# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_address
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_address     
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_phone       '+91-512-259 7259'
#TrackingRef '- Dalton.cif'

_publ_contact_author_name        V.Chandrasekhar
_publ_author_name                V.Chandrasekhar

data_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 835460'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 Cl12 N16 O16 P4 V4'
_chemical_formula_sum            'C44 H64 Cl12 N16 O16 P4 V4'
_chemical_formula_weight         1826.16

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   15.595(4)
_cell_length_b                   15.799(3)
_cell_length_c                   30.128(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7423(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6869
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3696
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            39354
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.50
_reflns_number_total             13685
_reflns_number_gt                12578
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0442P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(14)
_refine_ls_number_reflns         13685
_refine_ls_number_parameters     881
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.5825(2) 1.1189(2) 0.20821(11) 0.0224(8) Uani 1 1 d . . .
C2 C 0.6621(2) 1.0825(2) 0.21870(12) 0.0271(8) Uani 1 1 d . . .
H2 H 0.7012 1.1018 0.2397 0.032 Uiso 1 1 calc R . .
C3 C 0.6708(2) 1.0125(2) 0.19167(12) 0.0228(8) Uani 1 1 d . . .
C4 C 0.7401(2) 0.9464(2) 0.18917(14) 0.0318(9) Uani 1 1 d . . .
H4A H 0.7295 0.9034 0.2110 0.048 Uiso 1 1 calc R . .
H4B H 0.7948 0.9722 0.1948 0.048 Uiso 1 1 calc R . .
H4C H 0.7403 0.9214 0.1601 0.048 Uiso 1 1 calc R . .
C5 C 0.5410(2) 1.1942(2) 0.22757(12) 0.0266(8) Uani 1 1 d . . .
H5A H 0.5431 1.2400 0.2066 0.040 Uiso 1 1 calc R . .
H5B H 0.5706 1.2103 0.2542 0.040 Uiso 1 1 calc R . .
H5C H 0.4824 1.1813 0.2345 0.040 Uiso 1 1 calc R . .
C6 C 0.5873(2) 1.1111(2) 0.06369(11) 0.0201(7) Uani 1 1 d . . .
C7 C 0.6087(2) 1.0744(2) 0.02316(12) 0.0282(9) Uani 1 1 d . . .
H7 H 0.6555 1.0879 0.0054 0.034 Uiso 1 1 calc R . .
C8 C 0.5466(2) 1.0141(2) 0.01449(11) 0.0222(8) Uani 1 1 d . . .
C9 C 0.5317(3) 0.9551(3) -0.02315(13) 0.0343(10) Uani 1 1 d . . .
H9A H 0.4906 0.9130 -0.0145 0.051 Uiso 1 1 calc R . .
H9B H 0.5847 0.9281 -0.0310 0.051 Uiso 1 1 calc R . .
H9C H 0.5102 0.9862 -0.0482 0.051 Uiso 1 1 calc R . .
C10 C 0.6338(2) 1.1775(2) 0.08974(12) 0.0274(8) Uani 1 1 d . . .
H10A H 0.5930 1.2153 0.1030 0.041 Uiso 1 1 calc R . .
H10B H 0.6710 1.2087 0.0703 0.041 Uiso 1 1 calc R . .
H10C H 0.6672 1.1510 0.1126 0.041 Uiso 1 1 calc R . .
C11 C 0.2119(2) 0.8746(2) -0.05705(11) 0.0264(8) Uani 1 1 d . . .
C12 C 0.1335(2) 0.8958(2) -0.07651(11) 0.0236(8) Uani 1 1 d . . .
H12 H 0.1231 0.9058 -0.1064 0.028 Uiso 1 1 calc R . .
C13 C 0.0744(2) 0.8990(2) -0.04221(11) 0.0228(8) Uani 1 1 d . . .
C14 C -0.0197(3) 0.9154(3) -0.04117(13) 0.0348(10) Uani 1 1 d . . .
H14A H -0.0499 0.8626 -0.0393 0.052 Uiso 1 1 calc R . .
H14B H -0.0364 0.9447 -0.0677 0.052 Uiso 1 1 calc R . .
H14C H -0.0333 0.9496 -0.0158 0.052 Uiso 1 1 calc R . .
C15 C 0.2964(3) 0.8649(3) -0.07959(12) 0.0418(11) Uani 1 1 d . . .
H15A H 0.3351 0.9077 -0.0691 0.063 Uiso 1 1 calc R . .
H15B H 0.2889 0.8708 -0.1111 0.063 Uiso 1 1 calc R . .
H15C H 0.3195 0.8100 -0.0732 0.063 Uiso 1 1 calc R . .
C16 C 0.2558(2) 0.6464(2) 0.03369(11) 0.0209(7) Uani 1 1 d . . .
C17 C 0.2472(2) 0.5793(2) 0.06350(11) 0.0229(8) Uani 1 1 d . . .
H17 H 0.2451 0.5220 0.0565 0.028 Uiso 1 1 calc R . .
C18 C 0.2422(2) 0.6143(2) 0.10527(11) 0.0215(7) Uani 1 1 d . . .
C19 C 0.2330(3) 0.5781(2) 0.15024(12) 0.0318(9) Uani 1 1 d . . .
H19A H 0.2887 0.5651 0.1620 0.048 Uiso 1 1 calc R . .
H19B H 0.1993 0.5274 0.1488 0.048 Uiso 1 1 calc R . .
H19C H 0.2051 0.6185 0.1692 0.048 Uiso 1 1 calc R . .
C20 C 0.2614(3) 0.6447(2) -0.01585(12) 0.0315(9) Uani 1 1 d . . .
H20A H 0.2072 0.6609 -0.0283 0.047 Uiso 1 1 calc R . .
H20B H 0.2758 0.5885 -0.0255 0.047 Uiso 1 1 calc R . .
H20C H 0.3049 0.6835 -0.0255 0.047 Uiso 1 1 calc R . .
C21 C 0.3165(2) 0.8606(2) 0.31858(11) 0.0247(8) Uani 1 1 d . . .
C22 C 0.3883(2) 0.8968(2) 0.33911(11) 0.0259(8) Uani 1 1 d . . .
H22 H 0.3999 0.8981 0.3694 0.031 Uiso 1 1 calc R . .
C23 C 0.4380(2) 0.9300(2) 0.30609(11) 0.0233(8) Uani 1 1 d . . .
C24 C 0.5206(3) 0.9773(3) 0.30634(14) 0.0346(10) Uani 1 1 d . . .
H24A H 0.5616 0.9483 0.2881 0.052 Uiso 1 1 calc R . .
H24B H 0.5419 0.9809 0.3362 0.052 Uiso 1 1 calc R . .
H24C H 0.5115 1.0334 0.2949 0.052 Uiso 1 1 calc R . .
C25 C 0.2427(3) 0.8164(3) 0.33959(13) 0.0409(11) Uani 1 1 d . . .
H25A H 0.1903 0.8440 0.3313 0.061 Uiso 1 1 calc R . .
H25B H 0.2489 0.8180 0.3713 0.061 Uiso 1 1 calc R . .
H25C H 0.2413 0.7586 0.3298 0.061 Uiso 1 1 calc R . .
C26 C 0.0738(2) 0.7861(2) 0.26319(10) 0.0208(8) Uani 1 1 d . . .
C27 C 0.0024(2) 0.8241(3) 0.28178(14) 0.0346(10) Uani 1 1 d . . .
H27 H -0.0454 0.7969 0.2935 0.041 Uiso 1 1 calc R . .
C28 C 0.0159(3) 0.9100(3) 0.27950(16) 0.0441(11) Uani 1 1 d . . .
C29 C -0.0360(4) 0.9844(4) 0.2930(3) 0.101(3) Uani 1 1 d . . .
H29A H -0.0055 1.0160 0.3152 0.152 Uiso 1 1 calc R . .
H29B H -0.0897 0.9655 0.3050 0.152 Uiso 1 1 calc R . .
H29C H -0.0463 1.0197 0.2677 0.152 Uiso 1 1 calc R . .
C30 C 0.0889(3) 0.6940(2) 0.25560(13) 0.0348(10) Uani 1 1 d . . .
H30A H 0.0866 0.6823 0.2244 0.052 Uiso 1 1 calc R . .
H30B H 0.0455 0.6618 0.2706 0.052 Uiso 1 1 calc R . .
H30C H 0.1443 0.6787 0.2669 0.052 Uiso 1 1 calc R . .
C31 C 0.0862(3) 1.2911(2) 0.10968(12) 0.0281(9) Uani 1 1 d . . .
C32 C 0.1429(3) 1.3590(2) 0.10866(12) 0.0310(9) Uani 1 1 d . . .
H32 H 0.1293 1.4153 0.1031 0.037 Uiso 1 1 calc R . .
C33 C 0.2232(3) 1.3267(2) 0.11741(12) 0.0279(9) Uani 1 1 d . . .
C34 C 0.3096(3) 1.3656(3) 0.12316(14) 0.0363(10) Uani 1 1 d . . .
H34A H 0.3135 1.3909 0.1521 0.054 Uiso 1 1 calc R . .
H34B H 0.3182 1.4083 0.1009 0.054 Uiso 1 1 calc R . .
H34C H 0.3529 1.3228 0.1202 0.054 Uiso 1 1 calc R . .
C35 C -0.0091(3) 1.2901(3) 0.10350(14) 0.0390(11) Uani 1 1 d . . .
H35A H -0.0227 1.2648 0.0754 0.058 Uiso 1 1 calc R . .
H35B H -0.0306 1.3470 0.1042 0.058 Uiso 1 1 calc R . .
H35C H -0.0351 1.2579 0.1269 0.058 Uiso 1 1 calc R . .
C36 C -0.0340(2) 1.1298(2) 0.00934(12) 0.0289(9) Uani 1 1 d . . .
C37 C -0.1065(2) 1.1116(2) 0.03342(12) 0.0295(9) Uani 1 1 d . . .
H37 H -0.1629 1.1150 0.0235 0.035 Uiso 1 1 calc R . .
C38 C -0.0791(2) 1.0869(2) 0.07553(12) 0.0266(8) Uani 1 1 d . . .
C39 C -0.1323(3) 1.0621(3) 0.11461(14) 0.0432(11) Uani 1 1 d . . .
H39A H -0.1064 1.0145 0.1292 0.065 Uiso 1 1 calc R . .
