#------------------------------------------------------------------------------
#$Date: 2017-05-06 01:09:07 +0300 (Sat, 06 May 2017) $
#$Revision: 196441 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/25/7042542.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_7042542
loop_
_publ_author_name
'Bayaguud, Aruuhan'
'Li, JianDa'
'She, Shan'
'Wei, Yongge'
_publ_section_title
;
 A simple synthetic route to polyoxovanadate-based organic-inorganic
 hybrids using EEDQ as an ester coupling agent.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4602
_journal_page_last               4608
_journal_paper_doi               10.1039/c7dt00274b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C42 H78 O23 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C74 H150 N2 O23 V6'
_chemical_formula_weight         1741.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.329(4)
_cell_angle_beta                 96.637(5)
_cell_angle_gamma                116.297(5)
_cell_formula_units_Z            1
_cell_length_a                   11.4081(7)
_cell_length_b                   11.9363(6)
_cell_length_c                   18.8822(11)
_cell_measurement_reflns_used    5270
_cell_measurement_temperature    105.6
_cell_measurement_theta_max      29.1498
_cell_measurement_theta_min      2.9927
_cell_volume                     2199.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      105.6
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -36.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -77.0000 -150.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -84.0000  139.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega   -9.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   -5.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   37.0000 -150.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0238049000
_diffrn_orient_matrix_UB_12      -0.0064105000
_diffrn_orient_matrix_UB_13      0.0328334000
_diffrn_orient_matrix_UB_21      0.0464902000
_diffrn_orient_matrix_UB_22      -0.0209505000
_diffrn_orient_matrix_UB_23      0.0114880000
_diffrn_orient_matrix_UB_31      0.0484932000
_diffrn_orient_matrix_UB_32      0.0654348000
_diffrn_orient_matrix_UB_33      0.0184407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15055
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       'flat stick'
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0206P)²+0.9031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7165
_reflns_number_total             8630
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           exp_shiliuchun
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_original_cell_volume        2199.3(2)
_cod_database_code               7042542
_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   0.948
_shelx_estimated_absorpt_t_min   0.759
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C32(H32A,H32B), C30(H30A,H30B), C34(H34A,
 H34B), C2(H2A,H2B), C24(H24A,H24B), C35(H35A,H35B), C31(H31A,H31B), C1(H1A,
 H1B), C3(H3A,H3B), C23(H23A,H23B), C28(H28A,H28B), C27(H27A,H27B), C6(H6A,H6B),
  C36(H36A,H36B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B),
 C19(H19A,H19B), C15(H15A,H15B), C16(H16A,H16B), C8(H8A,H8B), C17(H17A,H17B),
 C20(H20A,H20B), C12(H12A,H12B), C14(H14A,H14B), C11(H11A,H11B), C18(H18A,H18B)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
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
V1 V 0.16099(3) 0.04614(3) 0.09922(2) 0.01311(9) Uani 1 1 d . . .
V2 V -0.00987(3) 0.18428(3) 0.03707(2) 0.01226(9) Uani 1 1 d . . .
V3 V -0.17181(3) -0.11789(3) 0.04715(2) 0.01253(9) Uani 1 1 d . . .
O5 O 0.14213(13) -0.10924(13) 0.04970(7) 0.0137(3) Uani 1 1 d . . .
O1 O 0.0000 0.0000 0.0000 0.0101(4) Uani 1 2 d S T P
O6 O -0.12630(14) -0.24421(12) 0.00878(8) 0.0135(3) Uani 1 1 d . . .
O7 O 0.26815(13) 0.13600(13) 0.04061(8) 0.0137(3) Uani 1 1 d . . .
O10 O -0.00817(13) -0.04613(12) 0.13319(7) 0.0121(3) Uani 1 1 d . . .
O9 O -0.14912(13) 0.06195(12) 0.08262(7) 0.0110(3) Uani 1 1 d . . .
O8 O 0.11934(13) 0.19669(12) 0.12424(7) 0.0114(3) Uani 1 1 d . . .
O4 O -0.28201(13) -0.18712(13) 0.09259(8) 0.0154(3) Uani 1 1 d . . .
O2 O 0.26452(14) 0.08732(13) 0.17632(8) 0.0166(3) Uani 1 1 d . . .
O3 O -0.01684(14) 0.31373(13) 0.07570(8) 0.0150(3) Uani 1 1 d . . .
N1 N 0.32685(16) 0.64451(15) 0.03973(9) 0.0126(4) Uani 1 1 d . . .
O12 O -0.05427(17) 0.28864(15) 0.29486(8) 0.0273(4) Uani 1 1 d . . .
