#------------------------------------------------------------------------------
#$Date: 2020-03-15 04:14:17 +0200 (Sun, 15 Mar 2020) $
#$Revision: 249394 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/01/7240129.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_7240129
loop_
_publ_author_name
'Wang, Yu'
'Lin, Xinjun'
'Huang, Bo'
'Chen, Weizhou'
'Xiao, Zicheng'
'Wu, Pingfan'
_publ_section_title
;
 The crystal packing, morphology and hydrophobicity of
 polyoxometalate-based amphiphilic materials
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00129E
_journal_year                    2020
_chemical_formula_moiety         'C35 H60 N O12.5 V3, C4 H9 N O, C8 H20 N'
_chemical_formula_sum            'C47 H89 N3 O13.5 V3'
_chemical_formula_weight         1065.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-12-30 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                99.871(4)
_cell_angle_beta                 90.774(4)
_cell_angle_gamma                117.159(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1207(4)
_cell_length_b                   10.7427(5)
_cell_length_c                   27.9069(12)
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.7390
_cell_volume                     2645.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  66.00   1.00   30.00    --    9.97  57.00  90.00   27
  2  ω    -20.00  84.00   1.00   30.00    --    9.97  77.00  60.00  104
  3  ω     49.00  76.00   1.00   30.00    --    9.97 178.00 150.00   27
  4  ω    -38.00  61.00   1.00   30.00    --  -11.85  57.00 -60.00   99
  5  ω    -88.00  10.00   1.00   30.00    --  -11.85 -77.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186840000
_diffrn_orient_matrix_UB_12      -0.0540776000
_diffrn_orient_matrix_UB_13      0.0035982000
_diffrn_orient_matrix_UB_21      0.0607156000
_diffrn_orient_matrix_UB_22      0.0271858000
_diffrn_orient_matrix_UB_23      -0.0142300000
_diffrn_orient_matrix_UB_31      0.0473060000
_diffrn_orient_matrix_UB_32      0.0455187000
_diffrn_orient_matrix_UB_33      0.0213893000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24023
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.658
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             1138
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0511
_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)+(0.0289P)²+1.8102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8402
_reflns_number_total             11088
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00129e2.cif
_cod_data_source_block           35-wo
_cod_original_formula_sum        'C47 H89 N3 O13.50 V3'
_cod_database_code               7240129
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'V O C N'
_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.
;
_reflns_odcompleteness_completeness 96.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14A) = Uanis(O14)
Uanis(C44A) = Uanis(C44)
Uanis(C56) = Uanis(C5A)
Uanis(C63) = Uanis(C63A)
Uanis(C5) = Uanis(C56A)
Uanis(N43A) = Uanis(N43)
3. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C44A)=Sof(O14A)=Sof(N43A)=
 Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=1-FVAR(1)
 Sof(O14)=Sof(N43)=Sof(C44)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C65(H65A,H65B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 N15(H15), C24(H24), C27(H27), C31(H31)
4.d Idealised Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C5A(H5AA,H5AB,H5AC)
4.e Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C3(H3A,H3B,
 H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C63A(H63D,H63E,H63F), C56A(H56D,H56E,H56F)
;
_olex2_date_sample_data_collection 2017-12-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.591
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.64306(4) 0.11384(4) 0.44493(2) 0.00902(10) Uani 1 1 d . . . . .
V2 V 0.58716(4) 0.21639(4) 0.54724(2) 0.00868(10) Uani 1 1 d . . . . .
V3 V 0.69460(4) -0.03139(4) 0.52140(2) 0.00875(10) Uani 1 1 d . . . . .
O1 O 0.76991(16) 0.05598(17) 0.47250(6) 0.0095(4) Uani 1 1 d . . . . .
O2 O 0.42185(16) 0.21104(17) 0.52025(6) 0.0091(4) Uani 1 1 d . . . . .
O3 O 0.5000 0.0000 0.5000 0.0066(5) Uani 1 2 d S T P . .
O4 O 0.73935(16) 0.15168(16) 0.56469(6) 0.0072(4) Uani 1 1 d . . . . .
O5 O 0.69318(17) 0.26469(17) 0.49342(6) 0.0097(4) Uani 1 1 d . . . . .
O6 O 0.52933(16) -0.09211(17) 0.40747(6) 0.0079(4) Uani 1 1 d . . . . .
O0AA O 0.45137(16) 0.11309(17) 0.42823(6) 0.0074(4) Uani 1 1 d . . . . .
O8 O 0.82722(17) -0.05014(18) 0.54553(7) 0.0125(4) Uani 1 1 d . . . . .
O9 O 0.66128(17) 0.36302(17) 0.58685(6) 0.0116(4) Uani 1 1 d . . . . .
O10 O 0.72648(17) 0.17999(18) 0.40009(7) 0.0131(4) Uani 1 1 d . . . . .
O11 O 0.20735(19) -0.34191(19) 0.28655(7) 0.0182(4) Uani 1 1 d . . . . .
O12 O -0.15251(19) -0.55889(18) 0.14161(7) 0.0164(4) Uani 1 1 d . . . . .
O13 O -0.00361(19) -0.06556(18) 0.15369(7) 0.0170(4) Uani 1 1 d . . . . .
N15 N 0.2720(2) -0.1066(2) 0.30649(8) 0.0108(5) Uani 1 1 d . . . . .
H15 H 0.2802 -0.0340 0.2953 0.013 Uiso 1 1 calc R . . . .
C17 C 0.3925(3) 0.0760(3) 0.37823(9) 0.0102(5) Uani 1 1 d . . . . .
H17A H 0.4694 0.1326 0.3594 0.012 Uiso 1 1 calc R . . . .
H17B H 0.3107 0.0987 0.3755 0.012 Uiso 1 1 calc R . . . .
C18 C 0.1998(3) -0.2380(3) 0.27679(10) 0.0129(6) Uani 1 1 d . . . . .
C19 C 0.1067(3) -0.2533(3) 0.23148(10) 0.0124(5) Uani 1 1 d . . . . .
C20 C 0.0849(3) 0.0812(3) 0.17722(10) 0.0159(6) Uani 1 1 d . . . . .
H20A H 0.1905 0.1084 0.1775 0.019 Uiso 1 1 calc R . . . .
H20B H 0.0621 0.0970 0.2107 0.019 Uiso 1 1 calc R . . . .
