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#$Date: 2016-08-07 10:53:59 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/30/1543098.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_1543098
loop_
_publ_author_name
'Qin, Lei'
'Hartley, Anna'
'Turner, Peter'
'Elmes, Robert B. P.'
'Jolliffe, Katrina A.'
_publ_section_title
;
 Macrocyclic squaramides: anion receptors with high sulfate binding
 affinity and selectivity in aqueous media
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4563
_journal_paper_doi               10.1039/C6SC01011C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C40 H48 N4 O14'
_chemical_formula_weight         808.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.174(5)
_cell_angle_beta                 91.268(4)
_cell_angle_gamma                107.342(5)
_cell_formula_units_Z            1
_cell_length_a                   6.0434(3)
_cell_length_b                   8.9035(5)
_cell_length_c                   20.1417(10)
_cell_measurement_reflns_used    5084
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      75.0670
_cell_measurement_theta_min      4.4700
_cell_volume                     1011.20(10)
_computing_cell_refinement
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_collection
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_reduction
;
  CrysAlisPro, Agilent Technologies,
;
_computing_molecular_graphics
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hï?1/2bschle,C.B., et al., 2011) 
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelxT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(1)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ω
_diffrn_orient_matrix_UB_11      -0.1780364000
_diffrn_orient_matrix_UB_12      -0.1636158000
_diffrn_orient_matrix_UB_13      -0.0325164000
_diffrn_orient_matrix_UB_21      0.0523146000
_diffrn_orient_matrix_UB_22      -0.0695655000
_diffrn_orient_matrix_UB_23      0.0607347000
_diffrn_orient_matrix_UB_31      -0.1934133000
_diffrn_orient_matrix_UB_32      0.0525825000
_diffrn_orient_matrix_UB_33      0.0371070000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9488
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.288
_diffrn_reflns_theta_min         4.492
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  CrysAlisPro, Agilent Technologies,
  Version 1.171.37.35
  Empirical absorption correction using spherical 
  harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         9488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0509
_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)+(0.03P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4992
_reflns_number_total             9488
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc01011c2.cif
_cod_data_source_block           kaj15pt1_s1423
_cod_depositor_comments
'Adding full bibliography for 1543095--1543098.cif.'
_cod_database_code               1543098
_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.
;
_cell_oxdiff_twin_number         2
_diffrn_oxdiff_twin_integration_method simultaneous
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 0.4846(3) 0.2381(2) -0.12894(9) 0.0397(4) Uani 1 1 d . . . . .
O2 O 0.4519(3) 0.1721(2) 0.02377(9) 0.0371(4) Uani 1 1 d . . . . .
O3 O 0.2280(3) 0.1375(2) 0.23827(9) 0.0415(4) Uani 1 1 d . . . . .
O4 O 0.3176(3) 0.3952(2) 0.29423(8) 0.0364(4) Uani 1 1 d . . . . .
O5 O 0.2352(4) 0.5494(3) 0.42773(10) 0.0634(7) Uani 1 1 d . . . . .
N1 N 1.0241(3) 0.2383(2) -0.12544(10) 0.0310(4) Uani 1 1 d . . . . .
H1N H 1.182(6) 0.235(4) -0.1086(15) 0.057(9) Uiso 1 1 d . . . . .
N2 N 1.0005(3) 0.1824(2) 0.03015(10) 0.0306(4) Uani 1 1 d . . . . .
H2N H 1.137(5) 0.184(3) 0.0172(14) 0.050(9) Uiso 1 1 d . . . . .
C1 C 0.8626(4) 0.2238(3) -0.08210(12) 0.0293(5) Uani 1 1 d . . . . .
C2 C 0.6208(4) 0.2231(3) -0.08533(13) 0.0329(5) Uani 1 1 d . . . . .
C3 C 0.6066(4) 0.1941(3) -0.01558(12) 0.0313(5) Uani 1 1 d . . . . .
C4 C 0.8501(4) 0.1974(3) -0.01477(12) 0.0289(5) Uani 1 1 d . . . . .
C5 C 0.9369(4) 0.1421(3) 0.09534(12) 0.0325(5) Uani 1 1 d . . . . .
H5A H 1.0737 0.1301 0.1192 0.039 Uiso 1 1 calc R U . . .
H5B H 0.8127 0.0371 0.0872 0.039 Uiso 1 1 calc R U . . .
C6 C 0.8530(4) 0.2665(3) 0.14064(11) 0.0303(5) Uani 1 1 d . . . . .
