#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309185.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_4309185
loop_
_publ_author_name
'Stanislav Groysman'
'Israel Goldberg'
'Zeev Goldschmidt'
'Moshe Kol'
_publ_section_title
;
Vanadium(III) and Vanadium(V) Amine Tris(Phenolate) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5073
_journal_page_last               5080
_journal_paper_doi               10.1021/ic050084i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C29 H30 Cl6 N O7 V'
_chemical_formula_weight         768.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 101.2230(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.5420(4)
_cell_length_b                   14.6950(4)
_cell_length_c                   23.9320(5)
_cell_measurement_temperature    110(2)
_cell_volume                     6396.2(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B. V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg Phi and Omega Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1224
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11759
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.8470
_exptl_absorpt_correction_T_min  0.7827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing (1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         11759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0582P)²+3.2773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                6825
_reflns_number_total             11759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050084isi20050518_103020_5.cif
_cod_data_source_block           mk134
_cod_original_formula_sum        'C29 H30 Cl6 N  O7 V'
_cod_database_code               4309185
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
V1 V 0.19016(5) 0.39883(6) -0.00818(3) 0.0221(2) Uani 1 1 d . . .
O2 O 0.15305(18) 0.3093(2) 0.03302(14) 0.0254(8) Uani 1 1 d . . .
O3 O 0.28842(18) 0.3763(2) 0.01959(14) 0.0239(8) Uani 1 1 d . . .
O4 O 0.20838(18) 0.5151(2) -0.03724(13) 0.0238(8) Uani 1 1 d . . .
O5 O 0.17946(18) 0.3447(2) -0.06703(14) 0.0273(9) Uani 1 1 d . . .
O6 O 0.0828(2) 0.4483(3) -0.02328(17) 0.0275(9) Uani 1 1 d . . .
H6A H 0.053(3) 0.413(4) -0.028(2) 0.024(18) Uiso 1 1 d . . .
H6B H 0.076(3) 0.485(4) -0.050(3) 0.05(2) Uiso 1 1 d . . .
N7 N 0.1962(2) 0.4849(3) 0.08003(16) 0.0190(9) Uani 1 1 d . . .
C8 C 0.1360(3) 0.2938(3) 0.0836(2) 0.0234(12) Uani 1 1 d . . .
C9 C 0.1242(3) 0.2029(4) 0.0983(2) 0.0273(12) Uani 1 1 d . . .
C10 C 0.1045(3) 0.1795(4) 0.1493(2) 0.0312(13) Uani 1 1 d . . .
H10 H 0.0967 0.1179 0.1584 0.037 Uiso 1 1 calc R . .
C11 C 0.0967(3) 0.2496(4) 0.1866(2) 0.0313(13) Uani 1 1 d . . .
C12 C 0.1090(3) 0.3390(4) 0.1743(2) 0.0279(13) Uani 1 1 d . . .
H12 H 0.1048 0.3850 0.2014 0.033 Uiso 1 1 calc R . .
C13 C 0.1276(3) 0.3631(3) 0.1223(2) 0.0228(12) Uani 1 1 d . . .
C14 C 0.1323(3) 0.4607(3) 0.1065(2) 0.0258(12) Uani 1 1 d . . .
H14A H 0.1346 0.4981 0.1413 0.031 Uiso 1 1 calc R . .
H14B H 0.0865 0.4773 0.0797 0.031 Uiso 1 1 calc R . .
C15 C 0.2646(3) 0.4680(3) 0.1224(2) 0.0221(12) Uani 1 1 d . . .
H15A H 0.2602 0.4078 0.1400 0.026 Uiso 1 1 calc R . .
H15B H 0.2678 0.5142 0.1529 0.026 Uiso 1 1 calc R . .
C16 C 0.1879(3) 0.5843(3) 0.0666(2) 0.0234(12) Uani 1 1 d . . .
H16A H 0.1879 0.6186 0.1022 0.028 Uiso 1 1 calc R . .
H16B H 0.1400 0.5948 0.0409 0.028 Uiso 1 1 calc R . .
C17 C 0.3443(3) 0.4209(3) 0.05260(19) 0.0202(11) Uani 1 1 d . . .
C18 C 0.4143(3) 0.4156(3) 0.03859(19) 0.0202(11) Uani 1 1 d . . .
C19 C 0.4745(3) 0.4609(3) 0.0702(2) 0.0218(12) Uani 1 1 d . . .