C26 C 0.18658(19) 0.54677(18) -0.00754(11) 0.0140(4) Uani 1 1 d . . .
H26A H 0.1420 0.4846 0.0194 0.017 Uiso 1 1 calc R . .
H26B H 0.1359 0.5929 -0.0135 0.017 Uiso 1 1 calc R . .
C22 C 0.3995(2) 0.57351(19) 0.06555(11) 0.0136(4) Uani 1 1 d . . .
H22A H 0.3911 0.5079 0.0228 0.016 Uiso 1 1 calc R . .
H22B H 0.4943 0.6355 0.0840 0.016 Uiso 1 1 calc R . .
O11 O -0.0314(2) 0.13895(17) 0.34099(9) 0.0376(5) Uani 1 1 d . . .
C5 C -0.0348(2) 0.1849(2) 0.29149(12) 0.0162(5) Uani 1 1 d . . .
C32 C 0.4373(2) 0.87263(19) -0.08859(12) 0.0176(5) Uani 1 1 d . . .
H32A H 0.4165 0.9407 -0.0957 0.021 Uiso 1 1 calc R . .
H32B H 0.5312 0.9140 -0.0632 0.021 Uiso 1 1 calc R . .
C30 C 0.4119(2) 0.72907(19) -0.00428(12) 0.0143(4) Uani 1 1 d . . .
H30A H 0.4271 0.6746 -0.0435 0.017 Uiso 1 1 calc R . .
H30B H 0.4987 0.7919 0.0283 0.017 Uiso 1 1 calc R . .
C34 C 0.3099(2) 0.72761(19) 0.10578(11) 0.0152(4) Uani 1 1 d . . .
H34A H 0.2486 0.6705 0.1302 0.018 Uiso 1 1 calc R . .
H34B H 0.2687 0.7754 0.0876 0.018 Uiso 1 1 calc R . .
C2 C -0.1489(2) 0.10976(19) 0.15816(11) 0.0135(4) Uani 1 1 d . . .
H2A H -0.2285 0.0474 0.1699 0.016 Uiso 1 1 calc R . .
H2B H -0.1528 0.1906 0.1645 0.016 Uiso 1 1 calc R . .
C24 C 0.4421(2) 0.4542(2) 0.15163(12) 0.0189(5) Uani 1 1 d . . .
H24A H 0.3975 0.3933 0.1792 0.023 Uiso 1 1 calc R . .
H24B H 0.4563 0.4068 0.1085 0.023 Uiso 1 1 calc R . .
C35 C 0.4401(2) 0.82428(19) 0.16308(11) 0.0180(5) Uani 1 1 d . . .
H35A H 0.4945 0.8929 0.1424 0.022 Uiso 1 1 calc R . .
H35B H 0.4905 0.7803 0.1749 0.022 Uiso 1 1 calc R . .
C31 C 0.3513(2) 0.80191(19) -0.03895(12) 0.0152(5) Uani 1 1 d . . .
H31A H 0.3455 0.8645 -0.0001 0.018 Uiso 1 1 calc R . .
H31B H 0.2610 0.7410 -0.0682 0.018 Uiso 1 1 calc R . .
C1 C 0.1052(2) 0.23804(19) 0.19762(11) 0.0144(4) Uani 1 1 d . . .
H1A H 0.1008 0.3186 0.2038 0.017 Uiso 1 1 calc R . .
H1B H 0.1833 0.2546 0.2334 0.017 Uiso 1 1 calc R . .
C4 C -0.0231(2) 0.13365(19) 0.21262(11) 0.0137(4) Uani 1 1 d . . .
C33 C 0.4170(2) 0.7848(2) -0.16430(12) 0.0241(5) Uani 1 1 d . . .
H33A H 0.4707 0.8361 -0.1931 0.036 Uiso 1 1 calc GR . .
H33B H 0.3240 0.7420 -0.1895 0.036 Uiso 1 1 calc GR . .
H33C H 0.4437 0.7208 -0.1580 0.036 Uiso 1 1 calc GR . .
C3 C -0.0161(2) 0.00662(19) 0.20658(11) 0.0148(4) Uani 1 1 d . . .
H3A H 0.0621 0.0233 0.2423 0.018 Uiso 1 1 calc R . .
H3B H -0.0954 -0.0563 0.2184 0.018 Uiso 1 1 calc R . .
C25 C 0.5786(2) 0.5598(2) 0.20047(13) 0.0235(5) Uani 1 1 d . . .
H25A H 0.6241 0.6199 0.1734 0.035 Uiso 1 1 calc GR . .
H25B H 0.6317 0.5205 0.2146 0.035 Uiso 1 1 calc GR . .