C21 C -0.0743(3) -0.4184(3) 0.16442(10) 0.0140(6) Uani 1 1 d . . . . .
C22 C 0.3365(2) -0.0828(2) 0.35673(9) 0.0086(5) Uani 1 1 d . . . . .
C24 C -0.0813(3) -0.3068(3) 0.14842(10) 0.0133(6) Uani 1 1 d . . . . .
H24 H -0.1455 -0.3242 0.1211 0.016 Uiso 1 1 calc R . . . .
C27 C 0.1034(3) -0.1385(3) 0.21533(10) 0.0136(6) Uani 1 1 d . . . . .
H27 H 0.1627 -0.0452 0.2320 0.016 Uiso 1 1 calc R . . . .
C29 C 0.0097(3) -0.1671(3) 0.17382(10) 0.0133(6) Uani 1 1 d . . . . .
C30 C 0.1277(3) 0.3268(3) 0.16677(11) 0.0178(6) Uani 1 1 d . . . . .
H30A H 0.0813 0.3713 0.1501 0.021 Uiso 1 1 calc R . . . .
H30B H 0.1165 0.3459 0.2013 0.021 Uiso 1 1 calc R . . . .
C31 C 0.0186(3) -0.3920(3) 0.20634(10) 0.0139(6) Uani 1 1 d . . . . .
H31 H 0.0213 -0.4677 0.2174 0.017 Uiso 1 1 calc R . . . .
C32 C 0.2934(3) 0.3959(3) 0.16024(11) 0.0198(6) Uani 1 1 d . . . . .
H32A H 0.3057 0.3697 0.1262 0.024 Uiso 1 1 calc R . . . .
H32B H 0.3424 0.3592 0.1797 0.024 Uiso 1 1 calc R . . . .
C33 C -0.3007(3) -0.9752(3) 0.04949(11) 0.0230(7) Uani 1 1 d . . . . .
H33A H -0.3907 -1.0093 0.0276 0.028 Uiso 1 1 calc R . . . .
H33B H -0.3308 -1.0077 0.0798 0.028 Uiso 1 1 calc R . . . .
C34 C -0.2235(3) -0.8128(3) 0.06030(11) 0.0200(6) Uani 1 1 d . . . . .
H34A H -0.1908 -0.7790 0.0304 0.024 Uiso 1 1 calc R . . . .
H34B H -0.1356 -0.7774 0.0834 0.024 Uiso 1 1 calc R . . . .
C35 C 0.0445(3) 0.1660(3) 0.14758(11) 0.0180(6) Uani 1 1 d . . . . .
H35A H -0.0619 0.1345 0.1471 0.022 Uiso 1 1 calc R . . . .
H35B H 0.0655 0.1457 0.1141 0.022 Uiso 1 1 calc R . . . .
C36 C -0.2002(3) -1.2785(3) -0.00490(11) 0.0220(6) Uani 1 1 d . . . . .
H36A H -0.1605 -1.2431 -0.0340 0.026 Uiso 1 1 calc R . . . .
H36B H -0.1164 -1.2535 0.0187 0.026 Uiso 1 1 calc R . . . .
C37 C -0.2506(3) -0.5932(3) 0.09839(10) 0.0177(6) Uani 1 1 d . . . . .
H37A H -0.1944 -0.5468 0.0731 0.021 Uiso 1 1 calc R . . . .
H37B H -0.3247 -0.5609 0.1056 0.021 Uiso 1 1 calc R . . . .
C38 C 0.2121(3) -0.1747(3) 0.38506(9) 0.0102(5) Uani 1 1 d . . . . .
H38A H 0.1294 -0.1532 0.3824 0.012 Uiso 1 1 calc R . . . .
H38B H 0.1763 -0.2746 0.3704 0.012 Uiso 1 1 calc R . . . .
C40 C -0.3257(3) -0.7532(3) 0.08138(10) 0.0189(6) Uani 1 1 d . . . . .
H40A H -0.4075 -0.7803 0.0567 0.023 Uiso 1 1 calc R . . . .
H40B H -0.3681 -0.7972 0.1088 0.023 Uiso 1 1 calc R . . . .
C41 C 0.4669(3) -0.1192(3) 0.35796(9) 0.0103(5) Uani 1 1 d . . . . .
H41A H 0.4315 -0.2190 0.3432 0.012 Uiso 1 1 calc R . . . .
H41B H 0.5434 -0.0619 0.3392 0.012 Uiso 1 1 calc R . . . .
C42 C -0.2125(3) -1.7513(3) -0.07852(12) 0.0255(7) Uani 1 1 d . . . . .
H42A H -0.1788 -1.7166 -0.1082 0.031 Uiso 1 1 calc R . . . .
H42B H -0.1247 -1.7261 -0.0568 0.031 Uiso 1 1 calc R . . . .
C45 C 0.3687(3) 0.5580(3) 0.17523(11) 0.0188(6) Uani 1 1 d . . . . .
H45A H 0.3625 0.5840 0.2099 0.023 Uiso 1 1 calc R . . . .
H45B H 0.3147 0.5939 0.1576 0.023 Uiso 1 1 calc R . . . .
C46 C 0.6127(3) 1.0838(3) 0.22612(12) 0.0265(7) Uani 1 1 d . . . . .
H46A H 0.5900 1.0525 0.1909 0.032 Uiso 1 1 calc R . . . .
H46B H 0.5187 1.0476 0.2405 0.032 Uiso 1 1 calc R . . . .
C47 C -0.2975(3) -1.6764(3) -0.05435(11) 0.0190(6) Uani 1 1 d . . . . .
H47A H -0.3344 -1.7134 -0.0252 0.023 Uiso 1 1 calc R . . . .
H47B H -0.3833 -1.6985 -0.0766 0.023 Uiso 1 1 calc R . . . .
C49 C -0.2071(3) -1.0433(3) 0.02668(11) 0.0226(7) Uani 1 1 d . . . . .
H49A H -0.1765 -1.0115 -0.0037 0.027 Uiso 1 1 calc R . . . .
H49B H -0.1175 -1.0111 0.0486 0.027 Uiso 1 1 calc R . . . .
C50 C -0.2039(3) -1.5152(3) -0.04021(11) 0.0209(6) Uani 1 1 d . . . . .
H50A H -0.1634 -1.4788 -0.0691 0.025 Uiso 1 1 calc R . . . .
H50B H -0.1206 -1.4931 -0.0169 0.025 Uiso 1 1 calc R . . . .
