#------------------------------------------------------------------------------
#$Date: 2017-03-04 04:04:19 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192967 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345426.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_4345426
loop_
_publ_author_name
'Schmidt, Anna-Corina'
'Hermsen, Marko'
'Rominger, Frank'
'Dehn, Richard'
'Teles, Joaquim Henrique'
'Schäfer, Ansgar'
'Trapp, Oliver'
'Schaub, Thomas'
_publ_section_title
;
 Synthesis of Mono- and Dinuclear Vanadium Complexes and Their Reactivity
 toward Dehydroperoxidation of Alkyl Hydroperoxides.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1319
_journal_page_last               1332
_journal_paper_doi               10.1021/acs.inorgchem.6b02322
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C13 H16 N O8 V'
_chemical_formula_weight         365.21
_chemical_name_common            '6 H2O'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.959(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.956(2)
_cell_length_b                   12.2604(17)
_cell_length_c                   15.964(2)
_cell_measurement_reflns_used    5202
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.43
_cell_volume                     3121.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.556
_diffrn_reflns_theta_min         1.276
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0444
_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)+(0.0373P)²+0.7845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4452
_reflns_number_total             5828
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02322_si_002.cif
_cod_data_source_block           cos5
_cod_original_cell_volume        3121.1(8)
_cod_database_code               4345426
_shelx_shelxl_version_number     2014/7
_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_min   0.923
_shelx_estimated_absorpt_t_max   0.948
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_1 V 0.59402(5) 0.66613(6) 0.20704(5) 0.0277(2) Uani 1 1 d D U . . .
O1_1 O 0.65546(19) 0.6284(2) 0.1372(2) 0.0395(8) Uani 1 1 d D U . . .
O2_1 O 0.5066(2) 0.7399(4) 0.2958(2) 0.0489(10) Uani 1 1 d D U . . .
H2A_1 H 0.521(3) 0.755(4) 0.3407(19) 0.059(17) Uiso 1 1 d D U . . .
H2B_1 H 0.4607(18) 0.721(5) 0.298(3) 0.069(18) Uiso 1 1 d D U . . .
N1_1 N 0.6182(2) 0.8295(3) 0.1915(2) 0.0252(9) Uani 1 1 d D U . . .
C2_1 C 0.6774(3) 0.8771(3) 0.2388(3) 0.0263(10) Uani 1 1 d D U . . .
C3_1 C 0.6962(3) 0.9854(4) 0.2274(3) 0.0363(12) Uani 1 1 d D U . . .
H3_1 H 0.7375 1.0207 0.2621 0.044 Uiso 1 1 calc R U . . .
C4_1 C 0.6529(3) 1.0421(4) 0.1635(3) 0.0407(12) Uani 1 1 d D U . . .
H4_1 H 0.6666 1.1161 0.1529 0.049 Uiso 1 1 calc R U . . .
C5_1 C 0.5903(3) 0.9919(3) 0.1155(3) 0.0343(11) Uani 1 1 d D U . . .
H5_1 H 0.5597 1.0306 0.0730 0.041 Uiso 1 1 calc R U . . .
C6_1 C 0.5737(2) 0.8838(3) 0.1315(3) 0.0236(9) Uani 1 1 d D U . . .
C7_1 C 0.7140(3) 0.7981(4) 0.3017(3) 0.0332(12) Uani 1 1 d D U . . .
O7_1 O 0.7698(2) 0.8266(3) 0.3517(2) 0.0469(10) Uani 1 1 d D U . . .
O8_1 O 0.68254(19) 0.7023(3) 0.29502(19) 0.0332(8) Uani 1 1 d D U . . .
C9_1 C 0.5094(3) 0.8111(4) 0.0902(3) 0.0249(11) Uani 1 1 d D U . . .
O9_1 O 0.46589(18) 0.8407(2) 0.03015(18) 0.0317(8) Uani 1 1 d D U . . .
O10_1 O 0.50524(17) 0.7155(2) 0.12482(18) 0.0274(8) Uani 1 1 d D U . . .
