#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/72/7107219.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7107219
loop_
_publ_author_name
'Carl Redshaw'
'Mark R. J. Elsegood'
'Joseph A. Wright'
'Hugo Baillie-Johnson'
'Takehiko Yamato'
'Stephen De Giovanni'
'Anja Mueller'
_publ_section_title
;
 Cellular uptake of a fluorescent vanadyl sulfonylcalix[4]arene
;
_journal_name_full               Chem.Commun.
_journal_page_first              1129
_journal_paper_doi               10.1039/c2cc16480a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C56 H80 O9 V2, 1.5(C2 H3 N)'
_chemical_formula_sum            'C59 H84.5 N1.5 O9 V2'
_chemical_formula_weight         1060.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.663(3)
_cell_length_b                   13.179(2)
_cell_length_c                   26.712(5)
_cell_measurement_reflns_used    4529
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.20
_cell_measurement_theta_min      2.38
_cell_volume                     5850.2(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           SYNCHROTRON
_diffrn_radiation_wavelength     0.6942
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36467
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        4
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       LATH
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1281P)²+10.5321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2686
_reflns_number_gt                4889
_reflns_number_total             8197
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2cc16480a.txt
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C59 H84.50 N1.50 O9 V2'
_cod_database_code               7107219
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'
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 0.59013(8) 0.52481(10) 0.19261(5) 0.0694(5) Uani 1 1 d . . .
V2 V 0.76791(8) 0.45674(10) 0.15543(6) 0.0752(5) Uani 1 1 d . . .
O5 O 0.6624(3) 0.4694(4) 0.15515(19) 0.0714(14) Uani 1 1 d . . .
O6 O 0.5198(3) 0.4449(4) 0.1971(2) 0.0840(17) Uani 1 1 d . . .
O8 O 0.7895(4) 0.3436(4) 0.1429(3) 0.109(2) Uani 1 1 d . . .
O1 O 0.6881(3) 0.3522(3) 0.25089(18) 0.0595(12) Uani 1 1 d DU . .
C45 C 0.6362(8) 0.2650(8) 0.2376(6) 0.065(4) Uani 0.505(14) 1 d PDU A 1
H45A H 0.6132 0.2722 0.2026 0.079 Uiso 0.505(14) 1 calc PR A 1
H45B H 0.5913 0.2630 0.2598 0.079 Uiso 0.505(14) 1 calc PR A 1
C46 C 0.6832(8) 0.1682(8) 0.2429(7) 0.075(5) Uani 0.505(14) 1 d PDU A 1
H46A H 0.7051 0.1597 0.2781 0.089 Uiso 0.505(14) 1 calc PR A 1
H46B H 0.7289 0.1704 0.2212 0.089 Uiso 0.505(14) 1 calc PR A 1
C47 C 0.6274(4) 0.0775(5) 0.2274(3) 0.071(2) Uani 1 1 d DU . .
H47A H 0.6584 0.0143 0.2300 0.107 Uiso 0.505(14) 1 calc PR A 1
H47B H 0.6052 0.0869 0.1927 0.107 Uiso 0.505(14) 1 calc PR A 1
H47C H 0.5833 0.0742 0.2497 0.107 Uiso 0.505(14) 1 calc PR A 1
H47D H 0.5877 0.0336 0.2418 0.107 Uiso 0.495(14) 1 calc PR A 2
H47E H 0.6813 0.0487 0.2342 0.107 Uiso 0.495(14) 1 calc PR A 2
H47F H 0.6151 0.0827 0.1910 0.107 Uiso 0.495(14) 1 calc PR A 2
C45X C 0.6854(10) 0.2481(9) 0.2283(6) 0.064(5) Uiso 0.495(14) 1 d PDU A 2
H45C H 0.6722 0.2534 0.1917 0.077 Uiso 0.495(14) 1 calc PR A 2
H45D H 0.7391 0.2160 0.2338 0.077 Uiso 0.495(14) 1 calc PR A 2
C46X C 0.6245(9) 0.1836(9) 0.2510(5) 0.065(4) Uiso 0.495(14) 1 d PDU A 2
H46C H 0.5702 0.2134 0.2444 0.078 Uiso 0.495(14) 1 calc PR A 2
H46D H 0.6365 0.1792 0.2878 0.078 Uiso 0.495(14) 1 calc PR A 2
O2 O 0.6255(3) 0.5625(3) 0.25346(18) 0.0600(12) Uani 1 1 d . . .
O3 O 0.7167(2) 0.6869(3) 0.19101(16) 0.0537(12) Uani 1 1 d D . .
C48 C 0.7168(4) 0.7405(5) 0.1434(3) 0.0592(18) Uani 1 1 d D . .
H48A H 0.7010 0.6925 0.1159 0.071 Uiso 1 1 calc R . .
H48B H 0.7723 0.7637 0.1387 0.071 Uiso 1 1 calc R . .
C49 C 0.6615(4) 0.8302(5) 0.1394(3) 0.065(2) Uani 1 1 d D . .
