# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 182/1429

data_global
 
# 1. SUBMISSION DETAILS
 
_publ_contact_autor
;
        Wenqin Pang
        Department of Chemistry
        Jilin University
        Jiefang Road 119
        Changchun 130023
        China
;
_publ_contact_author_phone        ?
_publ_contact_author_fax          '86 431 5671974'
_publ_contact_author_email        zhaoyn@263.net
_publ_requested_journal           'chemical communications'
 
#=================================================================
 
# 2. TITLE AND AUTHOR LIST
 
_publ_section_title
;
 Synthesis and structures of two new 12-member ring 
crown-shaped oxovanadium borophosphate
;
 
loop_
 _publ_author_name
 _publ_author_address
     'Yongnan Zhao, Guangshan Zhu, Wang Liu, Yongcun Zou and Wenqin Pang'
;    Key Laboratory of Inorganic Synthesis and Preparative Chemistry, 
     Department of Chemitry, 
     Jilin University, 
     Jiefang Road 119
     Changchun, 130023, 
     China
;
     
 
#=======================================================================

 
# 3. TEXT
 
_publ_section_abstract
;
Two new oxovanadium borophosphates were hydrothermally synthesized,
 they are structurally
analogues and both constructed by 12-menber ring clusters with cations 
encpsulated in the
 rings respectively;an extended network of hydrogen bonds between anions, 
cations and crystal
water molecules links the structure in three dimensions.
;
_publ_section_comment
;
the vanadium atoms are all five coordinated to form square
 pyramids with one short vanadyl
bond. the phosphorous are coordinated by four oxygen atoms. 
the boron atoms are linked to 
four oxygen atoms.
;
_publ_section_experimental
;
 The compounds were synthesised using V2O5, NH4VO3, KCl, H3PO4, H3BO3 and 
triethylenetetraamine
under hydrothermal conditions.
;
_publ_section_references
;
;
 
_publ_section_figure_captions
;
Figure 1. The asymmetric unit of VBP-J1
Figure 2. The 12-member ring clusters of VBP-J1 and VBP-J2
;
_publ_section_acknowledgements
;
 The authors are grateful to the finacial support of the National Sience 
 Foundation
 of China and the Key Laboratory of Inorganic Synthesis and Preparative 
 Chemistry of
 Jilin University.
;
 
#=======================================================================

 
data_vbp-j1
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             vbp-j1 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C24 H120 B6 N17 O86 P12 V12' 
_chemical_formula_weight          3071.15 
 
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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'P'  'P'   0.1023   0.0942 
 '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            orthorhombic
_symmetry_space_group_name_H-M    Pbca
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x-1/2, y-1/2, z' 
 
_cell_length_a                    21.454(11) 
_cell_length_b                    16.315(6) 
_cell_length_c                    29.651(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      10378(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     190 
_cell_measurement_theta_min       1.67 
_cell_measurement_theta_max       23.3
 
_exptl_crystal_description        rhombic 
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.966 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              6228 
_exptl_absorpt_coefficient_mu     1.343 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.8130
_exptl_absorpt_correction_T_max   0.9333 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Bruker CCD area detector '
_diffrn_measurement_method        'phi and omega scans '
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             20909 
_diffrn_reflns_av_R_equivalents   0.0638 
_diffrn_reflns_av_sigmaI/netI     0.0942 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -32 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          1.67 
_diffrn_reflns_theta_max          23.23 
_reflns_number_total              6902 
_reflns_number_gt                 4099 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXP-97' 
_computing_publication_material   'SHELXTL'
 
_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^)+(0.1411P)^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      SHELXL 
_refine_ls_extinction_coef        0.00000(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          6902 
_refine_ls_number_parameters      784 
_refine_ls_number_restraints      60 
_refine_ls_R_factor_all           0.1014 
_refine_ls_R_factor_gt            0.0586 
_refine_ls_wR_factor_ref          0.1901 
_refine_ls_wR_factor_gt           0.1708 
_refine_ls_goodness_of_fit_ref    0.840 
_refine_ls_restrained_S_all       0.847 
_refine_ls_shift/su_max           4.765 
_refine_ls_shift/su_mean          0.152 
 