O3_1 O 0.5852(10) 0.5525(11) 0.2858(8) 0.045(4) Uani 0.509(7) 1 d D U P A 1
O4_1 O 0.5129(6) 0.5454(7) 0.2298(6) 0.030(2) Uani 0.509(7) 1 d D U P A 1
C11_1 C 0.5095(6) 0.4460(7) 0.1771(7) 0.036(2) Uani 0.509(7) 1 d D U P A 1
H11_1 H 0.5540 0.4478 0.1345 0.043 Uiso 0.509(7) 1 calc R U P A 1
C12_1 C 0.5212(7) 0.3496(7) 0.2346(7) 0.041(3) Uani 0.509(7) 1 d D U P A 1
H12A_1 H 0.4833 0.3560 0.2822 0.050 Uiso 0.509(7) 1 calc R U P A 1
H12B_1 H 0.5797 0.3475 0.2573 0.050 Uiso 0.509(7) 1 calc R U P A 1
C13_1 C 0.5015(7) 0.2444(8) 0.1853(7) 0.052(3) Uani 0.509(7) 1 d D U P A 1
H13A_1 H 0.5432 0.2346 0.1414 0.062 Uiso 0.509(7) 1 calc R U P A 1
H13B_1 H 0.5057 0.1810 0.2237 0.062 Uiso 0.509(7) 1 calc R U P A 1
C14_1 C 0.4157(8) 0.2485(9) 0.1455(8) 0.058(3) Uani 0.509(7) 1 d D U P A 1
H14A_1 H 0.3737 0.2513 0.1897 0.069 Uiso 0.509(7) 1 calc R U P A 1
H14B_1 H 0.4056 0.1812 0.1123 0.069 Uiso 0.509(7) 1 calc R U P A 1
C15_1 C 0.4047(9) 0.3479(9) 0.0883(8) 0.062(4) Uani 0.509(7) 1 d D U P A 1
H15A_1 H 0.4427 0.3414 0.0408 0.074 Uiso 0.509(7) 1 calc R U P A 1
H15B_1 H 0.3463 0.3501 0.0652 0.074 Uiso 0.509(7) 1 calc R U P A 1
C16_1 C 0.4238(7) 0.4537(8) 0.1357(7) 0.046(3) Uani 0.509(7) 1 d D U P A 1
H16A_1 H 0.4216 0.5160 0.0963 0.055 Uiso 0.509(7) 1 calc R U P A 1
H16B_1 H 0.3813 0.4657 0.1785 0.055 Uiso 0.509(7) 1 calc R U P A 1
O3B_1 O 0.5943(11) 0.5287(12) 0.2617(9) 0.041(4) Uani 0.491(7) 1 d D U P A 2
O4B_1 O 0.5282(7) 0.5242(9) 0.1976(6) 0.034(3) Uani 0.491(7) 1 d D U P A 2
C11B_1 C 0.5414(6) 0.4386(7) 0.1336(6) 0.030(2) Uani 0.491(7) 1 d D U P A 2
H11B_1 H 0.5974 0.4494 0.1086 0.036 Uiso 0.491(7) 1 calc R U P A 2
C12B_1 C 0.5390(6) 0.3292(7) 0.1749(7) 0.043(3) Uani 0.491(7) 1 d D U P A 2
H12C_1 H 0.5813 0.3275 0.2217 0.052 Uiso 0.491(7) 1 calc R U P A 2
H12D_1 H 0.5546 0.2728 0.1339 0.052 Uiso 0.491(7) 1 calc R U P A 2
C13B_1 C 0.4540(7) 0.3008(10) 0.2086(7) 0.063(4) Uani 0.491(7) 1 d D U P A 2
H13C_1 H 0.4544 0.2242 0.2282 0.076 Uiso 0.491(7) 1 calc R U P A 2
H13D_1 H 0.4425 0.3483 0.2570 0.076 Uiso 0.491(7) 1 calc R U P A 2
C14B_1 C 0.3868(8) 0.3153(13) 0.1425(10) 0.078(5) Uani 0.491(7) 1 d D U P A 2
H14C_1 H 0.3316 0.3035 0.1675 0.094 Uiso 0.491(7) 1 calc R U P A 2
H14D_1 H 0.3936 0.2595 0.0984 0.094 Uiso 0.491(7) 1 calc R U P A 2
C15B_1 C 0.3881(7) 0.4278(13) 0.1026(9) 0.083(5) Uani 0.491(7) 1 d D U P A 2
H15C_1 H 0.3730 0.4829 0.1449 0.100 Uiso 0.491(7) 1 calc R U P A 2
H15D_1 H 0.3453 0.4307 0.0563 0.100 Uiso 0.491(7) 1 calc R U P A 2
C16B_1 C 0.4742(6) 0.4565(8) 0.0683(6) 0.050(3) Uani 0.491(7) 1 d D U P A 2
H16C_1 H 0.4849 0.4105 0.0188 0.060 Uiso 0.491(7) 1 calc R U P A 2
H16D_1 H 0.4744 0.5338 0.0503 0.060 Uiso 0.491(7) 1 calc R U P A 2
V1_2 V 0.72202(5) 0.66459(6) 0.58415(4) 0.02089(18) Uani 1 1 d D . . . .
O1_2 O 0.65183(18) 0.6112(2) 0.63868(18) 0.0298(7) Uani 1 1 d D . . . .
O2_2 O 0.8110(2) 0.7522(3) 0.50772(19) 0.0275(7) Uani 1 1 d D U . . .
H2A_2 H 0.797(3) 0.767(4) 0.4634(18) 0.045(15) Uiso 1 1 d D U . . .
