#------------------------------------------------------------------------------
#$Date: 2024-12-16 19:33:52 +0200 (Mon, 16 Dec 2024) $
#$Revision: 296876 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/75/7127539.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_7127539
loop_
_publ_author_name
'De, Sukanya'
'Jash, Moumita'
'Chowdhury, Chinmay'
_publ_section_title
;
 Palladium(ii) catalysed cascade strategy for the synthesis of
 dibenzo[5,6:7,8]cycloocta[1,2-b]indol-10-ols/-10(15H)-ones: easy access
 to 1,3,5,7-cyclooctatetraenes (COTs).
;
_journal_issue                   100
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15659
_journal_page_last               15662
_journal_paper_doi               10.1039/d0cc06538b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H25 N O4 S, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C32 H29 N O5 S'
_chemical_formula_weight         539.62
_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     iterative
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                97.243(9)
_cell_angle_beta                 100.218(5)
_cell_angle_gamma                97.968(9)
_cell_formula_units_Z            4
_cell_length_a                   8.748(3)
_cell_length_b                   14.050(5)
_cell_length_c                   22.585(8)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.13
_cell_measurement_theta_min      3.21
_cell_volume                     2673.0(16)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63419
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        62.501
_diffrn_reflns_theta_max         62.501
_diffrn_reflns_theta_min         2.012
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1525 before and 0.0880 after correction. The Ratio of minimum to maximum transmission is 0.7572. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0077(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0594P)²+2.9283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7251
_reflns_number_total             8479
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc06538b2.cif
_cod_data_source_block           su_5_22re1_0m_a
_cod_depositor_comments
;
Adding full bibliography for 7127535--7127539.cif.

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H58 N2 O10 S2'
_cod_original_formula_weight         1079.24
_cod_original_formula_moiety         '2(C30 H25 N O4 S), C4 H8 O2'
_cod_original_formula_units_Z            2
_cod_database_code               7127539
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H45), C8(H013)
2.b Secondary CH2 refined with riding coordinates:
 C39(H44A,H44B), C9(H01A,H01B), C025(H02G,H02H)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H33), C35(H36), C54(H55), C5(H00X), C49(H51), C57(H58), C50(H50),
 C55(H56), C20(H018), C14(H019), C44(H49), C47(H53), C11(H01E), C29(H01F),
 C58(H60), C2(H01H), C19(H01J), C17(H01K), C28(H01L), C13(H01M), C18(H01O),
 C48(H52), C4(H01R), C42(H47), C25(H01U), C34(H37), C43(H48), C12(H01Z),
 C26(H021), C41(H46)
2.d Idealised Me refined as rotating group:
 C52(H31A,H31B,H31C), C0aa(H01C,H01D,H01G), C59(H59A,H59B,H59C), C23(H02A,H02B,
 H02C), C30(H02D,H02E,H02F), C026(H02I,H02J,H02K)
2.e Idealised tetrahedral OH refined as rotating group:
 O6(H2), O2(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
S2 S -0.14767(9) 0.20023(6) 0.53767(4) 0.0371(2) Uani 1 1 d . . . . .
S1 S 0.34157(10) 0.65191(6) 0.94581(4) 0.0420(3) Uani 1 1 d . . . . .
O4 O -0.1764(3) 0.20880(17) 0.47447(10) 0.0415(6) Uani 1 1 d . . . . .
O2 O 0.0708(3) 0.55160(15) 0.73116(10) 0.0403(6) Uani 1 1 d . . . . .
H2 H 0.131177 0.587194 0.714916 0.060 Uiso 1 1 calc GR . . . .
O3 O -0.2707(3) 0.15517(16) 0.56378(10) 0.0412(6) Uani 1 1 d . . . . .
O8 O 0.2404(3) 0.71727(17) 0.96358(11) 0.0446(6) Uani 1 1 d . . . . .
O5 O 0.2538(3) 0.70954(18) 0.68426(11) 0.0473(6) Uani 1 1 d . . . . .
H5 H 0.296889 0.709552 0.653851 0.071 Uiso 1 1 calc GR . . . .
O1 O 0.2716(3) 0.46098(18) 0.45385(11) 0.0479(6) Uani 1 1 d . . . . .
O6 O 0.7040(3) 0.4186(2) 0.83640(12) 0.0570(7) Uani 1 1 d . . . . .
O7 O 0.3172(3) 0.55402(17) 0.95747(12) 0.0519(7) Uani 1 1 d . . . . .
