#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:40:18 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242082 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/20/4132040.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_4132040
loop_
_publ_author_name
'Yokoi, Hiroki'
'Hiroto, Satoru'
'Shinokubo, Hiroshi'
_publ_section_title
;
 Reversible σ-Bond Formation in Bowl-Shaped π-Radical Cations: The
 Effects of Curved and Planar Structures.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4649
_journal_page_last               4655
_journal_paper_doi               10.1021/jacs.8b00798
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C128.76 H137.19 Cl14.9 N2 O2.73 Sb2'
_chemical_formula_weight         2528.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.309(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.3774(8)
_cell_length_b                   12.2907(3)
_cell_length_c                   29.9008(7)
_cell_measurement_reflns_used    11220
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.3480
_cell_measurement_theta_min      1.8350
_cell_volume                     11898.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72103
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.772
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5204
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         10424
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0644P)²+61.6386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8781
_reflns_number_total             10424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b00798_si_004.cif
_cod_data_source_block           yokoi170820d8_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C128.76 H137.19 Cl14.90 N2 O2.73 Sb2'
_cod_database_code               4132040
_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.
;
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.903
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Sb1 Sb 0.40027(2) 0.91573(2) 0.17601(2) 0.02773(5) Uani 1 1 d . U . . .
Cl0A Cl 0.34951(4) 0.87608(12) 0.12007(4) 0.0284(3) Uani 0.637(2) 1 d . U P A 1
Cl2 Cl 0.34728(4) 0.97022(14) 0.22664(5) 0.0391(4) Uani 0.637(2) 1 d . U P A 1
Cl3 Cl 0.40152(4) 1.09931(11) 0.14873(5) 0.0325(4) Uani 0.637(2) 1 d . U P A 1
Cl4 Cl 0.45398(4) 0.87118(12) 0.12637(4) 0.0283(3) Uani 0.637(2) 1 d . U P A 1
Cl5 Cl 0.45149(4) 0.96586(15) 0.23025(4) 0.0416(4) Uani 0.637(2) 1 d . U P A 1
Cl6 Cl 0.39698(3) 0.73609(8) 0.20326(3) 0.0474(2) Uani 1 1 d . U . . .
O0AA O 0.43361(6) 0.26812(16) 0.49891(6) 0.0226(5) Uani 1 1 d . . . . .
N1 N 0.39752(7) 0.25575(19) 0.42924(7) 0.0172(5) Uani 1 1 d . . . . .
C2 C 0.57775(9) 0.4571(2) 0.38496(10) 0.0227(7) Uani 1 1 d . . . . .
C3 C 0.44418(8) 0.5570(2) 0.46572(9) 0.0189(7) Uani 1 1 d . . . . .
C5 C 0.40187(8) 0.5268(2) 0.46978(8) 0.0182(6) Uani 1 1 d . . . . .
C6 C 0.32741(8) 0.5689(2) 0.45214(9) 0.0212(7) Uani 1 1 d . . . . .
C7 C 0.36905(8) 0.6050(2) 0.46672(9) 0.0181(6) Uani 1 1 d . . . . .
C8 C 0.47350(8) 0.4721(2) 0.44663(9) 0.0184(6) Uani 1 1 d . . . . .
C9 C 0.38703(8) 0.1319(2) 0.36930(9) 0.0205(7) Uani 1 1 d . . . . .
C10 C 0.29213(8) 0.3101(2) 0.39079(9) 0.0214(7) Uani 1 1 d . . . . .
C11 C 0.32118(8) 0.4584(2) 0.44037(9) 0.0195(6) Uani 1 1 d . . . . .
C12 C 0.35842(8) 0.2900(2) 0.42628(9) 0.0185(6) Uani 1 1 d . . . . .
C13 C 0.41450(8) 0.1885(2) 0.39773(9) 0.0187(6) Uani 1 1 d . . . . .
C14 C 0.42164(8) 0.7458(2) 0.47448(9) 0.0209(7) Uani 1 1 d . . . . .
C15 C 0.51233(8) 0.5001(2) 0.42985(9) 0.0198(7) Uani 1 1 d . . . . .
H15 H 0.5233 0.5703 0.4360 0.024 Uiso 1 1 calc R U . . .
C16 C 0.33040(8) 0.2518(2) 0.39510(9) 0.0199(7) Uani 1 1 d . . . . .
C17 C 0.45330(8) 0.6660(2) 0.46942(9) 0.0201(7) Uani 1 1 d . . . . .
