#------------------------------------------------------------------------------
#$Date: 2021-11-30 02:03:46 +0200 (Tue, 30 Nov 2021) $
#$Revision: 270922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/89/7708955.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_7708955
loop_
_publ_author_name
'Jurowska, Anna'
'Hodorowicz, Maciej'
'Kruczała, Krzysztof'
'Szklarzewicz, Janusz'
_publ_section_title
;
 Anion--cation interactions in a series of salts with substituted Hphen,
 Hbpy and H2bpy cations and [W(CN)8]4− anion: polymer with
 “super-short” N--H⋯N hydrogen bridges containing
 exclusively anions and H+
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03224K
_journal_year                    2021
_chemical_formula_sum            'C44 H44 N14 O2 W'
_chemical_formula_weight         984.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.32210(10)
_cell_length_b                   10.98930(10)
_cell_length_c                   22.60420(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4302.87(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            128751
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.064
_diffrn_reflns_theta_min         3.210
_exptl_absorpt_coefficient_mu    5.421
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.832
_refine_diff_density_min         -2.456
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0435P)²+6.1641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8960
_reflns_number_total             9045
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03224k2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7708955
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.074
_shelx_estimated_absorpt_t_max   0.613
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
W1 W 0.24327(2) 0.36915(2) 0.42220(2) 0.00733(5) Uani 1 1 d . . . . .
N9 N 0.26274(12) 0.1832(2) 0.62959(9) 0.0173(4) Uani 1 1 d . . . . .
H9N H 0.288479 0.148661 0.600580 0.021 Uiso 1 1 calc R U . . .
N18 N 0.42553(12) 0.4002(2) 0.38059(9) 0.0149(4) Uani 1 1 d . . . . .
N25 N 0.08173(11) 0.01958(19) 0.54273(9) 0.0134(4) Uani 1 1 d . . . . .
H25N H 0.083390 0.095834 0.554548 0.016 Uiso 1 1 calc R U . . .
N31 N 0.01534(13) 0.1059(2) 0.63774(10) 0.0159(4) Uani 1 1 d . . . . .
N34 N 0.40375(12) 0.9656(2) 0.52155(10) 0.0166(4) Uani 1 1 d . . . . .
N45 N 0.44911(13) 1.0652(2) 0.62201(10) 0.0182(4) Uani 1 1 d . . . . .
N48 N 0.12510(12) 0.2802(2) 0.52967(9) 0.0187(4) Uani 1 1 d . . . . .
N50 N 0.06359(13) 0.4011(2) 0.37347(10) 0.0183(4) Uani 1 1 d . . . . .
N52 N 0.22436(13) 0.0807(2) 0.38172(9) 0.0157(4) Uani 1 1 d . . . . .
N54 N 0.25176(13) 0.36064(18) 0.27590(10) 0.0153(4) Uani 1 1 d . . . . .
N56 N 0.23159(13) 0.6587(2) 0.38273(10) 0.0166(4) Uani 1 1 d . . . . .
N15 N 0.25910(12) -0.0520(2) 0.60307(10) 0.0187(4) Uani 1 1 d . . . . .
N58 N 0.33893(13) 0.1925(2) 0.51572(9) 0.0192(4) Uani 1 1 d . . . . .
C57 C 0.23439(13) 0.5583(2) 0.39684(10) 0.0116(4) Uani 1 1 d . . . . .
C61 C 0.28197(14) 0.4822(2) 0.49558(10) 0.0132(5) Uani 1 1 d . . . . .
N60 N 0.30628(14) 0.5372(2) 0.53487(10) 0.0226(5) Uani 1 1 d . . . . .
C53 C 0.22841(13) 0.1824(2) 0.39492(10) 0.0110(4) Uani 1 1 d . . . . .
C19 C 0.36227(14) 0.3919(2) 0.39620(11) 0.0110(4) Uani 1 1 d . . . . .
C51 C 0.12579(14) 0.3902(2) 0.39113(11) 0.0119(4) Uani 1 1 d . . . . .