H25C H 0.5657 0.6054 0.2442 0.035 Uiso 1 1 calc GR . .
C23 C 0.3501(2) 0.50766(19) 0.12563(12) 0.0154(5) Uani 1 1 d . . .
H23A H 0.2589 0.4372 0.1061 0.019 Uiso 1 1 calc R . .
H23B H 0.3502 0.5700 0.1673 0.019 Uiso 1 1 calc R . .
C28 C 0.0339(2) 0.3828(2) -0.12665(12) 0.0190(5) Uani 1 1 d . . .
H28A H -0.0114 0.3215 -0.0994 0.023 Uiso 1 1 calc R . .
H28B H -0.0108 0.4350 -0.1297 0.023 Uiso 1 1 calc R . .
C27 C 0.1806(2) 0.47163(19) -0.08433(11) 0.0156(5) Uani 1 1 d . . .
H27A H 0.2251 0.4197 -0.0795 0.019 Uiso 1 1 calc R . .
H27B H 0.2270 0.5321 -0.1117 0.019 Uiso 1 1 calc R . .
C6 C -0.0790(2) 0.3453(2) 0.36327(12) 0.0246(5) Uani 1 1 d . . .
H6A H -0.0054 0.3714 0.4050 0.030 Uiso 1 1 calc R . .
H6B H -0.1615 0.2833 0.3728 0.030 Uiso 1 1 calc R . .
C36 C 0.4116(2) 0.8837(2) 0.23395(12) 0.0267(6) Uani 1 1 d . . .
H36A H 0.3497 0.8147 0.2519 0.032 Uiso 1 1 calc R . .
H36B H 0.3694 0.9352 0.2231 0.032 Uiso 1 1 calc R . .
C7 C -0.0900(3) 0.4626(2) 0.35153(12) 0.0261(6) Uani 1 1 d . . .
H7A H -0.1588 0.4348 0.3069 0.031 Uiso 1 1 calc R . .
H7B H -0.0054 0.5239 0.3436 0.031 Uiso 1 1 calc R . .
C9 C -0.1342(3) 0.6497(2) 0.40136(13) 0.0266(6) Uani 1 1 d . . .
H9A H -0.0476 0.7118 0.3959 0.032 Uiso 1 1 calc R . .
H9B H -0.1986 0.6212 0.3548 0.032 Uiso 1 1 calc R . .
C10 C -0.1765(3) 0.7185(2) 0.46244(13) 0.0297(6) Uani 1 1 d . . .
H10A H -0.1128 0.7466 0.5092 0.036 Uiso 1 1 calc R . .
H10B H -0.2639 0.6572 0.4675 0.036 Uiso 1 1 calc R . .
C13 C -0.2310(3) 1.0254(2) 0.49212(14) 0.0316(6) Uani 1 1 d . . .
H13A H -0.1402 1.0880 0.4924 0.038 Uiso 1 1 calc R . .
H13B H -0.2864 1.0019 0.4431 0.038 Uiso 1 1 calc R . .
C19 C -0.3881(2) 1.5859(2) 0.61350(13) 0.0272(6) Uani 1 1 d . . .
H19A H -0.2945 1.6522 0.6265 0.033 Uiso 1 1 calc R . .
H19B H -0.4222 1.5700 0.5610 0.033 Uiso 1 1 calc R . .
C15 C -0.2801(3) 1.2137(2) 0.53556(14) 0.0313(6) Uani 1 1 d . . .
H15A H -0.1878 1.2762 0.5387 0.038 Uiso 1 1 calc R . .
H15B H -0.3308 1.1925 0.4855 0.038 Uiso 1 1 calc R . .
C16 C -0.3368(3) 1.2777(2) 0.58977(15) 0.0336(6) Uani 1 1 d . . .
H16A H -0.4302 1.2165 0.5852 0.040 Uiso 1 1 calc R . .
H16B H -0.2884 1.2960 0.6400 0.040 Uiso 1 1 calc R . .
C8 C -0.1243(3) 0.5320(2) 0.41602(13) 0.0271(6) Uani 1 1 d . . .
H8A H -0.0556 0.5607 0.4608 0.032 Uiso 1 1 calc R . .
H8B H -0.2092 0.4715 0.4241 0.032 Uiso 1 1 calc R . .
C17 C -0.3282(3) 1.4032(2) 0.57785(14) 0.0304(6) Uani 1 1 d . . .
H17A H -0.3689 1.3867 0.5263 0.036 Uiso 1 1 calc R . .
H17B H -0.2343 1.4671 0.5871 0.036 Uiso 1 1 calc R . .
C20 C -0.4666(3) 1.6376(2) 0.65767(14) 0.0318(6) Uani 1 1 d . . .