H19 H 0.5215 0.4575 0.0601 0.026 Uiso 1 1 calc R . .
C20 C 0.4638(3) 0.5110(3) 0.1168(2) 0.0209(11) Uani 1 1 d . . .
C21 C 0.3952(3) 0.5156(3) 0.1323(2) 0.0230(12) Uani 1 1 d . . .
H21 H 0.3894 0.5504 0.1646 0.028 Uiso 1 1 calc R . .
C22 C 0.3356(3) 0.4698(3) 0.1011(2) 0.0207(12) Uani 1 1 d . . .
C23 C 0.2555(3) 0.5788(3) -0.0127(2) 0.0202(11) Uani 1 1 d . . .
C24 C 0.3131(3) 0.6077(3) -0.03863(19) 0.0212(11) Uani 1 1 d . . .
C25 C 0.3635(3) 0.6726(3) -0.0141(2) 0.0231(12) Uani 1 1 d . . .
H25 H 0.4029 0.6902 -0.0319 0.028 Uiso 1 1 calc R . .
C26 C 0.3552(3) 0.7113(4) 0.0371(2) 0.0253(12) Uani 1 1 d . . .
C27 C 0.2973(3) 0.6856(3) 0.0629(2) 0.0243(12) Uani 1 1 d . . .
H27 H 0.2915 0.7138 0.0975 0.029 Uiso 1 1 calc R . .
C28 C 0.2487(3) 0.6200(3) 0.0388(2) 0.0213(11) Uani 1 1 d . . .
Cl29 Cl 0.13348(8) 0.11721(9) 0.05070(6) 0.0374(4) Uani 1 1 d . . .
Cl30 Cl 0.06703(8) 0.22178(11) 0.24966(6) 0.0412(4) Uani 1 1 d . . .
Cl31 Cl 0.42700(7) 0.35177(9) -0.01947(5) 0.0274(3) Uani 1 1 d . . .
Cl32 Cl 0.53752(7) 0.56960(9) 0.15747(5) 0.0289(3) Uani 1 1 d . . .
Cl33 Cl 0.32332(7) 0.55786(9) -0.10240(5) 0.0288(3) Uani 1 1 d . . .
Cl34 Cl 0.41802(8) 0.79341(10) 0.06754(6) 0.0380(4) Uani 1 1 d . . .
V35 V 0.33563(5) 0.42763(6) 0.29141(3) 0.0229(2) Uani 1 1 d . . .
O36 O 0.4352(2) 0.3795(4) 0.33780(17) 0.0333(10) Uani 1 1 d . . .
H36A H 0.460(3) 0.357(3) 0.311(2) 0.025(14) Uiso 1 1 d . . .
H36B H 0.454(4) 0.429(5) 0.346(3) 0.07(3) Uiso 1 1 d . . .
O37 O 0.3721(2) 0.4945(2) 0.25243(14) 0.0305(9) Uani 1 1 d . . .
O38 O 0.33604(18) 0.5112(2) 0.34958(13) 0.0263(8) Uani 1 1 d . . .
O39 O 0.33687(18) 0.3244(2) 0.24711(13) 0.0251(8) Uani 1 1 d . . .
O40 O 0.23409(18) 0.4475(2) 0.26299(13) 0.0247(8) Uani 1 1 d . . .
N41 N 0.2932(2) 0.3276(3) 0.35755(16) 0.0221(10) Uani 1 1 d . . .
C42 C 0.3132(3) 0.2385(3) 0.2446(2) 0.0215(11) Uani 1 1 d . . .
C43 C 0.3036(3) 0.1911(4) 0.1932(2) 0.0269(13) Uani 1 1 d . . .
C44 C 0.2765(3) 0.1036(4) 0.1874(2) 0.0296(13) Uani 1 1 d . . .
H44 H 0.2706 0.0726 0.1519 0.036 Uiso 1 1 calc R . .
C45 C 0.2583(3) 0.0624(4) 0.2342(2) 0.0301(13) Uani 1 1 d . . .
C46 C 0.2690(3) 0.1050(4) 0.2868(2) 0.0260(12) Uani 1 1 d . . .
H46 H 0.2567 0.0746 0.3187 0.031 Uiso 1 1 calc R . .
C47 C 0.2977(3) 0.1920(4) 0.2927(2) 0.0255(12) Uani 1 1 d . . .
C48 C 0.3195(3) 0.2327(3) 0.3513(2) 0.0240(12) Uani 1 1 d . . .
