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#$Date: 2025-01-06 14:24:46 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297109 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717313.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_7717313
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
'4(C19 H21 N3 Np O4), 2(C16 H36 N), 2(C16 H34 N), 5(H2 O)'
_chemical_formula_sum            'C140 H234 N16 Np4 O21'
_chemical_formula_weight         3425.42
_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
;
2024-08-23 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.7700(10)
_cell_angle_beta                 98.4830(10)
_cell_angle_gamma                94.1060(10)
_cell_formula_units_Z            1
_cell_length_a                   9.9804(7)
_cell_length_b                   18.0918(13)
_cell_length_c                   21.0492(15)
_cell_measurement_reflns_used    6563
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.7625
_cell_measurement_theta_min      2.34
_cell_volume                     3738.3(5)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (G. Sheldrick)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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            33158
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_min         1.132
_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    2.824
_exptl_absorpt_correction_T_max  0.0285
_exptl_absorpt_correction_T_min  0.0107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS 2016/2: 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    1.522
_exptl_crystal_description       needle
_exptl_crystal_F_000             1726
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.0285
_exptl_transmission_factor_min   0.0107
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         17116
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10007
_reflns_number_total             17116
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02557a3.cif
_cod_data_source_block           m36a
_cod_depositor_comments
'Adding full bibliography for 7717312--7717314.cif.'
_cod_original_cell_volume        3738.2(5)
_cod_database_code               7717313
_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   0.0107
_shelx_estimated_absorpt_t_max   0.0285
_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 0.37893(3) -0.07339(2) 0.85541(2) 0.05053(9) Uani 1 1 d . . . . .
O1A O 0.6041(4) -0.1016(3) 0.8957(2) 0.0586(12) Uani 1 1 d . . . . .
O2A O 0.4547(4) -0.0789(3) 0.7524(2) 0.0632(13) Uani 1 1 d . . . . .
O3A O 0.4282(4) 0.0250(2) 0.8672(2) 0.0540(11) Uani 1 1 d . . . . .
O4A O 0.3165(5) -0.1712(2) 0.8450(2) 0.0595(12) Uani 1 1 d . . . . .
N1A N 0.3980(5) -0.0923(3) 0.9778(3) 0.0555(14) Uani 1 1 d . . . . .
N2A N 0.1736(5) -0.0564(3) 0.7646(3) 0.0568(15) Uani 1 1 d . . . . .
N3A N 0.1544(6) -0.0458(3) 0.9023(3) 0.0635(16) Uani 1 1 d . . . . .
C1A C 0.4778(7) -0.1320(4) 1.0102(3) 0.0588(18) Uani 1 1 d . . . . .
H1AA H 0.4573 -0.1417 1.0517 0.071 Uiso 1 1 calc R U . . .
C2A C 0.5967(7) -0.1646(4) 0.9920(3) 0.0528(17) Uani 1 1 d . . . . .
C3A C 0.6615(7) -0.2120(4) 1.0336(3) 0.0623(19) Uani 1 1 d . . . . .
H3AA H 0.6226 -0.2239 1.0706 0.075 Uiso 1 1 calc R U . . .
C4A C 0.7801(8) -0.2423(5) 1.0235(4) 0.072(2) Uani 1 1 d . . . . .
H4AA H 0.8205 -0.2756 1.0523 0.087 Uiso 1 1 calc R U . . .
C5A C 0.8393(7) -0.2234(5) 0.9707(4) 0.069(2) Uani 1 1 d . . . . .
H5AA H 0.9223 -0.2426 0.9636 0.083 Uiso 1 1 calc R U . . .
C6A C 0.7778(6) -0.1771(4) 0.9291(3) 0.0546(17) Uani 1 1 d . . . . .
H6AA H 0.8196 -0.1653 0.8929 0.066 Uiso 1 1 calc R U . . .
C7A C 0.6566(6) -0.1464(3) 0.9370(3) 0.0501(16) Uani 1 1 d . . . . .
C8A C 0.4118(7) -0.0859(4) 0.6911(3) 0.0562(18) Uani 1 1 d . . . . .
C9A C 0.5000(8) -0.0995(4) 0.6460(4) 0.0643(19) Uani 1 1 d . . . . .
H9AA H 0.5927 -0.1055 0.6614 0.077 Uiso 1 1 calc R U . . .
C10A C 0.4571(9) -0.1045(4) 0.5806(4) 0.075(2) Uani 1 1 d . . . . .
H10C H 0.5208 -0.1131 0.5522 0.090 Uiso 1 1 calc R U . . .
C11A C 0.3234(9) -0.0973(4) 0.5555(4) 0.075(2) Uani 1 1 d . . . . .
H11C H 0.2945 -0.1004 0.5103 0.090 Uiso 1 1 calc R U . . .
C12A C 0.2340(8) -0.0856(4) 0.5975(4) 0.070(2) Uani 1 1 d . . . . .
H12D H 0.1417 -0.0812 0.5803 0.084 Uiso 1 1 calc R U . . .
C13A C 0.2706(7) -0.0798(4) 0.6647(3) 0.0531(17) Uani 1 1 d . . . . .
C14A C 0.1658(7) -0.0675(4) 0.7037(4) 0.0602(18) Uani 1 1 d . . . . .
H14A H 0.0767 -0.0678 0.6802 0.072 Uiso 1 1 calc R U . . .
C15A C 0.0448(7) -0.0460(5) 0.7877(4) 0.068(2) Uani 1 1 d . . . . .
H15A H -0.0303 -0.0721 0.7565 0.081 Uiso 1 1 calc R U . . .
H15B H 0.0302 0.0077 0.7900 0.081 Uiso 1 1 calc R U . . .
C16A C 0.0409(7) -0.0739(5) 0.8512(4) 0.078(2) Uani 1 1 d . . . . .
H16D H 0.0391 -0.1288 0.8466 0.093 Uiso 1 1 calc R U . . .
H16E H -0.0452 -0.0612 0.8657 0.093 Uiso 1 1 calc R U . . .
C17A C 0.1491(8) -0.0863(6) 0.9598(4) 0.089(3) Uani 1 1 d . . . . .
H17C H 0.1381 -0.1404 0.9477 0.107 Uiso 1 1 calc R U . . .
H17D H 0.0703 -0.0727 0.9803 0.107 Uiso 1 1 calc R U . . .
C18A C 0.2846(8) -0.0662(5) 1.0085(4) 0.071(2) Uani 1 1 d . . . . .
H18C H 0.2985 -0.0117 1.0190 0.085 Uiso 1 1 calc R U . . .
H18D H 0.2797 -0.0906 1.0490 0.085 Uiso 1 1 calc R U . . .
C19A C 0.1418(8) 0.0367(4) 0.9159(4) 0.088(3) Uani 1 1 d . . . . .
H19C H 0.2126 0.0567 0.9514 0.132 Uiso 1 1 calc R U . . .
H19D H 0.0521 0.0441 0.9279 0.132 Uiso 1 1 calc R U . . .
