#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316443.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_4316443
loop_
_publ_author_name
'Ghulam Abbas'
'Yanhua Lan'
'George E. Kostakis'
'Wolfgang Wernsdorfer'
'Christopher E. Anson'
'Annie K. Powell'
_publ_contact_author
; 
Annie K. Powell
;
_publ_contact_author_email       annie.powell@kit.edu
_publ_contact_author_phone       '+49 721 608 2135'
_publ_section_title
;
 Series of Isostructural Planar Lanthanide Complexes
 [LnIII4(μ3-OH)2(mdeaH)2(piv)8] with Single Molecule Magnet Behavior for
 the Dy4 Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8067
_journal_page_last               8072
_journal_paper_doi               10.1021/ic1011605
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C50 H98 N2 O22 Tm4'
_chemical_formula_weight         1755.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.982(2)
_cell_angle_beta                 98.675(2)
_cell_angle_gamma                102.879(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5849(13)
_cell_length_b                   12.4410(14)
_cell_length_c                   12.6697(15)
_cell_measurement_reflns_used    3728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.18
_cell_volume                     1633.2(3)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.449
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.151
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6917
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0507P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                5097
_reflns_number_total             6917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011605_si_002_5.cif
_cod_data_source_block           ga17x
_cod_database_code               4316443
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.39905(3) 0.33633(3) 0.39523(3) 0.02000(10) Uani 1 1 d D . .
Tm2 Tm 0.72609(3) 0.41954(3) 0.44033(3) 0.01986(10) Uani 1 1 d . . .
O1 O 0.5662(4) 0.4989(4) 0.4255(4) 0.0212(11) Uani 1 1 d D . .
H1 H 0.552(5) 0.519(3) 0.371(3) 0.025 Uiso 1 1 d D . .
N1 N 0.7456(5) 0.2117(5) 0.4064(5) 0.0245(14) Uani 1 1 d . . .
C1 C 0.7037(8) 0.1870(7) 0.5032(8) 0.035(2) Uani 1 1 d . . .
H1A H 0.7606 0.2424 0.5772 0.042 Uiso 1 1 calc R . .
H1B H 0.7011 0.1048 0.4960 0.042 Uiso 1 1 calc R . .
C2 C 0.5758(7) 0.2029(7) 0.4997(8) 0.0309(19) Uani 1 1 d . . .
H2A H 0.5146 0.1308 0.4415 0.037 Uiso 1 1 calc R . .
H2B H 0.5573 0.2132 0.5755 0.037 Uiso 1 1 calc R . .
O2 O 0.5681(4) 0.3031(4) 0.4721(4) 0.0225(11) Uani 1 1 d . . .
C3 C 0.8758(7) 0.2171(7) 0.4179(8) 0.0331(19) Uani 1 1 d . . .
H3A H 0.8839 0.1356 0.3930 0.040 Uiso 1 1 calc R . .
H3B H 0.9208 0.2600 0.4995 0.040 Uiso 1 1 calc R . .
C4 C 0.9313(7) 0.2819(6) 0.3433(7) 0.0311(19) Uani 1 1 d . . .
H4A H 1.0198 0.2908 0.3544 0.037 Uiso 1 1 calc R . .
H4B H 0.8907 0.2377 0.2608 0.037 Uiso 1 1 calc R . .
O3 O 0.9091(5) 0.3973(5) 0.3842(5) 0.0278(13) Uani 1 1 d . . .
H3 H 0.928(8) 0.427(8) 0.346(8) 0.033 Uiso 1 1 d . . .
C5 C 0.6709(8) 0.1174(7) 0.2971(8) 0.041(2) Uani 1 1 d . . .
H5A H 0.6853 0.0416 0.2928 0.061 Uiso 1 1 calc R . .
H5B H 0.6934 0.1370 0.2326 0.061 Uiso 1 1 calc R . .
H5C H 0.5844 0.1110 0.2932 0.061 Uiso 1 1 calc R . .
O4 O 0.7119(4) 0.5373(4) 0.6386(4) 0.0214(11) Uani 1 1 d . . .