N2 N -0.0919(3) 0.31501(18) 0.57543(12) 0.0338(6) Uani 1 1 d . . . . .
N1 N 0.3274(3) 0.64317(19) 0.87042(12) 0.0381(7) Uani 1 1 d . . . . .
O00D O 0.5078(3) 0.7340(2) 0.62366(13) 0.0668(8) Uani 1 1 d . . . . .
O00E O 0.6954(3) 0.8319(2) 0.59576(12) 0.0695(9) Uani 1 1 d . . . . .
C39 C -0.0782(4) 0.3354(2) 0.64107(14) 0.0330(7) Uani 1 1 d . . . . .
C35 C 0.1357(4) 0.4205(2) 0.61627(15) 0.0356(7) Uani 1 1 d . . . . .
C34 C 0.0427(4) 0.3704(2) 0.56147(15) 0.0353(7) Uani 1 1 d . . . . .
C45 C 0.1151(4) 0.4554(2) 0.72870(15) 0.0390(8) Uani 1 1 d . . . . .
H45 H 0.232640 0.463066 0.738557 0.047 Uiso 1 1 calc R . . . .
C38 C 0.0573(4) 0.3986(2) 0.66514(15) 0.0357(7) Uani 1 1 d . . . . .
C00K C 0.3374(4) 0.9368(2) 0.85825(15) 0.0387(8) Uani 1 1 d . . . . .
C44 C 0.0503(4) 0.4120(2) 0.77949(15) 0.0406(8) Uani 1 1 d . . . . .
H44A H 0.107365 0.449781 0.819127 0.049 Uiso 1 1 calc R . . . .
H44B H -0.062012 0.418904 0.775361 0.049 Uiso 1 1 calc R . . . .
C33 C 0.0798(4) 0.3803(2) 0.50484(15) 0.0381(8) Uani 1 1 d . . . . .
H33 H 0.014118 0.346687 0.467978 0.046 Uiso 1 1 calc R . . . .
C00N C 0.1852(4) 0.8752(3) 0.86109(15) 0.0402(8) Uani 1 1 d . . . . .
C00O C 0.3705(4) 0.7186(2) 0.78965(15) 0.0372(8) Uani 1 1 d . . . . .
C00P C 0.4632(4) 0.6407(2) 0.79350(15) 0.0386(8) Uani 1 1 d . . . . .
C40 C -0.2178(4) 0.3043(2) 0.66683(15) 0.0360(7) Uani 1 1 d . . . . .
C54 C 0.0173(4) 0.1430(2) 0.55458(15) 0.0353(7) Uani 1 1 d . . . . .
C00S C 0.1614(4) 0.7734(3) 0.84841(15) 0.0396(8) Uani 1 1 d . . . . .
C36 C 0.2758(4) 0.4813(2) 0.61504(16) 0.0404(8) Uani 1 1 d . . . . .
H36 H 0.341126 0.515662 0.651796 0.048 Uiso 1 1 calc R . . . .
C32 C 0.2188(4) 0.4424(2) 0.50547(16) 0.0405(8) Uani 1 1 d . . . . .
C55 C 0.1069(4) 0.1240(3) 0.51100(16) 0.0428(8) Uani 1 1 d . . . . .
H55 H 0.081142 0.142644 0.471915 0.051 Uiso 1 1 calc R . . . .
C00W C 0.4390(4) 0.5964(2) 0.84317(16) 0.0396(8) Uani 1 1 d . . . . .
C00X C 0.5654(4) 0.6061(3) 0.75725(16) 0.0432(8) Uani 1 1 d . . . . .
H00X H 0.581701 0.634173 0.722282 0.052 Uiso 1 1 calc R . . . .
C51 C -0.5002(4) 0.2946(3) 0.65828(16) 0.0451(9) Uani 1 1 d . . . . .
H51 H -0.597642 0.308303 0.638072 0.054 Uiso 1 1 calc R . . . .
C00Z C 0.5376(4) 0.7052(2) 0.97603(15) 0.0401(8) Uani 1 1 d . . . . .
C58 C 0.1838(4) 0.0715(3) 0.62505(17) 0.0452(9) Uani 1 1 d . . . . .
H58 H 0.209344 0.053086 0.664196 0.054 Uiso 1 1 calc R . . . .
C011 C 0.2900(4) 0.7198(2) 0.83605(15) 0.0377(8) Uani 1 1 d . . . . .
C50 C -0.3631(4) 0.3240(2) 0.63830(16) 0.0393(8) Uani 1 1 d . . . . .