C7 C 0.6529(4) 0.2186(3) 0.17414(12) 0.0312(5) Uani 1 1 d . . . . .
H7 H 0.5712 0.1073 0.1690 0.037 Uiso 1 1 calc R U . . .
C8 C 0.5713(4) 0.3327(3) 0.21520(12) 0.0310(5) Uani 1 1 d . . . . .
C9 C 0.6887(4) 0.4965(3) 0.22162(12) 0.0312(5) Uani 1 1 d . . . . .
H9 H 0.6315 0.5744 0.2487 0.037 Uiso 1 1 calc R U . . .
C10 C 0.8884(4) 0.5457(3) 0.18871(12) 0.0300(5) Uani 1 1 d . . . . .
C11 C 0.9706(4) 0.4295(3) 0.14923(11) 0.0307(5) Uani 1 1 d . . . . .
H11 H 1.1101 0.4630 0.1278 0.037 Uiso 1 1 calc R U . . .
C12 C 1.0106(4) 0.7218(3) 0.19152(12) 0.0317(5) Uani 1 1 d . . . . .
H12A H 0.9485 0.7882 0.2269 0.038 Uiso 1 1 calc R U . . .
H12B H 1.1790 0.7463 0.2038 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3557(4) 0.2753(3) 0.24925(12) 0.0331(5) Uani 1 1 d . . . . .
C14 C 0.1029(4) 0.3535(3) 0.32652(13) 0.0390(6) Uani 1 1 d . . . . .
H14A H 0.1051 0.2751 0.3551 0.047 Uiso 1 1 calc R U . . .
H14B H -0.0308 0.3044 0.2918 0.047 Uiso 1 1 calc R U . . .
C15 C 0.0816(5) 0.5035(4) 0.36898(14) 0.0505(7) Uani 1 1 d . . . . .
H15A H 0.1186 0.5902 0.3429 0.061 Uiso 1 1 calc R U . . .
H15B H -0.0801 0.4858 0.3817 0.061 Uiso 1 1 calc R U . . .
O6A O 0.3033(5) 0.8571(3) 0.57728(12) 0.0430(6) Uani 0.7 1 d . . P A 1
O7A O 0.4456(5) 1.1846(3) 0.67081(14) 0.0483(7) Uani 0.7 1 d . . P A 1
C16A C 0.1857(8) 0.6899(5) 0.46946(19) 0.0437(9) Uani 0.7 1 d . . P A 1
H16A H 0.0259 0.6597 0.4840 0.052 Uiso 0.7 1 calc R U P A 1
H16B H 0.2051 0.7774 0.4442 0.052 Uiso 0.7 1 calc R U P A 1
C17A C 0.3645(7) 0.7398(5) 0.52938(19) 0.0425(9) Uani 0.7 1 d . . P A 1
H17A H 0.3626 0.6460 0.5492 0.051 Uiso 0.7 1 calc R U P A 1
H17B H 0.5222 0.7858 0.5153 0.051 Uiso 0.7 1 calc R U P A 1
C18A C 0.4497(7) 0.9068(5) 0.63944(18) 0.0422(9) Uani 0.7 1 d . . P A 1
H18A H 0.6137 0.9513 0.6299 0.051 Uiso 0.7 1 calc R U P A 1
H18B H 0.4370 0.8125 0.6600 0.051 Uiso 0.7 1 calc R U P A 1
C19A C 0.3814(7) 1.0314(4) 0.68822(18) 0.0433(9) Uani 0.7 1 d . . P A 1
H19A H 0.2106 0.9941 0.6904 0.052 Uiso 0.7 1 calc R U P A 1
H19B H 0.4549 1.0423 0.7340 0.052 Uiso 0.7 1 calc R U P A 1
C20A C 0.2792(8) 1.2032(5) 0.6246(2) 0.0502(10) Uani 0.7 1 d . . P A 1
H20A H 0.2758 1.1337 0.5802 0.075 Uiso 0.7 1 calc R U P A 1
H20B H 0.3221 1.3156 0.6200 0.075 Uiso 0.7 1 calc R U P A 1
H20C H 0.1251 1.1729 0.6417 0.075 Uiso 0.7 1 calc R U P A 1
O6B O 0.4349(13) 0.7783(9) 0.6064(4) 0.0603(19) Uiso 0.3 1 d . . P A 2
O7B O 0.2484(17) 1.0286(11) 0.5773(5) 0.082(3) Uiso 0.3 1 d . . P A 2
C16B C 0.282(2) 0.6649(14) 0.4886(6) 0.053(3) Uiso 0.3 1 d . . P A 2
