#------------------------------------------------------------------------------
#$Date: 2018-08-16 12:33:19 +0300 (Thu, 16 Aug 2018) $
#$Revision: 209783 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/48/7104836.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_7104836
loop_
_publ_author_name
'Gridley, Jonathan J.'
'Coogan, Michael P.'
'Knight, David W.'
'Malik, K. M. Abdul'
'Sharland, Christopher M.'
'Singkhonrat, Jirada'
'Williams, Siân'
_publ_section_title
;
 A stereoselective synthesis of anti-γ,δ-alkynyl- and
 -alkenyl-β-hydroxy-α-amino esters from tin(II) enolates of glycinate
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   20
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2550
_journal_page_last               2551
_journal_paper_doi               10.1039/b306291k
_journal_year                    2003
_chemical_formula_sum            'C23 H27 N O5 S'
_chemical_formula_weight         429.52
_chemical_name_common
;N-Tosyl-(1-methyl-2-hydroxy-5-phenyl-4-pentynyl)glycine ethyl
ester
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   34.330(7)
_cell_length_b                   13.750(3)
_cell_length_c                   19.899(4)
_cell_measurement_reflns_used    'all obs. data'
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.96
_cell_volume                     9199(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Nonius kappa CCD area detector'
_diffrn_measurement_method       'phi & omega scan to fill Ewald sphere'
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            114389
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    'calculated positions, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         20899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0680P)²+7.8178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                13802
_reflns_number_total             20899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306291k.txt
_cod_data_source_block           Compound_15
_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      P2(1)/c
_cod_database_code               7104836
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.511875(18) 0.61959(5) -0.11031(3) 0.02557(14) Uani 1 1 d . . .
S2 S 0.439243(18) 0.72070(5) 0.07523(3) 0.02702(15) Uani 1 1 d . . .
S3 S 0.063255(19) 0.18556(5) -0.08616(3) 0.02998(16) Uani 1 1 d . . .
S4 S -0.009749(18) 0.11169(5) 0.10737(3) 0.02545(14) Uani 1 1 d . . .
O1 O 0.54239(5) 0.61103(14) -0.04972(9) 0.0333(4) Uani 1 1 d . . .
O2 O 0.51673(5) 0.57477(14) -0.17289(9) 0.0336(4) Uani 1 1 d . . .
O3 O 0.39421(5) 0.66299(13) -0.21831(8) 0.0330(4) Uani 1 1 d . . .
O5 O 0.40480(5) 0.69730(13) -0.10605(8) 0.0308(4) Uani 1 1 d . . .
O6 O 0.40505(5) 0.48246(13) -0.05884(8) 0.0254(4) Uani 1 1 d . . .
H6 H 0.4229 0.4576 -0.0285 0.038 Uiso 1 1 calc R . .
O7 O 0.46938(5) 0.70104(14) 0.03629(9) 0.0324(4) Uani 1 1 d . . .
O8 O 0.44651(5) 0.69966(15) 0.14689(8) 0.0365(5) Uani 1 1 d . . .
O9 O 0.33377(5) 0.54140(15) -0.01628(9) 0.0345(4) Uani 1 1 d . . .
H9 H 0.3540 0.5206 -0.0292 0.052 Uiso 1 1 calc R . .
O10 O 0.33114(6) 0.76824(15) -0.02152(10) 0.0406(5) Uani 1 1 d . . .
O11 O 0.32482(6) 0.79130(15) 0.08810(11) 0.0480(5) Uani 1 1 d . . .
O12 O 0.16722(6) 0.25012(16) -0.00501(10) 0.0511(6) Uani 1 1 d . B .
O13 O 0.17826(6) 0.25187(16) -0.11221(10) 0.0479(6) Uani 1 1 d . . .
O14 O 0.05543(6) 0.15427(15) -0.15608(8) 0.0368(5) Uani 1 1 d . . .
O15 O 0.03417(5) 0.17067(14) -0.04440(8) 0.0339(4) Uani 1 1 d . . .
O16 O 0.16982(5) 0.02901(15) 0.01848(9) 0.0360(5) Uani 1 1 d . . .
H16 H 0.1505 0.0052 0.0330 0.054 Uiso 1 1 calc R . .
O4 O 0.09842(6) 0.18673(15) 0.09387(8) 0.0403(5) Uani 1 1 d . . .
O17 O 0.11106(5) 0.16536(14) 0.20784(8) 0.0356(5) Uani 1 1 d . D .
O18 O 0.09974(5) -0.02882(13) 0.06328(8) 0.0274(4) Uani 1 1 d . . .
H18 H 0.0814 -0.0494 0.0320 0.041 Uiso 1 1 calc R . .
O19 O -0.04024(5) 0.09844(14) 0.04712(9) 0.0335(4) Uani 1 1 d . . .
O20 O -0.01399(5) 0.07096(14) 0.17151(9) 0.0324(4) Uani 1 1 d . . .
N1 N 0.47207(6) 0.57253(15) -0.09031(9) 0.0245(4) Uani 1 1 d . . .
H1 H 0.4719 0.5566 -0.0475 0.029 Uiso 1 1 calc R . .
N2 N 0.40085(6) 0.65806(15) 0.03885(10) 0.0244(4) Uani 1 1 d . . .
