#------------------------------------------------------------------------------
#$Date: 2021-04-05 18:06:35 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/10/1561003.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_1561003
loop_
_publ_author_name
'Fertig, Alex A.'
'Rabbani, S. M. Gulam'
'Koch, Melissa D.'
'Brennessel, William W.'
'Miró, Pere'
'Matson, Ellen M.'
_publ_section_title
;
 Physicochemical implications of surface alkylation of high-valent,
 Lindqvist-type polyoxovanadate-alkoxide clusters.
;
_journal_issue                   12
_journal_name_full               Nanoscale
_journal_page_first              6162
_journal_page_last               6173
_journal_paper_doi               10.1039/d0nr09201k
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C9 H15 N2 O23 V6, C16 H36 N'
_chemical_formula_sum            'C25 H51 N3 O23 V6'
_chemical_formula_weight         1067.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.85930(10)
_cell_length_b                   17.31290(10)
_cell_length_c                   17.69540(10)
_cell_measurement_reflns_used    39776
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3150
_cell_measurement_theta_min      3.5960
_cell_volume                     4173.22(5)
_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      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 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  24.00   0.50    0.20    --  -49.75  19.00 -90.00   58
  2  ω     -5.00  24.00   0.50    0.20    --  -49.75  19.00 -30.00   58
  3  ω     -5.00  24.00   0.50    0.20    --  -49.75  19.00  60.00   58
  4  ω     22.00  89.00   0.50    0.20    --   49.75-112.00  47.00  134
  5  ω     34.00 112.00   0.50    0.81    --  105.75-112.00  47.00  156
  6  ω     34.00 127.00   0.50    0.81    --  105.75 -77.00  60.00  186
  7  ω     98.00 178.00   0.50    0.81    --  105.75  30.00  60.00  160
  8  ω    100.00 178.00   0.50    0.81    --  105.75 112.00 140.00  156
  9  ω     92.00 178.00   0.50    0.81    --  105.75 125.00 120.00  172
 10  ω     98.00 175.00   0.50    0.81    --  105.75  15.00 -90.00  154
 11  ω     98.00 175.00   0.50    0.81    --  105.75  15.00-150.00  154
 12  ω     98.00 175.00   0.50    0.81    --  105.75  15.00-120.00  154
 13  ω     42.00 121.00   0.50    0.20    --   49.75  38.00  30.00  158
 14  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00  60.00   92
 15  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00  60.00  150
 16  ω     34.00 127.00   0.50    0.81    --  105.75 -77.00 150.00  186
 17  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00  30.00   92
 18  ω     34.00 116.00   0.50    0.81    --  105.75-125.00 120.00  164
 19  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00 120.00  150
 20  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-120.00   92
 21  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00-180.00  150
 22  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-180.00   92
 23  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-150.00   92
 24  ω     29.00 121.00   0.50    0.20    --   49.75  77.00  60.00  184
 25  ω     29.00 121.00   0.50    0.20    --   49.75  77.00 150.00  184
 26  ω    -86.00   0.00   0.50    0.20    --  -49.75 112.00 140.00  172
 27  ω    -86.00 -12.00   0.50    0.81    --  -84.25 112.00 140.00  148
 28  ω   -121.00 -68.00   0.50    0.20    --  -49.75 -77.00-150.00  106
 29  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00-150.00  102
 30  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00-180.00  102
 31  ω   -121.00 -29.00   0.50    0.20    --  -49.75 -77.00 -90.00  184
 32  ω   -121.00 -29.00   0.50    0.20    --  -49.75 -77.00   0.00  184
 33  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00 120.00  102
 34  ω   -156.00 -78.00   0.50    0.81    --  -84.25-112.00  47.00  156
;
_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      0.1046485000
_diffrn_orient_matrix_UB_12      -0.0063475000
_diffrn_orient_matrix_UB_13      0.0475378000
_diffrn_orient_matrix_UB_21      -0.0007952000
_diffrn_orient_matrix_UB_22      0.0870808000
_diffrn_orient_matrix_UB_23      0.0177260000
_diffrn_orient_matrix_UB_31      -0.0429139000
_diffrn_orient_matrix_UB_32      -0.0170468000
_diffrn_orient_matrix_UB_33      0.0726172000
_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  0.0856
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71313
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.910
_diffrn_reflns_theta_min         3.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17550
_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            red-orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.047
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0645
_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)+(0.0530P)²+21.2508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8373
_reflns_number_total             8801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nr09201k2.cif
_cod_data_source_block           mataf22
_cod_depositor_comments
'Adding full bibliography for 1561002--1561005.cif.'
_cod_database_code               1561003
_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   0.314
_shelx_estimated_absorpt_t_min   0.141
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-N2 \\sim C8-N2'
 with sigma of 0.01
 N2-O22 \\sim N2-O23 \\sim N2'-O22' \\sim N2'-O23'
 with sigma of 0.01
 O22-O23 \\sim O22'-O23'
 with sigma of 0.02
 O16-C25 \\sim O10-C25' \\sim O9-C25"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
O22' \\sim N2' \\sim O23': within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
O10 \\sim C25': within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O9 \\sim C25": within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
4. Rigid body (RIGU) restrains
 C8, N2, O22, O23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14', C15', C16'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19', C20'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22', C23', C24'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C13, C14', C15', C16'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C13, C14, C15, C16}
{C18, C19', C20'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C18, C19, C20}
{C21, C22', C23', C24'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C21, C22, C23, C24}
6. Others
 1*[Sof(C25)+Sof(H25A)+Sof(H25B)+Sof(H25C)]+1*[Sof(C25')+Sof(H25D)+Sof(H25E)+
 Sof(H25F)]+1*[Sof(C25")+Sof(H25G)+Sof(H25H)+Sof(H25I)]=1 with esd of 0.0001
 1*[Sof(C25")+Sof(H25G)+Sof(H25H)+Sof(H25I)]+1*[Sof(H13A)+Sof(H13B)+Sof(H13C)+
 Sof(H13D)+Sof(C14)+Sof(H14A)+Sof(H14B)+Sof(C15)+Sof(H15A)+Sof(H15B)+Sof(C16)+
 Sof(H16A)+Sof(H16B)+Sof(H16C)+Sof(C14')+Sof(H14C)+Sof(H14D)+Sof(C15')+
 Sof(H15C)+Sof(H15D)+Sof(C16')+Sof(H16D)+Sof(H16E)+Sof(H16F)]=1 with esd of
 0.0001
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(2)
 Sof(C25")=Sof(H25G)=Sof(H25H)=Sof(H25I)=FVAR(3)
 Sof(N2')=Sof(O22')=Sof(O23')=1-FVAR(4)
 Sof(N2)=Sof(O22)=Sof(O23)=FVAR(4)
 Sof(H13C)=Sof(H13D)=Sof(C14')=Sof(H14C)=Sof(H14D)=Sof(C15')=Sof(H15C)=
 Sof(H15D)=Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(5)
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(5)
 Sof(H18C)=Sof(H18D)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(6)
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(6)
 Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22C)=Sof(H22D)=Sof(C23')=Sof(H23C)=
 Sof(H23D)=Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(7)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(7)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C13(H13C,H13D),
 C14(H14A,H14B), C15(H15A,H15B), C14'(H14C,H14D), C15'(H15C,H15D), C17(H17A,
 H17B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B), C19'(H19C,H19D),
 C21(H21A,H21B), C21(H21C,H21D), C22(H22A,H22B), C23(H23A,H23B), C22'(H22C,
 H22D), C23'(H23C,H23D)
7.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C25'(H25D,H25E,H25F), C25"(H25G,H25H,H25I), C12(H12A,
 H12B,H12C), C16(H16A,H16B,H16C), C16'(H16D,H16E,H16F), C20(H20A,H20B,H20C),
 C20'(H20D,H20E,H20F), C24(H24A,H24B,H24C), C24'(H24D,H24E,H24F)
;
_olex2_submission_original_sample_id mataf22
_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 3.942
_oxdiff_exptl_absorpt_empirical_full_min 0.556
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.62282(6) 0.64375(5) 0.52002(6) 0.0372(2) Uani 1 1 d . . . . .