H39B H -0.1889 1.0471 0.1048 0.065 Uiso 1 1 calc R . .
H39C H -0.1358 1.1088 0.1349 0.065 Uiso 1 1 calc R . .
C40 C -0.0197(3) 1.1593(3) -0.03722(13) 0.0405(11) Uani 1 1 d . . .
H40A H 0.0347 1.1875 -0.0392 0.061 Uiso 1 1 calc R . .
H40B H -0.0645 1.1979 -0.0455 0.061 Uiso 1 1 calc R . .
H40C H -0.0202 1.1115 -0.0569 0.061 Uiso 1 1 calc R . .
C41 C 0.4874(2) 0.7960(2) 0.13888(12) 0.0217(8) Uani 1 1 d . . .
C42 C 0.0247(2) 0.8170(2) 0.12206(11) 0.0249(8) Uani 1 1 d . . .
C43 C 0.2789(2) 1.1289(2) 0.00872(11) 0.0208(7) Uani 1 1 d . . .
C44 C 0.2531(2) 1.1358(2) 0.24778(11) 0.0211(7) Uani 1 1 d . . .
N1 N 0.54452(17) 1.07355(17) 0.17590(9) 0.0182(6) Uani 1 1 d . . .
N2 N 0.60068(18) 1.00988(17) 0.16635(9) 0.0206(6) Uani 1 1 d . . .
H2A H 0.5919 0.9722 0.1462 0.025 Uiso 1 1 calc R . .
N3 N 0.51548(18) 1.07591(18) 0.07949(9) 0.0179(6) Uani 1 1 d . . .
N4 N 0.49371(18) 1.01622(18) 0.04862(9) 0.0198(6) Uani 1 1 d . . .
H4 H 0.4500 0.9834 0.0512 0.024 Uiso 1 1 calc R . .
N5 N 0.20196(18) 0.86450(18) -0.01314(9) 0.0193(6) Uani 1 1 d . . .
N6 N 0.11824(18) 0.88001(18) -0.00530(9) 0.0213(6) Uani 1 1 d . . .
H6A H 0.0954 0.8779 0.0207 0.026 Uiso 1 1 calc R . .
N7 N 0.25579(18) 0.72027(18) 0.05577(9) 0.0212(6) Uani 1 1 d . . .
N8 N 0.24736(18) 0.69834(18) 0.09929(9) 0.0206(6) Uani 1 1 d . . .
H8A H 0.2455 0.7345 0.1206 0.025 Uiso 1 1 calc R . .
N9 N 0.32320(17) 0.87003(18) 0.27432(9) 0.0186(6) Uani 1 1 d . . .
N10 N 0.39659(18) 0.91289(18) 0.26785(9) 0.0211(6) Uani 1 1 d . . .
H10 H 0.4151 0.9278 0.2421 0.025 Uiso 1 1 calc R . .
N11 N 0.13059(18) 0.84519(19) 0.25014(9) 0.0199(6) Uani 1 1 d . . .
N12 N 0.0944(2) 0.9203(2) 0.26010(11) 0.0336(8) Uani 1 1 d . . .
H12A H 0.1178 0.9686 0.2549 0.040 Uiso 1 1 calc R . .
N13 N 0.1293(2) 1.21913(19) 0.11800(9) 0.0231(7) Uani 1 1 d . . .
N14 N 0.2124(2) 1.24361(19) 0.12257(9) 0.0241(7) Uani 1 1 d . . .
H14 H 0.2537 1.2091 0.1282 0.029 Uiso 1 1 calc R . .
N15 N 0.00634(19) 1.08938(19) 0.07796(9) 0.0216(6) Uani 1 1 d . . .
N16 N 0.03235(19) 1.11527(18) 0.03696(9) 0.0222(6) Uani 1 1 d . . .
H16 H 0.0852 1.1216 0.0295 0.027 Uiso 1 1 calc R . .
O1 O 0.44490(15) 1.19431(14) 0.13895(7) 0.0198(5) Uani 1 1 d . . .
O2 O 0.44232(14) 0.95766(13) 0.13055(7) 0.0162(5) Uani 1 1 d . . .
O3 O 0.33991(14) 0.84502(14) 0.10194(7) 0.0182(5) Uani 1 1 d . . .
O4 O 0.35853(13) 0.86621(14) 0.18399(7) 0.0172(5) Uani 1 1 d . . .
O5 O 0.36665(15) 0.82550(14) 0.01166(7) 0.0213(5) Uani 1 1 d . . .
O6 O 0.16670(14) 0.86755(15) 0.07868(7) 0.0191(5) Uani 1 1 d . . .
O7 O 0.09781(14) 0.96467(14) 0.13630(7) 0.0192(5) Uani 1 1 d . . .
O8 O 0.18154(14) 0.83401(14) 0.15940(7) 0.0170(5) Uani 1 1 d . . .
O9 O 0.26041(15) 0.74086(14) 0.22263(7) 0.0200(5) Uani 1 1 d . . .
O10 O 0.23601(14) 0.97694(13) 0.21836(7) 0.0160(5) Uani 1 1 d . . .
O11 O 0.35876(14) 1.06725(14) 0.18813(7) 0.0163(5) Uani 1 1 d . . .
O12 O 0.20629(15) 1.09646(15) 0.16520(7) 0.0190(5) Uani 1 1 d . . .
O13 O 0.02754(16) 1.11050(17) 0.16656(8) 0.0278(6) Uani 1 1 d . . .
O14 O 0.30350(14) 0.97560(14) 0.04306(7) 0.0160(5) Uani 1 1 d . . .
O15 O 0.18134(14) 1.06744(14) 0.07274(7) 0.0166(5) Uani 1 1 d . . .
O16 O 0.33517(14) 1.09938(14) 0.09265(7) 0.0179(5) Uani 1 1 d . . .
P1 P 0.39802(5) 0.87485(5) 0.13851(3) 0.01412(17) Uani 1 1 d . . .
P2 P 0.12847(5) 0.87781(6) 0.12413(3) 0.01620(18) Uani 1 1 d . . .
P3 P 0.27349(6) 1.06068(5) 0.05989(3) 0.01522(18) Uani 1 1 d . . .
P4 P 0.26469(6) 1.06043(5) 0.20031(3) 0.01504(18) Uani 1 1 d . . .
Cl1 Cl 0.55653(6) 0.81201(6) 0.18486(4) 0.0337(2) Uani 1 1 d . . .
Cl2 Cl 0.44578(6) 0.69162(5) 0.14254(3) 0.0267(2) Uani 1 1 d . . .
Cl3 Cl 0.54789(7) 0.80693(6) 0.08912(3) 0.0392(3) Uani 1 1 d . . .
Cl4 Cl -0.03394(6) 0.82912(7) 0.17148(3) 0.0337(2) Uani 1 1 d . . .
Cl5 Cl -0.03844(6) 0.85721(7) 0.07699(3) 0.0363(2) Uani 1 1 d . . .
Cl6 Cl 0.04169(7) 0.70729(6) 0.11262(4) 0.0394(3) Uani 1 1 d . . .
Cl7 Cl 0.23540(6) 1.23118(5) 0.01908(3) 0.0277(2) Uani 1 1 d . . .
Cl8 Cl 0.21540(6) 1.08032(6) -0.03373(3) 0.0298(2) Uani 1 1 d . . .
Cl9 Cl 0.38448(6) 1.14071(6) -0.01131(3) 0.0316(2) Uani 1 1 d . . .
Cl10 Cl 0.31727(6) 1.10491(6) 0.29335(3) 0.0276(2) Uani 1 1 d . . .
Cl11 Cl 0.14415(6) 1.14118(6) 0.26522(3) 0.0308(2) Uani 1 1 d . . .
Cl12 Cl 0.28527(7) 1.23975(5) 0.23073(3) 0.0303(2) Uani 1 1 d . . .
V1 V 0.43435(3) 1.09364(3) 0.135692(17) 0.01506(12) Uani 1 1 d . . .
V2 V 0.28666(4) 0.84968(4) 0.042255(18) 0.01644(13) Uani 1 1 d . . .
V3 V 0.24914(3) 0.84040(3) 0.216249(18) 0.01490(12) Uani 1 1 d . . .
