#------------------------------------------------------------------------------
#$Date: 2022-03-10 10:16:59 +0200 (Thu, 10 Mar 2022) $
#$Revision: 273584 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/47/8104707.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_8104707
loop_
_publ_author_name
'Shi, Qing'
'Zhang, Qi-Long'
'Xu, Hong'
'Huang, Ya-Li'
_publ_section_title
;
 Crystal structure of
 3,3′,3″-((1E,1′E,1″E)-((nitrilotris(ethane-2,1-diyl))tris(azaneylylidene))
 tris(methaneylylidene))tris(4-hydroxy-1-naphthaldehyde) monohydrate,
 C42H36N4O6·H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              773
_journal_page_last               775
_journal_paper_doi               10.1515/ncrs-2021-0120
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C42 H36 N4 O6, H2 O'
_chemical_formula_sum            'C42 H38 N4 O7'
_chemical_formula_weight         710.76
_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
_cell_angle_alpha                113.563(2)
_cell_angle_beta                 96.740(2)
_cell_angle_gamma                104.429(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8563(6)
_cell_length_b                   12.6263(6)
_cell_length_c                   13.4492(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      34.54
_cell_measurement_theta_min      2.49
_cell_volume                     1733.07(15)
_computing_cell_refinement       'SAINT (Brucker, 2012)[2]'
_computing_data_collection       'APEX2 (Brucker, 2012)[2]'
_computing_data_reduction        'SAINT (Brucker, 2012)[2]'
_computing_molecular_graphics    'Diamond 4.0[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[1]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_diffrn_ambient_temperature      301.72
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47868
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.489
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0470
_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)+(0.0633P)²+0.3643P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5360
_reflns_number_total             6780
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0120_suppl.cif
_cod_data_source_block           a
_cod_database_code               8104707
_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_max   0.981
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C35A-O3
 1.22 with sigma of 0.02
 C35-O3A
 1.22 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O1X) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C35A) = Uanis(C35)
Uanis(O1X) = Uanis(O1W)
4. Others
 Sof(C35A)=Sof(H35A)=Sof(O3A)=1-FVAR(1)
 Sof(O3)=Sof(C35)=Sof(H35)=FVAR(1)
 Sof(O1X)=Sof(H1XA)=Sof(H1XB)=1-FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(2)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O1X(H1XA,H1XB)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C26(H26A,H26B),
 C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C1(H1A), C2(H2), C5(H5), C7(H7), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C25(H25), C29(H29), C30(H30),
  C32(H32), C33(H33), C37(H37), C40(H40), C41(H41), C42(H42), C35A(H35A),
 C35(H35)
;
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
O1 O 0.67282(11) 0.17824(11) -0.05327(10) 0.0549(3) Uani 1 1 d . . . . .
O2 O 0.6140(2) -0.15380(18) 0.20935(17) 0.1136(7) Uani 1 1 d . . . . .
O4 O 0.56490(10) 0.41825(11) 0.38665(9) 0.0540(3) Uani 1 1 d . . . . .
O5 O 0.85768(14) 0.40747(13) 0.36701(11) 0.0694(4) Uani 1 1 d . . . . .
O6 O 1.01414(17) -0.07558(14) 0.23454(16) 0.0928(5) Uani 1 1 d . . . . .
N1 N 0.59053(11) 0.34105(11) 0.08463(11) 0.0437(3) Uani 1 1 d . . . . .
H1 H 0.6117 0.3148 0.0225 0.052 Uiso 1 1 calc R . . . .
N2 N 0.76003(11) 0.59836(11) 0.22108(10) 0.0415(3) Uani 1 1 d . . . . .
N3 N 0.74550(12) 0.61887(12) 0.45091(11) 0.0451(3) Uani 1 1 d . . . . .
H3 H 0.6848 0.5629 0.3989 0.054 Uiso 1 1 calc R . . . .
N4 N 0.90252(13) 0.43894(13) 0.19194(12) 0.0516(3) Uani 1 1 d . . . . .
