#------------------------------------------------------------------------------
#$Date: 2022-08-02 23:57:45 +0200 (Tue 02 de Aug de 2022) $
#$Revision: 277043 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/04/7130466.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_7130466
loop_
_publ_author_name
'Yu, Ke-Yin'
'Ge, Xiao-Min'
'Fan, Yi-Jun'
'Liu, Xiao-Tao'
'Yang, Xue'
'Yang, Yu-Han'
'Zhao, Xian-He'
'An, Xian-Tao'
'Fan, Chun-An'
_publ_section_title
;
 Iron(III)-catalyzed tandem annulation of indolyl-substituted
 p-quinone methides with ynamides for the synthesis of
 cyclopenta[b]indoles.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8710
_journal_page_last               8713
_journal_paper_doi               10.1039/d2cc03252j
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C47 H50 N2 O4 S'
_chemical_formula_sum            'C47 H50 N2 O4 S'
_chemical_formula_weight         738.95
_chemical_melting_point          472.6(5)
_chemical_name_systematic        'Compound 3ea'
_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     dual
_audit_creation_date             2021-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-15 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.888(2)
_cell_angle_beta                 96.944(2)
_cell_angle_gamma                114.393(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4470(2)
_cell_length_b                   13.1078(3)
_cell_length_c                   15.0372(2)
_cell_measurement_reflns_used    10961
_cell_measurement_temperature    302.34(10)
_cell_measurement_theta_max      76.1110
_cell_measurement_theta_min      3.9640
_cell_volume                     2070.93(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      302.34(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 114.00   0.50    0.38    --   46.57  37.00 -47.00  160
  2  ω    132.00 162.00   0.50    0.83    --  104.25  45.00 -30.00   60
  3  ω     96.00 128.00   0.50    0.83    --  104.25  45.00 -30.00   64
  4  ω     92.00 174.00   0.50    0.83    --  104.25  37.00 -47.00  164
  5  ω     91.00 172.00   0.50    0.83    --  104.25  15.00  60.00  162
  6  ω     -8.00  29.00   0.50    0.38    --   46.57 -19.00   0.00   74
  7  ω    -11.00  69.00   0.50    0.38    --   46.57 -77.00 150.00  160
  8  ω      0.00  44.00   0.50    0.38    --   46.57 -37.00 156.00   88
  9  ω     32.00  58.00   0.50    0.83    --  104.25-125.00 150.00   52
 10  ω     38.00  64.00   0.50    0.83    --  104.25-125.00 120.00   52
 11  ω     35.00 107.00   0.50    0.83    --  104.25-107.00 164.46  144
 12  ω     87.00 112.00   0.50    0.83    --  104.25-125.00 120.00   50
 13  ω     45.00  95.00   0.50    0.83    --  104.25 -94.00  30.00  100
 14  ω     32.00  98.00   0.50    0.83    --  104.25-125.00   0.00  132
 15  ω     38.00 108.00   0.50    0.83    --  104.25-125.00 -90.00  140
 16  ω     33.00  82.00   0.50    0.83    --  104.25 -94.00 -90.00   98
 17  ω     38.00  97.00   0.50    0.83    --  104.25 -94.00-180.00  118
 18  ω     36.00  63.00   0.50    0.83    --  104.25 -61.00-180.00   54
 19  ω     35.00  69.00   0.50    0.83    --  104.25 -61.00 -60.00   68
 20  ω     32.00  60.00   0.50    0.83    --  104.25 -61.00 -30.00   56
 21  ω     34.00  60.00   0.50    0.83    --  104.25 -61.00  30.00   52
 22  ω   -125.00 -38.00   0.50    0.83    -- -102.00 143.00  52.63  174
 23  ω    -98.00 -72.00   0.50    0.83    -- -102.00 125.00 150.00   52
 24  ω    -68.00 -29.00   0.50    0.83    -- -102.00 125.00 150.00   78
 25  ω   -121.00 -60.00   0.50    0.83    -- -102.00 138.00 -28.28  122
 26  ω   -122.00 -86.00   0.50    0.83    -- -102.00 139.00 -84.10   72
 27  ω    -94.00 -68.00   0.50    0.83    -- -102.00 125.00-120.00   52
 28  ω   -107.00 -78.00   0.50    0.83    -- -102.00 108.00 -90.30   58
