#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:02:23 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295182 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/24/1572403.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_1572403
loop_
_publ_author_name
'Amin, Md Khairul'
'Ye, Chunchun'
'Pang, Shuhua'
'Liu, Yuancheng'
'Taylor, Dominic'
'Nichol, Gary S.'
'McKeown, Neil B.'
_publ_section_title
;
 Triptycene-like naphthopleiadene as a readily accessible scaffold for
 supramolecular and materials chemistry.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14968
_journal_page_last               14976
_journal_paper_doi               10.1039/d4sc02755h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H20 O4, 1.5[CH4O]'
_chemical_formula_sum            'C33.5 H26 O5.5'
_chemical_formula_weight         516.54
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-04 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                97.683(4)
_cell_angle_beta                 106.716(4)
_cell_angle_gamma                100.894(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4986(5)
_cell_length_b                   11.6083(6)
_cell_length_c                   12.2425(6)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.1750
_cell_measurement_theta_min      3.8280
_cell_volume                     1374.87(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  12.00   1.00   30.00    --  -15.66 -22.00 -80.00   99
  2  ω    -43.00  56.00   1.00   30.00    --  -15.66  22.00  85.00   99
  3  ω    -54.00  45.00   1.00   30.00    --   17.38 -22.00 -80.00   99
  4  ω    -10.00  89.00   1.00   30.00    --   17.38  22.00  85.00   99
  5  ω    -39.00  11.00   1.00   30.00    --  -15.66 -77.00 120.00   50
  6  ω    -35.00  53.00   1.00   30.00    --  -15.66  38.00 150.00   88
  7  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00  60.00   48
  8  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00 -60.00   48
  9  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00 -30.00   48
 10  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00-120.00   48
 11  ω    -42.00  39.00   1.00   30.00    --  -15.66  77.00 -90.00   81
 12  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00  60.00   76
 13  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00-180.00   76
 14  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00 150.00   48
 15  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00 -30.00   76
 16  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00 -90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0142266000
_diffrn_orient_matrix_UB_12      0.0630581000
_diffrn_orient_matrix_UB_13      0.0178976000
_diffrn_orient_matrix_UB_21      0.0686015000
_diffrn_orient_matrix_UB_22      0.0046945000
_diffrn_orient_matrix_UB_23      0.0007288000
_diffrn_orient_matrix_UB_31      -0.0192555000
_diffrn_orient_matrix_UB_32      0.0058906000
_diffrn_orient_matrix_UB_33      -0.0590850000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_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            36195
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.328
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow cooling'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0626P)²+0.8917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5291
_reflns_number_total             6729
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc02755h2.cif
_cod_data_source_block           nm22008
_cod_depositor_comments
'Adding full bibliography for 1572402--1572407.cif.'
_cod_original_cell_volume        1374.87(12)
_cod_original_formula_sum        'C33.50 H26 O5.50'
_cod_database_code               1572403
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H20O4
_chemical_oxdiff_usercomment     '@ 120 K K71B49c'
_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   0.995
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 51 electrons were 
found in a volume of 404Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH4O] per Formula Unit 
which account for 54 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id K71B49c
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.038
_oxdiff_exptl_absorpt_empirical_full_min 0.915
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 -0.02343(13) 0.42936(12) 0.70554(11) 0.0194(3) Uani 1 1 d . . . . .
H1 H -0.097(3) 0.417(2) 0.722(2) 0.046(8) Uiso 1 1 d . . . . .
O2 O 0.64921(13) 0.30633(13) 0.90867(11) 0.0236(3) Uani 1 1 d . . . . .
H2 H 0.705(3) 0.280(3) 0.967(3) 0.063(9) Uiso 1 1 d . . . . .
O3 O 0.09061(13) 0.59673(13) 0.59577(13) 0.0262(3) Uani 1 1 d . . . . .
H3 H 0.045(3) 0.531(3) 0.618(3) 0.061(9) Uiso 1 1 d . . . . .
O4 O 0.73394(12) 0.39715(12) 0.74473(12) 0.0192(3) Uani 1 1 d . . . . .
H4 H 0.709(3) 0.372(3) 0.796(3) 0.056(9) Uiso 1 1 d . . . . .
C1 C 0.08015(17) 0.40436(15) 0.79035(15) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.19389(17) 0.38490(14) 0.76253(14) 0.0133(3) Uani 1 1 d . . . . .