H50 H -0.367639 0.358352 0.604537 0.047 Uiso 1 1 calc R . . . .
C013 C 0.3582(4) 0.7729(2) 0.73702(15) 0.0395(8) Uani 1 1 d . . . . .
H013 H 0.465274 0.786310 0.727089 0.047 Uiso 1 1 calc R . . . .
C56 C 0.2357(4) 0.0770(2) 0.52573(17) 0.0439(8) Uani 1 1 d . . . . .
H56 H 0.296299 0.062324 0.495823 0.053 Uiso 1 1 calc R . . . .
C41 C -0.2110(4) 0.2553(2) 0.71770(15) 0.0378(8) Uani 1 1 d . . . . .
C42 C -0.0622(4) 0.2327(2) 0.75092(15) 0.0399(8) Uani 1 1 d . . . . .
C017 C 0.2989(4) 0.8687(3) 0.74656(15) 0.0424(8) Uani 1 1 d . . . . .
H01A H 0.186319 0.855985 0.749153 0.051 Uiso 1 1 calc R . . . .
H01B H 0.307405 0.902311 0.711009 0.051 Uiso 1 1 calc R . . . .
C018 C 0.0140(4) 0.7197(3) 0.84818(16) 0.0444(9) Uani 1 1 d . . . . .
H018 H -0.001960 0.650702 0.839352 0.053 Uiso 1 1 calc R . . . .
C019 C 0.4213(4) 0.9995(2) 0.90970(16) 0.0436(8) Uani 1 1 d . . . . .
H019 H 0.382042 1.002248 0.946381 0.052 Uiso 1 1 calc R . . . .
C43 C 0.0639(4) 0.3069(3) 0.77985(15) 0.0410(8) Uani 1 1 d . . . . .
C01B C 0.3906(4) 0.9345(2) 0.80392(16) 0.0411(8) Uani 1 1 d . . . . .
C49 C -0.0480(4) 0.1356(3) 0.75567(16) 0.0458(9) Uani 1 1 d . . . . .
H49 H -0.134882 0.085604 0.738147 0.055 Uiso 1 1 calc R . . . .
C53 C -0.3525(4) 0.2262(3) 0.73661(16) 0.0441(8) Uani 1 1 d . . . . .
H53 H -0.350166 0.192179 0.770475 0.053 Uiso 1 1 calc R . . . .
C01E C 0.5299(4) 0.9943(3) 0.80276(17) 0.0451(9) Uani 1 1 d . . . . .
H01E H 0.566957 0.993571 0.765656 0.054 Uiso 1 1 calc R . . . .
C01F C 0.5865(4) 0.8008(3) 0.97092(16) 0.0445(9) Uani 1 1 d . . . . .
H01F H 0.514805 0.837836 0.951793 0.053 Uiso 1 1 calc R . . . .
C60 C 0.0560(4) 0.1173(2) 0.61172(16) 0.0439(8) Uani 1 1 d . . . . .
H60 H -0.005238 0.131194 0.641528 0.053 Uiso 1 1 calc R . . . .
C01H C 0.5143(4) 0.5206(3) 0.86071(17) 0.0447(8) Uani 1 1 d . . . . .
H01H H 0.496118 0.491210 0.895013 0.054 Uiso 1 1 calc R . . . .
C57 C 0.2770(4) 0.0515(2) 0.58236(17) 0.0409(8) Uani 1 1 d . . . . .
C01J C -0.1092(4) 0.7663(3) 0.86075(17) 0.0491(9) Uani 1 1 d . . . . .
H01J H -0.209443 0.729541 0.859923 0.059 Uiso 1 1 calc R . . . .
C01K C 0.0606(4) 0.9204(3) 0.87487(17) 0.0468(9) Uani 1 1 d . . . . .
H01K H 0.076018 0.989257 0.884669 0.056 Uiso 1 1 calc R . . . .
C01L C 0.7435(4) 0.8421(3) 0.99437(17) 0.0510(9) Uani 1 1 d . . . . .
H01L H 0.779146 0.907702 0.990730 0.061 Uiso 1 1 calc R . . . .
C01M C 0.5622(4) 1.0586(3) 0.90848(17) 0.0461(9) Uani 1 1 d . . . . .
H01M H 0.619874 1.100393 0.944129 0.055 Uiso 1 1 calc R . . . .
C01N C 0.6180(4) 0.4905(3) 0.82476(17) 0.0460(9) Uani 1 1 d . . . . .