H2 H 0.4016 0.6227 0.0023 0.029 Uiso 1 1 calc R . .
N3 N 0.10298(6) 0.13002(16) -0.04738(10) 0.0283(5) Uani 1 1 d . . .
H3 H 0.1038 0.1032 -0.0070 0.034 Uiso 1 1 calc R . .
N4 N 0.03036(6) 0.06631(15) 0.08833(9) 0.0235(4) Uani 1 1 d . . .
H4 H 0.0305 0.0483 0.0459 0.028 Uiso 1 1 calc R . .
C1 C 0.43930(7) 0.37217(18) -0.12467(12) 0.0269(5) Uani 1 1 d . . .
H1A H 0.4642 0.3808 -0.0892 0.032 Uiso 1 1 calc R . .
C2 C 0.41708(8) 0.2841(2) -0.10389(14) 0.0368(6) Uani 1 1 d . . .
H2B H 0.4091 0.2976 -0.0602 0.055 Uiso 1 1 calc R . .
H2C H 0.4345 0.2271 -0.0988 0.055 Uiso 1 1 calc R . .
H2D H 0.3933 0.2714 -0.1394 0.055 Uiso 1 1 calc R . .
C3 C 0.41411(7) 0.46557(18) -0.12533(11) 0.0231(5) Uani 1 1 d . . .
C4 C 0.43666(7) 0.55710(18) -0.14415(11) 0.0236(5) Uani 1 1 d . . .
H4A H 0.4453 0.5443 -0.1884 0.028 Uiso 1 1 calc R . .
C5 C 0.41016(7) 0.64708(18) -0.15282(11) 0.0233(5) Uani 1 1 d . . .
C6 C 0.45126(9) 0.3532(2) -0.19323(14) 0.0412(7) Uani 1 1 d . . .
H6B H 0.4694 0.4045 -0.2021 0.062 Uiso 1 1 calc R . .
H6C H 0.4275 0.3528 -0.2300 0.062 Uiso 1 1 calc R . .
H6D H 0.4647 0.2900 -0.1917 0.062 Uiso 1 1 calc R . .
C7 C 0.36761(10) 0.7473(2) -0.23264(14) 0.0447(8) Uani 1 1 d . . .
H7A H 0.3652 0.7670 -0.2812 0.054 Uiso 1 1 calc R . .
H7B H 0.3792 0.8025 -0.2033 0.054 Uiso 1 1 calc R . .
C8 C 0.32738(10) 0.7252(3) -0.2196(2) 0.0628(10) Uani 1 1 d . . .
H8A H 0.3097 0.7805 -0.2340 0.094 Uiso 1 1 calc R . .
H8B H 0.3292 0.7133 -0.1705 0.094 Uiso 1 1 calc R . .
H8C H 0.3168 0.6672 -0.2456 0.094 Uiso 1 1 calc R . .
C9 C 0.37601(8) 0.45554(19) -0.17470(12) 0.0275(6) Uani 1 1 d . . .
C10 C 0.34656(8) 0.4419(2) -0.21679(13) 0.0295(6) Uani 1 1 d . . .
C11 C 0.31234(8) 0.4239(2) -0.27009(13) 0.0341(6) Uani 1 1 d . . .
C12 C 0.27604(9) 0.4677(3) -0.27029(17) 0.0565(10) Uani 1 1 d . . .
H12 H 0.2727 0.5083 -0.2332 0.068 Uiso 1 1 calc R . .
C13 C 0.24443(10) 0.4520(3) -0.3249(2) 0.0722(12) Uani 1 1 d . . .
H13 H 0.2196 0.4827 -0.3254 0.087 Uiso 1 1 calc R . .
C14 C 0.24882(11) 0.3922(3) -0.37857(19) 0.0671(11) Uani 1 1 d . . .
H14 H 0.2271 0.3819 -0.4159 0.081 Uiso 1 1 calc R . .
C15 C 0.28413(11) 0.3483(3) -0.37777(17) 0.0618(10) Uani 1 1 d . . .
H15 H 0.2869 0.3059 -0.4142 0.074 Uiso 1 1 calc R . .
C16 C 0.31608(9) 0.3644(2) -0.32486(15) 0.0449(8) Uani 1 1 d . . .
H16A H 0.3409 0.3345 -0.3258 0.054 Uiso 1 1 calc R . .
C17 C 0.50293(7) 0.74433(19) -0.12533(12) 0.0253(5) Uani 1 1 d . . .
C18 C 0.48550(7) 0.77755(19) -0.19029(12) 0.0279(6) Uani 1 1 d . . .
H18A H 0.4797 0.7335 -0.2278 0.034 Uiso 1 1 calc R . .
C19 C 0.47653(8) 0.8755(2) -0.20015(13) 0.0301(6) Uani 1 1 d . . .
H19 H 0.4644 0.8978 -0.2446 0.036 Uiso 1 1 calc R . .
C20 C 0.48490(8) 0.9414(2) -0.14659(13) 0.0313(6) Uani 1 1 d . . .
C21 C 0.50302(8) 0.9065(2) -0.08187(13) 0.0357(6) Uani 1 1 d . . .
H21 H 0.5093 0.9508 -0.0446 0.043 Uiso 1 1 calc R . .
C22 C 0.51201(8) 0.8095(2) -0.07064(12) 0.0309(6) Uani 1 1 d . . .