C3 C 0.30430(17) 0.36095(14) 0.85073(14) 0.0136(3) Uani 1 1 d . . . . .
C4 C 0.42611(17) 0.33681(15) 0.83183(14) 0.0142(3) Uani 1 1 d . . . . .
C5 C 0.52993(17) 0.32452(15) 0.92651(15) 0.0168(3) Uani 1 1 d . . . . .
C6 C 0.51836(19) 0.32953(17) 1.03813(16) 0.0216(4) Uani 1 1 d . . . . .
H6 H 0.590(2) 0.324(2) 1.097(2) 0.035(6) Uiso 1 1 d . . . . .
C7 C 0.40017(19) 0.34503(16) 1.05556(15) 0.0203(4) Uani 1 1 d . . . . .
H7 H 0.392(2) 0.353(2) 1.132(2) 0.036(6) Uiso 1 1 d . . . . .
C8 C 0.29192(18) 0.36210(15) 0.96445(15) 0.0172(4) Uani 1 1 d . . . . .
C9 C 0.17166(19) 0.38060(17) 0.98607(15) 0.0207(4) Uani 1 1 d . . . . .
H9 H 0.167(2) 0.3786(19) 1.0597(19) 0.022(5) Uiso 1 1 d . . . . .
C10 C 0.06688(18) 0.40107(16) 0.90141(15) 0.0188(4) Uani 1 1 d . . . . .
H10 H -0.018(2) 0.4130(18) 0.9131(17) 0.020(5) Uiso 1 1 d . . . . .
C11 C 0.22381(18) 0.59787(16) 0.60389(15) 0.0186(4) Uani 1 1 d . . . . .
C12 C 0.28507(17) 0.50462(15) 0.62980(14) 0.0141(3) Uani 1 1 d . . . . .
C13 C 0.42892(16) 0.52191(14) 0.64453(13) 0.0126(3) Uani 1 1 d . . . . .
C14 C 0.50880(16) 0.43882(14) 0.68415(13) 0.0126(3) Uani 1 1 d . . . . .
C15 C 0.64822(17) 0.46882(15) 0.70014(14) 0.0152(3) Uani 1 1 d . . . . .
C16 C 0.71300(18) 0.57272(16) 0.67257(15) 0.0171(4) Uani 1 1 d . . . . .
H16 H 0.802(2) 0.5852(18) 0.6762(17) 0.017(5) Uiso 1 1 d . . . . .
C17 C 0.63934(18) 0.65225(16) 0.63457(14) 0.0166(3) Uani 1 1 d . . . . .
H17 H 0.681(2) 0.7260(18) 0.6152(16) 0.018(5) Uiso 1 1 d . . . . .
C18 C 0.49840(17) 0.63073(15) 0.62239(14) 0.0154(3) Uani 1 1 d . . . . .
C19 C 0.42645(19) 0.71876(16) 0.58903(16) 0.0205(4) Uani 1 1 d . . . . .
H19 H 0.479(2) 0.788(2) 0.5735(19) 0.029(6) Uiso 1 1 d . . . . .
C20 C 0.29300(19) 0.70391(17) 0.58122(17) 0.0226(4) Uani 1 1 d . . . . .
H20 H 0.239(2) 0.765(2) 0.5560(19) 0.030(6) Uiso 1 1 d . . . . .
C21 C 0.20880(16) 0.27460(15) 0.57641(14) 0.0132(3) Uani 1 1 d . . . . .
C22 C 0.10210(17) 0.20236(15) 0.48525(14) 0.0150(3) Uani 1 1 d . . . . .
H22 H 0.018(2) 0.2306(17) 0.4565(16) 0.013(5) Uiso 1 1 d . . . . .
C23 C 0.11314(17) 0.09201(15) 0.42840(14) 0.0159(3) Uani 1 1 d . . . . .
C24 C 0.00459(19) 0.01574(16) 0.33334(16) 0.0214(4) Uani 1 1 d . . . . .
H24 H -0.080(2) 0.0383(18) 0.3079(17) 0.021(5) Uiso 1 1 d . . . . .
C25 C 0.0191(2) -0.08925(17) 0.27918(17) 0.0257(4) Uani 1 1 d . . . . .
H25 H -0.058(2) -0.143(2) 0.2137(19) 0.028(6) Uiso 1 1 d . . . . .
C26 C 0.1441(2) -0.12401(17) 0.31762(18) 0.0267(4) Uani 1 1 d . . . . .
