#------------------------------------------------------------------------------
#$Date: 2020-08-22 02:42:33 +0300 (Sat, 22 Aug 2020) $
#$Revision: 255559 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/87/4038708.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_4038708
loop_
_publ_author_name
'Wrona-Piotrowicz, Anna'
'Makal, Anna'
'Zakrzewski, Janusz'
_publ_section_title
;
 Triflic Acid-Promoted Adamantylation and tert-Butylation of
 Pyrene: Fluorescent Properties of Pyrene-Decorated Adamantanes and a
 Channeled Crystal Structure of 1,3,5-Tris(pyren-2-yl)adamantane.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01060
_journal_year                    2020
_chemical_formula_moiety         'C58 H40'
_chemical_formula_sum            'C58 H40'
_chemical_formula_weight         736.90
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-22
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                117.369(5)
_cell_angle_beta                 91.410(4)
_cell_angle_gamma                93.755(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0569(4)
_cell_length_b                   17.1074(9)
_cell_length_c                   17.4187(9)
_cell_measurement_reflns_used    5590
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      2.8070
_cell_volume                     2123.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width tₑₓₚ ω θ κ φ Frames -------------------------------------------------------------------------- 1 ω -117.00 -10.00 1.00 1.00 -- -41.28 -77.00-150.00 107 2 ω -117.00 -17.00 1.00 1.00 -- -41.28 -77.00 -60.00 100 3 ω -93.00 -66.00 1.00 1.00 -- -41.28 -37.00 90.00 27 4 ω -59.00 -31.00 1.00 1.00 -- -41.28 -37.00 90.00 28 5 ω 1.00 80.00 1.00 1.00 -- 41.28 -99.00 60.00 79 6 ω 30.00 128.00 1.00 2.00 -- 106.16 -30.00 0.00 98 7 ω 133.00 174.00 1.00 2.00 -- 106.16 30.00-180.00 41 8 ω 47.00 119.00 1.00 2.00 -- 106.16 -30.00-180.00 72 9 ω 86.00 114.00 1.00 2.00 -- 106.16 30.00-180.00 28 10 ω 75.00 117.00 1.00 2.00 -- 106.16-125.00 30.00 42 11 ω 46.00 117.00 1.00 2.00 -- 106.16-125.00-150.00 71 12 ω 64.00 139.00 1.00 2.00 -- 106.16 -77.00-150.00 75 13 ω 126.00 170.00 1.00 2.00 -- 106.16 45.00-120.00 44 14 ω 80.00 121.00 1.00 2.00 -- 106.16 45.00-120.00 41 15 ω 34.00 61.00 1.00 2.00 -- 106.16-125.00 30.00 27 16 ω 26.00 101.00 1.00 2.00 -- 106.16 -94.00-150.00 75 17 ω 33.00 131.00 1.00 2.00 -- 106.16 -77.00 30.00 98 18 ω 105.00 178.00 1.00 2.00 -- 106.16 30.00 -30.00 73 19 ω 32.00 59.00 1.00 2.00 -- 106.16 -77.00 0.00 27'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0552445000
_diffrn_orient_matrix_UB_12      -0.0708290000
_diffrn_orient_matrix_UB_13      -0.0928270000
_diffrn_orient_matrix_UB_21      0.1378914000
_diffrn_orient_matrix_UB_22      0.0386252000
_diffrn_orient_matrix_UB_23      -0.0357037000
_diffrn_orient_matrix_UB_31      0.1216296000
_diffrn_orient_matrix_UB_32      -0.0620602000
_diffrn_orient_matrix_UB_33      0.0080395000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.803
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over 			a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0811
_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)+(0.0582P)²+4.7010P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6195
_reflns_number_total             8342
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c01060_si_002.cif
_cod_data_source_block           wpa603_mask
_cod_database_code               4038708
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C59 H41 Cl3'
_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   0.962
_shelx_estimated_absorpt_t_min   0.842
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C21(H21),
 C22(H22), C24(H24), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39),
  C41(H41), C42(H42), C44(H44), C52(H52), C54(H54), C55(H55), C57(H57),
 C58(H58), C59(H59), C61(H61), C62(H62), C64(H64)
;
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.836
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
C1 C 0.9707(4) 0.31364(19) 0.9355(2) 0.0245(6) Uani 1 1 d . . . . .
C2 C 1.0535(4) 0.23489(19) 0.9374(2) 0.0243(6) Uani 1 1 d . . . . .
H2A H 1.1286 0.2567 0.9887 0.029 Uiso 1 1 calc R . . . .
H2B H 0.9680 0.1941 0.9407 0.029 Uiso 1 1 calc R . . . .
C3 C 1.1518(4) 0.18529(19) 0.8556(2) 0.0244(6) Uani 1 1 d . . . . .