H22 H 0.5243 0.7872 -0.0262 0.037 Uiso 1 1 calc R . .
C23 C 0.47465(10) 1.0473(2) -0.15751(15) 0.0437(7) Uani 1 1 d . . .
H23A H 0.4882 1.0847 -0.1176 0.065 Uiso 1 1 calc R . .
H23B H 0.4458 1.0557 -0.1633 0.065 Uiso 1 1 calc R . .
H23C H 0.4833 1.0704 -0.1987 0.065 Uiso 1 1 calc R . .
C24 C 0.34926(11) 0.3806(2) 0.0797(2) 0.0620(10) Uani 1 1 d . . .
H24A H 0.3427 0.3700 0.0300 0.093 Uiso 1 1 calc R . .
H24B H 0.3248 0.3793 0.0980 0.093 Uiso 1 1 calc R . .
H24C H 0.3672 0.3290 0.1014 0.093 Uiso 1 1 calc R . .
C25 C 0.36952(8) 0.4788(2) 0.09478(14) 0.0354(6) Uani 1 1 d . . .
H25 H 0.3948 0.4766 0.0771 0.042 Uiso 1 1 calc R . .
C26 C 0.38077(9) 0.4962(2) 0.17153(15) 0.0459(8) Uani 1 1 d . . .
H26A H 0.3566 0.5030 0.1902 0.069 Uiso 1 1 calc R . .
H26B H 0.3966 0.5558 0.1805 0.069 Uiso 1 1 calc R . .
H26C H 0.3964 0.4410 0.1936 0.069 Uiso 1 1 calc R . .
C27 C 0.34342(7) 0.56117(19) 0.05545(12) 0.0265(5) Uani 1 1 d . . .
C28 C 0.30538(8) 0.5682(2) 0.07886(13) 0.0307(6) Uani 1 1 d . . .
C29 C 0.27540(8) 0.5754(2) 0.10077(14) 0.0341(6) Uani 1 1 d . . .
C30 C 0.23913(8) 0.5824(2) 0.12557(14) 0.0373(7) Uani 1 1 d . . .
C31 C 0.23778(9) 0.5507(3) 0.19136(16) 0.0584(10) Uani 1 1 d . . .
H31 H 0.2611 0.5261 0.2204 0.070 Uiso 1 1 calc R . .
C32 C 0.20228(10) 0.5550(3) 0.21455(18) 0.0726(13) Uani 1 1 d . . .
H32 H 0.2014 0.5335 0.2596 0.087 Uiso 1 1 calc R . .
C33 C 0.16845(9) 0.5900(3) 0.17269(18) 0.0656(11) Uani 1 1 d . . .
H33 H 0.1441 0.5912 0.1884 0.079 Uiso 1 1 calc R . .
C34 C 0.20496(9) 0.6201(2) 0.08431(15) 0.0448(8) Uani 1 1 d . . .
H34 H 0.2057 0.6436 0.0397 0.054 Uiso 1 1 calc R . .
C35 C 0.36491(7) 0.66113(18) 0.06772(12) 0.0242(5) Uani 1 1 d . . .
H35 H 0.3731 0.6715 0.1184 0.029 Uiso 1 1 calc R . .
C36 C 0.33816(8) 0.74513(19) 0.03776(14) 0.0303(6) Uani 1 1 d . . .
C37 C 0.29975(12) 0.8767(3) 0.0688(2) 0.0691(11) Uani 1 1 d . . .
H37A H 0.3047 0.9247 0.1067 0.083 Uiso 1 1 calc R . .
H37B H 0.3066 0.9075 0.0278 0.083 Uiso 1 1 calc R . .
C38 C 0.25958(12) 0.8507(3) 0.0547(3) 0.0979(17) Uani 1 1 d . . .
H38A H 0.2433 0.9080 0.0389 0.147 Uiso 1 1 calc R . .
H38B H 0.2523 0.8251 0.0964 0.147 Uiso 1 1 calc R . .
H38C H 0.2550 0.8006 0.0189 0.147 Uiso 1 1 calc R . .
C39 C 0.42530(8) 0.8441(2) 0.06496(13) 0.0304(6) Uani 1 1 d . . .
C40 C 0.41497(9) 0.8940(2) 0.11934(15) 0.0425(7) Uani 1 1 d . . .
H40 H 0.4178 0.8645 0.1633 0.051 Uiso 1 1 calc R . .
C41 C 0.40028(11) 0.9882(2) 0.10801(18) 0.0553(9) Uani 1 1 d . . .
H41 H 0.3930 1.0229 0.1449 0.066 Uiso 1 1 calc R . .
C42 C 0.39596(10) 1.0324(2) 0.04484(18) 0.0510(8) Uani 1 1 d . . .
C43 C 0.40722(9) 0.9810(2) -0.00798(16) 0.0435(7) Uani 1 1 d . . .
H43 H 0.4050 1.0111 -0.0516 0.052 Uiso 1 1 calc R . .
C44 C 0.42160(8) 0.8876(2) 0.00100(13) 0.0343(6) Uani 1 1 d . . .
H44 H 0.4289 0.8532 -0.0360 0.041 Uiso 1 1 calc R . .
C45 C 0.37897(13) 1.1328(3) 0.0326(2) 0.0810(14) Uani 1 1 d . . .
