#------------------------------------------------------------------------------
#$Date: 2019-12-18 08:29:46 +0200 (Wed, 18 Dec 2019) $
#$Revision: 245307 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243214.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243214
loop_
_publ_author_name
'Shaibah, Mohammed A. E.'
'Yathirajan, Hemmige S.'
'Manju, Nagaraj'
'Kalluraya, Balakrishna'
'Rathore, Ravindranath S.'
'Glidewell, Christopher'
_publ_section_title
;
Two isostructural
3-(5-aryloxy-3-methyl-1-phenyl-1H-pyrazol-4-yl)-1-(thiophen-2-yl)prop-2-en-1-ones:
disorder and supramolecular assembly
;
_journal_coeditor_code ZL2765
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 48
_journal_page_last 52
_journal_paper_doi 10.1107/S205698901901658X
_journal_volume 76
_journal_year 2020
_chemical_formula_iupac 'C23 H18 N2 O2 S'
_chemical_formula_moiety 'C23 H18 N2 O2 S'
_chemical_formula_sum 'C23 H18 N2 O2 S'
_chemical_formula_weight 386.45
_chemical_name_systematic
3-(3-Methyl-5-phenoxy-1-phenyl-1H-pyrazol-4-yl)-1-(thiophen-2-yl)prop-2-en-1-one
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary difmap
_audit_creation_method SHELXL-2014
_cell_angle_alpha 90
_cell_angle_beta 93.712(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.6158(5)
_cell_length_b 19.8846(11)
_cell_length_c 10.3773(6)
_cell_measurement_reflns_used 3725
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 25.604
_cell_measurement_theta_min 2.048
_cell_volume 1980.04(19)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker Kappa APEXII CCD
;
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0427
_diffrn_reflns_av_unetI/netI 0.0295
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 31970
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.604
_diffrn_reflns_theta_min 2.048
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.184
_exptl_absorpt_correction_T_max 0.973
_exptl_absorpt_correction_T_min 0.941
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.296
_exptl_crystal_description block
_exptl_crystal_F_000 808
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.150
_refine_diff_density_max 0.200
_refine_diff_density_min -0.144
_refine_ls_extinction_coef 0.0059(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 268
_refine_ls_number_reflns 3725
_refine_ls_number_restraints 10
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.0809
_refine_ls_R_factor_gt 0.0420
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.5730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0948
_refine_ls_wR_factor_ref 0.1165
_reflns_number_gt 2446
_reflns_number_total 3725
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zl2765sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2243214
_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.
;
_shelx_estimated_absorpt_t_min 0.964
_shelx_estimated_absorpt_t_max 0.973
_shelx_hkl_file
;
2 0 0 2649.33 46.60
3 0 0 89.09 3.50
4 0 0 3.70 1.50
5 0 0 93.09 4.40
7 0 0 -0.30 1.50
8 0 0 -0.50 1.30
8 0 0 2.90 2.10
8 0 0 0.20 2.00
9 0 0 30.00 4.10
9 0 0 30.30 4.50
9 0 0 34.80 4.60
9 0 0 41.90 4.70
10 0 0 12.90 3.30
10 0 0 9.20 3.40
10 0 0 9.10 3.20
10 0 0 5.90 3.00
11 0 0 17.80 3.90
11 0 0 19.90 4.00
11 0 0 11.70 3.90
11 0 0 13.00 3.00
0 -1 0 -1.30 0.10
0 -1 0 -1.10 0.10
0 -1 0 -1.20 0.10
0 -1 0 -1.20 0.10
0 1 0 -1.20 0.10
0 1 0 -1.10 0.10
0 1 0 -1.30 0.10
-1 -1 0 171.28 3.70
1 -1 0 129.09 3.00
-1 1 0 146.59 3.40
1 1 0 125.39 2.90
-1 1 0 164.08 3.30
2 -1 0 517.35 9.30
2 -1 0 518.55 10.10
2 -1 0 495.75 10.20
-2 -1 0 500.35 9.00
2 -1 0 500.05 9.20
-2 -1 0 478.55 9.00
-2 1 0 511.35 9.20
2 1 0 512.35 9.00
2 1 0 504.25 10.30
2 1 0 502.85 9.00
3 -1 0 82.79 3.30
3 -1 0 83.49 2.00
3 -1 0 86.09 2.00
3 -1 0 86.19 3.20
3 1 0 87.09 3.30
-3 1 0 82.99 2.00
-3 1 0 83.49 2.00
4 -1 0 84.89 3.70
4 -1 0 81.49 1.70