H48A H 0.3003 0.1931 0.3785 0.029 Uiso 1 1 calc R . .
H48B H 0.3738 0.2322 0.3621 0.029 Uiso 1 1 calc R . .
C49 C 0.2114(3) 0.3248(3) 0.3469(2) 0.0266(13) Uani 1 1 d . . .
H49A H 0.1960 0.2926 0.3790 0.032 Uiso 1 1 calc R . .
H49B H 0.1938 0.2887 0.3120 0.032 Uiso 1 1 calc R . .
C50 C 0.3236(3) 0.3540(4) 0.4181(2) 0.0270(13) Uani 1 1 d . . .
H50A H 0.3779 0.3489 0.4249 0.032 Uiso 1 1 calc R . .
H50B H 0.3057 0.3099 0.4436 0.032 Uiso 1 1 calc R . .
C51 C 0.1877(3) 0.4731(3) 0.2964(2) 0.0232(12) Uani 1 1 d . . .
C52 C 0.1507(3) 0.5567(4) 0.2893(2) 0.0271(12) Uani 1 1 d . . .
C53 C 0.1054(3) 0.5857(4) 0.3254(2) 0.0309(13) Uani 1 1 d . . .
H53 H 0.0807 0.6426 0.3199 0.037 Uiso 1 1 calc R . .
C54 C 0.0972(3) 0.5289(4) 0.3698(2) 0.0322(14) Uani 1 1 d . . .
C55 C 0.1299(3) 0.4447(4) 0.3769(2) 0.0274(13) Uani 1 1 d . . .
H55 H 0.1220 0.4064 0.4071 0.033 Uiso 1 1 calc R . .
C56 C 0.1743(3) 0.4154(3) 0.3400(2) 0.0246(12) Uani 1 1 d . . .
C57 C 0.3106(3) 0.5214(4) 0.3977(2) 0.0236(12) Uani 1 1 d . . .
C58 C 0.2872(3) 0.6083(3) 0.4120(2) 0.0253(12) Uani 1 1 d . . .
C59 C 0.2635(3) 0.6233(4) 0.4620(2) 0.0268(12) Uani 1 1 d . . .
H59 H 0.2472 0.6819 0.4708 0.032 Uiso 1 1 calc R . .
C60 C 0.2638(3) 0.5512(4) 0.4995(2) 0.0272(13) Uani 1 1 d . . .
C61 C 0.2818(3) 0.4639(4) 0.4854(2) 0.0280(13) Uani 1 1 d . . .
H61 H 0.2790 0.4148 0.5107 0.034 Uiso 1 1 calc R . .
C62 C 0.3040(3) 0.4485(3) 0.4344(2) 0.0214(11) Uani 1 1 d . . .
Cl63 Cl 0.32564(8) 0.24371(9) 0.13355(5) 0.0320(3) Uani 1 1 d . . .
Cl64 Cl 0.22159(9) -0.04775(10) 0.22613(6) 0.0430(4) Uani 1 1 d . . .
Cl65 Cl 0.16421(9) 0.62884(10) 0.23417(6) 0.0382(4) Uani 1 1 d . . .
Cl66 Cl 0.04577(9) 0.56626(11) 0.41946(7) 0.0472(4) Uani 1 1 d . . .
Cl67 Cl 0.28787(8) 0.69743(9) 0.36473(5) 0.0329(3) Uani 1 1 d . . .
Cl68 Cl 0.24003(8) 0.57345(10) 0.56548(6) 0.0372(4) Uani 1 1 d . . .
O69 O 0.0468(2) 0.9432(3) 0.38701(16) 0.0373(10) Uani 1 1 d . . .
C70 C 0.0464(4) 0.9973(5) 0.3361(2) 0.0483(17) Uani 1 1 d . . .
H70A H 0.0836 1.0463 0.3440 0.058 Uiso 1 1 calc R . .
H70B H -0.0025 1.0253 0.3230 0.058 Uiso 1 1 calc R . .
C71 C 0.0639(4) 0.9342(5) 0.2922(3) 0.0524(18) Uani 1 1 d . . .
H71A H 0.0880 0.9665 0.2644 0.063 Uiso 1 1 calc R . .
H71B H 0.0193 0.9030 0.2716 0.063 Uiso 1 1 calc R . .
C72 C 0.1167(4) 0.8674(4) 0.3283(3) 0.0484(17) Uani 1 1 d . . .
