# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Jonathan L. Sessler'
_publ_contact_author_address     
;
University of Texas at Austin
Department of Chemistry and Biochemistry
24th & Speedway
Austin
TX
78712-1167
UNITED STATES OF AMERICA
;

_publ_contact_author_email       SESSLER@MAIL.UTEXAS.EDU

_publ_section_title              
;
Coordination of oxovanadium(V) in an expanded
porphyrin macrocycle
;
loop_
_publ_author_name
'Jonathan L. Sessler'
'Vincent Lynch'
'Elisa Tomat'

# Attachment 'VOGRAND2.CIF'

data_vogrand
_database_code_depnum_ccdc_archive 'CCDC 610169'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H47 Cl6 N6 O2 V'
_chemical_formula_weight         907.48

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4914(2)
_cell_length_b                   13.0026(3)
_cell_length_c                   14.8379(5)
_cell_angle_alpha                89.426(1)
_cell_angle_beta                 88.093(1)
_cell_angle_gamma                61.536(1)
_cell_volume                     2117.44(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    7949
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       lathes
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16243
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_av_sigmaI/netI    0.2796
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9540
_reflns_number_gt                3447
_reflns_threshold_expression     >2sigma(I)

_publ_section_references         
;
Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97.
(1999) J. Appl. Cryst. 32, 115-119.

Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology,
276, Macromolecular Crystallography, part A, 307-326, C. W. Carter,
Jr. and R. M. Sweets, Eds., Academic Press.

Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens
Analytical X-ray Instruments, Inc., Madison, WI, USA.

;
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_reduction        
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

One methyl carbon, C37, on an ethyl group was found to be disordered. The
disorder was modeled by assigning the variable x to the site occupancy for C37
and (1-x) to the site occupancy for the alternate orientation represented by
atom, C37a. An isotropic displacement parameter was constrained to be equal for
C37 and C37a while the variable x was refined. The bond length to C36 was
restrained to be equal for C37 and C37a. The site occupancy factor refined to
85(2)% for C37. C37 was refined anisotropically while C37a was refined
isotropically.
A chlorine atom on one of the methylene chloride molecules was also
disordered. The solvent disorder was modeled in a similar manner to that
described above. The major component of the disorder, Cl2c, had a site
occupancy factor of 81(2)%, while the minor component, Cl3c, had a site
occupancy factor of 19(2)%. Both atoms were refined anisotropically.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9540
_refine_ls_number_parameters     517
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.2480
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.1355
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001