H4 H 0.8802 0.4655 0.2534 0.062 Uiso 1 1 calc R . . . .
C1 C 0.73993(17) -0.20695(16) -0.08058(17) 0.0616(5) Uani 1 1 d . . . . .
H1A H 0.7592 -0.2785 -0.1001 0.074 Uiso 1 1 calc R . . . .
C2 C 0.70537(15) -0.15823(15) 0.01654(16) 0.0526(4) Uani 1 1 d . . . . .
H2 H 0.7016 -0.1971 0.0626 0.063 Uiso 1 1 calc R . . . .
C3 C 0.67525(13) -0.04999(13) 0.04830(13) 0.0402(3) Uani 1 1 d . . . . .
C4 C 0.63472(14) 0.00249(15) 0.14884(13) 0.0446(4) Uani 1 1 d . . . . .
C5 C 0.61104(14) 0.10929(14) 0.17492(13) 0.0431(3) Uani 1 1 d . . . . .
H5 H 0.5863 0.1427 0.2404 0.052 Uiso 1 1 calc R . . . .
C6 C 0.62166(12) 0.17220(13) 0.10878(12) 0.0375(3) Uani 1 1 d . . . . .
C7 C 0.59061(13) 0.27939(13) 0.14202(12) 0.0406(3) Uani 1 1 d . . . . .
H7 H 0.5686 0.3081 0.2096 0.049 Uiso 1 1 calc R . . . .
C8 C 0.55727(15) 0.45134(15) 0.11765(15) 0.0504(4) Uani 1 1 d . . . . .
H8A H 0.5375 0.4724 0.1896 0.060 Uiso 1 1 calc R . . . .
H8B H 0.4867 0.4367 0.0633 0.060 Uiso 1 1 calc R . . . .
C9 C 0.65926(15) 0.55664(14) 0.12552(14) 0.0498(4) Uani 1 1 d . . . . .
H9A H 0.6868 0.5310 0.0572 0.060 Uiso 1 1 calc R . . . .
H9B H 0.6301 0.6240 0.1326 0.060 Uiso 1 1 calc R . . . .
C10 C 0.75461(17) 0.70437(14) 0.31734(14) 0.0506(4) Uani 1 1 d . . . . .
H10A H 0.6712 0.6981 0.3161 0.061 Uiso 1 1 calc R . . . .
H10B H 0.7928 0.7781 0.3110 0.061 Uiso 1 1 calc R . . . .
C11 C 0.81524(17) 0.71464(15) 0.42733(14) 0.0531(4) Uani 1 1 d . . . . .
H11A H 0.8948 0.7082 0.4247 0.064 Uiso 1 1 calc R . . . .
H11B H 0.8241 0.7939 0.4869 0.064 Uiso 1 1 calc R . . . .
C12 C 0.76748(14) 0.61120(14) 0.54377(13) 0.0440(4) Uani 1 1 d . . . . .
H12 H 0.8319 0.6725 0.6009 0.053 Uiso 1 1 calc R . . . .
C13 C 0.70084(14) 0.51669(14) 0.56429(12) 0.0411(3) Uani 1 1 d . . . . .
C14 C 0.60062(13) 0.41909(14) 0.47886(12) 0.0419(3) Uani 1 1 d . . . . .
C15 C 0.54290(14) 0.31796(14) 0.50257(13) 0.0445(4) Uani 1 1 d . . . . .
C16 C 0.45017(16) 0.21765(17) 0.41887(15) 0.0571(4) Uani 1 1 d . . . . .
H16 H 0.4248 0.2179 0.3509 0.069 Uiso 1 1 calc R . . . .
C17 C 0.39626(19) 0.11893(19) 0.43580(18) 0.0708(6) Uani 1 1 d . . . . .
H17 H 0.3345 0.0527 0.3798 0.085 Uiso 1 1 calc R . . . .