H2B_2 H 0.8565(17) 0.732(4) 0.509(3) 0.035(14) Uiso 1 1 d D U . . .
N1_2 N 0.6915(2) 0.8217(3) 0.6188(2) 0.0226(8) Uani 1 1 d D . . . .
C2_2 C 0.7280(2) 0.8648(3) 0.6875(2) 0.0230(10) Uani 1 1 d D . . . .
C3_2 C 0.7025(3) 0.9633(3) 0.7172(3) 0.0305(11) Uani 1 1 d D . . . .
H3_2 H 0.7272 0.9928 0.7672 0.037 Uiso 1 1 calc R U . . .
C4_2 C 0.6405(3) 1.0192(4) 0.6732(3) 0.0413(12) Uani 1 1 d D . . . .
H4_2 H 0.6220 1.0881 0.6928 0.050 Uiso 1 1 calc R U . . .
C5_2 C 0.6049(3) 0.9748(3) 0.6001(3) 0.0345(11) Uani 1 1 d D . . . .
H5_2 H 0.5621 1.0126 0.5692 0.041 Uiso 1 1 calc R U . . .
C6_2 C 0.6331(3) 0.8752(3) 0.5735(3) 0.0242(10) Uani 1 1 d D . . . .
C7_2 C 0.7958(3) 0.7898(4) 0.7219(3) 0.0254(10) Uani 1 1 d D . . . .
O7_2 O 0.83940(18) 0.8159(2) 0.78358(18) 0.0320(8) Uani 1 1 d D . . . .
O8_2 O 0.80178(18) 0.7004(2) 0.68032(17) 0.0252(7) Uani 1 1 d D . . . .
C9_2 C 0.6070(3) 0.8105(4) 0.4964(3) 0.0295(12) Uani 1 1 d D . . . .
O9_2 O 0.55655(18) 0.8469(2) 0.44406(18) 0.0348(8) Uani 1 1 d D . . . .
O10_2 O 0.64437(17) 0.7172(2) 0.49255(17) 0.0238(7) Uani 1 1 d D . . . .
O3_2 O 0.79740(17) 0.5475(2) 0.57723(17) 0.0258(7) Uani 1 1 d D . . . .
O4_2 O 0.73851(16) 0.5364(2) 0.50751(16) 0.0251(7) Uani 1 1 d D . . . .
C11_2 C 0.6874(3) 0.4350(3) 0.5173(3) 0.0271(10) Uani 1 1 d D . . . .
H11_2 H 0.6688 0.4278 0.5762 0.032 Uiso 1 1 calc R U . . .
C12_2 C 0.7397(3) 0.3386(3) 0.4936(3) 0.0365(12) Uani 1 1 d D . . . .
H12A_2 H 0.7881 0.3315 0.5337 0.044 Uiso 1 1 calc R U . . .
H12B_2 H 0.7616 0.3500 0.4370 0.044 Uiso 1 1 calc R U . . .
C13_2 C 0.6876(3) 0.2346(4) 0.4944(3) 0.0438(13) Uani 1 1 d D . . . .
H13A_2 H 0.7219 0.1720 0.4765 0.053 Uiso 1 1 calc R U . . .
H13B_2 H 0.6691 0.2200 0.5519 0.053 Uiso 1 1 calc R U . . .
C14_2 C 0.6120(3) 0.2478(4) 0.4353(4) 0.0581(17) Uani 1 1 d D . . . .
H14A_2 H 0.5769 0.1814 0.4372 0.070 Uiso 1 1 calc R U . . .
H14B_2 H 0.6310 0.2565 0.3773 0.070 Uiso 1 1 calc R U . . .
C15_2 C 0.5602(3) 0.3461(4) 0.4588(4) 0.0619(18) Uani 1 1 d D . . . .
H15A_2 H 0.5381 0.3354 0.5155 0.074 Uiso 1 1 calc R U . . .
H15B_2 H 0.5120 0.3539 0.4187 0.074 Uiso 1 1 calc R U . . .
C16_2 C 0.6133(3) 0.4490(3) 0.4579(3) 0.0425(13) Uani 1 1 d D . . . .
H16A_2 H 0.6326 0.4626 0.4006 0.051 Uiso 1 1 calc R U . . .
H16B_2 H 0.5795 0.5123 0.4751 0.051 Uiso 1 1 calc R U . . .