H45A H 0.3740 1.1473 -0.0166 0.122 Uiso 1 1 calc R . .
H45B H 0.3979 1.1801 0.0575 0.122 Uiso 1 1 calc R . .
H45C H 0.3539 1.1366 0.0490 0.122 Uiso 1 1 calc R . .
C46 C 0.12509(11) -0.0644(3) -0.16069(17) 0.0666(11) Uani 1 1 d . . .
H46A H 0.1493 -0.0629 -0.1798 0.100 Uiso 1 1 calc R . .
H46B H 0.1085 -0.0080 -0.1773 0.100 Uiso 1 1 calc R . .
H46C H 0.1103 -0.1243 -0.1753 0.100 Uiso 1 1 calc R . .
C47 C 0.13640(9) -0.0616(2) -0.08273(15) 0.0446(8) Uani 1 1 d . . .
H47 H 0.1111 -0.0593 -0.0652 0.053 Uiso 1 1 calc R . .
C48 C 0.16099(8) 0.0297(2) -0.05451(13) 0.0348(6) Uani 1 1 d . . .
C49 C 0.15830(12) -0.1534(3) -0.0542(2) 0.0708(11) Uani 1 1 d . . .
H49A H 0.1420 -0.2104 -0.0707 0.106 Uiso 1 1 calc R . .
H49B H 0.1634 -0.1517 -0.0039 0.106 Uiso 1 1 calc R . .
H49C H 0.1836 -0.1574 -0.0695 0.106 Uiso 1 1 calc R . .
C50 C 0.19926(8) 0.0329(2) -0.07721(14) 0.0391(7) Uani 1 1 d . . .
C51 C 0.22924(8) 0.0404(2) -0.09832(14) 0.0387(7) Uani 1 1 d . . .
C52 C 0.26486(8) 0.0542(2) -0.12510(14) 0.0377(7) Uani 1 1 d . . .
C53 C 0.27104(11) 0.1424(3) -0.15476(19) 0.0619(10) Uani 1 1 d . . .
H53 H 0.2522 0.1935 -0.1570 0.074 Uiso 1 1 calc R . .
C54 C 0.30524(14) 0.1553(4) -0.1813(2) 0.0877(15) Uani 1 1 d . . .
H54 H 0.3096 0.2157 -0.2018 0.105 Uiso 1 1 calc R . .
C55 C 0.33227(13) 0.0837(5) -0.1785(2) 0.0896(17) Uani 1 1 d . . .
H55 H 0.3555 0.0941 -0.1966 0.107 Uiso 1 1 calc R . .
C56 C 0.32644(10) -0.0037(4) -0.1498(2) 0.0818(15) Uani 1 1 d . . .
H56 H 0.3455 -0.0540 -0.1485 0.098 Uiso 1 1 calc R . .
C57 C 0.29271(9) -0.0198(3) -0.12243(17) 0.0539(9) Uani 1 1 d . . .
H57 H 0.2888 -0.0807 -0.1022 0.065 Uiso 1 1 calc R . .
C58 C 0.13765(8) 0.1245(2) -0.07958(12) 0.0332(6) Uani 1 1 d . . .
H58 H 0.1275 0.1178 -0.1301 0.040 Uiso 1 1 calc R . .
C59 C 0.16361(8) 0.2150(2) -0.06841(14) 0.0387(7) Uani 1 1 d . . .
C60 C 0.18927(13) 0.3409(3) 0.00905(19) 0.0701(12) Uani 1 1 d . . .
H60A H 0.2159 0.3352 -0.0026 0.084 Uiso 1 1 calc R A 1
H60B H 0.1747 0.3950 -0.0178 0.084 Uiso 1 1 calc R A 1
C61 C 0.1927(2) 0.3571(5) 0.0818(3) 0.076(2) Uani 0.595(7) 1 d P B 1
H61A H 0.1664 0.3722 0.0912 0.114 Uiso 0.595(7) 1 calc PR B 1
H61B H 0.2108 0.4117 0.0964 0.114 Uiso 0.595(7) 1 calc PR B 1
H61C H 0.2032 0.2984 0.1070 0.114 Uiso 0.595(7) 1 calc PR B 1
C61' C 0.2280(2) 0.3370(5) 0.0309(4) 0.047(2) Uani 0.405(7) 1 d P B 2
H61D H 0.2385 0.4031 0.0395 0.071 Uiso 0.405(7) 1 calc PR B 2
H61E H 0.2402 0.3058 -0.0041 0.071 Uiso 0.405(7) 1 calc PR B 2
H61F H 0.2341 0.2992 0.0734 0.071 Uiso 0.405(7) 1 calc PR B 2
C62 C 0.07445(8) 0.3101(2) -0.08598(13) 0.0339(6) Uani 1 1 d . . .
C63 C 0.08204(8) 0.3531(2) -0.14534(13) 0.0360(6) Uani 1 1 d . . .
H63 H 0.0802 0.3159 -0.1861 0.043 Uiso 1 1 calc R . .
C64 C 0.09226(9) 0.4500(2) -0.14464(14) 0.0411(7) Uani 1 1 d . . .
H64 H 0.0974 0.4793 -0.1852 0.049 Uiso 1 1 calc R . .
