#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:49:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179709 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/12/7001270.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_7001270
loop_
_publ_author_name
'Kirk Egdal, Rune'
'Bond, Andrew D.'
'McKenzie, Christine J.'
_publ_section_title
;
 Air oxidation of divanadium(IV) complexes
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3833
_journal_page_last               3839
_journal_paper_doi               10.1039/b901633c
_journal_year                    2009
_chemical_formula_moiety         'C36 H43 N6 O5 V2 3+, 3(Cl O4 -), H2 O'
_chemical_formula_sum            'C36 H45 Cl3 N6 O18 V2'
_chemical_formula_weight         1058.01
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.608(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8133(6)
_cell_length_b                   22.2245(11)
_cell_length_c                   18.1295(9)
_cell_measurement_reflns_used    3597
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.83
_cell_measurement_theta_min      2.44
_cell_volume                     4348.2(4)
_computing_cell_refinement       'SAINT v.7.06a (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-22 (Bruker Nonius, 2004)'
_computing_data_reduction        'SAINT v.7.06a'
_computing_molecular_graphics    'SHELXTL v.6.10'
_computing_publication_material  'SHELXTL v.6.10'
_computing_structure_refinement  'SHELXTL v.6.10'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice ω and φ 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  0.0831
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46075
_diffrn_reflns_theta_full        24.68
_diffrn_reflns_theta_max         24.68
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0417P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                4346
_reflns_number_total             7328
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b901633c.txt
_cod_data_source_block           1
_cod_original_cell_volume        4348.3(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001270
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 0.25289(5) 0.32380(2) 0.23773(3) 0.01757(15) Uani 1 1 d . . .
V2 V 0.56511(5) 0.35248(2) 0.17901(3) 0.01784(15) Uani 1 1 d . . .
O1 O 0.41118(17) 0.37419(9) 0.23538(10) 0.0166(5) Uani 1 1 d . . .
O2 O 0.22005(18) 0.30902(9) 0.15217(11) 0.0245(6) Uani 1 1 d . . .
O3 O 0.35611(19) 0.25248(9) 0.26940(13) 0.0253(6) Uani 1 1 d D . .
H31W H 0.4275(14) 0.2485(12) 0.2892(16) 0.038 Uiso 1 1 d D . .
H32W H 0.330(2) 0.2172(6) 0.2638(18) 0.038 Uiso 1 1 d D . .
O4 O 0.60266(18) 0.28678(9) 0.20586(11) 0.0233(5) Uani 1 1 d . . .
O5 O 0.44467(18) 0.33677(10) 0.09018(11) 0.0226(6) Uani 1 1 d D . .
H51W H 0.3701(12) 0.3278(13) 0.0956(15) 0.034 Uiso 1 1 d D . .
H52W H 0.461(2) 0.3171(12) 0.0524(11) 0.034 Uiso 1 1 d D . .
N1 N 0.2423(2) 0.35233(11) 0.35781(13) 0.0139(6) Uani 1 1 d . . .
N2 N 0.1478(2) 0.40410(11) 0.23045(14) 0.0167(6) Uani 1 1 d . . .
N3 N 0.1061(2) 0.27384(11) 0.27891(14) 0.0190(6) Uani 1 1 d . . .
N4 N 0.5713(2) 0.45111(11) 0.14232(13) 0.0154(6) Uani 1 1 d . . .
N5 N 0.6820(2) 0.39436(12) 0.26235(13) 0.0169(6) Uani 1 1 d . . .
N6 N 0.7078(2) 0.35853(12) 0.10419(13) 0.0173(6) Uani 1 1 d . . .
C1 C 0.4115(3) 0.42975(14) 0.27140(17) 0.0153(7) Uani 1 1 d . . .
C2 C 0.3965(2) 0.43147(14) 0.34767(17) 0.0150(7) Uani 1 1 d . . .
C3 C 0.3967(3) 0.48698(14) 0.38246(17) 0.0181(8) Uani 1 1 d . . .
H3 H 0.3865 0.4880 0.4341 0.022 Uiso 1 1 calc R . .
C4 C 0.4108(3) 0.54081(14) 0.34617(17) 0.0166(8) Uani 1 1 d . . .
C5 C 0.4252(2) 0.53719(14) 0.26957(17) 0.0176(8) Uani 1 1 d . . .
H5 H 0.4351 0.5733 0.2425 0.021 Uiso 1 1 calc R . .
C6 C 0.4256(3) 0.48280(14) 0.23248(16) 0.0143(7) Uani 1 1 d . . .
C7 C 0.4115(3) 0.60183(13) 0.38495(17) 0.0205(8) Uani 1 1 d . . .
C8 C 0.3813(3) 0.59642(16) 0.46614(18) 0.0392(10) Uani 1 1 d . . .