4 -1 0 90.99 3.80
4 -1 0 81.49 1.70
4 1 0 81.09 3.80
-4 1 0 82.69 1.80
-4 1 0 83.49 1.80
5 -1 0 13.60 1.90
5 -1 0 18.00 2.40
5 1 0 15.00 2.40
6 -1 0 12.90 2.00
7 -1 0 48.60 3.90
7 1 0 47.50 4.10
8 -1 0 21.70 3.30
8 -1 0 21.20 3.30
8 1 0 21.50 3.10
8 1 0 15.60 2.80
8 1 0 13.50 2.80
8 1 0 19.70 3.30
9 -1 0 32.00 4.30
9 -1 0 24.30 3.70
9 -1 0 31.10 4.00
9 1 0 28.20 4.00
9 1 0 28.90 4.30
9 1 0 47.50 5.20
9 1 0 31.50 4.20
10 -1 0 2.80 2.50
10 -1 0 -1.30 1.50
10 -1 0 -0.20 2.70
10 -1 0 2.70 2.50
10 1 0 0.80 2.40
10 1 0 1.50 2.00
10 1 0 1.10 2.50
10 1 0 2.80 2.60
11 -1 0 6.80 2.90
11 -1 0 5.60 2.70
11 -1 0 -3.50 2.40
11 -1 0 4.00 3.10
11 1 0 -0.60 2.70
11 1 0 3.60 2.40
11 1 0 6.80 3.20
11 1 0 -0.50 2.40
0 -2 0 770.32 13.70
0 2 0 708.53 13.50
1 -2 0 513.15 9.50
-1 -2 0 509.45 9.50
1 -2 0 511.05 9.30
1 -2 0 451.95 9.40
-1 -2 0 517.75 10.30
-1 -2 0 509.45 9.40
1 2 0 494.95 9.10
-1 2 0 492.65 9.50
-1 2 0 509.05 9.30
-1 2 0 496.35 9.40
1 2 0 502.45 9.40
1 2 0 429.66 10.10
1 2 0 470.35 9.20
1 2 0 487.15 9.40
-1 2 0 515.25 9.60
-2 -2 0 1628.24 31.60
2 -2 0 1631.24 29.20
2 -2 0 1636.34 29.50
2 -2 0 1634.04 29.20
2 -2 0 1655.53 29.50
-2 -2 0 1610.54 29.00
2 2 0 1615.44 29.50
2 2 0 1654.23 31.70
2 2 0 1617.54 29.00
2 2 0 1644.94 29.00
-2 2 0 1653.03 29.20
-2 2 0 1645.24 29.50
3 -2 0 113.19 3.60
3 -2 0 107.49 3.90
-3 -2 0 105.49 2.50
3 -2 0 106.49 2.80
3 -2 0 102.89 2.70
-3 -2 0 103.99 2.50
-3 2 0 104.49 2.80
3 2 0 104.79 2.50
3 2 0 106.09 3.70
3 2 0 104.19 2.50
3 2 0 106.19 4.10
4 -2 0 45.60 1.60
-4 -2 0 45.70 1.20
4 -2 0 52.79 2.80
4 -2 0 44.70 1.60
4 -2 0 43.10 3.00
-4 -2 0 45.00 1.20
4 2 0 42.40 3.00
4 2 0 46.10 1.20
4 2 0 46.90 3.00
-4 2 0 46.70 1.70
-4 2 0 45.50 1.70
4 2 0 44.90 1.10
5 -2 0 13.50 0.80
5 -2 0 12.10 1.80
5 -2 0 11.80 2.30
5 -2 0 15.00 0.80
5 2 0 12.10 2.20
-5 2 0 15.00 0.90
-5 2 0 13.40 0.90
5 2 0 9.50 1.90
6 -2 0 18.40 2.50
6 2 0 17.90 2.50
7 -2 0 25.80 2.80
7 2 0 39.70 3.70
7 2 0 26.30 3.40
8 -2 0 8.90 2.10
8 -2 0 11.00 2.50
8 2 0 10.00 2.60
8 2 0 11.90 2.90
8 2 0 9.70 2.50
9 -2 0 141.39 8.30
9 -2 0 119.99 6.70
9 -2 0 120.09 6.80
9 2 0 117.79 7.60
9 2 0 118.79 7.20
9 2 0 115.29 7.00
9 2 0 120.59 7.50
10 -2 0 6.30 2.60
10 -2 0 -0.10 2.10
10 -2 0 2.20 2.80
10 2 0 6.20 2.80
10 2 0 5.30 2.70
10 2 0 4.70 2.40
10 2 0 3.40 2.70
11 -2 0 1.70 2.40
11 -2 0 1.40 2.40
11 -2 0 2.90 2.40
11 -2 0 4.60 2.60
11 2 0 5.10 2.90
11 2 0 -0.80 2.90
11 2 0 0.20 2.60
11 2 0 4.70 2.90
0 -3 0 0.00 0.40
0 -3 0 -0.70 0.40
0 -3 0 -0.40 0.50
0 3 0 -0.40 0.30
0 3 0 -0.30 0.50
0 3 0 -0.20 0.60
0 3 0 0.30 0.50
0 3 0 0.20 0.40
-1 -3 0 352.26 7.50
1 -3 0 370.66 7.70
1 -3 0 353.76 7.60
-1 -3 0 368.56 8.20
1 -3 0 356.56 7.40
-1 -3 0 354.06 7.60
1 -3 0 363.86 7.00
1 3 0 358.26 7.50
-1 3 0 363.96 7.60
1 3 0 359.26 7.50
-1 3 0 357.16 7.60
1 3 0 362.46 7.00
-1 3 0 361.26 7.00
-1 3 0 364.56 7.40
1 3 0 364.36 8.20
-2 -3 0 56.29 2.10
2 -3 0 56.49 2.20
2 -3 0 57.59 2.30
-2 -3 0 59.49 2.70
-2 -3 0 58.19 2.10
2 -3 0 58.89 2.30
2 -3 0 55.79 2.20
2 3 0 56.79 1.90
-2 3 0 58.09 2.20
-2 3 0 57.69 2.20
2 3 0 59.19 2.00
2 3 0 59.89 2.30
2 3 0 61.29 2.60
-2 3 0 59.59 2.30
2 3 0 57.69 2.00
3 -3 0 37.90 1.80
3 -3 0 45.70 2.50
3 -3 0 50.49 2.40
-3 -3 0 38.40 1.70
3 -3 0 40.80 1.90
3 3 0 40.80 2.20
3 3 0 40.30 1.60
-3 3 0 40.70 1.90
3 3 0 43.40 1.70
-3 3 0 38.60 1.90
-3 3 0 43.60 2.20
3 3 0 41.70 2.50
4 -3 0 15.40 1.20
4 -3 0 13.40 1.10
4 -3 0 13.10 1.70
4 -3 0 14.90 1.90
-4 -3 0 11.00 1.00
-4 -3 0 13.40 1.10
-4 3 0 11.40 1.30
4 3 0 16.10 2.20
4 3 0 13.90 0.90
4 3 0 9.40 1.50
4 3 0 12.50 0.90
-5 -3 0 186.78 4.00
5 -3 0 189.08 4.50
5 -3 0 186.18 6.50
5 -3 0 189.38 4.60
5 -3 0 191.68 6.30
-5 -3 0 186.98 4.00
5 3 0 196.48 7.20
-5 3 0 179.18 4.50
-5 3 0 191.68 4.60
5 3 0 183.58 3.80
5 3 0 197.18 6.70
5 3 0 186.88 3.80
6 -3 0 40.40 1.50
6 -3 0 42.80 3.30
6 -3 0 39.90 1.60