H72A H 0.1173 0.8080 0.3089 0.058 Uiso 1 1 calc R . .
H72B H 0.1673 0.8921 0.3374 0.058 Uiso 1 1 calc R . .
C73 C 0.0842(3) 0.8590(4) 0.3809(3) 0.0454(16) Uani 1 1 d . . .
H73A H 0.0491 0.8075 0.3769 0.054 Uiso 1 1 calc R . .
H73B H 0.1234 0.8482 0.4147 0.054 Uiso 1 1 calc R . .
C74 C 0.5703(4) 0.2338(4) 0.2854(3) 0.0491(17) Uani 1 1 d . . .
H74A H 0.5653 0.1769 0.2629 0.059 Uiso 1 1 calc R . .
H74B H 0.5786 0.2181 0.3264 0.059 Uiso 1 1 calc R . .
C75 C 0.6313(4) 0.2900(5) 0.2728(3) 0.069(2) Uani 1 1 d . . .
H75A H 0.6723 0.2515 0.2655 0.082 Uiso 1 1 calc R . .
H75B H 0.6501 0.3322 0.3046 0.082 Uiso 1 1 calc R . .
C76 C 0.5957(4) 0.3416(5) 0.2198(3) 0.065(2) Uani 1 1 d . . .
H76A H 0.6204 0.4008 0.2173 0.079 Uiso 1 1 calc R . .
H76B H 0.5974 0.3058 0.1850 0.079 Uiso 1 1 calc R . .
C77 C 0.5183(4) 0.3550(5) 0.2271(3) 0.055(2) Uani 1 1 d . . .
H77A H 0.5112 0.4178 0.2401 0.066 Uiso 1 1 calc R . .
H77B H 0.4836 0.3443 0.1907 0.066 Uiso 1 1 calc R . .
O78 O 0.5066(2) 0.2893(3) 0.26970(17) 0.0467(11) Uani 1 1 d . . .
O79 O 0.0185(2) 0.6845(3) 0.06004(18) 0.0454(11) Uani 1 1 d . . .
C80 C 0.0411(3) 0.7555(4) 0.0262(3) 0.0464(17) Uani 1 1 d . . .
H80A H 0.0068 0.7600 -0.0110 0.056 Uiso 1 1 calc R . .
H80B H 0.0911 0.7431 0.0191 0.056 Uiso 1 1 calc R . .
C81 C 0.0406(4) 0.8419(5) 0.0591(3) 0.0576(19) Uani 1 1 d . . .
H81A H -0.0072 0.8736 0.0482 0.069 Uiso 1 1 calc R . .
H81B H 0.0803 0.8833 0.0527 0.069 Uiso 1 1 calc R . .
C82 C 0.0109(4) 0.7220(5) 0.1137(3) 0.0566(19) Uani 1 1 d . . .
H82A H 0.0312 0.6797 0.1450 0.068 Uiso 1 1 calc R . .
H82B H -0.0416 0.7329 0.1144 0.068 Uiso 1 1 calc R . .
C83 C 0.0531(4) 0.8107(5) 0.1204(3) 0.0554(19) Uani 1 1 d . . .
H83A H 0.0325 0.8543 0.1447 0.067 Uiso 1 1 calc R . .
H83B H 0.1059 0.8010 0.1363 0.067 Uiso 1 1 calc R . .
O84 O 0.4771(3) 0.0128(4) 0.1207(2) 0.0768(17) Uani 1 1 d . . .
C85 C 0.4753(5) 0.0256(5) 0.0635(3) 0.081(3) Uani 1 1 d . . .
H85A H 0.4345 -0.0094 0.0403 0.097 Uiso 1 1 calc R . .
H85B H 0.5221 0.0061 0.0532 0.097 Uiso 1 1 calc R . .
C86 C 0.5039(5) 0.1660(7) 0.1054(5) 0.116(4) Uani 1 1 d . . .
H86A H 0.4852 0.2273 0.1122 0.139 Uiso 1 1 calc R . .
H86B H 0.5569 0.1706 0.1042 0.139 Uiso 1 1 calc R . .
C87 C 0.4635(5) 0.1279(5) 0.0536(3) 0.070(2) Uani 1 1 d . . .
H87A H 0.4833 0.1487 0.0203 0.084 Uiso 1 1 calc R . .
H87B H 0.4107 0.1439 0.0480 0.084 Uiso 1 1 calc R . .
