#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/29/7002957.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_7002957
loop_
_publ_author_name
'Veltzé, Sune'
'Egdal, Rune Kirk'
'Johansson, Frank B.'
'Bond, Andrew D.'
'McKenzie, Christine J.'
_publ_section_title
;
 Coordinative flexibility in an acyclic bis(sulfonamide) ligand
;
_journal_issue                   47
_journal_name_full               'Dalton Transactions'
_journal_page_first              10495
_journal_page_last               10504
_journal_paper_doi               10.1039/b912617a
_journal_year                    2009
_chemical_formula_moiety
;
70 % : (C32 H34 N6 O7 S2 V 2+), (Cl O4 -)2, (C H4 O)2, H2 O
30 % : (C31 H32 N6 O7 S2 V 2+), (Cl O4 -)2, (C H4 O)2, 2(H2 O)
;
_chemical_formula_sum            'C33.7 H44 Cl2 N6 O18.3 S2 V'
_chemical_formula_weight         1011.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 119.576(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9275(11)
_cell_length_b                   25.6124(17)
_cell_length_c                   14.0430(10)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.30
_cell_volume                     4356.7(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            86785
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2094
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8891
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0500
_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)+(0.0692P)²+3.3202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                6006
_reflns_number_total             8891
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b912617a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C33.70 H44 Cl2 N6 O18.30 S2 V'
_cod_database_code               7002957
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.90988(4) 0.097661(19) 0.31361(4) 0.02229(15) Uani 1 1 d . . .
S1 S 0.73549(7) 0.08617(3) 0.51108(7) 0.0274(2) Uani 1 1 d . . .
S2 S 0.87051(7) 0.23022(3) 0.31595(7) 0.0302(2) Uani 1 1 d . . .
O1 O 0.80206(17) 0.12486(8) 0.34996(16) 0.0243(5) Uani 1 1 d . . .
O2 O 0.91172(19) 0.03633(8) 0.32901(18) 0.0323(5) Uani 1 1 d . . .
O11 O 0.7026(2) 0.08987(9) 0.59257(19) 0.0368(6) Uani 1 1 d . . .
O12 O 0.80940(19) 0.04539(9) 0.5198(2) 0.0357(6) Uani 1 1 d . . .
O21 O 0.7721(2) 0.22048(9) 0.21466(19) 0.0368(6) Uani 1 1 d . . .
O22 O 0.9154(2) 0.28180(8) 0.3363(2) 0.0424(6) Uani 1 1 d . . .
N1 N 0.6224(2) 0.07802(10) 0.3940(2) 0.0278(6) Uani 1 1 d . . .
N2 N 0.4889(2) -0.01121(11) 0.3044(2) 0.0286(6) Uani 1 1 d . . .
H2A H 0.4754 0.0126 0.3413 0.034 Uiso 1 1 calc R . .
N3 N 0.4252(2) 0.06061(11) 0.4069(2) 0.0323(7) Uani 1 1 d . . .
N4 N 0.9658(2) 0.18698(9) 0.3197(2) 0.0234(6) Uani 1 1 d . . .
N5 N 1.0228(2) 0.10054(10) 0.2544(2) 0.0279(6) Uani 1 1 d . A .
N6 N 1.0340(2) 0.11157(9) 0.4783(2) 0.0226(6) Uani 1 1 d . A .
C1 C 0.8154(2) 0.15950(12) 0.4249(2) 0.0243(7) Uani 1 1 d . . .
C2 C 0.7895(3) 0.14839(12) 0.5078(3) 0.0277(7) Uani 1 1 d . . .
C3 C 0.8014(3) 0.18558(14) 0.5844(3) 0.0396(9) Uani 1 1 d . . .
H3A H 0.7808 0.1770 0.6378 0.047 Uiso 1 1 calc R A .
C4 C 0.8426(4) 0.23518(15) 0.5853(3) 0.0472(10) Uani 1 1 d . . .
C5 C 0.8685(3) 0.24696(13) 0.5052(3) 0.0393(9) Uani 1 1 d . . .
H5A H 0.8961 0.2806 0.5036 0.047 Uiso 1 1 calc R A .
C6 C 0.8546(3) 0.21017(12) 0.4264(3) 0.0270(7) Uani 1 1 d . . .
C7 C 0.8529(5) 0.27559(19) 0.6681(4) 0.0804(17) Uani 1 1 d . . .
H7A H 0.8422 0.3105 0.6358 0.121 Uiso 1 1 calc R A .
H7B H 0.9264 0.2734 0.7329 0.121 Uiso 1 1 calc R . .
