#------------------------------------------------------------------------------
#$Date: 2021-09-13 11:22:28 +0300 (Mon, 13 Sep 2021) $
#$Revision: 269108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/30/4103026.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_4103026
loop_
_publ_author_name
'Zuo Xiao'
'Yutaka Matsuo'
'Eiichi Nakamura'
_publ_contact_author             'MATSUO, Yutaka'
_publ_contact_author_email       matsuo@chem.s.u-tokyo.ac.jp
_publ_section_title
;
 Copper-Catalyzed Formal [4 + 2] Annulation between Alkyne and Fullerene
 Bromide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12234
_journal_page_last               12236
_journal_paper_doi               10.1021/ja1056399
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C98 H29 Br, 1.5(C S2)'
_chemical_formula_sum            'C99.5 H29 Br S3'
_chemical_formula_weight         1400.31
_chemical_name_systematic
;
 C60Ph4CHCC6H4BrC6H3
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-03-25T16:48:33-00:00
_cell_angle_alpha                90
_cell_angle_beta                 129.5250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.6322(6)
_cell_length_b                   17.6805(3)
_cell_length_c                   25.6132(5)
_cell_measurement_reflns_used    67912
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.88
_cell_measurement_theta_min      3.00
_cell_measurement_wavelength     1.54187
_cell_volume                     12097.3(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67912
_diffrn_reflns_theta_full        71.88
_diffrn_reflns_theta_max         71.88
_diffrn_reflns_theta_min         3
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5672
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         11668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1682P)²+36.3540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2623
_refine_ls_wR_factor_ref         0.269
_reflns_number_gt                10014
_reflns_number_total             11668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1056399_si_003.cif
_cod_data_source_block           annulation_alkyneBr
_cod_depositor_comments
;

2021-09-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C199 H58 Br2 S6'
_cod_original_formula_weight         2800.63
_cod_original_formula_moiety         'C199 H58 Br2 S6'
_cod_original_formula_units_Z            4
_cod_database_code               4103026
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.33636(13) 0.0780(2) 0.93228(17) 0.0303(7) Uani 1 1 d .
C2 C 0.37583(13) 0.0748(2) 1.01033(17) 0.0299(7) Uani 1 1 d .
C3 C 0.35361(13) 0.0516(2) 1.03541(17) 0.0300(7) Uani 1 1 d .
C4 C 0.30304(13) 0.0245(2) 0.98019(18) 0.0308(7) Uani 1 1 d .
C5 C 0.29417(13) 0.0315(2) 0.92129(18) 0.0307(7) Uani 1 1 d .
C6 C 0.35464(13) 0.0499(2) 0.89318(18) 0.0310(7) Uani 1 1 d .
C7 C 0.43175(13) 0.0793(2) 1.05030(18) 0.0314(7) Uani 1 1 d .
C8 C 0.38061(13) 0.0327(2) 1.10911(18) 0.0303(7) Uani 1 1 d .
C9 C 0.27241(13) -0.0232(2) 0.99132(18) 0.0313(7) Uani 1 1 d .
C10 C 0.25536(13) -0.0131(2) 0.85806(18) 0.0319(7) Uani 1 1 d .
C11 C 0.40830(13) 0.0189(2) 0.94224(19) 0.0328(8) Uani 1 1 d .
C12 C 0.44265(13) 0.0333(2) 1.00983(19) 0.0315(7) Uani 1 1 d .
C13 C 0.45618(13) 0.0266(2) 1.11248(18) 0.0313(7) Uani 1 1 d .
C14 C 0.43332(13) 0.0057(2) 1.13857(17) 0.0324(7) Uani 1 1 d .
C15 C 0.35792(14) -0.0411(2) 1.11043(18) 0.0322(7) Uani 1 1 d .
C16 C 0.31014(14) -0.0655(2) 1.05899(18) 0.0324(7) Uani 1 1 d .
C17 C 0.25139(13) -0.0886(2) 0.94067(19) 0.0328(8) Uani 1 1 d .
C18 C 0.24370(13) -0.0844(2) 0.88120(18) 0.0331(8) Uani 1 1 d .
C19 C 0.28340(13) -0.0504(2) 0.83626(17) 0.0316(7) Uani 1 1 d .
C20 C 0.32695(14) -0.0228(2) 0.85294(18) 0.0326(8) Uani 1 1 d .
C21 C 0.41173(14) -0.0491(2) 0.91485(19) 0.0347(8) Uani 1 1 d .