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 0.52997(7) 0.25888(7) 0.84621(5) 0.0301(3) Uani 1 1 d . . .
O1 O 0.3937(3) 0.3217(3) 0.80799(18) 0.0323(8) Uani 1 1 d . . .
O2 O 0.5865(3) 0.3491(2) 0.83726(18) 0.0322(8) Uani 1 1 d . . .
N1 N 0.6113(3) 0.0999(3) 0.9083(2) 0.0293(10) Uani 1 1 d . . .
N2 N 0.4740(3) 0.2959(3) 0.9825(2) 0.0291(10) Uani 1 1 d . . .
N3 N 0.3515(4) 0.5576(4) 0.9291(3) 0.0302(10) Uani 1 1 d . . .
N4 N 0.3560(3) 0.6137(3) 0.7594(3) 0.0301(10) Uani 1 1 d . . .
N5 N 0.4871(4) 0.4156(4) 0.6627(3) 0.0286(10) Uani 1 1 d . . .
N6 N 0.6174(3) 0.1606(3) 0.7255(2) 0.0320(10) Uani 1 1 d . . .
C1 C 0.6942(4) -0.0133(4) 0.8792(3) 0.0312(12) Uani 1 1 d . . .
C2 C 0.7198(4) -0.0916(4) 0.9520(3) 0.0302(12) Uani 1 1 d . . .
C3 C 0.6527(4) -0.0278(4) 1.0261(3) 0.0303(12) Uani 1 1 d . . .
C4 C 0.5876(4) 0.0904(4) 0.9985(3) 0.0265(12) Uani 1 1 d . . .
C5 C 0.5094(4) 0.2030(4) 1.0396(3) 0.0289(12) Uani 1 1 d . . .
C6 C 0.4618(4) 0.2415(4) 1.1292(3) 0.0294(12) Uani 1 1 d . . .
C7 C 0.3976(4) 0.3609(4) 1.1256(3) 0.0287(12) Uani 1 1 d . . .
C8 C 0.4045(4) 0.3948(4) 1.0353(3) 0.0249(11) Uani 1 1 d . . .
C9 C 0.3507(4) 0.5109(4) 1.0091(3) 0.0305(12) Uani 1 1 d . . .
H9 H 0.3067 0.5670 1.0560 0.037 Uiso 1 1 d R . .
C10 C 0.2911(4) 0.6784(4) 0.9086(3) 0.0288(12) Uani 1 1 d . . .
C11 C 0.2316(4) 0.7655(4) 0.9737(3) 0.0311(12) Uani 1 1 d . . .
H11 H 0.2344 0.7449 1.0363 0.037 Uiso 1 1 d R . .
C12 C 0.1700(4) 0.8817(5) 0.9477(3) 0.0380(13) Uani 1 1 d . . .
H12 H 0.1288 0.9419 0.9924 0.046 Uiso 1 1 d R . .
C13 C 0.1672(4) 0.9118(4) 0.8577(4) 0.0417(14) Uani 1 1 d . . .
H13 H 0.1231 0.9924 0.8405 0.050 Uiso 1 1 d R . .
C14 C 0.2268(4) 0.8274(4) 0.7935(3) 0.0370(13) Uani 1 1 d . . .
H14 H 0.2270 0.8488 0.7314 0.044 Uiso 1 1 d R . .
C15 C 0.2901(4) 0.7080(5) 0.8176(3) 0.0323(13) Uani 1 1 d . . .
C16 C 0.3290(4) 0.6159(4) 0.6757(3) 0.0316(12) Uani 1 1 d . . .
H16 H 0.2667 0.6858 0.6495 0.038 Uiso 1 1 d R . .
C17 C 0.3949(4) 0.5110(4) 0.6231(3) 0.0312(13) Uani 1 1 d . . .
C18 C 0.3733(4) 0.4756(4) 0.5405(3) 0.0319(13) Uani 1 1 d . . .
C19 C 0.4527(4) 0.3546(4) 0.5315(3) 0.0318(12) Uani 1 1 d . . .
C20 C 0.5215(4) 0.3198(4) 0.6098(3) 0.0308(12) Uani 1 1 d . . .
C21 C 0.6099(4) 0.2028(4) 0.6390(3) 0.0311(12) Uani 1 1 d . . .
C22 C 0.6980(4) 0.1144(4) 0.5802(3) 0.0354(13) Uani 1 1 d . . .
C23 C 0.7556(5) 0.0158(4) 0.6302(3) 0.0382(14) Uani 1 1 d . . .
C24 C 0.7061(4) 0.0440(4) 0.7205(3) 0.0319(12) Uani 1 1 d . . .
C25 C 0.7399(4) -0.0349(4) 0.7915(3) 0.0336(13) Uani 1 1 d . . .
H25A H 0.8015 -0.1133 0.7775 0.040 Uiso 1 1 d R . .
C26 C 0.8109(4) -0.2184(4) 0.9503(3) 0.0404(14) Uani 1 1 d . . .
H26A H 0.8231 -0.2458 0.8891 0.048 Uiso 1 1 d R . .
H26B H 0.7805 -0.2621 0.9853 0.048 Uiso 1 1 d R . .
C27 C 0.9332(4) -0.2402(4) 0.9859(4) 0.0589(16) Uani 1 1 d . . .
H27A H 0.9909 -0.3221 0.9831 0.088 Uiso 1 1 d R . .
H27B H 0.9639 -0.1972 0.9503 0.088 Uiso 1 1 d R . .
H27C H 0.9209 -0.2136 1.0474 0.088 Uiso 1 1 d R . .
C28 C 0.6542(4) -0.0784(4) 1.1175(3) 0.0396(14) Uani 1 1 d . . .
H28A H 0.7073 -0.1613 1.1145 0.059 Uiso 1 1 d R . .
H28B H 0.6840 -0.0440 1.1602 0.059 Uiso 1 1 d R . .