H8A H 0.3831 0.6364 0.4889 0.059 Uiso 1 1 calc R . .
H8B H 0.4428 0.5705 0.4924 0.059 Uiso 1 1 calc R . .
H8C H 0.2986 0.5789 0.4691 0.059 Uiso 1 1 calc R . .
C9 C 0.3158(4) 0.64265(16) 0.3467(2) 0.0486(11) Uani 1 1 d . . .
H9A H 0.3168 0.6818 0.3716 0.073 Uiso 1 1 calc R . .
H9B H 0.2335 0.6245 0.3486 0.073 Uiso 1 1 calc R . .
H9C H 0.3350 0.6482 0.2950 0.073 Uiso 1 1 calc R . .
C10 C 0.5401(3) 0.63010(17) 0.3834(2) 0.0576(13) Uani 1 1 d . . .
H10A H 0.5405 0.6692 0.4083 0.086 Uiso 1 1 calc R . .
H10B H 0.5610 0.6356 0.3320 0.086 Uiso 1 1 calc R . .
H10C H 0.6014 0.6036 0.4088 0.086 Uiso 1 1 calc R . .
C11 C 0.3658(3) 0.37465(14) 0.38755(17) 0.0186(8) Uani 1 1 d . . .
H11A H 0.4300 0.3438 0.3803 0.022 Uiso 1 1 calc R . .
H11B H 0.3639 0.3827 0.4412 0.022 Uiso 1 1 calc R . .
C12 C 0.1460(3) 0.39975(14) 0.36342(16) 0.0185(8) Uani 1 1 d . . .
H12A H 0.1722 0.4279 0.4038 0.022 Uiso 1 1 calc R . .
H12B H 0.0673 0.3808 0.3761 0.022 Uiso 1 1 calc R . .
C13 C 0.1249(3) 0.43423(15) 0.29305(17) 0.0179(8) Uani 1 1 d . . .
C14 C 0.0783(3) 0.49195(15) 0.29132(19) 0.0239(8) Uani 1 1 d . . .
H14 H 0.0670 0.5131 0.3359 0.029 Uiso 1 1 calc R . .
C15 C 0.0484(3) 0.51851(16) 0.2235(2) 0.0309(9) Uani 1 1 d . . .
H15 H 0.0154 0.5581 0.2211 0.037 Uiso 1 1 calc R . .
C16 C 0.0664(3) 0.48748(16) 0.16009(19) 0.0298(9) Uani 1 1 d . . .
H16 H 0.0443 0.5049 0.1133 0.036 Uiso 1 1 calc R . .
C17 C 0.1171(3) 0.43054(15) 0.16475(18) 0.0222(8) Uani 1 1 d . . .
H17 H 0.1309 0.4093 0.1205 0.027 Uiso 1 1 calc R . .
C18 C 0.2045(3) 0.29760(13) 0.39782(16) 0.0175(8) Uani 1 1 d . . .
H18A H 0.2750 0.2692 0.4039 0.021 Uiso 1 1 calc R . .
H18B H 0.1785 0.3086 0.4474 0.021 Uiso 1 1 calc R . .
C19 C 0.0999(3) 0.26923(13) 0.35365(17) 0.0161(8) Uani 1 1 d . . .
C20 C 0.0032(3) 0.24014(14) 0.38351(18) 0.0238(8) Uani 1 1 d . . .
H20 H -0.0018 0.2388 0.4356 0.029 Uiso 1 1 calc R . .
C21 C -0.0871(3) 0.21282(15) 0.3379(2) 0.0297(9) Uani 1 1 d . . .
H21 H -0.1543 0.1924 0.3581 0.036 Uiso 1 1 calc R . .
C22 C -0.0782(3) 0.21564(15) 0.2626(2) 0.0311(9) Uani 1 1 d . . .
H22 H -0.1381 0.1964 0.2301 0.037 Uiso 1 1 calc R . .
C23 C 0.0183(3) 0.24664(14) 0.23529(19) 0.0254(8) Uani 1 1 d . . .
H23 H 0.0232 0.2490 0.1832 0.031 Uiso 1 1 calc R . .
C24 C 0.4490(3) 0.48061(14) 0.15157(16) 0.0190(8) Uani 1 1 d . . .
H24A H 0.3823 0.4576 0.1244 0.023 Uiso 1 1 calc R . .
H24B H 0.4494 0.5219 0.1311 0.023 Uiso 1 1 calc R . .
C25 C 0.6714(3) 0.48362(14) 0.18626(16) 0.0184(8) Uani 1 1 d . . .
H25A H 0.6442 0.5254 0.1951 0.022 Uiso 1 1 calc R . .
H25B H 0.7461 0.4855 0.1574 0.022 Uiso 1 1 calc R . .
C26 C 0.7045(3) 0.45400(15) 0.25896(17) 0.0165(8) Uani 1 1 d . . .
