#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:23:45 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261518 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/95/1559561.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_1559561
loop_
_publ_author_name
'Xing, Tian'
'Prior, Timothy J.'
'Elsegood, Mark R. J.'
'Semikolenova, Nina V.'
'Soshnikov, Igor E.'
'Bryliakov, Konstantin'
'Chen, Kai'
'Redshaw, Carl'
_publ_section_title
;
 Vanadium complexes derived from oxacalix[6]arenes: structural studies and
 use in the ring opening homo-/co-polymerization of
 ε-caprolactone/δ-valerolactone and ethylene polymerization
;
_journal_issue                   2
_journal_name_full               'Catalysis Science & Technology'
_journal_page_first              624
_journal_page_last               636
_journal_paper_doi               10.1039/D0CY01979H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C96 H108 N4 O8 V2, 4(C2 H3 N)'
_chemical_formula_sum            'C104 H120 N8 O8 V2'
_chemical_formula_weight         1711.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.8728(8)
_cell_angle_beta                 107.9966(7)
_cell_angle_gamma                99.2458(8)
_cell_formula_units_Z            1
_cell_length_a                   12.0966(2)
_cell_length_b                   12.3373(2)
_cell_length_c                   17.8971(3)
_cell_measurement_reflns_used    7770
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.26
_cell_volume                     2501.28(7)
_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'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6939
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29287
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         1.755
_diffrn_source                   'Daresbury SRS station 9.8'
_diffrn_standards_decay_%        4
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         12217
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1100P)²+0.3328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8563
_reflns_number_total             12217
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cy01979h2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 1559560--1559566.cif.'
_cod_database_code               1559561
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.991
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.87129(3) 0.58677(3) 0.58410(2) 0.03871(12) Uani 1 1 d . . . . .
O1 O 0.82922(14) 0.53273(12) 0.67251(8) 0.0440(3) Uani 1 1 d . . . . .
O2 O 0.61703(15) 0.40201(14) 0.65323(9) 0.0486(4) Uani 1 1 d . . . . .
H2 H 0.687(3) 0.433(3) 0.6630(19) 0.073 Uiso 1 1 d . U . . .
O3 O 0.24734(14) 0.40392(12) 0.51209(8) 0.0425(3) Uani 1 1 d . . . . .
O4 O 1.00665(15) 0.62887(14) 0.59306(11) 0.0534(4) Uani 1 1 d . . . . .
N1 N 0.84190(17) 0.74175(15) 0.61898(10) 0.0429(4) Uani 1 1 d . . . . .
N2 N 0.13605(17) 0.57884(15) 0.45171(11) 0.0439(4) Uani 1 1 d . . . . .
C1 C 0.8264(2) 0.82415(17) 0.56186(12) 0.0422(5) Uani 1 1 d . . . . .
C2 C 0.8958(2) 0.83652(18) 0.51245(14) 0.0467(5) Uani 1 1 d . . . . .
H2A H 0.955194 0.792702 0.517508 0.056 Uiso 1 1 calc R U . . .
C3 C 0.8784(2) 0.91247(19) 0.45605(14) 0.0499(5) Uani 1 1 d . . . . .
H3 H 0.927128 0.921194 0.423142 0.060 Uiso 1 1 calc R U . . .
C4 C 0.7911(2) 0.97640(18) 0.44637(14) 0.0502(5) Uani 1 1 d . . . . .
C5 C 0.7223(2) 0.9628(2) 0.49497(15) 0.0533(6) Uani 1 1 d . . . . .
H5 H 0.661574 1.005311 0.488875 0.064 Uiso 1 1 calc R U . . .
C6 C 0.7399(2) 0.88740(19) 0.55326(14) 0.0495(5) Uani 1 1 d . . . . .
H6 H 0.692262 0.879845 0.586891 0.059 Uiso 1 1 calc R U . . .
C7 C 0.7701(3) 1.0571(2) 0.38207(16) 0.0640(7) Uani 1 1 d . . . . .
H7A H 0.710866 1.099803 0.387182 0.096 Uiso 1 1 calc R U . . .
H7B H 0.741894 1.016427 0.330364 0.096 Uiso 1 1 calc R U . . .
H7C H 0.844186 1.107098 0.387251 0.096 Uiso 1 1 calc R U . . .
C8 C 0.8466(2) 0.77013(19) 0.68984(13) 0.0508(5) Uani 1 1 d . . . . .