C01O C -0.0846(4) 0.8669(3) 0.87451(17) 0.0504(9) Uani 1 1 d . . . . .
H01O H -0.168012 0.899125 0.883737 0.060 Uiso 1 1 calc R . . . .
C31 C 0.1696(5) 0.4208(3) 0.39667(17) 0.0520(9) Uani 1 1 d . . . . .
H31A H 0.217774 0.441882 0.363470 0.078 Uiso 1 1 calc GR . . . .
H31B H 0.068151 0.443428 0.395134 0.078 Uiso 1 1 calc GR . . . .
H31C H 0.153189 0.349649 0.392257 0.078 Uiso 1 1 calc GR . . . .
C52 C -0.4955(4) 0.2455(3) 0.70726(17) 0.0480(9) Uani 1 1 d . . . . .
H52 H -0.589505 0.225034 0.720965 0.058 Uiso 1 1 calc R . . . .
C01R C 0.6410(4) 0.5311(3) 0.77341(16) 0.0465(9) Uani 1 1 d . . . . .
H01R H 0.709639 0.506766 0.749226 0.056 Uiso 1 1 calc R . . . .
C01S C 0.5233(4) 0.7225(3) 0.51876(16) 0.0479(9) Uani 1 1 d . . . . .
H01C H 0.609865 0.694791 0.504775 0.072 Uiso 1 1 calc GR . . . .
H01D H 0.498443 0.775273 0.496070 0.072 Uiso 1 1 calc GR . . . .
H01G H 0.430228 0.671853 0.511878 0.072 Uiso 1 1 calc GR . . . .
C47 C 0.2159(5) 0.1832(3) 0.81276(17) 0.0538(10) Uani 1 1 d . . . . .
H47 H 0.310993 0.166519 0.833024 0.065 Uiso 1 1 calc R . . . .
C01U C 0.6415(5) 0.6504(3) 1.00352(17) 0.0534(10) Uani 1 1 d . . . . .
H01U H 0.606648 0.584143 1.006023 0.064 Uiso 1 1 calc R . . . .
C37 C 0.3175(4) 0.4906(2) 0.56006(16) 0.0415(8) Uani 1 1 d . . . . .
H37 H 0.414045 0.529920 0.558867 0.050 Uiso 1 1 calc R . . . .
C01W C 0.8485(5) 0.7882(3) 1.02308(17) 0.0576(11) Uani 1 1 d . . . . .
C48 C 0.0901(5) 0.1111(3) 0.78535(17) 0.0523(10) Uani 1 1 d . . . . .
H48 H 0.098475 0.044784 0.786907 0.063 Uiso 1 1 calc R . . . .
C01Y C 0.5706(4) 0.7611(3) 0.58436(17) 0.0462(9) Uani 1 1 d . . . . .
C01Z C 0.6165(4) 1.0553(3) 0.85463(17) 0.0470(9) Uani 1 1 d . . . . .
H01Z H 0.712787 1.094522 0.853012 0.056 Uiso 1 1 calc R . . . .
C59 C 0.4204(4) 0.0028(3) 0.59820(18) 0.0505(9) Uani 1 1 d . . . . .
H59A H 0.499894 0.046478 0.629598 0.076 Uiso 1 1 calc GR . . . .
H59B H 0.464332 -0.011786 0.561715 0.076 Uiso 1 1 calc GR . . . .
H59C H 0.389378 -0.057780 0.613509 0.076 Uiso 1 1 calc GR . . . .
C021 C 0.7944(5) 0.6921(3) 1.02699(18) 0.0612(11) Uani 1 1 d . . . . .
H021 H 0.864916 0.654542 1.046356 0.073 Uiso 1 1 calc R . . . .
C46 C 0.2023(4) 0.2804(3) 0.81049(16) 0.0486(9) Uani 1 1 d . . . . .
H46 H 0.288385 0.329709 0.830047 0.058 Uiso 1 1 calc R . . . .
C023 C 0.6941(6) 0.3759(3) 0.8901(2) 0.0679(12) Uani 1 1 d . . . . .
H02A H 0.585521 0.344430 0.887741 0.102 Uiso 1 1 calc GR . . . .
H02B H 0.725669 0.426597 0.925927 0.102 Uiso 1 1 calc GR . . . .
H02C H 0.764299 0.327349 0.893321 0.102 Uiso 1 1 calc GR . . . .
C024 C 1.0171(5) 0.8337(4) 1.0482(2) 0.0816(16) Uani 1 1 d . . . . .
