# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
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#  except for the purpose of generating routine backup copies 
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data_zj90n
_database_code_depnum_ccdc_archive 'CCDC 855049'
#TrackingRef '- zj90n.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H70 N2 O8 V2'
_chemical_formula_sum            'C41 H70 N2 O8 V2'
_chemical_formula_weight         820.87

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'



_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.977(6)
_cell_length_b                   15.717(4)
_cell_length_c                   23.165(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.54(5)
_cell_angle_gamma                90.00
_cell_volume                     8862(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3912
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3520
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_process_details   
;
CrysAlis CCD. Version 1.171.33 (Oxford Diffraction Ltd., 2009)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
Comput. Phys. Commun. (1998). 111, 243.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Kuma KM-4 CCD kappa-axis diffractometer'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48380
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         25.06
_reflns_number_total             7834
_reflns_number_gt                4859
_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       
;
CrysAlis CCD. Version 1.171.33 (Oxford Diffraction, 2009)
;
_computing_cell_refinement       
;
CrysAlis RED. Version 1.171.33 Oxford Diffraction, 2009)
;
_computing_data_reduction        
;
CrysAlis RED. Version 1.171.33 (Oxford Diffraction, 2009)
;
_computing_structure_solution    'SHELXTL. Version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL. Version 6.14 (Bruker, 2003)'
_computing_molecular_graphics    
' DIAMOND. Version 3.1f. (Brandenburg, K. 2007)'
_computing_publication_material  
;
SHELXTL. Version 6.14 (Bruker, 2003)
;




_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.
;

_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^)+(0.0599P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7834
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.81079(2) 0.25749(3) 0.78242(2) 0.01896(14) Uani 1 1 d . D .
V2 V 0.68242(2) 0.25686(3) 0.74944(3) 0.02097(14) Uani 1 1 d . C .
O1 O 0.86773(8) 0.27389(12) 0.86217(10) 0.0220(5) Uani 1 1 d . . .
O2 O 0.65019(8) 0.27468(13) 0.80467(10) 0.0248(5) Uani 1 1 d . . .
O3 O 0.82149(9) 0.15854(13) 0.77708(10) 0.0252(5) Uani 1 1 d . . .
O4 O 0.67041(9) 0.15727(13) 0.73978(11) 0.0289(5) Uani 1 1 d . . .
O5 O 0.73595(8) 0.26765(12) 0.71115(9) 0.0202(5) Uani 1 1 d . . .
O6 O 0.75788(8) 0.25002(13) 0.82219(9) 0.0203(5) Uani 1 1 d . . .
O7 O 0.62840(9) 0.29461(13) 0.67588(10) 0.0268(5) Uani 1 1 d . . .
O8 O 0.84024(9) 0.29878(13) 0.73134(10) 0.0241(5) Uani 1 1 d . . .
N1 N 0.79417(10) 0.41089(15) 0.78940(11) 0.0161(5) Uani 1 1 d . . .
N2 N 0.70157(10) 0.41025(15) 0.76277(11) 0.0161(5) Uani 1 1 d . . .
C1 C 0.75494(12) 0.43180(18) 0.81571(14) 0.0175(7) Uani 1 1 d . C .
H1A H 0.7568 0.4929 0.8268 0.021 Uiso 1 1 calc R . .
H1B H 0.7619 0.3973 0.8542 0.021 Uiso 1 1 calc R . .
C2 C 0.76777(12) 0.45013(19) 0.72425(13) 0.0194(7) Uani 1 1 d . C .
H2A H 0.7768 0.4175 0.6935 0.023 Uiso 1 1 calc R . .
H2B H 0.7802 0.5096 0.7253 0.023 Uiso 1 1 calc R . .
C3 C 0.70658(13) 0.44671(18) 0.70596(14) 0.0193(7) Uani 1 1 d . C .
H3A H 0.6903 0.5044 0.6962 0.023 Uiso 1 1 calc R . .
H3B H 0.6876 0.4101 0.6679 0.023 Uiso 1 1 calc R . .
C4 C 0.84870(12) 0.45003(18) 0.82614(14) 0.0187(7) Uani 1 1 d . D .
H4A H 0.8446 0.5127 0.8251 0.022 Uiso 1 1 calc R . .
H4B H 0.8730 0.4355 0.8055 0.022 Uiso 1 1 calc R . .
C5 C 0.87534(12) 0.42078(19) 0.89485(14) 0.0183(7) Uani 1 1 d . . .
C6 C 0.88368(12) 0.33359(19) 0.90845(15) 0.0207(7) Uani 1 1 d . D .
C7 C 0.91105(13) 0.3077(2) 0.97227(16) 0.0253(8) Uani 1 1 d . . .
H7A H 0.9173 0.2489 0.9822 0.030 Uiso 1 1 calc R D .
C8 C 0.92913(13) 0.3675(2) 1.02133(15) 0.0272(8) Uani 1 1 d . D .
H8A H 0.9482 0.3487 1.0643 0.033 Uiso 1 1 calc R . .
C9 C 0.92000(13) 0.4542(2) 1.00905(15) 0.0242(7) Uani 1 1 d . . .
C10 C 0.89331(12) 0.4789(2) 0.94460(15) 0.0219(7) Uani 1 1 d . D .
H10A H 0.8873 0.5378 0.9347 0.026 Uiso 1 1 calc R . .
C11 C 0.93699(14) 0.5223(2) 1.06169(16) 0.0283(8) Uani 1 1 d . D .
C12 C 0.96825(15) 0.5947(2) 1.04705(17) 0.0390(9) Uani 1 1 d . . .
H12A H 1.0012 0.5716 1.0449 0.058 Uiso 1 1 calc R D .
H12B H 0.9790 0.6376 1.0810 0.058 Uiso 1 1 calc R . .
H12C H 0.9445 0.6209 1.0060 0.058 Uiso 1 1 calc R . .
C13 C 0.97623(19) 0.4880(3) 1.12722(18) 0.0548(12) Uani 1 1 d . . .
H13A H 1.0094 0.4658 1.1252 0.082 Uiso 1 1 calc R D .
H13B H 0.9582 0.4422 1.1397 0.082 Uiso 1 1 calc R . .
H13C H 0.9863 0.5339 1.1589 0.082 Uiso 1 1 calc R . .
C14 C 0.88532(14) 0.5666(2) 1.06221(17) 0.0325(8) Uani 1 1 d . . .
H14A H 0.8992 0.6071 1.0985 0.039 Uiso 1 1 calc R D .
H14B H 0.8691 0.6015 1.0228 0.039 Uiso 1 1 calc R . .
C15 C 0.83744(16) 0.5183(3) 1.06646(18) 0.0405(10) Uani 1 1 d . A .
C16 C 0.8542(2) 0.4589(3) 1.1227(2) 0.0753(16) Uani 1 1 d . A 1
H16A H 0.8730 0.4094 1.1158 0.113 Uiso 1 1 calc R A 1
H16B H 0.8214 0.4402 1.1273 0.113 Uiso 1 1 calc R A 1
H16C H 0.8790 0.4886 1.1617 0.113 Uiso 1 1 calc R A 1
C17 C 0.80119(17) 0.4702(3) 1.0045(2) 0.0526(12) Uani 1 1 d . A 1
H17A H 0.8213 0.4209 0.9997 0.079 Uiso 1 1 calc R A 1
H17B H 0.7917 0.5082 0.9677 0.079 Uiso 1 1 calc R A 1
H17C H 0.7675 0.4510 1.0067 0.079 Uiso 1 1 calc R A 1
C18 C 0.80115(18) 0.5886(3) 1.0754(2) 0.0669(15) Uani 1 1 d . A 1
H18A H 0.8214 0.6166 1.1168 0.100 Uiso 1 1 calc R A 1
H18B H 0.7675 0.5630 1.0740 0.100 Uiso 1 1 calc R A 1
H18C H 0.7916 0.6306 1.0410 0.100 Uiso 1 1 calc R A 1
C19 C 0.65517(13) 0.45170(19) 0.76917(14) 0.0202(7) Uani 1 1 d . C .
H19A H 0.6211 0.4396 0.7302 0.024 Uiso 1 1 calc R . .
H19B H 0.6610 0.5140 0.7713 0.024 Uiso 1 1 calc R . .
C20 C 0.64675(12) 0.42431(19) 0.82721(14) 0.0198(7) Uani 1 1 d . . .
C21 C 0.64261(12) 0.3385(2) 0.83966(15) 0.0226(7) Uani 1 1 d . C .
C22 C 0.62893(13) 0.3166(2) 0.88923(16) 0.0277(8) Uani 1 1 d . . .
H22A H 0.6264 0.2584 0.8986 0.033 Uiso 1 1 calc R C .
C23 C 0.61913(13) 0.3787(2) 0.92469(16) 0.0291(8) Uani 1 1 d . C .
H23A H 0.6090 0.3621 0.9576 0.035 Uiso 1 1 calc R . .
C24 C 0.62353(13) 0.4655(2) 0.91424(15) 0.0233(7) Uani 1 1 d . . .
C25 C 0.63813(13) 0.4855(2) 0.86506(15) 0.0225(7) Uani 1 1 d . C .
H25A H 0.6424 0.5437 0.8571 0.027 Uiso 1 1 calc R . .
C26 C 0.61349(13) 0.5324(2) 0.95620(15) 0.0251(8) Uani 1 1 d . C .
C27 C 0.64557(14) 0.5063(2) 1.02673(16) 0.0363(9) Uani 1 1 d . . .
H27A H 0.6839 0.4949 1.0357 0.054 Uiso 1 1 calc R C .
H27B H 0.6291 0.4549 1.0350 0.054 Uiso 1 1 calc R . .
H27C H 0.6441 0.5525 1.0544 0.054 Uiso 1 1 calc R . .
C28 C 0.63505(16) 0.6199(2) 0.94925(18) 0.0392(9) Uani 1 1 d . . .
H28A H 0.6750 0.6172 0.9642 0.059 Uiso 1 1 calc R C .
H28B H 0.6262 0.6615 0.9749 0.059 Uiso 1 1 calc R . .
H28C H 0.6178 0.6372 0.9042 0.059 Uiso 1 1 calc R . .
C29 C 0.55197(13) 0.5354(2) 0.94452(15) 0.0271(8) Uani 1 1 d . . .
H29A H 0.5423 0.4766 0.9510 0.033 Uiso 1 1 calc R C .
H29B H 0.5511 0.5696 0.9800 0.033 Uiso 1 1 calc R . .
C30 C 0.50440(16) 0.5673(3) 0.88380(19) 0.0511(12) Uani 1 1 d . B .
C31 C 0.5037(3) 0.6738(4) 0.8901(3) 0.044(2) Uani 0.613(9) 1 d P B 3
H31A H 0.5061 0.6891 0.9322 0.066 Uiso 0.613(9) 1 calc PR B 3
H31B H 0.4695 0.6963 0.8566 0.066 Uiso 0.613(9) 1 calc PR B 3
H31C H 0.5351 0.6979 0.8851 0.066 Uiso 0.613(9) 1 calc PR B 3
C32 C 0.45196(16) 0.5554(3) 0.89220(19) 0.0507(11) Uani 1 1 d . B 3
H32A H 0.4550 0.5864 0.9303 0.076 Uiso 1 1 calc R B 3
H32B H 0.4465 0.4947 0.8973 0.076 Uiso 1 1 calc R B 3
H32C H 0.4207 0.5773 0.8544 0.076 Uiso 1 1 calc R B 3
C33 C 0.4986(3) 0.5449(7) 0.8242(3) 0.038(3) Uani 0.580(14) 1 d P B 3
H33A H 0.5293 0.5679 0.8173 0.057 Uiso 0.580(14) 1 calc PR B 3
H33B H 0.4640 0.5680 0.7919 0.057 Uiso 0.580(14) 1 calc PR B 3
H33C H 0.4982 0.4827 0.8207 0.057 Uiso 0.580(14) 1 calc PR B 3
C311 C 0.5181(5) 0.6310(8) 0.8441(5) 0.054(4) Uani 0.387(9) 1 d P B 4
H31D H 0.5255 0.6865 0.8655 0.081 Uiso 0.387(9) 1 calc PR B 4
H31E H 0.4870 0.6359 0.8018 0.081 Uiso 0.387(9) 1 calc PR B 4
H31F H 0.5507 0.6118 0.8393 0.081 Uiso 0.387(9) 1 calc PR B 4
C331 C 0.4974(4) 0.4770(9) 0.8308(4) 0.034(4) Uani 0.420(14) 1 d P B 4
H33D H 0.4881 0.4257 0.8481 0.051 Uiso 0.420(14) 1 calc PR B 4
H33E H 0.5322 0.4680 0.8278 0.051 Uiso 0.420(14) 1 calc PR B 4
H33F H 0.4682 0.4889 0.7882 0.051 Uiso 0.420(14) 1 calc PR B 4
C34 C 0.72423(14) 0.2602(2) 0.64488(15) 0.0278(8) Uani 1 1 d . . .
H34A H 0.7514 0.2939 0.6364 0.033 Uiso 1 1 calc R . .
H34B H 0.6874 0.2842 0.6185 0.033 Uiso 1 1 calc R . .
C35 C 0.72591(16) 0.1695(2) 0.62551(17) 0.0363(9) Uani 1 1 d . . .
H35A H 0.7150 0.1669 0.5794 0.055 Uiso 1 1 calc R . .
H35B H 0.7005 0.1353 0.6360 0.055 Uiso 1 1 calc R . .
H35C H 0.7633 0.1472 0.6486 0.055 Uiso 1 1 calc R . .
C36 C 0.76961(14) 0.18948(19) 0.87329(15) 0.0273(8) Uani 1 1 d . . .
H36A H 0.8062 0.1638 0.8848 0.033 Uiso 1 1 calc R . .
H36B H 0.7420 0.1433 0.8583 0.033 Uiso 1 1 calc R . .
C37 C 0.76893(14) 0.2302(2) 0.93167(15) 0.0317(8) Uani 1 1 d . . .
H37A H 0.7758 0.1868 0.9646 0.048 Uiso 1 1 calc R . .
H37B H 0.7330 0.2564 0.9204 0.048 Uiso 1 1 calc R . .
H37C H 0.7976 0.2739 0.9480 0.048 Uiso 1 1 calc R . .
C38 C 0.58437(16) 0.2449(3) 0.63191(19) 0.0497(11) Uani 1 1 d . C 5
H38A H 0.5614 0.2253 0.6531 0.060 Uiso 1 1 calc R C 5
H38B H 0.5996 0.1939 0.6202 0.060 Uiso 1 1 calc R C 5
C39 C 0.5507(2) 0.2898(3) 0.5753(2) 0.085(2) Uani 1 1 d . C 5
H39A H 0.5238 0.2507 0.5448 0.128 Uiso 1 1 calc R C 5
H39B H 0.5736 0.3140 0.5561 0.128 Uiso 1 1 calc R C 5
H39C H 0.5314 0.3358 0.5858 0.128 Uiso 1 1 calc R C 5
C40 C 0.87495(14) 0.2562(2) 0.70901(16) 0.0304(8) Uani 1 1 d . D 5
H40A H 0.8569 0.2531 0.6617 0.036 Uiso 1 1 calc R D 5
H40B H 0.8820 0.1974 0.7260 0.036 Uiso 1 1 calc R D 5
C41 C 0.92808(15) 0.3035(3) 0.73064(19) 0.0473(11) Uani 1 1 d . D 5
H41A H 0.9517 0.2751 0.7142 0.071 Uiso 1 1 calc R D 5
H41B H 0.9465 0.3044 0.7775 0.071 Uiso 1 1 calc R D 5
H41C H 0.9208 0.3620 0.7144 0.071 Uiso 1 1 calc R D 5

