) . . ?
V2 O12 V4 87.62(9) . . ?
V2 O12 V4 87.62(9) 7_575 . ?
V3 O12 V3 88.58(10) . 7_575 ?
V3 O12 V4 87.11(8) 7_575 . ?
V3 O12 V4 87.11(8) . . ?
O5 C1 C2 119.4(3) . . ?
O5 C1 C6 118.7(3) . . ?
C6 C1 C2 121.8(3) . . ?
C1 C2 C3 117.4(3) . . ?
C1 C2 C13 121.7(3) . . ?
C3 C2 C13 120.9(3) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.9(3) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.2(3) . . ?
C3 C4 C16 122.9(3) . . ?
C5 C4 C16 119.8(3) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 C4 122.7(3) . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C14 121.3(3) . . ?
C5 C6 C1 118.0(3) . . ?
C5 C6 C14 120.7(3) . . ?
O6 C7 C8 119.0(3) . . ?
O6 C7 C12 118.1(3) . . ?
C8 C7 C12 122.3(3) . . ?
C7 C8 C9 117.7(3) . . ?
C7 C8 C14 122.2(3) . . ?
C9 C8 C14 120.1(3) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 C8 122.4(3) . . ?
C10 C9 H9 118.8 . . ?
C9 C10 C20 114.7(4) . . ?
C9 C10 C20' 135.2(5) . . ?
C11 C10 C9 117.5(3) . . ?
C11 C10 C20 127.8(4) . . ?
C11 C10 C20' 107.3(5) . . ?
C10 C11 H11 118.7 . . ?
C10 C11 C12 122.6(4) . . ?
C12 C11 H11 118.7 . . ?
C7 C12 C11 117.4(3) . . ?
C7 C12 C15 122.6(3) . . ?
C11 C12 C15 119.7(4) . . ?
C2 C13 C2 113.7(4) . 7_575 ?
C2 C13 H13A 108.8 . . ?
C2 C13 H13A 108.8 7_575 . ?
C2 C13 H13B 108.8 . . ?
C2 C13 H13B 108.8 7_575 . ?
H13A C13 H13B 107.7 . . ?
C6 C14 H14A 109.0 . . ?
C6 C14 H14B 109.0 . . ?
C8 C14 C6 112.8(3) . . ?
C8 C14 H14A 109.0 . . ?
C8 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C12 C15 C12 110.3(4) 7_575 . ?
C12 C15 H15A 109.6 . . ?
C12 C15 H15A 109.6 7_575 . ?
C12 C15 H15B 109.6 . . ?
C12 C15 H15B 109.6 7_575 . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C4 108.2(3) . . ?
C18 C16 C4 111.9(3) . . ?
C18 C16 C17 109.5(4) . . ?
C19 C16 C4 110.9(3) . . ?
C19 C16 C17 108.6(4) . . ?
C19 C16 C18 107.7(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C10 109.1(4) . . ?
C21 C20 C22 110.2(5) . . ?
C22 C20 C10 112.3(5) . . ?
C23 C20 C10 106.9(4) . . ?
C23 C20 C21 109.5(5) . . ?
C23 C20 C22 108.6(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21' C20' C10 113.5(7) . . ?
C21' C20' C22' 107.4(8) . . ?
C22' C20' C10 115.4(8) . . ?
C23' C20' C10 103.3(7) . . ?
C23' C20' C21' 107.9(7) . . ?
C23' C20' C22' 108.8(7) . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C20' C22' H22D 109.5 . . ?
C20' C22' H22E 109.5 . . ?
C20' C22' H22F 109.5 . . ?
H22D C22' H22E 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C20' C23' H23D 109.5 . . ?
C20' C23' H23E 109.5 . . ?
C20' C23' H23F 109.5 . . ?
H23D C23' H23E 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
O7 C24 H24A 109.5 . . ?
O7 C24 H24B 109.5 . . ?
O7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O8 C25 H25A 109.5 . . ?
O8 C25 H25B 109.5 . . ?
O8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O9 C26 H26A 109.5 . . ?
O9 C26 H26B 109.5 . . ?
O9 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O10 C27 H27A 109.5 . . ?
O10 C27 H27B 109.5 . . ?
O10 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O11 C28 H28A 109.5 . . ?
O11 C28 H28B 109.5 . . ?
O11 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 P1 C29 102.2(3) . . ?
O2 P1 C35 116.1(4) . . ?
O2 P1 C36 114.0(4) . . ?
C35 P1 C29 106.4(5) . . ?
C36 P1 C29 111.2(6) . . ?
C36 P1 C35 106.7(6) . . ?
C30 C29 P1 120.1(8) . . ?
C34 C29 P1 121.8(8) . . ?
C34 C29 C30 117.3(11) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.0(11) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.0 . . ?
