#------------------------------------------------------------------------------
#$Date: 2025-01-06 14:24:46 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297109 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717314.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717314
loop_
_publ_author_name
'Mikeska, Emily R.'
'Curry, T. Davis'
'Wilson, Richard E.'
'Blakemore, James D.'
_publ_section_title
;
 Electroanalytical characterization of Np(VI)/Np(V) redox in a
 pentadentate ligand environment and stabilization of
 [NpVO₂]⁺ by hydrogen bonding.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19126
_journal_page_last               19142
_journal_paper_doi               10.1039/d4dt02557a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C19 H21 N3 Np O4), 2(C16 H36 N), 3(H2 O)'
_chemical_formula_sum            'C70 H120 N8 Np2 O11'
_chemical_formula_weight         1723.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V139 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-09-03 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.5620(10)
_cell_angle_beta                 97.9810(10)
_cell_angle_gamma                94.4390(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9521(4)
_cell_length_b                   18.0582(8)
_cell_length_c                   21.1643(9)
_cell_measurement_reflns_used    5779
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.228
_cell_measurement_theta_min      4.326
_cell_volume                     3745.2(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.134
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  0.0963
_exptl_absorpt_correction_T_min  0.0655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.0963
_exptl_transmission_factor_min   0.0655
_refine_diff_density_max         2.000
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         16536
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0467P)²+8.2708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11221
_reflns_number_total             16536
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02557a3.cif
_cod_data_source_block           m61a
_cod_depositor_comments
'Adding full bibliography for 7717312--7717314.cif.'
_cod_database_code               7717314
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.677
_shelx_estimated_absorpt_t_max   0.946
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1A Np 0.41900(3) 0.41247(2) 0.13000(2) 0.04096(9) Uani 1 1 d . . . . .
O1A O 0.6384(5) 0.3651(3) 0.1507(3) 0.0619(16) Uani 1 1 d . . . . .
O2A O 0.4379(6) 0.4331(3) 0.2419(3) 0.0560(14) Uani 1 1 d . . . . .
O3A O 0.3246(5) 0.3228(2) 0.1334(2) 0.0413(11) Uani 1 1 d . . . . .
O4A O 0.5025(5) 0.5057(3) 0.1233(2) 0.0547(14) Uani 1 1 d . . . . .
N1A N 0.4876(6) 0.3538(3) 0.0230(3) 0.0445(14) Uani 1 1 d . . . . .
N2A N 0.1977(6) 0.4640(3) 0.1584(3) 0.0441(14) Uani 1 1 d . . . . .
N3A N 0.2455(6) 0.4319(3) 0.0278(3) 0.0385(13) Uani 1 1 d . . . . .
C1A C 0.5893(8) 0.3151(4) 0.0141(4) 0.054(2) Uani 1 1 d . . . . .
H1A H 0.5848 0.2908 -0.0263 0.065 Uiso 1 1 calc R U . . .
C2A C 0.7074(8) 0.3054(4) 0.0588(5) 0.054(2) Uani 1 1 d . . . . .
C3A C 0.8082(8) 0.2671(5) 0.0328(5) 0.069(3) Uani 1 1 d . . . . .
H3A H 0.7916 0.2480 -0.0097 0.083 Uiso 1 1 calc R U . . .
C4A C 0.9306(10) 0.2577(6) 0.0694(7) 0.086(4) Uani 1 1 d . . . . .
H4A H 0.9961 0.2325 0.0517 0.103 Uiso 1 1 calc R U . . .
C5A C 0.9552(9) 0.2856(6) 0.1320(7) 0.088(4) Uani 1 1 d . . . . .
H5A H 1.0380 0.2790 0.1564 0.106 Uiso 1 1 calc R U . . .
C6A C 0.8591(8) 0.3236(5) 0.1599(5) 0.069(3) Uani 1 1 d . . . . .
H6A H 0.8791 0.3431 0.2021 0.083 Uiso 1 1 calc R U . . .
C7A C 0.7301(8) 0.3325(5) 0.1237(5) 0.060(2) Uani 1 1 d . . . . .
C8A C 0.3556(10) 0.4245(4) 0.2836(4) 0.052(2) Uani 1 1 d . . . . .
C9A C 0.4050(11) 0.4047(5) 0.3463(4) 0.068(3) Uani 1 1 d . . . . .
H9A H 0.4962 0.3961 0.3558 0.082 Uiso 1 1 calc R U . . .
C10A C 0.3250(13) 0.3978(5) 0.3923(4) 0.077(3) Uani 1 1 d . . . . .
H10A H 0.3614 0.3839 0.4322 0.092 Uiso 1 1 calc R U . . .
C11A C 0.1880(13) 0.4114(5) 0.3806(4) 0.079(3) Uani 1 1 d . . . . .
H11A H 0.1331 0.4074 0.4126 0.095 Uiso 1 1 calc R U . . .
C12A C 0.1353(11) 0.4308(5) 0.3207(4) 0.069(3) Uani 1 1 d . . . . .
H12A H 0.0439 0.4397 0.3127 0.083 Uiso 1 1 calc R U . . .
C13A C 0.2144(10) 0.4374(4) 0.2718(4) 0.054(2) Uani 1 1 d . . . . .
C14A C 0.1462(9) 0.4589(4) 0.2111(4) 0.051(2) Uani 1 1 d . . . . .
H14A H 0.0563 0.4700 0.2100 0.062 Uiso 1 1 calc R U . . .
C15A C 0.1030(8) 0.4840(4) 0.1041(3) 0.0465(18) Uani 1 1 d . . . . .
H15A H 0.1287 0.5343 0.0937 0.056 Uiso 1 1 calc R U . . .
H15B H 0.0114 0.4824 0.1150 0.056 Uiso 1 1 calc R U . . .
C16A C 0.1069(7) 0.4295(4) 0.0467(4) 0.0487(19) Uani 1 1 d . . . . .
H16A H 0.0801 0.3794 0.0572 0.058 Uiso 1 1 calc R U . . .
H16B H 0.0423 0.4417 0.0110 0.058 Uiso 1 1 calc R U . . .
C17A C 0.2490(8) 0.3674(4) -0.0188(4) 0.0502(19) Uani 1 1 d . . . . .
H17A H 0.1885 0.3736 -0.0578 0.060 Uiso 1 1 calc R U . . .
H17B H 0.2161 0.3222 -0.0012 0.060 Uiso 1 1 calc R U . . .
C18A C 0.3899(8) 0.3594(4) -0.0344(4) 0.0503(19) Uani 1 1 d . . . . .
H18A H 0.3887 0.3151 -0.0629 0.060 Uiso 1 1 calc R U . . .
H18B H 0.4187 0.4020 -0.0564 0.060 Uiso 1 1 calc R U . . .
C19A C 0.2774(8) 0.5025(4) -0.0014(4) 0.0479(18) Uani 1 1 d . . . . .
H19A H 0.3631 0.5011 -0.0172 0.072 Uiso 1 1 calc R U . . .
H19B H 0.2826 0.5436 0.0302 0.072 Uiso 1 1 calc R U . . .
H19C H 0.2071 0.5086 -0.0361 0.072 Uiso 1 1 calc R U . . .
Np1B Np 0.37414(3) -0.07627(2) 0.35610(2) 0.04068(9) Uani 1 1 d . . . . .
O1B O 0.4493(5) -0.0842(3) 0.2534(2) 0.0499(13) Uani 1 1 d . . . . .