-6 3 0 41.60 1.70
6 3 0 45.40 3.40
-6 3 0 42.80 1.70
6 3 0 39.40 3.70
7 -3 0 37.00 3.20
7 -3 0 33.10 3.10
7 3 0 33.90 3.50
7 3 0 34.70 4.00
8 -3 0 4.40 2.00
8 -3 0 4.90 2.00
8 3 0 3.90 2.00
8 3 0 2.10 2.00
8 3 0 3.90 2.30
9 -3 0 6.50 2.70
9 -3 0 8.50 3.20
9 -3 0 4.40 2.50
9 3 0 5.40 2.30
9 3 0 9.70 3.30
9 3 0 12.80 2.90
10 -3 0 2.00 2.10
10 -3 0 1.10 2.20
10 -3 0 1.90 2.50
10 3 0 -1.70 1.60
10 3 0 0.80 2.00
10 3 0 1.80 2.40
10 3 0 -0.20 2.10
11 -3 0 8.10 3.00
11 -3 0 2.90 2.50
11 -3 0 11.20 4.10
11 3 0 10.20 3.50
11 3 0 7.50 2.90
11 3 0 8.10 3.20
11 3 0 3.00 3.30
0 -4 0 1002.30 19.50
0 -4 0 1023.20 19.20
0 -4 0 1012.60 19.40
0 -4 0 1035.80 20.70
0 4 0 1025.00 19.50
0 4 0 1023.80 20.70
0 4 0 1026.30 19.50
0 4 0 1028.40 19.10
0 4 0 1006.60 18.90
-1 -4 0 29.80 1.80
-1 -4 0 34.70 2.00
1 -4 0 30.70 1.90
1 -4 0 33.60 1.60
1 -4 0 33.90 1.30
-1 -4 0 38.00 2.10
1 -4 0 31.90 2.10
1 -4 0 34.90 2.00
-1 4 0 31.90 1.60
1 4 0 29.60 1.80
-1 4 0 34.10 2.00
1 4 0 34.70 1.90
1 4 0 33.20 1.30
1 4 0 32.30 1.90
-1 4 0 34.30 1.00
-1 4 0 33.70 2.00
2 -4 0 228.18 5.90
2 -4 0 243.68 5.90
2 -4 0 236.38 5.80
-2 -4 0 240.68 5.80
2 -4 0 238.58 5.70
-2 -4 0 228.18 5.70
-2 -4 0 238.68 6.50
2 4 0 233.08 5.70
-2 4 0 233.18 5.90
-2 4 0 243.68 5.80
2 4 0 241.98 5.00
2 4 0 241.28 6.60
2 4 0 237.88 5.70
2 4 0 240.58 5.70
-2 4 0 242.38 6.00
3 -4 0 310.27 7.20
3 -4 0 308.37 7.40
-3 -4 0 311.47 6.90
3 -4 0 302.87 7.10
3 -4 0 312.67 7.70
-3 -4 0 306.27 8.30
-3 -4 0 304.97 7.00
-3 4 0 299.07 7.20
3 4 0 307.17 8.40
3 4 0 305.97 6.90
3 4 0 301.37 6.80
3 4 0 308.17 7.00
-3 4 0 302.87 7.20
3 4 0 307.87 7.60
-3 4 0 307.87 7.40
4 -4 0 -0.70 0.60
4 -4 0 -0.30 0.80
4 -4 0 -2.20 0.70
-4 -4 0 0.00 0.20
4 -4 0 -0.70 0.50
-4 -4 0 0.80 0.80
4 4 0 -0.60 0.50
4 4 0 -1.10 1.00
-4 4 0 -0.10 0.90
4 4 0 0.10 0.70
4 4 0 -0.90 0.50
-4 4 0 0.00 0.80
-4 4 0 -0.10 0.80
4 4 0 -1.40 0.90
5 -4 0 36.70 3.20
5 -4 0 37.80 1.90
-5 -4 0 33.60 1.70
-5 -4 0 36.00 1.80
5 -4 0 35.60 1.90
5 -4 0 36.80 2.80
5 4 0 37.40 1.60
5 4 0 38.40 2.60
5 4 0 34.40 2.70
5 4 0 35.90 3.30
5 4 0 35.90 1.60
-5 4 0 38.50 2.10
6 -4 0 7.40 1.90
6 -4 0 9.70 1.10
-6 -4 0 9.50 0.80
-6 -4 0 9.70 0.80
6 -4 0 11.30 1.20
-6 4 0 10.10 1.30
6 4 0 10.00 2.20
-6 4 0 11.20 1.30
6 4 0 10.50 0.60
6 4 0 8.00 1.80
6 4 0 9.70 0.60
7 -4 0 13.70 1.10
7 -4 0 12.60 2.40
7 -4 0 14.30 1.10
7 -4 0 19.00 2.60
7 4 0 17.20 3.10
7 4 0 18.60 2.70
-7 4 0 14.80 1.30
-7 4 0 15.50 1.30
7 4 0 15.50 2.90
8 -4 0 8.60 2.30
8 -4 0 7.50 2.30
8 4 0 9.40 2.70
8 4 0 2.30 1.80
8 4 0 6.50 2.50
9 -4 0 3.10 2.20
9 -4 0 0.80 2.00
9 -4 0 0.20 1.70
9 4 0 6.70 2.40
9 4 0 3.50 2.60
9 4 0 4.10 3.00
10 -4 0 -1.20 1.70
10 -4 0 4.10 3.20
10 -4 0 -1.40 2.00
10 4 0 1.40 2.60
10 4 0 -1.30 2.10
10 4 0 1.60 2.30
11 -4 0 0.40 2.40
11 -4 0 4.50 2.80
11 4 0 5.40 3.10
11 4 0 -4.10 2.40
11 4 0 -0.90 2.40
11 4 0 2.00 3.50
0 -5 0 -0.60 0.90
0 -5 0 -1.40 0.90
0 -5 0 0.60 0.70
0 5 0 -0.90 0.80
0 5 0 0.10 1.10
0 5 0 -0.80 0.90
0 5 0 0.10 0.60
0 5 0 0.00 0.90
1 -5 0 311.47 7.50
1 -5 0 307.97 6.00
1 -5 0 296.77 7.30
-1 -5 0 294.57 5.70
-1 -5 0 301.07 7.30
-1 -5 0 300.47 7.30
1 -5 0 290.57 8.10
1 -5 0 310.77 7.00
-1 -5 0 303.77 7.90
-1 5 0 300.27 7.40
1 5 0 293.87 6.00
1 5 0 296.27 7.30
-1 5 0 301.87 7.40
1 5 0 297.37 7.90
1 5 0 297.27 7.30
-1 5 0 301.57 5.90
-1 5 0 305.77 7.00
-2 -5 0 434.46 9.80
-2 -5 0 441.06 10.70
2 -5 0 437.16 9.90
2 -5 0 447.96 9.60
2 -5 0 428.46 9.80
-2 -5 0 441.46 9.70
2 -5 0 434.56 9.10
-2 5 0 442.26 9.60
2 5 0 444.26 8.30
2 5 0 447.06 9.70
-2 5 0 426.46 9.80
2 5 0 440.76 10.80
-2 5 0 421.16 9.80
2 5 0 433.66 9.10
2 5 0 436.56 9.60
-3 -5 0 42.20 2.80
3 -5 0 37.00 2.20
3 -5 0 38.50 2.30
-3 -5 0 37.50 2.20
3 -5 0 37.20 2.20
3 -5 0 34.40 2.30
-3 -5 0 38.00 2.10
3 5 0 41.20 2.30
-3 5 0 36.70 2.30
-3 5 0 34.80 2.20
3 5 0 37.10 2.10
-3 5 0 35.00 2.20
3 5 0 34.30 2.00
3 5 0 38.20 2.80