H19E H 0.1524 0.0626 0.8773 0.132 Uiso 1 1 calc R U . . .
Np1B Np 0.42063(3) 0.41356(2) 0.63087(2) 0.05097(9) Uani 1 1 d . . . . .
O1B O 0.6406(5) 0.3680(3) 0.6518(2) 0.0673(14) Uani 1 1 d . . . . .
O2B O 0.4401(5) 0.4328(3) 0.7435(2) 0.0619(13) Uani 1 1 d . . . . .
O3B O 0.3270(4) 0.3244(2) 0.6328(2) 0.0493(11) Uani 1 1 d . . . . .
O4B O 0.5028(4) 0.5065(2) 0.6252(2) 0.0603(12) Uani 1 1 d . . . . .
N1B N 0.4891(5) 0.3546(3) 0.5232(3) 0.0549(14) Uani 1 1 d . . . . .
N2B N 0.1994(6) 0.4652(3) 0.6593(3) 0.0527(14) Uani 1 1 d . . . . .
N3B N 0.2468(5) 0.4320(3) 0.5277(3) 0.0498(13) Uani 1 1 d . . . . .
C1B C 0.5885(7) 0.3162(4) 0.5145(4) 0.0603(19) Uani 1 1 d . . . . .
H1BA H 0.5829 0.2908 0.4731 0.072 Uiso 1 1 calc R U . . .
C2B C 0.7087(7) 0.3065(4) 0.5599(4) 0.064(2) Uani 1 1 d . . . . .
C3B C 0.8091(8) 0.2676(4) 0.5356(5) 0.079(2) Uani 1 1 d . . . . .
H3BA H 0.7908 0.2458 0.4926 0.095 Uiso 1 1 calc R U . . .
C4B C 0.9348(9) 0.2597(5) 0.5722(6) 0.097(3) Uani 1 1 d . . . . .
H4BA H 1.0021 0.2341 0.5545 0.117 Uiso 1 1 calc R U . . .
C5B C 0.9587(9) 0.2907(6) 0.6355(6) 0.110(4) Uani 1 1 d . . . . .
H5BA H 1.0447 0.2875 0.6610 0.132 Uiso 1 1 calc R U . . .
C6B C 0.8602(7) 0.3257(5) 0.6618(4) 0.081(3) Uani 1 1 d . . . . .
H6BA H 0.8784 0.3442 0.7057 0.097 Uiso 1 1 calc R U . . .
C7B C 0.7311(7) 0.3353(4) 0.6251(4) 0.067(2) Uani 1 1 d . . . . .
C8B C 0.3600(9) 0.4253(4) 0.7845(4) 0.062(2) Uani 1 1 d . . . . .
C9B C 0.4085(9) 0.4050(4) 0.8479(4) 0.074(2) Uani 1 1 d . . . . .
H9BA H 0.5007 0.3942 0.8574 0.089 Uiso 1 1 calc R U . . .
C10B C 0.3310(11) 0.4005(5) 0.8945(4) 0.086(3) Uani 1 1 d . . . . .
H10D H 0.3697 0.3876 0.9358 0.103 Uiso 1 1 calc R U . . .
C11B C 0.1941(11) 0.4145(5) 0.8832(4) 0.092(3) Uani 1 1 d . . . . .
H11D H 0.1397 0.4109 0.9164 0.110 Uiso 1 1 calc R U . . .
C12B C 0.1380(9) 0.4339(4) 0.8225(3) 0.073(2) Uani 1 1 d . . . . .
H12E H 0.0449 0.4433 0.8144 0.088 Uiso 1 1 calc R U . . .
C13B C 0.2176(8) 0.4394(4) 0.7738(3) 0.0603(19) Uani 1 1 d . . . . .
C14B C 0.1499(7) 0.4608(4) 0.7118(3) 0.0569(18) Uani 1 1 d . . . . .
H14B H 0.0585 0.4729 0.7105 0.068 Uiso 1 1 calc R U . . .
C15B C 0.1042(7) 0.4851(4) 0.6047(3) 0.0582(18) Uani 1 1 d . . . . .
H15C H 0.1288 0.5364 0.5943 0.070 Uiso 1 1 calc R U . . .
H15D H 0.0108 0.4828 0.6156 0.070 Uiso 1 1 calc R U . . .
C16B C 0.1106(7) 0.4299(4) 0.5464(3) 0.0566(18) Uani 1 1 d . . . . .
H16F H 0.0843 0.3789 0.5572 0.068 Uiso 1 1 calc R U . . .
H16G H 0.0444 0.4419 0.5094 0.068 Uiso 1 1 calc R U . . .
C17B C 0.2495(7) 0.3676(4) 0.4812(3) 0.0639(19) Uani 1 1 d . . . . .
H17E H 0.1867 0.3738 0.4412 0.077 Uiso 1 1 calc R U . . .
H17F H 0.2170 0.3218 0.4995 0.077 Uiso 1 1 calc R U . . .
C18B C 0.3900(7) 0.3594(4) 0.4651(3) 0.0621(19) Uani 1 1 d . . . . .
H18E H 0.3885 0.3140 0.4360 0.074 Uiso 1 1 calc R U . . .
H18F H 0.4182 0.4026 0.4422 0.074 Uiso 1 1 calc R U . . .
C19B C 0.2776(7) 0.5028(4) 0.4981(3) 0.0579(18) Uani 1 1 d . . . . .
H19F H 0.2766 0.5449 0.5297 0.087 Uiso 1 1 calc R U . . .
H19G H 0.2089 0.5072 0.4605 0.087 Uiso 1 1 calc R U . . .
H19H H 0.3676 0.5028 0.4848 0.087 Uiso 1 1 calc R U . . .
N1 N 0.5362(6) 0.1550(3) 0.7088(3) 0.0563(15) Uani 1 1 d . . . . .
C1 C 0.4727(7) 0.1810(4) 0.6457(3) 0.0584(18) Uani 1 1 d . . . . .
H1A H 0.5464 0.2005 0.6231 0.070 Uiso 1 1 calc R U . . .
H1B H 0.4181 0.2229 0.6550 0.070 Uiso 1 1 calc R U . . .
C2 C 0.3829(7) 0.1233(4) 0.6008(4) 0.064(2) Uani 1 1 d . . . . .
H2A H 0.3186 0.0968 0.6248 0.077 Uiso 1 1 calc R U . . .
H2B H 0.4394 0.0864 0.5834 0.077 Uiso 1 1 calc R U . . .
C3 C 0.3032(7) 0.1600(4) 0.5450(4) 0.064(2) Uani 1 1 d . . . . .
H3A H 0.2497 0.1982 0.5628 0.076 Uiso 1 1 calc R U . . .
H3B H 0.3682 0.1853 0.5207 0.076 Uiso 1 1 calc R U . . .
C4 C 0.2084(8) 0.1049(5) 0.4996(4) 0.083(2) Uani 1 1 d . . . . .