V2 V 0.60444(5) 0.73849(5) 0.35657(4) 0.02450(19) Uani 1 1 d . . . . .
V3 V 0.48522(5) 0.79729(4) 0.49149(4) 0.01821(16) Uani 1 1 d . . . . .
V4 V 0.67468(5) 0.79373(4) 0.60696(4) 0.01488(15) Uani 1 1 d . . . . .
V5 V 0.79353(5) 0.73325(5) 0.47294(4) 0.02298(18) Uani 1 1 d . . . . .
V6 V 0.65767(5) 0.88605(4) 0.44236(4) 0.02098(17) Uani 1 1 d . . . . .
O1 O 0.5994(3) 0.5564(2) 0.5386(3) 0.0614(15) Uani 1 1 d . . . . .
O2 O 0.5661(3) 0.7121(3) 0.2700(2) 0.0453(11) Uani 1 1 d . . . . .
O3 O 0.3716(2) 0.8125(2) 0.4896(2) 0.0302(7) Uani 1 1 d . . . . .
O4 O 0.7134(2) 0.8201(2) 0.69419(17) 0.0277(7) Uani 1 1 d . . . . .
O5 O 0.9076(2) 0.7189(3) 0.4756(2) 0.0442(11) Uani 1 1 d . . . . .
O6 O 0.6822(3) 0.9742(2) 0.4268(2) 0.0423(10) Uani 1 1 d . . . . .
O7 O 0.5827(2) 0.63661(19) 0.4058(2) 0.0311(8) Uani 1 1 d . . . . .
O8 O 0.4852(2) 0.68490(17) 0.51233(17) 0.0224(6) Uani 1 1 d . . . . .
O9 O 0.6524(2) 0.69057(18) 0.61410(18) 0.0251(7) Uani 1 1 d D U . . .
O10 O 0.7513(2) 0.6388(2) 0.5076(2) 0.0370(9) Uani 1 1 d D U . . .
O11 O 0.4721(2) 0.76190(17) 0.38143(15) 0.0179(6) Uani 1 1 d . . . . .
O12 O 0.5421(2) 0.81614(19) 0.58948(16) 0.0225(6) Uani 1 1 d . . . . .
O13 O 0.80659(19) 0.77076(16) 0.58199(15) 0.0163(5) Uani 1 1 d . . . . .
O14 O 0.7363(2) 0.7161(3) 0.3750(2) 0.0399(10) Uani 1 1 d . . . . .
O15 O 0.6259(2) 0.8420(2) 0.34897(17) 0.0356(9) Uani 1 1 d . . . . .
O16 O 0.5272(2) 0.89203(17) 0.45550(19) 0.0263(7) Uani 1 1 d D . . . .
O17 O 0.6957(2) 0.89531(16) 0.55800(16) 0.0191(6) Uani 1 1 d . . . . .
O18 O 0.7941(2) 0.8460(2) 0.45114(16) 0.0270(7) Uani 1 1 d . . . . .
O19 O 0.63938(19) 0.76590(16) 0.48204(15) 0.0146(5) Uani 1 1 d . . . . .
C1 C 0.4975(4) 0.5928(3) 0.3729(4) 0.0379(13) Uani 1 1 d . . . . .
H1A H 0.501781 0.541312 0.394890 0.046 Uiso 1 1 calc R U . . .
H1B H 0.493932 0.588079 0.317868 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4042(3) 0.6387(3) 0.4753(3) 0.0281(10) Uani 1 1 d . . . . .
H2A H 0.342949 0.661720 0.483052 0.034 Uiso 1 1 calc R U . . .
H2B H 0.408787 0.587361 0.497692 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3915(3) 0.7135(2) 0.3513(2) 0.0199(8) Uani 1 1 d . . . . .
H3A H 0.386464 0.708486 0.296116 0.024 Uiso 1 1 calc R U . . .
H3B H 0.331100 0.736437 0.361062 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4056(3) 0.6332(3) 0.3892(3) 0.0268(10) Uani 1 1 d . . . . .
N1 N 0.3169(3) 0.5866(2) 0.3517(3) 0.0351(10) Uani 1 1 d . . . . .
O20 O 0.3257(3) 0.5431(2) 0.2990(2) 0.0443(10) Uani 1 1 d . . . . .
O21 O 0.2404(3) 0.5970(3) 0.3742(3) 0.0549(12) Uani 1 1 d . . . . .
C5 C 0.7798(3) 0.9403(3) 0.5896(3) 0.0269(10) Uani 1 1 d . . . . .
H5A H 0.783744 0.946127 0.644643 0.032 Uiso 1 1 calc R U . . .
H5B H 0.774845 0.991257 0.566524 0.032 Uiso 1 1 calc R U . . .
C6 C 0.8740(3) 0.8936(3) 0.4870(3) 0.0319(11) Uani 1 1 d . . . . .
H6A H 0.867992 0.944716 0.464288 0.038 Uiso 1 1 calc R U . . .
H6B H 0.935767 0.871378 0.479348 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8873(3) 0.8199(3) 0.6129(2) 0.0208(8) Uani 1 1 d . . . . .
H7A H 0.948239 0.797175 0.604140 0.025 Uiso 1 1 calc R U . . .
H7B H 0.891117 0.825821 0.667849 0.025 Uiso 1 1 calc R U . . .
C8 C 0.8722(3) 0.8990(3) 0.5734(3) 0.0257(9) Uani 1 1 d D . . . .
