#------------------------------------------------------------------------------
#$Date: 2016-03-21 02:59:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178415 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/36/4023626.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_4023626
loop_
_publ_author_name
'Belén Vázquez'
'Raquel Pereira'
'Mart\in Pérez'
'Rosana Álvarez'
'Angel R. de Lera'
_publ_section_title
;
 Stereoselective Stille Coupling of Enantiopure Haloallenes and
 Alkenylstannanes for the Synthesis of Allenyl Carotenoids.
 Experimental and Computational Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6534
_journal_page_last               6541
_journal_paper_doi               10.1021/jo800756b
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C24 H29 N O5 S2'
_chemical_formula_weight         475.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.447(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2154(8)
_cell_length_b                   21.8191(17)
_cell_length_c                   11.5734(9)
_cell_measurement_temperature    173(2)
_cell_volume                     2474.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15659
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.874679
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          .49
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .24
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          1.064
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                7003
_reflns_number_total             9768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800756b_si_001.cif
_cod_data_source_block           ar1972s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4023626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C36 C 0.3722(3) -0.00704(16) 0.3743(3) 0.0572(10) Uani 1 1 d . . .
H36A H 0.3821 -0.0265 0.3009 0.086 Uiso 1 1 calc R . .
H36B H 0.3093 0.0277 0.3526 0.086 Uiso 1 1 calc R . .
H36C H 0.3359 -0.0369 0.4205 0.086 Uiso 1 1 calc R . .
C40 C 0.9314(3) 0.17335(18) 0.3139(3) 0.0782(12) Uani 1 1 d . . .
H40A H 0.9929 0.2056 0.3567 0.117 Uiso 1 1 calc R . .
H40B H 0.8490 0.1920 0.2605 0.117 Uiso 1 1 calc R . .
H40C H 0.9776 0.1490 0.2660 0.117 Uiso 1 1 calc R . .
C13 C 0.8810(3) 0.90967(14) 0.4562(3) 0.0525(9) Uani 1 1 d . . .
H13A H 0.9475 0.9228 0.4147 0.079 Uiso 1 1 calc R . .
H13B H 0.8777 0.9398 0.5181 0.079 Uiso 1 1 calc R . .
H13C H 0.7906 0.9063 0.3979 0.079 Uiso 1 1 calc R . .
C39 C 0.8929(3) 0.13307(16) 0.4023(3) 0.0512(9) Uani 1 1 d . . .
C12 C 1.0592(3) 0.85472(16) 0.6126(3) 0.0511(9) Uani 1 1 d . . .
H12A H 1.0894 0.8150 0.6504 0.077 Uiso 1 1 calc R . .
H12B H 1.0477 0.8836 0.6738 0.077 Uiso 1 1 calc R . .
H12C H 1.1277 0.8706 0.5758 0.077 Uiso 1 1 calc R . .
C38 C 0.5942(3) 0.12390(14) 0.7321(3) 0.0462(8) Uani 1 1 d . . .
H38A H 0.6760 0.1466 0.7759 0.069 Uiso 1 1 calc R . .
H38B H 0.5603 0.0999 0.7892 0.069 Uiso 1 1 calc R . .
H38C H 0.5237 0.1528 0.6894 0.069 Uiso 1 1 calc R . .
C16 C 0.4334(3) 0.77377(15) 0.6632(2) 0.0455(8) Uani 1 1 d . . .
H16A H 0.4211 0.7976 0.7312 0.068 Uiso 1 1 calc R . .
H16B H 0.4801 0.7352 0.6930 0.068 Uiso 1 1 calc R . .
H16C H 0.3440 0.7649 0.6067 0.068 Uiso 1 1 calc R . .
C22 C 0.7190(3) 0.83930(17) -0.0928(3) 0.0440(8) Uani 1 1 d . . .
H22 H 0.6433 0.8665 -0.1109 0.053 Uiso 1 1 calc R . .
C30 C 0.5740(3) 0.05763(14) 0.3771(2) 0.0450(8) Uani 1 1 d . . .
H30A H 0.5108 0.0920 0.3450 0.054 Uiso 1 1 calc R . .
H30B H 0.5886 0.0348 0.3079 0.054 Uiso 1 1 calc R . .
O9 O 0.9717(2) 0.11352(12) 0.4922(2) 0.0738(8) Uani 1 1 d . . .
