#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002748.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_7002748
loop_
_publ_author_name
'Rubčić, Mirta'
'Milić, Dalibor'
'Horvat, Gordan'
'Đilović, Ivica'
'Galić, Nives'
'Tomišić, Vladislav'
'Cindrić, Marina'
_publ_section_title
;
 Vanadium-induced formation of thiadiazole and thiazoline compounds.
 Mononuclear and dinuclear oxovanadium(v) complexes with open-chain and
 cyclized thiosemicarbazone ligands
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9914
_journal_page_last               9923
_journal_paper_doi               10.1039/b913653c
_journal_year                    2009
_chemical_formula_moiety         'C34 H34 N6 O7 S2 V2, 0.5(C3 H8 O)'
_chemical_formula_sum            'C35.5 H38 N6 O7.5 S2 V2'
_chemical_formula_weight         834.72
_chemical_name_systematic
'μ-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]-dipropoxo-divanadium(V) propanol hemisolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.835(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4762(5)
_cell_length_b                   17.2325(7)
_cell_length_c                   17.0544(6)
_cell_measurement_reflns_used    3940
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      34.8212
_cell_measurement_theta_min      3.7252
_cell_volume                     3876.3(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16269
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6706
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0449P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3288
_reflns_number_total             6706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913653c.txt
_cod_data_source_block           3c_x_0.5_PrOH
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C35.50 H38 N6 O7.50 S2 V2'
_cod_database_code               7002748
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0219(3) 0.7377(2) 0.54280(19) 0.0585(10) Uani 1 1 d . . .
C12 C 0.1091(3) 0.7043(2) 0.59085(19) 0.0545(9) Uani 1 1 d . . .
C13 C 0.0982(3) 0.6634(2) 0.65988(18) 0.0615(10) Uani 1 1 d . . .
H13 H 0.1550 0.6404 0.6916 0.074 Uiso 1 1 calc R . .
C14 C 0.0068(4) 0.6567(3) 0.6815(2) 0.0809(12) Uani 1 1 d . . .
H14 H 0.0012 0.6298 0.7277 0.097 Uiso 1 1 calc R . .
C15 C -0.0776(3) 0.6904(3) 0.6339(2) 0.0845(13) Uani 1 1 d . . .
H15 H -0.1402 0.6860 0.6484 0.101 Uiso 1 1 calc R . .
C16 C -0.0707(3) 0.7298(2) 0.5661(2) 0.0762(12) Uani 1 1 d . . .
H16 H -0.1286 0.7517 0.5350 0.091 Uiso 1 1 calc R . .
C17 C 0.2048(3) 0.7096(2) 0.56573(18) 0.0520(9) Uani 1 1 d . . .
C18 C 0.3713(3) 0.6958(2) 0.53735(18) 0.0548(9) Uani 1 1 d . . .
C19 C 0.5284(3) 0.6171(2) 0.5603(2) 0.0733(11) Uani 1 1 d . . .
C21 C 0.4217(3) 0.7046(2) 0.2987(2) 0.0638(10) Uani 1 1 d . . .
C22 C 0.3286(3) 0.6804(2) 0.25105(18) 0.0562(9) Uani 1 1 d . . .
C23 C 0.3290(3) 0.6412(2) 0.17826(19) 0.0666(11) Uani 1 1 d . . .
H23 H 0.2680 0.6243 0.1471 0.080 Uiso 1 1 calc R . .
C24 C 0.4165(4) 0.6279(3) 0.1531(2) 0.0847(13) Uani 1 1 d . . .
H24 H 0.4151 0.6029 0.1045 0.102 Uiso 1 1 calc R . .
C25 C 0.5066(4) 0.6512(3) 0.1992(3) 0.0987(15) Uani 1 1 d . . .
H25 H 0.5665 0.6418 0.1818 0.118 Uiso 1 1 calc R . .
C26 C 0.5101(3) 0.6891(3) 0.2720(2) 0.0846(13) Uani 1 1 d . . .
H26 H 0.5723 0.7040 0.3029 0.102 Uiso 1 1 calc R . .