C88 C 0.4920(7) 0.1026(9) 0.1493(3) 0.148(6) Uani 1 1 d . . .
H88A H 0.4496 0.1221 0.1659 0.178 Uiso 1 1 calc R . .
H88B H 0.5361 0.0993 0.1801 0.178 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
O5 V1 O3 99.97(16) . . ?
O5 V1 O2 96.91(16) . . ?
O3 V1 O2 97.12(15) . . ?
O5 V1 O4 97.20(16) . . ?
O3 V1 O4 93.42(15) . . ?
O2 V1 O4 160.64(14) . . ?
O5 V1 O6 94.03(17) . . ?
O3 V1 O6 165.65(16) . . ?
O2 V1 O6 84.21(17) . . ?
O4 V1 O6 81.64(17) . . ?
O5 V1 N7 175.46(16) . . ?
O3 V1 N7 84.57(14) . . ?
O2 V1 N7 82.39(13) . . ?
O4 V1 N7 82.49(13) . . ?
O6 V1 N7 81.44(14) . . ?
C8 O2 V1 141.6(3) . . ?
C17 O3 V1 136.0(3) . . ?
C23 O4 V1 128.1(3) . . ?
V1 O6 H6A 116(4) . . ?
V1 O6 H6B 111(4) . . ?
H6A O6 H6B 111(6) . . ?
C15 N7 C14 108.3(3) . . ?
C15 N7 C16 110.4(4) . . ?
C14 N7 C16 105.4(3) . . ?
C15 N7 V1 113.2(3) . . ?
C14 N7 V1 109.7(3) . . ?
C16 N7 V1 109.5(3) . . ?
O2 C8 C13 123.6(4) . . ?
O2 C8 C9 117.7(4) . . ?
C13 C8 C9 118.7(4) . . ?
C10 C9 C8 122.4(5) . . ?
C10 C9 Cl29 118.5(4) . . ?
C8 C9 Cl29 119.1(4) . . ?
C9 C10 C11 117.5(5) . . ?
C9 C10 H10 121.3 . . ?
C11 C10 H10 121.3 . . ?
C12 C11 C10 121.9(5) . . ?
C12 C11 Cl30 120.1(4) . . ?
C10 C11 Cl30 118.1(4) . . ?
C11 C12 C13 120.7(5) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C8 118.8(5) . . ?
C12 C13 C14 120.2(4) . . ?
C8 C13 C14 120.8(4) . . ?
C13 C14 N7 115.2(4) . . ?
C13 C14 H14A 108.5 . . ?
N7 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
N7 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
N7 C15 C22 117.0(4) . . ?
N7 C15 H15A 108.0 . . ?
C22 C15 H15A 108.0 . . ?
N7 C15 H15B 108.0 . . ?
C22 C15 H15B 108.0 . . ?
H15A C15 H15B 107.3 . . ?
N7 C16 C28 112.2(4) . . ?
N7 C16 H16A 109.2 . . ?
C28 C16 H16A 109.2 . . ?
N7 C16 H16B 109.2 . . ?
C28 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
O3 C17 C22 122.4(4) . . ?
O3 C17 C18 118.4(4) . . ?
C22 C17 C18 119.2(5) . . ?
C19 C18 C17 121.6(4) . . ?
C19 C18 Cl31 118.5(3) . . ?
C17 C18 Cl31 119.9(4) . . ?
C20 C19 C18 118.0(4) . . ?
C20 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
C19 C20 C21 121.5(5) . . ?
C19 C20 Cl32 119.6(4) . . ?
C21 C20 Cl32 119.0(4) . . ?
C22 C21 C20 120.4(4) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C17 119.2(4) . . ?
C21 C22 C15 119.1(4) . . ?
C17 C22 C15 121.5(5) . . ?
O4 C23 C24 120.5(4) . . ?
O4 C23 C28 121.7(4) . . ?
C24 C23 C28 117.7(5) . . ?
C25 C24 C23 122.1(4) . . ?
C25 C24 Cl33 118.9(3) . . ?
C23 C24 Cl33 119.0(4) . . ?
C24 C25 C26 118.4(4) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
C25 C26 C27 120.7(5) . . ?
C25 C26 Cl34 118.4(4) . . ?
C27 C26 Cl34 120.9(4) . . ?
C28 C27 C26 120.3(4) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C23 120.7(4) . . ?
C27 C28 C16 123.1(4) . . ?