H4A H 0.1560 0.1313 0.4665 0.124 Uiso 1 1 calc R U . . .
H4B H 0.1462 0.0782 0.5238 0.124 Uiso 1 1 calc R U . . .
H4C H 0.2615 0.0693 0.4791 0.124 Uiso 1 1 calc R U . . .
C5 C 0.6268(7) 0.0927(4) 0.6971(3) 0.0590(18) Uani 1 1 d . . . . .
H5A H 0.6634 0.0751 0.7392 0.071 Uiso 1 1 calc R U . . .
H5B H 0.5698 0.0507 0.6718 0.071 Uiso 1 1 calc R U . . .
C6 C 0.7444(6) 0.1131(4) 0.6623(4) 0.0604(19) Uani 1 1 d . . . . .
H6A H 0.7102 0.1354 0.6220 0.072 Uiso 1 1 calc R U . . .
H6B H 0.8085 0.1507 0.6897 0.072 Uiso 1 1 calc R U . . .
C7 C 0.8176(9) 0.0463(5) 0.6468(4) 0.090(3) Uani 1 1 d . . . . .
H7A H 0.7526 0.0090 0.6197 0.107 Uiso 1 1 calc R U . . .
H7B H 0.8504 0.0241 0.6873 0.107 Uiso 1 1 calc R U . . .
C8 C 0.9365(8) 0.0632(5) 0.6122(4) 0.082(2) Uani 1 1 d . . . . .
H8A H 0.9074 0.0909 0.5749 0.123 Uiso 1 1 calc R U . . .
H8B H 0.9708 0.0165 0.5977 0.123 Uiso 1 1 calc R U . . .
H8C H 1.0086 0.0930 0.6415 0.123 Uiso 1 1 calc R U . . .
C9 C 0.6202(7) 0.2221(4) 0.7466(3) 0.0597(18) Uani 1 1 d . . . . .
H9A H 0.5606 0.2633 0.7491 0.072 Uiso 1 1 calc R U . . .
H9B H 0.6929 0.2383 0.7220 0.072 Uiso 1 1 calc R U . . .
C10 C 0.6861(7) 0.2095(4) 0.8152(3) 0.070(2) Uani 1 1 d . . . . .
H10A H 0.6145 0.1997 0.8422 0.084 Uiso 1 1 calc R U . . .
H10B H 0.7394 0.1654 0.8141 0.084 Uiso 1 1 calc R U . . .
C11 C 0.7779(8) 0.2766(5) 0.8443(4) 0.076(2) Uani 1 1 d . . . . .
H11A H 0.7247 0.3207 0.8448 0.092 Uiso 1 1 calc R U . . .
H11B H 0.8501 0.2859 0.8175 0.092 Uiso 1 1 calc R U . . .
C12 C 0.8430(9) 0.2648(6) 0.9134(4) 0.111(3) Uani 1 1 d . . . . .
H12A H 0.9026 0.2241 0.9124 0.166 Uiso 1 1 calc R U . . .
H12B H 0.7716 0.2523 0.9391 0.166 Uiso 1 1 calc R U . . .
H12C H 0.8964 0.3105 0.9326 0.166 Uiso 1 1 calc R U . . .
C13 C 0.4281(8) 0.1253(4) 0.7463(4) 0.072(2) Uani 1 1 d . . . . .
H13A H 0.3789 0.0805 0.7217 0.087 Uiso 1 1 calc R U . . .
H13B H 0.4739 0.1096 0.7877 0.087 Uiso 1 1 calc R U . . .
C14 C 0.3251(8) 0.1787(5) 0.7608(6) 0.126(3) Uani 1 1 d D U . . .
H14 H 0.3455 0.2307 0.7601 0.152 Uiso 1 1 calc R U . . .
C15 C 0.2094(9) 0.1534(5) 0.7742(6) 0.138(3) Uani 1 1 d . U . . .
H15 H 0.1910 0.1012 0.7740 0.165 Uiso 1 1 calc R U . . .
C16 C 0.1015(8) 0.2030(5) 0.7900(4) 0.085(3) Uani 1 1 d D . . . .
H16A H 0.0394 0.2097 0.7506 0.128 Uiso 1 1 calc R U . . .
H16B H 0.1447 0.2514 0.8088 0.128 Uiso 1 1 calc R U . . .
H16C H 0.0504 0.1800 0.8209 0.128 Uiso 1 1 calc R U . . .
N2 N 0.5281(7) 0.6579(3) 0.8004(3) 0.0774(19) Uani 1 1 d . . . . .
C17 C 0.6139(9) 0.7258(4) 0.7871(4) 0.079(2) Uani 1 1 d . . . . .
H17A H 0.6921 0.7352 0.8222 0.095 Uiso 1 1 calc R U . . .
H17B H 0.5588 0.7692 0.7885 0.095 Uiso 1 1 calc R U . . .
C18 C 0.6683(9) 0.7216(5) 0.7231(4) 0.081(2) Uani 1 1 d . . . . .
H18A H 0.5948 0.7285 0.6875 0.097 Uiso 1 1 calc R U . . .
H18B H 0.7022 0.6723 0.7152 0.097 Uiso 1 1 calc R U . . .
C19 C 0.7836(10) 0.7825(6) 0.7258(4) 0.101(3) Uani 1 1 d . . . . .
H19A H 0.8637 0.7697 0.7555 0.121 Uiso 1 1 calc R U . . .
H19B H 0.7548 0.8300 0.7431 0.121 Uiso 1 1 calc R U . . .
C20 C 0.8236(12) 0.7923(5) 0.6591(5) 0.122(4) Uani 1 1 d . . . . .
H20A H 0.7426 0.8000 0.6286 0.183 Uiso 1 1 calc R U . . .
H20B H 0.8640 0.7477 0.6444 0.183 Uiso 1 1 calc R U . . .
H20C H 0.8899 0.8355 0.6617 0.183 Uiso 1 1 calc R U . . .
C21 C 0.4130(9) 0.6360(5) 0.7451(4) 0.093(3) Uani 1 1 d D . . . .