C65 C 0.09515(10) 0.5056(2) -0.08568(15) 0.0442(7) Uani 1 1 d . . .
C66 C 0.08782(11) 0.4606(2) -0.02687(15) 0.0513(8) Uani 1 1 d . . .
H66 H 0.0901 0.4977 0.0140 0.062 Uiso 1 1 calc R . .
C67 C 0.07740(10) 0.3644(2) -0.02613(14) 0.0445(8) Uani 1 1 d . . .
H67 H 0.0723 0.3354 0.0145 0.053 Uiso 1 1 calc R . .
C68 C 0.10662(12) 0.6109(2) -0.08567(19) 0.0628(10) Uani 1 1 d . . .
H68A H 0.1349 0.6162 -0.0871 0.094 Uiso 1 1 calc R . .
H68B H 0.1017 0.6422 -0.0439 0.094 Uiso 1 1 calc R . .
H68C H 0.0907 0.6431 -0.1260 0.094 Uiso 1 1 calc R . .
C69 C 0.08302(9) -0.2209(2) 0.10804(15) 0.0411(7) Uani 1 1 d . . .
H69A H 0.0911 -0.2098 0.0641 0.062 Uiso 1 1 calc R . .
H69B H 0.0649 -0.2767 0.1038 0.062 Uiso 1 1 calc R . .
H69C H 0.1066 -0.2340 0.1437 0.062 Uiso 1 1 calc R . .
C70 C 0.04856(9) -0.1472(2) 0.19512(15) 0.0420(7) Uani 1 1 d . . .
H70A H 0.0327 -0.0915 0.2048 0.063 Uiso 1 1 calc R . .
H70B H 0.0720 -0.1542 0.2322 0.063 Uiso 1 1 calc R . .
H70C H 0.0324 -0.2064 0.1919 0.063 Uiso 1 1 calc R . .
C71 C 0.06186(7) -0.13049(19) 0.12738(13) 0.0290(6) Uani 1 1 d . . .
H71 H 0.0374 -0.1204 0.0910 0.035 Uiso 1 1 calc R . .
C72 C 0.08834(7) -0.03980(19) 0.12842(11) 0.0243(5) Uani 1 1 d . . .
C73 C 0.12474(7) -0.0498(2) 0.18143(12) 0.0287(6) Uani 1 1 d . . .
C74 C 0.15204(8) -0.0638(2) 0.22811(13) 0.0328(6) Uani 1 1 d . . .
C75 C 0.18488(8) -0.0846(2) 0.28407(13) 0.0354(6) Uani 1 1 d . . .
C76 C 0.19875(9) -0.0151(3) 0.33467(15) 0.0481(8) Uani 1 1 d . . .
H76 H 0.1864 0.0469 0.3331 0.058 Uiso 1 1 calc R . .
C77 C 0.23064(10) -0.0376(3) 0.38715(17) 0.0612(10) Uani 1 1 d . . .
H77 H 0.2402 0.0095 0.4214 0.073 Uiso 1 1 calc R . .
C78 C 0.24840(10) -0.1266(3) 0.39009(18) 0.0603(10) Uani 1 1 d . . .
H78 H 0.2704 -0.1409 0.4261 0.072 Uiso 1 1 calc R . .
C79 C 0.23477(10) -0.1953(3) 0.34143(19) 0.0640(10) Uani 1 1 d . . .
H79 H 0.2470 -0.2575 0.3441 0.077 Uiso 1 1 calc R . .
C80 C 0.20317(9) -0.1745(3) 0.28829(16) 0.0502(8) Uani 1 1 d . . .
H80 H 0.1940 -0.2225 0.2544 0.060 Uiso 1 1 calc R . .
C81 C 0.06611(7) 0.05557(18) 0.14161(11) 0.0237(5) Uani 1 1 d . . .
H81 H 0.0580 0.0497 0.1870 0.028 Uiso 1 1 calc R . .
C82 C 0.09330(7) 0.1430(2) 0.14394(12) 0.0287(6) Uani 1 1 d . . .
C83 C 0.14060(11) 0.2434(3) 0.21583(16) 0.0579(10) Uani 1 1 d . . .
H83A H 0.1593 0.2346 0.2603 0.069 Uiso 1 1 calc R C 1
H83B H 0.1561 0.2369 0.1791 0.069 Uiso 1 1 calc R C 1
C84 C 0.12599(17) 0.3323(4) 0.2136(3) 0.0550(17) Uani 0.624(6) 1 d P D 1
H84A H 0.1097 0.3391 0.2485 0.083 Uiso 0.624(6) 1 calc PR D 1
H84B H 0.1096 0.3445 0.1681 0.083 Uiso 0.624(6) 1 calc PR D 1
H84C H 0.1479 0.3794 0.2227 0.083 Uiso 0.624(6) 1 calc PR D 1
C84' C 0.1760(2) 0.2296(7) 0.1966(4) 0.049(3) Uani 0.376(6) 1 d P D 2
H84D H 0.1713 0.2105 0.1482 0.074 Uiso 0.376(6) 1 calc PR D 2
H84E H 0.1909 0.1781 0.2248 0.074 Uiso 0.376(6) 1 calc PR D 2
H84F H 0.1914 0.2901 0.2030 0.074 Uiso 0.376(6) 1 calc PR D 2
C85 C -0.00187(7) 0.23735(18) 0.11871(12) 0.0251(5) Uani 1 1 d . . .
