# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021
#######################################################################
#
# 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_aks82
_database_code_depnum_ccdc_archive 'CCDC 2088890'
loop_
_audit_author_name
_audit_author_address
'Kallol Mukherjee'
;University of Hyderabad
India
;
_audit_update_record
;
2021-06-09 deposited with the CCDC. 2021-10-20 downloaded from the CCDC.
;
_audit_creation_date 2021-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H28 N2 O4 S'
_chemical_formula_sum 'C28 H28 N2 O4 S'
_chemical_formula_weight 488.58
_chemical_absolute_configuration ?
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H N O S'
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'
_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 hexagonal
_space_group_IT_number 169
_space_group_name_H-M_alt 'P 61'
_space_group_name_Hall 'P 61'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
_cell_length_a 22.7073(5)
_cell_length_b 22.7073(5)
_cell_length_c 9.0908(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 4059.4(2)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 15371
_cell_measurement_temperature 292(110)
_cell_measurement_theta_max 21.7740
_cell_measurement_theta_min 2.0640
_shelx_estimated_absorpt_T_max 0.985
_shelx_estimated_absorpt_T_min 0.970
_exptl_absorpt_coefficient_mu 0.154
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67337
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear whiteish white'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whiteish
_exptl_crystal_colour_primary white
_exptl_crystal_density_diffrn 1.199
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1548
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0460
_diffrn_reflns_av_unetI/netI 0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 39105
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.993
_diffrn_reflns_theta_min 2.071
_diffrn_ambient_environment air
_diffrn_ambient_temperature 292(110)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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 -34.00 22.00 0.50 12.00 -- -14.97 -94.00 30.00 112
2 \w 19.00 69.00 0.50 12.00 -- 16.22-125.00 0.00 100
3 \w 16.00 74.00 0.50 12.00 -- 16.22-136.00 -38.00 116
4 \w -23.00 42.00 0.50 12.00 -- -14.97 45.00 90.00 130
5 \w 42.00 68.00 0.50 12.00 -- 16.22 45.00 90.00 52
6 \w -10.00 90.00 0.50 12.00 -- 16.22 30.00 90.00 200
7 \w -4.00 21.00 0.50 12.00 -- 16.22 45.00 90.00 50
8 \w -55.00 -30.00 0.50 12.00 -- -14.97 136.00 26.00 50
9 \w 45.00 70.00 0.50 12.00 -- 16.22-133.00 139.00 50
10 \w -33.00 22.00 0.50 12.00 -- -14.97 -94.00 150.00 110
11 \w -53.00 34.00 0.50 12.00 -- 16.22 -45.00 -90.00 174
12 \w 41.00 81.00 0.50 12.00 -- 16.22 45.00-120.00 80
13 \w 4.00 29.00 0.50 12.00 -- 16.22 45.00-120.00 50
14 \w -57.00 -1.00 0.50 12.00 -- 16.22 -30.00-180.00 112
15 \w -67.00 -42.00 0.50 12.00 -- -14.97 133.00-152.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0358485000
_diffrn_orient_matrix_UB_12 0.0213650000
_diffrn_orient_matrix_UB_13 -0.0007447000
_diffrn_orient_matrix_UB_21 -0.0038668000
_diffrn_orient_matrix_UB_22 0.0286932000
_diffrn_orient_matrix_UB_23 0.0130022000
_diffrn_orient_matrix_UB_31 0.0010128000
_diffrn_orient_matrix_UB_32 -0.0046122000
_diffrn_orient_matrix_UB_33 0.0769152000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage 0.856
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.950
_reflns_number_gt 3797
_reflns_number_total 5690
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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 0.397
_refine_diff_density_min -0.165
_refine_diff_density_rms 0.035
_refine_ls_abs_structure_details
;
Flack x determined using 1331 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.02(4)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 321
_refine_ls_number_reflns 5690
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0831
_refine_ls_R_factor_gt 0.0519
_refine_ls_restrained_S_all 1.015
_refine_ls_shift/su_max 0.026
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1281
_refine_ls_wR_factor_ref 0.1450
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C5(H5), C4(H4), C16(H16), C22(H22), C20(H20), C21(H21), C8(H8),
C11(H11), C9(H9), C14(H14), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,
H26C), C23(H23A,H23B,H23C)
;
_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 0.93426(5) 0.60616(5) 0.35441(13) 0.0570(3) Uani 1 1 d . . . . .
O1 O 0.89513(13) 0.63940(15) 0.3412(4) 0.0719(8) Uani 1 1 d . . . . .
O2 O 0.81178(15) 0.48031(15) 0.3239(4) 0.0798(10) Uani 1 1 d . . . . .
O3 O 0.85784(14) 0.45084(16) 0.1408(4) 0.0849(11) Uani 1 1 d . . . . .
N1 N 0.92214(17) 0.54939(19) 0.2452(4) 0.0651(10) Uani 1 1 d . . . . .
N2 N 0.97900(19) 0.56182(19) 0.5606(5) 0.0718(10) Uani 1 1 d . . . . .
O4 O 1.16477(18) 0.6888(2) 0.1007(5) 0.1009(12) Uani 1 1 d . . . . .
C24 C 0.8586(2) 0.4925(2) 0.2442(5) 0.0606(11) Uani 1 1 d . . . . .
C6 C 1.0513(2) 0.7267(2) 0.4079(5) 0.0642(11) Uani 1 1 d . . . . .
C3 C 1.1245(2) 0.6993(3) 0.1974(5) 0.0687(11) Uani 1 1 d . . . . .
C17 C 0.9306(2) 0.5779(2) 0.5409(5) 0.0593(10) Uani 1 1 d . . . . .
C2 C 1.0572(2) 0.6520(2) 0.2240(5) 0.0625(11) Uani 1 1 d . . . . .
H2 H 1.036148 0.611227 0.172326 0.075 Uiso 1 1 calc R . . . .
C1 C 1.02141(19) 0.6659(2) 0.3281(4) 0.0558(10) Uani 1 1 d . . . . .
C25 C 0.7955(2) 0.3892(2) 0.0942(6) 0.0769(14) Uani 1 1 d . . . . .
C5 C 1.1192(2) 0.7726(2) 0.3738(6) 0.0796(14) Uani 1 1 d . . . . .
H5 H 1.140854 0.814028 0.423157 0.096 Uiso 1 1 calc R . . . .
C7 C 1.0148(3) 0.7451(2) 0.5208(7) 0.0797(14) Uani 1 1 d . . . . .
C15 C 0.9853(3) 0.7492(3) 0.7752(7) 0.0878(16) Uani 1 1 d . . . . .
C4 C 1.1548(2) 0.7600(2) 0.2738(6) 0.0802(15) Uani 1 1 d . . . . .
H4 H 1.199997 0.792154 0.255639 0.096 Uiso 1 1 calc R . . . .
C16 C 1.0203(3) 0.7324(2) 0.6597(7) 0.0872(16) Uani 1 1 d . . . . .
H16 H 1.046342 0.712729 0.685301 0.105 Uiso 1 1 calc R . . . .
C10 C 0.9497(3) 0.7789(3) 0.7356(8) 0.0937(17) Uani 1 1 d . . . . .
C22 C 0.9852(3) 0.5437(3) 0.6967(7) 0.0922(16) Uani 1 1 d . . . . .
H22 H 1.018880 0.532642 0.714105 0.111 Uiso 1 1 calc R . . . .
C18 C 0.8856(2) 0.5751(2) 0.6480(6) 0.0757(14) Uani 1 1 d . . . . .
C20 C 0.8970(4) 0.5554(3) 0.7874(7) 0.1000(19) Uani 1 1 d . . . . .
H20 H 0.869485 0.552748 0.865883 0.120 Uiso 1 1 calc R . . . .