H21A H 0.4522 0.6171 0.7073 0.112 Uiso 1 1 calc R U . A 1
H21B H 0.3539 0.5948 0.7576 0.112 Uiso 1 1 calc R U . A 1
C22 C 0.3264(10) 0.6983(6) 0.7257(5) 0.124(3) Uani 0.560(12) 1 d D U P B 1
H22C H 0.3844 0.7442 0.7226 0.149 Uiso 0.560(12) 1 calc R U P B 1
H22D H 0.2655 0.7085 0.7577 0.149 Uiso 0.560(12) 1 calc R U P B 1
C23 C 0.2400(18) 0.6710(9) 0.6573(8) 0.107(5) Uani 0.560(12) 1 d D U P B 1
H23C H 0.3018 0.6643 0.6250 0.128 Uiso 0.560(12) 1 calc R U P B 1
H23D H 0.1894 0.6225 0.6600 0.128 Uiso 0.560(12) 1 calc R U P B 1
C24 C 0.1459(16) 0.7251(10) 0.6376(8) 0.112(6) Uani 0.560(12) 1 d D U P B 1
H24D H 0.0774 0.7029 0.6020 0.168 Uiso 0.560(12) 1 calc R U P B 1
H24E H 0.1954 0.7682 0.6234 0.168 Uiso 0.560(12) 1 calc R U P B 1
H24F H 0.1011 0.7410 0.6740 0.168 Uiso 0.560(12) 1 calc R U P B 1
C22' C 0.3264(10) 0.6983(6) 0.7257(5) 0.124(3) Uani 0.440(12) 1 d D U P B 2
H22A H 0.3752 0.7296 0.6982 0.149 Uiso 0.440(12) 1 calc R U P B 2
H22B H 0.3183 0.7296 0.7651 0.149 Uiso 0.440(12) 1 calc R U P B 2
C23' C 0.1812(17) 0.6755(13) 0.6892(12) 0.114(5) Uani 0.440(12) 1 d D U P B 2
H23A H 0.1467 0.7178 0.6659 0.136 Uiso 0.440(12) 1 calc R U P B 2
H23B H 0.1843 0.6334 0.6571 0.136 Uiso 0.440(12) 1 calc R U P B 2
C24' C 0.085(2) 0.6529(19) 0.7361(15) 0.204(14) Uani 0.440(12) 1 d D U P B 2
H24A H 0.0127 0.6165 0.7138 0.306 Uiso 0.440(12) 1 calc R U P B 2
H24B H 0.0437 0.6969 0.7518 0.306 Uiso 0.440(12) 1 calc R U P B 2
H24C H 0.1353 0.6309 0.7726 0.306 Uiso 0.440(12) 1 calc R U P B 2
C25 C 0.4740(8) 0.6783(4) 0.8632(4) 0.079(2) Uani 1 1 d . . . . .
H25A H 0.5517 0.6988 0.8958 0.095 Uiso 1 1 calc R U . . .
H25B H 0.4123 0.7184 0.8554 0.095 Uiso 1 1 calc R U . . .
C26 C 0.3979(10) 0.6154(5) 0.8914(5) 0.108(3) Uani 1 1 d D . . . .
H26A H 0.3209 0.5932 0.8592 0.130 Uiso 1 1 calc R U . . .
H26B H 0.4597 0.5761 0.9025 0.130 Uiso 1 1 calc R U . . .
C27 C 0.3456(13) 0.6448(5) 0.9511(6) 0.132(4) Uani 1 1 d . U . . .
H27A H 0.4164 0.6803 0.9767 0.158 Uiso 1 1 calc R U . . .
H27B H 0.2649 0.6722 0.9381 0.158 Uiso 1 1 calc R U . . .
C28 C 0.3081(14) 0.5848(7) 0.9921(6) 0.167(4) Uani 1 1 d D U . . .
H28A H 0.2313 0.5524 0.9686 0.251 Uiso 1 1 calc R U . . .
H28B H 0.2824 0.6070 1.0318 0.251 Uiso 1 1 calc R U . . .
H28C H 0.3860 0.5554 1.0029 0.251 Uiso 1 1 calc R U . . .
C29 C 0.6127(9) 0.5921(5) 0.8074(4) 0.082(2) Uani 1 1 d . U . . .
H29A H 0.5525 0.5478 0.8128 0.099 Uiso 1 1 calc R U . . .
H29B H 0.6505 0.5825 0.7670 0.099 Uiso 1 1 calc R U . . .
C30 C 0.7274(11) 0.6011(6) 0.8624(5) 0.127(3) Uani 1 1 d D U . . .
H30A H 0.6926 0.6145 0.9029 0.153 Uiso 1 1 calc R U . . .
H30B H 0.7945 0.6416 0.8553 0.153 Uiso 1 1 calc R U . . .
C31 C 0.7948(12) 0.5291(7) 0.8677(6) 0.137(3) Uani 1 1 d . U . . .
H31A H 0.7265 0.4889 0.8741 0.165 Uiso 1 1 calc R U . . .
H31B H 0.8285 0.5160 0.8268 0.165 Uiso 1 1 calc R U . . .
C32 C 0.9084(13) 0.5334(8) 0.9208(7) 0.187(6) Uani 1 1 d D U . . .
H32A H 0.9704 0.5772 0.9180 0.281 Uiso 1 1 calc R U . . .
H32B H 0.9573 0.4885 0.9182 0.281 Uiso 1 1 calc R U . . .
H32C H 0.8734 0.5375 0.9619 0.281 Uiso 1 1 calc R U . . .
O1W O 0.7263(4) -0.0280(3) 0.8012(2) 0.0774(16) Uani 1 1 d . . . . .
H1WA H 0.6493 -0.0494 0.7690 0.116 Uiso 1 1 d . U . . .
H1WB H 0.7116 -0.0424 0.8435 0.116 Uiso 1 1 d . U . . .
O2W O 0.7793(5) 0.5347(3) 0.6782(2) 0.0816(16) Uani 1 1 d . . . . .
H2WA H 0.7823 0.4989 0.7110 0.122 Uiso 1 1 d . U . . .
H2WB H 0.6866 0.5300 0.6565 0.122 Uiso 1 1 d . U . . .
O3W O 0.7401(13) 0.4332(7) 0.7603(6) 0.103(4) Uani 0.5 1 d . . P . .
H3WA H 0.7220 0.4056 0.7170 0.155 Uiso 0.5 1 d . U P . .
H3WB H 0.6476 0.4429 0.7688 0.155 Uiso 0.5 1 d . U P . .
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'
Np Np -11.4937 4.1493 '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'
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 175.63(19) . . ?
O3A Np1A O1A 91.27(18) . . ?
O4A Np1A O1A 92.37(18) . . ?
O3A Np1A O2A 90.66(18) . . ?
O4A Np1A O2A 92.07(18) . . ?
O1A Np1A O2A 84.87(15) . . ?
O3A Np1A N1A 94.67(18) . . ?
O4A Np1A N1A 84.29(19) . . ?
O1A Np1A N1A 70.42(16) . . ?
O2A Np1A N1A 154.79(17) . . ?
O3A Np1A N2A 93.03(18) . . ?
O4A Np1A N2A 84.67(19) . . ?
O1A Np1A N2A 154.95(16) . . ?
O2A Np1A N2A 70.42(16) . . ?
N1A Np1A N2A 133.63(17) . . ?
O3A Np1A N3A 87.76(18) . . ?
O4A Np1A N3A 87.92(19) . . ?
O1A Np1A N3A 137.59(17) . . ?
O2A Np1A N3A 137.52(18) . . ?
N1A Np1A N3A 67.42(18) . . ?
N2A Np1A N3A 67.29(18) . . ?
C7A O1A Np1A 134.9(4) . . ?
C8A O2A Np1A 142.8(4) . . ?
C1A N1A C18A 116.6(6) . . ?
C1A N1A Np1A 127.5(5) . . ?