C30 C31 C32 122.0(12) . . ?
C32 C31 H31 119.0 . . ?
C31 C32 H32 120.5 . . ?
C33 C32 C31 119.0(12) . . ?
C33 C32 H32 120.5 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(12) . . ?
C34 C33 H33 120.1 . . ?
C29 C34 H34 119.0 . . ?
C33 C34 C29 122.0(11) . . ?
C33 C34 H34 119.0 . . ?
P1 C35 H35A 109.5 . . ?
P1 C35 H35B 109.5 . . ?
P1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
P1 C36 H36A 109.5 . . ?
P1 C36 H36B 109.5 . . ?
P1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
C37 C38 H38A 106.6 . . ?
C37 C38 H38B 106.6 . . ?
H38A C38 H38B 106.5 . . ?
O13 C38 C37 123.0(19) . . ?
O13 C38 H38A 106.6 . . ?
O13 C38 H38B 106.6 . . ?
C39 O13 C38 117.1(16) . . ?
O13 C39 H39A 108.1 . . ?
O13 C39 H39B 108.1 . . ?
O13 C39 C40 116.8(17) . . ?
H39A C39 H39B 107.3 . . ?
C40 C39 H39A 108.1 . . ?
C40 C39 H39B 108.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1 C41 C42 179(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 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 1.618(3) . ?
V1 O5 1.932(2) 7_575 ?
V1 O5 1.932(2) . ?
V1 O6 1.923(2) 7_575 ?
V1 O6 1.923(2) . ?
V1 O12 2.113(3) . ?
V2 O2 1.792(3) . ?
V2 O5 2.045(2) . ?
V2 O7 1.978(2) . ?
V2 O9 1.981(2) . ?
V2 O10 1.963(2) . ?
V2 O12 2.223(2) . ?
V3 O3 1.586(3) . ?
V3 O6 2.072(2) . ?
V3 O7 1.999(3) . ?
V3 O8 1.9972(19) . ?
V3 O11 1.988(2) . ?
V3 O12 2.378(2) . ?
V4 O4 1.593(3) . ?
V4 O10 2.007(2) 7_575 ?
V4 O10 2.007(2) . ?
V4 O11 2.008(3) 7_575 ?
V4 O11 2.008(3) . ?
V4 O12 2.453(3) . ?
O2 P1 1.617(3) . ?
O5 C1 1.380(3) . ?
O6 C7 1.384(4) . ?
O7 C24 1.418(4) . ?
O8 C25 1.414(6) . ?
O9 C26 1.420(6) . ?
O10 C27 1.389(5) . ?
O11 C28 1.366(5) . ?
C1 C2 1.400(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.400(4) . ?
C2 C13 1.522(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C4 C5 1.396(4) . ?
C4 C16 1.540(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(4) . ?
C6 C14 1.527(4) . ?
C7 C8 1.393(5) . ?
C7 C12 1.394(5) . ?
C8 C9 1.395(5) . ?
C8 C14 1.521(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.392(6) . ?
C10 C11 1.391(6) . ?
C10 C20 1.548(6) . ?
C10 C20' 1.559(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(5) . ?
C12 C15 1.516(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.536(5) . ?
C16 C18 1.525(5) . ?
C16 C19 1.516(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.529(6) . ?
C20 C22 1.530(6) . ?
C20 C23 1.527(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C20' C21' 1.535(7) . ?
C20' C22' 1.536(7) . ?
C20' C23' 1.529(7) . ?
C21' H21D 0.9800 . ?
C21' H21E 0.9800 . ?
C21' H21F 0.9800 . ?
C22' H22D 0.9800 . ?
C22' H22E 0.9800 . ?
C22' H22F 0.9800 . ?
C23' H23D 0.9800 . ?
C23' H23E 0.9800 . ?
C23' H23F 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
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 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
P1 C29 1.845(11) . ?
P1 C35 1.813(8) . ?
P1 C36 1.795(9) . ?
C29 C30 1.402(13) . ?
C29 C34 1.392(12) . ?
C30 H30 0.9500 . ?
C30 C31 1.299(15) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(16) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(15) . ?
C33 H33 0.9500 . ?
C33 C34 1.317(14) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 C38 1.49(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 O13 1.453(19) . ?
O13 C39 1.441(18) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.50(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N1 C41 1.08(3) . ?
C41 C42 1.52(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
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 -89.4(3) . . . . ?
V1 O5 C1 C6 87.3(3) . . . . ?
V1 O6 C7 C8 -84.5(3) . . . . ?
V1 O6 C7 C12 87.0(3) . . . . ?
V2 O5 C1 C2 90.9(3) . . . . ?
V2 O5 C1 C6 -92.4(3) . . . . ?
V3 O6 C7 C8 96.4(3) . . . . ?
