##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
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# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
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# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
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#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
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data_global
_audit_creation_method     'SHELX-97'
_journal_date_recd_electronic     2005-07-18
_journal_date_accepted     2005-09-14
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2005
_journal_volume     61
_journal_issue     10
_journal_page_first     m2039
_journal_page_last     m2041
_journal_paper_category     EM
_journal_coeditor_code     BV6028
_publ_contact_author_name     'Kevin Klausmeyer'
_publ_contact_author_address
;Department of Chemistry and Biochemistry,
Baylor University,
One Bear Place #97348,
Waco, Tx 76798-7348
USA
;
_publ_contact_author_email     kevin_klausmeyer@baylor.edu
_publ_contact_author_fax     254-710-4272
_publ_contact_author_phone     254-710-2665
_publ_section_title
;
Tris(tetraethylammonium)
μ-3-hydroxypropanolato-di-μ-methoxo-bis[tricarbonyltungsten(0)]
;
loop_
    _publ_author_name
    _publ_author_address
    'Klausmeyer, Kevin K.'
;
Department of Chemistry and Biochemistry
Baylor University
One Bear Place #97348
Waco
TX 76798-7348
USA
;
    'Adrian, Rafael A.'
;
Department of Chemistry and Biochemistry
Baylor University
One Bear Place #97348
Waco
TX 76798-7348
USA
;
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Tris(tetraethylammonium)
μ-3-hydroxypropanolato-di-μ-methoxo-bis[tricarbonyltungsten(0)]
;
_chemical_name_common     ?
_chemical_formula_moiety     '3C8 H20 N +, C11 H13 O10 W2 3-'
_chemical_formula_sum     'C35 H73 N3 O10 W2'
_chemical_formula_iupac     '(C8 H20 N)3 [W2 (C H3 O)2 (C3 H7 O2) (C O)6]'
_chemical_formula_weight     1063.63
_chemical_melting_point     ?
_symmetry_cell_setting     Orthorhombic
_symmetry_space_group_name_H-M     'P n m a'
_symmetry_space_group_name_Hall     '-P 2ac 2n'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z'
    'x+1/2, -y+1/2, -z+1/2'
    '-x, -y, -z'
    'x-1/2, y, -z-1/2'
    'x, -y-1/2, z'
    '-x-1/2, y-1/2, z-1/2'
_cell_length_a     16.9476(6)
_cell_length_b     24.1286(9)
_cell_length_c     10.2457(4)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     4189.7(3)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     6700
_cell_measurement_theta_min     2.47
_cell_measurement_theta_max     34.46
_cell_measurement_temperature     110(2)
_exptl_crystal_description     block
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.26
_exptl_crystal_size_mid     0.15
_exptl_crystal_size_min     0.13
_exptl_crystal_density_diffrn     1.686
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2120
_exptl_absorpt_coefficient_mu     5.540
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.2974
_exptl_absorpt_correction_T_max     0.4848
_exptl_special_details
;
     Refinement of F² against ALL reflections.  The weighted R-factor wR and
  goodness of fit S are based on F², conventional R-factors R are based
  on F, with F set to zero for negative F². The threshold expression of
  F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
  not relevant to the choice of reflections for refinement.  R-factors based
  on F² are statistically about twice as large as those based on F, and R-
  factors based on ALL data will be even larger.
;
_diffrn_ambient_temperature     110(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART CCD area-detector'
_diffrn_measurement_method     'φ and ω'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     27335
_diffrn_reflns_av_R_equivalents     0.0243
_diffrn_reflns_av_sigmaI/netI     0.0191
_diffrn_reflns_theta_min     2.16
_diffrn_reflns_theta_max     28.28
_diffrn_reflns_theta_full     26.00
_diffrn_measured_fraction_theta_max     0.973
_diffrn_measured_fraction_theta_full     0.980
_diffrn_reflns_limit_h_min     -22
_diffrn_reflns_limit_h_max     22
_diffrn_reflns_limit_k_min     -32
_diffrn_reflns_limit_k_max     23
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     11
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
  Refinement of F² against ALL reflections.  The weighted R-factor wR and
  goodness of fit S are based on F², conventional R-factors R are based
  on F, with F set to zero for negative F². The threshold expression of
  F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
  not relevant to the choice of reflections for refinement.  R-factors based
  on F² are statistically about twice as large as those based on F, and R-
  factors based on ALL data will be even larger.