C4 C 1.0288(4) 0.15111(19) 0.7752(2) 0.0248(6) Uani 1 1 d . . . . .
H4A H 0.9423 0.1105 0.7781 0.030 Uiso 1 1 calc R . . . .
H4B H 1.0876 0.1191 0.7233 0.030 Uiso 1 1 calc R . . . .
C5 C 0.9479(4) 0.2282(2) 0.7698(2) 0.0252(6) Uani 1 1 d . . . . .
C6 C 0.8542(4) 0.2769(2) 0.8531(2) 0.0247(6) Uani 1 1 d . . . . .
H6A H 0.8014 0.3252 0.8508 0.030 Uiso 1 1 calc R . . . .
H6B H 0.7672 0.2364 0.8558 0.030 Uiso 1 1 calc R . . . .
C7 C 1.1074(4) 0.3775(2) 0.9284(2) 0.0278(7) Uani 1 1 d . . . . .
H7A H 1.0564 0.4258 0.9250 0.033 Uiso 1 1 calc R . . . .
H7B H 1.1831 0.4022 0.9796 0.033 Uiso 1 1 calc R . . . .
C8 C 1.2851(4) 0.2532(2) 0.8538(2) 0.0257(6) Uani 1 1 d . . . . .
H8A H 1.3587 0.2765 0.9058 0.031 Uiso 1 1 calc R . . . .
H8B H 1.3515 0.2243 0.8043 0.031 Uiso 1 1 calc R . . . .
C9 C 1.0875(4) 0.2926(2) 0.7667(2) 0.0274(6) Uani 1 1 d . . . . .
H9A H 1.1503 0.2620 0.7160 0.033 Uiso 1 1 calc R . . . .
H9B H 1.0389 0.3408 0.7622 0.033 Uiso 1 1 calc R . . . .
C10 C 1.2040(4) 0.3292(2) 0.8484(2) 0.0268(6) Uani 1 1 d . . . . .
H10 H 1.2912 0.3705 0.8458 0.032 Uiso 1 1 calc R . . . .
C11 C 0.8836(4) 0.36563(19) 1.0183(2) 0.0243(6) Uani 1 1 d . . . . .
C12 C 0.9728(4) 0.3980(2) 1.0993(2) 0.0270(6) Uani 1 1 d . . . . .
H12 H 1.0794 0.3807 1.1008 0.032 Uiso 1 1 calc R . . . .
C13 C 0.9081(4) 0.4547(2) 1.1768(2) 0.0270(6) Uani 1 1 d . . . . .
C14 C 1.0017(5) 0.4906(2) 1.2584(2) 0.0376(8) Uani 1 1 d . . . . .
H14 H 1.1087 0.4740 1.2606 0.045 Uiso 1 1 calc R . . . .
C15 C 0.9369(5) 0.5489(3) 1.3333(2) 0.0408(8) Uani 1 1 d . . . . .
H15 H 1.0004 0.5711 1.3854 0.049 Uiso 1 1 calc R . . . .
C16 C 0.7723(5) 0.5764(2) 1.3326(2) 0.0368(8) Uani 1 1 d . . . . .
C17 C 0.7054(5) 0.6377(3) 1.4086(3) 0.0459(9) Uani 1 1 d . . . . .
H17 H 0.7673 0.6615 1.4613 0.055 Uiso 1 1 calc R . . . .
C18 C 0.5456(6) 0.6623(3) 1.4043(3) 0.0489(10) Uani 1 1 d . . . . .
H18 H 0.5023 0.7032 1.4547 0.059 Uiso 1 1 calc R . . . .
C19 C 0.4485(5) 0.6276(2) 1.3269(2) 0.0420(9) Uani 1 1 d . . . . .
H19 H 0.3421 0.6454 1.3260 0.050 Uiso 1 1 calc R . . . .
C20 C 0.5113(4) 0.5660(2) 1.2503(2) 0.0337(7) Uani 1 1 d . . . . .
C21 C 0.4194(4) 0.5295(2) 1.1691(2) 0.0335(7) Uani 1 1 d . . . . .
H21 H 0.3114 0.5447 1.1668 0.040 Uiso 1 1 calc R . . . .
C22 C 0.4850(4) 0.4729(2) 1.0948(2) 0.0315(7) Uani 1 1 d . . . . .
H22 H 0.4218 0.4515 1.0426 0.038 Uiso 1 1 calc R . . . .
C23 C 0.6497(4) 0.44535(19) 1.0947(2) 0.0262(6) Uani 1 1 d . . . . .
C24 C 0.7208(4) 0.38900(19) 1.0179(2) 0.0259(6) Uani 1 1 d . . . . .