H28C H 0.5736 -0.0634 1.1362 0.059 Uiso 1 1 d R . .
C29 C 0.4797(5) 0.1689(4) 1.2132(3) 0.0445(15) Uani 1 1 d . . .
H29A H 0.4370 0.2192 1.2636 0.067 Uiso 1 1 d R . .
H29B H 0.4485 0.1153 1.2041 0.067 Uiso 1 1 d R . .
H29C H 0.5650 0.1258 1.2252 0.067 Uiso 1 1 d R . .
C30 C 0.3308(4) 0.4415(4) 1.2047(3) 0.0399(14) Uani 1 1 d . . .
H30A H 0.3171 0.5190 1.1908 0.048 Uiso 1 1 d R . .
H30B H 0.3804 0.4150 1.2567 0.048 Uiso 1 1 d R . .
C31 C 0.2091(5) 0.4458(5) 1.2271(3) 0.0621(18) Uani 1 1 d . . .
H31A H 0.1684 0.4973 1.2773 0.093 Uiso 1 1 d R . .
H31B H 0.1593 0.4733 1.1753 0.093 Uiso 1 1 d R . .
H31C H 0.2231 0.3684 1.2417 0.093 Uiso 1 1 d R . .
C32 C 0.2763(4) 0.5520(4) 0.4764(3) 0.0390(14) Uani 1 1 d . . .
H32A H 0.3055 0.5297 0.4152 0.047 Uiso 1 1 d R . .
H32B H 0.2604 0.6312 0.4850 0.047 Uiso 1 1 d R . .
C33 C 0.1567(5) 0.5507(5) 0.4925(3) 0.0715(19) Uani 1 1 d . . .
H33A H 0.0974 0.6019 0.4511 0.107 Uiso 1 1 d R . .
H33B H 0.1719 0.4719 0.4827 0.107 Uiso 1 1 d R . .
H33C H 0.1263 0.5744 0.5532 0.107 Uiso 1 1 d R . .
C34 C 0.4495(4) 0.2820(4) 0.4556(3) 0.0446(14) Uani 1 1 d . . .
H34C H 0.5045 0.2010 0.4666 0.067 Uiso 1 1 d R . .
H34A H 0.4721 0.3064 0.4002 0.067 Uiso 1 1 d R . .
H34B H 0.3680 0.2939 0.4503 0.067 Uiso 1 1 d R . .
C35 C 0.7311(5) 0.1268(4) 0.4844(3) 0.0490(15) Uani 1 1 d . . .
H35C H 0.6933 0.2079 0.4678 0.073 Uiso 1 1 d R . .
H35A H 0.7056 0.0846 0.4456 0.073 Uiso 1 1 d R . .
H35B H 0.8181 0.0932 0.4780 0.073 Uiso 1 1 d R . .
C36 C 0.8542(5) -0.1039(4) 0.5994(3) 0.0468(15) Uani 1 1 d D . .
H36C H 0.8475 -0.1121 0.5359 0.056 Uiso 0.15 1 d PR . .
H36D H 0.8415 -0.1627 0.6300 0.056 Uiso 0.15 1 d PR . .
H36A H 0.9131 -0.1350 0.6457 0.056 Uiso 0.85 1 d PR . .
H36B H 0.8943 -0.0953 0.5457 0.056 Uiso 0.85 1 d PR . .
C37 C 0.8067(6) -0.1892(5) 0.5832(4) 0.067(2) Uani 0.85 1 d PD . .
H37C H 0.7626 -0.1927 0.6363 0.100 Uiso 0.85 1 d PR . .
H37A H 0.8727 -0.2658 0.5699 0.100 Uiso 0.85 1 d PR . .
H37B H 0.7533 -0.1640 0.5333 0.100 Uiso 0.85 1 d PR . .
C37A C 0.9799(16) -0.124(3) 0.617(2) 0.048(10) Uiso 0.15 1 d PD . .
H37D H 0.9776 -0.0493 0.6247 0.071 Uiso 0.15 1 d PR . .
H37E H 1.0088 -0.1686 0.6714 0.071 Uiso 0.15 1 d PR . .
H37F H 1.0336 -0.1650 0.5675 0.071 Uiso 0.15 1 d PR . .
Cl1A Cl 0.04245(14) 0.64423(14) 0.75094(11) 0.0815(6) Uani 1 1 d U . .
Cl2A Cl 0.10074(15) 0.45502(15) 0.87903(12) 0.0926(6) Uani 1 1 d U . .
C1A C 0.1286(5) 0.5017(5) 0.7775(4) 0.097(2) Uani 1 1 d U . .
H1AA H 0.2127 0.4831 0.7733 0.116 Uiso 1 1 d R . .
H1AB H 0.1156 0.4573 0.7319 0.116 Uiso 1 1 d R . .
Cl1B Cl 0.92769(13) 0.24154(14) 0.80472(10) 0.0724(5) Uani 1 1 d U . .
Cl2B Cl 0.97695(19) 0.1176(2) 0.63625(13) 0.1474(11) Uani 1 1 d U . .
C1B C 0.8733(6) 0.1945(6) 0.7207(4) 0.100(3) Uani 1 1 d U . .
H1BA H 0.8074 0.2614 0.6942 0.120 Uiso 1 1 d R . .
H1BB H 0.8413 0.1462 0.7463 0.120 Uiso 1 1 d R . .
Cl1C Cl 0.42960(19) 0.05363(16) 0.61542(11) 0.0934(6) Uani 1 1 d DU . .
Cl2C Cl 0.18566(19) 0.2089(2) 0.66956(13) 0.0855(7) Uani 0.81 1 d PDU . .
Cl3C Cl 0.1923(7) 0.2871(8) 0.6053(6) 0.119(4) Uani 0.19 1 d PDU . .
C1C C 0.3292(6) 0.1910(5) 0.6540(4) 0.078(2) Uani 1 1 d DU . .