C28 C -0.07329(14) -0.0354(2) 0.71618(11) 0.0161(5) Uani 1 1 d . . . . .
C49 C 0.16459(13) 0.3173(2) 0.49277(10) 0.0134(5) Uani 1 1 d . . . . .
C27 C -0.04066(14) -0.0865(2) 0.66563(11) 0.0142(5) Uani 1 1 d . . . . .
H27 H -0.048219 -0.170167 0.656664 0.017 Uiso 1 1 calc R U . . .
C55 C 0.24947(14) 0.36472(19) 0.32646(10) 0.0097(5) Uani 1 1 d . . . . .
C35 C 0.45553(14) 0.9013(2) 0.55331(11) 0.0149(5) Uani 1 1 d . . . . .
C20 C 0.04082(13) -0.0616(2) 0.57505(11) 0.0141(5) Uani 1 1 d . . . . .
C59 C 0.30806(13) 0.2538(2) 0.48159(10) 0.0130(5) Uani 1 1 d . . . . .
C43 C 0.52948(16) 1.0746(2) 0.70870(12) 0.0202(5) Uani 1 1 d . . . . .
H43 H 0.544368 1.118275 0.743159 0.024 Uiso 1 1 calc R U . . .
C40 C 0.48216(14) 0.9572(2) 0.60950(11) 0.0149(5) Uani 1 1 d . . . . .
C26 C 0.00308(13) -0.0131(2) 0.62861(10) 0.0131(5) Uani 1 1 d . . . . .
C21 C 0.03811(14) -0.1814(2) 0.55594(11) 0.0144(5) Uani 1 1 d . . . . .
H21 H 0.009344 -0.239398 0.577907 0.017 Uiso 1 1 calc R U . . .
C42 C 0.56316(14) 0.9625(2) 0.69593(11) 0.0156(5) Uani 1 1 d . . . . .
C39 C 0.37488(14) 0.9272(3) 0.46978(11) 0.0190(5) Uani 1 1 d . . . . .
H39 H 0.337481 0.974993 0.449570 0.023 Uiso 1 1 calc R U . . .
C41 C 0.53865(14) 0.9037(2) 0.64447(11) 0.0150(5) Uani 1 1 d . . . . .
H41 H 0.560443 0.827634 0.633511 0.018 Uiso 1 1 calc R U . . .
C10 C 0.21705(14) -0.0191(2) 0.65056(11) 0.0173(5) Uani 1 1 d . . . . .
C5 C 0.17940(14) 0.1670(3) 0.71104(11) 0.0181(5) Uani 1 1 d . . . . .
H5 H 0.149600 0.118559 0.737247 0.022 Uiso 1 1 calc R U . . .
C36 C 0.48167(14) 0.7923(2) 0.53030(11) 0.0163(5) Uani 1 1 d . . . . .
H36 H 0.517992 0.745185 0.551998 0.020 Uiso 1 1 calc R U . . .
C6 C 0.18283(14) 0.2927(3) 0.71927(11) 0.0185(5) Uani 1 1 d . . . . .
C11 C 0.17417(15) -0.1007(3) 0.68401(12) 0.0196(5) Uani 1 1 d . . . . .
H11 H 0.145542 -0.073004 0.717164 0.023 Uiso 1 1 calc R U . . .
C37 C 0.45532(15) 0.7508(2) 0.47574(12) 0.0183(5) Uani 1 1 d . . . . .
C23 C 0.11805(16) -0.1302(2) 0.47349(12) 0.0179(6) Uani 1 1 d . . . . .
H23 H 0.144754 -0.152146 0.438420 0.022 Uiso 1 1 calc R U . . .
C29 C -0.06039(15) 0.0880(2) 0.72640(11) 0.0185(5) Uani 1 1 d . . . . .
H29 H -0.081010 0.126249 0.760573 0.022 Uiso 1 1 calc R U . . .
C4 C 0.21909(15) 0.1120(2) 0.66492(11) 0.0165(5) Uani 1 1 d . . . . .