C27 C 0.7639(3) 0.48409(15) 0.31747(18) 0.0248(8) Uani 1 1 d . . .
H27 H 0.7754 0.5264 0.3147 0.030 Uiso 1 1 calc R . .
C28 C 0.8067(3) 0.45334(16) 0.37984(18) 0.0271(9) Uani 1 1 d . . .
H28 H 0.8479 0.4738 0.4203 0.033 Uiso 1 1 calc R . .
C29 C 0.7881(3) 0.39167(16) 0.38198(18) 0.0261(9) Uani 1 1 d . . .
H29 H 0.8189 0.3687 0.4233 0.031 Uiso 1 1 calc R . .
C30 C 0.7245(3) 0.36455(15) 0.32339(18) 0.0222(8) Uani 1 1 d . . .
H30 H 0.7097 0.3225 0.3259 0.027 Uiso 1 1 calc R . .
C31 C 0.6003(3) 0.44788(14) 0.06375(15) 0.0193(8) Uani 1 1 d . . .
H31A H 0.6208 0.4884 0.0454 0.023 Uiso 1 1 calc R . .
H31B H 0.5281 0.4322 0.0333 0.023 Uiso 1 1 calc R . .
C32 C 0.7093(3) 0.40628(15) 0.05902(17) 0.0202(8) Uani 1 1 d . . .
C33 C 0.8044(3) 0.41606(16) 0.01329(17) 0.0272(9) Uani 1 1 d . . .
H33 H 0.8035 0.4503 -0.0180 0.033 Uiso 1 1 calc R . .
C34 C 0.9002(3) 0.37580(16) 0.01353(18) 0.0284(9) Uani 1 1 d . . .
H34 H 0.9665 0.3817 -0.0177 0.034 Uiso 1 1 calc R . .
C35 C 0.8994(3) 0.32686(16) 0.05934(17) 0.0262(9) Uani 1 1 d . . .
H35 H 0.9653 0.2985 0.0606 0.031 Uiso 1 1 calc R . .
C36 C 0.8021(3) 0.31931(15) 0.10344(17) 0.0229(8) Uani 1 1 d . . .
H36 H 0.8015 0.2850 0.1347 0.027 Uiso 1 1 calc R . .
Cl1 Cl 0.04704(8) 0.38071(4) 0.57195(5) 0.0304(2) Uani 1 1 d . . .
O1A O 0.1662(2) 0.39267(13) 0.54663(14) 0.0600(8) Uani 1 1 d . . .
O1B O -0.0357(2) 0.42763(13) 0.54553(14) 0.0640(9) Uani 1 1 d . . .
O1C O 0.0532(2) 0.38225(11) 0.65162(12) 0.0396(7) Uani 1 1 d . . .
O1D O 0.0014(3) 0.32472(12) 0.54604(16) 0.0754(10) Uani 1 1 d . . .
Cl2 Cl 0.22905(7) 0.10707(4) 0.44969(5) 0.0273(2) Uani 1 1 d . . .
O2A O 0.2112(2) 0.16372(10) 0.48494(13) 0.0412(7) Uani 1 1 d . . .
O2B O 0.1450(2) 0.10255(11) 0.38520(12) 0.0403(7) Uani 1 1 d . . .
O2C O 0.3531(2) 0.10119(11) 0.42726(13) 0.0434(7) Uani 1 1 d . . .
O2D O 0.2027(3) 0.05994(12) 0.49951(15) 0.0661(9) Uani 1 1 d . . .
Cl3 Cl 0.59680(8) 0.22104(5) 0.42624(5) 0.0392(3) Uani 1 1 d . . .
O3A O 0.6173(2) 0.15861(12) 0.41868(16) 0.0674(9) Uani 1 1 d . . .
O3B O 0.4931(2) 0.23093(12) 0.47072(15) 0.0649(9) Uani 1 1 d . . .
O3C O 0.5673(2) 0.24648(12) 0.35482(13) 0.0538(8) Uani 1 1 d . . .
O3D O 0.7048(2) 0.25070(14) 0.45777(14) 0.0622(9) Uani 1 1 d . . .
O1W O 0.2549(2) 0.14585(11) 0.25592(13) 0.0327(6) Uani 1 1 d D . .
H11W H 0.220(2) 0.1358(16) 0.2939(9) 0.049 Uiso 1 1 d D . .
H12W H 0.198(2) 0.1439(17) 0.2222(10) 0.049 Uiso 1 1 d D . .
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'
Cl Cl 0.1484 0.1585 '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
O2 V1 O3 101.58(10) . . ?
O2 V1 O1 103.08(9) . . ?
O3 V1 O1 89.27(8) . . ?
O2 V1 N3 96.23(10) . . ?
O3 V1 N3 84.27(9) . . ?
O1 V1 N3 160.51(9) . . ?