H1CC H 0.3090 0.1824 0.7156 0.094 Uiso 0.19 1 d PR . .
H1CD H 0.3759 0.2320 0.6554 0.094 Uiso 0.19 1 d PR . .
H1CA H 0.3281 0.2479 0.6117 0.094 Uiso 0.81 1 d PR . .
H1CB H 0.3564 0.2041 0.7104 0.094 Uiso 0.81 1 d PR . .
H5N H 0.513(3) 0.413(3) 0.722(2) 0.006(10) Uiso 1 1 d . . .
H3N H 0.395(4) 0.508(4) 0.878(3) 0.067(18) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0349(6) 0.0287(6) 0.0251(5) 0.0002(4) 0.0017(4) -0.0140(5)
O1 0.033(2) 0.035(2) 0.0252(18) -0.0049(16) 0.0012(16) -0.0126(18)
O2 0.038(2) 0.036(2) 0.0296(18) 0.0025(16) 0.0016(16) -0.0238(19)
N1 0.033(3) 0.028(3) 0.026(2) 0.000(2) -0.001(2) -0.014(2)
N2 0.029(2) 0.031(3) 0.028(2) 0.001(2) 0.000(2) -0.015(2)
N3 0.038(3) 0.028(3) 0.023(3) -0.002(2) 0.002(2) -0.014(2)
N4 0.032(3) 0.027(3) 0.028(2) 0.001(2) 0.000(2) -0.012(2)
N5 0.037(3) 0.028(3) 0.019(2) 0.003(2) -0.003(2) -0.014(2)
N6 0.029(2) 0.034(3) 0.028(2) -0.001(2) 0.004(2) -0.011(2)
C1 0.032(3) 0.026(3) 0.031(3) 0.002(3) 0.001(3) -0.010(3)
C2 0.030(3) 0.028(3) 0.028(3) 0.004(3) 0.000(3) -0.010(3)
C3 0.033(3) 0.035(4) 0.028(3) 0.003(3) -0.006(3) -0.019(3)
C4 0.025(3) 0.031(3) 0.027(3) -0.001(3) 0.000(2) -0.017(3)
C5 0.031(3) 0.034(4) 0.027(3) 0.001(3) -0.001(3) -0.020(3)
C6 0.031(3) 0.032(3) 0.028(3) -0.001(3) 0.001(3) -0.017(3)
C7 0.032(3) 0.031(3) 0.028(3) -0.005(3) 0.006(2) -0.019(3)
C8 0.021(3) 0.017(3) 0.030(3) -0.001(3) 0.001(2) -0.003(3)
C9 0.021(3) 0.034(4) 0.033(3) -0.007(3) 0.005(2) -0.011(3)
C10 0.027(3) 0.024(3) 0.034(3) -0.001(3) -0.001(3) -0.011(3)
C11 0.028(3) 0.026(3) 0.036(3) 0.000(3) -0.002(3) -0.010(3)
C12 0.030(3) 0.035(4) 0.044(4) -0.010(3) -0.001(3) -0.011(3)
C13 0.041(3) 0.026(3) 0.050(4) 0.005(3) -0.006(3) -0.009(3)
C14 0.042(3) 0.032(4) 0.036(3) 0.000(3) 0.001(3) -0.017(3)
C15 0.027(3) 0.035(4) 0.037(3) -0.002(3) 0.002(3) -0.017(3)
C16 0.030(3) 0.026(3) 0.039(3) 0.007(3) 0.001(3) -0.014(3)
C17 0.030(3) 0.028(3) 0.034(3) 0.008(3) 0.003(3) -0.013(3)
C18 0.037(3) 0.040(4) 0.020(3) 0.001(3) 0.003(3) -0.020(3)
C19 0.040(3) 0.034(4) 0.023(3) 0.002(3) 0.004(3) -0.020(3)
C20 0.033(3) 0.031(4) 0.027(3) 0.001(3) 0.006(3) -0.015(3)
C21 0.038(3) 0.029(3) 0.027(3) -0.001(3) 0.000(3) -0.017(3)
C22 0.043(3) 0.027(3) 0.032(3) 0.000(3) 0.006(3) -0.014(3)
C23 0.048(4) 0.028(4) 0.033(3) -0.012(3) 0.014(3) -0.013(3)
C24 0.032(3) 0.025(3) 0.030(3) 0.002(3) 0.002(3) -0.007(3)
C25 0.036(3) 0.023(3) 0.036(3) -0.004(3) 0.004(3) -0.009(3)
C26 0.047(4) 0.036(4) 0.034(3) 0.002(3) -0.001(3) -0.017(3)
C27 0.041(4) 0.050(4) 0.073(4) 0.006(3) -0.019(3) -0.011(3)
C28 0.047(3) 0.035(3) 0.037(3) 0.008(3) -0.003(3) -0.020(3)
C29 0.058(4) 0.047(4) 0.033(3) -0.001(3) 0.002(3) -0.029(3)
C30 0.050(4) 0.043(4) 0.030(3) -0.006(3) 0.006(3) -0.025(3)
C31 0.061(4) 0.074(5) 0.057(4) -0.022(3) 0.026(3) -0.038(4)
C32 0.046(4) 0.037(4) 0.028(3) -0.002(3) -0.004(3) -0.016(3)
C33 0.046(4) 0.091(5) 0.056(4) -0.001(4) -0.005(3) -0.015(4)
C34 0.058(4) 0.040(4) 0.034(3) -0.006(3) 0.004(3) -0.022(3)
C35 0.065(4) 0.042(4) 0.032(3) -0.005(3) 0.015(3) -0.019(3)
C36 0.057(4) 0.043(4) 0.031(3) 0.000(3) 0.008(3) -0.017(3)