H7C H 0.7966 0.2692 0.6894 0.121 Uiso 1 1 calc R . .
C8 C 0.6268(3) 0.04972(13) 0.3053(3) 0.0340(8) Uani 1 1 d . . .
H8A H 0.7051 0.0433 0.3270 0.041 Uiso 1 1 calc R . .
H8B H 0.5948 0.0721 0.2392 0.041 Uiso 1 1 calc R . .
C9 C 0.5662(3) -0.00182(13) 0.2767(2) 0.0279(7) Uani 1 1 d . . .
C10 C 0.5872(3) -0.03908(15) 0.2193(3) 0.0416(9) Uani 1 1 d . . .
H10A H 0.6418 -0.0329 0.1988 0.050 Uiso 1 1 calc R . .
C11 C 0.5292(4) -0.08554(16) 0.1912(3) 0.0492(10) Uani 1 1 d . . .
H11A H 0.5437 -0.1115 0.1516 0.059 Uiso 1 1 calc R . .
C12 C 0.4503(4) -0.09370(16) 0.2211(3) 0.0498(10) Uani 1 1 d . . .
H12A H 0.4096 -0.1254 0.2024 0.060 Uiso 1 1 calc R . .
C13 C 0.4309(3) -0.05604(14) 0.2775(3) 0.0383(9) Uani 1 1 d . . .
H13A H 0.3762 -0.0613 0.2982 0.046 Uiso 1 1 calc R . .
C14 C 0.5363(3) 0.11881(13) 0.3650(3) 0.0354(8) Uani 1 1 d . . .
H14A H 0.4895 0.1202 0.2843 0.042 Uiso 1 1 calc R . .
H14B H 0.5728 0.1532 0.3897 0.042 Uiso 1 1 calc R . .
C15 C 0.4641(3) 0.10937(13) 0.4148(3) 0.0337(8) Uani 1 1 d . . .
C16 C 0.4357(3) 0.14907(15) 0.4622(4) 0.0485(10) Uani 1 1 d . . .
H16A H 0.4651 0.1831 0.4681 0.058 Uiso 1 1 calc R . .
C17 C 0.3638(3) 0.13872(17) 0.5010(4) 0.0535(11) Uani 1 1 d . . .
H17A H 0.3425 0.1658 0.5330 0.064 Uiso 1 1 calc R . .
C18 C 0.3235(3) 0.08913(17) 0.4932(3) 0.0458(10) Uani 1 1 d . . .
H18A H 0.2743 0.0811 0.5197 0.055 Uiso 1 1 calc R . .
C19 C 0.3563(3) 0.05131(15) 0.4455(3) 0.0383(9) Uani 1 1 d . . .
H19A H 0.3286 0.0169 0.4398 0.046 Uiso 1 1 calc R . .
C20 C 0.9748(3) 0.19216(12) 0.2184(3) 0.0304(8) Uani 1 1 d . . .
H20A H 1.0151 0.2245 0.2215 0.036 Uiso 1 1 calc R A .
H20B H 0.9003 0.1938 0.1530 0.036 Uiso 1 1 calc R . .
C21 C 1.0360(3) 0.14545(13) 0.2116(3) 0.0316(8) Uani 1 1 d . A .
C22 C 1.1007(3) 0.14817(16) 0.1628(3) 0.0418(9) Uani 1 1 d . . .
H22A H 1.1097 0.1803 0.1343 0.050 Uiso 1 1 calc R A .
C23 C 1.1523(3) 0.10347(18) 0.1559(3) 0.0506(11) Uani 1 1 d . . .
H23A H 1.1965 0.1045 0.1217 0.061 Uiso 1 1 calc R . .
C24 C 1.1393(3) 0.05774(17) 0.1986(3) 0.0462(10) Uani 1 1 d . . .
H24A H 1.1743 0.0267 0.1942 0.055 Uiso 1 1 calc R A .
C25 C 1.0751(3) 0.05728(14) 0.2477(3) 0.0374(8) Uani 1 1 d . A .
H25A H 1.0671 0.0255 0.2780 0.045 Uiso 1 1 calc R . .
C26 C 1.0750(3) 0.19394(12) 0.4206(3) 0.0290(7) Uani 1 1 d . . .
H26A H 1.0813 0.2303 0.4472 0.035 Uiso 1 1 calc R A .
H26B H 1.1345 0.1881 0.4026 0.035 Uiso 1 1 calc R . .
C27 C 1.0898(2) 0.15689(11) 0.5096(3) 0.0251(7) Uani 1 1 d . A .
C28 C 1.1614(3) 0.16811(13) 0.6178(3) 0.0363(8) Uani 1 1 d . . .