H8 H 0.846656 0.845550 0.701408 0.061 Uiso 1 1 calc R U . . .
C9 C 0.84137(19) 0.58258(18) 0.74228(12) 0.0431(5) Uani 1 1 d . . . . .
C10 C 0.8518(2) 0.69744(19) 0.75346(13) 0.0472(5) Uani 1 1 d . . . . .
C11 C 0.8620(2) 0.7444(2) 0.82780(13) 0.0530(6) Uani 1 1 d . . . . .
H11 H 0.869161 0.821968 0.834930 0.064 Uiso 1 1 calc R U . . .
C12 C 0.8620(2) 0.6809(2) 0.89112(13) 0.0520(6) Uani 1 1 d . . . . .
C13 C 0.8492(2) 0.5672(2) 0.87721(13) 0.0500(5) Uani 1 1 d . . . . .
H13 H 0.848014 0.522088 0.919601 0.060 Uiso 1 1 calc R U . . .
C14 C 0.8382(2) 0.51645(19) 0.80497(13) 0.0449(5) Uani 1 1 d . . . . .
C15 C 0.8810(3) 0.7355(2) 0.97289(14) 0.0642(7) Uani 1 1 d . U . . .
C16 C 1.0121(4) 0.7815(5) 1.0089(2) 0.1142(15) Uani 1 1 d . U . . .
H16A H 1.036333 0.836398 0.975468 0.171 Uiso 1 1 calc R U . . .
H16B H 1.057464 0.721616 1.013000 0.171 Uiso 1 1 calc R U . . .
H16C H 1.026753 0.816169 1.061534 0.171 Uiso 1 1 calc R U . . .
C17 C 0.8145(4) 0.8289(4) 0.9681(2) 0.1101(15) Uani 1 1 d . U . . .
H17A H 0.729788 0.801264 0.944736 0.165 Uiso 1 1 calc R U . . .
H17B H 0.840203 0.884070 0.935357 0.165 Uiso 1 1 calc R U . . .
H17C H 0.830067 0.862503 1.021138 0.165 Uiso 1 1 calc R U . . .
C18 C 0.8482(6) 0.6533(4) 1.0285(2) 0.145(2) Uani 1 1 d . U . . .
H18A H 0.872790 0.688776 1.081793 0.218 Uiso 1 1 calc R U . . .
H18B H 0.888113 0.590127 1.028800 0.218 Uiso 1 1 calc R U . . .
H18C H 0.762565 0.628181 1.010599 0.218 Uiso 1 1 calc R U . . .
C19 C 0.8235(2) 0.39256(19) 0.79303(13) 0.0458(5) Uani 1 1 d . . . . .
H19A H 0.878269 0.365065 0.839241 0.055 Uiso 1 1 calc R U . . .
H19B H 0.845939 0.374447 0.746214 0.055 Uiso 1 1 calc R U . . .
C20 C 0.6043(2) 0.34235(17) 0.71511(12) 0.0417(5) Uani 1 1 d . . . . .
C21 C 0.6989(2) 0.33335(17) 0.78194(12) 0.0417(5) Uani 1 1 d . . . . .
C22 C 0.6760(2) 0.26729(18) 0.84036(12) 0.0434(5) Uani 1 1 d . . . . .
H22 H 0.739862 0.260379 0.885891 0.052 Uiso 1 1 calc R U . . .
C23 C 0.5645(2) 0.21172(18) 0.83464(12) 0.0448(5) Uani 1 1 d . . . . .
C24 C 0.4719(2) 0.22603(17) 0.76811(13) 0.0428(5) Uani 1 1 d . . . . .
H24 H 0.394162 0.190626 0.763587 0.051 Uiso 1 1 calc R U . . .
C25 C 0.4894(2) 0.29026(17) 0.70814(12) 0.0411(4) Uani 1 1 d . . . . .
C26 C 0.5400(2) 0.1384(2) 0.89840(14) 0.0541(6) Uani 1 1 d . . . . .
C27 C 0.6540(3) 0.1278(3) 0.96323(18) 0.0823(10) Uani 1 1 d . . . . .
H27A H 0.691629 0.200215 0.990327 0.123 Uiso 1 1 calc R U . . .
H27B H 0.707796 0.099231 0.939810 0.123 Uiso 1 1 calc R U . . .