C37 0.085(6) 0.039(5) 0.059(5) -0.011(4) -0.006(4) -0.015(5)
Cl1A 0.0555(11) 0.0635(12) 0.0930(13) 0.0257(10) 0.0206(10) -0.0041(10)
Cl2A 0.0697(12) 0.0752(14) 0.1015(14) 0.0397(11) 0.0140(11) -0.0107(11)
C1A 0.056(4) 0.075(5) 0.111(6) 0.046(4) 0.015(4) 0.006(4)
Cl1B 0.0559(10) 0.0752(13) 0.0692(11) -0.0205(9) 0.0020(9) -0.0174(10)
Cl2B 0.1217(17) 0.268(3) 0.0905(15) -0.0905(18) 0.0502(14) -0.125(2)
C1B 0.075(5) 0.133(7) 0.091(5) -0.052(5) 0.018(4) -0.051(5)
Cl1C 0.1469(18) 0.0788(15) 0.0762(12) 0.0141(11) -0.0204(12) -0.0704(15)
Cl2C 0.0815(16) 0.131(2) 0.0669(14) 0.0017(14) 0.0038(12) -0.0694(16)
Cl3C 0.140(10) 0.149(10) 0.081(7) 0.045(7) -0.016(7) -0.079(8)
C1C 0.097(5) 0.080(5) 0.065(4) 0.007(4) -0.022(4) -0.047(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 1.618(3) . ?
V1 O2 1.635(3) . ?
V1 N1 2.044(4) . ?
V1 N2 2.101(3) . ?
V1 N6 2.149(4) . ?
N1 C4 1.379(5) . ?
N1 C1 1.399(5) . ?
N2 C5 1.367(5) . ?
N2 C8 1.390(5) . ?
N3 C9 1.330(5) . ?
N3 C10 1.416(5) . ?
N3 H3N 0.96(5) . ?
N4 C16 1.293(5) . ?
N4 C15 1.393(5) . ?
N5 C20 1.357(5) . ?
N5 C17 1.371(5) . ?
N5 H5N 0.94(3) . ?
N6 C21 1.380(5) . ?
N6 C24 1.388(5) . ?
C1 C25 1.380(5) . ?
C1 C2 1.413(6) . ?
C2 C3 1.376(6) . ?
C2 C26 1.492(6) . ?
C3 C4 1.418(6) . ?
C3 C28 1.498(6) . ?
C4 C5 1.444(6) . ?
C5 C6 1.432(5) . ?
C6 C7 1.367(6) . ?
C6 C29 1.514(6) . ?
C7 C8 1.420(6) . ?
C7 C30 1.516(5) . ?
C8 C9 1.385(6) . ?
C9 H9 0.9600 . ?
C10 C11 1.394(6) . ?
C10 C15 1.399(6) . ?
C11 C12 1.387(6) . ?
C11 H11 0.9600 . ?
C12 C13 1.384(6) . ?
C12 H12 0.9598 . ?
C13 C14 1.364(6) . ?
C13 H13 0.9600 . ?
C14 C15 1.415(6) . ?
C14 H14 0.9600 . ?
C16 C17 1.434(6) . ?
C16 H16 0.9600 . ?
C17 C18 1.393(6) . ?
C18 C19 1.409(6) . ?
C18 C32 1.506(6) . ?
C19 C20 1.407(6) . ?
C19 C34 1.490(6) . ?
C20 C21 1.462(6) . ?
C21 C22 1.429(6) . ?
C22 C23 1.359(6) . ?
C22 C35 1.496(5) . ?
C23 C24 1.432(6) . ?
C23 C36 1.515(6) . ?
C24 C25 1.391(6) . ?
C25 H25A 0.9601 . ?
C26 C27 1.527(6) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C27 H27A 0.9599 . ?
C27 H27B 0.9601 . ?
C27 H27C 0.9601 . ?
C28 H28A 0.9599 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9601 . ?
C29 H29A 0.9602 . ?
C29 H29B 0.9599 . ?
C29 H29C 0.9600 . ?
C30 C31 1.519(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C31 H31A 0.9601 . ?
C31 H31B 0.9598 . ?
C31 H31C 0.9599 . ?
C32 C33 1.514(6) . ?
C32 H32A 0.9601 . ?
C32 H32B 0.9601 . ?
C33 H33A 0.9599 . ?
C33 H33B 0.9602 . ?
C33 H33C 0.9600 . ?
C34 H34C 0.9601 . ?
C34 H34A 0.9599 . ?
C34 H34B 0.9600 . ?
C35 H35C 0.9601 . ?
C35 H35A 0.9601 . ?
C35 H35B 0.9600 . ?
C36 C37A 1.498(12) . ?
C36 C37 1.511(7) . ?
C36 H36C 0.9600 . ?
C36 H36D 0.9599 . ?
C36 H36A 0.9602 . ?
C36 H36B 0.9599 . ?
C37 H37C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37A H37D 0.9601 . ?
C37A H37E 0.9599 . ?
C37A H37F 0.9600 . ?
Cl1A C1A 1.691(6) . ?
Cl2A C1A 1.705(6) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9599 . ?
Cl1B C1B 1.690(6) . ?
Cl2B C1B 1.712(5) . ?
C1B H1BA 0.9599 . ?
C1B H1BB 0.9600 . ?
Cl1C C1C 1.712(6) . ?
Cl2C C1C 1.703(6) . ?
Cl3C C1C 1.741(8) . ?
C1C H1CC 0.9600 . ?
C1C H1CD 0.9600 . ?
C1C H1CA 0.9600 . ?
C1C H1CB 0.9600 . ?

