# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1998549'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;


_vrf_PLAT201_shelx               
;
RESPONSE:The small-scale disorder present is modelled 
using isotropic displacement parameters.     
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 C76 H94 N4 Na2 O11 V2, 5(C2 H3 N)
;

_chemical_formula_sum            'C86 H109 N9 Na2 O11 V2'
_chemical_formula_weight         1592.68

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'
V V 0.3005 0.5294 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.4214(3)
_cell_length_b                   14.2596(5)
_cell_length_c                   25.2549(7)
_cell_angle_alpha                85.709(3)
_cell_angle_beta                 78.946(2)
_cell_angle_gamma                69.251(3)
_cell_volume                     4435.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22399
_cell_measurement_theta_min      2.156
_cell_measurement_theta_max      27.514

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.281
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67352
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            80640
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.817
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             19896
_reflns_number_gt                13923
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+23.1004P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19896
_refine_ls_number_parameters     975
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0988
_refine_ls_wR_factor_ref         0.2326
_refine_ls_wR_factor_gt          0.2160
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_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_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
C1 C 0.6986(4) 0.2170(3) 0.78722(19) 0.0224(9) Uani 1 1 d . . . . .
C2 C 0.5986(4) 0.2075(3) 0.80980(19) 0.0227(9) Uani 1 1 d . . . . .
C3 C 0.5977(4) 0.1210(4) 0.8390(2) 0.0278(10) Uani 1 1 d . . . . .
H3 H 0.529884 0.114733 0.854245 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6928(4) 0.0425(4) 0.8471(2) 0.0266(10) Uani 1 1 d . . . . .
C5 C 0.7901(4) 0.0551(4) 0.8235(2) 0.0259(10) Uani 1 1 d . . . . .
H5 H 0.855895 0.003302 0.827999 0.031 Uiso 1 1 calc R U . . .
C6 C 0.7957(4) 0.1400(3) 0.79361(19) 0.0236(10) Uani 1 1 d . . . . .
C7 C 0.6875(4) -0.0492(4) 0.8814(2) 0.0303(11) Uani 1 1 d . . . . .
C8A C 0.6266(8) -0.1012(7) 0.8597(4) 0.0528(13) Uiso 0.726(6) 1 d . U P A 1
H8A H 0.660585 -0.121177 0.822370 0.079 Uiso 0.726(6) 1 calc R U P A 1
H8B H 0.627218 -0.161013 0.881659 0.079 Uiso 0.726(6) 1 calc R U P A 1
H8C H 0.551743 -0.056074 0.860618 0.079 Uiso 0.726(6) 1 calc R U P A 1
C9A C 0.6372(8) -0.0167(7) 0.9397(4) 0.0528(13) Uiso 0.726(6) 1 d . U P A 1
H9A H 0.679097 0.017500 0.953069 0.079 Uiso 0.726(6) 1 calc R U P A 1
H9B H 0.562397 0.029023 0.941177 0.079 Uiso 0.726(6) 1 calc R U P A 1
H9C H 0.637873 -0.075916 0.962218 0.079 Uiso 0.726(6) 1 calc R U P A 1
C10A C 0.8028(7) -0.1271(7) 0.8847(4) 0.0528(13) Uiso 0.726(6) 1 d . U P A 1
H10A H 0.845015 -0.094432 0.899025 0.079 Uiso 0.726(6) 1 calc R U P A 1
H10B H 0.795876 -0.182748 0.908511 0.079 Uiso 0.726(6) 1 calc R U P A 1
H10C H 0.839543 -0.152757 0.848533 0.079 Uiso 0.726(6) 1 calc R U P A 1
C8B C 0.5657(19) -0.0494(19) 0.8996(10) 0.0528(13) Uiso 0.274(6) 1 d . U P A 2
H8B1 H 0.533088 -0.045181 0.867554 0.079 Uiso 0.274(6) 1 calc R U P A 2
H8B2 H 0.567183 -0.111473 0.919483 0.079 Uiso 0.274(6) 1 calc R U P A 2
H8B3 H 0.522740 0.008315 0.922846 0.079 Uiso 0.274(6) 1 calc R U P A 2
C9B C 0.736(2) -0.0554(19) 0.9285(10) 0.0528(13) Uiso 0.274(6) 1 d . U P A 2
H9B1 H 0.731520 -0.114452 0.950031 0.079 Uiso 0.274(6) 1 calc R U P A 2
H9B2 H 0.811593 -0.061122 0.917295 0.079 Uiso 0.274(6) 1 calc R U P A 2
H9B3 H 0.696472 0.005133 0.950193 0.079 Uiso 0.274(6) 1 calc R U P A 2
C10B C 0.740(2) -0.1422(19) 0.8453(10) 0.0528(13) Uiso 0.274(6) 1 d . U P A 2
H10D H 0.703143 -0.132678 0.814310 0.079 Uiso 0.274(6) 1 calc R U P A 2
H10E H 0.816577 -0.152085 0.832633 0.079 Uiso 0.274(6) 1 calc R U P A 2
H10F H 0.733283 -0.201319 0.866068 0.079 Uiso 0.274(6) 1 calc R U P A 2
C11 C 0.9032(4) 0.1528(4) 0.77041(19) 0.0245(10) Uani 1 1 d . . . . .
H11A H 0.896853 0.191025 0.736090 0.029 Uiso 1 1 calc R U . . .
H11B H 0.959312 0.085922 0.762278 0.029 Uiso 1 1 calc R U . . .
C12 C 0.9142(3) 0.3107(3) 0.80454(19) 0.0211(5) Uani 1 1 d . . . . .
C13 C 0.9389(3) 0.2072(3) 0.80864(19) 0.0211(5) Uani 1 1 d . . . . .
C14 C 0.9942(3) 0.1542(4) 0.84929(19) 0.0261(10) Uani 1 1 d . . . . .
H14 H 1.010867 0.083627 0.851679 0.031 Uiso 1 1 calc R U . . .
C15 C 1.0253(4) 0.1998(4) 0.88588(19) 0.0257(10) Uani 1 1 d . . . . .
C16 C 1.0014(4) 0.3039(4) 0.88057(19) 0.0260(10) Uani 1 1 d . . . . .
H16 H 1.023325 0.337079 0.904985 0.031 Uiso 1 1 calc R U . . .
C17 C 0.9467(3) 0.3602(3) 0.84085(19) 0.0211(5) Uani 1 1 d . . . . .
C18 C 1.0818(4) 0.1427(4) 0.9324(2) 0.0330(12) Uani 1 1 d . . . . .
C19 C 1.0055(5) 0.1788(5) 0.9857(2) 0.0529(17) Uani 1 1 d . . . . .
H19A H 0.986986 0.251384 0.988769 0.079 Uiso 1 1 calc R U . . .
H19B H 0.939348 0.163716 0.986860 0.079 Uiso 1 1 calc R U . . .
H19C H 1.041155 0.144596 1.015726 0.079 Uiso 1 1 calc R U . . .
C20 C 1.1097(5) 0.0295(4) 0.9284(3) 0.0488(16) Uani 1 1 d . . . . .
H20A H 1.158772 0.005292 0.894260 0.073 Uiso 1 1 calc R U . . .
H20B H 1.145049 -0.004309 0.958579 0.073 Uiso 1 1 calc R U . . .
H20C H 1.043241 0.014812 0.929714 0.073 Uiso 1 1 calc R U . . .
C21 C 1.1879(5) 0.1618(5) 0.9313(3) 0.0477(16) Uani 1 1 d . . . . .
H21A H 1.236607 0.138506 0.897006 0.071 Uiso 1 1 calc R U . . .
H21B H 1.172256 0.233784 0.935059 0.071 Uiso 1 1 calc R U . . .
H21C H 1.222519 0.125336 0.961195 0.071 Uiso 1 1 calc R U . . .
C22 C 0.9141(4) 0.4726(3) 0.83989(18) 0.0230(10) Uani 1 1 d . . . . .
H22A H 0.834188 0.502684 0.844905 0.028 Uiso 1 1 calc R U . . .
H22B H 0.937539 0.493844 0.870397 0.028 Uiso 1 1 calc R U . . .
C23 C 0.9179(3) 0.6179(3) 0.79144(19) 0.0233(10) Uani 1 1 d . . . . .
H23A H 0.940132 0.641414 0.821637 0.028 Uiso 1 1 calc R U . . .
H23B H 0.837822 0.641340 0.797839 0.028 Uiso 1 1 calc R U . . .
C24 C 0.9292(3) 0.6479(3) 0.69129(19) 0.0217(9) Uani 1 1 d . . . . .
C25 C 0.9577(3) 0.6622(3) 0.73954(19) 0.0236(10) Uani 1 1 d . . . . .
C26 C 1.0180(3) 0.7248(3) 0.7402(2) 0.0231(10) Uani 1 1 d . . . . .
H26 H 1.036642 0.734657 0.773248 0.028 Uiso 1 1 calc R U . . .
C27 C 1.0514(3) 0.7730(4) 0.6936(2) 0.0253(10) Uani 1 1 d . . . . .
C28 C 1.0225(3) 0.7555(4) 0.6463(2) 0.0248(10) Uani 1 1 d . . . . .
H28 H 1.044960 0.786771 0.613995 0.030 Uiso 1 1 calc R U . . .
C29 C 0.9629(3) 0.6950(4) 0.64376(19) 0.0228(10) Uani 1 1 d . . . . .
C30 C 1.1188(4) 0.8409(4) 0.6928(2) 0.0302(11) Uani 1 1 d . . . . .
C31 C 1.1332(4) 0.8585(4) 0.7495(2) 0.0363(12) Uani 1 1 d . . . . .
H31A H 1.168599 0.793960 0.766277 0.054 Uiso 1 1 calc R U . . .
H31B H 1.178133 0.900468 0.747123 0.054 Uiso 1 1 calc R U . . .
H31C H 1.062233 0.892385 0.771490 0.054 Uiso 1 1 calc R U . . .
C32 C 1.2319(4) 0.7912(4) 0.6589(2) 0.0357(12) Uani 1 1 d . . . . .
H32A H 1.224695 0.779195 0.622368 0.054 Uiso 1 1 calc R U . . .
H32B H 1.273994 0.835579 0.657145 0.054 Uiso 1 1 calc R U . . .
H32C H 1.269062 0.727270 0.675675 0.054 Uiso 1 1 calc R U . . .
C33 C 1.0634(4) 0.9427(4) 0.6671(2) 0.0338(12) Uani 1 1 d . . . . .
H33A H 1.053753 0.932244 0.630794 0.051 Uiso 1 1 calc R U . . .
H33B H 0.992550 0.976308 0.689308 0.051 Uiso 1 1 calc R U . . .
H33C H 1.108451 0.984392 0.664941 0.051 Uiso 1 1 calc R U . . .
C34 C 0.9331(3) 0.6803(4) 0.59090(19) 0.0254(10) Uani 1 1 d . . . . .
H34A H 0.926182 0.613418 0.591171 0.031 Uiso 1 1 calc R U . . .
H34B H 0.992280 0.681767 0.561011 0.031 Uiso 1 1 calc R U . . .
C35 C 0.7295(3) 0.7462(4) 0.59977(18) 0.0225(9) Uani 1 1 d . . . . .
C36 C 0.8281(3) 0.7598(4) 0.58055(18) 0.0228(10) Uani 1 1 d . . . . .
C37 C 0.8283(4) 0.8478(4) 0.55233(19) 0.0264(10) Uani 1 1 d . . . . .
H37 H 0.895484 0.857539 0.540196 0.032 Uiso 1 1 calc R U . . .
C38 C 0.7337(4) 0.9220(4) 0.54126(19) 0.0255(10) Uani 1 1 d . . . . .
C39 C 0.6371(4) 0.9034(4) 0.55925(19) 0.0243(10) Uani 1 1 d . . . . .
H39 H 0.571729 0.951566 0.551248 0.029 Uiso 1 1 calc R U . . .
C40 C 0.6321(4) 0.8179(4) 0.58825(18) 0.0237(10) Uani 1 1 d . . . . .
C41 C 0.7342(4) 1.0165(4) 0.5082(2) 0.0312(11) Uani 1 1 d . . . . .
C42 C 0.8372(4) 1.0402(4) 0.5077(2) 0.0386(13) Uani 1 1 d . . . . .
H42A H 0.843031 1.050776 0.544668 0.058 Uiso 1 1 calc R U . . .
H42B H 0.900467 0.983968 0.491781 0.058 Uiso 1 1 calc R U . . .
H42C H 0.833834 1.101008 0.486153 0.058 Uiso 1 1 calc R U . . .
C43 C 0.7261(5) 1.0002(5) 0.4503(2) 0.0394(13) Uani 1 1 d . . . . .
H43A H 0.660380 0.984943 0.450333 0.059 Uiso 1 1 calc R U . . .
H43B H 0.723001 1.061071 0.428951 0.059 Uiso 1 1 calc R U . . .
H43C H 0.789634 0.944031 0.434579 0.059 Uiso 1 1 calc R U . . .
C44 C 0.6373(5) 1.1082(4) 0.5314(3) 0.0456(15) Uani 1 1 d . . . . .
H44A H 0.641863 1.119267 0.568541 0.068 Uiso 1 1 calc R U . . .
H44B H 0.638390 1.167529 0.509342 0.068 Uiso 1 1 calc R U . . .
H44C H 0.569851 1.096353 0.531004 0.068 Uiso 1 1 calc R U . . .
C45 C 0.5252(3) 0.8035(4) 0.60993(19) 0.0234(10) Uani 1 1 d . . . . .
H45A H 0.473570 0.835990 0.585185 0.028 Uiso 1 1 calc R U . . .
H45B H 0.536235 0.730942 0.611537 0.028 Uiso 1 1 calc R U . . .
C46 C 0.4964(3) 0.7891(4) 0.71206(19) 0.0233(10) Uani 1 1 d . . . . .
C47 C 0.4781(3) 0.8478(4) 0.66556(19) 0.0225(10) Uani 1 1 d . . . . .
C48 C 0.4186(3) 0.9502(4) 0.67150(19) 0.0243(10) Uani 1 1 d . . . . .
H48 H 0.406974 0.990178 0.639908 0.029 Uiso 1 1 calc R U . . .
C49 C 0.3757(3) 0.9963(4) 0.72132(19) 0.0243(10) Uani 1 1 d . . . . .
C50 C 0.3918(4) 0.9350(4) 0.7670(2) 0.0245(10) Uani 1 1 d . . . . .
H50 H 0.361075 0.963959 0.801687 0.029 Uiso 1 1 calc R U . . .
C51 C 0.4517(3) 0.8322(3) 0.76317(19) 0.0213(9) Uani 1 1 d . . . . .
C52 C 0.3139(4) 1.1097(4) 0.7239(2) 0.0288(11) Uani 1 1 d . . . . .
C53 C 0.3905(5) 1.1639(4) 0.6945(2) 0.0397(13) Uani 1 1 d . . . . .
H53A H 0.416569 1.140563 0.657152 0.060 Uiso 1 1 calc R U . . .
H53B H 0.351207 1.236391 0.694689 0.060 Uiso 1 1 calc R U . . .
H53C H 0.452213 1.149082 0.713034 0.060 Uiso 1 1 calc R U . . .
C54 C 0.2150(4) 1.1358(4) 0.6967(2) 0.0367(13) Uani 1 1 d . . . . .
H54A H 0.238007 1.111721 0.659459 0.055 Uiso 1 1 calc R U . . .
H54B H 0.165153 1.103714 0.716538 0.055 Uiso 1 1 calc R U . . .
H54C H 0.178221 1.208673 0.696749 0.055 Uiso 1 1 calc R U . . .
C55 C 0.2752(4) 1.1481(4) 0.7817(2) 0.0342(12) Uani 1 1 d . . . . .
H55A H 0.337623 1.132023 0.799854 0.051 Uiso 1 1 calc R U . . .
H55B H 0.238184 1.220886 0.781239 0.051 Uiso 1 1 calc R U . . .
H55C H 0.225115 1.115926 0.801028 0.051 Uiso 1 1 calc R U . . .
C56 C 0.4765(4) 0.7729(4) 0.81350(19) 0.0249(10) Uani 1 1 d . . . . .
H56A H 0.555641 0.748484 0.812563 0.030 Uiso 1 1 calc R U . . .
H56B H 0.441457 0.817359 0.845095 0.030 Uiso 1 1 calc R U . . .
C57 C 0.4845(4) 0.6264(4) 0.86366(19) 0.0235(10) Uani 1 1 d . . . . .
H57A H 0.460016 0.666734 0.896991 0.028 Uiso 1 1 calc R U . . .
H57B H 0.564446 0.604583 0.855063 0.028 Uiso 1 1 calc R U . . .
C58 C 0.4869(3) 0.4594(4) 0.83463(18) 0.0217(9) Uani 1 1 d . . . . .
C59 C 0.4512(3) 0.5354(3) 0.87349(18) 0.0217(9) Uani 1 1 d . . . . .
C60 C 0.3913(4) 0.5220(4) 0.92330(19) 0.0247(10) Uani 1 1 d . . . . .
H60 H 0.367818 0.573513 0.949398 0.030 Uiso 1 1 calc R U . . .
C61 C 0.3645(4) 0.4361(4) 0.9363(2) 0.0264(10) Uani 1 1 d . . . . .
C62 C 0.3994(4) 0.3636(4) 0.8963(2) 0.0256(10) Uani 1 1 d . . . . .
H62 H 0.381837 0.304489 0.903848 0.031 Uiso 1 1 calc R U . . .
C63 C 0.4584(3) 0.3730(3) 0.84594(19) 0.0214(9) Uani 1 1 d . . . . .
C64 C 0.2993(4) 0.4222(4) 0.9913(2) 0.0332(12) Uani 1 1 d . . . . .
C65 C 0.2912(7) 0.4990(6) 1.0318(2) 0.070(2) Uani 1 1 d . . . . .
H65A H 0.257876 0.566652 1.017705 0.104 Uiso 1 1 calc R U . . .
H65B H 0.246677 0.489509 1.065905 0.104 Uiso 1 1 calc R U . . .
H65C H 0.363810 0.490628 1.037929 0.104 Uiso 1 1 calc R U . . .
C66 C 0.1847(5) 0.4338(6) 0.9842(3) 0.0554(18) Uani 1 1 d . . . . .
H66A H 0.188666 0.384539 0.958142 0.083 Uiso 1 1 calc R U . . .
H66B H 0.143217 0.422711 1.019001 0.083 Uiso 1 1 calc R U . . .
H66C H 0.148996 0.501603 0.971031 0.083 Uiso 1 1 calc R U . . .
C67 C 0.3512(6) 0.3178(5) 1.0140(3) 0.063(2) Uani 1 1 d . . . . .
H67A H 0.356959 0.267363 0.988157 0.094 Uiso 1 1 calc R U . . .
H67B H 0.423624 0.310047 1.020160 0.094 Uiso 1 1 calc R U . . .
H67C H 0.306491 0.308929 1.048136 0.094 Uiso 1 1 calc R U . . .
C68 C 0.4935(3) 0.2916(3) 0.8039(2) 0.0237(10) Uani 1 1 d . . . . .
H68A H 0.502176 0.322286 0.767607 0.028 Uiso 1 1 calc R U . . .
H68B H 0.435558 0.262850 0.806435 0.028 Uiso 1 1 calc R U . . .
C71 C 0.5488(5) 0.4113(5) 0.6493(2) 0.0436(14) Uani 1 1 d . . . . .
C72 C 0.6035(6) 0.3047(5) 0.6386(3) 0.067(2) Uani 1 1 d . . . . .
H72A H 0.652089 0.275073 0.664569 0.100 Uiso 1 1 calc R U . . .
H72B H 0.645719 0.295381 0.601910 0.100 Uiso 1 1 calc R U . . .
H72C H 0.549705 0.271714 0.642127 0.100 Uiso 1 1 calc R U . . .
C73 C 0.9570(5) 0.2655(5) 0.6138(3) 0.0481(15) Uani 1 1 d . . . . .
C74 C 0.9420(7) 0.1875(6) 0.5864(4) 0.084(3) Uani 1 1 d . . . . .
H74A H 1.009483 0.129605 0.580904 0.125 Uiso 1 1 calc R U . . .
H74B H 0.921918 0.212780 0.551355 0.125 Uiso 1 1 calc R U . . .
H74C H 0.884282 0.167138 0.608296 0.125 Uiso 1 1 calc R U . . .
C83 C 1.3266(10) 0.3116(8) 0.5513(4) 0.097(3) Uani 1 1 d . . . . .
C84 C 1.2280(9) 0.2886(8) 0.5519(3) 0.091(3) Uani 1 1 d . . . . .
H84C H 1.204116 0.265725 0.588073 0.137 Uiso 1 1 calc R U . . .
H84A H 1.243343 0.235631 0.525761 0.137 Uiso 1 1 calc R U . . .
H84B H 1.170899 0.348909 0.542279 0.137 Uiso 1 1 calc R U . . .
C77 C 1.1973(4) 0.4658(4) 0.6586(3) 0.0388(13) Uani 1 1 d . . . . .
C78 C 1.2503(5) 0.5330(5) 0.6311(3) 0.0554(17) Uani 1 1 d . . . . .
H78A H 1.217037 0.563111 0.599757 0.083 Uiso 1 1 calc R U . . .
H78B H 1.327338 0.495320 0.619205 0.083 Uiso 1 1 calc R U . . .
H78C H 1.242233 0.585974 0.655885 0.083 Uiso 1 1 calc R U . . .
C79 C 0.7456(5) 1.0215(5) 0.6759(3) 0.0452(14) Uani 1 1 d . . . . .
C80 C 0.7148(6) 0.9395(5) 0.7002(3) 0.0563(18) Uani 1 1 d . . . . .
H80A H 0.667843 0.960220 0.735247 0.085 Uiso 1 1 calc R U . . .
H80B H 0.779761 0.882693 0.705381 0.085 Uiso 1 1 calc R U . . .
H80C H 0.675747 0.919433 0.676694 0.085 Uiso 1 1 calc R U . . .
C81 C 0.6829(4) 0.2225(4) 0.9834(2) 0.0338(12) Uani 1 1 d . . . . .
C82 C 0.6918(5) 0.2588(5) 0.9282(2) 0.0422(14) Uani 1 1 d . . . . .
H82A H 0.630181 0.320353 0.925171 0.063 Uiso 1 1 calc R U . . .
H82B H 0.692012 0.207709 0.904300 0.063 Uiso 1 1 calc R U . . .
H82C H 0.759321 0.272943 0.917882 0.063 Uiso 1 1 calc R U . . .
C75 C 0.2456(4) 0.5162(4) 0.7870(2) 0.0335(12) Uani 1 1 d . . . . .
C76 C 0.1951(4) 0.4483(4) 0.8176(2) 0.0366(13) Uani 1 1 d . . . . .
H76B H 0.178391 0.464679 0.856019 0.055 Uiso 1 1 calc R U . . .
H76C H 0.244909 0.378927 0.812315 0.055 Uiso 1 1 calc R U . . .
H76A H 0.128080 0.455844 0.804850 0.055 Uiso 1 1 calc R U . . .
C85 C 0.1106(5) 0.7008(5) 0.8897(2) 0.0468(16) Uani 1 1 d . . . . .
C86 C 0.1808(5) 0.7595(5) 0.8855(3) 0.0476(15) Uani 1 1 d . . . . .
H86A H 0.200816 0.761109 0.920673 0.071 Uiso 1 1 calc R U . . .
H86B H 0.142681 0.828089 0.874087 0.071 Uiso 1 1 calc R U . . .
H86C H 0.246340 0.729074 0.858874 0.071 Uiso 1 1 calc R U . . .
V1 V 0.70327(6) 0.41882(6) 0.77859(3) 0.02040(18) Uani 1 1 d . . . . .
V2 V 0.71347(6) 0.64037(6) 0.70186(3) 0.02038(18) Uani 1 1 d . . . . .
N1 N 0.5060(4) 0.4939(4) 0.6584(2) 0.0486(13) Uani 1 1 d . . . . .
N2 N 0.9703(5) 0.3262(5) 0.6354(2) 0.0590(15) Uani 1 1 d . . . . .
N7 N 1.4035(8) 0.3336(11) 0.5516(5) 0.171(6) Uani 1 1 d . . . . .
N4 N 1.1549(4) 0.4133(4) 0.6793(2) 0.0498(14) Uani 1 1 d . . . . .
N5 N 0.7709(5) 1.0863(5) 0.6561(3) 0.0662(17) Uani 1 1 d . . . . .
N6 N 0.6750(4) 0.1952(4) 1.0270(2) 0.0521(14) Uani 1 1 d . . . . .
N3 N 0.2842(3) 0.5696(4) 0.7633(2) 0.0402(11) Uani 1 1 d . . . . .
N8 N 0.0556(5) 0.6538(5) 0.8936(2) 0.0642(17) Uani 1 1 d . . . . .
O11 O 0.7090(2) 0.5261(2) 0.73552(13) 0.0235(7) Uani 1 1 d . . . . .
O1 O 0.7016(2) 0.2995(2) 0.75718(13) 0.0232(7) Uani 1 1 d . . . . .
O2 O 0.8608(2) 0.3652(2) 0.76562(13) 0.0215(7) Uani 1 1 d . . . . .
O3 O 0.9602(2) 0.5095(2) 0.79039(13) 0.0221(7) Uani 1 1 d . . . . .
O4 O 0.8715(2) 0.5867(2) 0.69055(13) 0.0222(7) Uani 1 1 d . . . . .
O5 O 0.7257(2) 0.6627(2) 0.62850(13) 0.0221(7) Uani 1 1 d . . . . .
O6 O 0.5564(2) 0.6894(2) 0.70769(12) 0.0208(7) Uani 1 1 d . . . . .
O7 O 0.4397(2) 0.6880(2) 0.82003(13) 0.0230(7) Uani 1 1 d . . . . .
O8 O 0.5459(2) 0.4718(2) 0.78670(12) 0.0217(7) Uani 1 1 d . . . . .
O9 O 0.6970(2) 0.4226(2) 0.84185(13) 0.0253(7) Uani 1 1 d . . . . .
O10 O 0.7089(2) 0.7316(2) 0.73589(14) 0.0260(7) Uani 1 1 d . . . . .
Na1 Na 0.96905(14) 0.42831(14) 0.70765(8) 0.0266(4) Uani 1 1 d . . . . .
Na2 Na 0.45165(14) 0.59968(14) 0.73886(8) 0.0247(4) Uani 1 1 d . . . . .
N9 N 0.7877(10) 0.3395(9) 0.5018(5) 0.088(2) Uiso 0.674(7) 1 d D U P B 1
C87 C 0.7834(12) 0.4076(11) 0.5246(6) 0.088(2) Uiso 0.674(7) 1 d D U P B 1
C88 C 0.7705(12) 0.4882(10) 0.5588(5) 0.088(2) Uiso 0.674(7) 1 d D U P B 1
H88A H 0.704343 0.544311 0.554450 0.133 Uiso 0.674(7) 1 calc R U P B 1
H88B H 0.833033 0.510230 0.548822 0.133 Uiso 0.674(7) 1 calc R U P B 1
H88C H 0.765229 0.465365 0.596433 0.133 Uiso 0.674(7) 1 calc R U P B 1
N10 N 0.753(2) 0.3116(19) 0.4830(10) 0.088(2) Uiso 0.326(7) 1 d . U P B 2
C91 C 0.547(2) 0.416(2) 0.4709(12) 0.088(2) Uiso 0.326(7) 1 d . U P B 2
H91A H 0.526643 0.485012 0.482479 0.133 Uiso 0.326(7) 1 calc R U P B 2
H91B H 0.498333 0.384458 0.492959 0.133 Uiso 0.326(7) 1 calc R U P B 2
H91C H 0.540880 0.414991 0.432906 0.133 Uiso 0.326(7) 1 calc R U P B 2
C90 C 0.665(3) 0.356(2) 0.4780(12) 0.088(2) Uiso 0.326(7) 1 d . U P B 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 O1 1.360(5) . ?
C1 C6 1.403(6) . ?
C1 C2 1.403(6) . ?
C2 C3 1.392(7) . ?
C2 C68 1.519(6) . ?
C3 C4 1.406(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(7) . ?
C4 C7 1.530(7) . ?
C5 C6 1.395(7) . ?
C5 H5 0.9500 . ?
C6 C11 1.518(6) . ?
C7 C9B 1.44(2) . ?
C7 C8A 1.477(10) . ?
C7 C9A 1.528(10) . ?
C7 C10B 1.54(2) . ?
C7 C10A 1.565(10) . ?
C7 C8B 1.61(2) . ?
C8A H8A 0.9800 . ?
C8A H8B 0.9800 . ?
C8A H8C 0.9800 . ?
C9A H9A 0.9800 . ?
C9A H9B 0.9800 . ?
C9A H9C 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 C13 1.522(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.358(5) . ?
C12 C13 1.393(6) . ?
C12 C17 1.413(6) . ?
C12 Na1 2.985(5) . ?
C13 C14 1.398(6) . ?
C14 C15 1.372(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.405(7) . ?
C15 C18 1.542(7) . ?
C16 C17 1.390(6) . ?
C16 H16 0.9500 . ?
C17 C22 1.504(6) . ?
C18 C19 1.526(8) . ?
C18 C20 1.530(8) . ?
C18 C21 1.536(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O3 1.435(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 O3 1.445(5) . ?
C23 C25 1.500(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O4 1.359(5) . ?
C24 C25 1.395(6) . ?
C24 C29 1.408(6) . ?
C24 Na1 2.994(5) . ?
C25 C26 1.403(6) . ?
C26 C27 1.396(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(7) . ?
C27 C30 1.539(7) . ?
C28 C29 1.379(6) . ?
C28 H28 0.9500 . ?
C29 C34 1.514(6) . ?
C30 C31 1.534(7) . ?
C30 C33 1.536(7) . ?
C30 C32 1.539(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.519(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.359(5) . ?
C35 C36 1.394(6) . ?
C35 C40 1.412(6) . ?
C36 C37 1.397(7) . ?
C37 C38 1.396(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.399(6) . ?
C38 C41 1.532(7) . ?
C39 C40 1.390(7) . ?
C39 H39 0.9500 . ?
C40 C45 1.514(6) . ?
C41 C43 1.528(7) . ?
C41 C42 1.531(7) . ?
C41 C44 1.537(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C47 1.511(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O6 1.364(6) . ?
C46 C47 1.399(7) . ?
C46 C51 1.401(6) . ?
C46 Na2 2.972(5) . ?
C47 C48 1.397(7) . ?
C48 C49 1.387(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.397(7) . ?
C49 C52 1.534(7) . ?
C50 C51 1.401(6) . ?
C50 H50 0.9500 . ?
C51 C56 1.498(6) . ?
C52 C55 1.526(7) . ?
C52 C54 1.527(7) . ?
C52 C53 1.546(7) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 O7 1.449(5) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O7 1.443(5) . ?
C57 C59 1.505(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 O8 1.350(5) . ?
C58 C59 1.407(6) . ?
C58 C63 1.409(6) . ?
C58 Na2 3.020(5) . ?
C59 C60 1.397(6) . ?
C60 C61 1.393(7) . ?
C60 H60 0.9500 . ?
C61 C62 1.395(7) . ?
C61 C64 1.533(7) . ?
C62 C63 1.387(6) . ?
C62 H62 0.9500 . ?
C63 C68 1.517(6) . ?
C64 C65 1.515(8) . ?
C64 C67 1.522(8) . ?
C64 C66 1.531(8) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C71 N1 1.132(8) . ?
C71 C72 1.455(9) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 N2 1.137(8) . ?
C73 C74 1.445(9) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C83 N7 1.182(15) . ?
C83 C84 1.469(15) . ?
C84 H84C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C77 N4 1.134(8) . ?
C77 C78 1.448(9) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 N5 1.143(8) . ?
C79 C80 1.433(9) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 N6 1.138(7) . ?
C81 C82 1.448(8) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C75 N3 1.140(7) . ?
C75 C76 1.465(8) . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C76 H76A 0.9800 . ?
C85 N8 1.147(9) . ?
C85 C86 1.452(10) . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
V1 O9 1.588(3) . ?
V1 O11 1.825(3) . ?
V1 O1 1.832(3) . ?
V1 O2 1.946(3) . ?
V1 O8 1.949(3) . ?
V2 O10 1.589(3) . ?
V2 O11 1.796(3) . ?
V2 O5 1.842(3) . ?
V2 O6 1.951(3) . ?
V2 O4 1.953(3) . ?
N1 Na2 2.459(6) . ?
N2 Na1 2.413(6) . ?
N4 Na1 2.396(5) . ?
N3 Na2 2.393(5) . ?
O2 Na1 2.231(3) . ?
O3 Na1 2.427(4) . ?
O4 Na1 2.232(4) . ?
O6 Na2 2.221(3) . ?
O7 Na2 2.435(4) . ?
O8 Na2 2.238(3) . ?
N9 C87 1.144(12) . ?
C87 C88 1.430(13) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
N10 C90 1.16(3) . ?
C91 C90 1.55(4) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 119.8(4) . . ?
O1 C1 C2 119.8(4) . . ?
C6 C1 C2 120.4(4) . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 C68 120.7(4) . . ?
C1 C2 C68 120.5(4) . . ?
C2 C3 C4 122.8(4) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 116.2(4) . . ?
C5 C4 C7 122.9(4) . . ?
C3 C4 C7 120.8(4) . . ?
C4 C5 C6 123.3(4) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C5 C6 C1 118.5(4) . . ?
C5 C6 C11 121.8(4) . . ?
C1 C6 C11 119.7(4) . . ?
C8A C7 C9A 111.2(6) . . ?
C9B C7 C4 110.6(11) . . ?
C8A C7 C4 111.4(5) . . ?
C9A C7 C4 109.4(5) . . ?
C9B C7 C10B 114.1(14) . . ?
C4 C7 C10B 108.2(10) . . ?
C8A C7 C10A 107.7(6) . . ?
C9A C7 C10A 104.8(6) . . ?
C4 C7 C10A 112.1(5) . . ?
C9B C7 C8B 109.6(14) . . ?
C4 C7 C8B 112.7(10) . . ?
C10B C7 C8B 101.5(13) . . ?
C7 C8A H8A 109.5 . . ?
C7 C8A H8B 109.5 . . ?
H8A C8A H8B 109.5 . . ?
C7 C8A H8C 109.5 . . ?
H8A C8A H8C 109.5 . . ?
H8B C8A H8C 109.5 . . ?
C7 C9A H9A 109.5 . . ?
C7 C9A H9B 109.5 . . ?
H9A C9A H9B 109.5 . . ?
C7 C9A H9C 109.5 . . ?
H9A C9A H9C 109.5 . . ?
H9B C9A H9C 109.5 . . ?
C7 C10A H10A 109.5 . . ?
C7 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C7 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C7 C8B H8B1 109.5 . . ?
C7 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7 C9B H9B1 109.5 . . ?
C7 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7 C10B H10D 109.5 . . ?
C7 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C6 C11 C13 112.6(4) . . ?
C6 C11 H11A 109.1 . . ?
C13 C11 H11A 109.1 . . ?
C6 C11 H11B 109.1 . . ?
C13 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
O2 C12 C13 121.3(4) . . ?
O2 C12 C17 119.0(4) . . ?
C13 C12 C17 119.7(4) . . ?
O2 C12 Na1 44.55(19) . . ?
C13 C12 Na1 127.5(3) . . ?
C17 C12 Na1 95.2(3) . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 C11 120.4(4) . . ?
C14 C13 C11 120.3(4) . . ?
C15 C14 C13 122.8(5) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
C14 C15 C16 117.2(4) . . ?
C14 C15 C18 123.2(4) . . ?
C16 C15 C18 119.6(5) . . ?
C17 C16 C15 122.3(5) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C12 118.7(4) . . ?
C16 C17 C22 120.3(4) . . ?
C12 C17 C22 120.7(4) . . ?
C19 C18 C20 108.7(5) . . ?
C19 C18 C21 109.8(5) . . ?
C20 C18 C21 107.6(5) . . ?
C19 C18 C15 108.5(4) . . ?
C20 C18 C15 111.7(5) . . ?
C21 C18 C15 110.5(4) . . ?
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 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C22 C17 112.5(4) . . ?
O3 C22 H22A 109.1 . . ?
C17 C22 H22A 109.1 . . ?
O3 C22 H22B 109.1 . . ?
C17 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
O3 C23 C25 111.6(4) . . ?
O3 C23 H23A 109.3 . . ?
C25 C23 H23A 109.3 . . ?
O3 C23 H23B 109.3 . . ?
C25 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
O4 C24 C25 119.5(4) . . ?
O4 C24 C29 120.9(4) . . ?
C25 C24 C29 119.5(4) . . ?
O4 C24 Na1 44.23(19) . . ?
C25 C24 Na1 96.1(3) . . ?
C29 C24 Na1 126.7(3) . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 C23 120.8(4) . . ?
C26 C25 C23 119.5(4) . . ?
C27 C26 C25 121.9(4) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 C26 116.7(4) . . ?
C28 C27 C30 120.0(4) . . ?
C26 C27 C30 123.3(4) . . ?
C29 C28 C27 123.5(4) . . ?
C29 C28 H28 118.3 . . ?
C27 C28 H28 118.3 . . ?
C28 C29 C24 118.9(4) . . ?
C28 C29 C34 120.6(4) . . ?
C24 C29 C34 120.4(4) . . ?
C31 C30 C33 108.8(4) . . ?
C31 C30 C32 108.0(4) . . ?
C33 C30 C32 108.8(4) . . ?
C31 C30 C27 112.0(4) . . ?
C33 C30 C27 109.7(4) . . ?
C32 C30 C27 109.4(4) . . ?
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 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 C36 112.8(4) . . ?
C29 C34 H34A 109.0 . . ?
C36 C34 H34A 109.0 . . ?
C29 C34 H34B 109.0 . . ?
C36 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
O5 C35 C36 120.8(4) . . ?
O5 C35 C40 118.8(4) . . ?
C36 C35 C40 120.4(4) . . ?
C35 C36 C37 119.0(4) . . ?
C35 C36 C34 120.2(4) . . ?
C37 C36 C34 120.8(4) . . ?
C38 C37 C36 122.6(4) . . ?
C38 C37 H37 118.7 . . ?
C36 C37 H37 118.7 . . ?
C37 C38 C39 116.5(4) . . ?
C37 C38 C41 122.7(4) . . ?
C39 C38 C41 120.7(4) . . ?
C40 C39 C38 123.2(4) . . ?
C40 C39 H39 118.4 . . ?
C38 C39 H39 118.4 . . ?
C39 C40 C35 118.2(4) . . ?
C39 C40 C45 121.6(4) . . ?
C35 C40 C45 120.1(4) . . ?
C43 C41 C42 108.9(4) . . ?
C43 C41 C38 108.3(4) . . ?
C42 C41 C38 112.4(4) . . ?
C43 C41 C44 108.9(5) . . ?
C42 C41 C44 107.5(5) . . ?
C38 C41 C44 110.8(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 C45 C40 111.0(4) . . ?
C47 C45 H45A 109.4 . . ?
C40 C45 H45A 109.4 . . ?
C47 C45 H45B 109.4 . . ?
C40 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
O6 C46 C47 120.0(4) . . ?
O6 C46 C51 119.9(4) . . ?
C47 C46 C51 120.1(4) . . ?
O6 C46 Na2 44.70(19) . . ?
C47 C46 Na2 126.4(3) . . ?
C51 C46 Na2 96.1(3) . . ?
C48 C47 C46 118.5(4) . . ?
C48 C47 C45 120.1(4) . . ?
C46 C47 C45 121.3(4) . . ?
C49 C48 C47 123.1(4) . . ?
C49 C48 H48 118.4 . . ?
C47 C48 H48 118.4 . . ?
C48 C49 C50 117.1(4) . . ?
C48 C49 C52 119.4(4) . . ?
C50 C49 C52 123.5(4) . . ?
C49 C50 C51 121.9(4) . . ?
C49 C50 H50 119.0 . . ?
C51 C50 H50 119.0 . . ?
C50 C51 C46 119.2(4) . . ?
C50 C51 C56 119.3(4) . . ?
C46 C51 C56 121.2(4) . . ?
C55 C52 C54 108.1(4) . . ?
C55 C52 C49 112.4(4) . . ?
C54 C52 C49 110.1(4) . . ?
C55 C52 C53 107.7(4) . . ?
C54 C52 C53 109.9(4) . . ?
C49 C52 C53 108.6(4) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O7 C56 C51 112.8(4) . . ?
O7 C56 H56A 109.0 . . ?
C51 C56 H56A 109.0 . . ?
O7 C56 H56B 109.0 . . ?
C51 C56 H56B 109.0 . . ?
H56A C56 H56B 107.8 . . ?
O7 C57 C59 112.1(4) . . ?
O7 C57 H57A 109.2 . . ?
C59 C57 H57A 109.2 . . ?
O7 C57 H57B 109.2 . . ?
C59 C57 H57B 109.2 . . ?
H57A C57 H57B 107.9 . . ?
O8 C58 C59 119.2(4) . . ?
O8 C58 C63 121.3(4) . . ?
C59 C58 C63 119.5(4) . . ?
O8 C58 Na2 43.32(19) . . ?
C59 C58 Na2 95.6(3) . . ?
C63 C58 Na2 128.0(3) . . ?
C60 C59 C58 119.2(4) . . ?
C60 C59 C57 119.9(4) . . ?
C58 C59 C57 120.7(4) . . ?
C61 C60 C59 122.8(5) . . ?
C61 C60 H60 118.6 . . ?
C59 C60 H60 118.6 . . ?
C60 C61 C62 116.2(4) . . ?
C60 C61 C64 122.1(5) . . ?
C62 C61 C64 121.6(4) . . ?
C63 C62 C61 123.6(4) . . ?
C63 C62 H62 118.2 . . ?
C61 C62 H62 118.2 . . ?
C62 C63 C58 118.7(4) . . ?
C62 C63 C68 121.1(4) . . ?
C58 C63 C68 120.2(4) . . ?
C65 C64 C67 108.6(6) . . ?
C65 C64 C66 108.5(5) . . ?
C67 C64 C66 108.3(5) . . ?
C65 C64 C61 111.8(4) . . ?
C67 C64 C61 110.5(5) . . ?
C66 C64 C61 108.9(4) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C63 C68 C2 113.7(4) . . ?
C63 C68 H68A 108.8 . . ?
C2 C68 H68A 108.8 . . ?
C63 C68 H68B 108.8 . . ?
C2 C68 H68B 108.8 . . ?
H68A C68 H68B 107.7 . . ?
N1 C71 C72 178.9(7) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N2 C73 C74 179.1(8) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N7 C83 C84 177.6(12) . . ?
C83 C84 H84C 109.5 . . ?
C83 C84 H84A 109.5 . . ?
H84C C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84C C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
N4 C77 C78 178.8(7) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N5 C79 C80 179.3(9) . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N6 C81 C82 179.1(7) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
N3 C75 C76 179.5(6) . . ?
C75 C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C76 H76A 109.5 . . ?
H76B C76 H76A 109.5 . . ?
H76C C76 H76A 109.5 . . ?
N8 C85 C86 179.2(7) . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
O9 V1 O11 120.85(16) . . ?
O9 V1 O1 112.40(16) . . ?
O11 V1 O1 126.75(15) . . ?
O9 V1 O2 92.22(14) . . ?
O11 V1 O2 89.13(13) . . ?
O1 V1 O2 89.74(14) . . ?
O9 V1 O8 91.40(14) . . ?
O11 V1 O8 89.18(13) . . ?
O1 V1 O8 88.70(13) . . ?
O2 V1 O8 176.37(14) . . ?
O10 V2 O11 119.84(17) . . ?
O10 V2 O5 114.85(16) . . ?
O11 V2 O5 125.30(15) . . ?
O10 V2 O6 92.06(14) . . ?
O11 V2 O6 90.07(13) . . ?
O5 V2 O6 88.93(13) . . ?
O10 V2 O4 91.85(15) . . ?
O11 V2 O4 89.95(14) . . ?
O5 V2 O4 87.37(13) . . ?
O6 V2 O4 175.48(14) . . ?
C71 N1 Na2 136.0(5) . . ?
C73 N2 Na1 159.8(6) . . ?
C77 N4 Na1 134.1(5) . . ?
C75 N3 Na2 142.7(4) . . ?
V2 O11 V1 171.8(2) . . ?
C1 O1 V1 129.3(3) . . ?
C12 O2 V1 120.1(3) . . ?
C12 O2 Na1 110.2(2) . . ?
V1 O2 Na1 125.49(15) . . ?
C22 O3 C23 108.5(3) . . ?
C22 O3 Na1 117.2(3) . . ?
C23 O3 Na1 117.7(3) . . ?
C24 O4 V2 120.9(3) . . ?
C24 O4 Na1 110.6(2) . . ?
V2 O4 Na1 124.30(16) . . ?
C35 O5 V2 129.2(3) . . ?
C46 O6 V2 121.7(3) . . ?
C46 O6 Na2 109.7(2) . . ?
V2 O6 Na2 124.61(16) . . ?
C57 O7 C56 108.1(3) . . ?
C57 O7 Na2 116.1(3) . . ?
C56 O7 Na2 117.5(3) . . ?
C58 O8 V1 118.4(3) . . ?
C58 O8 Na2 112.2(3) . . ?
V1 O8 Na2 124.93(16) . . ?
O2 Na1 O4 107.28(13) . . ?
O2 Na1 N4 142.49(18) . . ?
O4 Na1 N4 106.13(17) . . ?
O2 Na1 N2 91.75(18) . . ?
O4 Na1 N2 107.74(19) . . ?
N4 Na1 N2 93.9(2) . . ?
O2 Na1 O3 79.34(12) . . ?
O4 Na1 O3 78.95(12) . . ?
N4 Na1 O3 90.84(16) . . ?
N2 Na1 O3 170.27(19) . . ?
O2 Na1 C12 25.28(11) . . ?
O4 Na1 C12 124.56(14) . . ?
N4 Na1 C12 117.78(18) . . ?
N2 Na1 C12 101.50(19) . . ?
O3 Na1 C12 68.77(12) . . ?
O2 Na1 C24 124.16(14) . . ?
O4 Na1 C24 25.14(11) . . ?
N4 Na1 C24 83.47(16) . . ?
N2 Na1 C24 120.98(19) . . ?
O3 Na1 C24 67.98(12) . . ?
C12 Na1 C24 131.61(14) . . ?
O6 Na2 O8 107.37(13) . . ?
O6 Na2 N3 155.48(16) . . ?
O8 Na2 N3 95.90(16) . . ?
O6 Na2 O7 79.09(12) . . ?
O8 Na2 O7 80.08(12) . . ?
N3 Na2 O7 97.91(16) . . ?
O6 Na2 N1 95.12(17) . . ?
O8 Na2 N1 91.16(17) . . ?
N3 Na2 N1 91.94(19) . . ?
O7 Na2 N1 167.40(16) . . ?
O6 Na2 C46 25.59(11) . . ?
O8 Na2 C46 125.37(13) . . ?
N3 Na2 C46 130.90(16) . . ?
O7 Na2 C46 68.63(12) . . ?
N1 Na2 C46 110.38(18) . . ?
O6 Na2 C58 122.99(13) . . ?
O8 Na2 C58 24.45(11) . . ?
N3 Na2 C58 76.80(15) . . ?
O7 Na2 C58 68.29(12) . . ?
N1 Na2 C58 106.73(17) . . ?
C46 Na2 C58 131.29(14) . . ?
N9 C87 C88 172.8(17) . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
N10 C90 C91 180(4) . . ?