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 0.0222(3) 0.0137(3) 0.0216(3) -0.0004(2) 0.0100(2) 0.0013(2)
V2 0.0207(3) 0.0149(3) 0.0255(3) -0.0016(2) 0.0082(2) -0.0021(2)
O1 0.0214(12) 0.0180(12) 0.0244(12) 0.0018(9) 0.0077(10) 0.0010(9)
O2 0.0226(12) 0.0193(12) 0.0342(13) -0.0001(9) 0.0138(11) 0.0000(9)
O3 0.0291(13) 0.0175(12) 0.0287(13) -0.0028(9) 0.0122(11) 0.0037(9)
O4 0.0311(13) 0.0166(12) 0.0413(14) -0.0048(10) 0.0178(12) -0.0033(10)
O5 0.0239(12) 0.0193(12) 0.0162(11) -0.0014(8) 0.0076(9) 0.0007(9)
O6 0.0228(11) 0.0178(11) 0.0202(11) 0.0037(9) 0.0091(9) 0.0012(9)
O7 0.0215(12) 0.0228(12) 0.0262(13) -0.0055(10) 0.0008(10) -0.0021(10)
O8 0.0276(13) 0.0220(12) 0.0290(13) 0.0003(10) 0.0181(11) 0.0028(10)
N1 0.0186(14) 0.0154(13) 0.0157(13) 0.0004(10) 0.0086(11) 0.0002(10)
N2 0.0167(13) 0.0150(13) 0.0167(13) 0.0010(10) 0.0072(11) 0.0008(10)
C1 0.0228(17) 0.0109(15) 0.0216(17) 0.0016(12) 0.0122(14) 0.0015(12)
C2 0.0287(18) 0.0175(16) 0.0138(16) 0.0033(12) 0.0107(14) 0.0010(13)
C3 0.0271(18) 0.0143(16) 0.0157(16) 0.0002(12) 0.0085(14) 0.0039(13)
C4 0.0206(17) 0.0131(16) 0.0239(17) -0.0002(13) 0.0109(14) -0.0018(12)
C5 0.0152(16) 0.0214(17) 0.0217(17) -0.0012(13) 0.0112(14) -0.0011(13)
C6 0.0173(17) 0.0218(17) 0.0241(18) 0.0013(14) 0.0101(14) -0.0011(13)
C7 0.0251(18) 0.0241(18) 0.0267(18) 0.0053(14) 0.0111(15) 0.0012(14)
C8 0.0214(18) 0.039(2) 0.0196(18) 0.0027(15) 0.0074(15) 0.0003(15)
C9 0.0172(17) 0.033(2) 0.0251(18) 0.0005(14) 0.0112(15) -0.0013(14)
C10 0.0158(16) 0.0220(17) 0.0281(19) -0.0053(14) 0.0097(15) -0.0041(13)
C11 0.0251(19) 0.035(2) 0.0228(19) -0.0063(15) 0.0083(16) -0.0058(15)
C12 0.036(2) 0.047(2) 0.036(2) -0.0152(18) 0.0165(19) -0.0127(18)
C13 0.063(3) 0.048(3) 0.032(2) -0.0111(19) 0.001(2) -0.003(2)
C14 0.032(2) 0.040(2) 0.028(2) -0.0118(16) 0.0150(17) -0.0078(16)
C15 0.040(2) 0.053(3) 0.042(2) -0.026(2) 0.030(2) -0.0236(19)
C16 0.086(4) 0.088(4) 0.063(3) -0.003(3) 0.042(3) -0.040(3)
C17 0.043(3) 0.069(3) 0.058(3) -0.039(2) 0.034(2) -0.035(2)
C18 0.047(3) 0.092(4) 0.076(3) -0.052(3) 0.040(3) -0.026(3)
C19 0.0254(18) 0.0154(16) 0.0217(17) 0.0010(13) 0.0119(15) 0.0031(13)
C20 0.0130(16) 0.0246(17) 0.0234(17) 0.0035(14) 0.0095(14) -0.0016(13)
C21 0.0176(17) 0.0227(18) 0.0266(18) 0.0001(14) 0.0087(15) -0.0008(13)
C22 0.0275(19) 0.0221(18) 0.034(2) 0.0097(15) 0.0143(17) -0.0004(14)
C23 0.031(2) 0.032(2) 0.0297(19) 0.0043(15) 0.0184(17) -0.0013(15)
C24 0.0233(18) 0.0277(19) 0.0203(18) 0.0019(14) 0.0108(15) -0.0018(14)
C25 0.0224(18) 0.0185(17) 0.0274(19) 0.0006(14) 0.0116(15) -0.0023(13)
C26 0.0248(18) 0.032(2) 0.0211(18) -0.0026(14) 0.0128(15) -0.0018(15)
C27 0.0225(19) 0.053(2) 0.030(2) -0.0043(17) 0.0083(17) 0.0015(17)
C28 0.046(2) 0.041(2) 0.039(2) -0.0137(18) 0.027(2) -0.0104(18)
C29 0.0279(19) 0.032(2) 0.0218(18) -0.0008(14) 0.0107(16) 0.0040(15)
C30 0.030(2) 0.068(3) 0.040(3) 0.030(2) 0.0010(19) -0.013(2)
C31 0.043(4) 0.036(4) 0.048(4) 0.020(3) 0.015(3) 0.012(3)
C32 0.035(2) 0.061(3) 0.045(3) -0.008(2) 0.006(2) 0.020(2)
C33 0.028(4) 0.047(7) 0.033(4) 0.004(3) 0.007(3) 0.004(3)
C311 0.051(7) 0.060(8) 0.035(7) 0.023(6) 0.003(6) 0.004(6)
C331 0.023(5) 0.058(10) 0.020(5) -0.012(5) 0.006(4) -0.004(5)
C34 0.0327(19) 0.0268(19) 0.0214(17) -0.0009(14) 0.0093(15) -0.0002(15)
C35 0.050(2) 0.0262(19) 0.031(2) -0.0057(16) 0.0154(19) -0.0026(17)
C36 0.035(2) 0.0174(18) 0.0287(19) 0.0070(14) 0.0135(17) -0.0006(14)
C37 0.034(2) 0.040(2) 0.0207(18) 0.0068(15) 0.0112(16) 0.0058(16)
C38 0.035(2) 0.046(2) 0.045(2) -0.005(2) -0.0045(19) -0.017(2)
C39 0.069(3) 0.050(3) 0.070(4) 0.005(3) -0.032(3) -0.020(3)
C40 0.039(2) 0.0301(19) 0.0315(19) 0.0047(16) 0.0238(17) 0.0144(16)
C41 0.031(2) 0.066(3) 0.050(3) 0.015(2) 0.022(2) 0.015(2)