C46 C 0.62310(15) 0.9076(3) 0.73569(12) 0.0196(5) Uani 1 1 d . . . . .
H46A H 0.668167 0.961387 0.737549 0.029 Uiso 1 1 calc R U . . .
H46B H 0.638649 0.828133 0.720055 0.029 Uiso 1 1 calc R U . . .
H46C H 0.601699 0.897333 0.775464 0.029 Uiso 1 1 calc R U . . .
C8 C 0.26871(15) 0.3040(3) 0.63661(12) 0.0203(5) Uani 1 1 d . . . . .
H8 H 0.299931 0.350254 0.610443 0.024 Uiso 1 1 calc R U . . .
C44 C 0.47407(18) 1.1219(2) 0.67074(13) 0.0211(6) Uani 1 1 d . . . . .
H44 H 0.452609 1.199192 0.679909 0.025 Uiso 1 1 calc R U . . .
C22 C 0.07697(14) -0.2183(2) 0.50489(11) 0.0165(5) Uani 1 1 d . . . . .
C13 C 0.21756(16) -0.2582(3) 0.62023(13) 0.0222(5) Uani 1 1 d . . . . .
H13 H 0.219681 -0.341184 0.608555 0.027 Uiso 1 1 calc R U . . .
C7 C 0.22980(18) 0.3607(2) 0.68151(14) 0.0210(6) Uani 1 1 d . . . . .
H7 H 0.234740 0.446057 0.686973 0.025 Uiso 1 1 calc R U . . .
C38 C 0.39918(15) 0.8191(3) 0.44586(12) 0.0195(5) Uani 1 1 d . . . . .
H38 H 0.378173 0.790849 0.409499 0.023 Uiso 1 1 calc R U . . .
C12 C 0.17347(15) -0.2237(3) 0.66854(12) 0.0203(5) Uani 1 1 d . . . . .
C24 C 0.11998(14) -0.0118(2) 0.49316(11) 0.0170(5) Uani 1 1 d . . . . .
H24 H 0.148258 0.047779 0.471841 0.020 Uiso 1 1 calc R U . . .
C30 C -0.01686(16) 0.1549(3) 0.68593(12) 0.0188(5) Uani 1 1 d . . . . .
H30 H -0.009750 0.239350 0.692956 0.023 Uiso 1 1 calc R U . . .
C32 C -0.12153(18) -0.1108(3) 0.75787(13) 0.0233(6) Uani 1 1 d . . . . .
H32A H -0.175131 -0.082418 0.756645 0.035 Uiso 1 1 calc R U . . .
H32B H -0.101299 -0.102664 0.798206 0.035 Uiso 1 1 calc R U . . .
H32C H -0.119472 -0.196454 0.745829 0.035 Uiso 1 1 calc R U . . .
C16 C 0.12633(16) -0.3129(3) 0.70295(13) 0.0261(6) Uani 1 1 d . . . . .
H16A H 0.150602 -0.326997 0.741562 0.039 Uiso 1 1 calc R U . . .
H16B H 0.123268 -0.389869 0.681178 0.039 Uiso 1 1 calc R U . . .
H16C H 0.074224 -0.280290 0.708675 0.039 Uiso 1 1 calc R U . . .
C33 C 0.07443(17) -0.3481(3) 0.48569(13) 0.0228(6) Uani 1 1 d . . . . .
H33A H 0.119632 -0.391138 0.501360 0.034 Uiso 1 1 calc R U . . .
H33B H 0.074696 -0.352133 0.442384 0.034 Uiso 1 1 calc R U . . .
H33C H 0.027295 -0.386384 0.500727 0.034 Uiso 1 1 calc R U . . .
C47 C 0.4873(2) 0.6368(2) 0.44954(14) 0.0283(7) Uani 1 1 d . . . . .
H47A H 0.539163 0.622135 0.465378 0.042 Uiso 1 1 calc R U . . .
H47B H 0.489914 0.645199 0.406433 0.042 Uiso 1 1 calc R U . . .