H26 H 0.156(2) -0.196(2) 0.282(2) 0.039(7) Uiso 1 1 d . . . . .
C27 C 0.2501(2) -0.05374(16) 0.40964(16) 0.0228(4) Uani 1 1 d . . . . .
H27 H 0.340(2) -0.0765(19) 0.4382(18) 0.026(5) Uiso 1 1 d . . . . .
C28 C 0.23800(18) 0.05618(15) 0.46793(14) 0.0163(3) Uani 1 1 d . . . . .
C29 C 0.34616(17) 0.13235(15) 0.56284(15) 0.0157(3) Uani 1 1 d . . . . .
H29 H 0.433(2) 0.1054(17) 0.5905(16) 0.016(5) Uiso 1 1 d . . . . .
C30 C 0.33286(16) 0.23943(14) 0.61584(14) 0.0130(3) Uani 1 1 d . . . . .
C31 C 0.19323(16) 0.38958(14) 0.63872(14) 0.0122(3) Uani 1 1 d . . . . .
H31 H 0.0994(19) 0.3944(16) 0.5948(15) 0.009(4) Uiso 1 1 d . . . . .
C32 C 0.45074(16) 0.32119(15) 0.71443(14) 0.0131(3) Uani 1 1 d . . . . .
H32 H 0.521(2) 0.2816(17) 0.7236(16) 0.015(5) 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 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0329
0 -1 0 0.0230
0 0 -1 0.0684
1 0 -1 0.0911
-1 0 1 0.0793
-2 1 0 0.0917
2 -1 0 0.0917
1 -1 2 0.0917
-1 1 -2 0.0646
-1 0 2 0.0951
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
C1 O1 H1 110.4(18) . . ?
C5 O2 H2 114.4(19) . . ?
C11 O3 H3 114.7(18) . . ?
C15 O4 H4 107(2) . . ?
O1 C1 C2 117.92(15) . . ?
O1 C1 C10 119.15(15) . . ?
C2 C1 C10 122.93(16) . . ?
C1 C2 C3 118.69(15) . . ?
C1 C2 C31 117.16(14) . . ?
C3 C2 C31 124.14(14) . . ?
C4 C3 C2 123.92(15) . . ?
C8 C3 C2 117.91(15) . . ?
C8 C3 C4 118.17(15) . . ?
C3 C4 C32 125.11(14) . . ?
C5 C4 C3 118.27(15) . . ?
C5 C4 C32 116.61(15) . . ?
O2 C5 C4 117.96(15) . . ?
O2 C5 C6 119.12(15) . . ?
C4 C5 C6 122.92(16) . . ?
C5 C6 H6 119.0(15) . . ?
C7 C6 C5 119.31(16) . . ?
C7 C6 H6 121.7(15) . . ?
C6 C7 H7 120.8(14) . . ?
C6 C7 C8 120.97(17) . . ?
C8 C7 H7 118.0(14) . . ?
C7 C8 C3 120.17(16) . . ?
C9 C8 C3 120.25(16) . . ?
C9 C8 C7 119.57(16) . . ?
C8 C9 H9 117.6(13) . . ?
C10 C9 C8 121.27(16) . . ?
C10 C9 H9 121.1(13) . . ?
C1 C10 H10 117.8(12) . . ?
C9 C10 C1 118.87(16) . . ?
C9 C10 H10 123.3(12) . . ?
O3 C11 C12 124.22(16) . . ?
O3 C11 C20 112.90(15) . . ?
C12 C11 C20 122.87(16) . . ?
C11 C12 C13 118.16(15) . . ?
C11 C12 C31 117.08(15) . . ?
C13 C12 C31 124.75(14) . . ?
C14 C13 C12 124.10(15) . . ?
C18 C13 C12 118.16(14) . . ?
C18 C13 C14 117.70(15) . . ?
C13 C14 C32 123.93(14) . . ?
C15 C14 C13 118.43(15) . . ?
C15 C14 C32 117.60(14) . . ?
O4 C15 C14 122.06(15) . . ?
O4 C15 C16 114.94(15) . . ?
C14 C15 C16 123.00(15) . . ?
C15 C16 H16 120.5(13) . . ?
C17 C16 C15 119.43(16) . . ?
C17 C16 H16 120.0(13) . . ?
C16 C17 H17 121.8(12) . . ?
C16 C17 C18 120.57(16) . . ?
C18 C17 H17 117.6(12) . . ?