C21 C 0.9461(4) 0.5406(3) 0.8099(7) 0.107(2) Uani 1 1 d . . . . .
H21 H 0.953005 0.528156 0.903020 0.128 Uiso 1 1 calc R . . . .
C19 C 0.8299(3) 0.5914(3) 0.6230(7) 0.1005(18) Uani 1 1 d . . . . .
H19A H 0.849454 0.638484 0.597283 0.151 Uiso 1 1 calc GR . . . .
H19B H 0.803512 0.582338 0.711276 0.151 Uiso 1 1 calc GR . . . .
H19C H 0.801059 0.563656 0.544517 0.151 Uiso 1 1 calc GR . . . .
C8 C 0.9781(3) 0.7778(3) 0.4829(7) 0.0943(17) Uani 1 1 d . . . . .
H8 H 0.975134 0.787350 0.384619 0.113 Uiso 1 1 calc R . . . .
C27 C 0.7478(3) 0.4098(3) 0.0284(8) 0.0997(17) Uani 1 1 d . . . . .
H27A H 0.738179 0.435069 0.099700 0.150 Uiso 1 1 calc GR . . . .
H27B H 0.706301 0.369969 0.000182 0.150 Uiso 1 1 calc GR . . . .
H27C H 0.768596 0.437714 -0.056580 0.150 Uiso 1 1 calc GR . . . .
C11 C 0.9133(4) 0.7933(4) 0.8497(12) 0.128(3) Uani 1 1 d . . . . .
H11 H 0.887857 0.813653 0.824907 0.154 Uiso 1 1 calc R . . . .
C9 C 0.9470(4) 0.7958(3) 0.5869(9) 0.111(2) Uani 1 1 d . . . . .
H9 H 0.924325 0.818768 0.560712 0.134 Uiso 1 1 calc R . . . .
C28 C 0.8232(3) 0.3607(4) -0.0199(9) 0.137(3) Uani 1 1 d . . . . .
H28A H 0.846044 0.393899 -0.095658 0.205 Uiso 1 1 calc GR . . . .
H28B H 0.786310 0.320315 -0.062233 0.205 Uiso 1 1 calc GR . . . .
H28C H 0.854609 0.349792 0.025937 0.205 Uiso 1 1 calc GR . . . .
C26 C 0.7623(3) 0.3397(3) 0.2195(8) 0.1017(19) Uani 1 1 d . . . . .
H26A H 0.794555 0.329130 0.262561 0.153 Uiso 1 1 calc GR . . . .
H26B H 0.724036 0.298739 0.183064 0.153 Uiso 1 1 calc GR . . . .
H26C H 0.747243 0.359717 0.292642 0.153 Uiso 1 1 calc GR . . . .
C14 C 0.9881(5) 0.7327(3) 0.9200(9) 0.123(2) Uani 1 1 d . . . . .
H14 H 1.013195 0.712065 0.945343 0.147 Uiso 1 1 calc R . . . .
C12 C 0.9164(5) 0.7773(4) 0.9875(13) 0.147(4) Uani 1 1 d . . . . .
H12 H 0.893289 0.786547 1.060196 0.176 Uiso 1 1 calc R . . . .
C13 C 0.9548(6) 0.7462(4) 1.0247(10) 0.146(3) Uani 1 1 d . . . . .
H13 H 0.957020 0.734967 1.122110 0.176 Uiso 1 1 calc R . . . .
C23 C 1.1404(4) 0.6202(4) 0.0515(9) 0.130(2) Uani 1 1 d . . . . .
H23A H 1.109685 0.610219 -0.029387 0.195 Uiso 1 1 calc GR . . . .
H23B H 1.117127 0.589182 0.130782 0.195 Uiso 1 1 calc GR . . . .
H23C H 1.178190 0.615348 0.020462 0.195 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 0.0415(5) 0.0512(6) 0.0738(6) -0.0097(5) -0.0067(5) 0.0198(5)
O1 0.0534(16) 0.0662(18) 0.100(2) -0.0105(17) -0.0129(16) 0.0331(15)
O2 0.0543(18) 0.071(2) 0.094(2) -0.0247(17) 0.0104(17) 0.0166(15)
O3 0.0465(17) 0.077(2) 0.113(3) -0.0473(19) 0.0030(16) 0.0175(15)
N1 0.0427(18) 0.065(2) 0.078(2) -0.0206(18) -0.0038(16) 0.0194(17)
N2 0.058(2) 0.064(2) 0.086(3) 0.006(2) -0.0031(19) 0.0249(18)
O4 0.075(2) 0.105(3) 0.104(3) 0.015(2) 0.034(2) 0.031(2)
C24 0.046(2) 0.059(3) 0.076(3) -0.017(2) -0.006(2) 0.026(2)
C6 0.052(2) 0.049(2) 0.082(3) -0.003(2) 0.002(2) 0.017(2)
C3 0.055(2) 0.076(3) 0.072(3) 0.014(2) 0.007(2) 0.030(2)
C17 0.044(2) 0.049(2) 0.072(3) -0.008(2) -0.002(2) 0.0137(18)
C2 0.053(2) 0.059(3) 0.066(3) -0.003(2) -0.003(2) 0.020(2)
C1 0.042(2) 0.053(2) 0.064(2) 0.0007(19) -0.0042(18) 0.0175(18)
C25 0.050(3) 0.067(3) 0.097(4) -0.029(3) -0.006(2) 0.018(2)
C5 0.064(3) 0.050(2) 0.103(4) -0.008(3) -0.006(3) 0.012(2)
C7 0.070(3) 0.051(3) 0.098(4) -0.005(3) -0.019(3) 0.014(2)
C15 0.093(4) 0.053(3) 0.101(4) -0.008(3) 0.015(3) 0.024(3)
C4 0.049(3) 0.065(3) 0.105(4) 0.018(3) 0.003(3) 0.013(2)
C16 0.090(4) 0.056(3) 0.103(4) -0.004(3) -0.017(3) 0.027(3)
C10 0.094(4) 0.069(3) 0.098(4) -0.013(3) 0.004(3) 0.025(3)
C22 0.082(4) 0.081(4) 0.098(4) 0.017(3) -0.009(3) 0.030(3)
C18 0.058(3) 0.060(3) 0.086(4) -0.011(2) 0.014(2) 0.012(2)
C20 0.093(4) 0.086(4) 0.080(4) -0.005(3) 0.027(3) 0.014(3)
C21 0.100(5) 0.102(5) 0.086(4) 0.016(3) -0.001(4) 0.026(4)
C19 0.069(3) 0.101(4) 0.119(5) -0.015(4) 0.018(3) 0.033(3)
C8 0.101(4) 0.098(4) 0.099(4) -0.011(3) -0.012(3) 0.061(4)
C27 0.083(4) 0.084(4) 0.114(4) -0.018(3) -0.023(3) 0.029(3)
C11 0.114(5) 0.112(6) 0.158(8) -0.003(5) 0.025(5) 0.056(4)
C9 0.111(5) 0.104(5) 0.138(6) -0.025(4) -0.017(4) 0.068(4)
C28 0.091(4) 0.123(5) 0.165(7) -0.088(5) 0.008(4) 0.030(4)
C26 0.097(4) 0.063(3) 0.124(5) -0.021(3) -0.020(4) 0.024(3)
C14 0.173(7) 0.087(4) 0.104(5) -0.009(4) 0.001(5) 0.063(5)
C12 0.161(8) 0.104(6) 0.149(8) -0.007(5) 0.073(6) 0.046(5)
C13 0.223(10) 0.115(6) 0.100(5) 0.010(5) 0.037(6) 0.084(7)
C23 0.110(5) 0.138(6) 0.130(6) -0.024(5) 0.035(4) 0.053(5)
_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 1.430(3) . ?
