 
data_a01_sq
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C33 H92 N8 O28 V8' 
_chemical_formula_weight          1456.66

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'
 
_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                    14.200(7)
_cell_length_b                    14.687(7)
_cell_length_c                    16.060(8)
_cell_angle_alpha                 63.058(5)
_cell_angle_beta                  86.238(5)
_cell_angle_gamma                 87.833(5)
_cell_volume                      2979(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     4289
_cell_measurement_theta_min       2.19
_cell_measurement_theta_max       25.27
 
_exptl_crystal_description        block-shaped
_exptl_crystal_colour             black
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.624          
_exptl_crystal_F_000              1508
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.130
_exptl_crystal_size_mid           0.120
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     1.282
_shelx_estimated_absorpt_T_min    0.851
_shelx_estimated_absorpt_T_max    0.861
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.851
_exptl_absorpt_correction_T_max   0.861
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker Apex2 CCD'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             19981
_diffrn_reflns_av_unetI/netI      0.1239
_diffrn_reflns_av_R_equivalents   0.0948
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.424
_diffrn_reflns_theta_max          25.024
_diffrn_reflns_theta_full         25.024
_diffrn_measured_fraction_theta_max   0.981
_diffrn_measured_fraction_theta_full  0.981
_diffrn_reflns_Laue_measured_fraction_max    0.981
_diffrn_reflns_Laue_measured_fraction_full   0.981
_diffrn_reflns_point_group_measured_fraction_max   0.981
_diffrn_reflns_point_group_measured_fraction_full  0.981
_reflns_number_total              10336
_reflns_number_gt                 6542
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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        'APEX2 (Bruker, 2005)' 
_computing_cell_refinement        'SAINT (Bruker, 2005)'
_computing_data_reduction         'SAINT' 
_computing_structure_solution     'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material   '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)+(0.1660P)²+5.5141P] 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          10336
_refine_ls_number_parameters      694
_refine_ls_number_restraints      113
_refine_ls_R_factor_all           0.1462
_refine_ls_R_factor_gt            0.0975
_refine_ls_wR_factor_ref          0.2981
_refine_ls_wR_factor_gt           0.2715
_refine_ls_goodness_of_fit_ref    1.073
_refine_ls_restrained_S_all       1.087
_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
V1 V 0.13857(10) 0.60984(12) 0.82649(10) 0.0230(4) Uani 1 1 d . . . . .
V2 V 0.20059(11) 0.61348(12) 0.61399(10) 0.0241(4) Uani 1 1 d . . . . .
V3 V 0.34462(10) 0.52964(12) 0.75129(10) 0.0231(4) Uani 1 1 d . . . . .
V4 V 0.26543(11) 0.77445(11) 0.70335(10) 0.0233(4) Uani 1 1 d . . . . .
V5 V 0.32743(10) 0.54518(12) 0.94103(10) 0.0241(4) Uani 1 1 d . . . . .
V6 V 0.08738(11) 0.43206(12) 0.78102(11) 0.0267(4) Uani 1 1 d . . . . .
V7 V 0.44491(11) 0.73390(12) 0.59611(11) 0.0281(4) Uani 1 1 d . . . . .
V8 V 0.09324(11) 0.81958(12) 0.57230(11) 0.0281(4) Uani 1 1 d . . . . .
O1 O 0.2120(4) 0.5158(4) 0.7489(4) 0.0222(13) Uani 1 1 d . . . . .
O2 O 0.2764(4) 0.6478(4) 0.8080(4) 0.0232(13) Uani 1 1 d . . . . .
O3 O 0.2180(4) 0.8697(4) 0.5775(4) 0.0266(14) Uani 1 1 d . . . . .
O4 O 0.1459(4) 0.7084(5) 0.6995(4) 0.0247(14) Uani 1 1 d . . . . .
O5 O 0.3126(4) 0.6579(4) 0.6348(4) 0.0238(13) Uani 1 1 d . . . . .
O6 O 0.1933(4) 0.5052(5) 0.9457(4) 0.0255(14) Uani 1 1 d . . . . .
O7 O 0.3826(4) 0.8030(5) 0.6654(4) 0.0278(14) Uani 1 1 d . . . . .
O8 O 0.4631(4) 0.6099(5) 0.7186(4) 0.0253(14) Uani 1 1 d . . . . .
O9 O 0.0888(4) 0.6783(5) 0.8730(4) 0.0256(14) Uani 1 1 d . . . . .
O10 O 0.0515(4) 0.5289(5) 0.8292(4) 0.0254(14) Uani 1 1 d . . . . .
O11 O 0.1518(4) 0.7268(5) 0.5283(4) 0.0302(15) Uani 1 1 d . . . . .
O12 O 0.0743(4) 0.5439(5) 0.6518(4) 0.0263(14) Uani 1 1 d . . . . .
O13 O 0.2347(4) 0.8476(5) 0.7511(4) 0.0302(15) Uani 1 1 d . . . . .