;
_reflns_number_total     5181
_reflns_number_gt     4411
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0282
_refine_ls_R_factor_gt     0.0224
_refine_ls_wR_factor_gt     0.0556
_refine_ls_wR_factor_ref     0.0601
_refine_ls_goodness_of_fit_ref     1.019
_refine_ls_restrained_S_all     1.034
_refine_ls_number_reflns     5181
_refine_ls_number_parameters     274
_refine_ls_number_restraints     5
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0293P)²+7.8991P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.004
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     2.552
_refine_diff_density_min     -0.772
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'W' 'W' -0.8490 6.8722
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'APEX-2 (Bruker, 2003)'
_computing_cell_refinement     'APEX-2'
_computing_data_reduction     'SAINT-Plus (Bruker, 2003)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2000)'
_computing_publication_material     'SHELXTL'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    W1 0.120112(6) 0.682331(4) 1.400128(11) 0.02087(5) Uani d . 1 . . W
    O1 0.15179(18) 0.59719(10) 1.1764(2) 0.0476(6) Uani d . 1 . . O
    O2 -0.00686(13) 0.59786(9) 1.4974(2) 0.0351(5) Uani d . 1 . . O
    O3 0.24150(14) 0.61157(10) 1.5583(2) 0.0353(5) Uani d . 1 . . O
    O4 0.10259(17) 0.7500 1.5404(3) 0.0220(6) Uani d S 1 . . O
    O5 0.19831(17) 0.7500 1.3367(3) 0.0241(6) Uani d S 1 . . O
    N1 0.12964(15) 0.50237(11) 0.8078(3) 0.0286(5) Uani d . 1 . . N
    C1 0.13868(19) 0.63054(13) 1.2595(3) 0.0312(7) Uani d . 1 . . C
    C2 0.04105(18) 0.63060(12) 1.4595(3) 0.0257(6) Uani d . 1 . . C
    C3 0.19455(17) 0.63833(12) 1.4972(3) 0.0261(6) Uani d . 1 . . C
    C4 0.1402(3) 0.7500 1.6612(4) 0.0326(10) Uani d S 1 . . C
    H4A 0.1254 0.7826 1.7090 0.049 Uiso d PR 0.50 . . H
    H4B 0.1963 0.7500 1.6485 0.049 Uiso d SR 1 . . H
    C5 0.2808(3) 0.7500 1.3546(5) 0.0305(9) Uani d S 1 . . C
    H5A 0.3030 0.7835 1.3196 0.046 Uiso d PR 0.50 . . H
    H5B 0.2918 0.7500 1.4464 0.046 Uiso d SR 1 . . H
    O6 0.05275(17) 0.7500 1.3127(3) 0.0241(6) Uani d S 1 . . O
    C6 -0.01112(16) 0.7500 1.2256(3) 0.0380(11) Uani d S 1 . . C
    H6A -0.0300 0.7884 1.2127 0.046 Uiso calc PR 0.50 . . H
    H6B -0.0550 0.7280 1.2627 0.046 Uiso calc PR 0.50 . . H
    C7 0.01377(16) 0.7250(2) 1.0922(3) 0.0393(16) Uani d PR 0.50 . . C
    H7A 0.0259 0.6853 1.1055 0.047 Uiso calc PR 0.50 . . H
    H7B -0.0320 0.7271 1.0324 0.047 Uiso calc PR 0.50 . . H
    C8 0.07930(16) 0.7500 1.0294(3) 0.087(3) Uani d SR 1 . . C
    H8A 0.0794 0.7346 0.9398 0.104 Uiso calc PR 0.50 . . H
    H8B 0.0650 0.7896 1.0201 0.104 Uiso calc PR 0.50 . . H
    O7 0.15790(16) 0.7500 1.0679(3) 0.0588(12) Uani d SR 1 . . O