N2 N 0.9556(4) 0.9530(3) 0.6076(3) 0.0362(15) Uani 0.766(8) 1 d D U P A 1
O22 O 0.9580(4) 1.0177(3) 0.5816(3) 0.0407(14) Uani 0.766(8) 1 d D . P A 1
O23 O 1.0129(5) 0.9322(4) 0.6638(4) 0.068(2) Uani 0.766(8) 1 d D U P A 1
N2' N 0.9672(10) 0.9388(16) 0.6121(14) 0.054(3) Uani 0.234(8) 1 d D U P A 2
O22' O 0.9643(14) 0.9625(14) 0.6766(11) 0.059(4) Uani 0.234(8) 1 d D U P A 2
O23' O 1.0447(11) 0.9161(12) 0.5970(11) 0.054(4) Uani 0.234(8) 1 d D U P A 2
C25 C 0.4869(10) 0.9611(5) 0.4855(6) 0.046(3) Uani 0.550(3) 1 d D . P B 1
H25A H 0.417166 0.955446 0.480982 0.068 Uiso 0.550(3) 1 calc R U P B 1
H25B H 0.500696 1.005340 0.456555 0.068 Uiso 0.550(3) 1 calc R U P B 1
H25C H 0.516360 0.967844 0.538548 0.068 Uiso 0.550(3) 1 calc R U P B 1
C25' C 0.7829(13) 0.5633(8) 0.4936(12) 0.036(2) Uani 0.280(3) 1 d D U P C 2
H25D H 0.758183 0.549437 0.441054 0.054 Uiso 0.280(3) 1 calc R U P C 2
H25E H 0.758704 0.527474 0.527075 0.054 Uiso 0.280(3) 1 calc R U P C 2
H25F H 0.853389 0.561670 0.503104 0.054 Uiso 0.280(3) 1 calc R U P C 2
C25" C 0.609(2) 0.6440(15) 0.6656(14) 0.029(4) Uani 0.170(2) 1 d D U P D 3
H25G H 0.599921 0.592360 0.645914 0.044 Uiso 0.170(2) 1 calc R U P D 3
H25H H 0.546126 0.665366 0.670269 0.044 Uiso 0.170(2) 1 calc R U P D 3
H25I H 0.650771 0.643234 0.715210 0.044 Uiso 0.170(2) 1 calc R U P D 3
N3 N 0.8976(3) 0.6065(2) 0.2484(2) 0.0194(7) Uani 1 1 d . . . . .
C9 C 0.9702(3) 0.5525(3) 0.2206(2) 0.0224(9) Uani 1 1 d . . . . .
H9A H 0.934809 0.522718 0.177922 0.027 Uiso 1 1 calc R U . . .
H9B H 1.018011 0.583817 0.200874 0.027 Uiso 1 1 calc R U . . .
C10 C 1.0253(3) 0.4965(3) 0.2792(3) 0.0263(9) Uani 1 1 d . . . . .
H10A H 0.979161 0.463930 0.299397 0.032 Uiso 1 1 calc R U . . .
H10B H 1.063657 0.524946 0.321611 0.032 Uiso 1 1 calc R U . . .
C11 C 1.0933(3) 0.4466(3) 0.2403(3) 0.0287(10) Uani 1 1 d . . . . .
H11A H 1.056225 0.425252 0.193049 0.034 Uiso 1 1 calc R U . . .
H11B H 1.145146 0.478663 0.227014 0.034 Uiso 1 1 calc R U . . .
C12 C 1.1381(5) 0.3818(4) 0.2918(4) 0.0542(17) Uani 1 1 d . . . . .
H12A H 1.170837 0.402631 0.340015 0.081 Uiso 1 1 calc R U . . .
H12B H 1.184654 0.354590 0.267670 0.081 Uiso 1 1 calc R U . . .
H12C H 1.087434 0.346942 0.300452 0.081 Uiso 1 1 calc R U . . .
C13 C 0.9496(3) 0.6635(3) 0.3080(2) 0.0239(9) Uani 1 1 d D . . . .
H13A H 0.985696 0.634723 0.351140 0.029 Uiso 0.830(2) 1 calc R U P E 1
H13B H 0.900413 0.694119 0.326956 0.029 Uiso 0.830(2) 1 calc R U P E 1
H13C H 0.898003 0.694541 0.323135 0.029 Uiso 0.170(2) 1 calc R U P E 2
H13D H 0.977039 0.632753 0.352614 0.029 Uiso 0.170(2) 1 calc R U P E 2
C14 C 1.0207(7) 0.7183(6) 0.2778(4) 0.0244(15) Uani 0.830(2) 1 d D U P E 1
H14A H 1.070742 0.688563 0.259063 0.029 Uiso 0.830(2) 1 calc R U P E 1
H14B H 0.985336 0.748446 0.235364 0.029 Uiso 0.830(2) 1 calc R U P E 1
C15 C 1.0691(5) 0.7724(4) 0.3422(4) 0.0284(13) Uani 0.830(2) 1 d D U P E 1
H15A H 1.018051 0.799310 0.362535 0.034 Uiso 0.830(2) 1 calc R U P E 1
H15B H 1.105894 0.741578 0.383427 0.034 Uiso 0.830(2) 1 calc R U P E 1
C16 C 1.1371(4) 0.8313(4) 0.3173(4) 0.0317(13) Uani 0.830(2) 1 d D U P E 1
H16A H 1.185028 0.805476 0.293534 0.048 Uiso 0.830(2) 1 calc R U P E 1
H16B H 1.169642 0.859561 0.361371 0.048 Uiso 0.830(2) 1 calc R U P E 1
H16C H 1.099822 0.866342 0.281183 0.048 Uiso 0.830(2) 1 calc R U P E 1
C14' C 1.030(4) 0.720(3) 0.297(2) 0.027(5) Uani 0.170(2) 1 d D U P E 2
H14C H 1.003416 0.759221 0.259584 0.033 Uiso 0.170(2) 1 calc R U P E 2
H14D H 1.082274 0.693242 0.278580 0.033 Uiso 0.170(2) 1 calc R U P E 2
C15' C 1.069(3) 0.7579(19) 0.3748(18) 0.036(5) Uani 0.170(2) 1 d D U P E 2
H15C H 1.014404 0.775998 0.397204 0.044 Uiso 0.170(2) 1 calc R U P E 2
H15D H 1.104771 0.719817 0.409225 0.044 Uiso 0.170(2) 1 calc R U P E 2
C16' C 1.136(2) 0.8249(18) 0.367(2) 0.045(6) Uani 0.170(2) 1 d D U P E 2
H16D H 1.199108 0.805772 0.360698 0.067 Uiso 0.170(2) 1 calc R U P E 2
H16E H 1.143425 0.856478 0.412244 0.067 Uiso 0.170(2) 1 calc R U P E 2
H16F H 1.108232 0.855232 0.322826 0.067 Uiso 0.170(2) 1 calc R U P E 2
C17 C 0.8435(3) 0.6475(3) 0.1774(2) 0.0230(9) Uani 1 1 d . . . . .