C45 C 0.7740(3) -0.01621(16) 1.1185(3) 0.0483(9) Uani 1 1 d . . .
H45 H 0.8499 -0.0431 1.1438 0.058 Uiso 1 1 calc R . .
C26 C 0.6919(3) 0.11846(13) 0.5596(2) 0.0370(7) Uani 1 1 d . . .
H26A H 0.6330 0.1545 0.5299 0.044 Uiso 1 1 calc R . .
H26B H 0.7822 0.1338 0.6073 0.044 Uiso 1 1 calc R . .
C3 C 0.9235(3) 0.84681(14) 0.5159(3) 0.0344(7) Uani 1 1 d . . .
C37 C 0.7340(3) 0.03397(15) 0.7146(3) 0.0449(8) Uani 1 1 d . . .
H37A H 0.7657 0.0079 0.6590 0.067 Uiso 1 1 calc R . .
H37B H 0.6905 0.0085 0.7629 0.067 Uiso 1 1 calc R . .
H37C H 0.8119 0.0557 0.7679 0.067 Uiso 1 1 calc R . .
C31 C 0.3872(3) 0.04946(13) 0.5938(2) 0.0313(7) Uani 1 1 d . . .
C44 C 0.7956(3) 0.04411(17) 1.0907(3) 0.0434(9) Uani 1 1 d . . .
H44 H 0.8858 0.0575 1.0969 0.052 Uiso 1 1 calc R . .
C14 C 0.8407(3) 0.71519(14) 0.2699(3) 0.0418(8) Uani 1 1 d . . .
H14A H 0.7556 0.6966 0.2213 0.063 Uiso 1 1 calc R . .
H14B H 0.8928 0.6849 0.3273 0.063 Uiso 1 1 calc R . .
H14C H 0.8949 0.7287 0.2170 0.063 Uiso 1 1 calc R . .
C1 C 0.6851(2) 0.80133(13) 0.4902(2) 0.0351(7) Uani 1 1 d . . .
H1 H 0.6363 0.8360 0.4395 0.042 Uiso 1 1 calc R . .
C43 C 0.6899(3) 0.08470(15) 1.0545(3) 0.0370(8) Uani 1 1 d . . .
H43 H 0.7056 0.1261 1.0368 0.044 Uiso 1 1 calc R . .
C15 C 0.5173(3) 0.80977(16) 0.6004(2) 0.0390(7) Uani 1 1 d . . .
C5 C 0.8082(3) 0.76985(13) 0.3380(2) 0.0305(6) Uani 1 1 d . . .
C2 C 0.8174(2) 0.82372(14) 0.5777(2) 0.0369(7) Uani 1 1 d . . .
H2A H 0.8582 0.7898 0.6331 0.044 Uiso 1 1 calc R . .
H2B H 0.7961 0.8574 0.6269 0.044 Uiso 1 1 calc R . .
C28 C 0.5013(3) 0.04806(12) 0.5643(2) 0.0312(7) Uani 1 1 d . . .
C21 C 0.6998(3) 0.77764(16) -0.0712(3) 0.0397(8) Uani 1 1 d . . .
H21 H 0.6107 0.7635 -0.0751 0.048 Uiso 1 1 calc R . .
O5 O 0.73261(18) 0.81534(10) 0.25274(18) 0.0442(6) Uani 1 1 d . . .
H5 H 0.773(3) 0.8204(16) 0.209(3) 0.066 Uiso 1 1 d . . .
C29 C 0.5097(3) 0.01535(14) 0.4498(2) 0.0395(7) Uani 1 1 d . . .
C32 C 0.2760(3) 0.05125(13) 0.6270(2) 0.0326(7) Uani 1 1 d . . .
H32 H 0.2096 0.0814 0.5913 0.039 Uiso 1 1 calc R . .
O10 O 0.6021(2) -0.03586(11) 0.4803(2) 0.0526(6) Uani 1 1 d . . .
H10 H 0.564(3) -0.0668(16) 0.520(3) 0.079 Uiso 1 1 d . . .
C33 C 0.2462(3) 0.00971(13) 0.7161(2) 0.0309(7) Uani 1 1 d . . .
C34 C 0.1360(3) 0.02051(13) 0.7537(2) 0.0324(7) Uani 1 1 d . . .
H34 H 0.0760 0.0518 0.7127 0.039 Uiso 1 1 calc R . .