H20A H -0.5604 1.5719 0.6441 0.038 Uiso 1 1 calc R . .
H20B H -0.4334 1.6524 0.7101 0.038 Uiso 1 1 calc R . .
C12 C -0.2299(3) 0.9042(2) 0.50596(14) 0.0333(6) Uani 1 1 d . . .
H12A H -0.3197 0.8431 0.5080 0.040 Uiso 1 1 calc R . .
H12B H -0.1708 0.9284 0.5539 0.040 Uiso 1 1 calc R . .
C14 C -0.2831(3) 1.0902(2) 0.54874(15) 0.0347(6) Uani 1 1 d . . .
H14A H -0.2292 1.1117 0.5979 0.042 Uiso 1 1 calc R . .
H14B H -0.3747 1.0285 0.5474 0.042 Uiso 1 1 calc R . .
C11 C -0.1838(3) 0.8367(2) 0.44659(13) 0.0301(6) Uani 1 1 d . . .
H11A H -0.0957 0.8990 0.4429 0.036 Uiso 1 1 calc R . .
H11B H -0.2453 0.8089 0.3990 0.036 Uiso 1 1 calc R . .
C18 C -0.3964(3) 1.4606(2) 0.62694(14) 0.0295(6) Uani 1 1 d . . .
H18A H -0.3550 1.4784 0.6785 0.035 Uiso 1 1 calc R . .
H18B H -0.4902 1.3966 0.6182 0.035 Uiso 1 1 calc R . .
C37 C 0.5410(3) 0.9697(2) 0.29416(14) 0.0363(7) Uani 1 1 d . . .
H37A H 0.6004 1.0407 0.2775 0.054 Uiso 1 1 calc GR . .
H37B H 0.5838 0.9193 0.3042 0.054 Uiso 1 1 calc GR . .
H37C H 0.5200 1.0032 0.3386 0.054 Uiso 1 1 calc GR . .
C21 C -0.4563(3) 1.7632(3) 0.64492(14) 0.0409(7) Uani 1 1 d . . .
H21A H -0.4862 1.7503 0.5929 0.061 Uiso 1 1 calc GR . .
H21B H -0.3646 1.8308 0.6620 0.061 Uiso 1 1 calc GR . .
H21C H -0.5116 1.7878 0.6719 0.061 Uiso 1 1 calc GR . .
C29 C 0.0222(2) 0.3081(2) -0.20469(13) 0.0284(6) Uani 1 1 d . . .
H29A H 0.0622 0.3683 -0.2328 0.043 Uiso 1 1 calc GR . .
H29B H -0.0708 0.2511 -0.2285 0.043 Uiso 1 1 calc GR . .
H29C H 0.0680 0.2577 -0.2020 0.043 Uiso 1 1 calc GR . .
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
V2 V1 V3 65.852(12) 2 2
O5 V1 V2 34.65(4) . 2
O5 V1 V3 87.43(5) . 2
O5 V1 O1 81.86(4) . .
O5 V1 O7 93.60(6) . .
O5 V1 O10 89.90(6) . .
O5 V1 O8 158.31(6) . .
O1 V1 V2 47.239(10) . 2
O1 V1 V3 47.341(10) . 2
O7 V1 V2 88.11(4) . 2
O7 V1 V3 32.93(4) . 2
O7 V1 O1 80.25(4) . .
O7 V1 O10 156.95(6) . .
O7 V1 O8 86.39(6) . .
O10 V1 V2 81.90(4) . 2
O10 V1 V3 124.79(4) . 2
O10 V1 O1 77.70(4) . .
O10 V1 O8 82.11(5) . .
O8 V1 V2 123.79(4) . 2
O8 V1 V3 80.80(4) . 2
O8 V1 O1 76.75(4) . .
O2 V1 V2 138.79(5) . 2
O2 V1 V3 136.70(6) . 2
O2 V1 O5 104.49(7) . .
O2 V1 O1 171.95(5) . .
O2 V1 O7 103.98(7) . .
O2 V1 O10 97.15(7) . .
O2 V1 O8 96.53(6) . .
V1 V2 V3 66.464(13) 2 2
O5 V2 V1 33.84(4) 2 2
O5 V2 V3 89.37(4) 2 2
O5 V2 O1 81.77(4) 2 .
O5 V2 O9 86.65(6) 2 .
O5 V2 O8 158.62(6) 2 .
O1 V2 V1 47.957(10) . 2
O1 V2 V3 47.758(10) . 2
O6 V2 V1 87.84(4) 2 2
O6 V2 V3 34.43(4) 2 2
O6 V2 O5 94.31(6) 2 2
O6 V2 O1 82.18(4) 2 .