H16C H 0.1309 0.6551 0.5085 0.063 Uiso 0.3 1 calc R U P A 2
H16D H 0.3316 0.7714 0.4760 0.063 Uiso 0.3 1 calc R U P A 2
C17B C 0.458(2) 0.6717(13) 0.5464(5) 0.054(2) Uiso 0.3 1 d . . P A 2
H17C H 0.4307 0.5626 0.5556 0.065 Uiso 0.3 1 calc R U P A 2
H17D H 0.6178 0.7088 0.5325 0.065 Uiso 0.3 1 calc R U P A 2
C18B C 0.560(2) 0.9423(13) 0.6097(6) 0.059(3) Uiso 0.3 1 d . . P A 2
H18C H 0.6076 0.9566 0.5641 0.071 Uiso 0.3 1 calc R U P A 2
H18D H 0.7022 0.9729 0.6409 0.071 Uiso 0.3 1 calc R U P A 2
C19B C 0.417(2) 1.0521(16) 0.6343(6) 0.073(3) Uiso 0.3 1 d . . P A 2
H19C H 0.3364 1.0227 0.6744 0.088 Uiso 0.3 1 calc R U P A 2
H19D H 0.5164 1.1656 0.6467 0.088 Uiso 0.3 1 calc R U P A 2
C20B C 0.116(3) 1.134(2) 0.5911(9) 0.115(6) Uiso 0.3 1 d . . P A 2
H20D H 0.0680 1.1378 0.6374 0.172 Uiso 0.3 1 calc R U P A 2
H20E H -0.0218 1.0971 0.5587 0.172 Uiso 0.3 1 calc R U P A 2
H20F H 0.2101 1.2424 0.5870 0.172 Uiso 0.3 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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
C13 O4 C14 115.69(19) . .
C16B O5 C15 137.4(6) . .
C15 O5 C16A 105.5(3) . .
C1 N1 C12 122.0(2) . 2_765
C1 N1 H1N 116.6(16) . .
C12 N1 H1N 121.0(16) 2_765 .
C4 N2 C5 122.9(2) . .
C4 N2 H2N 117.0(19) . .
C5 N2 H2N 119.5(19) . .
N1 C1 C4 134.9(2) . .
N1 C1 C2 134.1(2) . .
C4 C1 C2 91.01(18) . .
O1 C2 C1 135.2(2) . .
O1 C2 C3 135.7(2) . .
C1 C2 C3 89.10(19) . .
O2 C3 C4 136.2(2) . .
O2 C3 C2 135.1(2) . .
C4 C3 C2 88.68(18) . .
N2 C4 C1 133.9(2) . .
N2 C4 C3 134.9(2) . .
C1 C4 C3 91.20(19) . .
N2 C5 C6 113.4(2) . .
N2 C5 H5A 108.9 . .
C6 C5 H5A 108.9 . .
N2 C5 H5B 108.9 . .
C6 C5 H5B 108.9 . .
H5A C5 H5B 107.7 . .
C11 C6 C7 118.8(2) . .
C11 C6 C5 121.2(2) . .
C7 C6 C5 120.0(2) . .
C6 C7 C8 120.6(2) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C7 C8 C9 119.7(2) . .
C7 C8 C13 118.4(2) . .
C9 C8 C13 121.8(2) . .
C10 C9 C8 120.3(2) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 C11 119.1(2) . .
C9 C10 C12 121.3(2) . .
C11 C10 C12 119.5(2) . .
C6 C11 C10 121.5(2) . .
C6 C11 H11 119.2 . .
C10 C11 H11 119.2 . .
N1 C12 C10 110.29(19) 2_765 .
N1 C12 H12A 109.6 2_765 .
C10 C12 H12A 109.6 . .
N1 C12 H12B 109.6 2_765 .
C10 C12 H12B 109.6 . .
H12A C12 H12B 108.1 . .
O3 C13 O4 123.4(2) . .
O3 C13 C8 125.0(2) . .
O4 C13 C8 111.6(2) . .
O4 C14 C15 107.7(2) . .
O4 C14 H14A 110.2 . .
C15 C14 H14A 110.2 . .
O4 C14 H14B 110.2 . .
C15 C14 H14B 110.2 . .
H14A C14 H14B 108.5 . .
O5 C15 C14 109.5(3) . .
O5 C15 H15A 109.8 . .
C14 C15 H15A 109.8 . .
O5 C15 H15B 109.8 . .
C14 C15 H15B 109.8 . .
H15A C15 H15B 108.2 . .