    H7 0.1605 0.7526 1.1496 0.088 Uiso calc PR 0.50 . . H
    C9 0.21424(19) 0.50277(14) 0.7599(4) 0.0361(7) Uani d . 1 . . C
    H9A 0.2238 0.4682 0.7103 0.043 Uiso calc R 1 . . H
    H9B 0.2207 0.5341 0.6986 0.043 Uiso calc R 1 . . H
    C10 0.2768(2) 0.50757(17) 0.8650(4) 0.0484(9) Uani d . 1 . . C
    H10A 0.3292 0.5071 0.8246 0.073 Uiso calc R 1 . . H
    H10B 0.2720 0.4763 0.9256 0.073 Uiso calc R 1 . . H
    H10C 0.2696 0.5424 0.9128 0.073 Uiso calc R 1 . . H
    C11 0.07718(19) 0.50265(14) 0.6875(3) 0.0336(7) Uani d . 1 . . C
    H11A 0.0895 0.5362 0.6357 0.040 Uiso calc R 1 . . H
    H11B 0.0908 0.4700 0.6334 0.040 Uiso calc R 1 . . H
    C12 -0.0102(2) 0.50168(17) 0.7132(4) 0.0445(9) Uani d . 1 . . C
    H12A -0.0388 0.5021 0.6301 0.067 Uiso calc R 1 . . H
    H12B -0.0250 0.5343 0.7647 0.067 Uiso calc R 1 . . H
    H12C -0.0239 0.4680 0.7617 0.067 Uiso calc R 1 . . H
    C13 0.1131(2) 0.55184(16) 0.8947(3) 0.0381(8) Uani d . 1 . . C
    H13A 0.1478 0.5497 0.9722 0.046 Uiso calc R 1 . . H
    H13B 0.0578 0.5496 0.9256 0.046 Uiso calc R 1 . . H
    C14 0.1253(2) 0.60758(16) 0.8293(4) 0.0464(9) Uani d . 1 . . C
    H14A 0.1125 0.6373 0.8910 0.070 Uiso calc R 1 . . H
    H14B 0.0908 0.6104 0.7528 0.070 Uiso calc R 1 . . H
    H14C 0.1805 0.6111 0.8018 0.070 Uiso calc R 1 . . H
    C15 0.1139(2) 0.45127(15) 0.8923(3) 0.0344(7) Uani d . 1 . . C
    H15A 0.1508 0.4517 0.9671 0.041 Uiso calc R 1 . . H
    H15B 0.0597 0.4538 0.9278 0.041 Uiso calc R 1 . . H
    C16 0.1224(2) 0.39619(15) 0.8209(4) 0.0463(9) Uani d . 1 . . C
    H16A 0.1097 0.3657 0.8806 0.069 Uiso calc R 1 . . H
    H16B 0.1768 0.3921 0.7898 0.069 Uiso calc R 1 . . H
    H16C 0.0862 0.3953 0.7463 0.069 Uiso calc R 1 . . H
    N2 -0.1305(2) 0.7500 1.6477(5) 0.0439(11) Uani d SPD 0.486(6) . 1 N
    C17 -0.0956(6) 0.7279(4) 1.5275(8) 0.060(3) Uani d PD 0.486(6) . 1 C
    H17A -0.0456 0.7085 1.5474 0.072 Uiso calc PR 0.486(6) . 1 H
    H17B -0.0841 0.7585 1.4659 0.072 Uiso calc PR 0.486(6) . 1 H
    C18 -0.1546(7) 0.6877(5) 1.4670(10) 0.067(3) Uani d PD 0.486(6) . 1 C
    H18A -0.1330 0.6730 1.3853 0.100 Uiso calc PR 0.486(6) . 1 H
    H18B -0.2041 0.7071 1.4490 0.100 Uiso calc PR 0.486(6) . 1 H
    H18C -0.1644 0.6571 1.5277 0.100 Uiso calc PR 0.486(6) . 1 H
    C19 -0.1544(4) 0.7116(3) 1.7505(7) 0.0343(17) Uani d PD 0.486(6) . 1 C
    H19A -0.2031 0.6920 1.7234 0.041 Uiso calc PR 0.486(6) . 1 H
    H19B -0.1662 0.7326 1.8311 0.041 Uiso calc PR 0.486(6) . 1 H
    C20 -0.0895(19) 0.6690(14) 1.778(2) 0.061(6) Uani d P 0.486(6) . 1 C
    H20A -0.1073 0.6436 1.8470 0.091 Uiso calc PR 0.486(6) . 1 H
    H20B -0.0417 0.6883 1.8076 0.091 Uiso calc PR 0.486(6) . 1 H
    H20C -0.0779 0.6480 1.6989 0.091 Uiso calc PR 0.486(6) . 1 H