O2B O 0.5987(5) -0.1033(3) 0.3955(2) 0.0501(13) Uani 1 1 d . . . . .
O3B O 0.4247(5) 0.0230(3) 0.3659(2) 0.0438(12) Uani 1 1 d . . . . .
O4B O 0.3119(6) -0.1749(3) 0.3482(3) 0.0572(14) Uani 1 1 d . . . . .
N1B N 0.1716(6) -0.0592(4) 0.2666(3) 0.0518(16) Uani 1 1 d . . . . .
N2B N 0.3931(6) -0.0905(3) 0.4779(3) 0.0457(15) Uani 1 1 d . . . . .
N3B N 0.1506(7) -0.0461(4) 0.4034(3) 0.0541(16) Uani 1 1 d . U . . .
C1B C 0.1632(8) -0.0680(4) 0.2059(4) 0.0487(19) Uani 1 1 d . . . . .
H1B H 0.0765 -0.0660 0.1834 0.058 Uiso 1 1 calc R U . . .
C2B C 0.2682(8) -0.0806(4) 0.1670(4) 0.0472(18) Uani 1 1 d . . . . .
C3B C 0.2321(9) -0.0839(4) 0.1004(4) 0.058(2) Uani 1 1 d . . . . .
H3B H 0.1427 -0.0768 0.0840 0.069 Uiso 1 1 calc R U . . .
C4B C 0.3209(11) -0.0971(5) 0.0586(4) 0.065(2) Uani 1 1 d . . . . .
H4B H 0.2929 -0.0999 0.0147 0.079 Uiso 1 1 calc R U . . .
C5B C 0.4543(10) -0.1061(5) 0.0834(4) 0.064(2) Uani 1 1 d . . . . .
H5B H 0.5172 -0.1147 0.0557 0.077 Uiso 1 1 calc R U . . .
C6B C 0.4946(8) -0.1026(4) 0.1474(4) 0.0506(19) Uani 1 1 d . . . . .
H6B H 0.5850 -0.1091 0.1623 0.061 Uiso 1 1 calc R U . . .
C7B C 0.4059(8) -0.0896(4) 0.1925(4) 0.0458(18) Uani 1 1 d . . . . .
C8B C 0.6517(7) -0.1466(4) 0.4379(3) 0.0408(16) Uani 1 1 d . . . . .
C9B C 0.7732(7) -0.1776(4) 0.4304(4) 0.0464(18) Uani 1 1 d . . . . .
H9B H 0.8146 -0.1672 0.3948 0.056 Uiso 1 1 calc R U . . .
C10B C 0.8338(8) -0.2228(5) 0.4738(4) 0.060(2) Uani 1 1 d . . . . .
H10B H 0.9152 -0.2421 0.4674 0.072 Uiso 1 1 calc R U . . .
C11B C 0.7740(9) -0.2400(5) 0.5274(4) 0.067(3) Uani 1 1 d . . . . .
H11B H 0.8128 -0.2717 0.5564 0.080 Uiso 1 1 calc R U . . .
C12B C 0.6588(8) -0.2095(4) 0.5358(4) 0.053(2) Uani 1 1 d . . . . .
H12B H 0.6206 -0.2200 0.5723 0.063 Uiso 1 1 calc R U . . .
C13B C 0.5915(7) -0.1630(4) 0.4938(3) 0.0419(16) Uani 1 1 d . . . . .
C14B C 0.4734(8) -0.1297(4) 0.5113(4) 0.0478(18) Uani 1 1 d . . . . .
H14B H 0.4533 -0.1377 0.5521 0.057 Uiso 1 1 calc R U . . .
C15B C 0.2805(10) -0.0606(5) 0.5089(4) 0.069(3) Uani 1 1 d . . . . .
H15C H 0.2950 -0.0069 0.5167 0.083 Uiso 1 1 calc R U . . .
H15D H 0.2740 -0.0825 0.5492 0.083 Uiso 1 1 calc R U . . .
C16B C 0.1415(11) -0.0847(7) 0.4571(5) 0.091(3) Uani 1 1 d . U . . .
H16C H 0.1339 -0.1379 0.4457 0.109 Uiso 1 1 calc R U . . .
H16D H 0.0615 -0.0726 0.4758 0.109 Uiso 1 1 calc R U . . .
C17B C 0.0355(11) -0.0704(6) 0.3533(5) 0.086(3) Uani 1 1 d . U . . .
H17C H 0.0250 -0.1244 0.3503 0.103 Uiso 1 1 calc R U . . .
H17D H -0.0462 -0.0534 0.3675 0.103 Uiso 1 1 calc R U . . .
C18B C 0.0407(9) -0.0471(6) 0.2903(5) 0.074(3) Uani 1 1 d . . . . .
H18C H 0.0265 0.0054 0.2902 0.089 Uiso 1 1 calc R U . . .
H18D H -0.0331 -0.0742 0.2611 0.089 Uiso 1 1 calc R U . . .
C19B C 0.1373(12) 0.0357(6) 0.4138(7) 0.100(4) Uani 1 1 d . . . . .
H19D H 0.1108 0.0556 0.3737 0.150 Uiso 1 1 d . U . . .
H19E H 0.2234 0.0601 0.4338 0.150 Uiso 1 1 d . U . . .
H19F H 0.0698 0.0434 0.4414 0.150 Uiso 1 1 d . U . . .
N1 N 0.5295(8) 0.6571(4) 0.3035(4) 0.067(2) Uani 1 1 d . . . . .
C1 C 0.6145(11) 0.7257(5) 0.2890(5) 0.074(3) Uani 1 1 d . . . . .
H1C H 0.5606 0.7680 0.2913 0.089 Uiso 1 1 calc R U . . .
H1D H 0.6926 0.7349 0.3223 0.089 Uiso 1 1 calc R U . . .
C2 C 0.6657(11) 0.7222(5) 0.2248(4) 0.077(3) Uani 1 1 d . . . . .
H2A H 0.5918 0.7289 0.1911 0.092 Uiso 1 1 calc R U . . .
H2B H 0.6983 0.6738 0.2164 0.092 Uiso 1 1 calc R U . . .
C3 C 0.7822(12) 0.7838(5) 0.2251(5) 0.089(4) Uani 1 1 d . . . . .
H3C H 0.7527 0.8314 0.2388 0.107 Uiso 1 1 calc R U . . .
H3D H 0.8600 0.7736 0.2553 0.107 Uiso 1 1 calc R U . . .
C4 C 0.8240(12) 0.7881(6) 0.1594(5) 0.091(3) Uani 1 1 d . . . . .
H4C H 0.8968 0.8266 0.1608 0.136 Uiso 1 1 calc R U . . .
H4D H 0.7476 0.7993 0.1296 0.136 Uiso 1 1 calc R U . . .
H4E H 0.8541 0.7412 0.1459 0.136 Uiso 1 1 calc R U . . .
C5 C 0.4184(12) 0.6325(5) 0.2500(5) 0.090(4) Uani 1 1 d . . . . .
H5C H 0.3628 0.5909 0.2625 0.108 Uiso 1 1 calc R U . . .
H5D H 0.4583 0.6151 0.2131 0.108 Uiso 1 1 calc R U . . .
C6 C 0.3277(13) 0.6940(7) 0.2310(6) 0.114(4) Uani 1 1 d D U . . .