H17 H 0.4813 0.6887 0.4686 0.024 Uiso 1 1 calc R U . . .
C18 C 0.39128(8) 0.4175(2) 0.46640(9) 0.0176(6) Uani 1 1 d . . . . .
C19 C 0.45968(8) 0.3660(2) 0.43835(9) 0.0179(6) Uani 1 1 d . . . . .
C20 C 0.38068(8) 0.7141(2) 0.47110(9) 0.0213(7) Uani 1 1 d . . . . .
H20 H 0.3598 0.7683 0.4718 0.026 Uiso 1 1 calc R U . . .
C21 C 0.34261(8) 0.1631(2) 0.36826(9) 0.0205(7) Uani 1 1 d . . . . .
C22 C 0.48039(8) 0.2921(2) 0.41016(9) 0.0181(6) Uani 1 1 d . . . . .
C23 C 0.53546(8) 0.4267(2) 0.40418(9) 0.0204(7) Uani 1 1 d . . . . .
C24 C 0.45806(8) 0.1937(2) 0.39262(9) 0.0197(7) Uani 1 1 d . . . . .
C25 C 0.51867(8) 0.3240(2) 0.39393(9) 0.0198(7) Uani 1 1 d . . . . .
H25 H 0.5338 0.2754 0.3755 0.024 Uiso 1 1 calc R U . . .
C26 C 0.42162(8) 0.3266(2) 0.46013(9) 0.0199(7) Uani 1 1 d . . . . .
C27 C 0.47438(9) 0.1166(2) 0.36376(10) 0.0238(7) Uani 1 1 d . . . . .
H27 H 0.5035 0.1113 0.3604 0.029 Uiso 1 1 calc R U . . .
C28 C 0.35352(8) 0.3874(2) 0.45070(9) 0.0186(6) Uani 1 1 d . . . . .
C29 C 0.27284(9) 0.1671(3) 0.33756(10) 0.0263(7) Uani 1 1 d . . . . .
C30 C 0.25951(9) 0.6042(2) 0.41922(10) 0.0239(7) Uani 1 1 d . . . . .
C31 C 0.29450(8) 0.6400(2) 0.44194(10) 0.0225(7) Uani 1 1 d . . . . .
H31 H 0.2963 0.7141 0.4508 0.027 Uiso 1 1 calc R U . . .
C32 C 0.26381(8) 0.2632(3) 0.36180(9) 0.0234(7) Uani 1 1 d . . . . .
H32 H 0.2375 0.2965 0.3580 0.028 Uiso 1 1 calc R U . . .
C33 C 0.25756(9) 0.4956(3) 0.40360(10) 0.0248(7) Uani 1 1 d . . . . .
H33 H 0.2343 0.4737 0.3863 0.030 Uiso 1 1 calc R U . . .
C34 C 0.43294(8) 0.8661(2) 0.48051(10) 0.0217(7) Uani 1 1 d . . . . .
C35 C 0.40043(10) 0.2196(3) 0.52379(10) 0.0279(8) Uani 1 1 d . . . . .
H35A H 0.3805 0.2759 0.5322 0.042 Uiso 1 1 calc R U . . .
H35B H 0.4116 0.1850 0.5508 0.042 Uiso 1 1 calc R U . . .
H35C H 0.3866 0.1647 0.5053 0.042 Uiso 1 1 calc R U . . .
C36 C 0.28810(8) 0.4203(2) 0.41261(10) 0.0218(7) Uani 1 1 d . . . . .
C37 C 0.44840(9) 0.0464(3) 0.33953(10) 0.0268(7) Uani 1 1 d . . . . .
H37 H 0.4604 -0.0101 0.3222 0.032 Uiso 1 1 calc R U . . .
C38 C 0.31207(9) 0.1200(3) 0.33989(10) 0.0257(7) Uani 1 1 d . . . . .
H38 H 0.3181 0.0582 0.3221 0.031 Uiso 1 1 calc R U . . .
C39 C 0.61004(9) 0.3736(3) 0.40088(12) 0.0327(8) Uani 1 1 d . . . . .
H39A H 0.6372 0.3934 0.3891 0.049 Uiso 1 1 calc R U . . .
H39B H 0.6024 0.3011 0.3900 0.049 Uiso 1 1 calc R U . . .
H39C H 0.6111 0.3732 0.4336 0.049 Uiso 1 1 calc R U . . .
C40 C 0.40555(9) 0.0570(2) 0.34008(10) 0.0241(7) Uani 1 1 d . . . . .