C18A N1A Np1A 114.7(4) . . ?
C14A N2A C15A 115.2(6) . . ?
C14A N2A Np1A 128.9(5) . . ?
C15A N2A Np1A 114.9(4) . . ?
C17A N3A C16A 110.2(6) . . ?
C17A N3A C19A 111.7(6) . . ?
C16A N3A C19A 107.3(6) . . ?
C17A N3A Np1A 108.8(4) . . ?
C16A N3A Np1A 105.8(4) . . ?
C19A N3A Np1A 112.9(4) . . ?
N1A C1A C2A 128.1(6) . . ?
N1A C1A H1AA 116.0 . . ?
C2A C1A H1AA 116.0 . . ?
C3A C2A C7A 118.4(6) . . ?
C3A C2A C1A 117.5(6) . . ?
C7A C2A C1A 124.0(6) . . ?
C4A C3A C2A 122.6(7) . . ?
C4A C3A H3AA 118.7 . . ?
C2A C3A H3AA 118.7 . . ?
C3A C4A C5A 118.9(7) . . ?
C3A C4A H4AA 120.6 . . ?
C5A C4A H4AA 120.6 . . ?
C6A C5A C4A 119.7(7) . . ?
C6A C5A H5AA 120.2 . . ?
C4A C5A H5AA 120.2 . . ?
C5A C6A C7A 123.1(7) . . ?
C5A C6A H6AA 118.4 . . ?
C7A C6A H6AA 118.4 . . ?
O1A C7A C6A 120.0(6) . . ?
O1A C7A C2A 122.7(6) . . ?
C6A C7A C2A 117.3(6) . . ?
O2A C8A C9A 121.7(7) . . ?
O2A C8A C13A 122.2(6) . . ?
C9A C8A C13A 116.1(6) . . ?
C10A C9A C8A 122.5(7) . . ?
C10A C9A H9AA 118.7 . . ?
C8A C9A H9AA 118.7 . . ?
C9A C10A C11A 121.4(8) . . ?
C9A C10A H10C 119.3 . . ?
C11A C10A H10C 119.3 . . ?
C12A C11A C10A 118.0(7) . . ?
C12A C11A H11C 121.0 . . ?
C10A C11A H11C 121.0 . . ?
C11A C12A C13A 123.7(7) . . ?
C11A C12A H12D 118.2 . . ?
C13A C12A H12D 118.2 . . ?
C12A C13A C14A 118.0(7) . . ?
C12A C13A C8A 118.2(7) . . ?
C14A C13A C8A 123.7(6) . . ?
N2A C14A C13A 130.2(7) . . ?
N2A C14A H14A 114.9 . . ?
C13A C14A H14A 114.9 . . ?
N2A C15A C16A 112.3(6) . . ?
N2A C15A H15A 109.1 . . ?
C16A C15A H15A 109.1 . . ?
N2A C15A H15B 109.1 . . ?
C16A C15A H15B 109.1 . . ?
H15A C15A H15B 107.9 . . ?
C15A C16A N3A 116.1(6) . . ?
C15A C16A H16D 108.3 . . ?
N3A C16A H16D 108.3 . . ?
C15A C16A H16E 108.3 . . ?
N3A C16A H16E 108.3 . . ?
H16D C16A H16E 107.4 . . ?
N3A C17A C18A 109.3(6) . . ?
N3A C17A H17C 109.8 . . ?
C18A C17A H17C 109.8 . . ?
N3A C17A H17D 109.8 . . ?
C18A C17A H17D 109.8 . . ?
H17C C17A H17D 108.3 . . ?
N1A C18A C17A 107.9(6) . . ?
N1A C18A H18C 110.1 . . ?
C17A C18A H18C 110.1 . . ?
N1A C18A H18D 110.1 . . ?
C17A C18A H18D 110.1 . . ?
H18C C18A H18D 108.4 . . ?
N3A C19A H19C 109.5 . . ?
N3A C19A H19D 109.5 . . ?
H19C C19A H19D 109.5 . . ?
N3A C19A H19E 109.5 . . ?
H19C C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
O3B Np1B O4B 175.31(18) . . ?
O3B Np1B O2B 90.37(17) . . ?
O4B Np1B O2B 91.62(18) . . ?
O3B Np1B O1B 95.43(17) . . ?
O4B Np1B O1B 88.97(18) . . ?
O2B Np1B O1B 85.11(17) . . ?
O3B Np1B N2B 83.38(18) . . ?
O4B Np1B N2B 93.24(19) . . ?
O2B Np1B N2B 71.31(17) . . ?
O1B Np1B N2B 156.36(17) . . ?
O3B Np1B N3B 86.44(17) . . ?
O4B Np1B N3B 89.28(17) . . ?
O2B Np1B N3B 139.03(17) . . ?
O1B Np1B N3B 135.85(17) . . ?
N2B Np1B N3B 67.75(17) . . ?
O3B Np1B N1B 84.64(17) . . ?
O4B Np1B N1B 95.41(19) . . ?
O2B Np1B N1B 153.72(17) . . ?
O1B Np1B N1B 69.76(17) . . ?
N2B Np1B N1B 133.24(17) . . ?
N3B Np1B N1B 66.51(17) . . ?
C7B O1B Np1B 143.5(5) . . ?
C8B O2B Np1B 135.4(5) . . ?
C1B N1B C18B 114.5(6) . . ?
C1B N1B Np1B 130.1(5) . . ?
C18B N1B Np1B 115.0(4) . . ?
C14B N2B C15B 114.7(6) . . ?
C14B N2B Np1B 127.8(5) . . ?
C15B N2B Np1B 115.6(4) . . ?
C16B N3B C17B 107.7(5) . . ?
C16B N3B C19B 110.4(5) . . ?
C17B N3B C19B 110.5(5) . . ?
C16B N3B Np1B 107.6(4) . . ?
C17B N3B Np1B 107.4(4) . . ?
C19B N3B Np1B 113.0(4) . . ?
N1B C1B C2B 128.2(7) . . ?
N1B C1B H1BA 115.9 . . ?
C2B C1B H1BA 115.9 . . ?
C3B C2B C7B 119.4(8) . . ?
C3B C2B C1B 116.2(8) . . ?
C7B C2B C1B 124.3(7) . . ?
C4B C3B C2B 122.4(9) . . ?
C4B C3B H3BA 118.8 . . ?
C2B C3B H3BA 118.8 . . ?
C5B C4B C3B 118.0(10) . . ?
C5B C4B H4BA 121.0 . . ?
C3B C4B H4BA 121.0 . . ?
C6B C5B C4B 121.1(10) . . ?
C6B C5B H5BA 119.5 . . ?
C4B C5B H5BA 119.5 . . ?
C5B C6B C7B 122.1(10) . . ?
C5B C6B H6BA 119.0 . . ?
C7B C6B H6BA 119.0 . . ?
O1B C7B C2B 122.9(7) . . ?
O1B C7B C6B 120.2(8) . . ?