C22 C 0.48111(13) -0.0223(2) 1.05294(19) 0.0336(8) Uani 1 1 d .
C23 C 0.48901(13) -0.0263(2) 1.11566(19) 0.0334(8) Uani 1 1 d .
C24 C 0.44280(13) -0.0669(2) 1.16892(17) 0.0336(8) Uani 1 1 d .
C25 C 0.39711(14) -0.0952(2) 1.15248(18) 0.0339(8) Uani 1 1 d .
C26 C 0.30060(14) -0.1454(2) 1.04811(19) 0.0345(8) Uani 1 1 d .
C27 C 0.26486(13) -0.1589(2) 0.97569(19) 0.0343(8) Uani 1 1 d .
C28 C 0.25009(13) -0.1516(2) 0.85556(18) 0.0351(8) Uani 1 1 d .
C29 C 0.27414(13) -0.1302(2) 0.82745(18) 0.0341(8) Uani 1 1 d .
C30 C 0.36209(13) -0.0750(2) 0.86031(18) 0.0336(8) Uani 1 1 d .
C31 C 0.45022(13) -0.1009(2) 0.95505(19) 0.0345(8) Uani 1 1 d .
C32 C 0.48598(13) -0.0874(2) 1.02684(19) 0.0342(8) Uani 1 1 d .
C33 C 0.50084(13) -0.0960(2) 1.14850(18) 0.0348(8) Uani 1 1 d .
C34 C 0.47702(13) -0.1170(2) 1.17606(18) 0.0346(8) Uani 1 1 d .
C35 C 0.38748(14) -0.1731(2) 1.14428(19) 0.0349(8) Uani 1 1 d .
C36 C 0.33796(15) -0.1988(2) 1.0906(2) 0.0363(8) Uani 1 1 d .
C37 C 0.26798(14) -0.2253(2) 0.9489(2) 0.0373(8) Uani 1 1 d .
C38 C 0.26063(14) -0.2213(2) 0.8872(2) 0.0370(8) Uani 1 1 d .
C39 C 0.30673(14) -0.1808(2) 0.83141(18) 0.0366(8) Uani 1 1 d .
C40 C 0.35213(14) -0.1518(2) 0.84795(19) 0.0357(8) Uani 1 1 d .
C41 C 0.44002(14) -0.1809(2) 0.9440(2) 0.0372(8) Uani 1 1 d .
C42 C 0.49772(13) -0.1592(2) 1.0607(2) 0.0365(8) Uani 1 1 d .
C43 C 0.50510(13) -0.1640(2) 1.12053(19) 0.0365(8) Uani 1 1 d .
C44 C 0.46653(14) -0.1969(2) 1.16620(18) 0.0358(8) Uani 1 1 d .
C45 C 0.42300(15) -0.2248(2) 1.15085(19) 0.0370(8) Uani 1 1 d .
C46 C 0.34163(15) -0.2667(2) 1.0624(2) 0.0387(8) Uani 1 1 d .
C47 C 0.30767(15) -0.2798(2) 0.9933(2) 0.0379(8) Uani 1 1 d .
C48 C 0.29528(15) -0.2730(2) 0.8925(2) 0.0385(8) Uani 1 1 d .
C49 C 0.31809(15) -0.2528(2) 0.8649(2) 0.0390(8) Uani 1 1 d .
C50 C 0.39166(14) -0.2060(2) 0.89120(19) 0.0369(8) Uani 1 1 d .
C51 C 0.46916(14) -0.2177(2) 1.0095(2) 0.0378(8) Uani 1 1 d .
C52 C 0.48409(14) -0.2263(2) 1.13147(19) 0.0365(8) Uani 1 1 d .
C53 C 0.39423(15) -0.2826(2) 1.0998(2) 0.0390(8) Uani 1 1 d .
C54 C 0.32457(15) -0.3095(2) 0.9582(2) 0.0386(8) Uani 1 1 d .
C55 C 0.37066(15) -0.2683(2) 0.9021(2) 0.0385(8) Uani 1 1 d .
C56 C 0.44886(15) -0.2774(2) 1.0198(2) 0.0392(9) Uani 1 1 d .
C57 C 0.45667(15) -0.2822(2) 1.0824(2) 0.0383(8) Uani 1 1 d .
C58 C 0.41078(15) -0.3109(2) 1.0658(2) 0.0390(8) Uani 1 1 d .
C59 C 0.37508(16) -0.3248(2) 0.9939(2) 0.0404(9) Uani 1 1 d .