H24 H 0.6580 0.3667 0.9656 0.031 Uiso 1 1 calc R . . . .
C25 C 0.7427(4) 0.47961(19) 1.1753(2) 0.0262(6) Uani 1 1 d . . . . .
C26 C 0.6757(4) 0.5403(2) 1.2528(2) 0.0307(7) Uani 1 1 d . . . . .
C31 C 1.2303(4) 0.10781(19) 0.8598(2) 0.0246(6) Uani 1 1 d . . . . .
C32 C 1.1318(4) 0.0319(2) 0.8457(2) 0.0273(6) Uani 1 1 d . . . . .
H32 H 1.0179 0.0288 0.8335 0.033 Uiso 1 1 calc R . . . .
C33 C 1.1994(4) -0.0405(2) 0.8494(2) 0.0268(6) Uani 1 1 d . . . . .
C34 C 1.0993(4) -0.1201(2) 0.8325(2) 0.0339(7) Uani 1 1 d . . . . .
H34 H 0.9862 -0.1256 0.8170 0.041 Uiso 1 1 calc R . . . .
C35 C 1.1669(4) -0.1868(2) 0.8390(3) 0.0379(8) Uani 1 1 d . . . . .
H35 H 1.0992 -0.2376 0.8274 0.046 Uiso 1 1 calc R . . . .
C36 C 1.3397(4) -0.1822(2) 0.8632(2) 0.0335(7) Uani 1 1 d . . . . .
C37 C 1.4122(5) -0.2500(3) 0.8728(3) 0.0444(9) Uani 1 1 d . . . . .
H37 H 1.3462 -0.3006 0.8637 0.053 Uiso 1 1 calc R . . . .
C38 C 1.5803(5) -0.2425(2) 0.8958(3) 0.0448(9) Uani 1 1 d . . . . .
H38 H 1.6255 -0.2883 0.9017 0.054 Uiso 1 1 calc R . . . .
C39 C 1.6819(4) -0.1685(2) 0.9102(2) 0.0356(8) Uani 1 1 d . . . . .
H39 H 1.7944 -0.1646 0.9260 0.043 Uiso 1 1 calc R . . . .
C40 C 1.6159(4) -0.0987(2) 0.9010(2) 0.0278(6) Uani 1 1 d . . . . .
C41 C 1.7156(4) -0.0190(2) 0.9175(2) 0.0296(7) Uani 1 1 d . . . . .
H41 H 1.8282 -0.0129 0.9343 0.035 Uiso 1 1 calc R . . . .
C42 C 1.6479(4) 0.0476(2) 0.9089(2) 0.0285(7) Uani 1 1 d . . . . .
H42 H 1.7157 0.0977 0.9185 0.034 Uiso 1 1 calc R . . . .
C43 C 1.4738(4) 0.0420(2) 0.8852(2) 0.0259(6) Uani 1 1 d . . . . .
C44 C 1.4023(4) 0.1115(2) 0.8784(2) 0.0256(6) Uani 1 1 d . . . . .
H44 H 1.4702 0.1610 0.8864 0.031 Uiso 1 1 calc R . . . .
C45 C 1.3725(4) -0.03483(19) 0.87036(19) 0.0243(6) Uani 1 1 d . . . . .
C46 C 1.4430(4) -0.1063(2) 0.8775(2) 0.0273(6) Uani 1 1 d . . . . .
C51 C 0.8262(4) 0.1919(2) 0.6895(2) 0.0261(6) Uani 1 1 d . . . . .
C52 C 0.6672(4) 0.1534(2) 0.6897(2) 0.0274(6) Uani 1 1 d . . . . .
H52 H 0.6394 0.1462 0.7377 0.033 Uiso 1 1 calc R . . . .
C53 C 0.5493(4) 0.1256(2) 0.6202(2) 0.0275(6) Uani 1 1 d . . . . .
C54 C 0.3829(4) 0.0907(2) 0.6217(2) 0.0324(7) Uani 1 1 d . . . . .
H54 H 0.3547 0.0810 0.6683 0.039 Uiso 1 1 calc R . . . .
C55 C 0.2669(4) 0.0717(2) 0.5572(2) 0.0350(7) Uani 1 1 d . . . . .
H55 H 0.1593 0.0514 0.5615 0.042 Uiso 1 1 calc R . . . .
C56 C 0.3049(4) 0.0817(2) 0.4823(2) 0.0346(7) Uani 1 1 d . . . . .
C57 C 0.1865(5) 0.0641(2) 0.4145(2) 0.0408(8) Uani 1 1 d . . . . .
H57 H 0.0768 0.0461 0.4181 0.049 Uiso 1 1 calc R . . . .
C58 C 0.2306(5) 0.0730(3) 0.3421(3) 0.0493(10) Uani 1 1 d . . . . .