C86 C -0.00683(9) 0.2973(2) 0.06137(13) 0.0413(7) Uani 1 1 d . . .
H86 H -0.0154 0.2709 0.0167 0.050 Uiso 1 1 calc R . .
C87 C 0.00070(11) 0.3949(2) 0.06994(14) 0.0489(8) Uani 1 1 d . . .
H87 H -0.0030 0.4358 0.0307 0.059 Uiso 1 1 calc R . .
C88 C 0.01367(8) 0.4358(2) 0.13472(13) 0.0345(6) Uani 1 1 d . . .
C89 C 0.01818(8) 0.3756(2) 0.19066(13) 0.0334(6) Uani 1 1 d . . .
H89 H 0.0267 0.4022 0.2353 0.040 Uiso 1 1 calc R . .
C90 C 0.01058(8) 0.2764(2) 0.18345(12) 0.0317(6) Uani 1 1 d . . .
H90 H 0.0139 0.2357 0.2228 0.038 Uiso 1 1 calc R . .
C91 C 0.02262(11) 0.5428(2) 0.14352(16) 0.0499(8) Uani 1 1 d . . .
H91A H 0.0058 0.5790 0.1062 0.075 Uiso 1 1 calc R . .
H91B H 0.0507 0.5543 0.1424 0.075 Uiso 1 1 calc R . .
H91C H 0.0173 0.5647 0.1876 0.075 Uiso 1 1 calc R . .
C92 C 0.16977(9) 0.6235(3) 0.10817(17) 0.0553(9) Uani 1 1 d . . .
H92 H 0.1464 0.6490 0.0797 0.066 Uiso 1 1 calc R . .
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
O2 S1 O1 120.22(11) . . ?
O2 S1 N1 107.01(11) . . ?
O1 S1 N1 105.54(11) . . ?
O2 S1 C17 108.65(11) . . ?
O1 S1 C17 107.22(11) . . ?
N1 S1 C17 107.59(11) . . ?
O8 S2 O7 120.07(11) . . ?
O8 S2 N2 107.53(11) . . ?
O7 S2 N2 105.58(10) . . ?
O8 S2 C39 107.42(12) . . ?
O7 S2 C39 109.05(12) . . ?
N2 S2 C39 106.44(12) . . ?
O14 S3 O15 120.30(11) . . ?
O14 S3 N3 107.27(12) . . ?
O15 S3 N3 105.93(11) . . ?
O14 S3 C62 107.08(12) . . ?
O15 S3 C62 108.38(12) . . ?
N3 S3 C62 107.26(12) . . ?
O20 S4 O19 120.53(11) . . ?
O20 S4 N4 107.60(11) . . ?
O19 S4 N4 105.41(10) . . ?
O20 S4 C85 108.18(11) . . ?
O19 S4 C85 107.43(11) . . ?
N4 S4 C85 106.98(11) . . ?
C5 O3 C7 116.0(2) . . ?
C36 O11 C37 117.1(2) . . ?
C59 O12 C60 115.9(2) . . ?
C82 O17 C83 116.5(2) . . ?
C4 N1 S1 119.42(15) . . ?
C35 N2 S2 118.97(15) . . ?
C58 N3 S3 119.87(17) . . ?
C81 N4 S4 119.85(15) . . ?
C6 C1 C2 110.2(2) . . ?
C6 C1 C3 112.7(2) . . ?
C2 C1 C3 110.5(2) . . ?
O6 C3 C9 107.47(19) . . ?
O6 C3 C1 110.55(18) . . ?
C9 C3 C1 110.3(2) . . ?
O6 C3 C4 107.49(19) . . ?
C9 C3 C4 109.35(19) . . ?
C1 C3 C4 111.55(19) . . ?
N1 C4 C5 110.69(19) . . ?
N1 C4 C3 108.64(18) . . ?
C5 C4 C3 111.55(19) . . ?
O5 C5 O3 124.7(2) . . ?
O5 C5 C4 124.0(2) . . ?
O3 C5 C4 111.3(2) . . ?
O3 C7 C8 111.6(3) . . ?
C10 C9 C3 175.1(3) . . ?
C9 C10 C11 176.9(3) . . ?
C12 C11 C16 118.7(3) . . ?
C12 C11 C10 121.9(2) . . ?
C16 C11 C10 119.3(2) . . ?
C11 C12 C13 119.7(3) . . ?
C14 C13 C12 120.5(3) . . ?
C15 C14 C13 119.7(3) . . ?
C14 C15 C16 120.8(3) . . ?
C15 C16 C11 120.6(3) . . ?
C18 C17 C22 120.1(2) . . ?
C18 C17 S1 120.50(19) . . ?
C22 C17 S1 119.37(19) . . ?
C19 C18 C17 119.6(2) . . ?
C20 C19 C18 121.4(2) . . ?
C19 C20 C21 118.0(3) . . ?
C19 C20 C23 121.1(2) . . ?
C21 C20 C23 120.9(2) . . ?
C22 C21 C20 121.7(2) . . ?
C21 C22 C17 119.2(2) . . ?
C26 C25 C24 110.6(3) . . ?
C26 C25 C27 113.3(2) . . ?