H27C H 0.635730 0.077095 1.001096 0.123 Uiso 1 1 calc R U . . .
C28 C 0.4809(4) 0.0232(2) 0.86093(18) 0.0828(10) Uani 1 1 d . . . . .
H28A H 0.466939 -0.024455 0.901563 0.124 Uiso 1 1 calc R U . . .
H28B H 0.532288 -0.006993 0.836260 0.124 Uiso 1 1 calc R U . . .
H28C H 0.405385 0.027210 0.820901 0.124 Uiso 1 1 calc R U . . .
C29 C 0.4603(3) 0.1873(3) 0.93490(18) 0.0743(8) Uani 1 1 d . . . . .
H29A H 0.387653 0.195899 0.893654 0.111 Uiso 1 1 calc R U . . .
H29B H 0.500888 0.259448 0.961414 0.111 Uiso 1 1 calc R U . . .
H29C H 0.440825 0.138375 0.973320 0.111 Uiso 1 1 calc R U . . .
C30 C 0.3867(2) 0.30813(17) 0.63894(13) 0.0435(5) Uani 1 1 d . . . . .
H30A H 0.319880 0.247052 0.632726 0.052 Uiso 1 1 calc R U . . .
H30B H 0.409652 0.306705 0.590456 0.052 Uiso 1 1 calc R U . . .
C31 C 0.27792(18) 0.46037(17) 0.58150(12) 0.0386(4) Uani 1 1 d . . . . .
C32 C 0.34690(18) 0.41652(17) 0.64843(12) 0.0399(4) Uani 1 1 d . . . . .
C33 C 0.3758(2) 0.4739(2) 0.72090(13) 0.0518(6) Uani 1 1 d . . . . .
H33 H 0.422201 0.443682 0.766014 0.062 Uiso 1 1 calc R U . . .
C34 C 0.3401(3) 0.5743(2) 0.73119(14) 0.0574(6) Uani 1 1 d . . . . .
C35 C 0.2779(2) 0.61864(19) 0.66470(14) 0.0494(5) Uani 1 1 d . . . . .
H35 H 0.255580 0.688198 0.669385 0.059 Uiso 1 1 calc R U . . .
C36 C 0.24641(19) 0.56375(17) 0.58982(12) 0.0412(4) Uani 1 1 d . . . . .
C37 C 0.3720(4) 0.6311(3) 0.81344(17) 0.0838(10) Uani 1 1 d D U . . .
C38 C 0.5057(6) 0.6644(8) 0.8458(4) 0.132(3) Uani 0.695(7) 1 d D U P A 1
H38A H 0.542477 0.599058 0.846442 0.198 Uiso 0.695(7) 1 calc R U P A 1
H38B H 0.532652 0.717463 0.812229 0.198 Uiso 0.695(7) 1 calc R U P A 1
H38C H 0.527859 0.698049 0.899464 0.198 Uiso 0.695(7) 1 calc R U P A 1
C39 C 0.3276(9) 0.5535(5) 0.8672(3) 0.114(3) Uani 0.695(7) 1 d D U P A 1
H39A H 0.359176 0.485054 0.867598 0.171 Uiso 0.695(7) 1 calc R U P A 1
H39B H 0.353932 0.588412 0.920744 0.171 Uiso 0.695(7) 1 calc R U P A 1
H39C H 0.241181 0.536950 0.847889 0.171 Uiso 0.695(7) 1 calc R U P A 1
C40 C 0.3225(7) 0.7338(4) 0.8142(3) 0.094(2) Uani 0.695(7) 1 d D U P A 1
H40A H 0.349995 0.785180 0.779863 0.142 Uiso 0.695(7) 1 calc R U P A 1
H40B H 0.236106 0.716240 0.795205 0.142 Uiso 0.695(7) 1 calc R U P A 1
H40C H 0.348857 0.767702 0.868060 0.142 Uiso 0.695(7) 1 calc R U P A 1
C38X C 0.4390(19) 0.5626(12) 0.8786(6) 0.115(5) Uani 0.305(7) 1 d D U P A 2
H38D H 0.388826 0.491654 0.878178 0.173 Uiso 0.305(7) 1 calc R U P A 2
H38E H 0.511505 0.550103 0.868935 0.173 Uiso 0.305(7) 1 calc R U P A 2
H38F H 0.459029 0.602722 0.930061 0.173 Uiso 0.305(7) 1 calc R U P A 2
C39X C 0.2516(13) 0.6374(16) 0.8264(8) 0.134(5) Uani 0.305(7) 1 d D U P A 2
H39D H 0.206734 0.562877 0.822787 0.200 Uiso 0.305(7) 1 calc R U P A 2
H39E H 0.265716 0.673059 0.878593 0.200 Uiso 0.305(7) 1 calc R U P A 2
H39F H 0.206620 0.680252 0.785939 0.200 Uiso 0.305(7) 1 calc R U P A 2
C40X C 0.4527(16) 0.7382(11) 0.8170(9) 0.149(6) Uani 0.305(7) 1 d D U P A 2
H40D H 0.474037 0.775793 0.869383 0.223 Uiso 0.305(7) 1 calc R U P A 2
H40E H 0.524211 0.724089 0.806616 0.223 Uiso 0.305(7) 1 calc R U P A 2
H40F H 0.412451 0.784701 0.777205 0.223 Uiso 0.305(7) 1 calc R U P A 2
C41 C 0.1825(2) 0.61811(19) 0.52374(13) 0.0459(5) Uani 1 1 d . . . . .