 29  ω    -62.00 -30.00   0.50    0.83    -- -102.00 125.00-120.00   64
 30  ω    -40.00  -8.00   0.50    0.38    --  -46.57  37.00 -47.00   64
 31  ω    -50.00  11.00   0.50    0.38    --  -46.57  57.00 -30.00  122
 32  ω   -103.00 -67.00   0.50    0.83    -- -102.00  77.00 120.00   72
 33  ω    -61.00 -35.00   0.50    0.83    -- -102.00  61.00  90.00   52
 34  ω   -175.00-138.00   0.50    0.83    -- -102.00 -61.00-120.00   74
 35  ω   -175.00 -89.00   0.50    0.83    -- -102.00 -15.00-120.00  172
 36  ω   -129.00-100.00   0.50    0.83    -- -102.00 -61.00-120.00   58
 37  ω   -120.00 -43.00   0.50    0.38    --  -46.57 -37.00 156.00  154
 38  ω   -175.00-107.00   0.50    0.83    -- -102.00 -37.00 156.00  136
 39  ω   -112.00 -86.00   0.50    0.38    --  -46.57-125.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0202667000
_diffrn_orient_matrix_UB_12      0.1080707000
_diffrn_orient_matrix_UB_13      -0.0306581000
_diffrn_orient_matrix_UB_21      0.1028745000
_diffrn_orient_matrix_UB_22      -0.0110926000
_diffrn_orient_matrix_UB_23      -0.0426487000
_diffrn_orient_matrix_UB_31      -0.0943082000
_diffrn_orient_matrix_UB_32      -0.0854422000
_diffrn_orient_matrix_UB_33      -0.0972576000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26451
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.392
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             788
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and methanol'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0469
_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)+(0.0659P)²+0.2917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6456
_reflns_number_total             8323
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03252j2.cif
_cod_data_source_block           Compound_3ea
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '472.15-473.15' was changed
to '472.6(5)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2070.93(7)
_cod_database_code               7130466
_shelx_shelxl_version_number     2018/1
_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.
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C15(H15)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C31(H31),
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C42(H42), C43(H43),
  C45(H45), C46(H46)
1.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C)
1.d Idealised tetrahedral OH refined as rotating group:
 O007(H007)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.624
_oxdiff_exptl_absorpt_empirical_full_min 0.257
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
S1 S 0.26897(4) -0.00539(3) 0.30498(3) 0.04107(12) Uani 1 1 d . . . . .
O1 O 0.21077(12) -0.06208(11) 0.20466(9) 0.0531(3) Uani 1 1 d . . . . .
O2 O 0.23049(13) -0.06912(12) 0.36829(10) 0.0553(3) Uani 1 1 d . . . . .
O3 O 0.41318(13) 0.19154(15) 0.51433(10) 0.0634(4) Uani 1 1 d . . . . .
O007 O 0.21283(19) 0.70899(14) 0.22817(13) 0.0763(5) Uani 1 1 d . . . . .
H007 H 0.189370 0.727953 0.275770 0.114 Uiso 1 1 calc R U . . .
N1 N -0.01549(13) 0.11825(13) 0.08454(10) 0.0443(3) Uani 1 1 d . . . . .
N2 N 0.25170(12) 0.11700(12) 0.34197(9) 0.0374(3) Uani 1 1 d . . . . .
C1 C 0.20927(17) 0.59979(15) 0.21382(13) 0.0461(4) Uani 1 1 d . . . . .
C2 C 0.15160(16) 0.52780(15) 0.26499(13) 0.0452(4) Uani 1 1 d . . . . .
C3 C 0.16175(16) 0.42310(15) 0.25060(12) 0.0447(4) Uani 1 1 d . . . . .
H3 H 0.128021 0.375556 0.285883 0.054 Uiso 1 1 calc R U . . .
C4 C 0.22029(15) 0.38737(14) 0.18560(12) 0.0400(3) Uani 1 1 d . . . . .
C5 C 0.26892(16) 0.45679(15) 0.13222(12) 0.0425(4) Uani 1 1 d . . . . .
H5 H 0.305745 0.431034 0.086952 0.051 Uiso 1 1 calc R U . . .
C6 C 0.26485(16) 0.56403(15) 0.14366(12) 0.0438(4) Uani 1 1 d . . . . .
C7 C 0.3150(2) 0.63712(18) 0.08026(15) 0.0589(5) Uani 1 1 d . . . . .