O14 O 0.3619(4) 0.4692(4) 0.8696(4) 0.0235(13) Uani 1 1 d . . . . .
O15 O 0.2399(5) 0.5515(5) 0.5572(4) 0.0299(15) Uani 1 1 d . . . . .
O16 O -0.0095(4) 0.3697(5) 0.7976(5) 0.0386(17) Uani 1 1 d . . . . .
O17 O 0.3821(4) 0.4508(5) 0.7126(4) 0.0284(14) Uani 1 1 d . . . . .
O18 O 0.3604(4) 0.4695(5) 1.0440(4) 0.0312(15) Uani 1 1 d . . . . .
O19 O 0.0569(5) 0.9090(5) 0.4757(5) 0.0380(17) Uani 1 1 d . . . . .
O20 O 0.5494(5) 0.7817(5) 0.5737(5) 0.0370(16) Uani 1 1 d . . . . .
O1A O 0.6594(7) 0.5845(9) 0.4958(10) 0.096(4) Uani 1 1 d D . . . .
O2A O -0.1927(6) 0.3577(9) 0.8502(8) 0.083(3) Uani 1 1 d D . . . .
O3A O -0.0022(6) 0.7878(7) 0.9508(6) 0.065(2) Uani 1 1 d D . . . .
N1 N 0.4507(5) 0.6371(6) 0.8895(5) 0.0292(18) Uani 1 1 d . . . . .
H1A H 0.499457 0.602263 0.921953 0.035 Uiso 1 1 calc R U . . .
H1B H 0.463426 0.650915 0.829933 0.035 Uiso 1 1 calc R U . . .
N2 N 0.1516(6) 0.3316(6) 0.9053(5) 0.0304(18) Uani 1 1 d . . . . .
H2A H 0.183852 0.367635 0.925731 0.036 Uiso 1 1 calc R U . . .
H2B H 0.107157 0.297332 0.949137 0.036 Uiso 1 1 calc R U . . .
N3 N 0.3829(6) 0.8355(6) 0.4702(5) 0.0341(19) Uani 1 1 d . . . . .
H3A H 0.324329 0.850895 0.483129 0.041 Uiso 1 1 calc R U . . .
H3B H 0.415735 0.893092 0.442964 0.041 Uiso 1 1 calc R U . . .
N4 N 0.0255(5) 0.8805(6) 0.6595(6) 0.0321(19) Uani 1 1 d . . . . .
H4A H 0.058276 0.862143 0.710134 0.039 Uiso 1 1 calc R U . . .
H4B H 0.025338 0.948400 0.628577 0.039 Uiso 1 1 calc R U . . .
N5 N 0.2864(5) 0.6674(6) 0.9745(5) 0.0304(18) Uani 1 1 d . . . . .
H5A H 0.249325 0.711693 0.931416 0.036 Uiso 1 1 calc R U . . .
H5B H 0.254585 0.642920 1.029772 0.036 Uiso 1 1 calc R U . . .
N6 N 0.1708(6) 0.3417(6) 0.7304(6) 0.0319(18) Uani 1 1 d . . . . .
H6A H 0.137646 0.327686 0.692524 0.038 Uiso 1 1 calc R U . . .
H6B H 0.221908 0.376044 0.698141 0.038 Uiso 1 1 calc R U . . .
N7 N -0.0335(6) 0.7317(7) 0.6163(6) 0.039(2) Uani 1 1 d . U . . .
H7A H -0.060855 0.736655 0.566094 0.046 Uiso 1 1 calc R U . . .
H7B H -0.018706 0.666284 0.650977 0.046 Uiso 1 1 calc R U . . .
N8 N 0.4641(6) 0.6475(6) 0.5188(5) 0.0350(19) Uani 1 1 d . . . . .
H8A H 0.522740 0.622729 0.523726 0.042 Uiso 1 1 calc R U . . .
H8B H 0.424510 0.595138 0.542368 0.042 Uiso 1 1 calc R U . . .
C1 C 0.5501(6) 0.5544(7) 0.7394(6) 0.027(2) Uani 1 1 d . . . . .
H1C H 0.601579 0.601344 0.720484 0.041 Uiso 1 1 calc R U . . .
H1D H 0.550702 0.510558 0.805495 0.041 Uiso 1 1 calc R U . . .
H1E H 0.556618 0.513793 0.706372 0.041 Uiso 1 1 calc R U . . .
C2 C 0.2395(8) 0.9761(8) 0.5408(8) 0.047(3) Uani 1 1 d . . . . .
H2C H 0.304161 0.983328 0.550708 0.071 Uiso 1 1 calc R U . . .
H2D H 0.229639 1.010060 0.474988 0.071 Uiso 1 1 calc R U . . .
H2E H 0.199060 1.006155 0.572131 0.071 Uiso 1 1 calc R U . . .
C3 C 0.0256(7) 0.5256(8) 0.5846(6) 0.036(2) Uani 1 1 d . . . . .