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
O1_1 V1_1 O3_1 108.4(5)
O1_1 V1_1 O3B_1 94.2(6)
O1_1 V1_1 O10_1 93.92(15)
O3_1 V1_1 O10_1 126.6(4)
O3B_1 V1_1 O10_1 124.3(4)
O1_1 V1_1 O8_1 96.89(15)
O3_1 V1_1 O8_1 76.3(4)
O3B_1 V1_1 O8_1 83.3(4)
O10_1 V1_1 O8_1 149.49(13)
O1_1 V1_1 O4_1 109.3(3)
O3_1 V1_1 O4_1 43.2(4)
O10_1 V1_1 O4_1 83.9(3)
O8_1 V1_1 O4_1 118.6(3)
O1_1 V1_1 O4B_1 91.6(3)
O3B_1 V1_1 O4B_1 42.9(4)
O10_1 V1_1 O4B_1 81.8(3)
O8_1 V1_1 O4B_1 126.1(3)
O1_1 V1_1 N1_1 94.40(15)
O3_1 V1_1 N1_1 145.0(4)
O3B_1 V1_1 N1_1 157.4(4)
O10_1 V1_1 N1_1 75.90(13)
O8_1 V1_1 N1_1 74.89(13)
O4_1 V1_1 N1_1 149.8(3)
O4B_1 V1_1 N1_1 157.2(3)
O1_1 V1_1 O2_1 172.38(16)
O3_1 V1_1 O2_1 79.2(5)
O3B_1 V1_1 O2_1 93.4(6)
O10_1 V1_1 O2_1 81.30(14)
O8_1 V1_1 O2_1 84.56(14)
O4_1 V1_1 O2_1 76.2(3)
O4B_1 V1_1 O2_1 93.5(3)
N1_1 V1_1 O2_1 78.72(15)
V1_1 O2_1 H2A_1 121(4)
V1_1 O2_1 H2B_1 122(4)
H2A_1 O2_1 H2B_1 108(4)
C2_1 N1_1 C6_1 122.4(3)
C2_1 N1_1 V1_1 119.5(3)
C6_1 N1_1 V1_1 118.1(3)
N1_1 C2_1 C3_1 120.3(4)
N1_1 C2_1 C7_1 110.6(4)
C3_1 C2_1 C7_1 129.1(4)
C2_1 C3_1 C4_1 118.2(4)
C2_1 C3_1 H3_1 120.9
C4_1 C3_1 H3_1 120.9
C5_1 C4_1 C3_1 120.9(4)
C5_1 C4_1 H4_1 119.6
C3_1 C4_1 H4_1 119.6
C6_1 C5_1 C4_1 117.7(4)
C6_1 C5_1 H5_1 121.1
C4_1 C5_1 H5_1 121.1
N1_1 C6_1 C5_1 120.5(4)
N1_1 C6_1 C9_1 110.8(3)
C5_1 C6_1 C9_1 128.7(4)
O7_1 C7_1 O8_1 126.1(4)
O7_1 C7_1 C2_1 120.6(4)
O8_1 C7_1 C2_1 113.2(4)
C7_1 O8_1 V1_1 121.7(3)
O9_1 C9_1 O10_1 124.6(4)
O9_1 C9_1 C6_1 122.2(4)
O10_1 C9_1 C6_1 113.2(3)
C9_1 O10_1 V1_1 120.6(2)
O4_1 O3_1 V1_1 72.9(6)
O3_1 O4_1 C11_1 114.6(9)
O3_1 O4_1 V1_1 63.8(6)
C11_1 O4_1 V1_1 121.0(6)
O4_1 C11_1 C16_1 102.4(8)
O4_1 C11_1 C12_1 107.4(8)
C16_1 C11_1 C12_1 114.2(8)
O4_1 C11_1 H11_1 110.8
C16_1 C11_1 H11_1 110.8
C12_1 C11_1 H11_1 110.8
C11_1 C12_1 C13_1 109.2(8)
C11_1 C12_1 H12A_1 109.8
C13_1 C12_1 H12A_1 109.8
C11_1 C12_1 H12B_1 109.8
C13_1 C12_1 H12B_1 109.8
H12A_1 C12_1 H12B_1 108.3
C14_1 C13_1 C12_1 111.0(9)
C14_1 C13_1 H13A_1 109.4
C12_1 C13_1 H13A_1 109.4
C14_1 C13_1 H13B_1 109.4
C12_1 C13_1 H13B_1 109.4
H13A_1 C13_1 H13B_1 108.0
C13_1 C14_1 C15_1 111.5(9)
C13_1 C14_1 H14A_1 109.3
C15_1 C14_1 H14A_1 109.3
C13_1 C14_1 H14B_1 109.3
C15_1 C14_1 H14B_1 109.3
H14A_1 C14_1 H14B_1 108.0
C16_1 C15_1 C14_1 111.4(9)
C16_1 C15_1 H15A_1 109.4
