# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_exp_1114
_database_code_depnum_ccdc_archive 'CCDC 1981382'
loop_
_audit_author_name
_audit_author_address
'Junliang Zhang'
;East China Normal University
China
;
_audit_update_record
;
2020-02-02 deposited with the CCDC. 2020-05-29 downloaded from the CCDC.
;
_audit_creation_date 2019-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C25 H23 N O5 S'
_chemical_formula_sum 'C25 H23 N O5 S'
_chemical_formula_weight 449.50
_chemical_absolute_configuration unk
_chemical_melting_point ?
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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 5.91430(10)
_cell_length_b 12.5172(3)
_cell_length_c 14.5829(3)
_cell_angle_alpha 90
_cell_angle_beta 97.421(2)
_cell_angle_gamma 90
_cell_volume 1070.54(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 13639
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 74.2160
_cell_measurement_theta_min 4.6380
_shelx_estimated_absorpt_T_max 0.776
_shelx_estimated_absorpt_T_min 0.671
_exptl_absorpt_coefficient_mu 1.667
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.13267
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_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 1.394
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 472
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.16
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1044
_diffrn_reflns_av_unetI/netI 0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 20571
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full 67.050
_diffrn_reflns_theta_max 67.050
_diffrn_reflns_theta_min 3.056
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -7.00 88.00 1.00 1.00 -- 0.00 57.00 30.00 95
2 \w -20.00 16.00 1.00 1.00 -- 0.00 57.00-150.00 36
3 \w 38.00 64.00 1.00 1.00 -- 0.00 38.00 30.00 26
4 \w 16.00 89.00 1.00 1.00 -- 0.00 57.00 -90.00 73
5 \w -23.00 12.00 1.00 1.00 -- 0.00 57.00 -90.00 35
6 \w -23.00 53.00 1.00 1.00 -- 0.00 19.00 90.00 76
7 \w 23.00 59.00 1.00 1.00 -- 0.00 57.00-150.00 36
8 \w -18.00 18.00 1.00 1.00 -- 0.00 38.00 30.00 36
9 \w 5.00 71.00 1.00 1.00 -- 0.00 38.00 -30.00 66
10 \w -19.00 57.00 1.00 1.00 -- 0.00 57.00 150.00 76
11 \w 125.00 185.00 1.00 1.00 -- 95.80 68.00 -31.97 60
12 \w 65.00 91.00 1.00 1.00 -- 95.80 78.00 25.77 26
13 \w 121.00 172.00 1.00 1.00 -- 95.80 78.00 25.77 51
14 \w 75.00 143.00 1.00 1.00 -- 95.80 45.00-180.00 68
15 \w 110.00 185.00 1.00 1.00 -- 95.80 80.00 138.88 75
16 \w 70.00 96.00 1.00 1.00 -- 95.80 68.00 -31.97 26
17 \w 67.00 93.00 1.00 1.00 -- 95.80 71.00 86.65 26
18 \w 64.00 90.00 1.00 1.00 -- 95.80 80.00 138.88 26
19 \w 64.00 90.00 1.00 1.00 -- 95.80 82.00 -30.00 26
20 \w 79.00 127.00 1.00 1.00 -- 95.80 -82.00 150.00 48
21 \w 71.00 97.00 1.00 1.00 -- 95.80 61.00-180.00 26
22 \w 65.00 97.00 1.00 1.00 -- 95.80 77.00 120.00 32
23 \w 75.00 185.00 1.00 1.00 -- 95.80 45.00-120.00 110
24 \w 15.00 126.00 1.00 1.00 -- 95.80 -82.00 30.00 111
25 \w 64.00 90.00 1.00 1.00 -- 95.80 82.00 0.00 26
26 \w 136.00 162.00 1.00 1.00 -- 95.80 82.00 0.00 26
27 \w 64.00 90.00 1.00 1.00 -- 95.80 82.00 -90.00 26
28 \w 43.00 68.00 1.00 1.00 -- 95.80 -82.00-150.00 25
29 \w 86.00 127.00 1.00 1.00 -- 95.80 -82.00-150.00 41
30 \w 137.00 164.00 1.00 1.00 -- 95.80 76.00 51.51 27
31 \w 65.00 91.00 1.00 1.00 -- 95.80 76.00 133.57 26
32 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00 -60.00 26
33 \w 75.00 118.00 1.00 1.00 -- 95.80 45.00 -30.00 43
34 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00-150.00 26
35 \w 65.00 106.00 1.00 1.00 -- 95.80 76.00 51.51 41
36 \w 94.00 185.00 1.00 1.00 -- 95.80 82.00 90.00 91
37 \w 155.00 185.00 1.00 1.00 -- 95.80 45.00 -30.00 30
38 \w 63.00 88.00 1.00 1.00 -- 95.80 82.00 90.00 25
39 \w 39.00 125.00 1.00 1.00 -- 95.80 -82.00 -60.00 86
40 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00-180.00 26
41 \w 75.00 185.00 1.00 1.00 -- 95.80 45.00 60.00 110
42 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00 -90.00 26
43 \w 71.00 97.00 1.00 1.00 -- 95.80 61.00 150.00 26
44 \w 75.00 183.00 1.00 1.00 -- 95.80 45.00-150.00 108
45 \w 75.00 103.00 1.00 1.00 -- 95.80 45.00 30.00 28
46 \w 64.00 126.00 1.00 1.00 -- 95.80 -77.00 60.00 62
47 \w 71.00 105.00 1.00 1.00 -- 95.80 61.00 -90.00 34
48 \w 125.00 183.00 1.00 1.00 -- 95.80 61.00 -90.00 58
49 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00-120.00 25
50 \w 65.00 128.00 1.00 1.00 -- 95.80 77.00 -30.00 63
51 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00 0.00 25
52 \w 63.00 89.00 1.00 1.00 -- 95.80 82.00 30.00 26
53 \w 34.00 59.00 1.00 1.00 -- 95.80 -77.00 60.00 25
54 \w 38.00 127.00 1.00 1.00 -- 95.80 -82.00 120.00 89
55 \w 68.00 94.00 1.00 1.00 -- 95.80 69.00 4.23 26
56 \w 131.00 157.00 1.00 1.00 -- 95.80 71.00 86.65 26
57 \w 134.00 177.00 1.00 1.00 -- 95.80 51.00 -58.52 43
58 \w 71.00 97.00 1.00 1.00 -- 95.80 61.00-120.00 26
59 \w 71.00 123.00 1.00 1.00 -- 95.80 61.00 90.00 52
60 \w 66.00 116.00 1.00 1.00 -- 95.80 77.00 60.00 50
61 \w 74.00 108.00 1.00 1.00 -- 95.80 51.00 -58.52 34
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.2612602000
_diffrn_orient_matrix_UB_12 0.0004696000
_diffrn_orient_matrix_UB_13 0.0247260000
_diffrn_orient_matrix_UB_21 0.0247815000
_diffrn_orient_matrix_UB_22 0.0513311000
_diffrn_orient_matrix_UB_23 -0.0941722000
_diffrn_orient_matrix_UB_31 -0.0124098000
_diffrn_orient_matrix_UB_32 0.1119236000
_diffrn_orient_matrix_UB_33 0.0430371000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.875
_reflns_Friedel_fraction_full 0.967
_reflns_Friedel_fraction_max 0.967
_reflns_number_gt 3642
_reflns_number_total 3747
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.455
_refine_diff_density_min -0.506
_refine_diff_density_rms 0.073
_refine_ls_abs_structure_details
;
Flack x determined using 1620 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.02(2)
_refine_ls_extinction_coef .
_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 291
_refine_ls_number_reflns 3747
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0532
_refine_ls_R_factor_gt 0.0523
_refine_ls_restrained_S_all 1.050
_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^)+(0.1164P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1408
_refine_ls_wR_factor_ref 0.1417
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C13(H13), C15(H15), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18),
C19(H19), C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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 0.50899(15) 0.33082(8) 0.63956(6) 0.0157(3) Uani 1 1 d . . . . .
O1 O 0.4103(5) 0.2462(3) 0.58209(19) 0.0222(7) Uani 1 1 d . . . . .
O2 O 0.7506(5) 0.3490(3) 0.65010(19) 0.0212(7) Uani 1 1 d . . . . .
O3 O 0.1917(5) 0.4180(2) 0.44416(18) 0.0172(6) Uani 1 1 d . . . . .
O4 O -0.0630(5) 0.4709(3) -0.0396(2) 0.0269(7) Uani 1 1 d . . . . .
O5 O 0.2629(5) 0.5628(3) -0.03407(19) 0.0227(7) Uani 1 1 d . . . . .
N1 N 0.3873(6) 0.4408(3) 0.5970(2) 0.0160(7) Uani 1 1 d . . . . .
C1 C 0.2198(7) 0.2669(3) 0.7597(3) 0.0166(8) Uani 1 1 d . . . . .
H1 H 0.119063 0.249981 0.707412 0.020 Uiso 1 1 calc R . . . .
C2 C 0.1613(7) 0.2464(4) 0.8467(3) 0.0183(8) Uani 1 1 d . . . . .
H2 H 0.020697 0.215481 0.852251 0.022 Uiso 1 1 calc R . . . .
C3 C 0.3096(7) 0.2712(3) 0.9267(3) 0.0181(8) Uani 1 1 d . . . . .