S1 N1 1.539(4) . ?
S1 C17 1.800(5) . ?
S1 C1 1.769(4) . ?
O2 C24 1.199(5) . ?
O3 C24 1.328(5) . ?
O3 C25 1.470(5) . ?
N1 C24 1.373(5) . ?
N2 C17 1.331(6) . ?
N2 C22 1.333(7) . ?
O4 C3 1.374(6) . ?
O4 C23 1.439(7) . ?
C6 C1 1.398(6) . ?
C6 C5 1.398(6) . ?
C6 C7 1.504(7) . ?
C3 C2 1.380(6) . ?
C3 C4 1.380(7) . ?
C17 C18 1.390(6) . ?
C2 H2 0.9300 . ?
C2 C1 1.383(6) . ?
C25 C27 1.503(7) . ?
C25 C28 1.514(7) . ?
C25 C26 1.511(8) . ?
C5 H5 0.9300 . ?
C5 C4 1.339(7) . ?
C7 C16 1.314(8) . ?
C7 C8 1.409(8) . ?
C15 C16 1.478(8) . ?
C15 C10 1.336(8) . ?
C15 C14 1.379(10) . ?
C4 H4 0.9300 . ?
C16 H16 0.9300 . ?
C10 C11 1.461(10) . ?
C10 C9 1.413(10) . ?
C22 H22 0.9300 . ?
C22 C21 1.338(9) . ?
C18 C20 1.411(9) . ?
C18 C19 1.502(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.331(9) . ?
C21 H21 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C8 H8 0.9300 . ?
C8 C9 1.359(9) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.315(13) . ?
C9 H9 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C13 1.343(12) . ?
C12 H12 0.9300 . ?
C12 C13 1.411(13) . ?
C13 H13 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 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 N1 119.3(2) . . ?
O1 S1 C17 109.7(2) . . ?
O1 S1 C1 109.61(19) . . ?
N1 S1 C17 110.6(2) . . ?
N1 S1 C1 102.60(19) . . ?
C1 S1 C17 103.62(18) . . ?
C24 O3 C25 123.1(3) . . ?
C24 N1 S1 117.1(3) . . ?
C17 N2 C22 116.0(5) . . ?
C3 O4 C23 117.3(4) . . ?
O2 C24 O3 124.6(4) . . ?
O2 C24 N1 127.4(4) . . ?
O3 C24 N1 107.9(4) . . ?
C1 C6 C7 124.4(4) . . ?
C5 C6 C1 115.6(4) . . ?
C5 C6 C7 120.0(4) . . ?
O4 C3 C2 123.5(5) . . ?
O4 C3 C4 116.9(4) . . ?
C2 C3 C4 119.6(5) . . ?
N2 C17 S1 109.1(3) . . ?
N2 C17 C18 125.6(5) . . ?
C18 C17 S1 125.2(4) . . ?
C3 C2 H2 120.3 . . ?
C3 C2 C1 119.4(4) . . ?
C1 C2 H2 120.3 . . ?
C6 C1 S1 119.5(3) . . ?
C2 C1 S1 118.5(3) . . ?
C2 C1 C6 122.0(4) . . ?
O3 C25 C27 108.5(4) . . ?
O3 C25 C28 101.4(4) . . ?
O3 C25 C26 112.1(4) . . ?
C27 C25 C28 112.2(6) . . ?
C27 C25 C26 111.3(4) . . ?
C26 C25 C28 111.0(5) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 C6 123.3(5) . . ?
C4 C5 H5 118.3 . . ?
C16 C7 C6 117.9(5) . . ?
C16 C7 C8 119.8(6) . . ?
C8 C7 C6 122.2(6) . . ?
C10 C15 C16 118.7(6) . . ?
C10 C15 C14 121.1(6) . . ?
C14 C15 C16 120.3(7) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C7 C16 C15 120.1(6) . . ?
C7 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C15 C10 C11 118.3(7) . . ?
C15 C10 C9 120.8(6) . . ?
C9 C10 C11 120.9(7) . . ?
N2 C22 H22 118.0 . . ?
N2 C22 C21 124.1(6) . . ?
C21 C22 H22 118.0 . . ?
C17 C18 C20 113.3(5) . . ?
C17 C18 C19 125.0(5) . . ?
C20 C18 C19 121.6(5) . . ?
C18 C20 H20 119.1 . . ?
C21 C20 C18 121.9(6) . . ?
C21 C20 H20 119.1 . . ?
C22 C21 H21 120.5 . . ?
C20 C21 C22 119.1(6) . . ?
C20 C21 H21 120.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.4(6) . . ?
C9 C8 H8 119.3 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(8) . . ?
C12 C11 H11 120.0 . . ?
C10 C9 H9 120.5 . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9 120.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C15 C14 H14 119.8 . . ?
C13 C14 C15 120.5(8) . . ?
C13 C14 H14 119.8 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(8) . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 120.3(8) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
O4 C23 H23A 109.5 . . ?
O4 C23 H23B 109.5 . . ?
O4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.568 277.3 71.8 ?
_shelx_res_file
;
TITL aks82_a.res in P6(1)
aks82.res
created by SHELXL-2018/3 at 18:03:08 on 07-May-2021
REM Old TITL AKS82 in P6(1)
REM SHELXT solution in P6(1)
REM R1 0.166, Rweak 0.044, Alpha 0.008, Orientation as input
REM Flack x = 0.099 ( 0.045 ) from Parsons' quotients
REM Formula found by SHELXT: C28 N2 O4 S
CELL 0.71073 22.7073 22.7073 9.0908 90 90 120
ZERR 6 0.0005 0.0005 0.0002 0 0 0
LATT -1
SYMM -Y,+X-Y,0.333+Z
SYMM +Y-X,-X,0.667+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.833+Z
SYMM -Y+X,+X,0.167+Z
SFAC C H N O S
UNIT 168 168 12 24 6
L.S. 10 0 0
PLAN 20
SIZE 0.2 0.15 0.1
BOND $H
list 4
ABIN
fmap 2 53
acta
OMIT -1 4 0
OMIT -2 3 0
REM
REM
REM
WGHT 0.078500
FVAR 0.34759
S1 5 0.934258 0.606157 0.354414 11.00000 0.04148 0.05117 =
0.07375 -0.00971 -0.00669 0.01977
O1 4 0.895127 0.639401 0.341210 11.00000 0.05338 0.06625 =
0.10029 -0.01055 -0.01288 0.03306
O2 4 0.811781 0.480314 0.323871 11.00000 0.05425 0.07128 =
0.09420 -0.02468 0.01041 0.01662
O3 4 0.857837 0.450837 0.140813 11.00000 0.04648 0.07744 =
0.11298 -0.04730 0.00299 0.01754
N1 3 0.922137 0.549392 0.245156 11.00000 0.04273 0.06477 =
0.07791 -0.02062 -0.00385 0.01940
N2 3 0.979002 0.561822 0.560631 11.00000 0.05800 0.06374 =
0.08609 0.00601 -0.00311 0.02487
O4 4 1.164770 0.688795 0.100685 11.00000 0.07488 0.10534 =
0.10376 0.01533 0.03387 0.03108
C24 1 0.858618 0.492530 0.244206 11.00000 0.04627 0.05858 =
0.07641 -0.01723 -0.00592 0.02579
C6 1 1.051322 0.726724 0.407867 11.00000 0.05153 0.04868 =