H58 H 0.1501 0.0618 0.2983 0.059 Uiso 1 1 calc R . . . .
C59 C 0.3947(6) 0.0986(3) 0.3350(3) 0.0513(10) Uani 1 1 d . . . . .
H59 H 0.4233 0.1026 0.2855 0.062 Uiso 1 1 calc R . . . .
C60 C 0.5168(5) 0.1182(3) 0.4008(2) 0.0418(9) Uani 1 1 d . . . . .
C61 C 0.6845(5) 0.1474(3) 0.3966(2) 0.0462(9) Uani 1 1 d . . . . .
H61 H 0.7167 0.1494 0.3466 0.055 Uiso 1 1 calc R . . . .
C62 C 0.7990(5) 0.1724(3) 0.4646(2) 0.0411(8) Uani 1 1 d . . . . .
H62 H 0.9065 0.1932 0.4608 0.049 Uiso 1 1 calc R . . . .
C63 C 0.7566(4) 0.1673(2) 0.5419(2) 0.0318(7) Uani 1 1 d . . . . .
C64 C 0.8695(4) 0.1959(2) 0.6142(2) 0.0315(7) Uani 1 1 d . . . . .
H64 H 0.9766 0.2183 0.6118 0.038 Uiso 1 1 calc R . . . .
C65 C 0.5925(4) 0.1341(2) 0.5458(2) 0.0295(7) Uani 1 1 d . . . . .
C66 C 0.4716(4) 0.1106(2) 0.4757(2) 0.0318(7) Uani 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 0.0181 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 3 0.0545
0 5 -3 0.0545
5 -3 1 0.1603
-5 -3 1 0.1644
0 -5 1 0.0500
0 5 -1 0.0500
5 -3 5 0.1582
3 5 2 0.1338
-5 3 -5 0.1679
-4 -3 -3 0.1509
0 2 9 0.0509
2 -1 10 0.0871
0 -3 -8 0.0283
0 8 3 0.0455
5 4 -4 0.1686
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
C6 C1 C2 108.0(2) . . ?
C6 C1 C7 107.4(2) . . ?
C7 C1 C2 109.0(2) . . ?
C11 C1 C2 111.4(2) . . ?
C11 C1 C6 113.4(2) . . ?
C11 C1 C7 107.5(2) . . ?
C3 C2 C1 111.5(2) . . ?
C4 C3 C2 108.1(2) . . ?
C8 C3 C2 106.9(2) . . ?
C8 C3 C4 109.9(2) . . ?
C31 C3 C2 109.8(2) . . ?
C31 C3 C4 110.4(2) . . ?
C31 C3 C8 111.7(2) . . ?
C3 C4 C5 111.2(2) . . ?
C4 C5 C6 107.8(2) . . ?
C9 C5 C4 108.5(2) . . ?
C9 C5 C6 108.9(2) . . ?
C51 C5 C4 109.9(2) . . ?
C51 C5 C6 110.3(2) . . ?
C51 C5 C9 111.3(2) . . ?
C1 C6 C5 112.2(2) . . ?
C10 C7 C1 110.5(2) . . ?
C10 C8 C3 110.8(2) . . ?
C10 C9 C5 110.1(2) . . ?
C7 C10 C8 109.5(3) . . ?
C7 C10 C9 110.3(2) . . ?
C9 C10 C8 109.6(3) . . ?
C12 C11 C1 119.6(3) . . ?
C24 C11 C1 122.6(3) . . ?
C24 C11 C12 117.6(3) . . ?
C13 C12 C11 122.7(3) . . ?
C12 C13 C14 122.6(3) . . ?
C12 C13 C25 119.1(3) . . ?
C25 C13 C14 118.3(3) . . ?
C15 C14 C13 121.3(3) . . ?
C14 C15 C16 121.0(3) . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 C26 119.5(3) . . ?
C26 C16 C15 118.7(3) . . ?
C18 C17 C16 119.4(4) . . ?
C19 C18 C17 122.1(4) . . ?
C18 C19 C20 119.8(4) . . ?
C19 C20 C21 122.4(3) . . ?
C19 C20 C26 119.3(3) . . ?
C21 C20 C26 118.3(3) . . ?
C22 C21 C20 121.8(3) . . ?
C21 C22 C23 121.6(3) . . ?
C24 C23 C22 122.1(3) . . ?
C24 C23 C25 120.2(3) . . ?
C25 C23 C22 117.7(3) . . ?
C11 C24 C23 121.6(3) . . ?
C23 C25 C13 118.8(3) . . ?
C23 C25 C26 120.8(3) . . ?
C26 C25 C13 120.4(3) . . ?
C16 C26 C20 119.9(3) . . ?
C16 C26 C25 120.2(3) . . ?