H47C H 0.453681 0.568101 0.459615 0.042 Uiso 1 1 calc R U . . .
C17 C 0.13474(17) 0.3509(3) 0.76607(13) 0.0233(6) Uani 1 1 d . . . . .
H17A H 0.084649 0.374218 0.749313 0.035 Uiso 1 1 calc R U . . .
H17B H 0.161168 0.423465 0.781108 0.035 Uiso 1 1 calc R U . . .
H17C H 0.126823 0.293160 0.798544 0.035 Uiso 1 1 calc R U . . .
C14 C 0.25870(15) -0.1705(3) 0.58894(13) 0.0214(5) Uani 1 1 d . . . . .
H14 H 0.288083 -0.196072 0.555759 0.026 Uiso 1 1 calc R U . . .
O1 O 0.23961(12) 0.36532(16) 0.16281(9) 0.0166(4) Uani 1 1 d . . . . .
O2 O 0.06225(13) 0.4217(2) 0.63762(10) 0.0292(5) Uani 1 1 d . . . . .
H2B H 0.027(2) 0.476(4) 0.6308(16) 0.032(10) Uiso 1 1 d . . . . .
H2A H 0.075(3) 0.386(4) 0.609(2) 0.061(16) Uiso 1 1 d . . . . .
H34N H 0.3917(18) 1.032(3) 0.5346(14) 0.014(7) Uiso 1 1 d . . . . .
H1A H 0.253(3) 0.364(4) 0.202(3) 0.064(16) Uiso 1 1 d . . . . .
H1B H 0.257(3) 0.432(6) 0.148(3) 0.085(19) Uiso 1 1 d . . . . .
H1C H 0.254(2) 0.290(3) 0.1446(15) 0.025(9) 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C53 W1 C59 71.38(9) . . ?
C53 W1 C19 98.38(9) . . ?
C59 W1 C19 75.07(9) . . ?
C53 W1 C57 146.13(9) . . ?
C59 W1 C57 140.00(9) . . ?
C19 W1 C57 83.31(9) . . ?
C53 W1 C51 84.11(9) . . ?
C59 W1 C51 138.73(9) . . ?
C19 W1 C51 142.84(9) . . ?
C57 W1 C51 75.22(9) . . ?
C53 W1 C55 72.51(8) . . ?
C59 W1 C55 125.49(9) . . ?
C19 W1 C55 71.39(9) . . ?
C57 W1 C55 76.14(8) . . ?
C51 W1 C55 74.18(9) . . ?
C53 W1 C61 142.83(9) . . ?
C59 W1 C61 72.71(9) . . ?
C19 W1 C61 81.32(9) . . ?
C57 W1 C61 71.02(9) . . ?
C51 W1 C61 118.28(9) . . ?
C55 W1 C61 139.25(9) . . ?
C53 W1 C49 83.44(9) . . ?
C59 W1 C49 73.50(9) . . ?
C19 W1 C49 146.08(9) . . ?
C57 W1 C49 113.70(9) . . ?
C51 W1 C49 71.07(9) . . ?
C55 W1 C49 139.33(9) . . ?
C61 W1 C49 77.49(9) . . ?
C8 N9 C4 123.1(2) . . ?
C8 N9 H9N 118.4 . . ?
C4 N9 H9N 118.4 . . ?
C24 N25 C20 122.6(2) . . ?
C24 N25 H25N 118.7 . . ?
C20 N25 H25N 118.7 . . ?
C30 N31 C26 116.8(2) . . ?
C39 N34 C35 123.2(2) . . ?
C39 N34 H34N 120(2) . . ?
C35 N34 H34N 117(2) . . ?
C44 N45 C40 116.6(2) . . ?
C14 N15 C10 116.6(2) . . ?
N56 C57 W1 178.2(2) . . ?
N60 C61 W1 175.7(2) . . ?
N52 C53 W1 176.2(2) . . ?
N18 C19 W1 177.1(2) . . ?
N50 C51 W1 178.7(2) . . ?