V3 O6 C7 C12 -92.1(4) . . . . ?
O2 P1 C29 C30 85.0(5) . . . . ?
O2 P1 C29 C34 -84.3(5) . . . . ?
O5 C1 C2 C3 179.8(3) . . . . ?
O5 C1 C2 C13 1.5(4) . . . . ?
O5 C1 C6 C5 179.9(3) . . . . ?
O5 C1 C6 C14 -2.0(4) . . . . ?
O6 C7 C8 C9 171.8(3) . . . . ?
O6 C7 C8 C14 -5.0(4) . . . . ?
O6 C7 C12 C11 -172.9(3) . . . . ?
O6 C7 C12 C15 0.5(5) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C1 C2 C13 C2 89.6(4) . . . 7_575 ?
C1 C6 C14 C8 -88.6(4) . . . . ?
C2 C1 C6 C5 -3.5(5) . . . . ?
C2 C1 C6 C14 174.5(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C16 177.2(3) . . . . ?
C3 C2 C13 C2 -88.6(4) . . . 7_575 ?
C3 C4 C5 C6 0.7(5) . . . . ?
C3 C4 C16 C17 -102.7(4) . . . . ?
C3 C4 C16 C18 18.0(5) . . . . ?
C3 C4 C16 C19 138.2(3) . . . . ?
C4 C5 C6 C1 1.5(5) . . . . ?
C4 C5 C6 C14 -176.6(3) . . . . ?
C5 C4 C16 C17 75.5(4) . . . . ?
C5 C4 C16 C18 -163.8(3) . . . . ?
C5 C4 C16 C19 -43.6(4) . . . . ?
C5 C6 C14 C8 89.3(4) . . . . ?
C6 C1 C2 C3 3.2(4) . . . . ?
C6 C1 C2 C13 -175.1(3) . . . . ?
C7 C8 C9 C10 -0.4(5) . . . . ?
C7 C8 C14 C6 96.4(4) . . . . ?
C7 C12 C15 C12 -92.8(4) . . . 7_575 ?
C8 C7 C12 C11 -1.7(5) . . . . ?
C8 C7 C12 C15 171.8(3) . . . . ?
C8 C9 C10 C11 1.2(5) . . . . ?
C8 C9 C10 C20 -177.6(4) . . . . ?
C8 C9 C10 C20' -175.7(6) . . . . ?
C9 C8 C14 C6 -80.2(4) . . . . ?
C9 C10 C11 C12 -2.4(5) . . . . ?
C9 C10 C20 C21 66.4(5) . . . . ?
C9 C10 C20 C22 -56.1(5) . . . . ?
C9 C10 C20 C23 -175.2(5) . . . . ?
C9 C10 C20' C21' -122.5(7) . . . . ?
C9 C10 C20' C22' 112.8(8) . . . . ?
C9 C10 C20' C23' -5.8(10) . . . . ?
C10 C11 C12 C7 2.6(5) . . . . ?
C10 C11 C12 C15 -171.1(3) . . . . ?
C11 C10 C20 C21 -112.3(5) . . . . ?
C11 C10 C20 C22 125.2(5) . . . . ?
C11 C10 C20 C23 6.1(7) . . . . ?
C11 C10 C20' C21' 60.4(8) . . . . ?
C11 C10 C20' C22' -64.3(8) . . . . ?
C11 C10 C20' C23' 177.0(6) . . . . ?
C11 C12 C15 C12 80.5(5) . . . 7_575 ?
C12 C7 C8 C9 0.6(5) . . . . ?
C12 C7 C8 C14 -176.1(3) . . . . ?
C13 C2 C3 C4 177.4(3) . . . . ?
C14 C8 C9 C10 176.5(3) . . . . ?
C16 C4 C5 C6 -177.6(3) . . . . ?
C20 C10 C11 C12 176.3(4) . . . . ?
C20' C10 C11 C12 175.3(5) . . . . ?
P1 C29 C30 C31 -169.7(6) . . . . ?
P1 C29 C34 C33 169.5(6) . . . . ?
C29 C30 C31 C32 0.0(5) . . . . ?
C30 C29 C34 C33 -0.1(4) . . . . ?
C30 C31 C32 C33 -0.1(5) . . . . ?
C31 C32 C33 C34 0.1(4) . . . . ?
C32 C33 C34 C29 0.0(5) . . . . ?
C34 C29 C30 C31 0.1(4) . . . . ?
C35 P1 C29 C30 -152.8(5) . . . . ?
C35 P1 C29 C34 37.8(6) . . . . ?
C36 P1 C29 C30 -37.0(7) . . . . ?
C36 P1 C29 C34 153.7(6) . . . . ?
C37 C38 O13 C39 170(2) . . . . ?
C38 O13 C39 C40 171.6(19) . . . . ?