H02D H 1.035950 0.899064 1.037339 0.122 Uiso 1 1 calc GR . . . .
H02E H 1.086601 0.793660 1.031020 0.122 Uiso 1 1 calc GR . . . .
H02F H 1.038625 0.837997 1.092624 0.122 Uiso 1 1 calc GR . . . .
C025 C 0.7479(6) 0.8832(5) 0.6573(2) 0.0913(18) Uani 1 1 d . . . . .
H02G H 0.791643 0.951454 0.655695 0.110 Uiso 1 1 calc R . . . .
H02H H 0.655863 0.883941 0.677197 0.110 Uiso 1 1 calc R . . . .
C026 C 0.8588(7) 0.8437(6) 0.6920(3) 0.135(3) Uani 1 1 d . . . . .
H02I H 0.954171 0.847839 0.674699 0.202 Uiso 1 1 calc GR . . . .
H02J H 0.818124 0.775394 0.692794 0.202 Uiso 1 1 calc GR . . . .
H02K H 0.884062 0.879537 0.733620 0.202 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 S2 N2 105.84(14) . . ?
O4 S2 C54 109.20(15) . . ?
O3 S2 O4 120.07(14) . . ?
O3 S2 N2 106.88(13) . . ?
O3 S2 C54 108.62(15) . . ?
N2 S2 C54 105.22(14) . . ?
O8 S1 N1 108.02(14) . . ?
O8 S1 C00Z 108.98(16) . . ?
O7 S1 O8 119.83(15) . . ?
O7 S1 N1 105.30(15) . . ?
O7 S1 C00Z 109.31(17) . . ?
N1 S1 C00Z 104.25(15) . . ?
C45 O2 H2 109.5 . . ?
C013 O5 H5 109.5 . . ?
C32 O1 C31 117.2(3) . . ?
C01N O6 C023 118.4(3) . . ?
C39 N2 S2 120.8(2) . . ?
C34 N2 S2 116.5(2) . . ?
C34 N2 C39 106.8(2) . . ?
C00W N1 S1 118.5(2) . . ?
C00W N1 C011 107.0(3) . . ?
C011 N1 S1 123.9(2) . . ?
C01Y O00E C025 118.3(3) . . ?
N2 C39 C40 118.2(3) . . ?
C38 C39 N2 108.6(3) . . ?
C38 C39 C40 131.7(3) . . ?
C34 C35 C38 108.4(3) . . ?
C34 C35 C36 119.1(3) . . ?
C36 C35 C38 132.5(3) . . ?
C35 C34 N2 107.7(3) . . ?
C33 C34 N2 129.1(3) . . ?
C33 C34 C35 123.1(3) . . ?
O2 C45 H45 108.5 . . ?
O2 C45 C38 110.0(3) . . ?
O2 C45 C44 105.0(3) . . ?
C38 C45 H45 108.5 . . ?
C38 C45 C44 116.1(3) . . ?
C44 C45 H45 108.5 . . ?
C39 C38 C35 108.4(3) . . ?
C39 C38 C45 130.2(3) . . ?
C35 C38 C45 120.5(3) . . ?
C019 C00K C00N 119.6(3) . . ?
C01B C00K C00N 120.3(3) . . ?
C01B C00K C019 120.0(3) . . ?
C45 C44 H44A 108.8 . . ?
C45 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C43 C44 C45 114.0(3) . . ?
C43 C44 H44A 108.8 . . ?
C43 C44 H44B 108.8 . . ?
C34 C33 H33 122.0 . . ?
C32 C33 C34 116.0(3) . . ?
C32 C33 H33 122.0 . . ?
C00S C00N C00K 122.3(3) . . ?
C01K C00N C00K 119.2(3) . . ?
C01K C00N C00S 118.5(3) . . ?
C00P C00O C013 121.5(3) . . ?
C011 C00O C00P 107.7(3) . . ?
C011 C00O C013 130.2(3) . . ?
C00W C00P C00O 108.8(3) . . ?
C00W C00P C00X 119.1(3) . . ?
C00X C00P C00O 132.1(3) . . ?
C50 C40 C39 117.7(3) . . ?
C50 C40 C41 119.2(3) . . ?
C41 C40 C39 123.2(3) . . ?
C55 C54 S2 120.2(3) . . ?
C60 C54 S2 119.0(2) . . ?
C60 C54 C55 120.8(3) . . ?
C00N C00S C011 121.7(3) . . ?
C018 C00S C00N 119.9(3) . . ?