H40 H 0.3889 0.0138 0.3208 0.029 Uiso 1 1 calc R U . . .
C41 C 0.59221(9) 0.5690(3) 0.40057(11) 0.0296(8) Uani 1 1 d . . . . .
H41A H 0.5724 0.6243 0.3906 0.044 Uiso 1 1 calc R U . . .
H41B H 0.6194 0.5846 0.3879 0.044 Uiso 1 1 calc R U . . .
H41C H 0.5941 0.5699 0.4333 0.044 Uiso 1 1 calc R U . . .
C42 C 0.22326(9) 0.6822(3) 0.40990(11) 0.0287(8) Uani 1 1 d . . . . .
C43 C 0.23265(10) 0.7985(3) 0.42392(13) 0.0405(9) Uani 1 1 d . . . . .
H43A H 0.2384 0.8007 0.4561 0.061 Uiso 1 1 calc R U . . .
H43B H 0.2088 0.8448 0.4172 0.061 Uiso 1 1 calc R U . . .
H43C H 0.2568 0.8250 0.4075 0.061 Uiso 1 1 calc R U . . .
C44 C 0.39925(11) 0.9417(3) 0.46194(12) 0.0370(9) Uani 1 1 d . . . . .
H44A H 0.4091 1.0171 0.4628 0.055 Uiso 1 1 calc R U . . .
H44B H 0.3743 0.9349 0.4802 0.055 Uiso 1 1 calc R U . . .
H44C H 0.3928 0.9212 0.4310 0.055 Uiso 1 1 calc R U . . .
C45 C 0.23858(9) 0.1185(3) 0.30797(11) 0.0370(9) Uani 1 1 d . . . . .
C46 C 0.57484(10) 0.4560(3) 0.33377(11) 0.0360(9) Uani 1 1 d . . . . .
H46A H 0.5535 0.5073 0.3239 0.054 Uiso 1 1 calc R U . . .
H46B H 0.5677 0.3826 0.3235 0.054 Uiso 1 1 calc R U . . .
H46C H 0.6015 0.4773 0.3211 0.054 Uiso 1 1 calc R U . . .
C47 C 0.47297(11) 0.8950(3) 0.45639(14) 0.0431(10) Uani 1 1 d . . . . .
H47A H 0.4703 0.8763 0.4246 0.065 Uiso 1 1 calc R U . . .
H47B H 0.4959 0.8541 0.4697 0.065 Uiso 1 1 calc R U . . .
H47C H 0.4783 0.9732 0.4594 0.065 Uiso 1 1 calc R U . . .
C48 C 0.21274(10) 0.6825(3) 0.35956(11) 0.0389(9) Uani 1 1 d . . . . .
H48A H 0.1894 0.7315 0.3540 0.058 Uiso 1 1 calc R U . . .
H48B H 0.2054 0.6087 0.3500 0.058 Uiso 1 1 calc R U . . .
H48C H 0.2368 0.7076 0.3426 0.058 Uiso 1 1 calc R U . . .
C49 C 0.43778(12) 0.8892(3) 0.53038(11) 0.0374(9) Uani 1 1 d . . . . .
H49A H 0.4451 0.9659 0.5348 0.056 Uiso 1 1 calc R U . . .
H49B H 0.4597 0.8430 0.5428 0.056 Uiso 1 1 calc R U . . .
H49C H 0.4117 0.8736 0.5456 0.056 Uiso 1 1 calc R U . . .
C50 C 0.18608(10) 0.6423(3) 0.43673(12) 0.0383(9) Uani 1 1 d . . . . .
H50A H 0.1927 0.6449 0.4687 0.058 Uiso 1 1 calc R U . . .
H50B H 0.1795 0.5673 0.4281 0.058 Uiso 1 1 calc R U . . .
H50C H 0.1622 0.6892 0.4305 0.058 Uiso 1 1 calc R U . . .
C51 C 0.20175(10) 0.0889(3) 0.33798(13) 0.0433(10) Uani 1 1 d . . . . .
H51A H 0.1794 0.0587 0.3196 0.065 Uiso 1 1 calc R U . . .
H51B H 0.1919 0.1544 0.3533 0.065 Uiso 1 1 calc R U . . .
H51C H 0.2105 0.0349 0.3602 0.065 Uiso 1 1 calc R U . . .
C52 C 0.22471(12) 0.2034(4) 0.27324(12) 0.0564(12) Uani 1 1 d . . . . .