C29 C28 C27 117.6(2) . . ?
C29 C28 C32 121.3(2) . . ?
C27 C28 C32 121.1(2) . . ?
N48 C49 W1 174.4(2) . . ?
C26 C27 C28 118.8(2) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
N54 C55 W1 178.7(2) . . ?
N34 C35 C36 118.2(2) . . ?
N34 C35 C40 116.4(2) . . ?
C36 C35 C40 125.4(2) . . ?
N25 C20 C21 118.3(2) . . ?
N25 C20 C26 115.9(2) . . ?
C21 C20 C26 125.7(2) . . ?
N58 C59 W1 175.8(2) . . ?
C44 C43 C42 119.5(2) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
N45 C40 C41 123.6(2) . . ?
N45 C40 C35 114.4(2) . . ?
C41 C40 C35 122.0(2) . . ?
N31 C26 C27 124.1(2) . . ?
N31 C26 C20 114.1(2) . . ?
C27 C26 C20 121.8(2) . . ?
C20 C21 C22 121.1(2) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C43 C42 C41 117.1(2) . . ?
C43 C42 C46 121.4(2) . . ?
C41 C42 C46 121.5(2) . . ?
N34 C39 C38 120.2(2) . . ?
N34 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C40 C41 C42 119.4(2) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
N15 C10 C11 123.4(3) . . ?
N15 C10 C4 115.1(2) . . ?
C11 C10 C4 121.5(2) . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C35 C36 C37 120.7(2) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C5 C6 C7 118.2(2) . . ?
C5 C6 C17 119.7(2) . . ?
C7 C6 C17 122.1(3) . . ?
C10 C11 C12 119.5(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C36 C37 C38 118.6(2) . . ?
C36 C37 C47 120.4(2) . . ?
C38 C37 C47 121.1(3) . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C28 C29 C30 119.3(2) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
N9 C4 C5 118.1(2) . . ?
N9 C4 C10 116.6(2) . . ?
C5 C4 C10 125.3(2) . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N9 C8 C7 120.0(2) . . ?
N9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
N45 C44 C43 123.8(2) . . ?
N45 C44 H44 118.1 . . ?
C43 C44 H44 118.1 . . ?
C23 C22 C21 117.8(2) . . ?
C23 C22 C33 122.0(2) . . ?
C21 C22 C33 120.2(2) . . ?
C12 C13 C14 119.6(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C8 C7 C6 119.9(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C39 C38 C37 119.1(2) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C13 C12 C11 117.2(2) . . ?
C13 C12 C16 122.2(3) . . ?
C11 C12 C16 120.6(3) . . ?
N25 C24 C23 120.0(2) . . ?
N25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
N31 C30 C29 123.3(3) . . ?
N31 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C33 H33A 109.5 . . ?
C22 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C22 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C37 C47 H47A 109.5 . . ?
C37 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C37 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C6 C17 H17A 109.5 . . ?
C6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N15 C14 C13 123.6(3) . . ?
N15 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
H1A O1 H1B 108(5) . . ?
H1A O1 H1C 109(3) . . ?
H1B O1 H1C 119(5) . . ?
H2B O2 H2A 113(4) . . ?
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
W1 C53 2.158(2) . ?
W1 C59 2.159(2) . ?
W1 C19 2.160(2) . ?
W1 C57 2.162(2) . ?
W1 C51 2.163(2) . ?
W1 C55 2.168(2) . ?
W1 C61 2.177(2) . ?
W1 C49 2.177(2) . ?
N9 C8 1.341(4) . ?
N9 C4 1.351(3) . ?
N9 H9N 0.8800 . ?
N18 C19 1.156(3) . ?
N25 C24 1.348(3) . ?
N25 C20 1.355(3) . ?
N25 H25N 0.8800 . ?
N31 C30 1.338(3) . ?
N31 C26 1.341(3) . ?
N34 C39 1.339(4) . ?
N34 C35 1.347(3) . ?
N34 H34N 0.82(3) . ?