C2B C7B C6B 116.9(8) . . ?
O2B C8B C9B 120.8(8) . . ?
O2B C8B C13B 124.6(7) . . ?
C9B C8B C13B 114.5(8) . . ?
C10B C9B C8B 123.6(9) . . ?
C10B C9B H9BA 118.2 . . ?
C8B C9B H9BA 118.2 . . ?
C9B C10B C11B 121.0(8) . . ?
C9B C10B H10D 119.5 . . ?
C11B C10B H10D 119.5 . . ?
C12B C11B C10B 119.2(9) . . ?
C12B C11B H11D 120.4 . . ?
C10B C11B H11D 120.4 . . ?
C13B C12B C11B 120.4(8) . . ?
C13B C12B H12E 119.8 . . ?
C11B C12B H12E 119.8 . . ?
C12B C13B C8B 121.2(7) . . ?
C12B C13B C14B 116.4(7) . . ?
C8B C13B C14B 122.4(7) . . ?
N2B C14B C13B 127.7(7) . . ?
N2B C14B H14B 116.1 . . ?
C13B C14B H14B 116.1 . . ?
N2B C15B C16B 108.4(5) . . ?
N2B C15B H15C 110.0 . . ?
C16B C15B H15C 110.0 . . ?
N2B C15B H15D 110.0 . . ?
C16B C15B H15D 110.0 . . ?
H15C C15B H15D 108.4 . . ?
N3B C16B C15B 112.2(5) . . ?
N3B C16B H16F 109.2 . . ?
C15B C16B H16F 109.2 . . ?
N3B C16B H16G 109.2 . . ?
C15B C16B H16G 109.2 . . ?
H16F C16B H16G 107.9 . . ?
N3B C17B C18B 111.8(5) . . ?
N3B C17B H17E 109.3 . . ?
C18B C17B H17E 109.3 . . ?
N3B C17B H17F 109.3 . . ?
C18B C17B H17F 109.3 . . ?
H17E C17B H17F 107.9 . . ?
N1B C18B C17B 111.6(6) . . ?
N1B C18B H18E 109.3 . . ?
C17B C18B H18E 109.3 . . ?
N1B C18B H18F 109.3 . . ?
C17B C18B H18F 109.3 . . ?
H18E C18B H18F 108.0 . . ?
N3B C19B H19F 109.5 . . ?
N3B C19B H19G 109.5 . . ?
H19F C19B H19G 109.5 . . ?
N3B C19B H19H 109.5 . . ?
H19F C19B H19H 109.5 . . ?
H19G C19B H19H 109.5 . . ?
C1 N1 C13 110.9(5) . . ?
C1 N1 C5 110.3(5) . . ?
C13 N1 C5 107.9(5) . . ?
C1 N1 C9 106.9(5) . . ?
C13 N1 C9 110.4(5) . . ?
C5 N1 C9 110.5(5) . . ?
N1 C1 C2 115.8(6) . . ?
N1 C1 H1A 108.3 . . ?
C2 C1 H1A 108.3 . . ?
N1 C1 H1B 108.3 . . ?
C2 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
C1 C2 C3 110.4(6) . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 112.6(7) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 115.4(5) . . ?
C6 C5 H5A 108.4 . . ?
N1 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
N1 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C7 C6 C5 111.3(6) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 113.8(7) . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
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 . . ?
N1 C9 C10 115.7(6) . . ?
N1 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N1 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C11 C10 C9 110.4(6) . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 C12 110.8(7) . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N1 115.7(7) . . ?
C14 C13 H13A 108.3 . . ?
N1 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
N1 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C15 C14 C13 119.6(8) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 123.0(9) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
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 . . ?
C17 N2 C29 110.5(7) . . ?
C17 N2 C21 111.2(6) . . ?
C29 N2 C21 106.7(6) . . ?
C17 N2 C25 106.1(6) . . ?
C29 N2 C25 110.9(6) . . ?
C21 N2 C25 111.5(7) . . ?
N2 C17 C18 115.9(6) . . ?
N2 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
N2 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 C19 108.8(7) . . ?
C17 C18 H18A 109.9 . . ?
C19 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
C19 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
C18 C19 C20 111.7(8) . . ?
C18 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 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 . . ?
C22' C21 N2 114.4(7) . . ?
C22 C21 N2 114.4(7) . . ?
C22 C21 H21A 108.7 . . ?
N2 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
N2 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 C23 106.3(8) . . ?
C21 C22 H22C 110.5 . . ?
C23 C22 H22C 110.5 . . ?
C21 C22 H22D 110.5 . . ?
C23 C22 H22D 110.5 . . ?
H22C C22 H22D 108.7 . . ?
C24 C23 C22 109.7(12) . . ?
C24 C23 H23C 109.7 . . ?
C22 C23 H23C 109.7 . . ?
C24 C23 H23D 109.7 . . ?
C22 C23 H23D 109.7 . . ?
H23C C23 H23D 108.2 . . ?
C23 C24 H24D 109.5 . . ?
C23 C24 H24E 109.5 . . ?
H24D C24 H24E 109.5 . . ?
C23 C24 H24F 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C21 C22' C23' 116.8(11) . . ?
C21 C22' H22A 108.1 . . ?
C23' C22' H22A 108.1 . . ?
C21 C22' H22B 108.1 . . ?
C23' C22' H22B 108.1 . . ?
H22A C22' H22B 107.3 . . ?
C24' C23' C22' 110.9(15) . . ?
C24' C23' H23A 109.5 . . ?
C22' C23' H23A 109.5 . . ?
C24' C23' H23B 109.5 . . ?
C22' C23' H23B 109.5 . . ?
H23A C23' H23B 108.1 . . ?
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 116.2(7) . . ?
C26 C25 H25A 108.2 . . ?
N2 C25 H25A 108.2 . . ?
C26 C25 H25B 108.2 . . ?
N2 C25 H25B 108.2 . . ?
H25A C25 H25B 107.4 . . ?
C27 C26 C25 109.9(8) . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
C25 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C28 C27 C26 112.8(8) . . ?
C28 C27 H27A 109.0 . . ?
C26 C27 H27A 109.0 . . ?
C28 C27 H27B 109.0 . . ?
C26 C27 H27B 109.0 . . ?
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 114.9(7) . . ?
C30 C29 H29A 108.5 . . ?
N2 C29 H29A 108.5 . . ?
C30 C29 H29B 108.5 . . ?
N2 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 109.4(10) . . ?
C29 C30 H30A 109.8 . . ?
C31 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
C31 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
C32 C31 C30 112.6(11) . . ?
C32 C31 H31A 109.1 . . ?
C30 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
C30 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
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 108.9 . . ?
H2WA O2W H2WB 105.4 . . ?
H3WA O3W H3WB 102.7 . . ?
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 1.803(4) . ?
Np1A O4A 1.821(5) . ?
Np1A O1A 2.385(4) . ?
Np1A O2A 2.397(4) . ?
Np1A N1A 2.602(6) . ?