C25 C26 C20 119.9(3) . . ?
C32 C31 C3 120.5(3) . . ?
C32 C31 C44 118.2(3) . . ?
C44 C31 C3 121.3(3) . . ?
C31 C32 C33 122.1(3) . . ?
C32 C33 C34 122.5(3) . . ?
C32 C33 C45 119.0(3) . . ?
C45 C33 C34 118.6(3) . . ?
C35 C34 C33 120.9(3) . . ?
C34 C35 C36 122.2(3) . . ?
C37 C36 C35 123.2(3) . . ?
C37 C36 C46 118.2(3) . . ?
C46 C36 C35 118.6(3) . . ?
C38 C37 C36 121.0(3) . . ?
C39 C38 C37 121.2(3) . . ?
C38 C39 C40 120.3(3) . . ?
C39 C40 C41 122.5(3) . . ?
C39 C40 C46 118.6(3) . . ?
C46 C40 C41 118.9(3) . . ?
C42 C41 C40 121.1(3) . . ?
C41 C42 C43 121.4(3) . . ?
C44 C43 C42 121.7(3) . . ?
C44 C43 C45 119.7(3) . . ?
C45 C43 C42 118.6(3) . . ?
C43 C44 C31 121.5(3) . . ?
C33 C45 C46 120.0(3) . . ?
C43 C45 C33 119.5(3) . . ?
C43 C45 C46 120.6(3) . . ?
C36 C46 C40 120.8(3) . . ?
C36 C46 C45 119.7(3) . . ?
C40 C46 C45 119.4(3) . . ?
C52 C51 C5 120.7(3) . . ?
C64 C51 C5 121.5(3) . . ?
C64 C51 C52 117.9(3) . . ?
C53 C52 C51 122.1(3) . . ?
C52 C53 C54 122.5(3) . . ?
C52 C53 C65 119.3(3) . . ?
C65 C53 C54 118.2(3) . . ?
C55 C54 C53 121.4(3) . . ?
C54 C55 C56 121.8(3) . . ?
C57 C56 C55 123.3(3) . . ?
C57 C56 C66 118.3(3) . . ?
C66 C56 C55 118.3(3) . . ?
C58 C57 C56 121.1(4) . . ?
C57 C58 C59 120.2(4) . . ?
C58 C59 C60 121.2(4) . . ?
C59 C60 C61 122.5(4) . . ?
C59 C60 C66 118.8(4) . . ?
C66 C60 C61 118.7(3) . . ?
C62 C61 C60 121.3(4) . . ?
C61 C62 C63 121.3(4) . . ?
C64 C63 C62 122.5(3) . . ?
C64 C63 C65 119.0(3) . . ?
C65 C63 C62 118.4(3) . . ?
C51 C64 C63 122.1(3) . . ?
C53 C65 C63 119.5(3) . . ?
C53 C65 C66 120.4(3) . . ?
C63 C65 C66 120.1(3) . . ?
C56 C66 C65 119.7(3) . . ?
C60 C66 C56 120.3(3) . . ?
C60 C66 C65 120.0(3) . . ?
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
C1 C2 1.555(4) . ?
C1 C6 1.536(4) . ?
C1 C7 1.548(4) . ?
C1 C11 1.522(4) . ?
C2 C3 1.552(4) . ?
C3 C4 1.546(4) . ?
C3 C8 1.541(4) . ?
C3 C31 1.536(4) . ?
C4 C5 1.547(4) . ?
C5 C6 1.548(4) . ?
C5 C9 1.542(4) . ?
C5 C51 1.536(4) . ?
C7 C10 1.519(5) . ?
C8 C10 1.532(4) . ?
C9 C10 1.530(4) . ?
C11 C12 1.412(4) . ?
C11 C24 1.396(4) . ?
C12 C13 1.390(5) . ?
C13 C14 1.432(5) . ?
C13 C25 1.429(4) . ?
C14 C15 1.370(5) . ?
C15 C16 1.437(5) . ?
C16 C17 1.406(5) . ?
C16 C26 1.419(5) . ?
C17 C18 1.391(6) . ?
C18 C19 1.390(6) . ?
C19 C20 1.399(5) . ?
C20 C21 1.419(5) . ?
C20 C26 1.428(5) . ?
C21 C22 1.357(5) . ?
C22 C23 1.438(4) . ?
C23 C24 1.404(4) . ?
C23 C25 1.418(4) . ?
C25 C26 1.419(5) . ?
C31 C32 1.393(4) . ?
C31 C44 1.406(4) . ?
C32 C33 1.412(4) . ?
C33 C34 1.439(4) . ?
C33 C45 1.419(4) . ?
C34 C35 1.344(5) . ?
C35 C36 1.431(5) . ?