C8 C 0.2127(3) 0.6510(3) 0.0254(2) 0.1042(10) Uani 1 1 d . . . . .
H8A H 0.142859 0.573616 -0.007177 0.156 Uiso 1 1 calc R U . . .
H8B H 0.241179 0.686534 -0.020658 0.156 Uiso 1 1 calc R U . . .
H8C H 0.190062 0.701640 0.069739 0.156 Uiso 1 1 calc R U . . .
C9 C 0.4218(3) 0.7606(2) 0.1407(2) 0.0888(9) Uani 1 1 d . . . . .
H9A H 0.394527 0.803669 0.187176 0.133 Uiso 1 1 calc R U . . .
H9B H 0.451614 0.804609 0.099827 0.133 Uiso 1 1 calc R U . . .
H9C H 0.486402 0.751057 0.173213 0.133 Uiso 1 1 calc R U . . .
C10 C 0.3637(3) 0.5747(2) 0.00626(19) 0.0827(8) Uani 1 1 d . . . . .
H10A H 0.427399 0.564092 0.038802 0.124 Uiso 1 1 calc R U . . .
H10B H 0.395893 0.623063 -0.031261 0.124 Uiso 1 1 calc R U . . .
H10C H 0.298327 0.497819 -0.035101 0.124 Uiso 1 1 calc R U . . .
C11 C 0.0748(2) 0.55852(19) 0.33085(16) 0.0606(5) Uani 1 1 d . . . . .
C12 C 0.1552(3) 0.6685(2) 0.42148(18) 0.0818(7) Uani 1 1 d . . . . .
H12A H 0.210610 0.651960 0.458046 0.123 Uiso 1 1 calc R U . . .
H12B H 0.104426 0.686869 0.459452 0.123 Uiso 1 1 calc R U . . .
H12C H 0.201097 0.735698 0.403823 0.123 Uiso 1 1 calc R U . . .
C13 C -0.0221(3) 0.5798(3) 0.2759(2) 0.0951(9) Uani 1 1 d . . . . .
H13A H 0.018046 0.648096 0.257842 0.143 Uiso 1 1 calc R U . . .
H13B H -0.072249 0.594269 0.316313 0.143 Uiso 1 1 calc R U . . .
H13C H -0.072388 0.510221 0.219360 0.143 Uiso 1 1 calc R U . . .
C14 C 0.0064(3) 0.4552(3) 0.3645(2) 0.0982(10) Uani 1 1 d . . . . .
H14A H -0.045608 0.383802 0.309690 0.147 Uiso 1 1 calc R U . . .
H14B H -0.042403 0.475363 0.403679 0.147 Uiso 1 1 calc R U . . .
H14C H 0.064420 0.441474 0.401113 0.147 Uiso 1 1 calc R U . . .
C15 C 0.21973(16) 0.26723(14) 0.16706(12) 0.0402(4) Uani 1 1 d . . . . .
H15 H 0.252956 0.251097 0.112003 0.048 Uiso 1 1 calc R U . . .
C16 C 0.09643(15) 0.16390(14) 0.14675(11) 0.0404(4) Uani 1 1 d . . . . .
C17 C 0.09514(15) 0.09721(14) 0.20184(11) 0.0391(3) Uani 1 1 d . . . . .
C18 C 0.21728(14) 0.15763(14) 0.26891(11) 0.0362(3) Uani 1 1 d . . . . .
C19 C 0.29135(15) 0.25560(14) 0.25088(12) 0.0394(3) Uani 1 1 d . . . . .
C20 C 0.42263(16) 0.33830(15) 0.29555(13) 0.0448(4) Uani 1 1 d . . . . .
C21 C 0.47586(18) 0.37074(18) 0.39211(15) 0.0583(5) Uani 1 1 d . . . . .
H21 H 0.427229 0.341805 0.430795 0.070 Uiso 1 1 calc R U . . .
C22 C 0.6003(2) 0.4455(2) 0.43179(19) 0.0751(7) Uani 1 1 d . . . . .
H22 H 0.634282 0.465577 0.496550 0.090 Uiso 1 1 calc R U . . .
C23 C 0.6736(2) 0.4902(2) 0.3767(2) 0.0820(7) Uani 1 1 d . . . . .