C51 C -0.2906(3) -1.2052(3) 0.01644(12) 0.0241(7) Uani 1 1 d . . . . .
H51A H -0.3786 -1.2367 -0.0061 0.029 Uiso 1 1 calc R . . . .
H51B H -0.3242 -1.2360 0.0467 0.029 Uiso 1 1 calc R . . . .
C52 C -0.2906(3) -1.4391(3) -0.01797(11) 0.0201(6) Uani 1 1 d . . . . .
H52A H -0.3755 -1.4636 -0.0410 0.024 Uiso 1 1 calc R . . . .
H52B H -0.3290 -1.4741 0.0113 0.024 Uiso 1 1 calc R . . . .
C53 C 0.5319(3) 0.6297(3) 0.16545(12) 0.0226(7) Uani 1 1 d . . . . .
H53A H 0.5385 0.5991 0.1312 0.027 Uiso 1 1 calc R . . . .
H53B H 0.5868 0.5976 0.1845 0.027 Uiso 1 1 calc R . . . .
C57 C 0.6876(3) 1.2447(3) 0.23825(13) 0.0311(8) Uani 1 1 d . . . . .
H57A H 0.7786 1.2813 0.2223 0.037 Uiso 1 1 calc R . . . .
H57B H 0.7153 1.2765 0.2733 0.037 Uiso 1 1 calc R . . . .
C58 C 0.6063(3) 0.7931(3) 0.17774(11) 0.0227(7) Uani 1 1 d . . . . .
H58A H 0.7024 0.8301 0.1648 0.027 Uiso 1 1 calc R . . . .
H58B H 0.5452 0.8246 0.1614 0.027 Uiso 1 1 calc R . . . .
C59 C 0.7048(3) 1.0193(3) 0.24390(12) 0.0248(7) Uani 1 1 d . . . . .
H59A H 0.7278 1.0512 0.2791 0.030 Uiso 1 1 calc R . . . .
H59B H 0.7985 1.0554 0.2295 0.030 Uiso 1 1 calc R . . . .
C62 C -0.3032(3) -1.9128(3) -0.09117(12) 0.0306(7) Uani 1 1 d . . . . .
H62A H -0.3872 -1.9391 -0.1143 0.046 Uiso 1 1 calc GR . . . .
H62B H -0.3379 -1.9483 -0.0620 0.046 Uiso 1 1 calc GR . . . .
H62C H -0.2417 -1.9531 -0.1052 0.046 Uiso 1 1 calc GR . . . .
C64 C 0.5896(4) 1.3065(4) 0.22256(13) 0.0364(8) Uani 1 1 d . . . . .
H64A H 0.5601 1.2739 0.1880 0.055 Uiso 1 1 calc GR . . . .
H64B H 0.6445 1.4089 0.2299 0.055 Uiso 1 1 calc GR . . . .
H64C H 0.5024 1.2760 0.2399 0.055 Uiso 1 1 calc GR . . . .
C65 C 0.6297(3) 0.8565(3) 0.23202(11) 0.0263(7) Uani 1 1 d . . . . .
H65A H 0.6904 0.8247 0.2484 0.032 Uiso 1 1 calc R . . . .
H65B H 0.5336 0.8201 0.2450 0.032 Uiso 1 1 calc R . . . .
O14 O 0.2655(16) 0.1680(19) 0.2972(6) 0.0167(14) Uani 0.780(4) 1 d . . . A 1
N43 N 0.0979(3) 0.2391(3) 0.32903(11) 0.0169(7) Uani 0.780(4) 1 d . . . A 1
C44 C 0.2231(4) 0.2652(4) 0.30767(13) 0.0144(8) Uani 0.780(4) 1 d . . . A 1
C56 C 0.0121(7) 0.1013(7) 0.3423(3) 0.0224(12) Uani 0.780(4) 1 d . . . A 1
H56A H 0.0101 0.0274 0.3170 0.034 Uiso 0.780(4) 1 calc R . . A 1
H56B H -0.0881 0.0855 0.3463 0.034 Uiso 0.780(4) 1 calc R . . A 1
H56C H 0.0575 0.0997 0.3725 0.034 Uiso 0.780(4) 1 calc R . . A 1
C63 C 0.0491(10) 0.3436(7) 0.3442(4) 0.0224(14) Uani 0.780(4) 1 d . . . A 1
H63A H 0.0801 0.3835 0.3784 0.034 Uiso 0.780(4) 1 calc GR . . A 1
H63B H -0.0578 0.2996 0.3387 0.034 Uiso 0.780(4) 1 calc GR . . A 1
H63C H 0.0921 0.4179 0.3258 0.034 Uiso 0.780(4) 1 calc GR . . A 1
N1 N -0.2772(2) -0.3876(2) 0.43559(8) 0.0122(5) Uani 1 1 d . . . . .
H1 H -0.3113 -0.3321 0.4590 0.015 Uiso 1 1 calc R . . . .
C2 C -0.1182(3) -0.3439(3) 0.45650(11) 0.0177(6) Uani 1 1 d . . . . .
H2 H -0.0521 -0.2510 0.4487 0.021 Uiso 1 1 calc R . . . .
C3 C -0.5440(3) -0.5792(3) 0.43053(11) 0.0166(6) Uani 1 1 d . . . . .
H3A H -0.5719 -0.5830 0.3971 0.025 Uiso 1 1 calc GR . . . .
H3B H -0.5601 -0.5077 0.4515 0.025 Uiso 1 1 calc GR . . . .
H3C H -0.6034 -0.6705 0.4389 0.025 Uiso 1 1 calc GR . . . .
C4 C -0.3824(3) -0.5424(3) 0.43697(11) 0.0151(6) Uani 1 1 d . . . . .
H4A H -0.3631 -0.6036 0.4113 0.018 Uiso 1 1 calc R . . . .
H4B H -0.3612 -0.5620 0.4681 0.018 Uiso 1 1 calc R . . . .
C5 C 0.3110(12) 0.4101(8) 0.2968(4) 0.0147(15) Uani 0.780(4) 1 d . . . A 1
H5A H 0.3560 0.4782 0.3269 0.022 Uiso 0.780(4) 1 calc GR . . A 1
H5B H 0.2462 0.4348 0.2798 0.022 Uiso 0.780(4) 1 calc GR . . A 1
H5C H 0.3877 0.4107 0.2768 0.022 Uiso 0.780(4) 1 calc GR . . A 1
C6 C -0.1116(3) -0.3257(3) 0.51199(11) 0.0198(6) Uani 1 1 d . . . . .