H28A H 1.1996 0.2005 0.6375 0.044 Uiso 1 1 calc R A .
C29 C 1.1778(3) 0.13254(14) 0.6972(3) 0.0416(9) Uani 1 1 d . . .
H29A H 1.2275 0.1398 0.7722 0.050 Uiso 1 1 calc R . .
C30 C 1.1205(3) 0.08585(13) 0.6662(3) 0.0348(8) Uani 1 1 d . . .
H30A H 1.1298 0.0605 0.7194 0.042 Uiso 1 1 calc R A .
C31 C 1.0501(3) 0.07687(12) 0.5573(3) 0.0275(7) Uani 1 1 d . A .
H31A H 1.0109 0.0448 0.5363 0.033 Uiso 1 1 calc R . .
C100 C 0.6779(5) 0.1129(3) 0.1002(5) 0.0552(16) Uani 0.70 1 d P A 1
H103 H 0.6534 0.1353 0.0357 0.083 Uiso 0.70 1 calc PR A 1
H102 H 0.6565 0.1288 0.1505 0.083 Uiso 0.70 1 calc PR A 1
H101 H 0.6433 0.0785 0.0774 0.083 Uiso 0.70 1 calc PR A 1
O100 O 0.79736(18) 0.10730(9) 0.15512(17) 0.0331(5) Uani 0.70 1 d P A 1
H100 H 0.8021 0.0875 0.1090 0.040 Uiso 0.70 1 d PR A 1
O1W O 0.79736(18) 0.10730(9) 0.15512(17) 0.0331(5) Uani 0.30 1 d P A 2
H1W H 0.8021 0.0875 0.1090 0.050 Uiso 0.30 1 d PR A 2
H2W H 0.7332 0.1198 0.1327 0.050 Uiso 0.30 1 d PR A 2
O2W O 0.5945(10) 0.1469(4) 0.0860(9) 0.073(3) Uiso 0.30 1 d P B 2
H3W H 0.6270 0.1581 0.0523 0.109 Uiso 0.30 1 d PR B 2
H4W H 0.5270 0.1379 0.0551 0.109 Uiso 0.30 1 d PR B 2
Cl1 Cl 0.77949(8) 0.20977(3) 0.88687(7) 0.0381(2) Uani 1 1 d D . .
O1A O 0.7387(3) 0.25912(11) 0.8381(3) 0.0664(9) Uani 1 1 d D . .
O1B O 0.7589(3) 0.17326(12) 0.8028(3) 0.0823(11) Uani 1 1 d D . .
O1C O 0.7277(3) 0.19287(13) 0.9461(3) 0.0776(10) Uani 1 1 d D . .
O1D O 0.8954(3) 0.21372(17) 0.9580(3) 0.0976(13) Uani 1 1 d D . .
Cl2 Cl 0.66161(8) -0.07344(4) -0.01506(8) 0.0485(3) Uani 1 1 d D . .
O2A O 0.6413(10) -0.0757(4) -0.1224(6) 0.075(4) Uani 0.50 1 d PD C 1
O2B O 0.6271(9) -0.1174(3) 0.0174(7) 0.103(3) Uani 0.50 1 d PD C 1
O2C O 0.7695(6) -0.0610(5) 0.0582(7) 0.137(5) Uani 0.50 1 d PD C 1
O2D O 0.5899(11) -0.0319(4) -0.0140(8) 0.146(6) Uani 0.50 1 d PD C 1
O2E O 0.7349(9) -0.1181(3) 0.0185(7) 0.115(3) Uani 0.50 1 d PD C 2
O2F O 0.5585(5) -0.0860(6) -0.0340(7) 0.201(9) Uani 0.50 1 d PD C 2
O2G O 0.6612(10) -0.0507(4) -0.1064(7) 0.081(4) Uani 0.50 1 d PD C 2
O2H O 0.7148(9) -0.0383(4) 0.0732(7) 0.095(3) Uani 0.50 1 d PD C 2
O3W O 0.8328(3) 0.04577(12) 0.0312(2) 0.0620(8) Uani 1 1 d . . .
H5W H 0.8146 0.0151 0.0393 0.093 Uiso 1 1 d R . .
H6W H 0.8408 0.0548 -0.0228 0.093 Uiso 1 1 d R . .
O1S O 0.8590(3) 0.07342(11) 0.8587(2) 0.0616(8) Uani 1 1 d . . .
H1S H 0.8291 0.1034 0.8419 0.092 Uiso 1 1 d R . .
C1S C 0.9612(4) 0.0773(2) 0.8621(4) 0.0707(14) Uani 1 1 d . . .