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
O1 V1 O2 108.96(15) . . ?
O1 V1 N1 125.52(14) . . ?
O2 V1 N1 125.20(15) . . ?
O1 V1 N2 95.30(14) . . ?
O2 V1 N2 95.89(14) . . ?
N1 V1 N2 75.31(15) . . ?
O1 V1 N6 95.83(14) . . ?
O2 V1 N6 96.13(14) . . ?
N1 V1 N6 84.70(15) . . ?
N2 V1 N6 160.00(16) . . ?
C4 N1 C1 105.8(4) . . ?
C4 N1 V1 120.4(3) . . ?
C1 N1 V1 133.8(3) . . ?
C5 N2 C8 105.8(4) . . ?
C5 N2 V1 117.3(3) . . ?
C8 N2 V1 137.0(3) . . ?
C9 N3 C10 126.0(4) . . ?
C9 N3 H3N 120(3) . . ?
C10 N3 H3N 114(3) . . ?
C16 N4 C15 122.2(4) . . ?
C20 N5 C17 109.5(4) . . ?
C20 N5 H5N 124(2) . . ?
C17 N5 H5N 126(2) . . ?
C21 N6 C24 105.4(4) . . ?
C21 N6 V1 127.5(3) . . ?
C24 N6 V1 126.6(3) . . ?
C25 C1 N1 121.0(4) . . ?
C25 C1 C2 129.6(5) . . ?
N1 C1 C2 109.4(4) . . ?
C3 C2 C1 107.6(4) . . ?
C3 C2 C26 126.3(4) . . ?
C1 C2 C26 125.9(4) . . ?
C2 C3 C4 106.9(4) . . ?
C2 C3 C28 124.5(5) . . ?
C4 C3 C28 128.6(4) . . ?
N1 C4 C3 110.3(4) . . ?
N1 C4 C5 112.0(4) . . ?
C3 C4 C5 137.7(4) . . ?
N2 C5 C6 110.8(4) . . ?
N2 C5 C4 114.8(4) . . ?
C6 C5 C4 134.3(5) . . ?
C7 C6 C5 106.0(4) . . ?
C7 C6 C29 125.4(4) . . ?
C5 C6 C29 128.6(4) . . ?
C6 C7 C8 107.9(4) . . ?
C6 C7 C30 125.5(4) . . ?
C8 C7 C30 126.6(4) . . ?
C9 C8 N2 128.0(4) . . ?
C9 C8 C7 122.5(4) . . ?
N2 C8 C7 109.5(4) . . ?
N3 C9 C8 130.2(4) . . ?
N3 C9 H9 114.3 . . ?
C8 C9 H9 115.5 . . ?
C11 C10 C15 120.2(5) . . ?
C11 C10 N3 123.1(4) . . ?
C15 C10 N3 116.7(4) . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 120.6(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 120.3(5) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.5(5) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 119.4 . . ?
N4 C15 C10 114.9(5) . . ?
N4 C15 C14 126.4(4) . . ?
C10 C15 C14 118.7(5) . . ?
N4 C16 C17 118.1(5) . . ?
N4 C16 H16 121.1 . . ?
C17 C16 H16 120.8 . . ?
N5 C17 C18 108.1(4) . . ?
N5 C17 C16 118.3(4) . . ?
C18 C17 C16 132.6(5) . . ?
C17 C18 C19 107.4(4) . . ?
C17 C18 C32 125.7(5) . . ?
C19 C18 C32 126.8(4) . . ?
C20 C19 C18 106.7(4) . . ?
C20 C19 C34 129.5(5) . . ?
C18 C19 C34 123.6(5) . . ?
N5 C20 C19 108.3(4) . . ?
N5 C20 C21 121.9(4) . . ?
C19 C20 C21 129.7(5) . . ?
N6 C21 C22 110.5(4) . . ?
N6 C21 C20 125.2(4) . . ?
C22 C21 C20 124.2(4) . . ?
C23 C22 C21 106.8(4) . . ?
C23 C22 C35 125.0(4) . . ?
C21 C22 C35 128.0(5) . . ?
C22 C23 C24 107.5(4) . . ?
C22 C23 C36 128.0(4) . . ?
C24 C23 C36 124.5(5) . . ?
N6 C24 C25 125.4(4) . . ?
N6 C24 C23 109.7(4) . . ?
C25 C24 C23 124.8(5) . . ?
C1 C25 C24 127.4(5) . . ?
C1 C25 H25A 116.5 . . ?
C24 C25 H25A 116.1 . . ?
C2 C26 C27 111.9(4) . . ?
C2 C26 H26A 108.4 . . ?
C27 C26 H26A 108.6 . . ?
C2 C26 H26B 110.1 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.2 . . ?
C26 C27 H27A 110.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 108.4 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C3 C28 H28A 108.5 . . ?
C3 C28 H28B 109.4 . . ?
H28A C28 H28B 109.5 . . ?
C3 C28 H28C 110.4 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C6 C29 H29A 109.6 . . ?
C6 C29 H29B 109.2 . . ?
H29A C29 H29B 109.5 . . ?
C6 C29 H29C 109.6 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C7 C30 C31 112.2(4) . . ?
C7 C30 H30A 109.3 . . ?
C31 C30 H30A 109.0 . . ?
C7 C30 H30B 109.3 . . ?
C31 C30 H30B 108.9 . . ?
H30A C30 H30B 108.1 . . ?
C30 C31 H31A 110.8 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 108.8 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C18 C32 C33 113.4(4) . . ?
C18 C32 H32A 109.9 . . ?
C33 C32 H32A 110.4 . . ?
C18 C32 H32B 108.0 . . ?
C33 C32 H32B 107.0 . . ?
H32A C32 H32B 107.9 . . ?
C32 C33 H33A 110.4 . . ?
C32 C33 H33B 107.3 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 110.7 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C19 C34 H34C 109.6 . . ?
C19 C34 H34A 109.4 . . ?
H34C C34 H34A 110.3 . . ?
C19 C34 H34B 109.4 . . ?
H34C C34 H34B 110.3 . . ?
H34A C34 H34B 107.8 . . ?
C22 C35 H35C 110.4 . . ?
C22 C35 H35A 109.5 . . ?
H35C C35 H35A 110.0 . . ?
C22 C35 H35B 109.0 . . ?
H35C C35 H35B 110.0 . . ?
H35A C35 H35B 108.0 . . ?
C37A C36 C37 131.1(13) . . ?
C37A C36 C23 112.8(13) . . ?
C37 C36 C23 113.2(4) . . ?
C37A C36 H36C 109.3 . . ?
C23 C36 H36C 108.9 . . ?
C37A C36 H36D 108.8 . . ?
C23 C36 H36D 109.0 . . ?
H36C C36 H36D 107.9 . . ?
C37 C36 H36A 108.2 . . ?
C23 C36 H36A 107.8 . . ?
C37 C36 H36B 110.5 . . ?
C23 C36 H36B 109.0 . . ?
H36A C36 H36B 108.0 . . ?
C36 C37 H37C 109.1 . . ?
C36 C37 H37A 110.7 . . ?
H36C C37 H37A 102.3 . . ?
H36D C37 H37A 101.3 . . ?
H37C C37 H37A 109.2 . . ?
C36 C37 H37B 110.1 . . ?
H37C C37 H37B 109.2 . . ?
H37A C37 H37B 108.5 . . ?
C36 C37A H37D 109.1 . . ?
C36 C37A H37E 110.0 . . ?
H37D C37A H37E 109.5 . . ?
C36 C37A H37F 109.3 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
Cl1A C1A Cl2A 118.1(3) . . ?
Cl1A C1A H1AA 108.5 . . ?
Cl2A C1A H1AA 108.7 . . ?
Cl1A C1A H1AB 106.4 . . ?
Cl2A C1A H1AB 106.9 . . ?
H1AA C1A H1AB 107.7 . . ?
Cl1B C1B Cl2B 115.3(4) . . ?
Cl1B C1B H1BA 108.3 . . ?
Cl2B C1B H1BA 107.9 . . ?
Cl1B C1B H1BB 108.6 . . ?
Cl2B C1B H1BB 108.6 . . ?
H1BA C1B H1BB 108.0 . . ?
Cl2C C1C Cl1C 112.0(3) . . ?
Cl1C C1C H1CC 106.4 . . ?
Cl3C C1C H1CC 106.0 . . ?
Cl1C C1C H1CD 105.0 . . ?
Cl3C C1C H1CD 105.7 . . ?
H1CC C1C H1CD 106.4 . . ?
Cl2C C1C H1CA 109.4 . . ?
Cl1C C1C H1CA 109.3 . . ?
Cl2C C1C H1CB 108.9 . . ?
Cl1C C1C H1CB 108.9 . . ?
H1CA C1C H1CB 108.2 . . ?