C17A O6A C18A 112.3(3) . .
C19A O7A C20A 113.6(3) . .
O5 C16A C17A 103.1(3) . .
O5 C16A H16A 111.1 . .
C17A C16A H16A 111.1 . .
O5 C16A H16B 111.1 . .
C17A C16A H16B 111.1 . .
H16A C16A H16B 109.1 . .
O6A C17A C16A 106.3(3) . .
O6A C17A H17A 110.5 . .
C16A C17A H17A 110.5 . .
O6A C17A H17B 110.5 . .
C16A C17A H17B 110.5 . .
H17A C17A H17B 108.7 . .
O6A C18A C19A 110.7(3) . .
O6A C18A H18A 109.5 . .
C19A C18A H18A 109.5 . .
O6A C18A H18B 109.5 . .
C19A C18A H18B 109.5 . .
H18A C18A H18B 108.1 . .
O7A C19A C18A 113.7(3) . .
O7A C19A H19A 108.8 . .
C18A C19A H19A 108.8 . .
O7A C19A H19B 108.8 . .
C18A C19A H19B 108.8 . .
H19A C19A H19B 107.7 . .
O7A C20A H20A 109.5 . .
O7A C20A H20B 109.5 . .
H20A C20A H20B 109.5 . .
O7A C20A H20C 109.5 . .
H20A C20A H20C 109.5 . .
H20B C20A H20C 109.5 . .
C18B O6B C17B 114.5(9) . .
C20B O7B C19B 111.2(11) . .
O5 C16B C17B 123.0(9) . .
O5 C16B H16C 106.6 . .
C17B C16B H16C 106.6 . .
O5 C16B H16D 106.6 . .
C17B C16B H16D 106.6 . .
H16C C16B H16D 106.5 . .
O6B C17B C16B 110.4(9) . .
O6B C17B H17C 109.6 . .
C16B C17B H17C 109.6 . .
O6B C17B H17D 109.6 . .
C16B C17B H17D 109.6 . .
H17C C17B H17D 108.1 . .
O6B C18B C19B 112.1(11) . .
O6B C18B H18C 109.2 . .
C19B C18B H18C 109.2 . .
O6B C18B H18D 109.2 . .
C19B C18B H18D 109.2 . .
H18C C18B H18D 107.9 . .
O7B C19B C18B 105.1(10) . .
O7B C19B H19C 110.7 . .
C18B C19B H19C 110.7 . .
O7B C19B H19D 110.7 . .
C18B C19B H19D 110.7 . .
H19C C19B H19D 108.8 . .
O7B C20B H20D 109.5 . .
O7B C20B H20E 109.5 . .
H20D C20B H20E 109.5 . .
O7B C20B H20F 109.5 . .
H20D C20B H20F 109.5 . .
H20E C20B H20F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C2 1.243(3) .
O2 C3 1.234(3) .
O3 C13 1.213(3) .
O4 C13 1.339(3) .
O4 C14 1.445(3) .
O5 C16B 1.401(12) .
O5 C15 1.403(4) .
O5 C16A 1.479(4) .
N1 C1 1.318(3) .
N1 C12 1.468(3) 2_765
N1 H1N 1.02(3) .
N2 C4 1.321(3) .
N2 C5 1.457(3) .
N2 H2N 0.87(3) .
C1 C4 1.420(3) .
C1 C2 1.460(3) .
C2 C3 1.477(3) .
C3 C4 1.463(3) .
C5 C6 1.510(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C11 1.387(3) .
C6 C7 1.393(3) .
C7 C8 1.397(3) .
C7 H7 0.9500 .
C8 C9 1.397(3) .
C8 C13 1.486(3) .
C9 C10 1.386(3) .
C9 H9 0.9500 .
C10 C11 1.398(3) .
C10 C12 1.510(3) .
C11 H11 0.9500 .
C12 N1 1.468(3) 2_765
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C14 C15 1.482(4) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
O6A C17A 1.419(4) .
O6A C18A 1.431(4) .
O7A C19A 1.418(4) .
O7A C20A 1.422(5) .
C16A C17A 1.507(6) .
C16A H16A 0.9900 .
C16A H16B 0.9900 .
C17A H17A 0.9900 .
C17A H17B 0.9900 .
C18A C19A 1.495(5) .
C18A H18A 0.9900 .
C18A H18B 0.9900 .
C19A H19A 0.9900 .
C19A H19B 0.9900 .
C20A H20A 0.9800 .
C20A H20B 0.9800 .
C20A H20C 0.9800 .
O6B C18B 1.417(13) .