C60 C 0.39866(15) -0.3038(2) 0.9652(2) 0.0395(9) Uani 1 1 d .
C61 C 0.35193(13) 0.1083(2) 0.84606(18) 0.0339(8) Uani 1 1 d .
C62 C 0.33075(13) 0.1799(2) 0.83447(19) 0.0368(8) Uani 1 1 d .
C63 C 0.32661(16) 0.2271(3) 0.7871(2) 0.0451(10) Uani 1 1 d .
H63 H 0.3109 0.275 0.7772 0.054 Uiso 1 1 calc R
C64 C 0.34484(15) 0.2057(3) 0.7543(2) 0.0455(10) Uani 1 1 d .
H64 H 0.3414 0.2385 0.7222 0.055 Uiso 1 1 calc R
C65 C 0.36783(14) 0.1368(3) 0.7685(2) 0.0412(9) Uani 1 1 d .
H65 H 0.3817 0.1225 0.7478 0.049 Uiso 1 1 calc R
C66 C 0.37067(14) 0.0883(2) 0.81321(19) 0.0373(8) Uani 1 1 d .
H66 H 0.3858 0.04 0.8218 0.045 Uiso 1 1 calc R
C67 C 0.45056(13) 0.1612(2) 1.06646(19) 0.0339(8) Uani 1 1 d .
C68 C 0.44660(14) 0.2052(2) 1.0186(2) 0.0409(9) Uani 1 1 d .
H68 H 0.4343 0.1833 0.9767 0.049 Uiso 1 1 calc R
C69 C 0.46027(17) 0.2807(3) 1.0310(3) 0.0483(10) Uani 1 1 d .
H69 H 0.4575 0.3105 0.9979 0.058 Uiso 1 1 calc R
C70 C 0.47820(16) 0.3128(3) 1.0928(3) 0.0533(11) Uani 1 1 d .
H70 H 0.4878 0.3645 1.1018 0.064 Uiso 1 1 calc R
C71 C 0.48193(19) 0.2696(3) 1.1402(3) 0.0549(11) Uani 1 1 d .
H71 H 0.4938 0.2917 1.1819 0.066 Uiso 1 1 calc R
C72 C 0.46851(16) 0.1941(3) 1.1279(2) 0.0467(10) Uani 1 1 d .
H72 H 0.4715 0.1645 1.1613 0.056 Uiso 1 1 calc R
C73 C 0.38276(13) 0.0958(2) 1.15233(19) 0.0335(8) Uani 1 1 d .
C74 C 0.36748(15) 0.1692(2) 1.1291(2) 0.0413(9) Uani 1 1 d .
H74 H 0.3545 0.1817 1.0845 0.05 Uiso 1 1 calc R
C75 C 0.37095(17) 0.2249(3) 1.1703(2) 0.0471(10) Uani 1 1 d .
H75 H 0.3596 0.2747 1.1535 0.056 Uiso 1 1 calc R
C76 C 0.39097(17) 0.2074(3) 1.2360(2) 0.0458(10) Uani 1 1 d .
H76 H 0.3937 0.2454 1.2644 0.055 Uiso 1 1 calc R
C77 C 0.40708(15) 0.1341(3) 1.2603(2) 0.0411(9) Uani 1 1 d .
H77 H 0.4209 0.1222 1.3054 0.049 Uiso 1 1 calc R
C78 C 0.40292(14) 0.0783(2) 1.21882(19) 0.0365(8) Uani 1 1 d .
H78 H 0.4137 0.0282 1.2354 0.044 Uiso 1 1 calc R
C79 C 0.23192(14) 0.0225(2) 0.98521(19) 0.0346(8) Uani 1 1 d .
C80 C 0.23674(16) 0.1002(3) 0.9962(2) 0.0440(9) Uani 1 1 d .
H80 H 0.2662 0.1252 1.01 0.053 Uiso 1 1 calc R
C81 C 0.19841(17) 0.1414(3) 0.9869(2) 0.0502(10) Uani 1 1 d .
H81 H 0.2021 0.1944 0.9947 0.06 Uiso 1 1 calc R
C82 C 0.15555(18) 0.1061(3) 0.9667(2) 0.0543(12) Uani 1 1 d .
H82 H 0.1294 0.1346 0.9597 0.065 Uiso 1 1 calc R
C83 C 0.15080(19) 0.0290(3) 0.9565(3) 0.0581(13) Uani 1 1 d .