N45 C44 1.337(4) . ?
N45 C40 1.347(3) . ?
N48 C49 1.154(3) . ?
N50 C51 1.154(3) . ?
N52 C53 1.158(4) . ?
N54 C55 1.145(3) . ?
N56 C57 1.149(3) . ?
N15 C14 1.341(4) . ?
N15 C10 1.348(3) . ?
N58 C59 1.155(3) . ?
C61 N60 1.153(3) . ?
C28 C29 1.393(4) . ?
C28 C27 1.394(3) . ?
C28 C32 1.509(4) . ?
C27 C26 1.389(3) . ?
C27 H27 0.9500 . ?
C35 C36 1.383(4) . ?
C35 C40 1.483(4) . ?
C20 C21 1.386(4) . ?
C20 C26 1.477(3) . ?
C43 C44 1.387(4) . ?
C43 C42 1.393(4) . ?
C43 H43 0.9500 . ?
C40 C41 1.387(4) . ?
C21 C22 1.397(3) . ?
C21 H21 0.9500 . ?
C42 C41 1.396(4) . ?
C42 C46 1.498(4) . ?
C39 C38 1.372(4) . ?
C39 H39 0.9500 . ?
C41 H41 0.9500 . ?
C10 C11 1.389(4) . ?
C10 C4 1.477(4) . ?
C5 C4 1.389(4) . ?
C5 C6 1.395(4) . ?
C5 H5 0.9500 . ?
C36 C37 1.390(4) . ?
C36 H36 0.9500 . ?
C6 C7 1.397(4) . ?
C6 C17 1.492(4) . ?
C11 C12 1.396(4) . ?
C11 H11 0.9500 . ?
C37 C38 1.400(4) . ?
C37 C47 1.493(4) . ?
C23 C24 1.375(4) . ?
C23 C22 1.396(4) . ?
C23 H23 0.9500 . ?
C29 C30 1.396(4) . ?
C29 H29 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C8 C7 1.370(4) . ?
C8 H8 0.9500 . ?
C44 H44 0.9500 . ?
C22 C33 1.492(4) . ?
C13 C12 1.387(4) . ?
C13 C14 1.393(4) . ?
C13 H13 0.9500 . ?
C7 H7 0.9500 . ?
C38 H38 0.9500 . ?
C12 C16 1.495(4) . ?
C24 H24 0.9500 . ?
C30 H30 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14 0.9500 . ?
O1 H1A 0.92(6) . ?
O1 H1B 0.86(6) . ?
O1 H1C 0.96(4) . ?
O2 H2B 0.87(4) . ?
O2 H2A 0.78(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N9 H9N N58 0.88 2.16 2.898(3) 140.5 . yes
N25 H25N N48 0.88 2.22 2.976(3) 143.2 . yes
C27 H27 N50 0.95 2.64 3.590(3) 176.7 3_556 yes
C21 H21 N50 0.95 2.44 3.391(3) 174.7 3_556 yes
C41 H41 N18 0.95 2.54 3.444(3) 160.0 3_666 yes
C36 H36 N18 0.95 2.41 3.331(3) 162.4 3_666 yes
C8 H8 N60 0.95 2.67 3.505(4) 146.4 . yes
C13 H13 N60 0.95 2.61 3.340(4) 133.7 1_545 yes
C24 H24 N52 0.95 2.46 3.267(3) 143.2 . yes
O2 H2B N50 0.87(4) 2.07(4) 2.933(3) 172(3) 3_566 yes
O2 H2A N48 0.78(6) 2.32(6) 3.094(3) 174(5) . yes
N34 H34N N58 0.82(3) 2.03(3) 2.738(3) 145(3) 1_565 yes
O1 H1A N54 0.92(6) 1.66(6) 2.565(3) 165(5) . yes
O1 H1B N52 0.86(6) 1.80(6) 2.648(3) 170(6) 2 yes
O1 H1C N56 0.96(4) 1.58(4) 2.543(3) 173(3) 2_545 yes