O2 V1 N2 91.55(10) . . ?
O3 V1 N2 166.80(10) . . ?
O1 V1 N2 89.08(8) . . ?
N3 V1 N2 93.03(9) . . ?
O2 V1 N1 163.83(9) . . ?
O3 V1 N1 90.41(9) . . ?
O1 V1 N1 87.72(8) . . ?
N3 V1 N1 73.99(9) . . ?
N2 V1 N1 76.44(9) . . ?
O4 V2 O5 102.93(10) . . ?
O4 V2 O1 105.22(9) . . ?
O5 V2 O1 86.33(8) . . ?
O4 V2 N6 94.14(10) . . ?
O5 V2 N6 87.71(9) . . ?
O1 V2 N6 160.57(9) . . ?
O4 V2 N5 93.20(10) . . ?
O5 V2 N5 163.83(10) . . ?
O1 V2 N5 90.44(8) . . ?
N6 V2 N5 90.16(9) . . ?
O4 V2 N4 163.50(9) . . ?
O5 V2 N4 87.90(9) . . ?
O1 V2 N4 87.67(8) . . ?
N6 V2 N4 73.64(9) . . ?
N5 V2 N4 76.13(9) . . ?
C1 O1 V1 116.82(16) . . ?
C1 O1 V2 117.36(16) . . ?
V1 O1 V2 125.69(10) . . ?
V1 O3 H31W 133.7(19) . . ?
V1 O3 H32W 121.9(18) . . ?
H31W O3 H32W 104.4(15) . . ?
V2 O5 H51W 121.2(19) . . ?
V2 O5 H52W 125.1(19) . . ?
H51W O5 H52W 103.0(15) . . ?
C18 N1 C12 109.4(2) . . ?
C18 N1 C11 111.2(2) . . ?
C12 N1 C11 110.7(2) . . ?
C18 N1 V1 105.70(17) . . ?
C12 N1 V1 109.87(17) . . ?
C11 N1 V1 109.86(17) . . ?
C17 N2 C13 118.4(3) . . ?
C17 N2 V1 121.6(2) . . ?
C13 N2 V1 119.4(2) . . ?
C23 N3 C19 118.3(3) . . ?
C23 N3 V1 123.3(2) . . ?
C19 N3 V1 118.4(2) . . ?
C31 N4 C25 110.3(2) . . ?
C31 N4 C24 111.8(2) . . ?
C25 N4 C24 110.2(2) . . ?
C31 N4 V2 104.17(18) . . ?
C25 N4 V2 110.00(17) . . ?
C24 N4 V2 110.15(17) . . ?
C30 N5 C26 117.9(3) . . ?
C30 N5 V2 121.8(2) . . ?
C26 N5 V2 119.9(2) . . ?
C32 N6 C36 118.0(3) . . ?
C32 N6 V2 118.5(2) . . ?
C36 N6 V2 123.3(2) . . ?
C6 C1 O1 120.7(3) . . ?
C6 C1 C2 120.1(3) . . ?
O1 C1 C2 119.2(3) . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 C11 121.6(3) . . ?
C1 C2 C11 119.6(3) . . ?
C4 C3 C2 123.5(3) . . ?
C4 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
C3 C4 C5 116.3(3) . . ?
C3 C4 C7 123.3(3) . . ?
C5 C4 C7 120.4(3) . . ?
C6 C5 C4 122.2(3) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C24 120.5(3) . . ?
C1 C6 C24 119.9(3) . . ?
C9 C7 C4 109.8(3) . . ?
C9 C7 C10 110.0(3) . . ?
C4 C7 C10 109.5(2) . . ?
C9 C7 C8 107.9(3) . . ?
C4 C7 C8 112.2(3) . . ?
C10 C7 C8 107.4(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C2 109.0(2) . . ?
N1 C11 H11A 109.9 . . ?
C2 C11 H11A 109.9 . . ?
N1 C11 H11B 109.9 . . ?
C2 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N1 C12 C13 112.0(2) . . ?
N1 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
N1 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N2 C13 C14 121.8(3) . . ?
N2 C13 C12 115.8(3) . . ?
C14 C13 C12 122.2(3) . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
N2 C17 C16 121.9(3) . . ?
N2 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C19 C18 N1 107.9(2) . . ?
C19 C18 H18A 110.1 . . ?
N1 C18 H18A 110.1 . . ?
C19 C18 H18B 110.1 . . ?
N1 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
N3 C19 C20 120.9(3) . . ?
N3 C19 C18 114.9(3) . . ?
C20 C19 C18 124.2(3) . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 118.9(3) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C23 C22 C21 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
N3 C23 C22 122.7(3) . . ?
N3 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
N4 C24 C6 109.1(2) . . ?
N4 C24 H24A 109.9 . . ?
C6 C24 H24A 109.9 . . ?