H3C H 0.025588 0.586775 0.526248 0.055 Uiso 1 1 calc R U . . .
H3D H 0.057143 0.471764 0.575121 0.055 Uiso 1 1 calc R U . . .
H3E H -0.038269 0.506105 0.607668 0.055 Uiso 1 1 calc R U . . .
C4 C 0.1319(7) 0.4712(8) 1.0313(6) 0.035(2) Uani 1 1 d . . . . .
H4C H 0.070597 0.455544 1.019487 0.053 Uiso 1 1 calc R U . . .
H4D H 0.158674 0.411329 1.080038 0.053 Uiso 1 1 calc R U . . .
H4E H 0.126100 0.524539 1.050261 0.053 Uiso 1 1 calc R U . . .
C5 C 0.4392(7) 0.7344(9) 0.8964(8) 0.044(3) Uani 1 1 d . . . . .
H5C H 0.408375 0.782900 0.840109 0.052 Uiso 1 1 calc R U . . .
C6 C 0.3737(8) 0.7192(9) 0.9771(9) 0.047(3) Uani 1 1 d . . . . .
H6C H 0.405406 0.669652 1.032313 0.056 Uiso 1 1 calc R U . . .
C7 C 0.3583(8) 0.8109(8) 0.9919(8) 0.043(3) Uani 1 1 d . . . . .
H7C H 0.324463 0.792010 1.051798 0.052 Uiso 1 1 calc R U . . .
H7D H 0.319549 0.859712 0.943497 0.052 Uiso 1 1 calc R U . . .
C8 C -0.1346(8) 0.8846(10) 0.7396(9) 0.051(3) Uani 1 1 d . U . . .
H8C H -0.108231 0.866092 0.799487 0.061 Uiso 1 1 calc R U . . .
H8D H -0.134254 0.958552 0.705499 0.061 Uiso 1 1 calc R U . . .
C9 C 0.3687(10) 0.8666(9) 0.3044(8) 0.056(3) Uani 1 1 d . . . . .
H9A H 0.308052 0.900706 0.299995 0.067 Uiso 1 1 calc R U . . .
H9B H 0.417167 0.918121 0.285227 0.067 Uiso 1 1 calc R U . . .
C10 C 0.5329(8) 0.7811(9) 0.8964(8) 0.046(3) Uani 1 1 d . . . . .
H10A H 0.569832 0.795576 0.838858 0.055 Uiso 1 1 calc R U . . .
H10B H 0.568320 0.733444 0.948459 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4466(12) 0.7124(9) 0.4202(8) 0.070(5) Uani 1 1 d . . . . .
C12 C 0.4549(9) 0.6655(9) 0.3575(7) 0.049(3) Uani 1 1 d . . . . .
H12A H 0.408473 0.611713 0.378089 0.058 Uiso 1 1 calc R U . . .
H12B H 0.516838 0.633933 0.362256 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5138(10) 0.8808(10) 0.9050(9) 0.063(4) Uani 1 1 d . . . . .
H13A H 0.573079 0.908552 0.909504 0.075 Uiso 1 1 calc R U . . .
H13B H 0.484266 0.930763 0.849558 0.075 Uiso 1 1 calc R U . . .
C14 C -0.1962(8) 0.7268(10) 0.6921(10) 0.058(3) Uani 1 1 d . U . . .
H14A H -0.193045 0.653371 0.729836 0.070 Uiso 1 1 calc R U . . .
H14B H -0.223245 0.739466 0.633842 0.070 Uiso 1 1 calc R U . . .
C15 C 0.4507(9) 0.8605(11) 0.9898(9) 0.059(3) Uani 1 1 d . . . . .
H15A H 0.437282 0.924515 0.992134 0.071 Uiso 1 1 calc R U . . .
H15B H 0.483858 0.816363 1.045104 0.071 Uiso 1 1 calc R U . . .
C16 C 0.2351(9) 0.1619(9) 0.9777(8) 0.051(3) Uani 1 1 d . . . . .
H16A H 0.267703 0.178797 1.019995 0.061 Uiso 1 1 calc R U . . .
H16B H 0.175581 0.130692 1.008858 0.061 Uiso 1 1 calc R U . . .
C17 C -0.2625(10) 0.7692(12) 0.7418(11) 0.073(3) Uani 1 1 d . U . . .
H17A H -0.319117 0.791413 0.706870 0.087 Uiso 1 1 calc R U . . .
H17B H -0.280469 0.713483 0.802259 0.087 Uiso 1 1 calc R U . . .
C18 C 0.3807(11) 0.7905(10) 0.4058(8) 0.065(4) Uani 1 1 d . U . . .
H18A H 0.320555 0.754202 0.424070 0.078 Uiso 1 1 calc R U . . .
C19 C 0.1989(13) 0.2458(10) 0.8105(8) 0.082(5) Uani 1 1 d . . . . .