C018 C00S C011 118.4(3) . . ?
C35 C36 H36 120.5 . . ?
C37 C36 C35 119.1(3) . . ?
C37 C36 H36 120.5 . . ?
O1 C32 C33 123.5(3) . . ?
O1 C32 C37 114.6(3) . . ?
C33 C32 C37 121.9(3) . . ?
C54 C55 H55 120.7 . . ?
C54 C55 C56 118.6(3) . . ?
C56 C55 H55 120.7 . . ?
C00P C00W N1 107.5(3) . . ?
C00P C00W C01H 123.4(3) . . ?
C01H C00W N1 129.1(3) . . ?
C00P C00X H00X 120.6 . . ?
C01R C00X C00P 118.8(3) . . ?
C01R C00X H00X 120.6 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C52 C51 C50 120.1(3) . . ?
C01F C00Z S1 119.2(3) . . ?
C01F C00Z C01U 121.1(4) . . ?
C01U C00Z S1 119.7(3) . . ?
C60 C58 H58 119.3 . . ?
C60 C58 C57 121.4(3) . . ?
C57 C58 H58 119.3 . . ?
N1 C011 C00S 119.6(3) . . ?
C00O C011 N1 108.9(3) . . ?
C00O C011 C00S 130.7(3) . . ?
C40 C50 H50 119.3 . . ?
C51 C50 C40 121.3(3) . . ?
C51 C50 H50 119.3 . . ?
O5 C013 C00O 108.3(3) . . ?
O5 C013 H013 107.9 . . ?
O5 C013 C017 109.0(3) . . ?
C00O C013 H013 107.9 . . ?
C00O C013 C017 115.8(3) . . ?
C017 C013 H013 107.9 . . ?
C55 C56 H56 119.2 . . ?
C57 C56 C55 121.6(3) . . ?
C57 C56 H56 119.2 . . ?
C40 C41 C42 122.6(3) . . ?
C53 C41 C40 118.0(3) . . ?
C53 C41 C42 119.4(3) . . ?
C43 C42 C41 121.3(3) . . ?
C49 C42 C41 119.5(3) . . ?
C49 C42 C43 119.2(3) . . ?
C013 C017 H01A 109.2 . . ?
C013 C017 H01B 109.2 . . ?
C013 C017 C01B 112.2(3) . . ?
H01A C017 H01B 107.9 . . ?
C01B C017 H01A 109.2 . . ?
C01B C017 H01B 109.2 . . ?
C00S C018 H018 119.7 . . ?
C01J C018 C00S 120.6(3) . . ?
C01J C018 H018 119.7 . . ?
C00K C019 H019 119.4 . . ?
C00K C019 C01M 121.1(3) . . ?
C01M C019 H019 119.4 . . ?
C42 C43 C44 121.1(3) . . ?
C46 C43 C44 120.4(3) . . ?
C46 C43 C42 118.5(3) . . ?
C00K C01B C017 121.1(3) . . ?
C00K C01B C01E 118.6(3) . . ?
C01E C01B C017 120.2(3) . . ?
C42 C49 H49 119.4 . . ?
C48 C49 C42 121.3(4) . . ?
C48 C49 H49 119.4 . . ?
C41 C53 H53 119.1 . . ?
C52 C53 C41 121.9(3) . . ?
C52 C53 H53 119.1 . . ?
C01B C01E H01E 119.2 . . ?
C01B C01E C01Z 121.5(3) . . ?
C01Z C01E H01E 119.2 . . ?
C00Z C01F H01F 120.7 . . ?
C00Z C01F C01L 118.7(4) . . ?
C01L C01F H01F 120.7 . . ?
C54 C60 H60 120.3 . . ?
C58 C60 C54 119.4(3) . . ?
C58 C60 H60 120.3 . . ?
C00W C01H H01H 122.1 . . ?
C00W C01H C01N 115.8(3) . . ?
C01N C01H H01H 122.1 . . ?
C58 C57 C59 120.9(3) . . ?
C56 C57 C58 118.2(3) . . ?
C56 C57 C59 120.9(3) . . ?
C018 C01J H01J 120.3 . . ?
C01O C01J C018 119.5(3) . . ?
C01O C01J H01J 120.3 . . ?
C00N C01K H01K 119.4 . . ?
C01O C01K C00N 121.3(3) . . ?
C01O C01K H01K 119.4 . . ?
C01F C01L H01L 119.6 . . ?
C01W C01L C01F 120.8(4) . . ?