H23 H 0.757180 0.539848 0.403580 0.098 Uiso 1 1 calc R U . . .
C24 C 0.6225(2) 0.4609(3) 0.2814(2) 0.0868(8) Uani 1 1 d . . . . .
H24 H 0.671818 0.491535 0.243705 0.104 Uiso 1 1 calc R U . . .
C25 C 0.4984(2) 0.3862(2) 0.24096(17) 0.0647(5) Uani 1 1 d . . . . .
H25 H 0.465124 0.367780 0.176365 0.078 Uiso 1 1 calc R U . . .
C26 C -0.02497(15) -0.00169(15) 0.17228(12) 0.0416(4) Uani 1 1 d . . . . .
C27 C -0.09336(16) 0.01530(16) 0.09962(12) 0.0439(4) Uani 1 1 d . . . . .
C28 C -0.21854(17) -0.06480(19) 0.05574(13) 0.0538(5) Uani 1 1 d . . . . .
C29 C -0.2987(2) -0.0489(3) -0.01662(17) 0.0757(7) Uani 1 1 d . . . . .
H29A H -0.296293 0.027625 0.010155 0.114 Uiso 1 1 calc R U . . .
H29B H -0.381268 -0.111474 -0.033125 0.114 Uiso 1 1 calc R U . . .
H29C H -0.269627 -0.052814 -0.073153 0.114 Uiso 1 1 calc R U . . .
C30 C -0.0407(2) 0.1735(2) 0.01842(15) 0.0629(5) Uani 1 1 d . . . . .
H30A H -0.087330 0.212827 0.041525 0.094 Uiso 1 1 calc R U . . .
H30B H -0.086555 0.112777 -0.043774 0.094 Uiso 1 1 calc R U . . .
H30C H 0.035086 0.231175 0.013877 0.094 Uiso 1 1 calc R U . . .
C31 C -0.26716(18) -0.1631(2) 0.08350(15) 0.0646(6) Uani 1 1 d . . . . .
H31 H -0.349169 -0.218698 0.055189 0.078 Uiso 1 1 calc R U . . .
C32 C -0.20030(18) -0.1835(2) 0.15136(15) 0.0627(5) Uani 1 1 d . . . . .
H32 H -0.237716 -0.252183 0.166082 0.075 Uiso 1 1 calc R U . . .
C33 C -0.07945(17) -0.10303(17) 0.19692(14) 0.0514(4) Uani 1 1 d . . . . .
H33 H -0.034983 -0.115849 0.243116 0.062 Uiso 1 1 calc R U . . .
C34 C 0.21754(15) 0.14506(14) 0.43049(12) 0.0404(4) Uani 1 1 d . . . . .
C35 C 0.10275(17) 0.13546(18) 0.42961(14) 0.0524(4) Uani 1 1 d . . . . .
H35 H 0.046737 0.110184 0.371402 0.063 Uiso 1 1 calc R U . . .
C36 C 0.0699(2) 0.1630(2) 0.51438(16) 0.0648(5) Uani 1 1 d . . . . .
H36 H -0.007473 0.156744 0.513106 0.078 Uiso 1 1 calc R U . . .
C37 C 0.1518(2) 0.1994(2) 0.59977(16) 0.0685(6) Uani 1 1 d . . . . .
H37 H 0.129633 0.217451 0.656692 0.082 Uiso 1 1 calc R U . . .
C38 C 0.2670(2) 0.2098(2) 0.60247(14) 0.0644(5) Uani 1 1 d . . . . .
H38 H 0.321948 0.234395 0.661098 0.077 Uiso 1 1 calc R U . . .
C39 C 0.30140(17) 0.18366(17) 0.51819(13) 0.0487(4) Uani 1 1 d . . . . .
C40 C 0.5125(2) 0.2659(3) 0.59840(19) 0.0862(8) Uani 1 1 d . . . . .
H40A H 0.587802 0.275092 0.582981 0.129 Uiso 1 1 calc R U . . .
H40B H 0.500915 0.229547 0.646250 0.129 Uiso 1 1 calc R U . . .
H40C H 0.515688 0.343181 0.622638 0.129 Uiso 1 1 calc R U . . .
C41 C 0.42604(16) 0.04043(16) 0.31733(12) 0.0441(4) Uani 1 1 d . . . . .
C42 C 0.4826(2) 0.0925(2) 0.25665(16) 0.0621(5) Uani 1 1 d . . . . .