N4 C24 H24B 109.9 . . ?
C6 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
N4 C25 C26 112.5(2) . . ?
N4 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
N4 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
N5 C26 C27 121.2(3) . . ?
N5 C26 C25 116.0(3) . . ?
C27 C26 C25 122.6(3) . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 118.2(3) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 H28 120.9 . . ?
C30 C29 C28 118.7(3) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
N5 C30 C29 123.4(3) . . ?
N5 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
N4 C31 C32 107.4(2) . . ?
N4 C31 H31A 110.2 . . ?
C32 C31 H31A 110.2 . . ?
N4 C31 H31B 110.2 . . ?
C32 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
N6 C32 C33 122.0(3) . . ?
N6 C32 C31 114.3(3) . . ?
C33 C32 C31 123.7(3) . . ?
C34 C33 C32 119.2(3) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 119.2(3) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C36 119.1(3) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
N6 C36 C35 122.5(3) . . ?
N6 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
O1D Cl1 O1A 111.30(17) . . ?
O1D Cl1 O1B 109.43(18) . . ?
O1A Cl1 O1B 108.38(18) . . ?
O1D Cl1 O1C 110.37(17) . . ?
O1A Cl1 O1C 109.50(15) . . ?
O1B Cl1 O1C 107.77(15) . . ?
O2D Cl2 O2A 109.04(15) . . ?
O2D Cl2 O2C 109.96(16) . . ?
O2A Cl2 O2C 111.24(14) . . ?
O2D Cl2 O2B 108.84(17) . . ?
O2A Cl2 O2B 109.18(14) . . ?
O2C Cl2 O2B 108.54(14) . . ?
O3A Cl3 O3D 111.24(18) . . ?
O3A Cl3 O3C 109.13(18) . . ?
O3D Cl3 O3C 108.04(16) . . ?
O3A Cl3 O3B 109.72(16) . . ?
O3D Cl3 O3B 110.58(18) . . ?
O3C Cl3 O3B 108.05(16) . . ?
H11W O1W H12W 103.7(15) . . ?
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 O2 1.603(2) . ?
V1 O3 2.002(2) . ?
V1 O1 2.0482(19) . ?
V1 N3 2.112(2) . ?
V1 N2 2.115(3) . ?
V1 N1 2.277(2) . ?
V2 O4 1.584(2) . ?
V2 O5 2.037(2) . ?
V2 O1 2.0644(19) . ?
V2 N6 2.122(2) . ?
V2 N5 2.123(2) . ?
V2 N4 2.293(2) . ?
O1 C1 1.397(3) . ?
O3 H31W 0.84(1) . ?
O3 H32W 0.84(1) . ?
O5 H51W 0.84(1) . ?
O5 H52W 0.84(1) . ?
N1 C18 1.486(3) . ?
N1 C12 1.489(3) . ?
N1 C11 1.494(3) . ?
N2 C17 1.351(4) . ?
N2 C13 1.354(4) . ?
N3 C23 1.341(4) . ?
N3 C19 1.365(4) . ?
N4 C31 1.479(3) . ?
N4 C25 1.490(4) . ?
N4 C24 1.495(3) . ?
N5 C30 1.346(4) . ?
N5 C26 1.350(4) . ?
N6 C32 1.341(4) . ?
N6 C36 1.342(4) . ?
C1 C6 1.387(4) . ?
C1 C2 1.403(4) . ?
C2 C3 1.385(4) . ?
C2 C11 1.502(4) . ?
C3 C4 1.378(4) . ?
C3 H3 0.950 . ?
C4 C5 1.410(4) . ?
C4 C7 1.527(4) . ?
C5 C6 1.383(4) . ?
C5 H5 0.950 . ?
C6 C24 1.505(4) . ?
C7 C9 1.512(4) . ?
C7 C10 1.528(4) . ?
C7 C8 1.532(4) . ?
C8 H8A 0.980 . ?
C8 H8B 0.980 . ?
C8 H8C 0.980 . ?
C9 H9A 0.980 . ?
C9 H9B 0.980 . ?
C9 H9C 0.980 . ?
C10 H10A 0.980 . ?
C10 H10B 0.980 . ?
C10 H10C 0.980 . ?
C11 H11A 0.990 . ?
C11 H11B 0.990 . ?
C12 C13 1.493(4) . ?
C12 H12A 0.990 . ?
C12 H12B 0.990 . ?
C13 C14 1.378(4) . ?
C14 C15 1.384(4) . ?
C14 H14 0.950 . ?
C15 C16 1.365(4) . ?
C15 H15 0.950 . ?
C16 C17 1.380(4) . ?
C16 H16 0.950 . ?
C17 H17 0.950 . ?
C18 C19 1.485(4) . ?
C18 H18A 0.990 . ?
C18 H18B 0.990 . ?
C19 C20 1.370(4) . ?