_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 O3 1.596(2) . ?
V1 O8 1.806(2) . ?
V1 O1 1.842(2) . ?
V1 O5 1.988(2) . ?
V1 O6 2.009(2) . ?
V1 N1 2.470(2) . ?
V2 O4 1.595(2) . ?
V2 O7 1.799(2) . ?
V2 O2 1.852(2) . ?
V2 O5 2.001(2) . ?
V2 O6 2.010(2) . ?
V2 N2 2.457(2) . ?
O1 C6 1.348(4) . ?
O2 C21 1.359(4) . ?
O5 C34 1.432(4) . ?
O6 C36 1.443(4) . ?
O7 C38 1.420(4) . ?
O8 C40 1.417(4) . ?
N1 C1 1.468(4) . ?
N1 C4 1.479(4) . ?
N1 C2 1.496(4) . ?
N2 C1 1.473(4) . ?
N2 C19 1.474(4) . ?
N2 C3 1.494(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.518(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.384(4) . ?
C5 C6 1.402(4) . ?
C6 C7 1.398(4) . ?
C7 C8 1.391(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.393(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.404(4) . ?
C9 C11 1.536(4) . ?
C10 H10A 0.9500 . ?
C11 C13 1.526(5) . ?
C11 C12 1.539(5) . ?
C11 C14 1.563(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.538(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.505(6) . ?
C15 C17 1.542(5) . ?
C15 C18 1.548(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.519(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C25 1.387(4) . ?
C20 C21 1.394(4) . ?
C21 C22 1.392(4) . ?
C22 C23 1.373(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.400(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.392(4) . ?
C24 C26 1.533(4) . ?
C25 H25A 0.9500 . ?
C26 C28 1.529(5) . ?
C26 C27 1.538(5) . ?
C26 C29 1.563(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.523(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C33 1.367(7) . ?
C30 C311 1.508(11) . ?
C30 C32 1.520(6) . ?
C30 C31 1.680(7) . ?
C30 C331 1.833(12) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C311 H31D 0.9800 . ?
C311 H31E 0.9800 . ?
C311 H31F 0.9800 . ?
C331 H33D 0.9800 . ?
C331 H33E 0.9800 . ?
C331 H33F 0.9800 . ?
C34 C35 1.501(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.503(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.421(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.496(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

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
O3 V1 O8 98.85(11) . . ?
O3 V1 O1 96.53(10) . . ?
O8 V1 O1 101.22(10) . . ?
O3 V1 O5 99.60(10) . . ?
O8 V1 O5 90.18(9) . . ?
O1 V1 O5 158.56(9) . . ?
O3 V1 O6 99.59(10) . . ?
O8 V1 O6 157.18(9) . . ?
O1 V1 O6 89.90(9) . . ?
O5 V1 O6 73.59(8) . . ?
O3 V1 N1 179.32(10) . . ?
O8 V1 N1 80.55(9) . . ?
O1 V1 N1 83.92(8) . . ?
O5 V1 N1 80.09(8) . . ?
O6 V1 N1 80.91(8) . . ?
O4 V2 O7 99.10(11) . . ?
O4 V2 O2 96.77(11) . . ?
O7 V2 O2 100.06(10) . . ?
O4 V2 O5 99.37(10) . . ?
O7 V2 O5 89.82(10) . . ?
O2 V2 O5 159.49(9) . . ?
O4 V2 O6 97.83(10) . . ?
O7 V2 O6 157.79(10) . . ?
O2 V2 O6 92.08(9) . . ?
O5 V2 O6 73.30(8) . . ?
O4 V2 N2 178.92(11) . . ?
O7 V2 N2 80.57(9) . . ?
O2 V2 N2 84.30(9) . . ?
O5 V2 N2 79.62(8) . . ?
O6 V2 N2 82.24(8) . . ?
C6 O1 V1 137.51(19) . . ?
C21 O2 V2 139.44(19) . . ?
C34 O5 V1 124.0(2) . . ?
C34 O5 V2 126.9(2) . . ?
V1 O5 V2 107.08(9) . . ?
C36 O6 V1 117.82(18) . . ?
C36 O6 V2 120.51(19) . . ?
V1 O6 V2 105.99(9) . . ?
C38 O7 V2 125.7(2) . . ?
C40 O8 V1 128.0(2) . . ?
C1 N1 C4 112.6(2) . . ?
C1 N1 C2 102.2(2) . . ?
C4 N1 C2 109.4(2) . . ?
C1 N1 V1 115.43(17) . . ?
C4 N1 V1 106.26(17) . . ?
C2 N1 V1 110.92(17) . . ?
C1 N2 C19 112.5(2) . . ?
C1 N2 C3 102.6(2) . . ?
C19 N2 C3 108.8(2) . . ?
C1 N2 V2 114.04(16) . . ?
C19 N2 V2 107.74(17) . . ?
C3 N2 V2 111.07(17) . . ?
N1 C1 N2 102.9(2) . . ?
N1 C1 H1A 111.2 . . ?
N2 C1 H1A 111.2 . . ?
N1 C1 H1B 111.2 . . ?
N2 C1 H1B 111.2 . . ?
H1A C1 H1B 109.1 . . ?
N1 C2 C3 104.7(2) . . ?
N1 C2 H2A 110.8 . . ?
C3 C2 H2A 110.8 . . ?
N1 C2 H2B 110.8 . . ?
C3 C2 H2B 110.8 . . ?
H2A C2 H2B 108.9 . . ?
N2 C3 C2 105.6(2) . . ?
N2 C3 H3A 110.6 . . ?
C2 C3 H3A 110.6 . . ?
N2 C3 H3B 110.6 . . ?
C2 C3 H3B 110.6 . . ?
H3A C3 H3B 108.8 . . ?
N1 C4 C5 112.6(2) . . ?
N1 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C10 C5 C6 119.5(3) . . ?
C10 C5 C4 120.9(3) . . ?
C6 C5 C4 119.5(3) . . ?
O1 C6 C7 118.7(3) . . ?
O1 C6 C5 122.4(3) . . ?
C7 C6 C5 118.8(3) . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C7 C8 C9 121.7(3) . . ?
C7 C8 H8A 119.1 . . ?
C9 C8 H8A 119.1 . . ?
C8 C9 C10 116.9(3) . . ?
C8 C9 C11 123.6(3) . . ?
C10 C9 C11 119.5(3) . . ?
C5 C10 C9 122.6(3) . . ?
C5 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
C13 C11 C9 112.7(3) . . ?
C13 C11 C12 105.6(3) . . ?
C9 C11 C12 110.1(3) . . ?
C13 C11 C14 112.8(3) . . ?
C9 C11 C14 110.8(3) . . ?
C12 C11 C14 104.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C11 123.8(3) . . ?
C15 C14 H14A 106.4 . . ?
C11 C14 H14A 106.4 . . ?
C15 C14 H14B 106.4 . . ?
C11 C14 H14B 106.4 . . ?
H14A C14 H14B 106.5 . . ?
C16 C15 C14 114.5(4) . . ?
C16 C15 C17 109.6(4) . . ?
C14 C15 C17 113.3(3) . . ?
C16 C15 C18 107.3(4) . . ?
C14 C15 C18 104.6(3) . . ?
C17 C15 C18 106.9(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
N2 C19 C20 114.9(2) . . ?
N2 C19 H19A 108.5 . . ?
C20 C19 H19A 108.5 . . ?
N2 C19 H19B 108.5 . . ?
C20 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C25 C20 C21 119.3(3) . . ?
C25 C20 C19 119.5(3) . . ?
C21 C20 C19 120.9(3) . . ?
O2 C21 C22 118.1(3) . . ?
O2 C21 C20 123.0(3) . . ?
C22 C21 C20 118.8(3) . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C22 C23 C24 122.5(3) . . ?
C22 C23 H23A 118.8 . . ?
C24 C23 H23A 118.8 . . ?
C25 C24 C23 115.9(3) . . ?
C25 C24 C26 123.6(3) . . ?
C23 C24 C26 120.5(3) . . ?
C20 C25 C24 123.0(3) . . ?
C20 C25 H25A 118.5 . . ?
C24 C25 H25A 118.5 . . ?
C28 C26 C24 111.8(3) . . ?
C28 C26 C27 106.6(3) . . ?
C24 C26 C27 108.6(3) . . ?
C28 C26 C29 112.2(3) . . ?
C24 C26 C29 112.1(3) . . ?
C27 C26 C29 105.1(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C26 125.4(3) . . ?
C30 C29 H29A 106.0 . . ?
C26 C29 H29A 106.0 . . ?
C30 C29 H29B 106.0 . . ?
C26 C29 H29B 106.0 . . ?
H29A C29 H29B 106.3 . . ?
C33 C30 C311 60.5(7) . . ?
C33 C30 C32 112.9(4) . . ?
C311 C30 C32 130.2(6) . . ?
C33 C30 C29 122.1(5) . . ?
C311 C30 C29 116.8(5) . . ?
C32 C30 C29 107.5(3) . . ?
C33 C30 C31 110.1(5) . . ?
C311 C30 C31 53.6(5) . . ?
C32 C30 C31 93.8(4) . . ?
C29 C30 C31 106.5(4) . . ?
C33 C30 C331 35.9(4) . . ?
C311 C30 C331 95.0(7) . . ?
C32 C30 C331 99.0(4) . . ?
C29 C30 C331 99.5(4) . . ?
C31 C30 C331 145.9(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C30 C311 H31D 109.5 . . ?
C30 C311 H31E 109.5 . . ?
C30 C311 H31F 109.5 . . ?
C30 C331 H33D 109.5 . . ?
C30 C331 H33E 109.5 . . ?
C30 C331 H33F 109.5 . . ?
O5 C34 C35 112.1(3) . . ?
O5 C34 H34A 109.2 . . ?
C35 C34 H34A 109.2 . . ?
O5 C34 H34B 109.2 . . ?
C35 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O6 C36 C37 111.9(3) . . ?
O6 C36 H36A 109.2 . . ?
C37 C36 H36A 109.2 . . ?
O6 C36 H36B 109.2 . . ?
C37 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O7 C38 C39 113.2(3) . . ?
O7 C38 H38A 108.9 . . ?
C39 C38 H38A 108.9 . . ?
O7 C38 H38B 108.9 . . ?
C39 C38 H38B 108.9 . . ?
H38A C38 H38B 107.8 . . ?
O8 C40 C41 109.4(3) . . ?
O8 C40 H40A 109.8 . . ?
C41 C40 H40A 109.8 . . ?
O8 C40 H40B 109.8 . . ?
C41 C40 H40B 109.8 . . ?
H40A C40 H40B 108.3 . . ?