O6B C17B 1.421(12) .
O7B C20B 1.400(17) .
O7B C19B 1.458(15) .
C16B C17B 1.540(15) .
C16B H16C 0.9900 .
C16B H16D 0.9900 .
C17B H17C 0.9900 .
C17B H17D 0.9900 .
C18B C19B 1.511(16) .
C18B H18C 0.9900 .
C18B H18D 0.9900 .
C19B H19C 0.9900 .
C19B H19D 0.9900 .
C20B H20D 0.9800 .
C20B H20E 0.9800 .
C20B H20F 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
N1 H1N O1 1.02(3) 1.87(3) 2.786(3) 147(2) 1_655
N2 H2N O2 0.87(3) 1.94(3) 2.762(3) 157(3) 1_655
C5 H5A O3 0.99 2.54 3.354(3) 139.8 1_655
C12 H12B O1 0.99 2.54 3.274(3) 130.4 2_765
C20A H20A O6A 0.98 2.51 3.092(5) 118.1 .
C17B H17C O5 0.99 2.55 3.181(12) 121.8 2_666
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_4
C12 N1 C1 C4 -175.2(2) 2_765 .
C12 N1 C1 C2 7.3(4) 2_765 .
N1 C1 C2 O1 -1.3(5) . .
C4 C1 C2 O1 -179.5(3) . .
N1 C1 C2 C3 177.7(3) . .
C4 C1 C2 C3 -0.52(19) . .
O1 C2 C3 O2 1.3(5) . .
C1 C2 C3 O2 -177.7(3) . .
O1 C2 C3 C4 179.5(3) . .
C1 C2 C3 C4 0.50(19) . .
C5 N2 C4 C1 -174.8(2) . .
C5 N2 C4 C3 5.3(4) . .
N1 C1 C4 N2 2.4(5) . .
C2 C1 C4 N2 -179.4(3) . .
N1 C1 C4 C3 -177.7(3) . .
C2 C1 C4 C3 0.5(2) . .
O2 C3 C4 N2 -2.4(5) . .
C2 C3 C4 N2 179.4(3) . .
O2 C3 C4 C1 177.7(3) . .
C2 C3 C4 C1 -0.52(19) . .
C4 N2 C5 C6 -62.4(3) . .
N2 C5 C6 C11 -45.4(3) . .
N2 C5 C6 C7 133.9(2) . .
C11 C6 C7 C8 0.5(4) . .
C5 C6 C7 C8 -178.8(2) . .
C6 C7 C8 C9 1.3(4) . .
C6 C7 C8 C13 179.4(2) . .
C7 C8 C9 C10 -1.5(4) . .
C13 C8 C9 C10 -179.5(2) . .
C8 C9 C10 C11 -0.1(4) . .
C8 C9 C10 C12 176.4(2) . .
C7 C6 C11 C10 -2.1(4) . .
C5 C6 C11 C10 177.2(2) . .
C9 C10 C11 C6 2.0(4) . .
C12 C10 C11 C6 -174.6(2) . .
C9 C10 C12 N1 -108.2(3) . 2_765
C11 C10 C12 N1 68.3(3) . 2_765
C14 O4 C13 O3 -4.2(4) . .
C14 O4 C13 C8 175.8(2) . .
C7 C8 C13 O3 -9.0(4) . .
C9 C8 C13 O3 169.0(3) . .
C7 C8 C13 O4 171.0(2) . .
C9 C8 C13 O4 -11.0(3) . .
C13 O4 C14 C15 -174.6(2) . .
C16B O5 C15 C14 -172.3(7) . .
C16A O5 C15 C14 -174.8(3) . .
O4 C14 C15 O5 -74.8(3) . .
C15 O5 C16A C17A -176.7(3) . .
C18A O6A C17A C16A 175.6(3) . .
O5 C16A C17A O6A -170.4(3) . .
C17A O6A C18A C19A 179.4(3) . .
C20A O7A C19A C18A 86.0(4) . .
O6A C18A C19A O7A -73.4(4) . .
C15 O5 C16B C17B 174.8(7) . .
C18B O6B C17B C16B -84.6(11) . .
O5 C16B C17B O6B -168.2(9) . .
C17B O6B C18B C19B 135.9(10) . .
C20B O7B C19B C18B -174.8(11) . .
O6B C18B C19B O7B -73.8(12) . .
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.9948 -0.0101 0.0016 0.0191 0.9941 -0.0195 0.0220 0.1060 1.0089
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6560 16540 6349
2 0.3440 16245 6349