V4 V 0.09885(4) 1.08908(4) 0.130562(18) 0.01830(13) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0209(18) 0.0259(19) 0.0203(17) 0.0031(15) 0.0015(15) -0.0067(15)
C2 0.023(2) 0.032(2) 0.0262(19) 0.0026(17) -0.0076(16) -0.0070(16)
C3 0.0169(18) 0.0228(19) 0.0285(19) 0.0063(16) 0.0008(16) -0.0006(14)
C4 0.021(2) 0.026(2) 0.048(2) 0.0057(18) -0.0040(18) 0.0033(16)
C5 0.025(2) 0.029(2) 0.0259(19) -0.0069(16) -0.0030(16) -0.0045(16)
C6 0.0185(18) 0.0223(19) 0.0195(17) 0.0034(14) -0.0010(14) -0.0008(14)
C7 0.024(2) 0.037(2) 0.0242(18) -0.0008(17) 0.0099(16) -0.0094(17)
C8 0.0154(18) 0.031(2) 0.0202(17) 0.0009(15) 0.0074(15) 0.0011(15)
C9 0.029(2) 0.044(3) 0.029(2) -0.0134(18) 0.0083(18) -0.0103(19)
C10 0.027(2) 0.026(2) 0.029(2) -0.0020(16) 0.0012(16) -0.0092(16)
C11 0.030(2) 0.029(2) 0.0196(17) -0.0023(16) 0.0017(16) -0.0091(16)
C12 0.031(2) 0.026(2) 0.0140(16) 0.0005(15) -0.0015(15) -0.0064(16)
C13 0.026(2) 0.0243(19) 0.0179(17) -0.0038(15) -0.0044(15) -0.0025(15)
C14 0.038(2) 0.044(3) 0.0224(19) -0.0055(18) -0.0068(18) 0.008(2)
C15 0.030(2) 0.077(3) 0.0192(19) 0.002(2) 0.0054(17) -0.009(2)
C16 0.0146(17) 0.0207(18) 0.0273(18) -0.0067(15) 0.0019(14) -0.0033(14)
C17 0.0168(18) 0.0208(18) 0.0312(19) -0.0063(15) 0.0006(15) -0.0014(14)
C18 0.0153(17) 0.0211(18) 0.0281(19) 0.0000(15) 0.0015(15) -0.0044(14)
C19 0.041(2) 0.024(2) 0.031(2) -0.0017(17) -0.0011(18) -0.0074(17)
C20 0.035(2) 0.031(2) 0.029(2) -0.0092(17) 0.0041(18) -0.0013(18)
C21 0.026(2) 0.029(2) 0.0188(17) 0.0034(16) -0.0017(15) 0.0049(16)
C22 0.030(2) 0.033(2) 0.0155(16) 0.0031(16) -0.0106(16) 0.0018(17)
C23 0.026(2) 0.0240(19) 0.0199(18) -0.0018(15) -0.0080(16) 0.0027(16)
C24 0.034(2) 0.036(2) 0.034(2) -0.0002(18) -0.0115(19) -0.0077(19)
C25 0.039(2) 0.061(3) 0.022(2) 0.0136(19) -0.0008(19) -0.013(2)
C26 0.0217(19) 0.028(2) 0.0127(16) 0.0040(14) -0.0004(14) -0.0033(15)
C27 0.023(2) 0.039(2) 0.042(2) 0.0069(19) 0.0082(18) -0.0039(17)
C28 0.033(2) 0.041(3) 0.058(3) 0.011(2) 0.028(2) 0.010(2)
C29 0.076(4) 0.049(3) 0.179(7) 0.026(4) 0.093(5) 0.028(3)
C30 0.035(2) 0.032(2) 0.037(2) -0.0015(18) 0.0123(19) -0.0109(18)
C31 0.038(2) 0.026(2) 0.0201(18) -0.0037(16) -0.0074(17) 0.0158(17)
C32 0.047(2) 0.020(2) 0.0262(19) -0.0030(16) -0.0060(18) 0.0104(18)
C33 0.040(2) 0.0195(19) 0.0244(19) -0.0015(15) 0.0021(17) 0.0046(16)
C34 0.036(2) 0.024(2) 0.049(3) 0.0040(19) 0.006(2) 0.0030(18)
C35 0.043(3) 0.034(2) 0.039(2) -0.012(2) -0.022(2) 0.0188(19)
C36 0.030(2) 0.034(2) 0.0235(19) 0.0012(17) -0.0068(17) 0.0034(17)
C37 0.0163(18) 0.036(2) 0.037(2) -0.0021(18) -0.0079(17) 0.0072(16)
C38 0.020(2) 0.028(2) 0.032(2) 0.0051(17) -0.0028(16) 0.0027(16)
C39 0.023(2) 0.068(3) 0.039(2) 0.018(2) -0.0009(19) 0.002(2)
C40 0.035(2) 0.063(3) 0.024(2) 0.007(2) -0.0100(18) 0.009(2)
C41 0.0246(19) 0.0155(17) 0.0250(18) 0.0035(15) 0.0049(15) -0.0004(14)
C42 0.0206(19) 0.031(2) 0.0230(19) 0.0032(16) -0.0056(15) -0.0055(16)
C43 0.0194(18) 0.0253(19) 0.0176(17) 0.0034(15) 0.0015(14) 0.0011(15)
C44 0.0214(18) 0.0245(18) 0.0174(16) 0.0036(14) 0.0005(14) 0.0043(15)
N1 0.0133(14) 0.0192(15) 0.0222(15) 0.0006(12) 0.0010(12) -0.0051(12)
N2 0.0186(16) 0.0188(15) 0.0244(15) -0.0028(12) -0.0048(13) -0.0010(12)
N3 0.0179(15) 0.0196(15) 0.0163(14) -0.0015(12) 0.0018(12) -0.0038(12)
N4 0.0207(16) 0.0210(15) 0.0178(15) -0.0005(12) 0.0024(13) -0.0072(12)
N5 0.0193(15) 0.0218(15) 0.0169(14) -0.0048(12) 0.0007(12) -0.0038(12)
N6 0.0224(16) 0.0254(16) 0.0161(14) 0.0011(12) 0.0053(12) -0.0003(13)
N7 0.0188(15) 0.0240(16) 0.0208(15) -0.0039(13) 0.0014(13) -0.0019(12)
N8 0.0244(16) 0.0175(15) 0.0200(14) -0.0027(12) 0.0011(13) -0.0027(12)
N9 0.0167(14) 0.0204(15) 0.0187(14) 0.0007(12) -0.0008(12) 0.0025(12)
N10 0.0214(16) 0.0221(16) 0.0199(14) 0.0036(13) -0.0010(13) -0.0031(13)
N11 0.0186(15) 0.0256(16) 0.0154(14) 0.0048(12) 0.0008(12) 0.0028(13)
N12 0.0262(18) 0.0240(17) 0.051(2) 0.0074(15) 0.0188(16) 0.0064(14)
N13 0.0275(17) 0.0243(16) 0.0176(15) -0.0006(13) -0.0042(13) 0.0077(13)
N14 0.0265(17) 0.0237(16) 0.0220(16) 0.0027(13) 0.0025(13) 0.0055(13)
N15 0.0203(16) 0.0267(17) 0.0178(15) 0.0012(13) -0.0016(12) 0.0025(13)
N16 0.0179(15) 0.0305(17) 0.0182(14) -0.0011(13) -0.0012(12) 0.0006(13)
O1 0.0209(13) 0.0195(12) 0.0191(12) -0.0007(10) -0.0021(10) -0.0015(10)
O2 0.0175(12) 0.0139(11) 0.0172(11) 0.0006(9) 0.0019(10) -0.0007(9)
O3 0.0198(12) 0.0179(12) 0.0169(11) -0.0009(10) -0.0012(10) -0.0019(10)
O4 0.0143(11) 0.0201(12) 0.0172(11) 0.0026(10) 0.0003(9) -0.0031(10)
O5 0.0229(13) 0.0239(13) 0.0171(12) -0.0035(10) 0.0024(10) -0.0030(10)
O6 0.0183(12) 0.0214(13) 0.0175(11) 0.0005(10) 0.0018(10) -0.0022(10)
O7 0.0190(12) 0.0228(13) 0.0157(11) 0.0036(10) 0.0000(10) 0.0037(10)
O8 0.0146(11) 0.0227(13) 0.0138(11) 0.0024(9) -0.0001(9) -0.0017(10)
O9 0.0186(12) 0.0234(13) 0.0180(12) 0.0021(10) -0.0017(10) -0.0017(10)
O10 0.0164(12) 0.0166(11) 0.0149(11) 0.0020(9) 0.0008(10) 0.0030(9)
O11 0.0166(12) 0.0174(12) 0.0148(11) 0.0003(9) 0.0012(10) -0.0003(9)
O12 0.0202(12) 0.0222(12) 0.0146(11) 0.0003(10) 0.0015(10) 0.0041(10)
O13 0.0233(14) 0.0383(15) 0.0217(12) 0.0010(11) 0.0030(11) 0.0079(11)
O14 0.0146(12) 0.0177(12) 0.0156(11) 0.0000(9) -0.0002(9) 0.0005(10)
O15 0.0157(12) 0.0198(12) 0.0143(11) 0.0028(9) -0.0020(9) 0.0000(10)
O16 0.0183(12) 0.0205(13) 0.0149(11) 0.0016(10) -0.0022(9) 0.0003(10)
P1 0.0122(4) 0.0140(4) 0.0161(4) -0.0005(3) 0.0014(3) 0.0000(3)
P2 0.0124(4) 0.0204(4) 0.0158(4) 0.0014(3) 0.0005(3) -0.0013(3)
P3 0.0161(4) 0.0169(4) 0.0127(4) 0.0015(3) 0.0011(3) -0.0007(3)
P4 0.0164(4) 0.0153(4) 0.0134(4) -0.0008(3) 0.0008(3) 0.0025(3)
Cl1 0.0214(5) 0.0273(5) 0.0525(6) 0.0124(4) -0.0139(4) -0.0026(4)
Cl2 0.0300(5) 0.0157(4) 0.0346(5) 0.0013(4) 0.0040(4) 0.0012(4)
Cl3 0.0397(6) 0.0309(5) 0.0469(6) 0.0105(5) 0.0287(5) 0.0137(5)
Cl4 0.0199(5) 0.0553(7) 0.0258(5) 0.0086(4) 0.0041(4) -0.0079(4)
Cl5 0.0193(5) 0.0636(7) 0.0258(5) 0.0121(5) -0.0079(4) -0.0085(5)
Cl6 0.0313(5) 0.0319(6) 0.0549(6) -0.0041(5) -0.0047(5) -0.0128(4)
Cl7 0.0384(5) 0.0203(4) 0.0244(4) 0.0070(4) 0.0011(4) 0.0036(4)
Cl8 0.0401(6) 0.0326(5) 0.0168(4) 0.0025(4) -0.0062(4) -0.0040(4)
Cl9 0.0275(5) 0.0367(5) 0.0307(5) 0.0125(4) 0.0110(4) -0.0030(4)
Cl10 0.0335(5) 0.0326(5) 0.0168(4) -0.0035(4) -0.0061(4) 0.0062(4)
Cl11 0.0244(5) 0.0386(6) 0.0295(5) -0.0079(4) 0.0066(4) 0.0090(4)
Cl12 0.0466(6) 0.0175(4) 0.0269(5) -0.0030(4) 0.0009(4) 0.0011(4)
V1 0.0149(3) 0.0144(3) 0.0159(3) -0.0002(2) 0.0005(2) -0.0008(2)
V2 0.0156(3) 0.0175(3) 0.0162(3) -0.0013(2) 0.0014(2) -0.0017(2)
V3 0.0140(3) 0.0162(3) 0.0145(3) 0.0021(2) 0.0005(2) 0.0004(2)
V4 0.0172(3) 0.0218(3) 0.0159(3) 0.0013(2) 0.0003(2) 0.0055(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
C1 N1 1.346(4) . ?
C1 C2 1.404(5) . ?
C1 C5 1.474(5) . ?
C2 C3 1.380(5) . ?
C2 H2 0.9300 . ?
C3 N2 1.334(4) . ?
C3 C4 1.505(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.338(4) . ?
C6 C7 1.392(5) . ?
C6 C10 1.498(5) . ?
C7 C8 1.383(5) . ?
C7 H7 0.9300 . ?
C8 N4 1.319(4) . ?
C8 C9 1.486(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N5 1.341(4) . ?
C11 C12 1.397(5) . ?
C11 C15 1.490(5) . ?
C12 C13 1.385(5) . ?