C20 C 0.2156(12) 0.2590(11) 0.8902(9) 0.076(5) Uani 1 1 d . . . . .
H20A H 0.276396 0.294084 0.873502 0.092 Uiso 1 1 calc R U . . .
C21 C 0.2592(10) 0.1764(10) 0.7891(9) 0.063(4) Uani 1 1 d . . . . .
H21A H 0.318361 0.210262 0.759859 0.076 Uiso 1 1 calc R U . . .
H21B H 0.229245 0.161500 0.744141 0.076 Uiso 1 1 calc R U . . .
C22 C 0.4412(12) 0.7383(11) 0.2563(8) 0.080(5) Uani 1 1 d . . . . .
H22A H 0.501980 0.767972 0.227577 0.096 Uiso 1 1 calc R U . . .
H22B H 0.422079 0.698889 0.225612 0.096 Uiso 1 1 calc R U . . .
C23 C -0.0712(10) 0.8449(12) 0.6881(11) 0.071(3) Uani 1 1 d . U . . .
C24 C 0.3741(14) 0.8207(14) 0.2369(11) 0.095(5) Uani 1 1 d . U . . .
H24A H 0.312019 0.795852 0.236050 0.113 Uiso 1 1 calc R U . . .
H24B H 0.389629 0.874563 0.174623 0.113 Uiso 1 1 calc R U . . .
C25 C 0.2941(12) 0.0858(13) 0.9573(11) 0.085(5) Uani 1 1 d . U . . .
H25A H 0.359855 0.102055 0.956034 0.102 Uiso 1 1 calc R U . . .
H25B H 0.283554 0.018849 1.009649 0.102 Uiso 1 1 calc R U . . .
C26 C 0.2801(12) 0.0774(12) 0.8730(11) 0.084(5) Uani 1 1 d . U . . .
H26A H 0.228306 0.031060 0.885164 0.100 Uiso 1 1 calc R U . . .
H26B H 0.336366 0.047095 0.857903 0.100 Uiso 1 1 calc R U . . .
C27 C -0.2326(11) 0.8518(13) 0.7575(12) 0.084(3) Uani 1 1 d . U . . .
H27A H -0.249458 0.834433 0.822412 0.100 Uiso 1 1 calc R U . . .
H27B H -0.270546 0.910978 0.719962 0.100 Uiso 1 1 calc R U . . .
C28 C -0.1010(9) 0.7650(11) 0.6706(11) 0.067(3) Uani 1 1 d . U . . .
C1A C 0.7341(17) 0.633(2) 0.514(2) 0.178(11) Uani 1 1 d D U . . .
C2A C -0.2265(13) 0.4425(16) 0.7710(14) 0.127(8) Uani 1 1 d D U . . .
C3A C 0.0643(12) 0.8614(14) 0.9494(16) 0.105(6) Uani 1 1 d D U . . .
O4A O 0.3784(10) 1.0192(11) 0.6901(11) 0.127(5) Uani 1 1 d D . . . .
O1W O 0.4781(13) 1.0310(11) 0.4018(15) 0.159(7) Uani 1 1 d . . . . .
O2W O 0.6888(17) 0.8049(18) 0.4422(14) 0.217(10) Uani 1 1 d . . . . .
O5A O 0.1109(12) 0.7872(18) 0.3467(12) 0.173(7) Uani 1 1 d D U . . .
C5A C 0.139(3) 0.690(2) 0.352(3) 0.205(14) Uani 1 1 d D U . . .
O3W O 0.9049(13) 0.7608(14) 0.3978(16) 0.210(9) Uani 1 1 d . U . . .
C4A C 0.466(2) 0.988(3) 0.649(3) 0.203(17) Uani 1 1 d 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
V1 O9 1.621(6) . ?
V1 O10 1.733(6) . ?
V1 O4 1.890(6) . ?
V1 O6 2.017(6) . ?
V1 O2 2.021(6) . ?
V1 O1 2.413(6) . ?
V1 V4 2.921(2) . ?
V2 O15 1.618(6) . ?
V2 O11 1.763(6) . ?
V2 O5 1.847(6) . ?
V2 O1 1.998(6) . ?
V2 O12 2.015(6) . ?
V2 O4 2.438(6) . ?
V2 V3 2.916(2) . ?
V3 O17 1.603(6) . ?
V3 O14 1.725(6) . ?
V3 O1 1.907(6) . ?
V3 O8 1.992(6) . ?
V3 O5 2.027(6) . ?
V3 O2 2.444(6) . ?
V4 O13 1.612(6) . ?
V4 O7 1.733(6) . ?
V4 O2 1.867(6) . ?
V4 O4 2.005(6) . ?
V4 O3 2.010(6) . ?
V5 O18 1.608(6) . ?
V5 O14 1.960(6) . ?
V5 O6 2.001(6) . ?
V5 N1 2.133(8) . ?
V5 O2 2.137(6) . ?
V5 N5 2.146(8) . ?