C10 C 1.3280(2) 0.80439(14) 0.2561(2) 0.0298(7) Uani 1 1 d . . .
H10A H 1.3760 0.7696 0.2961 0.036 Uiso 1 1 calc R . .
C6 C 0.7134(2) 0.75089(13) 0.4117(2) 0.0327(6) Uani 1 1 d . . .
H6A H 0.6258 0.7370 0.3563 0.039 Uiso 1 1 calc R . .
H6B H 0.7544 0.7157 0.4634 0.039 Uiso 1 1 calc R . .
C25 C 0.7093(3) 0.08306(13) 0.4529(2) 0.0387(7) Uani 1 1 d . . .
H25 H 0.7755 0.0488 0.4815 0.046 Uiso 1 1 calc R . .
C41 C 0.3469(3) -0.04095(14) 0.7618(3) 0.0373(7) Uani 1 1 d . . .
H41A H 0.4340 -0.0235 0.8090 0.056 Uiso 1 1 calc R . .
H41B H 0.3608 -0.0639 0.6934 0.056 Uiso 1 1 calc R . .
H41C H 0.3117 -0.0685 0.8128 0.056 Uiso 1 1 calc R . .
C4 C 0.9378(2) 0.80085(12) 0.4191(2) 0.0263(6) Uani 1 1 d . . .
C46 C 0.6448(3) -0.03812(16) 1.1102(3) 0.0426(8) Uani 1 1 d . . .
H46 H 0.6309 -0.0794 1.1300 0.051 Uiso 1 1 calc R . .
C7 C 1.0547(3) 0.79084(12) 0.3991(2) 0.0267(6) Uani 1 1 d . . .
O3 O 0.59819(17) 0.77342(9) 0.55689(16) 0.0389(5) Uani 1 1 d . . .
C18 C 1.1681(2) 0.78999(14) -0.0135(2) 0.0274(7) Uani 1 1 d . . .
O4 O 0.5129(2) 0.86449(11) 0.5891(2) 0.0589(6) Uani 1 1 d . . .
C48 C 0.3239(3) 0.03625(14) 1.0217(2) 0.0288(7) Uani 1 1 d . . .
C23 C 0.8465(3) 0.86105(15) -0.0880(3) 0.0429(8) Uani 1 1 d . . .
H23 H 0.8590 0.9031 -0.1035 0.052 Uiso 1 1 calc R . .
C20 C 0.8065(3) 0.73684(15) -0.0445(3) 0.0379(8) Uani 1 1 d . . .
H20 H 0.7926 0.6947 -0.0308 0.046 Uiso 1 1 calc R . .
O8 O 0.75858(19) 0.12340(9) 0.37401(16) 0.0488(5) Uani 1 1 d . . .
C8 C 1.1690(2) 0.78200(13) 0.3712(2) 0.0278(6) Uani 1 1 d . . .
H8 H 1.2255 0.7489 0.4087 0.033 Uiso 1 1 calc R . .
C47 C 0.5349(3) 0.00262(14) 1.0717(2) 0.0293(7) Uani 1 1 d . . .
C24 C 0.9565(3) 0.82129(14) -0.0603(2) 0.0290(7) Uani 1 1 d . . .
C42 C 0.5588(3) 0.06347(14) 1.0445(2) 0.0296(7) Uani 1 1 d . . .
C11 C 1.3870(3) 0.83547(14) 0.1671(2) 0.0329(7) Uani 1 1 d . . .
H11A H 1.4871 0.8389 0.2013 0.039 Uiso 1 1 calc R . .
H11B H 1.3491 0.8774 0.1516 0.039 Uiso 1 1 calc R . .
C27 C 0.6296(3) 0.08103(13) 0.6417(2) 0.0321(7) Uani 1 1 d . . .
C17 C 1.1274(3) 0.87479(13) 0.2370(3) 0.0341(7) Uani 1 1 d . . .
H17A H 1.1662 0.8974 0.1813 0.051 Uiso 1 1 calc R . .
H17B H 1.1237 0.9016 0.3040 0.051 Uiso 1 1 calc R . .
H17C H 1.0351 0.8610 0.1944 0.051 Uiso 1 1 calc R . .
C9 C 1.2154(2) 0.82019(13) 0.2853(2) 0.0259(6) Uani 1 1 d . . .
C35 C 0.0974(3) -0.01129(14) 0.8530(2) 0.0345(7) Uani 1 1 d . . .