O5 O 0.8654(4) 0.4653(4) 0.6209(4) 0.0246(11) Uani 1 1 d . . .
C6 C 0.8030(6) 0.5124(6) 0.6843(6) 0.0200(15) Uani 1 1 d . . .
C7 C 0.8310(7) 0.5323(6) 0.8105(7) 0.0262(17) Uani 1 1 d . . .
C8 C 0.7421(12) 0.5844(12) 0.8719(9) 0.088(5) Uani 1 1 d . . .
H8A H 0.6595 0.5297 0.8374 0.132 Uiso 1 1 calc R . .
H8B H 0.7441 0.6608 0.8645 0.132 Uiso 1 1 calc R . .
H8C H 0.7652 0.5965 0.9535 0.132 Uiso 1 1 calc R . .
C9 C 0.8351(10) 0.4191(9) 0.8271(9) 0.058(3) Uani 1 1 d . . .
H9A H 0.7543 0.3608 0.7936 0.087 Uiso 1 1 calc R . .
H9B H 0.8590 0.4349 0.9095 0.087 Uiso 1 1 calc R . .
H9C H 0.8947 0.3877 0.7890 0.087 Uiso 1 1 calc R . .
C10 C 0.9606(10) 0.6213(11) 0.8669(10) 0.079(4) Uani 1 1 d . . .
H10A H 1.0198 0.5888 0.8291 0.118 Uiso 1 1 calc R . .
H10B H 0.9822 0.6343 0.9488 0.118 Uiso 1 1 calc R . .
H10C H 0.9616 0.6970 0.8584 0.118 Uiso 1 1 calc R . .
O6 O 0.7113(5) 0.7262(4) 0.4888(5) 0.0357(14) Uani 1 1 d . . .
O7 O 0.8202(4) 0.5991(4) 0.4362(5) 0.0281(12) Uani 1 1 d . . .
C11 C 0.7780(7) 0.6819(6) 0.4285(7) 0.0273(17) Uani 1 1 d . . .
C12 C 0.8028(8) 0.7317(7) 0.3346(7) 0.036(2) Uani 1 1 d . . .
C13 C 0.6812(11) 0.7109(14) 0.2554(10) 0.096(5) Uani 1 1 d . . .
H13A H 0.6418 0.6253 0.2157 0.144 Uiso 1 1 calc R . .
H13B H 0.6946 0.7471 0.1985 0.144 Uiso 1 1 calc R . .
H13C H 0.6286 0.7468 0.3007 0.144 Uiso 1 1 calc R . .
C14 C 0.8818(9) 0.6719(8) 0.2653(8) 0.048(2) Uani 1 1 d . . .
H14A H 0.8409 0.5863 0.2283 0.072 Uiso 1 1 calc R . .
H14B H 0.9605 0.6854 0.3164 0.072 Uiso 1 1 calc R . .
H14C H 0.8953 0.7051 0.2064 0.072 Uiso 1 1 calc R . .
C15 C 0.8598(13) 0.8661(9) 0.3923(11) 0.083(4) Uani 1 1 d . . .
H15A H 0.8759 0.8993 0.3338 0.124 Uiso 1 1 calc R . .
H15B H 0.9365 0.8836 0.4480 0.124 Uiso 1 1 calc R . .
H15C H 0.8034 0.9017 0.4321 0.124 Uiso 1 1 calc R . .
O8 O 0.4540(5) 0.2960(4) 0.2194(4) 0.0283(12) Uani 1 1 d . . .
O9 O 0.6556(5) 0.3429(4) 0.2479(4) 0.0287(12) Uani 1 1 d . . .
C16 C 0.5487(7) 0.3016(6) 0.1833(6) 0.0232(16) Uani 1 1 d . . .
C17 C 0.5393(7) 0.2584(7) 0.0522(7) 0.0314(18) Uani 1 1 d . . .
C18 C 0.4131(11) 0.1708(9) -0.0139(9) 0.068(3) Uani 1 1 d . . .
H18A H 0.4081 0.1443 -0.0967 0.103 Uiso 1 1 calc R . .