V6 O16 1.621(6) . ?
V6 O10 1.942(6) . ?
V6 O12 1.995(6) . ?
V6 O1 2.093(6) . ?
V6 N2 2.113(7) . ?
V6 N6 2.135(8) . ?
V7 O20 1.613(7) . ?
V7 O7 1.969(6) . ?
V7 O8 2.010(6) . ?
V7 N3 2.120(8) . ?
V7 O5 2.131(6) . ?
V7 N8 2.140(8) . ?
V8 O19 1.614(7) . ?
V8 O11 1.938(6) . ?
V8 O3 1.965(6) . ?
V8 O4 2.118(6) . ?
V8 N4 2.140(8) . ?
V8 N7 2.142(9) . ?
O3 C2 1.436(12) . ?
O6 C4 1.468(11) . ?
O8 C1 1.426(10) . ?
O12 C3 1.446(10) . ?
O1A C1A 1.419(18) . ?
O2A C2A 1.414(15) . ?
O3A C3A 1.453(14) . ?
N1 C5 1.485(13) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C20 1.467(13) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C18 1.459(13) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C23 1.458(15) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C6 1.492(12) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N6 C19 1.477(13) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N7 C28 1.469(14) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N8 C11 1.464(13) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C2 H2E 0.9600 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C5 C6 1.480(14) . ?
C5 C10 1.519(14) . ?
C5 H5C 0.9800 . ?
C6 C7 1.477(14) . ?
C6 H6C 0.9800 . ?
C7 C15 1.516(16) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 C27 1.457(18) . ?
C8 C23 1.460(16) . ?
C8 H8C 0.9700 . ?
C8 H8D 0.9700 . ?
C9 C24 1.511(17) . ?
C9 C18 1.518(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C13 1.544(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C18 1.398(17) . ?
C11 C12 1.452(15) . ?
C12 C22 1.508(16) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C15 1.496(17) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C28 1.443(17) . ?
C14 C17 1.488(16) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C25 1.511(18) . ?
C16 C20 1.514(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C27 1.431(19) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9800 . ?
C19 C20 1.415(17) . ?
C19 C21 1.451(17) . ?
C20 H20A 0.9800 . ?
C21 C26 1.504(19) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C24 1.44(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.411(18) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.44(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
O4A C4A 1.525(17) . ?
O1W C4A 1.21(3) 2_676 ?
O5A C5A 1.439(18) . ?
 
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
O9 V1 O10 105.5(3) . . ?
O9 V1 O4 99.7(3) . . ?
O10 V1 O4 102.6(3) . . ?
O9 V1 O6 95.1(3) . . ?
O10 V1 O6 93.8(3) . . ?
O4 V1 O6 154.0(3) . . ?
O9 V1 O2 104.5(3) . . ?
O10 V1 O2 149.3(3) . . ?
O4 V1 O2 78.7(2) . . ?
O6 V1 O2 77.0(2) . . ?
O9 V1 O1 176.9(3) . . ?
O10 V1 O1 75.3(2) . . ?
O4 V1 O1 77.2(2) . . ?
O6 V1 O1 87.8(2) . . ?
O2 V1 O1 75.2(2) . . ?
O9 V1 V4 92.7(2) . . ?
O10 V1 V4 144.2(2) . . ?
O4 V1 V4 42.94(17) . . ?
O6 V1 V4 115.49(19) . . ?
O2 V1 V4 39.36(16) . . ?
O1 V1 V4 85.16(15) . . ?
O15 V2 O11 104.5(3) . . ?
O15 V2 O5 100.5(3) . . ?
O11 V2 O5 102.5(3) . . ?
O15 V2 O1 105.2(3) . . ?
O11 V2 O1 149.0(3) . . ?
O5 V2 O1 80.4(2) . . ?
O15 V2 O12 95.0(3) . . ?
O11 V2 O12 92.4(3) . . ?
O5 V2 O12 154.9(2) . . ?
O1 V2 O12 76.6(2) . . ?
O15 V2 O4 178.4(3) . . ?
O11 V2 O4 75.8(2) . . ?
O5 V2 O4 77.9(2) . . ?
O1 V2 O4 74.7(2) . . ?
O12 V2 O4 86.6(2) . . ?
O15 V2 V3 93.5(2) . . ?
O11 V2 V3 144.7(2) . . ?
O5 V2 V3 43.57(18) . . ?
O1 V2 V3 40.51(17) . . ?
O12 V2 V3 116.31(18) . . ?
O4 V2 V3 85.43(14) . . ?
O17 V3 O14 105.5(3) . . ?
O17 V3 O1 99.7(3) . . ?
O14 V3 O1 102.1(3) . . ?
O17 V3 O8 96.0(3) . . ?
O14 V3 O8 94.1(3) . . ?
O1 V3 O8 153.4(3) . . ?
O17 V3 O5 104.3(3) . . ?
O14 V3 O5 149.7(3) . . ?