C27 C 0.2348(3) 0.6955(2) 0.27751(18) 0.0546(9) Uani 1 1 d . . .
C28 C 0.0707(3) 0.7010(2) 0.30999(18) 0.0560(9) Uani 1 1 d . . .
C29 C -0.1005(3) 0.6415(2) 0.2984(2) 0.0668(11) Uani 1 1 d . . .
C110 C 0.5283(3) 0.5888(3) 0.6365(3) 0.1001(16) Uani 1 1 d . . .
H110 H 0.4857 0.6096 0.6677 0.120 Uiso 1 1 calc R . .
C111 C 0.5945(4) 0.5279(4) 0.6647(3) 0.127(2) Uani 1 1 d . . .
H111 H 0.5952 0.5069 0.7151 0.153 Uiso 1 1 calc R . .
C112 C 0.6578(5) 0.4991(4) 0.6193(4) 0.136(2) Uani 1 1 d . . .
H112 H 0.7016 0.4588 0.6393 0.163 Uiso 1 1 calc R . .
C113 C 0.6583(4) 0.5275(3) 0.5461(4) 0.137(2) Uani 1 1 d . . .
H113 H 0.7024 0.5074 0.5158 0.164 Uiso 1 1 calc R . .
C114 C 0.5924(4) 0.5872(3) 0.5162(3) 0.1013(16) Uani 1 1 d . . .
H114 H 0.5920 0.6069 0.4653 0.122 Uiso 1 1 calc R . .
C214 C -0.1741(3) 0.6343(3) 0.3437(3) 0.0866(13) Uani 1 1 d . . .
H214 H -0.1719 0.6661 0.3881 0.104 Uiso 1 1 calc R . .
C213 C -0.2509(4) 0.5804(3) 0.3238(4) 0.1114(17) Uani 1 1 d . . .
H213 H -0.2998 0.5756 0.3549 0.134 Uiso 1 1 calc R . .
C212 C -0.2548(5) 0.5342(3) 0.2583(4) 0.119(2) Uani 1 1 d . . .
H212 H -0.3062 0.4976 0.2449 0.143 Uiso 1 1 calc R . .
C211 C -0.1844(5) 0.5415(3) 0.2129(4) 0.116(2) Uani 1 1 d . . .
H211 H -0.1874 0.5095 0.1686 0.139 Uiso 1 1 calc R . .
C210 C -0.1068(3) 0.5965(3) 0.2314(3) 0.1002(16) Uani 1 1 d . . .
H210 H -0.0601 0.6025 0.1985 0.120 Uiso 1 1 calc R . .
N11 N 0.2239(2) 0.75851(15) 0.51250(14) 0.0499(7) Uani 1 1 d . . .
N12 N 0.3184(2) 0.75157(16) 0.49545(14) 0.0530(7) Uani 1 1 d . . .
N13 N 0.4631(3) 0.6778(2) 0.52620(17) 0.0693(9) Uani 1 1 d D . .
H13N H 0.479(3) 0.695(2) 0.4854(15) 0.083 Uiso 1 1 d D . .
N21 N 0.2266(2) 0.74944(15) 0.32955(13) 0.0487(7) Uani 1 1 d . . .
N22 N 0.1329(2) 0.75375(15) 0.34843(14) 0.0501(7) Uani 1 1 d . . .
N23 N -0.0227(3) 0.69644(18) 0.32428(17) 0.0645(9) Uani 1 1 d D . .
H23N H -0.037(3) 0.7312(17) 0.3576(17) 0.077 Uiso 1 1 d D . .
O4 O 0.23785(16) 0.87598(12) 0.41648(11) 0.0553(6) Uani 1 1 d . . .
O11 O 0.12936(18) 0.90094(13) 0.52607(12) 0.0688(7) Uani 1 1 d . . .
O12 O 0.02428(16) 0.77382(13) 0.47380(12) 0.0587(6) Uani 1 1 d . . .
O13 O 0.02748(17) 0.89326(13) 0.37652(12) 0.0634(7) Uani 1 1 d DU . .