C01W C01L H01L 119.6 . . ?
C019 C01M H01M 120.6 . . ?
C01Z C01M C019 118.9(3) . . ?
C01Z C01M H01M 120.6 . . ?
O6 C01N C01H 123.3(3) . . ?
O6 C01N C01R 114.4(3) . . ?
C01R C01N C01H 122.3(3) . . ?
C01J C01O H01O 119.9 . . ?
C01K C01O C01J 120.3(3) . . ?
C01K C01O H01O 119.9 . . ?
O1 C31 H31A 109.5 . . ?
O1 C31 H31B 109.5 . . ?
O1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C51 C52 C53 119.5(3) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C00X C01R C01N 120.6(3) . . ?
C00X C01R H01R 119.7 . . ?
C01N C01R H01R 119.7 . . ?
H01C C01S H01D 109.5 . . ?
H01C C01S H01G 109.5 . . ?
H01D C01S H01G 109.5 . . ?
C01Y C01S H01C 109.5 . . ?
C01Y C01S H01D 109.5 . . ?
C01Y C01S H01G 109.5 . . ?
C48 C47 H47 120.2 . . ?
C48 C47 C46 119.6(4) . . ?
C46 C47 H47 120.2 . . ?
C00Z C01U H01U 120.2 . . ?
C021 C01U C00Z 119.6(4) . . ?
C021 C01U H01U 120.2 . . ?
C36 C37 C32 120.7(3) . . ?
C36 C37 H37 119.7 . . ?
C32 C37 H37 119.7 . . ?
C01L C01W C024 120.2(4) . . ?
C021 C01W C01L 118.6(4) . . ?
C021 C01W C024 121.2(4) . . ?
C49 C48 H48 120.0 . . ?
C47 C48 C49 120.1(4) . . ?
C47 C48 H48 120.0 . . ?
O00D C01Y O00E 122.6(3) . . ?
O00D C01Y C01S 125.8(4) . . ?
O00E C01Y C01S 111.6(3) . . ?
C01E C01Z H01Z 120.1 . . ?
C01M C01Z C01E 119.8(3) . . ?
C01M C01Z H01Z 120.1 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C01U C021 C01W 121.2(4) . . ?
C01U C021 H021 119.4 . . ?
C01W C021 H021 119.4 . . ?
C43 C46 H46 119.3 . . ?
C47 C46 C43 121.3(4) . . ?
C47 C46 H46 119.3 . . ?
O6 C023 H02A 109.5 . . ?
O6 C023 H02B 109.5 . . ?
O6 C023 H02C 109.5 . . ?
H02A C023 H02B 109.5 . . ?
H02A C023 H02C 109.5 . . ?
H02B C023 H02C 109.5 . . ?
C01W C024 H02D 109.5 . . ?
C01W C024 H02E 109.5 . . ?
C01W C024 H02F 109.5 . . ?
H02D C024 H02E 109.5 . . ?
H02D C024 H02F 109.5 . . ?
H02E C024 H02F 109.5 . . ?
O00E C025 H02G 108.8 . . ?
O00E C025 H02H 108.8 . . ?
H02G C025 H02H 107.7 . . ?
C026 C025 O00E 113.9(5) . . ?
C026 C025 H02G 108.8 . . ?
C026 C025 H02H 108.8 . . ?
C025 C026 H02I 109.5 . . ?
C025 C026 H02J 109.5 . . ?
C025 C026 H02K 109.5 . . ?
H02I C026 H02J 109.5 . . ?
H02I C026 H02K 109.5 . . ?
H02J C026 H02K 109.5 . . ?
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
S2 O4 1.428(2) . ?
S2 O3 1.427(2) . ?
S2 N2 1.689(3) . ?
S2 C54 1.755(3) . ?
S1 O8 1.430(2) . ?
S1 O7 1.427(3) . ?
S1 N1 1.673(3) . ?
S1 C00Z 1.752(4) . ?
O2 H2 0.8400 . ?
O2 C45 1.454(4) . ?
O5 H5 0.8400 . ?
O5 C013 1.472(4) . ?
O1 C32 1.369(4) . ?
O1 C31 1.432(4) . ?
O6 C01N 1.365(4) . ?
O6 C023 1.429(5) . ?
N2 C39 1.454(4) . ?
N2 C34 1.426(4) . ?
N1 C00W 1.433(4) . ?
N1 C011 1.445(4) . ?
O00D C01Y 1.198(4) . ?
O00E C01Y 1.335(5) . ?