H6C H 0.2746 0.7058 0.2649 0.136 Uiso 1 1 calc R U . . .
H6D H 0.3834 0.7387 0.2246 0.136 Uiso 1 1 calc R U . . .
C7 C 0.2343(17) 0.6685(9) 0.1704(8) 0.154(6) Uani 1 1 d D U . . .
H7A H 0.2901 0.6542 0.1383 0.184 Uiso 1 1 calc R U . . .
H7B H 0.1801 0.6239 0.1783 0.184 Uiso 1 1 calc R U . . .
C8 C 0.145(2) 0.7186(12) 0.1439(10) 0.237(11) Uani 1 1 d D U . . .
H8A H 0.1960 0.7608 0.1311 0.285 Uiso 1 1 calc R U . . .
H8B H 0.0900 0.7348 0.1753 0.285 Uiso 1 1 calc R U . . .
H8C H 0.0865 0.6942 0.1073 0.285 Uiso 1 1 calc R U . . .
C9 C 0.4756(10) 0.6770(5) 0.3659(5) 0.072(3) Uani 1 1 d . . . . .
H9C H 0.5521 0.6970 0.3974 0.087 Uiso 1 1 calc R U . . .
H9D H 0.4157 0.7165 0.3585 0.087 Uiso 1 1 calc R U . . .
C10 C 0.3994(11) 0.6151(6) 0.3944(6) 0.091(3) Uani 1 1 d . . . . .
H10C H 0.4576 0.5750 0.4022 0.109 Uiso 1 1 calc R U . . .
H10D H 0.3202 0.5956 0.3642 0.109 Uiso 1 1 calc R U . . .
C11 C 0.3539(13) 0.6424(7) 0.4567(6) 0.095(3) Uani 1 1 d . U . . .
H11C H 0.2829 0.6755 0.4471 0.114 Uiso 1 1 calc R U . . .
H11D H 0.4303 0.6711 0.4829 0.114 Uiso 1 1 calc R U . . .
C12 C 0.3009(15) 0.5812(8) 0.4953(7) 0.128(5) Uani 1 1 d . U . . .
H12C H 0.2740 0.6031 0.5336 0.191 Uiso 1 1 calc R U . . .
H12D H 0.3713 0.5489 0.5065 0.191 Uiso 1 1 calc R U . . .
H12E H 0.2238 0.5530 0.4703 0.191 Uiso 1 1 calc R U . . .
C13 C 0.6142(11) 0.5917(5) 0.3117(5) 0.077(3) Uani 1 1 d . . . . .
H13A H 0.5550 0.5489 0.3192 0.092 Uiso 1 1 calc R U . A 1
H13B H 0.6484 0.5804 0.2718 0.092 Uiso 1 1 calc R U . A 1
C14 C 0.7310(11) 0.6011(6) 0.3636(6) 0.097(3) Uani 0.574(9) 1 d D . P B 1
H14C H 0.7015 0.6178 0.4035 0.116 Uiso 0.574(9) 1 calc R U P B 1
H14D H 0.7997 0.6379 0.3537 0.116 Uiso 0.574(9) 1 calc R U P B 1
C15 C 0.7895(18) 0.5257(10) 0.3698(9) 0.095(7) Uani 0.574(9) 1 d D . P B 1
H15E H 0.8161 0.5083 0.3295 0.115 Uiso 0.574(9) 1 calc R U P B 1
H15F H 0.7213 0.4894 0.3809 0.115 Uiso 0.574(9) 1 calc R U P B 1
C16 C 0.9140(18) 0.5349(14) 0.4223(9) 0.139(12) Uani 0.574(9) 1 d D . P B 1
H16E H 0.8877 0.5544 0.4616 0.166 Uiso 0.574(9) 1 calc R U P B 1
H16F H 0.9832 0.5686 0.4097 0.166 Uiso 0.574(9) 1 calc R U P B 1
H16G H 0.9488 0.4873 0.4284 0.166 Uiso 0.574(9) 1 calc R U P B 1
C14' C 0.7310(11) 0.6011(6) 0.3636(6) 0.097(3) Uani 0.426(9) 1 d D U P B 2
H14E H 0.6897 0.5943 0.4020 0.116 Uiso 0.426(9) 1 calc R U P B 2
H14F H 0.7607 0.6537 0.3656 0.116 Uiso 0.426(9) 1 calc R U P B 2
C15' C 0.865(2) 0.5633(16) 0.3763(15) 0.098(3) Uani 0.426(9) 1 d D U P B 2
H15G H 0.9000 0.5684 0.4217 0.117 Uiso 0.426(9) 1 calc R U P B 2
H15H H 0.8493 0.5106 0.3629 0.117 Uiso 0.426(9) 1 calc R U P B 2
C16' C 0.969(2) 0.6004(16) 0.3388(13) 0.103(4) Uani 0.426(9) 1 d D U P B 2
H16H H 0.9257 0.6078 0.2965 0.124 Uiso 0.426(9) 1 calc R U P B 2
H16I H 1.0422 0.5691 0.3360 0.124 Uiso 0.426(9) 1 calc R U P B 2
H16J H 1.0049 0.6477 0.3603 0.124 Uiso 0.426(9) 1 calc R U P B 2
N2 N 0.5349(6) 0.1530(3) 0.2095(3) 0.0457(15) Uani 1 1 d . . . . .
C17 C 0.4714(7) 0.1806(4) 0.1468(4) 0.0467(18) Uani 1 1 d . . . . .
H17E H 0.4176 0.2212 0.1563 0.056 Uiso 1 1 calc R U . . .
H17F H 0.5441 0.2005 0.1248 0.056 Uiso 1 1 calc R U . . .
C18 C 0.3821(8) 0.1231(4) 0.1017(4) 0.054(2) Uani 1 1 d . . . . .
H18E H 0.3168 0.0975 0.1247 0.065 Uiso 1 1 calc R U . . .
H18F H 0.4377 0.0865 0.0856 0.065 Uiso 1 1 calc R U . . .
C19 C 0.3072(8) 0.1595(4) 0.0463(4) 0.056(2) Uani 1 1 d . . . . .
H19G H 0.3730 0.1836 0.0227 0.067 Uiso 1 1 calc R U . . .
H19H H 0.2550 0.1976 0.0628 0.067 Uiso 1 1 calc R U . . .
C20 C 0.2111(9) 0.1035(5) 0.0007(4) 0.066(2) Uani 1 1 d . . . . .
H20A H 0.1654 0.1290 -0.0334 0.099 Uiso 1 1 calc R U . . .
H20B H 0.1450 0.0799 0.0237 0.099 Uiso 1 1 calc R U . . .
H20C H 0.2626 0.0665 -0.0168 0.099 Uiso 1 1 calc R U . . .
C21 C 0.4253(9) 0.1209(4) 0.2461(4) 0.062(2) Uani 1 1 d . . . . .
H21A H 0.4684 0.1038 0.2859 0.075 Uiso 1 1 calc R U . . .
H21B H 0.3754 0.0782 0.2210 0.075 Uiso 1 1 calc R U . . .
C22 C 0.3253(11) 0.1775(7) 0.2609(6) 0.105(4) Uani 1 1 d D U . . .
H22A H 0.3688 0.2104 0.2972 0.127 Uiso 1 1 calc R U . . .
H22B H 0.3104 0.2077 0.2247 0.127 Uiso 1 1 calc R U . . .