C36 C37 1.406(5) . ?
C36 C46 1.411(4) . ?
C37 C38 1.384(5) . ?
C38 C39 1.378(5) . ?
C39 C40 1.409(5) . ?
C40 C41 1.440(4) . ?
C40 C46 1.423(4) . ?
C41 C42 1.361(4) . ?
C42 C43 1.436(4) . ?
C43 C44 1.405(4) . ?
C43 C45 1.413(4) . ?
C45 C46 1.436(4) . ?
C51 C52 1.403(4) . ?
C51 C64 1.397(4) . ?
C52 C53 1.396(4) . ?
C53 C54 1.438(4) . ?
C53 C65 1.418(5) . ?
C54 C55 1.347(5) . ?
C55 C56 1.430(5) . ?
C56 C57 1.404(5) . ?
C56 C66 1.426(5) . ?
C57 C58 1.389(6) . ?
C58 C59 1.392(6) . ?
C59 C60 1.393(5) . ?
C60 C61 1.425(6) . ?
C60 C66 1.424(5) . ?
C61 C62 1.366(5) . ?
C62 C63 1.436(5) . ?
C63 C64 1.404(5) . ?
C63 C65 1.420(5) . ?
C65 C66 1.428(4) . ?
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
C1 C2 C3 C4 -59.2(3) . . . . ?
C1 C2 C3 C8 59.0(3) . . . . ?
C1 C2 C3 C31 -179.6(2) . . . . ?
C1 C7 C10 C8 -59.4(3) . . . . ?
C1 C7 C10 C9 61.3(3) . . . . ?
C1 C11 C12 C13 172.1(3) . . . . ?
C1 C11 C24 C23 -172.6(3) . . . . ?
C2 C1 C6 C5 -58.8(3) . . . . ?
C2 C1 C7 C10 57.2(3) . . . . ?
C2 C1 C11 C12 53.6(3) . . . . ?
C2 C1 C11 C24 -131.5(3) . . . . ?
C2 C3 C4 C5 59.8(3) . . . . ?
C2 C3 C8 C10 -60.6(3) . . . . ?
C2 C3 C31 C32 73.6(4) . . . . ?
C2 C3 C31 C44 -106.0(3) . . . . ?
C3 C4 C5 C6 -59.6(3) . . . . ?
C3 C4 C5 C9 58.2(3) . . . . ?
C3 C4 C5 C51 -179.8(2) . . . . ?
C3 C8 C10 C7 62.1(3) . . . . ?
C3 C8 C10 C9 -59.0(3) . . . . ?
C3 C31 C32 C33 -179.8(3) . . . . ?
C3 C31 C44 C43 177.8(3) . . . . ?
C4 C3 C8 C10 56.4(3) . . . . ?
C4 C3 C31 C32 -45.4(4) . . . . ?
C4 C3 C31 C44 135.0(3) . . . . ?
C4 C5 C6 C1 59.5(3) . . . . ?
C4 C5 C9 C10 -60.4(3) . . . . ?
C4 C5 C51 C52 78.1(3) . . . . ?
C4 C5 C51 C64 -101.7(3) . . . . ?
C5 C9 C10 C7 -59.5(3) . . . . ?
C5 C9 C10 C8 61.2(3) . . . . ?
C5 C51 C52 C53 175.3(3) . . . . ?
C5 C51 C64 C63 -176.6(3) . . . . ?
C6 C1 C2 C3 58.4(3) . . . . ?
C6 C1 C7 C10 -59.5(3) . . . . ?
C6 C1 C11 C12 175.6(3) . . . . ?
C6 C1 C11 C24 -9.4(4) . . . . ?
C6 C5 C9 C10 56.8(3) . . . . ?
C6 C5 C51 C52 -40.6(4) . . . . ?
C6 C5 C51 C64 139.5(3) . . . . ?
C7 C1 C2 C3 -57.9(3) . . . . ?
C7 C1 C6 C5 58.7(3) . . . . ?
C7 C1 C11 C12 -65.8(3) . . . . ?
C7 C1 C11 C24 109.1(3) . . . . ?
C8 C3 C4 C5 -56.5(3) . . . . ?
C8 C3 C31 C32 -168.0(3) . . . . ?
C8 C3 C31 C44 12.5(4) . . . . ?
C9 C5 C6 C1 -58.1(3) . . . . ?
C9 C5 C51 C52 -161.7(3) . . . . ?
C9 C5 C51 C64 18.5(4) . . . . ?
C11 C1 C2 C3 -176.4(2) . . . . ?
C11 C1 C6 C5 177.3(2) . . . . ?
C11 C1 C7 C10 178.1(2) . . . . ?
C11 C12 C13 C14 -177.1(3) . . . . ?