C31A C -0.0521(6) 0.9421(4) 0.3939(9) 0.077(2) Uani 0.729(6) 1 d PDU A 1
H31A H -0.0274 0.9950 0.4011 0.092 Uiso 0.729(6) 1 calc PR A 1
H31B H -0.0691 0.9253 0.4438 0.092 Uiso 0.729(6) 1 calc PR A 1
C32A C -0.1456(4) 0.9408(4) 0.3297(4) 0.0865(19) Uani 0.729(6) 1 d PDU A 1
H32A H -0.1282 0.9543 0.2789 0.104 Uiso 0.729(6) 1 calc PR A 1
H32B H -0.1928 0.9794 0.3414 0.104 Uiso 0.729(6) 1 calc PR A 1
C33A C -0.1970(19) 0.8611(12) 0.3221(9) 0.124(3) Uani 0.729(6) 1 d PDU A 1
H33A H -0.1555 0.8245 0.3011 0.186 Uiso 0.729(6) 1 calc PR A 1
H33B H -0.2620 0.8647 0.2866 0.186 Uiso 0.729(6) 1 calc PR A 1
H33C H -0.2056 0.8442 0.3739 0.186 Uiso 0.729(6) 1 calc PR A 1
C31B C -0.0397(15) 0.9554(9) 0.383(3) 0.077(2) Uani 0.271(6) 1 d PDU A 2
H31C H -0.0531 0.9856 0.3336 0.092 Uiso 0.271(6) 1 calc PR A 2
H31D H -0.0105 0.9894 0.4268 0.092 Uiso 0.271(6) 1 calc PR A 2
C32B C -0.1351(10) 0.9197(10) 0.3971(11) 0.0865(19) Uani 0.271(6) 1 d PDU A 2
H32C H -0.1782 0.9597 0.4123 0.104 Uiso 0.271(6) 1 calc PR A 2
H32D H -0.1191 0.8829 0.4409 0.104 Uiso 0.271(6) 1 calc PR A 2
C33B C -0.191(5) 0.879(4) 0.323(2) 0.124(3) Uani 0.271(6) 1 d PDU A 2
H33D H -0.1983 0.9135 0.2779 0.186 Uiso 0.271(6) 1 calc PR A 2
H33E H -0.2564 0.8630 0.3304 0.186 Uiso 0.271(6) 1 calc PR A 2
H33F H -0.1528 0.8340 0.3129 0.186 Uiso 0.271(6) 1 calc PR A 2
O21 O 0.35006(18) 0.87212(14) 0.30477(12) 0.0699(7) Uani 1 1 d . . .
O22 O 0.42582(17) 0.74068(13) 0.36912(12) 0.0614(7) Uani 1 1 d . . .
O23 O 0.44946(18) 0.87060(14) 0.45517(13) 0.0686(7) Uani 1 1 d DU . .
C41A C 0.5343(4) 0.9091(4) 0.4331(5) 0.094(2) Uani 0.842(8) 1 d PDU C 1
H41A H 0.5142 0.9610 0.4144 0.113 Uiso 0.842(8) 1 calc PR C 1
H41B H 0.5538 0.8811 0.3892 0.113 Uiso 0.842(8) 1 calc PR C 1
C42A C 0.6224(7) 0.9141(7) 0.5004(7) 0.129(3) Uani 0.842(8) 1 d PDU C 1
H42A H 0.6029 0.9420 0.5443 0.155 Uiso 0.842(8) 1 calc PR C 1
H42B H 0.6759 0.9433 0.4836 0.155 Uiso 0.842(8) 1 calc PR C 1
C43A C 0.6633(5) 0.8337(5) 0.5302(5) 0.148(3) Uani 0.842(8) 1 d PDU C 1
H43A H 0.6168 0.8093 0.5583 0.223 Uiso 0.842(8) 1 calc PR C 1
H43B H 0.7281 0.8395 0.5656 0.223 Uiso 0.842(8) 1 calc PR C 1
H43C H 0.6704 0.8022 0.4852 0.223 Uiso 0.842(8) 1 calc PR C 1
C41B C 0.5495(15) 0.880(3) 0.438(3) 0.094(2) Uani 0.158(8) 1 d PDU C 2
H41C H 0.5490 0.9240 0.4030 0.113 Uiso 0.158(8) 1 calc PR C 2