H35A H 0.1438 -0.0515 0.8682 0.041 Uiso 1 1 calc R . .
H35B H -0.0023 -0.0187 0.8287 0.041 Uiso 1 1 calc R . .
C19 C 0.9356(3) 0.75947(15) -0.0382(2) 0.0296(7) Uani 1 1 d . . .
N1 N 1.0927(2) 0.83726(12) -0.0466(2) 0.0321(6) Uani 1 1 d . . .
O7 O 0.09580(18) 0.09472(9) 0.96176(18) 0.0413(5) Uani 1 1 d . . .
N2 N 0.3989(2) -0.01189(11) 1.0586(2) 0.0304(6) Uani 1 1 d . . .
O2 O 1.39790(18) 0.73206(9) 0.05124(18) 0.0400(5) Uani 1 1 d . . .
O6 O 0.10633(19) -0.00001(10) 1.08076(19) 0.0453(6) Uani 1 1 d . . .
O1 O 1.39084(18) 0.83013(10) -0.05867(17) 0.0384(5) Uani 1 1 d . . .
S1 S 1.09054(7) 0.72110(3) 0.00425(7) 0.03563(19) Uani 1 1 d . . .
S4 S 0.14323(7) 0.03297(4) 0.98745(7) 0.03412(19) Uani 1 1 d . . .
S3 S 0.40522(7) 0.10280(4) 0.99900(7) 0.0387(2) Uani 1 1 d . . .
S2 S 1.34991(7) 0.79425(3) 0.02887(6) 0.03049(18) 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 0.0033 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'
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'
S S 0.1246 0.1234 '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
O9 C39 O8 123.2(3) . . ?
O9 C39 C40 124.4(3) . . ?
O8 C39 C40 112.3(3) . . ?
C23 C22 C21 120.5(3) . . ?
C29 C30 C25 111.6(2) . . ?
C46 C45 C44 121.6(3) . . ?
C25 C26 C27 113.8(2) . . ?
C12 C3 C4 110.7(2) . . ?
C12 C3 C13 108.1(3) . . ?
C4 C3 C13 109.0(2) . . ?
C12 C3 C2 107.9(2) . . ?
C4 C3 C2 110.4(2) . . ?
C13 C3 C2 110.6(2) . . ?
C32 C31 C28 178.0(3) . . ?
C43 C44 C45 121.5(3) . . ?
O3 C1 C6 105.2(2) . . ?
O3 C1 C2 109.8(2) . . ?
C6 C1 C2 110.5(2) . . ?
C44 C43 C42 117.9(3) . . ?
O4 C15 O3 123.7(3) . . ?
O4 C15 C16 124.5(3) . . ?
O3 C15 C16 111.8(3) . . ?
O5 C5 C14 109.6(2) . . ?
O5 C5 C6 105.4(2) . . ?
C14 C5 C6 110.3(2) . . ?
O5 C5 C4 108.2(2) . . ?
C14 C5 C4 112.6(2) . . ?
C6 C5 C4 110.6(2) . . ?
C1 C2 C3 113.8(2) . . ?
C31 C28 C29 120.8(2) . . ?
C31 C28 C27 120.9(2) . . ?
C29 C28 C27 118.3(2) . . ?
C20 C21 C22 121.6(3) . . ?
O10 C29 C36 109.2(2) . . ?
O10 C29 C30 104.6(2) . . ?
C36 C29 C30 110.7(2) . . ?
O10 C29 C28 110.0(2) . . ?
C36 C29 C28 112.4(2) . . ?
C30 C29 C28 109.6(2) . . ?
C31 C32 C33 124.1(3) . . ?
C34 C33 C32 118.7(3) . . ?
C34 C33 C41 124.8(3) . . ?
C32 C33 C41 116.4(2) . . ?
C33 C34 C35 126.9(3) . . ?
C9 C10 C11 127.0(3) . . ?
C1 C6 C5 113.7(2) . . ?
O8 C25 C26 110.2(2) . . ?
O8 C25 C30 106.2(2) . . ?
C26 C25 C30 111.2(2) . . ?
C7 C4 C3 121.4(2) . . ?
C7 C4 C5 119.4(2) . . ?
C3 C4 C5 119.0(2) . . ?
C45 C46 C47 117.8(3) . . ?
C4 C7 C8 176.1(3) . . ?
C15 O3 C1 118.8(2) . . ?