0.08220 -0.00266 0.00153 0.01731
C3 1 1.124460 0.699312 0.197436 11.00000 0.05453 0.07566 =
0.07198 0.01371 0.00735 0.02967
C17 1 0.930612 0.577858 0.540915 11.00000 0.04435 0.04882 =
0.07196 -0.00810 -0.00215 0.01366
C2 1 1.057208 0.652045 0.223967 11.00000 0.05259 0.05863 =
0.06555 -0.00342 -0.00288 0.01970
AFIX 43
H2 2 1.036148 0.611227 0.172326 11.00000 -1.20000
AFIX 0
C1 1 1.021409 0.665929 0.328064 11.00000 0.04181 0.05335 =
0.06374 0.00070 -0.00422 0.01749
C25 1 0.795535 0.389159 0.094207 11.00000 0.05044 0.06746 =
0.09723 -0.02943 -0.00632 0.01787
C5 1 1.119247 0.772615 0.373810 11.00000 0.06355 0.04985 =
0.10349 -0.00781 -0.00622 0.01190
AFIX 43
H5 2 1.140854 0.814028 0.423157 11.00000 -1.20000
AFIX 0
C7 1 1.014813 0.745068 0.520848 11.00000 0.06954 0.05061 =
0.09789 -0.00527 -0.01893 0.01433
C15 1 0.985330 0.749244 0.775157 11.00000 0.09306 0.05298 =
0.10060 -0.00774 0.01451 0.02388
C4 1 1.154782 0.759981 0.273756 11.00000 0.04906 0.06549 =
0.10544 0.01819 0.00321 0.01309
AFIX 43
H4 2 1.199997 0.792154 0.255639 11.00000 -1.20000
AFIX 0
C16 1 1.020346 0.732369 0.659672 11.00000 0.09050 0.05589 =
0.10290 -0.00370 -0.01731 0.02744
AFIX 43
H16 2 1.046342 0.712729 0.685301 11.00000 -1.20000
AFIX 0
C10 1 0.949668 0.778936 0.735554 11.00000 0.09363 0.06912 =
0.09790 -0.01326 0.00385 0.02530
C22 1 0.985228 0.543740 0.696742 11.00000 0.08243 0.08149 =
0.09788 0.01748 -0.00861 0.02993
AFIX 43
H22 2 1.018880 0.532642 0.714105 11.00000 -1.20000
AFIX 0
C18 1 0.885588 0.575109 0.647985 11.00000 0.05822 0.05990 =
0.08574 -0.01079 0.01431 0.01213
C20 1 0.897009 0.555422 0.787438 11.00000 0.09308 0.08578 =
0.08031 -0.00473 0.02657 0.01413
AFIX 43
H20 2 0.869485 0.552748 0.865883 11.00000 -1.20000
AFIX 0
C21 1 0.946054 0.540567 0.809937 11.00000 0.09989 0.10189 =
0.08595 0.01602 -0.00086 0.02648
AFIX 43
H21 2 0.953005 0.528156 0.903020 11.00000 -1.20000
AFIX 0
C19 1 0.829880 0.591362 0.623013 11.00000 0.06861 0.10127 =
0.11913 -0.01475 0.01826 0.03314
AFIX 137
H19A 2 0.849454 0.638484 0.597283 11.00000 -1.50000
H19B 2 0.803512 0.582338 0.711276 11.00000 -1.50000
H19C 2 0.801059 0.563656 0.544517 11.00000 -1.50000
AFIX 0
C8 1 0.978127 0.777812 0.482924 11.00000 0.10121 0.09752 =
0.09881 -0.01141 -0.01201 0.06066
AFIX 43
H8 2 0.975134 0.787350 0.384619 11.00000 -1.20000
AFIX 0
C27 1 0.747845 0.409846 0.028435 11.00000 0.08332 0.08421 =
0.11439 -0.01835 -0.02258 0.02894
AFIX 137
H27A 2 0.738179 0.435069 0.099700 11.00000 -1.50000
H27B 2 0.706301 0.369969 0.000182 11.00000 -1.50000
H27C 2 0.768596 0.437714 -0.056580 11.00000 -1.50000
AFIX 0
C11 1 0.913251 0.793255 0.849695 11.00000 0.11404 0.11214 =
0.15763 -0.00280 0.02512 0.05630
AFIX 43
H11 2 0.887857 0.813653 0.824907 11.00000 -1.20000
AFIX 0
C9 1 0.947023 0.795755 0.586938 11.00000 0.11096 0.10449 =
0.13785 -0.02465 -0.01744 0.06839
AFIX 43
H9 2 0.924325 0.818768 0.560712 11.00000 -1.20000
AFIX 0
C28 1 0.823151 0.360687 -0.019872 11.00000 0.09133 0.12268 =
0.16515 -0.08819 0.00805 0.03043
AFIX 137
H28A 2 0.846044 0.393899 -0.095658 11.00000 -1.50000
H28B 2 0.786310 0.320315 -0.062233 11.00000 -1.50000
H28C 2 0.854609 0.349792 0.025937 11.00000 -1.50000
AFIX 0
C26 1 0.762315 0.339677 0.219540 11.00000 0.09668 0.06320 =
0.12419 -0.02104 -0.01959 0.02410
AFIX 137
H26A 2 0.794555 0.329130 0.262561 11.00000 -1.50000
H26B 2 0.724036 0.298739 0.183064 11.00000 -1.50000
H26C 2 0.747243 0.359717 0.292642 11.00000 -1.50000
AFIX 0
C14 1 0.988087 0.732703 0.919998 11.00000 0.17350 0.08734 =
0.10424 -0.00903 0.00125 0.06312
AFIX 43
H14 2 1.013195 0.712065 0.945343 11.00000 -1.20000
AFIX 0
C12 1 0.916354 0.777320 0.987481 11.00000 0.16117 0.10355 =
0.14861 -0.00700 0.07288 0.04577
AFIX 43
H12 2 0.893289 0.786547 1.060196 11.00000 -1.20000
AFIX 0
C13 1 0.954769 0.746189 1.024691 11.00000 0.22347 0.11483 =
0.09999 0.00963 0.03651 0.08391
AFIX 43
H13 2 0.957020 0.734967 1.122110 11.00000 -1.20000
AFIX 0
C23 1 1.140415 0.620173 0.051544 11.00000 0.11007 0.13762 =
0.12994 -0.02416 0.03509 0.05251
AFIX 137
H23A 2 1.109685 0.610219 -0.029387 11.00000 -1.50000
H23B 2 1.117127 0.589182 0.130782 11.00000 -1.50000
H23C 2 1.178190 0.615348 0.020462 11.00000 -1.50000
AFIX 0
HKLF 4
REM aks82_a.res in P6(1)
REM wR2 = 0.1450, GooF = S = 1.015, Restrained GooF = 1.015 for all data
REM R1 = 0.0519 for 3797 Fo > 4sig(Fo) and 0.0831 for all 5690 data
REM 321 parameters refined using 1 restraints
END
WGHT 0.0785 0.0000
REM Highest difference peak 0.397, deepest hole -0.165, 1-sigma level 0.035
Q1 1 1.0457 0.7286 0.8503 11.00000 0.05 0.32
Q2 1 0.9766 0.7395 0.6072 11.00000 0.05 0.19
Q3 1 1.0411 0.7234 0.5701 11.00000 0.05 0.19
Q4 1 1.0643 0.7216 1.0156 11.00000 0.05 0.15
Q5 1 0.6429 0.4025 0.0469 11.00000 0.05 0.13
Q6 1 1.0755 0.7247 0.9664 11.00000 0.05 0.13
Q7 1 0.7403 0.3779 -0.2251 11.00000 0.05 0.12
Q8 1 1.1050 0.6321 -0.0423 11.00000 0.05 0.12
Q9 1 1.2018 0.8232 0.1513 11.00000 0.05 0.12
Q10 1 0.8418 0.3385 0.0949 11.00000 0.05 0.12