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
O3 V1 O1 C6 -165.5(3) . . . . ?
O8 V1 O1 C6 94.1(3) . . . . ?
O5 V1 O1 C6 -26.8(4) . . . . ?
O6 V1 O1 C6 -65.8(3) . . . . ?
N1 V1 O1 C6 15.1(3) . . . . ?
O4 V2 O2 C21 176.6(3) . . . . ?
O7 V2 O2 C21 -82.8(3) . . . . ?
O5 V2 O2 C21 34.9(5) . . . . ?
O6 V2 O2 C21 78.5(3) . . . . ?
N2 V2 O2 C21 -3.5(3) . . . . ?
O3 V1 O5 C34 -69.1(2) . . . . ?
O8 V1 O5 C34 30.0(2) . . . . ?
O1 V1 O5 C34 152.7(3) . . . . ?
O6 V1 O5 C34 -166.3(2) . . . . ?
N1 V1 O5 C34 110.3(2) . . . . ?
O3 V1 O5 V2 95.60(11) . . . . ?
O8 V1 O5 V2 -165.39(10) . . . . ?
O1 V1 O5 V2 -42.7(3) . . . . ?
O6 V1 O5 V2 -1.66(9) . . . . ?
N1 V1 O5 V2 -85.01(9) . . . . ?
O4 V2 O5 C34 70.3(2) . . . . ?
O7 V2 O5 C34 -28.9(2) . . . . ?
O2 V2 O5 C34 -148.2(3) . . . . ?
O6 V2 O5 C34 165.7(2) . . . . ?
N2 V2 O5 C34 -109.3(2) . . . . ?
O4 V2 O5 V1 -93.77(11) . . . . ?
O7 V2 O5 V1 167.04(10) . . . . ?
O2 V2 O5 V1 47.7(3) . . . . ?
O6 V2 O5 V1 1.67(9) . . . . ?
N2 V2 O5 V1 86.59(9) . . . . ?
O3 V1 O6 C36 42.8(2) . . . . ?
O8 V1 O6 C36 -173.6(2) . . . . ?
O1 V1 O6 C36 -53.8(2) . . . . ?
O5 V1 O6 C36 140.1(2) . . . . ?
N1 V1 O6 C36 -137.6(2) . . . . ?
O3 V1 O6 V2 -95.62(11) . . . . ?
O8 V1 O6 V2 47.9(3) . . . . ?
O1 V1 O6 V2 167.77(10) . . . . ?
O5 V1 O6 V2 1.65(9) . . . . ?
N1 V1 O6 V2 83.92(9) . . . . ?
O4 V2 O6 C36 -41.2(2) . . . . ?
O7 V2 O6 C36 179.3(2) . . . . ?
O2 V2 O6 C36 55.9(2) . . . . ?
O5 V2 O6 C36 -138.7(2) . . . . ?
N2 V2 O6 C36 139.8(2) . . . . ?
O4 V2 O6 V1 95.85(11) . . . . ?
O7 V2 O6 V1 -43.6(3) . . . . ?
O2 V2 O6 V1 -167.03(10) . . . . ?
O5 V2 O6 V1 -1.64(9) . . . . ?
N2 V2 O6 V1 -83.07(9) . . . . ?
O4 V2 O7 C38 10.0(3) . . . . ?
O2 V2 O7 C38 -88.6(3) . . . . ?
O5 V2 O7 C38 109.5(3) . . . . ?
O6 V2 O7 C38 149.3(3) . . . . ?
N2 V2 O7 C38 -171.0(3) . . . . ?
O3 V1 O8 C40 -14.8(3) . . . . ?
O1 V1 O8 C40 83.8(3) . . . . ?
O5 V1 O8 C40 -114.5(3) . . . . ?
O6 V1 O8 C40 -158.4(2) . . . . ?
N1 V1 O8 C40 165.6(3) . . . . ?
O3 V1 N1 C1 136(9) . . . . ?
O8 V1 N1 C1 165.2(2) . . . . ?
O1 V1 N1 C1 -92.33(19) . . . . ?
O5 V1 N1 C1 73.33(19) . . . . ?
O6 V1 N1 C1 -1.45(19) . . . . ?
O3 V1 N1 C4 -98(9) . . . . ?
O8 V1 N1 C4 -69.23(18) . . . . ?
O1 V1 N1 C4 33.26(18) . . . . ?
O5 V1 N1 C4 -161.08(18) . . . . ?
O6 V1 N1 C4 124.13(18) . . . . ?
O3 V1 N1 C2 21(9) . . . . ?
O8 V1 N1 C2 49.56(19) . . . . ?
O1 V1 N1 C2 152.04(19) . . . . ?
O5 V1 N1 C2 -42.30(18) . . . . ?
O6 V1 N1 C2 -117.08(19) . . . . ?
O4 V2 N2 C1 -96(6) . . . . ?
O7 V2 N2 C1 -168.0(2) . . . . ?
O2 V2 N2 C1 90.76(19) . . . . ?
O5 V2 N2 C1 -76.46(19) . . . . ?
O6 V2 N2 C1 -2.12(18) . . . . ?
O4 V2 N2 C19 139(6) . . . . ?
O7 V2 N2 C19 66.37(18) . . . . ?
O2 V2 N2 C19 -34.85(18) . . . . ?
O5 V2 N2 C19 157.92(18) . . . . ?
O6 V2 N2 C19 -127.74(18) . . . . ?
O4 V2 N2 C3 20(6) . . . . ?
O7 V2 N2 C3 -52.69(19) . . . . ?
O2 V2 N2 C3 -153.91(19) . . . . ?
O5 V2 N2 C3 38.86(18) . . . . ?
O6 V2 N2 C3 113.20(19) . . . . ?
C4 N1 C1 N2 163.2(2) . . . . ?
C2 N1 C1 N2 46.0(3) . . . . ?
V1 N1 C1 N2 -74.5(2) . . . . ?
C19 N2 C1 N1 -160.8(2) . . . . ?
C3 N2 C1 N1 -44.0(3) . . . . ?
V2 N2 C1 N1 76.2(2) . . . . ?
C1 N1 C2 C3 -29.6(3) . . . . ?
C4 N1 C2 C3 -149.1(2) . . . . ?
V1 N1 C2 C3 94.0(2) . . . . ?
C1 N2 C3 C2 24.7(3) . . . . ?
C19 N2 C3 C2 144.0(2) . . . . ?
V2 N2 C3 C2 -97.5(2) . . . . ?
N1 C2 C3 N2 3.0(3) . . . . ?
C1 N1 C4 C5 60.8(3) . . . . ?
C2 N1 C4 C5 173.7(2) . . . . ?
V1 N1 C4 C5 -66.5(3) . . . . ?
N1 C4 C5 C10 -125.6(3) . . . . ?
N1 C4 C5 C6 56.6(4) . . . . ?
V1 O1 C6 C7 147.1(2) . . . . ?
V1 O1 C6 C5 -34.9(4) . . . . ?
C10 C5 C6 O1 -179.2(3) . . . . ?
C4 C5 C6 O1 -1.3(4) . . . . ?
C10 C5 C6 C7 -1.2(4) . . . . ?
C4 C5 C6 C7 176.6(3) . . . . ?
O1 C6 C7 C8 178.7(3) . . . . ?
C5 C6 C7 C8 0.7(5) . . . . ?
C6 C7 C8 C9 1.1(5) . . . . ?
C7 C8 C9 C10 -2.1(5) . . . . ?
C7 C8 C9 C11 177.3(3) . . . . ?
C6 C5 C10 C9 0.1(5) . . . . ?
C4 C5 C10 C9 -177.7(3) . . . . ?
C8 C9 C10 C5 1.5(4) . . . . ?
C11 C9 C10 C5 -177.9(3) . . . . ?
C8 C9 C11 C13 13.3(5) . . . . ?
C10 C9 C11 C13 -167.2(3) . . . . ?
C8 C9 C11 C12 131.0(3) . . . . ?
C10 C9 C11 C12 -49.6(4) . . . . ?
C8 C9 C11 C14 -114.1(4) . . . . ?
C10 C9 C11 C14 65.3(4) . . . . ?
C13 C11 C14 C15 -73.9(4) . . . . ?
C9 C11 C14 C15 53.5(4) . . . . ?
C12 C11 C14 C15 172.0(3) . . . . ?
C11 C14 C15 C16 54.8(5) . . . . ?
C11 C14 C15 C17 -72.0(5) . . . . ?
C11 C14 C15 C18 172.0(3) . . . . ?
C1 N2 C19 C20 -64.0(3) . . . . ?
C3 N2 C19 C20 -177.0(2) . . . . ?
V2 N2 C19 C20 62.5(3) . . . . ?
N2 C19 C20 C25 133.5(3) . . . . ?
N2 C19 C20 C21 -52.3(4) . . . . ?
V2 O2 C21 C22 -161.7(2) . . . . ?
V2 O2 C21 C20 19.7(5) . . . . ?
C25 C20 C21 O2 179.7(3) . . . . ?
C19 C20 C21 O2 5.5(5) . . . . ?
C25 C20 C21 C22 1.1(5) . . . . ?
C19 C20 C21 C22 -173.0(3) . . . . ?
O2 C21 C22 C23 -177.9(3) . . . . ?
C20 C21 C22 C23 0.7(5) . . . . ?
C21 C22 C23 C24 -1.5(5) . . . . ?
C22 C23 C24 C25 0.5(5) . . . . ?
C22 C23 C24 C26 -178.5(3) . . . . ?
C21 C20 C25 C24 -2.2(5) . . . . ?
C19 C20 C25 C24 172.0(3) . . . . ?
C23 C24 C25 C20 1.4(5) . . . . ?
C26 C24 C25 C20 -179.6(3) . . . . ?
C25 C24 C26 C28 -14.3(4) . . . . ?
C23 C24 C26 C28 164.6(3) . . . . ?
C25 C24 C26 C27 -131.7(3) . . . . ?
C23 C24 C26 C27 47.3(4) . . . . ?
C25 C24 C26 C29 112.7(3) . . . . ?
C23 C24 C26 C29 -68.4(4) . . . . ?
C28 C26 C29 C30 57.5(4) . . . . ?
C24 C26 C29 C30 -69.2(4) . . . . ?
C27 C26 C29 C30 173.1(3) . . . . ?
C26 C29 C30 C33 44.8(7) . . . . ?
C26 C29 C30 C311 -25.6(8) . . . . ?
C26 C29 C30 C32 177.7(3) . . . . ?
C26 C29 C30 C31 -82.7(5) . . . . ?
C26 C29 C30 C331 75.0(5) . . . . ?
V1 O5 C34 C35 75.7(3) . . . . ?
V2 O5 C34 C35 -85.9(3) . . . . ?
V1 O6 C36 C37 127.6(2) . . . . ?
V2 O6 C36 C37 -100.2(3) . . . . ?
V2 O7 C38 C39 -174.7(3) . . . . ?
V1 O8 C40 C41 -121.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.064