3 5 0 37.80 1.70
-4 -5 0 116.19 3.80
4 -5 0 125.49 4.70
4 -5 0 125.69 4.50
4 -5 0 119.59 4.10
-4 -5 0 121.79 5.10
-4 -5 0 120.39 4.00
4 -5 0 119.29 4.00
-4 5 0 126.69 4.20
4 5 0 120.19 5.10
4 5 0 118.99 3.80
4 5 0 122.99 4.10
-4 5 0 121.09 4.20
4 5 0 118.39 3.70
4 5 0 126.79 4.60
-4 5 0 129.89 4.60
5 -5 0 5.40 1.90
5 -5 0 7.70 1.30
5 -5 0 6.30 1.50
-5 -5 0 2.80 0.80
-5 -5 0 7.40 1.20
5 -5 0 6.40 1.20
5 5 0 8.40 1.80
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3 -3 9 5.20 3.10
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-2 6 12 5.40 4.80
-2 6 12 9.20 4.40
2 6 -12 7.60 3.50
-1 -6 12 -5.00 3.30
1 -6 -12 -4.10 3.40
-1 -6 12 -0.60 2.80
1 -6 -12 -6.20 3.20
1 6 -12 3.40 3.10
-1 6 12 7.40 4.30
-1 6 12 -2.80 2.90
1 6 -12 -3.30 3.20
0 -6 -12 -0.60 3.50
0 -6 12 -2.70 2.50
0 -6 -12 4.70 3.30
0 -6 12 -1.90 2.50
0 6 12 -5.60 3.80
0 6 12 2.30 2.90
0 6 -12 -1.20 2.60
-1 -6 -12 -1.70 3.50
1 -6 12 -0.40 3.80
1 -6 12 0.50 3.70
-1 -6 -12 3.70 4.20
1 6 12 1.10 3.50
1 6 12 -2.90 4.50
-1 6 -12 -1.60 3.80
-1 -7 12 -8.90 3.00
-1 -7 12 6.40 4.20
1 -7 -12 3.90 4.30
1 -7 -12 9.30 5.60
1 7 -12 -0.40 4.10
-1 7 12 3.00 4.80
-1 7 12 4.50 4.10
0 -7 -12 -8.50 4.50
0 -7 -12 -5.00 3.70
0 -7 12 1.70 3.80
0 -7 12 -2.90 2.80
0 7 12 2.40 3.80
0 7 -12 -4.00 3.70
0 7 12 -2.60 3.10
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 77503
_shelx_res_file
;
TITL a3cg
CELL 0.71073 9.6158 19.8846 10.3773 90.000 93.712 90.000
ZERR 4.00 0.0005 0.0011 0.0006 0.000 0.002 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O S
UNIT 92 72 8 8 4
MERG 2
FMAP 2
PLAN 10
SIZE 0.150 0.200 0.200
OMIT -2 180.0
ACTA
BOND $H
CONF
HTAB
L.S. 20
TEMP 23.00
EXYZ C12 C22
EADP S11 C23
EADP C12 C22
EADP C13 S21
EADP C14 C25
EADP C15 C24
MPLA N31 N32 C33 C34 C35 C3 C2 C1 C12 S11 C13 C14 C15
MPLA C311 > C316
MPLA N31 > C35
MPLA C351 > C356
MPLA N31 > C35
MPLA C12 C1 C2 C3 C34
MPLA S11 C12 C13 C14 C15
MPLA S21 C22 C23 C24 C25
MPLA 7 O35 C351 C352 C353 C354 C355 C356 C35
WGHT 0.046700 0.573000
EXTI 0.005875
FVAR 0.43699 0.84369
C1 1 0.695223 0.386766 0.502121 11.00000 0.05225 0.04695 =
0.04498 0.00028 -0.00602 -0.00423
O1 4 0.769423 0.430973 0.551246 11.00000 0.09190 0.05351 =
0.08721 0.00938 -0.04746 -0.01755
C2 1 0.589487 0.401396 0.398228 11.00000 0.04933 0.04410 =
0.04909 -0.00025 -0.00849 -0.00347
AFIX 43
H2 2 0.537614 0.366277 0.360440 11.00000 -1.20000
AFIX 0
C3 1 0.565961 0.463985 0.356621 11.00000 0.04649 0.04430 =
0.04373 -0.00155 -0.00219 -0.00506
AFIX 43
H3 2 0.617487 0.497552 0.400019 11.00000 -1.20000
AFIX 0
PART 1
S11 5 0.826264 0.298165 0.672693 21.00000 0.08108 0.05365 =
0.06082 0.00923 -0.02426 -0.00266
C12 1 0.711135 0.316956 0.545968 21.00000 0.05497 0.04508 =
0.04423 -0.00023 -0.00383 0.00116
C13 1 0.649076 0.261479 0.501674 21.00000 0.13784 0.04753 =
0.08607 -0.00392 -0.05025 -0.01707
AFIX 43
H13 2 0.583688 0.261234 0.431604 21.00000 -1.20000
AFIX 0
C14 1 0.690381 0.203049 0.569487 21.00000 0.16706 0.03982 =
0.10428 0.00199 -0.04967 -0.00855
AFIX 43
H14 2 0.654654 0.160465 0.550556 21.00000 -1.20000
AFIX 0
C15 1 0.786501 0.215764 0.663866 21.00000 0.11297 0.05518 =
0.07025 0.01859 -0.01562 0.00719
AFIX 43
H15 2 0.826975 0.183142 0.718482 21.00000 -1.20000
AFIX 0
PART 0
PART 2
SAME 0.01 0.02 S11 > C15
S21 5 0.613813 0.253356 0.483922 -21.00000 0.13784 0.04753 =
0.08607 -0.00392 -0.05025 -0.01707
C22 1 0.711135 0.316956 0.545968 -21.00000 0.05497 0.04508 =
0.04423 -0.00023 -0.00383 0.00116
C23 1 0.813498 0.293472 0.625577 -21.00000 0.08108 0.05365 =
0.06082 0.00923 -0.02426 -0.00266
AFIX 43
H23 2 0.883703 0.320491 0.663510 -21.00000 -1.20000
AFIX 0
C24 1 0.805420 0.223876 0.646906 -21.00000 0.11297 0.05518 =
0.07025 0.01859 -0.01562 0.00719
AFIX 43
H24 2 0.858065 0.200913 0.711103 -21.00000 -1.20000
AFIX 0
C25 1 0.712952 0.195002 0.563661 -21.00000 0.16706 0.03982 =