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
O1 V1 N1 C4 -81.6(3) . . . . ?
O2 V1 N1 C4 91.2(3) . . . . ?
N2 V1 N1 C4 4.4(3) . . . . ?
N6 V1 N1 C4 -175.0(3) . . . . ?
O1 V1 N1 C1 98.8(4) . . . . ?
O2 V1 N1 C1 -88.4(4) . . . . ?
N2 V1 N1 C1 -175.2(4) . . . . ?
N6 V1 N1 C1 5.4(4) . . . . ?
O1 V1 N2 C5 121.3(3) . . . . ?
O2 V1 N2 C5 -129.0(3) . . . . ?
N1 V1 N2 C5 -4.1(3) . . . . ?
N6 V1 N2 C5 -2.3(6) . . . . ?
O1 V1 N2 C8 -57.3(4) . . . . ?
O2 V1 N2 C8 52.5(4) . . . . ?
N1 V1 N2 C8 177.4(4) . . . . ?
N6 V1 N2 C8 179.2(4) . . . . ?
O1 V1 N6 C21 53.3(4) . . . . ?
O2 V1 N6 C21 -56.6(4) . . . . ?
N1 V1 N6 C21 178.5(4) . . . . ?
N2 V1 N6 C21 176.8(4) . . . . ?
O1 V1 N6 C24 -136.1(3) . . . . ?
O2 V1 N6 C24 114.1(4) . . . . ?
N1 V1 N6 C24 -10.8(3) . . . . ?
N2 V1 N6 C24 -12.6(6) . . . . ?
C4 N1 C1 C25 -178.5(4) . . . . ?
V1 N1 C1 C25 1.2(6) . . . . ?
C4 N1 C1 C2 0.4(5) . . . . ?
V1 N1 C1 C2 -179.9(3) . . . . ?
C25 C1 C2 C3 179.2(5) . . . . ?
N1 C1 C2 C3 0.4(5) . . . . ?
C25 C1 C2 C26 3.8(8) . . . . ?
N1 C1 C2 C26 -175.0(4) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
C26 C2 C3 C4 174.3(4) . . . . ?
C1 C2 C3 C28 -179.8(4) . . . . ?
C26 C2 C3 C28 -4.5(7) . . . . ?
C1 N1 C4 C3 -1.1(5) . . . . ?
V1 N1 C4 C3 179.2(3) . . . . ?
C1 N1 C4 C5 175.8(3) . . . . ?
V1 N1 C4 C5 -3.9(5) . . . . ?
C2 C3 C4 N1 1.4(5) . . . . ?
C28 C3 C4 N1 -179.9(4) . . . . ?
C2 C3 C4 C5 -174.3(5) . . . . ?
C28 C3 C4 C5 4.4(9) . . . . ?
C8 N2 C5 C6 0.5(5) . . . . ?
V1 N2 C5 C6 -178.4(3) . . . . ?
C8 N2 C5 C4 -177.7(3) . . . . ?
V1 N2 C5 C4 3.4(5) . . . . ?
N1 C4 C5 N2 0.2(5) . . . . ?
C3 C4 C5 N2 175.8(5) . . . . ?
N1 C4 C5 C6 -177.5(5) . . . . ?
C3 C4 C5 C6 -1.8(9) . . . . ?
N2 C5 C6 C7 -0.7(5) . . . . ?
C4 C5 C6 C7 177.0(5) . . . . ?
N2 C5 C6 C29 -179.0(4) . . . . ?
C4 C5 C6 C29 -1.3(8) . . . . ?
C5 C6 C7 C8 0.6(5) . . . . ?
C29 C6 C7 C8 178.9(4) . . . . ?
C5 C6 C7 C30 -179.6(4) . . . . ?
C29 C6 C7 C30 -1.3(7) . . . . ?
C5 N2 C8 C9 178.1(4) . . . . ?
V1 N2 C8 C9 -3.3(7) . . . . ?
C5 N2 C8 C7 -0.2(5) . . . . ?
V1 N2 C8 C7 178.5(3) . . . . ?
C6 C7 C8 C9 -178.6(4) . . . . ?
C30 C7 C8 C9 1.6(7) . . . . ?
C6 C7 C8 N2 -0.3(5) . . . . ?
C30 C7 C8 N2 179.9(4) . . . . ?
C10 N3 C9 C8 178.7(4) . . . . ?
N2 C8 C9 N3 -0.4(8) . . . . ?
C7 C8 C9 N3 177.6(4) . . . . ?
C9 N3 C10 C11 6.4(7) . . . . ?
C9 N3 C10 C15 -171.7(4) . . . . ?
C15 C10 C11 C12 0.9(7) . . . . ?
N3 C10 C11 C12 -177.2(4) . . . . ?
C10 C11 C12 C13 0.0(7) . . . . ?
C11 C12 C13 C14 -1.1(7) . . . . ?
C12 C13 C14 C15 1.3(7) . . . . ?