C18 C 0.4344(2) 0.11853(19) 0.53676(18) 0.0728(6) Uani 1 1 d . . . . .
H18 H 0.3981 0.0512 0.5479 0.087 Uiso 1 1 calc R . . . .
C19 C 0.87199(16) 0.10065(18) 0.50848(18) 0.0615(5) Uani 1 1 d . . . . .
H19 H 0.8667 0.0538 0.5474 0.074 Uiso 1 1 calc R . . . .
C20 C 0.91004(15) 0.06424(15) 0.41139(17) 0.0543(4) Uani 1 1 d . . . . .
H20 H 0.9301 -0.0071 0.3854 0.065 Uiso 1 1 calc R . . . .
C21 C 0.91929(13) 0.13297(14) 0.35022(14) 0.0437(4) Uani 1 1 d . . . . .
C22 C 0.95756(14) 0.09777(14) 0.24645(14) 0.0467(4) Uani 1 1 d . . . . .
C23 C 0.95906(14) 0.16782(14) 0.19058(14) 0.0466(4) Uani 1 1 d . . . . .
H23 H 0.9816 0.1425 0.1231 0.056 Uiso 1 1 calc R . . . .
C24 C 0.92879(13) 0.27546(14) 0.22882(13) 0.0432(3) Uani 1 1 d . . . . .
C25 C 0.93273(14) 0.34164(15) 0.16545(14) 0.0477(4) Uani 1 1 d . . . . .
H25 H 0.9589 0.3132 0.1001 0.057 Uiso 1 1 calc R . . . .
C26 C 0.90287(18) 0.50816(18) 0.12679(16) 0.0585(5) Uani 1 1 d . . . . .
H26A H 0.8428 0.4589 0.0564 0.070 Uiso 1 1 calc R . . . .
H26B H 0.9808 0.5284 0.1105 0.070 Uiso 1 1 calc R . . . .
C27 C 0.87601(16) 0.62363(16) 0.19195(15) 0.0527(4) Uani 1 1 d . . . . .
H27A H 0.9392 0.6747 0.2600 0.063 Uiso 1 1 calc R . . . .
H27B H 0.8753 0.6684 0.1478 0.063 Uiso 1 1 calc R . . . .
C28 C 0.68638(13) 0.00916(13) -0.02121(12) 0.0394(3) Uani 1 1 d . . . . .
C29 C 0.72153(16) -0.04322(15) -0.12058(14) 0.0523(4) Uani 1 1 d . . . . .
H29 H 0.7280 -0.0048 -0.1670 0.063 Uiso 1 1 calc R . . . .
C30 C 0.74651(18) -0.15052(17) -0.15024(16) 0.0632(5) Uani 1 1 d . . . . .
H30 H 0.7679 -0.1855 -0.2173 0.076 Uiso 1 1 calc R . . . .
C31 C 0.66041(13) 0.12407(13) 0.00769(12) 0.0391(3) Uani 1 1 d . . . . .
C32 C 0.6099(2) -0.0547(2) 0.22167(19) 0.0730(6) Uani 1 1 d . . . . .
H32 H 0.5881 -0.0097 0.2857 0.088 Uiso 1 1 calc R . . . .
C33 C 0.73386(15) 0.51555(15) 0.66757(12) 0.0454(4) Uani 1 1 d . . . . .
H33 H 0.7973 0.5810 0.7223 0.054 Uiso 1 1 calc R . . . .
C34 C 0.67810(15) 0.42366(15) 0.69214(13) 0.0469(4) Uani 1 1 d . . . . .
C36 C 0.58160(15) 0.31893(15) 0.60675(13) 0.0468(4) Uani 1 1 d . . . . .
C37 C 0.52430(18) 0.21533(18) 0.62054(17) 0.0626(5) Uani 1 1 d . . . . .
H37 H 0.5481 0.2128 0.6877 0.075 Uiso 1 1 calc R . . . .
C38 C 0.88971(15) 0.31522(15) 0.33144(14) 0.0471(4) Uani 1 1 d . . . . .