data_zj30
_database_code_depnum_ccdc_archive 'CCDC 855050'
#TrackingRef '- zj30.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H52 N2 O2'
_chemical_formula_sum            'C33 H52 N2 O2'
_chemical_formula_weight         508.77

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2

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

_cell_length_a                   6.492(3)
_cell_length_b                   11.653(5)
_cell_length_c                   22.139(9)
_cell_angle_alpha                98.79(5)
_cell_angle_beta                 96.86(5)
_cell_angle_gamma                93.90(5)
_cell_volume                     1637.0(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4722
_cell_measurement_theta_min      3
_cell_measurement_theta_max      37

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   ANALYTICAL
_exptl_absorpt_correction_T_min  0.9826
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Kuma KM-4 CCD kappa-axis diffractometer'
_diffrn_measurement_method       \OMEGA
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18377
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7505
_reflns_number_gt                4042
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kuma KM4 software 1996'
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_structure_solution    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_structure_refinement  'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'SHELXTL-NT V5.1, Bruker AXS 1999'

_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.
;

_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^)+(0.0618P)^2^+0.0000P] 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         7505
_refine_ls_number_parameters     457
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1488
_refine_ls_wR_factor_gt          0.1362
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
O2 O 0.2768(2) 0.74712(11) 0.47742(6) 0.0373(3) Uani 1 1 d D . .
H2 H 0.370(2) 0.7196(18) 0.4576(9) 0.056 Uiso 1 1 d D . .
O1 O 1.2056(2) 0.54280(12) 0.36869(6) 0.0380(3) Uani 1 1 d D . .
H1 H 1.110(2) 0.5436(19) 0.3913(8) 0.057 Uiso 1 1 d D . .
N1 N 0.8263(2) 0.54575(13) 0.40488(7) 0.0297(4) Uani 1 1 d . . .
N2 N 0.6669(2) 0.70426(13) 0.45253(7) 0.0288(4) Uani 1 1 d . . .
C21 C 0.3813(3) 0.82415(16) 0.52652(9) 0.0313(4) Uani 1 1 d . C .
C6 C 1.1026(3) 0.51779(16) 0.30984(9) 0.0314(4) Uani 1 1 d . D .
C20 C 0.5889(3) 0.86740(15) 0.52690(8) 0.0288(4) Uani 1 1 d . . .
C5 C 0.8904(3) 0.47813(16) 0.29788(9) 0.0307(4) Uani 1 1 d . . .
C22 C 0.2788(3) 0.85942(17) 0.57640(9) 0.0342(5) Uani 1 1 d . . .
H22 H 0.1377 0.8312 0.5759 0.041 Uiso 1 1 calc R C .
C7 C 1.2113(3) 0.53088(17) 0.26086(9) 0.0348(5) Uani 1 1 d . . .
H7 H 1.3544 0.5587 0.2687 0.042 Uiso 1 1 calc R D .
C25 C 0.6857(3) 0.94349(15) 0.57870(8) 0.0300(4) Uani 1 1 d . C .
H25 H 0.8260 0.9729 0.5790 0.036 Uiso 1 1 calc R . .
C10 C 0.7957(3) 0.45389(16) 0.23666(9) 0.0346(5) Uani 1 1 d . D .
H10 H 0.6516 0.4281 0.2287 0.042 Uiso 1 1 calc R . .
C23 C 0.3795(3) 0.93556(16) 0.62717(9) 0.0333(5) Uani 1 1 d . C .
H23 H 0.3052 0.9590 0.6608 0.040 Uiso 1 1 calc R . .
C8 C 1.1146(3) 0.50407(17) 0.20092(9) 0.0376(5) Uani 1 1 d . D .
H8 H 1.1942 0.5118 0.1682 0.045 Uiso 1 1 calc R . .
C24 C 0.5871(3) 0.97882(15) 0.63035(8) 0.0294(4) Uani 1 1 d . . .
C9 C 0.9031(3) 0.46580(17) 0.18680(9) 0.0352(5) Uani 1 1 d . . .
C26 C 0.7012(3) 1.05783(16) 0.68802(8) 0.0322(5) Uani 1 1 d . A .
C11 C 0.7950(3) 0.43892(19) 0.11991(9) 0.0434(5) Uani 1 1 d . B .
C27A C 0.5571(6) 1.1125(4) 0.7309(2) 0.0485(12) Uani 0.570(4) 1 d P A 1
H27A H 0.6390 1.1670 0.7648 0.073 Uiso 0.570(4) 1 calc PR A 1
H27B H 0.4821 1.0513 0.7477 0.073 Uiso 0.570(4) 1 calc PR A 1
H27C H 0.4569 1.1546 0.7081 0.073 Uiso 0.570(4) 1 calc PR A 1
C29A C 0.8694(5) 0.9917(3) 0.72184(16) 0.0366(10) Uani 0.570(4) 1 d P A 1
H29A H 0.9710 0.9716 0.6928 0.044 Uiso 0.570(4) 1 calc PR A 1
H29B H 0.9445 1.0485 0.7566 0.044 Uiso 0.570(4) 1 calc PR A 1
C28A C 0.8282(8) 1.1609(4) 0.66808(19) 0.0482(12) Uani 0.570(4) 1 d P A 1
H28A H 0.9055 1.2102 0.7047 0.072 Uiso 0.570(4) 1 calc PR A 1
H28B H 0.7327 1.2072 0.6464 0.072 Uiso 0.570(4) 1 calc PR A 1
H28C H 0.9261 1.1300 0.6406 0.072 Uiso 0.570(4) 1 calc PR A 1
C28B C 0.9174(8) 1.1012(5) 0.6805(2) 0.0401(14) Uani 0.430(4) 1 d P A 2
H28D H 0.9127 1.1414 0.6446 0.060 Uiso 0.430(4) 1 calc PR A 2
H28E H 1.0026 1.0352 0.6744 0.060 Uiso 0.430(4) 1 calc PR A 2
H28F H 0.9784 1.1555 0.7176 0.060 Uiso 0.430(4) 1 calc PR A 2
C29B C 0.6949(7) 0.9986(4) 0.7460(2) 0.0366(13) Uani 0.430(4) 1 d P A 2
H29C H 0.5469 0.9809 0.7508 0.044 Uiso 0.430(4) 1 calc PR A 2
H29D H 0.7569 1.0562 0.7824 0.044 Uiso 0.430(4) 1 calc PR A 2
C27B C 0.5732(9) 1.1666(5) 0.6997(3) 0.0452(15) Uani 0.430(4) 1 d P A 2
H27D H 0.6356 1.2172 0.7379 0.068 Uiso 0.430(4) 1 calc PR A 2
H27E H 0.4291 1.1407 0.7033 0.068 Uiso 0.430(4) 1 calc PR A 2
H27F H 0.5750 1.2099 0.6651 0.068 Uiso 0.430(4) 1 calc PR A 2
C12A C 0.6592(7) 0.3177(4) 0.11100(18) 0.0599(12) Uani 0.647(4) 1 d P B 3
H12A H 0.5512 0.3236 0.1384 0.090 Uiso 0.647(4) 1 calc PR B 3
H12B H 0.7490 0.2570 0.1210 0.090 Uiso 0.647(4) 1 calc PR B 3
H12C H 0.5936 0.2974 0.0681 0.090 Uiso 0.647(4) 1 calc PR B 3
C13A C 0.9397(6) 0.4263(5) 0.07280(17) 0.0638(14) Uani 0.647(4) 1 d P B 3