H49A H 0.6786 0.8805 0.1656 0.078 Uiso 1 1 calc R . .
H49B H 0.6060 0.8082 0.1451 0.078 Uiso 1 1 calc R . .
C50 C 0.6624(5) 0.8793(7) 0.0875(3) 0.084(2) Uani 1 1 d D . .
H50A H 0.7178 0.8969 0.0810 0.126 Uiso 1 1 calc R . .
H50B H 0.6294 0.9409 0.0865 0.126 Uiso 1 1 calc R . .
H50C H 0.6407 0.8315 0.0619 0.126 Uiso 1 1 calc R . .
O4 O 0.8158(3) 0.4963(3) 0.21272(19) 0.0632(13) Uani 1 1 d . . .
C1 C 0.7156(4) 0.3548(5) 0.3014(3) 0.0565(18) Uani 1 1 d . A .
C2 C 0.7975(4) 0.3356(5) 0.3150(3) 0.0558(18) Uani 1 1 d . . .
C3 C 0.8212(4) 0.3320(5) 0.3654(3) 0.0587(19) Uani 1 1 d . A .
H3 H 0.8758 0.3157 0.3749 0.070 Uiso 1 1 calc R . .
C4 C 0.7705(4) 0.3507(5) 0.4033(3) 0.0576(18) Uani 1 1 d . . .
C5 C 0.6921(4) 0.3754(5) 0.3879(3) 0.0638(19) Uani 1 1 d . A .
H5 H 0.6561 0.3915 0.4127 0.077 Uiso 1 1 calc R . .
C6 C 0.6633(4) 0.3778(5) 0.3373(3) 0.0555(18) Uani 1 1 d . . .
C7 C 0.8031(5) 0.3460(6) 0.4586(3) 0.069(2) Uani 1 1 d . A .
C8 C 0.8769(5) 0.4169(6) 0.4670(3) 0.080(2) Uani 1 1 d . . .
H8A H 0.9195 0.3941 0.4462 0.119 Uiso 1 1 calc R A .
H8B H 0.8968 0.4150 0.5024 0.119 Uiso 1 1 calc R . .
H8C H 0.8613 0.4864 0.4577 0.119 Uiso 1 1 calc R . .
C9 C 0.8313(6) 0.2371(6) 0.4702(4) 0.095(3) Uani 1 1 d . . .
H9A H 0.7850 0.1911 0.4668 0.142 Uiso 1 1 calc R A .
H9B H 0.8560 0.2338 0.5046 0.142 Uiso 1 1 calc R . .
H9C H 0.8708 0.2170 0.4467 0.142 Uiso 1 1 calc R . .
C10 C 0.7398(5) 0.3798(8) 0.4932(3) 0.094(3) Uani 1 1 d . . .
H10A H 0.7269 0.4515 0.4870 0.141 Uiso 1 1 calc R A .
H10B H 0.7606 0.3710 0.5282 0.141 Uiso 1 1 calc R . .
H10C H 0.6911 0.3388 0.4867 0.141 Uiso 1 1 calc R . .
C11 C 0.5782(4) 0.4136(5) 0.3243(3) 0.0613(19) Uani 1 1 d . A .
H11A H 0.5625 0.3974 0.2887 0.074 Uiso 1 1 calc R . .
H11B H 0.5412 0.3772 0.3454 0.074 Uiso 1 1 calc R . .
C12 C 0.5924(4) 0.5959(5) 0.2964(3) 0.0540(17) Uani 1 1 d . A .
C13 C 0.5703(4) 0.5264(5) 0.3324(3) 0.0581(18) Uani 1 1 d . . .
C14 C 0.5424(4) 0.5653(6) 0.3756(3) 0.0628(19) Uani 1 1 d . A .
H14 H 0.5269 0.5191 0.4004 0.075 Uiso 1 1 calc R . .
C15 C 0.5356(4) 0.6697(5) 0.3850(3) 0.0601(19) Uani 1 1 d . . .
C16 C 0.5573(4) 0.7348(6) 0.3471(3) 0.0605(19) Uani 1 1 d . A .
H16 H 0.5519 0.8059 0.3519 0.073 Uiso 1 1 calc R . .
C17 C 0.5863(3) 0.7007(5) 0.3025(3) 0.0557(18) Uani 1 1 d . . .
C18 C 0.5056(5) 0.7131(6) 0.4329(3) 0.071(2) Uani 1 1 d . A .
C19 C 0.4256(5) 0.7671(8) 0.4202(3) 0.098(3) Uani 1 1 d . . .
H19A H 0.4324 0.8181 0.3942 0.147 Uiso 1 1 calc R A .
H19B H 0.4082 0.8003 0.4504 0.147 Uiso 1 1 calc R . .
H19C H 0.3850 0.7175 0.4080 0.147 Uiso 1 1 calc R . .
C20 C 0.4924(5) 0.6319(6) 0.4724(3) 0.081(2) Uani 1 1 d . . .
H20A H 0.4524 0.5828 0.4587 0.122 Uiso 1 1 calc R A .