_refine_diff_density_max         1.372
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.093

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1998555'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_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

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0966(2)
_cell_length_b                   12.3373(2)
_cell_length_c                   17.8971(3)
_cell_angle_alpha                90.8728(8)
_cell_angle_beta                 107.9966(7)
_cell_angle_gamma                99.2458(8)
_cell_volume                     2501.28(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7770
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.24

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_F_000             910
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.227
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6939
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_standards_decay_%        4
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29287
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.755
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             12217
_reflns_number_gt                8563
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1100P)²+0.3328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12217
_refine_ls_number_parameters     591
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1852
_refine_ls_wR_factor_gt          0.1637
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.037
_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_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 . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 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_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_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) . . . . ?

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

_refine_diff_density_max         0.868
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.057

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1998554'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_vrf_PLAT026_shelx               
;
RESPONSE: The crystals were too small for normal lab
sources and were examined using the rotating anode 
copper source at NCS southampton. This is the most
effective lab equipment in the world for recording
diffraction data. The 42 % observed data give a 
clear chemical structure. 
;

_vrf_PLAT201_shelx               
;
RESPONSE: Some portions of the structures are disordered over two 
positions. This small-scale
disorder was modelled using isotropic displacement parameters.     
;

_vrf_PLAT220_shelx               
;
RESPONSE:The carbon atoms at the centre of the complex have
relatively small displacement parameters. Those around the
outside such as the tBu groups have much larger displacement
parameters as would be expected chemically.      
;

_vrf_PLAT242_shelx               
;
RESPONSE:  This is the central atom of a t-Butyl group. The
group rocks about this atom. As expected chemically it has 
a smaller displacement parameter.  
;

_vrf_PLAT341_shelx               
;
RESPONSE: several portions of the structure were disordered. 
This disorder was modelled using standard techniques. The 
presence of different disorder components leads to a 
modest C-C bond precision. 
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C80 H90 Cl2 N2 O8 V2
;

_chemical_formula_sum            'C80 H90 Cl2 N2 O8 V2'
_chemical_formula_weight         1380.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   19.7039(9)
_cell_length_b                   20.0862(7)
_cell_length_c                   20.6921(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.114(5)
_cell_angle_gamma                90
_cell_volume                     7532.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6423
_cell_measurement_theta_min      2.603
_cell_measurement_theta_max      63.650

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_F_000             2912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    3.160
_shelx_estimated_absorpt_T_min   0.649
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7382
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  
;
Rigaku 007HF diffractometer equipped with Varimax confocal 
mirrors and an AFC11 goniometer and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            68213
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.625
_diffrn_reflns_theta_max         66.133
_diffrn_reflns_theta_full        66.133
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13175
_reflns_number_gt                5544
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0927P)²+7.4349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13175
_refine_ls_number_parameters     791
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.0850
_refine_ls_wR_factor_ref         0.2471
_refine_ls_wR_factor_gt          0.1975
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.5793(3) 0.7173(3) 0.7768(3) 0.0601(18) Uani 1 1 d . . . . .
C2 C 0.5845(3) 0.6620(3) 0.7383(3) 0.0563(17) Uani 1 1 d . . . . .
C3 C 0.6105(3) 0.6025(3) 0.7746(3) 0.0643(18) Uani 1 1 d . . . . .
H3 H 0.615047 0.564416 0.749305 0.077 Uiso 1 1 calc R U . . .
C4 C 0.6302(4) 0.5975(4) 0.8473(3) 0.071(2) Uani 1 1 d . . . . .
C5 C 0.6238(4) 0.6537(4) 0.8829(3) 0.074(2) Uani 1 1 d . . . . .
H5 H 0.636620 0.650687 0.932074 0.089 Uiso 1 1 calc R U . . .
C6 C 0.5994(3) 0.7142(3) 0.8499(3) 0.0667(19) Uani 1 1 d . . . . .
C7 C 0.6577(4) 0.5299(4) 0.8863(4) 0.086(2) Uani 1 1 d . . . . .
C8 C 0.6875(8) 0.4832(7) 0.8437(7) 0.108(2) Uiso 0.632(7) 1 d . U P A 1
H8A H 0.726877 0.505943 0.834507 0.162 Uiso 0.632(7) 1 calc R U P A 1
H8B H 0.707142 0.442508 0.870616 0.162 Uiso 0.632(7) 1 calc R U P A 1
H8C H 0.647371 0.471794 0.798946 0.162 Uiso 0.632(7) 1 calc R U P A 1
C9 C 0.7278(7) 0.5453(7) 0.9549(7) 0.108(2) Uiso 0.632(7) 1 d . U P A 1
H9A H 0.765983 0.565755 0.942077 0.162 Uiso 0.632(7) 1 calc R U P A 1
H9B H 0.714418 0.575908 0.984808 0.162 Uiso 0.632(7) 1 calc R U P A 1
H9C H 0.746794 0.503745 0.980464 0.162 Uiso 0.632(7) 1 calc R U P A 1
C10 C 0.5969(8) 0.4983(7) 0.9025(8) 0.108(2) Uiso 0.632(7) 1 d . U P A 1
H10A H 0.579967 0.529552 0.929345 0.162 Uiso 0.632(7) 1 calc R U P A 1
H10B H 0.555644 0.487011 0.858427 0.162 Uiso 0.632(7) 1 calc R U P A 1
H10C H 0.615415 0.457725 0.930097 0.162 Uiso 0.632(7) 1 calc R U P A 1
C8B C 0.7202(14) 0.5071(13) 0.8771(13) 0.108(2) Uiso 0.368(7) 1 d . U P A 2
H8B1 H 0.712815 0.511749 0.827658 0.162 Uiso 0.368(7) 1 calc R U P A 2
H8B2 H 0.763238 0.533301 0.906454 0.162 Uiso 0.368(7) 1 calc R U P A 2
H8B3 H 0.728516 0.460097 0.890786 0.162 Uiso 0.368(7) 1 calc R U P A 2
C9B C 0.6549(14) 0.5282(12) 0.9564(12) 0.108(2) Uiso 0.368(7) 1 d . U P A 2
H9B1 H 0.607440 0.545995 0.953441 0.162 Uiso 0.368(7) 1 calc R U P A 2
H9B2 H 0.660345 0.482203 0.973413 0.162 Uiso 0.368(7) 1 calc R U P A 2
H9B3 H 0.695067 0.555407 0.989081 0.162 Uiso 0.368(7) 1 calc R U P A 2
C10B C 0.5966(12) 0.4731(12) 0.8485(13) 0.108(2) Uiso 0.368(7) 1 d . U P A 2
H10D H 0.550019 0.484941 0.852312 0.162 Uiso 0.368(7) 1 calc R U P A 2
H10E H 0.588783 0.469922 0.798859 0.162 Uiso 0.368(7) 1 calc R U P A 2
H10F H 0.613950 0.430187 0.871575 0.162 Uiso 0.368(7) 1 calc R U P A 2
C11 C 0.5949(4) 0.7755(3) 0.8887(3) 0.077(2) Uani 1 1 d . . . . .
H11A H 0.618764 0.767339 0.939926 0.092 Uiso 1 1 calc R U . . .
H11B H 0.621601 0.812296 0.877024 0.092 Uiso 1 1 calc R U . . .
C12 C 0.5122(4) 0.8648(3) 0.8771(3) 0.077(2) Uani 1 1 d . . . . .
H12A H 0.542213 0.889320 0.856133 0.093 Uiso 1 1 calc R U . . .
H12B H 0.529479 0.877287 0.927311 0.093 Uiso 1 1 calc R U . . .
C13 C 0.4014(4) 0.8838(3) 0.7662(4) 0.0670(19) Uani 1 1 d . . . . .
C14 C 0.4325(4) 0.8820(3) 0.8396(4) 0.077(2) Uani 1 1 d . . . . .
C15 C 0.3885(5) 0.8961(4) 0.8758(4) 0.089(2) Uani 1 1 d . . . . .
H15 H 0.409983 0.894922 0.925724 0.107 Uiso 1 1 calc R U . . .
C16 C 0.3145(5) 0.9120(4) 0.8426(5) 0.095(3) Uani 1 1 d . . . . .
C17 C 0.2858(4) 0.9141(4) 0.7688(5) 0.091(2) Uani 1 1 d . . . . .
H17 H 0.235553 0.926131 0.744236 0.109 Uiso 1 1 calc R U . . .
C18 C 0.3277(4) 0.8992(3) 0.7303(4) 0.074(2) Uani 1 1 d . . . . .
C19 C 0.2633(6) 0.9244(6) 0.8812(5) 0.119(3) Uani 1 1 d . . . . .
C20 C 0.3037(6) 0.9147(7) 0.9597(6) 0.193(6) Uani 1 1 d . . . . .
H20A H 0.322211 0.868941 0.969237 0.290 Uiso 1 1 calc R U . . .
H20B H 0.345210 0.945865 0.977676 0.290 Uiso 1 1 calc R U . . .
H20C H 0.269782 0.923035 0.983042 0.290 Uiso 1 1 calc R U . . .
C21 C 0.2353(6) 0.9943(5) 0.8673(6) 0.155(4) Uani 1 1 d . . . . .
H21A H 0.209088 1.000966 0.816567 0.233 Uiso 1 1 calc R U . . .
H21B H 0.201508 1.002519 0.890774 0.233 Uiso 1 1 calc R U . . .
H21C H 0.276937 1.025349 0.885408 0.233 Uiso 1 1 calc R U . . .
C22 C 0.1987(6) 0.8758(5) 0.8563(6) 0.153(4) Uani 1 1 d . . . . .
H22A H 0.217382 0.830124 0.865566 0.229 Uiso 1 1 calc R U . . .
H22B H 0.166675 0.884497 0.881590 0.229 Uiso 1 1 calc R U . . .
H22C H 0.170414 0.881683 0.805765 0.229 Uiso 1 1 calc R U . . .
C23 C 0.2949(4) 0.8986(3) 0.6490(4) 0.077(2) Uani 1 1 d . . . . .
H23A H 0.257662 0.934481 0.631172 0.093 Uiso 1 1 calc R U . . .
H23B H 0.334505 0.907418 0.632054 0.093 Uiso 1 1 calc R U . . .
C24 C 0.2967(4) 0.7827(3) 0.6012(3) 0.0621(18) Uani 1 1 d . . . . .
C25 C 0.2597(4) 0.8333(4) 0.6212(3) 0.073(2) Uani 1 1 d . . . . .
C26 C 0.1901(4) 0.8202(4) 0.6179(4) 0.088(2) Uani 1 1 d . . . . .
H26 H 0.164572 0.854585 0.630534 0.105 Uiso 1 1 calc R U . . .
C27 C 0.1546(5) 0.7589(5) 0.5969(4) 0.087(2) Uani 1 1 d . . . . .
C28 C 0.1936(5) 0.7106(4) 0.5775(3) 0.080(2) Uani 1 1 d . . . . .
H28 H 0.171260 0.668265 0.563084 0.096 Uiso 1 1 calc R U . . .
C29 C 0.2638(4) 0.7211(4) 0.5781(3) 0.070(2) Uani 1 1 d . . . . .
C30 C 0.0754(5) 0.7491(6) 0.5933(4) 0.111(3) Uani 1 1 d . . . . .
C31 C 0.0672(5) 0.7836(5) 0.6576(5) 0.117(3) Uani 1 1 d . . . . .
H31A H 0.018630 0.773150 0.657709 0.176 Uiso 1 1 calc R U . . .
H31B H 0.071891 0.831947 0.654208 0.176 Uiso 1 1 calc R U . . .
H31C H 0.105821 0.767465 0.701250 0.176 Uiso 1 1 calc R U . . .
C32 C 0.0209(5) 0.7851(6) 0.5249(5) 0.146(4) Uani 1 1 d . . . . .
H32A H 0.022557 0.763016 0.483372 0.219 Uiso 1 1 calc R U . . .
H32B H 0.035557 0.831801 0.525561 0.219 Uiso 1 1 calc R U . . .
H32C H -0.029452 0.782925 0.523372 0.219 Uiso 1 1 calc R U . . .
C33 C 0.0553(5) 0.6758(6) 0.5912(5) 0.149(4) Uani 1 1 d . . . . .
H33A H 0.051471 0.656528 0.546396 0.223 Uiso 1 1 calc R U . . .
H33B H 0.007914 0.671379 0.595828 0.223 Uiso 1 1 calc R U . . .
H33C H 0.093642 0.652387 0.629993 0.223 Uiso 1 1 calc R U . . .
C34 C 0.2998(4) 0.6667(3) 0.5534(3) 0.071(2) Uani 1 1 d . . . . .
H34A H 0.290479 0.623820 0.571969 0.085 Uiso 1 1 calc R U . . .
H34B H 0.353778 0.674297 0.573655 0.085 Uiso 1 1 calc R U . . .
C35 C 0.2780(3) 0.7172(3) 0.4344(3) 0.0606(18) Uani 1 1 d . . . . .
C36 C 0.2735(3) 0.6609(3) 0.4728(3) 0.070(2) Uani 1 1 d . . . . .
C37 C 0.2486(3) 0.6026(3) 0.4362(3) 0.074(2) Uani 1 1 d . . . . .
H37 H 0.246401 0.563948 0.461691 0.089 Uiso 1 1 calc R U . . .
C38 C 0.2261(4) 0.5974(3) 0.3629(3) 0.073(2) Uani 1 1 d . . . . .
C39 C 0.2315(3) 0.6553(3) 0.3269(3) 0.0679(19) Uani 1 1 d . . . . .
H39 H 0.216969 0.653667 0.277416 0.081 Uiso 1 1 calc R U . . .
C40 C 0.2576(3) 0.7149(3) 0.3620(3) 0.0666(19) Uani 1 1 d . . . . .
C41 C 0.2003(4) 0.5321(3) 0.3241(3) 0.076(2) Uani 1 1 d . . . . .
C42 C 0.1507(4) 0.4936(4) 0.3510(4) 0.098(3) Uani 1 1 d . . . . .
H42A H 0.178436 0.481319 0.400215 0.148 Uiso 1 1 calc R U . . .
H42B H 0.133078 0.453164 0.322790 0.148 Uiso 1 1 calc R U . . .
H42C H 0.108423 0.521315 0.347318 0.148 Uiso 1 1 calc R U . . .
C43 C 0.1581(5) 0.5427(3) 0.2446(3) 0.110(3) Uani 1 1 d . . . . .
H43A H 0.141374 0.499652 0.221648 0.165 Uiso 1 1 calc R U . . .
H43B H 0.190822 0.563832 0.225145 0.165 Uiso 1 1 calc R U . . .
H43C H 0.115384 0.571483 0.236458 0.165 Uiso 1 1 calc R U . . .
C44 C 0.2699(4) 0.4905(3) 0.3351(4) 0.094(2) Uani 1 1 d . . . . .
H44A H 0.292805 0.476187 0.384268 0.141 Uiso 1 1 calc R U . . .
H44B H 0.304948 0.517640 0.323621 0.141 Uiso 1 1 calc R U . . .
H44C H 0.256029 0.451315 0.304481 0.141 Uiso 1 1 calc R U . . .
C45 C 0.2618(3) 0.7774(3) 0.3240(3) 0.0642(19) Uani 1 1 d . . . . .
H45A H 0.237544 0.770483 0.272596 0.077 Uiso 1 1 calc R U . . .
H45B H 0.236160 0.814191 0.337052 0.077 Uiso 1 1 calc R U . . .
C46 C 0.3486(3) 0.8629(3) 0.3355(3) 0.071(2) Uani 1 1 d . . . . .
H46A H 0.318214 0.889100 0.354691 0.085 Uiso 1 1 calc R U . . .
H46B H 0.332769 0.873891 0.285034 0.085 Uiso 1 1 calc R U . . .
C47 C 0.4566(4) 0.8850(3) 0.4486(3) 0.0645(19) Uani 1 1 d . . . . .
C48 C 0.4288(4) 0.8797(3) 0.3742(3) 0.068(2) Uani 1 1 d . . . . .
C49 C 0.4755(4) 0.8875(3) 0.3400(4) 0.078(2) Uani 1 1 d . . . . .
H49 H 0.456284 0.883327 0.290259 0.094 Uiso 1 1 calc R U . . .
C50 C 0.5510(4) 0.9017(3) 0.3763(4) 0.075(2) Uani 1 1 d . . . . .
C51 C 0.5749(4) 0.9111(3) 0.4479(4) 0.070(2) Uani 1 1 d . . . . .
H51 H 0.624583 0.924556 0.472906 0.084 Uiso 1 1 calc R U . . .
C52 C 0.5308(4) 0.9023(3) 0.4855(3) 0.0630(19) Uani 1 1 d . . . . .
C53 C 0.6026(4) 0.9041(5) 0.3362(4) 0.092(2) Uani 1 1 d . . . . .
C54 C 0.5701(4) 0.9489(4) 0.2713(4) 0.106(3) Uani 1 1 d . . . . .
H54A H 0.564578 0.994273 0.285957 0.159 Uiso 1 1 calc R U . . .
H54B H 0.521746 0.931729 0.240141 0.159 Uiso 1 1 calc R U . . .
H54C H 0.603240 0.949375 0.246229 0.159 Uiso 1 1 calc R U . . .
C55 C 0.6807(4) 0.9264(4) 0.3816(4) 0.118(3) Uani 1 1 d . . . . .
H55A H 0.678876 0.969236 0.403655 0.176 Uiso 1 1 calc R U . . .
H55B H 0.709191 0.931376 0.352330 0.176 Uiso 1 1 calc R U . . .
H55C H 0.704258 0.893102 0.418180 0.176 Uiso 1 1 calc R U . . .
C56 C 0.6069(5) 0.8324(5) 0.3101(5) 0.131(3) Uani 1 1 d . . . . .
H56A H 0.634844 0.832850 0.279948 0.196 Uiso 1 1 calc R U . . .
H56B H 0.556933 0.815746 0.283228 0.196 Uiso 1 1 calc R U . . .
H56C H 0.631686 0.803256 0.350522 0.196 Uiso 1 1 calc R U . . .
C57 C 0.5620(3) 0.9036(3) 0.5656(3) 0.068(2) Uani 1 1 d . . . . .
H57A H 0.599250 0.939415 0.583144 0.081 Uiso 1 1 calc R U . . .
H57B H 0.521851 0.913135 0.581725 0.081 Uiso 1 1 calc R U . . .
C58 C 0.5601(3) 0.7859(3) 0.6134(3) 0.0527(16) Uani 1 1 d . . . . .
C59 C 0.5971(4) 0.8374(3) 0.5949(3) 0.0599(18) Uani 1 1 d . . . . .
C60 C 0.6671(4) 0.8250(3) 0.5976(3) 0.069(2) Uani 1 1 d . . . . .
H60 H 0.692476 0.860178 0.585959 0.083 Uiso 1 1 calc R U . . .
C61 C 0.7028(4) 0.7634(4) 0.6167(3) 0.0691(19) Uani 1 1 d . . . . .
C62 C 0.6631(4) 0.7137(3) 0.6333(3) 0.0637(19) Uani 1 1 d . . . . .
H62 H 0.684184 0.670483 0.644402 0.076 Uiso 1 1 calc R U . . .
C63 C 0.5940(3) 0.7246(3) 0.6343(3) 0.0562(17) Uani 1 1 d . . . . .
C64 C 0.7812(4) 0.7550(4) 0.6199(4) 0.086(2) Uani 1 1 d . . . . .
C65 C 0.7874(4) 0.7826(4) 0.5541(4) 0.104(3) Uani 1 1 d . . . . .
H65A H 0.838111 0.777269 0.557594 0.156 Uiso 1 1 calc R U . . .
H65B H 0.774269 0.829894 0.549402 0.156 Uiso 1 1 calc R U . . .
H65C H 0.753652 0.758316 0.512924 0.156 Uiso 1 1 calc R U . . .
C66 C 0.8377(4) 0.7911(4) 0.6843(4) 0.103(3) Uani 1 1 d . . . . .
H66A H 0.887481 0.784121 0.685677 0.154 Uiso 1 1 calc R U . . .
H66B H 0.834909 0.773204 0.727257 0.154 Uiso 1 1 calc R U . . .
H66C H 0.826624 0.838811 0.680883 0.154 Uiso 1 1 calc R U . . .
C67 C 0.8055(4) 0.6820(4) 0.6276(5) 0.114(3) Uani 1 1 d . . . . .
H67A H 0.773966 0.657048 0.585933 0.171 Uiso 1 1 calc R U . . .
H67B H 0.801085 0.662969 0.669449 0.171 Uiso 1 1 calc R U . . .
H67C H 0.856909 0.679205 0.632499 0.171 Uiso 1 1 calc R U . . .
C68 C 0.5575(3) 0.6676(3) 0.6584(3) 0.0612(18) Uani 1 1 d . . . . .
H68A H 0.503430 0.674406 0.638265 0.073 Uiso 1 1 calc R U . . .
H68B H 0.567674 0.625098 0.639576 0.073 Uiso 1 1 calc R U . . .
N1 N 0.4225(3) 0.7346(2) 0.7283(2) 0.0638(15) Uani 1 1 d . . . . .
C70 C 0.4069(4) 0.6810(3) 0.7614(4) 0.0552(9) Uiso 0.663(11) 1 d G U P B 1
C71 C 0.4202(4) 0.6160(4) 0.7466(4) 0.0718(12) Uiso 0.663(11) 1 d G U P B 1
H71 H 0.436379 0.607366 0.709772 0.086 Uiso 0.663(11) 1 calc R U P B 1
C72 C 0.4098(4) 0.5635(3) 0.7856(5) 0.0745(12) Uiso 0.663(11) 1 d G U P B 1
H72 H 0.418854 0.519088 0.775398 0.089 Uiso 0.663(11) 1 calc R U P B 1
C73 C 0.3861(5) 0.5761(4) 0.8394(4) 0.0773(13) Uiso 0.663(11) 1 d G U P B 1
C74 C 0.3728(5) 0.6411(5) 0.8543(3) 0.0745(12) Uiso 0.663(11) 1 d G U P B 1
H74 H 0.356561 0.649723 0.891067 0.089 Uiso 0.663(11) 1 calc R U P B 1
C75 C 0.3832(5) 0.6936(3) 0.8153(4) 0.0718(12) Uiso 0.663(11) 1 d G U P B 1
H75 H 0.374085 0.738002 0.825441 0.086 Uiso 0.663(11) 1 calc R U P B 1
Cl1A Cl 0.3784(5) 0.5130(4) 0.8924(5) 0.124(2) Uani 0.663(11) 1 d . U P B 1
Cl1B Cl 0.3656(12) 0.5444(11) 0.9161(11) 0.171(8) Uani 0.337(11) 1 d . U P B 2
C70B C 0.3967(9) 0.6916(7) 0.7647(7) 0.0552(9) Uiso 0.337(11) 1 d G U P B 2
C71B C 0.4244(8) 0.6272(7) 0.7717(8) 0.0718(12) Uiso 0.337(11) 1 d G U P B 2
H71B H 0.451604 0.613372 0.744946 0.086 Uiso 0.337(11) 1 calc R U P B 2
C72B C 0.4123(8) 0.5830(7) 0.8177(10) 0.0745(12) Uiso 0.337(11) 1 d G U P B 2
H72B H 0.431265 0.538956 0.822507 0.089 Uiso 0.337(11) 1 calc R U P B 2
C73B C 0.3725(9) 0.6032(8) 0.8568(8) 0.0773(13) Uiso 0.337(11) 1 d G U P B 2
C74B C 0.3448(9) 0.6676(8) 0.8498(7) 0.0745(12) Uiso 0.337(11) 1 d G U P B 2
H74B H 0.317582 0.681467 0.876527 0.089 Uiso 0.337(11) 1 calc R U P B 2
C75B C 0.3569(9) 0.7118(6) 0.8037(8) 0.0718(12) Uiso 0.337(11) 1 d G U P B 2
H75B H 0.337921 0.755884 0.798966 0.086 Uiso 0.337(11) 1 calc R U P B 2
N2 N 0.4362(2) 0.7369(2) 0.4874(2) 0.0607(14) Uani 1 1 d . . . . .
C76A C 0.4606(4) 0.6880(3) 0.4531(3) 0.0657(9) Uiso 0.778(5) 1 d G U P C 1
C77A C 0.4481(4) 0.6218(4) 0.4647(4) 0.0854(12) Uiso 0.778(5) 1 d G U P C 1
H77A H 0.426404 0.610972 0.497060 0.102 Uiso 0.778(5) 1 calc R U P C 1
C78A C 0.4674(4) 0.5715(3) 0.4290(4) 0.0887(13) Uiso 0.778(5) 1 d G U P C 1
H78A H 0.458832 0.526282 0.436908 0.106 Uiso 0.778(5) 1 calc R U P C 1
C79A C 0.4991(4) 0.5874(3) 0.3817(4) 0.0920(13) Uiso 0.778(5) 1 d G U P C 1
C80A C 0.5116(3) 0.6536(3) 0.3701(3) 0.0887(13) Uiso 0.778(5) 1 d G U P C 1
H80A H 0.533274 0.664471 0.337768 0.106 Uiso 0.778(5) 1 calc R U P C 1
C81A C 0.4923(3) 0.7039(3) 0.4058(3) 0.0854(12) Uiso 0.778(5) 1 d G U P C 1
H81A H 0.500848 0.749162 0.397920 0.102 Uiso 0.778(5) 1 calc R U P C 1
Cl2A Cl 0.5220(2) 0.5241(2) 0.3391(3) 0.1520(18) Uani 0.778(5) 1 d . U P C 1
O1 O 0.5543(2) 0.77605(18) 0.74249(19) 0.0616(12) Uani 1 1 d . . . . .
O2 O 0.5199(2) 0.7941(2) 0.8704(2) 0.0670(12) Uani 1 1 d . . . . .
O3 O 0.4435(2) 0.8697(2) 0.7293(2) 0.0678(13) Uani 1 1 d . . . . .
O4 O 0.3666(2) 0.79592(19) 0.60206(19) 0.0626(12) Uani 1 1 d . . . . .
O5 O 0.3018(2) 0.77622(19) 0.46901(18) 0.0610(12) Uani 1 1 d . . . . .
O6 O 0.3390(2) 0.7940(2) 0.34360(19) 0.0657(12) Uani 1 1 d . . . . .
O7 O 0.4125(2) 0.87233(19) 0.4835(2) 0.0657(13) Uani 1 1 d . . . . .
O8 O 0.4900(2) 0.79807(18) 0.61129(18) 0.0569(11) Uani 1 1 d . . . . .
V1 V 0.45652(6) 0.79300(5) 0.69243(5) 0.0612(4) Uani 1 1 d . . . . .
V2 V 0.39966(6) 0.79471(5) 0.52013(5) 0.0613(4) Uani 1 1 d . . . . .
Cl2B Cl 0.5733(9) 0.5077(6) 0.4098(11) 0.155(7) Uani 0.222(5) 1 d . U P C 2
C76B C 0.4616(12) 0.6813(11) 0.4711(12) 0.0657(9) Uiso 0.222(5) 1 d G U P C 2
C77B C 0.4300(11) 0.6184(13) 0.4639(14) 0.0854(12) Uiso 0.222(5) 1 d G U P C 2
H77B H 0.385748 0.612418 0.471288 0.102 Uiso 0.222(5) 1 calc R U P C 2
C78B C 0.4631(13) 0.5644(10) 0.4460(13) 0.0887(13) Uiso 0.222(5) 1 d G U P C 2
H78B H 0.441470 0.521450 0.441038 0.106 Uiso 0.222(5) 1 calc R U P C 2
C79B C 0.5278(13) 0.5732(10) 0.4352(12) 0.0920(13) Uiso 0.222(5) 1 d G U P C 2
C81B C 0.5595(10) 0.6361(12) 0.4424(12) 0.0887(13) Uiso 0.222(5) 1 d G U P C 2
H81B H 0.603749 0.642107 0.435004 0.106 Uiso 0.222(5) 1 calc R U P C 2
C80B C 0.5264(12) 0.6901(9) 0.4603(12) 0.0854(12) Uiso 0.222(5) 1 d G U P C 2
H80B H 0.548027 0.733076 0.465255 0.102 Uiso 0.222(5) 1 calc R U P C 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 O1 1.366(6) . ?
C1 C2 1.393(8) . ?
C1 C6 1.407(8) . ?
C2 C3 1.398(7) . ?
C2 C68 1.531(7) . ?
C3 C4 1.402(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(9) . ?
C4 C7 1.563(9) . ?
C5 C6 1.384(8) . ?
C5 H5 0.9500 . ?
C6 C11 1.491(9) . ?
C7 C8B 1.40(2) . ?
C7 C9B 1.47(2) . ?
C7 C10 1.506(14) . ?
C7 C8 1.552(15) . ?
C7 C9 1.574(14) . ?
C7 C10B 1.62(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 O2 1.423(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.442(7) . ?
C12 C14 1.493(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O3 1.359(8) . ?
C13 C18 1.381(9) . ?
C13 C14 1.398(9) . ?
C14 C15 1.380(10) . ?
C15 C16 1.384(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.405(10) . ?
C16 C19 1.532(12) . ?
C17 C18 1.386(10) . ?
C17 H17 0.9500 . ?
C18 C23 1.547(9) . ?
C19 C21 1.495(12) . ?
C19 C20 1.515(12) . ?
C19 C22 1.524(12) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.489(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C29 1.391(9) . ?
C24 O4 1.396(7) . ?
C24 C25 1.405(9) . ?
C25 C26 1.372(9) . ?
C26 C27 1.398(11) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(10) . ?
C27 C30 1.544(11) . ?
C28 C29 1.395(9) . ?
C28 H28 0.9500 . ?
C29 C34 1.497(9) . ?
C30 C33 1.519(13) . ?
C30 C31 1.565(11) . ?
C30 C32 1.578(12) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.545(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.369(6) . ?
C35 C40 1.391(8) . ?
C35 C36 1.405(8) . ?
C36 C37 1.375(8) . ?
C37 C38 1.407(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.407(8) . ?
C38 C41 1.519(8) . ?
C39 C40 1.389(8) . ?
C39 H39 0.9500 . ?
C40 C45 1.501(8) . ?
C41 C42 1.513(10) . ?
C41 C43 1.539(8) . ?
C41 C44 1.543(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O6 1.451(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O6 1.415(6) . ?
C46 C48 1.503(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O7 1.356(7) . ?
C47 C52 1.401(8) . ?
C47 C48 1.421(9) . ?
C48 C49 1.373(9) . ?
C49 C50 1.407(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.380(9) . ?
C50 C53 1.546(10) . ?
C51 C52 1.387(9) . ?
C51 H51 0.9500 . ?
C52 C57 1.524(8) . ?
C53 C55 1.522(10) . ?
C53 C54 1.532(10) . ?
C53 C56 1.553(11) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C59 1.511(8) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C63 1.386(8) . ?
C58 O8 1.387(7) . ?
C58 C59 1.402(8) . ?
C59 C60 1.381(9) . ?
C60 C61 1.401(9) . ?
C60 H60 0.9500 . ?
C61 C62 1.392(9) . ?
C61 C64 1.529(10) . ?
C62 C63 1.388(8) . ?
C62 H62 0.9500 . ?
C63 C68 1.535(8) . ?
C64 C65 1.518(10) . ?
C64 C67 1.531(10) . ?
C64 C66 1.541(10) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
N1 C70B 1.367(12) . ?
N1 C70 1.374(7) . ?
N1 V1 1.665(5) . ?
C70 C71 1.3900 . ?
C70 C75 1.3900 . ?
C71 C72 1.3900 . ?
C71 H71 0.9500 . ?
C72 C73 1.3900 . ?
C72 H72 0.9500 . ?
C73 C74 1.3900 . ?
C73 Cl1A 1.722(11) . ?
C74 C75 1.3900 . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
Cl1B C73B 1.75(2) . ?
C70B C71B 1.3900 . ?
C70B C75B 1.3900 . ?
C71B C72B 1.3900 . ?
C71B H71B 0.9500 . ?
C72B C73B 1.3900 . ?
C72B H72B 0.9500 . ?
C73B C74B 1.3900 . ?
C74B C75B 1.3900 . ?
C74B H74B 0.9500 . ?
C75B H75B 0.9500 . ?
N2 C76B 1.321(18) . ?
N2 C76A 1.401(7) . ?
N2 V2 1.646(5) . ?
C76A C77A 1.3900 . ?
C76A C81A 1.3900 . ?
C77A C78A 1.3900 . ?
C77A H77A 0.9500 . ?
C78A C79A 1.3900 . ?
C78A H78A 0.9500 . ?
C79A C80A 1.3900 . ?
C79A Cl2A 1.706(6) . ?
C80A C81A 1.3900 . ?
C80A H80A 0.9500 . ?
C81A H81A 0.9500 . ?
O1 V1 1.826(4) . ?
O3 V1 1.782(4) . ?
O4 V1 2.010(4) . ?
O4 V2 2.041(5) . ?
O5 V2 1.836(4) . ?
O7 V2 1.794(4) . ?
O8 V2 2.023(3) . ?
O8 V1 2.033(4) . ?
Cl2B C79B 1.78(2) . ?
C76B C77B 1.3900 . ?
C76B C80B 1.3900 . ?
C77B C78B 1.3900 . ?
C77B H77B 0.9500 . ?
C78B C79B 1.3900 . ?
C78B H78B 0.9500 . ?
C79B C81B 1.3900 . ?
C81B C80B 1.3900 . ?
C81B H81B 0.9500 . ?
C80B H80B 0.9500 . ?