H6A H -0.1571 -0.2673 0.5246 0.030 Uiso 1 1 calc GR . . . .
H6B H -0.0093 -0.2808 0.5257 0.030 Uiso 1 1 calc GR . . . .
H6C H -0.1642 -0.4176 0.5206 0.030 Uiso 1 1 calc GR . . . .
C7 C -0.2053(3) -0.1934(3) 0.38755(11) 0.0196(6) Uani 1 1 d . . . . .
H7A H -0.2175 -0.1401 0.4169 0.029 Uiso 1 1 calc GR . . . .
H7B H -0.2371 -0.1688 0.3596 0.029 Uiso 1 1 calc GR . . . .
H7C H -0.1021 -0.1710 0.3870 0.029 Uiso 1 1 calc GR . . . .
C8 C -0.0615(3) -0.4483(3) 0.43511(12) 0.0224(7) Uani 1 1 d . . . . .
H8A H -0.1186 -0.5378 0.4449 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.0418 -0.4103 0.4468 0.034 Uiso 1 1 calc GR . . . .
H8C H -0.0717 -0.4626 0.4001 0.034 Uiso 1 1 calc GR . . . .
C9 C -0.2987(3) -0.3515(3) 0.38611(11) 0.0197(6) Uani 1 1 d . . . . .
H9 H -0.4033 -0.3720 0.3814 0.024 Uiso 1 1 calc R . . . .
C10 C -0.2734(4) -0.4407(4) 0.34254(12) 0.0386(8) Uani 1 1 d . . . . .
H10A H -0.1692 -0.4150 0.3434 0.058 Uiso 1 1 calc GR . . . .
H10B H -0.3053 -0.4236 0.3129 0.058 Uiso 1 1 calc GR . . . .
H10C H -0.3298 -0.5400 0.3437 0.058 Uiso 1 1 calc GR . . . .
C5A C 0.031(3) 0.072(3) 0.3369(11) 0.0224(12) Uani 0.220(4) 1 d . . . A 2
H5AA H -0.0625 0.0464 0.3193 0.034 Uiso 0.220(4) 1 calc R . . A 2
H5AB H 0.0321 0.1116 0.3706 0.034 Uiso 0.220(4) 1 calc R . . A 2
H5AC H 0.0455 -0.0110 0.3350 0.034 Uiso 0.220(4) 1 calc R . . A 2
C44A C 0.1589(14) 0.1842(15) 0.3142(5) 0.0144(8) Uani 0.220(4) 1 d . . . A 2
O14A O 0.246(6) 0.169(7) 0.293(2) 0.0167(14) Uani 0.220(4) 1 d . . . A 2
N43A N 0.1708(12) 0.3111(13) 0.3161(4) 0.0169(7) Uani 0.220(4) 1 d . . . A 2
C63A C 0.068(4) 0.376(4) 0.3420(17) 0.0224(14) Uani 0.220(4) 1 d . . . A 2
H63D H 0.0086 0.3863 0.3174 0.034 Uiso 0.220(4) 1 calc GR . . A 2
H63E H 0.1301 0.4670 0.3625 0.034 Uiso 0.220(4) 1 calc GR . . A 2
H63F H 0.0032 0.3118 0.3615 0.034 Uiso 0.220(4) 1 calc GR . . A 2
C56A C 0.310(5) 0.438(4) 0.3019(16) 0.0147(15) Uani 0.220(4) 1 d . . . A 2
H56D H 0.3412 0.5213 0.3271 0.022 Uiso 0.220(4) 1 calc GR . . A 2
H56E H 0.2840 0.4564 0.2716 0.022 Uiso 0.220(4) 1 calc GR . . A 2
H56F H 0.3895 0.4129 0.2981 0.022 Uiso 0.220(4) 1 calc GR . . A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
V3 V1 V2 65.713(15) . . ?
O1 V1 V2 89.04(5) . . ?
O1 V1 V3 32.95(5) . . ?
O1 V1 O3 80.35(5) . . ?
O1 V1 O6 85.88(7) . . ?
O1 V1 O0AA 156.82(7) . . ?
O3 V1 V2 47.022(12) . . ?
O3 V1 V3 47.478(11) . . ?
O5 V1 V2 34.59(5) . . ?
O5 V1 V3 86.34(6) . . ?
O5 V1 O1 93.76(7) . . ?
O5 V1 O3 81.54(6) . . ?
O5 V1 O6 158.33(7) . . ?
O5 V1 O0AA 90.34(7) . . ?
O6 V1 V2 123.81(5) . . ?
O6 V1 V3 81.62(5) . . ?
O6 V1 O3 77.03(5) . . ?
O0AA V1 V2 81.47(5) . . ?
O0AA V1 V3 124.98(5) . . ?
O0AA V1 O3 77.70(5) . . ?
O0AA V1 O6 82.03(6) . . ?
O10 V1 V2 138.80(6) . . ?
O10 V1 V3 136.61(6) . . ?
O10 V1 O1 103.74(8) . . ?
O10 V1 O3 172.12(6) . . ?
O10 V1 O5 104.69(8) . . ?
O10 V1 O6 96.40(8) . . ?
O10 V1 O0AA 97.23(8) . . ?
V3 V2 V1 66.246(15) 2_656 . ?
O2 V2 V1 87.77(6) . . ?
O2 V2 V3 36.11(5) . 2_656 ?
O2 V2 O3 83.52(5) . . ?
O2 V2 O4 160.17(7) . . ?
O2 V2 O5 94.10(7) . . ?
O2 V2 O6 91.55(7) . 2_656 ?
O3 V2 V1 47.493(12) . . ?
O3 V2 V3 47.489(12) . 2_656 ?
O4 V2 V1 80.64(5) . . ?
O4 V2 V3 124.08(5) . 2_656 ?
O4 V2 O3 76.78(5) . . ?
O5 V2 V1 32.95(5) . . ?
O5 V2 V3 89.36(5) . 2_656 ?
O5 V2 O3 80.38(5) . . ?
O5 V2 O4 84.90(7) . . ?
O5 V2 O6 157.33(7) . 2_656 ?
O6 V2 V1 125.71(5) 2_656 . ?
O6 V2 V3 82.37(5) 2_656 2_656 ?