H20B H 0.4730 0.6640 0.5023 0.122 Uiso 1 1 calc R . .
H20C H 0.5433 0.5969 0.4814 0.122 Uiso 1 1 calc R . .
C21 C 0.5702(6) 0.7864(7) 0.4562(4) 0.098(3) Uani 1 1 d . . .
H21A H 0.6210 0.7497 0.4629 0.147 Uiso 1 1 calc R A .
H21B H 0.5526 0.8138 0.4877 0.147 Uiso 1 1 calc R . .
H21C H 0.5780 0.8422 0.4328 0.147 Uiso 1 1 calc R . .
C22 C 0.6101(4) 0.7720(5) 0.2619(3) 0.0552(17) Uani 1 1 d . A .
H22A H 0.5824 0.8378 0.2654 0.066 Uiso 1 1 calc R . .
H22B H 0.5922 0.7434 0.2287 0.066 Uiso 1 1 calc R . .
C23 C 0.7505(4) 0.7432(5) 0.2319(2) 0.0486(16) Uani 1 1 d . A .
C24 C 0.7008(4) 0.7898(5) 0.2644(2) 0.0498(16) Uani 1 1 d . . .
C25 C 0.7355(4) 0.8520(5) 0.3015(3) 0.0523(16) Uani 1 1 d . A .
H25 H 0.7012 0.8845 0.3235 0.063 Uiso 1 1 calc R . .
C26 C 0.8171(4) 0.8697(5) 0.3085(3) 0.0527(17) Uani 1 1 d . . .
C27 C 0.8651(4) 0.8163(5) 0.2764(3) 0.0517(17) Uani 1 1 d . A .
H27 H 0.9217 0.8258 0.2802 0.062 Uiso 1 1 calc R . .
C28 C 0.8342(3) 0.7509(4) 0.2397(2) 0.0442(15) Uani 1 1 d . . .
C29 C 0.8553(4) 0.9438(5) 0.3479(3) 0.0621(18) Uani 1 1 d U A .
C30 C 0.9142(8) 0.8864(10) 0.3832(5) 0.087(5) Uani 0.694(15) 1 d PDU A 1
H30A H 0.8861 0.8308 0.3989 0.131 Uiso 0.694(15) 1 calc PR A 1
H30B H 0.9370 0.9326 0.4093 0.131 Uiso 0.694(15) 1 calc PR A 1
H30C H 0.9574 0.8587 0.3644 0.131 Uiso 0.694(15) 1 calc PR A 1
C31 C 0.7909(8) 0.9855(12) 0.3810(6) 0.092(5) Uani 0.694(15) 1 d PDU A 1
H31A H 0.7655 0.9290 0.3978 0.138 Uiso 0.694(15) 1 calc PR A 1
H31B H 0.7500 1.0225 0.3601 0.138 Uiso 0.694(15) 1 calc PR A 1
H31C H 0.8163 1.0315 0.4063 0.138 Uiso 0.694(15) 1 calc PR A 1
C32 C 0.8939(9) 1.0283(10) 0.3227(5) 0.078(4) Uani 0.694(15) 1 d PDU A 1
H32A H 0.9180 1.0752 0.3480 0.117 Uiso 0.694(15) 1 calc PR A 1
H32B H 0.8535 1.0642 0.3009 0.117 Uiso 0.694(15) 1 calc PR A 1
H32C H 0.9359 1.0015 0.3025 0.117 Uiso 0.694(15) 1 calc PR A 1
C30X C 0.9491(17) 0.947(3) 0.3464(13) 0.096(10) Uani 0.306(15) 1 d PDU A 2
H30D H 0.9716 0.9948 0.3718 0.145 Uiso 0.306(15) 1 calc PR A 2
H30E H 0.9630 0.9693 0.3131 0.145 Uiso 0.306(15) 1 calc PR A 2
H30F H 0.9712 0.8793 0.3534 0.145 Uiso 0.306(15) 1 calc PR A 2
C31X C 0.832(3) 0.915(4) 0.4005(13) 0.117(11) Uani 0.306(15) 1 d PDU A 2
H31D H 0.8569 0.9633 0.4251 0.175 Uiso 0.306(15) 1 calc PR A 2
H31E H 0.8511 0.8465 0.4087 0.175 Uiso 0.306(15) 1 calc PR A 2
H31F H 0.7734 0.9180 0.4014 0.175 Uiso 0.306(15) 1 calc PR A 2
C32X C 0.834(3) 1.053(2) 0.3326(16) 0.120(12) Uani 0.306(15) 1 d PDU A 2
H32D H 0.8591 1.0996 0.3575 0.180 Uiso 0.306(15) 1 calc PR A 2
H32E H 0.7755 1.0612 0.3307 0.180 Uiso 0.306(15) 1 calc PR A 2
H32F H 0.8539 1.0668 0.2996 0.180 Uiso 0.306(15) 1 calc PR A 2
C33 C 0.8923(4) 0.6855(5) 0.2131(3) 0.0518(16) Uani 1 1 d . A .