H1S1 H 1.0007 0.1082 0.9043 0.106 Uiso 1 1 calc R . .
H1S2 H 0.9491 0.0803 0.7873 0.106 Uiso 1 1 calc R . .
H1S3 H 1.0053 0.0460 0.8969 0.106 Uiso 1 1 calc R . .
O2S O 0.0665(5) 0.2418(2) 0.9262(5) 0.161(2) Uani 1 1 d . . .
H2S H 0.0130 0.2332 0.9359 0.241 Uiso 1 1 d R . .
C2S C 0.0974(8) 0.2107(4) 0.8581(9) 0.169(4) Uani 1 1 d . . .
H2S1 H 0.1390 0.2325 0.8337 0.254 Uiso 1 1 calc R . .
H2S2 H 0.0306 0.1976 0.7942 0.254 Uiso 1 1 calc R . .
H2S3 H 0.1434 0.1812 0.9008 0.254 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'
S S 0.1246 0.1234 '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 O1 106.43(10) . . ?
O2 V1 O100 102.97(11) . . ?
O1 V1 O100 88.02(9) . . ?
O2 V1 N5 97.09(11) . . ?
O1 V1 N5 156.23(10) . . ?
O100 V1 N5 83.36(10) . . ?
O2 V1 N6 93.90(10) . . ?
O1 V1 N6 88.45(9) . . ?
O100 V1 N6 163.07(10) . . ?
N5 V1 N6 93.39(10) . . ?
O2 V1 N4 162.85(11) . . ?
O1 V1 N4 85.86(8) . . ?
O100 V1 N4 89.10(9) . . ?
N5 V1 N4 71.94(9) . . ?
N6 V1 N4 74.13(9) . . ?
O12 S1 O11 118.82(14) . . ?
O12 S1 N1 106.76(14) . . ?
O11 S1 N1 106.43(14) . . ?
O12 S1 C2 111.25(14) . . ?
O11 S1 C2 105.60(14) . . ?
N1 S1 C2 107.41(14) . . ?
O21 S2 O22 118.08(15) . . ?
O21 S2 N4 105.43(13) . . ?
O22 S2 N4 109.66(14) . . ?
O21 S2 C6 110.67(15) . . ?
O22 S2 C6 109.21(15) . . ?
N4 S2 C6 102.62(13) . . ?
C1 O1 V1 129.05(19) . . ?
C8 N1 C14 118.7(3) . . ?
C8 N1 S1 119.5(2) . . ?
C14 N1 S1 115.6(2) . . ?
C9 N2 C13 122.1(3) . . ?
C9 N2 H2A 119.0 . . ?
C13 N2 H2A 119.0 . . ?
C19 N3 C15 118.2(3) . . ?
C26 N4 C20 111.6(2) . . ?
C26 N4 S2 111.4(2) . . ?
C20 N4 S2 109.99(19) . . ?
C26 N4 V1 107.93(17) . . ?
C20 N4 V1 103.20(17) . . ?
S2 N4 V1 112.52(12) . . ?
C21 N5 C25 118.0(3) . . ?
C21 N5 V1 119.7(2) . . ?
C25 N5 V1 122.0(2) . . ?
C27 N6 C31 117.6(3) . . ?
C27 N6 V1 122.0(2) . . ?
C31 N6 V1 120.0(2) . . ?
O1 C1 C6 122.3(3) . . ?
O1 C1 C2 122.1(3) . . ?
C6 C1 C2 115.6(3) . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 S1 119.2(2) . . ?
C1 C2 S1 119.3(2) . . ?
C2 C3 C4 121.7(3) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 117.8(3) . . ?
C5 C4 C7 121.1(3) . . ?
C3 C4 C7 121.0(3) . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C5 C6 C1 122.5(3) . . ?
C5 C6 S2 118.6(2) . . ?
C1 C6 S2 118.5(2) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 113.9(3) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C10 118.8(3) . . ?
N2 C9 C8 120.3(3) . . ?
C10 C9 C8 120.8(3) . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10A 119.9 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11A 120.4 . . ?
C10 C11 H11A 120.4 . . ?
C13 C12 C11 119.4(4) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
N2 C13 C12 120.3(3) . . ?
N2 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
N1 C14 C15 113.2(3) . . ?
N1 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
N1 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.8 . . ?
N3 C15 C16 121.8(3) . . ?
N3 C15 C14 116.5(3) . . ?
C16 C15 C14 121.6(3) . . ?
C15 C16 C17 119.1(4) . . ?
C15 C16 H16A 120.5 . . ?