H13A H 0.8596 0.4113 0.0316 0.096 Uiso 0.647(4) 1 calc PR B 3
H13B H 1.0237 0.3611 0.0784 0.096 Uiso 0.647(4) 1 calc PR B 3
H13C H 1.0315 0.4983 0.0773 0.096 Uiso 0.647(4) 1 calc PR B 3
C14A C 0.6254(5) 0.5270(3) 0.10819(15) 0.0450(10) Uani 0.647(4) 1 d P B 3
H14A H 0.5278 0.5225 0.1390 0.054 Uiso 0.647(4) 1 calc PR B 3
H14B H 0.5449 0.4980 0.0672 0.054 Uiso 0.647(4) 1 calc PR B 3
C12B C 0.5835(10) 0.3873(7) 0.1128(3) 0.0453(19) Uani 0.353(4) 1 d P B 4
H12D H 0.5329 0.3632 0.0689 0.068 Uiso 0.353(4) 1 calc PR B 4
H12E H 0.4950 0.4444 0.1310 0.068 Uiso 0.353(4) 1 calc PR B 4
H12F H 0.5788 0.3191 0.1338 0.068 Uiso 0.353(4) 1 calc PR B 4
C13B C 0.9335(12) 0.3444(8) 0.0860(3) 0.054(2) Uani 0.353(4) 1 d P B 4
H13D H 0.9242 0.2730 0.1043 0.081 Uiso 0.353(4) 1 calc PR B 4
H13E H 1.0791 0.3767 0.0914 0.081 Uiso 0.353(4) 1 calc PR B 4
H13F H 0.8809 0.3263 0.0420 0.081 Uiso 0.353(4) 1 calc PR B 4
C14B C 0.8283(8) 0.5473(5) 0.0860(2) 0.0359(17) Uani 0.353(4) 1 d P B 4
H14C H 0.7857 0.5222 0.0412 0.043 Uiso 0.353(4) 1 calc PR B 4
H14D H 0.9787 0.5736 0.0921 0.043 Uiso 0.353(4) 1 calc PR B 4
C30 C 0.8119(4) 0.8786(2) 0.74832(11) 0.0587(7) Uiso 1 1 d . . .
C15 C 0.6962(5) 0.6600(2) 0.11021(12) 0.0588(7) Uiso 1 1 d . . .
C31A C 0.769(3) 0.899(2) 0.8235(5) 0.113(7) Uani 0.249(6) 1 d P A 5
H31A H 0.6319 0.9273 0.8267 0.170 Uiso 0.249(6) 1 calc PR A 5
H31B H 0.8768 0.9561 0.8479 0.170 Uiso 0.249(6) 1 calc PR A 5
H31C H 0.7750 0.8246 0.8391 0.170 Uiso 0.249(6) 1 calc PR A 5
C32A C 1.003(2) 0.8662(14) 0.7379(8) 0.101(5) Uiso 0.249(6) 1 d P A 5
H32A H 1.0725 0.8244 0.7687 0.152 Uiso 0.249(6) 1 calc PR A 5
H32B H 1.0781 0.9431 0.7406 0.152 Uiso 0.249(6) 1 calc PR A 5
H32C H 1.0032 0.8217 0.6966 0.152 Uiso 0.249(6) 1 calc PR A 5
C33A C 0.6518(15) 0.7829(7) 0.7160(4) 0.043(3) Uani 0.249(6) 1 d P A 5
H33A H 0.6756 0.7111 0.7327 0.064 Uiso 0.249(6) 1 calc PR A 5
H33B H 0.6632 0.7698 0.6717 0.064 Uiso 0.249(6) 1 calc PR A 5
H33C H 0.5123 0.8053 0.7223 0.064 Uiso 0.249(6) 1 calc PR A 5
C31B C 0.6638(13) 0.8526(6) 0.7859(4) 0.179(4) Uani 0.751(6) 1 d P A 6
H31D H 0.5285 0.8297 0.7607 0.268 Uiso 0.751(6) 1 calc PR A 6
H31E H 0.6528 0.9214 0.8165 0.268 Uiso 0.751(6) 1 calc PR A 6
H31F H 0.7060 0.7883 0.8071 0.268 Uiso 0.751(6) 1 calc PR A 6
C32B C 1.0311(7) 0.8645(6) 0.7810(2) 0.138(3) Uani 0.751(6) 1 d P A 6
H32D H 1.0911 0.9396 0.8049 0.206 Uiso 0.751(6) 1 calc PR A 6
H32E H 1.1210 0.8381 0.7500 0.206 Uiso 0.751(6) 1 calc PR A 6
H32F H 1.0199 0.8070 0.8086 0.206 Uiso 0.751(6) 1 calc PR A 6
C33B C 0.7901(7) 0.7812(3) 0.6889(2) 0.0757(15) Uani 0.751(6) 1 d P A 6
H33D H 0.8056 0.7049 0.7015 0.114 Uiso 0.751(6) 1 calc PR A 6
H33E H 0.8986 0.7980 0.6635 0.114 Uiso 0.751(6) 1 calc PR A 6
H33F H 0.6527 0.7806 0.6650 0.114 Uiso 0.751(6) 1 calc PR A 6
C16A C 0.765(2) 0.7162(14) 0.1783(7) 0.085(4) Uani 0.63(2) 1 d P B 11
H16A H 0.7591 0.8008 0.1824 0.127 Uiso 0.63(2) 1 calc PR B 11
H16B H 0.9073 0.6986 0.1911 0.127 Uiso 0.63(2) 1 calc PR B 11
H16C H 0.6708 0.6847 0.2044 0.127 Uiso 0.63(2) 1 calc PR B 11
C17A C 0.7971(12) 0.7243(13) 0.0585(3) 0.091(4) Uani 0.63(2) 1 d P B 11
H17A H 0.7390 0.6842 0.0172 0.137 Uiso 0.63(2) 1 calc PR B 11
H17B H 0.9486 0.7214 0.0640 0.137 Uiso 0.63(2) 1 calc PR B 11
H17C H 0.7641 0.8057 0.0633 0.137 Uiso 0.63(2) 1 calc PR B 11
C18A C 0.4695(11) 0.7105(10) 0.0985(4) 0.063(2) Uani 0.63(2) 1 d P B 11
H18A H 0.3961 0.6721 0.0585 0.095 Uiso 0.63(2) 1 calc PR B 11
H18B H 0.4884 0.7948 0.0987 0.095 Uiso 0.63(2) 1 calc PR B 11
H18C H 0.3875 0.6952 0.1313 0.095 Uiso 0.63(2) 1 calc PR B 11
C16B C 0.829(3) 0.724(2) 0.1687(10) 0.046(4) Uani 0.37(2) 1 d P B 12
H16D H 0.8035 0.8069 0.1742 0.069 Uiso 0.37(2) 1 calc PR B 12
H16E H 0.9763 0.7163 0.1652 0.069 Uiso 0.37(2) 1 calc PR B 12
H16F H 0.7912 0.6906 0.2043 0.069 Uiso 0.37(2) 1 calc PR B 12
C17B C 0.831(3) 0.6813(11) 0.0761(12) 0.109(6) Uani 0.37(2) 1 d P B 12
H17D H 0.7693 0.6631 0.0328 0.163 Uiso 0.37(2) 1 calc PR B 12
H17E H 0.9478 0.6334 0.0830 0.163 Uiso 0.37(2) 1 calc PR B 12
H17F H 0.8825 0.7640 0.0860 0.163 Uiso 0.37(2) 1 calc PR B 12
C18B C 0.5024(17) 0.650(2) 0.0997(8) 0.091(4) Uani 0.37(2) 1 d P B 12
H18D H 0.4528 0.7265 0.0952 0.136 Uiso 0.37(2) 1 calc PR B 12
H18E H 0.4446 0.6216 0.1341 0.136 Uiso 0.37(2) 1 calc PR B 12
H18F H 0.4574 0.5951 0.0616 0.136 Uiso 0.37(2) 1 calc PR B 12
C19 C 0.7022(3) 0.83124(15) 0.47230(8) 0.0313(4) Uani 1 1 d . C 12
H19A H 0.6513 0.8716 0.4379 0.038 Uiso 1 1 calc R C 12
H19B H 0.8532 0.8539 0.4837 0.038 Uiso 1 1 calc R C 12
C4 C 0.7715(3) 0.45510(17) 0.35005(8) 0.0340(5) Uani 1 1 d . D 12
H4A H 0.6202 0.4519 0.3361 0.041 Uiso 1 1 calc R D 12
H4B H 0.8020 0.3783 0.3612 0.041 Uiso 1 1 calc R D 12
C3 C 0.7505(3) 0.63572(16) 0.49893(8) 0.0306(4) Uani 1 1 d . C 12
H3A H 0.6628 0.6356 0.5326 0.037 Uiso 1 1 calc R C 12
H3B H 0.8955 0.6644 0.5166 0.037 Uiso 1 1 calc R C 12
C2 C 0.7393(3) 0.51708(16) 0.45963(8) 0.0325(4) Uani 1 1 d . C 12
H2A H 0.8244 0.4635 0.4804 0.039 Uiso 1 1 calc R C 12
H2B H 0.5939 0.4818 0.4490 0.039 Uiso 1 1 calc R C 12
C1 C 0.7570(3) 0.66148(16) 0.39612(9) 0.0344(5) Uani 1 1 d . C 12
H1A H 0.8763 0.7152 0.3911 0.041 Uiso 1 1 calc R C 12
H1B H 0.6514 0.6542 0.3593 0.041 Uiso 1 1 calc R C 12