C17 C18 C13 120.69(15) . . ?
C17 C18 C19 119.10(16) . . ?
C19 C18 C13 120.21(16) . . ?
C18 C19 H19 115.2(13) . . ?
C20 C19 C18 120.95(17) . . ?
C20 C19 H19 123.8(13) . . ?
C11 C20 H20 118.1(13) . . ?
C19 C20 C11 119.40(16) . . ?
C19 C20 H20 122.4(13) . . ?
C22 C21 C30 120.07(15) . . ?
C22 C21 C31 120.63(14) . . ?
C30 C21 C31 119.25(14) . . ?
C21 C22 H22 118.7(11) . . ?
C21 C22 C23 121.44(15) . . ?
C23 C22 H22 119.8(11) . . ?
C22 C23 C24 122.65(16) . . ?
C22 C23 C28 118.66(15) . . ?
C24 C23 C28 118.68(16) . . ?
C23 C24 H24 119.0(12) . . ?
C25 C24 C23 121.26(17) . . ?
C25 C24 H24 119.8(12) . . ?
C24 C25 H25 120.4(13) . . ?
C24 C25 C26 119.99(18) . . ?
C26 C25 H25 119.6(13) . . ?
C25 C26 H26 121.4(15) . . ?
C27 C26 C25 120.42(18) . . ?
C27 C26 H26 118.2(15) . . ?
C26 C27 H27 121.8(12) . . ?
C26 C27 C28 120.89(18) . . ?
C28 C27 H27 117.3(12) . . ?
C23 C28 C27 118.75(16) . . ?
C29 C28 C23 118.61(15) . . ?
C29 C28 C27 122.64(16) . . ?
C28 C29 H29 117.7(11) . . ?
C30 C29 C28 121.45(15) . . ?
C30 C29 H29 120.9(11) . . ?
C21 C30 C32 119.54(14) . . ?
C29 C30 C21 119.75(15) . . ?
C29 C30 C32 120.69(14) . . ?
C2 C31 C12 113.15(13) . . ?
C2 C31 H31 106.1(10) . . ?
C12 C31 H31 103.8(10) . . ?
C21 C31 C2 112.66(13) . . ?
C21 C31 C12 115.88(13) . . ?
C21 C31 H31 103.8(10) . . ?
C4 C32 H32 105.2(12) . . ?
C14 C32 C4 113.56(13) . . ?
C14 C32 H32 103.9(12) . . ?
C30 C32 C4 114.55(14) . . ?
C30 C32 C14 113.59(13) . . ?
C30 C32 H32 104.6(12) . . ?
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
O1 H1 0.84(3) . ?
O1 C1 1.377(2) . ?
O2 H2 0.91(3) . ?
O2 C5 1.380(2) . ?
O3 H3 0.94(3) . ?
O3 C11 1.371(2) . ?
O4 H4 0.82(3) . ?
O4 C15 1.3863(19) . ?
C1 C2 1.381(2) . ?
C1 C10 1.411(2) . ?
C2 C3 1.438(2) . ?
C2 C31 1.522(2) . ?
C3 C4 1.434(2) . ?
C3 C8 1.434(2) . ?
C4 C5 1.389(2) . ?
C4 C32 1.526(2) . ?
C5 C6 1.401(3) . ?
C6 H6 0.90(2) . ?
C6 C7 1.358(3) . ?
C7 H7 0.96(2) . ?
C7 C8 1.411(2) . ?
C8 C9 1.411(3) . ?
C9 H9 0.92(2) . ?
C9 C10 1.360(3) . ?
C10 H10 0.97(2) . ?
C11 C12 1.387(2) . ?
C11 C20 1.410(3) . ?
C12 C13 1.440(2) . ?
C12 C31 1.529(2) . ?
C13 C14 1.437(2) . ?
C13 C18 1.435(2) . ?
C14 C15 1.388(2) . ?
C14 C32 1.525(2) . ?
C15 C16 1.401(2) . ?
C16 H16 0.91(2) . ?
C16 C17 1.358(2) . ?
C17 H17 0.98(2) . ?
C17 C18 1.413(2) . ?
C18 C19 1.417(2) . ?
C19 H19 0.96(2) . ?
C19 C20 1.352(3) . ?
C20 H20 1.01(2) . ?
C21 C22 1.371(2) . ?
C21 C30 1.410(2) . ?
C21 C31 1.507(2) . ?