H18B H 0.3500 0.2102 0.0034 0.103 Uiso 1 1 calc R . .
H18C H 0.4005 0.1021 0.0093 0.103 Uiso 1 1 calc R . .
C19 C 0.6398(12) 0.2057(13) 0.0239(9) 0.098(5) Uani 1 1 d . . .
H19A H 0.7187 0.2646 0.0669 0.147 Uiso 1 1 calc R . .
H19B H 0.6346 0.1822 -0.0588 0.147 Uiso 1 1 calc R . .
H19C H 0.6322 0.1358 0.0450 0.147 Uiso 1 1 calc R . .
C20 C 0.5540(10) 0.3695(9) 0.0200(9) 0.060(3) Uani 1 1 d . . .
H20A H 0.6348 0.4257 0.0609 0.091 Uiso 1 1 calc R . .
H20B H 0.4909 0.4072 0.0418 0.091 Uiso 1 1 calc R . .
H20C H 0.5455 0.3459 -0.0632 0.091 Uiso 1 1 calc R . .
O10 O 0.3458(4) 0.1262(4) 0.3113(5) 0.0288(12) Uani 1 1 d . . .
O11 O 0.2100(5) 0.2139(4) 0.2677(5) 0.0352(14) Uani 1 1 d . . .
C21 C 0.2404(7) 0.1196(7) 0.2608(7) 0.0272(17) Uani 1 1 d . . .
C22 C 0.1494(7) -0.0019(6) 0.1902(7) 0.0284(18) Uani 1 1 d . . .
C23 C 0.1784(9) -0.0976(7) 0.2278(9) 0.053(3) Uani 1 1 d . . .
H23A H 0.2604 -0.1016 0.2199 0.080 Uiso 1 1 calc R . .
H23B H 0.1186 -0.1742 0.1796 0.080 Uiso 1 1 calc R . .
H23C H 0.1752 -0.0795 0.3084 0.080 Uiso 1 1 calc R . .
C24 C 0.0190(7) 0.0032(7) 0.2020(8) 0.040(2) Uani 1 1 d . . .
H24A H 0.0147 0.0186 0.2820 0.060 Uiso 1 1 calc R . .
H24B H -0.0405 -0.0728 0.1518 0.060 Uiso 1 1 calc R . .
H24C H 0.0007 0.0671 0.1796 0.060 Uiso 1 1 calc R . .
C25 C 0.1533(8) -0.0258(8) 0.0668(8) 0.046(2) Uani 1 1 d . . .
H25A H 0.2349 -0.0300 0.0575 0.069 Uiso 1 1 calc R . .
H25B H 0.1350 0.0384 0.0452 0.069 Uiso 1 1 calc R . .
H25C H 0.0927 -0.1014 0.0173 0.069 Uiso 1 1 calc R . .
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'
Tm Tm -0.3139 5.2483 '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
O2 Tm1 O6 93.71(19) . 2_666 ?
O2 Tm1 O8 90.14(18) . . ?
O6 Tm1 O8 149.54(18) 2_666 . ?
O2 Tm1 O4 152.16(16) . 2_666 ?
O6 Tm1 O4 96.88(18) 2_666 2_666 ?
O8 Tm1 O4 93.56(17) . 2_666 ?
O2 Tm1 O1 71.82(16) . . ?
O6 Tm1 O1 134.85(18) 2_666 . ?
O8 Tm1 O1 74.83(17) . . ?
O4 Tm1 O1 82.55(16) 2_666 . ?
O2 Tm1 O11 134.59(17) . . ?
O6 Tm1 O11 76.2(2) 2_666 . ?
O8 Tm1 O11 79.65(19) . . ?
O4 Tm1 O11 73.12(16) 2_666 . ?
O1 Tm1 O11 143.32(18) . . ?
O2 Tm1 O10 79.00(17) . . ?
O6 Tm1 O10 75.94(18) 2_666 . ?
O8 Tm1 O10 75.18(18) . . ?
O4 Tm1 O10 128.57(16) 2_666 . ?
O1 Tm1 O10 137.60(17) . . ?
O11 Tm1 O10 55.59(16) . . ?