O6 V2 O9 159.26(6) 2 .
O6 V2 O8 89.25(6) 2 .
O9 V2 V1 81.45(4) . 2
O9 V2 V3 125.01(4) . 2
O9 V2 O1 77.45(4) . .
O8 V2 V1 125.59(4) . 2
O8 V2 V3 81.69(4) . 2
O8 V2 O1 77.83(4) . .
O8 V2 O9 82.74(5) . .
O3 V2 V1 137.66(5) . 2
O3 V2 V3 137.23(5) . 2
O3 V2 O5 103.96(7) . 2
O3 V2 O1 171.61(6) . .
O3 V2 O6 103.25(7) . 2
O3 V2 O9 96.58(6) . .
O3 V2 O8 95.68(6) . .
V2 V3 V1 66.040(12) 2 2
O1 V3 V1 47.480(10) . 2
O1 V3 V2 47.183(10) . 2
O6 V3 V1 88.58(5) . 2
O6 V3 V2 33.42(4) . 2
O6 V3 O1 80.59(4) . .
O6 V3 O10 86.78(6) . .
O6 V3 O9 157.30(6) . .
O7 V3 V1 34.40(4) 2 2
O7 V3 V2 87.78(5) 2 2
O7 V3 O1 81.86(5) 2 .
O7 V3 O6 94.19(6) 2 .
O7 V3 O10 158.42(6) 2 .
O7 V3 O9 88.83(6) 2 .
O10 V3 V1 124.26(4) . 2
O10 V3 V2 81.19(4) . 2
O10 V3 O1 77.02(4) . .
O9 V3 V1 81.26(4) . 2
O9 V3 V2 124.56(4) . 2
O9 V3 O1 77.58(4) . .
O9 V3 O10 82.37(5) . .
O4 V3 V1 139.04(5) . 2
O4 V3 V2 136.70(5) . 2
O4 V3 O1 171.57(5) . .
O4 V3 O6 103.52(7) . .
O4 V3 O7 104.95(7) . 2
O4 V3 O10 95.73(6) . .
O4 V3 O9 97.38(6) . .
V1 O5 V2 111.51(7) . 2
V1 O1 V1 180.0 2 .
V2 O1 V1 95.195(14) 2 2
V2 O1 V1 95.196(14) . .
V2 O1 V1 84.804(13) 2 .
V2 O1 V1 84.805(14) . 2
V2 O1 V2 180.0 . 2
V2 O1 V3 85.060(14) . 2
V2 O1 V3 85.061(13) 2 .
V2 O1 V3 94.939(13) 2 2
V2 O1 V3 94.940(13) . .
V3 O1 V1 94.821(14) . .
V3 O1 V1 85.180(14) . 2
V3 O1 V1 94.821(14) 2 2
V3 O1 V1 85.179(14) 2 .
V3 O1 V3 180.0 . 2
V2 O6 V3 112.15(7) 2 .
V3 O7 V1 112.68(7) 2 .
V1 O10 V3 109.81(6) . .
C3 O10 V1 119.08(11) . .
C3 O10 V3 118.85(12) . .
V3 O9 V2 109.51(6) . .
C2 O9 V2 118.03(11) . .
C2 O9 V3 119.11(12) . .
V2 O8 V1 109.71(6) . .
C1 O8 V1 118.73(12) . .
C1 O8 V2 119.10(12) . .
C26 N1 C22 110.25(14) . .
C30 N1 C26 111.27(15) . .
C30 N1 C22 106.87(15) . .
C30 N1 C34 110.46(15) . .
C34 N1 C26 107.23(15) . .
C34 N1 C22 110.80(15) . .
C5 O12 C6 117.97(18) . .
N1 C26 H26A 108.3 . .
N1 C26 H26B 108.3 . .
H26A C26 H26B 107.4 . .
C27 C26 N1 115.88(17) . .
C27 C26 H26A 108.3 . .
C27 C26 H26B 108.3 . .
N1 C22 H22A 108.3 . .
N1 C22 H22B 108.3 . .
H22A C22 H22B 107.4 . .
C23 C22 N1 115.86(16) . .
C23 C22 H22A 108.3 . .
C23 C22 H22B 108.3 . .
O12 C5 C4 109.33(18) . .
O11 C5 O12 124.7(2) . .
O11 C5 C4 125.96(19) . .
H32A C32 H32B 107.6 . .
C31 C32 H32A 108.7 . .
C31 C32 H32B 108.7 . .
C33 C32 H32A 108.7 . .
C33 C32 H32B 108.7 . .
C33 C32 C31 114.10(17) . .
N1 C30 H30A 108.6 . .