O6 V2 O3 78.48(5) 2_656 . ?
O6 V2 O4 82.41(7) 2_656 . ?
O9 V2 V1 135.94(6) . . ?
O9 V2 V3 139.86(6) . 2_656 ?
O9 V2 O2 104.24(8) . . ?
O9 V2 O3 171.06(6) . . ?
O9 V2 O4 95.24(7) . . ?
O9 V2 O5 103.16(8) . . ?
O9 V2 O6 96.65(8) . 2_656 ?
V1 V3 V2 65.913(15) . 2_656 ?
O1 V3 V1 35.02(5) . . ?
O1 V3 V2 86.80(5) . 2_656 ?
O1 V3 O2 93.79(8) . 2_656 ?
O1 V3 O3 82.72(5) . . ?
O1 V3 O4 91.22(7) . . ?
O1 V3 O0AA 159.17(7) . 2_656 ?
O2 V3 V1 89.74(5) 2_656 . ?
O2 V3 V2 34.05(5) 2_656 2_656 ?
O2 V3 O3 81.29(5) 2_656 . ?
O2 V3 O4 157.90(7) 2_656 . ?
O2 V3 O0AA 85.32(7) 2_656 2_656 ?
O3 V3 V1 47.783(11) . . ?
O3 V3 V2 47.319(11) . 2_656 ?
O4 V3 V1 82.11(5) . . ?
O4 V3 V2 125.12(5) . 2_656 ?
O4 V3 O3 78.01(5) . . ?
O4 V3 O0AA 82.43(7) . 2_656 ?
O0AA V3 V1 124.17(5) 2_656 . ?
O0AA V3 V2 80.84(5) 2_656 2_656 ?
O0AA V3 O3 76.56(4) 2_656 . ?
O8 V3 V1 139.31(7) . . ?
O8 V3 V2 137.00(6) . 2_656 ?
O8 V3 O1 104.86(8) . . ?
O8 V3 O2 103.11(8) . 2_656 ?
O8 V3 O3 170.78(7) . . ?
O8 V3 O4 96.35(8) . . ?
O8 V3 O0AA 95.58(8) . 2_656 ?
V3 O1 V1 112.03(8) . . ?
V2 O2 V3 109.83(8) . 2_656 ?
V1 O3 V1 180.00(2) 2_656 . ?
V2 O3 V1 85.485(16) . . ?
V2 O3 V1 85.485(16) 2_656 2_656 ?
V2 O3 V1 94.515(16) 2_656 . ?
V2 O3 V1 94.515(16) . 2_656 ?
V2 O3 V2 180.0 . 2_656 ?
V2 O3 V3 94.807(15) 2_656 2_656 ?
V2 O3 V3 85.193(16) . 2_656 ?
V2 O3 V3 85.192(16) 2_656 . ?
V2 O3 V3 94.808(15) . . ?
V3 O3 V1 84.739(16) 2_656 2_656 ?
V3 O3 V1 95.261(16) . 2_656 ?
V3 O3 V1 95.261(16) 2_656 . ?
V3 O3 V1 84.740(16) . . ?
V3 O3 V3 179.999(19) . 2_656 ?
V3 O4 V2 109.88(7) . . ?
C38 O4 V2 118.02(14) 2_656 . ?
C38 O4 V3 119.28(14) 2_656 . ?
V1 O5 V2 112.46(8) . . ?
V2 O6 V1 109.30(8) 2_656 . ?
C41 O6 V1 118.95(14) . . ?
C41 O6 V2 119.79(14) . 2_656 ?
V1 O0AA V3 109.99(8) . 2_656 ?
C17 O0AA V1 119.20(14) . . ?
C17 O0AA V3 117.86(13) . 2_656 ?
C21 O12 C37 117.9(2) . . ?
C29 O13 C20 117.9(2) . . ?
C18 N15 H15 118.3 . . ?
C18 N15 C22 123.3(2) . . ?
C22 N15 H15 118.3 . . ?
O0AA C17 H17A 109.2 . . ?
O0AA C17 H17B 109.2 . . ?
O0AA C17 C22 112.2(2) . . ?
H17A C17 H17B 107.9 . . ?
C22 C17 H17A 109.2 . . ?
C22 C17 H17B 109.2 . . ?
O11 C18 N15 121.8(2) . . ?
O11 C18 C19 120.4(2) . . ?
N15 C18 C19 117.8(2) . . ?
C27 C19 C18 123.9(2) . . ?
C31 C19 C18 115.5(2) . . ?
C31 C19 C27 120.6(2) . . ?
O13 C20 H20A 110.6 . . ?
O13 C20 H20B 110.6 . . ?
O13 C20 C35 105.6(2) . . ?
H20A C20 H20B 108.7 . . ?
C35 C20 H20A 110.6 . . ?
C35 C20 H20B 110.6 . . ?
O12 C21 C24 124.7(2) . . ?
O12 C21 C31 115.2(2) . . ?
C24 C21 C31 120.1(2) . . ?
N15 C22 C17 106.05(19) . . ?
N15 C22 C38 107.99(18) . . ?
N15 C22 C41 111.8(2) . . ?
C17 C22 C41 109.98(19) . . ?
C38 C22 C17 110.3(2) . . ?
C38 C22 C41 110.6(2) . . ?
C21 C24 H24 120.5 . . ?
C21 C24 C29 119.1(2) . . ?
C29 C24 H24 120.5 . . ?
C19 C27 H27 120.8 . . ?
C29 C27 C19 118.4(2) . . ?
C29 C27 H27 120.8 . . ?
O13 C29 C24 113.7(2) . . ?
O13 C29 C27 124.6(2) . . ?
C27 C29 C24 121.6(2) . . ?
H30A C30 H30B 107.6 . . ?
C32 C30 H30A 108.6 . . ?
C32 C30 H30B 108.6 . . ?
C32 C30 C35 114.6(2) . . ?
C35 C30 H30A 108.6 . . ?
C35 C30 H30B 108.6 . . ?
C19 C31 C21 120.2(2) . . ?
C19 C31 H31 119.9 . . ?
C21 C31 H31 119.9 . . ?
C30 C32 H32A 109.0 . . ?
C30 C32 H32B 109.0 . . ?
C30 C32 C45 112.8(2) . . ?
H32A C32 H32B 107.8 . . ?
C45 C32 H32A 109.0 . . ?