H41 H 0.173495 0.691263 0.534494 0.055 Uiso 1 1 calc R U . . .
C42 C 0.0822(2) 0.65254(18) 0.39581(13) 0.0435(5) Uani 1 1 d . . . . .
C43 C 0.1385(2) 0.7603(2) 0.39627(15) 0.0540(6) Uani 1 1 d . . . . .
H43 H 0.214375 0.785710 0.433100 0.065 Uiso 1 1 calc R U . . .
C44 C 0.0835(3) 0.8307(2) 0.34274(17) 0.0611(7) Uani 1 1 d . . . . .
H44 H 0.122593 0.904237 0.343773 0.073 Uiso 1 1 calc R U . . .
C45 C -0.0259(2) 0.7969(2) 0.28839(14) 0.0531(6) Uani 1 1 d . . . . .
C46 C -0.0810(2) 0.6896(2) 0.28843(15) 0.0543(6) Uani 1 1 d . . . . .
H46 H -0.156981 0.664541 0.251649 0.065 Uiso 1 1 calc R U . . .
C47 C -0.0273(2) 0.6175(2) 0.34125(14) 0.0503(5) Uani 1 1 d . . . . .
H47 H -0.066376 0.543853 0.339685 0.060 Uiso 1 1 calc R U . . .
C48 C -0.0853(3) 0.8755(3) 0.23086(18) 0.0727(8) Uani 1 1 d . . . . .
H48A H -0.115351 0.927174 0.258535 0.109 Uiso 1 1 calc R U . . .
H48B H -0.150981 0.833460 0.188359 0.109 Uiso 1 1 calc R U . . .
H48C H -0.027880 0.916384 0.208621 0.109 Uiso 1 1 calc R U . . .
N3 N 0.4355(3) 0.8117(3) 0.5400(3) 0.1114(12) Uani 1 1 d . . . . .
C49 C 0.4751(3) 0.7306(3) 0.5527(3) 0.0925(12) Uani 1 1 d . . . . .
C50 C 0.5222(4) 0.6304(3) 0.5638(3) 0.1113(16) Uani 1 1 d . . . . .
H50A H 0.460070 0.568348 0.537259 0.167 Uiso 1 1 calc R U . . .
H50B H 0.551616 0.619742 0.620184 0.167 Uiso 1 1 calc R U . . .
H50C H 0.587129 0.634724 0.541444 0.167 Uiso 1 1 calc R U . . .
N4 N 0.7700(5) -0.0024(4) 0.7793(3) 0.1456(19) Uani 1 1 d . . . . .
C51 C 0.6908(6) 0.0203(4) 0.7278(3) 0.1184(18) Uani 1 1 d . . . . .
C52 C 0.6013(4) 0.0563(3) 0.6653(3) 0.0962(12) Uani 1 1 d . . . . .
H52A H 0.548507 0.089444 0.687103 0.144 Uiso 1 1 calc R U . . .
H52B H 0.555868 -0.006734 0.628728 0.144 Uiso 1 1 calc R U . . .
H52C H 0.638201 0.111030 0.637153 0.144 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 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 0.0063 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0108 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2967 0.5131 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V1 O3 120.36(8) . 2_666 ?