C14_1 C15_1 H15A_1 109.4
C16_1 C15_1 H15B_1 109.4
C14_1 C15_1 H15B_1 109.4
H15A_1 C15_1 H15B_1 108.0
C11_1 C16_1 C15_1 109.2(8)
C11_1 C16_1 H16A_1 109.8
C15_1 C16_1 H16A_1 109.8
C11_1 C16_1 H16B_1 109.8
C15_1 C16_1 H16B_1 109.8
H16A_1 C16_1 H16B_1 108.3
O4B_1 O3B_1 V1_1 73.6(7)
O3B_1 O4B_1 C11B_1 113.3(9)
O3B_1 O4B_1 V1_1 63.4(7)
C11B_1 O4B_1 V1_1 124.8(7)
O4B_1 C11B_1 C16B_1 105.2(8)
O4B_1 C11B_1 C12B_1 109.0(8)
C16B_1 C11B_1 C12B_1 114.3(8)
O4B_1 C11B_1 H11B_1 109.4
C16B_1 C11B_1 H11B_1 109.4
C12B_1 C11B_1 H11B_1 109.4
C11B_1 C12B_1 C13B_1 113.5(9)
C11B_1 C12B_1 H12C_1 108.9
C13B_1 C12B_1 H12C_1 108.9
C11B_1 C12B_1 H12D_1 108.9
C13B_1 C12B_1 H12D_1 108.9
H12C_1 C12B_1 H12D_1 107.7
C14B_1 C13B_1 C12B_1 110.6(10)
C14B_1 C13B_1 H13C_1 109.5
C12B_1 C13B_1 H13C_1 109.5
C14B_1 C13B_1 H13D_1 109.5
C12B_1 C13B_1 H13D_1 109.5
H13C_1 C13B_1 H13D_1 108.1
C13B_1 C14B_1 C15B_1 112.7(11)
C13B_1 C14B_1 H14C_1 109.1
C15B_1 C14B_1 H14C_1 109.1
C13B_1 C14B_1 H14D_1 109.1
C15B_1 C14B_1 H14D_1 109.1
H14C_1 C14B_1 H14D_1 107.8
C14B_1 C15B_1 C16B_1 112.5(10)
C14B_1 C15B_1 H15C_1 109.1
C16B_1 C15B_1 H15C_1 109.1
C14B_1 C15B_1 H15D_1 109.1
C16B_1 C15B_1 H15D_1 109.1
H15C_1 C15B_1 H15D_1 107.8
C11B_1 C16B_1 C15B_1 110.4(9)
C11B_1 C16B_1 H16C_1 109.6
C15B_1 C16B_1 H16C_1 109.6
C11B_1 C16B_1 H16D_1 109.6
C15B_1 C16B_1 H16D_1 109.6
H16C_1 C16B_1 H16D_1 108.1
O1_2 V1_2 O3_2 100.52(14)
O1_2 V1_2 O10_2 95.94(14)
O3_2 V1_2 O10_2 126.00(12)
O1_2 V1_2 O8_2 96.41(14)
O3_2 V1_2 O8_2 79.72(11)
O10_2 V1_2 O8_2 148.50(11)
O1_2 V1_2 O4_2 96.93(13)
O3_2 V1_2 O4_2 43.19(10)
O10_2 V1_2 O4_2 84.12(11)
O8_2 V1_2 O4_2 122.82(11)
O1_2 V1_2 N1_2 93.48(14)
O3_2 V1_2 N1_2 152.26(13)
O10_2 V1_2 N1_2 75.44(13)
O8_2 V1_2 N1_2 74.98(12)
O4_2 V1_2 N1_2 157.91(12)
O1_2 V1_2 O2_2 174.43(14)
O3_2 V1_2 O2_2 85.03(13)
O10_2 V1_2 O2_2 80.25(12)
O8_2 V1_2 O2_2 85.00(12)
O4_2 V1_2 O2_2 86.77(12)
N1_2 V1_2 O2_2 81.66(13)
V1_2 O2_2 H2A_2 118(4)
V1_2 O2_2 H2B_2 117(3)
H2A_2 O2_2 H2B_2 110(4)
C6_2 N1_2 C2_2 121.9(3)
C6_2 N1_2 V1_2 118.7(3)
C2_2 N1_2 V1_2 119.3(3)
N1_2 C2_2 C3_2 120.6(4)
N1_2 C2_2 C7_2 110.2(3)
C3_2 C2_2 C7_2 129.2(4)
C2_2 C3_2 C4_2 118.8(4)
C2_2 C3_2 H3_2 120.6
C4_2 C3_2 H3_2 120.6
C3_2 C4_2 C5_2 119.9(4)
C3_2 C4_2 H4_2 120.1
C5_2 C4_2 H4_2 120.1
C6_2 C5_2 C4_2 118.6(4)