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 0.16195(7) 0.64034(10) 1.02204(5) 0.0269(4) Uani 1 1 d . . . 
V2 V 0.02492(7) 0.69374(10) 0.90126(5) 0.0303(4) Uani 1 1 d . . . 
V3 V 0.14801(7) 0.63375(10) 0.86270(5) 0.0279(4) Uani 1 1 d . . . 
V4 V -0.10331(8) 0.48327(11) 0.83879(7) 0.0279(8) Uani 1 1 d . . . 
V5 V 0.01499(7) 0.40216(10) 0.87457(5) 0.0289(7) Uani 1 1 d . . . 
V6 V 0.09764(7) 0.80585(10) 1.03715(5) 0.0285(4) Uani 1 1 d . . . 
P1 P 0.12248(11) 0.47117(17) 0.80961(8) 0.0305(7) Uani 1 1 d . . . 
P2 P 0.06044(11) 0.86944(16) 0.94052(8) 0.0293(6) Uani 1 1 d . . . 
P3 P -0.07077(12) 0.66634(16) 0.82042(8) 0.0306(6) Uani 1 1 d . . . 
P4 P 0.25143(11) 0.67016(16) 0.93577(7) 0.0271(6) Uani 1 1 d . . . 
P5 P -0.21792(12) 0.39801(19) 0.88102(8) 0.0408(8) Uani 1 1 d . . . 
P6 P 0.01934(13) 0.78897(17) 1.12534(8) 0.0376(7) Uani 1 1 d . . . 
O1 O 0.2364(3) 0.6338(4) 0.98184(18) 0.0299(15) Uani 1 1 d . . . 
O2 O 0.1359(3) 0.7391(4) 0.98935(17) 0.0277(15) Uani 1 1 d . . . 
O3 O -0.0129(2) 0.5022(3) 0.84472(18) 0.0260(15) Uani 1 1 d . . . 
O4 O -0.0755(3) 0.3879(4) 0.87402(18) 0.0280(15) Uani 1 1 d . . . 
O5 O 0.2257(3) 0.6137(4) 0.89799(19) 0.0333(16) Uani 1 1 d . . . 
O6 O 0.0582(3) 0.6136(4) 0.85775(18) 0.0263(15) Uani 1 1 d . . . 
O7 O 0.0915(3) 0.4026(4) 0.8371(2) 0.0436(18) Uani 1 1 d . . . 
O8 O -0.0065(3) 0.6477(4) 0.9437(2) 0.0434(18) Uani 1 1 d . . . 
O9 O -0.0432(3) 0.7177(4) 0.8584(2) 0.0392(17) Uani 1 1 d . . . 
O10 O 0.1646(3) 0.5214(4) 0.8407(2) 0.0414(18) Uani 1 1 d . . . 
O11 O 0.1470(3) 0.8722(4) 1.0545(2) 0.0418(18) Uani 1 1 d . . . 
O12 O 0.1567(3) 0.4369(4) 0.7703(2) 0.0439(18) Uani 1 1 d . . . 
O13 O 0.0242(3) 0.8196(4) 1.0767(2) 0.0444(18) Uani 1 1 d . . . 
O14 O 0.1296(3) 0.8448(4) 0.93284(18) 0.0274(15) Uani 1 1 d . . . 
O15 O 0.1158(3) 0.7019(4) 1.06796(18) 0.0288(15) Uani 1 1 d . . . 
O16 O 0.0854(3) 0.7570(4) 1.13989(19) 0.0370(17) Uani 1 1 d . . . 
O17 O -0.1851(3) 0.4780(4) 0.8689(2) 0.0438(18) Uani 1 1 d . . . 
O18 O 0.0697(3) 0.5290(4) 0.79169(18) 0.0302(15) Uani 1 1 d . . . 
O19 O 0.0453(3) 0.8611(4) 0.99119(19) 0.0351(16) Uani 1 1 d . . . 
O20 O 0.0184(3) 0.8114(4) 0.9134(2) 0.0377(17) Uani 1 1 d . . . 
O21 O -0.1159(3) 0.6031(4) 0.8387(2) 0.0402(17) Uani 1 1 d . . . 
O22 O 0.1195(3) 0.5632(4) 1.0104(2) 0.0436(18) Uani 1 1 d . . . 
O23 O 0.1672(3) 0.6933(4) 0.8230(2) 0.0464(19) Uani 1 1 d . . . 
O24 O 0.1153(2) 0.7009(4) 0.91176(18) 0.0262(15) Uani 1 1 d . . . 
O25 O 0.0520(3) 0.9567(4) 0.9243(2) 0.0383(17) Uani 1 1 d . . . 
O26 O 0.3199(3) 0.6842(4) 0.9301(2) 0.0366(17) Uani 1 1 d . . . 
O27 O -0.0005(4) 0.8541(4) 1.1574(2) 0.059(2) Uani 1 1 d . . . 
O28 O -0.1035(3) 0.7213(4) 0.7868(2) 0.0438(18) Uani 1 1 d . . . 
O29 O -0.1764(3) 0.3254(4) 0.8645(2) 0.0397(18) Uani 1 1 d . . . 
O30 O 0.2242(3) 0.6100(4) 1.0675(2) 0.0385(17) Uani 1 1 d . . . 
O31 O -0.0161(3) 0.6203(4) 0.79620(18) 0.0307(16) Uani 1 1 d . . . 
O32 O -0.1158(3) 0.4533(5) 0.7886(2) 0.057(2) Uani 1 1 d . . . 
O33 O 0.0263(3) 0.2829(4) 0.8722(3) 0.058(2) Uani 1 1 d . . . 
O34 O 0.2161(2) 0.7540(4) 0.93219(18) 0.0270(15) Uani 1 1 d . . . 
O35 O 0.0388(3) 0.4269(5) 0.9231(2) 0.051(2) Uani 1 1 d . . . 
O36 O -0.2797(3) 0.3921(6) 0.8580(2) 0.070(3) Uani 1 1 d . . . 
N1 N 1.1145(4) 1.1147(6) 0.1880(3) 0.065(3) Uani 1 1 d . . . 
H1A H 1.1030 1.1667 0.1912 0.080 Uiso 1 1 calc R . . 
H1B H 1.1506 1.1124 0.1732 0.080 Uiso 1 1 calc R . . 
H1C H 1.1190 1.0918 0.2151 0.080 Uiso 1 1 calc R . . 
N2 N 0.9640(5) 1.0115(7) 0.1627(3) 0.078(3) Uani 1 1 d . . . 
H2A H 0.9605 1.0310 0.1344 0.080 Uiso 1 1 calc R . . 
H2B H 0.9802 0.9607 0.1611 0.080 Uiso 1 1 calc R . . 
N3 N 0.8065(6) 0.9326(10) 0.1718(4) 0.128(6) Uani 1 1 d . . . 
H3A H 0.7799 0.9153 0.1503 0.080 Uiso 1 1 calc R . . 
H3B H 0.7901 0.9788 0.1835 0.080 Uiso 1 1 calc R . . 
N4 N 0.8869(6) 0.7645(8) 0.1973(4) 0.099(4) Uani 1 1 d . . . 
H4A H 0.9136 0.7961 0.1822 0.080 Uiso 1 1 calc R . . 
H4B H 0.8924 0.7125 0.1893 0.080 Uiso 1 1 calc R . . 
H4C H 0.8936 0.7698 0.2268 0.080 Uiso 1 1 calc R . . 
N5 N 0.0806(4) 0.4056(5) 0.4717(3) 0.044(2) Uani 1 1 d . . . 
H5A H 0.1067 0.3748 0.4558 0.080 Uiso 1 1 calc R . . 
H5B H 0.0683 0.4482 0.4552 0.080 Uiso 1 1 calc R . . 
H5C H 0.0475 0.3759 0.4795 0.080 Uiso 1 1 calc R . . 
N6 N 0.1601(4) 0.3033(5) 0.5358(3) 0.043(2) Uani 1 1 d . . . 
H6A H 0.1453 0.2803 0.5104 0.080 Uiso 1 1 calc R . . 
H6B H 0.1985 0.3228 0.5298 0.080 Uiso 1 1 calc R . . 
N7' N 0.1789(11) 0.1278(14) 0.5171(5) 0.076(8) Uani 0.05 1 d . . . 
H7'1 H 0.1477 0.0941 0.5255 0.080 Uiso 05 1 calc R . . 
H7'2 H 0.1623 0.1661 0.4988 0.080 Uiso 05 1 calc R . . 
N7 N 0.2234(16) 0.1650(17) 0.5164(8) 0.023(10) Uani 0.05 1 d . . . 
H7A H 0.2634 0.1818 0.5173 0.080 Uiso 0.05 1 calc R . . 
H7B H 0.2022 0.2015 0.4996 0.080 Uiso 0.05 1 calc R . . 
N8 N 0.1745(5) 0.1316(6) 0.4231(3) 0.072(3) Uani 1 1 d . . . 
H8A H 0.1525 0.1654 0.4404 0.080 Uiso 1 1 calc R . . 
H8B H 0.1511 0.1149 0.4001 0.080 Uiso 1 1 calc R . . 
H8C H 0.2079 0.1577 0.4126 0.080 Uiso 1 1 calc R . . 
N9 N 0.0000 0.5000 0.0000 0.056(4) Uani 1 2 d SD . . 
C1 C 1.0679(5) 1.0713(8) 0.1631(4) 0.067(4) Uani 1 1 d . . . 
H1D H 1.0825 1.0163 0.1566 0.080 Uiso 1 1 calc R . . 
H1E H 1.0603 1.0989 0.1347 0.080 Uiso 1 1 calc R . . 
C2 C 1.0079(6) 1.0665(9) 0.1896(4) 0.076(4) Uani 1 1 d . . . 
H2C H 0.9899 1.1207 0.1932 0.080 Uiso 1 1 calc R . . 
H2D H 1.0154 1.0435 0.2193 0.080 Uiso 1 1 calc R . . 
C3 C 0.9019(7) 1.0076(15) 0.1834(6) 0.161(10) Uani 1 1 d . . . 
H3C H 0.8846 1.0622 0.1868 0.080 Uiso 1 1 calc R . . 
H3D H 0.9043 0.9822 0.2130 0.080 Uiso 1 1 calc R . . 
C4 C 0.8601(8) 0.9542(16) 0.1506(5) 0.180(12) Uani 1 1 d . . . 
H4D H 0.8504 0.9856 0.1236 0.080 Uiso 1 1 calc R . . 
H4E H 0.8826 0.9054 0.1415 0.080 Uiso 1 1 calc R . . 
C5 C 0.8060(9) 0.8704(11) 0.2080(6) 0.118(6) Uani 1 1 d . . . 
H5D H 0.7645 0.8660 0.2210 0.080 Uiso 1 1 calc R . . 
H5E H 0.8348 0.8857 0.2318 0.080 Uiso 1 1 calc R . . 
C6 C 0.8254(7) 0.7887(12) 0.1872(5) 0.099(5) Uani 1 1 d . . . 
H6C H 0.7970 0.7465 0.1976 0.080 Uiso 1 1 calc R . . 
H6D H 0.8210 0.7926 0.1547 0.080 Uiso 1 1 calc R . . 
C7 C 0.1124(5) 0.4355(7) 0.5129(4) 0.050(3) Uani 1 1 d . . . 
H7C H 0.0893 0.4818 0.5248 0.080 Uiso 1 1 calc R . . 
H7D H 0.1536 0.4550 0.5046 0.080 Uiso 1 1 calc R . . 
C8 C 0.1189(5) 0.3726(7) 0.5490(3) 0.048(3) Uani 1 1 d . . . 
H8D H 0.1356 0.3984 0.5759 0.080 Uiso 1 1 calc R . . 
H8E H 0.0779 0.3513 0.5564 0.080 Uiso 1 1 calc R . . 
C9 C 0.1648(5) 0.2399(7) 0.5712(3) 0.053(3) Uani 1 1 d . . . 
H9A H 0.1842 0.2635 0.5978 0.080 Uiso 1 1 calc R . . 
H9B H 0.1232 0.2221 0.5795 0.080 Uiso 1 1 calc R . . 
C10 C 0.2019(9) 0.1673(12) 0.5561(5) 0.107(6) Uani 1 1 d . . . 
H10A H 0.2452 0.1971 0.5553 0.080 Uiso 1 1 d . . . 
H10B H 0.2038 0.1353 0.5818 0.080 Uiso 1 1 d . . . 
C11 C 0.2214(8) 0.0826(9) 0.4924(6) 0.094(5) Uani 1 1 d . . . 
H11A H 0.2637 0.1044 0.4824 0.080 Uiso 1 1 d . . . 
H11B H 0.2304 0.0294 0.5044 0.080 Uiso 1 1 d . . . 
C12 C 0.1937(7) 0.0627(8) 0.4489(5) 0.086(5) Uani 1 1 d . . . 
H12A H 0.2237 0.0316 0.4314 0.080 Uiso 1 1 calc R . . 
H12B H 0.1578 0.0278 0.4539 0.080 Uiso 1 1 calc R . . 
B1 B 0.0242(5) 0.5657(7) 0.8239(3) 0.029(3) Uani 1 1 d . . . 
B2 B 0.1481(5) 0.7580(7) 0.9427(3) 0.026(3) Uani 1 1 d . . . 
B3 B -0.1126(5) 0.3148(8) 0.8842(4) 0.035(3) Uani 1 1 d . . . 
OW6 O 0.1992(13) 0.9081(14) 0.1491(7) 0.150(10) Uani 1 1 d DU . . 
OW5 O 0.2295(13) 0.533(2) 0.2543(12) 0.52(3) Uani 1 1 d DU . . 
OW4 O 0.2158(13) 0.6254(14) 0.3525(8) 0.147(8) Uani 1 1 d DU . . 
OW3 O 0.2370(11) 0.2676(15) 0.1944(8) 0.138(8) Uani 1 1 d DU . . 
OW2 O 0.1011(9) 0.8759(19) 0.2170(6) 0.405(15) Uani 1 1 d DU . . 
OW1 O 0.0670(4) 0.2223(6) 0.4810(3) 0.061(2) Uani 1 1 d DU . . 
OW7 O 0.1468(17) 0.7228(16) 0.2353(7) 0.074(9) Uani 0.50 1 d PDU . . 
H5WA H 0.218(9) 0.581(6) 0.266(6) 0.080 Uiso 1 1 d D . . 
H5WB H 0.216(6) 0.481(3) 0.254(4) 0.080 Uiso 1 1 d D . . 
H6WA H 0.229(4) 0.896(8) 0.171(3) 0.080 Uiso 1 1 d D . . 
H6WB H 0.183(6) 0.949(7) 0.133(4) 0.080 Uiso 1 1 d D . . 
H2WA H 0.141(3) 0.856(7) 0.219(4) 0.080 Uiso 1 1 d D . . 
H2WB H 0.079(4) 0.909(7) 0.198(3) 0.080 Uiso 1 1 d D . . 
H1WB H 0.052(5) 0.202(7) 0.507(2) 0.080 Uiso 1 1 d D . . 
H1WA H 0.031(3) 0.221(8) 0.466(4) 0.080 Uiso 1 1 d D . . 
H4WB H 0.233(6) 0.637(8) 0.325(2) 0.080 Uiso 1 1 d D . . 
H4WA H 0.208(7) 0.573(4) 0.362(4) 0.080 Uiso 1 1 d D . . 
H9C H 0.015(6) 0.546(4) -0.018(4) 0.080 Uiso 1 1 d D . . 
H9D H 0.017(6) 0.457(6) 0.022(3) 0.080 Uiso 1 1 d D . . 
H3WA H 0.197(2) 0.282(8) 0.198(4) 0.080 Uiso 1 1 d D . . 
H3WB H 0.234(8) 0.323(3) 0.188(5) 0.080 Uiso 1 1 d D . . 
H7WB H 0.109(3) 0.708(7) 0.248(4) 0.080 Uiso 1 1 d D . . 
H7WA H 0.185(3) 0.742(7) 0.228(4) 0.080 Uiso 1 1 d 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 0.0239(9) 0.0245(11) 0.0322(8) 0.0037(7) -0.0010(6) -0.0012(8) 
V2 0.0263(9) 0.0328(12) 0.0318(9) -0.0029(7) 0.0001(7) 0.0019(8) 
V3 0.0236(9) 0.0313(11) 0.0287(8) -0.0041(7) 0.0017(6) -0.0013(7) 
V4 0.0236(10) 0.0320(14) 0.0282(15) 0.0075(9) -0.0038(8) -0.0022(9) 
V5 0.0256(10) 0.0264(13) 0.0346(10) 0.0015(7) 0.0001(7) 0.0014(8) 
V6 0.0298(9) 0.0282(11) 0.0275(8) 0.0000(7) -0.0006(7) 0.0005(8) 
P1 0.0314(14) 0.0311(18) 0.0289(13) -0.0076(12) 0.0044(11) -0.0021(12) 
P2 0.0342(15) 0.0246(18) 0.0290(13) 0.0001(11) -0.0040(10) 0.0049(12) 
P3 0.0325(14) 0.0258(18) 0.0334(13) 0.0045(11) -0.0080(11) 0.0021(12) 
P4 0.0226(13) 0.0279(17) 0.0307(13) -0.0014(11) -0.0008(10) 0.0004(11) 
P5 0.0232(14) 0.057(2) 0.0416(15) 0.0175(14) -0.0050(11) -0.0041(14) 
P6 0.0481(17) 0.0280(18) 0.0366(14) -0.0013(12) 0.0134(12) 0.0007(14) 
O1 0.030(4) 0.027(4) 0.032(3) 0.003(3) 0.002(3) 0.006(3) 
O2 0.029(3) 0.029(4) 0.025(3) -0.002(3) -0.002(3) 0.007(3) 
O3 0.023(3) 0.023(4) 0.033(3) 0.001(3) -0.002(3) -0.001(3) 
O4 0.032(4) 0.018(4) 0.034(3) 0.003(3) 0.003(3) -0.004(3) 
O5 0.026(3) 0.034(4) 0.040(4) -0.009(3) -0.005(3) 0.004(3) 
O6 0.023(3) 0.029(4) 0.027(3) -0.007(3) 0.000(2) -0.002(3) 
O7 0.033(4) 0.032(5) 0.065(5) 0.004(4) 0.019(3) 0.005(3) 
O8 0.036(4) 0.051(5) 0.043(4) 0.003(3) 0.007(3) 0.006(4) 
O9 0.035(4) 0.044(5) 0.038(4) -0.010(3) -0.014(3) 0.008(3) 
O10 0.026(4) 0.047(5) 0.051(4) -0.018(4) -0.003(3) 0.012(3) 
O11 0.041(4) 0.031(5) 0.053(4) -0.003(3) -0.004(3) -0.001(3) 
O12 0.037(4) 0.050(5) 0.044(4) -0.014(3) 0.008(3) 0.005(4) 
O13 0.041(4) 0.055(5) 0.037(4) 0.005(3) 0.010(3) 0.015(4) 
O14 0.033(4) 0.021(4) 0.029(3) 0.001(3) -0.001(3) 0.000(3) 
O15 0.032(4) 0.028(4) 0.027(3) 0.004(3) 0.000(3) 0.000(3) 
O16 0.059(5) 0.026(4) 0.026(3) -0.001(3) 0.000(3) -0.009(3) 
O17 0.028(4) 0.034(5) 0.070(5) 0.022(4) 0.007(3) 0.004(3) 
O18 0.031(4) 0.033(4) 0.027(3) -0.001(3) 0.003(3) 0.000(3) 
O19 0.040(4) 0.031(4) 0.034(4) 0.001(3) 0.002(3) 0.013(3) 
O20 0.036(4) 0.027(4) 0.050(4) -0.010(3) -0.009(3) 0.010(3) 
O21 0.029(4) 0.029(4) 0.063(4) 0.011(3) 0.003(3) 0.005(3) 
O22 0.033(4) 0.030(5) 0.068(5) -0.006(4) 0.000(3) -0.003(3) 
O23 0.043(4) 0.064(5) 0.032(4) 0.007(3) 0.006(3) -0.011(4) 
O24 0.024(3) 0.024(4) 0.031(3) -0.004(3) 0.000(3) 0.001(3) 
O25 0.046(4) 0.024(5) 0.044(4) -0.002(3) -0.007(3) 0.010(3) 
O26 0.025(4) 0.040(5) 0.046(4) -0.001(3) 0.000(3) -0.003(3) 
O27 0.093(6) 0.037(5) 0.048(4) -0.009(4) 0.011(4) 0.006(4) 
O28 0.058(5) 0.033(5) 0.041(4) 0.005(3) -0.011(3) 0.012(4) 
O29 0.033(4) 0.050(5) 0.036(4) 0.005(3) -0.006(3) -0.017(4) 
O30 0.021(3) 0.049(5) 0.046(4) 0.015(3) -0.001(3) -0.001(3) 
O31 0.030(4) 0.033(4) 0.029(3) 0.002(3) -0.001(3) 0.004(3) 
O32 0.054(5) 0.075(6) 0.043(4) -0.001(4) -0.014(3) -0.015(4) 
O33 0.039(4) 0.026(5) 0.110(6) 0.011(4) 0.011(4) -0.002(4) 
O34 0.023(3) 0.018(4) 0.039(3) 0.002(3) 0.001(3) -0.002(3) 
O35 0.052(5) 0.061(6) 0.041(4) 0.000(4) -0.010(3) 0.016(4) 
O36 0.031(4) 0.121(8) 0.057(5) 0.026(5) -0.015(4) -0.014(5) 
N1 0.069(7) 0.073(8) 0.051(6) 0.003(5) 0.004(5) 0.005(6) 
N2 0.094(8) 0.093(9) 0.047(6) 0.004(6) -0.002(6) 0.000(7) 
N3 0.098(11) 0.200(18) 0.087(10) -0.022(11) -0.011(9) -0.037(11) 
N4 0.111(11) 0.126(12) 0.059(7) -0.022(7) 0.002(7) 0.020(9) 
N5 0.045(5) 0.022(5) 0.064(6) 0.006(4) 0.001(4) -0.002(4) 
N6 0.032(5) 0.051(6) 0.047(5) 0.002(5) 0.005(4) 0.000(5) 
N7' 0.073(17) 0.096(16) 0.058(11) 0.005(10) -0.001(9) 0.014(14) 
N7 0.03(2) 0.000(18) 0.044(17) 0.003(12) 0.007(12) 0.004(13) 
N8 0.062(7) 0.083(9) 0.072(7) 0.000(6) -0.019(6) -0.019(6) 
N9 0.068(10) 0.037(10) 0.064(9) 0.023(7) -0.002(7) -0.006(8) 
C1 0.047(7) 0.092(11) 0.061(8) 0.004(7) -0.005(6) -0.008(7) 
C2 0.073(9) 0.093(12) 0.060(8) -0.011(7) 0.001(7) -0.018(8) 
C3 0.079(12) 0.31(3) 0.091(12) -0.094(15) 0.024(10) -0.057(15) 
C4 0.074(12) 0.41(4) 0.056(10) -0.028(16) 0.018(8) -0.073(18) 
C5 0.112(15) 0.120(17) 0.120(15) 0.013(13) -0.026(12) -0.024(13) 
C6 0.085(12) 0.132(17) 0.078(10) -0.007(10) -0.027(9) 0.010(11) 
C7 0.042(7) 0.045(8) 0.065(7) -0.011(6) 0.000(5) -0.006(6) 
C8 0.036(6) 0.059(9) 0.048(7) -0.014(6) -0.001(5) 0.007(6) 
C9 0.052(7) 0.072(9) 0.035(6) 0.006(6) 0.005(5) -0.018(7) 
C10 0.126(14) 0.126(16) 0.068(10) 0.049(10) 0.019(11) 0.047(12) 
C11 0.109(14) 0.041(11) 0.133(15) 0.028(10) -0.047(12) -0.019(9) 
C12 0.106(12) 0.041(10) 0.112(12) 0.027(9) 0.001(10) 0.011(8) 
B1 0.026(6) 0.036(8) 0.024(5) -0.004(5) -0.003(4) -0.006(5) 
B2 0.025(6) 0.027(8) 0.027(5) -0.003(5) -0.001(4) -0.006(5) 
B3 0.039(7) 0.029(9) 0.037(6) 0.006(5) -0.003(5) 0.002(6) 
OW6 0.23(3) 0.12(2) 0.105(17) -0.037(13) 0.037(15) -0.11(2) 
OW5 0.117(17) 1.02(6) 0.43(4) 0.030(5)  0.020(2) 0.028(4) 
OW4 0.20(2) 0.108(17) 0.129(17) -0.043(16) 0.020(17) 0.025(19) 
OW3 0.113(15) 0.17(2) 0.130(16) -0.049(16) -0.010(13) 0.089(16) 
OW2 0.027(2) 0.069(4) 0.0259(18) 0.034(2) 0.0158(15) 0.026(2) 
OW1 0.059(5) 0.072(6) 0.050(5) 0.000(4) -0.005(4) -0.012(5) 
OW7 0.15(3) 0.047(18) 0.029(12) -0.025(11) -0.003(14) -0.032(19) 
 