C23 C 0.1933(11) 0.1490(7) 0.2749(6) 0.107(3) Uani 1 1 d D U . . .
H23A H 0.2082 0.1193 0.3110 0.129 Uiso 1 1 d . U . . .
H23B H 0.1517 0.1169 0.2383 0.129 Uiso 1 1 d . U . . .
C24 C 0.0964(11) 0.2035(6) 0.2888(6) 0.097(3) Uani 1 1 d D U . . .
H24A H 0.0413 0.2131 0.2497 0.146 Uiso 1 1 calc R U . . .
H24B H 0.1458 0.2490 0.3078 0.146 Uiso 1 1 calc R U . . .
H24C H 0.0390 0.1839 0.3178 0.146 Uiso 1 1 calc R U . . .
C25 C 0.6194(7) 0.2200(4) 0.2469(4) 0.0482(18) Uani 1 1 d . . . . .
H25A H 0.6923 0.2358 0.2234 0.058 Uiso 1 1 calc R U . . .
H25B H 0.5619 0.2608 0.2494 0.058 Uiso 1 1 calc R U . . .
C26 C 0.6813(8) 0.2054(5) 0.3144(4) 0.055(2) Uani 1 1 d . . . . .
H26A H 0.7329 0.1621 0.3128 0.066 Uiso 1 1 calc R U . . .
H26B H 0.6091 0.1949 0.3398 0.066 Uiso 1 1 calc R U . . .
C27 C 0.7752(9) 0.2726(5) 0.3462(4) 0.062(2) Uani 1 1 d . . . . .
H27A H 0.8457 0.2837 0.3199 0.074 Uiso 1 1 calc R U . . .
H27B H 0.7228 0.3156 0.3483 0.074 Uiso 1 1 calc R U . . .
C28 C 0.8402(10) 0.2598(6) 0.4118(5) 0.083(3) Uani 1 1 d . . . . .
H28A H 0.8938 0.3042 0.4305 0.125 Uiso 1 1 calc R U . . .
H28B H 0.8977 0.2197 0.4097 0.125 Uiso 1 1 calc R U . . .
H28C H 0.7709 0.2472 0.4376 0.125 Uiso 1 1 calc R U . . .
C29 C 0.6251(8) 0.0902(4) 0.1973(4) 0.0495(19) Uani 1 1 d . . . . .
H29A H 0.6622 0.0733 0.2383 0.059 Uiso 1 1 calc R U . . .
H29B H 0.5683 0.0487 0.1736 0.059 Uiso 1 1 calc R U . . .
C30 C 0.7418(7) 0.1103(5) 0.1611(4) 0.052(2) Uani 1 1 d . . . . .
H30A H 0.7068 0.1311 0.1216 0.063 Uiso 1 1 calc R U . . .
H30B H 0.8047 0.1480 0.1865 0.063 Uiso 1 1 calc R U . . .
C31 C 0.8159(10) 0.0445(5) 0.1460(5) 0.074(3) Uani 1 1 d . . . . .
H31A H 0.7528 0.0073 0.1200 0.089 Uiso 1 1 calc R U . . .
H31B H 0.8482 0.0230 0.1856 0.089 Uiso 1 1 calc R U . . .
C32 C 0.9354(9) 0.0622(6) 0.1112(5) 0.074(3) Uani 1 1 d . . . . .
H32A H 0.9683 0.0167 0.0962 0.111 Uiso 1 1 calc R U . . .
H32B H 1.0067 0.0908 0.1397 0.111 Uiso 1 1 calc R U . . .
H32C H 0.9072 0.0903 0.0754 0.111 Uiso 1 1 calc R U . . .
O1W O 0.7363(11) 0.4313(6) 0.2589(5) 0.041(3) Uani 0.426(9) 1 d . . P B 2
H1WA H 0.7156 0.4165 0.2071 2.000 Uiso 0.4258 1 d . . P B 2
H1WB H 0.6358 0.4322 0.2706 2.000 Uiso 0.4258 1 d . . P B 2
O2W O 0.0715(16) -0.2713(8) 0.3557(9) 0.132(6) Uani 0.574(9) 1 d . . P B 1
H2WA H 0.1585 -0.2418 0.3488 0.473 Uiso 0.5742 1 d . . P B 1
H2WB H 0.0401 -0.3083 0.3197 0.173 Uiso 0.5742 1 d . . P B 1
O3W O 0.7772(6) 0.5383(4) 0.1775(3) 0.0742(18) Uani 1 1 d . . . . .
H3WA H 0.7991 0.4954 0.2027 0.100 Uiso 1 1 d . . . . .
H3WB H 0.6817 0.5297 0.1539 0.129 Uiso 1 1 d . . . . .
O4W O 0.7203(5) -0.0303(4) 0.3014(3) 0.0669(17) Uani 1 1 d . . . . .
H4WA H 0.6420 -0.0495 0.2703 0.078 Uiso 1 1 d . . . . .
H4WB H 0.7015 -0.0415 0.3441 0.229 Uiso 1 1 d . . . . .
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'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3A Np1A O4A 175.6(2) . . ?
O3A Np1A O2A 90.2(2) . . ?
O4A Np1A O2A 91.5(2) . . ?
O3A Np1A O1A 94.5(2) . . ?
O4A Np1A O1A 89.7(2) . . ?
O2A Np1A O1A 85.3(2) . . ?
O3A Np1A N2A 83.2(2) . . ?
O4A Np1A N2A 93.5(2) . . ?
O2A Np1A N2A 71.18(19) . . ?
O1A Np1A N2A 156.30(19) . . ?
O3A Np1A N3A 87.31(18) . . ?
O4A Np1A N3A 88.68(19) . . ?
O2A Np1A N3A 138.60(19) . . ?
O1A Np1A N3A 136.12(19) . . ?
N2A Np1A N3A 67.49(18) . . ?
O3A Np1A N1A 85.3(2) . . ?
O4A Np1A N1A 94.9(2) . . ?
O2A Np1A N1A 154.23(19) . . ?
O1A Np1A N1A 69.84(19) . . ?
N2A Np1A N1A 133.05(18) . . ?
N3A Np1A N1A 66.62(18) . . ?
C7A O1A Np1A 143.5(5) . . ?
C8A O2A Np1A 135.0(5) . . ?
C1A N1A C18A 114.6(7) . . ?
C1A N1A Np1A 129.9(5) . . ?
C18A N1A Np1A 115.2(5) . . ?
C14A N2A C15A 114.7(6) . . ?
C14A N2A Np1A 127.9(5) . . ?
C15A N2A Np1A 115.5(5) . . ?
C19A N3A C17A 110.2(6) . . ?
C19A N3A C16A 110.6(5) . . ?
C17A N3A C16A 107.9(6) . . ?
C19A N3A Np1A 113.1(4) . . ?
C17A N3A Np1A 107.0(4) . . ?
C16A N3A Np1A 107.9(4) . . ?
N1A C1A C2A 128.0(8) . . ?
N1A C1A H1A 116.0 . . ?
C2A C1A H1A 116.0 . . ?
C7A C2A C3A 119.8(8) . . ?
C7A C2A C1A 125.5(8) . . ?
C3A C2A C1A 114.7(9) . . ?
C4A C3A C2A 121.0(11) . . ?
C4A C3A H3A 119.5 . . ?
C2A C3A H3A 119.5 . . ?