C4 C 0.5173(7) 0.3203(4) 0.9156(3) 0.0194(8) Uani 1 1 d . . . . .
H4 H 0.616208 0.339379 0.967840 0.023 Uiso 1 1 calc R . . . .
C5 C 0.5789(6) 0.3410(3) 0.8292(3) 0.0178(8) Uani 1 1 d . . . . .
H5 H 0.718109 0.373213 0.823488 0.021 Uiso 1 1 calc R . . . .
C6 C 0.4305(6) 0.3132(3) 0.7505(3) 0.0159(8) Uani 1 1 d . . . . .
C7 C 0.4308(7) 0.5443(3) 0.6364(3) 0.0166(8) Uani 1 1 d . . . . .
C8 C 0.6242(7) 0.5802(4) 0.6918(3) 0.0192(9) Uani 1 1 d . . . . .
H8 H 0.745525 0.534705 0.710848 0.023 Uiso 1 1 calc R . . . .
C9 C 0.6286(8) 0.6884(4) 0.7180(3) 0.0230(9) Uani 1 1 d . . . . .
H9 H 0.756239 0.715384 0.754642 0.028 Uiso 1 1 calc R . . . .
C10 C 0.4465(8) 0.7554(4) 0.6903(3) 0.0256(9) Uani 1 1 d . . . . .
H10 H 0.452355 0.826333 0.709297 0.031 Uiso 1 1 calc R . . . .
C11 C 0.2556(8) 0.7180(4) 0.6345(3) 0.0238(10) Uani 1 1 d . . . . .
H11 H 0.134581 0.763566 0.615201 0.029 Uiso 1 1 calc R . . . .
C12 C 0.2473(7) 0.6109(4) 0.6075(3) 0.0175(8) Uani 1 1 d . . . . .
C13 C 0.0708(7) 0.5541(4) 0.5425(3) 0.0188(9) Uani 1 1 d . . . . .
H13 H -0.079640 0.555895 0.563794 0.023 Uiso 1 1 calc R . . . .
C14 C 0.0621(7) 0.5928(4) 0.4418(3) 0.0195(9) Uani 1 1 d . . . . .
H14A H -0.089013 0.583740 0.407961 0.023 Uiso 1 1 calc R . . . .
H14B H 0.106450 0.667236 0.439194 0.023 Uiso 1 1 calc R . . . .
C15 C 0.2340(7) 0.5204(3) 0.4042(3) 0.0167(9) Uani 1 1 d . . . . .
H15 H 0.388921 0.544166 0.427036 0.020 Uiso 1 1 calc R . . . .
C16 C 0.1635(7) 0.4379(3) 0.5373(3) 0.0168(8) Uani 1 1 d . . . . .
H16 H 0.060153 0.385840 0.560086 0.020 Uiso 1 1 calc R . . . .
C17 C 0.2077(7) 0.5105(3) 0.3002(3) 0.0174(8) Uani 1 1 d . . . . .
C18 C 0.3759(7) 0.5505(3) 0.2517(3) 0.0171(8) Uani 1 1 d . . . . .
H18 H 0.508457 0.578808 0.283836 0.020 Uiso 1 1 calc R . . . .
C19 C 0.3484(7) 0.5489(3) 0.1549(3) 0.0166(8) Uani 1 1 d . . . . .
H19 H 0.462129 0.575751 0.122866 0.020 Uiso 1 1 calc R . . . .
C20 C 0.1501(7) 0.5070(3) 0.1072(3) 0.0166(8) Uani 1 1 d . . . . .
C21 C -0.0159(7) 0.4634(4) 0.1556(3) 0.0202(9) Uani 1 1 d . . . . .
H21 H -0.146144 0.432871 0.123542 0.024 Uiso 1 1 calc R . . . .
C22 C 0.0124(7) 0.4653(3) 0.2520(3) 0.0197(9) Uani 1 1 d . . . . .
H22 H -0.099131 0.436394 0.284064 0.024 Uiso 1 1 calc R . . . .
C23 C 0.1023(7) 0.5091(4) 0.0041(3) 0.0186(8) Uani 1 1 d . . . . .
C24 C 0.2212(8) 0.5701(4) -0.1340(3) 0.0284(10) Uani 1 1 d . . . . .
H24A H 0.214807 0.499638 -0.160067 0.043 Uiso 1 1 calc GR . . . .
H24B H 0.342304 0.609670 -0.156092 0.043 Uiso 1 1 calc GR . . . .
H24C H 0.078874 0.606001 -0.151930 0.043 Uiso 1 1 calc GR . . . .
C25 C 0.2499(8) 0.2426(4) 1.0206(3) 0.0254(10) Uani 1 1 d . . . . .
H25A H 0.087824 0.247248 1.020250 0.038 Uiso 1 1 calc GR . . . .
H25B H 0.324230 0.291222 1.065686 0.038 Uiso 1 1 calc GR . . . .
H25C H 0.299622 0.171024 1.035866 0.038 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0209(5) 0.0137(5) 0.0138(4) 0.0009(4) 0.0073(3) 0.0028(3)
O1 0.0324(16) 0.0186(16) 0.0164(14) -0.0022(12) 0.0067(12) 0.0043(13)
O2 0.0200(14) 0.0242(17) 0.0215(13) 0.0027(12) 0.0106(11) 0.0053(12)
O3 0.0276(15) 0.0130(15) 0.0125(13) 0.0023(11) 0.0085(11) -0.0001(11)
O4 0.0316(17) 0.0310(19) 0.0183(15) -0.0020(13) 0.0040(12) -0.0096(14)
O5 0.0287(15) 0.0277(17) 0.0132(14) 0.0007(13) 0.0082(11) -0.0068(14)
N1 0.0246(17) 0.0093(16) 0.0150(15) 0.0012(13) 0.0056(13) 0.0034(13)
C1 0.0173(17) 0.014(2) 0.0194(19) -0.0001(16) 0.0045(15) 0.0001(15)
C2 0.0181(19) 0.016(2) 0.023(2) -0.0004(17) 0.0082(16) -0.0003(16)
C3 0.0234(19) 0.013(2) 0.019(2) -0.0003(16) 0.0096(16) 0.0041(16)
C4 0.0244(19) 0.019(2) 0.0150(17) 0.0004(17) 0.0022(15) -0.0023(17)
C5 0.0183(17) 0.016(2) 0.0191(18) -0.0012(17) 0.0030(14) -0.0021(16)
C6 0.0180(17) 0.013(2) 0.0168(18) -0.0020(16) 0.0028(14) 0.0043(15)
C7 0.023(2) 0.015(2) 0.0134(18) 0.0011(16) 0.0098(15) -0.0013(16)
C8 0.024(2) 0.019(2) 0.0161(19) 0.0005(16) 0.0098(16) 0.0000(16)
C9 0.030(2) 0.020(2) 0.021(2) -0.0029(18) 0.0109(17) -0.0078(18)
C10 0.038(2) 0.017(2) 0.024(2) -0.0027(18) 0.0121(18) -0.0010(18)
C11 0.034(2) 0.019(2) 0.021(2) -0.0014(18) 0.0115(18) 0.0050(17)
C12 0.024(2) 0.016(2) 0.0144(18) 0.0048(16) 0.0117(15) 0.0022(16)
C13 0.024(2) 0.019(2) 0.0154(19) 0.0004(17) 0.0101(16) 0.0044(17)
C14 0.027(2) 0.017(2) 0.016(2) 0.0033(17) 0.0068(16) 0.0047(16)
C15 0.027(2) 0.011(2) 0.0138(19) 0.0025(15) 0.0085(16) -0.0022(15)
C16 0.021(2) 0.018(2) 0.0128(18) 0.0014(16) 0.0087(15) -0.0002(16)
C17 0.026(2) 0.013(2) 0.0147(19) 0.0025(15) 0.0083(16) 0.0016(16)
C18 0.0202(19) 0.016(2) 0.0164(19) -0.0003(16) 0.0083(15) -0.0029(16)
C19 0.0209(19) 0.013(2) 0.0179(19) 0.0014(16) 0.0101(15) 0.0020(15)
C20 0.0244(19) 0.0139(19) 0.0131(18) -0.0003(15) 0.0082(15) 0.0011(15)
C21 0.024(2) 0.021(2) 0.0178(19) -0.0034(17) 0.0088(15) -0.0056(17)
C22 0.027(2) 0.019(2) 0.0153(18) 0.0006(17) 0.0109(16) -0.0029(17)
C23 0.024(2) 0.016(2) 0.017(2) -0.0008(16) 0.0084(16) 0.0004(16)
C24 0.042(3) 0.032(3) 0.013(2) 0.0051(19) 0.0124(18) 0.000(2)
C25 0.033(2) 0.023(2) 0.023(2) 0.0019(19) 0.0129(18) 0.0014(19)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.428(3) . ?
S1 O2 1.436(3) . ?
S1 N1 1.638(3) . ?
S1 C6 1.753(4) . ?
O3 C15 1.443(5) . ?
O3 C16 1.412(4) . ?
O4 C23 1.196(5) . ?
O5 C23 1.342(5) . ?
O5 C24 1.449(5) . ?
N1 C7 1.428(5) . ?
N1 C16 1.488(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.381(6) . ?
C1 C6 1.396(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.401(6) . ?
C3 C4 1.401(6) . ?
C3 C25 1.500(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(5) . ?
C7 C8 1.387(6) . ?