O00E C025 1.447(5) . ?
C39 C38 1.359(5) . ?
C39 C40 1.479(4) . ?
C35 C34 1.397(5) . ?
C35 C38 1.442(5) . ?
C35 C36 1.400(5) . ?
C34 C33 1.393(5) . ?
C45 H45 1.0000 . ?
C45 C38 1.515(5) . ?
C45 C44 1.523(5) . ?
C00K C00N 1.500(5) . ?
C00K C019 1.387(5) . ?
C00K C01B 1.385(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C43 1.499(5) . ?
C33 H33 0.9500 . ?
C33 C32 1.391(5) . ?
C00N C00S 1.402(5) . ?
C00N C01K 1.396(5) . ?
C00O C00P 1.453(5) . ?
C00O C011 1.362(5) . ?
C00O C013 1.487(5) . ?
C00P C00W 1.384(5) . ?
C00P C00X 1.408(5) . ?
C40 C50 1.400(5) . ?
C40 C41 1.408(5) . ?
C54 C55 1.385(5) . ?
C54 C60 1.381(5) . ?
C00S C011 1.485(5) . ?
C00S C018 1.400(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.371(5) . ?
C32 C37 1.405(5) . ?
C55 H55 0.9500 . ?
C55 C56 1.394(5) . ?
C00W C01H 1.389(5) . ?
C00X H00X 0.9500 . ?
C00X C01R 1.373(5) . ?
C51 H51 0.9500 . ?
C51 C50 1.384(5) . ?
C51 C52 1.373(5) . ?
C00Z C01F 1.377(5) . ?
C00Z C01U 1.385(5) . ?
C58 H58 0.9500 . ?
C58 C60 1.372(5) . ?
C58 C57 1.396(5) . ?
C50 H50 0.9500 . ?
C013 H013 1.0000 . ?
C013 C017 1.513(5) . ?
C56 H56 0.9500 . ?
C56 C57 1.372(5) . ?
C41 C42 1.480(5) . ?
C41 C53 1.405(5) . ?
C42 C43 1.409(5) . ?
C42 C49 1.403(5) . ?
C017 H01A 0.9900 . ?
C017 H01B 0.9900 . ?
C017 C01B 1.516(5) . ?
C018 H018 0.9500 . ?
C018 C01J 1.388(5) . ?
C019 H019 0.9500 . ?
C019 C01M 1.394(5) . ?
C43 C46 1.406(5) . ?
C01B C01E 1.387(5) . ?
C49 H49 0.9500 . ?
C49 C48 1.382(5) . ?
C53 H53 0.9500 . ?
C53 C52 1.387(5) . ?
C01E H01E 0.9500 . ?
C01E C01Z 1.390(5) . ?
C01F H01F 0.9500 . ?
C01F C01L 1.395(5) . ?
C60 H60 0.9500 . ?
C01H H01H 0.9500 . ?
C01H C01N 1.394(5) . ?
C57 C59 1.520(5) . ?
C01J H01J 0.9500 . ?
C01J C01O 1.386(5) . ?
C01K H01K 0.9500 . ?
C01K C01O 1.382(5) . ?
C01L H01L 0.9500 . ?
C01L C01W 1.394(6) . ?
C01M H01M 0.9500 . ?
C01M C01Z 1.380(5) . ?
C01N C01R 1.388(5) . ?
C01O H01O 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C52 H52 0.9500 . ?
C01R H01R 0.9500 . ?
C01S H01C 0.9800 . ?
C01S H01D 0.9800 . ?
C01S H01G 0.9800 . ?
C01S C01Y 1.476(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(6) . ?
C47 C46 1.394(5) . ?
C01U H01U 0.9500 . ?
C01U C021 1.366(6) . ?
C37 H37 0.9500 . ?
C01W C021 1.388(6) . ?
C01W C024 1.501(6) . ?
C48 H48 0.9500 . ?
C01Z H01Z 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C021 H021 0.9500 . ?
C46 H46 0.9500 . ?
C023 H02A 0.9800 . ?
C023 H02B 0.9800 . ?
C023 H02C 0.9800 . ?
C024 H02D 0.9800 . ?
C024 H02E 0.9800 . ?
C024 H02F 0.9800 . ?
C025 H02G 0.9900 . ?
C025 H02H 0.9900 . ?
C025 C026 1.361(8) . ?
C026 H02I 0.9800 . ?
C026 H02J 0.9800 . ?
C026 H02K 0.9800 . ?