H17A H 0.890598 0.677535 0.155499 0.028 Uiso 1 1 calc R U . . .
H17B H 0.816343 0.608825 0.139815 0.028 Uiso 1 1 calc R U . . .
C18 C 0.7616(4) 0.7004(3) 0.1902(3) 0.0297(10) Uani 1 1 d D . . . .
H18A H 0.788442 0.741330 0.225291 0.036 Uiso 0.574(14) 1 calc R U P F 1
H18B H 0.715069 0.671499 0.213789 0.036 Uiso 0.574(14) 1 calc R U P F 1
H18C H 0.784468 0.733706 0.233904 0.036 Uiso 0.426(14) 1 calc R U P F 2
H18D H 0.707142 0.670026 0.201337 0.036 Uiso 0.426(14) 1 calc R U P F 2
C19 C 0.7086(15) 0.7358(17) 0.1156(12) 0.048(4) Uani 0.574(14) 1 d D U P F 1
H19A H 0.659437 0.771428 0.127373 0.057 Uiso 0.574(14) 1 calc R U P F 1
H19B H 0.755547 0.765574 0.093183 0.057 Uiso 0.574(14) 1 calc R U P F 1
C20 C 0.6593(7) 0.6791(8) 0.0567(6) 0.051(3) Uani 0.574(14) 1 d D . P F 1
H20A H 0.707571 0.655587 0.031489 0.076 Uiso 0.574(14) 1 calc R U P F 1
H20B H 0.611645 0.705582 0.019376 0.076 Uiso 0.574(14) 1 calc R U P F 1
H20C H 0.627279 0.639988 0.081508 0.076 Uiso 0.574(14) 1 calc R U P F 1
C19' C 0.727(2) 0.749(2) 0.1189(16) 0.046(5) Uani 0.426(14) 1 d D U P F 2
H19C H 0.782486 0.779799 0.108717 0.055 Uiso 0.426(14) 1 calc R U P F 2
H19D H 0.707353 0.715363 0.075264 0.055 Uiso 0.426(14) 1 calc R U P F 2
C20' C 0.6435(10) 0.8033(8) 0.1252(10) 0.047(4) Uani 0.426(14) 1 d D . P F 2
H20D H 0.586323 0.773510 0.129681 0.071 Uiso 0.426(14) 1 calc R U P F 2
H20E H 0.629472 0.835163 0.080171 0.071 Uiso 0.426(14) 1 calc R U P F 2
H20F H 0.661255 0.835313 0.169904 0.071 Uiso 0.426(14) 1 calc R U P F 2
C21 C 0.8277(3) 0.5628(3) 0.2896(3) 0.0232(9) Uani 1 1 d D . . . .
H21A H 0.783545 0.599452 0.307067 0.028 Uiso 0.77(4) 1 calc R U P G 1
H21B H 0.865206 0.537820 0.334659 0.028 Uiso 0.77(4) 1 calc R U P G 1
H21C H 0.868370 0.540050 0.334547 0.028 Uiso 0.23(4) 1 calc R U P G 2
H21D H 0.788305 0.602024 0.308756 0.028 Uiso 0.23(4) 1 calc R U P G 2
C22 C 0.7667(9) 0.5017(7) 0.2394(7) 0.0235(17) Uani 0.77(4) 1 d D U P G 1
H22A H 0.809501 0.463769 0.222407 0.028 Uiso 0.77(4) 1 calc R U P G 1
H22B H 0.727641 0.525758 0.194455 0.028 Uiso 0.77(4) 1 calc R U P G 1
C23 C 0.6994(8) 0.4625(7) 0.2878(9) 0.041(3) Uani 0.77(4) 1 d D U P G 1
H23A H 0.739310 0.439811 0.333188 0.049 Uiso 0.77(4) 1 calc R U P G 1
H23B H 0.657388 0.501174 0.304781 0.049 Uiso 0.77(4) 1 calc R U P G 1
C24 C 0.6370(8) 0.4011(6) 0.2438(11) 0.051(4) Uani 0.77(4) 1 d D U P G 1
H24A H 0.585037 0.424714 0.207923 0.077 Uiso 0.77(4) 1 calc R U P G 1
H24B H 0.609550 0.369190 0.278850 0.077 Uiso 0.77(4) 1 calc R U P G 1
H24C H 0.676520 0.369984 0.216472 0.077 Uiso 0.77(4) 1 calc R U P G 1
C22' C 0.756(3) 0.500(2) 0.256(2) 0.024(4) Uani 0.23(4) 1 d D U P G 2
H22C H 0.792178 0.456553 0.240554 0.029 Uiso 0.23(4) 1 calc R U P G 2
H22D H 0.712955 0.519595 0.210591 0.029 Uiso 0.23(4) 1 calc R U P G 2
C23' C 0.694(3) 0.473(2) 0.314(3) 0.042(5) Uani 0.23(4) 1 d D U P G 2
H23C H 0.736678 0.448721 0.357911 0.050 Uiso 0.23(4) 1 calc R U P G 2
H23D H 0.662412 0.516643 0.333251 0.050 Uiso 0.23(4) 1 calc R U P G 2
C24' C 0.618(3) 0.416(3) 0.278(4) 0.058(8) Uani 0.23(4) 1 d D U P G 2
H24D H 0.568040 0.442342 0.243142 0.087 Uiso 0.23(4) 1 calc R U P G 2
H24E H 0.590127 0.390892 0.317220 0.087 Uiso 0.23(4) 1 calc R U P G 2
H24F H 0.648568 0.377806 0.250417 0.087 Uiso 0.23(4) 1 calc R U P G 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
O1 V1 O7 96.9(2) . . ?
O1 V1 O8 97.04(19) . . ?
O1 V1 O9 104.6(2) . . ?
O1 V1 O10 102.7(2) . . ?
O1 V1 O19 172.85(16) . . ?
O7 V1 O8 82.54(13) . . ?
O7 V1 O19 77.30(12) . . ?
O8 V1 O19 78.15(11) . . ?
O9 V1 O7 157.19(14) . . ?
O9 V1 O8 87.46(14) . . ?
O9 V1 O10 93.99(15) . . ?
O9 V1 O19 80.61(12) . . ?
O10 V1 O7 88.36(16) . . ?
O10 V1 O8 159.13(16) . . ?
O10 V1 O19 81.55(14) . . ?
O2 V2 O7 96.6(2) . . ?
O2 V2 O11 96.43(15) . . ?
O2 V2 O14 104.77(17) . . ?
O2 V2 O15 103.9(2) . . ?