C24 C25 C27 110.7(2) . . ?
O9 C27 C28 106.7(2) . . ?
O9 C27 C25 111.0(2) . . ?
C28 C27 C25 110.2(2) . . ?
O9 C27 C35 109.4(2) . . ?
C28 C27 C35 108.3(2) . . ?
C25 C27 C35 111.0(2) . . ?
C29 C28 C27 177.0(3) . . ?
C28 C29 C30 178.5(3) . . ?
C34 C30 C31 119.3(3) . . ?
C34 C30 C29 120.7(3) . . ?
C31 C30 C29 120.0(3) . . ?
C32 C31 C30 119.9(3) . . ?
C33 C32 C31 120.3(3) . . ?
C32 C33 C92 120.1(3) . . ?
C92 C34 C30 120.0(3) . . ?
N2 C35 C36 111.0(2) . . ?
N2 C35 C27 108.89(19) . . ?
C36 C35 C27 112.3(2) . . ?
O10 C36 O11 125.3(2) . . ?
O10 C36 C35 124.9(2) . . ?
O11 C36 C35 109.7(2) . . ?
C38 C37 O11 110.6(3) . . ?
C40 C39 C44 120.8(3) . . ?
C40 C39 S2 119.4(2) . . ?
C44 C39 S2 119.5(2) . . ?
C39 C40 C41 118.4(3) . . ?
C42 C41 C40 121.8(3) . . ?
C41 C42 C43 118.2(3) . . ?
C41 C42 C45 121.4(3) . . ?
C43 C42 C45 120.4(3) . . ?
C44 C43 C42 121.7(3) . . ?
C43 C44 C39 119.0(3) . . ?
C49 C47 C46 111.4(3) . . ?
C49 C47 C48 110.2(3) . . ?
C46 C47 C48 113.4(3) . . ?
O16 C48 C50 107.1(2) . . ?
O16 C48 C47 110.6(2) . . ?
C50 C48 C47 111.5(2) . . ?
O16 C48 C58 108.8(2) . . ?
C50 C48 C58 108.0(2) . . ?
C47 C48 C58 110.7(2) . . ?
C51 C50 C48 175.7(3) . . ?
C50 C51 C52 177.1(3) . . ?
C53 C52 C57 119.6(3) . . ?
C53 C52 C51 119.2(3) . . ?
C57 C52 C51 121.2(3) . . ?
C52 C53 C54 119.2(4) . . ?
C55 C54 C53 121.2(4) . . ?
C54 C55 C56 120.2(4) . . ?
C55 C56 C57 120.6(4) . . ?
C52 C57 C56 119.2(4) . . ?
N3 C58 C59 113.4(2) . . ?
N3 C58 C48 108.3(2) . . ?
C59 C58 C48 112.9(2) . . ?
O13 C59 O12 124.1(3) . . ?
O13 C59 C58 123.9(3) . . ?
O12 C59 C58 112.0(2) . . ?
C61' C60 C61 78.7(5) . . ?
C61' C60 O12 118.7(5) . . ?
C61 C60 O12 105.0(3) . . ?
C63 C62 C67 120.2(3) . . ?
C63 C62 S3 119.5(2) . . ?
C67 C62 S3 120.2(2) . . ?
C64 C63 C62 119.6(3) . . ?
C63 C64 C65 121.1(3) . . ?
C64 C65 C66 118.2(3) . . ?
C64 C65 C68 120.4(3) . . ?
C66 C65 C68 121.4(3) . . ?
C67 C66 C65 122.0(3) . . ?
C66 C67 C62 118.9(3) . . ?
C70 C71 C69 110.1(2) . . ?
C70 C71 C72 113.0(2) . . ?
C69 C71 C72 110.6(2) . . ?
O18 C72 C73 108.07(19) . . ?
O18 C72 C71 109.93(19) . . ?
C73 C72 C71 110.4(2) . . ?
O18 C72 C81 107.12(18) . . ?
C73 C72 C81 109.3(2) . . ?
C71 C72 C81 111.96(19) . . ?
C74 C73 C72 173.2(3) . . ?
C73 C74 C75 177.9(3) . . ?
C80 C75 C76 118.9(3) . . ?
C80 C75 C74 119.9(3) . . ?
C76 C75 C74 121.2(3) . . ?
C77 C76 C75 119.4(3) . . ?
C78 C77 C76 120.7(3) . . ?
C77 C78 C79 120.3(3) . . ?
C78 C79 C80 120.2(4) . . ?
C75 C80 C79 120.5(3) . . ?
N4 C81 C82 111.4(2) . . ?
N4 C81 C72 109.27(19) . . ?
C82 C81 C72 110.56(19) . . ?
O4 C82 O17 124.0(2) . . ?
O4 C82 C81 124.1(2) . . ?
O17 C82 C81 111.9(2) . . ?
C84 C83 C84' 118.5(5) . . ?
C84 C83 O17 115.2(4) . . ?
C84' C83 O17 120.4(5) . . ?
C90 C85 C86 119.9(2) . . ?
C90 C85 S4 120.84(19) . . ?
C86 C85 S4 119.2(2) . . ?
C87 C86 C85 119.3(3) . . ?
C86 C87 C88 121.8(3) . . ?
C89 C88 C87 118.0(3) . . ?