C45 C32 H32B 109.0 . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
C34 C33 C49 115.3(2) . . ?
C49 C33 H33A 108.5 . . ?
C49 C33 H33B 108.5 . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
C33 C34 C40 112.0(2) . . ?
H34A C34 H34B 107.9 . . ?
C40 C34 H34A 109.2 . . ?
C40 C34 H34B 109.2 . . ?
C20 C35 C30 113.9(2) . . ?
C20 C35 H35A 108.8 . . ?
C20 C35 H35B 108.8 . . ?
C30 C35 H35A 108.8 . . ?
C30 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
H36A C36 H36B 107.8 . . ?
C51 C36 H36A 109.0 . . ?
C51 C36 H36B 109.0 . . ?
C52 C36 H36A 109.0 . . ?
C52 C36 H36B 109.0 . . ?
C52 C36 C51 113.1(2) . . ?
O12 C37 H37A 110.2 . . ?
O12 C37 H37B 110.2 . . ?
O12 C37 C40 107.5(2) . . ?
H37A C37 H37B 108.5 . . ?
C40 C37 H37A 110.2 . . ?
C40 C37 H37B 110.2 . . ?
O4 C38 C22 112.49(19) 2_656 . ?
O4 C38 H38A 109.1 2_656 . ?
O4 C38 H38B 109.1 2_656 . ?
C22 C38 H38A 109.1 . . ?
C22 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C34 C40 H40A 108.6 . . ?
C34 C40 H40B 108.6 . . ?
C37 C40 C34 114.6(2) . . ?
C37 C40 H40A 108.6 . . ?
C37 C40 H40B 108.6 . . ?
H40A C40 H40B 107.6 . . ?
O6 C41 C22 110.40(19) . . ?
O6 C41 H41A 109.6 . . ?
O6 C41 H41B 109.6 . . ?
C22 C41 H41A 109.6 . . ?
C22 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
H42A C42 H42B 107.7 . . ?
C47 C42 H42A 108.8 . . ?
C47 C42 H42B 108.8 . . ?
C62 C42 H42A 108.8 . . ?
C62 C42 H42B 108.8 . . ?
C62 C42 C47 114.0(2) . . ?
C32 C45 H45A 108.9 . . ?
C32 C45 H45B 108.9 . . ?
C32 C45 C53 113.5(2) . . ?
H45A C45 H45B 107.7 . . ?
C53 C45 H45A 108.9 . . ?
C53 C45 H45B 108.9 . . ?
H46A C46 H46B 107.6 . . ?
C57 C46 H46A 108.7 . . ?
C57 C46 H46B 108.7 . . ?
C57 C46 C59 114.2(2) . . ?
C59 C46 H46A 108.7 . . ?
C59 C46 H46B 108.7 . . ?
C42 C47 H47A 108.9 . . ?
C42 C47 H47B 108.9 . . ?
C42 C47 C50 113.5(2) . . ?
H47A C47 H47B 107.7 . . ?
C50 C47 H47A 108.9 . . ?
C50 C47 H47B 108.9 . . ?
C33 C49 H49A 109.0 . . ?
C33 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
C51 C49 C33 112.7(2) . . ?
C51 C49 H49A 109.0 . . ?
C51 C49 H49B 109.0 . . ?
C47 C50 H50A 108.8 . . ?
C47 C50 H50B 108.8 . . ?
C47 C50 C52 113.6(2) . . ?
H50A C50 H50B 107.7 . . ?
C52 C50 H50A 108.8 . . ?
C52 C50 H50B 108.8 . . ?
C36 C51 H51A 108.6 . . ?
C36 C51 H51B 108.6 . . ?
C49 C51 C36 114.8(2) . . ?
C49 C51 H51A 108.6 . . ?
C49 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C36 C52 C50 114.3(2) . . ?
C36 C52 H52A 108.7 . . ?
C36 C52 H52B 108.7 . . ?
C50 C52 H52A 108.7 . . ?
C50 C52 H52B 108.7 . . ?
H52A C52 H52B 107.6 . . ?
C45 C53 H53A 108.8 . . ?
C45 C53 H53B 108.8 . . ?
C45 C53 C58 113.9(2) . . ?
H53A C53 H53B 107.7 . . ?
C58 C53 H53A 108.8 . . ?
C58 C53 H53B 108.8 . . ?
C46 C57 H57A 108.9 . . ?
C46 C57 H57B 108.9 . . ?
C46 C57 C64 113.1(3) . . ?
H57A C57 H57B 107.8 . . ?
C64 C57 H57A 108.9 . . ?
C64 C57 H57B 108.9 . . ?
C53 C58 H58A 108.7 . . ?
C53 C58 H58B 108.7 . . ?
H58A C58 H58B 107.6 . . ?
C65 C58 C53 114.3(3) . . ?
C65 C58 H58A 108.7 . . ?
C65 C58 H58B 108.7 . . ?
C46 C59 H59A 108.6 . . ?
C46 C59 H59B 108.6 . . ?
C46 C59 C65 114.6(2) . . ?
H59A C59 H59B 107.6 . . ?
C65 C59 H59A 108.6 . . ?
C65 C59 H59B 108.6 . . ?
C42 C62 H62A 109.5 . . ?
C42 C62 H62B 109.5 . . ?
C42 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C57 C64 H64A 109.5 . . ?
C57 C64 H64B 109.5 . . ?
C57 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C58 C65 C59 113.9(3) . . ?
C58 C65 H65A 108.8 . . ?
C58 C65 H65B 108.8 . . ?
C59 C65 H65A 108.8 . . ?
C59 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
C44 N43 C56 119.3(3) . . ?
C44 N43 C63 124.0(4) . . ?
C63 N43 C56 116.4(4) . . ?
O14 C44 N43 121.0(9) . . ?
O14 C44 C5 121.6(9) . . ?
N43 C44 C5 117.4(4) . . ?
N43 C56 H56A 109.5 . . ?
N43 C56 H56B 109.5 . . ?
N43 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N43 C63 H63A 109.5 . . ?
N43 C63 H63B 109.5 . . ?
N43 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C2 N1 H1 104.7 . . ?
C2 N1 C9 118.2(2) . . ?
C4 N1 H1 104.7 . . ?
C4 N1 C2 111.43(19) . . ?
C4 N1 C9 111.6(2) . . ?
C9 N1 H1 104.7 . . ?
N1 C2 H2 107.8 . . ?