O1 V3 O5 78.3(2) . . ?
O8 V3 O5 77.1(2) . . ?
O17 V3 O2 176.0(3) . . ?
O14 V3 O2 75.9(2) . . ?
O1 V3 O2 76.4(2) . . ?
O8 V3 O2 87.5(2) . . ?
O5 V3 O2 74.7(2) . . ?
O17 V3 V2 92.6(2) . . ?
O14 V3 V2 143.6(2) . . ?
O1 V3 V2 42.89(18) . . ?
O8 V3 V2 115.37(18) . . ?
O5 V3 V2 38.91(18) . . ?
O2 V3 V2 84.17(14) . . ?
O13 V4 O7 105.2(3) . . ?
O13 V4 O2 101.7(3) . . ?
O7 V4 O2 101.6(3) . . ?
O13 V4 O4 105.3(3) . . ?
O7 V4 O4 148.6(3) . . ?
O2 V4 O4 79.6(3) . . ?
O13 V4 O3 94.9(3) . . ?
O7 V4 O3 93.1(3) . . ?
O2 V4 O3 154.0(3) . . ?
O4 V4 O3 76.8(2) . . ?
O13 V4 V1 94.3(2) . . ?
O7 V4 V1 143.4(2) . . ?
O2 V4 V1 43.34(19) . . ?
O4 V4 V1 39.94(17) . . ?
O3 V4 V1 116.07(19) . . ?
O18 V5 O14 103.0(3) . . ?
O18 V5 O6 103.1(3) . . ?
O14 V5 O6 88.3(2) . . ?
O18 V5 N1 98.5(3) . . ?
O14 V5 N1 92.6(3) . . ?
O6 V5 N1 157.6(3) . . ?
O18 V5 O2 176.6(3) . . ?
O14 V5 O2 79.6(2) . . ?
O6 V5 O2 74.7(2) . . ?
N1 V5 O2 83.5(3) . . ?
O18 V5 N5 94.9(3) . . ?
O14 V5 N5 161.5(3) . . ?
O6 V5 N5 92.3(3) . . ?
N1 V5 N5 80.0(3) . . ?
O2 V5 N5 82.7(3) . . ?
O16 V6 O10 102.5(3) . . ?
O16 V6 O12 101.4(3) . . ?
O10 V6 O12 88.8(2) . . ?
O16 V6 O1 175.7(3) . . ?
O10 V6 O1 79.7(2) . . ?
O12 V6 O1 74.9(2) . . ?
O16 V6 N2 98.3(3) . . ?
O10 V6 N2 92.7(3) . . ?
O12 V6 N2 159.4(3) . . ?
O1 V6 N2 85.2(3) . . ?
O16 V6 N6 95.5(3) . . ?
O10 V6 N6 161.6(3) . . ?
O12 V6 N6 91.9(3) . . ?
O1 V6 N6 82.7(3) . . ?
N2 V6 N6 80.4(3) . . ?
O20 V7 O7 101.8(3) . . ?
O20 V7 O8 100.5(3) . . ?
O7 V7 O8 88.9(3) . . ?
O20 V7 N3 99.0(3) . . ?
O7 V7 N3 92.3(3) . . ?
O8 V7 N3 159.8(3) . . ?
O20 V7 O5 174.7(3) . . ?
O7 V7 O5 79.9(2) . . ?
O8 V7 O5 74.4(2) . . ?
N3 V7 O5 85.9(3) . . ?
O20 V7 N8 96.9(3) . . ?
O7 V7 N8 160.6(3) . . ?
O8 V7 N8 92.5(3) . . ?
N3 V7 N8 79.9(3) . . ?
O5 V7 N8 81.9(3) . . ?
O19 V8 O11 100.6(3) . . ?
O19 V8 O3 101.9(3) . . ?
O11 V8 O3 90.3(3) . . ?
O19 V8 O4 176.8(3) . . ?
O11 V8 O4 80.9(2) . . ?
O3 V8 O4 75.2(2) . . ?
O19 V8 N4 95.2(3) . . ?
O11 V8 N4 162.7(3) . . ?
O3 V8 N4 93.2(3) . . ?
O4 V8 N4 83.7(3) . . ?
O19 V8 N7 97.3(4) . . ?
O11 V8 N7 91.2(3) . . ?
O3 V8 N7 160.1(3) . . ?
O4 V8 N7 85.5(3) . . ?
N4 V8 N7 79.8(3) . . ?
V3 O1 V2 96.6(3) . . ?
V3 O1 V6 153.7(3) . . ?
V2 O1 V6 102.4(2) . . ?
V3 O1 V1 105.8(2) . . ?
V2 O1 V1 102.3(2) . . ?
V6 O1 V1 87.8(2) . . ?
V4 O2 V1 97.3(3) . . ?
V4 O2 V5 154.5(3) . . ?
V1 O2 V5 101.4(3) . . ?
V4 O2 V3 106.7(3) . . ?