    N2A -0.1305(2) 0.7500 1.6477(5) 0.0439(11) Uani d SPD 0.514(6) . 2 N
    C17A -0.2027(4) 0.7111(3) 1.6167(6) 0.0342(16) Uani d PD 0.514(6) . 2 C
    H17C -0.2165 0.6912 1.6981 0.041 Uiso calc PR 0.514(6) . 2 H
    H17D -0.2481 0.7350 1.5944 0.041 Uiso calc PR 0.514(6) . 2 H
    C18A -0.1946(6) 0.6680(3) 1.5089(8) 0.051(2) Uani d PD 0.514(6) . 2 C
    H18D -0.2443 0.6475 1.5002 0.076 Uiso calc PR 0.514(6) . 2 H
    H18E -0.1520 0.6422 1.5309 0.076 Uiso calc PR 0.514(6) . 2 H
    H18F -0.1824 0.6866 1.4263 0.076 Uiso calc PR 0.514(6) . 2 H
    C19A -0.0633(4) 0.7073(3) 1.7043(8) 0.049(2) Uani d PD 0.514(6) . 2 C
    H19C -0.0474 0.6821 1.6327 0.058 Uiso calc PR 0.514(6) . 2 H
    H19D -0.0163 0.7292 1.7289 0.058 Uiso calc PR 0.514(6) . 2 H
    C20A -0.0868(17) 0.6725(12) 1.820(2) 0.063(6) Uani d P 0.514(6) . 2 C
    H20D -0.0424 0.6489 1.8454 0.094 Uiso calc PR 0.514(6) . 2 H
    H20E -0.1320 0.6493 1.7960 0.094 Uiso calc PR 0.514(6) . 2 H
    H20F -0.1013 0.6968 1.8925 0.094 Uiso calc PR 0.514(6) . 2 H
_geom_special_details
;
  All esds (except the esd in the dihedral angle between two l.s. planes)
  are estimated using the full covariance matrix.  The cell esds are taken
  into account individually in the estimation of esds in distances, angles
  and torsion angles; correlations between esds in cell parameters are only
  used when they are defined by crystal symmetry.  An approximate (isotropic)
  treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    W1 C3 . 1.926(3) ?
    W1 C2 . 1.930(3) ?
    W1 C1 . 1.933(3) ?
    W1 O6 . 2.1844(18) Y
    W1 O4 . 2.1952(19) Y
    W1 O5 . 2.2010(19) Y
    O1 C1 . 1.193(4) ?
    O2 C2 . 1.198(4) ?
    O3 C3 . 1.201(4) ?
    O4 C4 . 1.392(5) Y
    O4 W1 7_575 2.1952(19) Y
    O5 C5 . 1.411(5) Y
    O5 W1 7_575 2.2010(19) Y
    N1 C13 . 1.515(4) ?
    N1 C9 . 1.516(4) ?
    N1 C11 . 1.520(4) ?
    N1 C15 . 1.530(4) ?
    C4 H4A . 0.9599 ?
    C4 H4B . 0.9600 ?
    C5 H5A . 0.9600 ?
    C5 H5B . 0.9587 ?
    O6 C6 . 1.403(4) Y
    O6 W1 7_575 2.1844(18) Y
    C6 C7 . 1.5522 ?
    C6 H6A . 0.9900 ?
    C6 H6B . 0.9900 ?
    C7 C8 . 1.4181 ?
    C7 H7A . 0.9900 ?
    C7 H7B . 0.9900 ?
    C8 O7 . 1.389(4) ?
    C8 H8A . 0.9900 ?
    C8 H8B . 0.9900 ?
    O7 H7 . 0.8400 ?
    C9 C10 . 1.515(5) ?
    C9 H9A . 0.9900 ?
    C9 H9B . 0.9900 ?
    C10 H10A . 0.9800 ?
    C10 H10B . 0.9800 ?
    C10 H10C . 0.9800 ?
    C11 C12 . 1.505(5) ?
    C11 H11A . 0.9900 ?
    C11 H11B . 0.9900 ?
    C12 H12A . 0.9800 ?
    C12 H12B . 0.9800 ?
    C12 H12C . 0.9800 ?
    C13 C14 . 1.517(5) ?
    C13 H13A . 0.9900 ?
    C13 H13B . 0.9900 ?
    C14 H14A . 0.9800 ?
    C14 H14B . 0.9800 ?
    C14 H14C . 0.9800 ?
    C15 C16 . 1.524(5) ?