H33A H 0.8648 0.6582 0.1818 0.062 Uiso 1 1 calc R . .
H33B H 0.9381 0.7276 0.2037 0.062 Uiso 1 1 calc R . .
C34 C 0.8832(4) 0.5053(5) 0.2448(3) 0.0548(17) Uani 1 1 d . A .
C35 C 0.9233(3) 0.5992(5) 0.2457(2) 0.0499(16) Uani 1 1 d . . .
C36 C 0.9893(4) 0.6092(5) 0.2803(3) 0.0542(17) Uani 1 1 d . A .
H36 H 1.0172 0.6721 0.2819 0.065 Uiso 1 1 calc R . .
C37 C 1.0168(3) 0.5317(5) 0.3129(3) 0.0545(17) Uani 1 1 d . . .
C38 C 0.9743(4) 0.4401(5) 0.3088(3) 0.0559(18) Uani 1 1 d . A .
H38 H 0.9923 0.3857 0.3301 0.067 Uiso 1 1 calc R . .
C39 C 0.9084(4) 0.4243(5) 0.2760(3) 0.0531(17) Uani 1 1 d . . .
C40 C 1.0876(4) 0.5491(5) 0.3507(3) 0.0610(19) Uani 1 1 d . A .
C41 C 1.0738(6) 0.6453(7) 0.3808(4) 0.095(3) Uani 1 1 d . . .
H41A H 1.0702 0.7038 0.3581 0.142 Uiso 1 1 calc R A .
H41B H 1.1188 0.6550 0.4060 0.142 Uiso 1 1 calc R . .
H41C H 1.0236 0.6388 0.3974 0.142 Uiso 1 1 calc R . .
C42 C 1.1646(4) 0.5591(9) 0.3227(3) 0.100(3) Uani 1 1 d . . .
H42A H 1.1806 0.4920 0.3111 0.150 Uiso 1 1 calc R A .
H42B H 1.2078 0.5874 0.3453 0.150 Uiso 1 1 calc R . .
H42C H 1.1544 0.6042 0.2937 0.150 Uiso 1 1 calc R . .
C43 C 1.0997(5) 0.4620(7) 0.3890(3) 0.087(3) Uani 1 1 d . . .
H43A H 1.0509 0.4540 0.4070 0.131 Uiso 1 1 calc R A .
H43B H 1.1453 0.4778 0.4130 0.131 Uiso 1 1 calc R . .
H43C H 1.1106 0.3988 0.3714 0.131 Uiso 1 1 calc R . .
C44 C 0.8599(4) 0.3272(5) 0.2765(3) 0.0579(18) Uani 1 1 d . A .
H44A H 0.8962 0.2692 0.2850 0.069 Uiso 1 1 calc R . .
H44B H 0.8328 0.3149 0.2428 0.069 Uiso 1 1 calc R . .
O7 O 0.5412(3) 0.6245(4) 0.1599(2) 0.0739(14) Uani 1 1 d DU B .
C51 C 0.4624(6) 0.6257(8) 0.1346(4) 0.111(3) Uani 1 1 d DU . .
H51A H 0.4393 0.6949 0.1353 0.133 Uiso 0.78(2) 1 calc PR B 1
H51B H 0.4263 0.5788 0.1513 0.133 Uiso 0.78(2) 1 calc PR B 1
H51C H 0.4285 0.6704 0.1541 0.133 Uiso 0.22(2) 1 calc PR B 2
H51D H 0.4401 0.5563 0.1366 0.133 Uiso 0.22(2) 1 calc PR B 2
C52 C 0.4715(7) 0.5906(15) 0.0780(4) 0.124(6) Uani 0.78(2) 1 d PDU B 1
H52A H 0.5069 0.6381 0.0611 0.149 Uiso 0.78(2) 1 calc PR B 1
H52B H 0.4952 0.5218 0.0773 0.149 Uiso 0.78(2) 1 calc PR B 1
C53 C 0.3876(8) 0.5909(13) 0.0520(6) 0.181(6) Uani 1 1 d DU . .
H53A H 0.3902 0.5698 0.0170 0.271 Uiso 0.78(2) 1 calc PR B 1
H53B H 0.3650 0.6594 0.0531 0.271 Uiso 0.78(2) 1 calc PR B 1
H53C H 0.3534 0.5436 0.0691 0.271 Uiso 0.78(2) 1 calc PR B 1
H53D H 0.3896 0.5992 0.0156 0.271 Uiso 0.22(2) 1 calc PR B 2
H53E H 0.3341 0.6097 0.0618 0.271 Uiso 0.22(2) 1 calc PR B 2
H53F H 0.3986 0.5199 0.0611 0.271 Uiso 0.22(2) 1 calc PR B 2
C52X C 0.4514(18) 0.660(2) 0.0794(7) 0.090(8) Uani 0.22(2) 1 d PDU B 2
H52C H 0.5031 0.6538 0.0635 0.108 Uiso 0.22(2) 1 calc PR B 2
H52D H 0.4337 0.7312 0.0774 0.108 Uiso 0.22(2) 1 calc PR B 2
O9 O 0.8035(3) 0.5297(4) 0.1076(2) 0.0856(16) Uani 1 1 d DU . .