C5A C4A C3A 119.7(11) . . ?
C5A C4A H4A 120.2 . . ?
C3A C4A H4A 120.2 . . ?
C4A C5A C6A 121.5(10) . . ?
C4A C5A H5A 119.2 . . ?
C6A C5A H5A 119.2 . . ?
C5A C6A C7A 120.1(11) . . ?
C5A C6A H6A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
O1A C7A C2A 122.2(7) . . ?
O1A C7A C6A 119.9(9) . . ?
C2A C7A C6A 117.9(9) . . ?
O2A C8A C9A 120.3(9) . . ?
O2A C8A C13A 123.5(7) . . ?
C9A C8A C13A 116.1(9) . . ?
C10A C9A C8A 122.8(10) . . ?
C10A C9A H9A 118.6 . . ?
C8A C9A H9A 118.6 . . ?
C9A C10A C11A 120.7(9) . . ?
C9A C10A H10A 119.7 . . ?
C11A C10A H10A 119.7 . . ?
C12A C11A C10A 118.8(10) . . ?
C12A C11A H11A 120.6 . . ?
C10A C11A H11A 120.6 . . ?
C11A C12A C13A 122.1(10) . . ?
C11A C12A H12A 118.9 . . ?
C13A C12A H12A 118.9 . . ?
C12A C13A C8A 119.5(8) . . ?
C12A C13A C14A 116.4(8) . . ?
C8A C13A C14A 124.0(8) . . ?
N2A C14A C13A 126.8(8) . . ?
N2A C14A H14A 116.6 . . ?
C13A C14A H14A 116.6 . . ?
N2A C15A C16A 109.2(6) . . ?
N2A C15A H15A 109.8 . . ?
C16A C15A H15A 109.8 . . ?
N2A C15A H15B 109.8 . . ?
C16A C15A H15B 109.8 . . ?
H15A C15A H15B 108.3 . . ?
N3A C16A C15A 111.0(6) . . ?
N3A C16A H16A 109.4 . . ?
C15A C16A H16A 109.4 . . ?
N3A C16A H16B 109.4 . . ?
C15A C16A H16B 109.4 . . ?
H16A C16A H16B 108.0 . . ?
N3A C17A C18A 111.9(6) . . ?
N3A C17A H17A 109.2 . . ?
C18A C17A H17A 109.2 . . ?
N3A C17A H17B 109.2 . . ?
C18A C17A H17B 109.2 . . ?
H17A C17A H17B 107.9 . . ?
N1A C18A C17A 111.9(6) . . ?
N1A C18A H18A 109.2 . . ?
C17A C18A H18A 109.2 . . ?
N1A C18A H18B 109.2 . . ?
C17A C18A H18B 109.2 . . ?
H18A C18A H18B 107.9 . . ?
N3A C19A H19A 109.5 . . ?
N3A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
N3A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
O3B Np1B O4B 176.0(2) . . ?
O3B Np1B O2B 91.02(19) . . ?
O4B Np1B O2B 92.1(2) . . ?
O3B Np1B O1B 90.7(2) . . ?
O4B Np1B O1B 92.1(2) . . ?
O2B Np1B O1B 84.82(16) . . ?
O3B Np1B N2B 93.9(2) . . ?
O4B Np1B N2B 84.8(2) . . ?
O2B Np1B N2B 70.85(18) . . ?
O1B Np1B N2B 155.29(18) . . ?
O3B Np1B N1B 92.3(2) . . ?
O4B Np1B N1B 86.0(2) . . ?
O2B Np1B N1B 154.71(19) . . ?
O1B Np1B N1B 70.07(18) . . ?
N2B Np1B N1B 133.8(2) . . ?
O3B Np1B N3B 87.3(2) . . ?
O4B Np1B N3B 88.7(2) . . ?
O2B Np1B N3B 137.61(19) . . ?
O1B Np1B N3B 137.53(19) . . ?
N2B Np1B N3B 67.0(2) . . ?
N1B Np1B N3B 67.6(2) . . ?
C7B O1B Np1B 142.8(5) . . ?
C8B O2B Np1B 134.8(4) . . ?
C1B N1B C18B 114.6(7) . . ?
C1B N1B Np1B 130.2(5) . . ?
C18B N1B Np1B 114.7(5) . . ?
C14B N2B C15B 117.0(6) . . ?
C14B N2B Np1B 127.2(5) . . ?
C15B N2B Np1B 114.8(5) . . ?
C16B N3B C17B 110.4(8) . . ?
C16B N3B C19B 113.9(8) . . ?
C17B N3B C19B 102.7(8) . . ?
C16B N3B Np1B 109.4(6) . . ?
C17B N3B Np1B 106.7(5) . . ?
C19B N3B Np1B 113.3(5) . . ?
N1B C1B C2B 129.5(7) . . ?
N1B C1B H1B 115.2 . . ?
C2B C1B H1B 115.2 . . ?
C3B C2B C7B 118.7(7) . . ?
C3B C2B C1B 117.7(7) . . ?
C7B C2B C1B 123.7(7) . . ?
C4B C3B C2B 123.3(8) . . ?
C4B C3B H3B 118.3 . . ?
C2B C3B H3B 118.3 . . ?
C3B C4B C5B 118.0(8) . . ?
C3B C4B H4B 121.0 . . ?
C5B C4B H4B 121.0 . . ?
C6B C5B C4B 120.9(8) . . ?
C6B C5B H5B 119.5 . . ?
C4B C5B H5B 119.5 . . ?
C5B C6B C7B 123.0(8) . . ?
C5B C6B H6B 118.5 . . ?
C7B C6B H6B 118.5 . . ?
O1B C7B C6B 121.2(7) . . ?
O1B C7B C2B 122.7(7) . . ?
C6B C7B C2B 116.1(7) . . ?
O2B C8B C9B 119.9(7) . . ?
O2B C8B C13B 122.7(6) . . ?
C9B C8B C13B 117.3(6) . . ?
C10B C9B C8B 122.3(7) . . ?
C10B C9B H9B 118.8 . . ?
C8B C9B H9B 118.8 . . ?
C9B C10B C11B 120.4(8) . . ?
C9B C10B H10B 119.8 . . ?
C11B C10B H10B 119.8 . . ?
C12B C11B C10B 117.9(8) . . ?
C12B C11B H11B 121.0 . . ?
C10B C11B H11B 121.0 . . ?
C11B C12B C13B 124.8(8) . . ?
C11B C12B H12B 117.6 . . ?
C13B C12B H12B 117.6 . . ?
C12B C13B C8B 117.2(7) . . ?
C12B C13B C14B 118.8(7) . . ?
C8B C13B C14B 123.8(6) . . ?
N2B C14B C13B 128.2(7) . . ?
N2B C14B H14B 115.9 . . ?
C13B C14B H14B 115.9 . . ?
N2B C15B C16B 104.7(7) . . ?
N2B C15B H15C 110.8 . . ?
C16B C15B H15C 110.8 . . ?
N2B C15B H15D 110.8 . . ?
C16B C15B H15D 110.8 . . ?
H15C C15B H15D 108.9 . . ?
N3B C16B C15B 108.1(8) . . ?
N3B C16B H16C 110.1 . . ?
C15B C16B H16C 110.1 . . ?
N3B C16B H16D 110.1 . . ?
C15B C16B H16D 110.1 . . ?
H16C C16B H16D 108.4 . . ?