C22 H22 0.987(19) . ?
C22 C23 1.415(2) . ?
C23 C24 1.420(2) . ?
C23 C28 1.421(2) . ?
C24 H24 0.96(2) . ?
C24 C25 1.364(3) . ?
C25 H25 0.99(2) . ?
C25 C26 1.414(3) . ?
C26 H26 0.94(3) . ?
C26 C27 1.365(3) . ?
C27 H27 1.01(2) . ?
C27 C28 1.423(2) . ?
C28 C29 1.417(2) . ?
C29 H29 1.00(2) . ?
C29 C30 1.374(2) . ?
C30 C32 1.510(2) . ?
C31 H31 0.993(18) . ?
C32 H32 0.93(2) . ?
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
O1 H1 O4 0.84(3) 1.85(3) 2.6925(18) 174(3) 1_455 yes
O3 H3 O1 0.94(3) 1.87(3) 2.7854(19) 163(3) . yes
O4 H4 O2 0.82(3) 1.86(3) 2.6776(19) 177(3) . yes
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
_geom_torsion_publ_flag
O1 C1 C2 C3 178.81(14) . . . . ?
O1 C1 C2 C31 -1.6(2) . . . . ?
O1 C1 C10 C9 -177.66(16) . . . . ?
O2 C5 C6 C7 -178.70(16) . . . . ?
O3 C11 C12 C13 -175.18(16) . . . . ?
O3 C11 C12 C31 5.8(3) . . . . ?
O3 C11 C20 C19 178.34(17) . . . . ?
O4 C15 C16 C17 -176.27(15) . . . . ?
C1 C2 C3 C4 178.59(15) . . . . ?
C1 C2 C3 C8 -1.8(2) . . . . ?
C1 C2 C31 C12 104.65(17) . . . . ?
C1 C2 C31 C21 -121.48(16) . . . . ?
C2 C1 C10 C9 1.6(3) . . . . ?
C2 C3 C4 C5 174.94(16) . . . . ?
C2 C3 C4 C32 -6.1(3) . . . . ?
C2 C3 C8 C7 -176.87(16) . . . . ?
C2 C3 C8 C9 3.0(2) . . . . ?
C3 C2 C31 C12 -75.7(2) . . . . ?
C3 C2 C31 C21 58.1(2) . . . . ?
C3 C4 C5 O2 -177.31(14) . . . . ?
C3 C4 C5 C6 2.8(3) . . . . ?
C3 C4 C32 C14 86.06(19) . . . . ?
C3 C4 C32 C30 -46.7(2) . . . . ?
C3 C8 C9 C10 -1.9(3) . . . . ?
C4 C3 C8 C7 2.7(2) . . . . ?
C4 C3 C8 C9 -177.42(16) . . . . ?
C4 C5 C6 C7 1.1(3) . . . . ?
C5 C4 C32 C14 -95.01(17) . . . . ?
C5 C4 C32 C30 132.20(16) . . . . ?
C5 C6 C7 C8 -3.2(3) . . . . ?
C6 C7 C8 C3 1.2(3) . . . . ?
C6 C7 C8 C9 -178.60(17) . . . . ?
C7 C8 C9 C10 177.93(17) . . . . ?
C8 C3 C4 C5 -4.6(2) . . . . ?
C8 C3 C4 C32 174.27(15) . . . . ?
C8 C9 C10 C1 -0.4(3) . . . . ?
C10 C1 C2 C3 -0.4(3) . . . . ?
C10 C1 C2 C31 179.21(15) . . . . ?
C11 C12 C13 C14 172.71(16) . . . . ?
C11 C12 C13 C18 -4.9(2) . . . . ?
C11 C12 C31 C2 -93.82(17) . . . . ?
C11 C12 C31 C21 133.87(16) . . . . ?
C12 C11 C20 C19 -2.6(3) . . . . ?
C12 C13 C14 C15 -176.88(15) . . . . ?
C12 C13 C14 C32 0.6(2) . . . . ?
C12 C13 C18 C17 -179.53(15) . . . . ?
C12 C13 C18 C19 1.1(2) . . . . ?
C13 C12 C31 C2 87.19(19) . . . . ?
C13 C12 C31 C21 -45.1(2) . . . . ?
C13 C14 C15 O4 176.05(14) . . . . ?
C13 C14 C15 C16 -4.1(2) . . . . ?
C13 C14 C32 C4 -76.23(19) . . . . ?