C23 C28 C16 116.1(4) . . ?
O37 V35 O39 96.64(16) . . ?
O37 V35 O38 95.23(16) . . ?
O39 V35 O38 166.47(15) . . ?
O37 V35 O40 101.58(17) . . ?
O39 V35 O40 92.45(15) . . ?
O38 V35 O40 91.49(15) . . ?
O37 V35 O36 95.01(18) . . ?
O39 V35 O36 85.34(18) . . ?
O38 V35 O36 87.19(18) . . ?
O40 V35 O36 163.41(15) . . ?
O37 V35 N41 173.69(17) . . ?
O39 V35 N41 85.30(14) . . ?
O38 V35 N41 82.22(14) . . ?
O40 V35 N41 84.30(14) . . ?
O36 V35 N41 79.13(15) . . ?
V35 O36 H36A 105(3) . . ?
V35 O36 H36B 97(5) . . ?
H36A O36 H36B 105(5) . . ?
C57 O38 V35 140.4(3) . . ?
C42 O39 V35 139.4(3) . . ?
C51 O40 V35 122.6(3) . . ?
C49 N41 C48 107.4(4) . . ?
C49 N41 C50 110.6(4) . . ?
C48 N41 C50 105.7(4) . . ?
C49 N41 V35 110.9(3) . . ?
C48 N41 V35 110.5(3) . . ?
C50 N41 V35 111.6(3) . . ?
O39 C42 C43 119.8(4) . . ?
O39 C42 C47 122.6(4) . . ?
C43 C42 C47 117.6(5) . . ?
C44 C43 C42 122.6(4) . . ?
C44 C43 Cl63 118.0(4) . . ?
C42 C43 Cl63 119.4(4) . . ?
C45 C44 C43 118.1(5) . . ?
C45 C44 H44 121.0 . . ?
C43 C44 H44 121.0 . . ?
C44 C45 C46 121.8(5) . . ?
C44 C45 Cl64 118.0(4) . . ?
C46 C45 Cl64 120.2(4) . . ?
C47 C46 C45 119.7(4) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C42 120.0(5) . . ?
C46 C47 C48 119.4(4) . . ?
C42 C47 C48 120.3(5) . . ?
N41 C48 C47 115.5(4) . . ?
N41 C48 H48A 108.4 . . ?
C47 C48 H48A 108.4 . . ?
N41 C48 H48B 108.4 . . ?
C47 C48 H48B 108.4 . . ?
H48A C48 H48B 107.5 . . ?
N41 C49 C56 115.2(4) . . ?
N41 C49 H49A 108.5 . . ?
C56 C49 H49A 108.5 . . ?
N41 C49 H49B 108.5 . . ?
C56 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
N41 C50 C62 115.1(4) . . ?
N41 C50 H50A 108.5 . . ?
C62 C50 H50A 108.5 . . ?
N41 C50 H50B 108.5 . . ?
C62 C50 H50B 108.5 . . ?
H50A C50 H50B 107.5 . . ?
O40 C51 C52 122.1(4) . . ?
O40 C51 C56 120.1(4) . . ?
C52 C51 C56 117.8(4) . . ?
C53 C52 C51 122.4(5) . . ?
C53 C52 Cl65 118.5(4) . . ?
C51 C52 Cl65 119.0(4) . . ?
C54 C53 C52 117.7(5) . . ?
C54 C53 H53 121.2 . . ?
C52 C53 H53 121.2 . . ?
C55 C54 C53 121.8(4) . . ?
C55 C54 Cl66 118.9(4) . . ?
C53 C54 Cl66 119.2(4) . . ?
C54 C55 C56 120.2(5) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C55 C56 C51 119.9(5) . . ?
C55 C56 C49 121.6(4) . . ?
C51 C56 C49 118.4(4) . . ?
O38 C57 C62 122.9(4) . . ?
O38 C57 C58 119.2(4) . . ?
C62 C57 C58 117.9(4) . . ?
C59 C58 C57 121.5(5) . . ?
C59 C58 Cl67 119.5(4) . . ?
C57 C58 Cl67 119.0(4) . . ?
C58 C59 C60 118.7(5) . . ?
C58 C59 H59 120.6 . . ?
C60 C59 H59 120.6 . . ?
C61 C60 C59 121.4(4) . . ?
C61 C60 Cl68 120.5(4) . . ?
C59 C60 Cl68 118.1(4) . . ?