O2 V2 O19 171.58(16) . . ?
O7 V2 O19 77.18(12) . . ?
O11 V2 O7 82.32(13) . . ?
O11 V2 O19 77.21(10) . . ?
O14 V2 O7 87.79(17) . . ?
O14 V2 O11 157.51(14) . . ?
O14 V2 O19 80.93(12) . . ?
O15 V2 O7 158.53(14) . . ?
O15 V2 O11 89.18(14) . . ?
O15 V2 O14 92.88(18) . . ?
O15 V2 O19 81.73(12) . . ?
O3 V3 O8 97.62(16) . . ?
O3 V3 O11 96.69(15) . . ?
O3 V3 O12 104.32(16) . . ?
O3 V3 O16 102.32(17) . . ?
O3 V3 O19 172.94(14) . . ?
O8 V3 O11 83.01(12) . . ?
O8 V3 O19 78.97(11) . . ?
O11 V3 O19 76.83(11) . . ?
O12 V3 O8 90.80(14) . . ?
O12 V3 O11 158.73(13) . . ?
O12 V3 O16 93.44(15) . . ?
O12 V3 O19 82.02(12) . . ?
O16 V3 O8 157.87(14) . . ?
O16 V3 O11 85.24(13) . . ?
O16 V3 O19 80.13(12) . . ?
O4 V4 O9 104.09(17) . . ?
O4 V4 O12 104.34(15) . . ?
O4 V4 O13 96.41(14) . . ?
O4 V4 O17 96.69(16) . . ?
O4 V4 O19 171.86(13) . . ?
O9 V4 O12 92.39(14) . . ?
O9 V4 O13 89.63(13) . . ?
O9 V4 O17 158.46(13) . . ?
O9 V4 O19 81.23(12) . . ?
O12 V4 O13 157.97(12) . . ?
O12 V4 O17 87.87(13) . . ?
O12 V4 O19 81.34(11) . . ?
O13 V4 O17 82.37(12) . . ?
O13 V4 O19 77.29(10) . . ?
O17 V4 O19 77.51(11) . . ?
O5 V5 O10 102.8(2) . . ?
O5 V5 O13 96.22(15) . . ?
O5 V5 O14 105.24(17) . . ?
O5 V5 O18 96.9(2) . . ?
O5 V5 O19 171.97(15) . . ?
O10 V5 O13 86.90(14) . . ?
O10 V5 O18 158.48(14) . . ?
O10 V5 O19 80.67(12) . . ?
O13 V5 O19 76.61(10) . . ?
O14 V5 O10 93.59(18) . . ?
O14 V5 O13 157.83(14) . . ?
O14 V5 O18 89.54(17) . . ?
O14 V5 O19 81.59(13) . . ?
O18 V5 O13 82.33(12) . . ?
O18 V5 O19 78.73(11) . . ?
O6 V6 O15 105.66(19) . . ?
O6 V6 O16 102.11(19) . . ?
O6 V6 O17 94.26(17) . . ?
O6 V6 O18 96.72(18) . . ?
O6 V6 O19 170.85(15) . . ?
O15 V6 O16 93.39(15) . . ?
O15 V6 O17 159.49(15) . . ?
O15 V6 O18 89.56(15) . . ?
O15 V6 O19 82.60(14) . . ?
O16 V6 O17 87.00(13) . . ?
O16 V6 O18 159.37(14) . . ?
O16 V6 O19 80.99(12) . . ?
O17 V6 O19 77.21(11) . . ?
O18 V6 O17 83.22(12) . . ?
O18 V6 O19 79.15(12) . . ?
V1 O7 V2 110.34(14) . . ?
C1 O7 V1 119.9(4) . . ?
C1 O7 V2 117.7(3) . . ?
V3 O8 V1 109.07(13) . . ?
C2 O8 V1 119.0(3) . . ?
C2 O8 V3 119.4(3) . . ?
V4 O9 V1 112.58(15) . . ?
C25" O9 V1 106.3(12) . . ?
C25" O9 V4 133.9(13) . . ?
V1 O10 V5 111.47(17) . . ?
C25' O10 V1 113.7(8) . . ?
C25' O10 V5 128.5(9) . . ?
V2 O11 V3 110.45(13) . . ?
C3 O11 V2 119.1(3) . . ?
C3 O11 V3 117.8(2) . . ?
V3 O12 V4 111.68(15) . . ?
V4 O13 V5 110.61(12) . . ?
C7 O13 V4 118.7(2) . . ?
C7 O13 V5 118.9(2) . . ?
V5 O14 V2 112.62(17) . . ?
V6 O15 V2 111.32(17) . . ?
V6 O16 V3 111.02(15) . . ?
C25 O16 V3 115.3(5) . . ?
C25 O16 V6 122.3(6) . . ?
V4 O17 V6 109.62(13) . . ?
C5 O17 V4 118.8(3) . . ?
C5 O17 V6 118.8(3) . . ?
V5 O18 V6 108.59(14) . . ?
C6 O18 V5 120.6(3) . . ?
C6 O18 V6 118.7(3) . . ?
V1 O19 V5 86.29(10) . . ?
V2 O19 V1 94.71(11) . . ?
V2 O19 V3 95.20(10) . . ?
V2 O19 V5 84.84(9) . . ?
V3 O19 V1 93.14(10) . . ?
V3 O19 V5 179.43(15) . . ?
V4 O19 V1 85.55(10) . . ?
V4 O19 V2 179.71(15) . . ?
V4 O19 V3 84.92(9) . . ?
V4 O19 V5 95.04(10) . . ?
V6 O19 V1 178.70(14) . . ?
V6 O19 V2 84.34(9) . . ?
V6 O19 V3 87.84(10) . . ?
V6 O19 V4 95.39(11) . . ?
V6 O19 V5 92.73(10) . . ?
O7 C1 H1A 109.8 . . ?
O7 C1 H1B 109.8 . . ?
O7 C1 C4 109.5(4) . . ?
H1A C1 H1B 108.2 . . ?
C4 C1 H1A 109.8 . . ?
C4 C1 H1B 109.8 . . ?
O8 C2 H2A 109.7 . . ?
O8 C2 H2B 109.7 . . ?
O8 C2 C4 109.6(4) . . ?
H2A C2 H2B 108.2 . . ?
C4 C2 H2A 109.7 . . ?
C4 C2 H2B 109.7 . . ?
O11 C3 H3A 109.7 . . ?
O11 C3 H3B 109.7 . . ?
O11 C3 C4 109.9(3) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C1 C4 C2 112.3(4) . . ?
C1 C4 C3 112.1(4) . . ?
C2 C4 C3 110.7(4) . . ?
N1 C4 C1 108.1(4) . . ?
N1 C4 C2 108.1(4) . . ?
N1 C4 C3 105.2(3) . . ?