    C15 H15A . 0.9900 ?
    C15 H15B . 0.9900 ?
    C16 H16A . 0.9800 ?
    C16 H16B . 0.9800 ?
    C16 H16C . 0.9800 ?
    N2 C19 7_575 1.460(7) ?
    N2 C19 . 1.460(7) ?
    N2 C17 . 1.467(8) ?
    N2 C17 7_575 1.467(8) ?
    C17 C18 . 1.525(12) ?
    C17 H17A . 0.9900 ?
    C17 H17B . 0.9900 ?
    C18 H18A . 0.9800 ?
    C18 H18B . 0.9800 ?
    C18 H18C . 0.9800 ?
    C19 C20 . 1.53(3) ?
    C19 H19A . 0.9900 ?
    C19 H19B . 0.9900 ?
    C20 H20A . 0.9800 ?
    C20 H20B . 0.9800 ?
    C20 H20C . 0.9800 ?
    C17A C18A . 1.522(9) ?
    C17A H17C . 0.9900 ?
    C17A H17D . 0.9900 ?
    C18A H18D . 0.9800 ?
    C18A H18E . 0.9800 ?
    C18A H18F . 0.9800 ?
    C19A C20A . 1.50(3) ?
    C19A H19C . 0.9900 ?
    C19A H19D . 0.9900 ?
    C20A H20D . 0.9800 ?
    C20A H20E . 0.9800 ?
    C20A H20F . 0.9800 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C3 W1 C2 . . 86.30(12) ?
    C3 W1 C1 . . 85.52(13) ?
    C2 W1 C1 . . 85.97(13) ?
    C3 W1 O6 . . 165.09(11) ?
    C2 W1 O6 . . 104.47(11) ?
    C1 W1 O6 . . 105.23(12) ?
    C3 W1 O4 . . 99.24(11) ?
    C2 W1 O4 . . 100.42(11) ?
    C1 W1 O4 . . 172.22(11) ?
    O6 W1 O4 . . 69.01(9) ?
    C3 W1 O5 . . 99.61(11) ?
    C2 W1 O5 . . 172.32(10) ?
    C1 W1 O5 . . 99.30(11) ?
    O6 W1 O5 . . 68.84(10) ?
    O4 W1 O5 . . 73.92(9) ?
    C4 O4 W1 . 7_575 121.34(15) Y
    C4 O4 W1 . . 121.34(15) ?
    W1 O4 W1 7_575 . 96.11(11) Y
    C5 O5 W1 . . 123.97(13) Y
    C5 O5 W1 . 7_575 123.97(13) ?
    W1 O5 W1 . 7_575 95.77(11) Y
    C13 N1 C9 . . 111.1(3) ?
    C13 N1 C11 . . 111.4(2) ?
    C9 N1 C11 . . 106.9(2) ?
    C13 N1 C15 . . 105.7(3) ?
    C9 N1 C15 . . 110.7(2) ?
    C11 N1 C15 . . 111.1(2) ?
    O1 C1 W1 . . 177.3(3) ?
    O2 C2 W1 . . 178.7(3) ?
    O3 C3 W1 . . 179.1(3) ?
    O4 C4 H4A . . 109.5 ?
    O4 C4 H4B . . 109.4 ?
    H4A C4 H4B . . 109.2 ?
    O5 C5 H5A . . 109.9 ?
    O5 C5 H5B . . 108.6 ?
    H5A C5 H5B . . 106.9 ?
    C6 O6 W1 . 7_575 131.62(5) Y
    C6 O6 W1 . . 131.62(5) ?
    W1 O6 W1 7_575 . 96.74(11) Y
    O6 C6 C7 . . 110.52(15) ?
    O6 C6 H6A . . 109.5 ?
    C7 C6 H6A . . 109.5 ?
    O6 C6 H6B . . 109.5 ?
    C7 C6 H6B . . 109.5 ?
    H6A C6 H6B . . 108.1 ?
    C8 C7 C6 . . 116.6 ?
    C8 C7 H7A . . 108.2 ?
    C6 C7 H7A . . 108.2 ?
    C8 C7 H7B . . 108.2 ?
    C6 C7 H7B . . 108.2 ?
    H7A C7 H7B . . 107.3 ?
    O7 C8 C7 . . 128.5 ?
    O7 C8 H8A . . 105.2 ?
    C7 C8 H8A . . 105.2 ?