H41D H 0.5658 0.8341 0.4105 0.113 Uiso 0.158(8) 1 calc PR C 2
C42B C 0.630(4) 0.892(5) 0.512(3) 0.129(3) Uani 0.158(8) 1 d PDU C 2
H42C H 0.6574 0.8419 0.5320 0.155 Uiso 0.158(8) 1 calc PR C 2
H42D H 0.6018 0.9169 0.5527 0.155 Uiso 0.158(8) 1 calc PR C 2
C43B C 0.716(2) 0.942(2) 0.492(2) 0.148(3) Uani 0.158(8) 1 d PDU C 2
H43D H 0.7221 0.9330 0.4378 0.223 Uiso 0.158(8) 1 calc PR C 2
H43E H 0.7787 0.9286 0.5276 0.223 Uiso 0.158(8) 1 calc PR C 2
H43F H 0.7012 0.9957 0.4990 0.223 Uiso 0.158(8) 1 calc PR C 2
S1 S 0.30660(7) 0.64986(6) 0.60266(5) 0.0653(3) Uani 1 1 d . . .
S2 S 0.12370(7) 0.64409(5) 0.24629(5) 0.0641(3) Uani 1 1 d . . .
V1 V 0.12373(4) 0.84815(3) 0.44922(3) 0.05387(19) Uani 1 1 d . A .
V2 V 0.34488(5) 0.83009(3) 0.38672(3) 0.0568(2) Uani 1 1 d . C .
O5 O 0.0772(16) 0.5300(8) 0.4275(8) 0.206(4) Uani 0.50 1 d PDU D -1
H5 H 0.0677 0.5765 0.4187 0.310 Uiso 0.50 1 calc PR D -1
C51 C 0.051(2) 0.5110(13) 0.5001(12) 0.206(4) Uani 0.50 1 d PDU D -1
H51A H 0.0862 0.5464 0.5406 0.248 Uiso 0.50 1 calc PR D -1
H51B H 0.0764 0.4593 0.5150 0.248 Uiso 0.50 1 calc PR D -1
C52 C -0.055(2) 0.5123(11) 0.5039(14) 0.206(4) Uani 0.50 1 d PDU D -1
H52A H -0.0960 0.5076 0.4502 0.248 Uiso 0.50 1 calc PR D -1
H52B H -0.0712 0.5618 0.5256 0.248 Uiso 0.50 1 calc PR D -1
C53 C -0.083(2) 0.4480(12) 0.5551(12) 0.206(4) Uani 0.50 1 d PDU D -1
H53A H -0.1546 0.4491 0.5532 0.310 Uiso 0.50 1 calc PR D -1
H53B H -0.0471 0.4548 0.6094 0.310 Uiso 0.50 1 calc PR D -1
H53C H -0.0648 0.3990 0.5353 0.310 Uiso 0.50 1 calc PR D -1
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'
S S 0.1246 0.1234 '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
O12 C11 C16 118.8(3) . . ?
O12 C11 C12 122.3(4) . . ?
C16 C11 C12 118.8(4) . . ?
C13 C12 C11 118.3(4) . . ?
C13 C12 C17 122.3(3) . . ?
C11 C12 C17 119.3(3) . . ?
C14 C13 C12 121.7(4) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C15 119.1(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C11 120.9(4) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
N11 C17 C12 124.4(3) . . ?
N11 C17 S1 112.5(3) . . ?
C12 C17 S1 123.0(3) . . ?
N12 C18 N13 120.7(3) . . ?
N12 C18 S1 113.2(3) . . ?
N13 C18 S1 126.2(3) . . ?
C114 C19 C110 120.5(4) . . ?
C114 C19 N13 117.8(4) . . ?
C110 C19 N13 121.7(4) . . ?
O22 C21 C26 120.1(4) . . ?
O22 C21 C22 121.5(4) . . ?
C26 C21 C22 118.4(4) . . ?
C21 C22 C23 119.0(4) . . ?