H83 H 0.1214 0.0042 0.9431 0.07 Uiso 1 1 calc R
C84 C 0.18887(16) -0.0130(3) 0.9658(2) 0.0473(10) Uani 1 1 d .
H84 H 0.1853 -0.0662 0.9588 0.057 Uiso 1 1 calc R
C85 C 0.20858(13) 0.0303(2) 0.80152(19) 0.0331(8) Uani 1 1 d .
C86 C 0.17411(15) 0.0553(3) 0.8088(2) 0.0424(9) Uani 1 1 d .
H86 H 0.1802 0.0467 0.8501 0.051 Uiso 1 1 calc R
C87 C 0.13145(16) 0.0924(3) 0.7569(2) 0.0464(10) Uani 1 1 d .
H87 H 0.1084 0.1093 0.7629 0.056 Uiso 1 1 calc R
C88 C 0.12143(16) 0.1054(2) 0.6962(2) 0.0447(9) Uani 1 1 d .
H88 H 0.0915 0.1305 0.6602 0.054 Uiso 1 1 calc R
C89 C 0.15530(17) 0.0817(3) 0.6886(2) 0.0475(10) Uani 1 1 d .
H89 H 0.1489 0.0907 0.6472 0.057 Uiso 1 1 calc R
C90 C 0.19894(16) 0.0444(2) 0.7410(2) 0.0418(9) Uani 1 1 d .
H90 H 0.2222 0.0286 0.7352 0.05 Uiso 1 1 calc R
C91 C 0.31653(13) 0.1585(2) 0.91523(18) 0.0333(8) Uani 1 1 d .
H91 H 0.3052 0.1781 0.9379 0.04 Uiso 1 1 calc R
C92 C 0.31351(14) 0.2043(2) 0.8714(2) 0.0364(8) Uani 1 1 d .
C93 C 0.29499(15) 0.2835(2) 0.8634(2) 0.0390(9) Uani 1 1 d .
C94 C 0.24691(15) 0.2970(3) 0.8404(2) 0.0417(9) Uani 1 1 d .
H94 H 0.2249 0.2558 0.8277 0.05 Uiso 1 1 calc R
C95 C 0.23084(16) 0.3712(3) 0.8359(2) 0.0432(9) Uani 1 1 d .
H95 H 0.1982 0.3805 0.8209 0.052 Uiso 1 1 calc R
C96 C 0.26254(17) 0.4298(3) 0.8532(2) 0.0442(9) Uani 1 1 d .
C97 C 0.31098(18) 0.4177(3) 0.8759(2) 0.0486(10) Uani 1 1 d .
H97 H 0.3327 0.4591 0.8878 0.058 Uiso 1 1 calc R
C98 C 0.32638(17) 0.3445(3) 0.8806(2) 0.0471(10) Uani 1 1 d .
H98 H 0.3592 0.3355 0.896 0.056 Uiso 1 1 calc R
C101 C 0.5 0.5 1 0.248(17) Uani 1 2 d S
C102 C 0.4144(5) 0.3843(7) 0.7865(7) 0.138(4) Uiso 1 1 d .
Br1 Br 0.24081(2) 0.53085(3) 0.84607(3) 0.0550(2) Uani 1 1 d .
S1 S 0.4556(2) 0.5106(3) 0.9997(3) 0.221(2) Uani 1 1 d .
S2 S 0.4204(2) 0.3887(4) 0.8492(4) 0.242(2) Uiso 1 1 d .
S3 S 0.4013(3) 0.3711(5) 0.7206(5) 0.297(4) 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_3
C91 C1 C5 104.2(3) .
C91 C1 C2 105.8(3) .
C5 C1 C2 99.9(3) .
C91 C1 C6 114.0(3) .
C5 C1 C6 115.9(3) .
C2 C1 C6 115.5(3) .
C3 C2 C7 124.8(3) .
C3 C2 C1 109.0(3) .
C7 C2 C1 124.9(3) .
C2 C3 C4 109.6(3) .
C2 C3 C8 125.1(3) .
C4 C3 C8 122.7(3) .
C5 C4 C3 109.5(3) .
C5 C4 C9 125.2(3) .
C3 C4 C9 123.4(3) .
C4 C5 C10 124.6(3) .
C4 C5 C1 109.5(3) .
C10 C5 C1 124.7(3) .
C11 C6 C20 99.4(3) .
C11 C6 C61 108.5(3) .
C20 C6 C61 109.4(3) .
C11 C6 C1 111.1(3) .
C20 C6 C1 111.0(3) .