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
O1 C1 C2 118.9(5) . . ?
O1 C1 C6 119.3(6) . . ?
C2 C1 C6 121.8(6) . . ?
C1 C2 C3 118.0(6) . . ?
C1 C2 C68 119.2(5) . . ?
C3 C2 C68 122.7(6) . . ?
C2 C3 C4 121.7(6) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 118.0(6) . . ?
C5 C4 C7 121.3(6) . . ?
C3 C4 C7 120.7(7) . . ?
C4 C5 C6 122.9(6) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 117.7(6) . . ?
C5 C6 C11 122.9(6) . . ?
C1 C6 C11 119.4(6) . . ?
C8B C7 C9B 120.2(14) . . ?
C10 C7 C8 112.5(9) . . ?
C8B C7 C4 111.2(12) . . ?
C9B C7 C4 112.9(11) . . ?
C10 C7 C4 109.6(7) . . ?
C8 C7 C4 111.2(8) . . ?
C10 C7 C9 112.1(9) . . ?
C8 C7 C9 103.7(9) . . ?
C4 C7 C9 107.4(7) . . ?
C8B C7 C10B 103.4(15) . . ?
C9B C7 C10B 98.7(13) . . ?
C4 C7 C10B 108.7(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8B H8B1 109.5 . . ?
C7 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7 C9B H9B1 109.5 . . ?
C7 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7 C10B H10D 109.5 . . ?
C7 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
O2 C11 C6 110.4(5) . . ?
O2 C11 H11A 109.6 . . ?
C6 C11 H11A 109.6 . . ?
O2 C11 H11B 109.6 . . ?
C6 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O2 C12 C14 107.8(5) . . ?
O2 C12 H12A 110.1 . . ?
C14 C12 H12A 110.1 . . ?
O2 C12 H12B 110.1 . . ?
C14 C12 H12B 110.1 . . ?
H12A C12 H12B 108.5 . . ?
O3 C13 C18 119.3(7) . . ?
O3 C13 C14 120.1(7) . . ?
C18 C13 C14 120.6(8) . . ?
C15 C14 C13 118.9(7) . . ?
C15 C14 C12 121.5(7) . . ?
C13 C14 C12 119.6(8) . . ?
C14 C15 C16 122.9(8) . . ?
C14 C15 H15 118.6 . . ?
C16 C15 H15 118.6 . . ?
C15 C16 C17 116.2(9) . . ?
C15 C16 C19 124.0(8) . . ?
C17 C16 C19 119.7(8) . . ?
C18 C17 C16 122.8(8) . . ?
C18 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
C13 C18 C17 118.5(7) . . ?
C13 C18 C23 119.0(7) . . ?
C17 C18 C23 122.5(7) . . ?
C21 C19 C20 109.0(9) . . ?
C21 C19 C22 109.9(9) . . ?
C20 C19 C22 107.3(10) . . ?
C21 C19 C16 108.7(9) . . ?
C20 C19 C16 111.2(8) . . ?
C22 C19 C16 110.7(8) . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C18 111.1(6) . . ?
C25 C23 H23A 109.4 . . ?
C18 C23 H23A 109.4 . . ?
C25 C23 H23B 109.4 . . ?
C18 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C29 C24 O4 119.8(7) . . ?
C29 C24 C25 121.3(7) . . ?
O4 C24 C25 118.8(6) . . ?
C26 C25 C24 118.0(7) . . ?
C26 C25 C23 119.6(8) . . ?
C24 C25 C23 122.3(7) . . ?
C25 C26 C27 123.6(8) . . ?
C25 C26 H26 118.2 . . ?
C27 C26 H26 118.2 . . ?
C28 C27 C26 115.9(8) . . ?
C28 C27 C30 124.0(9) . . ?
C26 C27 C30 120.0(9) . . ?
C27 C28 C29 123.4(8) . . ?
C27 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C24 C29 C28 117.7(8) . . ?
C24 C29 C34 123.2(7) . . ?
C28 C29 C34 119.2(7) . . ?
C33 C30 C27 111.8(9) . . ?
C33 C30 C31 110.0(8) . . ?
C27 C30 C31 110.1(7) . . ?
C33 C30 C32 109.9(8) . . ?
C27 C30 C32 107.7(7) . . ?
C31 C30 C32 107.3(8) . . ?
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 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 C36 114.9(5) . . ?
C29 C34 H34A 108.5 . . ?
C36 C34 H34A 108.5 . . ?
C29 C34 H34B 108.5 . . ?
C36 C34 H34B 108.5 . . ?
H34A C34 H34B 107.5 . . ?
O5 C35 C40 119.2(5) . . ?
O5 C35 C36 119.1(5) . . ?
C40 C35 C36 121.7(6) . . ?
C37 C36 C35 117.5(6) . . ?
C37 C36 C34 123.7(6) . . ?
C35 C36 C34 118.7(6) . . ?
C36 C37 C38 123.4(6) . . ?
C36 C37 H37 118.3 . . ?
C38 C37 H37 118.3 . . ?
C39 C38 C37 116.8(6) . . ?
C39 C38 C41 121.0(6) . . ?
C37 C38 C41 122.2(6) . . ?
C40 C39 C38 121.7(6) . . ?
C40 C39 H39 119.2 . . ?
C38 C39 H39 119.2 . . ?
C39 C40 C35 118.9(6) . . ?
C39 C40 C45 122.1(6) . . ?
C35 C40 C45 119.0(5) . . ?
C42 C41 C38 112.2(6) . . ?
C42 C41 C43 107.9(6) . . ?
C38 C41 C43 111.9(6) . . ?
C42 C41 C44 109.5(6) . . ?
C38 C41 C44 107.2(6) . . ?
C43 C41 C44 108.0(7) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O6 C45 C40 108.2(5) . . ?
O6 C45 H45A 110.1 . . ?
C40 C45 H45A 110.1 . . ?
O6 C45 H45B 110.1 . . ?
C40 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
O6 C46 C48 108.5(5) . . ?
O6 C46 H46A 110.0 . . ?
C48 C46 H46A 110.0 . . ?
O6 C46 H46B 110.0 . . ?
C48 C46 H46B 110.0 . . ?
H46A C46 H46B 108.4 . . ?
O7 C47 C52 120.4(6) . . ?
O7 C47 C48 120.5(6) . . ?
C52 C47 C48 119.1(7) . . ?
C49 C48 C47 119.9(7) . . ?
C49 C48 C46 121.9(6) . . ?
C47 C48 C46 118.2(7) . . ?
C48 C49 C50 122.0(7) . . ?
C48 C49 H49 119.0 . . ?
C50 C49 H49 119.0 . . ?
C51 C50 C49 116.4(8) . . ?
C51 C50 C53 123.6(7) . . ?
C49 C50 C53 120.0(7) . . ?
C50 C51 C52 124.1(7) . . ?
C50 C51 H51 118.0 . . ?
C52 C51 H51 118.0 . . ?
C51 C52 C47 118.3(7) . . ?
C51 C52 C57 122.3(6) . . ?
C47 C52 C57 119.1(7) . . ?
C55 C53 C54 110.0(7) . . ?
C55 C53 C50 113.3(7) . . ?
C54 C53 C50 110.7(7) . . ?
C55 C53 C56 108.0(8) . . ?
C54 C53 C56 107.5(7) . . ?
C50 C53 C56 107.1(7) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C59 C57 C52 110.3(5) . . ?
C59 C57 H57A 109.6 . . ?
C52 C57 H57A 109.6 . . ?
C59 C57 H57B 109.6 . . ?
C52 C57 H57B 109.6 . . ?
H57A C57 H57B 108.1 . . ?
C63 C58 O8 121.2(6) . . ?
C63 C58 C59 120.2(6) . . ?
O8 C58 C59 118.7(5) . . ?
C60 C59 C58 118.2(6) . . ?
C60 C59 C57 117.9(6) . . ?
C58 C59 C57 123.6(6) . . ?
C59 C60 C61 123.6(7) . . ?
C59 C60 H60 118.2 . . ?
C61 C60 H60 118.2 . . ?
C62 C61 C60 115.8(7) . . ?
C62 C61 C64 124.4(6) . . ?
C60 C61 C64 119.8(7) . . ?
C63 C62 C61 122.6(6) . . ?
C63 C62 H62 118.7 . . ?
C61 C62 H62 118.7 . . ?
C58 C63 C62 119.4(6) . . ?
C58 C63 C68 122.3(6) . . ?
C62 C63 C68 118.2(6) . . ?
C65 C64 C61 110.9(6) . . ?
C65 C64 C67 108.2(7) . . ?
C61 C64 C67 112.3(7) . . ?
C65 C64 C66 108.6(7) . . ?
C61 C64 C66 111.1(7) . . ?
C67 C64 C66 105.7(6) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C2 C68 C63 113.4(5) . . ?
C2 C68 H68A 108.9 . . ?
C63 C68 H68A 108.9 . . ?
C2 C68 H68B 108.9 . . ?
C63 C68 H68B 108.9 . . ?
H68A C68 H68B 107.7 . . ?
C70B N1 V1 173.0(7) . . ?
C70 N1 V1 169.5(5) . . ?
N1 C70 C71 121.8(5) . . ?
N1 C70 C75 118.0(5) . . ?
C71 C70 C75 120.0 . . ?
C72 C71 C70 120.0 . . ?
C72 C71 H71 120.0 . . ?
C70 C71 H71 120.0 . . ?
C71 C72 C73 120.0 . . ?
C71 C72 H72 120.0 . . ?
C73 C72 H72 120.0 . . ?
C74 C73 C72 120.0 . . ?
C74 C73 Cl1A 118.6(5) . . ?
C72 C73 Cl1A 121.2(5) . . ?
C73 C74 C75 120.0 . . ?
C73 C74 H74 120.0 . . ?
C75 C74 H74 120.0 . . ?
C74 C75 C70 120.0 . . ?
C74 C75 H75 120.0 . . ?
C70 C75 H75 120.0 . . ?
N1 C70B C71B 115.4(10) . . ?
N1 C70B C75B 123.5(10) . . ?
C71B C70B C75B 120.0 . . ?
C70B C71B C72B 120.0 . . ?
C70B C71B H71B 120.0 . . ?
C72B C71B H71B 120.0 . . ?
C73B C72B C71B 120.0 . . ?
C73B C72B H72B 120.0 . . ?
C71B C72B H72B 120.0 . . ?
C72B C73B C74B 120.0 . . ?
C72B C73B Cl1B 115.4(11) . . ?
C74B C73B Cl1B 124.5(11) . . ?
C75B C74B C73B 120.0 . . ?
C75B C74B H74B 120.0 . . ?
C73B C74B H74B 120.0 . . ?
C74B C75B C70B 120.0 . . ?
C74B C75B H75B 120.0 . . ?
C70B C75B H75B 120.0 . . ?
C76B N2 V2 166.5(11) . . ?
C76A N2 V2 174.0(4) . . ?
C77A C76A C81A 120.0 . . ?
C77A C76A N2 117.7(5) . . ?
C81A C76A N2 122.2(5) . . ?
C78A C77A C76A 120.0 . . ?
C78A C77A H77A 120.0 . . ?
C76A C77A H77A 120.0 . . ?
C77A C78A C79A 120.0 . . ?
C77A C78A H78A 120.0 . . ?
C79A C78A H78A 120.0 . . ?
C80A C79A C78A 120.0 . . ?
C80A C79A Cl2A 121.6(5) . . ?
C78A C79A Cl2A 118.4(5) . . ?
C81A C80A C79A 120.0 . . ?
C81A C80A H80A 120.0 . . ?
C79A C80A H80A 120.0 . . ?
C80A C81A C76A 120.0 . . ?
C80A C81A H81A 120.0 . . ?
C76A C81A H81A 120.0 . . ?
C1 O1 V1 122.7(4) . . ?
C11 O2 C12 111.7(5) . . ?
C13 O3 V1 130.0(4) . . ?
C24 O4 V1 120.8(3) . . ?
C24 O4 V2 128.5(3) . . ?
V1 O4 V2 108.7(2) . . ?
C35 O5 V2 123.0(4) . . ?
C46 O6 C45 111.5(4) . . ?
C47 O7 V2 127.9(4) . . ?
C58 O8 V2 121.6(3) . . ?
C58 O8 V1 127.4(3) . . ?
V2 O8 V1 108.5(2) . . ?
N1 V1 O3 105.5(2) . . ?
N1 V1 O1 97.8(2) . . ?
O3 V1 O1 102.48(18) . . ?
N1 V1 O4 94.2(2) . . ?
O3 V1 O4 98.63(17) . . ?
O1 V1 O4 151.87(19) . . ?
N1 V1 O8 136.2(2) . . ?
O3 V1 O8 117.3(2) . . ?
O1 V1 O8 82.29(18) . . ?
O4 V1 O8 71.54(16) . . ?
N2 V2 O7 106.4(2) . . ?
N2 V2 O5 98.6(2) . . ?
O7 V2 O5 102.84(17) . . ?
N2 V2 O8 92.33(19) . . ?
O7 V2 O8 98.45(16) . . ?
O5 V2 O8 152.12(18) . . ?
N2 V2 O4 133.2(2) . . ?
O7 V2 O4 119.0(2) . . ?
O5 V2 O4 82.86(17) . . ?
O8 V2 O4 71.09(16) . . ?
N2 C76B C77B 126.6(17) . . ?
N2 C76B C80B 113.4(17) . . ?
C77B C76B C80B 120.0 . . ?
C78B C77B C76B 120.0 . . ?
C78B C77B H77B 120.0 . . ?
C76B C77B H77B 120.0 . . ?
C77B C78B C79B 120.0 . . ?
C77B C78B H78B 120.0 . . ?
C79B C78B H78B 120.0 . . ?
C81B C79B C78B 120.0 . . ?
C81B C79B Cl2B 116.5(15) . . ?
C78B C79B Cl2B 123.5(15) . . ?
C80B C81B C79B 120.0 . . ?
C80B C81B H81B 120.0 . . ?
C79B C81B H81B 120.0 . . ?
C81B C80B C76B 120.0 . . ?
C81B C80B H80B 120.0 . . ?
C76B C80B H80B 120.0 . . ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.051

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1998552'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_vrf_PLAT201_final               
;
RESPONSE: One of the methyl groups is disordered over three
positions. The atom C30A is the central atom of two of these
orientations. This is a false alert.     
;

_vrf_PLAT315_final               
;
RESPONSE: This is a false alert.   The atom C30A is the central 
atom of a methyl group that is disordered over three orientations.
It does not need a hydrogen atom adding.   
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C82 H96 N2 O10 V2), 7(C2 H3 N)
;

_chemical_formula_sum            'C178 H213 N11 O20 V4'
_chemical_formula_weight         3030.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.03540(10)
_cell_length_b                   17.33960(10)
_cell_length_c                   20.19060(10)
_cell_angle_alpha                71.1680(10)
_cell_angle_beta                 84.4590(10)
_cell_angle_gamma                66.4560(10)
_cell_volume                     4260.59(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    105034
_cell_measurement_theta_min      3.436
_cell_measurement_theta_max      70.262

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_F_000             1610
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    2.303
_shelx_estimated_absorpt_T_min   0.682
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28549
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            28571
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.925
_diffrn_reflns_theta_max         68.449
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             28571
_reflns_number_gt                26256
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0925P)²+1.1609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28571
_refine_ls_number_parameters     970
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.046
_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_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 0.39351(3) 0.60440(2) 0.18003(2) 0.02557(10) Uani 1 1 d . . . . .
V2 V 0.16031(3) 0.76285(2) 0.17726(2) 0.02865(11) Uani 1 1 d . . . . .
O1 O 0.50597(11) 0.62329(9) 0.20178(7) 0.0281(3) Uani 1 1 d . . . . .
O2 O 0.64142(12) 0.45082(10) 0.18094(7) 0.0324(3) Uani 1 1 d . . . . .
O3 O 0.42849(12) 0.57707(10) 0.10042(7) 0.0325(3) Uani 1 1 d . . . . .
O4 O 0.23950(11) 0.63471(10) 0.17414(7) 0.0294(3) Uani 1 1 d . . . . .
O5 O 0.04885(11) 0.72951(11) 0.19166(8) 0.0330(3) Uani 1 1 d . . . . .
O6 O -0.08664(13) 0.91717(11) 0.16882(8) 0.0396(4) Uani 1 1 d . . . . .
O7 O 0.12542(12) 0.85230(10) 0.09714(8) 0.0337(3) Uani 1 1 d . . . . .
O8 O 0.31457(11) 0.73342(9) 0.17935(7) 0.0291(3) Uani 1 1 d . . . . .
C1 C 0.56143(16) 0.57801(13) 0.26334(10) 0.0266(4) Uani 1 1 d . . . . .
C2 C 0.51788(16) 0.59735(13) 0.32438(10) 0.0259(4) Uani 1 1 d . . . . .
C3 C 0.57548(16) 0.54856(14) 0.38743(11) 0.0270(4) Uani 1 1 d . . . . .
H3 H 0.546770 0.562148 0.428817 0.032 Uiso 1 1 calc R U . . .
C4 C 0.67360(16) 0.48058(14) 0.39221(11) 0.0282(4) Uani 1 1 d . . . . .
C5 C 0.71463(16) 0.46405(14) 0.32976(11) 0.0295(4) Uani 1 1 d . . . . .
H5 H 0.781556 0.418618 0.331330 0.035 Uiso 1 1 calc R U . . .
C6 C 0.66066(16) 0.51192(14) 0.26557(11) 0.0285(4) Uani 1 1 d . . . . .
C7 C 0.72913(17) 0.41906(15) 0.46290(11) 0.0322(5) Uani 1 1 d . . . . .
C8 C 0.7027(2) 0.33655(17) 0.48346(13) 0.0445(6) Uani 1 1 d . . . . .
H8A H 0.725003 0.307674 0.446953 0.067 Uiso 1 1 calc R U . . .
H8B H 0.738918 0.295259 0.527971 0.067 Uiso 1 1 calc R U . . .
H8C H 0.627520 0.354163 0.488546 0.067 Uiso 1 1 calc R U . . .
C9 C 0.69374(19) 0.46278(16) 0.52053(12) 0.0370(5) Uani 1 1 d . . . . .
H9A H 0.730975 0.421380 0.564689 0.055 Uiso 1 1 calc R U . . .
H9B H 0.708735 0.516211 0.507775 0.055 Uiso 1 1 calc R U . . .
H9C H 0.618785 0.478790 0.526114 0.055 Uiso 1 1 calc R U . . .
C10 C 0.84741(19) 0.3911(2) 0.45823(13) 0.0474(6) Uani 1 1 d . . . . .
H10A H 0.872206 0.362788 0.421518 0.071 Uiso 1 1 calc R U . . .
H10B H 0.864350 0.443448 0.446941 0.071 Uiso 1 1 calc R U . . .
H10C H 0.881195 0.349249 0.503256 0.071 Uiso 1 1 calc R U . . .
C11 C 0.70181(17) 0.49124(16) 0.19945(11) 0.0332(5) Uani 1 1 d . . . . .
H11A H 0.696003 0.546209 0.161527 0.040 Uiso 1 1 calc R U . . .
H11B H 0.775977 0.450393 0.206663 0.040 Uiso 1 1 calc R U . . .
C12 C 0.64006(18) 0.46243(17) 0.10748(11) 0.0362(5) Uani 1 1 d . . . . .
H12A H 0.707749 0.423680 0.094389 0.043 Uiso 1 1 calc R U . . .
H12B H 0.627284 0.524640 0.080211 0.043 Uiso 1 1 calc R U . . .
C13 C 0.45111(18) 0.49786(15) 0.08917(11) 0.0328(5) Uani 1 1 d . . . . .
C14 C 0.55464(18) 0.43869(16) 0.09231(11) 0.0345(5) Uani 1 1 d . . . . .
C15 C 0.57543(18) 0.35738(16) 0.08330(11) 0.0363(5) Uani 1 1 d . . . . .
H15 H 0.645662 0.316665 0.086012 0.044 Uiso 1 1 calc R U . . .
C16 C 0.49709(19) 0.33343(16) 0.07043(11) 0.0358(5) Uani 1 1 d . . . . .
C17 C 0.39477(19) 0.39566(16) 0.06564(11) 0.0356(5) Uani 1 1 d . . . . .
H17 H 0.340041 0.381572 0.055628 0.043 Uiso 1 1 calc R U . . .
C18 C 0.37026(17) 0.47753(16) 0.07501(10) 0.0329(5) Uani 1 1 d . . . . .
C19 C 0.5176(2) 0.24324(16) 0.06267(12) 0.0408(5) Uani 1 1 d . . . . .
C20 C 0.6342(2) 0.18292(19) 0.07113(16) 0.0549(7) Uani 1 1 d . . . . .
H20A H 0.644032 0.126038 0.065816 0.082 Uiso 1 1 calc R U . . .
H20B H 0.672449 0.211320 0.035268 0.082 Uiso 1 1 calc R U . . .
H20C H 0.660387 0.173041 0.117693 0.082 Uiso 1 1 calc R U . . .
C21 C 0.4785(2) 0.25506(17) -0.00964(14) 0.0434(6) Uani 1 1 d . . . . .
H21A H 0.492051 0.196927 -0.013972 0.065 Uiso 1 1 calc R U . . .
H21B H 0.403567 0.290900 -0.015211 0.065 Uiso 1 1 calc R U . . .
H21C H 0.514847 0.284911 -0.045992 0.065 Uiso 1 1 calc R U . . .
C22 C 0.4609(3) 0.1963(2) 0.11978(18) 0.0728(11) Uani 1 1 d . . . . .
H22A H 0.473805 0.138459 0.115053 0.109 Uiso 1 1 calc R U . . .
H22B H 0.486776 0.188011 0.165996 0.109 Uiso 1 1 calc R U . . .
H22C H 0.386067 0.232378 0.114726 0.109 Uiso 1 1 calc R U . . .
C23 C 0.25803(18) 0.54184(17) 0.07362(11) 0.0359(5) Uani 1 1 d . . . . .
H23A H 0.216698 0.538386 0.038420 0.043 Uiso 1 1 calc R U . . .
H23B H 0.255144 0.602985 0.059647 0.043 Uiso 1 1 calc R U . . .
C24 C 0.20395(16) 0.56719(14) 0.19250(11) 0.0294(4) Uani 1 1 d . . . . .
C25 C 0.21104(16) 0.52070(16) 0.14528(11) 0.0331(5) Uani 1 1 d . . . . .
C26 C 0.17800(18) 0.45098(18) 0.16579(13) 0.0399(5) Uani 1 1 d . . . . .
H26 H 0.182144 0.420494 0.133375 0.048 Uiso 1 1 calc R U . . .
C27 C 0.13911(19) 0.42359(19) 0.23148(14) 0.0423(6) Uani 1 1 d . . . . .
C28 C 0.13212(17) 0.47178(16) 0.27657(12) 0.0348(5) Uani 1 1 d . . . . .
H28 H 0.105214 0.455483 0.321607 0.042 Uiso 1 1 calc R U . . .
C29 C 0.16286(16) 0.54266(15) 0.25839(11) 0.0295(4) Uani 1 1 d . . . . .
C30A C 0.1112(3) 0.3372(3) 0.2599(2) 0.0338(4) Uiso 0.6175 1 d D U P A .
C31A C 0.1851(9) 0.2668(9) 0.2367(7) 0.0507(6) Uiso 0.355 1 d D U P A 1
H31A H 0.191102 0.288365 0.185836 0.076 Uiso 0.355 1 calc R U P A 1
H31B H 0.253034 0.246043 0.259859 0.076 Uiso 0.355 1 calc R U P A 1
H31C H 0.161837 0.217873 0.248356 0.076 Uiso 0.355 1 calc R U P A 1
C32A C 0.1006(7) 0.3074(6) 0.3350(4) 0.0507(6) Uiso 0.355 1 d D U P A 1
H32A H 0.049798 0.356509 0.349804 0.076 Uiso 0.355 1 calc R U P A 1
H32B H 0.076844 0.258693 0.347282 0.076 Uiso 0.355 1 calc R U P A 1
H32C H 0.168041 0.286864 0.358786 0.076 Uiso 0.355 1 calc R U P A 1
C33A C -0.0011(6) 0.3734(6) 0.2251(5) 0.0507(6) Uiso 0.355 1 d D U P A 1
H33A H -0.048943 0.421261 0.242480 0.076 Uiso 0.355 1 calc R U P A 1
H33B H 0.002214 0.395882 0.174146 0.076 Uiso 0.355 1 calc R U P A 1
H33C H -0.025921 0.325290 0.237291 0.076 Uiso 0.355 1 calc R U P A 1
C30B C 0.0886(5) 0.3647(4) 0.2388(3) 0.0338(4) Uiso 0.3825 1 d D U P B 2
C31B C 0.0010(6) 0.3921(5) 0.1860(4) 0.0507(6) Uiso 0.3825 1 d D U P B 2
H31D H -0.026509 0.345713 0.197126 0.076 Uiso 0.3825 1 calc R U P B 2
H31E H -0.054660 0.447608 0.188224 0.076 Uiso 0.3825 1 calc R U P B 2
H31F H 0.028015 0.400443 0.138696 0.076 Uiso 0.3825 1 calc R U P B 2
C32B C 0.0415(6) 0.3464(5) 0.3114(4) 0.0507(6) Uiso 0.3825 1 d D U P B 2
H32D H 0.007079 0.305849 0.315718 0.076 Uiso 0.3825 1 calc R U P B 2
H32E H 0.096906 0.319594 0.347733 0.076 Uiso 0.3825 1 calc R U P B 2
H32F H -0.009370 0.402197 0.316882 0.076 Uiso 0.3825 1 calc R U P B 2
C33B C 0.1719(9) 0.2763(9) 0.2283(7) 0.0507(6) Uiso 0.3825 1 d D U P B 2
H33D H 0.139000 0.234550 0.233100 0.076 Uiso 0.3825 1 calc R U P B 2
H33E H 0.200090 0.289338 0.181550 0.076 Uiso 0.3825 1 calc R U P B 2
H33F H 0.228429 0.250103 0.263803 0.076 Uiso 0.3825 1 calc R U P B 2
C31C C 0.1653(9) 0.2726(7) 0.3340(5) 0.0507(6) Uiso 0.2625 1 d D U P A 3
H31G H 0.240967 0.249804 0.330020 0.076 Uiso 0.2625 1 calc R U P A 3
H31H H 0.145460 0.305091 0.368201 0.076 Uiso 0.2625 1 calc R U P A 3
H31I H 0.142635 0.223120 0.349432 0.076 Uiso 0.2625 1 calc R U P A 3
C32C C -0.0023(8) 0.3673(7) 0.2724(6) 0.0507(6) Uiso 0.2625 1 d D U P A 3
H32G H -0.019890 0.403213 0.304067 0.076 Uiso 0.2625 1 calc R U P A 3
H32H H -0.041418 0.402829 0.227793 0.076 Uiso 0.2625 1 calc R U P A 3
H32I H -0.020188 0.315647 0.293650 0.076 Uiso 0.2625 1 calc R U P A 3
C33C C 0.1452(10) 0.2808(8) 0.2111(6) 0.0507(6) Uiso 0.2625 1 d D U P A 3
H33G H 0.220238 0.262876 0.204710 0.076 Uiso 0.2625 1 calc R U P A 3
H33H H 0.129255 0.228019 0.231541 0.076 Uiso 0.2625 1 calc R U P A 3
H33I H 0.108025 0.315201 0.165683 0.076 Uiso 0.2625 1 calc R U P A 3
C34 C 0.14793(16) 0.59084(14) 0.31170(11) 0.0286(4) Uani 1 1 d . . . . .
H34A H 0.167951 0.546881 0.358908 0.034 Uiso 1 1 calc R U . . .
H34B H 0.194665 0.623182 0.301386 0.034 Uiso 1 1 calc R U . . .
C35 C -0.00668(17) 0.72529(16) 0.25049(11) 0.0330(5) Uani 1 1 d . . . . .
C36 C 0.03701(17) 0.65566(15) 0.31185(11) 0.0305(4) Uani 1 1 d . . . . .
C37 C -0.02232(17) 0.64960(16) 0.37138(12) 0.0339(5) Uani 1 1 d . . . . .
H37 H 0.006696 0.601955 0.412954 0.041 Uiso 1 1 calc R U . . .
C38 C -0.12316(18) 0.71167(17) 0.37147(13) 0.0374(5) Uani 1 1 d . . . . .
C39 C -0.16263(18) 0.78203(17) 0.31002(13) 0.0398(5) Uani 1 1 d . . . . .
H39 H -0.230150 0.826139 0.309784 0.048 Uiso 1 1 calc R U . . .
C40 C -0.10687(17) 0.78994(17) 0.24919(12) 0.0379(5) Uani 1 1 d . . . . .
C41 C -0.1920(2) 0.70507(18) 0.43531(14) 0.0459(6) Uani 1 1 d . . . . .
C42 C -0.1364(2) 0.6244(2) 0.49823(14) 0.0491(6) Uani 1 1 d . . . . .
H42A H -0.115391 0.570278 0.485155 0.074 Uiso 1 1 calc R U . . .
H42B H -0.074673 0.629055 0.512537 0.074 Uiso 1 1 calc R U . . .
H42C H -0.183654 0.622233 0.537203 0.074 Uiso 1 1 calc R U . . .
C43 C -0.2887(2) 0.6958(2) 0.41434(17) 0.0628(8) Uani 1 1 d . . . . .
H43A H -0.267033 0.641819 0.401061 0.094 Uiso 1 1 calc R U . . .
H43B H -0.334549 0.692506 0.454052 0.094 Uiso 1 1 calc R U . . .
H43C H -0.326020 0.747303 0.374585 0.094 Uiso 1 1 calc R U . . .
C44 C -0.2243(3) 0.7888(2) 0.45613(18) 0.0714(10) Uani 1 1 d . . . . .
H44A H -0.259903 0.840676 0.416113 0.107 Uiso 1 1 calc R U . . .
H44B H -0.271450 0.786454 0.495172 0.107 Uiso 1 1 calc R U . . .
H44C H -0.162469 0.793276 0.470506 0.107 Uiso 1 1 calc R U . . .
C45 C -0.14852(18) 0.86575(18) 0.18259(13) 0.0430(6) Uani 1 1 d . . . . .
H45A H -0.145495 0.842676 0.143191 0.052 Uiso 1 1 calc R U . . .
H45B H -0.221920 0.902944 0.187761 0.052 Uiso 1 1 calc R U . . .
C46 C -0.08652(18) 0.96431(17) 0.09558(12) 0.0401(5) Uani 1 1 d . . . . .
H46A H -0.154631 1.014159 0.080437 0.048 Uiso 1 1 calc R U . . .
H46B H -0.074240 0.924225 0.067306 0.048 Uiso 1 1 calc R U . . .
C47 C 0.10234(18) 0.94001(15) 0.08662(11) 0.0349(5) Uani 1 1 d . . . . .
C48 C -0.00183(18) 0.99853(16) 0.08519(11) 0.0372(5) Uani 1 1 d . . . . .
C49 C -0.0229(2) 1.08711(17) 0.07417(12) 0.0423(6) Uani 1 1 d . . . . .
H49 H -0.093284 1.127005 0.073088 0.051 Uiso 1 1 calc R U . . .
C50 C 0.0552(2) 1.11991(16) 0.06459(13) 0.0417(6) Uani 1 1 d . . . . .
C51 C 0.1581(2) 1.05970(16) 0.06590(12) 0.0383(5) Uani 1 1 d . . . . .
H51 H 0.212604 1.080562 0.058843 0.046 Uiso 1 1 calc R U . . .
C52 C 0.18298(18) 0.96986(15) 0.07727(11) 0.0350(5) Uani 1 1 d . . . . .
C53 C 0.0275(2) 1.21864(18) 0.05014(16) 0.0525(7) Uani 1 1 d . . . . .
C54 C -0.0527(3) 1.2538(3) 0.1013(3) 0.0947(14) Uani 1 1 d . . . . .
H54A H -0.069542 1.317130 0.091288 0.142 Uiso 1 1 calc R U . . .
H54B H -0.115973 1.244981 0.096020 0.142 Uiso 1 1 calc R U . . .
H54C H -0.024087 1.221908 0.149362 0.142 Uiso 1 1 calc R U . . .
C55 C -0.0175(3) 1.2675(2) -0.0250(2) 0.0809(13) Uani 1 1 d . . . . .
H55A H -0.035748 1.331064 -0.035320 0.121 Uiso 1 1 calc R U . . .
H55B H 0.034402 1.245341 -0.057687 0.121 Uiso 1 1 calc R U . . .
H55C H -0.079849 1.257334 -0.030085 0.121 Uiso 1 1 calc R U . . .
C56 C 0.1231(3) 1.2384(2) 0.0554(2) 0.0712(10) Uani 1 1 d . . . . .
H56A H 0.101859 1.302267 0.045782 0.107 Uiso 1 1 calc R U . . .
H56B H 0.155057 1.206976 0.102647 0.107 Uiso 1 1 calc R U . . .
H56C H 0.173433 1.218749 0.021118 0.107 Uiso 1 1 calc R U . . .
C57 C 0.29552(18) 0.90494(15) 0.08180(12) 0.0352(5) Uani 1 1 d . . . . .
H57A H 0.299359 0.855263 0.066152 0.042 Uiso 1 1 calc R U . . .
H57B H 0.337205 0.935056 0.050130 0.042 Uiso 1 1 calc R U . . .
C58 C 0.34998(16) 0.78524(14) 0.20172(11) 0.0290(4) Uani 1 1 d . . . . .
C59 C 0.34087(16) 0.86891(14) 0.15613(11) 0.0317(5) Uani 1 1 d . . . . .
C60 C 0.37163(17) 0.92188(15) 0.18119(13) 0.0355(5) Uani 1 1 d . . . . .
H60 H 0.366849 0.977808 0.150077 0.043 Uiso 1 1 calc R U . . .
C61 C 0.40891(17) 0.89694(14) 0.24940(13) 0.0350(5) Uani 1 1 d . . . . .
C62 C 0.41893(17) 0.81281(14) 0.29250(12) 0.0314(4) Uani 1 1 d . . . . .
H62 H 0.445618 0.793168 0.339143 0.038 Uiso 1 1 calc R U . . .
C63 C 0.39130(16) 0.75648(14) 0.26979(11) 0.0287(4) Uani 1 1 d . . . . .
C64 C 0.4409(2) 0.95830(16) 0.27398(15) 0.0431(6) Uani 1 1 d . . . . .
C65 C 0.3576(2) 1.05311(17) 0.25131(17) 0.0508(7) Uani 1 1 d . . . . .
H65A H 0.379199 1.091460 0.267428 0.076 Uiso 1 1 calc R U . . .
H65B H 0.348962 1.075153 0.200139 0.076 Uiso 1 1 calc R U . . .
H65C H 0.291392 1.053174 0.271904 0.076 Uiso 1 1 calc R U . . .
C66 C 0.5440(2) 0.9580(2) 0.2402(2) 0.0586(8) Uani 1 1 d . . . . .
H66A H 0.566145 0.996843 0.255196 0.088 Uiso 1 1 calc R U . . .
H66B H 0.597249 0.897561 0.254845 0.088 Uiso 1 1 calc R U . . .
H66C H 0.534209 0.979227 0.189136 0.088 Uiso 1 1 calc R U . . .
C67 C 0.4552(3) 0.9282(2) 0.35404(17) 0.0621(8) Uani 1 1 d . . . . .
H67A H 0.475543 0.969036 0.367638 0.093 Uiso 1 1 calc R U . . .
H67B H 0.389589 0.928027 0.375581 0.093 Uiso 1 1 calc R U . . .
H67C H 0.509452 0.868404 0.369979 0.093 Uiso 1 1 calc R U . . .
C68 C 0.40766(16) 0.66564(13) 0.32099(10) 0.0269(4) Uani 1 1 d . . . . .
H68A H 0.389703 0.671381 0.368280 0.032 Uiso 1 1 calc R U . . .
H68B H 0.359362 0.644032 0.307419 0.032 Uiso 1 1 calc R U . . .
N1 N 0.41441(13) 0.50737(12) 0.24000(9) 0.0276(4) Uani 1 1 d . . . . .
C71 C 0.42592(16) 0.42724(14) 0.28869(11) 0.0282(4) Uani 1 1 d . . . . .
C72 C 0.43826(19) 0.41417(15) 0.36003(11) 0.0341(5) Uani 1 1 d . . . . .
H72 H 0.439627 0.460441 0.374878 0.041 Uiso 1 1 calc R U . . .
C73 C 0.4484(2) 0.33427(17) 0.40857(12) 0.0405(5) Uani 1 1 d . . . . .
H73 H 0.457805 0.325274 0.456864 0.049 Uiso 1 1 calc R U . . .
C74 C 0.4450(2) 0.26657(16) 0.38740(13) 0.0413(5) Uani 1 1 d . . . . .
C75 C 0.4335(2) 0.27866(17) 0.31654(14) 0.0429(6) Uani 1 1 d . . . . .
H75 H 0.431605 0.232364 0.301973 0.051 Uiso 1 1 calc R U . . .
C76 C 0.4249(2) 0.35822(16) 0.26767(13) 0.0383(5) Uani 1 1 d . . . . .
H76 H 0.418117 0.366212 0.219284 0.046 Uiso 1 1 calc R U . . .
O9 O 0.45346(18) 0.19107(12) 0.44034(10) 0.0565(5) Uani 1 1 d . . . . .
C77 C 0.4438(3) 0.1215(2) 0.4213(2) 0.0715(10) Uani 1 1 d . . . . .
H77A H 0.451176 0.071186 0.463399 0.107 Uiso 1 1 calc R U . . .
H77B H 0.375334 0.143202 0.398486 0.107 Uiso 1 1 calc R U . . .
H77C H 0.498207 0.102520 0.388892 0.107 Uiso 1 1 calc R U . . .
N2 N 0.13843(14) 0.81263(12) 0.23800(9) 0.0322(4) Uani 1 1 d . . . . .
C81 C 0.12266(17) 0.85425(15) 0.28830(12) 0.0350(5) Uani 1 1 d . . . . .
C82 C 0.0999(3) 0.81462(18) 0.35636(14) 0.0548(7) Uani 1 1 d . . . . .
H82 H 0.092940 0.759504 0.368074 0.066 Uiso 1 1 calc R U . . .
C83 C 0.0874(3) 0.8559(2) 0.40671(16) 0.0683(10) Uani 1 1 d . . . . .
H83 H 0.072236 0.828667 0.453146 0.082 Uiso 1 1 calc R U . . .
C84 C 0.0966(2) 0.9361(2) 0.39016(16) 0.0568(7) Uani 1 1 d . . . . .
C85 C 0.1161(2) 0.9777(2) 0.32170(18) 0.0575(8) Uani 1 1 d . . . . .
H85 H 0.120976 1.033610 0.310101 0.069 Uiso 1 1 calc R U . . .
C86 C 0.1284(2) 0.9372(2) 0.27080(16) 0.0495(6) Uani 1 1 d . . . . .
H86 H 0.140733 0.965708 0.223991 0.059 Uiso 1 1 calc R U . . .
O10 O 0.0839(2) 0.96922(18) 0.44462(14) 0.0815(8) Uani 1 1 d . . . . .
C87 C 0.0986(4) 1.0494(3) 0.4317(3) 0.0981(15) Uani 1 1 d . . . . .
H87A H 0.087298 1.066038 0.474678 0.147 Uiso 1 1 calc R U . . .
H87B H 0.169601 1.040843 0.416707 0.147 Uiso 1 1 calc R U . . .
H87C H 0.048857 1.096437 0.394816 0.147 Uiso 1 1 calc R U . . .
N3 N 0.8888(3) 0.2116(3) 0.3110(4) 0.150(2) Uani 1 1 d . . . . .
C91 C 0.8009(3) 0.2351(2) 0.3075(2) 0.0765(11) Uani 1 1 d . . . . .
C92 C 0.6915(3) 0.2653(2) 0.3023(2) 0.0667(9) Uani 1 1 d . . . . .
H92A H 0.661869 0.274016 0.346523 0.100 Uiso 1 1 calc R U . . .
H92B H 0.672903 0.221252 0.292286 0.100 Uiso 1 1 calc R U . . .
H92C H 0.663969 0.321482 0.264319 0.100 Uiso 1 1 calc R U . . .
C94 C -0.0924(4) 0.6124(4) 0.1553(3) 0.0537(14) Uani 0.5 1 d . . P . .
H94A H -0.113555 0.676766 0.141206 0.080 Uiso 0.5 1 calc R U P . .
H94B H -0.016638 0.583368 0.162270 0.080 Uiso 0.5 1 calc R U P . .
H94C H -0.125155 0.592995 0.199182 0.080 Uiso 0.5 1 calc R U P . .
N5 N 0.6579(4) 0.8819(4) 0.0612(2) 0.133(2) Uani 1 1 d . . . . .
C95 C 0.6477(3) 0.8281(3) 0.1072(2) 0.0735(10) Uani 1 1 d . . . . .
C96 C 0.6333(3) 0.7605(2) 0.16508(19) 0.0658(8) Uani 1 1 d . . . . .
H96A H 0.631272 0.713865 0.148500 0.099 Uiso 1 1 calc R U . . .
H96B H 0.567596 0.785951 0.186889 0.099 Uiso 1 1 calc R U . . .
H96C H 0.690975 0.735210 0.199523 0.099 Uiso 1 1 calc R U . . .
N6 N -0.3363(3) 1.0628(3) 0.3144(3) 0.135(2) Uani 1 1 d . . . . .
C97 C -0.2514(3) 1.0405(3) 0.3038(3) 0.0797(12) Uani 1 1 d . . . . .
C98 C -0.1452(3) 1.0156(4) 0.2862(3) 0.122(2) Uani 1 1 d . . . . .
H98A H -0.131431 0.983509 0.252038 0.183 Uiso 1 1 calc R U . . .
H98B H -0.101068 0.977419 0.328485 0.183 Uiso 1 1 calc R U . . .
H98C H -0.129964 1.068787 0.266005 0.183 Uiso 1 1 calc R U . . .
C93 C -0.1244(6) 0.5894(5) 0.1021(4) 0.0746(19) Uiso 0.5 1 d . . P . .
N4B N -0.1523(8) 0.5731(6) 0.0589(5) 0.113(3) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.6560(18) . ?
V1 O3 1.7896(14) . ?
V1 O1 1.8523(15) . ?
V1 O4 2.0161(15) . ?
V1 O8 2.0580(15) . ?
V2 N2 1.6559(18) . ?
V2 O7 1.7858(15) . ?
V2 O5 1.8417(16) . ?
V2 O8 2.0176(15) . ?
V2 O4 2.0688(15) . ?
O1 C1 1.355(2) . ?
O2 C12 1.432(2) . ?
O2 C11 1.433(3) . ?
O3 C13 1.370(3) . ?
O4 C24 1.381(3) . ?
O5 C35 1.354(3) . ?
O6 C45 1.428(3) . ?
O6 C46 1.440(3) . ?
O7 C47 1.369(3) . ?
O8 C58 1.386(3) . ?
C1 C6 1.400(3) . ?
C1 C2 1.401(3) . ?
C2 C3 1.395(3) . ?
C2 C68 1.518(3) . ?
C3 C4 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.402(3) . ?
C4 C7 1.533(3) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 C11 1.496(3) . ?
C7 C9 1.527(3) . ?
C7 C10 1.535(3) . ?
C7 C8 1.538(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.499(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.393(3) . ?
C13 C14 1.397(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.392(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.399(3) . ?
C16 C19 1.531(3) . ?
C17 C18 1.393(3) . ?
C17 H17 0.9500 . ?
C18 C23 1.520(3) . ?
C19 C21 1.532(3) . ?
C19 C22 1.536(4) . ?
C19 C20 1.541(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.526(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C29 1.402(3) . ?
C24 C25 1.408(3) . ?
C25 C26 1.391(4) . ?
C26 C27 1.394(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(3) . ?
C27 C30B 1.424(7) . ?
C27 C30A 1.611(5) . ?
C28 C29 1.390(3) . ?
C28 H28 0.9500 . ?
C29 C34 1.516(3) . ?
C30A C31A 1.432(12) . ?
C30A C32A 1.450(8) . ?
C30A C32C 1.489(10) . ?
C30A C33C 1.521(11) . ?
C30A C33A 1.585(9) . ?
C30A C31C 1.589(10) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C30B C31B 1.528(9) . ?
C30B C32B 1.538(9) . ?
C30B C33B 1.578(12) . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C31C H31G 0.9800 . ?
C31C H31H 0.9800 . ?
C31C H31I 0.9800 . ?
C32C H32G 0.9800 . ?
C32C H32H 0.9800 . ?
C32C H32I 0.9800 . ?
C33C H33G 0.9800 . ?
C33C H33H 0.9800 . ?
C33C H33I 0.9800 . ?
C34 C36 1.513(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.399(3) . ?
C35 C40 1.401(3) . ?
C36 C37 1.394(3) . ?
C37 C38 1.395(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.397(4) . ?
C38 C41 1.536(3) . ?
C39 C40 1.390(3) . ?
C39 H39 0.9500 . ?
C40 C45 1.508(3) . ?
C41 C44 1.524(4) . ?
C41 C42 1.534(4) . ?
C41 C43 1.542(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C48 1.498(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C52 1.396(4) . ?
C47 C48 1.404(3) . ?
C48 C49 1.387(4) . ?
C49 C50 1.397(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.401(3) . ?
C50 C53 1.528(4) . ?
C51 C52 1.397(3) . ?
C51 H51 0.9500 . ?
C52 C57 1.520(3) . ?
C53 C54 1.530(5) . ?
C53 C56 1.532(5) . ?
C53 C55 1.532(4) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C59 1.520(3) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C63 1.398(3) . ?
C58 C59 1.407(3) . ?
C59 C60 1.395(3) . ?
C60 C61 1.390(3) . ?
C60 H60 0.9500 . ?
C61 C62 1.395(3) . ?
C61 C64 1.532(3) . ?
C62 C63 1.393(3) . ?
C62 H62 0.9500 . ?
C63 C68 1.519(3) . ?
C64 C67 1.536(4) . ?
C64 C65 1.537(4) . ?
C64 C66 1.537(4) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
N1 C71 1.376(3) . ?
C71 C76 1.399(3) . ?
C71 C72 1.401(3) . ?
C72 C73 1.376(3) . ?
C72 H72 0.9500 . ?
C73 C74 1.391(4) . ?
C73 H73 0.9500 . ?
C74 O9 1.367(3) . ?
C74 C75 1.393(4) . ?
C75 C76 1.379(3) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
O9 C77 1.437(4) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
N2 C81 1.380(3) . ?
C81 C82 1.394(4) . ?
C81 C86 1.400(4) . ?
C82 C83 1.382(4) . ?
C82 H82 0.9500 . ?
C83 C84 1.378(5) . ?
C83 H83 0.9500 . ?
C84 O10 1.364(3) . ?
C84 C85 1.396(5) . ?
C85 C86 1.383(4) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
O10 C87 1.423(5) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
N3 C91 1.136(5) . ?
C91 C92 1.413(5) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C94 C93 1.425(10) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
N5 C95 1.129(5) . ?
C95 C96 1.428(5) . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
N6 C97 1.119(5) . ?
C97 C98 1.419(6) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C93 N4B 1.143(11) . ?