H52A H 0.2482 0.2237 0.2545 0.085 Uiso 1 1 calc R U . . .
H52B H 0.2143 0.2681 0.2887 0.085 Uiso 1 1 calc R U . . .
H52C H 0.2028 0.1726 0.2544 0.085 Uiso 1 1 calc R U . . .
C53 C 0.25205(12) 0.0155(4) 0.28416(15) 0.0740(13) Uani 1 1 d . . . . .
H53A H 0.2757 0.0317 0.2649 0.111 Uiso 1 1 calc R U . . .
H53B H 0.2291 -0.0123 0.2659 0.111 Uiso 1 1 calc R U . . .
H53C H 0.2600 -0.0395 0.3063 0.111 Uiso 1 1 calc R U . . .
C54 C 0.2444(3) 0.41560(16) 0.52915(14) 0.073(3) Uani 0.5 1 d D . P B -1
H54A H 0.2614 0.4197 0.5563 0.110 Uiso 0.5 1 calc R U P B -1
H54B H 0.2155 0.4307 0.5366 0.110 Uiso 0.5 1 calc R U P B -1
H54C H 0.2541 0.4694 0.5074 0.110 Uiso 0.5 1 calc R U P B -1
C59 C 0.24768(14) 0.30375(15) 0.50940(11) 0.0407(18) Uani 0.5 1 d DG . P B -1
C60 C 0.21757(15) 0.2658(3) 0.48000(13) 0.050(3) Uani 0.5 1 d DG . P B -1
H60 H 0.1945 0.3102 0.4727 0.060 Uiso 0.5 1 calc R U P B -1
C61 C 0.22125(19) 0.1628(3) 0.46122(16) 0.078(3) Uani 0.5 1 d G . P B -1
H61 H 0.2007 0.1368 0.4411 0.094 Uiso 0.5 1 calc R U P B -1
C62 C 0.2550(2) 0.0978(2) 0.4718(2) 0.071(3) Uani 0.5 1 d G . P B -1
H62 H 0.2576 0.0274 0.4590 0.085 Uiso 0.5 1 calc R U P B -1
C63 C 0.28515(18) 0.1358(3) 0.5012(2) 0.075(3) Uani 0.5 1 d G . P B -1
H63 H 0.3083 0.0914 0.5085 0.090 Uiso 0.5 1 calc R U P B -1
C64 C 0.28147(14) 0.2388(3) 0.52002(14) 0.068(3) Uani 0.5 1 d DG . P B -1
H64 H 0.3021 0.2647 0.5401 0.082 Uiso 0.5 1 calc R U P B -1
C65 C 0.0310(3) 0.7914(8) 0.2292(3) 0.108(3) Uani 0.611(5) 1 d D U P C 1
H65A H 0.0340 0.7211 0.2444 0.162 Uiso 0.611(5) 1 calc R U P C 1
H65B H 0.0125 0.7832 0.2034 0.162 Uiso 0.611(5) 1 calc R U P C 1
H65C H 0.0193 0.8446 0.2500 0.162 Uiso 0.611(5) 1 calc R U P C 1
C1T C 0.10909(15) 0.7968(4) 0.23602(15) 0.1031(14) Uani 0.611(5) 1 d DG U P C 1
H1T H 0.1069 0.7434 0.2589 0.124 Uiso 0.611(5) 1 calc R U P C 1
C2T C 0.07391(14) 0.8313(5) 0.21326(18) 0.1022(13) Uani 0.611(5) 1 d DG U P C 1
C3T C 0.0771(2) 0.9094(5) 0.17983(19) 0.1073(14) Uani 0.611(5) 1 d DG U P C 1
H3T H 0.0530 0.9330 0.1643 0.129 Uiso 0.611(5) 1 calc R U P C 1
C4T C 0.1154(2) 0.9529(5) 0.16916(18) 0.1097(14) Uani 0.611(5) 1 d G U P C 1
H4T H 0.1175 1.0063 0.1463 0.132 Uiso 0.611(5) 1 calc R U P C 1
C5T C 0.15055(19) 0.9184(5) 0.1919(2) 0.1092(14) Uani 0.611(5) 1 d G U P C 1
H5T H 0.1767 0.9482 0.1846 0.131 Uiso 0.611(5) 1 calc R U P C 1
C6T C 0.14741(14) 0.8403(5) 0.22535(19) 0.1056(14) Uani 0.611(5) 1 d G U P C 1