O4 V1 O1 119.49(8) . . ?
O3 V1 O1 120.09(7) 2_666 . ?
O4 V1 N2 97.27(8) . 2_666 ?
O3 V1 N2 87.95(7) 2_666 2_666 ?
O1 V1 N2 87.12(7) . 2_666 ?
O4 V1 N1 94.58(8) . . ?
O3 V1 N1 86.57(7) 2_666 . ?
O1 V1 N1 86.53(7) . . ?
N2 V1 N1 168.13(7) 2_666 . ?
C9 O1 V1 131.18(14) . . ?
C20 O2 H2 110(2) . . ?
C31 O3 V1 131.67(13) . 2_666 ?
C8 N1 C1 117.87(19) . . ?
C8 N1 V1 124.00(15) . . ?
C1 N1 V1 117.87(13) . . ?
C41 N2 C42 116.41(19) . . ?
C41 N2 V1 123.06(15) . 2_666 ?
C42 N2 V1 120.44(14) . 2_666 ?
C6 C1 C2 119.3(2) . . ?
C6 C1 N1 120.7(2) . . ?
C2 C1 N1 119.9(2) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 121.4(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 C7 121.0(2) . . ?
C3 C4 C7 120.8(2) . . ?
C4 C5 C6 121.2(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 119.9(2) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C10 126.1(2) . . ?
N1 C8 H8 117.0 . . ?
C10 C8 H8 117.0 . . ?
O1 C9 C14 118.1(2) . . ?
O1 C9 C10 122.30(19) . . ?
C14 C9 C10 119.5(2) . . ?
C11 C10 C9 119.5(2) . . ?
C11 C10 C8 117.9(2) . . ?
C9 C10 C8 122.6(2) . . ?
C12 C11 C10 122.0(2) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C11 C12 C13 116.8(2) . . ?
C11 C12 C15 120.6(2) . . ?
C13 C12 C15 122.6(2) . . ?
C14 C13 C12 123.7(2) . . ?
C14 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
C13 C14 C9 118.6(2) . . ?
C13 C14 C19 121.4(2) . . ?
C9 C14 C19 120.0(2) . . ?
C17 C15 C16 108.0(3) . . ?
C17 C15 C18 109.8(4) . . ?
C16 C15 C18 106.9(4) . . ?
C17 C15 C12 111.8(2) . . ?
C16 C15 C12 107.8(3) . . ?
C18 C15 C12 112.2(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 C21 113.56(19) . . ?
C14 C19 H19A 108.9 . . ?
C21 C19 H19A 108.9 . . ?
C14 C19 H19B 108.9 . . ?
C21 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
O2 C20 C21 122.9(2) . . ?
O2 C20 C25 116.17(18) . . ?
C21 C20 C25 120.90(19) . . ?
C20 C21 C22 118.0(2) . . ?
C20 C21 C19 122.33(19) . . ?
C22 C21 C19 119.70(19) . . ?
C23 C22 C21 122.9(2) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C22 C23 C24 117.15(19) . . ?
C22 C23 C26 122.8(2) . . ?
C24 C23 C26 120.1(2) . . ?
C25 C24 C23 122.4(2) . . ?
C25 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C24 C25 C20 118.57(19) . . ?
C24 C25 C30 121.0(2) . . ?
C20 C25 C30 120.40(19) . . ?
C29 C26 C28 110.1(3) . . ?
C29 C26 C27 108.8(2) . . ?
C28 C26 C27 107.8(3) . . ?
C29 C26 C23 109.4(2) . . ?
C28 C26 C23 109.1(2) . . ?
C27 C26 C23 111.6(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C30 C32 112.45(17) . . ?
C25 C30 H30A 109.1 . . ?
C32 C30 H30A 109.1 . . ?
C25 C30 H30B 109.1 . . ?
C32 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
O3 C31 C32 118.75(18) . . ?
O3 C31 C36 122.37(18) . . ?
C32 C31 C36 118.85(19) . . ?
C33 C32 C31 118.6(2) . . ?
C33 C32 C30 122.38(19) . . ?
C31 C32 C30 118.98(18) . . ?
C32 C33 C34 123.5(2) . . ?
C32 C33 H33 118.3 . . ?
C34 C33 H33 118.3 . . ?
C35 C34 C33 117.1(2) . . ?