H42 H 0.440532 0.111552 0.213879 0.075 Uiso 1 1 calc R U . . .
C43 C 0.6019(2) 0.1161(2) 0.25963(19) 0.0716(6) Uani 1 1 d . . . . .
H43 H 0.639759 0.151821 0.218736 0.086 Uiso 1 1 calc R U . . .
C44 C 0.66671(19) 0.0881(2) 0.32186(16) 0.0619(5) Uani 1 1 d . . . . .
C45 C 0.6089(2) 0.0381(2) 0.38334(16) 0.0667(6) Uani 1 1 d . . . . .
H45 H 0.651282 0.020154 0.426860 0.080 Uiso 1 1 calc R U . . .
C46 C 0.48932(19) 0.0141(2) 0.38165(15) 0.0593(5) Uani 1 1 d . . . . .
H46 H 0.451913 -0.019541 0.423667 0.071 Uiso 1 1 calc R U . . .
C47 C 0.7949(2) 0.1087(3) 0.3209(2) 0.0881(8) Uani 1 1 d . . . . .
H47A H 0.852713 0.183651 0.370339 0.132 Uiso 1 1 calc R U . . .
H47B H 0.807616 0.110964 0.259643 0.132 Uiso 1 1 calc R U . . .
H47C H 0.806114 0.044702 0.332253 0.132 Uiso 1 1 calc R U . . .
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
O1 S1 O2 120.03(8) . . ?
O1 S1 N2 106.62(7) . . ?
O1 S1 C41 106.31(8) . . ?
O2 S1 N2 107.10(7) . . ?
O2 S1 C41 108.42(8) . . ?
N2 S1 C41 107.84(7) . . ?
C39 O3 C40 117.99(18) . . ?
C1 O007 H007 109.5 . . ?
C16 N1 C27 106.75(13) . . ?
C16 N1 C30 123.38(16) . . ?
C27 N1 C30 129.86(16) . . ?
C18 N2 S1 116.58(10) . . ?
C18 N2 C34 118.67(12) . . ?
C34 N2 S1 118.91(10) . . ?
O007 C1 C2 121.58(16) . . ?
O007 C1 C6 115.81(16) . . ?
C2 C1 C6 122.60(15) . . ?
C1 C2 C11 122.40(16) . . ?
C3 C2 C1 116.90(15) . . ?
C3 C2 C11 120.64(16) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.17(15) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C15 119.83(15) . . ?
C5 C4 C3 119.06(15) . . ?
C5 C4 C15 120.85(15) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.35(16) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C7 122.04(15) . . ?
C5 C6 C1 116.66(15) . . ?
C5 C6 C7 121.28(16) . . ?
C8 C7 C6 109.9(2) . . ?
C9 C7 C6 110.88(18) . . ?
C9 C7 C8 110.0(2) . . ?
C9 C7 C10 106.8(2) . . ?
C10 C7 C6 111.36(16) . . ?
C10 C7 C8 107.8(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C2 111.70(18) . . ?
C12 C11 C13 110.0(2) . . ?
C12 C11 C14 106.5(2) . . ?
C13 C11 C2 110.19(19) . . ?
C14 C11 C2 111.02(17) . . ?
C14 C11 C13 107.3(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C15 H15 108.4 . . ?
C4 C15 C19 116.09(14) . . ?
C16 C15 C4 114.50(14) . . ?
C16 C15 H15 108.4 . . ?
C16 C15 C19 100.66(13) . . ?
C19 C15 H15 108.4 . . ?
N1 C16 C15 135.53(15) . . ?
C17 C16 N1 111.78(15) . . ?
C17 C16 C15 112.67(14) . . ?
C16 C17 C18 107.08(14) . . ?
C16 C17 C26 107.35(14) . . ?
C26 C17 C18 145.55(15) . . ?
N2 C18 C17 124.20(14) . . ?
C19 C18 N2 125.88(14) . . ?
C19 C18 C17 109.92(14) . . ?
C18 C19 C15 109.51(14) . . ?
C18 C19 C20 129.03(15) . . ?
C20 C19 C15 121.33(14) . . ?
C21 C20 C19 122.10(16) . . ?
C21 C20 C25 117.48(17) . . ?
C25 C20 C19 120.42(17) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 121.0(2) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.7(2) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.3(2) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(2) . . ?