C20 C21 1.380(4) . ?
C20 H20 0.950 . ?
C21 C22 1.375(4) . ?
C21 H21 0.950 . ?
C22 C23 1.369(4) . ?
C22 H22 0.950 . ?
C23 H23 0.950 . ?
C24 H24A 0.990 . ?
C24 H24B 0.990 . ?
C25 C26 1.496(4) . ?
C25 H25A 0.990 . ?
C25 H25B 0.990 . ?
C26 C27 1.378(4) . ?
C27 C28 1.376(4) . ?
C27 H27 0.950 . ?
C28 C29 1.386(4) . ?
C28 H28 0.950 . ?
C29 C30 1.368(4) . ?
C29 H29 0.950 . ?
C30 H30 0.950 . ?
C31 C32 1.505(4) . ?
C31 H31A 0.990 . ?
C31 H31B 0.990 . ?
C32 C33 1.378(4) . ?
C33 C34 1.368(4) . ?
C33 H33 0.950 . ?
C34 C35 1.369(4) . ?
C34 H34 0.950 . ?
C35 C36 1.371(4) . ?
C35 H35 0.950 . ?
C36 H36 0.950 . ?
Cl1 O1D 1.408(3) . ?
Cl1 O1A 1.420(2) . ?
Cl1 O1B 1.436(3) . ?
Cl1 O1C 1.442(2) . ?
Cl2 O2D 1.424(3) . ?
Cl2 O2A 1.430(2) . ?
Cl2 O2C 1.432(2) . ?
Cl2 O2B 1.439(2) . ?
Cl3 O3A 1.413(3) . ?
Cl3 O3D 1.429(3) . ?
Cl3 O3C 1.430(2) . ?
Cl3 O3B 1.438(2) . ?
O1W H11W 0.84(1) . ?
O1W H12W 0.84(1) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O2B 0.84(1) 2.03(1) 2.861(3) 174(4) .
O1W H12W O1C 0.84(1) 2.05(1) 2.865(3) 165(3) 4_565
O3 H31W O3C 0.84(1) 1.87(1) 2.681(3) 165(3) .
O3 H31W O4 0.84(1) 2.64(3) 3.066(3) 113(2) .
O3 H32W O1W 0.84(1) 1.78(1) 2.615(3) 172(3) .
O5 H51W O2 0.84(1) 2.02(1) 2.808(3) 156(3) .
O5 H51W O2A 0.84(1) 2.56(3) 3.067(3) 119(2) 4_565
O5 H52W O3B 0.84(1) 1.88(1) 2.715(3) 176(3) 4_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 C1 127.18(19) . . . . ?
O3 V1 O1 C1 -131.1(2) . . . . ?
N3 V1 O1 C1 -60.7(4) . . . . ?
N2 V1 O1 C1 35.8(2) . . . . ?
N1 V1 O1 C1 -40.67(19) . . . . ?
O2 V1 O1 V2 -48.67(14) . . . . ?
O3 V1 O1 V2 53.05(13) . . . . ?
N3 V1 O1 V2 123.5(3) . . . . ?
N2 V1 O1 V2 -140.04(12) . . . . ?
N1 V1 O1 V2 143.49(12) . . . . ?
O4 V2 O1 C1 130.59(19) . . . . ?
O5 V2 O1 C1 -127.00(19) . . . . ?
N6 V2 O1 C1 -54.6(4) . . . . ?
N5 V2 O1 C1 37.2(2) . . . . ?
N4 V2 O1 C1 -38.95(19) . . . . ?
O4 V2 O1 V1 -53.59(14) . . . . ?
O5 V2 O1 V1 48.82(12) . . . . ?
N6 V2 O1 V1 121.3(2) . . . . ?
N5 V2 O1 V1 -147.03(12) . . . . ?
N4 V2 O1 V1 136.87(12) . . . . ?
O2 V1 N1 C18 88.6(4) . . . . ?
O3 V1 N1 C18 -49.53(17) . . . . ?
O1 V1 N1 C18 -138.79(17) . . . . ?
N3 V1 N1 C18 34.39(17) . . . . ?
N2 V1 N1 C18 131.61(18) . . . . ?
O2 V1 N1 C12 -29.2(4) . . . . ?
O3 V1 N1 C12 -167.43(18) . . . . ?
O1 V1 N1 C12 103.32(18) . . . . ?
N3 V1 N1 C12 -83.50(19) . . . . ?
N2 V1 N1 C12 13.72(18) . . . . ?
O2 V1 N1 C11 -151.3(3) . . . . ?
O3 V1 N1 C11 70.56(18) . . . . ?
O1 V1 N1 C11 -18.69(18) . . . . ?
N3 V1 N1 C11 154.49(19) . . . . ?
N2 V1 N1 C11 -108.29(18) . . . . ?