C54 C 0.8405(8) 0.5011(11) 0.0621(4) 0.150(5) Uani 1 1 d DU . .
H54A H 0.8402 0.4265 0.0580 0.180 Uiso 1 1 calc R . .
H54B H 0.8969 0.5254 0.0632 0.180 Uiso 1 1 calc R . .
C55 C 0.7916(13) 0.5499(17) 0.0208(6) 0.247(9) Uani 1 1 d DU . .
H55A H 0.8152 0.5363 -0.0114 0.297 Uiso 1 1 calc R . .
H55B H 0.7908 0.6243 0.0261 0.297 Uiso 1 1 calc R . .
C56 C 0.7046(14) 0.507(3) 0.0191(13) 0.42(2) Uani 1 1 d DU . .
H56A H 0.6715 0.5407 -0.0079 0.635 Uiso 1 1 calc R . .
H56B H 0.6817 0.5206 0.0513 0.635 Uiso 1 1 calc R . .
H56C H 0.7056 0.4342 0.0130 0.635 Uiso 1 1 calc R . .
N1 N 0.7645(7) 0.6731(9) 0.4413(4) 0.140(4) Uani 1 1 d D . .
C57 C 0.7795(6) 0.6447(7) 0.4019(4) 0.089(3) Uani 1 1 d D . .
C58 C 0.7960(4) 0.6076(5) 0.3553(3) 0.068(2) Uani 1 1 d D . .
H58A H 0.7609 0.5496 0.3467 0.102 Uiso 1 1 calc R . .
H58B H 0.8524 0.5860 0.3562 0.102 Uiso 1 1 calc R . .
H58C H 0.7865 0.6610 0.3300 0.102 Uiso 1 1 calc R . .
N2 N 1.0199(12) 0.2123(15) 0.4072(7) 0.126(6) Uani 0.50 1 d PDU . .
C59 C 1.056(2) 0.229(3) 0.4459(9) 0.117(9) Uani 0.327(15) 1 d PDU C 1
C60 C 1.072(2) 0.266(3) 0.4941(9) 0.123(12) Uani 0.327(15) 1 d PDU C 1
C59X C 1.064(4) 0.168(4) 0.436(2) 0.128(14) Uiso 0.173(15) 1 d PDU C 2
C60X C 1.128(3) 0.157(5) 0.471(2) 0.125(17) Uiso 0.173(15) 1 d PDU . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
O6 V1 O7 102.6(3) .
O6 V1 O2 108.4(3) .
O7 V1 O2 111.3(2) .
O6 V1 O5 107.7(3) .
O7 V1 O5 109.7(3) .
O2 V1 O5 116.2(2) .
O8 V2 O9 105.8(3) .
O8 V2 O4 111.7(3) .
O9 V2 O4 108.6(2) .
O8 V2 O5 109.4(3) .
O9 V2 O5 109.8(3) .
O4 V2 O5 111.4(2) .
V2 O5 V1 138.7(3) .
C1 O1 C45 113.6(8) .
C1 O1 C45X 114.3(8) .
C45 O1 C45X 35.4(7) .
O1 C45 C46 110.5(9) .
C45 C46 C47 109.4(9) .
C46X C47 C46 39.3(7) .
C46X C45X O1 111.2(10) .
C45X C46X C47 108.1(10) .
C12 O2 V1 137.0(4) .
C23 O3 C48 113.5(5) .
O3 C48 C49 113.8(5) .
C48 C49 C50 110.5(6) .
C34 O4 V2 151.0(4) .
C6 C1 O1 120.1(6) .
C6 C1 C2 120.8(7) .
O1 C1 C2 119.1(7) .
C3 C2 C1 117.4(7) .
C3 C2 C44 119.9(6) .
C1 C2 C44 122.6(7) .
C2 C3 C4 124.1(6) .
C5 C4 C3 116.0(7) .
C5 C4 C7 123.8(7) .
C3 C4 C7 120.1(6) .
C4 C5 C6 123.0(7) .
C1 C6 C5 118.5(6) .
C1 C6 C11 122.7(7) .
C5 C6 C11 118.6(7) .
C10 C7 C9 111.6(7) .
C10 C7 C4 111.1(6) .
C9 C7 C4 108.3(6) .
C10 C7 C8 108.3(7) .
C9 C7 C8 107.9(7) .
C4 C7 C8 109.7(6) .
C13 C11 C6 111.4(5) .
O2 C12 C17 116.6(6) .
O2 C12 C13 120.3(6) .
C17 C12 C13 123.0(7) .
C14 C13 C12 117.1(7) .
C14 C13 C11 121.8(7) .
C12 C13 C11 121.1(7) .
C13 C14 C15 123.5(7) .
C16 C15 C14 116.4(7) .
C16 C15 C18 119.9(7) .
C14 C15 C18 123.7(7) .
C17 C16 C15 123.1(7) .