Q11 1 1.0405 0.6672 1.0147 11.00000 0.05 0.12
Q12 1 1.1194 0.6633 0.0163 11.00000 0.05 0.11
Q13 1 0.8979 0.7610 0.7361 11.00000 0.05 0.11
Q14 1 0.8150 0.5170 0.2526 11.00000 0.05 0.11
Q15 1 0.7991 0.5013 0.1120 11.00000 0.05 0.11
Q16 1 0.9196 0.5812 0.1512 11.00000 0.05 0.11
Q17 1 1.1157 0.7377 0.9289 11.00000 0.05 0.10
Q18 1 1.0404 0.6765 0.4353 11.00000 0.05 0.10
Q19 1 1.0791 0.6859 0.7580 11.00000 0.05 0.10
Q20 1 0.9818 0.8597 0.7975 11.00000 0.05 0.10
;
_shelx_res_checksum 92898
_shelx_hkl_file
;
0 0 -11-3.09796 2.76069 1
0 0 -10 0.96338 2.15322 1
0 0 -9-1.76330 2.10659 1
0 0 -9 0.74282 2.08123 10
0 0 -8-1.57714 2.30765 1
0 0 -8 0.66882 1.59829 10
0 0 -7 1.77519 1.65922 10
0 0 -7 2.07447 1.65355 1
0 0 -6 210.756 11.7790 10
0 0 -6 196.371 12.0068 1
0 0 -5 0.61090 0.63265 7
0 0 -5 1.28469 1.08552 10
0 0 -4 1.14971 0.97118 8
0 0 -4-0.08868 0.37470 14
0 0 -4 1.36936 0.95910 10
0 0 -4 0.33446 0.74753 3
0 0 -4-0.34916 0.88485 15
0 0 -4-0.22767 0.54404 4
0 0 -4 0.31472 0.79757 2
0 0 -4 0.76671 0.57124 7
0 0 -4 0.95048 0.42328 6
0 0 -4 0.17100 0.50046 11
0 0 -3 0.20037 0.41459 7
0 0 -3 0.55332 0.44066 4
0 0 -3 1.27668 0.74712 10
0 0 -3-0.12659 0.28294 6
0 0 -3 0.38599 0.40666 11
0 0 -3 0.59287 0.61334 8
0 0 -3-0.27098 0.68667 15
0 0 -3-0.25660 0.53093 3
0 0 -3-0.24214 0.50100 2
0 0 -2 0.42257 0.29155 7
0 0 -2 0.16525 0.36940 2
0 0 -2-0.09060 0.22972 6
0 0 -2 0.60877 0.54208 8
0 0 -2 0.08705 0.25483 11
0 0 -2 0.34911 0.32979 3
0 0 -2 0.13152 0.35138 4
0 0 -2 0.33623 0.51206 10
0 0 -2 1.11356 0.47036 15
0 0 -1 0.19084 0.18024 15
0 0 -1 0.16896 0.18881 2
0 0 -1-0.10396 0.12421 8
0 0 -1 0.62337 0.35282 3
0 0 1 0.09192 0.19019 9
0 0 1-0.09219 0.13488 3
0 0 1 0.97904 0.45014 8
0 0 1-0.08792 0.10505 2
0 0 2 0.18001 0.48109 2
0 0 2-0.16970 0.43032 4
0 0 2 0.18784 0.44907 3
0 0 2 0.88887 0.62274 8
0 0 2 0.82966 0.37494 6
0 0 2 0.93913 0.54982 9
0 0 3 0.27551 0.57003 2
0 0 3-0.18297 0.43714 6
0 0 3 0.28787 0.64332 9
0 0 3 0.26551 0.63433 4
0 0 4 1.12318 0.89447 2
0 0 4-0.39330 0.81377 9
0 0 4 0.37086 0.99061 4
0 0 4-0.48436 0.76543 6
0 0 5-0.50270 1.04008 9
0 0 5 0.47282 1.05664 4
0 0 6 193.113 11.9287 9
0 0 7-2.91635 2.22308 9
0 0 8 0.84492 1.88846 9
0 0 9 0.96173 1.99013 9
-1 1 -11-3.02403 2.08583 1
0 -1 -11-1.04025 2.32496 1
1 0 -11-1.05174 2.35062 1
0 1 -11 1.02672 2.12454 1
1 -1 -11 1.05840 2.19007 1
-1 0 -11-1.01651 2.57604 1
0 1 -10 6.68837 3.02276 1
-1 0 -10 6.63305 3.20438 1
0 -1 -10 2.90958 2.46132 1
-1 1 -10 6.58938 2.97811 1
1 0 -10 0.97847 2.19083 1
1 -1 -10 1.96984 2.35691 1
-1 1 -9 8.61737 3.09652 1
1 0 -9 8.92745 3.11745 1
-1 1 -9 5.97804 2.83191 10
1 -1 -9 10.8066 3.32346 1
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0 0 0 0.00 0.00 0
TITL AKS82 in P6(1)
REM P6(1) (#169 in standard setting)
CELL 0.71073 22.707254 22.707254 9.090779 90.0000 90.0000 120.0000
ZERR 57.00 0.000547 0.000547 0.000227 0.0000 0.0000 0.0000
LATT -1
SYMM -y, x-y, z+1/3
SYMM -x+y,-x, z+2/3
SYMM -x,-y, z+1/2
SYMM y,-x+y, z+5/6
SYMM x-y, x, z+1/6
SFAC C H N O S
UNIT 57.00 57.00 57.00 57.00 57.00
TREF
HKLF 4
END
;
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20 6 2 0.1011 -0.0115
20 6 3 -0.5733 -0.3003
20 7 0 0.1693 -0.0005
20 7 1 -0.8052 0.1577
21 1 0 0.0515 -0.0004
21 1 1 -0.9528 0.4112
21 1 2 -0.1745 0.1083
21 1 3 0.8759 0.5673
21 1 4 0.1459 0.0801
21 1 5 0.0187 0.3976
21 2 0 0.0381 -0.0003
21 2 1 -1.1647 0.5218
21 2 2 0.0374 0.2844
21 2 3 0.5706 0.1739
21 2 4 0.5365 -0.0506
21 3 0 0.0409 -0.0007
21 3 1 -1.3290 0.4747
21 3 2 0.1797 0.4203
21 3 3 0.1147 -0.1260
21 3 4 0.7855 -0.2757
21 4 0 0.1142 -0.0016
21 4 1 -1.3564 0.3238
21 4 2 0.2158 0.4004
21 4 3 -0.2949 -0.2558
21 5 0 0.2192 -0.0022
21 5 1 -1.1822 0.1704
21 5 2 0.1544 0.2322
21 5 3 -0.4893 -0.2683
21 6 0 0.2631 -0.0018
21 6 1 -0.8453 0.0801
22 1 0 0.0777 0.0005
22 1 1 -1.0809 0.5456
22 1 2 -0.0998 0.1916
22 1 3 0.7730 0.3713
22 1 4 0.2907 0.0112
22 2 0 0.1084 -0.0000
22 2 1 -1.1809 0.5438
22 2 2 0.1095 0.4094
22 2 3 0.3982 -0.0012
22 2 4 0.5528 -0.1285
22 3 0 0.1672 -0.0013
22 3 1 -1.1919 0.3866
22 3 2 0.2288 0.5159
22 3 3 -0.0054 -0.2046
22 4 0 0.2490 -0.0024
22 4 1 -1.0545 0.1729
22 5 0 0.2838 -0.0025
22 5 1 -0.7671 0.0137
23 1 0 0.0885 0.0011
23 1 1 -0.9241 0.5268
23 1 2 0.0072 0.3212
23 1 3 0.5541 0.2079
23 2 0 0.1258 -0.0000
23 2 1 -0.8973 0.3953
23 2 3 0.2398 -0.0602
23 3 0 0.1740 -0.0015
24 1 0 0.0353 0.0016
0 0 0 0.0 0.0
;
_shelx_fab_checksum 50201
_olex2_submission_original_sample_id AKS82
_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 1.624
_oxdiff_exptl_absorpt_empirical_full_min 0.633
#######################################################################
#
# 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_AKS95
_audit_block_doi 10.5517/ccdc.csd.cc28st1y
_database_code_depnum_ccdc_archive 'CCDC 2109210'
loop_
_audit_author_name
_audit_author_address
'kallol Mukherjee'
;University of Hyderabad
India
;
_audit_update_record
;
2021-09-11 deposited with the CCDC. 2021-10-20 downloaded from the CCDC.