C39 C 0.88716(14) 0.23985(15) 0.39186(14) 0.0450(4) Uani 1 1 d . . . . .
C40 C 0.84899(17) 0.27474(18) 0.49113(16) 0.0580(4) Uani 1 1 d . . . . .
H40 H 0.8283 0.3457 0.5183 0.070 Uiso 1 1 calc R . . . .
C41 C 0.84143(17) 0.20636(19) 0.54918(18) 0.0632(5) Uani 1 1 d . . . . .
H41 H 0.8160 0.2308 0.6152 0.076 Uiso 1 1 calc R . . . .
C42 C 0.99614(17) -0.00763(16) 0.19591(18) 0.0621(5) Uani 1 1 d . . . . .
H42 H 1.0087 -0.0255 0.1248 0.074 Uiso 1 1 calc R . . . .
O3 O 0.7964(2) 0.5211(2) 0.87907(15) 0.0734(8) Uani 0.672(4) 1 d D . P A 1
C35A C 0.724(3) 0.425(2) 0.800(2) 0.0602(18) Uani 0.328(4) 1 d D . P A 1
H35A H 0.6984 0.3542 0.8096 0.072 Uiso 0.328(4) 1 calc R . P A 1
O3A O 0.6662(6) 0.3918(5) 0.8569(4) 0.096(2) Uani 0.328(4) 1 d D . P A 2
C35 C 0.7162(12) 0.4418(9) 0.8064(11) 0.0602(18) Uani 0.672(4) 1 d D . P A 2
H35 H 0.7905 0.5011 0.8467 0.072 Uiso 0.672(4) 1 calc R . P A 2
O1W O 1.1141(3) -0.2607(3) 0.1164(3) 0.0865(7) Uani 0.561(4) 1 d . U P B 1
H1WA H 1.1767 -0.2286 0.1001 0.130 Uiso 0.561(4) 1 d R . P B 1
H1WB H 1.0670 -0.2215 0.1104 0.130 Uiso 0.561(4) 1 d R . P B 1
O1X O 1.1651(4) -0.2285(4) 0.1835(4) 0.0865(7) Uani 0.439(4) 1 d . U P B 2
H1XA H 1.1426 -0.1661 0.2104 0.130 Uiso 0.439(4) 1 d R . P B 2
H1XB H 1.2338 -0.2080 0.1707 0.130 Uiso 0.439(4) 1 d R . P B 2
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'
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
C7 N1 H1 117.6 . .
C7 N1 C8 124.74(14) . .
C8 N1 H1 117.6 . .
C9 N2 C10 111.03(13) . .
C9 N2 C27 111.82(13) . .
C10 N2 C27 111.53(13) . .
C11 N3 H3 117.4 . .
C12 N3 H3 117.4 . .
C12 N3 C11 125.20(14) . .
C25 N4 H4 117.1 . .
C25 N4 C26 125.84(15) . .
C26 N4 H4 117.1 . .
C2 C1 H1A 119.8 . .
C2 C1 C30 120.40(17) . .
C30 C1 H1A 119.8 . .
C1 C2 H2 119.4 . .
C1 C2 C3 121.16(17) . .
C3 C2 H2 119.4 . .
C2 C3 C4 122.82(15) . .
C28 C3 C2 117.99(14) . .
C28 C3 C4 119.19(13) . .
C3 C4 C32 124.39(15) . .
C5 C4 C3 118.94(14) . .
C5 C4 C32 116.56(15) . .
C4 C5 H5 118.0 . .
C4 C5 C6 123.98(14) . .
C6 C5 H5 118.0 . .
C5 C6 C31 119.61(13) . .
C7 C6 C5 118.95(13) . .
C7 C6 C31 121.42(13) . .
N1 C7 C6 124.30(14) . .
N1 C7 H7 117.9 . .
C6 C7 H7 117.9 . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
N1 C8 C9 110.72(14) . .