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 V1 O3 103.48(8) . . ?
N1 V1 O1 99.23(8) . . ?
O3 V1 O1 103.65(7) . . ?
N1 V1 O4 92.30(7) . . ?
O3 V1 O4 98.47(7) . . ?
O1 V1 O4 151.80(6) . . ?
N1 V1 O8 133.52(7) . . ?
O3 V1 O8 121.44(6) . . ?
O1 V1 O8 82.31(6) . . ?
O4 V1 O8 71.22(6) . . ?
N2 V2 O7 103.70(8) . . ?
N2 V2 O5 98.91(8) . . ?
O7 V2 O5 103.70(7) . . ?
N2 V2 O8 93.08(8) . . ?
O7 V2 O8 98.48(7) . . ?
O5 V2 O8 151.38(7) . . ?
N2 V2 O4 135.52(8) . . ?
O7 V2 O4 119.28(6) . . ?
O5 V2 O4 82.41(6) . . ?
O8 V2 O4 70.97(6) . . ?
C1 O1 V1 123.00(12) . . ?
C12 O2 C11 112.94(17) . . ?
C13 O3 V1 128.59(13) . . ?
C24 O4 V1 119.27(12) . . ?
C24 O4 V2 127.69(12) . . ?
V1 O4 V2 108.68(7) . . ?
C35 O5 V2 124.22(14) . . ?
C45 O6 C46 112.97(19) . . ?
C47 O7 V2 128.54(13) . . ?
C58 O8 V2 118.79(12) . . ?
C58 O8 V1 128.44(12) . . ?
V2 O8 V1 109.05(7) . . ?
O1 C1 C6 119.93(18) . . ?
O1 C1 C2 119.34(18) . . ?
C6 C1 C2 120.72(19) . . ?
C3 C2 C1 118.35(19) . . ?
C3 C2 C68 122.07(18) . . ?
C1 C2 C68 119.45(18) . . ?
C2 C3 C4 122.72(19) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.01(19) . . ?
C3 C4 C7 122.02(18) . . ?
C5 C4 C7 120.58(19) . . ?
C6 C5 C4 122.23(19) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 118.94(19) . . ?
C5 C6 C11 122.32(19) . . ?
C1 C6 C11 118.61(18) . . ?
C9 C7 C4 112.09(18) . . ?
C9 C7 C10 107.81(19) . . ?
C4 C7 C10 111.15(18) . . ?
C9 C7 C8 108.44(19) . . ?
C4 C7 C8 107.79(18) . . ?
C10 C7 C8 109.5(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 C6 107.76(17) . . ?
O2 C11 H11A 110.2 . . ?
C6 C11 H11A 110.2 . . ?
O2 C11 H11B 110.2 . . ?
C6 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O2 C12 C14 107.64(18) . . ?
O2 C12 H12A 110.2 . . ?
C14 C12 H12A 110.2 . . ?
O2 C12 H12B 110.2 . . ?
C14 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
O3 C13 C18 119.34(19) . . ?
O3 C13 C14 119.6(2) . . ?
C18 C13 C14 121.1(2) . . ?
C15 C14 C13 118.6(2) . . ?
C15 C14 C12 121.5(2) . . ?
C13 C14 C12 119.9(2) . . ?
C14 C15 C16 122.4(2) . . ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
C15 C16 C17 117.2(2) . . ?
C15 C16 C19 123.4(2) . . ?
C17 C16 C19 119.4(2) . . ?
C18 C17 C16 122.4(2) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C17 C18 C13 118.4(2) . . ?
C17 C18 C23 121.3(2) . . ?
C13 C18 C23 120.2(2) . . ?
C16 C19 C21 110.2(2) . . ?
C16 C19 C22 109.1(2) . . ?
C21 C19 C22 109.6(3) . . ?
C16 C19 C20 112.0(2) . . ?
C21 C19 C20 108.1(2) . . ?
C22 C19 C20 107.7(2) . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 C25 111.02(18) . . ?
C18 C23 H23A 109.4 . . ?
C25 C23 H23A 109.4 . . ?
C18 C23 H23B 109.4 . . ?
C25 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
O4 C24 C29 120.91(18) . . ?
O4 C24 C25 119.86(19) . . ?
C29 C24 C25 119.2(2) . . ?
C26 C25 C24 118.9(2) . . ?
C26 C25 C23 119.0(2) . . ?
C24 C25 C23 122.1(2) . . ?
C25 C26 C27 123.3(2) . . ?
C25 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C26 C27 C28 116.2(2) . . ?
C26 C27 C30B 115.9(3) . . ?
C28 C27 C30B 126.1(3) . . ?
C26 C27 C30A 124.7(2) . . ?
C28 C27 C30A 118.9(2) . . ?
C30B C27 C30A 19.0(3) . . ?
C29 C28 C27 122.8(2) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C28 C29 C24 119.57(19) . . ?
C28 C29 C34 117.18(19) . . ?
C24 C29 C34 123.2(2) . . ?
C31A C30A C32A 110.8(7) . . ?
C32C C30A C33C 112.8(7) . . ?
C31A C30A C33A 112.2(6) . . ?
C32A C30A C33A 106.8(5) . . ?
C32C C30A C31C 104.6(6) . . ?
C33C C30A C31C 105.5(7) . . ?
C31A C30A C27 110.3(7) . . ?
C32A C30A C27 114.8(4) . . ?
C32C C30A C27 107.8(5) . . ?
C33C C30A C27 112.5(6) . . ?
C33A C30A C27 101.6(4) . . ?
C31C C30A C27 113.4(5) . . ?
C30A C31A H31A 109.5 . . ?
C30A C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C30A C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C30A C32A H32A 109.5 . . ?
C30A C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C30A C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C30A C33A H33A 109.5 . . ?
C30A C33A H33B 109.5 . . ?
H33A C33A H33B 109.5 . . ?
C30A C33A H33C 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C27 C30B C31B 118.1(5) . . ?
C27 C30B C32B 110.3(5) . . ?
C31B C30B C32B 105.9(6) . . ?
C27 C30B C33B 107.9(7) . . ?
C31B C30B C33B 103.6(6) . . ?
C32B C30B C33B 110.9(7) . . ?
C30B C31B H31D 109.5 . . ?
C30B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30B C32B H32D 109.5 . . ?
C30B C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30B C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C30B C33B H33D 109.5 . . ?
C30B C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C30B C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C30A C31C H31G 109.5 . . ?
C30A C31C H31H 109.5 . . ?
H31G C31C H31H 109.5 . . ?
C30A C31C H31I 109.5 . . ?
H31G C31C H31I 109.5 . . ?
H31H C31C H31I 109.5 . . ?
C30A C32C H32G 109.5 . . ?
C30A C32C H32H 109.5 . . ?
H32G C32C H32H 109.5 . . ?
C30A C32C H32I 109.5 . . ?
H32G C32C H32I 109.5 . . ?
H32H C32C H32I 109.5 . . ?
C30A C33C H33G 109.5 . . ?
C30A C33C H33H 109.5 . . ?
H33G C33C H33H 109.5 . . ?
C30A C33C H33I 109.5 . . ?
H33G C33C H33I 109.5 . . ?
H33H C33C H33I 109.5 . . ?
C36 C34 C29 112.68(17) . . ?
C36 C34 H34A 109.1 . . ?
C29 C34 H34A 109.1 . . ?
C36 C34 H34B 109.1 . . ?
C29 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
O5 C35 C36 119.20(19) . . ?
O5 C35 C40 119.9(2) . . ?
C36 C35 C40 120.9(2) . . ?
C37 C36 C35 118.9(2) . . ?
C37 C36 C34 122.3(2) . . ?
C35 C36 C34 118.78(19) . . ?
C36 C37 C38 121.7(2) . . ?
C36 C37 H37 119.1 . . ?
C38 C37 H37 119.1 . . ?
C37 C38 C39 117.7(2) . . ?
C37 C38 C41 123.0(2) . . ?
C39 C38 C41 119.3(2) . . ?
C40 C39 C38 122.5(2) . . ?
C40 C39 H39 118.8 . . ?
C38 C39 H39 118.8 . . ?
C39 C40 C35 118.3(2) . . ?
C39 C40 C45 123.0(2) . . ?
C35 C40 C45 118.8(2) . . ?
C44 C41 C42 109.1(3) . . ?
C44 C41 C38 109.1(2) . . ?
C42 C41 C38 112.4(2) . . ?
C44 C41 C43 110.1(3) . . ?
C42 C41 C43 108.1(2) . . ?
C38 C41 C43 107.9(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O6 C45 C40 108.52(19) . . ?
O6 C45 H45A 110.0 . . ?
C40 C45 H45A 110.0 . . ?
O6 C45 H45B 110.0 . . ?
C40 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
O6 C46 C48 108.29(19) . . ?
O6 C46 H46A 110.0 . . ?
C48 C46 H46A 110.0 . . ?
O6 C46 H46B 110.0 . . ?
C48 C46 H46B 110.0 . . ?
H46A C46 H46B 108.4 . . ?
O7 C47 C52 119.3(2) . . ?
O7 C47 C48 119.6(2) . . ?
C52 C47 C48 121.0(2) . . ?
C49 C48 C47 118.4(2) . . ?
C49 C48 C46 121.9(2) . . ?
C47 C48 C46 119.7(2) . . ?
C48 C49 C50 122.5(2) . . ?
C48 C49 H49 118.7 . . ?
C50 C49 H49 118.7 . . ?
C49 C50 C51 117.5(2) . . ?
C49 C50 C53 120.5(2) . . ?
C51 C50 C53 122.0(3) . . ?
C52 C51 C50 121.9(3) . . ?
C52 C51 H51 119.0 . . ?
C50 C51 H51 119.0 . . ?
C47 C52 C51 118.6(2) . . ?
C47 C52 C57 120.3(2) . . ?
C51 C52 C57 121.0(2) . . ?
C50 C53 C54 110.6(3) . . ?
C50 C53 C56 112.2(2) . . ?
C54 C53 C56 109.0(3) . . ?
C50 C53 C55 108.2(2) . . ?
C54 C53 C55 109.6(3) . . ?
C56 C53 C55 107.2(3) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C59 C57 C52 111.22(18) . . ?
C59 C57 H57A 109.4 . . ?
C52 C57 H57A 109.4 . . ?
C59 C57 H57B 109.4 . . ?
C52 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
O8 C58 C63 120.63(18) . . ?
O8 C58 C59 119.53(19) . . ?
C63 C58 C59 119.8(2) . . ?
C60 C59 C58 118.4(2) . . ?
C60 C59 C57 118.9(2) . . ?
C58 C59 C57 122.7(2) . . ?
C61 C60 C59 123.3(2) . . ?
C61 C60 H60 118.4 . . ?
C59 C60 H60 118.4 . . ?
C60 C61 C62 116.5(2) . . ?
C60 C61 C64 120.9(2) . . ?
C62 C61 C64 122.5(2) . . ?
C63 C62 C61 122.5(2) . . ?
C63 C62 H62 118.7 . . ?
C61 C62 H62 118.7 . . ?
C62 C63 C58 119.32(19) . . ?
C62 C63 C68 117.83(19) . . ?
C58 C63 C68 122.85(19) . . ?
C61 C64 C67 112.0(2) . . ?
C61 C64 C65 110.5(2) . . ?
C67 C64 C65 107.6(2) . . ?
C61 C64 C66 107.9(2) . . ?
C67 C64 C66 109.5(3) . . ?
C65 C64 C66 109.4(2) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C2 C68 C63 113.92(16) . . ?
C2 C68 H68A 108.8 . . ?
C63 C68 H68A 108.8 . . ?
C2 C68 H68B 108.8 . . ?
C63 C68 H68B 108.8 . . ?
H68A C68 H68B 107.7 . . ?
C71 N1 V1 176.51(16) . . ?
N1 C71 C76 120.5(2) . . ?
N1 C71 C72 120.18(19) . . ?
C76 C71 C72 119.3(2) . . ?
C73 C72 C71 119.9(2) . . ?
C73 C72 H72 120.0 . . ?
C71 C72 H72 120.0 . . ?
C72 C73 C74 120.4(2) . . ?
C72 C73 H73 119.8 . . ?
C74 C73 H73 119.8 . . ?
O9 C74 C73 115.2(2) . . ?
O9 C74 C75 124.7(2) . . ?
C73 C74 C75 120.1(2) . . ?
C76 C75 C74 119.6(2) . . ?
C76 C75 H75 120.2 . . ?
C74 C75 H75 120.2 . . ?
C75 C76 C71 120.6(2) . . ?
C75 C76 H76 119.7 . . ?
C71 C76 H76 119.7 . . ?
C74 O9 C77 117.1(2) . . ?
O9 C77 H77A 109.5 . . ?
O9 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
O9 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C81 N2 V2 178.53(17) . . ?
N2 C81 C82 120.4(2) . . ?
N2 C81 C86 119.9(2) . . ?
C82 C81 C86 119.7(2) . . ?
C83 C82 C81 119.7(3) . . ?
C83 C82 H82 120.1 . . ?
C81 C82 H82 120.1 . . ?
C84 C83 C82 120.6(3) . . ?
C84 C83 H83 119.7 . . ?
C82 C83 H83 119.7 . . ?
O10 C84 C83 114.9(3) . . ?
O10 C84 C85 124.9(3) . . ?
C83 C84 C85 120.2(3) . . ?
C86 C85 C84 119.7(3) . . ?
C86 C85 H85 120.1 . . ?
C84 C85 H85 120.1 . . ?
C85 C86 C81 120.0(3) . . ?
C85 C86 H86 120.0 . . ?
C81 C86 H86 120.0 . . ?
C84 O10 C87 117.5(3) . . ?
O10 C87 H87A 109.5 . . ?
O10 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
O10 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
N3 C91 C92 179.2(6) . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
N5 C95 C96 179.1(4) . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
N6 C97 C98 176.6(7) . . ?
C97 C98 H98A 109.5 . . ?
C97 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C97 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N4B C93 C94 178.1(10) . . ?

_refine_diff_density_max         0.613
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.054

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1998550'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 C74 H96 O16 V4, 6(C2 H3 N)
;

_chemical_formula_sum            'C86 H114 N6 O16 V4'
_chemical_formula_weight         1691.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4983(4)
_cell_length_b                   13.6976(2)
_cell_length_c                   14.1554(3)
_cell_angle_alpha                68.166(2)
_cell_angle_beta                 79.128(2)
_cell_angle_gamma                75.546(2)
_cell_volume                     2165.92(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    52074
_cell_measurement_theta_min      3.6410
_cell_measurement_theta_max      70.2340

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    4.049
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71144
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            95054
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.673
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7886
_reflns_number_gt                7406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'

_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0897P)²+0.6883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7886
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1319
_refine_ls_wR_factor_gt          0.1308
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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_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
O1 O 0.36503(11) 0.75774(11) 0.57167(10) 0.0285(3) Uani 1 1 d . . . . .
O2 O 0.35072(11) 0.58117(11) 0.74466(10) 0.0284(3) Uani 1 1 d . . . . .
O3 O 0.29214(11) 0.49479(10) 0.61991(10) 0.0258(3) Uani 1 1 d . . . . .
O4 O 0.34948(11) 0.35270(11) 0.52116(10) 0.0277(3) Uani 1 1 d . . . . .
O5 O 0.27208(12) 0.69237(12) 0.46028(11) 0.0318(3) Uani 1 1 d . . . . .
O6 O 0.45709(11) 0.56143(11) 0.54466(10) 0.0267(3) Uani 1 1 d . . . . .
O7 O 0.48300(12) 0.33323(12) 0.65922(11) 0.0326(3) Uani 1 1 d . . . . .
O8 O 0.16808(11) 0.67750(11) 0.63966(11) 0.0291(3) Uani 1 1 d . . . . .
V1 V 0.30299(3) 0.65031(3) 0.57427(2) 0.02497(12) Uani 1 1 d . . . . .
V2 V 0.43078(3) 0.41911(3) 0.56032(2) 0.02453(11) Uani 1 1 d . . . . .
C1 C 0.42792(16) 0.77348(15) 0.63083(15) 0.0278(4) Uani 1 1 d . . . . .
C2 C 0.51454(16) 0.82849(15) 0.58195(15) 0.0276(4) Uani 1 1 d . . . . .
C3 C 0.57523(16) 0.85134(16) 0.64169(16) 0.0294(4) Uani 1 1 d . . . . .
H3 H 0.634573 0.888164 0.608922 0.035 Uiso 1 1 calc R U . . .
C4 C 0.55199(17) 0.82212(16) 0.74776(16) 0.0309(4) Uani 1 1 d . . . . .
C5 C 0.46816(17) 0.76238(17) 0.79450(16) 0.0319(4) Uani 1 1 d . . . . .
H5 H 0.452788 0.738886 0.866917 0.038 Uiso 1 1 calc R U . . .
C6 C 0.40704(17) 0.73665(16) 0.73775(16) 0.0300(4) Uani 1 1 d . . . . .
C7 C 0.61219(18) 0.85414(18) 0.81372(17) 0.0342(5) Uani 1 1 d . . . . .
C8 C 0.6605(2) 0.7544(2) 0.90038(18) 0.0409(5) Uani 1 1 d . . . . .
H8A H 0.600361 0.718858 0.943147 0.061 Uiso 1 1 calc R U . . .
H8B H 0.697994 0.775851 0.942261 0.061 Uiso 1 1 calc R U . . .
H8C H 0.714075 0.704741 0.871059 0.061 Uiso 1 1 calc R U . . .
C9 C 0.7062(2) 0.9124(2) 0.75140(19) 0.0405(5) Uani 1 1 d . . . . .
H9A H 0.761329 0.865381 0.720188 0.061 Uiso 1 1 calc R U . . .
H9B H 0.741705 0.931299 0.796596 0.061 Uiso 1 1 calc R U . . .
H9C H 0.675689 0.977861 0.697570 0.061 Uiso 1 1 calc R U . . .
C10 C 0.5266(2) 0.9307(2) 0.8604(2) 0.0431(5) Uani 1 1 d . . . . .
H10A H 0.496835 0.995338 0.805449 0.065 Uiso 1 1 calc R U . . .
H10B H 0.562714 0.950719 0.904415 0.065 Uiso 1 1 calc R U . . .
H10C H 0.465917 0.894835 0.901173 0.065 Uiso 1 1 calc R U . . .
C11 C 0.32339(18) 0.66584(17) 0.78853(16) 0.0314(4) Uani 1 1 d . . . . .
H11A H 0.327420 0.635110 0.863380 0.038 Uiso 1 1 calc R U . . .
H11B H 0.247283 0.707384 0.775630 0.038 Uiso 1 1 calc R U . . .
C12 C 0.33187(17) 0.47629(16) 0.81370(15) 0.0297(4) Uani 1 1 d . . . . .
H12A H 0.325600 0.474379 0.885105 0.036 Uiso 1 1 calc R U . . .
H12B H 0.397137 0.421252 0.804016 0.036 Uiso 1 1 calc R U . . .
C13 C 0.21597(16) 0.45251(15) 0.70073(14) 0.0252(4) Uani 1 1 d . . . . .
C14 C 0.22927(16) 0.44799(15) 0.79816(15) 0.0270(4) Uani 1 1 d . . . . .
C15 C 0.14962(17) 0.41086(16) 0.87925(15) 0.0288(4) Uani 1 1 d . . . . .
H15 H 0.158396 0.406740 0.945926 0.035 Uiso 1 1 calc R U . . .
C16 C 0.05768(17) 0.37972(16) 0.86478(15) 0.0286(4) Uani 1 1 d . . . . .
C17 C 0.04895(17) 0.38467(15) 0.76623(15) 0.0277(4) Uani 1 1 d . . . . .
H17 H -0.012720 0.362954 0.755105 0.033 Uiso 1 1 calc R U . . .
C18 C 0.12703(16) 0.42020(15) 0.68334(15) 0.0258(4) Uani 1 1 d . . . . .
C19 C -0.03525(18) 0.34375(18) 0.94985(15) 0.0335(5) Uani 1 1 d . . . . .
C20 C -0.00601(19) 0.3289(2) 1.05517(16) 0.0382(5) Uani 1 1 d . . . . .
H20A H 0.063000 0.275654 1.069871 0.057 Uiso 1 1 calc R U . . .
H20B H -0.066259 0.304196 1.107462 0.057 Uiso 1 1 calc R U . . .
H20C H 0.003966 0.397484 1.055630 0.057 Uiso 1 1 calc R U . . .
C21 C -0.0577(2) 0.2375(2) 0.95304(19) 0.0469(6) Uani 1 1 d . . . . .
H21A H -0.077460 0.245990 0.886263 0.070 Uiso 1 1 calc R U . . .
H21B H -0.119088 0.217040 1.005756 0.070 Uiso 1 1 calc R U . . .
H21C H 0.009213 0.181535 0.969150 0.070 Uiso 1 1 calc R U . . .
C22 C -0.14145(19) 0.4304(2) 0.92562(17) 0.0408(5) Uani 1 1 d . . . . .
H22A H -0.128875 0.498142 0.925876 0.061 Uiso 1 1 calc R U . . .
H22B H -0.202789 0.407835 0.977544 0.061 Uiso 1 1 calc R U . . .
H22C H -0.160263 0.440475 0.858035 0.061 Uiso 1 1 calc R U . . .
C23 C 0.11861(16) 0.41358(15) 0.58086(14) 0.0263(4) Uani 1 1 d . . . . .
H23A H 0.039690 0.429089 0.568681 0.032 Uiso 1 1 calc R U . . .
H23B H 0.156667 0.466651 0.525251 0.032 Uiso 1 1 calc R U . . .
C24 C 0.28768(16) 0.27395(15) 0.55741(14) 0.0260(4) Uani 1 1 d . . . . .
C25 C 0.17313(17) 0.30134(16) 0.58287(14) 0.0271(4) Uani 1 1 d . . . . .
C26 C 0.11066(17) 0.22057(16) 0.61988(15) 0.0292(4) Uani 1 1 d . . . . .
H26 H 0.033014 0.238985 0.637827 0.035 Uiso 1 1 calc R U . . .
C27 C 0.15826(18) 0.11443(17) 0.63127(16) 0.0319(4) Uani 1 1 d . . . . .
C28 C 0.27279(18) 0.09029(16) 0.60393(15) 0.0311(4) Uani 1 1 d . . . . .
H28 H 0.307088 0.018035 0.611304 0.037 Uiso 1 1 calc R U . . .
C29 C 0.66179(17) 0.83244(16) 0.43345(15) 0.0284(4) Uani 1 1 d . . . . .
C30 C 0.0917(2) 0.02404(18) 0.67544(19) 0.0394(5) Uani 1 1 d . . . . .
C32 C -0.0318(2) 0.0648(2) 0.6957(2) 0.0536(7) Uani 1 1 d . . . . .
H32A H -0.044199 0.102999 0.744404 0.080 Uiso 1 1 calc R U . . .
H32B H -0.070105 0.004082 0.724349 0.080 Uiso 1 1 calc R U . . .
H32C H -0.061014 0.113798 0.631379 0.080 Uiso 1 1 calc R U . . .
C33 C 0.1359(3) -0.0544(2) 0.7759(2) 0.0575(7) Uani 1 1 d . . . . .
H33A H 0.129893 -0.015891 0.823391 0.086 Uiso 1 1 calc R U . . .
H33B H 0.213961 -0.086520 0.762259 0.086 Uiso 1 1 calc R U . . .
H33C H 0.092161 -0.111039 0.806424 0.086 Uiso 1 1 calc R U . . .
C34 C 0.1081(3) -0.0352(2) 0.5984(2) 0.0578(7) Uani 1 1 d . . . . .
H34A H 0.065603 -0.092882 0.625755 0.087 Uiso 1 1 calc R U . . .
H34B H 0.187134 -0.065794 0.587084 0.087 Uiso 1 1 calc R U . . .
H34C H 0.081991 0.015416 0.533333 0.087 Uiso 1 1 calc R U . . .
C35 C 0.53951(17) 0.86197(16) 0.46631(15) 0.0289(4) Uani 1 1 d . . . . .
H35A H 0.497312 0.826829 0.440134 0.035 Uiso 1 1 calc R U . . .
H35B H 0.514315 0.940521 0.435735 0.035 Uiso 1 1 calc R U . . .
C36 C 0.06360(16) 0.69436(17) 0.60362(15) 0.0292(4) Uani 1 1 d . . . . .
H36A H 0.066562 0.642132 0.569660 0.035 Uiso 1 1 calc R U . . .
H36B H 0.046982 0.767480 0.552818 0.035 Uiso 1 1 calc R U . . .
C37 C -0.02676(17) 0.68093(18) 0.69245(16) 0.0318(4) Uani 1 1 d . . . . .
H37A H -0.038308 0.741056 0.718417 0.038 Uiso 1 1 calc R U . . .
H37B H -0.003042 0.613395 0.748574 0.038 Uiso 1 1 calc R U . . .
C38 C -0.13536(19) 0.6783(2) 0.66102(18) 0.0396(5) Uani 1 1 d . . . . .
H38A H -0.157546 0.743939 0.603734 0.059 Uiso 1 1 calc R U . . .
H38B H -0.193150 0.673577 0.719043 0.059 Uiso 1 1 calc R U . . .
H38C H -0.125491 0.615801 0.639997 0.059 Uiso 1 1 calc R U . . .
N1 N 0.2294(3) 0.0447(3) 1.0137(2) 0.0835(9) Uani 1 1 d . . . . .
C39 C 0.2579(3) 0.0951(2) 0.9329(2) 0.0513(6) Uani 1 1 d . . . . .
C40 C 0.2920(3) 0.1610(2) 0.8317(2) 0.0549(7) Uani 1 1 d . . . . .
H40A H 0.233314 0.224293 0.808406 0.082 Uiso 1 1 calc R U . . .
H40B H 0.305841 0.119953 0.785268 0.082 Uiso 1 1 calc R U . . .
H40C H 0.360280 0.183692 0.832074 0.082 Uiso 1 1 calc R U . . .
N2 N 0.5979(3) 0.3020(3) 0.9221(3) 0.0946(11) Uani 1 1 d . . . . .
C41 C 0.6365(3) 0.2503(3) 0.8694(3) 0.0707(9) Uani 1 1 d . . . . .
C42 C 0.6856(3) 0.1887(2) 0.8029(2) 0.0608(7) Uani 1 1 d . . . . .
H42A H 0.738387 0.226182 0.749661 0.091 Uiso 1 1 calc R U . . .
H42B H 0.627092 0.180200 0.770837 0.091 Uiso 1 1 calc R U . . .
H42C H 0.724657 0.117826 0.843004 0.091 Uiso 1 1 calc R U . . .
N3 N 0.8057(2) 0.4094(2) 0.67132(18) 0.0550(6) Uani 1 1 d . . . . .
C43 C 0.7273(2) 0.4650(2) 0.6951(2) 0.0475(6) Uani 1 1 d . . . . .
C44 C 0.6289(2) 0.5347(2) 0.72680(19) 0.0431(5) Uani 1 1 d . . . . .
H44A H 0.642545 0.607744 0.704360 0.065 Uiso 1 1 calc R U . . .
H44B H 0.613417 0.507664 0.801515 0.065 Uiso 1 1 calc R U . . .
H44C H 0.564955 0.535150 0.695700 0.065 Uiso 1 1 calc R U . . .


_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
O1 C1 1.354(3) . ?
O1 V1 1.8128(14) . ?
O2 C11 1.451(2) . ?
O2 C12 1.453(2) . ?
O2 V1 2.3732(14) . ?
O3 C13 1.386(2) . ?
O3 V2 1.9977(13) . ?
O3 V1 2.0152(13) . ?
O4 C24 1.370(2) . ?
O4 V2 1.7934(14) . ?
O5 V1 1.5866(15) . ?
O6 V2 1.8303(13) 2_666 ?
O6 V2 1.9822(14) . ?
O6 V1 2.0667(14) . ?
O7 V2 1.5830(15) . ?
O8 C36 1.425(3) . ?
O8 V1 1.7869(14) . ?
V2 V2 2.9675(6) 2_666 ?
C1 C2 1.398(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.395(3) . ?
C2 C35 1.519(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.403(3) . ?
C4 C7 1.538(3) . ?
C5 C6 1.389(3) . ?
C6 C11 1.502(3) . ?
C7 C9 1.533(3) . ?
C7 C8 1.536(3) . ?
C7 C10 1.540(3) . ?
C12 C14 1.504(3) . ?
C13 C18 1.386(3) . ?
C13 C14 1.397(3) . ?
C14 C15 1.398(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.395(3) . ?
C16 C19 1.536(3) . ?
C17 C18 1.395(3) . ?
C18 C23 1.511(3) . ?
C19 C20 1.530(3) . ?
C19 C21 1.532(3) . ?
C19 C22 1.540(3) . ?
C23 C25 1.510(3) . ?
C24 C25 1.399(3) . ?
C24 C29 1.404(3) 2_666 ?
C25 C26 1.398(3) . ?
C26 C27 1.387(3) . ?
C27 C28 1.399(3) . ?
C27 C30 1.536(3) . ?
C28 C29 1.386(3) 2_666 ?
C29 C35 1.510(3) . ?
C30 C32 1.516(3) . ?
C30 C33 1.532(4) . ?
C30 C34 1.543(4) . ?
C36 C37 1.512(3) . ?
C37 C38 1.518(3) . ?
N1 C39 1.137(4) . ?
C39 C40 1.431(4) . ?
N2 C41 1.174(5) . ?
C41 C42 1.446(5) . ?
N3 C43 1.161(4) . ?
C43 C44 1.466(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
C1 O1 V1 137.13(13) . . ?
C11 O2 C12 116.03(14) . . ?
C11 O2 V1 110.14(12) . . ?
C12 O2 V1 121.24(11) . . ?
C13 O3 V2 129.25(11) . . ?
C13 O3 V1 120.95(11) . . ?
V2 O3 V1 107.25(6) . . ?
C24 O4 V2 142.95(13) . . ?
V2 O6 V2 102.15(6) 2_666 . ?
V2 O6 V1 135.12(7) 2_666 . ?
V2 O6 V1 105.87(6) . . ?
C36 O8 V1 127.21(12) . . ?
O5 V1 O8 99.86(7) . . ?
O5 V1 O1 100.97(7) . . ?
O8 V1 O1 102.34(6) . . ?
O5 V1 O3 101.19(7) . . ?
O8 V1 O3 89.29(6) . . ?
O1 V1 O3 152.74(6) . . ?
O5 V1 O6 95.07(7) . . ?
O8 V1 O6 157.22(6) . . ?
O1 V1 O6 91.50(6) . . ?
O3 V1 O6 70.89(5) . . ?
O5 V1 O2 177.99(6) . . ?
O8 V1 O2 80.86(6) . . ?
O1 V1 O2 80.67(6) . . ?
O3 V1 O2 76.92(5) . . ?
O6 V1 O2 83.69(5) . . ?
O7 V2 O4 106.09(7) . . ?
O7 V2 O6 107.50(7) . 2_666 ?
O4 V2 O6 101.29(6) . 2_666 ?
O7 V2 O6 108.51(7) . . ?
O4 V2 O6 143.91(6) . . ?
O6 V2 O6 77.85(6) 2_666 . ?
O7 V2 O3 102.32(7) . . ?
O4 V2 O3 89.99(6) . . ?
O6 V2 O3 143.49(6) 2_666 . ?
O6 V2 O3 73.01(5) . . ?
O7 V2 V2 113.43(6) . 2_666 ?
O4 V2 V2 131.33(5) . 2_666 ?
O6 V2 V2 40.77(4) 2_666 2_666 ?
O6 V2 V2 37.08(4) . 2_666 ?
O3 V2 V2 107.49(4) . 2_666 ?
O1 C1 C2 117.97(18) . . ?
O1 C1 C6 121.40(18) . . ?
C2 C1 C6 120.64(19) . . ?
C3 C2 C1 118.45(18) . . ?
C3 C2 C35 122.02(18) . . ?
C1 C2 C35 119.53(18) . . ?
C4 C3 C2 122.41(18) . . ?
C3 C4 C5 117.41(19) . . ?
C3 C4 C7 123.01(18) . . ?
C5 C4 C7 119.57(19) . . ?
C6 C5 C4 121.78(19) . . ?
C5 C6 C1 119.08(19) . . ?
C5 C6 C11 121.52(19) . . ?
C1 C6 C11 119.33(18) . . ?
C9 C7 C8 108.83(19) . . ?
C9 C7 C4 112.56(18) . . ?
C8 C7 C4 110.22(18) . . ?
C9 C7 C10 108.04(19) . . ?
C8 C7 C10 109.13(19) . . ?
C4 C7 C10 107.98(18) . . ?
O2 C11 C6 106.65(15) . . ?
O2 C12 C14 113.65(17) . . ?
O3 C13 C18 120.23(17) . . ?
O3 C13 C14 118.06(17) . . ?
C18 C13 C14 121.66(17) . . ?
C13 C14 C15 118.54(19) . . ?
C13 C14 C12 119.15(17) . . ?
C15 C14 C12 122.20(18) . . ?
C16 C15 C14 121.70(19) . . ?
C15 C16 C17 117.48(17) . . ?
C15 C16 C19 123.89(18) . . ?
C17 C16 C19 118.61(18) . . ?
C16 C17 C18 122.72(19) . . ?
C13 C18 C17 117.89(18) . . ?
C13 C18 C23 121.90(17) . . ?
C17 C18 C23 119.99(18) . . ?
C20 C19 C21 108.51(19) . . ?
C20 C19 C16 111.91(18) . . ?
C21 C19 C16 110.38(17) . . ?
C20 C19 C22 109.19(18) . . ?
C21 C19 C22 108.8(2) . . ?
C16 C19 C22 108.00(17) . . ?
C25 C23 C18 107.67(16) . . ?
O4 C24 C25 119.19(17) . . ?
O4 C24 C29 120.41(17) . 2_666 ?
C25 C24 C29 120.39(18) . 2_666 ?
C26 C25 C24 118.86(19) . . ?
C26 C25 C23 119.74(18) . . ?
C24 C25 C23 121.12(17) . . ?
C27 C26 C25 122.20(19) . . ?
C26 C27 C28 117.32(19) . . ?
C26 C27 C30 122.88(19) . . ?
C28 C27 C30 119.76(19) . . ?
C29 C28 C27 122.65(19) 2_666 . ?
C28 C29 C24 118.57(19) 2_666 2_666 ?
C28 C29 C35 120.48(18) 2_666 . ?
C24 C29 C35 120.93(18) 2_666 . ?
C32 C30 C33 109.1(2) . . ?
C32 C30 C27 112.84(19) . . ?
C33 C30 C27 108.6(2) . . ?
C32 C30 C34 108.1(2) . . ?
C33 C30 C34 109.4(2) . . ?
C27 C30 C34 108.86(19) . . ?
C29 C35 C2 112.13(17) . . ?
O8 C36 C37 109.72(16) . . ?
C36 C37 C38 111.44(17) . . ?
N1 C39 C40 178.6(4) . . ?
N2 C41 C42 178.5(4) . . ?
N3 C43 C44 179.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C36 O8 V1 O5 19.64(16) . . . . ?
C36 O8 V1 O1 123.26(15) . . . . ?
C36 O8 V1 O3 -81.60(15) . . . . ?
C36 O8 V1 O6 -110.56(19) . . . . ?
C36 O8 V1 O2 -158.46(16) . . . . ?
C1 O1 V1 O5 -165.53(18) . . . . ?
C1 O1 V1 O8 91.70(18) . . . . ?
C1 O1 V1 O3 -21.7(2) . . . . ?
C1 O1 V1 O6 -70.08(18) . . . . ?
C1 O1 V1 O2 13.28(17) . . . . ?
C24 O4 V2 O7 30.0(2) . . . . ?
C24 O4 V2 O6 142.2(2) . . . 2_666 ?
C24 O4 V2 O6 -133.0(2) . . . . ?
C24 O4 V2 O3 -72.8(2) . . . . ?
C24 O4 V2 V2 173.63(18) . . . 2_666 ?
V1 O1 C1 C2 138.92(16) . . . . ?
V1 O1 C1 C6 -41.5(3) . . . . ?
O1 C1 C2 C3 175.86(17) . . . . ?
C6 C1 C2 C3 -3.8(3) . . . . ?
O1 C1 C2 C35 -3.8(3) . . . . ?
C6 C1 C2 C35 176.54(18) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C35 C2 C3 C4 179.17(18) . . . . ?
C2 C3 C4 C5 3.6(3) . . . . ?
C2 C3 C4 C7 -175.22(18) . . . . ?
C3 C4 C5 C6 -2.6(3) . . . . ?
C7 C4 C5 C6 176.31(19) . . . . ?
C4 C5 C6 C1 -1.5(3) . . . . ?
C4 C5 C6 C11 175.37(19) . . . . ?
O1 C1 C6 C5 -174.84(18) . . . . ?
C2 C1 C6 C5 4.8(3) . . . . ?
O1 C1 C6 C11 8.2(3) . . . . ?
C2 C1 C6 C11 -172.19(18) . . . . ?
C3 C4 C7 C9 -5.0(3) . . . . ?
C5 C4 C7 C9 176.18(19) . . . . ?
C3 C4 C7 C8 -126.7(2) . . . . ?
C5 C4 C7 C8 54.5(2) . . . . ?
C3 C4 C7 C10 114.2(2) . . . . ?
C5 C4 C7 C10 -64.6(3) . . . . ?
C12 O2 C11 C6 144.98(17) . . . . ?
V1 O2 C11 C6 -72.48(17) . . . . ?
C5 C6 C11 O2 -127.5(2) . . . . ?
C1 C6 C11 O2 49.4(2) . . . . ?
C11 O2 C12 C14 103.6(2) . . . . ?
V1 O2 C12 C14 -34.5(2) . . . . ?
V2 O3 C13 C18 -88.5(2) . . . . ?
V1 O3 C13 C18 112.04(17) . . . . ?
V2 O3 C13 C14 94.15(19) . . . . ?
V1 O3 C13 C14 -65.3(2) . . . . ?
O3 C13 C14 C15 176.63(17) . . . . ?
C18 C13 C14 C15 -0.7(3) . . . . ?
O3 C13 C14 C12 -7.2(3) . . . . ?
C18 C13 C14 C12 175.44(18) . . . . ?
O2 C12 C14 C13 54.3(2) . . . . ?
O2 C12 C14 C15 -129.73(19) . . . . ?
C13 C14 C15 C16 -0.7(3) . . . . ?
C12 C14 C15 C16 -176.70(18) . . . . ?
C14 C15 C16 C17 1.4(3) . . . . ?
C14 C15 C16 C19 -176.81(19) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C19 C16 C17 C18 177.55(18) . . . . ?
O3 C13 C18 C17 -175.96(16) . . . . ?
C14 C13 C18 C17 1.3(3) . . . . ?
O3 C13 C18 C23 9.4(3) . . . . ?
C14 C13 C18 C23 -173.30(18) . . . . ?
C16 C17 C18 C13 -0.6(3) . . . . ?
C16 C17 C18 C23 174.13(18) . . . . ?
C15 C16 C19 C20 -9.1(3) . . . . ?
C17 C16 C19 C20 172.71(19) . . . . ?
C15 C16 C19 C21 -130.1(2) . . . . ?
C17 C16 C19 C21 51.7(3) . . . . ?
C15 C16 C19 C22 111.1(2) . . . . ?
C17 C16 C19 C22 -67.1(2) . . . . ?
C13 C18 C23 C25 91.0(2) . . . . ?
C17 C18 C23 C25 -83.5(2) . . . . ?
V2 O4 C24 C25 92.1(3) . . . . ?
V2 O4 C24 C29 -89.5(2) . . . 2_666 ?
O4 C24 C25 C26 -179.95(17) . . . . ?
C29 C24 C25 C26 1.6(3) 2_666 . . . ?
O4 C24 C25 C23 -6.0(3) . . . . ?
C29 C24 C25 C23 175.53(18) 2_666 . . . ?
C18 C23 C25 C26 87.8(2) . . . . ?
C18 C23 C25 C24 -86.1(2) . . . . ?
C24 C25 C26 C27 -0.6(3) . . . . ?
C23 C25 C26 C27 -174.66(19) . . . . ?
C25 C26 C27 C28 -0.1(3) . . . . ?
C25 C26 C27 C30 177.7(2) . . . . ?
C26 C27 C28 C29 -0.2(3) . . . 2_666 ?
C30 C27 C28 C29 -178.0(2) . . . 2_666 ?
C26 C27 C30 C32 5.2(3) . . . . ?
C28 C27 C30 C32 -177.0(2) . . . . ?
C26 C27 C30 C33 -115.8(2) . . . . ?
C28 C27 C30 C33 62.0(3) . . . . ?
C26 C27 C30 C34 125.2(2) . . . . ?
C28 C27 C30 C34 -57.0(3) . . . . ?
C28 C29 C35 C2 -102.5(2) 2_666 . . . ?
C24 C29 C35 C2 75.8(2) 2_666 . . . ?
C3 C2 C35 C29 48.4(2) . . . . ?
C1 C2 C35 C29 -131.94(19) . . . . ?
V1 O8 C36 C37 162.74(13) . . . . ?
O8 C36 C37 C38 -169.79(18) . . . . ?