O2 Tm1 O1 87.68(16) . 2_666 ?
O6 Tm1 O1 70.80(17) 2_666 2_666 ?
O8 Tm1 O1 139.60(17) . 2_666 ?
O4 Tm1 O1 71.80(16) 2_666 2_666 ?
O1 Tm1 O1 66.2(2) . 2_666 ?
O11 Tm1 O1 127.59(17) . 2_666 ?
O10 Tm1 O1 143.17(18) . 2_666 ?
O2 Tm2 O9 94.62(19) . . ?
O2 Tm2 O7 149.19(17) . . ?
O9 Tm2 O7 91.15(19) . . ?
O2 Tm2 O1 72.71(16) . . ?
O9 Tm2 O1 80.67(18) . . ?
O7 Tm2 O1 78.45(17) . . ?
O2 Tm2 O3 135.66(17) . . ?
O9 Tm2 O3 80.11(19) . . ?
O7 Tm2 O3 75.15(18) . . ?
O1 Tm2 O3 146.81(18) . . ?
O2 Tm2 O5 96.03(17) . . ?
O9 Tm2 O5 156.27(17) . . ?
O7 Tm2 O5 90.49(18) . . ?
O1 Tm2 O5 122.79(16) . . ?
O3 Tm2 O5 77.44(18) . . ?
O2 Tm2 O4 75.32(17) . . ?
O9 Tm2 O4 151.39(16) . . ?
O7 Tm2 O4 85.28(17) . . ?
O1 Tm2 O4 70.79(16) . . ?
O3 Tm2 O4 125.79(17) . . ?
O5 Tm2 O4 52.31(15) . . ?
O2 Tm2 N1 67.54(17) . . ?
O9 Tm2 N1 82.46(19) . . ?
O7 Tm2 N1 143.26(19) . . ?
O1 Tm2 N1 135.07(18) . . ?
O3 Tm2 N1 68.12(18) . . ?
O5 Tm2 N1 82.13(18) . . ?
O4 Tm2 N1 116.45(17) . . ?
Tm2 O1 Tm1 101.69(18) . . ?
Tm2 O1 Tm1 107.30(19) . 2_666 ?
Tm1 O1 Tm1 113.8(2) . 2_666 ?
Tm2 O1 H1 118(4) . . ?
Tm1 O1 H1 106(3) . . ?
Tm1 O1 H1 110(3) 2_666 . ?
C5 N1 C3 110.4(6) . . ?
C5 N1 C1 109.2(6) . . ?
C3 N1 C1 109.9(6) . . ?
C5 N1 Tm2 116.2(5) . . ?
C3 N1 Tm2 108.5(4) . . ?
C1 N1 Tm2 102.4(4) . . ?
N1 C1 C2 108.3(6) . . ?
N1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
N1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 110.8(6) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 O2 Tm1 127.0(4) . . ?
C2 O2 Tm2 122.8(4) . . ?
Tm1 O2 Tm2 106.99(19) . . ?
N1 C3 C4 110.2(6) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 C3 104.4(6) . . ?
O3 C4 H4A 110.9 . . ?
C3 C4 H4A 110.9 . . ?
O3 C4 H4B 110.9 . . ?
C3 C4 H4B 110.9 . . ?
H4A C4 H4B 108.9 . . ?
C4 O3 Tm2 121.7(4) . . ?
C4 O3 H3 107(7) . . ?
Tm2 O3 H3 116(7) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 O4 Tm1 155.3(4) . 2_666 ?
C6 O4 Tm2 91.1(4) . . ?
Tm1 O4 Tm2 102.86(18) 2_666 . ?
C6 O5 Tm2 96.7(4) . . ?
O5 C6 O4 118.5(7) . . ?
O5 C6 C7 120.5(6) . . ?
O4 C6 C7 120.9(6) . . ?
C9 C7 C6 110.6(6) . . ?
C9 C7 C8 110.3(8) . . ?
C6 C7 C8 113.0(6) . . ?
C9 C7 C10 106.9(8) . . ?
C6 C7 C10 107.7(7) . . ?