C11 C12 C13 C25 1.8(4) . . . . ?
C12 C11 C24 C23 2.4(4) . . . . ?
C12 C13 C14 C15 177.5(3) . . . . ?
C12 C13 C25 C23 0.2(4) . . . . ?
C12 C13 C25 C26 -177.3(3) . . . . ?
C13 C14 C15 C16 -0.1(6) . . . . ?
C13 C25 C26 C16 -0.4(4) . . . . ?
C13 C25 C26 C20 178.8(3) . . . . ?
C14 C13 C25 C23 179.2(3) . . . . ?
C14 C13 C25 C26 1.7(4) . . . . ?
C14 C15 C16 C17 -178.6(4) . . . . ?
C14 C15 C16 C26 1.5(5) . . . . ?
C15 C16 C17 C18 179.7(4) . . . . ?
C15 C16 C26 C20 179.6(3) . . . . ?
C15 C16 C26 C25 -1.2(5) . . . . ?
C16 C17 C18 C19 0.5(6) . . . . ?
C17 C16 C26 C20 -0.3(5) . . . . ?
C17 C16 C26 C25 178.8(3) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C18 C19 C20 C21 -178.8(3) . . . . ?
C18 C19 C20 C26 -0.7(5) . . . . ?
C19 C20 C21 C22 176.8(3) . . . . ?
C19 C20 C26 C16 0.9(5) . . . . ?
C19 C20 C26 C25 -178.3(3) . . . . ?
C20 C21 C22 C23 1.6(5) . . . . ?
C21 C20 C26 C16 179.1(3) . . . . ?
C21 C20 C26 C25 -0.1(4) . . . . ?
C21 C22 C23 C24 -178.1(3) . . . . ?
C21 C22 C23 C25 -0.3(4) . . . . ?
C22 C23 C24 C11 177.2(3) . . . . ?
C22 C23 C25 C13 -178.7(3) . . . . ?
C22 C23 C25 C26 -1.2(4) . . . . ?
C23 C25 C26 C16 -177.8(3) . . . . ?
C23 C25 C26 C20 1.4(4) . . . . ?
C24 C11 C12 C13 -3.1(4) . . . . ?
C24 C23 C25 C13 -0.9(4) . . . . ?
C24 C23 C25 C26 176.6(3) . . . . ?
C25 C13 C14 C15 -1.4(5) . . . . ?
C25 C23 C24 C11 -0.5(4) . . . . ?
C26 C16 C17 C18 -0.3(6) . . . . ?
C26 C20 C21 C22 -1.4(5) . . . . ?
C31 C3 C4 C5 179.9(2) . . . . ?
C31 C3 C8 C10 179.3(3) . . . . ?
C31 C32 C33 C34 -178.2(3) . . . . ?
C31 C32 C33 C45 1.7(5) . . . . ?
C32 C31 C44 C43 -1.8(5) . . . . ?
C32 C33 C34 C35 -178.1(3) . . . . ?
C32 C33 C45 C43 -1.4(5) . . . . ?
C32 C33 C45 C46 177.8(3) . . . . ?
C33 C34 C35 C36 0.4(6) . . . . ?
C33 C45 C46 C36 0.3(5) . . . . ?
C33 C45 C46 C40 -178.2(3) . . . . ?
C34 C33 C45 C43 178.6(3) . . . . ?
C34 C33 C45 C46 -2.2(5) . . . . ?
C34 C35 C36 C37 178.1(4) . . . . ?
C34 C35 C36 C46 -2.3(6) . . . . ?
C35 C36 C37 C38 179.6(4) . . . . ?
C35 C36 C46 C40 -179.6(3) . . . . ?
C35 C36 C46 C45 2.0(5) . . . . ?
C36 C37 C38 C39 0.2(7) . . . . ?
C37 C36 C46 C40 0.0(5) . . . . ?
C37 C36 C46 C45 -178.4(3) . . . . ?
C37 C38 C39 C40 -0.5(6) . . . . ?
C38 C39 C40 C41 178.3(4) . . . . ?
C38 C39 C40 C46 0.5(5) . . . . ?
C39 C40 C41 C42 -179.4(3) . . . . ?
C39 C40 C46 C36 -0.3(5) . . . . ?
C39 C40 C46 C45 178.2(3) . . . . ?
C40 C41 C42 C43 1.6(5) . . . . ?
C41 C40 C46 C36 -178.2(3) . . . . ?
C41 C40 C46 C45 0.3(5) . . . . ?
C41 C42 C43 C44 178.3(3) . . . . ?
C41 C42 C43 C45 -0.3(5) . . . . ?
C42 C43 C44 C31 -176.5(3) . . . . ?
C42 C43 C45 C33 178.2(3) . . . . ?