C21 C22 C27 119.7(3) . . ?
C23 C22 C27 121.3(4) . . ?
C24 C23 C22 121.3(4) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 119.7(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 121.0(4) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 120.5(4) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
N21 C27 C22 122.7(3) . . ?
N21 C27 S2 112.7(3) . . ?
C22 C27 S2 124.6(3) . . ?
N22 C28 N23 118.6(3) . . ?
N22 C28 S2 113.8(3) . . ?
N23 C28 S2 127.6(3) . . ?
C210 C29 C214 119.1(4) . . ?
C210 C29 N23 123.7(4) . . ?
C214 C29 N23 117.2(4) . . ?
C19 C110 C111 117.6(5) . . ?
C19 C110 H110 121.2 . . ?
C111 C110 H110 121.2 . . ?
C112 C111 C110 120.6(5) . . ?
C112 C111 H111 119.7 . . ?
C110 C111 H111 119.7 . . ?
C113 C112 C111 121.4(5) . . ?
C113 C112 H112 119.3 . . ?
C111 C112 H112 119.3 . . ?
C112 C113 C114 119.2(5) . . ?
C112 C113 H113 120.4 . . ?
C114 C113 H113 120.4 . . ?
C19 C114 C113 120.7(5) . . ?
C19 C114 H114 119.7 . . ?
C113 C114 H114 119.7 . . ?
C213 C214 C29 120.7(5) . . ?
C213 C214 H214 119.6 . . ?
C29 C214 H214 119.6 . . ?
C212 C213 C214 119.7(6) . . ?
C212 C213 H213 120.2 . . ?
C214 C213 H213 120.2 . . ?
C211 C212 C213 120.2(5) . . ?
C211 C212 H212 119.9 . . ?
C213 C212 H212 119.9 . . ?
C212 C211 C210 121.0(5) . . ?
C212 C211 H211 119.5 . . ?
C210 C211 H211 119.5 . . ?
C29 C210 C211 119.2(5) . . ?
C29 C210 H210 120.4 . . ?
C211 C210 H210 120.4 . . ?
C17 N11 N12 114.7(3) . . ?
C17 N11 V1 127.6(2) . . ?
N12 N11 V1 117.7(2) . . ?
C18 N12 N11 111.9(3) . . ?
C18 N12 V2 133.4(2) . . ?
N11 N12 V2 114.23(18) . . ?
C18 N13 C19 129.4(3) . . ?
C18 N13 H13N 117(3) . . ?
C19 N13 H13N 111(3) . . ?
C27 N21 N22 114.2(3) . . ?
C27 N21 V2 126.8(2) . . ?
N22 N21 V2 118.96(19) . . ?
C28 N22 N21 111.7(3) . . ?
C28 N22 V1 135.0(3) . . ?
N21 N22 V1 113.13(19) . . ?
C28 N23 C29 130.5(3) . . ?
C28 N23 H23N 115(2) . . ?
C29 N23 H23N 115(2) . . ?
V1 O4 V2 138.64(13) . . ?
C11 O12 V1 129.2(2) . . ?
C31B O13 V1 131.5(18) . . ?
C31A O13 V1 125.4(6) . . ?
O13 C31A C32A 113.1(9) . . ?
O13 C31A H31A 109.0 . . ?
C32A C31A H31A 109.0 . . ?
O13 C31A H31B 109.0 . . ?
C32A C31A H31B 109.0 . . ?
H31A C31A H31B 107.8 . . ?
C31A C32A C33A 112.1(10) . . ?
C31A C32A H32A 109.2 . . ?
C33A C32A H32A 109.2 . . ?
C31A C32A H32B 109.2 . . ?
C33A C32A H32B 109.2 . . ?
H32A C32A H32B 107.9 . . ?
O13 C31B C32B 106.6(11) . . ?
O13 C31B H31C 110.4 . . ?
C32B C31B H31C 110.4 . . ?
O13 C31B H31D 110.4 . . ?
C32B C31B H31D 110.4 . . ?
H31C C31B H31D 108.6 . . ?
C31B C32B C33B 110.6(15) . . ?