C7 C12 1.390(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.406(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.386(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.396(7) . ?
C12 C13 1.496(6) . ?
C13 H13 0.9800 . ?
C13 C14 1.541(5) . ?
C13 C16 1.560(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.517(6) . ?
C15 H15 0.9800 . ?
C15 C17 1.509(5) . ?
C16 H16 0.9800 . ?
C17 C18 1.387(6) . ?
C17 C22 1.392(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.400(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(6) . ?
C20 C21 1.393(6) . ?
C20 C23 1.492(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.394(6) . ?
C22 H22 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
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 120.41(18) . . ?
O1 S1 N1 105.96(17) . . ?
O1 S1 C6 108.12(19) . . ?
O2 S1 N1 106.84(18) . . ?
O2 S1 C6 107.45(17) . . ?
N1 S1 C6 107.44(18) . . ?
C16 O3 C15 106.2(3) . . ?
C23 O5 C24 114.3(3) . . ?
C7 N1 S1 124.3(3) . . ?
C7 N1 C16 111.0(3) . . ?
C16 N1 S1 121.0(3) . . ?
C2 C1 H1 120.0 . . ?
C2 C1 C6 119.9(4) . . ?
C6 C1 H1 120.0 . . ?
C1 C2 H2 119.4 . . ?
C1 C2 C3 121.3(4) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C4 117.7(4) . . ?
C2 C3 C25 120.8(4) . . ?
C4 C3 C25 121.5(4) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(4) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 S1 119.2(3) . . ?
C1 C6 C5 119.9(4) . . ?
C5 C6 S1 120.9(3) . . ?
C8 C7 N1 128.3(4) . . ?
C8 C7 C12 122.4(4) . . ?
C12 C7 N1 109.2(3) . . ?
C7 C8 H8 121.5 . . ?
C7 C8 C9 117.1(4) . . ?
C9 C8 H8 121.5 . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(4) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.1(4) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 C11 119.5(4) . . ?
C7 C12 C13 111.2(4) . . ?
C11 C12 C13 129.1(4) . . ?
C12 C13 H13 112.1 . . ?
C12 C13 C14 112.9(4) . . ?
C12 C13 C16 104.6(3) . . ?
C14 C13 H13 112.1 . . ?
C14 C13 C16 102.5(3) . . ?
C16 C13 H13 112.1 . . ?
C13 C14 H14A 111.3 . . ?
C13 C14 H14B 111.3 . . ?
H14A C14 H14B 109.2 . . ?
C15 C14 C13 102.4(3) . . ?
C15 C14 H14A 111.3 . . ?
C15 C14 H14B 111.3 . . ?
O3 C15 C14 103.1(3) . . ?
O3 C15 H15 109.7 . . ?
O3 C15 C17 109.4(3) . . ?
C14 C15 H15 109.7 . . ?
C17 C15 C14 115.2(3) . . ?
C17 C15 H15 109.7 . . ?
O3 C16 N1 111.1(3) . . ?
O3 C16 C13 107.3(3) . . ?
O3 C16 H16 111.4 . . ?
N1 C16 C13 103.9(3) . . ?
N1 C16 H16 111.4 . . ?
C13 C16 H16 111.4 . . ?
C18 C17 C15 119.7(4) . . ?
C18 C17 C22 119.5(4) . . ?
C22 C17 C15 120.8(4) . . ?
C17 C18 H18 119.6 . . ?
C17 C18 C19 120.8(4) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.5(4) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 119.9(4) . . ?
C19 C20 C23 122.4(4) . . ?
C21 C20 C23 117.6(4) . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.3(4) . . ?
C22 C21 H21 119.9 . . ?
C17 C22 C21 120.0(4) . . ?
C17 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
O4 C23 O5 123.6(4) . . ?
O4 C23 C20 124.4(4) . . ?
O5 C23 C20 112.0(3) . . ?
O5 C24 H24A 109.5 . . ?
O5 C24 H24B 109.5 . . ?
O5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C3 C25 H25A 109.5 . . ?
C3 C25 H25B 109.5 . . ?
C3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
_iucr_refine_instructions_details
;
TITL exp_1114_a.res in P2(1)
exp_1114.res
created by SHELXL-2017/1 at 15:01:29 on 10-Dec-2019
REM Old TITL exp_1114 in P2(1)
REM SHELXT solution in P2(1)
REM R1 0.093, Rweak 0.031, Alpha 0.003, Orientation as input
REM Flack x = -0.023 ( 0.023 ) from Parsons' quotients
REM Formula found by SHELXT: C25 N O5 S
CELL 1.54184 5.9143 12.5172 14.5829 90 97.421 90
ZERR 2 0.0001 0.0003 0.0003 0 0.002 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O S
UNIT 50 46 2 10 2
L.S. 64
PLAN 6
SIZE 0.26 0.22 0.16
BOND $H
list 4
fmap 2 53
ACTA
SHEL 999 0.837
OMIT 4 -13 1
OMIT 0 5 17
OMIT -1 5 17
OMIT -3 -14 1
OMIT 2 -14 0
OMIT 0 13 9
OMIT -5 -4 14
OMIT -2 -14 1
OMIT -3 -14 3
OMIT 6 2 8
OMIT 1 -14 0
OMIT 1 -6 4
OMIT -1 -1 5
OMIT -2 0 4
OMIT 2 -1 6
OMIT -2 -5 8
REM
REM
REM
WGHT 0.116400
FVAR 0.97733
S1 5 0.508991 0.330819 0.639562 11.00000 0.02094 0.01369 =
0.01376 0.00094 0.00728 0.00281
O1 4 0.410344 0.246150 0.582086 11.00000 0.03245 0.01861 =
0.01640 -0.00220 0.00671 0.00429
O2 4 0.750638 0.349022 0.650100 11.00000 0.02001 0.02423 =
0.02152 0.00275 0.01058 0.00530
O3 4 0.191664 0.417951 0.444156 11.00000 0.02756 0.01299 =
0.01251 0.00225 0.00846 -0.00014
O4 4 -0.063024 0.470879 -0.039578 11.00000 0.03161 0.03096 =
0.01831 -0.00201 0.00403 -0.00961
O5 4 0.262853 0.562811 -0.034066 11.00000 0.02868 0.02767 =
0.01324 0.00073 0.00821 -0.00679
N1 3 0.387344 0.440771 0.597000 11.00000 0.02457 0.00932 =
0.01498 0.00118 0.00564 0.00336
C1 1 0.219848 0.266934 0.759728 11.00000 0.01730 0.01365 =
0.01935 -0.00005 0.00448 0.00005
AFIX 43
H1 2 0.119063 0.249981 0.707412 11.00000 -1.20000
AFIX 0
C2 1 0.161292 0.246376 0.846703 11.00000 0.01809 0.01552 =
0.02275 -0.00043 0.00817 -0.00029
AFIX 43
H2 2 0.020697 0.215481 0.852251 11.00000 -1.20000
AFIX 0
C3 1 0.309588 0.271163 0.926702 11.00000 0.02340 0.01326 =
0.01949 -0.00027 0.00963 0.00405
C4 1 0.517251 0.320253 0.915606 11.00000 0.02439 0.01883 =
0.01495 0.00035 0.00222 -0.00232
AFIX 43
H4 2 0.616208 0.339379 0.967840 11.00000 -1.20000
AFIX 0
C5 1 0.578919 0.340998 0.829194 11.00000 0.01832 0.01615 =
0.01909 -0.00121 0.00298 -0.00214
AFIX 43
H5 2 0.718109 0.373213 0.823488 11.00000 -1.20000
AFIX 0
C6 1 0.430461 0.313182 0.750452 11.00000 0.01804 0.01305 =
0.01680 -0.00200 0.00284 0.00435
C7 1 0.430772 0.544328 0.636413 11.00000 0.02343 0.01486 =
0.01344 0.00105 0.00983 -0.00131
C8 1 0.624165 0.580198 0.691840 11.00000 0.02424 0.01899 =
0.01614 0.00053 0.00977 -0.00001
AFIX 43
H8 2 0.745525 0.534705 0.710848 11.00000 -1.20000
AFIX 0
C9 1 0.628625 0.688386 0.718023 11.00000 0.03050 0.02000 =
0.02064 -0.00293 0.01092 -0.00785
AFIX 43
H9 2 0.756239 0.715384 0.754642 11.00000 -1.20000
AFIX 0
C10 1 0.446525 0.755363 0.690268 11.00000 0.03782 0.01717 =
0.02401 -0.00274 0.01212 -0.00095
AFIX 43
H10 2 0.452355 0.826333 0.709297 11.00000 -1.20000
AFIX 0
C11 1 0.255563 0.717952 0.634454 11.00000 0.03381 0.01865 =
0.02100 -0.00138 0.01149 0.00505
AFIX 43
H11 2 0.134581 0.763566 0.615201 11.00000 -1.20000
AFIX 0
C12 1 0.247251 0.610889 0.607522 11.00000 0.02407 0.01638 =
0.01445 0.00479 0.01174 0.00217
C13 1 0.070798 0.554123 0.542461 11.00000 0.02420 0.01886 =
0.01545 0.00044 0.01014 0.00437
AFIX 13
H13 2 -0.079640 0.555895 0.563794 11.00000 -1.20000
AFIX 0
C14 1 0.062091 0.592801 0.441781 11.00000 0.02655 0.01662 =
0.01634 0.00333 0.00683 0.00467
AFIX 23
H14A 2 -0.089013 0.583740 0.407961 11.00000 -1.20000