_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 O22 1.591(7) . ? 
V1 O15 1.960(6) . ? 
V1 O30 1.962(6) . ? 
V1 O2 1.961(6) . ? 
V1 O1 1.996(6) . ? 
V2 O8 1.614(6) . ? 
V2 O20 1.959(6) . ? 
V2 O6 1.971(6) . ? 
V2 O24 1.968(6) . ? 
V2 O9 1.976(6) . ? 
V3 O23 1.582(6) . ? 
V3 O24 1.952(6) . ? 
V3 O6 1.960(6) . ? 
V3 O10 1.979(6) . ? 
V3 O5 1.995(6) . ? 
V4 O32 1.589(7) . ? 
V4 O4 1.967(6) . ? 
V4 O3 1.972(6) . ? 
V4 O21 1.974(7) . ? 
V4 O17 1.972(6) . ? 
V5 O35 1.579(7) . ? 
V5 O3 1.951(6) . ? 
V5 O4 1.956(6) . ? 
V5 O33 1.962(7) . ? 
V5 O7 1.983(6) . ? 
V6 O11 1.599(7) . ? 
V6 O15 1.966(6) . ? 
V6 O2 1.967(6) . ? 
V6 O13 1.978(6) . ? 
V6 O19 1.983(6) . ? 
P1 O12 1.486(6) . ? 
P1 O10 1.528(7) . ? 
P1 O7 1.535(7) . ? 
P1 O18 1.566(6) . ? 
P2 O25 1.514(7) . ? 
P2 O20 1.534(7) . ? 
P2 O19 1.543(6) . ? 
P2 O14 1.554(6) . ? 
P3 O21 1.514(7) . ? 
P3 O9 1.522(6) . ? 
P3 O28 1.514(6) . ? 
P3 O31 1.567(6) . ? 
P4 O26 1.496(6) . ? 
P4 O1 1.524(6) . ? 
P4 O5 1.552(6) . ? 
P4 O34 1.567(6) . ? 
P5 O36 1.494(7) . ? 
P5 O17 1.525(7) . ? 
P5 O30 1.537(6) 5_567 ? 
P5 O29 1.561(7) . ? 
P6 O27 1.488(7) . ? 
P6 O33 1.529(7) 5_567 ? 
P6 O13 1.529(7) . ? 
P6 O16 1.570(7) . ? 
O2 B2 1.441(11) . ? 
O3 B1 1.447(12) . ? 
O4 B3 1.465(13) . ? 
O6 B1 1.466(11) . ? 
O14 B2 1.499(12) . ? 
O15 B3 1.446(12) 5_567 ? 
O16 B3 1.490(13) 5_567 ? 
O18 B1 1.490(12) . ? 
O24 B2 1.485(11) . ? 
O29 B3 1.496(12) . ? 
O30 P5 1.537(6) 5_567 ? 
O31 B1 1.488(12) . ? 
O33 P6 1.529(7) 5_567 ? 
O34 B2 1.493(11) . ? 
N1 C1 1.430(14) . ? 
N1 H1A 0.8900 . ? 
N1 H1B 0.8900 . ? 
N1 H1C 0.8900 . ? 
N2 C3 1.469(16) . ? 
N2 C2 1.526(15) . ? 
N2 H2A 0.9000 . ? 
N2 H2B 0.9000 . ? 
N3 C4 1.357(17) . ? 
N3 C5 1.479(18) . ? 
N3 H3A 0.9000 . ? 
N3 H3B 0.9000 . ? 
N4 C6 1.411(16) . ? 
N4 H4A 0.8900 . ? 
N4 H4B 0.8900 . ? 
N4 H4C 0.8900 . ? 
N5 C7 1.481(12) . ? 
N5 H5A 0.8900 . ? 
N5 H5B 0.8900 . ? 
N5 H5C 0.8900 . ? 
N6 C9 1.478(13) . ? 
N6 C8 1.489(12) . ? 
N6 H6A 0.9000 . ? 
N6 H6B 0.9000 . ? 
N7' C11 1.38(2) . ? 
N7' C10 1.41(2) . ? 
N7' H7'1 0.9000 . ? 
N7' H7'2 0.9000 . ? 
N7 C10 1.26(3) . ? 
N7 C11 1.52(3) . ? 
N7 H7A 0.9000 . ? 
N7 H7B 0.9000 . ? 
N7 H10A 1.35(3) . ? 
N8 C12 1.420(14) . ? 
N8 H8A 0.8900 . ? 
N8 H8B 0.8900 . ? 
N8 H8C 0.8900 . ? 
N9 H9C 0.98(3) . ? 
N9 H9D 1.02(5) . ? 
C1 C2 1.509(15) . ? 
C1 H1D 0.9700 . ? 
C1 H1E 0.9700 . ? 
C2 H2C 0.9700 . ? 
C2 H2D 0.9700 . ? 
C3 C4 1.59(2) . ? 
C3 H3C 0.9700 . ? 
C3 H3D 0.9700 . ? 
C4 H4D 0.9700 . ? 
C4 H4E 0.9700 . ? 
C5 C6 1.53(2) . ? 
C5 H5D 0.9700 . ? 
C5 H5E 0.9700 . ? 
C6 H6C 0.9700 . ? 
C6 H6D 0.9700 . ? 
C7 C8 1.490(14) . ? 
C7 H7C 0.9700 . ? 
C7 H7D 0.9700 . ? 
C8 H8D 0.9700 . ? 
C8 H8E 0.9700 . ? 
C9 C10 1.497(19) . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C10 H10A 1.05(2) . ? 
C10 H10B 0.924(13) . ? 
C11 C12 1.456(19) . ? 
C11 H11A 1.020(18) . ? 
C11 H11B 0.958(14) . ? 
C12 H12A 0.9700 . ? 
C12 H12B 0.9700 . ? 
B3 O15 1.446(12) 5_567 ? 
B3 O16 1.490(13) 5_567 ? 
OW6 H6WA 0.94(3) . ? 
OW6 H6WB 0.90(2) . ? 
OW5 H5WA 0.90(4) . ? 
OW5 H5WB 0.90(2) . ? 
OW4 H4WB 0.90(2) . ? 
OW4 H4WA 0.91(2) . ? 
OW3 H3WA 0.89(2) . ? 
OW3 H3WB 0.93(3) . ? 
OW2 H2WA 0.91(2) . ? 
OW2 H2WB 0.92(3) . ? 
OW1 H1WB 0.90(2) . ? 
OW1 H1WA 0.89(2) . ? 
OW7 H7WB 0.93(3) . ? 
OW7 H7WA 0.91(3) . ? 
 