C18B C17B N3B 118.3(9) . . ?
C18B C17B H17C 107.7 . . ?
N3B C17B H17C 107.7 . . ?
C18B C17B H17D 107.7 . . ?
N3B C17B H17D 107.7 . . ?
H17C C17B H17D 107.1 . . ?
C17B C18B N1B 113.4(8) . . ?
C17B C18B H18C 108.9 . . ?
N1B C18B H18C 108.9 . . ?
C17B C18B H18D 108.9 . . ?
N1B C18B H18D 108.9 . . ?
H18C C18B H18D 107.7 . . ?
N3B C19B H19D 109.6 . . ?
N3B C19B H19E 109.2 . . ?
H19D C19B H19E 109.8 . . ?
N3B C19B H19F 109.2 . . ?
H19D C19B H19F 109.8 . . ?
H19E C19B H19F 109.1 . . ?
C5 N1 C13 105.4(7) . . ?
C5 N1 C1 111.8(7) . . ?
C13 N1 C1 111.2(8) . . ?
C5 N1 C9 112.5(8) . . ?
C13 N1 C9 109.5(7) . . ?
C1 N1 C9 106.6(7) . . ?
C2 C1 N1 116.0(7) . . ?
C2 C1 H1C 108.3 . . ?
N1 C1 H1C 108.3 . . ?
C2 C1 H1D 108.3 . . ?
N1 C1 H1D 108.3 . . ?
H1C C1 H1D 107.4 . . ?
C1 C2 C3 109.6(8) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 111.0(8) . . ?
C4 C3 H3C 109.4 . . ?
C2 C3 H3C 109.4 . . ?
C4 C3 H3D 109.4 . . ?
C2 C3 H3D 109.4 . . ?
H3C C3 H3D 108.0 . . ?
C3 C4 H4C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N1 C5 C6 113.0(8) . . ?
N1 C5 H5C 109.0 . . ?
C6 C5 H5C 109.0 . . ?
N1 C5 H5D 109.0 . . ?
C6 C5 H5D 109.0 . . ?
H5C C5 H5D 107.8 . . ?
C7 C6 C5 109.2(11) . . ?
C7 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
C7 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.3 . . ?
C8 C7 C6 118.0(14) . . ?
C8 C7 H7A 107.8 . . ?
C6 C7 H7A 107.8 . . ?
C8 C7 H7B 107.8 . . ?
C6 C7 H7B 107.8 . . ?
H7A C7 H7B 107.2 . . ?
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 . . ?
C10 C9 N1 116.9(8) . . ?
C10 C9 H9C 108.1 . . ?
N1 C9 H9C 108.1 . . ?
C10 C9 H9D 108.1 . . ?
N1 C9 H9D 108.1 . . ?
H9C C9 H9D 107.3 . . ?
C9 C10 C11 111.2(9) . . ?
C9 C10 H10C 109.4 . . ?
C11 C10 H10C 109.4 . . ?
C9 C10 H10D 109.4 . . ?
C11 C10 H10D 109.4 . . ?
H10C C10 H10D 108.0 . . ?
C10 C11 C12 114.8(10) . . ?
C10 C11 H11C 108.6 . . ?
C12 C11 H11C 108.6 . . ?
C10 C11 H11D 108.6 . . ?
C12 C11 H11D 108.6 . . ?
H11C C11 H11D 107.5 . . ?
C11 C12 H12C 109.5 . . ?
C11 C12 H12D 109.5 . . ?
H12C C12 H12D 109.5 . . ?
C11 C12 H12E 109.5 . . ?
H12C C12 H12E 109.5 . . ?
H12D C12 H12E 109.5 . . ?
C14' C13 N1 116.4(8) . . ?
C14 C13 N1 116.4(8) . . ?
C14 C13 H13A 108.2 . . ?
N1 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
N1 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 C15 107.8(11) . . ?
C13 C14 H14C 110.2 . . ?
C15 C14 H14C 110.2 . . ?
C13 C14 H14D 110.2 . . ?
C15 C14 H14D 110.2 . . ?
H14C C14 H14D 108.5 . . ?
C14 C15 C16 108.5(13) . . ?
C14 C15 H15E 110.0 . . ?
C16 C15 H15E 110.0 . . ?
C14 C15 H15F 110.0 . . ?
C16 C15 H15F 110.0 . . ?
H15E C15 H15F 108.4 . . ?
C15 C16 H16E 109.5 . . ?
C15 C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
C15 C16 H16G 109.5 . . ?
H16E C16 H16G 109.5 . . ?
H16F C16 H16G 109.5 . . ?
C13 C14' C15' 133.6(16) . . ?
C13 C14' H14E 103.8 . . ?
C15' C14' H14E 103.8 . . ?
C13 C14' H14F 103.8 . . ?
C15' C14' H14F 103.8 . . ?
H14E C14' H14F 105.4 . . ?
C16' C15' C14' 108.8(15) . . ?
C16' C15' H15G 109.9 . . ?
C14' C15' H15G 109.9 . . ?
C16' C15' H15H 109.9 . . ?
C14' C15' H15H 109.9 . . ?
H15G C15' H15H 108.3 . . ?
C15' C16' H16H 109.5 . . ?
C15' C16' H16I 109.5 . . ?
H16H C16' H16I 109.5 . . ?
C15' C16' H16J 109.5 . . ?
H16H C16' H16J 109.5 . . ?
H16I C16' H16J 109.5 . . ?
C17 N2 C21 110.7(6) . . ?
C17 N2 C25 106.4(5) . . ?
C21 N2 C25 111.9(6) . . ?
C17 N2 C29 110.7(6) . . ?
C21 N2 C29 106.6(5) . . ?
C25 N2 C29 110.7(6) . . ?
C18 C17 N2 115.6(6) . . ?
C18 C17 H17E 108.4 . . ?
N2 C17 H17E 108.4 . . ?
C18 C17 H17F 108.4 . . ?
N2 C17 H17F 108.4 . . ?
H17E C17 H17F 107.4 . . ?
C17 C18 C19 110.6(6) . . ?
C17 C18 H18E 109.5 . . ?
C19 C18 H18E 109.5 . . ?
C17 C18 H18F 109.5 . . ?
C19 C18 H18F 109.5 . . ?
H18E C18 H18F 108.1 . . ?
C18 C19 C20 112.3(7) . . ?
C18 C19 H19G 109.1 . . ?
C20 C19 H19G 109.1 . . ?
C18 C19 H19H 109.1 . . ?
C20 C19 H19H 109.1 . . ?
H19G C19 H19H 107.9 . . ?
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 . . ?
N2 C21 C22 112.6(7) . . ?
N2 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
N2 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C23 C22 C21 117.6(10) . . ?
C23 C22 H22A 107.9 . . ?
C21 C22 H22A 107.9 . . ?
C23 C22 H22B 107.9 . . ?
C21 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23 C24 117.6(10) . . ?
C22 C23 H23A 107.8 . . ?
C24 C23 H23A 108.1 . . ?
C22 C23 H23B 106.6 . . ?
C24 C23 H23B 108.0 . . ?
H23A C23 H23B 108.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N2 114.3(6) . . ?
C26 C25 H25A 108.7 . . ?
N2 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
N2 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C25 C26 C27 111.0(6) . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C26 112.6(8) . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N2 115.5(6) . . ?
C30 C29 H29A 108.4 . . ?