C16 C17 C12 116.8(7) .
C16 C17 C22 122.6(6) .
C12 C17 C22 120.6(6) .
C15 C18 C19 109.0(7) .
C15 C18 C20 113.0(6) .
C19 C18 C20 108.1(7) .
C15 C18 C21 108.2(6) .
C19 C18 C21 111.7(8) .
C20 C18 C21 106.9(7) .
C17 C22 C24 112.1(5) .
C24 C23 C28 120.6(6) .
C24 C23 O3 119.9(5) .
C28 C23 O3 119.5(6) .
C25 C24 C23 118.4(6) .
C25 C24 C22 118.9(6) .
C23 C24 C22 122.7(6) .
C26 C25 C24 123.7(6) .
C25 C26 C27 115.7(6) .
C25 C26 C29 123.6(6) .
C27 C26 C29 120.7(6) .
C28 C27 C26 123.3(6) .
C27 C28 C23 117.9(6) .
C27 C28 C33 118.3(5) .
C23 C28 C33 123.7(5) .
C32 C29 C30 112.2(9) .
C32 C29 C32X 42.9(19) .
C30 C29 C32X 139.9(15) .
C32 C29 C31X 138.8(17) .
C30 C29 C31X 60.0(18) .
C32X C29 C31X 114(3) .
C32 C29 C26 109.9(7) .
C30 C29 C26 109.0(7) .
C32X C29 C26 109.7(14) .
C31X C29 C26 110.6(16) .
C32 C29 C31 109.8(9) .
C30 C29 C31 105.4(10) .
C32X C29 C31 70(2) .
C31X C29 C31 47.7(17) .
C26 C29 C31 110.4(7) .
C32 C29 C30X 59.9(15) .
C30 C29 C30X 55.1(15) .
C32X C29 C30X 100(2) .
C31X C29 C30X 110(2) .
C26 C29 C30X 111.3(11) .
C31 C29 C30X 137.9(12) .
C35 C33 C28 111.4(5) .
O4 C34 C39 120.3(6) .
O4 C34 C35 117.1(6) .
C39 C34 C35 122.6(6) .
C36 C35 C34 116.5(6) .
C36 C35 C33 122.4(6) .
C34 C35 C33 120.9(6) .
C35 C36 C37 123.5(6) .
C36 C37 C38 116.2(6) .
C36 C37 C40 120.6(6) .
C38 C37 C40 123.1(6) .
C39 C38 C37 123.9(6) .
C38 C39 C34 117.2(6) .
C38 C39 C44 121.7(6) .
C34 C39 C44 120.9(6) .
C37 C40 C41 109.7(6) .
C37 C40 C42 108.9(6) .
C41 C40 C42 110.4(7) .
C37 C40 C43 112.9(6) .
C41 C40 C43 106.7(7) .
C42 C40 C43 108.3(7) .
C39 C44 C2 109.7(5) .
C51 O7 V1 128.5(5) .
O7 C51 C52X 119.6(12) .
O7 C51 C52 107.1(8) .
C52X C51 C52 35.9(12) .
C53 C52 C51 106.5(11) .
C52 C53 C52X 37.0(12) .
C51 C52X C53 108.3(13) .
C54 O9 V2 131.3(7) .
O9 C54 C55 105.5(10) .
C54 C55 C56 109.2(16) .
C54 C55 C60X 84(2) 2_755
C56 C55 C60X 154(3) 2_755
N1 C57 C58 178.0(12) .
C59 N2 C59X 43(3) .
N2 C59 C60 159(4) .
N2 C59X C60X 156(4) .
C59X C60X C55 129(5) 2_745
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O6 1.587(5) .
V1 O7 1.746(5) .
V1 O2 1.760(5) .
V1 O5 1.778(5) .
V2 O8 1.576(6) .
V2 O9 1.738(6) .
V2 O4 1.753(5) .
V2 O5 1.766(5) .
O1 C1 1.393(8) .
O1 C45 1.466(10) .
O1 C45X 1.497(12) .
C45 C46 1.498(13) .
C46 C47 1.552(12) .
C47 C46X 1.536(12) .
C45X C46X 1.487(14) .
O2 C12 1.381(8) .
O3 C23 1.404(7) .
O3 C48 1.455(7) .
C48 C49 1.499(8) .
C49 C50 1.531(9) .
O4 C34 1.366(7) .
C1 C6 1.375(10) .
C1 C2 1.410(9) .
C2 C3 1.378(10) .
C2 C44 1.518(10) .
C3 C4 1.387(10) .
C4 C5 1.379(10) .
C4 C7 1.537(10) .
C5 C6 1.401(10) .
C6 C11 1.510(9) .
C7 C10 1.519(11) .
C7 C9 1.534(11) .
C7 C8 1.549(10) .
C11 C13 1.510(10) .
C12 C17 1.394(9) .
C12 C13 1.397(10) .
C13 C14 1.374(10) .
C14 C15 1.404(10) .
C15 C16 1.395(10) .
C15 C18 1.520(11) .