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 
O22 V1 O15 105.5(3) . . ? 
O22 V1 O30 109.8(3) . . ? 
O15 V1 O30 89.7(3) . . ? 
O22 V1 O2 112.3(3) . . ? 
O15 V1 O2 77.2(2) . . ? 
O30 V1 O2 137.8(3) . . ? 
O22 V1 O1 106.6(3) . . ? 
O15 V1 O1 147.8(3) . . ? 
O30 V1 O1 81.5(2) . . ? 
O2 V1 O1 88.7(2) . . ? 
O8 V2 O20 106.4(3) . . ? 
O8 V2 O6 110.7(3) . . ? 
O20 V2 O6 142.8(3) . . ? 
O8 V2 O24 108.4(3) . . ? 
O20 V2 O24 89.0(3) . . ? 
O6 V2 O24 77.7(2) . . ? 
O8 V2 O9 106.6(3) . . ? 
O20 V2 O9 82.7(3) . . ? 
O6 V2 O9 88.7(2) . . ? 
O24 V2 O9 145.0(3) . . ? 
O23 V3 O24 107.7(3) . . ? 
O23 V3 O6 107.7(3) . . ? 
O24 V3 O6 78.3(2) . . ? 
O23 V3 O10 106.1(3) . . ? 
O24 V3 O10 146.2(3) . . ? 
O6 V3 O10 89.8(3) . . ? 
O23 V3 O5 105.9(3) . . ? 
O24 V3 O5 90.1(2) . . ? 
O6 V3 O5 146.4(3) . . ? 
O10 V3 O5 82.6(2) . . ? 
O32 V4 O4 107.7(3) . . ? 
O32 V4 O3 107.3(3) . . ? 
O4 V4 O3 77.2(2) . . ? 
O32 V4 O21 106.3(4) . . ? 
O4 V4 O21 145.7(3) . . ? 
O3 V4 O21 88.8(3) . . ? 
O32 V4 O17 105.1(3) . . ? 
O4 V4 O17 89.7(3) . . ? 
O3 V4 O17 147.4(3) . . ? 
O21 V4 O17 85.6(3) . . ? 
O35 V5 O3 107.4(3) . . ? 
O35 V5 O4 111.0(3) . . ? 
O3 V5 O4 78.0(2) . . ? 
O35 V5 O33 104.2(4) . . ? 
O3 V5 O33 148.4(3) . . ? 
O4 V5 O33 90.2(3) . . ? 
O35 V5 O7 104.0(3) . . ? 
O3 V5 O7 89.8(3) . . ? 
O4 V5 O7 144.9(3) . . ? 
O33 V5 O7 83.2(3) . . ? 
O11 V6 O15 107.6(3) . . ? 
O11 V6 O2 109.3(3) . . ? 
O15 V6 O2 77.0(2) . . ? 
O11 V6 O13 105.0(3) . . ? 
O15 V6 O13 88.9(3) . . ? 
O2 V6 O13 145.4(3) . . ? 
O11 V6 O19 106.8(3) . . ? 
O15 V6 O19 145.5(3) . . ? 
O2 V6 O19 89.6(2) . . ? 
O13 V6 O19 84.5(3) . . ? 
O12 P1 O10 112.4(4) . . ? 
O12 P1 O7 110.9(4) . . ? 
O10 P1 O7 109.0(4) . . ? 
O12 P1 O18 108.6(4) . . ? 
O10 P1 O18 108.0(4) . . ? 
O7 P1 O18 107.9(4) . . ? 
O25 P2 O20 110.1(4) . . ? 
O25 P2 O19 111.5(4) . . ? 
O20 P2 O19 109.4(4) . . ? 
O25 P2 O14 108.1(4) . . ? 
O20 P2 O14 108.9(3) . . ? 
O19 P2 O14 108.8(3) . . ? 
O21 P3 O9 111.1(4) . . ? 
O21 P3 O28 110.0(4) . . ? 
O9 P3 O28 110.0(4) . . ? 
O21 P3 O31 108.4(4) . . ? 
O9 P3 O31 108.1(4) . . ? 
O28 P3 O31 109.2(4) . . ? 
O26 P4 O1 111.5(3) . . ? 
O26 P4 O5 111.0(3) . . ? 
O1 P4 O5 109.9(4) . . ? 
O26 P4 O34 109.5(4) . . ? 
O1 P4 O34 107.4(3) . . ? 
O5 P4 O34 107.3(3) . . ? 
O36 P5 O17 110.9(4) . . ? 
O36 P5 O30 111.7(4) . 5_567 ? 
O17 P5 O30 110.3(4) . 5_567 ? 
O36 P5 O29 108.4(4) . . ? 
O17 P5 O29 108.2(4) . . ? 
O30 P5 O29 107.2(4) 5_567 . ? 
O27 P6 O33 109.5(4) . 5_567 ? 
O27 P6 O13 112.8(4) . . ? 
O33 P6 O13 109.8(4) 5_567 . ? 
O27 P6 O16 108.7(4) . . ? 
O33 P6 O16 108.0(4) 5_567 . ? 
O13 P6 O16 107.9(4) . . ? 
P4 O1 V1 133.1(4) . . ? 
B2 O2 V1 126.7(6) . . ? 
B2 O2 V6 130.4(6) . . ? 
V1 O2 V6 102.6(2) . . ? 
B1 O3 V5 128.7(5) . . ? 
B1 O3 V4 128.0(5) . . ? 
V5 O3 V4 102.2(3) . . ? 
B3 O4 V5 129.4(6) . . ? 
B3 O4 V4 126.1(6) . . ? 
V5 O4 V4 102.2(3) . . ? 
P4 O5 V3 125.3(4) . . ? 
B1 O6 V3 129.0(5) . . ? 
B1 O6 V2 128.4(5) . . ? 
V3 O6 V2 101.3(3) . . ? 
P1 O7 V5 131.2(4) . . ? 
P3 O9 V2 130.9(4) . . ? 
P1 O10 V3 126.1(4) . . ? 
P6 O13 V6 125.2(4) . . ? 
B2 O14 P2 118.0(5) . . ? 
B3 O15 V1 127.5(6) 5_567 . ? 
B3 O15 V6 127.5(6) 5_567 . ? 
V1 O15 V6 102.7(3) . . ? 
B3 O16 P6 118.9(6) 5_567 . ? 
B1 O18 P1 119.9(5) . . ? 
P2 O19 V6 126.1(4) . . ? 
P2 O20 V2 131.3(4) . . ? 
P3 O21 V4 126.0(4) . . ? 
B2 O24 V3 130.0(5) . . ? 
B2 O24 V2 127.1(5) . . ? 
V3 O24 V2 101.7(3) . . ? 
B3 O29 P5 119.2(6) . . ? 
P5 O30 V1 130.1(4) 5_567 . ? 
B1 O31 P3 118.0(5) . . ? 
P6 O33 V5 132.9(4) 5_567 . ? 
B2 O34 P4 119.7(6) . . ? 
C1 N1 H1A 109.5 . . ? 
C1 N1 H1B 109.4 . . ? 
H1A N1 H1B 109.5 . . ? 
C1 N1 H1C 109.5 . . ? 
H1A N1 H1C 109.5 . . ? 
H1B N1 H1C 109.5 . . ? 
C3 N2 C2 111.4(10) . . ? 
C3 N2 H2A 109.2 . . ? 
C2 N2 H2A 109.5 . . ? 
C3 N2 H2B 109.5 . . ? 
C2 N2 H2B 109.1 . . ? 
H2A N2 H2B 108.0 . . ? 
C4 N3 C5 121.5(17) . . ? 
C4 N3 H3A 106.9 . . ? 
C5 N3 H3A 107.0 . . ? 
C4 N3 H3B 106.9 . . ? 
C5 N3 H3B 107.1 . . ? 
H3A N3 H3B 106.7 . . ? 
C6 N4 H4A 109.5 . . ? 
C6 N4 H4B 109.4 . . ? 
H4A N4 H4B 109.5 . . ? 
C6 N4 H4C 109.5 . . ? 
H4A N4 H4C 109.5 . . ? 
H4B N4 H4C 109.5 . . ? 
C7 N5 H5A 109.5 . . ? 
C7 N5 H5B 109.5 . . ? 
H5A N5 H5B 109.5 . . ? 
C7 N5 H5C 109.4 . . ? 
H5A N5 H5C 109.5 . . ? 
H5B N5 H5C 109.5 . . ? 
C9 N6 C8 112.6(8) . . ? 
C9 N6 H6A 109.1 . . ? 
C8 N6 H6A 109.0 . . ? 
C9 N6 H6B 109.0 . . ? 
C8 N6 H6B 109.1 . . ? 
H6A N6 H6B 107.8 . . ? 
C11 N7' C10 116.5(19) . . ? 
C11 N7' H7'1 108.3 . . ? 
C10 N7' H7'1 108.1 . . ? 
C11 N7' H7'2 108.1 . . ? 
C10 N7' H7'2 108.2 . . ? 
H7'1 N7' H7'2 107.4 . . ? 
C10 N7 C11 117(2) . . ? 
C10 N7 H7A 108.3 . . ? 
C11 N7 H7A 107.7 . . ? 
C10 N7 H7B 108.3 . . ? 
C11 N7 H7B 108.2 . . ? 
H7A N7 H7B 107.3 . . ? 
C10 N7 H10A 47.1(14) . . ? 
C11 N7 H10A 138.8(19) . . ? 
H7A N7 H10A 62.0 . . ? 
H7B N7 H10A 113.0 . . ? 
C12 N8 H8A 109.6 . . ? 
C12 N8 H8B 109.3 . . ? 
H8A N8 H8B 109.5 . . ? 
C12 N8 H8C 109.5 . . ? 
H8A N8 H8C 109.5 . . ? 
H8B N8 H8C 109.5 . . ? 
H9C N9 H9D 139(10) . . ? 
N1 C1 C2 110.7(10) . . ? 
N1 C1 H1D 109.5 . . ? 
C2 C1 H1D 109.4 . . ? 
N1 C1 H1E 109.5 . . ? 
C2 C1 H1E 109.6 . . ? 
H1D C1 H1E 108.1 . . ? 
C1 C2 N2 106.5(10) . . ? 
C1 C2 H2C 110.3 . . ? 
N2 C2 H2C 110.2 . . ? 
C1 C2 H2D 110.5 . . ? 
N2 C2 H2D 110.6 . . ? 
H2C C2 H2D 108.6 . . ? 
N2 C3 C4 106.3(12) . . ? 
N2 C3 H3C 110.6 . . ? 
C4 C3 H3C 110.6 . . ? 
N2 C3 H3D 110.3 . . ? 
C4 C3 H3D 110.3 . . ? 
H3C C3 H3D 108.7 . . ? 
N3 C4 C3 109.7(13) . . ? 
N3 C4 H4D 109.9 . . ? 
C3 C4 H4D 109.5 . . ? 
N3 C4 H4E 109.6 . . ? 
C3 C4 H4E 109.9 . . ? 
H4D C4 H4E 108.2 . . ? 
N3 C5 C6 107.6(16) . . ? 
N3 C5 H5D 110.1 . . ? 
C6 C5 H5D 110.2 . . ? 
N3 C5 H5E 110.2 . . ? 
C6 C5 H5E 110.3 . . ? 
H5D C5 H5E 108.5 . . ? 
N4 C6 C5 114.4(14) . . ? 
N4 C6 H6C 108.7 . . ? 
C5 C6 H6C 108.6 . . ? 
N4 C6 H6D 108.7 . . ? 
C5 C6 H6D 108.7 . . ? 
H6C C6 H6D 107.6 . . ? 
N5 C7 C8 114.1(9) . . ? 
N5 C7 H7C 108.7 . . ? 
C8 C7 H7C 108.8 . . ? 
N5 C7 H7D 108.7 . . ? 
C8 C7 H7D 108.7 . . ? 
H7C C7 H7D 107.6 . . ? 
N6 C8 C7 112.9(8) . . ? 
N6 C8 H8D 109.0 . . ? 
C7 C8 H8D 109.0 . . ? 
N6 C8 H8E 109.0 . . ? 
C7 C8 H8E 109.0 . . ? 
H8D C8 H8E 107.8 . . ? 
C10 C9 N6 112.1(9) . . ? 
C10 C9 H9A 109.4 . . ? 
N6 C9 H9A 109.2 . . ? 
C10 C9 H9B 108.9 . . ? 
N6 C9 H9B 109.2 . . ? 
H9A C9 H9B 107.9 . . ? 
N7 C10 N7' 49.7(14) . . ? 
N7 C10 C9 119.8(16) . . ? 
N7' C10 C9 114.8(14) . . ? 
N7 C10 H10A 70.7(19) . . ? 
N7' C10 H10A 120.3(17) . . ? 
C9 C10 H10A 96.4(15) . . ? 
N7 C10 H10B 137(2) . . ? 
N7' C10 H10B 116(2) . . ? 
C9 C10 H10B 102.9(14) . . ? 
H10A C10 H10B 104.0(16) . . ? 
N7' C11 C12 108.6(15) . . ? 
N7' C11 N7 45.6(12) . . ? 
C12 C11 N7 128.6(15) . . ? 
N7' C11 H11A 123.8(19) . . ? 
C12 C11 H11A 100.7(16) . . ? 
N7 C11 H11A 78.6(16) . . ? 
N7' C11 H11B 115(2) . . ? 
C12 C11 H11B 102.2(14) . . ? 
N7 C11 H11B 128.2(18) . . ? 
H11A C11 H11B 104.1(16) . . ? 
N8 C12 C11 114.7(12) . . ? 
N8 C12 H12A 108.7 . . ? 
C11 C12 H12A 108.4 . . ? 
N8 C12 H12B 108.6 . . ? 
C11 C12 H12B 108.7 . . ? 
H12A C12 H12B 107.5 . . ? 
O3 B1 O6 111.3(7) . . ? 
O3 B1 O18 110.3(8) . . ? 
O6 B1 O18 109.1(7) . . ? 
O3 B1 O31 110.1(7) . . ? 
O6 B1 O31 110.4(8) . . ? 
O18 B1 O31 105.6(7) . . ? 
O2 B2 O24 111.8(8) . . ? 
O2 B2 O14 110.0(7) . . ? 
O24 B2 O14 110.2(7) . . ? 
O2 B2 O34 111.7(7) . . ? 
O24 B2 O34 107.8(7) . . ? 
O14 B2 O34 105.1(7) . . ? 
O15 B3 O4 112.3(8) 5_567 . ? 
O15 B3 O16 109.9(8) 5_567 5_567 ? 
O4 B3 O16 109.1(8) . 5_567 ? 
O15 B3 O29 111.1(8) 5_567 . ? 
O4 B3 O29 108.8(8) . . ? 
O16 B3 O29 105.3(8) 5_567 . ? 
H6WA OW6 H6WB 144(10) . . ? 
H5WA OW5 H5WB 138(10) . . ? 
H4WB OW4 H4WA 122(10) . . ? 
H3WA OW3 H3WB 73(10) . . ? 
H2WA OW2 H2WB 137(8) . . ? 
H1WB OW1 H1WA 96(10) . . ? 
H7WB OW7 H7WA 169(10) . . ? 
 