_refine_diff_density_max         1.009
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.063

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1998553'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H90 F6 N2 O8 V2'
_chemical_formula_sum            'C82 H90 F6 N2 O8 V2'
_chemical_formula_weight         1447.43

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   20.0005(13)
_cell_length_b                   19.9315(8)
_cell_length_c                   22.023(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.080(10)
_cell_angle_gamma                90
_cell_volume                     7885.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6486
_cell_measurement_theta_min      2.113
_cell_measurement_theta_max      25.802

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_F_000             3040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.305
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55466
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            86670
_diffrn_reflns_av_unetI/netI     0.1393
_diffrn_reflns_av_R_equivalents  0.1918
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.863
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_full        25.028
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13936
_reflns_number_gt                6929
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Shedlrick, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1194P)²+17.6429P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13936
_refine_ls_number_parameters     886
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.0964
_refine_ls_wR_factor_ref         0.2734
_refine_ls_wR_factor_gt          0.2235
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.4970(3) 0.1084(3) 0.4516(3) 0.0252(14) Uani 1 1 d . . . . .
C2 C 0.5309(3) 0.0916(3) 0.5200(3) 0.0246(14) Uani 1 1 d . . . . .
C3 C 0.6078(4) 0.0825(3) 0.5512(4) 0.0298(16) Uani 1 1 d . . . . .
H3 H 0.631019 0.070259 0.597649 0.036 Uiso 1 1 calc R U . . .
C4 C 0.6520(4) 0.0903(3) 0.5177(4) 0.0321(16) Uani 1 1 d . . . . .
C5 C 0.6144(4) 0.1044(3) 0.4481(4) 0.0301(15) Uani 1 1 d . . . . .
H5 H 0.642549 0.108369 0.423028 0.036 Uiso 1 1 calc R U . . .
C6 C 0.5387(4) 0.1126(3) 0.4152(3) 0.0268(15) Uani 1 1 d . . . . .
C7 C 0.7360(4) 0.0872(4) 0.5515(4) 0.0415(18) Uani 1 1 d . . . . .
C8 C 0.7674(4) 0.0704(5) 0.6264(4) 0.063(2) Uani 1 1 d . . . . .
H8A H 0.821852 0.068933 0.646068 0.095 Uiso 1 1 calc R U . . .
H8B H 0.752011 0.104829 0.649480 0.095 Uiso 1 1 calc R U . . .
H8C H 0.748490 0.026595 0.631984 0.095 Uiso 1 1 calc R U . . .
C9 C 0.7650(4) 0.0351(4) 0.5180(4) 0.052(2) Uani 1 1 d . . . . .
H9A H 0.819488 0.034294 0.540978 0.078 Uiso 1 1 calc R U . . .
H9B H 0.745579 -0.009254 0.521091 0.078 Uiso 1 1 calc R U . . .
H9C H 0.748392 0.046889 0.470317 0.078 Uiso 1 1 calc R U . . .
C10 C 0.7666(4) 0.1569(4) 0.5438(5) 0.070(3) Uani 1 1 d . . . . .
H10A H 0.821165 0.155815 0.565465 0.106 Uiso 1 1 calc R U . . .
H10B H 0.748593 0.167441 0.495681 0.106 Uiso 1 1 calc R U . . .
H10C H 0.749380 0.191399 0.565347 0.106 Uiso 1 1 calc R U . . .
C11 C 0.5018(4) 0.1298(3) 0.3415(3) 0.0310(16) Uani 1 1 d . . . . .
H11A H 0.535220 0.118660 0.320511 0.037 Uiso 1 1 calc R U . . .
H11B H 0.455321 0.103624 0.318315 0.037 Uiso 1 1 calc R U . . .
C12 C 0.4335(3) 0.2165(3) 0.2679(3) 0.0266(14) Uani 1 1 d . . . . .
H12A H 0.396525 0.180064 0.248156 0.032 Uiso 1 1 calc R U . . .
H12B H 0.459447 0.223095 0.239002 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3474(3) 0.2790(3) 0.3010(3) 0.0227(14) Uani 1 1 d . . . . .
C14 C 0.3958(3) 0.2799(3) 0.2719(3) 0.0250(14) Uani 1 1 d . . . . .
C15 C 0.4065(3) 0.3403(3) 0.2455(3) 0.0270(15) Uani 1 1 d . . . . .
H15 H 0.437972 0.340951 0.223375 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3724(3) 0.3998(3) 0.2504(3) 0.0272(15) Uani 1 1 d . . . . .
C17 C 0.3252(3) 0.3966(3) 0.2812(3) 0.0269(15) Uani 1 1 d . . . . .
H17 H 0.301146 0.436580 0.284503 0.032 Uiso 1 1 calc R U . . .
C18 C 0.3114(3) 0.3374(3) 0.3076(3) 0.0229(14) Uani 1 1 d . . . . .
C19 C 0.3895(4) 0.4658(3) 0.2252(3) 0.0292(15) Uani 1 1 d . . . . .
C20 C 0.4254(4) 0.4558(3) 0.1785(4) 0.0414(19) Uani 1 1 d . . . . .
H20A H 0.435162 0.499627 0.163810 0.062 Uiso 1 1 calc R U . . .
H20B H 0.472367 0.431511 0.202307 0.062 Uiso 1 1 calc R U . . .
H20C H 0.391961 0.429913 0.138955 0.062 Uiso 1 1 calc R U . . .
C21 C 0.3187(4) 0.5067(3) 0.1883(4) 0.0372(17) Uani 1 1 d . . . . .
H21A H 0.294556 0.513675 0.218076 0.056 Uiso 1 1 calc R U . . .
H21B H 0.331191 0.550316 0.175365 0.056 Uiso 1 1 calc R U . . .
H21C H 0.284658 0.482604 0.147609 0.056 Uiso 1 1 calc R U . . .
C22 C 0.4436(4) 0.5066(3) 0.2878(4) 0.0420(18) Uani 1 1 d . . . . .
H22A H 0.420809 0.513434 0.318658 0.063 Uiso 1 1 calc R U . . .
H22B H 0.490342 0.481841 0.311123 0.063 Uiso 1 1 calc R U . . .
H22C H 0.453588 0.550215 0.272946 0.063 Uiso 1 1 calc R U . . .
C23 C 0.2627(3) 0.3346(3) 0.3436(3) 0.0264(14) Uani 1 1 d . . . . .
H23A H 0.240064 0.379308 0.340995 0.032 Uiso 1 1 calc R U . . .
H23B H 0.294248 0.324616 0.391971 0.032 Uiso 1 1 calc R U . . .
C24 C 0.2079(3) 0.2184(3) 0.3449(3) 0.0261(14) Uani 1 1 d . . . . .
C25 C 0.2010(3) 0.2828(3) 0.3157(3) 0.0299(15) Uani 1 1 d . . . . .
C26 C 0.1353(4) 0.2985(3) 0.2607(4) 0.0381(17) Uani 1 1 d . . . . .
H26 H 0.129877 0.342129 0.241881 0.046 Uiso 1 1 calc R U . . .
C27 C 0.0766(4) 0.2540(4) 0.2315(4) 0.0451(19) Uani 1 1 d . . . . .
C28 C 0.0868(4) 0.1904(4) 0.2602(4) 0.0441(19) Uani 1 1 d . . . . .
H28 H 0.048170 0.158206 0.240267 0.053 Uiso 1 1 calc R U . . .
C29 C 0.1509(4) 0.1719(3) 0.3168(3) 0.0330(16) Uani 1 1 d . . . . .
C30 C 0.0037(4) 0.2706(5) 0.1698(5) 0.069(3) Uani 1 1 d . . . . .
C31 C 0.0006(6) 0.2343(6) 0.1083(5) 0.096(4) Uani 1 1 d . . . . .
H31A H 0.042938 0.248016 0.100111 0.144 Uiso 1 1 calc R U . . .
H31B H 0.002752 0.185749 0.116164 0.144 Uiso 1 1 calc R U . . .
H31C H -0.045952 0.245526 0.068874 0.144 Uiso 1 1 calc R U . . .
C32 C -0.0029(4) 0.3481(5) 0.1571(5) 0.080(3) Uani 1 1 d . . . . .
H32A H -0.000889 0.371082 0.197212 0.120 Uiso 1 1 calc R U . . .
H32B H 0.038267 0.363501 0.147937 0.120 Uiso 1 1 calc R U . . .
H32C H -0.050362 0.358255 0.118155 0.120 Uiso 1 1 calc R U . . .
C33 C -0.0623(4) 0.2494(6) 0.1830(7) 0.121(6) Uani 1 1 d . . . . .
H33A H -0.060056 0.273032 0.222838 0.181 Uiso 1 1 calc R U . . .
H33B H -0.108924 0.260652 0.143613 0.181 Uiso 1 1 calc R U . . .
H33C H -0.060220 0.200875 0.190903 0.181 Uiso 1 1 calc R U . . .
C34 C 0.1529(4) 0.1032(3) 0.3469(3) 0.0321(16) Uani 1 1 d . . . . .
H34A H 0.205158 0.090273 0.375794 0.039 Uiso 1 1 calc R U . . .
H34B H 0.131072 0.069782 0.310172 0.039 Uiso 1 1 calc R U . . .
C35 C 0.1448(3) 0.1199(3) 0.4568(3) 0.0273(15) Uani 1 1 d . . . . .
C36 C 0.1096(4) 0.1033(3) 0.3888(4) 0.0301(16) Uani 1 1 d . . . . .
C37 C 0.0343(4) 0.0897(3) 0.3600(4) 0.0333(16) Uani 1 1 d . . . . .
H37 H 0.009979 0.077420 0.313616 0.040 Uiso 1 1 calc R U . . .
C38 C -0.0075(4) 0.0935(3) 0.3971(4) 0.0376(18) Uani 1 1 d . . . . .
C39 C 0.0303(4) 0.1101(3) 0.4649(4) 0.0366(17) Uani 1 1 d . . . . .
H39 H 0.003354 0.112441 0.491241 0.044 Uiso 1 1 calc R U . . .
C40 C 0.1052(4) 0.1234(3) 0.4953(4) 0.0313(16) Uani 1 1 d . . . . .
C41 C -0.0910(4) 0.0790(3) 0.3630(4) 0.0413(18) Uani 1 1 d . . . . .
C42 C -0.1300(5) 0.1263(5) 0.3032(5) 0.080(3) Uani 1 1 d . . . . .
H42A H -0.106669 0.122639 0.272432 0.120 Uiso 1 1 calc R U . . .
H42B H -0.182687 0.114160 0.279184 0.120 Uiso 1 1 calc R U . . .
H42C H -0.125513 0.172542 0.319719 0.120 Uiso 1 1 calc R U . . .
C43 C -0.1040(5) 0.0075(4) 0.3339(6) 0.082(3) Uani 1 1 d . . . . .
H43A H -0.080346 0.002676 0.303437 0.124 Uiso 1 1 calc R U . . .
H43B H -0.082226 -0.024939 0.370902 0.124 Uiso 1 1 calc R U . . .
H43C H -0.157533 -0.000766 0.308767 0.124 Uiso 1 1 calc R U . . .
C44 C -0.1269(5) 0.0853(6) 0.4086(5) 0.086(3) Uani 1 1 d . . . . .
H44A H -0.102454 0.055141 0.447319 0.129 Uiso 1 1 calc R U . . .
H44B H -0.122488 0.131696 0.424724 0.129 Uiso 1 1 calc R U . . .
H44C H -0.179662 0.073313 0.384188 0.129 Uiso 1 1 calc R U . . .
C45 C 0.1452(4) 0.1420(3) 0.5681(4) 0.0390(18) Uani 1 1 d . . . . .
H45A H 0.113714 0.131587 0.591234 0.047 Uiso 1 1 calc R U . . .
H45B H 0.191787 0.115705 0.590051 0.047 Uiso 1 1 calc R U . . .
C46 C 0.2145(4) 0.2314(3) 0.6406(4) 0.0363(17) Uani 1 1 d . . . . .
H46A H 0.249484 0.194090 0.662507 0.044 Uiso 1 1 calc R U . . .
H46B H 0.187891 0.241854 0.668189 0.044 Uiso 1 1 calc R U . . .
C47 C 0.3054(3) 0.2859(3) 0.6077(3) 0.0255(14) Uani 1 1 d . . . . .
C48 C 0.2564(3) 0.2917(3) 0.6362(3) 0.0283(15) Uani 1 1 d . . . . .
C49 C 0.2484(4) 0.3538(3) 0.6604(3) 0.0342(16) Uani 1 1 d . . . . .
H49 H 0.215163 0.358294 0.680448 0.041 Uiso 1 1 calc R U . . .
C50 C 0.2878(4) 0.4101(3) 0.6563(4) 0.0349(17) Uani 1 1 d . . . . .
C51 C 0.3368(4) 0.4025(3) 0.6281(3) 0.0313(16) Uani 1 1 d . . . . .
H51 H 0.364312 0.440407 0.625618 0.038 Uiso 1 1 calc R U . . .
C52 C 0.3473(3) 0.3403(3) 0.6027(3) 0.0251(14) Uani 1 1 d . . . . .
C53 C 0.2766(4) 0.4795(3) 0.6806(4) 0.0444(19) Uani 1 1 d . . . . .
C54A C 0.2550(9) 0.5313(6) 0.6225(6) 0.047(4) Uiso 0.64(2) 1 d . . P A 1
H54A H 0.209698 0.516380 0.583663 0.071 Uiso 0.64(2) 1 calc R U P A 1
H54B H 0.245950 0.575009 0.638018 0.071 Uiso 0.64(2) 1 calc R U P A 1
H54C H 0.295585 0.535424 0.609278 0.071 Uiso 0.64(2) 1 calc R U P A 1
C55A C 0.2143(8) 0.4788(6) 0.7046(8) 0.055(4) Uiso 0.64(2) 1 d . . P A 1
H55A H 0.167298 0.464545 0.667250 0.082 Uiso 0.64(2) 1 calc R U P A 1
H55B H 0.227766 0.447392 0.742446 0.082 Uiso 0.64(2) 1 calc R U P A 1
H55C H 0.208472 0.523895 0.719286 0.082 Uiso 0.64(2) 1 calc R U P A 1
C56A C 0.3446(7) 0.5012(7) 0.7394(7) 0.044(4) Uiso 0.64(2) 1 d . . P A 1
H56A H 0.336375 0.545543 0.754108 0.066 Uiso 0.64(2) 1 calc R U P A 1
H56B H 0.356679 0.468928 0.776294 0.066 Uiso 0.64(2) 1 calc R U P A 1
H56C H 0.385855 0.503578 0.726865 0.066 Uiso 0.64(2) 1 calc R U P A 1
C54B C 0.2190(15) 0.5180(11) 0.6249(11) 0.048(7) Uiso 0.36(2) 1 d . . P A 2
H54D H 0.231035 0.519371 0.586346 0.072 Uiso 0.36(2) 1 calc R U P A 2
H54E H 0.170438 0.496426 0.611203 0.072 Uiso 0.36(2) 1 calc R U P A 2
H54F H 0.217109 0.563850 0.640206 0.072 Uiso 0.36(2) 1 calc R U P A 2
C55B C 0.3521(13) 0.5181(13) 0.7145(16) 0.056(7) Uiso 0.36(2) 1 d . . P A 2
H55D H 0.388673 0.490824 0.750999 0.083 Uiso 0.36(2) 1 calc R U P A 2
H55E H 0.370449 0.527226 0.680684 0.083 Uiso 0.36(2) 1 calc R U P A 2
H55F H 0.344677 0.560639 0.733036 0.083 Uiso 0.36(2) 1 calc R U P A 2
C56B C 0.263(2) 0.4749(16) 0.742(2) 0.094(12) Uiso 0.36(2) 1 d . . P A 2
H56D H 0.302357 0.448837 0.776871 0.141 Uiso 0.36(2) 1 calc R U P A 2
H56E H 0.261292 0.520063 0.758724 0.141 Uiso 0.36(2) 1 calc R U P A 2
H56F H 0.214621 0.452639 0.729720 0.141 Uiso 0.36(2) 1 calc R U P A 2
C57 C 0.3971(3) 0.3316(3) 0.5682(3) 0.0262(14) Uani 1 1 d . . . . .
H57A H 0.424580 0.373953 0.572406 0.031 Uiso 1 1 calc R U . . .
H57B H 0.365598 0.323496 0.519493 0.031 Uiso 1 1 calc R U . . .
C58 C 0.4402(3) 0.2106(3) 0.5648(3) 0.0224(14) Uani 1 1 d . . . . .
C59 C 0.4529(3) 0.2746(3) 0.5960(3) 0.0224(14) Uani 1 1 d . . . . .
C60 C 0.5181(3) 0.2857(3) 0.6531(3) 0.0272(15) Uani 1 1 d . . . . .
H60 H 0.527524 0.329406 0.672273 0.033 Uiso 1 1 calc R U . . .
C61 C 0.5715(3) 0.2353(3) 0.6845(3) 0.0299(15) Uani 1 1 d . . . . .
C62 C 0.5558(4) 0.1733(3) 0.6526(3) 0.0286(15) Uani 1 1 d . . . . .
H62 H 0.590349 0.137805 0.672422 0.034 Uiso 1 1 calc R U . . .
C63 C 0.4938(3) 0.1606(3) 0.5948(3) 0.0253(14) Uani 1 1 d . . . . .
C64 C 0.6416(4) 0.2453(3) 0.7486(4) 0.0428(19) Uani 1 1 d . . . . .
C65 C 0.6327(4) 0.2083(4) 0.8072(4) 0.053(2) Uani 1 1 d . . . . .
H65A H 0.678067 0.214325 0.849465 0.080 Uiso 1 1 calc R U . . .
H65B H 0.590147 0.227059 0.812248 0.080 Uiso 1 1 calc R U . . .
H65C H 0.624445 0.160363 0.796716 0.080 Uiso 1 1 calc R U . . .
C66 C 0.6560(4) 0.3201(4) 0.7690(5) 0.063(3) Uani 1 1 d . . . . .
H66A H 0.702139 0.324240 0.810938 0.094 Uiso 1 1 calc R U . . .
H66B H 0.660799 0.345463 0.732998 0.094 Uiso 1 1 calc R U . . .
H66C H 0.614369 0.337980 0.776105 0.094 Uiso 1 1 calc R U . . .
C67 C 0.7101(4) 0.2178(3) 0.7437(4) 0.0445(19) Uani 1 1 d . . . . .
H67A H 0.754178 0.225454 0.786603 0.067 Uiso 1 1 calc R U . . .
H67B H 0.703859 0.169544 0.734337 0.067 Uiso 1 1 calc R U . . .
H67C H 0.716306 0.240677 0.707169 0.067 Uiso 1 1 calc R U . . .
C68 C 0.4868(4) 0.0919(3) 0.5605(3) 0.0296(15) Uani 1 1 d . . . . .
H68A H 0.505403 0.056183 0.595219 0.035 Uiso 1 1 calc R U . . .
H68B H 0.433789 0.082527 0.530294 0.035 Uiso 1 1 calc R U . . .
C71 C 0.5030(4) 0.3028(3) 0.4692(4) 0.0323(16) Uani 1 1 d . . . . .
C72 C 0.4869(4) 0.3705(3) 0.4495(4) 0.051(2) Uani 1 1 d . . . . .
H72 H 0.438403 0.383748 0.417680 0.061 Uiso 1 1 calc R U . . .
C73 C 0.5431(5) 0.4168(4) 0.4775(4) 0.055(2) Uani 1 1 d . . . . .
H73 H 0.533046 0.462461 0.464131 0.067 Uiso 1 1 calc R U . . .
C74 C 0.6123(4) 0.3995(3) 0.5236(4) 0.049(2) Uani 1 1 d . . . . .
C75 C 0.6283(4) 0.3321(4) 0.5419(5) 0.057(2) Uani 1 1 d . . . . .
H75 H 0.676928 0.319079 0.573557 0.068 Uiso 1 1 calc R U . . .
C76 C 0.5731(4) 0.2848(4) 0.5139(4) 0.048(2) Uani 1 1 d . . . . .
H76 H 0.584080 0.238893 0.525769 0.057 Uiso 1 1 calc R U . . .
C77 C 0.6719(5) 0.4507(4) 0.5547(5) 0.066(3) Uani 1 1 d D . . . .
C81 C 0.1567(4) 0.3189(3) 0.4394(4) 0.0367(17) Uani 1 1 d . . . . .
C82 C 0.1813(4) 0.3859(3) 0.4500(4) 0.046(2) Uani 1 1 d . . . . .
H82 H 0.231990 0.396136 0.478150 0.055 Uiso 1 1 calc R U . . .
C83 C 0.1303(5) 0.4371(4) 0.4186(4) 0.055(2) Uani 1 1 d . . . . .
H83 H 0.146015 0.482598 0.426605 0.066 Uiso 1 1 calc R U . . .
C84 C 0.0587(5) 0.4224(4) 0.3770(5) 0.060(2) Uani 1 1 d . . . . .
C85 C 0.0334(5) 0.3555(5) 0.3673(5) 0.072(3) Uani 1 1 d . . . . .
H85 H -0.017469 0.345570 0.339227 0.086 Uiso 1 1 calc R U . . .
C86 C 0.0836(4) 0.3041(4) 0.3991(5) 0.058(2) Uani 1 1 d . . . . .
H86 H 0.067217 0.258829 0.393012 0.070 Uiso 1 1 calc R U . . .
N1 N 0.4457(3) 0.2561(2) 0.4422(3) 0.0246(12) Uani 1 1 d . . . . .
N2 N 0.2078(3) 0.2676(2) 0.4668(3) 0.0301(13) Uani 1 1 d . . . . .
O1 O 0.4231(2) 0.12119(18) 0.4209(2) 0.0258(10) Uani 1 1 d . . . . .
O2 O 0.4856(2) 0.19958(18) 0.3348(2) 0.0239(9) Uani 1 1 d . . . . .
O3 O 0.3355(2) 0.22064(18) 0.3265(2) 0.0246(10) Uani 1 1 d . . . . .
O4 O 0.2714(2) 0.20173(18) 0.4022(2) 0.0254(10) Uani 1 1 d . . . . .
O5 O 0.2193(2) 0.13188(18) 0.4868(2) 0.0281(10) Uani 1 1 d . . . . .
O6 O 0.1620(2) 0.2120(2) 0.5736(2) 0.0317(11) Uani 1 1 d . . . . .
O7 O 0.3137(2) 0.22555(18) 0.5829(2) 0.0243(10) Uani 1 1 d . . . . .
O8 O 0.3772(2) 0.19791(18) 0.5070(2) 0.0235(9) Uani 1 1 d . . . . .
C87 C 0.0035(6) 0.4801(5) 0.3391(6) 0.096(4) Uani 1 1 d D U . . .
F1A F 0.7351(6) 0.4289(6) 0.6007(6) 0.0885(15) Uiso 0.476(5) 1 d D U P B 1
F2A F 0.6864(7) 0.4815(6) 0.5083(6) 0.0885(15) Uiso 0.476(5) 1 d D U P B 1
F3A F 0.6485(6) 0.5007(6) 0.5813(6) 0.0885(15) Uiso 0.476(5) 1 d D U P B 1
F1B F 0.7350(6) 0.4343(5) 0.5516(6) 0.0885(15) Uiso 0.524(5) 1 d D U P B 2
F2B F 0.6525(6) 0.5105(5) 0.5265(6) 0.0885(15) Uiso 0.524(5) 1 d D U P B 2
F3B F 0.6933(6) 0.4575(6) 0.6209(5) 0.0885(15) Uiso 0.524(5) 1 d D U P B 2
F4A F 0.0348(5) 0.5213(5) 0.3112(5) 0.0973(16) Uiso 0.684(6) 1 d D U P C 1
F5A F -0.0071(5) 0.5170(5) 0.3834(5) 0.0973(16) Uiso 0.684(6) 1 d D U P C 1
F6A F -0.0602(5) 0.4568(4) 0.2962(5) 0.0973(16) Uiso 0.684(6) 1 d D U P C 1
F4B F -0.0290(11) 0.4721(10) 0.2757(8) 0.0973(16) Uiso 0.316(6) 1 d D U P C 2
F5B F 0.0362(10) 0.5399(8) 0.3553(10) 0.0973(16) Uiso 0.316(6) 1 d D U P C 2
F6B F -0.0445(10) 0.4821(10) 0.3672(10) 0.0973(16) Uiso 0.316(6) 1 d D U P C 2
V1 V 0.37848(6) 0.20000(5) 0.41586(5) 0.0235(3) Uani 1 1 d . . . . .
V2 V 0.26996(6) 0.20677(5) 0.49297(6) 0.0246(3) Uani 1 1 d . . . . .


_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 O1 1.352(7) . ?
C1 C6 1.391(9) . ?
C1 C2 1.394(9) . ?
C2 C3 1.393(8) . ?
C2 C68 1.504(8) . ?
C3 C4 1.388(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.407(9) . ?
C4 C7 1.510(9) . ?
C5 C6 1.370(9) . ?
C5 H5 0.9500 . ?
C6 C11 1.498(9) . ?
C7 C8 1.522(11) . ?
C7 C9 1.528(9) . ?
C7 C10 1.558(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O2 1.421(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.422(7) . ?
C12 C14 1.496(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O3 1.357(7) . ?
C13 C14 1.375(8) . ?
C13 C18 1.410(8) . ?
C14 C15 1.394(8) . ?
C15 C16 1.395(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(8) . ?
C16 C19 1.523(8) . ?
C17 C18 1.396(8) . ?
C17 H17 0.9500 . ?
C18 C23 1.504(8) . ?
C19 C20 1.504(9) . ?
C19 C21 1.524(9) . ?
C19 C22 1.556(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.516(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O4 1.380(7) . ?
C24 C29 1.386(9) . ?
C24 C25 1.414(9) . ?
C25 C26 1.376(9) . ?
C26 C27 1.383(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(10) . ?
C27 C30 1.530(11) . ?
C28 C29 1.389(9) . ?
C28 H28 0.9500 . ?
C29 C34 1.514(9) . ?
C30 C31 1.512(15) . ?
C30 C33 1.530(12) . ?
C30 C32 1.566(12) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.516(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.360(7) . ?
C35 C36 1.385(9) . ?
C35 C40 1.395(9) . ?
C36 C37 1.380(9) . ?
C37 C38 1.406(9) . ?
C37 H37 0.9500 . ?
C38 C39 1.385(10) . ?
C38 C41 1.528(9) . ?
C39 C40 1.371(9) . ?
C39 H39 0.9500 . ?
C40 C45 1.489(10) . ?
C41 C44 1.475(11) . ?
C41 C42 1.525(12) . ?
C41 C43 1.536(11) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O6 1.429(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O6 1.437(8) . ?
C46 C48 1.491(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O7 1.360(7) . ?
C47 C48 1.381(8) . ?
C47 C52 1.404(8) . ?
C48 C49 1.386(9) . ?
C49 C50 1.396(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.381(9) . ?
C50 C53 1.532(9) . ?
C51 C52 1.415(8) . ?
C51 H51 0.9500 . ?
C52 C57 1.503(8) . ?
C53 C56A 1.471(14) . ?
C53 C54B 1.48(2) . ?
C53 C56B 1.50(3) . ?
C53 C54A 1.550(14) . ?
C53 C55A 1.554(14) . ?
C53 C55B 1.56(3) . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9800 . ?
C55A H55B 0.9800 . ?
C55A H55C 0.9800 . ?
C56A H56A 0.9800 . ?
C56A H56B 0.9800 . ?
C56A H56C 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
C55B H55F 0.9800 . ?
C56B H56D 0.9800 . ?
C56B H56E 0.9800 . ?
C56B H56F 0.9800 . ?
C57 C59 1.519(8) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 O8 1.364(7) . ?
C58 C63 1.398(8) . ?
C58 C59 1.419(8) . ?
C59 C60 1.374(9) . ?
C60 C61 1.407(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.388(8) . ?
C61 C64 1.501(9) . ?
C62 C63 1.354(9) . ?
C62 H62 0.9500 . ?
C63 C68 1.541(8) . ?
C64 C67 1.522(9) . ?
C64 C66 1.548(9) . ?
C64 C65 1.563(11) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C71 C76 1.361(10) . ?
C71 N1 1.392(8) . ?
C71 C72 1.410(9) . ?
C72 C73 1.374(10) . ?
C72 H72 0.9500 . ?
C73 C74 1.353(11) . ?
C73 H73 0.9500 . ?
C74 C75 1.400(10) . ?
C74 C77 1.488(11) . ?
C75 C76 1.374(10) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 F1A 1.299(11) . ?
C77 F2B 1.320(11) . ?
C77 F2A 1.326(11) . ?
C77 F1B 1.334(11) . ?
C77 F3B 1.335(11) . ?
C77 F3A 1.341(11) . ?
C81 C86 1.367(10) . ?
C81 N2 1.382(8) . ?
C81 C82 1.407(10) . ?
C82 C83 1.391(10) . ?
C82 H82 0.9500 . ?
C83 C84 1.350(11) . ?
C83 H83 0.9500 . ?
C84 C85 1.411(12) . ?
C84 C87 1.557(13) . ?
C85 C86 1.389(11) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
N1 V1 1.645(5) . ?
N2 V2 1.649(5) . ?
O1 V1 1.786(4) . ?
O3 V1 1.815(4) . ?
O4 V2 2.015(4) . ?
O4 V1 2.028(4) . ?
O5 V2 1.775(4) . ?
O7 V2 1.818(4) . ?
O8 V1 2.019(4) . ?
O8 V2 2.036(4) . ?
C87 F4B 1.265(14) . ?
C87 F6A 1.294(11) . ?
C87 F5A 1.311(11) . ?
C87 F5B 1.330(14) . ?
C87 F4A 1.335(11) . ?
C87 F6B 1.353(14) . ?

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
O1 C1 C6 120.1(6) . . ?
O1 C1 C2 119.4(6) . . ?
C6 C1 C2 120.5(6) . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 C68 121.1(6) . . ?
C1 C2 C68 120.4(6) . . ?
C4 C3 C2 123.1(7) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C5 116.2(6) . . ?
C3 C4 C7 124.4(7) . . ?
C5 C4 C7 119.4(6) . . ?
C6 C5 C4 122.5(6) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 119.3(6) . . ?
C5 C6 C11 120.3(6) . . ?
C1 C6 C11 120.3(6) . . ?
C4 C7 C8 112.5(6) . . ?
C4 C7 C9 111.5(6) . . ?
C8 C7 C9 108.1(6) . . ?
C4 C7 C10 108.4(6) . . ?
C8 C7 C10 108.7(7) . . ?
C9 C7 C10 107.6(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 C6 108.5(5) . . ?
O2 C11 H11A 110.0 . . ?
C6 C11 H11A 110.0 . . ?
O2 C11 H11B 110.0 . . ?
C6 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
O2 C12 C14 107.3(5) . . ?
O2 C12 H12A 110.3 . . ?
C14 C12 H12A 110.3 . . ?
O2 C12 H12B 110.3 . . ?
C14 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
O3 C13 C14 119.4(5) . . ?
O3 C13 C18 118.3(5) . . ?
C14 C13 C18 122.2(5) . . ?
C13 C14 C15 118.4(5) . . ?
C13 C14 C12 119.6(5) . . ?
C15 C14 C12 122.0(5) . . ?
C14 C15 C16 122.1(6) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C17 C16 C15 117.4(5) . . ?
C17 C16 C19 121.8(5) . . ?
C15 C16 C19 120.7(5) . . ?
C16 C17 C18 123.0(5) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C17 C18 C13 116.8(5) . . ?
C17 C18 C23 123.0(5) . . ?
C13 C18 C23 120.2(5) . . ?
C20 C19 C16 112.7(5) . . ?
C20 C19 C21 108.5(6) . . ?
C16 C19 C21 110.6(5) . . ?
C20 C19 C22 108.6(5) . . ?
C16 C19 C22 108.0(5) . . ?
C21 C19 C22 108.3(5) . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 C25 114.3(5) . . ?
C18 C23 H23A 108.7 . . ?
C25 C23 H23A 108.7 . . ?
C18 C23 H23B 108.7 . . ?
C25 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
O4 C24 C29 119.4(5) . . ?
O4 C24 C25 120.1(5) . . ?
C29 C24 C25 120.5(6) . . ?
C26 C25 C24 118.1(6) . . ?
C26 C25 C23 119.6(6) . . ?
C24 C25 C23 122.3(6) . . ?
C25 C26 C27 123.4(6) . . ?
C25 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C26 C27 C28 116.6(7) . . ?
C26 C27 C30 123.9(7) . . ?
C28 C27 C30 119.5(7) . . ?
C29 C28 C27 122.8(7) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C24 C29 C28 118.5(6) . . ?
C24 C29 C34 123.5(6) . . ?
C28 C29 C34 117.9(6) . . ?
C31 C30 C33 109.8(9) . . ?
C31 C30 C27 109.8(8) . . ?
C33 C30 C27 109.7(7) . . ?
C31 C30 C32 110.2(8) . . ?
C33 C30 C32 107.1(8) . . ?
C27 C30 C32 110.2(7) . . ?
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 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 C36 110.7(5) . . ?
C29 C34 H34A 109.5 . . ?
C36 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
C36 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
O5 C35 C36 119.7(6) . . ?
O5 C35 C40 119.3(6) . . ?
C36 C35 C40 121.0(6) . . ?
C37 C36 C35 118.5(6) . . ?
C37 C36 C34 121.3(6) . . ?
C35 C36 C34 120.2(6) . . ?
C36 C37 C38 122.0(7) . . ?
C36 C37 H37 119.0 . . ?
C38 C37 H37 119.0 . . ?
C39 C38 C37 117.3(6) . . ?
C39 C38 C41 122.4(7) . . ?
C37 C38 C41 120.3(7) . . ?
C40 C39 C38 122.3(7) . . ?
C40 C39 H39 118.9 . . ?
C38 C39 H39 118.9 . . ?
C39 C40 C35 118.9(6) . . ?
C39 C40 C45 121.9(6) . . ?
C35 C40 C45 119.2(6) . . ?
C44 C41 C42 108.6(7) . . ?
C44 C41 C38 113.7(7) . . ?
C42 C41 C38 109.9(6) . . ?
C44 C41 C43 108.7(7) . . ?
C42 C41 C43 106.6(8) . . ?
C38 C41 C43 109.1(6) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O6 C45 C40 109.2(5) . . ?
O6 C45 H45A 109.8 . . ?
C40 C45 H45A 109.8 . . ?
O6 C45 H45B 109.8 . . ?
C40 C45 H45B 109.8 . . ?
H45A C45 H45B 108.3 . . ?
O6 C46 C48 109.1(5) . . ?
O6 C46 H46A 109.9 . . ?
C48 C46 H46A 109.9 . . ?
O6 C46 H46B 109.9 . . ?
C48 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
O7 C47 C48 119.5(5) . . ?
O7 C47 C52 117.9(5) . . ?
C48 C47 C52 122.6(5) . . ?
C47 C48 C49 118.3(6) . . ?
C47 C48 C46 119.6(5) . . ?
C49 C48 C46 122.1(6) . . ?
C48 C49 C50 122.0(6) . . ?
C48 C49 H49 119.0 . . ?
C50 C49 H49 119.0 . . ?
C51 C50 C49 118.2(6) . . ?
C51 C50 C53 119.8(6) . . ?
C49 C50 C53 122.0(6) . . ?
C50 C51 C52 122.2(6) . . ?
C50 C51 H51 118.9 . . ?
C52 C51 H51 118.9 . . ?
C47 C52 C51 116.6(5) . . ?
C47 C52 C57 120.1(5) . . ?
C51 C52 C57 123.2(5) . . ?
C54B C53 C56B 113.1(17) . . ?
C56A C53 C50 110.6(7) . . ?
C54B C53 C50 111.1(10) . . ?
C56B C53 C50 111.8(14) . . ?
C56A C53 C54A 110.2(9) . . ?
C50 C53 C54A 110.2(7) . . ?
C56A C53 C55A 105.7(9) . . ?
C50 C53 C55A 111.8(7) . . ?
C54A C53 C55A 108.2(8) . . ?
C54B C53 C55B 112.2(14) . . ?
C56B C53 C55B 97.2(17) . . ?
C50 C53 C55B 110.7(10) . . ?
C53 C54A H54A 109.5 . . ?
C53 C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53 C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53 C55A H55A 109.5 . . ?
C53 C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C53 C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
C53 C56A H56A 109.5 . . ?
C53 C56A H56B 109.5 . . ?
H56A C56A H56B 109.5 . . ?
C53 C56A H56C 109.5 . . ?
H56A C56A H56C 109.5 . . ?
H56B C56A H56C 109.5 . . ?
C53 C54B H54D 109.5 . . ?
C53 C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53 C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C53 C55B H55D 109.5 . . ?
C53 C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C53 C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
C53 C56B H56D 109.5 . . ?
C53 C56B H56E 109.5 . . ?
H56D C56B H56E 109.5 . . ?
C53 C56B H56F 109.5 . . ?
H56D C56B H56F 109.5 . . ?
H56E C56B H56F 109.5 . . ?
C52 C57 C59 114.5(5) . . ?
C52 C57 H57A 108.6 . . ?
C59 C57 H57A 108.6 . . ?
C52 C57 H57B 108.6 . . ?
C59 C57 H57B 108.6 . . ?
H57A C57 H57B 107.6 . . ?
O8 C58 C63 120.7(5) . . ?
O8 C58 C59 120.9(5) . . ?
C63 C58 C59 118.4(6) . . ?
C60 C59 C58 118.9(5) . . ?
C60 C59 C57 118.9(5) . . ?
C58 C59 C57 122.3(5) . . ?
C59 C60 C61 123.1(5) . . ?
C59 C60 H60 118.5 . . ?
C61 C60 H60 118.5 . . ?
C62 C61 C60 115.7(6) . . ?
C62 C61 C64 120.2(6) . . ?
C60 C61 C64 124.1(6) . . ?
C63 C62 C61 123.5(6) . . ?
C63 C62 H62 118.2 . . ?
C61 C62 H62 118.2 . . ?
C62 C63 C58 120.4(5) . . ?
C62 C63 C68 118.4(5) . . ?
C58 C63 C68 121.0(6) . . ?
C61 C64 C67 112.6(6) . . ?
C61 C64 C66 112.3(6) . . ?
C67 C64 C66 108.0(6) . . ?
C61 C64 C65 108.4(6) . . ?
C67 C64 C65 108.7(6) . . ?
C66 C64 C65 106.7(7) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C2 C68 C63 110.1(5) . . ?
C2 C68 H68A 109.6 . . ?
C63 C68 H68A 109.6 . . ?
C2 C68 H68B 109.6 . . ?
C63 C68 H68B 109.6 . . ?
H68A C68 H68B 108.2 . . ?
C76 C71 N1 121.7(6) . . ?
C76 C71 C72 119.9(6) . . ?
N1 C71 C72 118.4(6) . . ?
C73 C72 C71 118.2(7) . . ?
C73 C72 H72 120.9 . . ?
C71 C72 H72 120.9 . . ?
C74 C73 C72 122.1(7) . . ?
C74 C73 H73 118.9 . . ?
C72 C73 H73 118.9 . . ?
C73 C74 C75 119.3(7) . . ?
C73 C74 C77 121.3(7) . . ?
C75 C74 C77 119.4(7) . . ?
C76 C75 C74 119.5(7) . . ?
C76 C75 H75 120.2 . . ?
C74 C75 H75 120.2 . . ?
C71 C76 C75 120.8(7) . . ?
C71 C76 H76 119.6 . . ?
C75 C76 H76 119.6 . . ?
F1A C77 F2A 106.9(9) . . ?
F2B C77 F1B 106.7(8) . . ?
F2B C77 F3B 108.0(8) . . ?
F1B C77 F3B 103.0(9) . . ?
F1A C77 F3A 108.3(10) . . ?
F2A C77 F3A 103.2(8) . . ?
F1A C77 C74 115.9(8) . . ?
F2B C77 C74 113.1(8) . . ?
F2A C77 C74 111.4(9) . . ?
F1B C77 C74 113.1(8) . . ?
F3B C77 C74 112.2(8) . . ?
F3A C77 C74 110.3(8) . . ?
C86 C81 N2 119.9(6) . . ?
C86 C81 C82 120.5(6) . . ?
N2 C81 C82 119.5(6) . . ?
C83 C82 C81 119.2(7) . . ?
C83 C82 H82 120.4 . . ?
C81 C82 H82 120.4 . . ?
C84 C83 C82 120.3(8) . . ?
C84 C83 H83 119.8 . . ?
C82 C83 H83 119.8 . . ?
C83 C84 C85 120.8(7) . . ?
C83 C84 C87 119.6(8) . . ?
C85 C84 C87 119.6(8) . . ?
C86 C85 C84 119.2(8) . . ?
C86 C85 H85 120.4 . . ?
C84 C85 H85 120.4 . . ?
C81 C86 C85 119.9(8) . . ?
C81 C86 H86 120.0 . . ?
C85 C86 H86 120.0 . . ?
C71 N1 V1 175.9(5) . . ?
C81 N2 V2 174.5(5) . . ?
C1 O1 V1 127.2(3) . . ?
C11 O2 C12 111.6(4) . . ?
C13 O3 V1 123.8(4) . . ?
C24 O4 V2 119.1(3) . . ?
C24 O4 V1 128.8(4) . . ?
V2 O4 V1 109.14(19) . . ?
C35 O5 V2 130.6(4) . . ?
C45 O6 C46 112.8(5) . . ?
C47 O7 V2 122.3(4) . . ?
C58 O8 V1 120.9(3) . . ?
C58 O8 V2 127.2(3) . . ?
V1 O8 V2 108.65(19) . . ?
F6A C87 F5A 108.3(9) . . ?
F4B C87 F5B 111.2(13) . . ?
F6A C87 F4A 113.3(11) . . ?
F5A C87 F4A 105.0(9) . . ?
F4B C87 F6B 112.6(13) . . ?
F5B C87 F6B 102.4(11) . . ?
F4B C87 C84 113.5(12) . . ?
F6A C87 C84 111.4(9) . . ?
F5A C87 C84 108.9(10) . . ?
F5B C87 C84 111.6(12) . . ?
F4A C87 C84 109.6(8) . . ?
F6B C87 C84 104.8(12) . . ?
N1 V1 O1 105.5(2) . . ?
N1 V1 O3 98.8(2) . . ?
O1 V1 O3 104.60(18) . . ?
N1 V1 O8 91.6(2) . . ?
O1 V1 O8 98.31(18) . . ?
O3 V1 O8 151.16(17) . . ?
N1 V1 O4 133.4(2) . . ?
O1 V1 O4 119.39(17) . . ?
O3 V1 O4 82.49(17) . . ?
O8 V1 O4 70.99(16) . . ?
N2 V2 O5 105.9(2) . . ?
N2 V2 O7 99.0(2) . . ?
O5 V2 O7 103.95(19) . . ?
N2 V2 O4 91.6(2) . . ?
O5 V2 O4 97.97(18) . . ?
O7 V2 O4 151.87(17) . . ?
N2 V2 O8 134.4(2) . . ?
O5 V2 O8 117.79(17) . . ?
O7 V2 O8 83.26(17) . . ?
O4 V2 O8 70.92(16) . . ?