C16 C17 1.393(10) .
C17 C22 1.509(9) .
C18 C19 1.526(11) .
C18 C20 1.530(11) .
C18 C21 1.544(11) .
C22 C24 1.527(8) .
C23 C24 1.385(9) .
C23 C28 1.400(8) .
C24 C25 1.381(9) .
C25 C26 1.379(9) .
C26 C27 1.402(9) .
C26 C29 1.539(9) .
C27 C28 1.377(9) .
C28 C33 1.512(9) .
C29 C32 1.472(14) .
C29 C30 1.513(14) .
C29 C32X 1.53(3) .
C29 C31X 1.53(3) .
C29 C31 1.542(14) .
C29 C30X 1.57(3) .
C33 C35 1.501(9) .
C34 C39 1.400(9) .
C34 C35 1.406(9) .
C35 C36 1.390(9) .
C36 C37 1.397(9) .
C37 C38 1.399(9) .
C37 C40 1.514(9) .
C38 C39 1.371(9) .
C39 C44 1.515(9) .
C40 C41 1.527(11) .
C40 C42 1.538(10) .
C40 C43 1.541(10) .
O7 C51 1.433(10) .
C51 C52X 1.539(15) .
C51 C52 1.601(12) .
C52 C53 1.515(12) .
C53 C52X 1.540(15) .
O9 C54 1.452(10) .
C54 C55 1.471(12) .
C55 C56 1.552(13) .
C55 C60X 1.95(6) 2_755
N1 C57 1.161(12) .
C57 C58 1.384(13) .
N2 C59 1.175(14) .
N2 C59X 1.176(15) .
C59 C60 1.386(16) .
C59X C60X 1.383(16) .
C60X C55 1.95(6) 2_745
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O8 V2 O5 V1 134.2(5) .
O9 V2 O5 V1 -110.2(5) .
O4 V2 O5 V1 10.2(5) .
O6 V1 O5 V2 -135.6(5) .
O7 V1 O5 V2 113.5(5) .
O2 V1 O5 V2 -13.8(6) .
C1 O1 C45 C46 -66.5(15) .
C45X O1 C45 C46 32.7(13) .
O1 C45 C46 C47 -178.6(11) .
C45 C46 C47 C46X -31.0(12) .
C1 O1 C45X C46X 66.2(14) .
C45 O1 C45X C46X -30.8(13) .
O1 C45X C46X C47 -178.0(10) .
C46 C47 C46X C45X 32.9(13) .
O6 V1 O2 C12 -49.0(7) .
O7 V1 O2 C12 63.1(6) .
O5 V1 O2 C12 -170.5(6) .
C23 O3 C48 C49 -68.1(7) .
O3 C48 C49 C50 -177.5(6) .
O8 V2 O4 C34 48.7(10) .
O9 V2 O4 C34 -67.6(10) .
O5 V2 O4 C34 171.3(9) .
C45 O1 C1 C6 -71.5(9) .
C45X O1 C1 C6 -110.3(9) .
C45 O1 C1 C2 109.7(8) .
C45X O1 C1 C2 70.8(9) .
C6 C1 C2 C3 5.5(9) .
O1 C1 C2 C3 -175.6(5) .
C6 C1 C2 C44 -169.7(6) .
O1 C1 C2 C44 9.2(9) .
C1 C2 C3 C4 -3.1(9) .
C44 C2 C3 C4 172.2(6) .
C2 C3 C4 C5 -0.9(9) .
C2 C3 C4 C7 -179.3(6) .
C3 C4 C5 C6 2.6(9) .
C7 C4 C5 C6 -179.0(6) .
O1 C1 C6 C5 177.2(5) .
C2 C1 C6 C5 -4.0(9) .
O1 C1 C6 C11 -7.9(9) .
C2 C1 C6 C11 170.9(6) .
C4 C5 C6 C1 -0.2(10) .
C4 C5 C6 C11 -175.4(6) .
C5 C4 C7 C10 -4.4(10) .
C3 C4 C7 C10 173.9(7) .
C5 C4 C7 C9 118.5(8) .
C3 C4 C7 C9 -63.3(8) .
C5 C4 C7 C8 -124.1(7) .
C3 C4 C7 C8 54.2(9) .
C1 C6 C11 C13 -103.7(8) .
C5 C6 C11 C13 71.2(8) .
V1 O2 C12 C17 -93.4(7) .
V1 O2 C12 C13 89.4(8) .
O2 C12 C13 C14 176.1(5) .
C17 C12 C13 C14 -0.9(9) .
O2 C12 C13 C11 -2.8(9) .
C17 C12 C13 C11 -179.8(6) .
C6 C11 C13 C14 -97.3(8) .
C6 C11 C13 C12 81.6(8) .
C12 C13 C14 C15 -0.2(10) .
C11 C13 C14 C15 178.7(6) .
C13 C14 C15 C16 1.4(10) .
C13 C14 C15 C18 -179.4(6) .
C14 C15 C16 C17 -1.7(10) .
C18 C15 C16 C17 179.1(6) .