C17 C16 H16A 120.5 . . ?
C18 C17 C16 119.6(4) . . ?
C18 C17 H17A 120.2 . . ?
C16 C17 H17A 120.2 . . ?
C17 C18 C19 118.0(4) . . ?
C17 C18 H18A 121.0 . . ?
C19 C18 H18A 121.0 . . ?
N3 C19 C18 123.3(4) . . ?
N3 C19 H19A 118.3 . . ?
C18 C19 H19A 118.3 . . ?
N4 C20 C21 107.9(3) . . ?
N4 C20 H20A 110.1 . . ?
C21 C20 H20A 110.1 . . ?
N4 C20 H20B 110.1 . . ?
C21 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
N5 C21 C22 122.0(3) . . ?
N5 C21 C20 116.4(3) . . ?
C22 C21 C20 121.6(3) . . ?
C21 C22 C23 119.0(4) . . ?
C21 C22 H22A 120.5 . . ?
C23 C22 H22A 120.5 . . ?
C24 C23 C22 119.6(3) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C25 119.2(3) . . ?
C23 C24 H24A 120.4 . . ?
C25 C24 H24A 120.4 . . ?
N5 C25 C24 122.3(4) . . ?
N5 C25 H25A 118.9 . . ?
C24 C25 H25A 118.9 . . ?
N4 C26 C27 111.9(2) . . ?
N4 C26 H26A 109.2 . . ?
C27 C26 H26A 109.2 . . ?
N4 C26 H26B 109.2 . . ?
C27 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
N6 C27 C28 122.0(3) . . ?
N6 C27 C26 116.9(3) . . ?
C28 C27 C26 121.0(3) . . ?
C29 C28 C27 120.0(3) . . ?
C29 C28 H28A 120.0 . . ?
C27 C28 H28A 120.0 . . ?
C28 C29 C30 118.7(3) . . ?
C28 C29 H29A 120.7 . . ?
C30 C29 H29A 120.7 . . ?
C31 C30 C29 118.8(3) . . ?
C31 C30 H30A 120.6 . . ?
C29 C30 H30A 120.6 . . ?
N6 C31 C30 123.0(3) . . ?
N6 C31 H31A 118.5 . . ?
C30 C31 H31A 118.5 . . ?
C100 O100 V1 131.5(3) . . ?
C100 O100 H100 98.8 . . ?
V1 O100 H100 117.4 . . ?
V1 O1W H1W 117.4 . . ?
V1 O1W H2W 124.0 . . ?
H1W O1W H2W 113.9 . . ?
H3W O2W H4W 124.4 . . ?
H5W O3W H6W 123.3 . . ?
O1C Cl1 O1A 110.99(19) . . ?
O1C Cl1 O1B 109.6(2) . . ?
O1A Cl1 O1B 108.53(19) . . ?
O1C Cl1 O1D 110.0(2) . . ?
O1A Cl1 O1D 108.8(2) . . ?
O1B Cl1 O1D 108.9(2) . . ?
O2C Cl2 O2B 111.7(5) . . ?
O2C Cl2 O2A 112.5(6) . . ?
O2B Cl2 O2A 113.9(5) . . ?
O2C Cl2 O2D 108.8(6) . . ?
O2B Cl2 O2D 103.7(5) . . ?
O2A Cl2 O2D 105.4(5) . . ?
O2F Cl2 O2G 113.0(5) . . ?
O2F Cl2 O2H 111.6(6) . . ?
O2G Cl2 O2H 107.5(5) . . ?
O2F Cl2 O2E 112.5(6) . . ?
O2G Cl2 O2E 108.0(5) . . ?
O2H Cl2 O2E 103.8(5) . . ?
C1S O1S H1S 107.2 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 122.0 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
V1 O2 1.584(2) . ?
V1 O1 1.939(2) . ?
V1 O100 2.007(2) . ?
V1 N5 2.112(3) . ?
V1 N6 2.125(3) . ?
V1 N4 2.404(2) . ?
S1 O12 1.429(2) . ?
S1 O11 1.431(2) . ?
S1 N1 1.635(3) . ?
S1 C2 1.772(3) . ?
S2 O21 1.428(3) . ?
S2 O22 1.429(2) . ?
S2 N4 1.709(3) . ?
S2 C6 1.748(3) . ?
O1 C1 1.318(4) . ?
N1 C8 1.468(4) . ?
N1 C14 1.487(4) . ?
N2 C9 1.335(4) . ?
N2 C13 1.346(4) . ?
N2 H2A 0.880 . ?
N3 C19 1.336(4) . ?
N3 C15 1.343(4) . ?