N1 C30 H30B 108.6 . .
N1 C30 C31 114.70(16) . .
H30A C30 H30B 107.6 . .
C31 C30 H30A 108.6 . .
C31 C30 H30B 108.6 . .
N1 C34 H34A 108.6 . .
N1 C34 H34B 108.6 . .
N1 C34 C35 114.69(16) . .
H34A C34 H34B 107.6 . .
C35 C34 H34A 108.6 . .
C35 C34 H34B 108.6 . .
O9 C2 H2A 109.1 . .
O9 C2 H2B 109.1 . .
O9 C2 C4 112.36(16) . .
H2A C2 H2B 107.9 . .
C4 C2 H2A 109.1 . .
C4 C2 H2B 109.1 . .
H24A C24 H24B 107.7 . .
C25 C24 H24A 108.9 . .
C25 C24 H24B 108.9 . .
C25 C24 C23 113.42(17) . .
C23 C24 H24A 108.9 . .
C23 C24 H24B 108.9 . .
C34 C35 H35A 109.4 . .
C34 C35 H35B 109.4 . .
C34 C35 C36 111.15(18) . .
H35A C35 H35B 108.0 . .
C36 C35 H35A 109.4 . .
C36 C35 H35B 109.4 . .
C32 C31 H31A 109.5 . .
C32 C31 H31B 109.5 . .
C30 C31 C32 110.55(17) . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 108.1 . .
O8 C1 H1A 109.4 . .
O8 C1 H1B 109.4 . .
O8 C1 C4 111.09(15) . .
H1A C1 H1B 108.0 . .
C4 C1 H1A 109.4 . .
C4 C1 H1B 109.4 . .
C5 C4 C2 107.24(16) . .
C5 C4 C1 108.73(16) . .
C2 C4 C1 110.22(17) . .
C3 C4 C5 109.17(17) . .
C3 C4 C2 110.78(16) . .
C3 C4 C1 110.61(16) . .
C32 C33 H33A 109.5 . .
C32 C33 H33B 109.5 . .
C32 C33 H33C 109.5 . .
H33A C33 H33B 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
O10 C3 C4 110.99(16) . .
O10 C3 H3A 109.4 . .
O10 C3 H3B 109.4 . .
C4 C3 H3A 109.4 . .
C4 C3 H3B 109.4 . .
H3A C3 H3B 108.0 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25B 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C22 C23 C24 109.64(17) . .
C22 C23 H23A 109.7 . .
C22 C23 H23B 109.7 . .
C24 C23 H23A 109.7 . .
C24 C23 H23B 109.7 . .
H23A C23 H23B 108.2 . .
H28A C28 H28B 107.9 . .
C27 C28 H28A 109.2 . .
C27 C28 H28B 109.2 . .
C29 C28 H28A 109.2 . .
C29 C28 H28B 109.2 . .
C29 C28 C27 112.08(19) . .
C26 C27 C28 109.97(17) . .
C26 C27 H27A 109.7 . .
C26 C27 H27B 109.7 . .
C28 C27 H27A 109.7 . .
C28 C27 H27B 109.7 . .
H27A C27 H27B 108.2 . .
O12 C6 H6A 110.6 . .
O12 C6 H6B 110.6 . .
O12 C6 C7 105.65(18) . .
H6A C6 H6B 108.7 . .
C7 C6 H6A 110.6 . .
C7 C6 H6B 110.6 . .
C35 C36 H36A 109.4 . .
C35 C36 H36B 109.4 . .
C35 C36 C37 111.1(2) . .
H36A C36 H36B 108.0 . .
C37 C36 H36A 109.4 . .
C37 C36 H36B 109.4 . .
C6 C7 H7A 108.8 . .
C6 C7 H7B 108.8 . .
C6 C7 C8 113.9(2) . .
H7A C7 H7B 107.7 . .
C8 C7 H7A 108.8 . .
C8 C7 H7B 108.8 . .
H9A C9 H9B 107.6 . .
C10 C9 H9A 108.7 . .
C10 C9 H9B 108.7 . .
C10 C9 C8 114.0(2) . .
C8 C9 H9A 108.7 . .
C8 C9 H9B 108.7 . .
C9 C10 H10A 109.0 . .
C9 C10 H10B 109.0 . .
C9 C10 C11 112.7(2) . .
H10A C10 H10B 107.8 . .
C11 C10 H10A 109.0 . .
C11 C10 H10B 109.0 . .
H13A C13 H13B 107.6 . .
C12 C13 H13A 108.7 . .
C12 C13 H13B 108.7 . .
C14 C13 H13A 108.7 . .
C14 C13 H13B 108.7 . .