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
O1 C1 C2 C3 -176.4(5) . . . . ?
C6 C1 C2 C3 2.9(8) . . . . ?
O1 C1 C2 C68 -3.6(7) . . . . ?
C6 C1 C2 C68 175.6(5) . . . . ?
C1 C2 C3 C4 1.2(8) . . . . ?
C68 C2 C3 C4 -171.5(5) . . . . ?
C2 C3 C4 C5 -3.8(8) . . . . ?
C2 C3 C4 C7 174.0(5) . . . . ?
C3 C4 C5 C6 2.5(8) . . . . ?
C7 C4 C5 C6 -175.4(5) . . . . ?
C4 C5 C6 C1 1.4(8) . . . . ?
C4 C5 C6 C11 177.9(5) . . . . ?
O1 C1 C6 C5 175.1(5) . . . . ?
C2 C1 C6 C5 -4.1(8) . . . . ?
O1 C1 C6 C11 -1.5(8) . . . . ?
C2 C1 C6 C11 179.3(5) . . . . ?
C3 C4 C7 C8 3.3(9) . . . . ?
C5 C4 C7 C8 -179.1(6) . . . . ?
C3 C4 C7 C9 124.9(7) . . . . ?
C5 C4 C7 C9 -57.4(8) . . . . ?
C3 C4 C7 C10 -116.9(7) . . . . ?
C5 C4 C7 C10 60.8(8) . . . . ?
C5 C6 C11 O2 -101.3(6) . . . . ?
C1 C6 C11 O2 75.2(6) . . . . ?
O3 C13 C14 C15 179.3(5) . . . . ?
C18 C13 C14 C15 -2.9(9) . . . . ?
O3 C13 C14 C12 0.9(9) . . . . ?
C18 C13 C14 C12 178.7(6) . . . . ?
O2 C12 C14 C13 -69.6(7) . . . . ?
O2 C12 C14 C15 112.0(6) . . . . ?
C13 C14 C15 C16 2.9(10) . . . . ?
C12 C14 C15 C16 -178.7(6) . . . . ?
C14 C15 C16 C17 -1.8(10) . . . . ?
C14 C15 C16 C19 175.8(6) . . . . ?
C15 C16 C17 C18 0.7(10) . . . . ?
C19 C16 C17 C18 -176.9(6) . . . . ?
C16 C17 C18 C13 -0.7(9) . . . . ?
C16 C17 C18 C23 177.3(6) . . . . ?
O3 C13 C18 C17 179.7(5) . . . . ?
C14 C13 C18 C17 1.8(9) . . . . ?
O3 C13 C18 C23 1.6(8) . . . . ?
C14 C13 C18 C23 -176.2(6) . . . . ?
C17 C16 C19 C20 -165.4(6) . . . . ?
C15 C16 C19 C20 17.1(9) . . . . ?
C17 C16 C19 C21 -43.8(9) . . . . ?
C15 C16 C19 C21 138.8(6) . . . . ?
C17 C16 C19 C22 74.6(8) . . . . ?
C15 C16 C19 C22 -102.9(7) . . . . ?
C17 C18 C23 C25 126.8(6) . . . . ?
C13 C18 C23 C25 -55.3(8) . . . . ?
O4 C24 C25 C26 -176.7(6) . . . . ?
C29 C24 C25 C26 2.6(9) . . . . ?
O4 C24 C25 C23 2.3(9) . . . . ?
C29 C24 C25 C23 -178.4(6) . . . . ?
C18 C23 C25 C26 -83.8(7) . . . . ?
C18 C23 C25 C24 97.3(7) . . . . ?
C24 C25 C26 C27 -1.9(10) . . . . ?
C23 C25 C26 C27 179.1(6) . . . . ?
C25 C26 C27 C28 -0.4(11) . . . . ?
C25 C26 C27 C30 -179.1(8) . . . . ?
C26 C27 C28 C29 2.2(11) . . . . ?
C30 C27 C28 C29 -179.0(8) . . . . ?
O4 C24 C29 C28 178.3(6) . . . . ?
C25 C24 C29 C28 -0.9(10) . . . . ?
O4 C24 C29 C34 2.0(9) . . . . ?
C25 C24 C29 C34 -177.2(6) . . . . ?
C27 C28 C29 C24 -1.5(11) . . . . ?
C27 C28 C29 C34 175.0(7) . . . . ?
C26 C27 C30 C31 106.9(9) . . . . ?
C28 C27 C30 C31 -71.8(9) . . . . ?
C26 C27 C30 C33 -132.4(9) . . . . ?
C28 C27 C30 C33 49.0(12) . . . . ?
C26 C27 C30 C32 -14.7(12) . . . . ?
C28 C27 C30 C32 166.6(8) . . . . ?
C24 C29 C34 C36 98.1(7) . . . . ?
C28 C29 C34 C36 -78.2(8) . . . . ?
O5 C35 C36 C37 178.3(5) . . . . ?
C40 C35 C36 C37 -0.5(8) . . . . ?
O5 C35 C36 C34 -4.3(8) . . . . ?
C40 C35 C36 C34 176.8(5) . . . . ?
C29 C34 C36 C37 88.5(7) . . . . ?
C29 C34 C36 C35 -88.7(7) . . . . ?
C35 C36 C37 C38 1.2(9) . . . . ?
C34 C36 C37 C38 -176.1(5) . . . . ?
C36 C37 C38 C39 -1.3(9) . . . . ?
C36 C37 C38 C41 179.1(6) . . . . ?
C37 C38 C39 C40 0.8(9) . . . . ?
C41 C38 C39 C40 -179.7(6) . . . . ?
C38 C39 C40 C35 -0.2(9) . . . . ?
C38 C39 C40 C45 179.4(6) . . . . ?
O5 C35 C40 C39 -178.9(5) . . . . ?
C36 C35 C40 C39 0.0(8) . . . . ?
O5 C35 C40 C45 1.5(8) . . . . ?
C36 C35 C40 C45 -179.6(5) . . . . ?
C39 C38 C41 C44 0.7(10) . . . . ?
C37 C38 C41 C44 -179.7(7) . . . . ?
C39 C38 C41 C42 122.7(8) . . . . ?
C37 C38 C41 C42 -57.8(9) . . . . ?
C39 C38 C41 C43 -120.8(8) . . . . ?
C37 C38 C41 C43 58.7(9) . . . . ?
C39 C40 C45 O6 -106.1(6) . . . . ?
C35 C40 C45 O6 73.5(7) . . . . ?
O7 C47 C48 C49 -179.3(6) . . . . ?
C52 C47 C48 C49 0.2(10) . . . . ?
O7 C47 C48 C46 1.2(9) . . . . ?
C52 C47 C48 C46 -179.2(6) . . . . ?
O6 C46 C48 C47 -68.1(8) . . . . ?
O6 C46 C48 C49 112.5(7) . . . . ?
C47 C48 C49 C50 0.5(10) . . . . ?
C46 C48 C49 C50 179.9(6) . . . . ?
C48 C49 C50 C51 -1.0(10) . . . . ?
C48 C49 C50 C53 177.5(7) . . . . ?
C49 C50 C51 C52 0.8(10) . . . . ?
C53 C50 C51 C52 -177.7(6) . . . . ?
O7 C47 C52 C51 179.2(5) . . . . ?
C48 C47 C52 C51 -0.4(9) . . . . ?
O7 C47 C52 C57 2.4(9) . . . . ?
C48 C47 C52 C57 -177.2(6) . . . . ?
C50 C51 C52 C47 -0.2(10) . . . . ?
C50 C51 C52 C57 176.5(6) . . . . ?
C51 C50 C53 C56A -67.6(11) . . . . ?
C49 C50 C53 C56A 113.9(10) . . . . ?
C51 C50 C53 C54B 86.7(15) . . . . ?
C49 C50 C53 C54B -91.7(15) . . . . ?
C51 C50 C53 C56B -145.9(19) . . . . ?
C49 C50 C53 C56B 36(2) . . . . ?
C51 C50 C53 C54A 54.5(10) . . . . ?
C49 C50 C53 C54A -124.0(9) . . . . ?
C51 C50 C53 C55A 174.8(9) . . . . ?
C49 C50 C53 C55A -3.7(11) . . . . ?
C51 C50 C53 C55B -38.7(16) . . . . ?
C49 C50 C53 C55B 142.9(15) . . . . ?
C47 C52 C57 C59 -54.4(8) . . . . ?
C51 C52 C57 C59 129.0(6) . . . . ?
O8 C58 C59 C60 -178.2(5) . . . . ?
C63 C58 C59 C60 2.0(9) . . . . ?
O8 C58 C59 C57 1.5(9) . . . . ?
C63 C58 C59 C57 -178.4(5) . . . . ?
C52 C57 C59 C60 -82.2(7) . . . . ?
C52 C57 C59 C58 98.1(7) . . . . ?
C58 C59 C60 C61 -3.5(9) . . . . ?
C57 C59 C60 C61 176.8(6) . . . . ?
C59 C60 C61 C62 2.3(9) . . . . ?
C59 C60 C61 C64 -177.2(6) . . . . ?
C60 C61 C62 C63 0.4(9) . . . . ?
C64 C61 C62 C63 180.0(6) . . . . ?
C61 C62 C63 C58 -1.8(10) . . . . ?
C61 C62 C63 C68 173.6(6) . . . . ?
O8 C58 C63 C62 -179.3(5) . . . . ?
C59 C58 C63 C62 0.6(9) . . . . ?
O8 C58 C63 C68 5.4(9) . . . . ?
C59 C58 C63 C68 -174.7(5) . . . . ?
C62 C61 C64 C67 47.6(9) . . . . ?
C60 C61 C64 C67 -132.9(7) . . . . ?
C62 C61 C64 C66 169.7(7) . . . . ?
C60 C61 C64 C66 -10.8(10) . . . . ?
C62 C61 C64 C65 -72.7(8) . . . . ?
C60 C61 C64 C65 106.8(7) . . . . ?
C3 C2 C68 C63 79.6(7) . . . . ?
C1 C2 C68 C63 -92.9(6) . . . . ?
C62 C63 C68 C2 -80.3(7) . . . . ?
C58 C63 C68 C2 95.2(7) . . . . ?
C76 C71 C72 C73 -1.3(12) . . . . ?
N1 C71 C72 C73 178.4(7) . . . . ?
C71 C72 C73 C74 -0.9(13) . . . . ?
C72 C73 C74 C75 2.2(14) . . . . ?
C72 C73 C74 C77 -178.4(8) . . . . ?
C73 C74 C75 C76 -1.3(13) . . . . ?
C77 C74 C75 C76 179.3(8) . . . . ?
N1 C71 C76 C75 -177.5(7) . . . . ?
C72 C71 C76 C75 2.1(12) . . . . ?
C74 C75 C76 C71 -0.9(13) . . . . ?
C73 C74 C77 F1A 176.7(10) . . . . ?
C75 C74 C77 F1A -3.9(13) . . . . ?
C73 C74 C77 F2B -7.9(13) . . . . ?
C75 C74 C77 F2B 171.5(9) . . . . ?
C73 C74 C77 F2A -60.9(12) . . . . ?
C75 C74 C77 F2A 118.6(10) . . . . ?
C73 C74 C77 F1B -129.4(10) . . . . ?
C75 C74 C77 F1B 50.0(12) . . . . ?
C73 C74 C77 F3B 114.5(10) . . . . ?
C75 C74 C77 F3B -66.1(11) . . . . ?
C73 C74 C77 F3A 53.2(12) . . . . ?
C75 C74 C77 F3A -127.4(10) . . . . ?
C86 C81 C82 C83 -0.4(11) . . . . ?
N2 C81 C82 C83 176.0(7) . . . . ?
C81 C82 C83 C84 -2.0(12) . . . . ?
C82 C83 C84 C85 3.3(14) . . . . ?
C82 C83 C84 C87 -176.5(8) . . . . ?
C83 C84 C85 C86 -2.3(14) . . . . ?
C87 C84 C85 C86 177.5(9) . . . . ?
N2 C81 C86 C85 -175.0(8) . . . . ?
C82 C81 C86 C85 1.4(13) . . . . ?
C84 C85 C86 C81 -0.1(14) . . . . ?
C6 C1 O1 V1 -91.5(6) . . . . ?
C2 C1 O1 V1 87.8(6) . . . . ?
C6 C11 O2 C12 -164.3(5) . . . . ?
C14 C12 O2 C11 155.9(5) . . . . ?
C14 C13 O3 V1 101.2(6) . . . . ?
C18 C13 O3 V1 -76.7(6) . . . . ?
C29 C24 O4 V2 -80.1(6) . . . . ?
C25 C24 O4 V2 99.2(6) . . . . ?
C29 C24 O4 V1 121.5(5) . . . . ?
C25 C24 O4 V1 -59.2(7) . . . . ?
C36 C35 O5 V2 86.7(6) . . . . ?
C40 C35 O5 V2 -94.4(6) . . . . ?
C40 C45 O6 C46 -167.0(5) . . . . ?
C48 C46 O6 C45 152.4(5) . . . . ?
C48 C47 O7 V2 101.9(6) . . . . ?
C52 C47 O7 V2 -77.6(6) . . . . ?
C63 C58 O8 V1 -80.7(6) . . . . ?
C59 C58 O8 V1 99.5(5) . . . . ?
C63 C58 O8 V2 121.9(5) . . . . ?
C59 C58 O8 V2 -57.9(7) . . . . ?
C83 C84 C87 F4B 125.0(14) . . . . ?
C85 C84 C87 F4B -54.8(15) . . . . ?
C83 C84 C87 F6A 173.2(9) . . . . ?
C85 C84 C87 F6A -6.6(14) . . . . ?
C83 C84 C87 F5A -67.4(12) . . . . ?
C85 C84 C87 F5A 112.8(10) . . . . ?
C83 C84 C87 F5B -1.6(15) . . . . ?
C85 C84 C87 F5B 178.6(12) . . . . ?
C83 C84 C87 F4A 47.0(13) . . . . ?
C85 C84 C87 F4A -132.8(10) . . . . ?
C83 C84 C87 F6B -111.7(13) . . . . ?
C85 C84 C87 F6B 68.5(14) . . . . ?
C1 O1 V1 N1 11.3(5) . . . . ?
C1 O1 V1 O3 114.9(5) . . . . ?
C1 O1 V1 O8 -82.7(5) . . . . ?
C1 O1 V1 O4 -155.5(5) . . . . ?
C13 O3 V1 N1 -16.8(5) . . . . ?
C13 O3 V1 O1 -125.4(4) . . . . ?
C13 O3 V1 O8 93.1(5) . . . . ?
C13 O3 V1 O4 116.1(4) . . . . ?
C35 O5 V2 N2 11.0(6) . . . . ?
C35 O5 V2 O7 114.8(5) . . . . ?
C35 O5 V2 O4 -83.0(5) . . . . ?
C35 O5 V2 O8 -155.6(5) . . . . ?
C47 O7 V2 N2 -16.7(5) . . . . ?
C47 O7 V2 O5 -125.7(4) . . . . ?
C47 O7 V2 O4 94.1(5) . . . . ?
C47 O7 V2 O8 117.2(4) . . . . ?

_refine_diff_density_max         1.140
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.096

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1998551'
loop_
_audit_author_name
_audit_author_address
'Kai Chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;

_vrf_PLAT201_shelx               
;
RESPONSE: small-scale disorder was modelled using isotropic 
displacement parameters.     
;


_vrf_PLAT213_shelx               
;
RESPONSE: The unbound acetonitrile molecules are poorly located
This results in slightly odd displacement parameters for some
atoms.     
;




_vrf_PLAT241_shelx               
;
RESPONSE: The unbound acetonitrile molecules are poorly located
This results in slightly odd displacement parameters for some
atoms.     
;



_vrf_PLAT220_shelx               
;
RESPONSE: The central atoms of the oxacalixarene have relatively
small displacement parameters. Those of the peripheral methyl 
groups are much larger as expected chemically.   
;


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C82 H96 N2 O8 V2), 7CH3CN, 0.5CH2Cl2
;

_chemical_formula_sum            'C355 H421 Cl2 N21 O32 V8'
_chemical_formula_weight         5972.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   19.7899(3)
_cell_length_b                   20.6775(3)
_cell_length_c                   22.7696(5)
_cell_angle_alpha                69.271(2)
_cell_angle_beta                 76.567(2)
_cell_angle_gamma                78.6270(10)
_cell_volume                     8407.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    34621
_cell_measurement_theta_min      2.181
_cell_measurement_theta_max      27.483