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
O2 0.0254(8) 0.0402(8) 0.0436(9) -0.0005(7) 0.0031(6) 0.0012(6)
O1 0.0251(8) 0.0475(9) 0.0407(9) 0.0042(7) 0.0057(6) 0.0031(6)
N1 0.0271(9) 0.0292(9) 0.0333(9) 0.0059(7) 0.0061(7) 0.0004(7)
N2 0.0260(8) 0.0301(9) 0.0312(9) 0.0065(7) 0.0054(7) 0.0017(7)
C21 0.0252(10) 0.0300(10) 0.0374(11) 0.0053(9) -0.0013(8) 0.0031(8)
C6 0.0278(11) 0.0304(11) 0.0354(11) 0.0022(8) 0.0036(9) 0.0061(8)
C20 0.0253(10) 0.0272(10) 0.0355(11) 0.0097(8) 0.0040(8) 0.0040(8)
C5 0.0253(10) 0.0289(10) 0.0377(11) 0.0025(8) 0.0076(8) 0.0014(8)
C22 0.0215(10) 0.0371(11) 0.0440(12) 0.0061(9) 0.0052(9) 0.0032(8)
C7 0.0209(10) 0.0400(12) 0.0440(12) 0.0043(9) 0.0084(9) 0.0043(8)
C25 0.0254(10) 0.0268(10) 0.0395(11) 0.0109(9) 0.0039(8) 0.0025(8)
C10 0.0255(10) 0.0346(11) 0.0420(12) 0.0012(9) 0.0052(9) 0.0006(8)
C23 0.0295(11) 0.0339(11) 0.0389(11) 0.0071(9) 0.0088(9) 0.0085(9)
C8 0.0285(11) 0.0481(13) 0.0393(12) 0.0082(10) 0.0125(9) 0.0094(9)
C24 0.0281(10) 0.0256(10) 0.0356(11) 0.0079(8) 0.0042(8) 0.0049(8)
C9 0.0283(11) 0.0417(12) 0.0356(11) 0.0033(9) 0.0073(9) 0.0050(9)
C26 0.0302(11) 0.0320(11) 0.0339(11) 0.0043(9) 0.0032(8) 0.0022(8)
C11 0.0391(13) 0.0540(14) 0.0354(12) -0.0003(10) 0.0073(10) 0.0045(10)
C27A 0.046(2) 0.047(3) 0.048(3) -0.006(2) -0.003(2) 0.014(2)
C29A 0.033(2) 0.039(2) 0.037(2) 0.0049(16) 0.0055(16) 0.0000(16)
C28A 0.067(3) 0.032(2) 0.041(2) 0.0055(19) -0.002(2) -0.010(2)
C28B 0.040(3) 0.038(3) 0.038(3) 0.003(2) 0.000(2) -0.012(2)
C29B 0.023(2) 0.043(3) 0.043(3) 0.005(2) 0.005(2) 0.001(2)
C27B 0.052(3) 0.032(3) 0.048(4) 0.002(3) 0.001(3) 0.006(3)
C12A 0.067(3) 0.062(3) 0.043(2) -0.008(2) -0.003(2) -0.001(2)
C13A 0.048(2) 0.104(4) 0.037(2) -0.003(3) 0.0106(18) 0.017(3)
C14A 0.0302(19) 0.064(2) 0.0384(19) 0.0057(16) -0.0003(14) -0.0015(16)
C12B 0.039(4) 0.057(5) 0.037(4) 0.001(3) 0.007(3) -0.004(3)
C13B 0.064(5) 0.059(5) 0.037(4) -0.005(4) 0.012(3) 0.019(4)
C14B 0.025(3) 0.053(4) 0.030(3) 0.008(3) 0.006(2) 0.004(3)
C31A 0.115(14) 0.18(2) 0.030(7) -0.019(8) 0.021(7) -0.029(11)
C33A 0.040(6) 0.032(5) 0.061(7) 0.022(4) 0.006(5) 0.007(4)
C31B 0.194(9) 0.143(6) 0.207(9) -0.030(6) 0.158(8) -0.032(5)
C32B 0.067(3) 0.285(9) 0.066(3) 0.054(4) -0.013(2) 0.037(4)
C33B 0.071(3) 0.065(3) 0.105(3) 0.049(2) 0.012(2) 0.024(2)
C16A 0.079(9) 0.072(6) 0.087(9) -0.018(5) -0.031(5) 0.039(6)
C17A 0.061(4) 0.162(10) 0.065(4) 0.039(5) 0.030(3) 0.017(5)
C18A 0.042(3) 0.079(5) 0.068(3) 0.022(3) -0.012(2) 0.007(3)
C16B 0.062(10) 0.038(5) 0.035(5) -0.004(3) 0.006(6) 0.009(6)
C17B 0.116(12) 0.052(7) 0.177(18) 0.054(7) 0.048(12) 0.010(6)
C18B 0.047(6) 0.081(10) 0.143(10) 0.003(8) 0.019(6) 0.021(6)
C19 0.0287(11) 0.0315(11) 0.0341(11) 0.0068(8) 0.0048(8) 0.0011(8)
C4 0.0274(11) 0.0343(11) 0.0390(11) 0.0030(9) 0.0057(9) -0.0014(8)
C3 0.0265(10) 0.0330(11) 0.0344(11) 0.0102(9) 0.0065(8) 0.0019(8)
C2 0.0276(10) 0.0348(11) 0.0371(11) 0.0114(9) 0.0068(8) 0.0013(8)
C1 0.0369(12) 0.0330(11) 0.0345(11) 0.0075(9) 0.0066(9) 0.0040(9)