C12 H12 0.9300 . ?
C13 N6 1.339(4) . ?
C13 C14 1.491(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N7 1.343(4) . ?
C16 C17 1.396(5) . ?
C16 C20 1.495(5) . ?
C17 C18 1.376(5) . ?
C17 H17 0.9300 . ?
C18 N8 1.342(4) . ?
C18 C19 1.477(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N9 1.346(4) . ?
C21 C22 1.402(5) . ?
C21 C25 1.487(5) . ?
C22 C23 1.365(5) . ?
C22 H22 0.9300 . ?
C23 N10 1.348(4) . ?
C23 C24 1.490(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N11 1.345(4) . ?
C26 C27 1.383(5) . ?
C26 C30 1.492(5) . ?
C27 C28 1.375(6) . ?
C27 H27 0.9300 . ?
C28 N12 1.366(5) . ?
C28 C29 1.484(6) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N13 1.344(4) . ?
C31 C32 1.391(6) . ?
C31 C35 1.499(6) . ?
C32 C33 1.378(6) . ?
C32 H32 0.9300 . ?
C33 N14 1.332(5) . ?
C33 C34 1.491(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N16 1.348(4) . ?
C36 C37 1.374(5) . ?
C36 C40 1.495(5) . ?
C37 C38 1.394(5) . ?
C37 H37 0.9300 . ?
C38 N15 1.335(5) . ?
C38 C39 1.493(5) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 Cl1 1.774(4) . ?
C41 Cl2 1.776(3) . ?
C41 Cl3 1.780(4) . ?
C41 P1 1.869(3) . ?
C42 Cl4 1.758(4) . ?
C42 Cl6 1.776(4) . ?
C42 Cl5 1.794(4) . ?
C42 P2 1.884(4) . ?
C43 Cl9 1.763(4) . ?
C43 Cl7 1.780(4) . ?
C43 Cl8 1.791(3) . ?
C43 P3 1.883(3) . ?
C44 Cl10 1.768(3) . ?
C44 Cl11 1.780(4) . ?
C44 Cl12 1.792(4) . ?
C44 P4 1.870(4) . ?
N1 N2 1.365(4) . ?
N1 V1 2.126(3) . ?
N2 H2A 0.8600 . ?
N3 N4 1.367(4) . ?
N3 V1 2.132(3) . ?
N4 H4 0.8600 . ?
N5 N6 1.349(4) . ?
N5 V2 2.141(3) . ?
N6 H6A 0.8600 . ?
N7 N8 1.362(4) . ?
N7 V2 2.140(3) . ?
N8 H8A 0.8600 . ?
N9 N10 1.344(4) . ?
N9 V3 2.148(3) . ?
N10 H10 0.8600 . ?
N11 N12 1.347(4) . ?
N11 V3 2.113(3) . ?
N12 H12A 0.8600 . ?
N13 N14 1.359(4) . ?
N13 V4 2.143(3) . ?
N14 H14 0.8600 . ?
N15 N16 1.363(4) . ?
N15 V4 2.143(3) . ?
N16 H16 0.8600 . ?
O1 V1 1.602(2) . ?
O2 P1 1.499(2) . ?
O2 V1 2.157(2) . ?
O3 P1 1.502(2) . ?
O3 V2 1.982(2) . ?
O4 P1 1.508(2) . ?
O4 V3 2.005(2) . ?
O5 V2 1.597(2) . ?
O6 P2 1.502(2) . ?
O6 V2 2.187(2) . ?
O7 P2 1.499(2) . ?
O7 V4 1.973(2) . ?
O8 P2 1.514(2) . ?
O8 V3 2.014(2) . ?
O9 V3 1.594(2) . ?
O10 P4 1.495(2) . ?
O10 V3 2.168(2) . ?
O11 P4 1.516(2) . ?
O11 V1 2.015(2) . ?
O12 P4 1.507(2) . ?
O12 V4 1.978(2) . ?
O13 V4 1.590(2) . ?
O14 P3 1.511(2) . ?
O14 V2 2.007(2) . ?
O15 P3 1.492(2) . ?
O15 V4 2.192(2) . ?
O16 P3 1.508(2) . ?
O16 V1 2.020(2) . ?

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
N1 C1 C2 109.5(3) . . ?
N1 C1 C5 121.5(3) . . ?
C2 C1 C5 129.0(3) . . ?
C3 C2 C1 106.4(3) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
N2 C3 C2 106.4(3) . . ?
N2 C3 C4 122.6(3) . . ?
C2 C3 C4 131.0(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C7 109.9(3) . . ?
N3 C6 C10 120.7(3) . . ?
C7 C6 C10 129.4(3) . . ?
C8 C7 C6 106.5(3) . . ?
C8 C7 H7 126.7 . . ?
C6 C7 H7 126.7 . . ?
N4 C8 C7 105.8(3) . . ?
N4 C8 C9 120.9(3) . . ?
C7 C8 C9 133.3(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 C12 109.9(3) . . ?
N5 C11 C15 122.7(3) . . ?
C12 C11 C15 127.4(3) . . ?
C13 C12 C11 106.1(3) . . ?
C13 C12 H12 126.9 . . ?
C11 C12 H12 126.9 . . ?
N6 C13 C12 105.8(3) . . ?
N6 C13 C14 121.6(3) . . ?
C12 C13 C14 132.6(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N7 C16 C17 109.9(3) . . ?
N7 C16 C20 120.7(3) . . ?
C17 C16 C20 129.4(3) . . ?
C18 C17 C16 106.8(3) . . ?
C18 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
N8 C18 C17 105.7(3) . . ?
N8 C18 C19 120.8(3) . . ?
C17 C18 C19 133.5(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N9 C21 C22 109.2(3) . . ?
N9 C21 C25 122.3(3) . . ?
C22 C21 C25 128.5(3) . . ?
C23 C22 C21 106.8(3) . . ?
C23 C22 H22 126.6 . . ?
C21 C22 H22 126.6 . . ?
N10 C23 C22 105.9(3) . . ?
N10 C23 C24 121.3(3) . . ?
C22 C23 C24 132.8(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N11 C26 C27 110.3(3) . . ?
N11 C26 C30 121.9(3) . . ?
C27 C26 C30 127.8(3) . . ?
C28 C27 C26 106.5(3) . . ?
C28 C27 H27 126.7 . . ?
C26 C27 H27 126.7 . . ?
N12 C28 C27 106.0(4) . . ?
N12 C28 C29 120.8(4) . . ?
C27 C28 C29 133.2(4) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N13 C31 C32 109.8(3) . . ?
N13 C31 C35 120.7(4) . . ?
C32 C31 C35 129.5(3) . . ?
C33 C32 C31 106.7(3) . . ?
C33 C32 H32 126.6 . . ?
C31 C32 H32 126.6 . . ?
N14 C33 C32 105.8(3) . . ?
N14 C33 C34 120.5(3) . . ?
C32 C33 C34 133.7(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N16 C36 C37 105.7(3) . . ?
N16 C36 C40 121.2(3) . . ?
C37 C36 C40 133.1(3) . . ?
C36 C37 C38 106.7(3) . . ?
C36 C37 H37 126.7 . . ?
C38 C37 H37 126.7 . . ?
N15 C38 C37 110.4(3) . . ?
N15 C38 C39 121.3(3) . . ?
C37 C38 C39 128.4(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 H40A 109.5 . . ?
C36 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C36 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Cl1 C41 Cl2 107.80(18) . . ?
Cl1 C41 Cl3 108.76(19) . . ?
Cl2 C41 Cl3 109.62(19) . . ?
Cl1 C41 P1 111.30(18) . . ?
Cl2 C41 P1 110.29(19) . . ?
Cl3 C41 P1 109.03(18) . . ?
Cl4 C42 Cl6 108.67(19) . . ?
Cl4 C42 Cl5 108.5(2) . . ?
Cl6 C42 Cl5 107.86(19) . . ?
Cl4 C42 P2 111.28(19) . . ?
Cl6 C42 P2 112.0(2) . . ?
Cl5 C42 P2 108.40(19) . . ?
Cl9 C43 Cl7 108.66(19) . . ?
Cl9 C43 Cl8 108.50(18) . . ?
Cl7 C43 Cl8 107.67(18) . . ?
Cl9 C43 P3 112.49(18) . . ?
Cl7 C43 P3 111.03(17) . . ?
Cl8 C43 P3 108.33(18) . . ?
Cl10 C44 Cl11 108.93(18) . . ?
Cl10 C44 Cl12 108.49(19) . . ?
Cl11 C44 Cl12 107.96(18) . . ?
Cl10 C44 P4 111.29(18) . . ?
Cl11 C44 P4 110.39(19) . . ?
Cl12 C44 P4 109.70(17) . . ?
C1 N1 N2 105.2(3) . . ?
C1 N1 V1 133.5(2) . . ?
N2 N1 V1 120.6(2) . . ?
C3 N2 N1 112.5(3) . . ?
C3 N2 H2A 123.8 . . ?
N1 N2 H2A 123.8 . . ?
C6 N3 N4 104.6(3) . . ?
C6 N3 V1 136.5(2) . . ?
N4 N3 V1 118.9(2) . . ?
C8 N4 N3 113.1(3) . . ?
C8 N4 H4 123.4 . . ?
N3 N4 H4 123.4 . . ?
C11 N5 N6 105.3(3) . . ?
C11 N5 V2 135.3(2) . . ?
N6 N5 V2 118.7(2) . . ?
C13 N6 N5 112.9(3) . . ?
C13 N6 H6A 123.6 . . ?
N5 N6 H6A 123.6 . . ?
C16 N7 N8 104.8(3) . . ?
C16 N7 V2 137.4(2) . . ?
N8 N7 V2 116.6(2) . . ?
C18 N8 N7 112.7(3) . . ?
C18 N8 H8A 123.6 . . ?
N7 N8 H8A 123.6 . . ?
N10 N9 C21 105.4(3) . . ?
N10 N9 V3 116.7(2) . . ?
C21 N9 V3 137.8(2) . . ?
N9 N10 C23 112.6(3) . . ?
N9 N10 H10 123.7 . . ?
C23 N10 H10 123.7 . . ?
C26 N11 N12 105.7(3) . . ?
C26 N11 V3 133.8(2) . . ?
N12 N11 V3 120.4(2) . . ?
N11 N12 C28 111.4(3) . . ?
N11 N12 H12A 124.3 . . ?