C62 C61 C60 119.6(5) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C61 C62 C57 120.4(5) . . ?
C61 C62 C50 120.5(4) . . ?
C57 C62 C50 119.0(4) . . ?
C73 O69 C70 107.9(4) . . ?
O69 C70 C71 106.7(5) . . ?
O69 C70 H70A 110.4 . . ?
C71 C70 H70A 110.4 . . ?
O69 C70 H70B 110.4 . . ?
C71 C70 H70B 110.4 . . ?
H70A C70 H70B 108.6 . . ?
C70 C71 C72 101.8(5) . . ?
C70 C71 H71A 111.4 . . ?
C72 C71 H71A 111.4 . . ?
C70 C71 H71B 111.4 . . ?
C72 C71 H71B 111.4 . . ?
H71A C71 H71B 109.3 . . ?
C73 C72 C71 102.1(5) . . ?
C73 C72 H72A 111.3 . . ?
C71 C72 H72A 111.3 . . ?
C73 C72 H72B 111.3 . . ?
C71 C72 H72B 111.3 . . ?
H72A C72 H72B 109.2 . . ?
O69 C73 C72 107.2(5) . . ?
O69 C73 H73A 110.3 . . ?
C72 C73 H73A 110.3 . . ?
O69 C73 H73B 110.3 . . ?
C72 C73 H73B 110.3 . . ?
H73A C73 H73B 108.5 . . ?
O78 C74 C75 104.8(5) . . ?
O78 C74 H74A 110.8 . . ?
C75 C74 H74A 110.8 . . ?
O78 C74 H74B 110.8 . . ?
C75 C74 H74B 110.8 . . ?
H74A C74 H74B 108.9 . . ?
C74 C75 C76 102.9(6) . . ?
C74 C75 H75A 111.2 . . ?
C76 C75 H75A 111.2 . . ?
C74 C75 H75B 111.2 . . ?
C76 C75 H75B 111.2 . . ?
H75A C75 H75B 109.1 . . ?
C77 C76 C75 104.0(5) . . ?
C77 C76 H76A 111.0 . . ?
C75 C76 H76A 111.0 . . ?
C77 C76 H76B 111.0 . . ?
C75 C76 H76B 111.0 . . ?
H76A C76 H76B 109.0 . . ?
O78 C77 C76 105.9(5) . . ?
O78 C77 H77A 110.6 . . ?
C76 C77 H77A 110.6 . . ?
O78 C77 H77B 110.6 . . ?
C76 C77 H77B 110.6 . . ?
H77A C77 H77B 108.7 . . ?
C74 O78 C77 109.6(4) . . ?
C82 O79 C80 108.6(5) . . ?
O79 C80 C81 106.7(5) . . ?
O79 C80 H80A 110.4 . . ?
C81 C80 H80A 110.4 . . ?
O79 C80 H80B 110.4 . . ?
C81 C80 H80B 110.4 . . ?
H80A C80 H80B 108.6 . . ?
C80 C81 C83 103.8(6) . . ?
C80 C81 H81A 111.0 . . ?
C83 C81 H81A 111.0 . . ?
C80 C81 H81B 111.0 . . ?
C83 C81 H81B 111.0 . . ?
H81A C81 H81B 109.0 . . ?
O79 C82 C83 106.8(5) . . ?
O79 C82 H82A 110.4 . . ?
C83 C82 H82A 110.4 . . ?
O79 C82 H82B 110.4 . . ?
C83 C82 H82B 110.4 . . ?
H82A C82 H82B 108.6 . . ?
C81 C83 C82 100.4(5) . . ?
C81 C83 H83A 111.7 . . ?
C82 C83 H83A 111.7 . . ?
C81 C83 H83B 111.7 . . ?
C82 C83 H83B 111.7 . . ?
H83A C83 H83B 109.5 . . ?
C85 O84 C88 107.6(7) . . ?
O84 C85 C87 105.2(6) . . ?
O84 C85 H85A 110.7 . . ?
C87 C85 H85A 110.7 . . ?
O84 C85 H85B 110.7 . . ?
C87 C85 H85B 110.7 . . ?
H85A C85 H85B 108.8 . . ?
C87 C86 C88 104.3(8) . . ?
C87 C86 H86A 110.9 . . ?
C88 C86 H86A 110.9 . . ?
C87 C86 H86B 110.9 . . ?
C88 C86 H86B 110.9 . . ?