C6_2 C5_2 H5_2 120.7
C4_2 C5_2 H5_2 120.7
N1_2 C6_2 C5_2 120.0(4)
N1_2 C6_2 C9_2 110.6(3)
C5_2 C6_2 C9_2 129.4(4)
O7_2 C7_2 O8_2 125.9(4)
O7_2 C7_2 C2_2 120.8(4)
O8_2 C7_2 C2_2 113.4(3)
C7_2 O8_2 V1_2 121.6(2)
O9_2 C9_2 O10_2 125.7(4)
O9_2 C9_2 C6_2 121.4(4)
O10_2 C9_2 C6_2 112.8(4)
C9_2 O10_2 V1_2 121.9(3)
O4_2 O3_2 V1_2 73.47(16)
O3_2 O4_2 C11_2 110.0(3)
O3_2 O4_2 V1_2 63.34(15)
C11_2 O4_2 V1_2 120.1(2)
O4_2 C11_2 C16_2 105.1(3)
O4_2 C11_2 C12_2 108.5(3)
C16_2 C11_2 C12_2 111.4(4)
O4_2 C11_2 H11_2 110.6
C16_2 C11_2 H11_2 110.6
C12_2 C11_2 H11_2 110.6
C11_2 C12_2 C13_2 110.4(4)
C11_2 C12_2 H12A_2 109.6
C13_2 C12_2 H12A_2 109.6
C11_2 C12_2 H12B_2 109.6
C13_2 C12_2 H12B_2 109.6
H12A_2 C12_2 H12B_2 108.1
C14_2 C13_2 C12_2 109.2(4)
C14_2 C13_2 H13A_2 109.8
C12_2 C13_2 H13A_2 109.8
C14_2 C13_2 H13B_2 109.8
C12_2 C13_2 H13B_2 109.8
H13A_2 C13_2 H13B_2 108.3
C13_2 C14_2 C15_2 111.1(4)
C13_2 C14_2 H14A_2 109.4
C15_2 C14_2 H14A_2 109.4
C13_2 C14_2 H14B_2 109.4
C15_2 C14_2 H14B_2 109.4
H14A_2 C14_2 H14B_2 108.0
C14_2 C15_2 C16_2 110.4(4)
C14_2 C15_2 H15A_2 109.6
C16_2 C15_2 H15A_2 109.6
C14_2 C15_2 H15B_2 109.6
C16_2 C15_2 H15B_2 109.6
H15A_2 C15_2 H15B_2 108.1
C11_2 C16_2 C15_2 109.1(4)
C11_2 C16_2 H16A_2 109.9
C15_2 C16_2 H16A_2 109.9
C11_2 C16_2 H16B_2 109.9
C15_2 C16_2 H16B_2 109.9
H16A_2 C16_2 H16B_2 108.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1_1 O1_1 1.579(3)
V1_1 O3_1 1.885(13)
V1_1 O3B_1 1.897(16)
V1_1 O10_1 1.992(3)
V1_1 O8_1 2.007(3)
V1_1 O4_1 2.008(9)
V1_1 O4B_1 2.035(11)
V1_1 N1_1 2.057(3)
V1_1 O2_1 2.215(4)
O2_1 H2A_1 0.77(2)
O2_1 H2B_1 0.77(2)
N1_1 C2_1 1.325(5)
N1_1 C6_1 1.348(5)
C2_1 C3_1 1.375(6)
C2_1 C7_1 1.499(5)
C3_1 C4_1 1.398(6)
C3_1 H3_1 0.9500
C4_1 C5_1 1.382(6)
C4_1 H4_1 0.9500
C5_1 C6_1 1.376(5)
C5_1 H5_1 0.9500
C6_1 C9_1 1.496(5)
C7_1 O7_1 1.227(5)
C7_1 O8_1 1.280(5)
C9_1 O9_1 1.219(5)
C9_1 O10_1 1.299(5)
O3_1 O4_1 1.438(10)
O4_1 C11_1 1.480(10)
C11_1 C16_1 1.501(11)
C11_1 C12_1 1.504(10)
C11_1 H11_1 1.0000
C12_1 C13_1 1.539(11)
C12_1 H12A_1 0.9900
C12_1 H12B_1 0.9900
C13_1 C14_1 1.490(12)
C13_1 H13A_1 0.9900
C13_1 H13B_1 0.9900
C14_1 C15_1 1.530(13)
C14_1 H14A_1 0.9900
C14_1 H14B_1 0.9900
C15_1 C16_1 1.526(12)
C15_1 H15A_1 0.9900
C15_1 H15B_1 0.9900
C16_1 H16A_1 0.9900
C16_1 H16B_1 0.9900
O3B_1 O4B_1 1.445(11)