C31B C32B H32C 109.5 . . ?
C33B C32B H32C 109.5 . . ?
C31B C32B H32D 109.5 . . ?
C33B C32B H32D 109.5 . . ?
H32C C32B H32D 108.1 . . ?
C32B C33B H33D 109.5 . . ?
C32B C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C32B C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C21 O22 V2 125.62(19) . . ?
C41A O23 V2 125.1(4) . . ?
C41B O23 V2 124(2) . . ?
O23 C41A C42A 112.3(6) . . ?
O23 C41A H41A 109.1 . . ?
C42A C41A H41A 109.1 . . ?
O23 C41A H41B 109.1 . . ?
C42A C41A H41B 109.1 . . ?
H41A C41A H41B 107.9 . . ?
C41A C42A C43A 112.4(7) . . ?
C41A C42A H42A 109.1 . . ?
C43A C42A H42A 109.1 . . ?
C41A C42A H42B 109.1 . . ?
C43A C42A H42B 109.1 . . ?
H42A C42A H42B 107.9 . . ?
C42A C43A H43A 109.5 . . ?
C42A C43A H43B 109.5 . . ?
H43A C43A H43B 109.5 . . ?
C42A C43A H43C 109.5 . . ?
H43A C43A H43C 109.5 . . ?
H43B C43A H43C 109.5 . . ?
O23 C41B C42B 114(3) . . ?
O23 C41B H41C 108.8 . . ?
C42B C41B H41C 108.8 . . ?
O23 C41B H41D 108.8 . . ?
C42B C41B H41D 108.8 . . ?
H41C C41B H41D 107.7 . . ?
C41B C42B C43B 111(2) . . ?
C41B C42B H42C 109.5 . . ?
C43B C42B H42C 109.5 . . ?
C41B C42B H42D 109.5 . . ?
C43B C42B H42D 109.5 . . ?
H42C C42B H42D 108.1 . . ?
C42B C43B H43D 109.5 . . ?
C42B C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C42B C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C17 S1 C18 87.72(18) . . ?
C28 S2 C27 87.63(19) . . ?
O11 V1 O13 103.29(11) . . ?
O11 V1 O4 101.77(12) . . ?
O13 V1 O4 102.35(10) . . ?
O11 V1 O12 96.73(11) . . ?
O13 V1 O12 90.10(10) . . ?
O4 V1 O12 154.53(10) . . ?
O11 V1 N11 94.44(10) . . ?
O13 V1 N11 160.29(10) . . ?
O4 V1 N11 82.03(10) . . ?
O12 V1 N11 79.21(10) . . ?
O11 V1 N22 170.32(10) . . ?
O13 V1 N22 86.21(9) . . ?
O4 V1 N22 77.61(10) . . ?
O12 V1 N22 81.22(10) . . ?
N11 V1 N22 75.89(9) . . ?
O21 V2 O23 103.11(12) . . ?
O21 V2 O4 103.26(11) . . ?
O23 V2 O4 102.40(10) . . ?
O21 V2 O22 95.63(11) . . ?
O23 V2 O22 91.05(11) . . ?
O4 V2 O22 153.49(11) . . ?
O21 V2 N21 93.26(11) . . ?
O23 V2 N21 161.63(10) . . ?
O4 V2 N21 81.51(10) . . ?
O22 V2 N21 78.96(10) . . ?
O21 V2 N12 170.11(11) . . ?
O23 V2 N12 86.39(10) . . ?
O4 V2 N12 76.94(10) . . ?
O22 V2 N12 81.29(10) . . ?
N21 V2 N12 76.94(9) . . ?
C51 O5 H5 109.5 . . ?
O5 C51 C52 118.1(14) . . ?
O5 C51 H51A 107.8 . . ?
C52 C51 H51A 107.8 . . ?
O5 C51 H51B 107.8 . . ?
C52 C51 H51B 107.8 . . ?
H51A C51 H51B 107.1 . . ?
C51 C52 C53 112.3(13) . . ?
C51 C52 H52A 109.1 . . ?
C53 C52 H52A 109.1 . . ?
C51 C52 H52B 109.1 . . ?