H6T H 0.1714 0.8167 0.2409 0.127 Uiso 0.611(5) 1 calc R U P C 1
C68 C 0.1499(3) 0.7784(9) 0.2600(3) 0.079(3) Uani 0.389(5) 1 d D U P C 2
H68A H 0.1616 0.8268 0.2829 0.119 Uiso 0.389(5) 1 calc R U P C 2
H68B H 0.1720 0.7348 0.2468 0.119 Uiso 0.389(5) 1 calc R U P C 2
H68C H 0.1295 0.7300 0.2738 0.119 Uiso 0.389(5) 1 calc R U P C 2
C7T C 0.15358(19) 0.9155(5) 0.20034(18) 0.0769(15) Uani 0.389(5) 1 d DG U P C 2
H7T H 0.1824 0.9212 0.2059 0.092 Uiso 0.389(5) 1 calc R U P C 2
C8T C 0.1298(2) 0.8433(5) 0.2251(2) 0.0737(14) Uani 0.389(5) 1 d DG U P C 2
C9T C 0.0876(2) 0.8349(7) 0.2170(3) 0.0772(15) Uani 0.389(5) 1 d DG U P C 2
H9T H 0.0714 0.7856 0.2339 0.093 Uiso 0.389(5) 1 calc R U P C 2
C10T C 0.0692(2) 0.8987(7) 0.1841(3) 0.0809(15) Uani 0.389(5) 1 d G U P C 2
H10T H 0.0404 0.8930 0.1785 0.097 Uiso 0.389(5) 1 calc R U P C 2
C11T C 0.0930(2) 0.9709(7) 0.1593(2) 0.0794(15) Uani 0.389(5) 1 d G U P C 2
H11T H 0.0804 1.0144 0.1368 0.095 Uiso 0.389(5) 1 calc R U P C 2
C12T C 0.1351(2) 0.9793(6) 0.1674(2) 0.0783(15) Uani 0.389(5) 1 d G U P C 2
H12T H 0.1514 1.0286 0.1505 0.094 Uiso 0.389(5) 1 calc R U P C 2
Cl11 Cl 0.44839(10) 0.9579(3) 0.22888(11) 0.0582(9) Uani 0.363(2) 1 d . U P A 3
Cl12 Cl 0.34913(8) 0.8560(2) 0.12224(9) 0.0373(7) Uani 0.363(2) 1 d . U P A 3
Cl13 Cl 0.45194(14) 0.8596(4) 0.12909(16) 0.0929(15) Uani 0.363(2) 1 d . U P A
3
Cl14 Cl 0.40288(11) 1.0855(3) 0.14577(12) 0.0709(11) Uani 0.363(2) 1 d . U P A
3
Cl15 Cl 0.34639(10) 0.9589(3) 0.22351(10) 0.0508(8) Uani 0.363(2) 1 d . U P A 3
Cl1 Cl 0.16021(9) 0.2874(2) 0.15695(8) 0.1253(9) Uani 0.7254 1 d . . P D 1
Cl7 Cl 0.07356(11) 0.2475(2) 0.14556(9) 0.1372(11) Uani 0.7254 1 d . . P D 1
C4 C 0.1154(3) 0.2533(5) 0.1822(2) 0.080(2) Uani 0.7254 1 d . . P D 1
H4B H 0.1094 0.3073 0.2059 0.096 Uiso 0.7254 1 calc R U P D 1
H4A H 0.1187 0.1815 0.1968 0.096 Uiso 0.7254 1 calc R U P D 1
C0AA C 0.0180(3) 0.1942(7) 0.2056(3) 0.0467(10) Uani 0.476(5) 1 d . U P E 4
H0AA H -0.0060 0.2441 0.2064 0.056 Uiso 0.476(5) 1 calc R U P E 4
H0AB H 0.0426 0.2360 0.2152 0.056 Uiso 0.476(5) 1 calc R U P E 4
C1AA C 0.0240(3) 0.1585(8) 0.1596(3) 0.0672(19) Uani 0.476(5) 1 d . U P E 4
H1AA H 0.0528 0.1705 0.1511 0.101 Uiso 0.476(5) 1 calc R U P E 4
H1AB H 0.0058 0.2002 0.1397 0.101 Uiso 0.476(5) 1 calc R U P E 4
H1AC H 0.0174 0.0809 0.1572 0.101 Uiso 0.476(5) 1 calc R U P E 4