V1 O2 V3 101.2(2) . . ?
V5 O2 V3 86.6(2) . . ?
C2 O3 V8 123.3(6) . . ?
C2 O3 V4 117.4(6) . . ?
V8 O3 V4 106.4(3) . . ?
V1 O4 V4 97.1(2) . . ?
V1 O4 V8 155.9(3) . . ?
V4 O4 V8 101.1(3) . . ?
V1 O4 V2 104.8(3) . . ?
V4 O4 V2 101.5(2) . . ?
V8 O4 V2 87.0(2) . . ?
V2 O5 V3 97.5(3) . . ?
V2 O5 V7 155.6(3) . . ?
V3 O5 V7 101.2(2) . . ?
C4 O6 V5 121.9(5) . . ?
C4 O6 V1 116.6(5) . . ?
V5 O6 V1 106.4(3) . . ?
V4 O7 V7 117.7(3) . . ?
C1 O8 V3 117.5(5) . . ?
C1 O8 V7 122.3(5) . . ?
V3 O8 V7 106.8(3) . . ?
V1 O10 V6 116.9(3) . . ?
V2 O11 V8 116.2(3) . . ?
C3 O12 V6 120.0(6) . . ?
C3 O12 V2 119.4(6) . . ?
V6 O12 V2 105.3(3) . . ?
V3 O14 V5 117.3(3) . . ?
C5 N1 V5 112.1(6) . . ?
C5 N1 H1A 109.2 . . ?
V5 N1 H1A 109.2 . . ?
C5 N1 H1B 109.2 . . ?
V5 N1 H1B 109.2 . . ?
H1A N1 H1B 107.9 . . ?
C20 N2 V6 111.4(6) . . ?
C20 N2 H2A 109.3 . . ?
V6 N2 H2A 109.3 . . ?
C20 N2 H2B 109.3 . . ?
V6 N2 H2B 109.3 . . ?
H2A N2 H2B 108.0 . . ?
C18 N3 V7 111.3(7) . . ?
C18 N3 H3A 109.4 . . ?
V7 N3 H3A 109.4 . . ?
C18 N3 H3B 109.4 . . ?
V7 N3 H3B 109.4 . . ?
H3A N3 H3B 108.0 . . ?
C23 N4 V8 112.0(7) . . ?
C23 N4 H4A 109.2 . . ?
V8 N4 H4A 109.2 . . ?
C23 N4 H4B 109.2 . . ?
V8 N4 H4B 109.2 . . ?
H4A N4 H4B 107.9 . . ?
C6 N5 V5 108.1(6) . . ?
C6 N5 H5A 110.1 . . ?
V5 N5 H5A 110.1 . . ?
C6 N5 H5B 110.1 . . ?
V5 N5 H5B 110.1 . . ?
H5A N5 H5B 108.4 . . ?
C19 N6 V6 109.2(6) . . ?
C19 N6 H6A 109.8 . . ?
V6 N6 H6A 109.8 . . ?
C19 N6 H6B 109.8 . . ?
V6 N6 H6B 109.8 . . ?
H6A N6 H6B 108.3 . . ?
C28 N7 V8 112.9(7) . . ?
C28 N7 H7A 109.0 . . ?
V8 N7 H7A 109.0 . . ?
C28 N7 H7B 109.0 . . ?
V8 N7 H7B 109.0 . . ?
H7A N7 H7B 107.8 . . ?
C11 N8 V7 110.1(6) . . ?
C11 N8 H8A 109.6 . . ?
V7 N8 H8A 109.6 . . ?
C11 N8 H8B 109.6 . . ?
V7 N8 H8B 109.6 . . ?
H8A N8 H8B 108.1 . . ?
O8 C1 H1C 109.5 . . ?
O8 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O8 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
O3 C2 H2C 109.5 . . ?
O3 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
O3 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
O12 C3 H3C 109.5 . . ?
O12 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
O12 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
O6 C4 H4C 109.5 . . ?
O6 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
O6 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C6 C5 N1 109.5(9) . . ?
C6 C5 C10 113.8(9) . . ?
N1 C5 C10 112.8(9) . . ?
C6 C5 H5C 106.7 . . ?
N1 C5 H5C 106.7 . . ?
C10 C5 H5C 106.7 . . ?
C7 C6 C5 114.3(10) . . ?
C7 C6 N5 115.4(9) . . ?
C5 C6 N5 110.1(9) . . ?
C7 C6 H6C 105.3 . . ?
C5 C6 H6C 105.3 . . ?
N5 C6 H6C 105.3 . . ?
C6 C7 C15 111.6(9) . . ?
C6 C7 H7C 109.3 . . ?
C15 C7 H7C 109.3 . . ?
C6 C7 H7D 109.3 . . ?
C15 C7 H7D 109.3 . . ?
H7C C7 H7D 108.0 . . ?
C27 C8 C23 117.9(11) . . ?
C27 C8 H8C 107.8 . . ?