O2 V1 N2 C17 -19.0(2) . . . . ?
O3 V1 N2 C17 166.9(3) . . . . ?
O1 V1 N2 C17 84.0(2) . . . . ?
N3 V1 N2 C17 -115.4(2) . . . . ?
N1 V1 N2 C17 171.9(2) . . . . ?
O2 V1 N2 C13 170.1(2) . . . . ?
O3 V1 N2 C13 -4.0(5) . . . . ?
O1 V1 N2 C13 -86.8(2) . . . . ?
N3 V1 N2 C13 73.8(2) . . . . ?
N1 V1 N2 C13 1.0(2) . . . . ?
O2 V1 N3 C23 -4.9(3) . . . . ?
O3 V1 N3 C23 -105.9(2) . . . . ?
O1 V1 N3 C23 -177.2(2) . . . . ?
N2 V1 N3 C23 87.0(2) . . . . ?
N1 V1 N3 C23 162.0(3) . . . . ?
O2 V1 N3 C19 175.5(2) . . . . ?
O3 V1 N3 C19 74.4(2) . . . . ?
O1 V1 N3 C19 3.1(4) . . . . ?
N2 V1 N3 C19 -92.7(2) . . . . ?
N1 V1 N3 C19 -17.7(2) . . . . ?
O4 V2 N4 C31 79.7(4) . . . . ?
O5 V2 N4 C31 -51.96(17) . . . . ?
O1 V2 N4 C31 -138.37(17) . . . . ?
N6 V2 N4 C31 36.27(16) . . . . ?
N5 V2 N4 C31 130.60(18) . . . . ?
O4 V2 N4 C25 -38.5(4) . . . . ?
O5 V2 N4 C25 -170.20(18) . . . . ?
O1 V2 N4 C25 103.38(18) . . . . ?
N6 V2 N4 C25 -81.97(18) . . . . ?
N5 V2 N4 C25 12.36(17) . . . . ?
O4 V2 N4 C24 -160.2(3) . . . . ?
O5 V2 N4 C24 68.11(18) . . . . ?
O1 V2 N4 C24 -18.31(17) . . . . ?
N6 V2 N4 C24 156.33(19) . . . . ?
N5 V2 N4 C24 -109.34(18) . . . . ?
O4 V2 N5 C30 -18.7(2) . . . . ?
O5 V2 N5 C30 164.8(3) . . . . ?
O1 V2 N5 C30 86.5(2) . . . . ?
N6 V2 N5 C30 -112.9(2) . . . . ?
N4 V2 N5 C30 174.0(2) . . . . ?
O4 V2 N5 C26 168.5(2) . . . . ?
O5 V2 N5 C26 -7.9(4) . . . . ?
O1 V2 N5 C26 -86.2(2) . . . . ?
N6 V2 N5 C26 74.4(2) . . . . ?
N4 V2 N5 C26 1.3(2) . . . . ?
O4 V2 N6 C32 173.1(2) . . . . ?
O5 V2 N6 C32 70.3(2) . . . . ?
O1 V2 N6 C32 -1.9(4) . . . . ?
N5 V2 N6 C32 -93.7(2) . . . . ?
N4 V2 N6 C32 -18.2(2) . . . . ?
O4 V2 N6 C36 -12.0(2) . . . . ?
O5 V2 N6 C36 -114.9(2) . . . . ?
O1 V2 N6 C36 172.9(2) . . . . ?
N5 V2 N6 C36 81.2(2) . . . . ?
N4 V2 N6 C36 156.7(2) . . . . ?
V1 O1 C1 C6 -118.3(2) . . . . ?
V2 O1 C1 C6 57.9(3) . . . . ?
V1 O1 C1 C2 61.3(3) . . . . ?
V2 O1 C1 C2 -122.5(2) . . . . ?
C6 C1 C2 C3 -0.2(4) . . . . ?
O1 C1 C2 C3 -179.8(2) . . . . ?
C6 C1 C2 C11 172.5(3) . . . . ?
O1 C1 C2 C11 -7.0(4) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C11 C2 C3 C4 -172.6(3) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C2 C3 C4 C7 -179.7(3) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C7 C4 C5 C6 179.8(3) . . . . ?
C4 C5 C6 C1 -0.1(4) . . . . ?
C4 C5 C6 C24 -176.3(3) . . . . ?
O1 C1 C6 C5 179.8(2) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
O1 C1 C6 C24 -4.0(4) . . . . ?
C2 C1 C6 C24 176.5(3) . . . . ?
C3 C4 C7 C9 -125.9(3) . . . . ?
C5 C4 C7 C9 54.2(4) . . . . ?
C3 C4 C7 C10 113.2(3) . . . . ?
C5 C4 C7 C10 -66.7(4) . . . . ?
C3 C4 C7 C8 -6.0(4) . . . . ?