_diffrn_measured_fraction_theta_max    0.929 
_diffrn_reflns_theta_full              23.23 
_diffrn_measured_fraction_theta_full   0.929 
_refine_diff_density_max    1.294 
_refine_diff_density_min   -0.647 
_refine_diff_density_rms    0.130 
 
#=======================================================================

 
data_vbp-j2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             vbp-j2 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C28 H128 B6 K N20 O84 P12 V12' 
_chemical_formula_weight          3176.38 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'K'  'K'   0.2009   0.2494 
 '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' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthrombic 
_symmetry_space_group_name_H-M    Pbca 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x-1/2, y-1/2, z' 
 
_cell_length_a                    21.537(2) 
_cell_length_b                    16.2667(13) 
_cell_length_c                    29.717(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      10410.8(18) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     150 
_cell_measurement_theta_min       1.67 
_cell_measurement_theta_max       23.3 
 
_exptl_crystal_description        rhombic 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.027 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              6452 
_exptl_absorpt_coefficient_mu     1.381 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.7820 
_exptl_absorpt_correction_T_max   0.9205
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Bruker CCD area detector '
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             20918 
_diffrn_reflns_av_R_equivalents   0.0945 
_diffrn_reflns_av_sigmaI/netI     0.0758 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          1.67 
_diffrn_reflns_theta_max          23.29 
_reflns_number_total              7345 
_reflns_number_gt                 5235 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXP-97'
_computing_publication_material   'SHELXTL' 
 
_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^)+(0.1056P)^2^+41.3646P] 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          7345 
_refine_ls_number_parameters      759 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0839 
_refine_ls_R_factor_gt            0.0576 
_refine_ls_wR_factor_ref          0.1754 
_refine_ls_wR_factor_gt           0.1540 
_refine_ls_goodness_of_fit_ref    0.950 
_refine_ls_restrained_S_all       0.950 
_refine_ls_shift/su_max           3.199 
_refine_ls_shift/su_mean          0.104 
 
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 0.09553(6) 0.69226(7) 0.46216(4) 0.0247(3) Uani 1 1 d . . . 
V2 V 0.01471(6) 1.09477(8) 0.62421(4) 0.0267(3) Uani 1 1 d . . . 
V3 V 0.02290(6) 0.80723(7) 0.59800(4) 0.0255(3) Uani 1 1 d . . . 
V4 V -0.10329(6) 1.01689(8) 0.66170(4) 0.0307(3) Uani 1 1 d . . . 
V5 V 0.14611(6) 0.86229(8) 0.63807(4) 0.0259(3) Uani 1 1 d . . . 
V6 V 0.15828(5) 0.85905(7) 0.47821(4) 0.0235(3) Uani 1 1 d . . . 
P1 P 0.21660(9) 0.89746(15) 0.38178(7) 0.0399(9) Uani 1 1 d . . . 
P2 P 0.01767(10) 0.71216(12) 0.37402(6) 0.0336(5) Uani 1 1 d . . . 
P3 P -0.07234(9) 0.83255(12) 0.67959(6) 0.0280(5) Uani 1 1 d . . . 
P4 P 0.24850(9) 0.82723(12) 0.56432(6) 0.0242(4) Uani 1 1 d . . . 
P5 P 0.05694(9) 0.62977(11) 0.55864(6) 0.0245(4) Uani 1 1 d . . . 
P6 P 0.12136(9) 1.02616(12) 0.69059(6) 0.0256(4) Uani 1 1 d . . . 
K1 K 0.0000 1.0000 0.5000 0.0391(6) Uani 1 2 d S . . 
O1 O 0.2786(3) 0.8901(5) 0.3598(2) 0.067(2) Uani 1 1 d . . . 
O2 O 0.1749(2) 0.8244(3) 0.36439(16) 0.0373(13) Uani 1 1 d . . . 
O3 O -0.0042(3) 0.6501(4) 0.34011(19) 0.0533(17) Uani 1 1 d . . . 
O4 O 0.0836(2) 0.7433(3) 0.35887(15) 0.0344(13) Uani 1 1 d . . . 
O5 O 0.0229(2) 0.6769(3) 0.42160(17) 0.0406(14) Uani 1 1 d . . . 
O6 O 0.2215(2) 0.8904(3) 0.43336(16) 0.0365(13) Uani 1 1 d . . . 
O7 O 0.1135(2) 0.7961(3) 0.43156(15) 0.0284(12) Uani 1 1 d . . . 
O8 O 0.1456(2) 0.6257(3) 0.44613(17) 0.0376(13) Uani 1 1 d . . . 
O9 O 0.2321(2) 0.8666(3) 0.51886(15) 0.0294(12) Uani 1 1 d . . . 
O10 O 0.1151(2) 0.9355(3) 0.49010(18) 0.0388(13) Uani 1 1 d . . . 
O11 O 0.1331(2) 0.7598(3) 0.51067(14) 0.0245(11) Uani 1 1 d . . . 
O12 O 0.0432(2) 0.6368(3) 0.50792(16) 0.0349(13) Uani 1 1 d . . . 
O13 O 0.0477(2) 0.5432(3) 0.57531(17) 0.0341(12) Uani 1 1 d . . . 
O14 O 0.3166(2) 0.8123(3) 0.56865(16) 0.0319(12) Uani 1 1 d . . . 
O15 O 0.2127(2) 0.7430(3) 0.56760(14) 0.0234(11) Uani 1 1 d . . . 
O16 O 0.1264(2) 0.6545(3) 0.56689(15) 0.0244(11) Uani 1 1 d . . . 
O17 O 0.0155(2) 0.6889(3) 0.58484(17) 0.0327(12) Uani 1 1 d . . . 
O18 O 0.1126(2) 0.7978(3) 0.58791(15) 0.0240(11) Uani 1 1 d . . . 
O19 O 0.2240(2) 0.8815(3) 0.60345(16) 0.0305(12) Uani 1 1 d . . . 
O20 O 0.1643(2) 0.8008(3) 0.67813(17) 0.0414(14) Uani 1 1 d . . . 
O21 O 0.0570(2) 0.8844(3) 0.64243(15) 0.0248(11) Uani 1 1 d . . . 
O22 O -0.0456(2) 0.7830(3) 0.64053(17) 0.0354(13) Uani 1 1 d . . . 
O23 O 0.1638(2) 0.9742(3) 0.66120(17) 0.0366(13) Uani 1 1 d . . . 
O24 O -0.0074(2) 0.8563(3) 0.55615(17) 0.0372(13) Uani 1 1 d . . . 
O25 O -0.1038(2) 0.7763(3) 0.71281(17) 0.0400(14) Uani 1 1 d . . . 
O26 O -0.0175(2) 0.8784(3) 0.70444(15) 0.0292(12) Uani 1 1 d . . . 
O27 O 0.0683(2) 0.9687(3) 0.70900(15) 0.0268(11) Uani 1 1 d . . . 
O28 O 0.1548(2) 1.0635(3) 0.72989(17) 0.0385(13) Uani 1 1 d . . . 
O29 O -0.0141(2) 0.9960(3) 0.65574(15) 0.0255(11) Uani 1 1 d . . . 
O30 O 0.0910(2) 1.0937(3) 0.66185(18) 0.0370(13) Uani 1 1 d . . . 
O31 O -0.1173(2) 0.8971(3) 0.66238(19) 0.0383(13) Uani 1 1 d . . . 
O32 O -0.1155(3) 1.0494(4) 0.71188(18) 0.0467(15) Uani 1 1 d . . . 
O33 O -0.1841(2) 1.0218(4) 0.6304(2) 0.0471(15) Uani 1 1 d . . . 
O34 O -0.0751(2) 1.1114(3) 0.62570(15) 0.0271(11) Uani 1 1 d . . . 
O35 O 0.0274(2) 1.2144(3) 0.6248(2) 0.0464(15) Uani 1 1 d . . . 
O36 O 0.0368(3) 1.0691(4) 0.57495(17) 0.0435(15) Uani 1 1 d . . . 
B1 B 0.0230(4) 0.9334(5) 0.6762(2) 0.0243(18) Uani 1 1 d . . . 
B2 B 0.1455(4) 0.7404(5) 0.5577(3) 0.0221(17) Uani 1 1 d . . . 
B3 B -0.1110(4) 1.1850(5) 0.6166(3) 0.029(2) Uani 1 1 d . . . 
N1 N 0.0816(3) 0.0951(4) 0.0294(2) 0.0364(16) Uani 1 1 d . . . 
H1A H 0.0799 0.0553 0.0499 0.080 Uiso 1 1 calc . . . 
H1B H 0.0433 0.1104 0.0220 0.080 Uiso 1 1 calc . . . 
H1C H 0.1021 0.1379 0.0406 0.080 Uiso 1 1 calc . . . 
N2 N 0.1629(3) 0.1957(4) -0.0356(2) 0.0389(17) Uani 1 1 d . . . 
H2A H 0.2015 0.1763 -0.0309 0.080 Uiso 1 1 calc . . . 
H2B H 0.1496 0.2182 -0.0097 0.080 Uiso 1 1 calc . . . 
N3' C 0.1813(8) 0.3747(10) -0.0153(5) 0.023(3) Uani 0.50 1 d P . . 
H3'1 H 0.1484 0.4108 -0.0257 0.09(4) Uiso 0.50 1 calc PR . . 
H3'2 H 0.1625 0.3346 0.0046 0.09(4) Uiso 0.50 1 calc PR . . 
N3 C 0.2222(12) 0.3383(14) -0.0155(6) 0.040(5) Uani 0.50 1 d P . . 
H3A H 0.2634 0.3157 -0.0109 0.09(4) Uiso 0.50 1 calc PR . . 
H3B H 0.1939 0.3031 0.0010 0.09(4) Uiso 0.50 1 calc PR . . 
N4 N 0.1745(4) 0.3694(5) 0.0771(3) 0.058(2) Uani 1 1 d . . . 
H4A H 0.1574 0.3872 0.1026 0.080 Uiso 1 1 calc . . . 
H4B H 0.2065 0.3367 0.0835 0.080 Uiso 1 1 calc . . . 
H4C H 0.1464 0.3414 0.0613 0.080 Uiso 1 1 calc . . . 
N5 N 0.1127(4) 0.2580(5) 0.6979(3) 0.063(2) Uani 1 1 d . . . 
H5A H 0.1043 0.2092 0.6859 0.080 Uiso 1 1 calc . . . 
H5B H 0.0866 0.2954 0.6869 0.080 Uiso 1 1 calc . . . 
H5C H 0.1086 0.2553 0.7276 0.080 Uiso 1 1 calc . . . 
N6 N 0.1974(4) 0.4321(7) 0.6709(3) 0.079(3) Uani 1 1 d . . . 
H6A H 0.2129 0.4770 0.6846 0.080 Uiso 1 1 calc . . . 
H6B H 0.2242 0.4178 0.6491 0.080 Uiso 1 1 calc . . . 
N7 N 0.0338(3) 0.5081(4) 0.6620(2) 0.0455(18) Uani 1 1 d . . . 
H7A H 0.0174 0.4576 0.6587 0.080 Uiso 1 1 calc . . . 
H7B H 0.0382 0.5302 0.6344 0.080 Uiso 1 1 calc . . . 
N8 N -0.1166(3) 0.6139(5) 0.6872(2) 0.0433(18) Uani 1 1 d . . . 
H8A H -0.1506 0.6180 0.6702 0.080 Uiso 1 1 calc . . . 
H8B H -0.1035 0.6639 0.6946 0.080 Uiso 1 1 calc . . . 
H8C H -0.1254 0.5857 0.7120 0.080 Uiso 1 1 calc . . . 
C1 C 0.1143(4) 0.0643(5) -0.0114(3) 0.047(2) Uani 1 1 d . . . 
H1D H 0.1552 0.0451 -0.0027 0.080 Uiso 1 1 calc . . . 
H1E H 0.0916 0.0176 -0.0232 0.080 Uiso 1 1 calc . . . 
C2 C 0.1214(4) 0.1259(5) -0.0476(3) 0.042(2) Uani 1 1 d . . . 
H2C H 0.0808 0.1474 -0.0552 0.080 Uiso 1 1 calc . . . 
H2D H 0.1378 0.0988 -0.0741 0.080 Uiso 1 1 calc . . . 
C3 C 0.1656(4) 0.2608(6) -0.0707(3) 0.050(2) Uani 1 1 d . . . 
H3A H 0.1784 0.2366 -0.0990 0.080 Uiso 1 1 calc . . . 
H3B H 0.1245 0.2841 -0.0748 0.080 Uiso 1 1 calc . . . 
C4 C 0.2093(8) 0.3268(9) -0.0583(6) 0.097(6) Uani 1 1 d . . . 
H4D H 0.193(13) 0.378(15) -0.029(9) 0.08 Uiso 1 1 d . . . 
H4E H 0.217(9) 0.367(13) -0.085(7) 0.08 Uiso 1 1 d . . . 
C5 C 0.2217(8) 0.4195(7) 0.0086(6) 0.112(6) Uani 1 1 d . . . 
H5D H 0.1997 0.4574 0.0000 0.08 Uiso 1 1 d . . . 
H5E H 0.2582 0.4128 0.0016 0.08 Uiso 1 1 d . . . 
C6 C 0.1961(6) 0.4393(6) 0.0509(4) 0.075(3) Uani 1 1 d . . . 
H6C H 0.1615 0.4765 0.0463 0.080 Uiso 1 1 calc . . . 
H6D H 0.2272 0.4684 0.0683 0.080 Uiso 1 1 calc . . . 
C7 C 0.1768(5) 0.2815(7) 0.6866(3) 0.063(3) Uani 1 1 d . . . 
H7C H 0.1813 0.2821 0.6541 0.080 Uiso 1 1 calc . . . 
H7D H 0.2049 0.2402 0.6984 0.080 Uiso 1 1 calc . . . 
C8 C 0.1952(5) 0.3636(8) 0.7047(4) 0.070(3) Uani 1 1 d . . . 
H8D H 0.2358 0.3586 0.7184 0.080 Uiso 1 1 calc . . . 
H8E H 0.1661 0.3787 0.7282 0.080 Uiso 1 1 calc . . . 
C9 C 0.1381(5) 0.4544(9) 0.6498(3) 0.077(4) Uani 1 1 d . . . 
H9A H 0.1173 0.4049 0.6395 0.080 Uiso 1 1 calc . . . 
H9B H 0.1460 0.4889 0.6238 0.080 Uiso 1 1 calc . . . 
C10 C 0.0951(4) 0.5009(9) 0.6831(4) 0.077(4) Uani 1 1 d . . . 
H10A H 0.0919 0.4709 0.7112 0.080 Uiso 1 1 calc . . . 
H10B H 0.1118 0.5551 0.6894 0.080 Uiso 1 1 calc . . . 
C11 C -0.0097(4) 0.5604(6) 0.6892(3) 0.049(2) Uani 1 1 d . . . 
H11A H -0.0193 0.5338 0.7176 0.080 Uiso 1 1 calc . . . 
H11B H 0.0089 0.6135 0.6955 0.080 Uiso 1 1 calc . . . 
C12 C -0.0676(4) 0.5708(6) 0.6616(3) 0.049(2) Uani 1 1 d . . . 
H12A H -0.0579 0.6019 0.6347 0.080 Uiso 1 1 calc . . . 
H12B H -0.0827 0.5172 0.6525 0.080 Uiso 1 1 calc . . . 
OW1 O 0.1526(3) 0.7781(3) 0.26950(17) 0.0436(14) Uani 1 1 d . . . 
H51A H 0.1909 0.8057 0.2613 0.080 Uiso 1 1 calc . . . 
H51B H 0.1283 0.8057 0.2924 0.080 Uiso 1 1 calc . . . 
OW2 O -0.0661(3) 0.7762(4) 0.4804(2) 0.0516(16) Uani 1 1 d . . . 
H52A H -0.0270 0.8038 0.4748 0.080 Uiso 1 1 calc . . . 
H52B H -0.0930 0.8038 0.5018 0.080 Uiso 1 1 calc . . . 
OW3 O 0.2152(5) 0.6220(7) 0.6446(4) 0.134(4) Uani 1 1 d . . . 
H53A H 0.2543 0.6493 0.6386 0.080 Uiso 1 1 calc . . . 
H53B H 0.1896 0.6493 0.6670 0.080 Uiso 1 1 calc . . . 
C14 C -0.3131(10) 0.9196(15) 0.6430(7) 0.163(10) Uani 1 1 d . . . 
H54A H -0.3489 0.9035 0.6601 2.6(6) Uiso 1 1 calc R . . 
H54B H -0.3084 0.8834 0.6177 2.6(6) Uiso 1 1 calc R . . 
H54C H -0.3183 0.9749 0.6325 2.6(6) Uiso 1 1 calc R . . 
OW4 O -0.2366(6) 0.7776(13) 0.6928(5) 0.228(10) Uani 1 1 d . . . 
H55A H -0.1970 0.8051 0.6893 0.080 Uiso 1 1 calc . . . 
H55B H -0.2654 0.8051 0.7129 0.080 Uiso 1 1 calc . . . 
OW5 O 0.2718(5) 1.0505(15) 0.7413(5) 0.329(15) Uani 1 1 d . . . 
H56A H 0.3108 1.0780 0.7350 0.080 Uiso 1 1 calc . . . 
H56B H 0.2458 1.0780 0.7633 0.080 Uiso 1 1 calc . . . 
C13 C 0.1207(11) 0.8910(13) 0.7900(6) 0.151(8) Uani 1 1 d . . . 
H57A H 0.1585 0.8710 0.8032 2.6(6) Uiso 1 1 calc R . . 
H57B H 0.0943 0.9127 0.8132 2.6(6) Uiso 1 1 calc R . . 
H57C H 0.1303 0.9337 0.7688 2.6(6) Uiso 1 1 calc R . . 
OW6 O 0.0272(9) 0.7194(18) 0.7569(6) 0.315(14) Uani 1 1 d . . . 
H58A H 0.0667 0.7467 0.7524 0.080 Uiso 1 1 calc . . . 
H58B H -0.0001 0.7467 0.7782 0.080 Uiso 1 1 calc . . . 
N9 N 0.0905(8) 0.6728(11) 0.2682(4) 0.147(7) Uani 1 1 d . . . 
H59A H 0.0753 0.7130 0.2835 2.6(6) Uiso 1 1 calc R . . 
H59C H 0.0869 0.6723 0.2394 2.6(6) Uiso 1 1 calc R . . 
N10 N 0.2626(7) 1.0848(7) 0.3311(6) 0.153(8) Uani 1 1 d . . . 
H60B H 0.2264 1.0773 0.3426 2.6(6) Uiso 1 1 calc R . . 
H60C H 0.2662 1.0951 0.3028 2.6(6) Uiso 1 1 calc R . . 
 