N4 C26 1.492(4) . ?
N4 C20 1.496(4) . ?
N5 C21 1.351(4) . ?
N5 C25 1.355(4) . ?
N6 C27 1.345(4) . ?
N6 C31 1.351(4) . ?
C1 C6 1.404(4) . ?
C1 C2 1.407(4) . ?
C2 C3 1.385(5) . ?
C3 C4 1.392(5) . ?
C3 H3A 0.950 . ?
C4 C5 1.373(5) . ?
C4 C7 1.510(5) . ?
C5 C6 1.393(5) . ?
C5 H5A 0.950 . ?
C7 H7A 0.980 . ?
C7 H7B 0.980 . ?
C7 H7C 0.980 . ?
C8 C9 1.510(4) . ?
C8 H8A 0.990 . ?
C8 H8B 0.990 . ?
C9 C10 1.370(5) . ?
C10 C11 1.382(5) . ?
C10 H10A 0.950 . ?
C11 C12 1.372(6) . ?
C11 H11A 0.950 . ?
C12 C13 1.357(5) . ?
C12 H12A 0.950 . ?
C13 H13A 0.950 . ?
C14 C15 1.503(5) . ?
C14 H14A 0.990 . ?
C14 H14B 0.990 . ?
C15 C16 1.375(5) . ?
C16 C17 1.382(6) . ?
C16 H16A 0.950 . ?
C17 C18 1.371(6) . ?
C17 H17A 0.950 . ?
C18 C19 1.378(5) . ?
C18 H18A 0.950 . ?
C19 H19A 0.950 . ?
C20 C21 1.499(5) . ?
C20 H20A 0.990 . ?
C20 H20B 0.990 . ?
C21 C22 1.377(5) . ?
C22 C23 1.380(5) . ?
C22 H22A 0.950 . ?
C23 C24 1.367(6) . ?
C23 H23A 0.950 . ?
C24 C25 1.372(5) . ?
C24 H24A 0.950 . ?
C25 H25A 0.950 . ?
C26 C27 1.500(4) . ?
C26 H26A 0.990 . ?
C26 H26B 0.990 . ?
C27 C28 1.374(5) . ?
C28 C29 1.369(5) . ?
C28 H28A 0.950 . ?
C29 C30 1.383(5) . ?
C29 H29A 0.950 . ?
C30 C31 1.368(5) . ?
C30 H30A 0.950 . ?
C31 H31A 0.950 . ?
C100 O100 1.455(6) . ?
C100 H103 0.980 . ?
C100 H102 0.980 . ?
C100 H101 0.980 . ?
O100 H100 0.850 . ?
O1W H1W 0.850 . ?
O1W H2W 0.850 . ?
O2W H3W 0.850 . ?
O2W H4W 0.850 . ?
O3W H5W 0.850 . ?
O3W H6W 0.850 . ?
Cl1 O1A 1.416(3) . ?
Cl1 O1B 1.420(3) . ?
Cl1 O1C 1.411(3) . ?
Cl1 O1D 1.422(3) . ?
Cl2 O2A 1.391(6) . ?
Cl2 O2B 1.388(5) . ?
Cl2 O2C 1.376(6) . ?
Cl2 O2D 1.464(6) . ?
Cl2 O2E 1.448(6) . ?
Cl2 O2F 1.363(6) . ?
Cl2 O2G 1.407(6) . ?
Cl2 O2H 1.410(6) . ?
O1S C1S 1.405(6) . ?
O1S H1S 0.850 . ?
C1S H1S1 0.980 . ?
C1S H1S2 0.980 . ?
C1S H1S3 0.980 . ?
O2S C2S 1.463(9) . ?
O2S H2S 0.850 . ?
C2S H2S1 0.980 . ?
C2S H2S2 0.980 . ?
C2S H2S3 0.980 . ?
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
O1S H1S O1B 0.85 1.98 2.832(4) 179.8 .
O2S H2S O1D 0.85 1.88 2.729(7) 179.5 1_455
O3W H5W O2C 0.85 2.10 2.955(11) 179.5 .
O3W H6W O1S 0.85 1.87 2.715(4) 179.1 1_554
O2W H4W O2B 0.85 1.94 2.789(15) 179.2 3_655
O2W H3W O1C 0.85 2.66 3.505(12) 179.8 1_554
O1W H1W O3W 0.85 1.73 2.570(4) 171.0 .
O1W H2W O2W 0.85 1.84 2.692(12) 179.2 .
O100 H100 O3W 0.85 1.73 2.570(4) 171.0 .
N2 H2A N3 0.88 1.87 2.740(4) 171.7 .