H8A C8 H8B 108.1 . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
N2 C9 C8 111.81(12) . .
N2 C9 H9A 109.3 . .
N2 C9 H9B 109.3 . .
C8 C9 H9A 109.3 . .
C8 C9 H9B 109.3 . .
H9A C9 H9B 107.9 . .
N2 C10 H10A 109.1 . .
N2 C10 H10B 109.1 . .
N2 C10 C11 112.57(13) . .
H10A C10 H10B 107.8 . .
C11 C10 H10A 109.1 . .
C11 C10 H10B 109.1 . .
N3 C11 C10 110.75(14) . .
N3 C11 H11A 109.5 . .
N3 C11 H11B 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 108.1 . .
N3 C12 H12 117.8 . .
N3 C12 C13 124.48(15) . .
C13 C12 H12 117.8 . .
C12 C13 C14 120.23(14) . .
C12 C13 C33 119.98(14) . .
C33 C13 C14 119.77(14) . .
O4 C14 C13 122.14(14) . .
O4 C14 C15 120.87(14) . .
C13 C14 C15 116.98(13) . .
C16 C15 C14 118.68(15) . .
C16 C15 C36 120.08(16) . .
C36 C15 C14 121.21(14) . .
C15 C16 H16 119.6 . .
C17 C16 C15 120.79(18) . .
C17 C16 H16 119.6 . .
C16 C17 H17 120.2 . .
C16 C17 C18 119.51(19) . .
C18 C17 H17 120.2 . .
C17 C18 H18 119.4 . .
C37 C18 C17 121.20(19) . .
C37 C18 H18 119.4 . .
C20 C19 H19 119.6 . .
C20 C19 C41 120.74(17) . .
C41 C19 H19 119.6 . .
C19 C20 H20 119.4 . .
C19 C20 C21 121.22(16) . .
C21 C20 H20 119.4 . .
C20 C21 C22 123.42(15) . .
C39 C21 C20 117.61(15) . .
C39 C21 C22 118.96(14) . .
C23 C22 C21 119.19(14) . .
C23 C22 C42 116.06(16) . .
C42 C22 C21 124.74(16) . .
C22 C23 H23 118.0 . .
C22 C23 C24 124.07(15) . .
C24 C23 H23 118.0 . .
C23 C24 C25 120.12(15) . .
C23 C24 C38 119.38(14) . .
C25 C24 C38 120.48(14) . .
N4 C25 C24 124.44(16) . .
N4 C25 H25 117.8 . .
C24 C25 H25 117.8 . .
N4 C26 H26A 109.7 . .
N4 C26 H26B 109.7 . .
N4 C26 C27 109.72(14) . .
H26A C26 H26B 108.2 . .
C27 C26 H26A 109.7 . .
C27 C26 H26B 109.7 . .
N2 C27 C26 112.04(13) . .
N2 C27 H27A 109.2 . .
N2 C27 H27B 109.2 . .
C26 C27 H27A 109.2 . .
C26 C27 H27B 109.2 . .
H27A C27 H27B 107.9 . .
C3 C28 C31 121.35(13) . .
C29 C28 C3 119.55(14) . .
C29 C28 C31 119.10(14) . .
C28 C29 H29 119.7 . .
C30 C29 C28 120.69(17) . .
C30 C29 H29 119.7 . .
C1 C30 H30 119.9 . .
C29 C30 C1 120.15(17) . .
C29 C30 H30 119.9 . .
O1 C31 C6 121.76(14) . .
O1 C31 C28 121.32(13) . .
C6 C31 C28 116.92(13) . .
O2 C32 C4 127.9(2) . .
O2 C32 H32 116.1 . .
C4 C32 H32 116.1 . .
C13 C33 H33 118.1 . .
C34 C33 C13 123.74(15) . .
C34 C33 H33 118.1 . .
C33 C34 C36 118.99(14) . .
C33 C34 C35A 120.5(10) . .
C33 C34 C35 116.7(5) . .