C89 C88 C91 120.6(3) . . ?
C87 C88 C91 121.4(3) . . ?
C88 C89 C90 121.4(2) . . ?
C85 C90 C89 119.6(2) . . ?
C33 C92 C34 120.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.4292(18) . ?
S1 O1 1.4330(18) . ?
S1 N1 1.632(2) . ?
S1 C17 1.757(3) . ?
S2 O8 1.4267(18) . ?
S2 O7 1.4382(18) . ?
S2 N2 1.618(2) . ?
S2 C39 1.764(3) . ?
S3 O14 1.4288(18) . ?
S3 O15 1.4370(18) . ?
S3 N3 1.616(2) . ?
S3 C62 1.754(3) . ?
S4 O20 1.4280(17) . ?
S4 O19 1.4347(18) . ?
S4 N4 1.625(2) . ?
S4 C85 1.756(3) . ?
O3 C5 1.326(3) . ?
O3 C7 1.467(3) . ?
O5 C5 1.203(3) . ?
O6 C3 1.438(3) . ?
O9 C27 1.425(3) . ?
O10 C36 1.198(3) . ?
O11 C36 1.342(3) . ?
O11 C37 1.461(4) . ?
O12 C59 1.333(3) . ?
O12 C60 1.458(4) . ?
O13 C59 1.203(3) . ?
O16 C48 1.422(3) . ?
O4 C82 1.207(3) . ?
O17 C82 1.330(3) . ?
O17 C83 1.463(4) . ?
O18 C72 1.436(3) . ?
N1 C4 1.464(3) . ?
N2 C35 1.463(3) . ?
N3 C58 1.464(3) . ?
N4 C81 1.458(3) . ?
C1 C6 1.525(3) . ?
C1 C2 1.532(4) . ?
C1 C3 1.547(3) . ?
C3 C9 1.475(3) . ?
C3 C4 1.562(3) . ?
C4 C5 1.525(3) . ?
C7 C8 1.488(5) . ?
C9 C10 1.190(3) . ?
C10 C11 1.436(4) . ?
C11 C12 1.383(4) . ?
C11 C16 1.390(4) . ?
C12 C13 1.388(4) . ?
C13 C14 1.380(5) . ?
C14 C15 1.351(5) . ?
C15 C16 1.376(4) . ?
C17 C18 1.387(3) . ?
C17 C22 1.396(3) . ?
C18 C19 1.386(4) . ?
C19 C20 1.384(4) . ?
C20 C21 1.397(4) . ?
C20 C23 1.503(4) . ?
C21 C22 1.377(4) . ?
C24 C25 1.521(4) . ?
C25 C26 1.517(4) . ?
C25 C27 1.554(4) . ?
C27 C28 1.476(3) . ?
C27 C35 1.556(3) . ?
C28 C29 1.200(3) . ?
C29 C30 1.433(4) . ?
C30 C34 1.389(4) . ?
C30 C31 1.389(4) . ?
C31 C32 1.389(4) . ?
C32 C33 1.373(5) . ?
C33 C92 1.373(4) . ?
C34 C92 1.386(4) . ?
C35 C36 1.520(4) . ?
C37 C38 1.397(5) . ?
C39 C40 1.386(4) . ?
C39 C44 1.388(4) . ?
C40 C41 1.392(4) . ?
C41 C42 1.377(5) . ?
C42 C43 1.385(4) . ?
C42 C45 1.499(5) . ?
C43 C44 1.375(4) . ?
C46 C47 1.522(4) . ?
C47 C49 1.520(5) . ?
C47 C48 1.553(4) . ?
C48 C50 1.474(4) . ?
C48 C58 1.558(4) . ?
C50 C51 1.192(4) . ?
C51 C52 1.442(4) . ?
C52 C53 1.384(5) . ?
C52 C57 1.390(4) . ?
C53 C54 1.393(5) . ?
C54 C55 1.347(7) . ?
C55 C56 1.362(7) . ?
C56 C57 1.394(5) . ?
C58 C59 1.520(4) . ?
C60 C61' 1.312(8) . ?
C60 C61 1.445(7) . ?
C62 C63 1.392(4) . ?
C62 C67 1.392(4) . ?
C63 C64 1.377(4) . ?
C64 C65 1.386(4) . ?
C65 C66 1.390(4) . ?
C65 C68 1.501(4) . ?
C66 C67 1.372(4) . ?
C69 C71 1.528(4) . ?
C70 C71 1.525(4) . ?
C71 C72 1.541(3) . ?
C72 C73 1.470(3) . ?
C72 C81 1.566(3) . ?
C73 C74 1.194(3) . ?
C74 C75 1.444(4) . ?
C75 C80 1.381(4) . ?
C75 C76 1.400(4) . ?
C76 C77 1.386(4) . ?
C77 C78 1.363(5) . ?
C78 C79 1.366(5) . ?
C79 C80 1.383(4) . ?
C81 C82 1.517(3) . ?
C83 C84 1.318(6) . ?
C83 C84' 1.360(8) . ?
C85 C90 1.381(3) . ?
C85 C86 1.390(3) . ?
C86 C87 1.371(4) . ?
C87 C88 1.394(4) . ?
C88 C89 1.371(4) . ?
C88 C91 1.505(4) . ?
C89 C90 1.391(4) . ?