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 121.9(2) . . . . ?
O100 V1 O1 C1 -135.1(2) . . . . ?
N5 V1 O1 C1 -66.6(4) . . . . ?
N6 V1 O1 C1 28.3(2) . . . . ?
N4 V1 O1 C1 -45.9(2) . . . . ?
O12 S1 N1 C8 -24.0(3) . . . . ?
O11 S1 N1 C8 -151.9(2) . . . . ?
C2 S1 N1 C8 95.4(3) . . . . ?
O12 S1 N1 C14 -176.1(2) . . . . ?
O11 S1 N1 C14 56.1(2) . . . . ?
C2 S1 N1 C14 -56.6(2) . . . . ?
O21 S2 N4 C26 178.14(19) . . . . ?
O22 S2 N4 C26 50.0(2) . . . . ?
C6 S2 N4 C26 -65.9(2) . . . . ?
O21 S2 N4 C20 53.9(2) . . . . ?
O22 S2 N4 C20 -74.2(2) . . . . ?
C6 S2 N4 C20 169.8(2) . . . . ?
O21 S2 N4 V1 -60.52(15) . . . . ?
O22 S2 N4 V1 171.37(14) . . . . ?
C6 S2 N4 V1 55.39(16) . . . . ?
O2 V1 N4 C26 -28.9(4) . . . . ?
O1 V1 N4 C26 107.71(19) . . . . ?
O100 V1 N4 C26 -164.21(19) . . . . ?
N5 V1 N4 C26 -80.90(19) . . . . ?
N6 V1 N4 C26 18.15(18) . . . . ?
O2 V1 N4 C20 89.3(4) . . . . ?
O1 V1 N4 C20 -134.07(19) . . . . ?
O100 V1 N4 C20 -45.99(19) . . . . ?
N5 V1 N4 C20 37.32(18) . . . . ?
N6 V1 N4 C20 136.4(2) . . . . ?
O2 V1 N4 S2 -152.2(3) . . . . ?
O1 V1 N4 S2 -15.56(13) . . . . ?
O100 V1 N4 S2 72.52(14) . . . . ?
N5 V1 N4 S2 155.83(16) . . . . ?
N6 V1 N4 S2 -105.12(14) . . . . ?
O2 V1 N5 C21 169.4(2) . . . . ?
O1 V1 N5 C21 -2.4(4) . . . . ?
O100 V1 N5 C21 67.0(2) . . . . ?
N6 V1 N5 C21 -96.3(2) . . . . ?
N4 V1 N5 C21 -24.2(2) . . . . ?
O2 V1 N5 C25 -4.0(3) . . . . ?
O1 V1 N5 C25 -175.8(2) . . . . ?
O100 V1 N5 C25 -106.4(3) . . . . ?
N6 V1 N5 C25 90.3(3) . . . . ?
N4 V1 N5 C25 162.4(3) . . . . ?
O2 V1 N6 C27 162.6(2) . . . . ?
O1 V1 N6 C27 -91.1(2) . . . . ?
O100 V1 N6 C27 -13.1(5) . . . . ?
N5 V1 N6 C27 65.2(2) . . . . ?
N4 V1 N6 C27 -4.9(2) . . . . ?
O2 V1 N6 C31 -25.0(2) . . . . ?
O1 V1 N6 C31 81.4(2) . . . . ?
O100 V1 N6 C31 159.4(3) . . . . ?
N5 V1 N6 C31 -122.3(2) . . . . ?
N4 V1 N6 C31 167.5(2) . . . . ?
V1 O1 C1 C6 58.1(4) . . . . ?
V1 O1 C1 C2 -123.0(3) . . . . ?
O1 C1 C2 C3 -178.4(3) . . . . ?
C6 C1 C2 C3 0.5(5) . . . . ?
O1 C1 C2 S1 -0.8(4) . . . . ?
C6 C1 C2 S1 178.2(2) . . . . ?
O12 S1 C2 C3 -124.0(3) . . . . ?
O11 S1 C2 C3 6.2(3) . . . . ?
N1 S1 C2 C3 119.5(3) . . . . ?
O12 S1 C2 C1 58.3(3) . . . . ?
O11 S1 C2 C1 -171.5(3) . . . . ?
N1 S1 C2 C1 -58.2(3) . . . . ?
C1 C2 C3 C4 -2.0(6) . . . . ?
S1 C2 C3 C4 -179.6(3) . . . . ?
C2 C3 C4 C5 1.9(6) . . . . ?
C2 C3 C4 C7 178.8(4) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C7 C4 C5 C6 -177.4(4) . . . . ?