C16 N4 C15 C10 152.7(4) . . . . ?
C16 N4 C15 C14 -28.8(7) . . . . ?
C11 C10 C15 N4 178.1(4) . . . . ?
N3 C10 C15 N4 -3.8(6) . . . . ?
C11 C10 C15 C14 -0.6(7) . . . . ?
N3 C10 C15 C14 177.5(4) . . . . ?
C13 C14 C15 N4 -179.0(4) . . . . ?
C13 C14 C15 C10 -0.4(7) . . . . ?
C15 N4 C16 C17 -174.5(4) . . . . ?
C20 N5 C17 C18 -2.4(5) . . . . ?
C20 N5 C17 C16 167.8(4) . . . . ?
N4 C16 C17 N5 -3.2(6) . . . . ?
N4 C16 C17 C18 164.1(4) . . . . ?
N5 C17 C18 C19 1.6(5) . . . . ?
C16 C17 C18 C19 -166.7(4) . . . . ?
N5 C17 C18 C32 177.7(4) . . . . ?
C16 C17 C18 C32 9.4(8) . . . . ?
C17 C18 C19 C20 -0.2(5) . . . . ?
C32 C18 C19 C20 -176.3(4) . . . . ?
C17 C18 C19 C34 174.3(4) . . . . ?
C32 C18 C19 C34 -1.8(7) . . . . ?
C17 N5 C20 C19 2.3(5) . . . . ?
C17 N5 C20 C21 -173.8(4) . . . . ?
C18 C19 C20 N5 -1.2(5) . . . . ?
C34 C19 C20 N5 -175.3(4) . . . . ?
C18 C19 C20 C21 174.4(4) . . . . ?
C34 C19 C20 C21 0.4(8) . . . . ?
C24 N6 C21 C22 -2.9(5) . . . . ?
V1 N6 C21 C22 169.4(3) . . . . ?
C24 N6 C21 C20 174.9(4) . . . . ?
V1 N6 C21 C20 -12.8(6) . . . . ?
N5 C20 C21 N6 38.3(7) . . . . ?
C19 C20 C21 N6 -136.8(5) . . . . ?
N5 C20 C21 C22 -144.2(4) . . . . ?
C19 C20 C21 C22 40.7(7) . . . . ?
N6 C21 C22 C23 3.0(5) . . . . ?
C20 C21 C22 C23 -174.8(4) . . . . ?
N6 C21 C22 C35 -171.9(4) . . . . ?
C20 C21 C22 C35 10.2(7) . . . . ?
C21 C22 C23 C24 -1.8(5) . . . . ?
C35 C22 C23 C24 173.3(4) . . . . ?
C21 C22 C23 C36 178.1(4) . . . . ?
C35 C22 C23 C36 -6.8(8) . . . . ?
C21 N6 C24 C25 -176.7(4) . . . . ?
V1 N6 C24 C25 11.0(6) . . . . ?
C21 N6 C24 C23 1.7(5) . . . . ?
V1 N6 C24 C23 -170.6(3) . . . . ?
C22 C23 C24 N6 0.1(5) . . . . ?
C36 C23 C24 N6 -179.8(4) . . . . ?
C22 C23 C24 C25 178.5(5) . . . . ?
C36 C23 C24 C25 -1.4(8) . . . . ?
N1 C1 C25 C24 -5.7(7) . . . . ?
C2 C1 C25 C24 175.6(5) . . . . ?
N6 C24 C25 C1 -0.7(8) . . . . ?
C23 C24 C25 C1 -178.9(5) . . . . ?
C3 C2 C26 C27 -79.4(6) . . . . ?
C1 C2 C26 C27 95.1(6) . . . . ?
C6 C7 C30 C31 -78.5(6) . . . . ?
C8 C7 C30 C31 101.3(5) . . . . ?
C17 C18 C32 C33 -90.6(6) . . . . ?
C19 C18 C32 C33 84.8(6) . . . . ?
C22 C23 C36 C37A 96.4(15) . . . . ?
C24 C23 C36 C37A -83.7(14) . . . . ?
C22 C23 C36 C37 -100.7(6) . . . . ?
C24 C23 C36 C37 79.2(6) . . . . ?

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
N3 H3N O2 0.96(5) 2.37(5) 3.170(5) 141(4) .
N5 H5N O2 0.94(3) 1.95(4) 2.854(5) 160(3) .
C1A H1AA O1 0.96 2.30 3.056(7) 134.6 .
C1C H1CB O1 0.96 2.33 3.203(6) 151.3 .

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.081