C2AA C 0.0102(2) 0.0961(6) 0.2416(2) 0.0386(11) Uani 0.476(5) 1 d . U P E 4
H2AA H 0.0093 0.0274 0.2244 0.046 Uiso 0.476(5) 1 calc R U P E 4
H2AB H 0.0350 0.0925 0.2610 0.046 Uiso 0.476(5) 1 calc R U P E 4
C1 C 0.0281(3) 0.0885(11) 0.2233(4) 0.2555(12) Uani 0.3627 1 d D U P F 5
H1A H 0.0376 0.0287 0.2430 0.307 Uiso 0.3627 1 calc R U P F 5
H1B H 0.0107 0.0539 0.1999 0.307 Uiso 0.3627 1 calc R U P F 5
O3AA O 0.0000 0.1512(10) 0.2500 0.2566(12) Uani 0.7254 2 d DS TU P F 5
C4AA C 0.0643(3) 0.126(2) 0.2006(6) 0.263(2) Uani 0.3627 1 d D U P F 5
H4AA H 0.0581 0.1352 0.1687 0.395 Uiso 0.3627 1 calc . U P G 5
H4AB H 0.0865 0.0720 0.2042 0.395 Uiso 0.3627 1 calc . U P H 5
H4AC H 0.0732 0.1954 0.2133 0.395 Uiso 0.3627 1 calc . U P I 5
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'
Cl Cl 0.1484 0.1585 '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'
Sb Sb -0.5866 1.5461 '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
Cl11 Sb1 Cl14 92.32(12) . .
Cl11 Sb1 Cl13 89.68(15) . .
Cl14 Sb1 Cl13 90.22(16) . .
Cl11 Sb1 Cl15 92.11(12) . .
Cl14 Sb1 Cl15 93.62(12) . .
Cl13 Sb1 Cl15 175.69(15) . .
Cl11 Sb1 Cl6 90.30(9) . .
Cl14 Sb1 Cl6 176.80(10) . .
Cl13 Sb1 Cl6 87.95(13) . .
Cl15 Sb1 Cl6 88.12(8) . .
Cl6 Sb1 Cl4 92.00(4) . .
Cl6 Sb1 Cl0A 91.08(4) . .
Cl4 Sb1 Cl0A 91.08(4) . .
Cl6 Sb1 Cl2 90.55(5) . .
Cl4 Sb1 Cl2 177.01(6) . .
Cl0A Sb1 Cl2 90.42(5) . .
Cl6 Sb1 Cl5 92.25(5) . .
Cl4 Sb1 Cl5 88.60(4) . .
Cl0A Sb1 Cl5 176.67(6) . .
Cl2 Sb1 Cl5 89.76(5) . .
Cl6 Sb1 Cl3 178.33(4) . .
Cl4 Sb1 Cl3 89.46(5) . .
Cl0A Sb1 Cl3 88.09(5) . .
Cl2 Sb1 Cl3 88.01(5) . .
Cl5 Sb1 Cl3 88.59(6) . .
Cl11 Sb1 Cl12 175.33(11) . .
Cl14 Sb1 Cl12 92.34(11) . .
Cl13 Sb1 Cl12 90.06(13) . .
Cl15 Sb1 Cl12 87.83(10) . .
Cl6 Sb1 Cl12 85.04(7) . .
C26 O0AA C35 115.6(2) . .
C12 N1 C13 121.8(2) . .
C12 N1 C26 110.5(2) . .
C13 N1 C26 124.7(2) . .
C41 C2 C46 109.3(3) . .
C41 C2 C23 112.2(2) . .
C46 C2 C23 108.8(2) . .
C41 C2 C39 107.4(2) . .
C46 C2 C39 109.9(3) . .
C23 C2 C39 109.2(2) . .
C17 C3 C5 116.9(2) . .
C17 C3 C8 124.2(2) . .
C5 C3 C8 117.1(2) . .
C18 C5 C3 118.8(2) . .
C18 C5 C7 117.4(2) . .
C3 C5 C7 122.1(3) . .
C31 C6 C11 115.7(3) . .
C31 C6 C7 124.2(3) . .
C11 C6 C7 119.2(2) . .
C20 C7 C5 115.9(2) . .
C20 C7 C6 124.0(2) . .
C5 C7 C6 119.3(2) . .
C15 C8 C19 116.9(2) . .
C15 C8 C3 122.0(3) . .
C19 C8 C3 120.3(2) . .
C40 C9 C13 115.3(2) . .
C40 C9 C21 124.8(3) . .