0.10428 0.00199 -0.04967 -0.00855
AFIX 43
H25 2 0.704181 0.148846 0.551142 -21.00000 -1.20000
AFIX 0
PART 0
N31 3 0.313854 0.490259 0.087171 11.00000 0.04021 0.03693 =
0.04729 0.00334 -0.00336 0.00073
N32 3 0.367627 0.554396 0.099229 11.00000 0.04890 0.03503 =
0.05708 0.00506 -0.00541 -0.00315
C33 1 0.460271 0.551298 0.199045 11.00000 0.04276 0.03897 =
0.05093 0.00111 -0.00022 -0.00237
C34 1 0.470594 0.485901 0.252793 11.00000 0.03926 0.04015 =
0.04372 0.00160 -0.00020 -0.00016
C35 1 0.375860 0.449196 0.176961 11.00000 0.03934 0.03454 =
0.04502 0.00218 0.00155 0.00117
C311 1 0.211846 0.476060 -0.014769 11.00000 0.03716 0.03969 =
0.04251 -0.00250 -0.00281 0.00495
C312 1 0.112248 0.427040 -0.001918 11.00000 0.04707 0.04251 =
0.05340 -0.00201 -0.00446 0.00403
AFIX 43
H312 2 0.111303 0.402007 0.073721 11.00000 -1.20000
AFIX 0
C313 1 0.014288 0.415519 -0.102063 11.00000 0.04849 0.05082 =
0.06552 -0.01078 -0.00816 0.00103
AFIX 43
H313 2 -0.053206 0.382585 -0.093702 11.00000 -1.20000
AFIX 0
C314 1 0.015093 0.452235 -0.214574 11.00000 0.05544 0.06774 =
0.05697 -0.01838 -0.01488 0.01270
AFIX 43
H314 2 -0.050819 0.443851 -0.282237 11.00000 -1.20000
AFIX 0
C315 1 0.114123 0.501377 -0.226044 11.00000 0.06309 0.07057 =
0.04414 0.00257 -0.00373 0.00900
AFIX 43
H315 2 0.114591 0.526572 -0.301518 11.00000 -1.20000
AFIX 0
C316 1 0.212674 0.513526 -0.126414 11.00000 0.04726 0.05519 =
0.04696 0.00255 0.00164 0.00248
AFIX 43
H316 2 0.279418 0.546849 -0.134481 11.00000 -1.20000
AFIX 0
C331 1 0.542606 0.612311 0.238617 11.00000 0.06216 0.04512 =
0.07382 0.00159 -0.00816 -0.00769
AFIX 137
H31A 2 0.635290 0.608218 0.210243 11.00000 -1.50000
H31B 2 0.546836 0.616535 0.330943 11.00000 -1.50000
H31C 2 0.498678 0.651445 0.200133 11.00000 -1.50000
AFIX 0
O35 4 0.350641 0.382099 0.173448 11.00000 0.05252 0.03324 =
0.05153 0.00044 0.00358 -0.00102
C351 1 0.272205 0.353382 0.267989 11.00000 0.04110 0.03977 =
0.05151 0.01051 -0.00470 -0.00248
C352 1 0.263350 0.284759 0.262306 11.00000 0.07142 0.04197 =
0.09312 0.00758 0.00950 -0.00528
AFIX 43
H352 2 0.309474 0.260853 0.200932 11.00000 -1.20000
AFIX 0
C353 1 0.185649 0.251935 0.348260 11.00000 0.09406 0.05425 =
0.13793 0.02659 0.02304 -0.01138
AFIX 43
H353 2 0.178621 0.205307 0.345340 11.00000 -1.20000
AFIX 0
C354 1 0.118326 0.287093 0.438313 11.00000 0.09277 0.08659 =
0.11504 0.04622 0.02738 -0.01115
AFIX 43
H354 2 0.065621 0.264388 0.496499 11.00000 -1.20000
AFIX 0
C355 1 0.128140 0.355651 0.443248 11.00000 0.08591 0.09549 =
0.07775 0.01424 0.02865 -0.00171
AFIX 43
H355 2 0.082028 0.379328 0.504942 11.00000 -1.20000
AFIX 0
C356 1 0.206479 0.390278 0.356812 11.00000 0.06278 0.05461 =
0.06404 0.00342 0.00932 -0.00250
AFIX 43
H356 2 0.213822 0.436900 0.359433 11.00000 -1.20000
AFIX 0
HKLF 4
REM a3cg
REM R1 = 0.0420 for 2446 Fo > 4sig(Fo) and 0.0809 for all 3725 data
REM 268 parameters refined using 10 restraints
END
WGHT 0.0467 0.5730
REM Instructions for potential hydrogen bonds
HTAB C2 O35
EQIV $1 -x+1, y-1/2, -z+1/2
HTAB C14 N32_$1
HTAB C25 N32_$1
HTAB C312 O35
EQIV $2 -x+1, y+1/2, -z+1/2
HTAB C331 S21_$2
REM Highest difference peak 0.200, deepest hole -0.144, 1-sigma level 0.036
Q1 1 0.6349 0.6002 0.2819 11.00000 0.05 0.20
Q2 1 0.5697 0.6341 0.1498 11.00000 0.05 0.18
Q3 1 0.5233 0.2505 0.4406 11.00000 0.05 0.18
Q4 1 0.8158 0.4023 0.5022 11.00000 0.05 0.17
Q5 1 0.4927 0.6465 0.2658 11.00000 0.05 0.16
Q6 1 0.4491 0.4615 0.2172 11.00000 0.05 0.15
Q7 1 0.6633 0.3452 0.5603 11.00000 0.05 0.15
Q8 1 0.7358 0.3390 0.4911 11.00000 0.05 0.15
Q9 1 0.6067 0.2600 0.3852 11.00000 0.05 0.14
Q10 1 0.4594 0.6618 0.2821 11.00000 0.05 0.14
;
_shelx_res_checksum 53918
_shelxl_version_number 2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.6952(2) 0.38677(11) 0.5021(2) 0.0485(5) Uani d 1 . .