C36 C34 C35A 120.2(10) . .
C36 C34 C35 124.2(5) . .
C15 C36 C34 119.14(15) . .
C37 C36 C15 117.34(16) . .
C37 C36 C34 123.51(16) . .
C18 C37 C36 121.07(18) . .
C18 C37 H37 119.5 . .
C36 C37 H37 119.5 . .
O5 C38 C24 122.02(15) . .
O5 C38 C39 121.10(15) . .
C24 C38 C39 116.88(13) . .
C21 C39 C38 121.48(15) . .
C40 C39 C21 119.86(15) . .
C40 C39 C38 118.64(14) . .
C39 C40 H40 119.4 . .
C41 C40 C39 121.25(17) . .
C41 C40 H40 119.4 . .
C19 C41 H41 120.3 . .
C40 C41 C19 119.32(18) . .
C40 C41 H41 120.3 . .
O6 C42 C22 128.2(2) . .
O6 C42 H42 115.9 . .
C22 C42 H42 115.9 . .
C34 C35A H35A 120.0 . .
O3 C35A C34 120(2) . .
O3 C35A H35A 120.0 . .
C34 C35 H35 115.0 . .
O3A C35 C34 130.0(9) . .
O3A C35 H35 115.0 . .
H1WA O1W H1WB 104.5 . .
H1XA O1X H1XB 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C31 1.2601(18) .
O2 C32 1.209(2) .
O4 C14 1.2576(18) .
O5 C38 1.2439(19) .
O6 C42 1.214(2) .
N1 H1 0.8600 .
N1 C7 1.2971(19) .
N1 C8 1.453(2) .
N2 C9 1.4634(19) .
N2 C10 1.466(2) .
N2 C27 1.468(2) .
N3 H3 0.8600 .
N3 C11 1.455(2) .
N3 C12 1.292(2) .
N4 H4 0.8600 .
N4 C25 1.290(2) .
N4 C26 1.464(2) .
C1 H1A 0.9300 .
C1 C2 1.364(3) .
C1 C30 1.384(3) .
C2 H2 0.9300 .
C2 C3 1.411(2) .
C3 C4 1.447(2) .
C3 C28 1.410(2) .
C4 C5 1.362(2) .
C4 C32 1.447(2) .
C5 H5 0.9300 .
C5 C6 1.407(2) .
C6 C7 1.404(2) .
C6 C31 1.433(2) .
C7 H7 0.9300 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C9 1.516(2) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 C11 1.507(2) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12 0.9300 .
C12 C13 1.403(2) .
C13 C14 1.438(2) .
C13 C33 1.405(2) .
C14 C15 1.464(2) .
C15 C16 1.398(2) .
C15 C36 1.416(2) .
C16 H16 0.9300 .
C16 C17 1.370(3) .
C17 H17 0.9300 .
C17 C18 1.382(3) .
C18 H18 0.9300 .
C18 C37 1.367(3) .
C19 H19 0.9300 .
C19 C20 1.372(3) .
C19 C41 1.384(3) .
C20 H20 0.9300 .
C20 C21 1.409(2) .
C21 C22 1.451(2) .
C21 C39 1.408(2) .
C22 C23 1.369(2) .
C22 C42 1.448(2) .
C23 H23 0.9300 .
C23 C24 1.403(2) .
C24 C25 1.409(2) .
C24 C38 1.443(2) .
C25 H25 0.9300 .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C26 C27 1.507(3) .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C28 C29 1.399(2) .
C28 C31 1.466(2) .
C29 H29 0.9300 .
C29 C30 1.370(3) .
C30 H30 0.9300 .
C32 H32 0.9300 .
C33 H33 0.9300 .
C33 C34 1.367(2) .
C34 C36 1.449(2) .
C34 C35A 1.48(3) .
C34 C35 1.456(15) .
C36 C37 1.410(2) .
C37 H37 0.9300 .
C38 C39 1.475(2) .