C13 C9 C21 119.5(2) . .
C32 C10 C16 114.6(3) . .
C32 C10 C36 125.9(3) . .
C16 C10 C36 119.0(2) . .
C28 C11 C6 116.0(2) . .
C28 C11 C36 118.8(3) . .
C6 C11 C36 124.2(3) . .
N1 C12 C16 123.9(3) . .
N1 C12 C28 110.0(2) . .
C16 C12 C28 124.2(3) . .
N1 C13 C9 117.2(2) . .
N1 C13 C24 116.7(2) . .
C9 C13 C24 125.5(2) . .
C20 C14 C17 119.1(3) . .
C20 C14 C34 120.5(2) . .
C17 C14 C34 120.2(2) . .
C8 C15 C23 121.4(3) . .
C12 C16 C21 117.5(2) . .
C12 C16 C10 117.1(3) . .
C21 C16 C10 125.3(3) . .
C3 C17 C14 121.6(3) . .
C28 C18 C5 120.7(3) . .
C28 C18 C26 110.0(2) . .
C5 C18 C26 124.6(2) . .
C8 C19 C22 123.5(2) . .
C8 C19 C26 119.5(2) . .
C22 C19 C26 116.9(2) . .
C14 C20 C7 122.3(3) . .
C38 C21 C16 115.9(3) . .
C38 C21 C9 126.4(3) . .
C16 C21 C9 117.4(2) . .
C25 C22 C19 117.1(3) . .
C25 C22 C24 122.2(2) . .
C19 C22 C24 119.8(2) . .
C15 C23 C25 119.3(2) . .
C15 C23 C2 121.9(3) . .
C25 C23 C2 118.7(2) . .
C27 C24 C13 114.7(3) . .
C27 C24 C22 125.6(2) . .
C13 C24 C22 118.3(2) . .
C22 C25 C23 121.4(3) . .
O0AA C26 C19 107.5(2) . .
O0AA C26 N1 110.6(2) . .
C19 C26 N1 110.7(2) . .
O0AA C26 C18 116.9(2) . .
C19 C26 C18 111.1(2) . .
N1 C26 C18 99.9(2) . .
C24 C27 C37 120.8(3) . .
C18 C28 C11 125.3(3) . .
C18 C28 C12 107.9(2) . .
C11 C28 C12 120.1(2) . .
C38 C29 C32 120.6(3) . .
C38 C29 C45 121.4(3) . .
C32 C29 C45 117.9(3) . .
C31 C30 C33 119.7(3) . .
C31 C30 C42 120.7(3) . .
C33 C30 C42 119.7(3) . .
C30 C31 C6 121.5(3) . .
C10 C32 C29 122.0(3) . .
C36 C33 C30 122.5(3) . .
C49 C34 C47 109.6(3) . .
C49 C34 C14 108.5(2) . .
C47 C34 C14 111.8(2) . .
C49 C34 C44 108.1(3) . .
C47 C34 C44 107.0(3) . .
C14 C34 C44 111.9(2) . .
C33 C36 C11 115.3(3) . .
C33 C36 C10 125.5(3) . .
C11 C36 C10 118.6(2) . .
C40 C37 C27 122.0(3) . .
C29 C38 C21 120.8(3) . .
C37 C40 C9 119.8(3) . .
C43 C42 C50 108.2(3) . .
C43 C42 C30 112.6(3) . .
C50 C42 C30 107.9(3) . .
C43 C42 C48 108.0(3) . .
C50 C42 C48 110.0(3) . .
C30 C42 C48 110.0(3) . .
C53 C45 C29 112.7(3) . .
C53 C45 C52 109.4(3) . .
C29 C45 C52 109.4(3) . .
C53 C45 C51 107.6(3) . .
C29 C45 C51 108.4(3) . .
C52 C45 C51 109.2(3) . .
C60 C59 C64 120.0 . .
C60 C59 C54 120.4(4) . .
C64 C59 C54 119.6(4) . .
C59 C60 C61 120.0 . .
C60 C61 C62 120.0 . .
C63 C62 C61 120.0 . .
C62 C63 C64 120.0 . .
C63 C64 C59 120.0 . .
C2T C1T C6T 120.0 . .
C1T C2T C3T 120.0 . .
C1T C2T C65 119.1(4) . .
C3T C2T C65 120.6(4) . .
C4T C3T C2T 120.0 . .
C3T C4T C5T 120.0 . .
C4T C5T C6T 120.0 . .