Np1A N2A 2.637(6) . ?
Np1A N3A 2.644(5) . ?
O1A C7A 1.306(7) . ?
O2A C8A 1.293(8) . ?
N1A C1A 1.266(8) . ?
N1A C18A 1.476(8) . ?
N2A C14A 1.275(8) . ?
N2A C15A 1.460(8) . ?
N3A C17A 1.461(9) . ?
N3A C16A 1.477(9) . ?
N3A C19A 1.518(9) . ?
C1A C2A 1.453(9) . ?
C1A H1AA 0.9500 . ?
C2A C3A 1.390(9) . ?
C2A C7A 1.424(9) . ?
C3A C4A 1.378(10) . ?
C3A H3AA 0.9500 . ?
C4A C5A 1.383(10) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.363(9) . ?
C5A H5AA 0.9500 . ?
C6A C7A 1.395(9) . ?
C6A H6AA 0.9500 . ?
C8A C9A 1.409(9) . ?
C8A C13A 1.451(9) . ?
C9A C10A 1.375(10) . ?
C9A H9AA 0.9500 . ?
C10A C11A 1.379(10) . ?
C10A H10C 0.9500 . ?
C11A C12A 1.362(10) . ?
C11A H11C 0.9500 . ?
C12A C13A 1.404(9) . ?
C12A H12D 0.9500 . ?
C13A C14A 1.442(9) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.466(10) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A H16D 0.9900 . ?
C16A H16E 0.9900 . ?
C17A C18A 1.577(10) . ?
C17A H17C 0.9900 . ?
C17A H17D 0.9900 . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
C19A H19C 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
Np1B O3B 1.811(4) . ?
Np1B O4B 1.836(4) . ?
Np1B O2B 2.351(5) . ?
Np1B O1B 2.391(5) . ?
Np1B N2B 2.592(6) . ?
Np1B N3B 2.628(5) . ?
Np1B N1B 2.643(6) . ?
O1B C7B 1.291(9) . ?
O2B C8B 1.267(9) . ?
N1B C1B 1.279(8) . ?
N1B C18B 1.466(8) . ?
N2B C14B 1.282(8) . ?
N2B C15B 1.460(8) . ?
N3B C16B 1.469(8) . ?
N3B C17B 1.476(8) . ?
N3B C19B 1.492(8) . ?
C1B C2B 1.447(10) . ?
C1B H1BA 0.9500 . ?
C2B C3B 1.403(10) . ?
C2B C7B 1.415(11) . ?
C3B C4B 1.393(12) . ?
C3B H3BA 0.9500 . ?
C4B C5B 1.391(14) . ?
C4B H4BA 0.9500 . ?
C5B C6B 1.369(13) . ?
C5B H5BA 0.9500 . ?
C6B C7B 1.429(9) . ?
C6B H6BA 0.9500 . ?
C8B C9B 1.430(10) . ?
C8B C13B 1.450(11) . ?
C9B C10B 1.339(11) . ?
C9B H9BA 0.9500 . ?
C10B C11B 1.397(12) . ?
C10B H10D 0.9500 . ?
C11B C12B 1.393(10) . ?
C11B H11D 0.9500 . ?
C12B C13B 1.391(10) . ?
C12B H12E 0.9500 . ?
C13B C14B 1.466(9) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.543(9) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C16B H16F 0.9900 . ?
C16B H16G 0.9900 . ?
C17B C18B 1.505(9) . ?
C17B H17E 0.9900 . ?
C17B H17F 0.9900 . ?
C18B H18E 0.9900 . ?
C18B H18F 0.9900 . ?
C19B H19F 0.9800 . ?
C19B H19G 0.9800 . ?
C19B H19H 0.9800 . ?
N1 C1 1.504(8) . ?
N1 C13 1.518(8) . ?
N1 C5 1.525(8) . ?
N1 C9 1.530(8) . ?
C1 C2 1.509(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.534(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.509(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.508(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.498(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.504(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.535(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.505(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.538(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.510(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.288(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.510(11) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N2 C17 1.513(10) . ?
N2 C29 1.511(9) . ?
N2 C21 1.520(9) . ?
N2 C25 1.532(10) . ?
C17 C18 1.524(11) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.527(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.534(12) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22' 1.509(10) . ?
C21 C22 1.509(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.594(14) . ?
C22 H22C 0.9900 . ?
C22 H22D 0.9900 . ?
C23 C24 1.443(15) . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C22' C23' 1.551(15) . ?
C22' H22A 0.9900 . ?
C22' H22B 0.9900 . ?
C23' C24' 1.532(19) . ?
C23' H23A 0.9900 . ?
C23' H23B 0.9900 . ?
C24' H24A 0.9800 . ?
C24' H24B 0.9800 . ?
C24' H24C 0.9800 . ?
C25 C26 1.525(11) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.509(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.492(14) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.495(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.512(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.464(14) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1W H1WA 0.9843 . ?
O1W H1WB 0.9734 . ?
O2W H2WA 0.9751 . ?
O2W H2WB 0.9649 . ?
O3W H3WA 0.9968 . ?
O3W H3WB 0.9905 . ?
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 -179.7(7) . . . . ?
Np1A N1A C1A C2A 14.0(11) . . . . ?
N1A C1A C2A C3A -174.3(7) . . . . ?
N1A C1A C2A C7A 11.0(12) . . . . ?
C7A C2A C3A C4A -0.7(11) . . . . ?
C1A C2A C3A C4A -175.7(7) . . . . ?
C2A C3A C4A C5A 1.8(12) . . . . ?
C3A C4A C5A C6A -1.8(12) . . . . ?
C4A C5A C6A C7A 0.6(12) . . . . ?
Np1A O1A C7A C6A 149.0(5) . . . . ?
Np1A O1A C7A C2A -32.5(10) . . . . ?
C5A C6A C7A O1A 179.0(7) . . . . ?
C5A C6A C7A C2A 0.5(10) . . . . ?
C3A C2A C7A O1A -179.0(6) . . . . ?
C1A C2A C7A O1A -4.3(10) . . . . ?
C3A C2A C7A C6A -0.5(10) . . . . ?
C1A C2A C7A C6A 174.2(6) . . . . ?
Np1A O2A C8A C9A -168.2(5) . . . . ?
Np1A O2A C8A C13A 12.2(11) . . . . ?
O2A C8A C9A C10A -177.6(7) . . . . ?
C13A C8A C9A C10A 1.9(10) . . . . ?
C8A C9A C10A C11A -0.8(12) . . . . ?
C9A C10A C11A C12A -0.5(12) . . . . ?
C10A C11A C12A C13A 0.6(12) . . . . ?
C11A C12A C13A C14A -179.9(7) . . . . ?
C11A C12A C13A C8A 0.5(11) . . . . ?
O2A C8A C13A C12A 177.8(6) . . . . ?
C9A C8A C13A C12A -1.7(10) . . . . ?
O2A C8A C13A C14A -1.8(11) . . . . ?