_exptl_crystal_description       'flat fragment'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_F_000             3172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.294
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74421
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            110251
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.889
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             38573
_reflns_number_gt                24217
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1211P)²+17.9933P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         38573
_refine_ls_number_parameters     1863
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0881
_refine_ls_wR_factor_ref         0.2564
_refine_ls_wR_factor_gt          0.2230
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.018
_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_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
C1 C 0.47519(19) -0.01788(19) 0.23738(17) 0.0186(7) Uani 1 1 d . . . . .
C2 C 0.5303(2) -0.07091(19) 0.25283(18) 0.0207(8) Uani 1 1 d . . . . .
C3 C 0.5755(2) -0.0913(2) 0.20382(19) 0.0237(8) Uani 1 1 d . . . . .
H3 H 0.613549 -0.126817 0.213958 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5665(2) -0.0612(2) 0.14038(19) 0.0238(8) Uani 1 1 d . . . . .
C5 C 0.5111(2) -0.0082(2) 0.12658(19) 0.0226(8) Uani 1 1 d . . . . .
H5 H 0.504115 0.013130 0.083639 0.027 Uiso 1 1 calc R U . . .
C6 C 0.46536(19) 0.0144(2) 0.17448(18) 0.0199(8) Uani 1 1 d . . . . .
C7 C 0.5400(2) -0.1027(2) 0.32111(19) 0.0242(8) Uani 1 1 d . . . . .
H7A H 0.495853 -0.118911 0.348590 0.029 Uiso 1 1 calc R U . . .
H7B H 0.576872 -0.143345 0.325607 0.029 Uiso 1 1 calc R U . . .
C8 C 0.6186(2) -0.0861(2) 0.0887(2) 0.0312(9) Uani 1 1 d . . . . .
C9 C 0.6914(2) -0.0672(3) 0.0850(2) 0.0456(13) Uani 1 1 d . . . . .
H9A H 0.705491 -0.088609 0.126852 0.068 Uiso 1 1 calc R U . . .
H9B H 0.725510 -0.084577 0.053491 0.068 Uiso 1 1 calc R U . . .
H9C H 0.689372 -0.016451 0.072138 0.068 Uiso 1 1 calc R U . . .
C10 C 0.6212(3) -0.1652(3) 0.1064(2) 0.0440(12) Uani 1 1 d . . . . .
H10A H 0.634132 -0.188139 0.148707 0.066 Uiso 1 1 calc R U . . .
H10B H 0.575031 -0.176330 0.107148 0.066 Uiso 1 1 calc R U . . .
H10C H 0.655995 -0.181690 0.074821 0.066 Uiso 1 1 calc R U . . .
C11 C 0.5983(2) -0.0520(3) 0.0229(2) 0.0388(11) Uani 1 1 d . . . . .
H11A H 0.596378 -0.001305 0.010655 0.058 Uiso 1 1 calc R U . . .
H11B H 0.633278 -0.069088 -0.008270 0.058 Uiso 1 1 calc R U . . .
H11C H 0.552314 -0.063729 0.024057 0.058 Uiso 1 1 calc R U . . .
C12 C 0.40826(19) 0.0754(2) 0.15949(18) 0.0209(8) Uani 1 1 d . . . . .
H12A H 0.408542 0.092226 0.112972 0.025 Uiso 1 1 calc R U . . .
H12B H 0.419210 0.113834 0.170688 0.025 Uiso 1 1 calc R U . . .
C13 C 0.30234(19) 0.0759(2) 0.24959(18) 0.0202(8) Uani 1 1 d . . . . .
C14 C 0.3353(2) 0.0588(2) 0.19415(18) 0.0216(8) Uani 1 1 d . . . . .
C15 C 0.2997(2) 0.0241(2) 0.17062(19) 0.0235(8) Uani 1 1 d . . . . .
H15 H 0.322113 0.012112 0.133524 0.028 Uiso 1 1 calc R U . . .
C16 C 0.2327(2) 0.0063(2) 0.1991(2) 0.0272(9) Uani 1 1 d . . . . .
C17 C 0.2019(2) 0.0243(2) 0.2532(2) 0.0277(9) Uani 1 1 d . . . . .
H17 H 0.156184 0.012675 0.273650 0.033 Uiso 1 1 calc R U . . .
C18 C 0.2349(2) 0.0588(2) 0.27917(19) 0.0232(8) Uani 1 1 d . . . . .
C19 C 0.1968(2) -0.0321(3) 0.1706(2) 0.0341(10) Uani 1 1 d . . . . .
C20 C 0.1943(4) 0.0087(4) 0.1017(3) 0.073(2) Uani 1 1 d . . . . .
H20A H 0.241920 0.016386 0.078406 0.110 Uiso 1 1 calc R U . . .
H20B H 0.173880 -0.017340 0.083123 0.110 Uiso 1 1 calc R U . . .
H20C H 0.165579 0.053800 0.098635 0.110 Uiso 1 1 calc R U . . .
C21 C 0.2385(4) -0.1044(3) 0.1755(4) 0.0705(19) Uani 1 1 d . . . . .
H21A H 0.240195 -0.131141 0.220370 0.106 Uiso 1 1 calc R U . . .
H21B H 0.215623 -0.129179 0.157512 0.106 Uiso 1 1 calc R U . . .
H21C H 0.286265 -0.098975 0.151660 0.106 Uiso 1 1 calc R U . . .
C22 C 0.1229(3) -0.0444(5) 0.2074(4) 0.094(3) Uani 1 1 d . . . . .
H22A H 0.124927 -0.071036 0.252238 0.141 Uiso 1 1 calc R U . . .
H22B H 0.093978 0.000587 0.204528 0.141 Uiso 1 1 calc R U . . .
H22C H 0.102278 -0.070552 0.189016 0.141 Uiso 1 1 calc R U . . .
C23 C 0.1952(2) 0.0762(2) 0.3389(2) 0.0261(9) Uani 1 1 d . . . . .
H23A H 0.169619 0.036793 0.367703 0.031 Uiso 1 1 calc R U . . .
H23B H 0.229147 0.082212 0.361822 0.031 Uiso 1 1 calc R U . . .
C24 C 0.1641(2) 0.2061(2) 0.31412(19) 0.0246(8) Uani 1 1 d . . . . .
C25 C 0.1437(2) 0.1418(2) 0.3234(2) 0.0290(9) Uani 1 1 d . . . . .
C26 C 0.0754(2) 0.1415(3) 0.3152(2) 0.0346(10) Uani 1 1 d . . . . .
H26 H 0.059831 0.098144 0.322873 0.042 Uiso 1 1 calc R U . . .
C27 C 0.0292(2) 0.2035(3) 0.2961(2) 0.0398(11) Uani 1 1 d . . . . .
C28 C 0.0518(2) 0.2654(3) 0.2892(2) 0.0360(10) Uani 1 1 d . . . . .
H28 H 0.020842 0.307499 0.278016 0.043 Uiso 1 1 calc R U . . .
C29 C 0.1185(2) 0.2683(2) 0.2981(2) 0.0283(9) Uani 1 1 d . . . . .
C30 C -0.0436(3) 0.2013(3) 0.2831(3) 0.0565(16) Uani 1 1 d . . . . .
C31 C -0.0353(4) 0.1670(6) 0.2346(6) 0.135(5) Uani 1 1 d . . . . .
H31A H -0.006568 0.192871 0.195126 0.203 Uiso 1 1 calc R U . . .
H31B H -0.012466 0.119155 0.250279 0.203 Uiso 1 1 calc R U . . .
H31C H -0.081500 0.166261 0.226195 0.203 Uiso 1 1 calc R U . . .
C32 C -0.0873(4) 0.1650(5) 0.3457(5) 0.108(3) Uani 1 1 d . . . . .
H32A H -0.091003 0.189994 0.375889 0.162 Uiso 1 1 calc R U . . .
H32B H -0.134241 0.164194 0.338863 0.162 Uiso 1 1 calc R U . . .
H32C H -0.065206 0.117088 0.362948 0.162 Uiso 1 1 calc R U . . .
C33 C -0.0828(3) 0.2749(4) 0.2586(5) 0.091(3) Uani 1 1 d . . . . .
H33A H -0.088846 0.298627 0.290246 0.137 Uiso 1 1 calc R U . . .
H33B H -0.055704 0.301485 0.218357 0.137 Uiso 1 1 calc R U . . .
H33C H -0.128827 0.271602 0.251556 0.137 Uiso 1 1 calc R U . . .
C34 C 0.1422(2) 0.3358(2) 0.2891(2) 0.0306(9) Uani 1 1 d . . . . .
H34A H 0.101243 0.370334 0.295680 0.037 Uiso 1 1 calc R U . . .
H34B H 0.172363 0.329150 0.320434 0.037 Uiso 1 1 calc R U . . .
C35 C 0.2214(2) 0.4138(2) 0.2166(2) 0.0265(9) Uani 1 1 d . . . . .
H35A H 0.234906 0.408579 0.257458 0.032 Uiso 1 1 calc R U . . .
H35B H 0.193773 0.460103 0.201930 0.032 Uiso 1 1 calc R U . . .
C36 C 0.3370(2) 0.3513(2) 0.18307(17) 0.0210(8) Uani 1 1 d . . . . .
C37 C 0.2856(2) 0.4077(2) 0.16777(18) 0.0220(8) Uani 1 1 d . . . . .
C38 C 0.2957(2) 0.4570(2) 0.10734(19) 0.0258(8) Uani 1 1 d . . . . .
H38 H 0.261076 0.496158 0.096777 0.031 Uiso 1 1 calc R U . . .
C39 C 0.3553(2) 0.4508(2) 0.06158(19) 0.0263(9) Uani 1 1 d . . . . .
C40 C 0.4059(2) 0.3941(2) 0.07915(18) 0.0231(8) Uani 1 1 d . . . . .
H40 H 0.447076 0.389327 0.048984 0.028 Uiso 1 1 calc R U . . .
C41 C 0.3983(2) 0.3438(2) 0.13946(18) 0.0207(8) Uani 1 1 d . . . . .
C42 C 0.3608(2) 0.5049(2) -0.00578(19) 0.0289(9) Uani 1 1 d . . . . .
C43 C 0.3573(4) 0.5775(3) -0.0032(2) 0.0591(17) Uani 1 1 d . . . . .
H43A H 0.395551 0.579147 0.016708 0.089 Uiso 1 1 calc R U . . .
H43B H 0.361777 0.610816 -0.046613 0.089 Uiso 1 1 calc R U . . .
H43C H 0.312312 0.589651 0.021928 0.089 Uiso 1 1 calc R U . . .
C44 C 0.4299(3) 0.4903(3) -0.0493(2) 0.0593(17) Uani 1 1 d . . . . .
H44A H 0.433737 0.443357 -0.052006 0.089 Uiso 1 1 calc R U . . .
H44B H 0.430558 0.524649 -0.092070 0.089 Uiso 1 1 calc R U . . .
H44C H 0.469338 0.493457 -0.031712 0.089 Uiso 1 1 calc R U . . .
C45 C 0.3023(3) 0.5001(3) -0.0364(3) 0.0566(16) Uani 1 1 d . . . . .
H45A H 0.305730 0.452586 -0.037481 0.085 Uiso 1 1 calc R U . . .
H45B H 0.256908 0.511749 -0.011488 0.085 Uiso 1 1 calc R U . . .
H45C H 0.306373 0.532914 -0.080029 0.085 Uiso 1 1 calc R U . . .
C46 C 0.45245(19) 0.2801(2) 0.15763(17) 0.0197(7) Uani 1 1 d . . . . .
H46A H 0.492352 0.283636 0.121650 0.024 Uiso 1 1 calc R U . . .
H46B H 0.431225 0.237958 0.164409 0.024 Uiso 1 1 calc R U . . .
C47 C 0.45298(19) 0.22935(19) 0.27835(18) 0.0195(7) Uani 1 1 d . . . . .
C48 C 0.4800(2) 0.27156(19) 0.21768(17) 0.0194(7) Uani 1 1 d . . . . .
C49 C 0.5351(2) 0.3077(2) 0.21082(18) 0.0217(8) Uani 1 1 d . . . . .
H49 H 0.553906 0.335969 0.169365 0.026 Uiso 1 1 calc R U . . .
C50 C 0.5640(2) 0.30416(19) 0.26288(18) 0.0214(8) Uani 1 1 d . . . . .
C51 C 0.5328(2) 0.2652(2) 0.32242(18) 0.0221(8) Uani 1 1 d . . . . .
H51 H 0.549448 0.264140 0.358702 0.027 Uiso 1 1 calc R U . . .
C52 C 0.47784(19) 0.22701(19) 0.33197(17) 0.0190(7) Uani 1 1 d . . . . .
C53 C 0.6273(2) 0.3422(2) 0.2525(2) 0.0284(9) Uani 1 1 d . . . . .
C54 C 0.6023(3) 0.4208(2) 0.2354(2) 0.0404(11) Uani 1 1 d . . . . .
H54A H 0.580887 0.436504 0.197193 0.061 Uiso 1 1 calc R U . . .
H54B H 0.567806 0.429955 0.271012 0.061 Uiso 1 1 calc R U . . .
H54C H 0.642426 0.445957 0.227155 0.061 Uiso 1 1 calc R U . . .
C55 C 0.6839(2) 0.3271(3) 0.1983(2) 0.0378(11) Uani 1 1 d . . . . .
H55A H 0.664120 0.341855 0.159204 0.057 Uiso 1 1 calc R U . . .
H55B H 0.723311 0.352801 0.190979 0.057 Uiso 1 1 calc R U . . .
H55C H 0.700205 0.277007 0.210184 0.057 Uiso 1 1 calc R U . . .
C56 C 0.6605(3) 0.3183(3) 0.3120(2) 0.0446(13) Uani 1 1 d . . . . .
H56A H 0.676548 0.268230 0.323232 0.067 Uiso 1 1 calc R U . . .
H56B H 0.700470 0.343745 0.303583 0.067 Uiso 1 1 calc R U . . .
H56C H 0.625850 0.327743 0.347440 0.067 Uiso 1 1 calc R U . . .
C57 C 0.4513(2) 0.1816(2) 0.39934(17) 0.0217(8) Uani 1 1 d . . . . .
H57A H 0.444000 0.208408 0.429159 0.026 Uiso 1 1 calc R U . . .
H57B H 0.405802 0.167320 0.400952 0.026 Uiso 1 1 calc R U . . .
C58 C 0.4996(2) 0.0569(2) 0.40733(16) 0.0200(8) Uani 1 1 d . . . . .
C59 C 0.5039(2) 0.1172(2) 0.41954(17) 0.0209(8) Uani 1 1 d . . . . .
C60 C 0.5608(2) 0.1188(2) 0.44527(17) 0.0240(8) Uani 1 1 d . . . . .
H60 H 0.563685 0.159579 0.454243 0.029 Uiso 1 1 calc R U . . .
C61 C 0.6136(2) 0.0630(2) 0.45829(18) 0.0265(9) Uani 1 1 d . . . . .
C62 C 0.6068(2) 0.0028(2) 0.44607(18) 0.0257(9) Uani 1 1 d . . . . .
H62 H 0.641815 -0.036278 0.454874 0.031 Uiso 1 1 calc R U . . .
C63 C 0.5501(2) -0.0010(2) 0.42134(17) 0.0226(8) Uani 1 1 d . . . . .
C64 C 0.6789(2) 0.0694(2) 0.4806(2) 0.0344(10) Uani 1 1 d D . . . .
C65A C 0.7380(6) 0.0851(7) 0.4195(5) 0.0355(9) Uiso 0.383(6) 1 d D U P A 1
H65A H 0.720074 0.124037 0.385062 0.053 Uiso 0.383(6) 1 calc R U P A 1
H65B H 0.778426 0.097275 0.429561 0.053 Uiso 0.383(6) 1 calc R U P A 1
H65C H 0.752376 0.043637 0.405954 0.053 Uiso 0.383(6) 1 calc R U P A 1
C66A C 0.6680(6) 0.1413(5) 0.4985(6) 0.0355(9) Uiso 0.383(6) 1 d D U P A 1
H66A H 0.652037 0.180823 0.463368 0.053 Uiso 0.383(6) 1 calc R U P A 1
H66B H 0.632896 0.137417 0.537470 0.053 Uiso 0.383(6) 1 calc R U P A 1
H66C H 0.712530 0.148759 0.505449 0.053 Uiso 0.383(6) 1 calc R U P A 1
C67A C 0.7019(6) 0.0133(6) 0.5322(5) 0.0355(9) Uiso 0.383(6) 1 d D U P A 1
H67A H 0.743620 0.023587 0.541795 0.053 Uiso 0.383(6) 1 calc R U P A 1
H67B H 0.664661 0.006938 0.569856 0.053 Uiso 0.383(6) 1 calc R U P A 1
H67C H 0.713383 -0.029493 0.520659 0.053 Uiso 0.383(6) 1 calc R U P A 1
C66B C 0.6581(4) 0.0949(4) 0.5375(3) 0.0355(9) Uiso 0.617(6) 1 d D U P A 2
H66D H 0.626530 0.064462 0.571033 0.053 Uiso 0.617(6) 1 calc R U P A 2
H66E H 0.700038 0.094071 0.553808 0.053 Uiso 0.617(6) 1 calc R U P A 2
H66F H 0.634121 0.142619 0.524769 0.053 Uiso 0.617(6) 1 calc R U P A 2
C67B C 0.7200(4) -0.0080(4) 0.5084(4) 0.0355(9) Uiso 0.617(6) 1 d D U P A 2
H67D H 0.689072 -0.036420 0.544407 0.053 Uiso 0.617(6) 1 calc R U P A 2
H67E H 0.734020 -0.029705 0.474789 0.053 Uiso 0.617(6) 1 calc R U P A 2
H67F H 0.761730 -0.004494 0.522782 0.053 Uiso 0.617(6) 1 calc R U P A 2
C65B C 0.7260(4) 0.1104(4) 0.4273(3) 0.0355(9) Uiso 0.617(6) 1 d D U P A 2
H65D H 0.736748 0.090349 0.392585 0.053 Uiso 0.617(6) 1 calc R U P A 2
H65E H 0.703476 0.158505 0.412171 0.053 Uiso 0.617(6) 1 calc R U P A 2
H65F H 0.769394 0.109957 0.441210 0.053 Uiso 0.617(6) 1 calc R U P A 2
C68 C 0.5448(2) -0.0656(2) 0.40760(18) 0.0252(8) Uani 1 1 d . . . . .
H68A H 0.578592 -0.104541 0.428040 0.030 Uiso 1 1 calc R U . . .
H68B H 0.497033 -0.079175 0.424929 0.030 Uiso 1 1 calc R U . . .
C70 C 0.5863(2) 0.1028(2) 0.23682(18) 0.0224(8) Uani 1 1 d . . . . .
C71 C 0.6271(2) 0.1225(2) 0.2687(2) 0.0307(9) Uani 1 1 d . . . . .
H71 H 0.606593 0.132518 0.307118 0.037 Uiso 1 1 calc R U . . .
C72 C 0.6970(2) 0.1275(3) 0.2443(2) 0.0408(12) Uani 1 1 d . . . . .
H72 H 0.723975 0.142422 0.265426 0.049 Uiso 1 1 calc R U . . .
C73 C 0.7293(3) 0.1110(3) 0.1890(2) 0.0448(13) Uani 1 1 d . . . . .
C74 C 0.6882(3) 0.0905(3) 0.1588(2) 0.0463(13) Uani 1 1 d . . . . .
H74 H 0.709151 0.079396 0.120996 0.056 Uiso 1 1 calc R U . . .
C75 C 0.6177(2) 0.0857(2) 0.1818(2) 0.0327(10) Uani 1 1 d . . . . .
H75 H 0.590925 0.070842 0.160405 0.039 Uiso 1 1 calc R U . . .
C76 C 0.8064(3) 0.1144(5) 0.1641(4) 0.087(3) Uani 1 1 d . . . . .
H76A H 0.831506 0.067073 0.173329 0.130 Uiso 1 1 calc R U . . .
H76B H 0.823944 0.140321 0.184915 0.130 Uiso 1 1 calc R U . . .
H76C H 0.813999 0.138124 0.117903 0.130 Uiso 1 1 calc R U . . .
C77 C 0.2551(2) 0.2278(2) 0.13972(19) 0.0229(8) Uani 1 1 d . . . . .
C78 C 0.2957(2) 0.2514(2) 0.0791(2) 0.0282(9) Uani 1 1 d . . . . .
H78 H 0.339341 0.267232 0.073942 0.034 Uiso 1 1 calc R U . . .
C79 C 0.2713(2) 0.2515(2) 0.0264(2) 0.0329(10) Uani 1 1 d . . . . .
H79 H 0.298590 0.267730 -0.014951 0.039 Uiso 1 1 calc R U . . .
C80 C 0.2076(2) 0.2280(2) 0.0333(2) 0.0332(10) Uani 1 1 d . . . . .
C81 C 0.1679(2) 0.2073(2) 0.0929(2) 0.0350(10) Uani 1 1 d . . . . .
H81 H 0.123701 0.192784 0.097731 0.042 Uiso 1 1 calc R U . . .
C82 C 0.1898(2) 0.2068(2) 0.1465(2) 0.0311(9) Uani 1 1 d . . . . .
H82 H 0.161020 0.192470 0.187306 0.037 Uiso 1 1 calc R U . . .
C83 C 0.1825(3) 0.2261(3) -0.0238(3) 0.0446(13) Uani 1 1 d . . . . .
H83A H 0.174954 0.178349 -0.017094 0.067 Uiso 1 1 calc R U . . .
H83B H 0.217928 0.241431 -0.062094 0.067 Uiso 1 1 calc R U . . .
H83C H 0.138507 0.257130 -0.029182 0.067 Uiso 1 1 calc R U . . .
C101 C 0.2985(2) 0.4496(2) 0.36461(18) 0.0243(8) Uani 1 1 d . . . . .
C102 C 0.3685(2) 0.4279(2) 0.34461(19) 0.0267(9) Uani 1 1 d . . . . .
C103 C 0.4117(2) 0.3978(2) 0.3907(2) 0.0312(9) Uani 1 1 d . . . . .
H103 H 0.459683 0.383104 0.377627 0.037 Uiso 1 1 calc R U . . .
C104 C 0.3861(3) 0.3888(2) 0.4553(2) 0.0361(11) Uani 1 1 d . . . . .
C105 C 0.3154(3) 0.4107(2) 0.4725(2) 0.0335(10) Uani 1 1 d . . . . .
H105 H 0.296843 0.404134 0.516355 0.040 Uiso 1 1 calc R U . . .
C106 C 0.2709(2) 0.4418(2) 0.4286(2) 0.0286(9) Uani 1 1 d . . . . .
C107 C 0.3961(2) 0.4364(2) 0.2756(2) 0.0282(9) Uani 1 1 d . . . . .
H10D H 0.442980 0.409122 0.270737 0.034 Uiso 1 1 calc R U . . .
H10E H 0.364412 0.419221 0.258214 0.034 Uiso 1 1 calc R U . . .
C108 C 0.4318(3) 0.3551(3) 0.5064(2) 0.0519(14) Uani 1 1 d . . . . .
C109 C 0.4022(5) 0.2841(4) 0.5524(4) 0.086(2) Uani 1 1 d . . . . .
H10F H 0.353453 0.294525 0.571963 0.129 Uiso 1 1 calc R U . . .
H10G H 0.404340 0.253348 0.527527 0.129 Uiso 1 1 calc R U . . .
H10H H 0.430546 0.260984 0.585893 0.129 Uiso 1 1 calc R U . . .
C110 C 0.5039(4) 0.3298(4) 0.4818(3) 0.092(3) Uani 1 1 d . . . . .
H11D H 0.502845 0.301984 0.455124 0.138 Uiso 1 1 calc R U . . .
H11E H 0.529416 0.369664 0.456371 0.138 Uiso 1 1 calc R U . . .
H11F H 0.527384 0.300960 0.517679 0.138 Uiso 1 1 calc R U . . .
C111 C 0.4241(5) 0.3980(4) 0.5477(4) 0.092(3) Uani 1 1 d . . . . .
H11G H 0.374276 0.411959 0.561215 0.138 Uiso 1 1 calc R U . . .
H11H H 0.445460 0.371035 0.585280 0.138 Uiso 1 1 calc R U . . .
H11I H 0.447493 0.439739 0.523971 0.138 Uiso 1 1 calc R U . . .
C169 C 0.1952(2) 0.4699(2) 0.4473(2) 0.0308(10) Uani 1 1 d . . . . .
H16A H 0.176293 0.440761 0.490842 0.037 Uiso 1 1 calc R U . . .
H16B H 0.167101 0.467336 0.417623 0.037 Uiso 1 1 calc R U . . .
C113 C 0.1660(2) 0.6013(2) 0.39552(19) 0.0251(8) Uani 1 1 d . . . . .
C114 C 0.1891(2) 0.5448(2) 0.44547(19) 0.0289(9) Uani 1 1 d . . . . .
C115 C 0.2096(3) 0.5578(2) 0.4946(2) 0.0355(11) Uani 1 1 d . . . . .
H115 H 0.225083 0.519270 0.528474 0.043 Uiso 1 1 calc R U . . .
C116 C 0.2083(3) 0.6247(2) 0.4958(2) 0.0375(11) Uani 1 1 d . . . . .
C117 C 0.1828(3) 0.6798(2) 0.4466(2) 0.0332(10) Uani 1 1 d . . . . .
H117 H 0.180183 0.726091 0.446743 0.040 Uiso 1 1 calc R U . . .
C118 C 0.1610(2) 0.6692(2) 0.39689(19) 0.0261(9) Uani 1 1 d . . . . .
C119 C 0.2361(3) 0.6381(3) 0.5481(3) 0.0486(13) Uiso 1 1 d D . . . .
C12D C 0.2949(8) 0.5813(7) 0.5729(7) 0.0654(10) Uiso 0.477(6) 1 d . U P B 1
H12C H 0.284333 0.535993 0.575320 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12D H 0.339310 0.591463 0.543788 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12E H 0.298509 0.580222 0.615437 0.098 Uiso 0.477(6) 1 calc R U P B 1
C12E C 0.2366(8) 0.7097(7) 0.5393(7) 0.0654(10) Uiso 0.477(6) 1 d . U P B 1
H12F H 0.194392 0.737037 0.523181 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12G H 0.237393 0.715056 0.580228 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12H H 0.278194 0.726298 0.508579 0.098 Uiso 0.477(6) 1 calc R U P B 1
C12F C 0.1701(7) 0.6231(7) 0.6094(7) 0.0654(10) Uiso 0.477(6) 1 d . U P B 1
H12I H 0.161752 0.574335 0.622533 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12J H 0.181728 0.632134 0.645035 0.098 Uiso 0.477(6) 1 calc R U P B 1
H12K H 0.127780 0.653785 0.596683 0.098 Uiso 0.477(6) 1 calc R U P B 1
C12A C 0.2587(7) 0.5741(5) 0.5990(6) 0.0654(10) Uiso 0.523(6) 1 d D U P B 2
H12L H 0.292323 0.542642 0.579497 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12M H 0.280808 0.586928 0.626940 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12N H 0.217810 0.550652 0.624124 0.098 Uiso 0.523(6) 1 calc R U P B 2
C12C C 0.1839(6) 0.6877(6) 0.5774(6) 0.0654(10) Uiso 0.523(6) 1 d D U P B 2
H12O H 0.169451 0.729538 0.543388 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12P H 0.142741 0.664601 0.602415 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12Q H 0.205739 0.700877 0.605231 0.098 Uiso 0.523(6) 1 calc R U P B 2
C12B C 0.3010(6) 0.6816(6) 0.5141(6) 0.0654(10) Uiso 0.523(6) 1 d D U P B 2
H12R H 0.286547 0.723833 0.480448 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12S H 0.316758 0.694550 0.545644 0.098 Uiso 0.523(6) 1 calc R U P B 2
H12T H 0.339353 0.653008 0.495271 0.098 Uiso 0.523(6) 1 calc R U P B 2
C123 C 0.1327(2) 0.7331(2) 0.34667(19) 0.0248(8) Uani 1 1 d . . . . .
H12U H 0.137847 0.722124 0.306796 0.030 Uiso 1 1 calc R U . . .
H12V H 0.160935 0.771264 0.337425 0.030 Uiso 1 1 calc R U . . .
C124 C 0.0054(2) 0.7143(2) 0.3800(2) 0.0322(10) Uani 1 1 d . . . . .
C125 C 0.0562(2) 0.7578(2) 0.3674(2) 0.0329(10) Uani 1 1 d . . . . .
C126 C 0.0351(2) 0.8230(3) 0.3752(3) 0.0513(15) Uani 1 1 d . . . . .
H126 H 0.069515 0.852100 0.368776 0.062 Uiso 1 1 calc R U . . .
C127 C -0.0358(3) 0.8469(4) 0.3922(4) 0.085(3) Uani 1 1 d . . . . .
C128 C -0.0849(3) 0.8034(4) 0.3995(4) 0.077(2) Uani 1 1 d . . . . .
H128 H -0.133286 0.819447 0.409145 0.093 Uiso 1 1 calc R U . . .
C129 C -0.0658(2) 0.7379(3) 0.3932(3) 0.0460(14) Uani 1 1 d . . . . .
C130 C -0.0587(3) 0.9194(5) 0.3990(6) 0.172(7) Uani 1 1 d D . . . .
C13D C 0.0020(7) 0.9641(7) 0.3822(6) 0.0654(10) Uiso 0.553(7) 1 d . U P C 1
H13A H 0.045147 0.933451 0.392634 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13B H 0.009035 0.990650 0.336566 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13C H -0.009827 0.996399 0.406947 0.098 Uiso 0.553(7) 1 calc R U P C 1
C13F C -0.0877(7) 0.8848(6) 0.4931(6) 0.0654(10) Uiso 0.553(7) 1 d . U P C 1
H13D H -0.047764 0.856622 0.512593 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13E H -0.104028 0.924499 0.508999 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13F H -0.125742 0.856197 0.504218 0.098 Uiso 0.553(7) 1 calc R U P C 1
C13E C -0.1136(6) 0.9496(6) 0.3889(6) 0.0654(10) Uiso 0.553(7) 1 d . U P C 1
H13G H -0.119257 0.994769 0.395553 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13H H -0.117019 0.956939 0.344658 0.098 Uiso 0.553(7) 1 calc R U P C 1
H13I H -0.150400 0.922329 0.417927 0.098 Uiso 0.553(7) 1 calc R U P C 1
C13A C 0.0030(7) 0.9461(8) 0.4098(7) 0.0654(10) Uiso 0.447(7) 1 d D U P C 2
H13J H 0.044642 0.939289 0.378381 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13K H -0.008706 0.995770 0.404933 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13L H 0.012553 0.920116 0.452886 0.098 Uiso 0.447(7) 1 calc R U P C 2
C13C C -0.1181(6) 0.9299(8) 0.4451(6) 0.0654(10) Uiso 0.447(7) 1 d D U P C 2
H13M H -0.125818 0.978762 0.443368 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13N H -0.159433 0.918350 0.435943 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13O H -0.109972 0.899802 0.487685 0.098 Uiso 0.447(7) 1 calc R U P C 2
C13B C -0.0893(8) 0.9714(8) 0.3299(6) 0.0654(10) Uiso 0.447(7) 1 d D U P C 2
H13P H -0.053035 0.969467 0.292842 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13Q H -0.131265 0.954686 0.327492 0.098 Uiso 0.447(7) 1 calc R U P C 2
H13R H -0.100944 1.019624 0.330220 0.098 Uiso 0.447(7) 1 calc R U P C 2
C134 C -0.1183(3) 0.6888(3) 0.4054(3) 0.0535(16) Uani 1 1 d . . . . .
H13S H -0.108501 0.645889 0.441090 0.064 Uiso 1 1 calc R U . . .
H13T H -0.166106 0.711108 0.417368 0.064 Uiso 1 1 calc R U . . .
C135 C -0.1406(2) 0.6070(3) 0.3631(3) 0.0480(14) Uani 1 1 d . . . . .
H13U H -0.192387 0.613985 0.374027 0.058 Uiso 1 1 calc R U . . .
H13V H -0.122500 0.571960 0.400458 0.058 Uiso 1 1 calc R U . . .
C136 C -0.0486(2) 0.5570(2) 0.2893(2) 0.0330(10) Uani 1 1 d . . . . .
C137 C -0.1186(2) 0.5808(3) 0.3062(3) 0.0399(12) Uani 1 1 d . . . . .
C138 C -0.1666(2) 0.5765(3) 0.2723(3) 0.0453(13) Uani 1 1 d . . . . .
H138 H -0.214413 0.593678 0.282967 0.054 Uiso 1 1 calc R U . . .
C139 C -0.1466(2) 0.5476(3) 0.2229(3) 0.0429(12) Uani 1 1 d . . . . .
C140 C -0.0764(2) 0.5242(2) 0.2080(2) 0.0375(11) Uani 1 1 d . . . . .
H140 H -0.061848 0.504314 0.174623 0.045 Uiso 1 1 calc R U . . .
C141 C -0.0262(2) 0.5285(2) 0.2398(2) 0.0313(10) Uani 1 1 d . . . . .
C142 C -0.1977(3) 0.5415(3) 0.1845(3) 0.0496(14) Uani 1 1 d . . . . .
C143 C -0.1969(3) 0.4641(3) 0.1935(3) 0.0485(13) Uani 1 1 d . . . . .
H14A H -0.149112 0.443951 0.180398 0.073 Uiso 1 1 calc R U . . .
H14B H -0.213504 0.439194 0.238572 0.073 Uiso 1 1 calc R U . . .
H14C H -0.227765 0.459815 0.167436 0.073 Uiso 1 1 calc R U . . .
C144 C -0.1740(4) 0.5781(4) 0.1130(3) 0.081(2) Uani 1 1 d . . . . .
H14D H -0.125756 0.559057 0.099618 0.122 Uiso 1 1 calc R U . . .
H14E H -0.204852 0.570418 0.088720 0.122 Uiso 1 1 calc R U . . .
H14F H -0.176259 0.628208 0.104949 0.122 Uiso 1 1 calc R U . . .
C145 C -0.2723(3) 0.5709(4) 0.2053(5) 0.095(3) Uani 1 1 d . . . . .
H14G H -0.302747 0.565652 0.179295 0.142 Uiso 1 1 calc R U . . .
H14H H -0.288310 0.545562 0.250309 0.142 Uiso 1 1 calc R U . . .
H14I H -0.274099 0.620372 0.199614 0.142 Uiso 1 1 calc R U . . .
C146 C 0.0513(2) 0.5057(2) 0.2201(2) 0.0303(9) Uani 1 1 d . . . . .
H14J H 0.074699 0.490024 0.257729 0.036 Uiso 1 1 calc R U . . .
H14K H 0.056649 0.465886 0.204162 0.036 Uiso 1 1 calc R U . . .
C147 C 0.1261(2) 0.6052(2) 0.18202(19) 0.0241(8) Uani 1 1 d . . . . .
C148 C 0.0861(2) 0.5653(2) 0.1684(2) 0.0267(9) Uani 1 1 d . . . . .
C149 C 0.0766(2) 0.5816(2) 0.1060(2) 0.0304(9) Uani 1 1 d . . . . .
H149 H 0.048746 0.554773 0.097230 0.037 Uiso 1 1 calc R U . . .
C150 C 0.1060(2) 0.6354(3) 0.0560(2) 0.0338(10) Uani 1 1 d . . . . .
C151 C 0.1461(2) 0.6737(2) 0.0710(2) 0.0305(9) Uani 1 1 d . . . . .
H151 H 0.167154 0.710733 0.037627 0.037 Uiso 1 1 calc R U . . .
C152 C 0.1566(2) 0.6600(2) 0.1329(2) 0.0243(8) Uani 1 1 d . . . . .
C153 C 0.0904(3) 0.6532(3) -0.0114(2) 0.0433(12) Uani 1 1 d . . . . .
C154 C 0.0136(3) 0.6832(3) -0.0118(3) 0.0587(16) Uani 1 1 d . . . . .
H15A H -0.016014 0.650464 0.021253 0.088 Uiso 1 1 calc R U . . .
H15B H 0.005222 0.727659 -0.003220 0.088 Uiso 1 1 calc R U . . .
H15C H 0.002339 0.690940 -0.053621 0.088 Uiso 1 1 calc R U . . .
C155 C 0.0996(4) 0.5865(4) -0.0304(3) 0.073(2) Uani 1 1 d . . . . .
H15D H 0.069169 0.553422 0.001144 0.110 Uiso 1 1 calc R U . . .
H15E H 0.087003 0.598861 -0.072524 0.110 Uiso 1 1 calc R U . . .
H15F H 0.148525 0.565089 -0.031791 0.110 Uiso 1 1 calc R U . . .
C156 C 0.1383(4) 0.7018(5) -0.0615(3) 0.096(3) Uani 1 1 d . . . . .
H15G H 0.187139 0.680940 -0.059993 0.144 Uiso 1 1 calc R U . . .
H15H H 0.128093 0.709638 -0.103790 0.144 Uiso 1 1 calc R U . . .
H15I H 0.130977 0.746357 -0.053389 0.144 Uiso 1 1 calc R U . . .
C157 C 0.2003(2) 0.7057(2) 0.1444(2) 0.0262(9) Uani 1 1 d . . . . .
H15J H 0.188671 0.702303 0.190007 0.031 Uiso 1 1 calc R U . . .
H15K H 0.187629 0.754782 0.119000 0.031 Uiso 1 1 calc R U . . .
C158 C 0.3091(2) 0.6173(2) 0.15527(17) 0.0216(8) Uani 1 1 d . . . . .
C159 C 0.2788(2) 0.6860(2) 0.12702(18) 0.0240(8) Uani 1 1 d . . . . .
C160 C 0.3226(2) 0.7346(2) 0.08705(19) 0.0267(9) Uani 1 1 d . . . . .
H160 H 0.302372 0.780773 0.067463 0.032 Uiso 1 1 calc R U . . .
C161 C 0.3951(2) 0.7185(2) 0.0744(2) 0.0288(9) Uani 1 1 d . . . . .
C162 C 0.4238(2) 0.6503(2) 0.10325(19) 0.0276(9) Uani 1 1 d . . . . .
H162 H 0.473123 0.638269 0.095478 0.033 Uiso 1 1 calc R U . . .
C163 C 0.3814(2) 0.5987(2) 0.14364(18) 0.0250(8) Uani 1 1 d . . . . .
C164 C 0.4404(2) 0.7757(3) 0.0315(2) 0.0389(11) Uani 1 1 d . . . . .
C165 C 0.4170(3) 0.8085(4) -0.0333(3) 0.0658(18) Uani 1 1 d . . . . .
H16C H 0.367087 0.826469 -0.027121 0.099 Uiso 1 1 calc R U . . .
H16D H 0.444162 0.846815 -0.059770 0.099 Uiso 1 1 calc R U . . .
H16E H 0.424668 0.773192 -0.054480 0.099 Uiso 1 1 calc R U . . .
C166 C 0.5182(3) 0.7482(3) 0.0205(3) 0.0505(14) Uani 1 1 d . . . . .
H16F H 0.534199 0.726932 0.061579 0.076 Uiso 1 1 calc R U . . .
H16G H 0.525462 0.713156 -0.000979 0.076 Uiso 1 1 calc R U . . .
H16H H 0.544956 0.786779 -0.006269 0.076 Uiso 1 1 calc R U . . .
C167 C 0.4316(3) 0.8315(3) 0.0641(3) 0.0544(15) Uani 1 1 d . . . . .
H16I H 0.446674 0.810056 0.105562 0.082 Uiso 1 1 calc R U . . .
H16J H 0.460192 0.868476 0.037108 0.082 Uiso 1 1 calc R U . . .
H16K H 0.382239 0.851311 0.070277 0.082 Uiso 1 1 calc R U . . .
C168 C 0.4117(2) 0.5248(2) 0.17383(18) 0.0271(9) Uani 1 1 d . . . . .
H16Q H 0.388940 0.492629 0.163438 0.033 Uiso 1 1 calc R U . . .
H16R H 0.462476 0.518448 0.156813 0.033 Uiso 1 1 calc R U . . .
C170 C 0.3254(2) 0.6502(2) 0.2958(2) 0.0305(10) Uani 1 1 d . . . . .
C171 C 0.3430(3) 0.7119(3) 0.2494(2) 0.0412(12) Uani 1 1 d . . . . .
H171 H 0.321392 0.730795 0.212725 0.049 Uiso 1 1 calc R U . . .
C172 C 0.3925(3) 0.7458(3) 0.2573(2) 0.0444(12) Uani 1 1 d . . . . .
H172 H 0.404891 0.787967 0.225304 0.053 Uiso 1 1 calc R U . . .
C173 C 0.4245(3) 0.7194(3) 0.3109(2) 0.0420(12) Uani 1 1 d . . . . .
C174 C 0.4041(3) 0.6593(3) 0.3577(3) 0.0545(15) Uani 1 1 d . . . . .
H174 H 0.423861 0.641753 0.395424 0.065 Uiso 1 1 calc R U . . .
C175 C 0.3557(3) 0.6244(3) 0.3506(2) 0.0468(14) Uani 1 1 d . . . . .
H175 H 0.342817 0.582668 0.383026 0.056 Uiso 1 1 calc R U . . .
C176 C 0.4804(3) 0.7562(3) 0.3171(3) 0.0544(15) Uani 1 1 d . . . . .
H17A H 0.526370 0.729041 0.310515 0.082 Uiso 1 1 calc R U . . .
H17B H 0.470690 0.760546 0.359865 0.082 Uiso 1 1 calc R U . . .
H17C H 0.480185 0.802650 0.285051 0.082 Uiso 1 1 calc R U . . .
C177 C 0.0030(2) 0.7501(3) 0.2082(3) 0.0413(12) Uani 1 1 d . . . . .
C178 C -0.0159(3) 0.7428(3) 0.1557(4) 0.070(2) Uani 1 1 d . . . . .
H178 H -0.009776 0.698339 0.150427 0.084 Uiso 1 1 calc R U . . .
C179 C -0.0440(5) 0.8018(4) 0.1110(4) 0.105(3) Uani 1 1 d . . . . .
H179 H -0.056075 0.796915 0.074962 0.126 Uiso 1 1 calc R U . . .
C180 C -0.0547(5) 0.8669(4) 0.1177(5) 0.102(3) Uani 1 1 d . . . . .
C181 C -0.0362(4) 0.8724(3) 0.1720(4) 0.076(2) Uani 1 1 d . . . . .
H181 H -0.044011 0.916703 0.177955 0.091 Uiso 1 1 calc R U . . .
C182 C -0.0076(3) 0.8160(3) 0.2161(3) 0.0487(13) Uani 1 1 d . . . . .
H182 H 0.005079 0.821228 0.251782 0.058 Uiso 1 1 calc R U . . .
C183 C -0.0894(7) 0.9309(5) 0.0708(5) 0.149(5) Uani 1 1 d . . . . .
H18A H -0.084080 0.922949 0.029960 0.223 Uiso 1 1 calc R U . . .
H18B H -0.067139 0.971795 0.064350 0.223 Uiso 1 1 calc R U . . .
H18C H -0.139356 0.938907 0.088267 0.223 Uiso 1 1 calc R U . . .
C200 C 0.3202(3) 0.8836(3) 0.3273(3) 0.0612(16) Uani 1 1 d . . . . .
H20D H 0.337392 0.921404 0.333784 0.092 Uiso 1 1 calc R U . . .
H20E H 0.319979 0.894524 0.281776 0.092 Uiso 1 1 calc R U . . .
H20F H 0.350846 0.839965 0.342247 0.092 Uiso 1 1 calc R U . . .
C201 C 0.2500(3) 0.8760(3) 0.3627(3) 0.0543(14) Uani 1 1 d . . . . .
C210 C 0.7691(7) 0.9371(10) 0.2582(6) 0.250(13) Uani 1 1 d . . . . .
C211 C 0.7244(4) 0.9350(6) 0.3137(4) 0.121(4) Uani 1 1 d . . . . .
H21D H 0.676436 0.950186 0.305379 0.181 Uiso 1 1 calc R U . . .
H21E H 0.736927 0.966124 0.332389 0.181 Uiso 1 1 calc R U . . .
H21F H 0.727622 0.887274 0.343493 0.181 Uiso 1 1 calc R U . . .
C220 C 0.7247(3) 0.7865(3) 0.5135(3) 0.0480(13) Uani 1 1 d . . . . .
C221 C 0.7291(3) 0.7308(3) 0.5722(2) 0.0456(12) Uani 1 1 d . . . . .
H22D H 0.722273 0.750105 0.607089 0.068 Uiso 1 1 calc R U . . .
H22E H 0.775230 0.703093 0.569162 0.068 Uiso 1 1 calc R U . . .
H22F H 0.692651 0.701068 0.580721 0.068 Uiso 1 1 calc R U . . .
C230 C 0.0730(3) 0.3987(3) 0.1069(3) 0.0513(14) Uani 1 1 d . . . . .
C231 C 0.1465(3) 0.3935(3) 0.0821(3) 0.0454(12) Uani 1 1 d . . . . .
H23C H 0.160613 0.440409 0.061511 0.068 Uiso 1 1 calc R U . . .
H23D H 0.156931 0.368909 0.050675 0.068 Uiso 1 1 calc R U . . .
H23E H 0.172414 0.367782 0.116982 0.068 Uiso 1 1 calc R U . . .
C240 C 0.0467(3) 0.3733(4) 0.4395(3) 0.0589(16) Uani 1 1 d . . . . .
C241 C -0.0240(7) 0.4177(7) 0.4579(6) 0.149(4) Uiso 1 1 d . . . . .
C260 C 0.1689(6) 0.8826(6) 0.0141(5) 0.045(2) Uiso 0.5 1 d . . P . .
C261 C 0.0938(10) 0.8760(10) 0.0401(9) 0.108(6) Uiso 0.5 1 d . . P . .
H26A H 0.089264 0.833503 0.077109 0.163 Uiso 0.5 1 calc R U P . .
H26B H 0.070946 0.873402 0.007285 0.163 Uiso 0.5 1 calc R U P . .
H26C H 0.071416 0.916597 0.053222 0.163 Uiso 0.5 1 calc R U P . .
C250 C 0.7430(5) 0.7569(5) 0.2535(8) 0.151(6) Uani 1 1 d . . . . .
C251 C 0.8101(6) 0.7615(5) 0.2154(6) 0.138(4) Uani 1 1 d . . . . .
H25A H 0.838798 0.716070 0.227290 0.207 Uiso 1 1 calc R U . . .
H25B H 0.832241 0.796271 0.221928 0.207 Uiso 1 1 calc R U . . .
H25C H 0.806014 0.775513 0.170345 0.207 Uiso 1 1 calc R U . . .
N1 N 0.51618(17) 0.09682(16) 0.26191(15) 0.0213(7) Uani 1 1 d . . . . .
N2 N 0.27820(17) 0.22531(17) 0.19334(15) 0.0223(7) Uani 1 1 d . . . . .
N3 N 0.27989(18) 0.61294(18) 0.28712(16) 0.0258(7) Uani 1 1 d . . . . .
N4 N 0.02887(18) 0.6913(2) 0.25426(19) 0.0324(8) Uani 1 1 d . . . . .
N200 N 0.1935(3) 0.8709(3) 0.3907(3) 0.0780(18) Uani 1 1 d . . . . .
N210 N 0.7959(5) 0.9293(5) 0.2062(6) 0.134(3) Uani 1 1 d . . . . .
N220 N 0.7209(3) 0.8307(3) 0.4676(3) 0.095(2) Uani 1 1 d . . . . .
N230 N 0.0155(3) 0.4030(4) 0.1278(3) 0.092(2) Uani 1 1 d . . . . .
N240 N 0.1003(4) 0.3485(6) 0.4340(4) 0.140(4) Uani 1 1 d . . . . .
N250 N 0.6902(5) 0.7446(5) 0.2764(5) 0.138(4) Uani 1 1 d . . . . .
N260 N 0.2217(7) 0.8901(7) 0.0019(6) 0.086(4) Uiso 0.5 1 d . . P . .
O1 O 0.43061(13) 0.00346(13) 0.28436(12) 0.0195(5) Uani 1 1 d . . . . .
O2 O 0.33587(13) 0.11128(13) 0.27380(12) 0.0206(5) Uani 1 1 d . . . . .
O3 O 0.23094(14) 0.20856(14) 0.31935(12) 0.0233(6) Uani 1 1 d . . . . .
O4 O 0.18057(15) 0.35997(15) 0.22547(13) 0.0279(6) Uani 1 1 d . . . . .
O5 O 0.32880(13) 0.30226(13) 0.24211(12) 0.0206(5) Uani 1 1 d . . . . .
O6 O 0.40373(13) 0.18615(13) 0.28640(12) 0.0192(5) Uani 1 1 d . . . . .
O7 O 0.44437(13) 0.05507(13) 0.38118(12) 0.0202(5) Uani 1 1 d . . . . .
O8 O 0.55979(14) -0.05119(14) 0.34006(12) 0.0228(6) Uani 1 1 d . . . . .
O9 O 0.25483(15) 0.47824(14) 0.32113(13) 0.0245(6) Uani 1 1 d . . . . .
O10 O 0.14945(14) 0.58876(14) 0.34473(13) 0.0246(6) Uani 1 1 d . . . . .
O11 O 0.02692(15) 0.64799(15) 0.37929(14) 0.0302(7) Uani 1 1 d . . . . .
O12 O -0.11380(16) 0.67127(18) 0.34823(18) 0.0447(9) Uani 1 1 d . . . . .
O13 O 0.00005(15) 0.55835(16) 0.32263(15) 0.0341(7) Uani 1 1 d . . . . .
O14 O 0.13503(14) 0.58995(14) 0.24417(13) 0.0230(6) Uani 1 1 d . . . . .
O15 O 0.26617(14) 0.56990(14) 0.19468(12) 0.0224(6) Uani 1 1 d . . . . .
O16 O 0.40074(15) 0.50903(14) 0.24167(13) 0.0259(6) Uani 1 1 d . . . . .
V1 V 0.43534(3) 0.08403(3) 0.29926(3) 0.01789(14) Uani 1 1 d . . . . .
V2 V 0.30774(3) 0.21396(3) 0.25909(3) 0.01928(15) Uani 1 1 d . . . . .
V3 V 0.22746(3) 0.56601(3) 0.27728(3) 0.02070(15) Uani 1 1 d . . . . .
V4 V 0.05789(4) 0.62062(4) 0.30878(3) 0.02614(17) Uani 1 1 d . . . . .
C300 C 0.5271(4) 0.5929(4) 0.2459(4) 0.0259(18) Uani 0.5 1 d . . P . .
H30A H 0.530183 0.556634 0.226024 0.031 Uiso 1 1 calc R U . . .
H30B H 0.476655 0.609517 0.255428 0.031 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5575(9) 0.6517(9) 0.1944(8) 0.321(7) Uiso 0.5 1 d . . P . .
Cl2 Cl 0.5507(4) 0.5494(4) 0.3179(3) 0.145(2) Uiso 0.5 1 d . . P . .