O4B_1 C11B_1 1.484(10)
C11B_1 C16B_1 1.487(11)
C11B_1 C12B_1 1.496(10)
C11B_1 H11B_1 1.0000
C12B_1 C13B_1 1.515(12)
C12B_1 H12C_1 0.9900
C12B_1 H12D_1 0.9900
C13B_1 C14B_1 1.490(13)
C13B_1 H13C_1 0.9900
C13B_1 H13D_1 0.9900
C14B_1 C15B_1 1.519(15)
C14B_1 H14C_1 0.9900
C14B_1 H14D_1 0.9900
C15B_1 C16B_1 1.537(13)
C15B_1 H15C_1 0.9900
C15B_1 H15D_1 0.9900
C16B_1 H16C_1 0.9900
C16B_1 H16D_1 0.9900
V1_2 O1_2 1.584(3)
V1_2 O3_2 1.878(3)
V1_2 O10_2 1.991(3)
V1_2 O8_2 2.009(3)
V1_2 O4_2 2.015(3)
V1_2 N1_2 2.067(3)
V1_2 O2_2 2.186(3)
O2_2 H2A_2 0.76(2)
O2_2 H2B_2 0.77(2)
N1_2 C6_2 1.333(5)
N1_2 C2_2 1.333(5)
C2_2 C3_2 1.365(5)
C2_2 C7_2 1.509(5)
C3_2 C4_2 1.377(6)
C3_2 H3_2 0.9500
C4_2 C5_2 1.391(6)
C4_2 H4_2 0.9500
C5_2 C6_2 1.374(5)
C5_2 H5_2 0.9500
C6_2 C9_2 1.511(6)
C7_2 O7_2 1.229(4)
C7_2 O8_2 1.286(5)
C9_2 O9_2 1.224(5)
C9_2 O10_2 1.293(5)
O3_2 O4_2 1.439(3)
O4_2 C11_2 1.497(4)
C11_2 C16_2 1.499(6)
C11_2 C12_2 1.503(5)
C11_2 H11_2 1.0000
C12_2 C13_2 1.523(6)
C12_2 H12A_2 0.9900
C12_2 H12B_2 0.9900
C13_2 C14_2 1.515(7)
C13_2 H13A_2 0.9900
C13_2 H13B_2 0.9900
C14_2 C15_2 1.516(7)
C14_2 H14A_2 0.9900
C14_2 H14B_2 0.9900
C15_2 C16_2 1.519(6)
C15_2 H15A_2 0.9900
C15_2 H15B_2 0.9900
C16_2 H16A_2 0.9900
C16_2 H16B_2 0.9900
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
C6_1 N1_1 C2_1 C3_1 -0.5(6)
V1_1 N1_1 C2_1 C3_1 178.0(3)
C6_1 N1_1 C2_1 C7_1 178.1(4)
V1_1 N1_1 C2_1 C7_1 -3.4(5)
N1_1 C2_1 C3_1 C4_1 -1.8(7)
C7_1 C2_1 C3_1 C4_1 179.9(5)
C2_1 C3_1 C4_1 C5_1 2.9(7)
C3_1 C4_1 C5_1 C6_1 -1.6(7)
C2_1 N1_1 C6_1 C5_1 1.8(6)
V1_1 N1_1 C6_1 C5_1 -176.7(3)
C2_1 N1_1 C6_1 C9_1 -178.0(4)
V1_1 N1_1 C6_1 C9_1 3.5(4)
C4_1 C5_1 C6_1 N1_1 -0.7(6)
C4_1 C5_1 C6_1 C9_1 179.1(4)
N1_1 C2_1 C7_1 O7_1 -179.7(4)
C3_1 C2_1 C7_1 O7_1 -1.3(8)
N1_1 C2_1 C7_1 O8_1 1.8(6)
C3_1 C2_1 C7_1 O8_1 -179.8(5)
O7_1 C7_1 O8_1 V1_1 -177.8(4)
C2_1 C7_1 O8_1 V1_1 0.6(6)
N1_1 C6_1 C9_1 O9_1 -174.7(4)
C5_1 C6_1 C9_1 O9_1 5.4(7)
N1_1 C6_1 C9_1 O10_1 5.3(5)
C5_1 C6_1 C9_1 O10_1 -174.6(4)
O9_1 C9_1 O10_1 V1_1 167.6(3)
C6_1 C9_1 O10_1 V1_1 -12.4(5)
O1_1 V1_1 O3_1 O4_1 -98.9(6)
O10_1 V1_1 O3_1 O4_1 10.8(9)
O8_1 V1_1 O3_1 O4_1 168.3(7)
N1_1 V1_1 O3_1 O4_1 132.9(6)
O2_1 V1_1 O3_1 O4_1 81.3(6)
V1_1 O3_1 O4_1 C11_1 114.0(7)
O3_1 O4_1 C11_1 C16_1 172.4(10)
V1_1 O4_1 C11_1 C16_1 -114.5(8)