H14B 2 0.106450 0.667236 0.439194 11.00000 -1.20000
AFIX 0
C15 1 0.233994 0.520351 0.404218 11.00000 0.02661 0.01121 =
0.01384 0.00251 0.00851 -0.00219
AFIX 13
H15 2 0.388921 0.544166 0.427036 11.00000 -1.20000
AFIX 0
C16 1 0.163518 0.437860 0.537318 11.00000 0.02111 0.01814 =
0.01277 0.00136 0.00870 -0.00020
AFIX 13
H16 2 0.060153 0.385840 0.560086 11.00000 -1.20000
AFIX 0
C17 1 0.207718 0.510473 0.300229 11.00000 0.02572 0.01337 =
0.01471 0.00250 0.00835 0.00157
C18 1 0.375864 0.550532 0.251701 11.00000 0.02016 0.01614 =
0.01641 -0.00026 0.00829 -0.00288
AFIX 43
H18 2 0.508457 0.578808 0.283836 11.00000 -1.20000
AFIX 0
C19 1 0.348382 0.548913 0.154904 11.00000 0.02089 0.01288 =
0.01789 0.00139 0.01007 0.00201
AFIX 43
H19 2 0.462129 0.575751 0.122866 11.00000 -1.20000
AFIX 0
C20 1 0.150091 0.506951 0.107153 11.00000 0.02435 0.01392 =
0.01305 -0.00029 0.00824 0.00110
C21 1 -0.015889 0.463374 0.155612 11.00000 0.02379 0.02071 =
0.01779 -0.00336 0.00881 -0.00564
AFIX 43
H21 2 -0.146144 0.432871 0.123542 11.00000 -1.20000
AFIX 0
C22 1 0.012434 0.465295 0.251981 11.00000 0.02657 0.01924 =
0.01534 0.00061 0.01094 -0.00292
AFIX 43
H22 2 -0.099131 0.436394 0.284064 11.00000 -1.20000
AFIX 0
C23 1 0.102279 0.509114 0.004143 11.00000 0.02433 0.01596 =
0.01706 -0.00080 0.00840 0.00036
C24 1 0.221197 0.570149 -0.133963 11.00000 0.04220 0.03215 =
0.01328 0.00513 0.01238 -0.00031
AFIX 137
H24A 2 0.214807 0.499638 -0.160067 11.00000 -1.50000
H24B 2 0.342304 0.609670 -0.156092 11.00000 -1.50000
H24C 2 0.078874 0.606001 -0.151930 11.00000 -1.50000
AFIX 0
C25 1 0.249946 0.242592 1.020579 11.00000 0.03260 0.02279 =
0.02323 0.00189 0.01287 0.00138
AFIX 137
H25A 2 0.087824 0.247248 1.020250 11.00000 -1.50000
H25B 2 0.324230 0.291222 1.065686 11.00000 -1.50000
H25C 2 0.299622 0.171024 1.035866 11.00000 -1.50000
AFIX 0
HKLF 4
REM exp_1114_a.res in P2(1)
REM R1 = 0.0523 for 3642 Fo > 4sig(Fo) and 0.0532 for all 3747 data
REM 291 parameters refined using 1 restraints
END
WGHT 0.1166 0.0000
REM Highest difference peak 0.455, deepest hole -0.506, 1-sigma level 0.073
Q1 1 0.6348 0.3314 0.7518 11.00000 0.05 0.45
Q2 1 0.5202 0.3937 0.7811 11.00000 0.05 0.36
Q3 1 0.5179 0.2600 0.5011 11.00000 0.05 0.30
Q4 1 0.3994 0.3240 0.5184 11.00000 0.05 0.30
Q5 1 0.5995 0.3433 0.5563 11.00000 0.05 0.29
Q6 1 0.4972 0.4016 0.4990 11.00000 0.05 0.28
REM The information below was added by Olex2.
REM
REM R1 = 0.0523 for 3642 Fo > 4sig(Fo) and 0.0532 for all 21798 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.45, deepest hole -0.51
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0532
REM R1_gt = 0.0523
REM wR_ref = 0.1417
REM GOOF = 1.050
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 21798
REM Reflections_gt = 3642
REM Parameters = n/a
REM Hole = -0.51
REM Peak = 0.45
REM Flack = -0.02(2)
;
_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 3.234
_oxdiff_exptl_absorpt_empirical_full_min 0.352
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_exp_815
_database_code_depnum_ccdc_archive 'CCDC 1981384'
loop_
_audit_author_name
_audit_author_address
'Junliang Zhang'
;East China Normal University
China
;
_audit_update_record
;
2020-02-02 deposited with the CCDC. 2020-05-29 downloaded from the CCDC.
;
_audit_creation_date 2019-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C17 H17 N O3 S)'
_chemical_formula_sum 'C34 H34 N2 O6 S2'
_chemical_formula_weight 630.75
_chemical_absolute_configuration ad
_chemical_melting_point ?
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'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 8.90430(10)
_cell_length_b 10.79480(10)
_cell_length_c 31.6319(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3040.46(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 39460
_cell_measurement_temperature 100.0(4)
_cell_measurement_theta_max 74.2070
_cell_measurement_theta_min 4.3100
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.998
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.23950
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_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 1.378
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1328
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.16
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0768
_diffrn_reflns_av_unetI/netI 0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 39
_diffrn_reflns_limit_l_min -39
_diffrn_reflns_number 75990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.528
_diffrn_reflns_theta_min 4.328
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.0(4)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 30.00 74.00 1.00 1.00 -- 0.00 38.00 60.00 44
2 \w -19.00 82.00 1.00 1.00 -- 0.00 38.00-150.00 101
3 \w 60.00 88.00 1.00 1.00 -- 0.00 77.00 -30.00 28
4 \w -26.00 20.00 1.00 1.00 -- 0.00 -19.00 -60.00 46
5 \w -71.00 -45.00 1.00 1.00 -- 0.00 -19.00 -60.00 26
6 \w -14.00 26.00 1.00 1.00 -- 0.00 38.00 60.00 40
7 \w -17.00 56.00 1.00 1.00 -- 0.00 38.00 -30.00 73
8 \w -28.00 -3.00 1.00 1.00 -- 0.00 77.00 -30.00 25
9 \w -30.00 87.00 1.00 1.00 -- 0.00 82.00 -90.00 117
10 \w -73.00 -33.00 1.00 1.00 -- 0.00 -57.00 -60.00 40
11 \w -16.00 21.00 1.00 1.00 -- 0.00 -57.00 -60.00 37
12 \w -13.00 79.00 1.00 1.00 -- 0.00 38.00 120.00 92
13 \w 24.00 49.00 1.00 1.00 -- 0.00 77.00 -30.00 25
14 \w 63.00 88.00 1.00 1.00 -- 95.80 81.00 136.93 25
15 \w 72.00 180.00 1.00 1.00 -- 95.80 57.00 -44.20 108
16 \w 152.00 178.00 1.00 1.00 -- 95.80 78.00 52.49 26
17 \w 71.00 163.00 1.00 1.00 -- 95.80 58.00-103.70 92
18 \w 132.00 185.00 1.00 1.00 -- 95.80 79.00-156.68 53
19 \w 65.00 96.00 1.00 1.00 -- 95.80 78.00 52.49 31
20 \w 75.00 121.00 1.00 1.00 -- 95.80 45.00 170.13 46
21 \w 31.00 107.00 1.00 1.00 -- 95.80 -82.00 60.00 76
22 \w 64.00 89.00 1.00 1.00 -- 95.80 79.00-156.68 25
23 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00-180.00 25
24 \w 63.00 98.00 1.00 1.00 -- 95.80 82.00 30.00 35
25 \w 102.00 128.00 1.00 1.00 -- 95.80 82.00 30.00 26
26 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00 0.00 25
27 \w 118.00 185.00 1.00 1.00 -- 95.80 77.00 0.00 67
28 \w 63.00 88.00 1.00 1.00 -- 95.80 82.00 60.00 25
29 \w 105.00 184.00 1.00 1.00 -- 95.80 82.00 60.00 79
30 \w 63.00 89.00 1.00 1.00 -- 95.80 82.00-120.00 26
31 \w 6.00 128.00 1.00 1.00 -- 95.80 -82.00 120.00 122
32 \w 64.00 127.00 1.00 1.00 -- 95.80 -82.00 -90.00 63
33 \w 146.00 172.00 1.00 1.00 -- 95.80 79.00 -40.56 26
34 \w 153.00 184.00 1.00 1.00 -- 95.80 70.00 90.93 31
35 \w 117.00 183.00 1.00 1.00 -- 95.80 82.00 150.00 66
36 \w 63.00 93.00 1.00 1.00 -- 95.80 82.00 150.00 30
37 \w 11.00 58.00 1.00 1.00 -- 95.80 -82.00 -90.00 47