C6 C2 N1 109.2(2) . . ?
C6 C2 H2 107.8 . . ?
C8 C2 N1 113.3(2) . . ?
C8 C2 H2 107.8 . . ?
C8 C2 C6 110.6(2) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
C3 C4 N1 113.5(2) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C44 C5 H5A 109.5 . . ?
C44 C5 H5B 109.5 . . ?
C44 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C7 H7A 109.5 . . ?
C9 C7 H7B 109.5 . . ?
C9 C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9 106.5 . . ?
C7 C9 N1 110.5(2) . . ?
C7 C9 H9 106.5 . . ?
C7 C9 C10 111.6(2) . . ?
C10 C9 N1 114.6(2) . . ?
C10 C9 H9 106.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C44A C5A H5AA 109.5 . . ?
C44A C5A H5AB 109.5 . . ?
C44A C5A H5AC 109.5 . . ?
O14A C44A C5A 127(4) . . ?
O14A C44A N43A 112(4) . . ?
N43A C44A C5A 120.8(14) . . ?
C44A N43A C63A 127.9(15) . . ?
C44A N43A C56A 123.7(16) . . ?
C56A N43A C63A 107.4(17) . . ?
N43A C63A H63D 109.5 . . ?
N43A C63A H63E 109.5 . . ?
N43A C63A H63F 109.5 . . ?
H63D C63A H63E 109.5 . . ?
H63D C63A H63F 109.5 . . ?
H63E C63A H63F 109.5 . . ?
N43A C56A H56D 109.5 . . ?
N43A C56A H56E 109.5 . . ?
N43A C56A H56F 109.5 . . ?
H56D C56A H56E 109.5 . . ?
H56D C56A H56F 109.5 . . ?
H56E C56A H56F 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 V2 3.0364(6) . ?
V1 V3 3.0190(6) . ?
V1 O1 1.8688(17) . ?
V1 O3 2.2454(4) . ?
V1 O5 1.7870(17) . ?
V1 O6 2.0402(16) . ?
V1 O0AA 1.9851(15) . ?
V1 O10 1.6030(18) . ?
V2 V3 3.0206(6) 2_656 ?
V2 O2 1.7981(16) . ?
V2 O3 2.2284(4) . ?
V2 O4 2.0411(16) . ?
V2 O5 1.8652(17) . ?
V2 O6 1.9879(17) 2_656 ?
V2 O9 1.6024(17) . ?
V3 V2 3.0206(6) 2_656 ?
V3 O1 1.7715(17) . ?
V3 O2 1.8925(17) 2_656 ?
V3 O3 2.2345(4) . ?
V3 O4 1.9723(16) . ?
V3 O0AA 2.0553(17) 2_656 ?
V3 O8 1.6013(17) . ?
O2 V3 1.8926(16) 2_656 ?
O3 V1 2.2453(4) 2_656 ?
O3 V2 2.2284(4) 2_656 ?
O3 V3 2.2345(4) 2_656 ?
O4 C38 1.421(3) 2_656 ?
O6 V2 1.9879(17) 2_656 ?
O6 C41 1.436(3) . ?
O0AA V3 2.0553(17) 2_656 ?
O0AA C17 1.425(3) . ?
O11 C18 1.228(3) . ?
O12 C21 1.370(3) . ?
O12 C37 1.435(3) . ?
O13 C20 1.435(3) . ?
O13 C29 1.366(3) . ?
N15 H15 0.8600 . ?
N15 C18 1.361(3) . ?
N15 C22 1.469(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C22 1.532(3) . ?
C18 C19 1.506(4) . ?
C19 C27 1.398(4) . ?
C19 C31 1.385(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C35 1.506(4) . ?
C21 C24 1.379(4) . ?
C21 C31 1.395(4) . ?
C22 C38 1.531(3) . ?
C22 C41 1.540(3) . ?
C24 H24 0.9300 . ?
C24 C29 1.400(4) . ?
C27 H27 0.9300 . ?
C27 C29 1.385(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C32 1.521(4) . ?
C30 C35 1.524(4) . ?
C31 H31 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C45 1.522(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.521(4) . ?
C33 C49 1.526(4) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C40 1.522(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C51 1.524(4) . ?
C36 C52 1.510(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C40 1.509(4) . ?
C38 O4 1.421(3) 2_656 ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C47 1.518(4) . ?
C42 C62 1.518(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C53 1.523(4) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C57 1.507(4) . ?
C46 C59 1.513(4) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C50 1.520(4) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C51 1.517(4) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 C52 1.523(4) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 C58 1.532(4) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C64 1.519(4) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C65 1.518(4) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C65 1.525(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
O14 C44 1.291(16) . ?
N43 C44 1.339(5) . ?
N43 C56 1.452(7) . ?
N43 C63 1.425(10) . ?
C44 C5 1.487(10) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
N1 H1 0.9800 . ?
N1 C2 1.530(3) . ?
N1 C4 1.519(3) . ?
N1 C9 1.535(3) . ?
C2 H2 0.9800 . ?
C2 C6 1.524(4) . ?
C2 C8 1.520(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C4 1.497(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 C9 1.514(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9 0.9800 . ?
C9 C10 1.515(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C5A H5AA 0.9600 . ?
C5A H5AB 0.9600 . ?
C5A H5AC 0.9600 . ?
C5A C44A 1.54(3) . ?
C44A O14A 1.13(7) . ?
C44A N43A 1.305(19) . ?
N43A C63A 1.61(5) . ?
N43A C56A 1.56(4) . ?
C63A H63D 0.9600 . ?
C63A H63E 0.9600 . ?
C63A H63F 0.9600 . ?
C56A H56D 0.9600 . ?
C56A H56E 0.9600 . ?
C56A H56F 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 V2 O2 V3 50.90(7) . . . 2_656 ?
V1 O6 C41 C22 -68.8(2) . . . . ?
V1 O0AA C17 C22 70.1(2) . . . . ?
V2 V1 O1 V3 43.07(8) . . . . ?
V2 V3 O1 V1 50.76(7) 2_656 . . . ?
V2 O6 C41 C22 69.9(2) 2_656 . . . ?
V3 V1 O5 V2 -50.71(7) . . . . ?
V3 V2 O5 V1 -43.67(8) 2_656 . . . ?
V3 O0AA C17 C22 -67.5(2) 2_656 . . . ?
O1 V1 O5 V2 -82.83(9) . . . . ?