C61 C6 C1 116.1(3) .
C2 C7 C67 112.0(3) .
C2 C7 C12 105.9(3) .
C67 C7 C12 115.9(3) .
C2 C7 C13 106.9(3) .
C67 C7 C13 115.5(3) .
C12 C7 C13 99.6(3) .
C3 C8 C15 107.2(3) .
C3 C8 C73 116.4(3) .
C15 C8 C73 113.1(3) .
C3 C8 C14 106.1(3) .
C15 C8 C14 100.9(3) .
C73 C8 C14 111.8(3) .
C4 C9 C17 105.8(3) .
C4 C9 C79 113.0(3) .
C17 C9 C79 113.5(3) .
C4 C9 C16 106.7(3) .
C17 C9 C16 101.0(3) .
C79 C9 C16 115.7(3) .
C5 C10 C85 116.0(3) .
C5 C10 C19 106.0(3) .
C85 C10 C19 113.8(3) .
C5 C10 C18 106.6(3) .
C85 C10 C18 113.2(3) .
C19 C10 C18 99.7(3) .
C12 C11 C21 120.0(3) .
C12 C11 C6 126.6(3) .
C21 C11 C6 109.4(3) .
C11 C12 C22 118.6(3) .
C11 C12 C7 124.3(3) .
C22 C12 C7 110.3(3) .
C14 C13 C23 118.6(3) .
C14 C13 C7 123.7(3) .
C23 C13 C7 110.2(3) .
C13 C14 C24 120.2(3) .
C13 C14 C8 123.3(3) .
C24 C14 C8 109.6(3) .
C16 C15 C25 119.8(4) .
C16 C15 C8 124.6(3) .
C25 C15 C8 109.3(3) .
C15 C16 C26 118.9(3) .
C15 C16 C9 124.5(3) .
C26 C16 C9 109.4(3) .
C18 C17 C27 120.0(4) .
C18 C17 C9 123.5(3) .
C27 C17 C9 109.7(3) .
C17 C18 C28 118.9(4) .
C17 C18 C10 123.7(3) .
C28 C18 C10 110.0(3) .
C20 C19 C29 119.4(3) .
C20 C19 C10 123.9(3) .
C29 C19 C10 110.4(3) .
C19 C20 C30 119.0(3) .
C19 C20 C6 126.7(3) .
C30 C20 C6 109.4(3) .
C31 C21 C30 120.1(4) .
C31 C21 C11 122.0(3) .
C30 C21 C11 108.8(3) .
C32 C22 C12 122.0(3) .
C32 C22 C23 119.7(4) .
C12 C22 C23 108.2(3) .
C33 C23 C13 121.8(3) .
C33 C23 C22 119.1(3) .
C13 C23 C22 108.7(3) .
C34 C24 C14 121.6(3) .
C34 C24 C25 120.0(4) .
C14 C24 C25 108.9(3) .
C35 C25 C15 121.5(4) .
C35 C25 C24 119.8(3) .
C15 C25 C24 109.0(3) .
C36 C26 C16 121.8(4) .
C36 C26 C27 119.8(4) .
C16 C26 C27 108.3(3) .
C37 C27 C17 121.3(3) .
C37 C27 C26 119.7(4) .
C17 C27 C26 109.3(3) .
C38 C28 C18 121.7(3) .
C38 C28 C29 119.9(4) .
C18 C28 C29 108.2(3) .
C39 C29 C19 122.1(3) .
C39 C29 C28 119.3(4) .
C19 C29 C28 108.6(3) .
C40 C30 C21 120.3(4) .
C40 C30 C20 122.0(3) .
C21 C30 C20 108.2(3) .
C21 C31 C32 118.5(3) .
C21 C31 C41 120.1(3) .
C32 C31 C41 108.5(3) .
C22 C32 C31 118.7(3) .
C22 C32 C42 120.8(3) .
C31 C32 C42 107.9(3) .
C23 C33 C34 119.0(3) .
C23 C33 C43 121.0(3) .
C34 C33 C43 107.4(3) .
C24 C34 C33 118.5(4) .
C24 C34 C44 120.1(3) .
C33 C34 C44 109.1(3) .
C25 C35 C36 118.9(3) .
C25 C35 C45 119.8(3) .
C36 C35 C45 108.7(3) .
C26 C36 C35 119.0(4) .
C26 C36 C46 120.1(4) .
C35 C36 C46 108.1(3) .
C27 C37 C38 119.0(4) .
C27 C37 C47 120.2(4) .