C15 C16 C17 C12 0.7(9) .
C15 C16 C17 C22 -179.6(6) .
O2 C12 C17 C16 -176.5(5) .
C13 C12 C17 C16 0.6(9) .
O2 C12 C17 C22 3.8(9) .
C13 C12 C17 C22 -179.1(6) .
C16 C15 C18 C19 65.4(9) .
C14 C15 C18 C19 -113.8(8) .
C16 C15 C18 C20 -174.4(6) .
C14 C15 C18 C20 6.4(10) .
C16 C15 C18 C21 -56.2(9) .
C14 C15 C18 C21 124.6(8) .
C16 C17 C22 C24 98.6(7) .
C12 C17 C22 C24 -81.7(8) .
C48 O3 C23 C24 102.6(6) .
C48 O3 C23 C28 -77.9(7) .
C28 C23 C24 C25 6.3(9) .
O3 C23 C24 C25 -174.2(5) .
C28 C23 C24 C22 -171.4(6) .
O3 C23 C24 C22 8.1(9) .
C17 C22 C24 C25 -75.1(8) .
C17 C22 C24 C23 102.6(7) .
C23 C24 C25 C26 -0.7(10) .
C22 C24 C25 C26 177.1(6) .
C24 C25 C26 C27 -2.7(10) .
C24 C25 C26 C29 176.3(6) .
C25 C26 C27 C28 0.7(9) .
C29 C26 C27 C28 -178.4(6) .
C26 C27 C28 C23 4.6(9) .
C26 C27 C28 C33 -170.5(6) .
C24 C23 C28 C27 -8.1(9) .
O3 C23 C28 C27 172.4(5) .
C24 C23 C28 C33 166.7(6) .
O3 C23 C28 C33 -12.8(9) .
C25 C26 C29 C32 -115.5(10) .
C27 C26 C29 C32 63.4(10) .
C25 C26 C29 C30 121.1(9) .
C27 C26 C29 C30 -59.9(10) .
C25 C26 C29 C32X -70(2) .
C27 C26 C29 C32X 109(2) .
C25 C26 C29 C31X 57(2) .
C27 C26 C29 C31X -124(2) .
C25 C26 C29 C31 5.8(12) .
C27 C26 C29 C31 -175.3(9) .
C25 C26 C29 C30X -179.9(17) .
C27 C26 C29 C30X -1.0(18) .
C27 C28 C33 C35 75.5(7) .
C23 C28 C33 C35 -99.4(7) .
V2 O4 C34 C39 -83.1(11) .
V2 O4 C34 C35 98.5(9) .
O4 C34 C35 C36 176.8(6) .
C39 C34 C35 C36 -1.5(9) .
O4 C34 C35 C33 0.9(9) .
C39 C34 C35 C33 -177.5(6) .
C28 C33 C35 C36 -85.6(7) .
C28 C33 C35 C34 90.1(7) .
C34 C35 C36 C37 0.6(9) .
C33 C35 C36 C37 176.5(6) .
C35 C36 C37 C38 0.6(10) .
C35 C36 C37 C40 -178.1(6) .
C36 C37 C38 C39 -1.1(10) .
C40 C37 C38 C39 177.6(6) .
C37 C38 C39 C34 0.3(10) .
C37 C38 C39 C44 -174.2(6) .
O4 C34 C39 C38 -177.2(6) .
C35 C34 C39 C38 1.1(10) .
O4 C34 C39 C44 -2.7(10) .
C35 C34 C39 C44 175.6(6) .
C36 C37 C40 C41 51.3(9) .
C38 C37 C40 C41 -127.3(8) .
C36 C37 C40 C42 -69.6(9) .
C38 C37 C40 C42 111.8(8) .
C36 C37 C40 C43 170.1(7) .
C38 C37 C40 C43 -8.5(10) .
C38 C39 C44 C2 85.4(7) .
C34 C39 C44 C2 -88.8(8) .
C3 C2 C44 C39 -72.6(8) .
C1 C2 C44 C39 102.5(7) .
O6 V1 O7 C51 -11.3(8) .
O2 V1 O7 C51 -127.0(7) .
O5 V1 O7 C51 103.0(7) .
V1 O7 C51 C52X -126.9(15) .
V1 O7 C51 C52 -90.0(10) .
O7 C51 C52 C53 179.2(11) .
C52X C51 C52 C53 -63.5(14) .
C51 C52 C53 C52X 60.7(13) .
O7 C51 C52X C53 140.7(17) .
C52 C51 C52X C53 62.8(14) .
C52 C53 C52X C51 -66.3(14) .
O8 V2 O9 C54 4.4(9) .
O4 V2 O9 C54 124.5(8) .
O5 V2 O9 C54 -113.5(8) .
V2 O9 C54 C55 125.1(13) .
O9 C54 C55 C56 -62(2) .
O9 C54 C55 C60X 95(2) 2_755
C59X N2 C59 C60 -141(14) .
C59 N2 C59X C60X -31(16) .
N2 C59X C60X C55 -142(17) 2_745