N1 C18 S1 118.49(19) . . ?
N1 C18 S2 122.1(2) . . ?
S1 C18 S2 119.11(17) . . ?
N2 C48 S3 117.7(2) . . ?
N2 C48 S4 121.3(2) . . ?
S3 C48 S4 120.89(17) . . ?
C22 C23 C24 119.5(3) . . ?
C21 C20 C19 117.5(3) . . ?
C39 O8 C25 117.1(2) . . ?
C7 C8 C9 124.2(2) . . ?
N2 C47 C42 115.0(3) . . ?
N2 C47 C46 125.1(3) . . ?
C42 C47 C46 119.8(3) . . ?
C23 C24 N1 125.9(3) . . ?
C23 C24 C19 119.3(3) . . ?
N1 C24 C19 114.7(2) . . ?
C43 C42 C47 121.4(3) . . ?
C43 C42 S3 128.9(3) . . ?
C47 C42 S3 109.7(2) . . ?
C10 C11 S2 111.4(2) . . ?
C38 C27 C26 108.8(2) . . ?
C38 C27 C28 111.0(2) . . ?
C26 C27 C28 109.0(2) . . ?
C38 C27 C37 107.1(2) . . ?
C26 C27 C37 110.5(2) . . ?
C28 C27 C37 110.4(2) . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 C17 125.4(3) . . ?
C8 C9 C17 115.2(2) . . ?
C34 C35 S4 111.2(2) . . ?
C20 C19 C24 121.6(3) . . ?
C20 C19 S1 128.3(3) . . ?
C24 C19 S1 110.0(2) . . ?
C18 N1 C24 109.1(2) . . ?
C48 N2 C47 109.3(2) . . ?
C19 S1 C18 87.65(14) . . ?
O6 S4 O7 118.82(13) . . ?
O6 S4 C48 109.28(13) . . ?
O7 S4 C48 106.09(13) . . ?
O6 S4 C35 109.04(14) . . ?
O7 S4 C35 109.82(14) . . ?
C48 S4 C35 102.53(13) . . ?
C48 S3 C42 88.31(14) . . ?
O1 S2 O2 119.26(12) . . ?
O1 S2 C11 109.21(13) . . ?
O2 S2 C11 109.84(14) . . ?
O1 S2 C18 108.90(12) . . ?
O2 S2 C18 105.96(13) . . ?
C11 S2 C18 102.30(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C36 C29 1.510(4) . ?
C40 C39 1.484(4) . ?
C13 C3 1.542(4) . ?
C39 O9 1.199(3) . ?
C39 O8 1.334(3) . ?
C12 C3 1.525(4) . ?
C38 C27 1.521(4) . ?
C16 C15 1.495(4) . ?
C22 C23 1.372(4) . ?
C22 C21 1.392(4) . ?
C30 C29 1.517(4) . ?
C30 C25 1.517(3) . ?
C45 C46 1.381(4) . ?
C45 C44 1.387(4) . ?
C26 C25 1.509(4) . ?
C26 C27 1.522(4) . ?
C3 C4 1.541(3) . ?
C3 C2 1.543(3) . ?
C37 C27 1.547(4) . ?
C31 C32 1.298(3) . ?
C31 C28 1.305(4) . ?
C44 C43 1.367(4) . ?
C14 C5 1.518(4) . ?
C1 O3 1.464(3) . ?
C1 C6 1.506(4) . ?
C1 C2 1.522(3) . ?
C43 C42 1.391(4) . ?
C15 O4 1.201(3) . ?
C15 O3 1.342(3) . ?
C5 O5 1.457(3) . ?
C5 C6 1.518(3) . ?
C5 C4 1.545(3) . ?
C28 C29 1.529(4) . ?
C28 C27 1.541(4) . ?
C21 C20 1.373(4) . ?
C29 O10 1.440(3) . ?
C32 C33 1.468(4) . ?
C33 C34 1.338(3) . ?
C33 C41 1.500(4) . ?
C34 C35 1.488(4) . ?
C10 C9 1.333(3) . ?
C10 C11 1.495(3) . ?
C25 O8 1.457(3) . ?
C4 C7 1.298(3) . ?
C46 C47 1.402(4) . ?
C7 C8 1.310(3) . ?
C18 N1 1.279(4) . ?
C18 S1 1.738(3) . ?
C18 S2 1.784(3) . ?
C48 N2 1.299(3) . ?