N2 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
N2 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C31 C30 C29 111.9(7) . . ?
C31 C30 H30A 109.2 . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C32 113.8(8) . . ?
C30 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
H1WA O1W H1WB 101.3 . . ?
H2WA O2W H2WB 110.8 . . ?
H3WA O3W H3WB 110.1 . . ?
H4WA O4W H4WB 108.6 . . ?
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
Np1A O3A 1.818(4) . ?
Np1A O4A 1.841(5) . ?
Np1A O2A 2.353(5) . ?
Np1A O1A 2.400(5) . ?
Np1A N2A 2.587(6) . ?
Np1A N3A 2.633(5) . ?
Np1A N1A 2.638(6) . ?
O1A C7A 1.301(10) . ?
O2A C8A 1.293(10) . ?
N1A C1A 1.303(10) . ?
N1A C18A 1.460(9) . ?
N2A C14A 1.295(10) . ?
N2A C15A 1.465(9) . ?
N3A C19A 1.483(8) . ?
N3A C17A 1.486(9) . ?
N3A C16A 1.487(9) . ?
C1A C2A 1.431(11) . ?
C1A H1A 0.9300 . ?
C2A C7A 1.409(13) . ?
C2A C3A 1.416(12) . ?
C3A C4A 1.378(13) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.370(16) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.393(14) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.427(11) . ?
C6A H6A 0.9300 . ?
C8A C9A 1.428(11) . ?
C8A C13A 1.432(12) . ?
C9A C10A 1.345(14) . ?
C9A H9A 0.9300 . ?
C10A C11A 1.394(15) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.381(12) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.389(12) . ?
C12A H12A 0.9300 . ?
C13A C14A 1.458(10) . ?
C14A H14A 0.9300 . ?
C15A C16A 1.523(11) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C17A C18A 1.500(11) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C18A H18A 0.9700 . ?
C18A H18B 0.9700 . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
Np1B O3B 1.815(5) . ?
Np1B O4B 1.829(5) . ?
Np1B O2B 2.373(5) . ?
Np1B O1B 2.395(5) . ?
Np1B N2B 2.589(6) . ?
Np1B N1B 2.618(7) . ?
Np1B N3B 2.643(6) . ?
O1B C7B 1.296(9) . ?
O2B C8B 1.311(8) . ?
N1B C1B 1.276(10) . ?
N1B C18B 1.486(10) . ?
N2B C14B 1.278(9) . ?
N2B C15B 1.493(10) . ?
N3B C16B 1.379(12) . ?
N3B C17B 1.469(12) . ?
N3B C19B 1.498(12) . ?
C1B C2B 1.440(11) . ?
C1B H1B 0.9300 . ?
C2B C3B 1.401(11) . ?
C2B C7B 1.426(11) . ?
C3B C4B 1.358(12) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.384(13) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.355(11) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.409(10) . ?
C6B H6B 0.9300 . ?
C8B C9B 1.395(10) . ?
C8B C13B 1.434(10) . ?
C9B C10B 1.375(10) . ?
C9B H9B 0.9300 . ?
C10B C11B 1.392(12) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.338(12) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.400(10) . ?
C12B H12B 0.9300 . ?
C13B C14B 1.444(11) . ?
C14B H14B 0.9300 . ?
C15B C16B 1.652(14) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
C16B H16C 0.9700 . ?
C16B H16D 0.9700 . ?
C17B C18B 1.429(13) . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
C18B H18C 0.9700 . ?
C18B H18D 0.9700 . ?
C19B H19D 0.9540 . ?
C19B H19E 0.9622 . ?
C19B H19F 0.9620 . ?
N1 C5 1.490(12) . ?
N1 C13 1.508(10) . ?
N1 C1 1.517(12) . ?
N1 C9 1.526(12) . ?
C1 C2 1.516(13) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C3 1.543(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.510(14) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C5 C6 1.523(15) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 C7 1.501(14) . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.406(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.507(14) . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 C11 1.518(14) . ?
C10 H10C 0.9700 . ?
C10 H10D 0.9700 . ?
C11 C12 1.519(16) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C12 H12C 0.9600 . ?
C12 H12D 0.9600 . ?
C12 H12E 0.9600 . ?
C13 C14' 1.476(14) . ?
C13 C14 1.476(14) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.526(15) . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C15 C16 1.535(18) . ?
C15 H15E 0.9700 . ?
C15 H15F 0.9700 . ?
C16 H16E 0.9600 . ?
C16 H16F 0.9600 . ?
C16 H16G 0.9600 . ?
C14' C15' 1.546(18) . ?
C14' H14E 0.9700 . ?
C14' H14F 0.9700 . ?
C15' C16' 1.528(19) . ?
C15' H15G 0.9700 . ?
C15' H15H 0.9700 . ?
C16' H16H 0.9600 . ?
C16' H16I 0.9600 . ?
C16' H16J 0.9600 . ?
N2 C17 1.520(9) . ?
N2 C21 1.522(9) . ?
N2 C25 1.528(9) . ?
N2 C29 1.531(9) . ?
C17 C18 1.508(10) . ?
C17 H17E 0.9700 . ?
C17 H17F 0.9700 . ?
C18 C19 1.516(11) . ?
C18 H18E 0.9700 . ?
C18 H18F 0.9700 . ?
C19 C20 1.530(11) . ?
C19 H19G 0.9700 . ?
C19 H19H 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.530(13) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.450(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.475(12) . ?
C23 H23A 0.9616 . ?
C23 H23B 0.9624 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.522(10) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.532(11) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.489(13) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.512(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.486(11) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.508(12) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O1W H1WA 1.0990 . ?
O1W H1WB 1.0637 . ?
O2W H2WA 1.0135 . ?
O2W H2WB 0.9816 . ?
O3W H3WA 0.9882 . ?
O3W H3WB 1.0055 . ?
O4W H4WA 0.9740 . ?
O4W H4WB 0.9779 . ?
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
C18A N1A C1A C2A 173.5(7) . . . . ?
Np1A N1A C1A C2A -13.1(11) . . . . ?
N1A C1A C2A C7A 5.1(12) . . . . ?
N1A C1A C2A C3A -173.0(7) . . . . ?
C7A C2A C3A C4A -2.0(11) . . . . ?
C1A C2A C3A C4A 176.1(7) . . . . ?
C2A C3A C4A C5A 0.2(13) . . . . ?
C3A C4A C5A C6A 0.0(14) . . . . ?
C4A C5A C6A C7A 1.7(13) . . . . ?
Np1A O1A C7A C2A -7.1(13) . . . . ?
Np1A O1A C7A C6A 172.4(6) . . . . ?
C3A C2A C7A O1A -176.8(7) . . . . ?
C1A C2A C7A O1A 5.2(12) . . . . ?
C3A C2A C7A C6A 3.6(11) . . . . ?
C1A C2A C7A C6A -174.4(7) . . . . ?
C5A C6A C7A O1A 177.0(7) . . . . ?
C5A C6A C7A C2A -3.4(11) . . . . ?
Np1A O2A C8A C9A 147.1(6) . . . . ?
Np1A O2A C8A C13A -36.1(11) . . . . ?
O2A C8A C9A C10A 177.3(8) . . . . ?
C13A C8A C9A C10A 0.3(12) . . . . ?
C8A C9A C10A C11A -1.1(14) . . . . ?
C9A C10A C11A C12A 1.0(14) . . . . ?