O20 N1 C4 118.3(4) . . ?
O21 N1 C4 117.6(4) . . ?
O21 N1 O20 124.0(4) . . ?
O17 C5 H5A 109.9 . . ?
O17 C5 H5B 109.9 . . ?
O17 C5 C8 108.7(4) . . ?
H5A C5 H5B 108.3 . . ?
C8 C5 H5A 109.9 . . ?
C8 C5 H5B 109.9 . . ?
O18 C6 H6A 109.9 . . ?
O18 C6 H6B 109.9 . . ?
O18 C6 C8 108.9(3) . . ?
H6A C6 H6B 108.3 . . ?
C8 C6 H6A 109.9 . . ?
C8 C6 H6B 109.9 . . ?
O13 C7 H7A 109.9 . . ?
O13 C7 H7B 109.9 . . ?
O13 C7 C8 109.0(3) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
C6 C8 C5 112.4(4) . . ?
C7 C8 C5 112.2(4) . . ?
C7 C8 C6 111.8(4) . . ?
N2 C8 C5 103.8(4) . . ?
N2 C8 C6 106.4(4) . . ?
N2 C8 C7 109.7(4) . . ?
N2' C8 C5 112.6(9) . . ?
N2' C8 C6 107.5(10) . . ?
N2' C8 C7 99.5(13) . . ?
O22 N2 C8 119.2(5) . . ?
O23 N2 C8 118.6(5) . . ?
O23 N2 O22 121.9(6) . . ?
O22' N2' C8 113.3(15) . . ?
O23' N2' C8 118.5(14) . . ?
O23' N2' O22' 119.7(17) . . ?
O16 C25 H25A 109.5 . . ?
O16 C25 H25B 109.5 . . ?
O16 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C25' H25D 109.5 . . ?
O10 C25' H25E 109.5 . . ?
O10 C25' H25F 109.5 . . ?
H25D C25' H25E 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
O9 C25" H25G 109.5 . . ?
O9 C25" H25H 109.5 . . ?
O9 C25" H25I 109.5 . . ?
H25G C25" H25H 109.5 . . ?
H25G C25" H25I 109.5 . . ?
H25H C25" H25I 109.5 . . ?
C9 N3 C13 111.5(3) . . ?
C17 N3 C9 106.0(3) . . ?
C17 N3 C13 111.6(3) . . ?
C17 N3 C21 111.6(3) . . ?
C21 N3 C9 111.6(3) . . ?
C21 N3 C13 104.6(3) . . ?
N3 C9 H9A 108.1 . . ?
N3 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C10 C9 N3 116.9(3) . . ?
C10 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C9 C10 C11 109.1(4) . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.6(4) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 108.7 . . ?
N3 C13 H13B 108.7 . . ?
N3 C13 H13C 105.7 . . ?
N3 C13 H13D 105.7 . . ?
N3 C13 C14 114.3(4) . . ?
H13A C13 H13B 107.6 . . ?
H13C C13 H13D 106.2 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C14' C13 N3 126.3(12) . . ?
C14' C13 H13C 105.7 . . ?
C14' C13 H13D 105.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 C13 109.9(5) . . ?
C15 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C14 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 C14 114.1(5) . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
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 . . ?
C13 C14' H14C 110.1 . . ?
C13 C14' H14D 110.1 . . ?
C13 C14' C15' 108.0(19) . . ?
H14C C14' H14D 108.4 . . ?
C15' C14' H14C 110.1 . . ?
C15' C14' H14D 110.1 . . ?
C14' C15' H15C 109.3 . . ?
C14' C15' H15D 109.3 . . ?
H15C C15' H15D 107.9 . . ?
C16' C15' C14' 112(2) . . ?
C16' C15' H15C 109.3 . . ?
C16' C15' H15D 109.3 . . ?
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 . . ?
N3 C17 H17A 108.4 . . ?
N3 C17 H17B 108.4 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N3 115.6(3) . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
C17 C18 H18C 109.7 . . ?
C17 C18 H18D 109.7 . . ?
C17 C18 C19 111.9(13) . . ?
C17 C18 C19' 110.0(16) . . ?
H18A C18 H18B 107.9 . . ?
H18C C18 H18D 108.2 . . ?
C19 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C19' C18 H18C 109.7 . . ?
C19' C18 H18D 109.7 . . ?
C18 C19 H19A 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 C18 115.2(18) . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
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 . . ?
C18 C19' H19C 108.7 . . ?
C18 C19' H19D 108.7 . . ?
H19C C19' H19D 107.6 . . ?
C20' C19' C18 114(2) . . ?
C20' C19' H19C 108.7 . . ?
C20' C19' H19D 108.7 . . ?
C19' C20' H20D 109.5 . . ?
C19' C20' H20E 109.5 . . ?
C19' C20' H20F 109.5 . . ?
H20D C20' H20E 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
N3 C21 H21A 108.9 . . ?
N3 C21 H21B 108.9 . . ?
N3 C21 H21C 105.6 . . ?
N3 C21 H21D 105.6 . . ?
N3 C21 C22 113.5(6) . . ?
H21A C21 H21B 107.7 . . ?
H21C C21 H21D 106.1 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C22' C21 N3 126.7(15) . . ?
C22' C21 H21C 105.6 . . ?
C22' C21 H21D 105.6 . . ?
C21 C22 H22A 110.1 . . ?
C21 C22 H22B 110.1 . . ?
C21 C22 C23 108.0(6) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.1 . . ?
C23 C22 H22B 110.1 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 C22 112.1(8) . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22' H22C 109.4 . . ?
C21 C22' H22D 109.4 . . ?
C21 C22' C23' 111(2) . . ?
H22C C22' H22D 108.0 . . ?
C23' C22' H22C 109.4 . . ?
C23' C22' H22D 109.4 . . ?
C22' C23' H23C 109.6 . . ?
C22' C23' H23D 109.6 . . ?
H23C C23' H23D 108.1 . . ?
C24' C23' C22' 110(2) . . ?
C24' C23' H23C 109.6 . . ?
C24' C23' H23D 109.6 . . ?
C23' C24' H24D 109.5 . . ?
C23' C24' H24E 109.5 . . ?
C23' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 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 1.594(4) . ?
V1 O7 1.998(4) . ?
V1 O8 2.017(3) . ?
V1 O9 1.829(3) . ?
V1 O10 1.836(4) . ?
V1 O19 2.244(3) . ?
V2 O2 1.594(3) . ?
V2 O7 2.015(4) . ?
V2 O11 2.005(3) . ?
V2 O14 1.838(3) . ?
V2 O15 1.826(4) . ?
V2 O19 2.235(3) . ?
V3 O3 1.591(3) . ?
V3 O8 1.981(3) . ?
V3 O11 2.018(3) . ?
V3 O12 1.798(3) . ?
V3 O16 1.889(3) . ?