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 0.0249(7) 0.0289(7) 0.0203(6) 0.0020(5) -0.0019(5) -0.0014(5) 
V2 0.0242(7) 0.0316(7) 0.0244(7) 0.0006(5) -0.0002(5) -0.0012(5) 
V3 0.0212(7) 0.0321(7) 0.0231(6) -0.0019(5) -0.0003(5) -0.0010(5) 
V4 0.0250(7) 0.0389(8) 0.0283(7) 0.0072(6) 0.0024(5) 0.0036(6) 
V5 0.0204(7) 0.0333(7) 0.0242(6) -0.0046(5) -0.0012(5) 0.0012(5) 
V6 0.0207(7) 0.0265(7) 0.0233(6) 0.0032(5) 0.0009(5) 0.0009(5) 
P1 0.0215(13) 0.0649(17) 0.0332(13) 0.0186(11) 0.0035(9) 0.0051(10) 
P2 0.0449(13) 0.0285(11) 0.0274(10) -0.0021(9) -0.0132(9) 0.0010(9) 
P3 0.0271(11) 0.0314(10) 0.0254(10) 0.0039(8) 0.0072(8) -0.0024(9) 
P4 0.0190(10) 0.0306(10) 0.0230(9) -0.0033(8) 0.0016(8) 0.0006(8) 
P5 0.0269(11) 0.0246(10) 0.0221(9) -0.0011(8) 0.0028(8) -0.0040(8) 
P6 0.0221(11) 0.0316(10) 0.0230(9) -0.0058(8) -0.0032(8) 0.0017(8) 
K1 0.0341(15) 0.0466(15) 0.0366(14) -0.0065(11) -0.0025(11) 0.0055(12) 
O1 0.024(3) 0.130(7) 0.048(4) 0.029(4) 0.014(3) 0.013(4) 
O2 0.032(3) 0.053(3) 0.027(3) 0.009(2) 0.009(2) 0.019(3) 
O3 0.078(5) 0.042(4) 0.040(3) -0.005(3) -0.024(3) -0.005(3) 
O4 0.048(3) 0.036(3) 0.019(2) 0.000(2) -0.003(2) 0.007(3) 
O5 0.036(3) 0.055(4) 0.031(3) 0.013(3) -0.010(2) -0.013(3) 
O6 0.026(3) 0.053(3) 0.030(3) 0.014(3) 0.003(2) -0.003(2) 
O7 0.032(3) 0.034(3) 0.019(2) 0.002(2) -0.002(2) 0.003(2) 
O8 0.041(3) 0.033(3) 0.039(3) -0.002(2) 0.001(3) 0.004(2) 
O9 0.024(3) 0.036(3) 0.028(3) 0.003(2) -0.004(2) -0.006(2) 
O10 0.034(3) 0.033(3) 0.049(3) -0.002(3) -0.001(3) 0.002(2) 
O11 0.024(3) 0.031(3) 0.018(2) 0.002(2) -0.002(2) -0.006(2) 
O12 0.033(3) 0.044(3) 0.029(3) 0.004(2) -0.003(2) -0.014(2) 
O13 0.040(3) 0.027(3) 0.036(3) -0.002(2) 0.005(2) -0.006(2) 
O14 0.022(3) 0.041(3) 0.033(3) -0.003(2) 0.000(2) -0.001(2) 
O15 0.020(3) 0.026(3) 0.024(2) 0.000(2) 0.003(2) 0.001(2) 
O16 0.027(3) 0.025(3) 0.021(2) 0.001(2) 0.000(2) 0.001(2) 
O17 0.023(3) 0.031(3) 0.044(3) -0.009(2) 0.006(2) -0.005(2) 
O18 0.020(3) 0.030(3) 0.023(2) -0.007(2) 0.002(2) -0.003(2) 
O19 0.020(3) 0.040(3) 0.032(3) -0.013(2) 0.006(2) -0.003(2) 
O20 0.038(3) 0.055(4) 0.031(3) 0.006(3) -0.006(2) 0.006(3) 
O21 0.017(3) 0.032(3) 0.025(3) -0.006(2) -0.003(2) 0.002(2) 
O22 0.027(3) 0.047(3) 0.033(3) -0.010(3) 0.006(2) -0.009(2) 
O23 0.027(3) 0.045(3) 0.038(3) -0.017(3) 0.005(2) -0.008(2) 
O24 0.032(3) 0.044(3) 0.035(3) 0.004(3) -0.006(2) 0.004(3) 
O25 0.044(3) 0.042(3) 0.035(3) 0.007(3) 0.009(3) -0.010(3) 
O26 0.031(3) 0.033(3) 0.024(3) 0.004(2) 0.003(2) 0.000(2) 
O27 0.025(3) 0.032(3) 0.024(2) -0.004(2) -0.002(2) 0.000(2) 
O28 0.032(3) 0.052(3) 0.031(3) -0.015(3) -0.004(2) -0.003(3) 
O29 0.022(3) 0.028(3) 0.026(3) 0.003(2) 0.002(2) 0.002(2) 
O30 0.033(3) 0.034(3) 0.044(3) 0.004(3) -0.014(3) -0.007(2) 
O31 0.023(3) 0.036(3) 0.055(3) 0.005(3) 0.002(3) -0.002(2) 
O32 0.051(4) 0.057(4) 0.033(3) 0.003(3) 0.010(3) 0.012(3) 
O33 0.028(3) 0.056(4) 0.057(4) 0.020(3) -0.012(3) -0.005(3) 
O34 0.029(3) 0.029(3) 0.024(3) 0.007(2) -0.003(2) 0.001(2) 
O35 0.033(3) 0.029(3) 0.076(4) 0.008(3) -0.008(3) -0.002(2) 
O36 0.037(3) 0.063(4) 0.030(3) -0.012(3) 0.009(2) -0.014(3) 
B1 0.022(5) 0.037(5) 0.014(4) -0.003(4) 0.000(3) 0.002(4) 
B2 0.020(5) 0.026(4) 0.020(4) -0.003(3) 0.004(3) -0.001(3) 
B3 0.031(5) 0.033(5) 0.023(4) 0.002(4) 0.002(4) 0.005(4) 
N1 0.040(4) 0.032(4) 0.037(4) 0.004(3) -0.001(3) 0.004(3) 
N2 0.025(4) 0.057(4) 0.036(4) 0.004(3) -0.003(3) -0.002(3) 
N3' 0.018(9) 0.034(9) 0.018(7) -0.004(7) 0.003(6) 0.002(8) 
N3 0.049(16) 0.044(10) 0.025(8) 0.016(7) -0.019(8) -0.012(11) 
N4 0.068(6) 0.041(4) 0.066(5) -0.012(4) 0.023(4) 0.011(4) 
N5 0.085(7) 0.061(5) 0.043(4) -0.010(4) -0.009(4) 0.005(5) 
N6 0.055(6) 0.112(8) 0.069(6) -0.024(6) 0.004(5) 0.012(5) 
N7 0.042(4) 0.051(4) 0.044(4) 0.002(3) 0.006(3) 0.003(4) 
N8 0.040(4) 0.060(5) 0.030(4) 0.009(3) 0.001(3) 0.001(4) 
C1 0.037(5) 0.042(5) 0.062(6) -0.007(5) 0.003(4) 0.000(4) 
C2 0.037(5) 0.053(5) 0.036(5) -0.008(4) 0.000(4) 0.000(4) 
C3 0.053(6) 0.064(6) 0.032(4) 0.009(4) -0.001(4) 0.018(5) 
C4 0.119(12) 0.084(10) 0.086(12) 0.041(9) -0.020(10) -0.044(9) 
C5 0.146(14) 0.042(7) 0.148(14) 0.020(8) 0.096(12) 0.014(8) 
C6 0.094(9) 0.040(6) 0.091(8) 0.016(6) -0.019(7) -0.007(6) 
C7 0.064(7) 0.068(7) 0.058(6) -0.020(5) 0.015(5) 0.003(6) 
C8 0.061(7) 0.089(9) 0.061(6) 0.013(6) 0.017(6) 0.004(6) 
C9 0.039(6) 0.155(12) 0.038(5) -0.013(6) -0.003(4) 0.014(7) 
C10 0.036(6) 0.137(11) 0.057(6) -0.033(7) -0.010(5) 0.021(6) 
C11 0.042(5) 0.064(6) 0.040(5) -0.003(4) 0.004(4) 0.018(5) 
C12 0.031(5) 0.073(7) 0.043(5) -0.001(5) 0.003(4) 0.011(5) 
OW1 0.060(4) 0.045(3) 0.025(3) -0.015(3) 0.005(3) 0.009(3) 
OW2 0.052(4) 0.051(4) 0.052(4) -0.002(3) 0.010(3) -0.009(3) 
OW3 0.155(10) 0.119(9) 0.126(8) 0.025(7) -0.002(8) 0.023(7) 
C14 0.153(19) 0.20(2) 0.136(16) -0.080(16) -0.006(14) -0.080(17) 
OW4 0.106(9) 0.40(3) 0.176(13) -0.132(16) 0.038(9) -0.083(13) 
OW5 0.065(7) 0.73(4) 0.194(13) -0.29(2) -0.057(8) 0.125(14) 
C13 0.25(2) 0.121(14) 0.087(12) 0.023(11) -0.020(13) -0.061(15) 
OW6 0.23(2) 0.51(4) 0.210(18) -0.18(2) -0.073(15) 0.10(2) 
N9 0.201(16) 0.164(13) 0.077(8) -0.076(9) 0.064(10) -0.107(13) 
N10 0.141(13) 0.075(8) 0.243(19) 0.029(10) 0.154(13) -0.005(8) 
 