C28 N12 H12A 124.3 . . ?
C31 N13 N14 104.8(3) . . ?
C31 N13 V4 137.1(3) . . ?
N14 N13 V4 117.8(2) . . ?
C33 N14 N13 112.9(3) . . ?
C33 N14 H14 123.6 . . ?
N13 N14 H14 123.6 . . ?
C38 N15 N16 104.8(3) . . ?
C38 N15 V4 135.4(2) . . ?
N16 N15 V4 118.1(2) . . ?
C36 N16 N15 112.5(3) . . ?
C36 N16 H16 123.8 . . ?
N15 N16 H16 123.8 . . ?
P1 O2 V1 146.21(14) . . ?
P1 O3 V2 155.01(15) . . ?
P1 O4 V3 143.71(14) . . ?
P2 O6 V2 144.17(14) . . ?
P2 O7 V4 152.64(15) . . ?
P2 O8 V3 149.32(14) . . ?
P4 O10 V3 147.03(14) . . ?
P4 O11 V1 140.41(14) . . ?
P4 O12 V4 149.31(15) . . ?
P3 O14 V2 147.71(14) . . ?
P3 O15 V4 141.48(13) . . ?
P3 O16 V1 152.92(15) . . ?
O2 P1 O3 115.74(13) . . ?
O2 P1 O4 114.37(13) . . ?
O3 P1 O4 113.05(13) . . ?
O2 P1 C41 103.82(14) . . ?
O3 P1 C41 104.19(14) . . ?
O4 P1 C41 103.82(14) . . ?
O7 P2 O6 116.64(13) . . ?
O7 P2 O8 114.91(13) . . ?
O6 P2 O8 111.92(13) . . ?
O7 P2 C42 101.61(15) . . ?
O6 P2 C42 104.81(15) . . ?
O8 P2 C42 105.05(14) . . ?
O15 P3 O16 114.56(13) . . ?
O15 P3 O14 116.69(13) . . ?
O16 P3 O14 112.50(13) . . ?
O15 P3 C43 102.39(14) . . ?
O16 P3 C43 105.97(14) . . ?
O14 P3 C43 102.74(14) . . ?
O10 P4 O12 114.06(13) . . ?
O10 P4 O11 116.11(13) . . ?
O12 P4 O11 112.83(13) . . ?
O10 P4 C44 104.76(14) . . ?
O12 P4 C44 103.74(14) . . ?
O11 P4 C44 103.51(14) . . ?
O1 V1 O11 102.56(10) . . ?
O1 V1 O16 94.21(11) . . ?
O11 V1 O16 93.71(9) . . ?
O1 V1 N1 91.73(11) . . ?
O11 V1 N1 89.72(10) . . ?
O16 V1 N1 172.33(10) . . ?
O1 V1 N3 96.79(11) . . ?
O11 V1 N3 160.51(10) . . ?
O16 V1 N3 87.16(10) . . ?
N1 V1 N3 87.33(11) . . ?
O1 V1 O2 170.78(11) . . ?
O11 V1 O2 83.34(9) . . ?
O16 V1 O2 92.45(9) . . ?
N1 V1 O2 81.13(10) . . ?
N3 V1 O2 77.17(10) . . ?
O5 V2 O3 100.80(11) . . ?
O5 V2 O14 98.15(11) . . ?
O3 V2 O14 88.34(9) . . ?
O5 V2 N7 93.27(11) . . ?
O3 V2 N7 83.46(10) . . ?
O14 V2 N7 167.02(10) . . ?
O5 V2 N5 93.33(11) . . ?
O3 V2 N5 165.85(10) . . ?
O14 V2 N5 88.96(10) . . ?
N7 V2 N5 96.55(11) . . ?
O5 V2 O6 171.24(11) . . ?
O3 V2 O6 84.72(9) . . ?
O14 V2 O6 88.74(9) . . ?
N7 V2 O6 80.52(10) . . ?
N5 V2 O6 81.34(10) . . ?
O9 V3 O4 99.51(11) . . ?
O9 V3 O8 96.36(10) . . ?
O4 V3 O8 92.48(9) . . ?
O9 V3 N11 94.21(12) . . ?
O4 V3 N11 166.20(11) . . ?
O8 V3 N11 87.41(10) . . ?
O9 V3 N9 93.30(11) . . ?
O4 V3 N9 83.86(10) . . ?
O8 V3 N9 170.13(10) . . ?
N11 V3 N9 93.96(11) . . ?
O9 V3 O10 171.34(10) . . ?
O4 V3 O10 83.82(9) . . ?
O8 V3 O10 91.46(9) . . ?
N11 V3 O10 82.39(10) . . ?
N9 V3 O10 79.05(10) . . ?
O13 V4 O7 98.43(12) . . ?
O13 V4 O12 102.71(11) . . ?
O7 V4 O12 91.12(10) . . ?
O13 V4 N13 94.11(12) . . ?
O7 V4 N13 166.53(11) . . ?
O12 V4 N13 81.29(10) . . ?
O13 V4 N15 91.90(12) . . ?
O7 V4 N15 93.52(10) . . ?
O12 V4 N15 163.85(10) . . ?
N13 V4 N15 90.96(11) . . ?
O13 V4 O15 170.31(11) . . ?
O7 V4 O15 85.36(9) . . ?
O12 V4 O15 86.06(9) . . ?
N13 V4 O15 83.05(10) . . ?
N15 V4 O15 78.92(10) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.075

#===END

data_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 835461'
#TrackingRef '- Dalton.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H68 N8 O16 P4 V4'
_chemical_formula_sum            'C36 H68 N8 O16 P4 V4'
_chemical_formula_weight         1196.63

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'
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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   14.365(4)
_cell_length_b                   12.815(3)
_cell_length_c                   30.310(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.245(5)
_cell_angle_gamma                90.00
_cell_volume                     5580(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4889
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      25.98

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            32576
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.00
_reflns_number_total             11963
_reflns_number_gt                8431
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0657P)^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         11963
_refine_ls_number_parameters     633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1433
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_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
C1 C 1.1330(2) 0.1467(3) 0.86343(12) 0.0221(8) Uani 1 1 d . . .
C2 C 1.1583(2) 0.1215(3) 0.90982(12) 0.0309(9) Uani 1 1 d . . .
H2A H 1.1290 0.1704 0.9293 0.046 Uiso 1 1 calc R . .
H2B H 1.2247 0.1256 0.9134 0.046 Uiso 1 1 calc R . .
H2C H 1.1377 0.0521 0.9167 0.046 Uiso 1 1 calc R . .
C3 C 1.1911(2) 0.1581(3) 0.82725(12) 0.0243(8) Uani 1 1 d . . .
H3 H 1.2556 0.1520 0.8272 0.029 Uiso 1 1 calc R . .
C4 C 1.1347(2) 0.1802(3) 0.79137(12) 0.0217(8) Uani 1 1 d . . .
C5 C 1.1560(2) 0.1983(3) 0.74395(12) 0.0276(8) Uani 1 1 d . . .
H5A H 1.1028 0.2287 0.7296 0.041 Uiso 1 1 calc R . .
H5B H 1.1708 0.1331 0.7301 0.041 Uiso 1 1 calc R . .
H5C H 1.2081 0.2449 0.7415 0.041 Uiso 1 1 calc R . .
C6 C 0.7741(2) 0.2840(3) 1.04727(11) 0.0238(8) Uani 1 1 d . . .
C7 C 0.6782(2) 0.3135(3) 1.06138(12) 0.0335(9) Uani 1 1 d . . .
H7A H 0.6691 0.3870 1.0569 0.050 Uiso 1 1 calc R . .
H7B H 0.6705 0.2973 1.0921 0.050 Uiso 1 1 calc R . .
H7C H 0.6334 0.2753 1.0443 0.050 Uiso 1 1 calc R . .
C8 C 0.8450(2) 0.2377(3) 1.07152(12) 0.0248(8) Uani 1 1 d . . .
H8 H 0.8425 0.2179 1.1010 0.030 Uiso 1 1 calc R . .
C9 C 0.9201(2) 0.2264(3) 1.04361(11) 0.0207(7) Uani 1 1 d . . .
C10 C 1.0146(2) 0.1819(3) 1.05003(13) 0.0313(9) Uani 1 1 d . . .
H10A H 1.0165 0.1127 1.0380 0.047 Uiso 1 1 calc R . .
H10B H 1.0289 0.1792 1.0810 0.047 Uiso 1 1 calc R . .
H10C H 1.0595 0.2250 1.0353 0.047 Uiso 1 1 calc R . .
C11 C 0.4003(2) 0.3100(3) 0.93768(12) 0.0236(8) Uani 1 1 d . . .
C12 C 0.3834(3) 0.3137(3) 0.98650(12) 0.0344(9) Uani 1 1 d . . .
H12A H 0.4369 0.2869 1.0018 0.052 Uiso 1 1 calc R . .
H12B H 0.3299 0.2720 0.9935 0.052 Uiso 1 1 calc R . .
H12C H 0.3725 0.3845 0.9954 0.052 Uiso 1 1 calc R . .
C13 C 0.3454(2) 0.3370(3) 0.90210(12) 0.0264(8) Uani 1 1 d . . .
H13 H 0.2848 0.3622 0.9030 0.032 Uiso 1 1 calc R . .
C14 C 0.3984(2) 0.3191(3) 0.86455(12) 0.0240(8) Uani 1 1 d . . .
C15 C 0.3748(2) 0.3387(3) 0.81745(12) 0.0300(9) Uani 1 1 d . . .
H15A H 0.4135 0.3937 0.8063 0.045 Uiso 1 1 calc R . .
H15B H 0.3106 0.3588 0.8151 0.045 Uiso 1 1 calc R . .
H15C H 0.3851 0.2763 0.8007 0.045 Uiso 1 1 calc R . .
C16 C 0.6452(2) 0.4127(3) 0.69217(11) 0.0226(8) Uani 1 1 d . . .
C17 C 0.5442(2) 0.4261(3) 0.68159(13) 0.0299(9) Uani 1 1 d . . .
H17A H 0.5077 0.3850 0.7016 0.045 Uiso 1 1 calc R . .
H17B H 0.5324 0.4037 0.6519 0.045 Uiso 1 1 calc R . .
H17C H 0.5275 0.4984 0.6845 0.045 Uiso 1 1 calc R . .