C25 C24 H24 119.7 . . ?
C20 C25 H25 119.5 . . ?
C24 C25 C20 120.9(2) . . ?
C24 C25 H25 119.5 . . ?
C27 C26 C17 105.61(14) . . ?
C33 C26 C17 134.20(16) . . ?
C33 C26 C27 120.14(16) . . ?
N1 C27 C26 108.45(14) . . ?
N1 C27 C28 130.37(16) . . ?
C28 C27 C26 121.18(17) . . ?
C27 C28 C29 124.4(2) . . ?
C31 C28 C27 115.73(17) . . ?
C31 C28 C29 119.88(19) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N1 C30 H30A 109.5 . . ?
N1 C30 H30B 109.5 . . ?
N1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31 118.2 . . ?
C28 C31 C32 123.66(18) . . ?
C32 C31 H31 118.2 . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.7(2) . . ?
C33 C32 H32 119.7 . . ?
C26 C33 H33 120.8 . . ?
C32 C33 C26 118.50(18) . . ?
C32 C33 H33 120.8 . . ?
C35 C34 N2 120.62(15) . . ?
C35 C34 C39 119.30(16) . . ?
C39 C34 N2 120.07(15) . . ?
C34 C35 H35 119.6 . . ?
C34 C35 C36 120.78(19) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 120.2 . . ?
C37 C36 C35 119.6(2) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(2) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 H38 119.9 . . ?
C37 C38 C39 120.3(2) . . ?
C39 C38 H38 119.9 . . ?
O3 C39 C34 116.52(16) . . ?
O3 C39 C38 124.11(17) . . ?
C38 C39 C34 119.36(19) . . ?
O3 C40 H40A 109.5 . . ?
O3 C40 H40B 109.5 . . ?
O3 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 S1 119.86(13) . . ?
C42 C41 C46 119.99(18) . . ?
C46 C41 S1 119.88(15) . . ?
C41 C42 H42 120.2 . . ?
C41 C42 C43 119.59(19) . . ?
C43 C42 H42 120.2 . . ?
C42 C43 H43 119.2 . . ?
C42 C43 C44 121.7(2) . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C47 121.1(2) . . ?
C45 C44 C43 117.69(19) . . ?
C45 C44 C47 121.2(2) . . ?
C44 C45 H45 119.3 . . ?
C44 C45 C46 121.43(19) . . ?
C46 C45 H45 119.3 . . ?
C41 C46 C45 119.6(2) . . ?
C41 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 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
S1 O1 1.4248(13) . ?
S1 O2 1.4314(13) . ?
S1 N2 1.6595(13) . ?
S1 C41 1.7603(18) . ?
O3 C39 1.362(2) . ?
O3 C40 1.424(3) . ?
O007 H007 0.8200 . ?
O007 C1 1.369(2) . ?
N1 C16 1.365(2) . ?
N1 C27 1.397(2) . ?
N1 C30 1.455(2) . ?
N2 C18 1.4385(19) . ?
N2 C34 1.444(2) . ?
C1 C2 1.403(2) . ?
C1 C6 1.409(3) . ?
C2 C3 1.391(2) . ?
C2 C11 1.544(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(2) . ?
C4 C5 1.379(2) . ?
C4 C15 1.519(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(2) . ?
C6 C7 1.538(2) . ?
C7 C8 1.535(4) . ?
C7 C9 1.529(3) . ?
C7 C10 1.533(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.530(4) . ?
C11 C13 1.542(4) . ?
C11 C14 1.530(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.492(2) . ?
C15 C19 1.534(2) . ?
C16 C17 1.356(2) . ?
C17 C18 1.467(2) . ?
C17 C26 1.427(2) . ?
C18 C19 1.359(2) . ?
C19 C20 1.473(2) . ?
C20 C21 1.387(3) . ?
C20 C25 1.393(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.385(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.366(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.372(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.383(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.426(2) . ?
C26 C33 1.396(3) . ?
C27 C28 1.409(3) . ?
C28 C29 1.501(3) . ?
C28 C31 1.383(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C32 1.390(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.374(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.380(2) . ?
C34 C39 1.396(2) . ?
C35 H35 0.9300 . ?
C35 C36 1.385(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.364(3) . ?
C37 H37 0.9300 . ?
C37 C38 1.378(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.386(3) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.376(3) . ?