C13 C14 C32 C30 57.0(2) . . . . ?
C13 C18 C19 C20 2.2(3) . . . . ?
C14 C13 C18 C17 2.7(2) . . . . ?
C14 C13 C18 C19 -176.71(15) . . . . ?
C14 C15 C16 C17 3.9(3) . . . . ?
C15 C14 C32 C4 101.31(17) . . . . ?
C15 C14 C32 C30 -125.44(16) . . . . ?
C15 C16 C17 C18 -0.2(3) . . . . ?
C16 C17 C18 C13 -3.0(3) . . . . ?
C16 C17 C18 C19 176.37(16) . . . . ?
C17 C18 C19 C20 -177.15(17) . . . . ?
C18 C13 C14 C15 0.8(2) . . . . ?
C18 C13 C14 C32 178.31(14) . . . . ?
C18 C19 C20 C11 -1.6(3) . . . . ?
C20 C11 C12 C13 5.8(3) . . . . ?
C20 C11 C12 C31 -173.21(16) . . . . ?
C21 C22 C23 C24 -179.62(16) . . . . ?
C21 C22 C23 C28 0.3(2) . . . . ?
C21 C30 C32 C4 67.25(19) . . . . ?
C21 C30 C32 C14 -65.5(2) . . . . ?
C22 C21 C30 C29 -0.2(2) . . . . ?
C22 C21 C30 C32 178.53(15) . . . . ?
C22 C21 C31 C2 111.32(17) . . . . ?
C22 C21 C31 C12 -116.15(17) . . . . ?
C22 C23 C24 C25 178.97(17) . . . . ?
C22 C23 C28 C27 -178.95(16) . . . . ?
C22 C23 C28 C29 0.2(2) . . . . ?
C23 C24 C25 C26 0.1(3) . . . . ?
C23 C28 C29 C30 -0.6(2) . . . . ?
C24 C23 C28 C27 0.9(2) . . . . ?
C24 C23 C28 C29 -179.96(16) . . . . ?
C24 C25 C26 C27 0.7(3) . . . . ?
C25 C26 C27 C28 -0.7(3) . . . . ?
C26 C27 C28 C23 -0.2(3) . . . . ?
C26 C27 C28 C29 -179.22(17) . . . . ?
C27 C28 C29 C30 178.44(16) . . . . ?
C28 C23 C24 C25 -0.9(3) . . . . ?
C28 C29 C30 C21 0.7(2) . . . . ?
C28 C29 C30 C32 -178.09(15) . . . . ?
C29 C30 C32 C4 -113.99(17) . . . . ?
C29 C30 C32 C14 113.23(17) . . . . ?
C30 C21 C22 C23 -0.2(2) . . . . ?
C30 C21 C31 C2 -66.16(19) . . . . ?
C30 C21 C31 C12 66.37(19) . . . . ?
C31 C2 C3 C4 -1.0(3) . . . . ?
C31 C2 C3 C8 178.59(14) . . . . ?
C31 C12 C13 C14 -8.3(3) . . . . ?
C31 C12 C13 C18 174.03(15) . . . . ?
C31 C21 C22 C23 -177.69(15) . . . . ?
C31 C21 C30 C29 177.26(15) . . . . ?
C31 C21 C30 C32 -4.0(2) . . . . ?
C32 C4 C5 O2 3.7(2) . . . . ?
C32 C4 C5 C6 -176.17(16) . . . . ?
C32 C14 C15 O4 -1.6(2) . . . . ?
C32 C14 C15 C16 178.22(15) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0009 0.9993 -0.0005 0.0630 0.0048 0.0059
-0.0009 -0.9993 0.0005 -0.0630 -0.0048 -0.0059
-0.0002 -0.0002 -0.9992 -0.0179 -0.0007 0.0590
0.9994 -0.0008 -0.9994 -0.0037 0.0678 0.0398
-0.9994 0.0008 0.9994 0.0037 -0.0678 -0.0398
-1.9983 1.0005 -0.0000 0.0347 -0.1324 0.0444
1.9983 -1.0005 0.0000 -0.0347 0.1324 -0.0444
0.9991 -0.9996 1.9986 -0.0130 0.0653 -0.1432
-0.9991 0.9996 -1.9986 0.0130 -0.0653 0.1432
-0.9992 0.0010 1.9986 0.0216 -0.0671 -0.0988
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.018 0.000 0.000 404.4 51.1 '3 MeOH'