C18 C 0.7219(2) 0.4077(3) 0.66555(11) 0.0216(7) Uani 1 1 d . . .
H18 H 0.7227 0.4092 0.6349 0.026 Uiso 1 1 calc R . .
C19 C 0.7987(2) 0.3999(3) 0.69380(11) 0.0194(7) Uani 1 1 d . . .
C20 C 0.8998(2) 0.3928(3) 0.68216(12) 0.0263(8) Uani 1 1 d . . .
H20A H 0.9342 0.4438 0.6987 0.039 Uiso 1 1 calc R . .
H20B H 0.9073 0.4057 0.6512 0.039 Uiso 1 1 calc R . .
H20C H 0.9226 0.3243 0.6891 0.039 Uiso 1 1 calc R . .
C21 C 0.6978(2) 0.0216(3) 0.94821(11) 0.0213(7) Uani 1 1 d . . .
C22 C 0.7309(3) -0.0617(3) 0.91546(12) 0.0283(8) Uani 1 1 d . . .
H22A H 0.7326 -0.1284 0.9298 0.042 Uiso 1 1 calc R . .
H22B H 0.7921 -0.0442 0.9052 0.042 Uiso 1 1 calc R . .
H22C H 0.6887 -0.0646 0.8908 0.042 Uiso 1 1 calc R . .
C23 C 0.5988(2) -0.0031(3) 0.96326(13) 0.0301(9) Uani 1 1 d . . .
H23A H 0.5579 -0.0046 0.9381 0.045 Uiso 1 1 calc R . .
H23B H 0.5782 0.0497 0.9835 0.045 Uiso 1 1 calc R . .
H23C H 0.5979 -0.0698 0.9776 0.045 Uiso 1 1 calc R . .
C24 C 0.7638(3) 0.0233(3) 0.98900(12) 0.0294(9) Uani 1 1 d . . .
H24A H 0.7612 -0.0429 1.0037 0.044 Uiso 1 1 calc R . .
H24B H 0.7445 0.0774 1.0089 0.044 Uiso 1 1 calc R . .
H24C H 0.8264 0.0366 0.9795 0.044 Uiso 1 1 calc R . .
C25 C 0.5328(2) 0.5576(3) 0.89434(12) 0.0295(9) Uani 1 1 d . . .
H25A H 0.5058 0.6236 0.9021 0.044 Uiso 1 1 calc R . .
H25B H 0.5506 0.5210 0.9207 0.044 Uiso 1 1 calc R . .
H25C H 0.4881 0.5169 0.8782 0.044 Uiso 1 1 calc R . .
C26 C 0.6924(3) 0.6383(3) 0.89156(13) 0.0303(9) Uani 1 1 d . . .
H26A H 0.7443 0.6534 0.8728 0.046 Uiso 1 1 calc R . .
H26B H 0.7132 0.5981 0.9164 0.046 Uiso 1 1 calc R . .
H26C H 0.6653 0.7025 0.9017 0.046 Uiso 1 1 calc R . .
C27 C 0.6192(2) 0.5759(3) 0.86560(12) 0.0219(8) Uani 1 1 d . . .
C28 C 0.5918(3) 0.6359(3) 0.82377(13) 0.0318(9) Uani 1 1 d . . .
H28A H 0.5441 0.5982 0.8083 0.048 Uiso 1 1 calc R . .
H28B H 0.6452 0.6434 0.8051 0.048 Uiso 1 1 calc R . .
H28C H 0.5689 0.7037 0.8317 0.048 Uiso 1 1 calc R . .
C29 C 0.7008(2) -0.0106(3) 0.78381(12) 0.0257(8) Uani 1 1 d . . .
H29A H 0.6797 -0.0635 0.7637 0.039 Uiso 1 1 calc R . .
H29B H 0.6482 0.0257 0.7957 0.039 Uiso 1 1 calc R . .
H29C H 0.7355 -0.0425 0.8074 0.039 Uiso 1 1 calc R . .
C30 C 0.7635(2) 0.0670(3) 0.75916(11) 0.0187(7) Uani 1 1 d . . .
C31 C 0.7109(2) 0.1198(3) 0.72109(12) 0.0278(8) Uani 1 1 d . . .
H31A H 0.7499 0.1719 0.7079 0.042 Uiso 1 1 calc R . .
H31B H 0.6554 0.1521 0.7322 0.042 Uiso 1 1 calc R . .
H31C H 0.6944 0.0685 0.6994 0.042 Uiso 1 1 calc R . .
C32 C 0.8497(2) 0.0088(3) 0.74208(12) 0.0273(8) Uani 1 1 d . . .
H32A H 0.8305 -0.0462 0.7226 0.041 Uiso 1 1 calc R . .
H32B H 0.8835 -0.0203 0.7666 0.041 Uiso 1 1 calc R . .
H32C H 0.8891 0.0566 0.7264 0.041 Uiso 1 1 calc R . .
C33 C 1.0538(2) 0.4945(3) 0.94290(11) 0.0264(8) Uani 1 1 d . . .
H33A H 1.0765 0.4302 0.9551 0.040 Uiso 1 1 calc R . .
H33B H 1.0048 0.5212 0.9611 0.040 Uiso 1 1 calc R . .
H33C H 1.1037 0.5443 0.9417 0.040 Uiso 1 1 calc R . .
C34 C 1.0162(2) 0.4749(3) 0.89604(11) 0.0196(7) Uani 1 1 d . . .
C35 C 0.9761(2) 0.5751(3) 0.87666(12) 0.0250(8) Uani 1 1 d . . .
H35A H 1.0232 0.6282 0.8765 0.038 Uiso 1 1 calc R . .
H35B H 0.9245 0.5979 0.8943 0.038 Uiso 1 1 calc R . .
H35C H 0.9552 0.5624 0.8470 0.038 Uiso 1 1 calc R . .
C36 C 1.0942(2) 0.4317(3) 0.86677(12) 0.0266(8) Uani 1 1 d . . .
H36A H 1.0697 0.4165 0.8380 0.040 Uiso 1 1 calc R . .
H36B H 1.1188 0.3691 0.8797 0.040 Uiso 1 1 calc R . .
H36C H 1.1429 0.4827 0.8643 0.040 Uiso 1 1 calc R . .
N1 N 1.04415(18) 0.1614(2) 0.85069(9) 0.0189(6) Uani 1 1 d . . .
N2 N 1.04798(18) 0.1816(2) 0.80667(9) 0.0198(6) Uani 1 1 d . . .
H2 H 0.9998 0.1939 0.7906 0.024 Uiso 1 1 calc R . .
N3 N 0.80404(18) 0.3007(2) 1.00555(9) 0.0190(6) Uani 1 1 d . . .
N4 N 0.89219(18) 0.2651(2) 1.00471(9) 0.0198(6) Uani 1 1 d . . .
H4 H 0.9269 0.2671 0.9817 0.024 Uiso 1 1 calc R . .
N5 N 0.48260(18) 0.2812(2) 0.87650(9) 0.0199(6) Uani 1 1 d . . .
N6 N 0.48128(19) 0.2764(2) 0.92132(9) 0.0206(6) Uani 1 1 d . . .
H6 H 0.5270 0.2544 0.9372 0.025 Uiso 1 1 calc R . .
N7 N 0.77000(18) 0.3999(2) 0.73608(9) 0.0187(6) Uani 1 1 d . . .
N8 N 0.67597(18) 0.4081(2) 0.73386(9) 0.0216(6) Uani 1 1 d . . .
H8A H 0.6403 0.4100 0.7566 0.026 Uiso 1 1 calc R . .
O1 O 0.94848(15) 0.05828(18) 0.91615(8) 0.0227(5) Uani 1 1 d . . .
O2 O 0.63889(15) 0.13903(16) 0.88041(7) 0.0176(5) Uani 1 1 d . . .
O3 O 0.79528(14) 0.19238(17) 0.91531(7) 0.0178(5) Uani 1 1 d . . .
O4 O 0.65282(14) 0.22909(16) 0.95437(7) 0.0174(5) Uani 1 1 d . . .
O5 O 0.67670(15) 0.44525(18) 0.97491(7) 0.0235(5) Uani 1 1 d . . .
O6 O 0.67692(14) 0.37381(17) 0.88799(7) 0.0181(5) Uani 1 1 d . . .
O7 O 0.59863(14) 0.39581(17) 0.81766(7) 0.0176(5) Uani 1 1 d . . .
O8 O 0.75858(14) 0.47457(17) 0.82541(7) 0.0184(5) Uani 1 1 d . . .
O9 O 0.84842(14) 0.42109(17) 0.92781(7) 0.0176(5) Uani 1 1 d . . .
O10 O 0.89564(14) 0.33395(16) 0.85489(7) 0.0156(5) Uani 1 1 d . . .
O11 O 0.96910(14) 0.27805(17) 0.92270(7) 0.0170(5) Uani 1 1 d . . .
O12 O 0.72869(14) 0.24196(16) 0.81124(7) 0.0166(5) Uani 1 1 d . . .
O13 O 0.85132(14) 0.10651(17) 0.83546(7) 0.0163(5) Uani 1 1 d . . .
O14 O 0.87647(14) 0.23643(16) 0.77398(7) 0.0174(5) Uani 1 1 d . . .
O15 O 0.54209(15) 0.18586(18) 0.80004(8) 0.0228(5) Uani 1 1 d . . .
O16 O 0.93112(14) 0.45150(18) 0.78011(7) 0.0206(5) Uani 1 1 d . . .
P1 P 0.69699(6) 0.14872(7) 0.92235(3) 0.01670(19) Uani 1 1 d . . .
P2 P 0.66769(6) 0.45126(7) 0.84911(3) 0.01680(19) Uani 1 1 d . . .
P3 P 0.92661(6) 0.37588(7) 0.90015(3) 0.01628(19) Uani 1 1 d . . .
P4 P 0.80530(6) 0.16471(7) 0.79746(3) 0.01667(19) Uani 1 1 d . . .
V1 V 0.91935(4) 0.15684(4) 0.887453(19) 0.01674(14) Uani 1 1 d . . .
V2 V 0.73277(4) 0.35802(4) 0.949219(18) 0.01720(14) Uani 1 1 d . . .
V3 V 0.59941(4) 0.24498(4) 0.837151(19) 0.01734(14) Uani 1 1 d . . .