38 \w 63.00 88.00 1.00 1.00 -- 95.80 82.00 -90.00 25
39 \w 71.00 108.00 1.00 1.00 -- 95.80 61.00-150.00 37
40 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00 90.00 26
41 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00-120.00 25
42 \w 65.00 167.00 1.00 1.00 -- 95.80 77.00 -30.00 102
43 \w 52.00 78.00 1.00 1.00 -- 95.80 -82.00 -30.00 26
44 \w 18.00 120.00 1.00 1.00 -- 95.80 -61.00 120.00 102
45 \w 64.00 113.00 1.00 1.00 -- 95.80 79.00 -40.56 49
46 \w 71.00 123.00 1.00 1.00 -- 95.80 61.00-120.00 52
47 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00 30.00 25
48 \w 63.00 89.00 1.00 1.00 -- 95.80 82.00 120.00 26
49 \w 75.00 156.00 1.00 1.00 -- 95.80 45.00-150.00 81
50 \w 65.00 91.00 1.00 1.00 -- 95.80 77.00 -90.00 26
51 \w 63.00 88.00 1.00 1.00 -- 95.80 82.00 0.00 25
52 \w 119.00 144.00 1.00 1.00 -- 95.80 82.00 0.00 25
53 \w 75.00 101.00 1.00 1.00 -- 95.80 61.00 90.00 26
54 \w 114.00 181.00 1.00 1.00 -- 95.80 61.00 90.00 67
55 \w 113.00 138.00 1.00 1.00 -- 95.80 77.00 120.00 25
56 \w 75.00 100.00 1.00 1.00 -- 95.80 45.00 30.00 25
57 \w 75.00 103.00 1.00 1.00 -- 95.80 45.00 90.00 28
58 \w 63.00 88.00 1.00 1.00 -- 95.80 82.00 90.00 25
59 \w 63.00 89.00 1.00 1.00 -- 95.80 81.00 -57.09 26
60 \w 71.00 97.00 1.00 1.00 -- 95.80 59.00 134.30 26
61 \w 63.00 89.00 1.00 1.00 -- 95.80 82.00 -30.00 26
62 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00 -60.00 25
63 \w 65.00 90.00 1.00 1.00 -- 95.80 77.00 120.00 25
64 \w 140.00 174.00 1.00 1.00 -- 95.80 45.00 120.00 34
65 \w 76.00 103.00 1.00 1.00 -- 95.80 45.00 120.00 27
66 \w 103.00 128.00 1.00 1.00 -- 95.80 82.00-120.00 25
67 \w 120.00 185.00 1.00 1.00 -- 95.80 81.00 136.93 65
68 \w 93.00 119.00 1.00 1.00 -- 95.80 -82.00-180.00 26
69 \w 75.00 114.00 1.00 1.00 -- 95.80 45.00 -60.00 39
70 \w 68.00 167.00 1.00 1.00 -- 95.80 69.00 25.48 99
71 \w 68.00 93.00 1.00 1.00 -- 95.80 70.00 90.93 25
72 \w 130.00 165.00 1.00 1.00 -- 95.80 44.00-163.69 35
73 \w 82.00 111.00 1.00 1.00 -- 95.80 -82.00 -30.00 29
74 \w 76.00 102.00 1.00 1.00 -- 95.80 44.00-163.69 26
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0112666000
_diffrn_orient_matrix_UB_12 0.0916480000
_diffrn_orient_matrix_UB_13 0.0371948000
_diffrn_orient_matrix_UB_21 0.0000644000
_diffrn_orient_matrix_UB_22 -0.1092103000
_diffrn_orient_matrix_UB_23 0.0313264000
_diffrn_orient_matrix_UB_31 0.1727098000
_diffrn_orient_matrix_UB_32 0.0060697000
_diffrn_orient_matrix_UB_33 0.0024052000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.758
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.990
_reflns_number_gt 6061
_reflns_number_total 6165
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.180
_refine_diff_density_min -0.356
_refine_diff_density_rms 0.045
_refine_ls_abs_structure_details
;
Flack x determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.013(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 399
_refine_ls_number_reflns 6165
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0306
_refine_ls_R_factor_gt 0.0300
_refine_ls_restrained_S_all 1.036
_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/[\s^2^(Fo^2^)+(0.0380P)^2^+0.9283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0748
_refine_ls_wR_factor_ref 0.0751
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C7(H7), C8(H8), C24(H24), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
C9(H9A,H9B), C10(H10A,H10B), C25(H25A,H25B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
C19(H19), C20(H20), C21(H21), C22(H22), C29(H29), C30(H30), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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 -0.29512(6) 0.47038(5) 0.53635(2) 0.02276(13) Uani 1 1 d . . . . .
O1 O 0.0365(2) 0.43288(15) 0.49807(5) 0.0281(4) Uani 1 1 d . . . . .
O2 O -0.3149(2) 0.40020(16) 0.49840(5) 0.0287(4) Uani 1 1 d . . . . .
O3 O -0.4167(2) 0.54257(16) 0.55291(5) 0.0286(4) Uani 1 1 d . . . . .
N1 N -0.1575(2) 0.56679(18) 0.52608(6) 0.0240(4) Uani 1 1 d . . . . .
C1 C -0.1046(3) 0.6611(2) 0.55374(7) 0.0219(5) Uani 1 1 d . . . . .
C2 C -0.1657(3) 0.7030(2) 0.59163(7) 0.0254(5) Uani 1 1 d . . . . .
H2 H -0.252092 0.667571 0.602889 0.030 Uiso 1 1 calc R . . . .
C3 C -0.0926(3) 0.7998(2) 0.61197(7) 0.0276(5) Uani 1 1 d . . . . .
H3 H -0.130350 0.828989 0.637512 0.033 Uiso 1 1 calc R . . . .
C4 C 0.0355(3) 0.8540(2) 0.59505(8) 0.0284(5) Uani 1 1 d . . . . .
H4 H 0.082175 0.918947 0.609232 0.034 Uiso 1 1 calc R . . . .
C5 C 0.0944(3) 0.8114(2) 0.55683(8) 0.0274(5) Uani 1 1 d . . . . .
H5 H 0.179893 0.847655 0.545303 0.033 Uiso 1 1 calc R . . . .
C6 C 0.0236(3) 0.7144(2) 0.53638(7) 0.0226(5) Uani 1 1 d . . . . .
C7 C 0.0651(3) 0.6521(2) 0.49523(7) 0.0243(5) Uani 1 1 d . . . . .
H7 H 0.055621 0.708666 0.471133 0.029 Uiso 1 1 calc R . . . .
C8 C -0.0462(3) 0.5427(2) 0.49217(7) 0.0244(5) Uani 1 1 d . . . . .
H8 H -0.095522 0.542135 0.464478 0.029 Uiso 1 1 calc R . . . .
C9 C 0.1804(3) 0.4642(2) 0.51576(8) 0.0296(5) Uani 1 1 d . . . . .
H9A H 0.255019 0.402244 0.508534 0.035 Uiso 1 1 calc R . . . .
H9B H 0.174450 0.471000 0.546291 0.035 Uiso 1 1 calc R . . . .
C10 C 0.2187(3) 0.5878(2) 0.49603(8) 0.0297(5) Uani 1 1 d . . . . .
H10A H 0.258979 0.577675 0.467746 0.036 Uiso 1 1 calc R . . . .
H10B H 0.290257 0.633324 0.513165 0.036 Uiso 1 1 calc R . . . .
C11 C -0.2329(3) 0.3709(2) 0.57701(7) 0.0230(5) Uani 1 1 d . . . . .
C12 C -0.2824(3) 0.3897(2) 0.61837(7) 0.0256(5) Uani 1 1 d . . . . .
H12 H -0.344664 0.456229 0.624855 0.031 Uiso 1 1 calc R . . . .
C13 C -0.2373(3) 0.3079(2) 0.64959(7) 0.0269(5) Uani 1 1 d . . . . .
H13 H -0.269202 0.320902 0.677240 0.032 Uiso 1 1 calc R . . . .
C14 C -0.1456(3) 0.2067(2) 0.64074(7) 0.0243(5) Uani 1 1 d . . . . .
C15 C -0.0961(3) 0.1917(2) 0.59912(8) 0.0259(5) Uani 1 1 d . . . . .
H15 H -0.032824 0.125771 0.592670 0.031 Uiso 1 1 calc R . . . .
C16 C -0.1387(3) 0.2723(2) 0.56719(7) 0.0251(5) Uani 1 1 d . . . . .
H16 H -0.104875 0.260672 0.539662 0.030 Uiso 1 1 calc R . . . .
C17 C -0.1041(3) 0.1161(2) 0.67491(8) 0.0300(5) Uani 1 1 d . . . . .
H17A H -0.064903 0.160178 0.698838 0.045 Uiso 1 1 calc GR . . . .
H17B H -0.029306 0.059886 0.664424 0.045 Uiso 1 1 calc GR . . . .
H17C H -0.191657 0.070315 0.683262 0.045 Uiso 1 1 calc GR . . . .
S2 S 0.44466(6) 0.89248(5) 0.72696(2) 0.02031(12) Uani 1 1 d . . . . .
O4 O 0.4880(2) 0.69132(17) 0.65445(6) 0.0327(4) Uani 1 1 d . . . . .
O5 O 0.59833(18) 0.85579(17) 0.72984(6) 0.0302(4) Uani 1 1 d . . . . .
O6 O 0.37195(19) 0.94789(15) 0.76271(5) 0.0244(3) Uani 1 1 d . . . . .
N2 N 0.3514(2) 0.76716(17) 0.71517(6) 0.0202(4) Uani 1 1 d . . . . .
C18 C 0.1925(2) 0.7539(2) 0.71632(6) 0.0183(4) Uani 1 1 d . . . . .