;
_audit_creation_date 2021-09-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_chemical_formula_moiety 'C25 H32 N2 O5 S'
_chemical_formula_sum 'C25 H32 N2 O5 S'
_chemical_formula_weight 472.61
_chemical_absolute_configuration unk
_chemical_oxdiff_formula 'C H N O S'
_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2
_symmetry_Int_Tables_number 19
_cell_length_a 9.2225(2)
_cell_length_b 15.1104(3)
_cell_length_c 18.1484(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2529.08(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 14452
_cell_measurement_temperature 111(15)
_cell_measurement_theta_max 26.7550
_cell_measurement_theta_min 2.2360
_exptl_absorpt_coefficient_mu 0.165
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.65105
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'clear whiteish white'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whiteish
_exptl_crystal_colour_primary white
_exptl_crystal_density_diffrn 1.2411
_exptl_crystal_description block
_exptl_crystal_F_000 1008.9858
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.1
_diffrn_reflns_av_R_equivalents 0.0257
_diffrn_reflns_av_unetI/netI 0.0278
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 17182
_diffrn_reflns_theta_full 26.3699
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 2.24
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 111(15)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix3000
_diffrn_measured_fraction_theta_full 0.9850
_diffrn_measured_fraction_theta_max 0.9850
_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 -35.00 4.00 0.50 25.00 -- -14.97 -94.00 60.00 78
2 \w -53.00 43.00 0.50 25.00 -- 16.22 -61.00 60.00 192
3 \w -34.00 13.00 0.50 25.00 -- -14.97 -94.00 120.00 94
4 \w 43.00 80.00 0.50 25.00 -- 16.22 35.00 142.00 74
5 \w -60.00 2.00 0.50 25.00 -- -14.97 110.00 -4.00 124
6 \w -51.00 44.00 0.50 25.00 -- -14.97 92.00 -90.00 190
7 \w -35.00 14.00 0.50 25.00 -- 16.22 -94.00 0.00 98
8 \w -44.00 38.00 0.50 25.00 -- 16.22 -45.00-150.00 164
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0466965000
_diffrn_orient_matrix_UB_12 -0.0093118000
_diffrn_orient_matrix_UB_13 -0.0301022000
_diffrn_orient_matrix_UB_21 -0.0589591000
_diffrn_orient_matrix_UB_22 -0.0187498000
_diffrn_orient_matrix_UB_23 -0.0196079000
_diffrn_orient_matrix_UB_31 -0.0161501000
_diffrn_orient_matrix_UB_32 0.0419916000
_diffrn_orient_matrix_UB_33 -0.0154140000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage 0.972
_reflns_limit_h_max 11
_reflns_limit_h_min -11
_reflns_limit_k_max 18
_reflns_limit_k_min -18
_reflns_limit_l_max 22
_reflns_limit_l_min -22
_reflns_number_gt 4889
_reflns_number_total 5105
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression I>=2u(I)
_computing_cell_refinement 'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.3602
_refine_diff_density_min -0.2472
_refine_diff_density_rms 0.0382
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack 0.04(5)
_refine_ls_d_res_high 0.8001
_refine_ls_d_res_low 9.0742
_refine_ls_goodness_of_fit_ref 1.0345
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_constraints 48
_refine_ls_number_parameters 306
_refine_ls_number_reflns 5105
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0313
_refine_ls_R_factor_gt 0.0298
_refine_ls_restrained_S_all 1.0345
_refine_ls_shift/su_max 0.0000
_refine_ls_shift/su_mean 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.5513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0741
_refine_ls_wR_factor_ref 0.0749
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C5(H5), C7(H7), C8(H8), C2(H2), C3(H3), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
C20(H20a,H20b,H20c), C23(H23a,H23b,H23c), C25(H25a,H25b,H25c), C24(H24a,H24b,
H24c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,
H14b,H14c)
;
_atom_sites_solution_primary dual
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_refinement_flags_posn
S1 S 0.68374(4) 0.66571(2) 0.17588(2) 0.01478(9) Uani 1.000000 .
O1 O 0.83340(12) 0.44803(7) 0.21805(6) 0.0213(2) Uani 1.000000 .
O3 O 0.78737(12) 0.71388(7) 0.13187(6) 0.0200(2) Uani 1.000000 .
O2 O 0.95018(13) 0.57998(8) 0.22375(7) 0.0263(3) Uani 1.000000 .
O5 O 0.29986(14) 0.99972(8) 0.09605(6) 0.0290(3) Uani 1.000000 .
O4 O 0.48788(15) 0.92640(9) 0.04754(6) 0.0329(3) Uani 1.000000 .
N1 N 0.70549(14) 0.56618(8) 0.19239(7) 0.0170(3) Uani 1.000000 .
N2 N 0.52526(16) 0.69277(9) 0.06092(8) 0.0245(3) Uani 1.000000 .
C6 C 0.58433(16) 0.81083(10) 0.25438(8) 0.0162(3) Uani 1.000000 .
C9 C 0.40213(18) 0.95047(10) 0.10299(9) 0.0197(3) Uani 1.000000 .
C5 C 0.54692(16) 0.85106(9) 0.32093(9) 0.0175(3) Uani 1.000000 .
H5 H 0.50246(16) 0.90629(9) 0.31977(9) 0.0210(4) Uiso 1.000000 R
C7 C 0.55109(16) 0.85386(9) 0.18349(8) 0.0161(3) Uani 1.000000 .
H7 H 0.60966(16) 0.84100(9) 0.14318(8) 0.0193(4) Uiso 1.000000 R
C21 C 0.84204(17) 0.53661(10) 0.21294(8) 0.0172(3) Uani 1.000000 .
C1 C 0.64966(16) 0.72637(10) 0.25805(8) 0.0157(3) Uani 1.000000 .
C15 C 0.50951(17) 0.66608(10) 0.13007(8) 0.0176(3) Uani 1.000000 .
C16 C 0.37929(17) 0.64417(10) 0.16444(9) 0.0197(3) Uani 1.000000 .
C8 C 0.44222(17) 0.90985(10) 0.17420(9) 0.0196(3) Uani 1.000000 .
H8 H 0.38718(17) 0.92465(10) 0.21533(9) 0.0236(4) Uiso 1.000000 R
C4 C 0.57365(17) 0.81162(10) 0.38927(8) 0.0178(3) Uani 1.000000 .
C2 C 0.67796(16) 0.68643(9) 0.32493(8) 0.0179(3) Uani 1.000000 .
H2 H 0.72118(16) 0.63086(9) 0.32645(8) 0.0215(4) Uiso 1.000000 R
C20 C 0.36369(19) 0.61144(12) 0.24225(9) 0.0262(4) Uani 1.000000 .