V4 V 0.84643(4) 0.38167(4) 0.795422(18) 0.01636(14) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0155(16) 0.0208(18) 0.030(2) -0.0014(15) -0.0029(15) 0.0048(13)
C2 0.0220(19) 0.035(2) 0.036(2) 0.0034(19) -0.0018(17) 0.0014(16)
C3 0.0142(16) 0.026(2) 0.033(2) 0.0000(16) 0.0035(15) -0.0004(14)
C4 0.0206(17) 0.0178(18) 0.027(2) -0.0019(15) 0.0062(15) -0.0009(14)
C5 0.0256(19) 0.029(2) 0.028(2) -0.0001(17) 0.0075(16) 0.0008(16)
C6 0.0255(18) 0.0248(19) 0.0211(19) -0.0013(16) 0.0053(15) -0.0067(15)
C7 0.026(2) 0.053(3) 0.022(2) 0.0063(19) 0.0083(16) 0.0010(18)
C8 0.030(2) 0.026(2) 0.0176(18) 0.0031(16) 0.0006(15) -0.0027(15)
C9 0.0261(18) 0.0172(17) 0.0188(18) 0.0012(14) -0.0037(15) -0.0039(14)
C10 0.032(2) 0.031(2) 0.031(2) 0.0058(18) -0.0009(17) 0.0035(17)
C11 0.0194(17) 0.0203(18) 0.031(2) 0.0013(16) 0.0054(15) -0.0015(14)
C12 0.032(2) 0.039(2) 0.032(2) -0.0030(19) 0.0061(18) 0.0049(18)
C13 0.0164(17) 0.026(2) 0.037(2) 0.0015(17) 0.0033(16) 0.0030(14)
C14 0.0171(17) 0.0217(19) 0.033(2) 0.0089(16) -0.0016(15) -0.0021(14)
C15 0.0166(17) 0.039(2) 0.035(2) 0.0101(19) -0.0011(16) -0.0004(16)
C16 0.0255(18) 0.0220(19) 0.0204(18) -0.0012(15) -0.0028(15) 0.0006(14)
C17 0.0231(18) 0.039(2) 0.028(2) 0.0050(18) -0.0051(16) 0.0039(16)
C18 0.0268(18) 0.0236(19) 0.0145(17) 0.0001(15) -0.0004(14) 0.0000(15)
C19 0.0226(17) 0.0168(17) 0.0187(18) -0.0016(14) 0.0019(14) -0.0015(14)
C20 0.0262(19) 0.033(2) 0.0200(19) -0.0013(17) 0.0017(15) -0.0003(16)
C21 0.0210(17) 0.0190(18) 0.0239(19) 0.0052(15) 0.0002(14) -0.0011(14)
C22 0.034(2) 0.0165(19) 0.034(2) 0.0008(16) -0.0007(17) -0.0018(15)
C23 0.0268(19) 0.029(2) 0.035(2) 0.0124(18) 0.0070(17) -0.0032(16)
C24 0.040(2) 0.023(2) 0.025(2) 0.0061(16) -0.0025(17) -0.0012(16)
C25 0.0278(19) 0.027(2) 0.034(2) -0.0015(17) 0.0103(17) 0.0033(16)
C26 0.032(2) 0.023(2) 0.037(2) -0.0073(17) 0.0059(17) -0.0017(16)
C27 0.0225(17) 0.0163(17) 0.0270(19) 0.0004(15) 0.0051(15) 0.0046(14)
C28 0.033(2) 0.024(2) 0.038(2) 0.0077(18) 0.0046(18) 0.0086(16)
C29 0.0252(18) 0.026(2) 0.026(2) -0.0049(16) 0.0015(15) -0.0069(15)
C30 0.0207(17) 0.0189(18) 0.0164(17) -0.0068(14) 0.0016(14) -0.0007(13)
C31 0.031(2) 0.029(2) 0.023(2) -0.0024(17) -0.0068(16) -0.0031(16)
C32 0.0257(19) 0.028(2) 0.029(2) -0.0068(17) 0.0061(16) -0.0014(16)
C33 0.034(2) 0.027(2) 0.0185(19) 0.0003(16) -0.0034(16) -0.0115(16)
C34 0.0204(17) 0.0214(18) 0.0170(18) 0.0023(14) -0.0009(14) -0.0023(14)
C35 0.0272(19) 0.0226(19) 0.025(2) 0.0009(16) -0.0018(16) -0.0068(15)
C36 0.0234(18) 0.028(2) 0.028(2) 0.0016(17) 0.0037(15) -0.0035(15)
N1 0.0219(15) 0.0171(15) 0.0176(15) 0.0001(12) 0.0004(12) 0.0010(11)
N2 0.0144(13) 0.0240(16) 0.0208(16) -0.0023(13) 0.0000(12) 0.0000(11)
N3 0.0161(14) 0.0231(15) 0.0176(15) -0.0029(12) 0.0004(11) -0.0022(11)
N4 0.0188(14) 0.0210(15) 0.0196(15) 0.0003(12) 0.0027(12) -0.0010(11)
N5 0.0167(14) 0.0246(16) 0.0184(15) 0.0007(13) 0.0004(12) -0.0007(12)
N6 0.0203(14) 0.0211(15) 0.0204(16) 0.0030(13) 0.0044(12) 0.0030(12)
N7 0.0142(13) 0.0231(16) 0.0188(15) 0.0009(12) 0.0011(11) -0.0012(11)
N8 0.0190(14) 0.0246(16) 0.0212(16) -0.0004(13) 0.0023(12) 0.0047(12)
O1 0.0201(12) 0.0227(13) 0.0252(13) 0.0024(11) -0.0003(10) 0.0013(10)
O2 0.0190(11) 0.0179(12) 0.0160(12) 0.0018(10) 0.0011(9) 0.0007(9)
O3 0.0170(11) 0.0188(12) 0.0176(12) 0.0018(10) 0.0014(9) -0.0022(9)
O4 0.0174(11) 0.0168(12) 0.0179(12) 0.0012(10) 0.0023(9) 0.0007(9)
O5 0.0255(13) 0.0257(13) 0.0193(13) -0.0031(11) 0.0056(10) 0.0016(10)
O6 0.0160(11) 0.0190(12) 0.0192(12) 0.0015(10) 0.0033(9) 0.0016(9)
O7 0.0154(11) 0.0186(12) 0.0187(12) 0.0037(10) 0.0028(9) 0.0017(9)
O8 0.0182(11) 0.0180(12) 0.0191(12) 0.0012(10) 0.0016(10) 0.0001(9)
O9 0.0181(11) 0.0172(12) 0.0174(12) -0.0023(10) 0.0028(9) -0.0033(9)
O10 0.0140(11) 0.0164(12) 0.0163(12) -0.0004(10) 0.0008(9) 0.0002(9)
O11 0.0177(11) 0.0177(12) 0.0157(12) 0.0013(10) -0.0004(9) -0.0032(9)
O12 0.0155(11) 0.0183(12) 0.0159(12) 0.0001(10) 0.0014(9) 0.0021(9)
O13 0.0170(11) 0.0175(12) 0.0144(11) -0.0020(10) -0.0004(9) 0.0015(9)
O14 0.0166(11) 0.0173(12) 0.0182(12) -0.0011(10) 0.0047(9) -0.0012(9)
O15 0.0198(12) 0.0251(13) 0.0235(13) -0.0013(11) 0.0008(10) -0.0003(10)
O16 0.0189(12) 0.0243(13) 0.0186(12) 0.0012(10) 0.0014(10) -0.0044(10)
P1 0.0159(4) 0.0170(4) 0.0172(4) 0.0003(4) 0.0014(3) -0.0010(3)
P2 0.0170(4) 0.0165(4) 0.0169(4) 0.0009(4) 0.0020(3) 0.0008(3)
P3 0.0170(4) 0.0165(4) 0.0154(4) -0.0011(4) 0.0005(3) -0.0018(3)
P4 0.0163(4) 0.0171(4) 0.0166(4) -0.0023(4) 0.0018(3) -0.0007(3)
V1 0.0161(3) 0.0168(3) 0.0174(3) 0.0000(2) 0.0010(2) 0.0006(2)
V2 0.0173(3) 0.0179(3) 0.0164(3) -0.0007(2) 0.0026(2) 0.0002(2)
V3 0.0153(3) 0.0179(3) 0.0188(3) -0.0001(2) 0.0010(2) -0.0002(2)
V4 0.0156(3) 0.0175(3) 0.0160(3) 0.0000(2) 0.0012(2) -0.0005(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
C1 N1 1.345(4) . ?
C1 C3 1.388(5) . ?
C1 C2 1.487(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 N2 1.332(4) . ?
C4 C5 1.489(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.354(4) . ?
C6 C8 1.387(5) . ?
C6 C7 1.493(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.381(5) . ?
C8 H8 0.9300 . ?
C9 N4 1.339(4) . ?
C9 C10 1.484(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N6 1.338(4) . ?
C11 C13 1.377(5) . ?
C11 C12 1.502(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.391(5) . ?
C13 H13 0.9300 . ?
C14 N5 1.351(4) . ?
C14 C15 1.487(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N8 1.338(4) . ?
C16 C18 1.370(5) . ?
C16 C17 1.495(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.398(4) . ?
C18 H18 0.9300 . ?
C19 N7 1.348(4) . ?
C19 C20 1.498(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C23 1.529(4) . ?
C21 C22 1.535(5) . ?
C21 C24 1.555(5) . ?
C21 P1 1.808(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C27 1.538(5) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.535(5) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.533(5) . ?
C27 P2 1.814(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.538(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.534(5) . ?
C30 C32 1.538(4) . ?
C30 P4 1.808(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.538(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.524(5) . ?
C34 C36 1.535(5) . ?
C34 P3 1.812(3) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 N2 1.360(4) . ?
N1 V1 2.116(3) . ?
N2 H2 0.8600 . ?
N3 N4 1.346(3) . ?
N3 V2 2.119(3) . ?
N4 H4 0.8600 . ?
N5 N6 1.360(4) . ?
N5 V3 2.115(3) . ?
N6 H6 0.8600 . ?
N7 N8 1.356(3) . ?
N7 V4 2.116(3) . ?
N8 H8A 0.8600 . ?
O1 V1 1.589(2) . ?
O2 P1 1.523(2) . ?
O2 V3 1.969(2) . ?
O3 P1 1.534(2) . ?
O3 V1 2.027(2) . ?
O4 P1 1.553(2) . ?
O4 V2 2.019(2) . ?