H86A C86 H86B 108.9 . . ?
C86 C87 C85 102.5(8) . . ?
C86 C87 H87A 111.3 . . ?
C85 C87 H87A 111.3 . . ?
C86 C87 H87B 111.3 . . ?
C85 C87 H87B 111.3 . . ?
H87A C87 H87B 109.2 . . ?
C86 C88 O84 106.1(7) . . ?
C86 C88 H88A 110.5 . . ?
O84 C88 H88A 110.5 . . ?
C86 C88 H88B 110.5 . . ?
O84 C88 H88B 110.5 . . ?
H88A C88 H88B 108.7 . . ?
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 O5 1.596(3) . ?
V1 O3 1.844(3) . ?
V1 O2 1.855(3) . ?
V1 O4 1.899(3) . ?
V1 O6 2.083(4) . ?
V1 N7 2.444(4) . ?
O2 C8 1.329(5) . ?
O3 C17 1.345(6) . ?
O4 C23 1.336(6) . ?
O6 H6A 0.75(5) . ?
O6 H6B 0.82(6) . ?
N7 C15 1.483(6) . ?
N7 C14 1.493(5) . ?
N7 C16 1.498(6) . ?
C8 C13 1.404(7) . ?
C8 C9 1.409(7) . ?
C9 C10 1.383(7) . ?
C9 Cl29 1.729(5) . ?
C10 C11 1.390(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(7) . ?
C11 Cl30 1.751(5) . ?
C12 C13 1.401(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.490(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C22 1.501(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C28 1.510(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.401(6) . ?
C17 C18 1.404(6) . ?
C18 C19 1.389(7) . ?
C18 Cl31 1.730(5) . ?
C19 C20 1.382(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(6) . ?
C20 Cl32 1.744(5) . ?
C21 C22 1.382(7) . ?
C21 H21 0.9500 . ?
C23 C24 1.401(6) . ?
C23 C28 1.401(6) . ?
C24 C25 1.384(7) . ?
C24 Cl33 1.737(5) . ?
C25 C26 1.385(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.392(6) . ?
C26 Cl34 1.736(5) . ?
C27 C28 1.369(7) . ?
C27 H27 0.9500 . ?
V35 O37 1.593(3) . ?
V35 O39 1.854(3) . ?
V35 O38 1.855(3) . ?
V35 O40 1.896(3) . ?
V35 O36 2.085(4) . ?
V35 N41 2.402(4) . ?
O36 H36A 0.91(5) . ?
O36 H36B 0.81(7) . ?
O38 C57 1.334(5) . ?
O39 C42 1.333(6) . ?
O40 C51 1.337(5) . ?
N41 C49 1.489(6) . ?
N41 C48 1.495(6) . ?
N41 C50 1.501(6) . ?
C42 C43 1.395(7) . ?
C42 C47 1.415(6) . ?
C43 C44 1.378(7) . ?
C43 Cl63 1.742(5) . ?
C44 C45 1.373(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(7) . ?
C45 Cl64 1.752(6) . ?
C46 C47 1.381(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.506(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C56 1.493(7) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C62 1.506(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.400(7) . ?
C51 C56 1.404(7) . ?
C52 C53 1.386(7) . ?
C52 Cl65 1.747(5) . ?
C53 C54 1.382(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.374(7) . ?
C54 Cl66 1.750(5) . ?
C55 C56 1.388(6) . ?
C55 H55 0.9500 . ?
C57 C62 1.406(7) . ?
C57 C58 1.412(7) . ?
C58 C59 1.371(7) . ?
C58 Cl67 1.732(5) . ?
C59 C60 1.388(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.384(7) . ?
C60 Cl68 1.751(4) . ?
C61 C62 1.380(6) . ?
C61 H61 0.9500 . ?
O69 C73 1.439(7) . ?
O69 C70 1.454(7) . ?
C70 C71 1.484(8) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.530(9) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.501(8) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 O78 1.425(7) . ?
C74 C75 1.478(9) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 C76 1.515(9) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 C77 1.491(9) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 O78 1.452(7) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
O79 C82 1.429(7) . ?
O79 C80 1.433(7) . ?
C80 C81 1.495(9) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C81 C83 1.512(9) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 C83 1.513(9) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
O84 C85 1.377(8) . ?
O84 C88 1.488(12) . ?
C85 C87 1.530(10) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 C87 1.431(11) . ?
C86 C88 1.452(14) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