C39 C40 1.397(2) .
C40 H40 0.9300 .
C40 C41 1.371(2) .
C41 H41 0.9300 .
C42 H42 0.9300 .
O3 C35A 1.257(19) .
C35A H35A 0.9300 .
O3A C35 1.210(16) .
C35 H35 0.9300 .
O1W H1WA 0.8500 .
O1W H1WB 0.8499 .
O1X H1XA 0.8499 .
O1X H1XB 0.8501 .
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
N1 H1 O1 0.86 1.98 2.6445(17) 133.0 .
N3 H3 O4 0.86 1.95 2.6192(17) 134.0 .
N4 H4 O5 0.86 1.96 2.6309(18) 134.1 .
C7 H7 O4 0.93 2.24 3.1434(19) 164.0 .
C9 H9A O3A 0.97 2.50 3.396(6) 153.5 1_554
O1W H1WA O1 0.85 2.00 2.844(3) 171.1 2_755
O1W H1WB O6 0.85 2.22 2.872(3) 133.3 .
O1X H1XA O6 0.85 2.10 2.890(4) 154.0 .
O1X H1XB O1 0.85 2.13 2.870(4) 145.1 2_755
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
O4 C14 C15 C16 2.6(2) . . . .
O4 C14 C15 C36 -179.19(14) . . . .
O5 C38 C39 C21 177.78(16) . . . .
O5 C38 C39 C40 -0.6(3) . . . .
N1 C8 C9 N2 -70.35(18) . . . .
N2 C10 C11 N3 -70.85(19) . . . .
N3 C12 C13 C14 0.3(2) . . . .
N3 C12 C13 C33 178.64(14) . . . .
N4 C26 C27 N2 -58.12(19) . . . .
C1 C2 C3 C4 178.07(16) . . . .
C1 C2 C3 C28 -2.4(2) . . . .
C2 C1 C30 C29 1.8(3) . . . .
C2 C3 C4 C5 178.01(14) . . . .
C2 C3 C4 C32 -6.0(3) . . . .
C2 C3 C28 C29 2.7(2) . . . .
C2 C3 C28 C31 -178.10(13) . . . .
C3 C4 C5 C6 1.1(2) . . . .
C3 C4 C32 O2 -3.0(4) . . . .
C3 C28 C29 C30 -0.8(2) . . . .
C3 C28 C31 O1 178.48(13) . . . .
C3 C28 C31 C6 -0.9(2) . . . .
C4 C3 C28 C29 -177.80(14) . . . .
C4 C3 C28 C31 1.4(2) . . . .
C4 C5 C6 C7 177.71(14) . . . .
C4 C5 C6 C31 -0.5(2) . . . .
C5 C4 C32 O2 173.0(2) . . . .
C5 C6 C7 N1 -176.07(14) . . . .
C5 C6 C31 O1 -178.98(14) . . . .
C5 C6 C31 C28 0.4(2) . . . .
C7 N1 C8 C9 122.35(16) . . . .
C7 C6 C31 O1 2.8(2) . . . .
C7 C6 C31 C28 -177.80(12) . . . .
C8 N1 C7 C6 179.28(13) . . . .
C9 N2 C10 C11 153.23(14) . . . .
C9 N2 C27 C26 -77.19(16) . . . .
C10 N2 C9 C8 -96.95(15) . . . .
C10 N2 C27 C26 157.81(13) . . . .
C11 N3 C12 C13 -178.54(15) . . . .
C12 N3 C11 C10 -172.37(15) . . . .
C12 C13 C14 O4 -4.3(2) . . . .
C12 C13 C14 C15 174.23(13) . . . .
C12 C13 C33 C34 -176.26(14) . . . .
C13 C14 C15 C16 -175.94(14) . . . .
C13 C14 C15 C36 2.3(2) . . . .
C13 C33 C34 C36 1.9(2) . . . .
C13 C33 C34 C35A 175.7(15) . . . .