C5 C4 C7 C8 174.1(3) . . . . ?
C18 N1 C11 C2 -177.4(2) . . . . ?
C12 N1 C11 C2 -55.6(3) . . . . ?
V1 N1 C11 C2 66.0(3) . . . . ?
C3 C2 C11 N1 109.2(3) . . . . ?
C1 C2 C11 N1 -63.3(3) . . . . ?
C18 N1 C12 C13 -141.1(2) . . . . ?
C11 N1 C12 C13 96.0(3) . . . . ?
V1 N1 C12 C13 -25.5(3) . . . . ?
C17 N2 C13 C14 -3.8(4) . . . . ?
V1 N2 C13 C14 167.3(2) . . . . ?
C17 N2 C13 C12 172.6(2) . . . . ?
V1 N2 C13 C12 -16.2(3) . . . . ?
N1 C12 C13 N2 28.1(3) . . . . ?
N1 C12 C13 C14 -155.5(3) . . . . ?
N2 C13 C14 C15 3.3(5) . . . . ?
C12 C13 C14 C15 -172.9(3) . . . . ?
C13 C14 C15 C16 -0.6(5) . . . . ?
C14 C15 C16 C17 -1.5(5) . . . . ?
C13 N2 C17 C16 1.6(4) . . . . ?
V1 N2 C17 C16 -169.4(2) . . . . ?
C15 C16 C17 N2 1.1(5) . . . . ?
C12 N1 C18 C19 72.1(3) . . . . ?
C11 N1 C18 C19 -165.4(2) . . . . ?
V1 N1 C18 C19 -46.2(2) . . . . ?
C23 N3 C19 C20 -3.2(4) . . . . ?
V1 N3 C19 C20 176.5(2) . . . . ?
C23 N3 C19 C18 176.6(3) . . . . ?
V1 N3 C19 C18 -3.7(3) . . . . ?
N1 C18 C19 N3 35.0(3) . . . . ?
N1 C18 C19 C20 -145.2(3) . . . . ?
N3 C19 C20 C21 2.7(5) . . . . ?
C18 C19 C20 C21 -177.1(3) . . . . ?
C19 C20 C21 C22 -0.3(5) . . . . ?
C20 C21 C22 C23 -1.5(5) . . . . ?
C19 N3 C23 C22 1.4(5) . . . . ?
V1 N3 C23 C22 -178.3(2) . . . . ?
C21 C22 C23 N3 1.0(5) . . . . ?
C31 N4 C24 C6 -179.6(2) . . . . ?
C25 N4 C24 C6 -56.5(3) . . . . ?
V2 N4 C24 C6 65.0(3) . . . . ?
C5 C6 C24 N4 111.7(3) . . . . ?
C1 C6 C24 N4 -64.5(3) . . . . ?
C31 N4 C25 C26 -137.7(2) . . . . ?
C24 N4 C25 C26 98.3(3) . . . . ?
V2 N4 C25 C26 -23.3(3) . . . . ?
C30 N5 C26 C27 -3.0(4) . . . . ?
V2 N5 C26 C27 170.0(2) . . . . ?
C30 N5 C26 C25 171.7(2) . . . . ?
V2 N5 C26 C25 -15.3(3) . . . . ?
N4 C25 C26 N5 26.0(4) . . . . ?
N4 C25 C26 C27 -159.3(3) . . . . ?
N5 C26 C27 C28 2.9(4) . . . . ?
C25 C26 C27 C28 -171.6(3) . . . . ?
C26 C27 C28 C29 -0.1(5) . . . . ?
C27 C28 C29 C30 -2.2(4) . . . . ?
C26 N5 C30 C29 0.6(4) . . . . ?
V2 N5 C30 C29 -172.3(2) . . . . ?
C28 C29 C30 N5 2.1(5) . . . . ?
C25 N4 C31 C32 69.0(3) . . . . ?
C24 N4 C31 C32 -168.0(2) . . . . ?
V2 N4 C31 C32 -49.0(2) . . . . ?
C36 N6 C32 C33 -0.7(4) . . . . ?
V2 N6 C32 C33 174.5(2) . . . . ?
C36 N6 C32 C31 -179.8(3) . . . . ?
V2 N6 C32 C31 -4.6(3) . . . . ?
N4 C31 C32 N6 38.1(3) . . . . ?
N4 C31 C32 C33 -141.0(3) . . . . ?
N6 C32 C33 C34 0.3(5) . . . . ?
C31 C32 C33 C34 179.4(3) . . . . ?
C32 C33 C34 C35 -0.2(5) . . . . ?
C33 C34 C35 C36 0.4(5) . . . . ?
C32 N6 C36 C35 0.9(4) . . . . ?
V2 N6 C36 C35 -174.0(2) . . . . ?
C34 C35 C36 N6 -0.8(5) . . . . ?