C41 C46 1.377(2) . ?
C42 H42 0.9300 . ?
C42 C43 1.378(3) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(3) . ?
C44 C45 1.380(3) . ?
C44 C47 1.507(3) . ?
C45 H45 0.9300 . ?
C45 C46 1.384(3) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
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
S1 N2 C18 C17 72.53(18) . . . . ?
S1 N2 C18 C19 -107.00(17) . . . . ?
S1 N2 C34 C35 -110.01(16) . . . . ?
S1 N2 C34 C39 70.74(19) . . . . ?
S1 C41 C42 C43 -172.92(19) . . . . ?
S1 C41 C46 C45 172.67(17) . . . . ?
O1 S1 N2 C18 -16.48(13) . . . . ?
O1 S1 N2 C34 136.28(12) . . . . ?
O1 S1 C41 C42 42.72(18) . . . . ?
O1 S1 C41 C46 -131.28(16) . . . . ?
O2 S1 N2 C18 -146.15(12) . . . . ?
O2 S1 N2 C34 6.62(14) . . . . ?
O2 S1 C41 C42 173.04(16) . . . . ?
O2 S1 C41 C46 -0.96(18) . . . . ?
O007 C1 C2 C3 -174.96(18) . . . . ?
O007 C1 C2 C11 7.9(3) . . . . ?
O007 C1 C6 C5 176.12(17) . . . . ?
O007 C1 C6 C7 -5.8(3) . . . . ?
N1 C16 C17 C18 -177.04(14) . . . . ?
N1 C16 C17 C26 1.8(2) . . . . ?
N1 C27 C28 C29 -3.9(3) . . . . ?
N1 C27 C28 C31 176.28(18) . . . . ?
N2 S1 C41 C42 -71.31(17) . . . . ?
N2 S1 C41 C46 114.69(16) . . . . ?
N2 C18 C19 C15 179.77(14) . . . . ?
N2 C18 C19 C20 3.9(3) . . . . ?
N2 C34 C35 C36 -179.59(18) . . . . ?
N2 C34 C39 O3 -0.6(2) . . . . ?
N2 C34 C39 C38 -179.75(17) . . . . ?
C1 C2 C3 C4 -3.2(3) . . . . ?
C1 C2 C11 C12 -70.4(3) . . . . ?
C1 C2 C11 C13 52.2(3) . . . . ?
C1 C2 C11 C14 170.9(2) . . . . ?
C1 C6 C7 C8 -57.3(3) . . . . ?
C1 C6 C7 C9 64.5(3) . . . . ?
C1 C6 C7 C10 -176.7(2) . . . . ?
C2 C1 C6 C5 -5.0(3) . . . . ?
C2 C1 C6 C7 173.04(18) . . . . ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C2 C3 C4 C15 -175.09(16) . . . . ?
C3 C2 C11 C12 112.5(2) . . . . ?
C3 C2 C11 C13 -124.9(2) . . . . ?
C3 C2 C11 C14 -6.2(3) . . . . ?
C3 C4 C5 C6 2.2(3) . . . . ?
C3 C4 C15 C16 49.5(2) . . . . ?
C3 C4 C15 C19 -67.2(2) . . . . ?
C4 C5 C6 C1 0.7(3) . . . . ?
C4 C5 C6 C7 -177.43(17) . . . . ?
C4 C15 C16 N1 52.5(3) . . . . ?
C4 C15 C16 C17 -129.24(16) . . . . ?
C4 C15 C19 C18 126.32(16) . . . . ?
C4 C15 C19 C20 -57.4(2) . . . . ?
C5 C4 C15 C16 -124.55(17) . . . . ?
C5 C4 C15 C19 118.74(18) . . . . ?
C5 C6 C7 C8 120.7(2) . . . . ?
C5 C6 C7 C9 -117.5(2) . . . . ?
C5 C6 C7 C10 1.3(3) . . . . ?
C6 C1 C2 C3 6.2(3) . . . . ?
C6 C1 C2 C11 -170.91(18) . . . . ?
C11 C2 C3 C4 174.02(18) . . . . ?
C15 C4 C5 C6 176.36(16) . . . . ?
C15 C16 C17 C18 4.25(19) . . . . ?
C15 C16 C17 C26 -176.87(14) . . . . ?
C15 C19 C20 C21 148.27(18) . . . . ?