_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
O2 C21 1.375(2) . ?
O2 H2 0.841(3) . ?
O1 C6 1.370(2) . ?
O1 H1 0.842(3) . ?
N1 C2 1.470(2) . ?
N1 C4 1.473(2) . ?
N1 C1 1.483(2) . ?
N2 C3 1.471(2) . ?
N2 C19 1.472(2) . ?
N2 C1 1.475(2) . ?
C21 C22 1.380(3) . ?
C21 C20 1.405(3) . ?
C6 C7 1.384(3) . ?
C6 C5 1.404(3) . ?
C20 C25 1.392(3) . ?
C20 C19 1.509(3) . ?
C5 C10 1.398(3) . ?
C5 C4 1.510(3) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C7 C8 1.378(3) . ?
C7 H7 0.9500 . ?
C25 C24 1.398(3) . ?
C25 H25 0.9500 . ?
C10 C9 1.393(3) . ?
C10 H10 0.9500 . ?
C23 C24 1.396(3) . ?
C23 H23 0.9500 . ?
C8 C9 1.398(3) . ?
C8 H8 0.9500 . ?
C24 C26 1.533(3) . ?
C9 C11 1.538(3) . ?
C26 C28B 1.496(5) . ?
C26 C27A 1.514(4) . ?
C26 C29B 1.552(5) . ?
C26 C28A 1.559(5) . ?
C26 C29A 1.563(4) . ?
C26 C27B 1.568(5) . ?
C11 C12B 1.442(7) . ?
C11 C13A 1.483(4) . ?
C11 C14B 1.580(6) . ?
C11 C14A 1.581(4) . ?
C11 C12A 1.586(5) . ?
C11 C13B 1.621(7) . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C29A C30 1.562(4) . ?
C29A H29A 0.9900 . ?
C29A H29B 0.9900 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29B C30 1.641(5) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A C15 1.579(4) . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B C15 1.673(6) . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C30 C32A 1.304(15) . ?
C30 C31B 1.392(6) . ?
C30 C33A 1.502(9) . ?
C30 C32B 1.548(5) . ?
C30 C33B 1.586(5) . ?
C30 C31A 1.703(12) . ?
C15 C18B 1.246(11) . ?
C15 C17B 1.260(16) . ?
C15 C16B 1.53(3) . ?
C15 C16A 1.548(16) . ?
C15 C18A 1.629(9) . ?
C15 C17A 1.635(10) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C3 C2 1.509(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
C21 O2 H2 105.3(16) . . ?
C6 O1 H1 104.3(16) . . ?
C2 N1 C4 113.47(15) . . ?
C2 N1 C1 105.89(14) . . ?
C4 N1 C1 113.84(15) . . ?
C3 N2 C19 114.13(15) . . ?
C3 N2 C1 105.56(14) . . ?
C19 N2 C1 113.98(15) . . ?
O2 C21 C22 118.88(17) . . ?
O2 C21 C20 121.52(17) . . ?
C22 C21 C20 119.61(18) . . ?
O1 C6 C7 119.13(17) . . ?
O1 C6 C5 121.76(17) . . ?
C7 C6 C5 119.11(18) . . ?
C25 C20 C21 118.25(17) . . ?
C25 C20 C19 121.46(17) . . ?
C21 C20 C19 120.29(17) . . ?
C10 C5 C6 118.64(17) . . ?
C10 C5 C4 120.98(17) . . ?
C6 C5 C4 120.27(17) . . ?
C21 C22 C23 120.67(18) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C8 C7 C6 120.92(18) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C20 C25 C24 123.37(18) . . ?
C20 C25 H25 118.3 . . ?
C24 C25 H25 118.3 . . ?
C9 C10 C5 122.97(18) . . ?
C9 C10 H10 118.5 . . ?
C5 C10 H10 118.5 . . ?
C22 C23 C24 121.88(17) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C7 C8 C9 122.00(18) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C23 C24 C25 116.20(18) . . ?
C23 C24 C26 121.66(17) . . ?
C25 C24 C26 122.13(17) . . ?
C10 C9 C8 116.34(18) . . ?
C10 C9 C11 121.90(18) . . ?
C8 C9 C11 121.76(18) . . ?
C28B C26 C27A 128.6(3) . . ?
C28B C26 C24 113.3(2) . . ?
C27A C26 C24 113.7(2) . . ?
C28B C26 C29B 112.5(3) . . ?
C27A C26 C29B 67.5(3) . . ?
C24 C26 C29B 111.2(2) . . ?
C27A C26 C28A 106.2(3) . . ?
C24 C26 C28A 109.1(2) . . ?
C29B C26 C28A 138.0(3) . . ?
C28B C26 C29A 68.1(3) . . ?
C27A C26 C29A 112.3(3) . . ?
C24 C26 C29A 110.48(19) . . ?
C29B C26 C29A 49.8(2) . . ?
C28A C26 C29A 104.4(3) . . ?
C28B C26 C27B 107.6(3) . . ?
C24 C26 C27B 106.7(2) . . ?
C29B C26 C27B 105.2(3) . . ?
C28A C26 C27B 73.6(3) . . ?
C29A C26 C27B 141.0(3) . . ?
C12B C11 C13A 126.3(3) . . ?
C12B C11 C9 114.7(3) . . ?
C13A C11 C9 114.3(2) . . ?
C12B C11 C14B 115.2(4) . . ?
C13A C11 C14B 64.2(3) . . ?
C9 C11 C14B 110.6(3) . . ?
C12B C11 C14A 66.1(4) . . ?
C13A C11 C14A 113.7(3) . . ?
C9 C11 C14A 110.84(19) . . ?
C14B C11 C14A 55.7(2) . . ?
C13A C11 C12A 106.1(3) . . ?
C9 C11 C12A 108.3(2) . . ?
C14B C11 C12A 140.3(3) . . ?
C14A C11 C12A 102.7(3) . . ?
C12B C11 C13B 108.0(4) . . ?
C9 C11 C13B 104.0(3) . . ?
C14B C11 C13B 103.0(4) . . ?
C14A C11 C13B 143.8(3) . . ?
C12A C11 C13B 74.7(4) . . ?
C26 C27A H27A 109.5 . . ?
C26 C27A H27B 109.5 . . ?
C26 C27A H27C 109.5 . . ?
C30 C29A C26 122.2(3) . . ?
C30 C29A H29A 106.8 . . ?
C26 C29A H29A 106.8 . . ?
C30 C29A H29B 106.8 . . ?
C26 C29A H29B 106.8 . . ?
H29A C29A H29B 106.6 . . ?
C26 C28A H28A 109.5 . . ?
C26 C28A H28B 109.5 . . ?
C26 C28A H28C 109.5 . . ?
C26 C28B H28D 109.5 . . ?
C26 C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C26 C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C26 C29B C30 118.0(3) . . ?
C26 C29B H29C 107.8 . . ?
C30 C29B H29C 107.8 . . ?
C26 C29B H29D 107.8 . . ?
C30 C29B H29D 107.8 . . ?
H29C C29B H29D 107.2 . . ?
C26 C27B H27D 109.5 . . ?
C26 C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C26 C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C11 C12A H12A 109.5 . . ?
C11 C12A H12B 109.5 . . ?
C11 C12A H12C 109.5 . . ?
C11 C13A H13A 109.5 . . ?
C11 C13A H13B 109.5 . . ?
C11 C13A H13C 109.5 . . ?
C11 C14A C15 119.6(2) . . ?
C11 C14A H14A 107.4 . . ?
C15 C14A H14A 107.4 . . ?
C11 C14A H14B 107.4 . . ?
C15 C14A H14B 107.4 . . ?
H14A C14A H14B 107.0 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B H12E 109.5 . . ?
C11 C12B H12F 109.5 . . ?
C11 C13B H13D 109.5 . . ?
C11 C13B H13E 109.5 . . ?
C11 C13B H13F 109.5 . . ?
C11 C14B C15 114.2(3) . . ?
C11 C14B H14C 108.7 . . ?
C15 C14B H14C 108.7 . . ?
C11 C14B H14D 108.7 . . ?
C15 C14B H14D 108.7 . . ?
H14C C14B H14D 107.6 . . ?
C32A C30 C31B 144.0(9) . . ?
C32A C30 C33A 116.0(8) . . ?
C31B C30 C33A 68.2(5) . . ?
C31B C30 C32B 109.0(5) . . ?
C33A C30 C32B 127.0(5) . . ?
C32A C30 C29A 77.8(8) . . ?
C31B C30 C29A 131.9(4) . . ?
C33A C30 C29A 124.0(4) . . ?
C32B C30 C29A 97.7(3) . . ?
C32A C30 C33B 75.8(8) . . ?
C31B C30 C33B 109.7(4) . . ?
C32B C30 C33B 102.4(3) . . ?
C29A C30 C33B 102.2(2) . . ?
C32A C30 C29B 124.9(8) . . ?
C31B C30 C29B 84.3(4) . . ?
C33A C30 C29B 104.6(4) . . ?
C32B C30 C29B 128.2(4) . . ?
C29A C30 C29B 48.3(2) . . ?
C33B C30 C29B 120.1(3) . . ?
C32A C30 C31A 116.5(10) . . ?
C33A C30 C31A 105.4(7) . . ?
C32B C30 C31A 79.0(7) . . ?
C29A C30 C31A 115.8(8) . . ?
C33B C30 C31A 141.6(8) . . ?
C29B C30 C31A 84.1(8) . . ?
C18B C15 C17B 130.7(19) . . ?
C18B C15 C16B 126.4(9) . . ?
C17B C15 C16B 93.5(15) . . ?
C18B C15 C16A 109.2(8) . . ?
C17B C15 C16A 112.0(16) . . ?
C18B C15 C14A 73.7(11) . . ?
C17B C15 C14A 115.9(7) . . ?
C16B C15 C14A 117.4(9) . . ?
C16A C15 C14A 108.4(7) . . ?
C17B C15 C18A 118.8(11) . . ?
C16B C15 C18A 112.5(10) . . ?
C16A C15 C18A 100.1(7) . . ?
C14A C15 C18A 99.8(4) . . ?
C18B C15 C17A 110.7(13) . . ?
C16B C15 C17A 100.1(7) . . ?
C16A C15 C17A 116.1(7) . . ?
C14A C15 C17A 129.5(5) . . ?
C18A C15 C17A 94.9(5) . . ?
C18B C15 C14B 119.4(9) . . ?
C17B C15 C14B 64.8(6) . . ?
C16B C15 C14B 105.0(9) . . ?
C16A C15 C14B 114.0(6) . . ?
C14A C15 C14B 53.9(2) . . ?
C18A C15 C14B 141.6(4) . . ?
C17A C15 C14B 85.9(5) . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31B 109.5 . . ?
C30 C31A H31C 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C32A H32B 109.5 . . ?
C30 C32A H32C 109.5 . . ?
C30 C33A H33A 109.5 . . ?
C30 C33A H33B 109.5 . . ?
C30 C33A H33C 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
C30 C32B H32D 109.5 . . ?
C30 C32B H32E 109.5 . . ?
C30 C32B H32F 109.5 . . ?
C30 C33B H33D 109.5 . . ?
C30 C33B H33E 109.5 . . ?
C30 C33B H33F 109.5 . . ?
C15 C16A H16A 109.5 . . ?
C15 C16A H16B 109.5 . . ?
C15 C16A H16C 109.5 . . ?
C15 C17A H17A 109.5 . . ?
C15 C17A H17B 109.5 . . ?
C15 C17A H17C 109.5 . . ?
C15 C18A H18A 109.5 . . ?
C15 C18A H18B 109.5 . . ?
C15 C18A H18C 109.5 . . ?
C15 C16B H16D 109.5 . . ?
C15 C16B H16E 109.5 . . ?
C15 C16B H16F 109.5 . . ?
C15 C17B H17D 109.5 . . ?
C15 C17B H17E 109.5 . . ?
C15 C17B H17F 109.5 . . ?
C15 C18B H18D 109.5 . . ?
C15 C18B H18E 109.5 . . ?
C15 C18B H18F 109.5 . . ?
N2 C19 C20 109.88(15) . . ?
N2 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
N2 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
N1 C4 C5 111.95(16) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C3 C2 100.23(15) . . ?
N2 C3 H3A 111.7 . . ?
C2 C3 H3A 111.7 . . ?
N2 C3 H3B 111.7 . . ?
C2 C3 H3B 111.7 . . ?
H3A C3 H3B 109.5 . . ?
N1 C2 C3 101.52(15) . . ?
N1 C2 H2A 111.5 . . ?
C3 C2 H2A 111.5 . . ?
N1 C2 H2B 111.5 . . ?
C3 C2 H2B 111.5 . . ?
H2A C2 H2B 109.3 . . ?
N2 C1 N1 105.20(15) . . ?
N2 C1 H1A 110.7 . . ?
N1 C1 H1A 110.7 . . ?
N2 C1 H1B 110.7 . . ?
N1 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?

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
O1 H1 N1 0.842(3) 1.903(11) 2.679(2) 153(2) .
O2 H2 N2 0.841(3) 1.963(12) 2.718(2) 149(2) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.051