V3 O19 2.240(3) . ?
V4 O4 1.604(3) . ?
V4 O9 1.821(3) . ?
V4 O12 1.847(3) . ?
V4 O13 1.998(3) . ?
V4 O17 2.005(3) . ?
V4 O19 2.227(3) . ?
V5 O5 1.593(3) . ?
V5 O10 1.877(4) . ?
V5 O13 2.012(3) . ?
V5 O14 1.793(3) . ?
V5 O18 1.990(4) . ?
V5 O19 2.244(3) . ?
V6 O6 1.599(4) . ?
V6 O15 1.799(3) . ?
V6 O16 1.869(3) . ?
V6 O17 2.023(3) . ?
V6 O18 1.993(3) . ?
V6 O19 2.225(3) . ?
O7 C1 1.434(5) . ?
O8 C2 1.434(5) . ?
O9 C25" 1.432(11) . ?
O10 C25' 1.416(10) . ?
O11 C3 1.419(5) . ?
O13 C7 1.431(5) . ?
O16 C25 1.459(9) . ?
O17 C5 1.427(5) . ?
O18 C6 1.432(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.526(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.532(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.540(6) . ?
C4 N1 1.518(5) . ?
N1 O20 1.221(6) . ?
N1 O21 1.214(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C8 1.538(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C8 1.537(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.533(6) . ?
C8 N2 1.523(6) . ?
C8 N2' 1.532(10) . ?
N2 O22 1.212(6) . ?
N2 O23 1.208(6) . ?
N2' O22' 1.220(9) . ?
N2' O23' 1.218(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25' H25D 0.9600 . ?
C25' H25E 0.9600 . ?
C25' H25F 0.9600 . ?
C25" H25G 0.9600 . ?
C25" H25H 0.9600 . ?
C25" H25I 0.9600 . ?
N3 C9 1.519(5) . ?
N3 C13 1.525(5) . ?
N3 C17 1.516(6) . ?
N3 C21 1.518(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.519(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.532(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.506(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C13 C14 1.534(7) . ?
C13 C14' 1.522(18) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.530(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.508(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C14' H14C 0.9700 . ?
C14' H14D 0.9700 . ?
C14' C15' 1.53(2) . ?
C15' H15C 0.9700 . ?
C15' H15D 0.9700 . ?
C15' C16' 1.51(2) . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.507(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 C19 1.516(11) . ?
C18 C19' 1.521(15) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.50(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20' 1.51(4) . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C21 C22 1.532(8) . ?
C21 C22' 1.518(17) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.535(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.496(10) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?
C22' C23' 1.53(2) . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C23' C24' 1.50(2) . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 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 O7 C1 C4 68.5(5) . . . . ?
V1 O8 C2 C4 -68.4(4) . . . . ?
V2 O7 C1 C4 -70.4(5) . . . . ?
V2 O11 C3 C4 68.5(4) . . . . ?
V3 O8 C2 C4 69.3(4) . . . . ?
V3 O11 C3 C4 -69.8(4) . . . . ?
V4 O13 C7 C8 -69.8(4) . . . . ?
V4 O17 C5 C8 69.6(4) . . . . ?
V5 O13 C7 C8 69.8(4) . . . . ?
V5 O18 C6 C8 -68.5(5) . . . . ?
V6 O17 C5 C8 -68.1(4) . . . . ?
V6 O18 C6 C8 69.7(5) . . . . ?
O1 V1 O9 V4 -176.4(2) . . . . ?
O1 V1 O9 C25" -21.8(13) . . . . ?
O1 V1 O10 V5 173.0(2) . . . . ?
O1 V1 O10 C25' 18.4(10) . . . . ?
O2 V2 O14 V5 -174.8(3) . . . . ?
O2 V2 O15 V6 173.83(19) . . . . ?
O3 V3 O12 V4 175.13(19) . . . . ?
O3 V3 O16 V6 -174.05(17) . . . . ?
O3 V3 O16 C25 41.5(6) . . . . ?
O4 V4 O9 V1 -172.35(17) . . . . ?
O4 V4 O9 C25" 42.6(16) . . . . ?
O4 V4 O12 V3 175.75(18) . . . . ?
O5 V5 O10 V1 173.75(19) . . . . ?
O5 V5 O10 C25' -36.4(10) . . . . ?
O5 V5 O14 V2 -174.6(3) . . . . ?
O6 V6 O15 V2 175.8(2) . . . . ?
O6 V6 O16 V3 -170.43(19) . . . . ?
O6 V6 O16 C25 -28.8(6) . . . . ?
O7 V1 O9 V4 -15.9(5) . . . . ?
O7 V1 O9 C25" 138.7(13) . . . . ?
O7 V1 O10 V5 76.27(19) . . . . ?
O7 V1 O10 C25' -78.3(10) . . . . ?
O7 V2 O14 V5 -78.5(2) . . . . ?
O7 V2 O15 V6 11.1(5) . . . . ?
O7 C1 C4 C2 -62.4(6) . . . . ?
O7 C1 C4 C3 62.9(5) . . . . ?
O7 C1 C4 N1 178.5(4) . . . . ?
O8 V1 O9 V4 -79.77(17) . . . . ?
O8 V1 O9 C25" 74.8(13) . . . . ?
O8 V1 O10 V5 12.3(5) . . . . ?
O8 V1 O10 C25' -142.2(10) . . . . ?
O8 V3 O12 V4 77.05(18) . . . . ?
O8 V3 O16 V6 -20.2(4) . . . . ?
O8 V3 O16 C25 -164.7(6) . . . . ?
O8 C2 C4 C1 63.0(5) . . . . ?
O8 C2 C4 C3 -63.2(5) . . . . ?
O8 C2 C4 N1 -177.9(4) . . . . ?
O9 V1 O10 V5 -81.01(19) . . . . ?
O9 V1 O10 C25' 124.4(10) . . . . ?
O9 V4 O12 V3 -79.05(19) . . . . ?
O10 V1 O9 V4 79.4(2) . . . . ?
O10 V1 O9 C25" -126.1(13) . . . . ?
O10 V5 O14 V2 81.1(2) . . . . ?
O11 V2 O14 V5 -14.8(6) . . . . ?
O11 V2 O15 V6 77.41(18) . . . . ?
O11 V3 O12 V4 4.5(5) . . . . ?
O11 V3 O16 V6 -78.23(16) . . . . ?
O11 V3 O16 C25 137.3(6) . . . . ?
O11 C3 C4 C1 -61.7(5) . . . . ?
O11 C3 C4 C2 64.6(4) . . . . ?
O11 C3 C4 N1 -178.9(4) . . . . ?
O12 V3 O16 V6 80.48(17) . . . . ?
O12 V3 O16 C25 -64.0(6) . . . . ?
O12 V4 O9 V1 82.23(18) . . . . ?