C42 C43 C45 C46 -1.0(4) . . . . ?
C43 C45 C46 C36 179.5(3) . . . . ?
C43 C45 C46 C40 1.0(5) . . . . ?
C44 C31 C32 C33 -0.2(5) . . . . ?
C44 C43 C45 C33 -0.5(5) . . . . ?
C44 C43 C45 C46 -179.6(3) . . . . ?
C45 C33 C34 C35 1.9(5) . . . . ?
C45 C43 C44 C31 2.1(5) . . . . ?
C46 C36 C37 C38 0.0(6) . . . . ?
C46 C40 C41 C42 -1.6(5) . . . . ?
C51 C5 C6 C1 179.5(2) . . . . ?
C51 C5 C9 C10 178.6(2) . . . . ?
C51 C52 C53 C54 -176.4(3) . . . . ?
C51 C52 C53 C65 1.9(5) . . . . ?
C52 C51 C64 C63 3.5(5) . . . . ?
C52 C53 C54 C55 174.0(3) . . . . ?
C52 C53 C65 C63 2.5(5) . . . . ?
C52 C53 C65 C66 -176.6(3) . . . . ?
C53 C54 C55 C56 2.6(5) . . . . ?
C53 C65 C66 C56 2.4(5) . . . . ?
C53 C65 C66 C60 -179.2(3) . . . . ?
C54 C53 C65 C63 -179.2(3) . . . . ?
C54 C53 C65 C66 1.7(4) . . . . ?
C54 C55 C56 C57 -178.8(3) . . . . ?
C54 C55 C56 C66 1.6(5) . . . . ?
C55 C56 C57 C58 -178.5(4) . . . . ?
C55 C56 C66 C60 177.5(3) . . . . ?
C55 C56 C66 C65 -4.1(5) . . . . ?
C56 C57 C58 C59 1.0(6) . . . . ?
C57 C56 C66 C60 -2.1(5) . . . . ?
C57 C56 C66 C65 176.3(3) . . . . ?
C57 C58 C59 C60 -1.9(7) . . . . ?
C58 C59 C60 C61 -177.9(4) . . . . ?
C58 C59 C60 C66 0.9(6) . . . . ?
C59 C60 C61 C62 175.2(4) . . . . ?
C59 C60 C66 C56 1.2(5) . . . . ?
C59 C60 C66 C65 -177.3(3) . . . . ?
C60 C61 C62 C63 2.3(6) . . . . ?
C61 C60 C66 C56 180.0(3) . . . . ?
C61 C60 C66 C65 1.5(5) . . . . ?
C61 C62 C63 C64 -177.3(4) . . . . ?
C61 C62 C63 C65 1.0(5) . . . . ?
C62 C63 C64 C51 179.0(3) . . . . ?
C62 C63 C65 C53 177.9(3) . . . . ?
C62 C63 C65 C66 -3.0(5) . . . . ?
C63 C65 C66 C56 -176.7(3) . . . . ?
C63 C65 C66 C60 1.7(5) . . . . ?
C64 C51 C52 C53 -4.8(5) . . . . ?
C64 C63 C65 C53 -3.7(5) . . . . ?
C64 C63 C65 C66 175.4(3) . . . . ?
C65 C53 C54 C55 -4.3(5) . . . . ?
C65 C63 C64 C51 0.7(5) . . . . ?
C66 C56 C57 C58 1.0(5) . . . . ?
C66 C60 C61 C62 -3.6(6) . . . . ?
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
-0.0000 -5.0000 2.9999 0.0757 -0.3002 0.3344
0.0000 5.0000 -2.9999 -0.0757 0.3002 -0.3344
5.0000 -3.0000 1.0000 -0.1566 0.5379 0.8024
-5.0000 -2.9999 0.9999 0.3959 -0.8410 -0.4139
-0.0000 -4.9999 0.9999 0.2613 -0.2288 0.3183
0.0000 4.9999 -0.9999 -0.2613 0.2288 -0.3183
5.0000 -3.0001 5.0001 -0.5279 0.3951 0.8345
3.0000 4.9998 2.0002 -0.7055 0.5354 0.0707
-5.0000 3.0001 -5.0001 0.5279 -0.3951 -0.8345
-4.0000 -2.9998 -3.0002 0.7119 -0.5603 -0.3245
0.0000 1.9997 9.0002 -0.9771 -0.2441 -0.0517
2.0000 -1.0002 10.0001 -0.9679 -0.1199 0.3857
-0.0000 -2.9998 -8.0002 0.9551 0.1698 0.1218
0.0000 7.9998 3.0002 -0.8451 0.2019 -0.4723
5.0000 4.0000 -3.9999 -0.1882 0.9868 0.3277
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 -0.047 0.500 0.500 376.2 146.0 ?