C35 C34 C37 122.4(2) . . ?
C33 C34 C37 120.5(2) . . ?
C34 C35 C36 121.6(2) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 120.2(2) . . ?
C35 C36 C41 117.19(19) . . ?
C31 C36 C41 122.61(19) . . ?
C40 C37 C39 108.0(5) . . ?
C40 C37 C38 106.4(5) . . ?
C39 C37 C38 110.3(5) . . ?
C40 C37 C34 113.5(3) . . ?
C40X C37 C34 108.4(7) . . ?
C39 C37 C34 110.1(3) . . ?
C38 C37 C34 108.4(4) . . ?
C40X C37 C38X 107.1(10) . . ?
C34 C37 C38X 112.3(5) . . ?
C40X C37 C39X 116.8(10) . . ?
C34 C37 C39X 105.2(6) . . ?
C38X C37 C39X 107.3(10) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C38X H38D 109.5 . . ?
C37 C38X H38E 109.5 . . ?
H38D C38X H38E 109.5 . . ?
C37 C38X H38F 109.5 . . ?
H38D C38X H38F 109.5 . . ?
H38E C38X H38F 109.5 . . ?
C37 C39X H39D 109.5 . . ?
C37 C39X H39E 109.5 . . ?
H39D C39X H39E 109.5 . . ?
C37 C39X H39F 109.5 . . ?
H39D C39X H39F 109.5 . . ?
H39E C39X H39F 109.5 . . ?
C37 C40X H40D 109.5 . . ?
C37 C40X H40E 109.5 . . ?
H40D C40X H40E 109.5 . . ?
C37 C40X H40F 109.5 . . ?
H40D C40X H40F 109.5 . . ?
H40E C40X H40F 109.5 . . ?
N2 C41 C36 127.4(2) . . ?
N2 C41 H41 116.3 . . ?
C36 C41 H41 116.3 . . ?
C47 C42 C43 118.9(2) . . ?
C47 C42 N2 120.2(2) . . ?
C43 C42 N2 121.0(2) . . ?
C44 C43 C42 119.9(2) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 121.7(2) . . ?
C45 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
C44 C45 C46 117.9(2) . . ?
C44 C45 C48 121.0(3) . . ?
C46 C45 C48 121.1(2) . . ?
C45 C46 C47 121.4(2) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 H46 119.3 . . ?
C42 C47 C46 120.3(2) . . ?
C42 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N3 C49 C50 176.9(5) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N4 C51 C52 175.1(6) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O4 1.5933(17) . ?
V1 O3 1.8890(15) 2_666 ?
V1 O1 1.9046(15) . ?
V1 N2 2.1117(19) 2_666 ?
V1 N1 2.1192(18) . ?
O1 C9 1.339(3) . ?
O2 C20 1.373(2) . ?
O2 H2 0.84(3) . ?
O3 C31 1.331(2) . ?
N1 C8 1.292(3) . ?
N1 C1 1.445(3) . ?
N2 C41 1.288(3) . ?
N2 C42 1.438(3) . ?
C1 C6 1.376(3) . ?
C1 C2 1.390(3) . ?
C2 C3 1.379(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(4) . ?
C4 C7 1.522(3) . ?
C5 C6 1.398(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.452(3) . ?
C8 H8 0.9500 . ?
C9 C14 1.404(3) . ?
C9 C10 1.408(3) . ?
C10 C11 1.405(3) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(4) . ?
C12 C15 1.536(3) . ?
C13 C14 1.387(3) . ?
C13 H13 0.9500 . ?
C14 C19 1.514(3) . ?
C15 C17 1.497(5) . ?
C15 C16 1.523(5) . ?
C15 C18 1.523(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.518(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.397(3) . ?
C20 C25 1.401(3) . ?
C21 C22 1.402(3) . ?
C22 C23 1.384(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(3) . ?
C23 C26 1.537(3) . ?
C24 C25 1.392(3) . ?
C24 H24 0.9500 . ?
C25 C30 1.507(3) . ?
C26 C29 1.511(4) . ?
C26 C28 1.526(4) . ?
C26 C27 1.530(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C32 1.516(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.404(3) . ?
C31 C36 1.407(3) . ?
C32 C33 1.385(3) . ?
C33 C34 1.403(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.371(3) . ?
C34 C37 1.529(4) . ?