C53 C52 H52B 109.1 . . ?
H52A C52 H52B 107.9 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 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
C11 O12 1.337(4) . ?
C11 C16 1.393(5) . ?
C11 C12 1.410(5) . ?
C12 C13 1.405(5) . ?
C12 C17 1.443(5) . ?
C13 C14 1.362(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.359(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 N11 1.303(4) . ?
C17 S1 1.728(3) . ?
C18 N12 1.317(4) . ?
C18 N13 1.326(4) . ?
C18 S1 1.739(4) . ?
C19 C114 1.358(5) . ?
C19 C110 1.388(5) . ?
C19 N13 1.412(5) . ?
C21 O22 1.343(4) . ?
C21 C26 1.387(5) . ?
C21 C22 1.410(5) . ?
C22 C23 1.414(4) . ?
C22 C27 1.451(5) . ?
C23 C24 1.354(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.365(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.395(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 N21 1.305(4) . ?
C27 S2 1.727(4) . ?
C28 N22 1.316(4) . ?
C28 N23 1.333(4) . ?
C28 S2 1.723(4) . ?
C29 C210 1.370(5) . ?
C29 C214 1.383(6) . ?
C29 N23 1.414(5) . ?
C110 C111 1.398(6) . ?
C110 H110 0.9300 . ?
C111 C112 1.359(7) . ?
C111 H111 0.9300 . ?
C112 C113 1.342(7) . ?
C112 H112 0.9300 . ?
C113 C114 1.386(6) . ?
C113 H113 0.9300 . ?
C114 H114 0.9300 . ?
C214 C213 1.380(6) . ?
C214 H214 0.9300 . ?
C213 C212 1.365(7) . ?
C213 H213 0.9300 . ?
C212 C211 1.348(7) . ?
C212 H212 0.9300 . ?
C211 C210 1.398(7) . ?
C211 H211 0.9300 . ?
C210 H210 0.9300 . ?
N11 N12 1.368(3) . ?
N11 V1 2.185(3) . ?
N12 V2 2.381(3) . ?
N13 H13N 0.828(18) . ?
N21 N22 1.368(3) . ?
N21 V2 2.188(3) . ?
N22 V1 2.388(3) . ?
N23 H23N 0.873(18) . ?
O4 V1 1.805(2) . ?
O4 V2 1.806(2) . ?
O11 V1 1.584(2) . ?
O12 V1 1.960(2) . ?
O13 C31B 1.420(10) . ?
O13 C31A 1.441(6) . ?
O13 V1 1.779(2) . ?
C31A C32A 1.490(12) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C32A C33A 1.531(14) . ?
C32A H32A 0.9700 . ?
C32A H32B 0.9700 . ?
C33A H33A 0.9600 . ?
C33A H33B 0.9600 . ?
C33A H33C 0.9600 . ?
C31B C32B 1.490(10) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C32B C33B 1.507(10) . ?
C32B H32C 0.9700 . ?
C32B H32D 0.9700 . ?
C33B H33D 0.9600 . ?
C33B H33E 0.9600 . ?
C33B H33F 0.9600 . ?
O21 V2 1.588(2) . ?
O22 V2 1.946(2) . ?
O23 C41A 1.437(5) . ?
O23 C41B 1.442(10) . ?
O23 V2 1.778(2) . ?
C41A C42A 1.475(6) . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C42A C43A 1.538(13) . ?
C42A H42A 0.9700 . ?
C42A H42B 0.9700 . ?
C43A H43A 0.9600 . ?
C43A H43B 0.9600 . ?
C43A H43C 0.9600 . ?
C41B C42B 1.493(18) . ?
C41B H41C 0.9700 . ?
C41B H41D 0.9700 . ?
C42B C43B 1.53(2) . ?
C42B H42C 0.9700 . ?
C42B H42D 0.9700 . ?
C43B H43D 0.9600 . ?
C43B H43E 0.9600 . ?
C43B H43F 0.9600 . ?
O5 C51 1.396(10) . ?
O5 H5 0.8200 . ?
C51 C52 1.445(8) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.504(10) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