C4 C5 C6 C1 -0.8(6) . . . . ?
C4 C5 C6 S2 171.2(3) . . . . ?
O1 C1 C6 C5 179.7(3) . . . . ?
C2 C1 C6 C5 0.8(5) . . . . ?
O1 C1 C6 S2 7.7(4) . . . . ?
C2 C1 C6 S2 -171.2(2) . . . . ?
O21 S2 C6 C5 -121.5(3) . . . . ?
O22 S2 C6 C5 10.1(3) . . . . ?
N4 S2 C6 C5 126.4(3) . . . . ?
O21 S2 C6 C1 50.8(3) . . . . ?
O22 S2 C6 C1 -177.5(2) . . . . ?
N4 S2 C6 C1 -61.2(3) . . . . ?
C14 N1 C8 C9 -95.6(3) . . . . ?
S1 N1 C8 C9 113.2(3) . . . . ?
C13 N2 C9 C10 -0.1(5) . . . . ?
C13 N2 C9 C8 178.0(3) . . . . ?
N1 C8 C9 N2 20.2(4) . . . . ?
N1 C8 C9 C10 -161.7(3) . . . . ?
N2 C9 C10 C11 -0.2(5) . . . . ?
C8 C9 C10 C11 -178.3(3) . . . . ?
C9 C10 C11 C12 0.3(6) . . . . ?
C10 C11 C12 C13 0.0(6) . . . . ?
C9 N2 C13 C12 0.4(5) . . . . ?
C11 C12 C13 N2 -0.3(6) . . . . ?
C8 N1 C14 C15 123.5(3) . . . . ?
S1 N1 C14 C15 -84.2(3) . . . . ?
C19 N3 C15 C16 0.7(5) . . . . ?
C19 N3 C15 C14 -176.8(3) . . . . ?
N1 C14 C15 N3 -46.3(4) . . . . ?
N1 C14 C15 C16 136.2(4) . . . . ?
N3 C15 C16 C17 -1.1(6) . . . . ?
C14 C15 C16 C17 176.3(3) . . . . ?
C15 C16 C17 C18 0.9(6) . . . . ?
C16 C17 C18 C19 -0.4(6) . . . . ?
C15 N3 C19 C18 -0.2(5) . . . . ?
C17 C18 C19 N3 0.0(6) . . . . ?
C26 N4 C20 C21 70.0(3) . . . . ?
S2 N4 C20 C21 -165.9(2) . . . . ?
V1 N4 C20 C21 -45.7(3) . . . . ?
C25 N5 C21 C22 -0.2(5) . . . . ?
V1 N5 C21 C22 -173.9(3) . . . . ?
C25 N5 C21 C20 178.7(3) . . . . ?
V1 N5 C21 C20 5.0(4) . . . . ?
N4 C20 C21 N5 31.3(4) . . . . ?
N4 C20 C21 C22 -149.8(3) . . . . ?
N5 C21 C22 C23 1.0(5) . . . . ?
C20 C21 C22 C23 -177.9(3) . . . . ?
C21 C22 C23 C24 -0.8(6) . . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C21 N5 C25 C24 -0.6(5) . . . . ?
V1 N5 C25 C24 172.9(3) . . . . ?
C23 C24 C25 N5 0.8(6) . . . . ?
C20 N4 C26 C27 -141.0(3) . . . . ?
S2 N4 C26 C27 95.7(3) . . . . ?
V1 N4 C26 C27 -28.3(3) . . . . ?
C31 N6 C27 C28 0.2(4) . . . . ?
V1 N6 C27 C28 172.8(2) . . . . ?
C31 N6 C27 C26 177.3(3) . . . . ?
V1 N6 C27 C26 -10.1(4) . . . . ?
N4 C26 C27 N6 27.0(4) . . . . ?
N4 C26 C27 C28 -155.9(3) . . . . ?
N6 C27 C28 C29 0.2(5) . . . . ?
C26 C27 C28 C29 -176.7(3) . . . . ?
C27 C28 C29 C30 -0.5(6) . . . . ?
C28 C29 C30 C31 0.3(5) . . . . ?
C27 N6 C31 C30 -0.4(5) . . . . ?
V1 N6 C31 C30 -173.2(3) . . . . ?
C29 C30 C31 N6 0.1(5) . . . . ?
O2 V1 O100 C100 86.8(4) . . . . ?
O1 V1 O100 C100 -19.6(4) . . . . ?
N5 V1 O100 C100 -177.4(4) . . . . ?
N6 V1 O100 C100 -97.7(5) . . . . ?
N4 V1 O100 C100 -105.5(4) . . . . ?