C15 C19 C20 C25 -32.3(2) . . . . ?
C16 N1 C27 C26 -0.82(19) . . . . ?
C16 N1 C27 C28 179.09(18) . . . . ?
C16 C15 C19 C18 2.13(17) . . . . ?
C16 C15 C19 C20 178.37(15) . . . . ?
C16 C17 C18 N2 177.69(14) . . . . ?
C16 C17 C18 C19 -2.71(19) . . . . ?
C16 C17 C26 C27 -2.24(19) . . . . ?
C16 C17 C26 C33 175.1(2) . . . . ?
C17 C18 C19 C15 0.18(19) . . . . ?
C17 C18 C19 C20 -175.68(16) . . . . ?
C17 C26 C27 N1 1.88(18) . . . . ?
C17 C26 C27 C28 -178.04(16) . . . . ?
C17 C26 C33 C32 -178.6(2) . . . . ?
C18 N2 C34 C35 42.2(2) . . . . ?
C18 N2 C34 C39 -137.07(16) . . . . ?
C18 C17 C26 C27 175.9(2) . . . . ?
C18 C17 C26 C33 -6.8(4) . . . . ?
C18 C19 C20 C21 -36.3(3) . . . . ?
C18 C19 C20 C25 143.2(2) . . . . ?
C19 C15 C16 N1 177.75(19) . . . . ?
C19 C15 C16 C17 -3.96(18) . . . . ?
C19 C20 C21 C22 177.8(2) . . . . ?
C19 C20 C25 C24 -177.9(2) . . . . ?
C20 C21 C22 C23 0.6(4) . . . . ?
C21 C20 C25 C24 1.6(3) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C22 C23 C24 C25 -0.5(5) . . . . ?
C23 C24 C25 C20 -0.5(4) . . . . ?
C25 C20 C21 C22 -1.6(3) . . . . ?
C26 C17 C18 N2 -0.4(4) . . . . ?
C26 C17 C18 C19 179.2(2) . . . . ?
C26 C27 C28 C29 175.96(19) . . . . ?
C26 C27 C28 C31 -3.8(3) . . . . ?
C27 N1 C16 C15 177.65(18) . . . . ?
C27 N1 C16 C17 -0.64(19) . . . . ?
C27 C26 C33 C32 -1.6(3) . . . . ?
C27 C28 C31 C32 1.1(3) . . . . ?
C28 C31 C32 C33 1.3(4) . . . . ?
C29 C28 C31 C32 -178.6(2) . . . . ?
C30 N1 C16 C15 -3.0(3) . . . . ?
C30 N1 C16 C17 178.68(16) . . . . ?
C30 N1 C27 C26 179.91(18) . . . . ?
C30 N1 C27 C28 -0.2(3) . . . . ?
C31 C32 C33 C26 -1.1(3) . . . . ?
C33 C26 C27 N1 -175.92(16) . . . . ?
C33 C26 C27 C28 4.2(3) . . . . ?
C34 N2 C18 C17 -80.30(19) . . . . ?
C34 N2 C18 C19 100.17(19) . . . . ?
C34 C35 C36 C37 -0.4(3) . . . . ?
C35 C34 C39 O3 -179.86(17) . . . . ?
C35 C34 C39 C38 1.0(3) . . . . ?
C35 C36 C37 C38 0.4(4) . . . . ?
C36 C37 C38 C39 0.2(4) . . . . ?
C37 C38 C39 O3 180.0(2) . . . . ?
C37 C38 C39 C34 -1.0(3) . . . . ?
C39 C34 C35 C36 -0.3(3) . . . . ?
C40 O3 C39 C34 159.5(2) . . . . ?
C40 O3 C39 C38 -21.4(3) . . . . ?
C41 S1 N2 C18 97.34(12) . . . . ?
C41 S1 N2 C34 -109.89(13) . . . . ?
C41 C42 C43 C44 0.5(4) . . . . ?
C42 C41 C46 C45 -1.3(3) . . . . ?
C42 C43 C44 C45 -1.7(4) . . . . ?
C42 C43 C44 C47 176.9(2) . . . . ?
C43 C44 C45 C46 1.4(3) . . . . ?
C44 C45 C46 C41 0.0(3) . . . . ?
C46 C41 C42 C43 1.1(3) . . . . ?
C47 C44 C45 C46 -177.2(2) . . . . ?