C35 C36 1.405(3) . ?
C35 H35 0.9500 . ?
C36 C41 1.440(3) . ?
C37 C40 1.487(5) . ?
C37 C40X 1.499(11) . ?
C37 C39 1.520(7) . ?
C37 C38 1.523(7) . ?
C37 C38X 1.549(10) . ?
C37 C39X 1.557(13) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C38X H38D 0.9800 . ?
C38X H38E 0.9800 . ?
C38X H38F 0.9800 . ?
C39X H39D 0.9800 . ?
C39X H39E 0.9800 . ?
C39X H39F 0.9800 . ?
C40X H40D 0.9800 . ?
C40X H40E 0.9800 . ?
C40X H40F 0.9800 . ?
C41 H41 0.9500 . ?
C42 C47 1.379(3) . ?
C42 C43 1.392(3) . ?
C43 C44 1.390(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.374(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.383(4) . ?
C45 C48 1.521(3) . ?
C46 C47 1.392(3) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N3 C49 1.173(5) . ?
C49 C50 1.434(5) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N4 C51 1.181(7) . ?
C51 C52 1.429(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84(3) 1.91(3) 2.723(2) 165(3) . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 C6 -48.6(3) . . . . ?
V1 N1 C1 C6 136.93(18) . . . . ?
C8 N1 C1 C2 134.4(2) . . . . ?
V1 N1 C1 C2 -40.1(3) . . . . ?
C6 C1 C2 C3 0.7(3) . . . . ?
N1 C1 C2 C3 177.7(2) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C2 C3 C4 C7 -177.9(2) . . . . ?
C3 C4 C5 C6 0.6(4) . . . . ?
C7 C4 C5 C6 178.9(2) . . . . ?
C2 C1 C6 C5 0.3(3) . . . . ?
N1 C1 C6 C5 -176.7(2) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C1 N1 C8 C10 174.5(2) . . . . ?
V1 N1 C8 C10 -11.4(4) . . . . ?
V1 O1 C9 C14 -159.72(16) . . . . ?
V1 O1 C9 C10 23.2(3) . . . . ?
O1 C9 C10 C11 178.8(2) . . . . ?
C14 C9 C10 C11 1.7(4) . . . . ?
O1 C9 C10 C8 1.9(4) . . . . ?
C14 C9 C10 C8 -175.2(2) . . . . ?
N1 C8 C10 C11 177.1(2) . . . . ?
N1 C8 C10 C9 -6.0(4) . . . . ?
C9 C10 C11 C12 -0.1(4) . . . . ?
C8 C10 C11 C12 176.9(2) . . . . ?
C10 C11 C12 C13 -1.1(4) . . . . ?
C10 C11 C12 C15 176.2(2) . . . . ?
C11 C12 C13 C14 0.7(4) . . . . ?
C15 C12 C13 C14 -176.5(2) . . . . ?
C12 C13 C14 C9 0.8(4) . . . . ?
C12 C13 C14 C19 -179.5(2) . . . . ?
O1 C9 C14 C13 -179.2(2) . . . . ?
C10 C9 C14 C13 -2.0(3) . . . . ?
O1 C9 C14 C19 1.0(3) . . . . ?
C10 C9 C14 C19 178.3(2) . . . . ?
C11 C12 C15 C17 42.0(4) . . . . ?
C13 C12 C15 C17 -140.9(3) . . . . ?
C11 C12 C15 C16 -76.6(4) . . . . ?
C13 C12 C15 C16 100.5(4) . . . . ?
C11 C12 C15 C18 165.9(4) . . . . ?
C13 C12 C15 C18 -17.0(5) . . . . ?
C13 C14 C19 C21 78.9(3) . . . . ?
C9 C14 C19 C21 -101.4(2) . . . . ?
O2 C20 C21 C22 -178.0(2) . . . . ?
C25 C20 C21 C22 2.3(3) . . . . ?
O2 C20 C21 C19 2.3(3) . . . . ?
C25 C20 C21 C19 -177.4(2) . . . . ?
C14 C19 C21 C20 68.2(3) . . . . ?
C14 C19 C21 C22 -111.5(2) . . . . ?
C20 C21 C22 C23 -0.3(3) . . . . ?
C19 C21 C22 C23 179.4(2) . . . . ?
C21 C22 C23 C24 -1.8(3) . . . . ?