H20a H 0.4392(8) 0.5696(6) 0.2527(2) 0.0393(6) Uiso 1.000000 GR
H20b H 0.3709(13) 0.66047(16) 0.27569(10) 0.0393(6) Uiso 1.000000 GR
H20c H 0.2710(6) 0.5834(7) 0.2480(2) 0.0393(6) Uiso 1.000000 GR
C3 C 0.64173(18) 0.72947(11) 0.38980(8) 0.0200(3) Uani 1.000000 .
H3 H 0.66340(18) 0.70285(11) 0.43467(8) 0.0240(4) Uiso 1.000000 R
C22 C 0.96156(18) 0.39361(11) 0.23763(10) 0.0251(4) Uani 1.000000 .
C17 C 0.25573(19) 0.65607(11) 0.12066(10) 0.0269(4) Uani 1.000000 .
H17 H 0.16449(19) 0.64427(11) 0.14015(10) 0.0323(5) Uiso 1.000000 R
C18 C 0.2682(2) 0.68508(12) 0.04902(10) 0.0319(4) Uani 1.000000 .
H18 H 0.1861(2) 0.69355(12) 0.02014(10) 0.0383(5) Uiso 1.000000 R
C11 C 0.5301(2) 0.86052(11) 0.45997(9) 0.0248(4) Uani 1.000000 .
C19 C 0.4044(2) 0.70136(12) 0.02078(10) 0.0320(4) Uani 1.000000 .
H19 H 0.4126(2) 0.71903(12) -0.02813(10) 0.0384(5) Uiso 1.000000 R
C23 C 1.07328(18) 0.40077(12) 0.17725(11) 0.0301(4) Uani 1.000000 .
H23a H 1.0292(4) 0.3867(8) 0.13078(14) 0.0452(6) Uiso 1.000000 GR
H23b H 1.1106(10) 0.4600(3) 0.1757(5) 0.0452(6) Uiso 1.000000 GR
H23c H 1.1511(7) 0.3602(6) 0.1868(4) 0.0452(6) Uiso 1.000000 GR
C25 C 1.0206(2) 0.41989(14) 0.31249(10) 0.0377(5) Uani 1.000000 .
H25a H 1.0625(14) 0.4779(4) 0.3095(2) 0.0565(7) Uiso 1.000000 GR
H25b H 0.9431(4) 0.4201(9) 0.3479(2) 0.0565(7) Uiso 1.000000 GR
H25c H 1.0934(11) 0.3782(6) 0.3275(4) 0.0565(7) Uiso 1.000000 GR
C24 C 0.8970(2) 0.30097(12) 0.23903(13) 0.0410(5) Uani 1.000000 .
H24a H 0.8219(12) 0.2983(3) 0.2756(6) 0.0615(8) Uiso 1.000000 GR
H24b H 0.8570(15) 0.2873(4) 0.1915(3) 0.0615(8) Uiso 1.000000 GR
H24c H 0.9714(4) 0.25890(16) 0.2509(8) 0.0615(8) Uiso 1.000000 GR
C10 C 0.4447(3) 0.96079(17) -0.02344(11) 0.0529(7) Uani 1.000000 .
H10a H 0.5128(11) 0.9419(9) -0.06024(19) 0.0793(10) Uiso 1.000000 GR
H10b H 0.3499(8) 0.9390(9) -0.0357(4) 0.0793(10) Uiso 1.000000 GR
H10c H 0.4428(17) 1.02427(17) -0.0216(3) 0.0793(10) Uiso 1.000000 GR
C12 C 0.5336(3) 0.80073(15) 0.52722(11) 0.0488(6) Uani 1.000000 .
H12a H 0.4720(14) 0.7505(6) 0.5190(4) 0.0731(9) Uiso 1.000000 GR
H12b H 0.6311(4) 0.7810(9) 0.5357(5) 0.0731(9) Uiso 1.000000 GR
H12c H 0.4999(17) 0.8330(4) 0.5695(2) 0.0731(9) Uiso 1.000000 GR
C13 C 0.3742(3) 0.89446(17) 0.45278(11) 0.0511(6) Uani 1.000000 .
H13a H 0.3704(4) 0.9401(8) 0.4160(7) 0.0766(10) Uiso 1.000000 GR
H13b H 0.3118(4) 0.8466(3) 0.4386(9) 0.0766(10) Uiso 1.000000 GR
H13c H 0.3427(7) 0.9180(10) 0.4992(3) 0.0766(10) Uiso 1.000000 GR
C14 C 0.6313(3) 0.93868(18) 0.47095(13) 0.0671(9) Uani 1.000000 .
H14a H 0.7278(6) 0.91752(18) 0.4801(11) 0.1007(13) Uiso 1.000000 GR
H14b H 0.6312(18) 0.9748(8) 0.4274(5) 0.1007(13) Uiso 1.000000 GR
H14c H 0.5990(14) 0.9731(8) 0.5122(7) 0.1007(13) Uiso 1.000000 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.01458(16) 0.01441(17) 0.01535(16) 0.00097(13) -0.00003(15) 0.00000(14)
O1 0.0157(5) 0.0153(5) 0.0329(6) 0.0026(4) 0.0009(5) 0.0044(5)
O3 0.0198(6) 0.0206(6) 0.0196(5) -0.0001(5) 0.0042(5) 0.0017(4)
O2 0.0187(6) 0.0212(6) 0.0389(7) -0.0021(5) -0.0057(5) 0.0021(5)
O5 0.0331(7) 0.0302(6) 0.0236(6) 0.0161(6) -0.0036(5) 0.0003(5)
O4 0.0401(8) 0.0415(8) 0.0170(6) 0.0234(6) 0.0061(5) 0.0086(5)
N1 0.0159(6) 0.0141(6) 0.0209(6) 0.0003(5) -0.0001(5) -0.0009(5)
N2 0.0284(7) 0.0257(8) 0.0192(7) -0.0017(6) -0.0064(6) 0.0023(5)
C6 0.0143(7) 0.0162(7) 0.0182(7) -0.0018(6) 0.0006(6) 0.0019(6)
C9 0.0234(8) 0.0152(7) 0.0205(8) 0.0025(7) -0.0021(7) -0.0003(6)
C5 0.0177(7) 0.0147(7) 0.0200(7) 0.0019(6) 0.0024(7) 0.0002(6)
C7 0.0179(7) 0.0148(7) 0.0156(7) -0.0011(6) 0.0006(6) -0.0009(6)
C21 0.0182(8) 0.0168(8) 0.0166(7) 0.0024(6) 0.0020(6) -0.0009(6)
C1 0.0137(7) 0.0161(7) 0.0173(7) -0.0003(6) 0.0009(6) -0.0016(6)
C15 0.0186(7) 0.0130(7) 0.0212(7) 0.0017(6) -0.0042(6) -0.0014(6)
C16 0.0192(7) 0.0145(7) 0.0255(8) 0.0001(6) -0.0013(7) -0.0036(6)
C8 0.0222(8) 0.0212(8) 0.0155(7) 0.0039(6) 0.0013(7) -0.0004(6)
C4 0.0159(7) 0.0204(8) 0.0172(7) 0.0000(6) 0.0025(6) 0.0005(6)
C2 0.0196(7) 0.0149(7) 0.0192(7) 0.0015(6) -0.0008(7) 0.0021(6)
C20 0.0215(8) 0.0299(9) 0.0272(9) -0.0026(7) 0.0008(7) 0.0033(7)
C3 0.0232(8) 0.0210(8) 0.0158(7) 0.0010(7) -0.0000(6) 0.0032(6)
C22 0.0197(8) 0.0227(8) 0.0330(9) 0.0089(7) 0.0027(7) 0.0073(7)
C17 0.0201(8) 0.0248(9) 0.0359(9) 0.0018(7) -0.0063(7) -0.0043(7)
C18 0.0305(9) 0.0286(10) 0.0367(10) 0.0024(8) -0.0156(8) -0.0014(8)
C11 0.0331(9) 0.0242(8) 0.0173(8) 0.0033(7) 0.0060(7) 0.0001(6)
C19 0.0379(10) 0.0330(10) 0.0252(9) -0.0016(8) -0.0129(8) 0.0048(7)
C23 0.0256(9) 0.0292(9) 0.0357(10) 0.0112(7) 0.0057(8) 0.0068(8)
C25 0.0362(10) 0.0460(12) 0.0309(10) 0.0149(9) -0.0019(9) 0.0099(9)
C24 0.0340(10) 0.0215(9) 0.0675(15) 0.0067(8) 0.0064(11) 0.0143(9)
C10 0.0713(17) 0.0676(16) 0.0197(9) 0.0393(13) 0.0078(10) 0.0138(9)
C12 0.0773(17) 0.0482(13) 0.0207(9) 0.0269(12) 0.0145(10) 0.0061(8)
C13 0.0563(15) 0.0700(16) 0.0270(10) 0.0348(13) 0.0111(10) 0.0004(10)
C14 0.092(2) 0.0656(16) 0.0436(13) -0.0401(16) 0.0264(14) -0.0334(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4426(11) . ?