O3_1 O4_1 C11_1 C12_1 51.8(11)
V1_1 O4_1 C11_1 C12_1 124.9(8)
O4_1 C11_1 C12_1 C13_1 169.3(9)
C16_1 C11_1 C12_1 C13_1 56.5(13)
C11_1 C12_1 C13_1 C14_1 -55.6(13)
C12_1 C13_1 C14_1 C15_1 56.6(14)
C13_1 C14_1 C15_1 C16_1 -56.3(15)
O4_1 C11_1 C16_1 C15_1 -171.7(9)
C12_1 C11_1 C16_1 C15_1 -56.0(13)
C14_1 C15_1 C16_1 C11_1 54.0(15)
O1_1 V1_1 O3B_1 O4B_1 -87.9(7)
O10_1 V1_1 O3B_1 O4B_1 9.7(10)
O8_1 V1_1 O3B_1 O4B_1 175.6(7)
N1_1 V1_1 O3B_1 O4B_1 160.1(10)
O2_1 V1_1 O3B_1 O4B_1 91.5(7)
V1_1 O3B_1 O4B_1 C11B_1 118.6(8)
O3B_1 O4B_1 C11B_1 C16B_1 -172.7(10)
V1_1 O4B_1 C11B_1 C16B_1 -99.8(9)
O3B_1 O4B_1 C11B_1 C12B_1 64.3(12)
V1_1 O4B_1 C11B_1 C12B_1 137.2(8)
O4B_1 C11B_1 C12B_1 C13B_1 65.4(11)
C16B_1 C11B_1 C12B_1 C13B_1 -52.0(12)
C11B_1 C12B_1 C13B_1 C14B_1 51.8(14)
C12B_1 C13B_1 C14B_1 C15B_1 -53.1(15)
C13B_1 C14B_1 C15B_1 C16B_1 54.2(16)
O4B_1 C11B_1 C16B_1 C15B_1 -69.0(11)
C12B_1 C11B_1 C16B_1 C15B_1 50.5(12)
C14B_1 C15B_1 C16B_1 C11B_1 -51.4(14)
C6_2 N1_2 C2_2 C3_2 4.3(6)
V1_2 N1_2 C2_2 C3_2 -172.7(3)
C6_2 N1_2 C2_2 C7_2 -175.7(4)
V1_2 N1_2 C2_2 C7_2 7.2(4)
N1_2 C2_2 C3_2 C4_2 -2.2(6)
C7_2 C2_2 C3_2 C4_2 177.8(4)
C2_2 C3_2 C4_2 C5_2 0.1(7)
C3_2 C4_2 C5_2 C6_2 0.0(7)
C2_2 N1_2 C6_2 C5_2 -4.2(6)
V1_2 N1_2 C6_2 C5_2 172.9(3)
C2_2 N1_2 C6_2 C9_2 176.2(4)
V1_2 N1_2 C6_2 C9_2 -6.7(5)
C4_2 C5_2 C6_2 N1_2 2.0(7)
C4_2 C5_2 C6_2 C9_2 -178.5(5)
N1_2 C2_2 C7_2 O7_2 177.4(4)
C3_2 C2_2 C7_2 O7_2 -2.6(7)
N1_2 C2_2 C7_2 O8_2 -2.4(5)
C3_2 C2_2 C7_2 O8_2 177.5(4)
O7_2 C7_2 O8_2 V1_2 176.6(3)
C2_2 C7_2 O8_2 V1_2 -3.6(5)
N1_2 C6_2 C9_2 O9_2 -176.8(4)
C5_2 C6_2 C9_2 O9_2 3.7(8)
N1_2 C6_2 C9_2 O10_2 2.1(5)
C5_2 C6_2 C9_2 O10_2 -177.4(4)
O9_2 C9_2 O10_2 V1_2 -177.5(4)
C6_2 C9_2 O10_2 V1_2 3.6(5)
O1_2 V1_2 O3_2 O4_2 88.93(19)
O10_2 V1_2 O3_2 O4_2 -16.4(2)
O8_2 V1_2 O3_2 O4_2 -176.38(18)
N1_2 V1_2 O3_2 O4_2 -152.0(3)
O2_2 V1_2 O3_2 O4_2 -90.58(17)
V1_2 O3_2 O4_2 C11_2 -114.5(2)
O3_2 O4_2 C11_2 C16_2 163.3(3)
V1_2 O4_2 C11_2 C16_2 93.3(3)
O3_2 O4_2 C11_2 C12_2 -77.5(4)
V1_2 O4_2 C11_2 C12_2 -147.5(3)
O4_2 C11_2 C12_2 C13_2 -174.5(4)
C16_2 C11_2 C12_2 C13_2 -59.3(5)
C11_2 C12_2 C13_2 C14_2 57.2(5)
C12_2 C13_2 C14_2 C15_2 -57.0(6)
C13_2 C14_2 C15_2 C16_2 58.0(7)
O4_2 C11_2 C16_2 C15_2 176.1(4)
C12_2 C11_2 C16_2 C15_2 58.9(5)
C14_2 C15_2 C16_2 C11_2 -57.7(6)