C48 S3 1.730(3) . ?
C48 S4 1.776(3) . ?
C23 C24 1.384(4) . ?
C20 C19 1.391(4) . ?
C8 C9 1.475(4) . ?
C47 N2 1.390(3) . ?
C47 C42 1.402(4) . ?
C24 N1 1.399(3) . ?
C24 C19 1.401(4) . ?
C42 S3 1.734(3) . ?
C11 S2 1.780(3) . ?
C17 C9 1.501(4) . ?
C35 S4 1.778(3) . ?
C19 S1 1.734(3) . ?
O7 S4 1.434(2) . ?
O2 S2 1.441(2) . ?
O6 S4 1.434(2) . ?
O1 S2 1.4331(19) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10 O4 0.96(3) 1.84(4) 2.791(3) 170(3) 1_545
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
C46 C45 C44 C43 0.4(5) . . . . ?
C45 C44 C43 C42 -1.0(5) . . . . ?
O3 C1 C2 C3 173.0(2) . . . . ?
C6 C1 C2 C3 57.3(3) . . . . ?
C12 C3 C2 C1 -168.2(2) . . . . ?
C4 C3 C2 C1 -47.0(3) . . . . ?
C13 C3 C2 C1 73.8(3) . . . . ?
C32 C31 C28 C29 159(9) . . . . ?
C32 C31 C28 C27 -23(9) . . . . ?
C23 C22 C21 C20 0.1(5) . . . . ?
C25 C30 C29 O10 -65.2(3) . . . . ?
C25 C30 C29 C36 177.3(3) . . . . ?
C25 C30 C29 C28 52.8(3) . . . . ?
C31 C28 C29 O10 -115.7(3) . . . . ?
C27 C28 C29 O10 66.2(3) . . . . ?
C31 C28 C29 C36 6.2(4) . . . . ?
C27 C28 C29 C36 -171.9(3) . . . . ?
C31 C28 C29 C30 129.8(3) . . . . ?
C27 C28 C29 C30 -48.3(3) . . . . ?
C28 C31 C32 C33 -61(9) . . . . ?
C31 C32 C33 C34 172.1(3) . . . . ?
C31 C32 C33 C41 -5.6(4) . . . . ?
C32 C33 C34 C35 -172.2(3) . . . . ?
C41 C33 C34 C35 5.3(5) . . . . ?
O3 C1 C6 C5 -177.5(2) . . . . ?
C2 C1 C6 C5 -59.0(3) . . . . ?
O5 C5 C6 C1 -66.5(3) . . . . ?
C14 C5 C6 C1 175.3(2) . . . . ?
C4 C5 C6 C1 50.1(3) . . . . ?
C27 C26 C25 O8 175.3(2) . . . . ?
C27 C26 C25 C30 57.8(3) . . . . ?
C29 C30 C25 O8 -179.0(2) . . . . ?
C29 C30 C25 C26 -59.1(3) . . . . ?
C12 C3 C4 C7 -24.8(4) . . . . ?
C13 C3 C4 C7 94.0(3) . . . . ?
C2 C3 C4 C7 -144.2(3) . . . . ?
C12 C3 C4 C5 159.9(2) . . . . ?
C13 C3 C4 C5 -81.3(3) . . . . ?
C2 C3 C4 C5 40.4(3) . . . . ?
O5 C5 C4 C7 -102.4(3) . . . . ?
C14 C5 C4 C7 18.8(4) . . . . ?
C6 C5 C4 C7 142.6(3) . . . . ?
O5 C5 C4 C3 73.0(3) . . . . ?
C14 C5 C4 C3 -165.8(2) . . . . ?
C6 C5 C4 C3 -42.0(3) . . . . ?
C44 C45 C46 C47 0.5(5) . . . . ?
C3 C4 C7 C8 -120(4) . . . . ?
C5 C4 C7 C8 55(4) . . . . ?
O4 C15 O3 C1 -0.9(4) . . . . ?
C16 C15 O3 C1 178.6(2) . . . . ?
C6 C1 O3 C15 -156.5(2) . . . . ?
C2 C1 O3 C15 84.6(3) . . . . ?
C21 C22 C23 C24 -0.6(5) . . . . ?
C22 C21 C20 C19 0.8(4) . . . . ?
O9 C39 O8 C25 -4.9(5) . . . . ?
C40 C39 O8 C25 178.4(3) . . . . ?