O2 V2 O5 V1 -79.50(9) . . . . ?
O2 V3 O1 V1 84.11(9) 2_656 . . . ?
O3 V1 O1 V3 -3.40(7) . . . . ?
O3 V1 O5 V2 -3.18(7) . . . . ?
O3 V2 O2 V3 3.44(7) . . . 2_656 ?
O3 V2 O5 V1 3.21(7) . . . . ?
O3 V3 O1 V1 3.40(7) . . . . ?
O4 V2 O2 V3 -3.1(3) . . . 2_656 ?
O4 V2 O5 V1 80.64(9) . . . . ?
O4 V3 O1 V1 -74.35(9) . . . . ?
O5 V1 O1 V3 77.35(9) . . . . ?
O5 V2 O2 V3 83.25(9) . . . 2_656 ?
O6 V1 O1 V3 -80.93(9) . . . . ?
O6 V1 O5 V2 5.5(2) . . . . ?
O6 V2 O2 V3 -74.78(9) 2_656 . . 2_656 ?
O6 V2 O5 V1 24.5(2) 2_656 . . . ?
O0AA V1 O1 V3 -22.3(2) . . . . ?
O0AA V1 O5 V2 74.33(9) . . . . ?
O0AA V3 O1 V1 -2.7(3) 2_656 . . . ?
O0AA C17 C22 N15 176.86(18) . . . . ?
O0AA C17 C22 C38 60.2(2) . . . . ?
O0AA C17 C22 C41 -62.1(3) . . . . ?
O8 V3 O1 V1 -171.25(9) . . . . ?
O9 V2 O2 V3 -172.05(9) . . . 2_656 ?
O9 V2 O5 V1 174.84(9) . . . . ?
O10 V1 O1 V3 -176.52(9) . . . . ?
O10 V1 O5 V2 171.90(9) . . . . ?
O11 C18 C19 C27 -173.6(2) . . . . ?
O11 C18 C19 C31 7.9(4) . . . . ?
O12 C21 C24 C29 -177.1(2) . . . . ?
O12 C21 C31 C19 177.9(2) . . . . ?
O12 C37 C40 C34 -70.5(3) . . . . ?
O13 C20 C35 C30 -179.9(2) . . . . ?
N15 C18 C19 C27 7.5(4) . . . . ?
N15 C18 C19 C31 -171.0(2) . . . . ?
N15 C22 C38 O4 -175.77(19) . . . 2_656 ?
N15 C22 C41 O6 178.87(18) . . . . ?
C17 C22 C38 O4 -60.3(3) . . . 2_656 ?
C17 C22 C41 O6 61.4(3) . . . . ?
C18 N15 C22 C17 -174.6(2) . . . . ?
C18 N15 C22 C38 -56.4(3) . . . . ?
C18 N15 C22 C41 65.5(3) . . . . ?
C18 C19 C27 C29 -178.1(2) . . . . ?
C18 C19 C31 C21 178.7(2) . . . . ?
C19 C27 C29 O13 -179.3(2) . . . . ?
C19 C27 C29 C24 0.5(4) . . . . ?
C20 O13 C29 C24 179.8(2) . . . . ?
C20 O13 C29 C27 -0.4(4) . . . . ?
C21 O12 C37 C40 -178.5(2) . . . . ?
C21 C24 C29 O13 178.1(2) . . . . ?
C21 C24 C29 C27 -1.7(4) . . . . ?
C22 N15 C18 O11 -13.7(4) . . . . ?
C22 N15 C18 C19 165.1(2) . . . . ?
C24 C21 C31 C19 -1.4(4) . . . . ?
C27 C19 C31 C21 0.2(4) . . . . ?
C29 O13 C20 C35 -179.0(2) . . . . ?
C30 C32 C45 C53 -175.8(2) . . . . ?
C31 C19 C27 C29 0.3(4) . . . . ?
C31 C21 C24 C29 2.2(4) . . . . ?
C32 C30 C35 C20 70.0(3) . . . . ?
C32 C45 C53 C58 176.8(3) . . . . ?
C33 C34 C40 C37 173.2(2) . . . . ?
C33 C49 C51 C36 -178.2(3) . . . . ?
C34 C33 C49 C51 -179.6(3) . . . . ?
C35 C30 C32 C45 174.3(2) . . . . ?
C37 O12 C21 C24 -1.0(4) . . . . ?
C37 O12 C21 C31 179.7(2) . . . . ?
C38 C22 C41 O6 -60.7(2) . . . . ?
C41 C22 C38 O4 61.6(3) . . . 2_656 ?
C42 C47 C50 C52 177.5(3) . . . . ?
C45 C53 C58 C65 69.3(3) . . . . ?
C46 C59 C65 C58 66.0(3) . . . . ?
C47 C50 C52 C36 -178.5(2) . . . . ?
C49 C33 C34 C40 178.1(2) . . . . ?
C51 C36 C52 C50 179.0(3) . . . . ?
C52 C36 C51 C49 -175.8(3) . . . . ?
C53 C58 C65 C59 179.7(2) . . . . ?
C57 C46 C59 C65 179.8(3) . . . . ?
C59 C46 C57 C64 -176.8(3) . . . . ?
C62 C42 C47 C50 177.9(3) . . . . ?
C56 N43 C44 O14 2.5(9) . . . . ?
C56 N43 C44 C5 -177.2(6) . . . . ?
C63 N43 C44 O14 176.2(9) . . . . ?
C63 N43 C44 C5 -3.6(8) . . . . ?
C2 N1 C4 C3 163.7(2) . . . . ?
C2 N1 C9 C7 -55.1(3) . . . . ?
C2 N1 C9 C10 72.0(3) . . . . ?
C4 N1 C2 C6 -74.3(3) . . . . ?
C4 N1 C2 C8 49.5(3) . . . . ?
C4 N1 C9 C7 173.7(2) . . . . ?
C4 N1 C9 C10 -59.2(3) . . . . ?
C9 N1 C2 C6 154.5(2) . . . . ?
C9 N1 C2 C8 -81.8(3) . . . . ?
C9 N1 C4 C3 -61.8(3) . . . . ?
C5A C44A N43A C63A 2(3) . . . . ?
C5A C44A N43A C56A 170(2) . . . . ?
O14A C44A N43A C63A 179(4) . . . . ?
O14A C44A N43A C56A -13(4) . . . . ?