C38 C37 C47 108.0(3) .
C28 C38 C37 118.9(4) .
C28 C38 C48 120.7(3) .
C37 C38 C48 108.1(4) .
C29 C39 C40 118.5(4) .
C29 C39 C49 120.8(3) .
C40 C39 C49 107.8(3) .
C30 C40 C39 118.8(3) .
C30 C40 C50 119.8(4) .
C39 C40 C50 108.3(3) .
C50 C41 C31 119.7(4) .
C50 C41 C51 120.1(4) .
C31 C41 C51 108.1(3) .
C43 C42 C32 120.1(4) .
C43 C42 C51 119.7(4) .
C32 C42 C51 108.2(3) .
C42 C43 C52 120.0(4) .
C42 C43 C33 119.3(4) .
C52 C43 C33 108.3(3) .
C45 C44 C34 120.4(3) .
C45 C44 C52 120.2(4) .
C34 C44 C52 107.5(3) .
C44 C45 C53 120.5(3) .
C44 C45 C35 119.9(4) .
C53 C45 C35 107.1(3) .
C47 C46 C53 120.1(4) .
C47 C46 C36 120.3(4) .
C53 C46 C36 107.7(4) .
C46 C47 C54 120.3(4) .
C46 C47 C37 119.8(4) .
C54 C47 C37 108.1(3) .
C49 C48 C38 119.5(4) .
C49 C48 C54 119.7(4) .
C38 C48 C54 108.4(3) .
C48 C49 C39 119.8(4) .
C48 C49 C55 119.8(4) .
C39 C49 C55 108.2(3) .
C41 C50 C55 119.8(4) .
C41 C50 C40 120.0(4) .
C55 C50 C40 107.9(3) .
C56 C51 C41 120.0(4) .
C56 C51 C42 120.4(4) .
C41 C51 C42 107.3(4) .
C57 C52 C43 120.3(4) .
C57 C52 C44 119.7(3) .
C43 C52 C44 107.7(3) .
C58 C53 C45 119.6(4) .
C58 C53 C46 119.8(4) .
C45 C53 C46 108.3(3) .
C59 C54 C47 119.9(4) .
C59 C54 C48 120.5(4) .
C47 C54 C48 107.3(3) .
C60 C55 C50 120.2(4) .
C60 C55 C49 120.3(4) .
C50 C55 C49 107.8(4) .
C51 C56 C57 119.8(4) .
C51 C56 C60 120.3(4) .
C57 C56 C60 108.2(3) .
C52 C57 C56 119.8(4) .
C52 C57 C58 120.2(3) .
C56 C57 C58 107.3(4) .
C53 C58 C59 119.7(4) .
C53 C58 C57 119.8(4) .
C59 C58 C57 108.8(3) .
C54 C59 C58 120.3(4) .
C54 C59 C60 119.7(4) .
C58 C59 C60 107.5(3) .
C55 C60 C56 119.7(4) .
C55 C60 C59 120.0(4) .
C56 C60 C59 108.1(4) .
C66 C61 C62 119.0(3) .
C66 C61 C6 118.8(3) .
C62 C61 C6 122.3(3) .
C61 C62 C63 118.3(3) .
C61 C62 C92 120.2(3) .
C63 C62 C92 121.5(4) .
C64 C63 C62 121.8(4) .
C64 C63 H63 119.1 .
C62 C63 H63 119.1 .
C65 C64 C63 119.5(4) .
C65 C64 H64 120.2 .
C63 C64 H64 120.2 .
C64 C65 C66 119.6(4) .
C64 C65 H65 120.2 .
C66 C65 H65 120.2 .
C65 C66 C61 121.8(4) .
C65 C66 H66 119.1 .
C61 C66 H66 119.1 .
C68 C67 C72 119.0(4) .
C68 C67 C7 120.5(3) .
C72 C67 C7 120.3(4) .
C67 C68 C69 120.9(4) .
C67 C68 H68 119.5 .
C69 C68 H68 119.5 .
C68 C69 C70 119.4(4) .
C68 C69 H69 120.3 .
C70 C69 H69 120.3 .
C71 C70 C69 120.0(4) .
C71 C70 H70 120 .
C69 C70 H70 120 .
C70 C71 C72 120.6(5) .
C70 C71 H71 119.7 .
C72 C71 H71 119.7 .
C71 C72 C67 120.1(4) .
C71 C72 H72 119.9 .
C67 C72 H72 119.9 .
C74 C73 C78 119.2(4) .