O O1 0.76942(19) 0.43097(8) 0.55125(17) 0.0798(6) Uani d 1 . .
C C2 0.5895(2) 0.40140(11) 0.3982(2) 0.0480(5) Uani d 1 . .
H H2 0.5376 0.3663 0.3604 0.058 Uiso calc 1 . .
C C3 0.5660(2) 0.46399(10) 0.35662(19) 0.0451(5) Uani d 1 . .
H H3 0.6175 0.4976 0.4000 0.054 Uiso calc 1 . .
S S11 0.82626(11) 0.29817(5) 0.67269(8) 0.0664(3) Uani d 0.844(3) A 1
C C12 0.7111(2) 0.31696(10) 0.5460(2) 0.0484(5) Uani d 0.844(3) A 1
C C13 0.6491(14) 0.2615(5) 0.5017(13) 0.0930(17) Uani d 0.844(3) A 1
H H13 0.5837 0.2612 0.4316 0.112 Uiso calc 0.844(3) A 1
C C14 0.6904(13) 0.2030(2) 0.5695(15) 0.106(3) Uani d 0.844(3) A 1
H H14 0.6547 0.1605 0.5506 0.128 Uiso calc 0.844(3) A 1
C C15 0.7865(9) 0.2158(3) 0.6639(9) 0.080(2) Uani d 0.844(3) A 1
H H15 0.8270 0.1831 0.7185 0.096 Uiso calc 0.844(3) A 1
S S21 0.614(2) 0.2534(7) 0.484(2) 0.0930(17) Uani d 0.156(3) A 2
C C22 0.7111(2) 0.31696(10) 0.5460(2) 0.0484(5) Uani d 0.156(3) A 2
C C23 0.813(2) 0.2935(10) 0.626(2) 0.0664(3) Uani d 0.156(3) A 2
H H23 0.8837 0.3205 0.6635 0.080 Uiso calc 0.156(3) A 2
C C24 0.805(6) 0.2239(12) 0.647(6) 0.080(2) Uani d 0.156(3) A 2
H H24 0.8581 0.2009 0.7111 0.096 Uiso calc 0.156(3) A 2
C C25 0.713(8) 0.1950(8) 0.564(9) 0.106(3) Uani d 0.156(3) A 2
H H25 0.7042 0.1488 0.5511 0.128 Uiso calc 0.156(3) A 2
N N31 0.31385(16) 0.49026(8) 0.08717(15) 0.0417(4) Uani d 1 . .
N N32 0.36763(17) 0.55440(8) 0.09923(17) 0.0474(4) Uani d 1 . .
C C33 0.4603(2) 0.55130(10) 0.1990(2) 0.0444(5) Uani d 1 . .
C C34 0.4706(2) 0.48590(10) 0.25279(19) 0.0412(5) Uani d 1 . .
C C35 0.3759(2) 0.44920(9) 0.17696(18) 0.0397(5) Uani d 1 . .
C C311 0.2118(2) 0.47606(10) -0.01477(19) 0.0400(5) Uani d 1 . .
C C312 0.1122(2) 0.42704(10) -0.0019(2) 0.0480(5) Uani d 1 . .
H H312 0.1113 0.4020 0.0737 0.058 Uiso calc 1 . .
C C313 0.0143(2) 0.41552(11) -0.1021(2) 0.0555(6) Uani d 1 . .
H H313 -0.0532 0.3826 -0.0937 0.067 Uiso calc 1 . .
C C314 0.0151(2) 0.45223(12) -0.2146(2) 0.0609(7) Uani d 1 . .
H H314 -0.0508 0.4439 -0.2822 0.073 Uiso calc 1 . .
C C315 0.1141(3) 0.50138(13) -0.2260(2) 0.0596(6) Uani d 1 . .
H H315 0.1146 0.5266 -0.3015 0.071 Uiso calc 1 . .
C C316 0.2127(2) 0.51353(11) -0.1264(2) 0.0499(5) Uani d 1 . .
H H316 0.2794 0.5468 -0.1345 0.060 Uiso calc 1 . .
C C331 0.5426(2) 0.61231(11) 0.2386(2) 0.0609(6) Uani d 1 . .
H H31A 0.6353 0.6082 0.2102 0.091 Uiso calc 1 . .
H H31B 0.5468 0.6165 0.3309 0.091 Uiso calc 1 . .
H H31C 0.4987 0.6514 0.2001 0.091 Uiso calc 1 . .
O O35 0.35064(14) 0.38210(6) 0.17345(13) 0.0458(4) Uani d 1 . .
C C351 0.2722(2) 0.35338(10) 0.2680(2) 0.0445(5) Uani d 1 . .
C C352 0.2634(3) 0.28476(12) 0.2623(3) 0.0687(7) Uani d 1 . .
H H352 0.3095 0.2609 0.2009 0.082 Uiso calc 1 . .
C C353 0.1856(3) 0.25194(15) 0.3483(4) 0.0947(10) Uani d 1 . .
H H353 0.1786 0.2053 0.3453 0.114 Uiso calc 1 . .