C19 C 0.0855(3) 0.8362(2) 0.73102(7) 0.0218(4) Uani 1 1 d . . . . .
H19 H 0.112187 0.913755 0.741379 0.026 Uiso 1 1 calc R . . . .
C20 C -0.0637(3) 0.7983(2) 0.72971(7) 0.0254(5) Uani 1 1 d . . . . .
H20 H -0.138096 0.851636 0.739400 0.030 Uiso 1 1 calc R . . . .
C21 C -0.1042(3) 0.6825(2) 0.71425(7) 0.0257(5) Uani 1 1 d . . . . .
H21 H -0.204672 0.658831 0.713849 0.031 Uiso 1 1 calc R . . . .
C22 C 0.0055(3) 0.6022(2) 0.69942(7) 0.0263(5) Uani 1 1 d . . . . .
H22 H -0.021096 0.525078 0.688682 0.032 Uiso 1 1 calc R . . . .
C23 C 0.1546(3) 0.6376(2) 0.70070(7) 0.0212(5) Uani 1 1 d . . . . .
C24 C 0.2919(3) 0.5704(2) 0.68509(9) 0.0310(6) Uani 1 1 d . . . . .
H24 H 0.305400 0.490132 0.699041 0.037 Uiso 1 1 calc R . . . .
C25 C 0.2956(4) 0.5594(3) 0.63641(11) 0.0549(10) Uani 1 1 d . . . . .
H25A H 0.352357 0.487224 0.627530 0.066 Uiso 1 1 calc R . . . .
H25B H 0.194903 0.554381 0.624813 0.066 Uiso 1 1 calc R . . . .
C26 C 0.3719(3) 0.6766(4) 0.62327(9) 0.0475(8) Uani 1 1 d . . . . .
H26A H 0.414174 0.669015 0.595128 0.057 Uiso 1 1 calc R . . . .
H26B H 0.302717 0.745973 0.623779 0.057 Uiso 1 1 calc R . . . .
C27 C 0.4241(3) 0.6598(2) 0.69383(8) 0.0244(5) Uani 1 1 d . . . . .
H27 H 0.498764 0.621073 0.712344 0.029 Uiso 1 1 calc R . . . .
C28 C 0.4245(3) 0.9958(2) 0.68417(7) 0.0207(4) Uani 1 1 d . . . . .
C29 C 0.5178(3) 0.9831(2) 0.64912(8) 0.0254(5) Uani 1 1 d . . . . .
H29 H 0.590298 0.921157 0.648252 0.030 Uiso 1 1 calc R . . . .
C30 C 0.5006(3) 1.0643(2) 0.61553(7) 0.0272(5) Uani 1 1 d . . . . .
H30 H 0.563643 1.057055 0.592213 0.033 Uiso 1 1 calc R . . . .
C31 C 0.3918(3) 1.1563(2) 0.61587(7) 0.0269(5) Uani 1 1 d . . . . .
C32 C 0.3006(3) 1.1671(2) 0.65146(8) 0.0305(5) Uani 1 1 d . . . . .
H32 H 0.227055 1.228237 0.652194 0.037 Uiso 1 1 calc R . . . .
C33 C 0.3172(3) 1.0886(2) 0.68577(8) 0.0273(5) Uani 1 1 d . . . . .
H33 H 0.257166 1.098162 0.709594 0.033 Uiso 1 1 calc R . . . .
C34 C 0.3707(4) 1.2417(2) 0.57878(8) 0.0345(6) Uani 1 1 d . . . . .
H34A H 0.401023 1.323951 0.586495 0.052 Uiso 1 1 calc GR . . . .
H34B H 0.266773 1.242260 0.570657 0.052 Uiso 1 1 calc GR . . . .
H34C H 0.430677 1.213308 0.555498 0.052 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0219(3) 0.0235(3) 0.0229(3) -0.0008(2) 0.0025(2) 0.0020(2)
O1 0.0299(10) 0.0241(8) 0.0304(8) 0.0001(7) 0.0057(7) 0.0058(7)
O2 0.0298(10) 0.0316(9) 0.0246(8) -0.0046(7) -0.0026(7) -0.0002(8)
O3 0.0245(9) 0.0292(9) 0.0320(8) 0.0014(7) 0.0054(7) 0.0058(7)
N1 0.0262(11) 0.0245(9) 0.0214(9) -0.0028(7) 0.0060(8) 0.0004(8)
C1 0.0270(13) 0.0191(10) 0.0195(10) 0.0022(8) 0.0003(9) 0.0045(9)
C2 0.0305(14) 0.0236(11) 0.0221(11) 0.0024(9) 0.0047(10) 0.0043(10)
C3 0.0385(15) 0.0229(11) 0.0215(11) -0.0009(9) -0.0022(10) 0.0063(10)
C4 0.0336(14) 0.0212(11) 0.0305(12) -0.0011(9) -0.0076(10) 0.0031(10)
C5 0.0266(13) 0.0237(11) 0.0318(12) 0.0048(9) -0.0004(10) 0.0012(10)
C6 0.0242(12) 0.0217(11) 0.0219(10) 0.0049(9) 0.0009(9) 0.0045(9)
C7 0.0272(13) 0.0247(11) 0.0209(10) 0.0067(9) 0.0039(9) 0.0018(10)
C8 0.0278(13) 0.0267(11) 0.0185(10) 0.0006(9) 0.0040(9) 0.0063(10)
C9 0.0322(14) 0.0323(13) 0.0242(11) 0.0015(10) 0.0020(10) 0.0115(12)
C10 0.0258(13) 0.0354(13) 0.0278(12) -0.0001(10) 0.0054(10) 0.0039(11)
C11 0.0252(12) 0.0217(11) 0.0222(11) -0.0007(9) 0.0020(9) -0.0003(9)
C12 0.0253(12) 0.0249(11) 0.0267(11) -0.0044(9) 0.0052(10) 0.0016(10)
C13 0.0301(14) 0.0293(12) 0.0213(11) -0.0034(10) 0.0026(9) -0.0009(10)
C14 0.0249(12) 0.0226(11) 0.0253(11) -0.0019(9) -0.0011(9) -0.0041(9)
C15 0.0262(13) 0.0235(11) 0.0279(11) -0.0011(9) 0.0015(10) 0.0033(10)
C16 0.0295(13) 0.0228(11) 0.0231(11) -0.0020(9) 0.0055(9) 0.0021(10)
C17 0.0341(14) 0.0302(12) 0.0257(11) 0.0018(10) -0.0031(10) -0.0003(11)
S2 0.0137(3) 0.0250(3) 0.0222(2) -0.0003(2) -0.00305(19) -0.0018(2)
O4 0.0276(10) 0.0379(10) 0.0325(9) -0.0021(8) 0.0057(7) 0.0097(8)
O5 0.0135(8) 0.0397(9) 0.0374(9) 0.0047(8) -0.0078(7) -0.0017(7)
O6 0.0249(9) 0.0281(8) 0.0204(8) -0.0031(6) -0.0004(6) -0.0051(7)
N2 0.0132(9) 0.0209(9) 0.0265(9) -0.0015(7) -0.0012(7) 0.0022(7)
C18 0.0144(11) 0.0225(10) 0.0182(10) 0.0021(8) -0.0019(8) -0.0002(9)
C19 0.0182(11) 0.0258(11) 0.0215(10) -0.0013(9) 0.0009(9) 0.0007(9)
C20 0.0178(12) 0.0357(12) 0.0226(10) 0.0029(10) 0.0020(9) 0.0026(10)
C21 0.0154(11) 0.0377(13) 0.0241(11) 0.0085(9) -0.0010(9) -0.0066(10)
C22 0.0261(13) 0.0270(11) 0.0259(11) 0.0047(10) -0.0041(9) -0.0070(10)
C23 0.0214(11) 0.0187(10) 0.0234(11) 0.0016(8) -0.0016(9) -0.0009(9)
C24 0.0257(13) 0.0208(11) 0.0464(15) -0.0082(10) -0.0036(12) 0.0050(10)
C25 0.0323(17) 0.074(2) 0.058(2) -0.0452(18) 0.0005(15) 0.0090(16)
C26 0.0349(17) 0.079(2) 0.0280(13) -0.0159(14) 0.0018(12) 0.0191(16)
C27 0.0190(12) 0.0229(11) 0.0314(12) 0.0019(9) 0.0004(9) 0.0078(9)
C28 0.0151(11) 0.0231(11) 0.0239(10) -0.0015(8) -0.0021(8) -0.0025(8)
C29 0.0182(12) 0.0276(12) 0.0303(12) -0.0028(9) 0.0019(9) -0.0003(9)
C30 0.0273(13) 0.0307(12) 0.0238(11) -0.0025(10) 0.0052(9) -0.0057(10)
C31 0.0329(14) 0.0227(11) 0.0250(11) -0.0015(9) -0.0040(10) -0.0100(10)
C32 0.0305(14) 0.0275(12) 0.0335(12) 0.0004(10) 0.0008(11) 0.0064(11)
C33 0.0262(13) 0.0287(12) 0.0271(11) -0.0006(9) 0.0055(10) 0.0017(10)
C34 0.0519(18) 0.0231(11) 0.0285(13) 0.0013(10) -0.0052(12) -0.0097(11)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.4303(17) . ?
S1 O3 1.4333(17) . ?