_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 O8 1.600(5) . ? 
V1 O7 1.957(5) . ? 
V1 O12 1.983(5) . ? 
V1 O11 1.985(4) . ? 
V1 O5 1.991(5) . ? 
V2 O36 1.594(5) . ? 
V2 O34 1.954(5) . ? 
V2 O29 1.961(5) . ? 
V2 O35 1.965(5) . ? 
V2 O30 1.988(5) . ? 
V3 O24 1.615(5) . ? 
V3 O18 1.961(5) . ? 
V3 O21 1.964(5) . ? 
V3 O17 1.971(5) . ? 
V3 O22 1.982(5) . ? 
V4 O32 1.604(5) . ? 
V4 O29 1.960(5) . ? 
V4 O34 1.968(5) . ? 
V4 O31 1.973(5) . ? 
V4 O33 1.975(5) . ? 
V5 O20 1.604(5) . ? 
V5 O21 1.958(5) . ? 
V5 O18 1.960(4) . ? 
V5 O23 1.983(5) . ? 
V5 O19 1.992(5) . ? 
V6 O10 1.593(5) . ? 
V6 O11 1.957(5) . ? 
V6 O6 1.973(5) . ? 
V6 O7 1.975(5) . ? 
V6 O9 2.000(5) . ? 
P1 O1 1.492(6) . ? 
P1 O33 1.532(6) 5_576 ? 
P1 O6 1.541(5) . ? 
P1 O2 1.576(6) . ? 
P2 O3 1.503(6) . ? 
P2 O5 1.530(5) . ? 
P2 O35 1.539(6) 5_576 ? 
P2 O4 1.574(6) . ? 
P3 O25 1.507(5) . ? 
P3 O31 1.517(6) . ? 
P3 O22 1.527(5) . ? 
P3 O26 1.579(5) . ? 
P4 O14 1.492(5) . ? 
P4 O9 1.537(5) . ? 
P4 O19 1.553(5) . ? 
P4 O15 1.575(5) . ? 
P5 O13 1.506(5) . ? 
P5 O17 1.526(5) . ? 
P5 O12 1.540(5) . ? 
P5 O16 1.567(5) . ? 
P6 O28 1.501(5) . ? 
P6 O23 1.520(5) . ? 
P6 O30 1.538(5) . ? 
P6 O27 1.574(5) . ? 
K1 O36 2.617(5) . ? 
K1 O36 2.617(5) 5_576 ? 
K1 O10 2.707(5) . ? 
K1 O10 2.707(5) 5_576 ? 
K1 O24 2.877(5) . ? 
K1 O24 2.877(5) 5_576 ? 
O2 B3 1.497(10) 5_576 ? 
O4 B3 1.496(10) 5_576 ? 
O7 B3 1.466(9) 5_576 ? 
O11 B2 1.456(9) . ? 
O15 B2 1.479(9) . ? 
O16 B2 1.483(9) . ? 
O18 B2 1.476(9) . ? 
O21 B1 1.476(9) . ? 
O26 B1 1.505(9) . ? 
O27 B1 1.493(9) . ? 
O29 B1 1.430(9) . ? 
O33 P1 1.532(6) 5_576 ? 
O34 B3 1.450(10) . ? 
O35 P2 1.539(6) 5_576 ? 
B3 O7 1.466(9) 5_576 ? 
B3 O4 1.496(10) 5_576 ? 
B3 O2 1.497(10) 5_576 ? 
N1 C1 1.489(11) . ? 
N1 H1A 0.8900 . ? 
N1 H1B 0.8902 . ? 
N1 H1C 0.8898 . ? 
N2 C2 1.489(11) . ? 
N2 C3 1.487(11) . ? 
N2 H2A 0.9002 . ? 
N2 H2B 0.8993 . ? 
N3' C5 1.34(2) . ? 
N3' C4 1.61(2) . ? 
N3' H3'1 0.9700 . ? 
N3' H3'2 0.9700 . ? 
N3' H5D 1.475(16) . ? 
N3 C4 1.32(2) . ? 
N3 C5 1.50(3) . ? 
N3 H3A 0.9700 . ? 
N3 H3B 0.9700 . ? 
N3 H5E 1.526(17) . ? 
N4 C6 1.455(13) . ? 
N4 H4A 0.8890 . ? 
N4 H4B 0.8892 . ? 
N4 H4C 0.8914 . ? 
N5 C7 1.470(13) . ? 
N5 H5A 0.8907 . ? 
N5 H5B 0.8897 . ? 
N5 H5C 0.8909 . ? 
N6 C9 1.470(13) . ? 
N6 C8 1.499(14) . ? 
N6 H6A 0.9040 . ? 
N6 H6B 0.9009 . ? 
N7 C10 1.465(11) . ? 
N7 C11 1.503(10) . ? 
N7 H7A 0.8981 . ? 
N7 H7B 0.8993 . ? 
N8 C12 1.477(11) . ? 
N8 H8A 0.8893 . ? 
N8 H8B 0.8920 . ? 
N8 H8C 0.8876 . ? 
C1 C2 1.477(12) . ? 
C1 H1D 0.9713 . ? 
C1 H1E 0.9689 . ? 
C2 H2C 0.9694 . ? 
C2 H2D 0.9701 . ? 
C3 C4 1.473(16) . ? 
C3 H3A 0.9730 . ? 
C3 H3B 0.9706 . ? 
C4 H4D 1.3(3) . ? 
C4 H4E 1.0(2) . ? 
C5 C6 1.410(17) . ? 
C5 H5D 0.818(14) . ? 
C5 H5E 0.821(14) . ? 
C6 H5D 1.544(12) . ? 
C6 H6C 0.9681 . ? 
C6 H6D 0.9699 . ? 
C7 C8 1.493(15) . ? 
C7 H7C 0.9682 . ? 
C7 H7D 0.9726 . ? 
C8 H8D 0.9740 . ? 
C8 H8E 0.9674 . ? 
C9 C10 1.552(14) . ? 
C9 H9A 0.9663 . ? 
C9 H9B 0.9706 . ? 
C10 H10A 0.9714 . ? 
C10 H10B 0.9709 . ? 
C11 C12 1.502(12) . ? 
C11 H11A 0.9695 . ? 
C11 H11B 0.9718 . ? 
C12 H12A 0.9710 . ? 
C12 H12B 0.9678 . ? 
OW1 H51A 0.9687 . ? 
OW1 H51B 0.9700 . ? 
OW2 H52A 0.9695 . ? 
OW2 H52B 0.9696 . ? 
OW3 H53A 0.9721 . ? 
OW3 H53B 0.9710 . ? 
C14 N10 1.33(2) 5_576 ? 
C14 H54A 0.9788 . ? 
C14 H54B 0.9803 . ? 
C14 H54C 0.9801 . ? 
OW4 H55A 0.9741 . ? 
OW4 H55B 0.9674 . ? 
OW5 H56A 0.9668 . ? 
OW5 H56B 0.9651 . ? 
C13 N9 1.39(2) 7_576 ? 
C13 H57A 0.9890 . ? 
C13 H57B 0.9891 . ? 
C13 H57C 0.9889 . ? 
OW6 H58A 0.9570 . ? 
OW6 H58B 0.9761 . ? 
N9 C13 1.39(2) 7_575 ? 
N9 H59A 0.8600 . ? 
N9 H59C 0.8600 . ? 
N10 C14 1.33(2) 5_576 ? 
N10 H60B 0.8600 . ? 
N10 H60C 0.8600 . ? 
 