C14 C13 C12 114.1(2) . .
H19A C19 H19B 107.7 . .
C20 C19 H19A 108.8 . .
C20 C19 H19B 108.8 . .
C20 C19 C18 113.8(2) . .
C18 C19 H19A 108.8 . .
C18 C19 H19B 108.8 . .
H15A C15 H15B 107.6 . .
C16 C15 H15A 108.6 . .
C16 C15 H15B 108.6 . .
C16 C15 C14 114.8(2) . .
C14 C15 H15A 108.6 . .
C14 C15 H15B 108.6 . .
C15 C16 H16A 108.7 . .
C15 C16 H16B 108.7 . .
H16A C16 H16B 107.6 . .
C17 C16 C15 114.2(2) . .
C17 C16 H16A 108.7 . .
C17 C16 H16B 108.7 . .
C7 C8 C9 111.8(2) . .
C7 C8 H8A 109.3 . .
C7 C8 H8B 109.3 . .
C9 C8 H8A 109.3 . .
C9 C8 H8B 109.3 . .
H8A C8 H8B 107.9 . .
C16 C17 H17A 108.7 . .
C16 C17 H17B 108.7 . .
C16 C17 C18 114.3(2) . .
H17A C17 H17B 107.6 . .
C18 C17 H17A 108.7 . .
C18 C17 H17B 108.7 . .
C19 C20 H20A 108.9 . .
C19 C20 H20B 108.9 . .
H20A C20 H20B 107.7 . .
C21 C20 C19 113.6(2) . .
C21 C20 H20A 108.9 . .
C21 C20 H20B 108.9 . .
C13 C12 H12A 108.9 . .
C13 C12 H12B 108.9 . .
C13 C12 C11 113.5(2) . .
H12A C12 H12B 107.7 . .
C11 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
C13 C14 C15 113.7(2) . .
C13 C14 H14A 108.8 . .
C13 C14 H14B 108.8 . .
C15 C14 H14A 108.8 . .
C15 C14 H14B 108.8 . .
H14A C14 H14B 107.7 . .
C10 C11 H11A 108.9 . .
C10 C11 H11B 108.9 . .
C12 C11 C10 113.4(2) . .
C12 C11 H11A 108.9 . .
C12 C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C19 C18 H18A 108.9 . .
C19 C18 H18B 108.9 . .
C17 C18 C19 113.6(2) . .
C17 C18 H18A 108.9 . .
C17 C18 H18B 108.9 . .
H18A C18 H18B 107.7 . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37B 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
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 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 V2 3.0253(5) 2
V1 V3 3.0500(5) 2
V1 O5 1.8108(13) .
V1 O1 2.2560(4) .
V1 O7 1.8673(14) .
V1 O10 2.0073(14) .
V1 O8 2.0379(13) .
V1 O2 1.6010(14) .
V2 V1 3.0253(5) 2
V2 V3 3.0292(5) 2
V2 O5 1.8487(14) 2
V2 O1 2.2303(3) .
V2 O6 1.8012(14) 2
V2 O9 2.0370(14) .
V2 O8 2.0134(14) .
V2 O3 1.6141(13) .
V3 V1 3.0500(5) 2
V3 V2 3.0292(5) 2
V3 O1 2.2509(4) .
V3 O6 1.8493(13) .
V3 O7 1.7968(14) 2
V3 O10 2.0478(13) .
V3 O9 2.0065(13) .
V3 O4 1.6145(14) .
O5 V2 1.8488(14) 2
O1 V1 2.2559(4) 2
O1 V2 2.2303(3) 2
O1 V3 2.2509(4) 2
O6 V2 1.8012(14) 2
O7 V3 1.7968(14) 2
O10 C3 1.436(2) .
O9 C2 1.428(2) .
O8 C1 1.429(2) .
N1 C26 1.525(2) .
N1 C22 1.528(2) .
N1 C30 1.516(3) .
N1 C34 1.522(2) .
O12 C5 1.343(2) .
O12 C6 1.454(2) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C26 C27 1.524(3) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C22 C23 1.526(3) .
O11 C5 1.178(3) .
C5 C4 1.539(3) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C32 C31 1.531(3) .
C32 C33 1.522(3) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C30 C31 1.522(3) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C34 C35 1.526(3) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C4 1.543(3) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C24 C25 1.528(3) .
C24 C23 1.532(3) .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C35 C36 1.527(3) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C1 C4 1.547(3) .
C4 C3 1.536(3) .
C33 H33A 0.9600 .
C33 H33B 0.9600 .
C33 H33C 0.9600 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C28 C27 1.533(3) .
C28 C29 1.522(3) .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.516(3) .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
C36 C37 1.528(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.524(3) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.531(3) .