S1 N1 1.640(2) . ?
S1 C11 1.765(2) . ?
O1 C8 1.408(3) . ?
O1 C9 1.439(3) . ?
N1 C1 1.422(3) . ?
N1 C8 1.483(3) . ?
C1 C2 1.392(3) . ?
C1 C6 1.392(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.389(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.396(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(3) . ?
C6 C7 1.511(3) . ?
C7 H7 0.9800 . ?
C7 C8 1.546(3) . ?
C7 C10 1.534(3) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.512(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.395(3) . ?
C11 C16 1.390(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.384(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.392(3) . ?
C14 C15 1.398(3) . ?
C14 C17 1.504(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.386(3) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
S2 O5 1.4274(17) . ?
S2 O6 1.4337(16) . ?
S2 N2 1.6307(19) . ?
S2 C28 1.763(2) . ?
O4 C26 1.437(3) . ?
O4 C27 1.411(3) . ?
N2 C18 1.422(3) . ?
N2 C27 1.489(3) . ?
C18 C19 1.383(3) . ?
C18 C23 1.391(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.390(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.390(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.382(3) . ?
C23 C24 1.505(3) . ?
C24 H24 0.9800 . ?
C24 C25 1.545(4) . ?
C24 C27 1.547(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.495(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27 0.9800 . ?
C28 C29 1.392(3) . ?
C28 C33 1.386(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.386(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.387(4) . ?
C31 C32 1.393(4) . ?
C31 C34 1.504(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.385(4) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
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 O3 120.13(11) . . ?
O2 S1 N1 105.17(10) . . ?
O2 S1 C11 109.14(11) . . ?
O3 S1 N1 106.97(10) . . ?
O3 S1 C11 107.56(11) . . ?
N1 S1 C11 107.20(11) . . ?
C8 O1 C9 108.64(18) . . ?
C1 N1 S1 125.42(16) . . ?
C1 N1 C8 110.45(19) . . ?
C8 N1 S1 122.07(16) . . ?
C2 C1 N1 129.3(2) . . ?
C6 C1 N1 109.0(2) . . ?
C6 C1 C2 121.7(2) . . ?
C1 C2 H2 121.3 . . ?
C3 C2 C1 117.4(2) . . ?
C3 C2 H2 121.3 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.5(2) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C7 110.9(2) . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C7 128.9(2) . . ?
C6 C7 H7 111.8 . . ?
C6 C7 C8 103.72(18) . . ?
C6 C7 C10 113.9(2) . . ?
C8 C7 H7 111.8 . . ?
C10 C7 H7 111.8 . . ?
C10 C7 C8 103.09(19) . . ?
O1 C8 N1 113.66(18) . . ?
O1 C8 C7 107.5(2) . . ?
O1 C8 H8 110.4 . . ?
N1 C8 C7 104.41(18) . . ?
N1 C8 H8 110.4 . . ?
C7 C8 H8 110.4 . . ?
O1 C9 H9A 110.9 . . ?
O1 C9 H9B 110.9 . . ?
O1 C9 C10 104.35(19) . . ?
H9A C9 H9B 108.9 . . ?
C10 C9 H9A 110.9 . . ?
C10 C9 H9B 110.9 . . ?
C7 C10 H10A 111.4 . . ?
C7 C10 H10B 111.4 . . ?
C9 C10 C7 101.8(2) . . ?
C9 C10 H10A 111.4 . . ?
C9 C10 H10B 111.4 . . ?
H10A C10 H10B 109.3 . . ?
C12 C11 S1 119.69(18) . . ?
C16 C11 S1 119.49(17) . . ?
C16 C11 C12 120.8(2) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.0(2) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 119.1 . . ?
C12 C13 C14 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C15 117.8(2) . . ?
C13 C14 C17 120.7(2) . . ?
C15 C14 C17 121.6(2) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(2) . . ?
C16 C15 H15 119.1 . . ?
C11 C16 H16 120.6 . . ?
C15 C16 C11 118.9(2) . . ?
C15 C16 H16 120.6 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 S2 O6 119.90(11) . . ?
O5 S2 N2 105.83(10) . . ?
O5 S2 C28 108.78(11) . . ?
O6 S2 N2 107.25(10) . . ?
O6 S2 C28 107.20(10) . . ?
N2 S2 C28 107.28(10) . . ?
C27 O4 C26 106.8(2) . . ?
C18 N2 S2 125.75(16) . . ?
C18 N2 C27 111.46(18) . . ?
C27 N2 S2 121.84(16) . . ?
C19 C18 N2 129.0(2) . . ?
C19 C18 C23 122.1(2) . . ?
C23 C18 N2 108.85(19) . . ?
C18 C19 H19 121.3 . . ?
C18 C19 C20 117.3(2) . . ?
C20 C19 H19 121.3 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.6(2) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.8(2) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(2) . . ?
C23 C22 H22 120.2 . . ?
C18 C23 C24 110.8(2) . . ?
C22 C23 C18 119.5(2) . . ?
C22 C23 C24 129.6(2) . . ?
C23 C24 H24 112.2 . . ?
C23 C24 C25 112.4(2) . . ?
C23 C24 C27 104.98(18) . . ?
C25 C24 H24 112.2 . . ?
C25 C24 C27 102.1(2) . . ?
C27 C24 H24 112.2 . . ?
C24 C25 H25A 111.2 . . ?
C24 C25 H25B 111.2 . . ?
H25A C25 H25B 109.1 . . ?
C26 C25 C24 102.8(2) . . ?
C26 C25 H25A 111.2 . . ?
C26 C25 H25B 111.2 . . ?
O4 C26 C25 103.3(3) . . ?
O4 C26 H26A 111.1 . . ?
O4 C26 H26B 111.1 . . ?
C25 C26 H26A 111.1 . . ?
C25 C26 H26B 111.1 . . ?
H26A C26 H26B 109.1 . . ?
O4 C27 N2 112.85(18) . . ?
O4 C27 C24 107.4(2) . . ?
O4 C27 H27 110.9 . . ?
N2 C27 C24 103.64(18) . . ?
N2 C27 H27 110.9 . . ?
C24 C27 H27 110.9 . . ?
C29 C28 S2 119.25(18) . . ?
C33 C28 S2 120.00(18) . . ?
C33 C28 C29 120.7(2) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 C28 118.9(2) . . ?
C30 C29 H29 120.6 . . ?
C29 C30 H30 119.2 . . ?
C29 C30 C31 121.6(2) . . ?
C31 C30 H30 119.2 . . ?
C30 C31 C32 118.2(2) . . ?
C30 C31 C34 121.3(2) . . ?
C32 C31 C34 120.4(2) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.3(2) . . ?
C33 C32 H32 119.3 . . ?
C28 C33 H33 120.4 . . ?
C32 C33 C28 119.2(2) . . ?