C C354 0.1183(3) 0.28709(17) 0.4383(4) 0.0972(11) Uani d 1 . .
H H354 0.0656 0.2644 0.4965 0.117 Uiso calc 1 . .
C C355 0.1281(3) 0.35565(16) 0.4432(3) 0.0854(9) Uani d 1 . .
H H355 0.0820 0.3793 0.5049 0.102 Uiso calc 1 . .
C C356 0.2065(2) 0.39028(12) 0.3568(2) 0.0603(6) Uani d 1 . .
H H356 0.2138 0.4369 0.3594 0.072 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0522(13) 0.0469(13) 0.0450(12) -0.0042(10) -0.0060(10) 0.0003(10)
O1 0.0919(13) 0.0535(10) 0.0872(13) -0.0176(9) -0.0475(10) 0.0094(9)
C2 0.0493(12) 0.0441(12) 0.0491(12) -0.0035(10) -0.0085(10) -0.0002(10)
C3 0.0465(12) 0.0443(12) 0.0437(12) -0.0051(9) -0.0022(10) -0.0015(9)
S11 0.0811(6) 0.0537(5) 0.0608(6) -0.0027(4) -0.0243(5) 0.0092(4)
C12 0.0550(13) 0.0451(13) 0.0442(12) 0.0012(10) -0.0038(10) -0.0002(10)
C13 0.138(7) 0.048(2) 0.086(4) -0.017(2) -0.050(3) -0.004(2)
C14 0.167(6) 0.0398(17) 0.104(3) -0.009(3) -0.050(5) 0.002(3)
C15 0.113(4) 0.055(2) 0.070(4) 0.007(2) -0.016(3) 0.0186(17)
S21 0.138(7) 0.048(2) 0.086(4) -0.017(2) -0.050(3) -0.004(2)
C22 0.0550(13) 0.0451(13) 0.0442(12) 0.0012(10) -0.0038(10) -0.0002(10)
C23 0.0811(6) 0.0537(5) 0.0608(6) -0.0027(4) -0.0243(5) 0.0092(4)
C24 0.113(4) 0.055(2) 0.070(4) 0.007(2) -0.016(3) 0.0186(17)
C25 0.167(6) 0.0398(17) 0.104(3) -0.009(3) -0.050(5) 0.002(3)
N31 0.0402(9) 0.0369(9) 0.0473(10) 0.0007(7) -0.0034(8) 0.0033(8)
N32 0.0489(10) 0.0350(10) 0.0571(11) -0.0031(8) -0.0054(9) 0.0051(8)
C33 0.0428(11) 0.0390(12) 0.0509(13) -0.0024(9) -0.0002(10) 0.0011(10)
C34 0.0393(11) 0.0401(11) 0.0437(11) -0.0002(9) -0.0002(9) 0.0016(9)
C35 0.0393(11) 0.0345(11) 0.0450(11) 0.0012(9) 0.0016(9) 0.0022(9)
C311 0.0372(11) 0.0397(11) 0.0425(11) 0.0050(9) -0.0028(9) -0.0025(9)
C312 0.0471(12) 0.0425(12) 0.0534(13) 0.0040(10) -0.0045(10) -0.0020(10)
C313 0.0485(13) 0.0508(14) 0.0655(15) 0.0010(11) -0.0082(11) -0.0108(12)
C314 0.0554(14) 0.0677(16) 0.0570(15) 0.0127(13) -0.0149(11) -0.0184(13)
C315 0.0631(15) 0.0706(16) 0.0441(13) 0.0090(13) -0.0037(12) 0.0026(11)
C316 0.0473(12) 0.0552(14) 0.0470(13) 0.0025(10) 0.0016(10) 0.0025(10)
C331 0.0622(15) 0.0451(13) 0.0738(16) -0.0077(11) -0.0082(12) 0.0016(12)
O35 0.0525(9) 0.0332(8) 0.0515(9) -0.0010(6) 0.0036(7) 0.0004(6)
C351 0.0411(11) 0.0398(12) 0.0515(13) -0.0025(9) -0.0047(10) 0.0105(10)
C352 0.0714(16) 0.0420(14) 0.093(2) -0.0053(12) 0.0095(15) 0.0076(13)
C353 0.094(2) 0.0543(17) 0.138(3) -0.0114(16) 0.023(2) 0.0266(19)
C354 0.093(2) 0.087(2) 0.115(3) -0.0112(18) 0.027(2) 0.046(2)
C355 0.086(2) 0.095(2) 0.0777(19) -0.0017(17) 0.0287(16) 0.0142(17)
C356 0.0628(15) 0.0546(14) 0.0640(15) -0.0025(12) 0.0093(12) 0.0034(12)
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
O1 C1 C2 121.57(19)
O1 C1 C12 120.34(19)
C2 C1 C12 118.09(18)
C3 C2 C1 121.35(19)
C3 C2 H2 119.3
C1 C2 H2 119.3
C2 C3 C34 127.83(19)
C2 C3 H3 116.1
C34 C3 H3 116.1
C15 S11 C12 92.15(19)
C13 C12 C1 130.3(5)
C13 C12 S11 110.0(5)
C1 C12 S11 119.77(15)
C12 C13 C14 114.2(6)
C12 C13 H13 122.9
C14 C13 H13 122.9
C15 C14 C13 111.9(4)
C15 C14 H14 124.0
C13 C14 H14 124.0
C14 C15 S11 111.7(4)
C14 C15 H15 124.1
S11 C15 H15 124.1
C24 C23 H23 123.3
C25 C24 C23 111.4(14)
C25 C24 H24 124.3
C23 C24 H24 124.3
C24 C25 S21 110.8(12)
C24 C25 H25 124.6
S21 C25 H25 124.6
C35 N31 N32 110.54(15)
C35 N31 C311 130.24(16)
N32 N31 C311 119.16(15)
C33 N32 N31 104.92(15)
N32 C33 C34 112.18(17)
N32 C33 C331 119.74(18)
C34 C33 C331 128.03(19)
C35 C34 C33 103.60(17)
C35 C34 C3 129.46(18)
C33 C34 C3 126.81(18)
N31 C35 O35 120.45(17)
N31 C35 C34 108.73(17)
O35 C35 C34 130.44(17)
C316 C311 C312 120.35(19)
C316 C311 N31 118.45(18)
C312 C311 N31 121.18(18)