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 
O8 V1 O7 108.2(2) . . ? 
O8 V1 O12 106.2(3) . . ? 
O7 V1 O12 145.5(2) . . ? 
O8 V1 O11 108.4(2) . . ? 
O7 V1 O11 77.24(19) . . ? 
O12 V1 O11 89.16(19) . . ? 
O8 V1 O5 105.3(3) . . ? 
O7 V1 O5 89.0(2) . . ? 
O12 V1 O5 84.9(2) . . ? 
O11 V1 O5 146.1(2) . . ? 
O36 V2 O34 110.6(2) . . ? 
O36 V2 O29 108.6(3) . . ? 
O34 V2 O29 77.85(19) . . ? 
O36 V2 O35 103.1(3) . . ? 
O34 V2 O35 90.0(2) . . ? 
O29 V2 O35 148.4(2) . . ? 
O36 V2 O30 105.5(3) . . ? 
O34 V2 O30 143.8(2) . . ? 
O29 V2 O30 89.2(2) . . ? 
O35 V2 O30 83.6(2) . . ? 
O24 V3 O18 108.6(2) . . ? 
O24 V3 O21 110.7(2) . . ? 
O18 V3 O21 77.58(19) . . ? 
O24 V3 O17 107.3(3) . . ? 
O18 V3 O17 88.5(2) . . ? 
O21 V3 O17 142.0(2) . . ? 
O24 V3 O22 106.8(3) . . ? 
O18 V3 O22 144.6(2) . . ? 
O21 V3 O22 88.7(2) . . ? 
O17 V3 O22 82.6(2) . . ? 
O32 V4 O29 107.6(3) . . ? 
O32 V4 O34 107.4(3) . . ? 
O29 V4 O34 77.5(2) . . ? 
O32 V4 O31 106.9(3) . . ? 
O29 V4 O31 88.8(2) . . ? 
O34 V4 O31 145.5(2) . . ? 
O32 V4 O33 106.3(3) . . ? 
O29 V4 O33 145.9(2) . . ? 
O34 V4 O33 89.1(2) . . ? 
O31 V4 O33 84.8(2) . . ? 
O20 V5 O21 107.8(2) . . ? 
O20 V5 O18 108.7(3) . . ? 
O21 V5 O18 77.75(19) . . ? 
O20 V5 O23 105.6(3) . . ? 
O21 V5 O23 89.8(2) . . ? 
O18 V5 O23 145.7(2) . . ? 
O20 V5 O19 106.0(3) . . ? 
O21 V5 O19 146.2(2) . . ? 
O18 V5 O19 90.07(19) . . ? 
O23 V5 O19 82.7(2) . . ? 
O10 V6 O11 111.9(2) . . ? 
O10 V6 O6 110.6(3) . . ? 
O11 V6 O6 137.5(2) . . ? 
O10 V6 O7 106.0(2) . . ? 
O11 V6 O7 77.46(19) . . ? 
O6 V6 O7 89.8(2) . . ? 
O10 V6 O9 106.4(2) . . ? 
O11 V6 O9 88.47(19) . . ? 
O6 V6 O9 81.0(2) . . ? 
O7 V6 O9 147.5(2) . . ? 
O1 P1 O33 112.0(4) . 5_576 ? 
O1 P1 O6 111.6(3) . . ? 
O33 P1 O6 109.3(3) 5_576 . ? 
O1 P1 O2 107.8(4) . . ? 
O33 P1 O2 108.0(3) 5_576 . ? 
O6 P1 O2 108.0(3) . . ? 
O3 P2 O5 113.0(3) . . ? 
O3 P2 O35 109.8(3) . 5_576 ? 
O5 P2 O35 108.4(3) . 5_576 ? 
O3 P2 O4 107.9(3) . . ? 
O5 P2 O4 108.6(3) . . ? 
O35 P2 O4 109.0(3) 5_576 . ? 
O25 P3 O31 110.7(3) . . ? 
O25 P3 O22 110.3(3) . . ? 
O31 P3 O22 110.5(3) . . ? 
O25 P3 O26 108.5(3) . . ? 
O31 P3 O26 108.0(3) . . ? 
O22 P3 O26 108.8(3) . . ? 
O14 P4 O9 111.7(3) . . ? 
O14 P4 O19 111.2(3) . . ? 
O9 P4 O19 110.1(3) . . ? 
O14 P4 O15 109.5(3) . . ? 
O9 P4 O15 107.7(3) . . ? 
O19 P4 O15 106.4(3) . . ? 
O13 P5 O17 110.1(3) . . ? 
O13 P5 O12 111.5(3) . . ? 
O17 P5 O12 109.9(3) . . ? 
O13 P5 O16 108.3(3) . . ? 
O17 P5 O16 108.5(3) . . ? 
O12 P5 O16 108.5(3) . . ? 
O28 P6 O23 112.6(3) . . ? 
O28 P6 O30 110.3(3) . . ? 
O23 P6 O30 109.5(3) . . ? 
O28 P6 O27 108.6(3) . . ? 
O23 P6 O27 107.8(3) . . ? 
O30 P6 O27 108.0(3) . . ? 
O36 K1 O36 180.000(1) . 5_576 ? 
O36 K1 O10 88.96(17) . . ? 
O36 K1 O10 91.04(17) 5_576 . ? 
O36 K1 O10 91.04(17) . 5_576 ? 
O36 K1 O10 88.96(17) 5_576 5_576 ? 
O10 K1 O10 180.000(1) . 5_576 ? 
O36 K1 O24 82.66(17) . . ? 
O36 K1 O24 97.34(17) 5_576 . ? 
O10 K1 O24 78.40(15) . . ? 
O10 K1 O24 101.60(15) 5_576 . ? 
O36 K1 O24 97.34(17) . 5_576 ? 
O36 K1 O24 82.66(17) 5_576 5_576 ? 
O10 K1 O24 101.60(15) . 5_576 ? 
O10 K1 O24 78.40(15) 5_576 5_576 ? 
O24 K1 O24 180.000(1) . 5_576 ? 
B3 O2 P1 118.5(5) 5_576 . ? 
B3 O4 P2 117.8(5) 5_576 . ? 
P2 O5 V1 124.7(3) . . ? 
P1 O6 V6 130.1(3) . . ? 
B3 O7 V1 128.9(5) 5_576 . ? 
B3 O7 V6 126.6(5) 5_576 . ? 
V1 O7 V6 102.6(2) . . ? 
P4 O9 V6 133.5(3) . . ? 
V6 O10 K1 149.5(3) . . ? 
B2 O11 V6 126.9(4) . . ? 
B2 O11 V1 130.6(4) . . ? 
V6 O11 V1 102.2(2) . . ? 
P5 O12 V1 126.5(3) . . ? 
B2 O15 P4 119.4(4) . . ? 
B2 O16 P5 118.5(4) . . ? 
P5 O17 V3 132.0(3) . . ? 
B2 O18 V5 128.7(4) . . ? 
B2 O18 V3 127.9(4) . . ? 
V5 O18 V3 101.8(2) . . ? 
P4 O19 V5 125.7(3) . . ? 
B1 O21 V5 129.1(4) . . ? 
B1 O21 V3 128.1(4) . . ? 
V5 O21 V3 101.8(2) . . ? 
P3 O22 V3 131.3(3) . . ? 
P6 O23 V5 126.4(3) . . ? 
V3 O24 K1 145.6(3) . . ? 
B1 O26 P3 117.0(4) . . ? 
B1 O27 P6 118.4(4) . . ? 
B1 O29 V4 129.2(4) . . ? 
B1 O29 V2 127.7(4) . . ? 
V4 O29 V2 102.2(2) . . ? 
P6 O30 V2 132.1(3) . . ? 
P3 O31 V4 126.1(3) . . ? 
P1 O33 V4 123.3(4) 5_576 . ? 
B3 O34 V2 129.6(5) . . ? 
B3 O34 V4 125.6(5) . . ? 
V2 O34 V4 102.1(2) . . ? 
P2 O35 V2 132.9(3) 5_576 . ? 
V2 O36 K1 143.5(3) . . ? 
O29 B1 O21 111.8(5) . . ? 
O29 B1 O27 111.6(6) . . ? 
O21 B1 O27 109.1(6) . . ? 
O29 B1 O26 109.7(6) . . ? 
O21 B1 O26 110.2(6) . . ? 
O27 B1 O26 104.2(5) . . ? 
O11 B2 O18 111.1(6) . . ? 
O11 B2 O15 111.4(6) . . ? 
O18 B2 O15 109.3(5) . . ? 
O11 B2 O16 109.3(6) . . ? 
O18 B2 O16 110.5(5) . . ? 
O15 B2 O16 105.2(6) . . ? 
O34 B3 O7 112.0(6) . 5_576 ? 
O34 B3 O4 110.2(6) . 5_576 ? 
O7 B3 O4 109.1(6) 5_576 5_576 ? 
O34 B3 O2 109.6(6) . 5_576 ? 
O7 B3 O2 110.8(6) 5_576 5_576 ? 
O4 B3 O2 105.0(6) 5_576 5_576 ? 
C1 N1 H1A 109.5 . . ? 
C1 N1 H1B 109.4 . . ? 
H1A N1 H1B 109.5 . . ? 
C1 N1 H1C 109.5 . . ? 
H1A N1 H1C 109.5 . . ? 
H1B N1 H1C 109.5 . . ? 
C2 N2 C3 113.6(6) . . ? 
C2 N2 H2A 108.8 . . ? 
C3 N2 H2A 108.9 . . ? 
C2 N2 H2B 108.8 . . ? 
C3 N2 H2B 108.9 . . ? 
H2A N2 H2B 107.8 . . ? 
C5 N3' C4 116.1(13) . . ? 
C5 N3' H3'1 108.1 . . ? 
C4 N3' H3'1 108.3 . . ? 
C5 N3' H3'2 108.3 . . ? 
C4 N3' H3'2 108.3 . . ? 
H3'1 N3' H3'2 107.4 . . ? 
C5 N3' H5D 33.4(7) . . ? 
C4 N3' H5D 125.8(11) . . ? 
H3'1 N3' H5D 74.9 . . ? 
H3'2 N3' H5D 122.5 . . ? 
C4 N3 C5 125.9(18) . . ? 
C4 N3 H3A 106.6 . . ? 
C5 N3 H3A 106.4 . . ? 
C4 N3 H3B 105.6 . . ? 
C5 N3 H3B 105.0 . . ? 
H3A N3 H3B 106.0 . . ? 
C4 N3 H5E 122.9(13) . . ? 
C5 N3 H5E 31.4(7) . . ? 
H3A N3 H5E 78.7 . . ? 
H3B N3 H5E 127.9 . . ? 
C6 N4 H4A 109.4 . . ? 
C6 N4 H4B 109.6 . . ? 
H4A N4 H4B 109.6 . . ? 
C6 N4 H4C 109.4 . . ? 
H4A N4 H4C 109.4 . . ? 
H4B N4 H4C 109.4 . . ? 
C7 N5 H5A 109.5 . . ? 
C7 N5 H5B 109.5 . . ? 
H5A N5 H5B 109.4 . . ? 
C7 N5 H5C 109.6 . . ? 
H5A N5 H5C 109.3 . . ? 
H5B N5 H5C 109.4 . . ? 
C9 N6 C8 116.2(9) . . ? 
C9 N6 H6A 108.5 . . ? 
C8 N6 H6A 108.1 . . ? 
C9 N6 H6B 108.5 . . ? 
C8 N6 H6B 108.3 . . ? 
H6A N6 H6B 107.0 . . ? 
C10 N7 C11 112.1(7) . . ? 
C10 N7 H7A 109.3 . . ? 
C11 N7 H7A 109.1 . . ? 
C10 N7 H7B 109.1 . . ? 
C11 N7 H7B 109.1 . . ? 
H7A N7 H7B 108.1 . . ? 
C12 N8 H8A 109.4 . . ? 
C12 N8 H8B 109.3 . . ? 
H8A N8 H8B 109.4 . . ? 
C12 N8 H8C 109.5 . . ? 
H8A N8 H8C 109.8 . . ? 
H8B N8 H8C 109.5 . . ? 
C2 C1 N1 114.4(7) . . ? 
C2 C1 H1D 108.7 . . ? 
N1 C1 H1D 108.5 . . ? 
C2 C1 H1E 108.8 . . ? 
N1 C1 H1E 108.7 . . ? 
H1D C1 H1E 107.6 . . ? 
C1 C2 N2 113.9(7) . . ? 
C1 C2 H2C 108.8 . . ? 
N2 C2 H2C 108.7 . . ? 
C1 C2 H2D 108.8 . . ? 
N2 C2 H2D 108.7 . . ? 
H2C C2 H2D 107.7 . . ? 
C4 C3 N2 111.6(8) . . ? 
C4 C3 H3A 109.2 . . ? 
N2 C3 H3A 109.2 . . ? 
C4 C3 H3B 109.8 . . ? 
N2 C3 H3B 109.3 . . ? 
H3A C3 H3B 107.7 . . ? 
N3 C4 C3 118.7(13) . . ? 
N3 C4 N3' 40.9(13) . . ? 
C3 C4 N3' 108.1(12) . . ? 
N3 C4 H4D 45(10) . . ? 
C3 C4 H4D 118(10) . . ? 
N3' C4 H4D 12(10) . . ? 
N3 C4 H4E 127(10) . . ? 
C3 C4 H4E 112(10) . . ? 
N3' C4 H4E 111(10) . . ? 
H4D C4 H4E 99(10) . . ? 
N3' C5 C6 110.1(13) . . ? 
N3' C5 N3 43.4(10) . . ? 
C6 C5 N3 128.9(12) . . ? 
N3' C5 H5D 82.4(19) . . ? 
C6 C5 H5D 83.1(10) . . ? 
N3 C5 H5D 121(2) . . ? 
N3' C5 H5E 114.6(16) . . ? 
C6 C5 H5E 129(2) . . ? 
N3 C5 H5E 75.9(13) . . ? 
H5D C5 H5E 125.2(15) . . ? 
C5 C6 N4 115.1(9) . . ? 
C5 C6 H5D 31.8(6) . . ? 
N4 C6 H5D 133.6(9) . . ? 
C5 C6 H6C 108.5 . . ? 
N4 C6 H6C 108.7 . . ? 
H5D C6 H6C 77.4 . . ? 
C5 C6 H6D 108.1 . . ? 
N4 C6 H6D 108.5 . . ? 
H5D C6 H6D 113.1 . . ? 
H6C C6 H6D 107.7 . . ? 
N5 C7 C8 113.5(8) . . ? 
N5 C7 H7C 109.1 . . ? 
C8 C7 H7C 108.9 . . ? 
N5 C7 H7D 108.9 . . ? 
C8 C7 H7D 108.7 . . ? 
H7C C7 H7D 107.6 . . ? 
C7 C8 N6 115.6(9) . . ? 
C7 C8 H8D 108.4 . . ? 
N6 C8 H8D 108.3 . . ? 
C7 C8 H8E 108.6 . . ? 
N6 C8 H8E 108.4 . . ? 
H8D C8 H8E 107.3 . . ? 
N6 C9 C10 111.6(8) . . ? 
N6 C9 H9A 109.3 . . ? 
C10 C9 H9A 109.4 . . ? 
N6 C9 H9B 109.2 . . ? 
C10 C9 H9B 109.1 . . ? 
H9A C9 H9B 108.2 . . ? 
N7 C10 C9 107.6(8) . . ? 
N7 C10 H10A 110.1 . . ? 
C9 C10 H10A 110.2 . . ? 
N7 C10 H10B 110.2 . . ? 
C9 C10 H10B 110.4 . . ? 
H10A C10 H10B 108.3 . . ? 
C12 C11 N7 106.7(7) . . ? 
C12 C11 H11A 110.4 . . ? 
N7 C11 H11A 110.5 . . ? 
C12 C11 H11B 110.4 . . ? 
N7 C11 H11B 110.4 . . ? 
H11A C11 H11B 108.5 . . ? 
N8 C12 C11 111.5(7) . . ? 
N8 C12 H12A 109.3 . . ? 
C11 C12 H12A 109.2 . . ? 
N8 C12 H12B 109.3 . . ? 
C11 C12 H12B 109.3 . . ? 
H12A C12 H12B 108.1 . . ? 
H51A OW1 H51B 114.9 . . ? 
H52A OW2 H52B 114.7 . . ? 
H53A OW3 H53B 114.0 . . ? 
N10 C14 H54A 111.1 5_576 . ? 
N10 C14 H54B 112.3 5_576 . ? 
H54A C14 H54B 107.2 . . ? 
N10 C14 H54C 112.0 5_576 . ? 
H54A C14 H54C 106.9 . . ? 
H54B C14 H54C 107.0 . . ? 
H55A OW4 H55B 114.4 . . ? 
H56A OW5 H56B 115.4 . . ? 
N9 C13 H57A 112.6 7_576 . ? 
N9 C13 H57B 112.8 7_576 . ? 
H57A C13 H57B 106.2 . . ? 
N9 C13 H57C 112.6 7_576 . ? 
H57A C13 H57C 106.2 . . ? 
H57B C13 H57C 105.9 . . ? 
H58A OW6 H58B 115.0 . . ? 
C13 N9 H59A 120.0 7_575 . ? 
C13 N9 H59C 120.0 7_575 . ? 
H59A N9 H59C 120.0 . . ? 
C14 N10 H60B 119.5 5_576 . ? 
C14 N10 H60C 120.5 5_576 . ? 
H60B N10 H60C 120.0 . . ? 
 
_diffrn_measured_fraction_theta_max    0.980 
_diffrn_reflns_theta_full              23.29 
_diffrn_measured_fraction_theta_full   0.980 
_refine_diff_density_max    1.749 
_refine_diff_density_min   -0.648 
_refine_diff_density_rms    0.129 
#=======================================================================