C9 C8 1.533(3) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 C11 1.533(3) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C12 1.525(3) .
C13 C14 1.524(3) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19 C20 1.529(3) .
C19 C18 1.530(3) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.528(3) .
C15 C14 1.529(3) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 C17 1.521(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 C18 1.524(3) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C20 C21 1.520(3) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 C11 1.529(3) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C37 H37A 0.9600 .
C37 H37B 0.9600 .
C37 H37C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 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_4
V1 V3 O6 V2 45.58(6) 2 2
V1 O10 C3 C4 70.05(18) . .
V1 O8 C1 C4 -68.60(18) . .
V2 V1 O7 V3 45.42(6) 2 2
V2 O9 C2 C4 -68.22(18) . .
V2 O8 C1 C4 69.58(18) . .
V3 V1 O5 V2 -49.05(7) 2 2
V3 O10 C3 C4 -68.47(18) . .
V3 O9 C2 C4 68.63(19) . .
O5 V1 O7 V3 79.64(8) . 2
O1 V1 O5 V2 -1.80(6) . 2
O1 V1 O7 V3 -1.46(6) . 2
O1 V3 O6 V2 -1.49(6) . 2
O7 V1 O5 V2 -81.41(8) . 2
O7 V3 O6 V2 79.54(8) 2 2
O10 V1 O5 V2 75.79(8) . 2
O10 V1 O7 V3 -18.61(18) . 2
O10 V3 O6 V2 -78.85(8) . 2
O9 V3 O6 V2 -17.5(2) . 2
O9 C2 C4 C5 179.88(16) . .
O9 C2 C4 C1 61.7(2) . .
O9 C2 C4 C3 -61.1(2) . .
O8 V1 O5 V2 7.9(2) . 2
O8 V1 O7 V3 -78.62(7) . 2
O8 C1 C4 C5 -178.59(16) . .
O8 C1 C4 C2 -61.3(2) . .
O8 C1 C4 C3 61.5(2) . .
O4 V3 O6 V2 -173.98(7) . 2
O2 V1 O5 V2 173.14(8) . 2
O2 V1 O7 V3 -174.46(7) . 2
N1 C26 C27 C28 -177.10(16) . .
N1 C22 C23 C24 -173.73(16) . .
N1 C30 C31 C32 -174.06(16) . .
N1 C34 C35 C36 -168.68(17) . .
O12 C5 C4 C2 -53.9(2) . .
O12 C5 C4 C1 65.3(2) . .
O12 C5 C4 C3 -173.93(16) . .
O12 C6 C7 C8 176.65(19) . .
C26 N1 C22 C23 -72.8(2) . .
C26 N1 C30 C31 56.0(2) . .
C26 N1 C34 C35 175.12(17) . .
C22 N1 C26 C27 -71.0(2) . .
C22 N1 C30 C31 176.44(16) . .
C22 N1 C34 C35 54.8(2) . .
O11 C5 C4 C2 124.0(2) . .
O11 C5 C4 C1 -116.8(2) . .
O11 C5 C4 C3 4.0(3) . .
C5 O12 C6 C7 177.34(18) . .
C5 C4 C3 O10 178.70(16) . .
C30 N1 C26 C27 47.4(2) . .
C30 N1 C22 C23 166.19(16) . .
C30 N1 C34 C35 -63.5(2) . .
C34 N1 C26 C27 168.26(17) . .
C34 N1 C22 C23 45.8(2) . .
C34 N1 C30 C31 -63.0(2) . .
C34 C35 C36 C37 174.17(19) . .
C2 C4 C3 O10 60.8(2) . .
C1 C4 C3 O10 -61.7(2) . .
C33 C32 C31 C30 78.2(2) . .
C25 C24 C23 C22 73.9(2) . .
C6 O12 C5 O11 -2.9(3) . .
C6 O12 C5 C4 175.06(18) . .
C6 C7 C8 C9 180.0(2) . .
C9 C10 C11 C12 178.3(2) . .
C10 C9 C8 C7 176.6(2) . .
C13 C12 C11 C10 177.3(2) . .
C15 C16 C17 C18 174.5(2) . .
C16 C15 C14 C13 177.8(2) . .
C16 C17 C18 C19 -179.3(2) . .
C8 C9 C10 C11 179.3(2) . .
C20 C19 C18 C17 175.0(2) . .
C12 C13 C14 C15 178.4(2) . .
C14 C13 C12 C11 177.2(2) . .
C14 C15 C16 C17 177.8(2) . .
C18 C19 C20 C21 179.2(2) . .
C29 C28 C27 C26 178.45(18) . .