C9A C8A C13A C14A 178.7(6) . . . . ?
C15A N2A C14A C13A 179.9(7) . . . . ?
Np1A N2A C14A C13A -12.3(11) . . . . ?
C12A C13A C14A N2A -175.8(7) . . . . ?
C8A C13A C14A N2A 3.8(12) . . . . ?
C14A N2A C15A C16A 148.2(7) . . . . ?
Np1A N2A C15A C16A -21.4(8) . . . . ?
N2A C15A C16A N3A 53.2(9) . . . . ?
C17A N3A C16A C15A -171.4(7) . . . . ?
C19A N3A C16A C15A 66.8(8) . . . . ?
Np1A N3A C16A C15A -53.9(8) . . . . ?
C16A N3A C17A C18A 169.6(6) . . . . ?
C19A N3A C17A C18A -71.3(8) . . . . ?
Np1A N3A C17A C18A 54.0(7) . . . . ?
C1A N1A C18A C17A -128.9(7) . . . . ?
Np1A N1A C18A C17A 39.2(7) . . . . ?
N3A C17A C18A N1A -63.6(8) . . . . ?
C18B N1B C1B C2B 173.6(6) . . . . ?
Np1B N1B C1B C2B -14.0(10) . . . . ?
N1B C1B C2B C3B -173.4(7) . . . . ?
N1B C1B C2B C7B 4.6(11) . . . . ?
C7B C2B C3B C4B -3.9(11) . . . . ?
C1B C2B C3B C4B 174.2(7) . . . . ?
C2B C3B C4B C5B 1.4(12) . . . . ?
C3B C4B C5B C6B 2.1(14) . . . . ?
C4B C5B C6B C7B -2.9(13) . . . . ?
Np1B O1B C7B C2B -6.4(12) . . . . ?
Np1B O1B C7B C6B 174.5(5) . . . . ?
C3B C2B C7B O1B -176.1(6) . . . . ?
C1B C2B C7B O1B 5.9(11) . . . . ?
C3B C2B C7B C6B 3.0(10) . . . . ?
C1B C2B C7B C6B -175.0(6) . . . . ?
C5B C6B C7B O1B 179.4(7) . . . . ?
C5B C6B C7B C2B 0.3(11) . . . . ?
Np1B O2B C8B C9B 147.8(5) . . . . ?
Np1B O2B C8B C13B -35.5(11) . . . . ?
O2B C8B C9B C10B 175.9(8) . . . . ?
C13B C8B C9B C10B -1.1(11) . . . . ?
C8B C9B C10B C11B 1.1(14) . . . . ?
C9B C10B C11B C12B -0.4(14) . . . . ?
C10B C11B C12B C13B -0.2(12) . . . . ?
C11B C12B C13B C8B 0.1(11) . . . . ?
C11B C12B C13B C14B -179.4(7) . . . . ?
O2B C8B C13B C12B -176.4(7) . . . . ?
C9B C8B C13B C12B 0.5(10) . . . . ?
O2B C8B C13B C14B 3.1(11) . . . . ?
C9B C8B C13B C14B -180.0(6) . . . . ?
C15B N2B C14B C13B 177.5(6) . . . . ?
Np1B N2B C14B C13B 13.7(10) . . . . ?
C12B C13B C14B N2B -175.5(7) . . . . ?
C8B C13B C14B N2B 5.0(11) . . . . ?
C14B N2B C15B C16B -131.0(6) . . . . ?
Np1B N2B C15B C16B 34.8(6) . . . . ?
C17B N3B C16B C15B 168.6(5) . . . . ?
C19B N3B C16B C15B -70.7(7) . . . . ?
Np1B N3B C16B C15B 53.1(6) . . . . ?
N2B C15B C16B N3B -60.5(7) . . . . ?
C16B N3B C17B C18B -173.0(6) . . . . ?
C19B N3B C17B C18B 66.4(7) . . . . ?
Np1B N3B C17B C18B -57.3(6) . . . . ?
C1B N1B C18B C17B 150.2(6) . . . . ?
Np1B N1B C18B C17B -23.5(7) . . . . ?
N3B C17B C18B N1B 55.6(8) . . . . ?
C13 N1 C1 C2 -58.8(7) . . . . ?
C5 N1 C1 C2 60.7(7) . . . . ?
C9 N1 C1 C2 -179.2(5) . . . . ?
N1 C1 C2 C3 168.9(5) . . . . ?
C1 C2 C3 C4 -178.3(6) . . . . ?
C1 N1 C5 C6 61.0(8) . . . . ?
C13 N1 C5 C6 -177.7(6) . . . . ?
C9 N1 C5 C6 -57.0(7) . . . . ?
N1 C5 C6 C7 -173.7(6) . . . . ?
C5 C6 C7 C8 -179.8(7) . . . . ?
C1 N1 C9 C10 175.7(5) . . . . ?
C13 N1 C9 C10 54.9(7) . . . . ?
C5 N1 C9 C10 -64.3(7) . . . . ?
N1 C9 C10 C11 173.7(6) . . . . ?
C9 C10 C11 C12 179.3(6) . . . . ?
C1 N1 C13 C14 -57.2(9) . . . . ?
C5 N1 C13 C14 -178.1(7) . . . . ?
C9 N1 C13 C14 61.1(9) . . . . ?
N1 C13 C14 C15 158.9(11) . . . . ?
C13 C14 C15 C16 179.2(10) . . . . ?
C29 N2 C17 C18 65.4(9) . . . . ?
C21 N2 C17 C18 -52.9(9) . . . . ?
C25 N2 C17 C18 -174.3(7) . . . . ?
N2 C17 C18 C19 -163.4(7) . . . . ?
C17 C18 C19 C20 -168.2(8) . . . . ?
C17 N2 C21 C22' -52.6(11) . . . . ?
C29 N2 C21 C22' -173.1(9) . . . . ?
C25 N2 C21 C22' 65.7(10) . . . . ?
C17 N2 C21 C22 -52.6(11) . . . . ?
C29 N2 C21 C22 -173.1(9) . . . . ?
C25 N2 C21 C22 65.7(10) . . . . ?
N2 C21 C22 C23 165.3(10) . . . . ?
C21 C22 C23 C24 175.3(14) . . . . ?
N2 C21 C22' C23' -158.0(13) . . . . ?
C21 C22' C23' C24' 79(2) . . . . ?
C17 N2 C25 C26 -172.8(7) . . . . ?
C29 N2 C25 C26 -52.8(10) . . . . ?
C21 N2 C25 C26 66.0(9) . . . . ?
N2 C25 C26 C27 -177.4(8) . . . . ?
C25 C26 C27 C28 -162.6(11) . . . . ?
C17 N2 C29 C30 62.5(10) . . . . ?
C21 N2 C29 C30 -176.5(8) . . . . ?
C25 N2 C29 C30 -54.9(10) . . . . ?
N2 C29 C30 C31 174.6(8) . . . . ?
C29 C30 C31 C32 -179.8(10) . . . . ?