    O7 C8 H8B . . 105.2 ?
    C7 C8 H8B . . 105.2 ?
    H8A C8 H8B . . 105.9 ?
    C8 O7 H7 . . 109.5 ?
    C10 C9 N1 . . 115.6(3) ?
    C10 C9 H9A . . 108.4 ?
    N1 C9 H9A . . 108.4 ?
    C10 C9 H9B . . 108.4 ?
    N1 C9 H9B . . 108.4 ?
    H9A C9 H9B . . 107.4 ?
    C9 C10 H10A . . 109.5 ?
    C9 C10 H10B . . 109.5 ?
    H10A C10 H10B . . 109.5 ?
    C9 C10 H10C . . 109.5 ?
    H10A C10 H10C . . 109.5 ?
    H10B C10 H10C . . 109.5 ?
    C12 C11 N1 . . 115.7(3) ?
    C12 C11 H11A . . 108.4 ?
    N1 C11 H11A . . 108.4 ?
    C12 C11 H11B . . 108.4 ?
    N1 C11 H11B . . 108.4 ?
    H11A C11 H11B . . 107.4 ?
    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 ?
    N1 C13 C14 . . 114.4(3) ?
    N1 C13 H13A . . 108.7 ?
    C14 C13 H13A . . 108.7 ?
    N1 C13 H13B . . 108.7 ?
    C14 C13 H13B . . 108.7 ?
    H13A C13 H13B . . 107.6 ?
    C13 C14 H14A . . 109.5 ?
    C13 C14 H14B . . 109.5 ?
    H14A C14 H14B . . 109.5 ?
    C13 C14 H14C . . 109.5 ?
    H14A C14 H14C . . 109.5 ?
    H14B C14 H14C . . 109.5 ?
    C16 C15 N1 . . 114.5(3) ?
    C16 C15 H15A . . 108.6 ?
    N1 C15 H15A . . 108.6 ?
    C16 C15 H15B . . 108.6 ?
    N1 C15 H15B . . 108.6 ?
    H15A C15 H15B . . 107.6 ?
    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 ?
    C19 N2 C19 7_575 . 78.9(6) ?
    C19 N2 C17 7_575 . 161.5(5) ?
    C19 N2 C17 . . 119.1(5) ?
    C19 N2 C17 7_575 7_575 119.1(5) ?
    C19 N2 C17 . 7_575 161.5(5) ?
    N2 C17 C18 . . 108.0(7) ?
    N2 C17 H17A . . 110.1 ?
    C18 C17 H17A . . 110.1 ?
    N2 C17 H17B . . 110.1 ?
    C18 C17 H17B . . 110.1 ?
    H17A C17 H17B . . 108.4 ?
    C17 C18 H18A . . 109.5 ?
    C17 C18 H18B . . 109.5 ?
    H18A C18 H18B . . 109.5 ?
    C17 C18 H18C . . 109.5 ?
    H18A C18 H18C . . 109.5 ?
    H18B C18 H18C . . 109.5 ?
    N2 C19 C20 . . 111.2(13) ?
    N2 C19 H19A . . 109.4 ?
    C20 C19 H19A . . 109.4 ?
    N2 C19 H19B . . 109.4 ?
    C20 C19 H19B . . 109.4 ?
    H19A C19 H19B . . 108.0 ?
    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 ?
    C18A C17A H17C . . 107.6 ?
    C18A C17A H17D . . 107.6 ?
    H17C C17A H17D . . 107.0 ?
    C17A C18A H18D . . 109.5 ?
    C17A C18A H18E . . 109.5 ?
    H18D C18A H18E . . 109.5 ?
    C17A C18A H18F . . 109.5 ?
    H18D C18A H18F . . 109.5 ?
    H18E C18A H18F . . 109.5 ?
    C20A C19A H19C . . 108.2 ?
    C20A C19A H19D . . 108.2 ?
    H19C C19A H19D . . 107.3 ?
    C19A C20A H20D . . 109.5 ?
    C19A C20A H20E . . 109.5 ?
    H20D C20A H20E . . 109.5 ?
    C19A C20A H20F . . 109.5 ?
    H20D C20A H20F . . 109.5 ?
    H20E C20A H20F . . 109.5 ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O7 H7 O5 . 0.84 2.02 2.838(4) 163 Y
    O7 H7 O6 . 0.84 2.48 3.077(4) 129 Y