C13 C33 C34 C35 -174.6(7) . . . .
C14 C13 C33 C34 2.1(2) . . . .
C14 C15 C16 C17 177.71(17) . . . .
C14 C15 C36 C34 1.6(2) . . . .
C14 C15 C36 C37 -177.33(15) . . . .
C15 C16 C17 C18 -0.2(3) . . . .
C15 C36 C37 C18 -0.5(3) . . . .
C16 C15 C36 C34 179.81(15) . . . .
C16 C15 C36 C37 0.9(2) . . . .
C16 C17 C18 C37 0.5(3) . . . .
C17 C18 C37 C36 -0.2(3) . . . .
C19 C20 C21 C22 -179.21(16) . . . .
C19 C20 C21 C39 -0.5(2) . . . .
C20 C19 C41 C40 0.3(3) . . . .
C20 C21 C22 C23 177.35(14) . . . .
C20 C21 C22 C42 -3.1(2) . . . .
C20 C21 C39 C38 -177.75(14) . . . .
C20 C21 C39 C40 0.6(2) . . . .
C21 C22 C23 C24 1.9(2) . . . .
C21 C22 C42 O6 -7.7(3) . . . .
C21 C39 C40 C41 -0.3(3) . . . .
C22 C21 C39 C38 1.0(2) . . . .
C22 C21 C39 C40 179.41(15) . . . .
C22 C23 C24 C25 -179.88(14) . . . .
C22 C23 C24 C38 -2.0(2) . . . .
C23 C22 C42 O6 171.8(2) . . . .
C23 C24 C25 N4 177.47(15) . . . .
C23 C24 C38 O5 -177.36(16) . . . .
C23 C24 C38 C39 1.5(2) . . . .
C24 C38 C39 C21 -1.1(2) . . . .
C24 C38 C39 C40 -179.53(15) . . . .
C25 N4 C26 C27 -173.34(16) . . . .
C25 C24 C38 O5 0.5(3) . . . .
C25 C24 C38 C39 179.39(14) . . . .
C26 N4 C25 C24 -178.48(16) . . . .
C27 N2 C9 C8 137.78(14) . . . .
C27 N2 C10 C11 -81.33(16) . . . .
C28 C3 C4 C5 -1.5(2) . . . .
C28 C3 C4 C32 174.47(16) . . . .
C28 C29 C30 C1 -1.5(3) . . . .
C29 C28 C31 O1 -2.3(2) . . . .
C29 C28 C31 C6 178.36(13) . . . .
C30 C1 C2 C3 0.2(3) . . . .
C31 C6 C7 N1 2.1(2) . . . .
C31 C28 C29 C30 180.00(15) . . . .
C32 C4 C5 C6 -175.22(16) . . . .
C33 C13 C14 O4 177.37(14) . . . .
C33 C13 C14 C15 -4.1(2) . . . .
C33 C34 C36 C15 -3.8(2) . . . .
C33 C34 C36 C37 175.11(16) . . . .
C33 C34 C35A O3 15(3) . . . .
C33 C34 C35 O3A 161.1(11) . . . .
C34 C36 C37 C18 -179.42(18) . . . .
C36 C15 C16 C17 -0.5(3) . . . .
C36 C34 C35A O3 -171.1(18) . . . .
C36 C34 C35 O3A -15.2(17) . . . .
C38 C24 C25 N4 -0.4(3) . . . .
C38 C39 C40 C41 178.09(17) . . . .
C39 C21 C22 C23 -1.3(2) . . . .
C39 C21 C22 C42 178.21(15) . . . .
C39 C40 C41 C19 -0.1(3) . . . .
C41 C19 C20 C21 0.0(3) . . . .
C42 C22 C23 C24 -177.70(15) . . . .
C35A C34 C36 C15 -177.5(15) . . . .
C35A C34 C36 C37 1.4(15) . . . .
C35 C34 C36 C15 172.5(7) . . . .
C35 C34 C36 C37 -8.6(7) . . . .