C32 C33 H33 120.4 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
_shelx_res_file
;
TITL exp_815_a.res in P2(1)2(1)2(1)
exp_815.res
created by SHELXL-2016/6 at 15:15:55 on 13-May-2019
REM Old TITL exp_815 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.074, Rweak 0.033, Alpha 0.003, Orientation as input
REM Flack x = 0.027 ( 0.005 ) from Parsons' quotients
REM Formula found by SHELXT: C34 N3 O5 S2
CELL 1.54184 8.9043 10.7948 31.6319 90 90 90
ZERR 4 0.0001 0.0001 0.0002 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O S
UNIT 136 136 8 24 8
L.S. 64
PLAN 6
BOND $H
list 4
fmap 2 53
ACTA
OMIT 0 6 0
OMIT 2 0 9
OMIT -3 2 9
OMIT 0 1 13
OMIT 3 2 9
REM
REM
REM
WGHT 0.038000 0.928300
FVAR 0.49949
S1 5 -0.295122 0.470377 0.536346 11.00000 0.02189 0.02348 =
0.02290 -0.00079 0.00254 0.00199
O1 4 0.036496 0.432883 0.498067 11.00000 0.02986 0.02412 =
0.03043 0.00014 0.00575 0.00576
O2 4 -0.314851 0.400198 0.498398 11.00000 0.02981 0.03159 =
0.02459 -0.00456 -0.00264 -0.00022
O3 4 -0.416731 0.542572 0.552905 11.00000 0.02451 0.02920 =
0.03201 0.00142 0.00540 0.00581
N1 3 -0.157461 0.566787 0.526083 11.00000 0.02617 0.02451 =
0.02138 -0.00283 0.00602 0.00041
C1 1 -0.104623 0.661102 0.553738 11.00000 0.02705 0.01906 =
0.01946 0.00222 0.00032 0.00454
C2 1 -0.165704 0.703005 0.591628 11.00000 0.03054 0.02356 =
0.02211 0.00237 0.00467 0.00431
AFIX 43
H2 2 -0.252092 0.667571 0.602889 11.00000 -1.20000
AFIX 0
C3 1 -0.092639 0.799793 0.611969 11.00000 0.03854 0.02294 =
0.02145 -0.00090 -0.00223 0.00631
AFIX 43
H3 2 -0.130350 0.828989 0.637512 11.00000 -1.20000
AFIX 0
C4 1 0.035518 0.854040 0.595045 11.00000 0.03362 0.02119 =
0.03049 -0.00109 -0.00756 0.00312
AFIX 43
H4 2 0.082175 0.918947 0.609232 11.00000 -1.20000
AFIX 0
C5 1 0.094431 0.811421 0.556825 11.00000 0.02661 0.02374 =
0.03180 0.00484 -0.00042 0.00117
AFIX 43
H5 2 0.179893 0.847655 0.545303 11.00000 -1.20000
AFIX 0
C6 1 0.023607 0.714426 0.536378 11.00000 0.02425 0.02174 =
0.02195 0.00494 0.00089 0.00447
C7 1 0.065138 0.652149 0.495230 11.00000 0.02724 0.02467 =
0.02087 0.00668 0.00386 0.00180
AFIX 13
H7 2 0.055621 0.708666 0.471133 11.00000 -1.20000
AFIX 0
C8 1 -0.046182 0.542668 0.492171 11.00000 0.02783 0.02673 =
0.01854 0.00062 0.00403 0.00625
AFIX 13
H8 2 -0.095522 0.542135 0.464478 11.00000 -1.20000
AFIX 0
C9 1 0.180403 0.464196 0.515760 11.00000 0.03223 0.03228 =
0.02416 0.00151 0.00196 0.01153
AFIX 23
H9A 2 0.255019 0.402244 0.508534 11.00000 -1.20000
H9B 2 0.174450 0.471000 0.546291 11.00000 -1.20000
AFIX 0
C10 1 0.218742 0.587779 0.496033 11.00000 0.02582 0.03543 =
0.02781 -0.00010 0.00537 0.00393
AFIX 23
H10A 2 0.258979 0.577675 0.467746 11.00000 -1.20000
H10B 2 0.290257 0.633324 0.513165 11.00000 -1.20000
AFIX 0
C11 1 -0.232877 0.370873 0.577013 11.00000 0.02519 0.02166 =
0.02216 -0.00073 0.00198 -0.00025
C12 1 -0.282378 0.389735 0.618369 11.00000 0.02533 0.02486 =
0.02668 -0.00442 0.00520 0.00158
AFIX 43
H12 2 -0.344664 0.456229 0.624855 11.00000 -1.20000
AFIX 0
C13 1 -0.237326 0.307924 0.649595 11.00000 0.03008 0.02934 =
0.02129 -0.00341 0.00256 -0.00090
AFIX 43
H13 2 -0.269202 0.320902 0.677240 11.00000 -1.20000
AFIX 0
C14 1 -0.145585 0.206732 0.640739 11.00000 0.02486 0.02259 =
0.02530 -0.00194 -0.00112 -0.00411
C15 1 -0.096076 0.191673 0.599118 11.00000 0.02616 0.02352 =
0.02793 -0.00109 0.00148 0.00329
AFIX 43
H15 2 -0.032824 0.125771 0.592670 11.00000 -1.20000
AFIX 0
C16 1 -0.138717 0.272325 0.567190 11.00000 0.02948 0.02281 =
0.02312 -0.00200 0.00548 0.00207
AFIX 43
H16 2 -0.104875 0.260672 0.539662 11.00000 -1.20000
AFIX 0
C17 1 -0.104113 0.116081 0.674905 11.00000 0.03411 0.03020 =
0.02571 0.00178 -0.00306 -0.00028
AFIX 137
H17A 2 -0.064903 0.160178 0.698838 11.00000 -1.50000
H17B 2 -0.029306 0.059886 0.664424 11.00000 -1.50000
H17C 2 -0.191657 0.070315 0.683262 11.00000 -1.50000
AFIX 0
S2 5 0.444657 0.892479 0.726962 11.00000 0.01374 0.02502 =
0.02219 -0.00026 -0.00305 -0.00179
O4 4 0.487984 0.691319 0.654446 11.00000 0.02760 0.03794 =
0.03252 -0.00212 0.00572 0.00973
O5 4 0.598331 0.855794 0.729835 11.00000 0.01351 0.03971 =
0.03736 0.00475 -0.00776 -0.00168
O6 4 0.371948 0.947893 0.762710 11.00000 0.02486 0.02807 =
0.02038 -0.00308 -0.00044 -0.00511
N2 3 0.351356 0.767163 0.715170 11.00000 0.01321 0.02092 =
0.02650 -0.00148 -0.00116 0.00218
C18 1 0.192517 0.753930 0.716315 11.00000 0.01439 0.02248 =
0.01816 0.00212 -0.00194 -0.00022
C19 1 0.085465 0.836194 0.731025 11.00000 0.01823 0.02581 =
0.02150 -0.00132 0.00088 0.00067
AFIX 43
H19 2 0.112187 0.913755 0.741379 11.00000 -1.20000
AFIX 0
C20 1 -0.063694 0.798258 0.729708 11.00000 0.01776 0.03569 =
0.02264 0.00289 0.00202 0.00260
AFIX 43
H20 2 -0.138096 0.851636 0.739400 11.00000 -1.20000
AFIX 0
C21 1 -0.104246 0.682466 0.714251 11.00000 0.01539 0.03773 =
0.02407 0.00854 -0.00097 -0.00657
AFIX 43
H21 2 -0.204672 0.658831 0.713849 11.00000 -1.20000
AFIX 0
C22 1 0.005515 0.602217 0.699420 11.00000 0.02608 0.02704 =
0.02593 0.00472 -0.00413 -0.00698
AFIX 43
H22 2 -0.021096 0.525078 0.688682 11.00000 -1.20000
AFIX 0
C23 1 0.154599 0.637604 0.700702 11.00000 0.02141 0.01872 =
0.02340 0.00156 -0.00157 -0.00088
C24 1 0.291904 0.570418 0.685087 11.00000 0.02572 0.02084 =
0.04637 -0.00816 -0.00359 0.00499
AFIX 13
H24 2 0.305400 0.490132 0.699041 11.00000 -1.20000
AFIX 0
C25 1 0.295566 0.559353 0.636412 11.00000 0.03228 0.07398 =
0.05831 -0.04520 0.00047 0.00897
AFIX 23
H25A 2 0.352357 0.487224 0.627530 11.00000 -1.20000
H25B 2 0.194903 0.554381 0.624813 11.00000 -1.20000
AFIX 0
C26 1 0.371917 0.676589 0.623274 11.00000 0.03490 0.07949 =
0.02797 -0.01593 0.00181 0.01906
AFIX 23
H26A 2 0.414174 0.669015 0.595128 11.00000 -1.20000
H26B 2 0.302717 0.745973 0.623779 11.00000 -1.20000
AFIX 0
C27 1 0.424069 0.659846 0.693834 11.00000 0.01902 0.02287 =
0.03141 0.00192 0.00036 0.00776
AFIX 13
H27 2 0.498764 0.621073 0.712344 11.00000 -1.20000
AFIX 0
C28 1 0.424491 0.995757 0.684172 11.00000 0.01511 0.02307 =
0.02394 -0.00153 -0.00209 -0.00252
C29 1 0.517752 0.983084 0.649121 11.00000 0.01822 0.02762 =
0.03034 -0.00281 0.00190 -0.00033
AFIX 43
H29 2 0.590298 0.921157 0.648252 11.00000 -1.20000
AFIX 0
C30 1 0.500645 1.064347 0.615530 11.00000 0.02728 0.03070 =
0.02376 -0.00247 0.00523 -0.00575
AFIX 43
H30 2 0.563643 1.057055 0.592213 11.00000 -1.20000
AFIX 0
C31 1 0.391783 1.156300 0.615868 11.00000 0.03291 0.02270 =
0.02496 -0.00147 -0.00401 -0.00996
C32 1 0.300595 1.167099 0.651460 11.00000 0.03053 0.02753 =
0.03351 0.00036 0.00084 0.00638
AFIX 43
H32 2 0.227055 1.228237 0.652194 11.00000 -1.20000
AFIX 0
C33 1 0.317247 1.088637 0.685766 11.00000 0.02617 0.02873 =
0.02713 -0.00063 0.00549 0.00173
AFIX 43
H33 2 0.257166 1.098162 0.709594 11.00000 -1.20000
AFIX 0
C34 1 0.370654 1.241672 0.578776 11.00000 0.05186 0.02312 =
0.02855 0.00128 -0.00520 -0.00970
AFIX 137
H34A 2 0.401023 1.323951 0.586495 11.00000 -1.50000
H34B 2 0.266773 1.242260 0.570657 11.00000 -1.50000
H34C 2 0.430677 1.213308 0.555498 11.00000 -1.50000
AFIX 0
HKLF 4
REM exp_815_a.res in P2(1)2(1)2(1)
REM R1 = 0.0300 for 6061 Fo > 4sig(Fo) and 0.0306 for all 6165 data
REM 399 parameters refined using 0 restraints
END
WGHT 0.0378 0.9298
REM Highest difference peak 0.180, deepest hole -0.356, 1-sigma level 0.045
Q1 1 0.4448 0.8967 0.7846 11.00000 0.05 0.18
Q2 1 0.2827 0.3588 0.4800 11.00000 0.05 0.14
Q3 1 0.5851 0.8792 0.6391 11.00000 0.05 0.14
Q4 1 -0.3402 0.2819 0.6808 11.00000 0.05 0.13
Q5 1 -0.3182 0.6925 0.5995 11.00000 0.05 0.13
Q6 1 -0.0979 0.5214 0.5962 11.00000 0.05 0.13
;
_shelx_res_checksum 92400
_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 6.536
_oxdiff_exptl_absorpt_empirical_full_min 0.306