C313 C312 C311 119.4(2)
C313 C312 H312 120.3
C311 C312 H312 120.3
C312 C313 C314 120.7(2)
C312 C313 H313 119.6
C314 C313 H313 119.6
C315 C314 C313 119.5(2)
C315 C314 H314 120.3
C313 C314 H314 120.3
C314 C315 C316 120.4(2)
C314 C315 H315 119.8
C316 C315 H315 119.8
C315 C316 C311 119.7(2)
C315 C316 H316 120.2
C311 C316 H316 120.2
C33 C331 H31A 109.5
C33 C331 H31B 109.5
H31A C331 H31B 109.5
C33 C331 H31C 109.5
H31A C331 H31C 109.5
H31B C331 H31C 109.5
C35 O35 C351 119.13(15)
C356 C351 C352 122.3(2)
C356 C351 O35 123.30(19)
C352 C351 O35 114.3(2)
C353 C352 C351 118.9(3)
C353 C352 H352 120.5
C351 C352 H352 120.5
C354 C353 C352 120.4(3)
C354 C353 H353 119.8
C352 C353 H353 119.8
C353 C354 C355 120.1(3)
C353 C354 H354 119.9
C355 C354 H354 119.9
C354 C355 C356 120.6(3)
C354 C355 H355 119.7
C356 C355 H355 119.7
C351 C356 C355 117.6(2)
C351 C356 H356 121.2
C355 C356 H356 121.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.223(2)
C1 C2 1.462(3)
C1 C12 1.466(3)
C2 C3 1.332(3)
C2 H2 0.9300
C3 C34 1.437(3)
C3 H3 0.9300
S11 C15 1.684(5)
S11 C12 1.705(2)
C12 C13 1.322(7)
C13 C14 1.402(10)
C13 H13 0.9300
C14 C15 1.327(5)
C14 H14 0.9300
C15 H15 0.9300
S21 C25 1.685(12)
C23 C24 1.404(14)
C23 H23 0.9300
C24 C25 1.329(9)
C24 H24 0.9300
C25 H25 0.9300
N31 C35 1.349(2)
N31 N32 1.379(2)
N31 C311 1.424(2)
N32 C33 1.323(3)
C33 C34 1.416(3)
C33 C331 1.492(3)
C34 C35 1.374(3)
C35 O35 1.356(2)
C311 C316 1.378(3)
C311 C312 1.379(3)
C312 C313 1.376(3)
C312 H312 0.9300
C313 C314 1.377(3)
C313 H313 0.9300
C314 C315 1.375(3)
C314 H314 0.9300
C315 C316 1.378(3)
C315 H315 0.9300
C316 H316 0.9300
C331 H31A 0.9600
C331 H31B 0.9600
C331 H31C 0.9600
O35 C351 1.398(2)
C351 C356 1.365(3)
C351 C352 1.368(3)
C352 C353 1.366(4)
C352 H352 0.9300
C353 C354 1.364(4)
C353 H353 0.9300
C354 C355 1.367(4)
C354 H354 0.9300
C355 C356 1.391(3)
C355 H355 0.9300
C356 H356 0.9300
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C14 H14 N32 2_645 0.93 2.62 3.462(9) 151 y
C25 H25 N32 2_645 0.93 2.51 3.33(5) 148 y
C314 H314 O1 1_454 0.93 2.38 3.305(3) 175 y
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
O1 C1 C2 C3 -2.8(3)
C12 C1 C2 C3 177.6(2)
C1 C2 C3 C34 177.2(2)
O1 C1 C12 C13 -175.3(10)
C2 C1 C12 C13 4.3(11)
O1 C1 C12 S11 4.0(3)
C2 C1 C12 S11 -176.40(16)
C15 S11 C12 C13 -0.6(9)
C15 S11 C12 C1 180.0(4)
C1 C12 C13 C14 -179.5(10)
S11 C12 C13 C14 1.1(17)
C12 C13 C14 C15 -1(2)
C13 C14 C15 S11 0.7(17)
C12 S11 C15 C14 -0.1(11)
C23 C24 C25 S21 -12(9)
C35 N31 N32 C33 -1.3(2)
C311 N31 N32 C33 -178.64(17)
N31 N32 C33 C34 0.8(2)
N31 N32 C33 C331 178.55(18)
N32 C33 C34 C35 0.0(2)
C331 C33 C34 C35 -177.6(2)
N32 C33 C34 C3 176.16(19)
C331 C33 C34 C3 -1.4(4)
C2 C3 C34 C35 4.2(4)
C2 C3 C34 C33 -171.0(2)
N32 N31 C35 O35 -172.30(16)
C311 N31 C35 O35 4.7(3)
N32 N31 C35 C34 1.3(2)
C311 N31 C35 C34 178.29(18)
C33 C34 C35 N31 -0.8(2)
C3 C34 C35 N31 -176.83(19)
C33 C34 C35 O35 172.0(2)
C3 C34 C35 O35 -4.1(4)
C35 N31 C311 C316 -148.8(2)
N32 N31 C311 C316 27.9(3)
C35 N31 C311 C312 32.6(3)
N32 N31 C311 C312 -150.69(18)
C316 C311 C312 C313 0.5(3)
N31 C311 C312 C313 179.09(18)
C311 C312 C313 C314 0.2(3)
C312 C313 C314 C315 -0.7(3)
C313 C314 C315 C316 0.6(3)
C314 C315 C316 C311 0.1(3)
C312 C311 C316 C315 -0.6(3)
N31 C311 C316 C315 -179.25(18)
N31 C35 O35 C351 -109.5(2)
C34 C35 O35 C351 78.5(3)
C35 O35 C351 C356 7.1(3)
C35 O35 C351 C352 -174.51(18)
C356 C351 C352 C353 0.2(4)
O35 C351 C352 C353 -178.2(2)
C351 C352 C353 C354 -0.1(5)
C352 C353 C354 C355 0.0(5)
C353 C354 C355 C356 0.0(5)
C352 C351 C356 C355 -0.2(4)
O35 C351 C356 C355 178.1(2)
C354 C355 C356 C351 0.0(4)
_cod_database_fobs_code 2243214