C21 C22 C23 C26 179.3(2) . . . . ?
C22 C23 C24 C25 2.0(3) . . . . ?
C26 C23 C24 C25 -179.1(2) . . . . ?
C23 C24 C25 C20 0.0(3) . . . . ?
C23 C24 C25 C30 -177.1(2) . . . . ?
O2 C20 C25 C24 178.13(19) . . . . ?
C21 C20 C25 C24 -2.2(3) . . . . ?
O2 C20 C25 C30 -4.8(3) . . . . ?
C21 C20 C25 C30 174.95(19) . . . . ?
C22 C23 C26 C29 115.6(3) . . . . ?
C24 C23 C26 C29 -63.3(3) . . . . ?
C22 C23 C26 C28 -123.9(3) . . . . ?
C24 C23 C26 C28 57.2(3) . . . . ?
C22 C23 C26 C27 -4.9(4) . . . . ?
C24 C23 C26 C27 176.2(2) . . . . ?
C24 C25 C30 C32 97.8(2) . . . . ?
C20 C25 C30 C32 -79.3(3) . . . . ?
V1 O3 C31 C32 162.35(15) 2_666 . . . ?
V1 O3 C31 C36 -19.5(3) 2_666 . . . ?
O3 C31 C32 C33 -178.2(2) . . . . ?
C36 C31 C32 C33 3.6(3) . . . . ?
O3 C31 C32 C30 1.6(3) . . . . ?
C36 C31 C32 C30 -176.63(19) . . . . ?
C25 C30 C32 C33 -18.9(3) . . . . ?
C25 C30 C32 C31 161.33(19) . . . . ?
C31 C32 C33 C34 -0.2(4) . . . . ?
C30 C32 C33 C34 180.0(2) . . . . ?
C32 C33 C34 C35 -3.0(4) . . . . ?
C32 C33 C34 C37 178.0(3) . . . . ?
C33 C34 C35 C36 2.9(4) . . . . ?
C37 C34 C35 C36 -178.1(3) . . . . ?
C34 C35 C36 C31 0.4(4) . . . . ?
C34 C35 C36 C41 -179.2(2) . . . . ?
O3 C31 C36 C35 178.2(2) . . . . ?
C32 C31 C36 C35 -3.7(3) . . . . ?
O3 C31 C36 C41 -2.3(3) . . . . ?
C32 C31 C36 C41 175.9(2) . . . . ?
C35 C34 C37 C40 3.8(6) . . . . ?
C33 C34 C37 C40 -177.3(4) . . . . ?
C35 C34 C37 C40X -63.6(9) . . . . ?
C33 C34 C37 C40X 115.3(9) . . . . ?
C35 C34 C37 C39 125.1(5) . . . . ?
C33 C34 C37 C39 -56.0(6) . . . . ?
C35 C34 C37 C38 -114.2(5) . . . . ?
C33 C34 C37 C38 64.7(6) . . . . ?
C35 C34 C37 C38X 178.3(10) . . . . ?
C33 C34 C37 C38X -2.7(11) . . . . ?
C35 C34 C37 C39X 62.0(8) . . . . ?
C33 C34 C37 C39X -119.1(8) . . . . ?
C42 N2 C41 C36 -176.6(2) . . . . ?
V1 N2 C41 C36 6.7(3) 2_666 . . . ?
C35 C36 C41 N2 -173.2(2) . . . . ?
C31 C36 C41 N2 7.2(4) . . . . ?
C41 N2 C42 C47 -134.3(2) . . . . ?
V1 N2 C42 C47 42.4(3) 2_666 . . . ?
C41 N2 C42 C43 44.9(3) . . . . ?
V1 N2 C42 C43 -138.4(2) 2_666 . . . ?
C47 C42 C43 C44 0.6(4) . . . . ?
N2 C42 C43 C44 -178.6(2) . . . . ?
C42 C43 C44 C45 -0.3(4) . . . . ?
C43 C44 C45 C46 0.2(4) . . . . ?
C43 C44 C45 C48 179.3(3) . . . . ?
C44 C45 C46 C47 -0.5(4) . . . . ?
C48 C45 C46 C47 -179.6(3) . . . . ?
C43 C42 C47 C46 -0.9(4) . . . . ?
N2 C42 C47 C46 178.3(2) . . . . ?
C45 C46 C47 C42 0.9(4) . . . . ?