C74 C73 C8 122.6(3) .
C78 C73 C8 118.1(3) .
C73 C74 C75 120.7(4) .
C73 C74 H74 119.6 .
C75 C74 H74 119.6 .
C76 C75 C74 119.9(4) .
C76 C75 H75 120.1 .
C74 C75 H75 120.1 .
C75 C76 C77 120.0(4) .
C75 C76 H76 120 .
C77 C76 H76 120 .
C78 C77 C76 120.2(4) .
C78 C77 H77 119.9 .
C76 C77 H77 119.9 .
C77 C78 C73 120.0(4) .
C77 C78 H78 120 .
C73 C78 H78 120 .
C84 C79 C80 118.9(4) .
C84 C79 C9 120.1(4) .
C80 C79 C9 120.9(3) .
C79 C80 C81 120.2(4) .
C79 C80 H80 119.9 .
C81 C80 H80 119.9 .
C82 C81 C80 120.6(5) .
C82 C81 H81 119.7 .
C80 C81 H81 119.7 .
C81 C82 C83 119.5(4) .
C81 C82 H82 120.3 .
C83 C82 H82 120.3 .
C82 C83 C84 120.5(5) .
C82 C83 H83 119.8 .
C84 C83 H83 119.8 .
C79 C84 C83 120.3(5) .
C79 C84 H84 119.9 .
C83 C84 H84 119.9 .
C90 C85 C86 118.4(4) .
C90 C85 C10 120.5(3) .
C86 C85 C10 121.1(3) .
C87 C86 C85 120.6(4) .
C87 C86 H86 119.7 .
C85 C86 H86 119.7 .
C86 C87 C88 121.0(4) .
C86 C87 H87 119.5 .
C88 C87 H87 119.5 .
C89 C88 C87 118.9(4) .
C89 C88 H88 120.5 .
C87 C88 H88 120.5 .
C88 C89 C90 120.7(4) .
C88 C89 H89 119.6 .
C90 C89 H89 119.6 .
C85 C90 C89 120.3(4) .
C85 C90 H90 119.8 .
C89 C90 H90 119.8 .
C92 C91 C1 126.1(3) .
C92 C91 H91 116.9 .
C1 C91 H91 116.9 .
C91 C92 C62 121.2(4) .
C91 C92 C93 118.6(3) .
C62 C92 C93 120.1(3) .
C94 C93 C98 119.1(4) .
C94 C93 C92 120.8(4) .
C98 C93 C92 120.1(3) .
C93 C94 C95 120.2(4) .
C93 C94 H94 119.9 .
C95 C94 H94 119.9 .
C96 C95 C94 119.3(4) .
C96 C95 H95 120.3 .
C94 C95 H95 120.3 .
C95 C96 C97 121.6(4) .
C95 C96 Br1 119.7(3) .
C97 C96 Br1 118.6(4) .
C98 C97 C96 118.4(4) .
C98 C97 H97 120.8 .
C96 C97 H97 120.8 .
C97 C98 C93 121.4(4) .
C97 C98 H98 119.3 .
C93 C98 H98 119.3 .
S1 C101 S1 180.000(3) 5_667
S3 C102 S2 170.1(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C91 1.518(5) .
C1 C5 1.539(5) .
C1 C2 1.546(5) .
C1 C6 1.568(4) .
C2 C3 1.342(5) .
C2 C7 1.510(5) .
C3 C4 1.465(5) .
C3 C8 1.517(5) .
C4 C5 1.340(5) .
C4 C9 1.517(5) .
C5 C10 1.511(5) .
C6 C11 1.536(5) .
C6 C20 1.542(5) .
C6 C61 1.545(5) .
C7 C67 1.532(5) .
C7 C12 1.542(5) .
C7 C13 1.551(5) .
C8 C15 1.534(5) .
C8 C73 1.540(5) .
C8 C14 1.542(5) .
C9 C17 1.532(5) .
C9 C79 1.538(5) .
C9 C16 1.546(5) .
C10 C85 1.525(5) .
C10 C19 1.542(5) .
C10 C18 1.551(5) .
C11 C12 1.362(5) .
C11 C21 1.435(5) .
C12 C22 1.445(5) .
C13 C14 1.372(5) .
C13 C23 1.434(5) .
C14 C24 1.427(6) .
C15 C16 1.373(5) .
C15 C25 1.434(5) .
C16 C26 1.436(5) .
C17 C18 1.371(5) .
C17 C27 1.427(5) .
C18 C28 1.442(6) .