_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 O1 1.363(4) . ?
C1 C6 1.392(5) . ?
C1 C2 1.396(5) . ?
C2 C3 1.394(5) . ?
C2 C7 1.501(5) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(6) . ?
C4 C8 1.538(5) . ?
C5 C6 1.400(5) . ?
C5 H5 0.9500 . ?
C6 C12 1.515(5) . ?
C7 O8 1.430(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C11 1.523(6) . ?
C8 C10 1.534(7) . ?
C8 C9 1.541(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.516(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O2 1.388(4) . ?
C13 C18 1.399(5) . ?
C13 C14 1.410(5) . ?
C14 C15 1.395(5) . ?
C15 C16 1.392(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(6) . ?
C16 C19 1.535(5) . ?
C17 C18 1.395(5) . ?
C17 H17 0.9500 . ?
C18 C23 1.530(5) . ?
C19 C20 1.502(8) . ?
C19 C22 1.528(7) . ?
C19 C21 1.538(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.510(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O3 1.367(5) . ?
C24 C25 1.397(6) . ?
C24 C29 1.402(6) . ?
C25 C26 1.408(6) . ?
C26 C27 1.414(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(7) . ?
C27 C30 1.549(7) . ?
C28 C29 1.396(6) . ?
C28 H28 0.9500 . ?
C29 C34 1.491(6) . ?
C30 C31 1.475(10) . ?
C30 C32 1.505(10) . ?
C30 C33 1.537(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O4 1.433(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O4 1.433(5) . ?
C35 C37 1.499(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 O5 1.364(4) . ?
C36 C37 1.388(6) . ?
C36 C41 1.399(5) . ?
C37 C38 1.390(6) . ?
C38 C39 1.399(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.388(6) . ?
C39 C42 1.540(6) . ?
C40 C41 1.394(5) . ?
C40 H40 0.9500 . ?
C41 C46 1.522(5) . ?
C42 C43 1.511(7) . ?
C42 C45 1.519(6) . ?
C42 C44 1.537(7) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.528(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O6 1.388(4) . ?
C47 C48 1.394(5) . ?
C47 C52 1.401(5) . ?
C48 C49 1.390(5) . ?
C49 C50 1.405(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.379(5) . ?
C50 C53 1.537(5) . ?
C51 C52 1.400(5) . ?
C51 H51 0.9500 . ?
C52 C57 1.521(5) . ?
C53 C56 1.525(6) . ?
C53 C54 1.537(6) . ?
C53 C55 1.539(6) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C59 1.519(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 O7 1.374(4) . ?
C58 C59 1.391(5) . ?
C58 C63 1.392(5) . ?
C59 C60 1.396(5) . ?
C60 C61 1.391(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.403(6) . ?
C61 C64 1.539(6) . ?
C62 C63 1.394(6) . ?
C62 H62 0.9500 . ?
C63 C68 1.504(5) . ?
C64 C67A 1.417(10) . ?
C64 C65B 1.456(8) . ?
C64 C66B 1.509(8) . ?
C64 C65A 1.576(10) . ?
C64 C67B 1.621(8) . ?
C64 C66A 1.640(10) . ?
C65A H65A 0.9800 . ?
C65A H65B 0.9800 . ?
C65A H65C 0.9800 . ?
C66A H66A 0.9800 . ?
C66A H66B 0.9800 . ?
C66A H66C 0.9800 . ?
C67A H67A 0.9800 . ?
C67A H67B 0.9800 . ?
C67A H67C 0.9800 . ?
C66B H66D 0.9800 . ?
C66B H66E 0.9800 . ?
C66B H66F 0.9800 . ?
C67B H67D 0.9800 . ?
C67B H67E 0.9800 . ?
C67B H67F 0.9800 . ?
C65B H65D 0.9800 . ?
C65B H65E 0.9800 . ?
C65B H65F 0.9800 . ?
C68 O8 1.428(4) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C70 N1 1.385(5) . ?
C70 C75 1.395(6) . ?
C70 C71 1.399(6) . ?
C71 C72 1.375(6) . ?
C71 H71 0.9500 . ?
C72 C73 1.397(7) . ?
C72 H72 0.9500 . ?
C73 C74 1.384(7) . ?
C73 C76 1.506(7) . ?
C74 C75 1.381(6) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 N2 1.381(5) . ?
C77 C78 1.396(6) . ?
C77 C82 1.401(6) . ?
C78 C79 1.394(6) . ?
C78 H78 0.9500 . ?
C79 C80 1.396(6) . ?
C79 H79 0.9500 . ?
C80 C81 1.367(7) . ?
C80 C83 1.511(6) . ?
C81 C82 1.382(6) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C101 O9 1.363(5) . ?
C101 C102 1.391(6) . ?
C101 C106 1.394(5) . ?
C102 C103 1.401(6) . ?
C102 C107 1.498(6) . ?
C103 C104 1.398(6) . ?
C103 H103 0.9500 . ?
C104 C105 1.391(7) . ?
C104 C108 1.524(7) . ?
C105 C106 1.387(6) . ?
C105 H105 0.9500 . ?
C106 C169 1.515(6) . ?
C107 O16 1.435(5) . ?
C107 H10D 0.9900 . ?
C107 H10E 0.9900 . ?
C108 C110 1.471(9) . ?
C108 C111 1.471(8) . ?
C108 C109 1.601(9) . ?
C109 H10F 0.9800 . ?
C109 H10G 0.9800 . ?
C109 H10H 0.9800 . ?
C110 H11D 0.9800 . ?
C110 H11E 0.9800 . ?
C110 H11F 0.9800 . ?
C111 H11G 0.9800 . ?
C111 H11H 0.9800 . ?
C111 H11I 0.9800 . ?
C169 C114 1.517(6) . ?
C169 H16A 0.9900 . ?
C169 H16B 0.9900 . ?
C113 O10 1.391(5) . ?
C113 C118 1.398(6) . ?
C113 C114 1.399(6) . ?
C114 C115 1.397(6) . ?
C115 C116 1.389(6) . ?
C115 H115 0.9500 . ?
C116 C117 1.393(7) . ?
C116 C119 1.547(7) . ?
C117 C118 1.398(6) . ?
C117 H117 0.9500 . ?
C118 C123 1.518(6) . ?
C119 C12E 1.423(14) . ?
C119 C12A 1.489(11) . ?
C119 C12C 1.520(11) . ?
C119 C12D 1.532(15) . ?
C119 C12B 1.598(11) . ?
C119 C12F 1.661(14) . ?
C12D H12C 0.9800 . ?
C12D H12D 0.9800 . ?
C12D H12E 0.9800 . ?
C12E H12F 0.9800 . ?
C12E H12G 0.9800 . ?
C12E H12H 0.9800 . ?
C12F H12I 0.9800 . ?
C12F H12J 0.9800 . ?
C12F H12K 0.9800 . ?
C12A H12L 0.9800 . ?
C12A H12M 0.9800 . ?
C12A H12N 0.9800 . ?
C12C H12O 0.9800 . ?
C12C H12P 0.9800 . ?
C12C H12Q 0.9800 . ?
C12B H12R 0.9800 . ?
C12B H12S 0.9800 . ?
C12B H12T 0.9800 . ?
C123 C125 1.521(6) . ?
C123 H12U 0.9900 . ?
C123 H12V 0.9900 . ?
C124 O11 1.357(5) . ?
C124 C125 1.394(6) . ?
C124 C129 1.397(6) . ?
C125 C126 1.391(6) . ?
C126 C127 1.403(7) . ?
C126 H126 0.9500 . ?
C127 C128 1.395(7) . ?
C127 C130 1.530(9) . ?
C128 C129 1.382(7) . ?
C128 H128 0.9500 . ?
C129 C134 1.506(6) . ?
C130 C13E 1.169(14) . ?
C130 C13C 1.420(12) . ?
C130 C13A 1.537(12) . ?
C130 C13D 1.557(14) . ?
C130 C13B 1.727(14) . ?
C130 C13F 1.985(17) . ?
C13D H13A 0.9800 . ?
C13D H13B 0.9800 . ?
C13D H13C 0.9800 . ?
C13F H13D 0.9800 . ?
C13F H13E 0.9800 . ?
C13F H13F 0.9800 . ?
C13E H13G 0.9800 . ?
C13E H13H 0.9800 . ?
C13E H13I 0.9800 . ?
C13A H13J 0.9800 . ?
C13A H13K 0.9800 . ?
C13A H13L 0.9800 . ?
C13C H13M 0.9800 . ?
C13C H13N 0.9800 . ?
C13C H13O 0.9800 . ?
C13B H13P 0.9800 . ?
C13B H13Q 0.9800 . ?
C13B H13R 0.9800 . ?
C134 O12 1.449(6) . ?
C134 H13S 0.9900 . ?
C134 H13T 0.9900 . ?
C135 O12 1.429(5) . ?
C135 C137 1.518(7) . ?
C135 H13U 0.9900 . ?
C135 H13V 0.9900 . ?
C136 O13 1.367(5) . ?
C136 C137 1.387(6) . ?
C136 C141 1.397(6) . ?
C137 C138 1.389(7) . ?
C138 C139 1.398(7) . ?
C138 H138 0.9500 . ?
C139 C140 1.382(7) . ?
C139 C142 1.530(7) . ?
C140 C141 1.390(6) . ?
C140 H140 0.9500 . ?
C141 C146 1.523(6) . ?
C142 C145 1.517(8) . ?
C142 C144 1.536(9) . ?
C142 C143 1.536(8) . ?
C143 H14A 0.9800 . ?
C143 H14B 0.9800 . ?
C143 H14C 0.9800 . ?
C144 H14D 0.9800 . ?
C144 H14E 0.9800 . ?
C144 H14F 0.9800 . ?
C145 H14G 0.9800 . ?
C145 H14H 0.9800 . ?
C145 H14I 0.9800 . ?
C146 C148 1.519(6) . ?
C146 H14J 0.9900 . ?
C146 H14K 0.9900 . ?
C147 O14 1.382(5) . ?
C147 C152 1.398(6) . ?
C147 C148 1.399(5) . ?
C148 C149 1.388(6) . ?
C149 C150 1.388(7) . ?
C149 H149 0.9500 . ?
C150 C151 1.392(6) . ?
C150 C153 1.538(6) . ?
C151 C152 1.394(6) . ?
C151 H151 0.9500 . ?
C152 C157 1.520(6) . ?
C153 C156 1.508(9) . ?
C153 C154 1.524(7) . ?
C153 C155 1.552(8) . ?
C154 H15A 0.9800 . ?
C154 H15B 0.9800 . ?
C154 H15C 0.9800 . ?
C155 H15D 0.9800 . ?
C155 H15E 0.9800 . ?
C155 H15F 0.9800 . ?
C156 H15G 0.9800 . ?
C156 H15H 0.9800 . ?
C156 H15I 0.9800 . ?
C157 C159 1.522(6) . ?
C157 H15J 0.9900 . ?
C157 H15K 0.9900 . ?
C158 O15 1.356(5) . ?
C158 C163 1.395(5) . ?
C158 C159 1.410(6) . ?
C159 C160 1.385(6) . ?
C160 C161 1.393(6) . ?
C160 H160 0.9500 . ?
C161 C162 1.394(6) . ?
C161 C164 1.533(6) . ?
C162 C163 1.409(6) . ?
C162 H162 0.9500 . ?
C163 C168 1.501(6) . ?
C164 C165 1.529(8) . ?
C164 C166 1.529(7) . ?
C164 C167 1.541(7) . ?
C165 H16C 0.9800 . ?
C165 H16D 0.9800 . ?
C165 H16E 0.9800 . ?
C166 H16F 0.9800 . ?
C166 H16G 0.9800 . ?
C166 H16H 0.9800 . ?
C167 H16I 0.9800 . ?
C167 H16J 0.9800 . ?
C167 H16K 0.9800 . ?
C168 O16 1.434(5) . ?
C168 H16Q 0.9900 . ?
C168 H16R 0.9900 . ?
C170 N3 1.380(5) . ?
C170 C171 1.383(6) . ?
C170 C175 1.397(6) . ?
C171 C172 1.388(6) . ?
C171 H171 0.9500 . ?
C172 C173 1.394(7) . ?
C172 H172 0.9500 . ?
C173 C174 1.379(7) . ?
C173 C176 1.516(7) . ?
C174 C175 1.377(7) . ?
C174 H174 0.9500 . ?
C175 H175 0.9500 . ?
C176 H17A 0.9800 . ?
C176 H17B 0.9800 . ?
C176 H17C 0.9800 . ?
C177 N4 1.392(6) . ?
C177 C178 1.397(7) . ?
C177 C182 1.406(7) . ?
C178 C179 1.395(9) . ?
C178 H178 0.9500 . ?
C179 C180 1.376(10) . ?
C179 H179 0.9500 . ?
C180 C181 1.416(10) . ?
C180 C183 1.531(10) . ?
C181 C182 1.366(8) . ?
C181 H181 0.9500 . ?
C182 H182 0.9500 . ?
C183 H18A 0.9800 . ?
C183 H18B 0.9800 . ?
C183 H18C 0.9800 . ?
C200 C201 1.442(9) . ?
C200 H20D 0.9800 . ?
C200 H20E 0.9800 . ?
C200 H20F 0.9800 . ?
C201 N200 1.155(8) . ?
C210 N210 1.234(15) . ?
C210 C211 1.355(13) . ?
C211 H21D 0.9800 . ?
C211 H21E 0.9800 . ?
C211 H21F 0.9800 . ?
C220 N220 1.125(7) . ?
C220 C221 1.430(7) . ?
C221 H22D 0.9800 . ?
C221 H22E 0.9800 . ?
C221 H22F 0.9800 . ?
C230 N230 1.126(7) . ?
C230 C231 1.431(8) . ?
C231 H23C 0.9800 . ?
C231 H23D 0.9800 . ?
C231 H23E 0.9800 . ?
C240 N240 1.082(9) . ?
C240 C241 1.572(14) . ?
C260 N260 1.044(15) . ?
C260 C261 1.48(2) . ?
C261 H26A 0.9800 . ?
C261 H26B 0.9800 . ?
C261 H26C 0.9800 . ?
C250 N250 1.089(12) . ?
C250 C251 1.409(15) . ?
C251 H25A 0.9800 . ?
C251 H25B 0.9800 . ?
C251 H25C 0.9800 . ?
N1 V1 1.652(3) . ?
N2 V2 1.656(3) . ?
N3 V3 1.652(3) . ?
N4 V4 1.650(4) . ?
O1 V1 1.837(3) . ?
O2 V2 2.012(3) . ?
O2 V1 2.095(3) . ?
O3 V2 1.787(3) . ?
O5 V2 1.839(3) . ?
O6 V1 2.016(3) . ?
O6 V2 2.047(3) . ?
O7 V1 1.786(3) . ?
O9 V3 1.779(3) . ?
O10 V3 2.022(3) . ?
O10 V4 2.055(3) . ?
O11 V4 1.823(3) . ?
O13 V4 1.787(3) . ?
O14 V4 2.033(3) . ?
O14 V3 2.044(3) . ?
O15 V3 1.838(3) . ?
C300 Cl1 1.472(18) . ?
C300 Cl2 1.690(11) . ?
C300 H30A 0.9900 . ?
C300 H30B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 119.2(3) . . ?
O1 C1 C2 119.8(3) . . ?
C6 C1 C2 121.1(3) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C7 122.2(4) . . ?
C1 C2 C7 119.1(3) . . ?
C2 C3 C4 122.0(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C8 119.2(4) . . ?
C5 C4 C8 122.9(4) . . ?
C4 C5 C6 121.6(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 118.8(4) . . ?
C1 C6 C12 119.1(3) . . ?
C5 C6 C12 122.0(3) . . ?
O8 C7 C2 108.5(3) . . ?
O8 C7 H7A 110.0 . . ?
C2 C7 H7A 110.0 . . ?
O8 C7 H7B 110.0 . . ?
C2 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
C11 C8 C10 108.2(4) . . ?
C11 C8 C4 112.6(4) . . ?
C10 C8 C4 109.1(4) . . ?
C11 C8 C9 108.0(4) . . ?
C10 C8 C9 110.3(4) . . ?
C4 C8 C9 108.6(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 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C12 C14 114.3(3) . . ?
C6 C12 H12A 108.7 . . ?
C14 C12 H12A 108.7 . . ?
C6 C12 H12B 108.7 . . ?
C14 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O2 C13 C18 120.1(3) . . ?
O2 C13 C14 120.1(3) . . ?
C18 C13 C14 119.8(3) . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 C12 118.5(3) . . ?
C13 C14 C12 122.9(3) . . ?
C16 C15 C14 122.9(4) . . ?
C16 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
C17 C16 C15 116.8(4) . . ?
C17 C16 C19 123.2(4) . . ?
C15 C16 C19 120.0(4) . . ?
C16 C17 C18 122.9(4) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C17 C18 C13 119.0(3) . . ?
C17 C18 C23 117.9(3) . . ?
C13 C18 C23 123.1(3) . . ?
C20 C19 C22 110.0(5) . . ?
C20 C19 C16 109.9(4) . . ?
C22 C19 C16 111.6(4) . . ?
C20 C19 C21 109.4(5) . . ?
C22 C19 C21 106.7(5) . . ?
C16 C19 C21 109.2(4) . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C18 112.3(3) . . ?
C25 C23 H23A 109.2 . . ?
C18 C23 H23A 109.2 . . ?
C25 C23 H23B 109.2 . . ?
C18 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
O3 C24 C25 119.0(4) . . ?
O3 C24 C29 119.2(4) . . ?
C25 C24 C29 121.7(4) . . ?
C24 C25 C26 117.5(4) . . ?
C24 C25 C23 120.0(4) . . ?
C26 C25 C23 122.5(4) . . ?
C25 C26 C27 122.3(4) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C26 117.5(4) . . ?
C28 C27 C30 122.0(5) . . ?
C26 C27 C30 120.6(4) . . ?
C27 C28 C29 122.4(4) . . ?
C27 C28 H28 118.8 . . ?
C29 C28 H28 118.8 . . ?
C28 C29 C24 118.6(4) . . ?
C28 C29 C34 121.4(4) . . ?
C24 C29 C34 120.0(4) . . ?
C31 C30 C32 113.1(7) . . ?
C31 C30 C33 108.2(7) . . ?
C32 C30 C33 106.1(6) . . ?
C31 C30 C27 109.8(5) . . ?
C32 C30 C27 108.0(6) . . ?
C33 C30 C27 111.6(5) . . ?
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 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C34 C29 108.0(3) . . ?
O4 C34 H34A 110.1 . . ?
C29 C34 H34A 110.1 . . ?
O4 C34 H34B 110.1 . . ?
C29 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
O4 C35 C37 108.2(3) . . ?
O4 C35 H35A 110.1 . . ?
C37 C35 H35A 110.0 . . ?
O4 C35 H35B 110.0 . . ?
C37 C35 H35B 110.0 . . ?
H35A C35 H35B 108.4 . . ?
O5 C36 C37 119.9(3) . . ?
O5 C36 C41 118.6(3) . . ?
C37 C36 C41 121.5(3) . . ?
C36 C37 C38 118.5(4) . . ?
C36 C37 C35 119.3(4) . . ?
C38 C37 C35 122.2(4) . . ?
C37 C38 C39 122.0(4) . . ?
C37 C38 H38 119.0 . . ?
C39 C38 H38 119.0 . . ?
C40 C39 C38 117.5(4) . . ?
C40 C39 C42 123.3(4) . . ?
C38 C39 C42 119.2(4) . . ?
C39 C40 C41 122.4(4) . . ?
C39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
C40 C41 C36 118.0(4) . . ?
C40 C41 C46 122.2(3) . . ?
C36 C41 C46 119.7(3) . . ?
C43 C42 C45 111.1(5) . . ?
C43 C42 C44 107.5(4) . . ?
C45 C42 C44 106.5(4) . . ?
C43 C42 C39 111.0(4) . . ?
C45 C42 C39 108.7(4) . . ?
C44 C42 C39 112.0(4) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C41 C46 C48 113.7(3) . . ?
C41 C46 H46A 108.8 . . ?
C48 C46 H46A 108.8 . . ?
C41 C46 H46B 108.8 . . ?
C48 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?
O6 C47 C48 120.7(3) . . ?
O6 C47 C52 118.7(3) . . ?
C48 C47 C52 120.5(3) . . ?
C49 C48 C47 118.9(3) . . ?
C49 C48 C46 117.8(3) . . ?
C47 C48 C46 123.4(3) . . ?
C48 C49 C50 122.5(3) . . ?
C48 C49 H49 118.8 . . ?
C50 C49 H49 118.8 . . ?
C51 C50 C49 116.6(3) . . ?
C51 C50 C53 122.8(3) . . ?
C49 C50 C53 120.6(3) . . ?
C50 C51 C52 123.2(3) . . ?
C50 C51 H51 118.4 . . ?
C52 C51 H51 118.4 . . ?
C51 C52 C47 118.2(3) . . ?
C51 C52 C57 118.5(3) . . ?
C47 C52 C57 123.2(3) . . ?
C56 C53 C54 109.0(4) . . ?
C56 C53 C50 111.9(3) . . ?
C54 C53 C50 108.4(4) . . ?
C56 C53 C55 107.4(4) . . ?
C54 C53 C55 110.2(4) . . ?
C50 C53 C55 110.0(3) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C59 C57 C52 110.1(3) . . ?
C59 C57 H57A 109.6 . . ?
C52 C57 H57A 109.6 . . ?
C59 C57 H57B 109.6 . . ?
C52 C57 H57B 109.6 . . ?
H57A C57 H57B 108.2 . . ?
O7 C58 C59 118.9(3) . . ?
O7 C58 C63 120.0(3) . . ?
C59 C58 C63 121.1(4) . . ?
C58 C59 C60 118.3(4) . . ?
C58 C59 C57 120.1(3) . . ?
C60 C59 C57 121.3(3) . . ?
C61 C60 C59 122.6(4) . . ?
C61 C60 H60 118.7 . . ?
C59 C60 H60 118.7 . . ?
C60 C61 C62 117.3(4) . . ?
C60 C61 C64 120.9(4) . . ?
C62 C61 C64 121.7(4) . . ?
C63 C62 C61 121.7(4) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
C58 C63 C62 119.0(4) . . ?
C58 C63 C68 120.3(4) . . ?
C62 C63 C68 120.6(4) . . ?
C65B C64 C66B 114.8(5) . . ?
C67A C64 C61 117.4(6) . . ?
C65B C64 C61 110.4(4) . . ?
C66B C64 C61 110.6(4) . . ?
C67A C64 C65A 112.0(7) . . ?
C61 C64 C65A 106.2(5) . . ?
C65B C64 C67B 108.3(5) . . ?
C66B C64 C67B 103.6(5) . . ?
C61 C64 C67B 108.8(4) . . ?
C67A C64 C66A 108.2(7) . . ?
C61 C64 C66A 110.5(5) . . ?
C65A C64 C66A 101.4(6) . . ?
C64 C65A H65A 109.5 . . ?
C64 C65A H65B 109.5 . . ?
H65A C65A H65B 109.5 . . ?
C64 C65A H65C 109.5 . . ?
H65A C65A H65C 109.5 . . ?
H65B C65A H65C 109.5 . . ?
C64 C66A H66A 109.5 . . ?
C64 C66A H66B 109.5 . . ?
H66A C66A H66B 109.5 . . ?
C64 C66A H66C 109.5 . . ?
H66A C66A H66C 109.5 . . ?
H66B C66A H66C 109.5 . . ?
C64 C67A H67A 109.5 . . ?
C64 C67A H67B 109.5 . . ?
H67A C67A H67B 109.5 . . ?
C64 C67A H67C 109.5 . . ?
H67A C67A H67C 109.5 . . ?
H67B C67A H67C 109.5 . . ?
C64 C66B H66D 109.5 . . ?
C64 C66B H66E 109.5 . . ?
H66D C66B H66E 109.5 . . ?
C64 C66B H66F 109.5 . . ?
H66D C66B H66F 109.5 . . ?
H66E C66B H66F 109.5 . . ?
C64 C67B H67D 109.5 . . ?
C64 C67B H67E 109.5 . . ?
H67D C67B H67E 109.5 . . ?
C64 C67B H67F 109.5 . . ?
H67D C67B H67F 109.5 . . ?
H67E C67B H67F 109.5 . . ?
C64 C65B H65D 109.5 . . ?
C64 C65B H65E 109.5 . . ?
H65D C65B H65E 109.5 . . ?
C64 C65B H65F 109.5 . . ?
H65D C65B H65F 109.5 . . ?
H65E C65B H65F 109.5 . . ?
O8 C68 C63 108.4(3) . . ?
O8 C68 H68A 110.0 . . ?
C63 C68 H68A 110.0 . . ?
O8 C68 H68B 110.0 . . ?
C63 C68 H68B 110.0 . . ?
H68A C68 H68B 108.4 . . ?
N1 C70 C75 120.5(4) . . ?
N1 C70 C71 119.9(3) . . ?
C75 C70 C71 119.5(4) . . ?
C72 C71 C70 119.8(4) . . ?
C72 C71 H71 120.1 . . ?
C70 C71 H71 120.1 . . ?
C71 C72 C73 121.5(4) . . ?
C71 C72 H72 119.3 . . ?
C73 C72 H72 119.3 . . ?
C74 C73 C72 117.7(4) . . ?
C74 C73 C76 121.5(5) . . ?
C72 C73 C76 120.8(5) . . ?
C75 C74 C73 122.2(4) . . ?
C75 C74 H74 118.9 . . ?
C73 C74 H74 118.9 . . ?
C74 C75 C70 119.2(4) . . ?
C74 C75 H75 120.4 . . ?
C70 C75 H75 120.4 . . ?
C73 C76 H76A 109.5 . . ?
C73 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C73 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N2 C77 C78 120.8(4) . . ?
N2 C77 C82 119.3(4) . . ?
C78 C77 C82 119.9(4) . . ?
C79 C78 C77 119.1(4) . . ?
C79 C78 H78 120.5 . . ?
C77 C78 H78 120.5 . . ?
C78 C79 C80 121.1(4) . . ?
C78 C79 H79 119.4 . . ?
C80 C79 H79 119.4 . . ?
C81 C80 C79 118.5(4) . . ?
C81 C80 C83 120.6(4) . . ?
C79 C80 C83 120.8(4) . . ?
C80 C81 C82 122.2(4) . . ?
C80 C81 H81 118.9 . . ?
C82 C81 H81 118.9 . . ?
C81 C82 C77 119.1(4) . . ?
C81 C82 H82 120.4 . . ?
C77 C82 H82 120.4 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
O9 C101 C102 119.7(3) . . ?
O9 C101 C106 118.5(4) . . ?
C102 C101 C106 121.8(4) . . ?
C101 C102 C103 118.2(4) . . ?
C101 C102 C107 120.3(4) . . ?
C103 C102 C107 121.5(4) . . ?
C104 C103 C102 121.8(4) . . ?
C104 C103 H103 119.1 . . ?
C102 C103 H103 119.1 . . ?
C105 C104 C103 117.3(4) . . ?
C105 C104 C108 119.9(4) . . ?
C103 C104 C108 122.7(5) . . ?
C106 C105 C104 123.0(4) . . ?
C106 C105 H105 118.5 . . ?
C104 C105 H105 118.5 . . ?
C105 C106 C101 117.9(4) . . ?
C105 C106 C169 122.5(4) . . ?
C101 C106 C169 119.6(4) . . ?
O16 C107 C102 108.4(3) . . ?
O16 C107 H10D 110.0 . . ?
C102 C107 H10D 110.0 . . ?
O16 C107 H10E 110.0 . . ?
C102 C107 H10E 110.0 . . ?
H10D C107 H10E 108.4 . . ?
C110 C108 C111 116.3(6) . . ?
C110 C108 C104 113.8(5) . . ?
C111 C108 C104 111.1(5) . . ?
C110 C108 C109 101.9(6) . . ?
C111 C108 C109 105.1(6) . . ?
C104 C108 C109 107.3(5) . . ?
C108 C109 H10F 109.5 . . ?
C108 C109 H10G 109.5 . . ?
H10F C109 H10G 109.5 . . ?
C108 C109 H10H 109.5 . . ?
H10F C109 H10H 109.5 . . ?
H10G C109 H10H 109.5 . . ?
C108 C110 H11D 109.5 . . ?
C108 C110 H11E 109.5 . . ?
H11D C110 H11E 109.5 . . ?
C108 C110 H11F 109.5 . . ?
H11D C110 H11F 109.5 . . ?
H11E C110 H11F 109.5 . . ?
C108 C111 H11G 109.5 . . ?
C108 C111 H11H 109.5 . . ?
H11G C111 H11H 109.5 . . ?
C108 C111 H11I 109.5 . . ?
H11G C111 H11I 109.5 . . ?
H11H C111 H11I 109.5 . . ?
C106 C169 C114 110.9(3) . . ?
C106 C169 H16A 109.5 . . ?
C114 C169 H16A 109.5 . . ?
C106 C169 H16B 109.5 . . ?
C114 C169 H16B 109.5 . . ?
H16A C169 H16B 108.0 . . ?
O10 C113 C118 121.2(4) . . ?
O10 C113 C114 119.1(3) . . ?
C118 C113 C114 119.8(4) . . ?
C115 C114 C113 118.9(4) . . ?
C115 C114 C169 118.5(4) . . ?
C113 C114 C169 122.5(4) . . ?
C116 C115 C114 122.7(4) . . ?
C116 C115 H115 118.7 . . ?
C114 C115 H115 118.7 . . ?
C115 C116 C117 117.0(4) . . ?
C115 C116 C119 121.9(4) . . ?
C117 C116 C119 121.1(4) . . ?
C116 C117 C118 122.2(4) . . ?
C116 C117 H117 118.9 . . ?
C118 C117 H117 118.9 . . ?
C117 C118 C113 119.3(4) . . ?
C117 C118 C123 117.4(4) . . ?
C113 C118 C123 123.2(4) . . ?
C12A C119 C12C 110.3(7) . . ?
C12E C119 C12D 122.7(9) . . ?
C12E C119 C116 114.7(7) . . ?
C12A C119 C116 114.8(6) . . ?
C12C C119 C116 111.5(6) . . ?
C12D C119 C116 111.7(7) . . ?
C12A C119 C12B 108.9(7) . . ?
C12C C119 C12B 102.6(7) . . ?
C116 C119 C12B 107.9(6) . . ?
C12E C119 C12F 97.7(8) . . ?
C12D C119 C12F 103.0(8) . . ?
C116 C119 C12F 102.8(6) . . ?
C119 C12D H12C 109.5 . . ?
C119 C12D H12D 109.5 . . ?
H12C C12D H12D 109.5 . . ?
C119 C12D H12E 109.5 . . ?
H12C C12D H12E 109.5 . . ?
H12D C12D H12E 109.5 . . ?
C119 C12E H12F 109.5 . . ?
C119 C12E H12G 109.5 . . ?
H12F C12E H12G 109.5 . . ?
C119 C12E H12H 109.5 . . ?
H12F C12E H12H 109.5 . . ?
H12G C12E H12H 109.5 . . ?
C119 C12F H12I 109.5 . . ?
C119 C12F H12J 109.5 . . ?
H12I C12F H12J 109.5 . . ?
C119 C12F H12K 109.5 . . ?
H12I C12F H12K 109.5 . . ?
H12J C12F H12K 109.5 . . ?
C119 C12A H12L 109.5 . . ?
C119 C12A H12M 109.5 . . ?
H12L C12A H12M 109.5 . . ?
C119 C12A H12N 109.5 . . ?
H12L C12A H12N 109.5 . . ?
H12M C12A H12N 109.5 . . ?
C119 C12C H12O 109.5 . . ?
C119 C12C H12P 109.5 . . ?
H12O C12C H12P 109.5 . . ?
C119 C12C H12Q 109.5 . . ?
H12O C12C H12Q 109.5 . . ?
H12P C12C H12Q 109.5 . . ?
C119 C12B H12R 109.5 . . ?
C119 C12B H12S 109.5 . . ?
H12R C12B H12S 109.5 . . ?
C119 C12B H12T 109.5 . . ?
H12R C12B H12T 109.5 . . ?
H12S C12B H12T 109.5 . . ?
C118 C123 C125 112.6(3) . . ?
C118 C123 H12U 109.1 . . ?
C125 C123 H12U 109.1 . . ?
C118 C123 H12V 109.1 . . ?
C125 C123 H12V 109.1 . . ?
H12U C123 H12V 107.8 . . ?
O11 C124 C125 118.3(4) . . ?
O11 C124 C129 120.6(4) . . ?
C125 C124 C129 121.1(4) . . ?
C126 C125 C124 118.5(4) . . ?
C126 C125 C123 121.7(4) . . ?
C124 C125 C123 119.9(4) . . ?
C125 C126 C127 121.8(4) . . ?
C125 C126 H126 119.1 . . ?
C127 C126 H126 119.1 . . ?
C128 C127 C126 117.5(5) . . ?
C128 C127 C130 121.0(5) . . ?
C126 C127 C130 121.5(5) . . ?
C129 C128 C127 122.3(5) . . ?
C129 C128 H128 118.8 . . ?
C127 C128 H128 118.8 . . ?
C128 C129 C124 118.5(4) . . ?
C128 C129 C134 122.6(4) . . ?
C124 C129 C134 118.7(4) . . ?
C13E C130 C127 120.8(9) . . ?
C13C C130 C127 119.5(9) . . ?
C13C C130 C13A 108.1(9) . . ?
C127 C130 C13A 109.9(8) . . ?
C13E C130 C13D 116.7(11) . . ?
C127 C130 C13D 114.4(7) . . ?
C13C C130 C13B 99.9(8) . . ?
C127 C130 C13B 106.3(9) . . ?
C13A C130 C13B 112.9(9) . . ?
C13E C130 C13F 95.2(9) . . ?
C127 C130 C13F 95.0(8) . . ?
C13D C130 C13F 108.8(9) . . ?
C130 C13D H13A 109.5 . . ?
C130 C13D H13B 109.5 . . ?
H13A C13D H13B 109.5 . . ?
C130 C13D H13C 109.5 . . ?
H13A C13D H13C 109.5 . . ?
H13B C13D H13C 109.5 . . ?
C130 C13F H13D 109.5 . . ?
C130 C13F H13E 109.5 . . ?
H13D C13F H13E 109.5 . . ?
C130 C13F H13F 109.5 . . ?
H13D C13F H13F 109.5 . . ?
H13E C13F H13F 109.5 . . ?
C130 C13E H13G 109.5 . . ?
C130 C13E H13H 109.5 . . ?
H13G C13E H13H 109.5 . . ?
C130 C13E H13I 109.5 . . ?
H13G C13E H13I 109.5 . . ?
H13H C13E H13I 109.5 . . ?
C130 C13A H13J 109.5 . . ?
C130 C13A H13K 109.5 . . ?
H13J C13A H13K 109.5 . . ?
C130 C13A H13L 109.5 . . ?
H13J C13A H13L 109.5 . . ?
H13K C13A H13L 109.5 . . ?
C130 C13C H13M 109.5 . . ?
C130 C13C H13N 109.5 . . ?
H13M C13C H13N 109.5 . . ?
C130 C13C H13O 109.5 . . ?
H13M C13C H13O 109.5 . . ?
H13N C13C H13O 109.5 . . ?
C130 C13B H13P 109.5 . . ?
C130 C13B H13Q 109.5 . . ?
H13P C13B H13Q 109.5 . . ?
C130 C13B H13R 109.5 . . ?
H13P C13B H13R 109.5 . . ?
H13Q C13B H13R 109.5 . . ?
O12 C134 C129 109.4(4) . . ?
O12 C134 H13S 109.8 . . ?
C129 C134 H13S 109.8 . . ?
O12 C134 H13T 109.8 . . ?
C129 C134 H13T 109.8 . . ?
H13S C134 H13T 108.3 . . ?
O12 C135 C137 109.7(4) . . ?
O12 C135 H13U 109.7 . . ?
C137 C135 H13U 109.7 . . ?
O12 C135 H13V 109.7 . . ?
C137 C135 H13V 109.7 . . ?
H13U C135 H13V 108.2 . . ?
O13 C136 C137 120.5(4) . . ?
O13 C136 C141 118.0(4) . . ?
C137 C136 C141 121.4(4) . . ?
C136 C137 C138 118.7(4) . . ?
C136 C137 C135 119.1(4) . . ?
C138 C137 C135 122.2(4) . . ?
C137 C138 C139 121.9(4) . . ?
C137 C138 H138 119.1 . . ?
C139 C138 H138 119.1 . . ?
C140 C139 C138 117.4(5) . . ?
C140 C139 C142 118.9(5) . . ?
C138 C139 C142 123.7(5) . . ?
C139 C140 C141 122.9(4) . . ?
C139 C140 H140 118.6 . . ?
C141 C140 H140 118.6 . . ?
C140 C141 C136 117.8(4) . . ?
C140 C141 C146 121.7(4) . . ?
C136 C141 C146 120.4(4) . . ?
C145 C142 C139 112.8(5) . . ?
C145 C142 C144 109.5(6) . . ?
C139 C142 C144 110.3(4) . . ?
C145 C142 C143 108.0(5) . . ?
C139 C142 C143 108.9(5) . . ?
C144 C142 C143 107.1(5) . . ?
C142 C143 H14A 109.5 . . ?
C142 C143 H14B 109.5 . . ?
H14A C143 H14B 109.5 . . ?
C142 C143 H14C 109.5 . . ?
H14A C143 H14C 109.5 . . ?
H14B C143 H14C 109.5 . . ?
C142 C144 H14D 109.5 . . ?
C142 C144 H14E 109.5 . . ?
H14D C144 H14E 109.5 . . ?
C142 C144 H14F 109.5 . . ?
H14D C144 H14F 109.5 . . ?
H14E C144 H14F 109.5 . . ?
C142 C145 H14G 109.5 . . ?
C142 C145 H14H 109.5 . . ?
H14G C145 H14H 109.5 . . ?
C142 C145 H14I 109.5 . . ?
H14G C145 H14I 109.5 . . ?
H14H C145 H14I 109.5 . . ?
C148 C146 C141 110.8(4) . . ?
C148 C146 H14J 109.5 . . ?
C141 C146 H14J 109.5 . . ?
C148 C146 H14K 109.5 . . ?
C141 C146 H14K 109.5 . . ?
H14J C146 H14K 108.1 . . ?
O14 C147 C152 120.7(3) . . ?
O14 C147 C148 119.4(4) . . ?
C152 C147 C148 119.9(4) . . ?
C149 C148 C147 119.0(4) . . ?
C149 C148 C146 119.0(4) . . ?
C147 C148 C146 122.0(4) . . ?
C150 C149 C148 122.8(4) . . ?
C150 C149 H149 118.6 . . ?
C148 C149 H149 118.6 . . ?
C149 C150 C151 116.8(4) . . ?
C149 C150 C153 120.2(4) . . ?
C151 C150 C153 122.9(4) . . ?
C150 C151 C152 122.6(4) . . ?
C150 C151 H151 118.7 . . ?
C152 C151 H151 118.7 . . ?
C151 C152 C147 118.8(4) . . ?
C151 C152 C157 118.5(4) . . ?
C147 C152 C157 122.7(4) . . ?
C156 C153 C154 111.6(6) . . ?
C156 C153 C150 112.4(4) . . ?
C154 C153 C150 109.1(4) . . ?
C156 C153 C155 106.9(6) . . ?
C154 C153 C155 105.6(5) . . ?
C150 C153 C155 111.0(4) . . ?
C153 C154 H15A 109.5 . . ?
C153 C154 H15B 109.5 . . ?
H15A C154 H15B 109.5 . . ?
C153 C154 H15C 109.5 . . ?
H15A C154 H15C 109.5 . . ?
H15B C154 H15C 109.5 . . ?
C153 C155 H15D 109.5 . . ?
C153 C155 H15E 109.5 . . ?
H15D C155 H15E 109.5 . . ?
C153 C155 H15F 109.5 . . ?
H15D C155 H15F 109.5 . . ?
H15E C155 H15F 109.5 . . ?
C153 C156 H15G 109.5 . . ?
C153 C156 H15H 109.5 . . ?
H15G C156 H15H 109.5 . . ?
C153 C156 H15I 109.5 . . ?
H15G C156 H15I 109.5 . . ?
H15H C156 H15I 109.5 . . ?
C152 C157 C159 113.5(3) . . ?
C152 C157 H15J 108.9 . . ?
C159 C157 H15J 108.9 . . ?
C152 C157 H15K 108.9 . . ?
C159 C157 H15K 108.9 . . ?
H15J C157 H15K 107.7 . . ?
O15 C158 C163 120.8(4) . . ?
O15 C158 C159 118.3(3) . . ?
C163 C158 C159 120.9(4) . . ?
C160 C159 C158 118.4(4) . . ?
C160 C159 C157 122.1(4) . . ?
C158 C159 C157 119.4(3) . . ?
C159 C160 C161 122.7(4) . . ?
C159 C160 H160 118.6 . . ?
C161 C160 H160 118.6 . . ?
C160 C161 C162 117.8(4) . . ?
C160 C161 C164 119.7(4) . . ?
C162 C161 C164 122.5(4) . . ?
C161 C162 C163 121.7(4) . . ?
C161 C162 H162 119.1 . . ?
C163 C162 H162 119.1 . . ?
C158 C163 C162 118.5(4) . . ?
C158 C163 C168 119.4(4) . . ?
C162 C163 C168 122.1(4) . . ?
C165 C164 C166 108.3(4) . . ?
C165 C164 C161 109.5(4) . . ?
C166 C164 C161 112.6(4) . . ?
C165 C164 C167 110.0(5) . . ?
C166 C164 C167 107.8(4) . . ?
C161 C164 C167 108.6(4) . . ?
C164 C165 H16C 109.5 . . ?
C164 C165 H16D 109.5 . . ?
H16C C165 H16D 109.5 . . ?
C164 C165 H16E 109.5 . . ?
H16C C165 H16E 109.5 . . ?
H16D C165 H16E 109.5 . . ?
C164 C166 H16F 109.5 . . ?
C164 C166 H16G 109.5 . . ?
H16F C166 H16G 109.5 . . ?
C164 C166 H16H 109.5 . . ?
H16F C166 H16H 109.5 . . ?
H16G C166 H16H 109.5 . . ?
C164 C167 H16I 109.5 . . ?
C164 C167 H16J 109.5 . . ?
H16I C167 H16J 109.5 . . ?
C164 C167 H16K 109.5 . . ?
H16I C167 H16K 109.5 . . ?
H16J C167 H16K 109.5 . . ?
O16 C168 C163 109.6(3) . . ?
O16 C168 H16Q 109.7 . . ?
C163 C168 H16Q 109.7 . . ?
O16 C168 H16R 109.7 . . ?
C163 C168 H16R 109.7 . . ?
H16Q C168 H16R 108.2 . . ?
N3 C170 C171 120.3(4) . . ?
N3 C170 C175 119.9(4) . . ?
C171 C170 C175 119.7(4) . . ?
C170 C171 C172 119.1(4) . . ?
C170 C171 H171 120.4 . . ?
C172 C171 H171 120.4 . . ?
C171 C172 C173 121.6(4) . . ?
C171 C172 H172 119.2 . . ?
C173 C172 H172 119.2 . . ?
C174 C173 C172 118.2(4) . . ?
C174 C173 C176 121.3(5) . . ?
C172 C173 C176 120.5(4) . . ?
C175 C174 C173 121.2(5) . . ?
C175 C174 H174 119.4 . . ?
C173 C174 H174 119.4 . . ?
C174 C175 C170 120.1(4) . . ?
C174 C175 H175 120.0 . . ?
C170 C175 H175 120.0 . . ?
C173 C176 H17A 109.5 . . ?
C173 C176 H17B 109.5 . . ?
H17A C176 H17B 109.5 . . ?
C173 C176 H17C 109.5 . . ?
H17A C176 H17C 109.5 . . ?
H17B C176 H17C 109.5 . . ?
N4 C177 C178 119.7(5) . . ?
N4 C177 C182 120.4(5) . . ?
C178 C177 C182 119.9(5) . . ?
C179 C178 C177 119.1(6) . . ?
C179 C178 H178 120.4 . . ?
C177 C178 H178 120.4 . . ?
C180 C179 C178 122.0(6) . . ?
C180 C179 H179 119.0 . . ?
C178 C179 H179 119.0 . . ?
C179 C180 C181 117.6(6) . . ?
C179 C180 C183 122.1(7) . . ?
C181 C180 C183 120.2(7) . . ?
C182 C181 C180 121.9(6) . . ?
C182 C181 H181 119.1 . . ?
C180 C181 H181 119.1 . . ?
C181 C182 C177 119.5(5) . . ?
C181 C182 H182 120.3 . . ?
C177 C182 H182 120.3 . . ?
C180 C183 H18A 109.5 . . ?
C180 C183 H18B 109.5 . . ?
H18A C183 H18B 109.5 . . ?
C180 C183 H18C 109.5 . . ?
H18A C183 H18C 109.5 . . ?
H18B C183 H18C 109.5 . . ?
C201 C200 H20D 109.5 . . ?
C201 C200 H20E 109.5 . . ?
H20D C200 H20E 109.5 . . ?
C201 C200 H20F 109.5 . . ?
H20D C200 H20F 109.5 . . ?
H20E C200 H20F 109.5 . . ?
N200 C201 C200 179.0(8) . . ?
N210 C210 C211 162(2) . . ?
C210 C211 H21D 109.5 . . ?
C210 C211 H21E 109.5 . . ?
H21D C211 H21E 109.5 . . ?
C210 C211 H21F 109.5 . . ?
H21D C211 H21F 109.5 . . ?
H21E C211 H21F 109.5 . . ?
N220 C220 C221 179.3(8) . . ?
C220 C221 H22D 109.5 . . ?
C220 C221 H22E 109.5 . . ?
H22D C221 H22E 109.5 . . ?
C220 C221 H22F 109.5 . . ?
H22D C221 H22F 109.5 . . ?
H22E C221 H22F 109.5 . . ?
N230 C230 C231 178.1(6) . . ?
C230 C231 H23C 109.5 . . ?
C230 C231 H23D 109.5 . . ?
H23C C231 H23D 109.5 . . ?
C230 C231 H23E 109.5 . . ?
H23C C231 H23E 109.5 . . ?
H23D C231 H23E 109.5 . . ?
N240 C240 C241 165.3(9) . . ?
N260 C260 C261 170.6(15) . . ?
C260 C261 H26A 109.5 . . ?
C260 C261 H26B 109.5 . . ?
H26A C261 H26B 109.5 . . ?
C260 C261 H26C 109.5 . . ?
H26A C261 H26C 109.5 . . ?
H26B C261 H26C 109.5 . . ?
N250 C250 C251 165.5(18) . . ?
C250 C251 H25A 109.5 . . ?
C250 C251 H25B 109.5 . . ?
H25A C251 H25B 109.5 . . ?
C250 C251 H25C 109.5 . . ?
H25A C251 H25C 109.5 . . ?
H25B C251 H25C 109.5 . . ?
C70 N1 V1 173.7(3) . . ?
C77 N2 V2 174.4(3) . . ?
C170 N3 V3 178.0(3) . . ?
C177 N4 V4 178.6(3) . . ?
C1 O1 V1 123.2(2) . . ?
C13 O2 V2 120.1(2) . . ?
C13 O2 V1 128.4(2) . . ?
V2 O2 V1 108.34(11) . . ?
C24 O3 V2 127.8(2) . . ?
C35 O4 C34 112.8(3) . . ?
C36 O5 V2 124.8(2) . . ?
C47 O6 V1 119.0(2) . . ?
C47 O6 V2 127.8(2) . . ?
V1 O6 V2 110.10(11) . . ?
C58 O7 V1 129.3(2) . . ?
C68 O8 C7 112.7(3) . . ?
C101 O9 V3 132.5(2) . . ?
C113 O10 V3 119.4(2) . . ?
C113 O10 V4 128.4(2) . . ?
V3 O10 V4 108.97(12) . . ?
C124 O11 V4 126.4(3) . . ?
C135 O12 C134 111.1(4) . . ?
C136 O13 V4 131.6(3) . . ?
C147 O14 V4 120.9(2) . . ?
C147 O14 V3 127.3(2) . . ?
V4 O14 V3 108.97(12) . . ?
C158 O15 V3 123.4(2) . . ?
C168 O16 C107 112.6(3) . . ?
N1 V1 O7 102.25(14) . . ?
N1 V1 O1 98.91(13) . . ?
O7 V1 O1 103.78(12) . . ?
N1 V1 O6 93.59(13) . . ?
O7 V1 O6 99.62(11) . . ?
O1 V1 O6 150.36(11) . . ?
N1 V1 O2 135.83(14) . . ?
O7 V1 O2 120.51(11) . . ?
O1 V1 O2 82.23(11) . . ?
O6 V1 O2 70.23(10) . . ?
N2 V2 O3 104.37(14) . . ?
N2 V2 O5 99.82(14) . . ?
O3 V2 O5 103.24(12) . . ?
N2 V2 O2 92.43(14) . . ?
O3 V2 O2 98.16(12) . . ?
O5 V2 O2 151.73(11) . . ?
N2 V2 O6 135.33(13) . . ?
O3 V2 O6 118.69(12) . . ?
O5 V2 O6 82.24(11) . . ?
O2 V2 O6 71.29(10) . . ?
N3 V3 O9 105.29(16) . . ?
N3 V3 O15 98.30(14) . . ?
O9 V3 O15 102.31(12) . . ?
N3 V3 O10 92.50(14) . . ?
O9 V3 O10 98.62(12) . . ?
O15 V3 O10 152.92(12) . . ?
N3 V3 O14 133.69(15) . . ?
O9 V3 O14 119.57(12) . . ?
O15 V3 O14 83.65(11) . . ?
O10 V3 O14 71.08(11) . . ?
N4 V4 O13 105.39(17) . . ?
N4 V4 O11 99.76(16) . . ?
O13 V4 O11 101.21(13) . . ?
N4 V4 O14 93.28(15) . . ?
O13 V4 O14 98.50(12) . . ?
O11 V4 O14 152.47(13) . . ?
N4 V4 O10 133.67(14) . . ?
O13 V4 O10 119.54(14) . . ?
O11 V4 O10 82.93(12) . . ?
O14 V4 O10 70.64(11) . . ?
Cl1 C300 Cl2 128.5(8) . . ?
Cl1 C300 H30A 105.2 . . ?
Cl2 C300 H30A 105.2 . . ?
Cl1 C300 H30B 105.2 . . ?
Cl2 C300 H30B 105.2 . . ?
H30A C300 H30B 105.9 . . ?

_refine_diff_density_max         2.043
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.100