O12 V4 O9 C25" -62.9(16) . . . . ?
O13 V4 O9 V1 -75.83(17) . . . . ?
O13 V4 O9 C25" 139.1(16) . . . . ?
O13 V4 O12 V3 15.9(5) . . . . ?
O13 V5 O10 V1 78.07(19) . . . . ?
O13 V5 O10 C25' -132.1(10) . . . . ?
O13 V5 O14 V2 -9.5(6) . . . . ?
O13 C7 C8 C5 63.2(4) . . . . ?
O13 C7 C8 C6 -64.2(4) . . . . ?
O13 C7 C8 N2 178.0(4) . . . . ?
O13 C7 C8 N2' -177.5(8) . . . . ?
O14 V2 O15 V6 -80.2(2) . . . . ?
O14 V5 O10 V1 -79.7(2) . . . . ?
O14 V5 O10 C25' 70.1(10) . . . . ?
O15 V2 O14 V5 80.0(2) . . . . ?
O15 V6 O16 V3 82.75(19) . . . . ?
O15 V6 O16 C25 -135.7(5) . . . . ?
O16 V3 O12 V4 -81.22(18) . . . . ?
O16 V6 O15 V2 -80.67(19) . . . . ?
O17 V4 O9 V1 -8.0(5) . . . . ?
O17 V4 O9 C25" -153.1(16) . . . . ?
O17 V4 O12 V3 79.39(18) . . . . ?
O17 V6 O15 V2 9.8(5) . . . . ?
O17 V6 O16 V3 -76.71(17) . . . . ?
O17 V6 O16 C25 64.9(5) . . . . ?
O17 C5 C8 C6 64.0(5) . . . . ?
O17 C5 C8 C7 -63.1(5) . . . . ?
O17 C5 C8 N2 178.5(4) . . . . ?
O17 C5 C8 N2' -174.4(13) . . . . ?
O18 V5 O10 V1 18.2(5) . . . . ?
O18 V5 O10 C25' 168.0(10) . . . . ?
O18 V5 O14 V2 -77.5(2) . . . . ?
O18 V6 O15 V2 78.90(19) . . . . ?
O18 V6 O16 V3 -15.0(5) . . . . ?
O18 V6 O16 C25 126.5(6) . . . . ?
O18 C6 C8 C5 -64.6(5) . . . . ?
O18 C6 C8 C7 62.7(5) . . . . ?
O18 C6 C8 N2 -177.5(4) . . . . ?
O18 C6 C8 N2' 170.9(12) . . . . ?
O19 V1 O9 V4 -1.36(15) . . . . ?
O19 V1 O9 C25" 153.2(13) . . . . ?
O19 V1 O10 V5 -1.13(17) . . . . ?
O19 V1 O10 C25' -155.7(10) . . . . ?
O19 V2 O14 V5 -1.1(2) . . . . ?
O19 V2 O15 V6 0.22(17) . . . . ?
O19 V3 O12 V4 -1.69(16) . . . . ?
O19 V3 O16 V6 -0.80(15) . . . . ?
O19 V3 O16 C25 -145.3(6) . . . . ?
O19 V4 O9 V1 1.37(15) . . . . ?
O19 V4 O9 C25" -143.7(16) . . . . ?
O19 V4 O12 V3 1.70(16) . . . . ?
O19 V5 O10 V1 1.14(17) . . . . ?
O19 V5 O10 C25' 151.0(10) . . . . ?
O19 V5 O14 V2 1.1(2) . . . . ?
O19 V6 O15 V2 -0.22(17) . . . . ?
O19 V6 O16 V3 0.80(15) . . . . ?
O19 V6 O16 C25 142.4(5) . . . . ?
C1 C4 N1 O20 -21.6(6) . . . . ?
C1 C4 N1 O21 161.0(5) . . . . ?
C2 C4 N1 O20 -143.4(5) . . . . ?
C2 C4 N1 O21 39.2(6) . . . . ?
C3 C4 N1 O20 98.3(5) . . . . ?
C3 C4 N1 O21 -79.1(6) . . . . ?
C5 C8 N2 O22 -62.4(7) . . . . ?
C5 C8 N2 O23 111.6(9) . . . . ?
C5 C8 N2' O22' 39(3) . . . . ?
C5 C8 N2' O23' -173(2) . . . . ?
C6 C8 N2 O22 56.3(8) . . . . ?
C6 C8 N2 O23 -129.6(8) . . . . ?
C6 C8 N2' O22' 164(2) . . . . ?
C6 C8 N2' O23' -48(3) . . . . ?
C7 C8 N2 O22 177.5(6) . . . . ?
C7 C8 N2 O23 -8.5(10) . . . . ?
C7 C8 N2' O22' -80(3) . . . . ?
C7 C8 N2' O23' 68(3) . . . . ?
N3 C9 C10 C11 179.2(4) . . . . ?
N3 C13 C14 C15 -179.6(6) . . . . ?
N3 C13 C14' C15' -173(2) . . . . ?
N3 C17 C18 C19 -177.3(11) . . . . ?
N3 C17 C18 C19' 168.8(14) . . . . ?
N3 C21 C22 C23 -179.8(7) . . . . ?
N3 C21 C22' C23' -177(2) . . . . ?
C9 N3 C13 C14 62.7(7) . . . . ?
C9 N3 C13 C14' 57(4) . . . . ?
C9 N3 C17 C18 175.7(4) . . . . ?
C9 N3 C21 C22 -59.5(8) . . . . ?
C9 N3 C21 C22' -61(3) . . . . ?
C9 C10 C11 C12 -171.1(5) . . . . ?
C13 N3 C9 C10 66.0(5) . . . . ?
C13 N3 C17 C18 -62.7(5) . . . . ?
C13 N3 C21 C22 179.8(7) . . . . ?
C13 N3 C21 C22' 179(3) . . . . ?
C13 C14 C15 C16 -177.3(7) . . . . ?
C13 C14' C15' C16' -170(4) . . . . ?
C17 N3 C9 C10 -172.4(4) . . . . ?
C17 N3 C13 C14 -55.7(7) . . . . ?
C17 N3 C13 C14' -61(4) . . . . ?
C17 N3 C21 C22 58.9(8) . . . . ?
C17 N3 C21 C22' 58(3) . . . . ?
C17 C18 C19 C20 61.5(17) . . . . ?
C17 C18 C19' C20' 178.6(17) . . . . ?
C21 N3 C9 C10 -50.6(5) . . . . ?
C21 N3 C13 C14 -176.5(6) . . . . ?
C21 N3 C13 C14' 178(4) . . . . ?
C21 N3 C17 C18 53.9(5) . . . . ?
C21 C22 C23 C24 -179.6(10) . . . . ?
C21 C22' C23' C24' 175(4) . . . . ?