C19 C20 1.369(5) .
C19 C29 1.434(6) .
C20 C30 1.440(5) .
C21 C31 1.389(6) .
C21 C30 1.435(5) .
C22 C32 1.395(5) .
C22 C23 1.449(5) .
C23 C33 1.398(6) .
C24 C34 1.395(5) .
C24 C25 1.443(5) .
C25 C35 1.400(6) .
C26 C36 1.399(5) .
C26 C27 1.452(5) .
C27 C37 1.397(6) .
C28 C38 1.389(6) .
C28 C29 1.456(5) .
C29 C39 1.392(5) .
C30 C40 1.388(6) .
C31 C32 1.440(5) .
C31 C41 1.441(6) .
C32 C42 1.442(6) .
C33 C34 1.435(5) .
C33 C43 1.454(6) .
C34 C44 1.441(6) .
C35 C36 1.427(6) .
C35 C45 1.454(5) .
C36 C46 1.449(6) .
C37 C38 1.434(5) .
C37 C47 1.457(6) .
C38 C48 1.445(6) .
C39 C40 1.437(5) .
C39 C49 1.443(6) .
C40 C50 1.445(6) .
C41 C50 1.396(6) .
C41 C51 1.449(6) .
C42 C43 1.386(5) .
C42 C51 1.456(6) .
C43 C52 1.444(6) .
C44 C45 1.384(6) .
C44 C52 1.456(5) .
C45 C53 1.446(6) .
C46 C47 1.386(6) .
C46 C53 1.447(6) .
C47 C54 1.448(5) .
C48 C49 1.401(5) .
C48 C54 1.451(6) .
C49 C55 1.445(6) .
C50 C55 1.443(6) .
C51 C56 1.384(6) .
C52 C57 1.392(6) .
C53 C58 1.406(6) .
C54 C59 1.390(6) .
C55 C60 1.397(6) .
C56 C57 1.448(6) .
C56 C60 1.450(6) .
C57 C58 1.451(6) .
C58 C59 1.443(6) .
C59 C60 1.450(5) .
C61 C66 1.396(5) .
C61 C62 1.398(6) .
C62 C63 1.403(5) .
C62 C92 1.468(5) .
C63 C64 1.386(6) .
C63 H63 0.95 .
C64 C65 1.372(6) .
C64 H64 0.95 .
C65 C66 1.383(6) .
C65 H65 0.95 .
C66 H66 0.95 .
C67 C68 1.383(6) .
C67 C72 1.399(6) .
C68 C69 1.384(6) .
C68 H68 0.95 .
C69 C70 1.400(7) .
C69 H69 0.95 .
C70 C71 1.370(8) .
C70 H70 0.95 .
C71 C72 1.382(7) .
C71 H71 0.95 .
C72 H72 0.95 .
C73 C74 1.384(6) .
C73 C78 1.404(5) .
C74 C75 1.393(6) .
C74 H74 0.95 .
C75 C76 1.385(6) .
C75 H75 0.95 .
C76 C77 1.392(6) .
C76 H76 0.95 .
C77 C78 1.389(6) .
C77 H77 0.95 .
C78 H78 0.95 .
C79 C84 1.386(6) .
C79 C80 1.390(6) .
C80 C81 1.396(6) .
C80 H80 0.95 .
C81 C82 1.372(7) .
C81 H81 0.95 .
C82 C83 1.379(8) .
C82 H82 0.95 .
C83 C84 1.395(6) .
C83 H83 0.95 .
C84 H84 0.95 .
C85 C90 1.385(5) .
C85 C86 1.393(5) .
C86 C87 1.370(6) .
C86 H86 0.95 .
C87 C88 1.381(6) .
C87 H87 0.95 .
C88 C89 1.371(6) .
C88 H88 0.95 .
C89 C90 1.392(6) .
C89 H89 0.95 .
C90 H90 0.95 .
C91 C92 1.334(5) .
C91 H91 0.95 .
C92 C93 1.499(6) .
C93 C94 1.388(5) .
C93 C98 1.390(6) .
C94 C95 1.400(6) .
C94 H94 0.95 .
C95 C96 1.362(7) .
C95 H95 0.95 .
C96 C97 1.399(6) .
C96 Br1 1.903(4) .
C97 C98 1.375(6) .
C97 H97 0.95 .
C98 H98 0.95 .
C101 S1 1.546(7) .
C101 S1 1.546(7) 5_667
C102 S3 1.462(14) .
C102 S2 1.483(13) .