C8 C7 C10 108.1(9) . . ?
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 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 O6 Tm1 132.6(5) . 2_666 ?
C11 O7 Tm2 130.6(5) . . ?
O7 C11 O6 125.4(7) . . ?
O7 C11 C12 119.2(7) . . ?
O6 C11 C12 115.4(7) . . ?
C14 C12 C13 109.4(8) . . ?
C14 C12 C15 112.3(8) . . ?
C13 C12 C15 106.8(9) . . ?
C14 C12 C11 111.6(7) . . ?
C13 C12 C11 108.2(8) . . ?
C15 C12 C11 108.4(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 O8 Tm1 138.5(5) . . ?
C16 O9 Tm2 132.4(5) . . ?
O8 C16 O9 124.0(7) . . ?
O8 C16 C17 119.9(7) . . ?
O9 C16 C17 116.2(6) . . ?
C19 C17 C18 112.0(9) . . ?
C19 C17 C20 108.7(9) . . ?
C18 C17 C20 108.6(8) . . ?
C19 C17 C16 110.6(7) . . ?
C18 C17 C16 110.2(7) . . ?
C20 C17 C16 106.6(7) . . ?
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 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 O10 Tm1 91.9(4) . . ?
C21 O11 Tm1 91.9(4) . . ?
O10 C21 O11 120.5(7) . . ?
O10 C21 C22 119.6(7) . . ?
O11 C21 C22 120.0(6) . . ?
O10 C21 Tm1 60.5(4) . . ?
O11 C21 Tm1 60.1(4) . . ?
C22 C21 Tm1 177.5(6) . . ?
C25 C22 C23 111.4(7) . . ?
C25 C22 C21 106.5(6) . . ?
C23 C22 C21 112.1(7) . . ?
C25 C22 C24 108.3(7) . . ?
C23 C22 C24 109.2(7) . . ?
C21 C22 C24 109.2(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
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
Tm1 O2 2.237(5) . ?
Tm1 O6 2.295(5) 2_666 ?
Tm1 O8 2.337(5) . ?
Tm1 O4 2.341(4) 2_666 ?
Tm1 O1 2.348(5) . ?
Tm1 O11 2.360(5) . ?
Tm1 O10 2.371(5) . ?
Tm1 O1 2.419(5) 2_666 ?
Tm2 O2 2.243(5) . ?
Tm2 O9 2.250(5) . ?
Tm2 O7 2.278(5) . ?
Tm2 O1 2.296(4) . ?
Tm2 O3 2.380(5) . ?
Tm2 O5 2.407(5) . ?
Tm2 O4 2.515(5) . ?
Tm2 N1 2.547(6) . ?
O1 Tm1 2.419(5) 2_666 ?
O1 H1 0.82(3) . ?
N1 C5 1.473(10) . ?
N1 C3 1.477(9) . ?
N1 C1 1.481(10) . ?
C1 C2 1.533(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.417(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.549(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.455(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 H3 0.72(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O4 C6 1.274(8) . ?
O4 Tm1 2.341(4) 2_666 ?
O5 C6 1.252(8) . ?
C6 C7 1.508(10) . ?
C7 C9 1.500(11) . ?
C7 C8 1.516(12) . ?
C7 C10 1.553(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O6 C11 1.257(9) . ?
O6 Tm1 2.295(5) 2_666 ?
O7 C11 1.259(9) . ?
C11 C12 1.544(11) . ?
C12 C14 1.511(12) . ?
C12 C13 1.518(13) . ?
C12 C15 1.528(12) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O8 C16 1.247(8) . ?
O9 C16 1.267(9) . ?
C16 C17 1.548(11) . ?
C17 C19 1.493(12) . ?
C17 C18 1.534(13) . ?
C17 C20 1.546(12) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O10 C21 1.261(8) . ?
O11 C21 1.280(8) . ?
C21 C22 1.524(10) . ?
C22 C25 1.503(12) . ?
C22 C23 1.502(11) . ?
C22 C24 1.554(11) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
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
O3 H3 O5 0.72(8) 2.37(9) 2.807(7) 121(9) 2_766