C26 C25 O8 C39 84.0(3) . . . . ?
C30 C25 O8 C39 -155.5(3) . . . . ?
C4 C7 C8 C9 34(4) . . . . ?
C45 C46 C47 N2 -179.9(3) . . . . ?
C45 C46 C47 C42 -0.8(4) . . . . ?
C22 C23 C24 N1 -176.8(3) . . . . ?
C22 C23 C24 C19 0.2(4) . . . . ?
C44 C43 C42 C47 0.7(4) . . . . ?
C44 C43 C42 S3 -178.8(2) . . . . ?
N2 C47 C42 C43 179.4(2) . . . . ?
C46 C47 C42 C43 0.2(4) . . . . ?
N2 C47 C42 S3 -1.0(3) . . . . ?
C46 C47 C42 S3 179.8(2) . . . . ?
C9 C10 C11 S2 -102.4(3) . . . . ?
C25 C26 C27 C38 -170.1(2) . . . . ?
C25 C26 C27 C28 -49.0(3) . . . . ?
C25 C26 C27 C37 72.5(3) . . . . ?
C31 C28 C27 C38 -12.6(4) . . . . ?
C29 C28 C27 C38 165.5(3) . . . . ?
C31 C28 C27 C26 -132.3(3) . . . . ?
C29 C28 C27 C26 45.7(3) . . . . ?
C31 C28 C27 C37 106.1(3) . . . . ?
C29 C28 C27 C37 -75.8(3) . . . . ?
C11 C10 C9 C8 177.0(2) . . . . ?
C11 C10 C9 C17 -2.6(4) . . . . ?
C7 C8 C9 C10 -174.7(3) . . . . ?
C7 C8 C9 C17 4.9(4) . . . . ?
C33 C34 C35 S4 99.7(3) . . . . ?
C21 C20 C19 C24 -1.2(4) . . . . ?
C21 C20 C19 S1 174.7(2) . . . . ?
C23 C24 C19 C20 0.7(4) . . . . ?
N1 C24 C19 C20 178.0(2) . . . . ?
C23 C24 C19 S1 -175.9(2) . . . . ?
N1 C24 C19 S1 1.5(3) . . . . ?
S1 C18 N1 C24 0.7(3) . . . . ?
S2 C18 N1 C24 -173.11(18) . . . . ?
C23 C24 N1 C18 175.7(3) . . . . ?
C19 C24 N1 C18 -1.4(3) . . . . ?
S3 C48 N2 C47 -0.1(3) . . . . ?
S4 C48 N2 C47 176.45(18) . . . . ?
C42 C47 N2 C48 0.7(3) . . . . ?
C46 C47 N2 C48 179.9(3) . . . . ?
C20 C19 S1 C18 -177.1(3) . . . . ?
C24 C19 S1 C18 -0.8(2) . . . . ?
N1 C18 S1 C19 0.1(2) . . . . ?
S2 C18 S1 C19 174.09(16) . . . . ?
N2 C48 S4 O6 45.2(3) . . . . ?
S3 C48 S4 O6 -138.45(17) . . . . ?
N2 C48 S4 O7 174.4(2) . . . . ?
S3 C48 S4 O7 -9.2(2) . . . . ?
N2 C48 S4 C35 -70.4(2) . . . . ?
S3 C48 S4 C35 105.97(18) . . . . ?
C34 C35 S4 O6 -178.95(19) . . . . ?
C34 C35 S4 O7 49.3(2) . . . . ?
C34 C35 S4 C48 -63.2(2) . . . . ?
N2 C48 S3 C42 -0.4(2) . . . . ?
S4 C48 S3 C42 -176.96(18) . . . . ?
C43 C42 S3 C48 -179.7(3) . . . . ?
C47 C42 S3 C48 0.8(2) . . . . ?
C10 C11 S2 O1 171.65(19) . . . . ?
C10 C11 S2 O2 -55.8(2) . . . . ?
C10 C11 S2 C18 56.4(2) . . . . ?
N1 C18 S2 O1 -46.3(3) . . . . ?
S1 C18 S2 O1 139.88(15) . . . . ?
N1 C18 S2 O2 -175.8(2) . . . . ?
S1 C18 S2 O2 10.44(19) . . . . ?
N1 C18 S2 C11 69.2(3) . . . . ?
S1 C18 S2 C11 -104.62(18) . . . . ?