C10A C11A C12A C13A -0.2(14) . . . . ?
C11A C12A C13A C8A -0.6(12) . . . . ?
C11A C12A C13A C14A -179.5(8) . . . . ?
O2A C8A C13A C12A -176.4(7) . . . . ?
C9A C8A C13A C12A 0.5(11) . . . . ?
O2A C8A C13A C14A 2.5(12) . . . . ?
C9A C8A C13A C14A 179.4(7) . . . . ?
C15A N2A C14A C13A 177.7(7) . . . . ?
Np1A N2A C14A C13A 14.5(11) . . . . ?
C12A C13A C14A N2A -175.6(8) . . . . ?
C8A C13A C14A N2A 5.5(12) . . . . ?
C14A N2A C15A C16A -129.7(7) . . . . ?
Np1A N2A C15A C16A 35.7(7) . . . . ?
C19A N3A C16A C15A -71.0(7) . . . . ?
C17A N3A C16A C15A 168.4(6) . . . . ?
Np1A N3A C16A C15A 53.1(6) . . . . ?
N2A C15A C16A N3A -60.8(8) . . . . ?
C19A N3A C17A C18A 66.5(8) . . . . ?
C16A N3A C17A C18A -172.7(6) . . . . ?
Np1A N3A C17A C18A -56.8(7) . . . . ?
C1A N1A C18A C17A 150.5(7) . . . . ?
Np1A N1A C18A C17A -23.9(7) . . . . ?
N3A C17A C18A N1A 55.7(8) . . . . ?
C18B N1B C1B C2B 179.8(8) . . . . ?
Np1B N1B C1B C2B -9.3(12) . . . . ?
N1B C1B C2B C3B -176.2(8) . . . . ?
N1B C1B C2B C7B 3.7(13) . . . . ?
C7B C2B C3B C4B 1.5(12) . . . . ?
C1B C2B C3B C4B -178.5(8) . . . . ?
C2B C3B C4B C5B -1.3(13) . . . . ?
C3B C4B C5B C6B 0.6(13) . . . . ?
C4B C5B C6B C7B -0.2(13) . . . . ?
Np1B O1B C7B C6B -171.4(5) . . . . ?
Np1B O1B C7B C2B 10.6(13) . . . . ?
C5B C6B C7B O1B -177.7(8) . . . . ?
C5B C6B C7B C2B 0.4(11) . . . . ?
C3B C2B C7B O1B 177.1(7) . . . . ?
C1B C2B C7B O1B -2.9(12) . . . . ?
C3B C2B C7B C6B -1.0(10) . . . . ?
C1B C2B C7B C6B 179.0(7) . . . . ?
Np1B O2B C8B C9B 149.5(5) . . . . ?
Np1B O2B C8B C13B -31.9(10) . . . . ?
O2B C8B C9B C10B 179.4(7) . . . . ?
C13B C8B C9B C10B 0.7(11) . . . . ?
C8B C9B C10B C11B 0.6(13) . . . . ?
C9B C10B C11B C12B -1.8(14) . . . . ?
C10B C11B C12B C13B 1.8(14) . . . . ?
C11B C12B C13B C8B -0.5(12) . . . . ?
C11B C12B C13B C14B -175.5(8) . . . . ?
O2B C8B C13B C12B -179.4(7) . . . . ?
C9B C8B C13B C12B -0.7(10) . . . . ?
O2B C8B C13B C14B -4.7(11) . . . . ?
C9B C8B C13B C14B 173.9(7) . . . . ?
C15B N2B C14B C13B -178.1(8) . . . . ?
Np1B N2B C14B C13B 14.2(11) . . . . ?
C12B C13B C14B N2B -174.5(8) . . . . ?
C8B C13B C14B N2B 10.9(12) . . . . ?
C14B N2B C15B C16B -129.2(8) . . . . ?
Np1B N2B C15B C16B 40.0(8) . . . . ?
C17B N3B C16B C15B 174.8(8) . . . . ?
C19B N3B C16B C15B -70.2(10) . . . . ?
Np1B N3B C16B C15B 57.7(8) . . . . ?
N2B C15B C16B N3B -66.6(10) . . . . ?
C16B N3B C17B C18B -168.4(10) . . . . ?
C19B N3B C17B C18B 69.8(11) . . . . ?
Np1B N3B C17B C18B -49.6(11) . . . . ?
N3B C17B C18B N1B 48.6(13) . . . . ?
C1B N1B C18B C17B 153.2(9) . . . . ?
Np1B N1B C18B C17B -19.1(10) . . . . ?
C5 N1 C1 C2 -49.9(11) . . . . ?
C13 N1 C1 C2 67.6(10) . . . . ?
C9 N1 C1 C2 -173.1(8) . . . . ?
N1 C1 C2 C3 -163.4(8) . . . . ?
C1 C2 C3 C4 -173.0(9) . . . . ?
C13 N1 C5 C6 -175.5(10) . . . . ?
C1 N1 C5 C6 -54.6(13) . . . . ?
C9 N1 C5 C6 65.3(13) . . . . ?
N1 C5 C6 C7 170.6(11) . . . . ?
C5 C6 C7 C8 -178.2(17) . . . . ?
C5 N1 C9 C10 63.3(10) . . . . ?
C13 N1 C9 C10 -53.5(11) . . . . ?
C1 N1 C9 C10 -173.8(8) . . . . ?
N1 C9 C10 C11 179.0(9) . . . . ?
C9 C10 C11 C12 -168.7(10) . . . . ?
C5 N1 C13 C14' -178.5(10) . . . . ?
C1 N1 C13 C14' 60.2(11) . . . . ?
C9 N1 C13 C14' -57.3(12) . . . . ?
C5 N1 C13 C14 -178.5(10) . . . . ?
C1 N1 C13 C14 60.2(11) . . . . ?
C9 N1 C13 C14 -57.3(12) . . . . ?
N1 C13 C14 C15 172.0(11) . . . . ?
C13 C14 C15 C16 178.3(13) . . . . ?
N1 C13 C14' C15' -157.3(15) . . . . ?
C13 C14' C15' C16' 83(3) . . . . ?
C21 N2 C17 C18 -58.0(8) . . . . ?
C25 N2 C17 C18 -179.8(6) . . . . ?
C29 N2 C17 C18 59.9(8) . . . . ?
N2 C17 C18 C19 170.8(6) . . . . ?
C17 C18 C19 C20 -177.8(7) . . . . ?
C17 N2 C21 C22 -58.7(10) . . . . ?
C25 N2 C21 C22 59.7(10) . . . . ?
C29 N2 C21 C22 -179.1(8) . . . . ?
N2 C21 C22 C23 159.2(10) . . . . ?
C21 C22 C23 C24 -179.5(11) . . . . ?
C17 N2 C25 C26 174.6(6) . . . . ?
C21 N2 C25 C26 53.7(8) . . . . ?
C29 N2 C25 C26 -65.1(7) . . . . ?
N2 C25 C26 C27 174.5(6) . . . . ?
C25 C26 C27 C28 -178.7(7) . . . . ?
C17 N2 C29 C30 59.4(8) . . . . ?
C21 N2 C29 C30 179.9(7) . . . . ?
C25 N2 C29 C30 -58.2(8) . . . . ?
N2 C29 C30 C31 -174.6(7) . . . . ?
C29 C30 C31 C32 -178.6(8) . . . . ?