O5 V2 1.584(2) . ?
O6 P2 1.546(2) . ?
O6 V2 2.029(2) . ?
O7 P2 1.546(2) . ?
O7 V3 2.021(2) . ?
O8 P2 1.522(2) . ?
O8 V4 1.961(2) . ?
O9 P3 1.519(2) . ?
O9 V2 1.960(2) . ?
O10 P3 1.537(2) . ?
O10 V4 2.028(2) . ?
O11 P3 1.552(2) . ?
O11 V1 2.015(2) . ?
O12 P4 1.539(2) . ?
O12 V3 2.020(2) . ?
O13 P4 1.521(2) . ?
O13 V1 1.960(2) . ?
O14 P4 1.550(2) . ?
O14 V4 2.019(2) . ?
O15 V3 1.584(2) . ?
O16 V4 1.581(2) . ?
P1 V2 2.8491(14) . ?
P2 V3 2.8422(14) . ?
P3 V1 2.8352(15) . ?
P4 V4 2.8431(15) . ?

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
N1 C1 C3 109.3(3) . . ?
N1 C1 C2 122.0(3) . . ?
C3 C1 C2 128.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C1 106.9(3) . . ?
C4 C3 H3 126.5 . . ?
C1 C3 H3 126.5 . . ?
N2 C4 C3 105.9(3) . . ?
N2 C4 C5 122.0(3) . . ?
C3 C4 C5 132.1(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C8 109.1(3) . . ?
N3 C6 C7 121.6(3) . . ?
C8 C6 C7 129.3(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C6 107.1(3) . . ?
C9 C8 H8 126.5 . . ?
C6 C8 H8 126.5 . . ?
N4 C9 C8 105.6(3) . . ?
N4 C9 C10 121.9(3) . . ?
C8 C9 C10 132.5(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 C13 106.6(3) . . ?
N6 C11 C12 121.3(3) . . ?
C13 C11 C12 132.0(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 C14 106.6(3) . . ?
C11 C13 H13 126.7 . . ?
C14 C13 H13 126.7 . . ?
N5 C14 C13 109.4(3) . . ?
N5 C14 C15 121.2(3) . . ?
C13 C14 C15 129.4(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N8 C16 C18 106.9(3) . . ?
N8 C16 C17 121.6(3) . . ?
C18 C16 C17 131.4(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 C19 106.1(3) . . ?
C16 C18 H18 126.9 . . ?
C19 C18 H18 126.9 . . ?
N7 C19 C18 109.8(3) . . ?
N7 C19 C20 121.7(3) . . ?
C18 C19 C20 128.6(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C21 C22 109.9(3) . . ?
C23 C21 C24 109.3(3) . . ?
C22 C21 C24 109.5(3) . . ?
C23 C21 P1 108.2(2) . . ?
C22 C21 P1 110.4(2) . . ?
C24 C21 P1 109.6(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C25 H25A 109.5 . . ?
C27 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C27 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C26 109.6(3) . . ?
C28 C27 C25 109.9(3) . . ?
C26 C27 C25 110.0(3) . . ?
C28 C27 P2 108.1(2) . . ?
C26 C27 P2 109.7(2) . . ?
C25 C27 P2 109.5(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C29 111.3(3) . . ?
C31 C30 C32 110.8(3) . . ?
C29 C30 C32 108.9(3) . . ?
C31 C30 P4 109.8(2) . . ?
C29 C30 P4 109.2(2) . . ?
C32 C30 P4 106.6(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 110.9(3) . . ?
C35 C34 C33 110.4(3) . . ?
C36 C34 C33 109.8(3) . . ?
C35 C34 P3 110.4(2) . . ?
C36 C34 P3 107.9(2) . . ?
C33 C34 P3 107.3(2) . . ?
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 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C1 N1 N2 105.4(3) . . ?
C1 N1 V1 130.5(2) . . ?
N2 N1 V1 124.0(2) . . ?
C4 N2 N1 112.4(3) . . ?
C4 N2 H2 123.8 . . ?
N1 N2 H2 123.8 . . ?
N4 N3 C6 105.5(3) . . ?
N4 N3 V2 123.6(2) . . ?
C6 N3 V2 130.8(2) . . ?
C9 N4 N3 112.8(3) . . ?
C9 N4 H4 123.6 . . ?
N3 N4 H4 123.6 . . ?
C14 N5 N6 105.5(3) . . ?
C14 N5 V3 129.7(2) . . ?
N6 N5 V3 124.6(2) . . ?
C11 N6 N5 111.8(3) . . ?
C11 N6 H6 124.1 . . ?
N5 N6 H6 124.1 . . ?
C19 N7 N8 105.2(3) . . ?
C19 N7 V4 130.4(2) . . ?
N8 N7 V4 124.3(2) . . ?
C16 N8 N7 112.0(3) . . ?
C16 N8 H8A 124.0 . . ?
N7 N8 H8A 124.0 . . ?
P1 O2 V3 130.90(13) . . ?
P1 O3 V1 141.91(14) . . ?
P1 O4 V2 105.09(12) . . ?
P2 O6 V2 142.52(14) . . ?
P2 O7 V3 104.87(11) . . ?
P2 O8 V4 130.87(14) . . ?
P3 O9 V2 130.92(13) . . ?
P3 O10 V4 141.84(14) . . ?
P3 O11 V1 104.56(12) . . ?
P4 O12 V3 141.03(14) . . ?
P4 O13 V1 131.39(14) . . ?
P4 O14 V4 104.87(12) . . ?
O2 P1 O3 114.53(13) . . ?
O2 P1 O4 110.60(12) . . ?
O3 P1 O4 102.93(12) . . ?
O2 P1 C21 106.91(14) . . ?
O3 P1 C21 112.62(14) . . ?
O4 P1 C21 109.18(15) . . ?
O2 P1 V2 114.39(9) . . ?
O3 P1 V2 62.07(9) . . ?
O4 P1 V2 43.16(8) . . ?
C21 P1 V2 136.35(12) . . ?
O8 P2 O7 110.41(12) . . ?
O8 P2 O6 114.50(12) . . ?
O7 P2 O6 103.15(12) . . ?
O8 P2 C27 106.75(14) . . ?
O7 P2 C27 109.19(14) . . ?
O6 P2 C27 112.77(15) . . ?
O8 P2 V3 114.74(9) . . ?
O7 P2 V3 43.42(8) . . ?
O6 P2 V3 61.87(9) . . ?
C27 P2 V3 136.19(12) . . ?
O9 P3 O10 114.45(12) . . ?
O9 P3 O11 110.82(13) . . ?
O10 P3 O11 102.85(12) . . ?
O9 P3 C34 107.33(14) . . ?
O10 P3 C34 112.72(14) . . ?
O11 P3 C34 108.54(14) . . ?
O9 P3 V1 115.19(9) . . ?
O10 P3 V1 61.47(8) . . ?
O11 P3 V1 43.45(8) . . ?
C34 P3 V1 135.22(11) . . ?
O13 P4 O12 114.76(12) . . ?
O13 P4 O14 110.67(12) . . ?
O12 P4 O14 102.53(13) . . ?
O13 P4 C30 106.78(14) . . ?
O12 P4 C30 112.56(14) . . ?
O14 P4 C30 109.49(14) . . ?
O13 P4 V4 113.97(9) . . ?
O12 P4 V4 61.70(9) . . ?
O14 P4 V4 43.33(8) . . ?
C30 P4 V4 137.02(12) . . ?
O1 V1 O13 107.93(11) . . ?
O1 V1 O11 103.34(11) . . ?
O13 V1 O11 148.73(9) . . ?
O1 V1 O3 100.40(10) . . ?
O13 V1 O3 88.43(9) . . ?
O11 V1 O3 85.20(9) . . ?
O1 V1 N1 95.08(11) . . ?
O13 V1 N1 90.36(10) . . ?
O11 V1 N1 87.62(10) . . ?
O3 V1 N1 164.07(10) . . ?
O1 V1 P3 134.70(9) . . ?
O13 V1 P3 116.93(7) . . ?
O11 V1 P3 31.99(6) . . ?
O3 V1 P3 75.69(7) . . ?
N1 V1 P3 90.76(8) . . ?
O5 V2 O9 107.76(11) . . ?
O5 V2 O4 104.41(11) . . ?
O9 V2 O4 147.81(9) . . ?
O5 V2 O6 100.33(11) . . ?
O9 V2 O6 89.34(9) . . ?
O4 V2 O6 85.96(9) . . ?
O5 V2 N3 95.36(11) . . ?
O9 V2 N3 90.15(10) . . ?
O4 V2 N3 85.81(10) . . ?
O6 V2 N3 163.67(10) . . ?
O5 V2 P1 135.50(9) . . ?
O9 V2 P1 116.46(7) . . ?
O4 V2 P1 31.75(6) . . ?
O6 V2 P1 76.25(7) . . ?
N3 V2 P1 89.42(8) . . ?
O15 V3 O2 106.88(11) . . ?
O15 V3 O12 101.00(10) . . ?
O2 V3 O12 89.03(9) . . ?
O15 V3 O7 104.34(11) . . ?
O2 V3 O7 148.79(9) . . ?
O12 V3 O7 84.76(9) . . ?
O15 V3 N5 95.41(11) . . ?
O2 V3 N5 90.16(10) . . ?
O12 V3 N5 163.08(10) . . ?
O7 V3 N5 87.21(10) . . ?
O15 V3 P2 135.51(9) . . ?
O2 V3 P2 117.27(7) . . ?
O12 V3 P2 75.52(7) . . ?
O7 V3 P2 31.71(6) . . ?
N5 V3 P2 89.89(8) . . ?
O16 V4 O8 106.85(11) . . ?
O16 V4 O14 105.16(11) . . ?
O8 V4 O14 147.97(9) . . ?
O16 V4 O10 99.55(10) . . ?
O8 V4 O10 89.64(9) . . ?
O14 V4 O10 86.21(9) . . ?
O16 V4 N7 94.87(11) . . ?
O8 V4 N7 89.67(10) . . ?
O14 V4 N7 86.51(10) . . ?
O10 V4 N7 165.13(10) . . ?
O16 V4 P4 136.05(9) . . ?
O8 V4 P4 116.71(7) . . ?
O14 V4 P4 31.80(6) . . ?
O10 V4 P4 75.96(6) . . ?
N7 V4 P4 91.12(8) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.110
#===END