C5T C6T C1T 120.0 . .
C8T C7T C12T 120.0 . .
C7T C8T C9T 120.0 . .
C7T C8T C68 118.9(5) . .
C9T C8T C68 121.1(5) . .
C10T C9T C8T 120.0 . .
C11T C10T C9T 120.0 . .
C10T C11T C12T 120.0 . .
C11T C12T C7T 120.0 . .
Cl1 C4 Cl7 113.3(4) . .
C1AA C0AA C2AA 114.9(7) . .
C2AA C2AA C0AA 121.4(7) 2 .
C4AA C1 O3AA 127.9(13) . .
C1 O3AA C1 115.1(13) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Cl11 2.273(3) .
Sb1 Cl14 2.276(4) .
Sb1 Cl13 2.295(5) .
Sb1 Cl15 2.317(3) .
Sb1 Cl6 2.3560(10) .
Sb1 Cl4 2.3571(12) .
Sb1 Cl0A 2.3886(13) .
Sb1 Cl2 2.3898(14) .
Sb1 Cl5 2.3941(15) .
Sb1 Cl3 2.3997(14) .
Sb1 Cl12 2.416(3) .
O0AA C26 1.417(3) .
O0AA C35 1.440(4) .
N1 C12 1.337(3) .
N1 C13 1.370(3) .
N1 C26 1.488(4) .
C2 C41 1.525(4) .
C2 C46 1.533(4) .
C2 C23 1.534(4) .
C2 C39 1.538(4) .
C3 C17 1.377(4) .
C3 C5 1.425(4) .
C3 C8 1.523(4) .
C5 C18 1.390(4) .
C5 C7 1.435(4) .
C6 C31 1.410(4) .
C6 C11 1.417(4) .
C6 C7 1.483(4) .
C7 C20 1.398(4) .
C8 C15 1.399(4) .
C8 C19 1.401(4) .
C9 C40 1.406(4) .
C9 C13 1.410(4) .
C9 C21 1.488(4) .
C10 C32 1.384(4) .
C10 C16 1.436(4) .
C10 C36 1.510(4) .
C11 C28 1.397(4) .
C11 C36 1.430(4) .
C12 C16 1.379(4) .
C12 C28 1.411(4) .
C13 C24 1.421(4) .
C14 C20 1.385(4) .
C14 C17 1.427(4) .
C14 C34 1.534(4) .
C15 C23 1.404(4) .
C16 C21 1.412(4) .
C18 C28 1.359(4) .
C18 C26 1.500(4) .
C19 C22 1.411(4) .
C19 C26 1.478(4) .
C21 C38 1.403(4) .
C22 C25 1.390(4) .
C22 C24 1.503(4) .
C23 C25 1.408(4) .
C24 C27 1.388(4) .
C27 C37 1.404(4) .
C29 C38 1.397(4) .
C29 C32 1.418(4) .
C29 C45 1.536(4) .
C30 C31 1.390(4) .
C30 C33 1.416(4) .
C30 C42 1.539(4) .
C33 C36 1.379(4) .
C34 C49 1.525(4) .
C34 C47 1.528(4) .
C34 C44 1.534(4) .
C37 C40 1.394(4) .
C42 C43 1.520(5) .
C42 C50 1.531(5) .
C42 C48 1.542(5) .
C45 C53 1.518(5) .
C45 C52 1.538(6) .
C45 C51 1.540(5) .
C54 C59 1.5001(18) .
C59 C60 1.3900 .
C59 C64 1.3900 .
C60 C61 1.3900 .
C61 C62 1.3900 .
C62 C63 1.3900 .
C63 C64 1.3900 .
C65 C2T 1.552(9) .
C1T C2T 1.3900 .
C1T C6T 1.3900 .
C2T C3T 1.3900 .
C3T C4T 1.3900 .
C4T C5T 1.3900 .
C5T C6T 1.3900 .
C68 C8T 1.464(11) .
C7T C8T 1.3900 .
C7T C12T 1.3900 .
C8T C9T 1.3900 .
C9T C10T 1.3900 .
C10T C11T 1.3900 .
C11T C12T 1.3900 .
Cl1 C4 1.693(8) .
Cl7 C4 1.738(8) .
C0AA C1AA 1.458(12) .
C0AA C2AA 1.635(11) .
C2AA C2AA 0.832(14) 2
C1 C4AA 1.435(9) .
C1 O3AA 1.437(8) .
O3AA C1 1.437(8) 2