C23 C8 H8C 107.8 . . ?
C27 C8 H8D 107.8 . . ?
C23 C8 H8D 107.8 . . ?
H8C C8 H8D 107.2 . . ?
C24 C9 C18 114.7(11) . . ?
C24 C9 H9A 108.6 . . ?
C18 C9 H9A 108.6 . . ?
C24 C9 H9B 108.6 . . ?
C18 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C5 C10 C13 109.1(9) . . ?
C5 C10 H10A 109.9 . . ?
C13 C10 H10A 109.9 . . ?
C5 C10 H10B 109.9 . . ?
C13 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C18 C11 C12 120.5(11) . . ?
C18 C11 N8 113.7(10) . . ?
C12 C11 N8 117.6(9) . . ?
C11 C12 C22 114.4(10) . . ?
C11 C12 H12A 108.7 . . ?
C22 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C22 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C15 C13 C10 110.3(11) . . ?
C15 C13 H13A 109.6 . . ?
C10 C13 H13A 109.6 . . ?
C15 C13 H13B 109.6 . . ?
C10 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C28 C14 C17 117.5(11) . . ?
C28 C14 H14A 107.9 . . ?
C17 C14 H14A 107.9 . . ?
C28 C14 H14B 107.9 . . ?
C17 C14 H14B 107.9 . . ?
H14A C14 H14B 107.2 . . ?
C13 C15 C7 113.5(10) . . ?
C13 C15 H15A 108.9 . . ?
C7 C15 H15A 108.9 . . ?
C13 C15 H15B 108.9 . . ?
C7 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C25 C16 C20 112.7(10) . . ?
C25 C16 H16A 109.1 . . ?
C20 C16 H16A 109.1 . . ?
C25 C16 H16B 109.1 . . ?
C20 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C27 C17 C14 119.2(12) . . ?
C27 C17 H17A 107.5 . . ?
C14 C17 H17A 107.5 . . ?
C27 C17 H17B 107.5 . . ?
C14 C17 H17B 107.5 . . ?
H17A C17 H17B 107.0 . . ?
C11 C18 N3 115.4(11) . . ?
C11 C18 C9 115.4(11) . . ?
N3 C18 C9 114.9(10) . . ?
C11 C18 H18A 102.8 . . ?
N3 C18 H18A 102.8 . . ?
C9 C18 H18A 102.8 . . ?
C20 C19 C21 118.9(12) . . ?
C20 C19 N6 112.7(11) . . ?
C21 C19 N6 116.7(10) . . ?
C19 C20 N2 114.8(11) . . ?
C19 C20 C16 115.3(11) . . ?
N2 C20 C16 114.8(10) . . ?
C19 C20 H20A 103.2 . . ?
N2 C20 H20A 103.2 . . ?
C16 C20 H20A 103.2 . . ?
C19 C21 C26 114.0(12) . . ?
C19 C21 H21A 108.8 . . ?
C26 C21 H21A 108.8 . . ?
C19 C21 H21B 108.8 . . ?
C26 C21 H21B 108.8 . . ?
H21A C21 H21B 107.6 . . ?
C24 C22 C12 117.5(11) . . ?
C24 C22 H22A 107.9 . . ?
C12 C22 H22A 107.9 . . ?
C24 C22 H22B 107.9 . . ?
C12 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C28 C23 N4 118.1(11) . . ?
C28 C23 C8 119.9(12) . . ?
N4 C23 C8 121.9(11) . . ?
C22 C24 C9 116.0(14) . . ?
C22 C24 H24A 108.3 . . ?
C9 C24 H24A 108.3 . . ?
C22 C24 H24B 108.3 . . ?
C9 C24 H24B 108.3 . . ?
H24A C24 H24B 107.4 . . ?
C26 C25 C16 118.9(13) . . ?
C26 C25 H25A 107.6 . . ?
C16 C25 H25A 107.6 . . ?
C26 C25 H25B 107.6 . . ?
C16 C25 H25B 107.6 . . ?
H25A C25 H25B 107.0 . . ?
C25 C26 C21 115.2(13) . . ?
C25 C26 H26A 108.5 . . ?
C21 C26 H26A 108.5 . . ?
C25 C26 H26B 108.5 . . ?
C21 C26 H26B 108.5 . . ?
H26A C26 H26B 107.5 . . ?
C17 C27 C8 121.4(13) . . ?
C17 C27 H27A 107.0 . . ?
C8 C27 H27A 107.0 . . ?
C17 C27 H27B 107.0 . . ?
C8 C27 H27B 107.0 . . ?
H27A C27 H27B 106.7 . . ?
C23 C28 C14 122.8(12) . . ?
C23 C28 N7 116.1(11) . . ?
C14 C28 N7 120.5(11) . . ?
O1W C4A O4A 164(4) 2_676 . ?
 
_refine_diff_density_max    1.334
_refine_diff_density_min   -0.967
_refine_diff_density_rms    0.180