S1 N1 1.5466(12) . ?
S1 C1 1.7784(15) . ?
S1 C15 1.8093(15) . ?
O1 C21 1.3440(18) . ?
O1 C22 1.4832(18) . ?
O2 C21 1.2094(19) . ?
O5 C9 1.2080(19) . ?
O4 C9 1.331(2) . ?
O4 C10 1.445(2) . ?
N1 C21 1.3873(19) . ?
N2 C15 1.326(2) . ?
N2 C19 1.338(2) . ?
C6 C5 1.395(2) . ?
C6 C7 1.474(2) . ?
C6 C1 1.413(2) . ?
C9 C8 1.478(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.398(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.324(2) . ?
C1 C2 1.380(2) . ?
C15 C16 1.393(2) . ?
C16 C20 1.503(2) . ?
C16 C17 1.401(2) . ?
C8 H8 0.9300 . ?
C4 C3 1.391(2) . ?
C4 C11 1.534(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.386(2) . ?
C20 H20a 0.9600 . ?
C20 H20b 0.9600 . ?
C20 H20c 0.9600 . ?
C3 H3 0.9300 . ?
C22 C23 1.508(2) . ?
C22 C25 1.516(3) . ?
C22 C24 1.521(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.377(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.379(3) . ?
C11 C12 1.519(2) . ?
C11 C13 1.532(3) . ?
C11 C14 1.518(3) . ?
C19 H19 0.9300 . ?
C23 H23a 0.9600 . ?
C23 H23b 0.9600 . ?
C23 H23c 0.9600 . ?
C25 H25a 0.9600 . ?
C25 H25b 0.9600 . ?
C25 H25c 0.9600 . ?
C24 H24a 0.9600 . ?
C24 H24b 0.9600 . ?
C24 H24c 0.9600 . ?
C10 H10a 0.9600 . ?
C10 H10b 0.9600 . ?
C10 H10c 0.9600 . ?
C12 H12a 0.9600 . ?
C12 H12b 0.9600 . ?
C12 H12c 0.9600 . ?
C13 H13a 0.9600 . ?
C13 H13b 0.9600 . ?
C13 H13c 0.9600 . ?
C14 H14a 0.9600 . ?
C14 H14b 0.9600 . ?
C14 H14c 0.9600 . ?
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
N1 S1 O3 120.79(7) . . ?
C1 S1 O3 108.75(7) . . ?
C1 S1 N1 111.21(7) . . ?
C15 S1 O3 109.41(7) . . ?
C15 S1 N1 101.96(7) . . ?
C15 S1 C1 103.11(7) . . ?
C22 O1 C21 121.43(13) . . ?
C10 O4 C9 114.36(14) . . ?
C21 N1 S1 118.89(10) . . ?
C19 N2 C15 116.97(15) . . ?
C7 C6 C5 120.80(13) . . ?
C1 C6 C5 117.26(13) . . ?
C1 C6 C7 121.90(13) . . ?
O4 C9 O5 123.60(14) . . ?
C8 C9 O5 122.85(15) . . ?
C8 C9 O4 113.53(13) . . ?
H5 C5 C6 118.70(8) . . ?
C4 C5 C6 122.59(13) . . ?
C4 C5 H5 118.70(9) . . ?
H7 C7 C6 118.28(8) . . ?
C8 C7 C6 123.43(14) . . ?
C8 C7 H7 118.28(10) . . ?
O2 C21 O1 125.27(14) . . ?
N1 C21 O1 106.59(13) . . ?
N1 C21 O2 128.14(14) . . ?
C6 C1 S1 120.08(11) . . ?
C2 C1 S1 118.60(11) . . ?
C2 C1 C6 121.13(13) . . ?
N2 C15 S1 109.79(12) . . ?
C16 C15 S1 123.99(12) . . ?
C16 C15 N2 126.18(15) . . ?
C20 C16 C15 125.55(14) . . ?
C17 C16 C15 114.64(14) . . ?
C17 C16 C20 119.81(15) . . ?
C7 C8 C9 124.52(14) . . ?
H8 C8 C9 117.74(8) . . ?
H8 C8 C7 117.74(10) . . ?
C3 C4 C5 117.79(14) . . ?
C11 C4 C5 119.38(14) . . ?
C11 C4 C3 122.82(14) . . ?
H2 C2 C1 120.12(9) . . ?
C3 C2 C1 119.75(13) . . ?
C3 C2 H2 120.12(9) . . ?
H20a C20 C16 109.5 . . ?
H20b C20 C16 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 C16 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
C2 C3 C4 121.44(14) . . ?
H3 C3 C4 119.28(9) . . ?
H3 C3 C2 119.28(9) . . ?
C23 C22 O1 109.30(13) . . ?
C25 C22 O1 110.82(14) . . ?
C25 C22 C23 112.78(15) . . ?
C24 C22 O1 101.67(13) . . ?
C24 C22 C23 110.22(16) . . ?
C24 C22 C25 111.49(16) . . ?
H17 C17 C16 119.73(10) . . ?
C18 C17 C16 120.55(16) . . ?
C18 C17 H17 119.73(11) . . ?
H18 C18 C17 120.52(11) . . ?
C19 C18 C17 118.96(16) . . ?
C19 C18 H18 120.52(10) . . ?
C12 C11 C4 112.34(14) . . ?
C13 C11 C4 109.60(15) . . ?
C13 C11 C12 106.70(17) . . ?
C14 C11 C4 108.88(15) . . ?
C14 C11 C12 110.14(19) . . ?
C14 C11 C13 109.13(19) . . ?
C18 C19 N2 122.63(16) . . ?
H19 C19 N2 118.68(10) . . ?
H19 C19 C18 118.68(10) . . ?
H23a C23 C22 109.5 . . ?
H23b C23 C22 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 C22 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?
H25a C25 C22 109.5 . . ?
H25b C25 C22 109.5 . . ?
H25b C25 H25a 109.5 . . ?
H25c C25 C22 109.5 . . ?
H25c C25 H25a 109.5 . . ?
H25c C25 H25b 109.5 . . ?
H24a C24 C22 109.5 . . ?
H24b C24 C22 109.5 . . ?
H24b C24 H24a 109.5 . . ?
H24c C24 C22 109.5 . . ?
H24c C24 H24a 109.5 . . ?
H24c C24 H24b 109.5 . . ?
H10a C10 O4 109.5 . . ?
H10b C10 O4 109.5 . . ?
H10b C10 H10a 109.5 . . ?
H10c C10 O4 109.5 . . ?
H10c C10 H10a 109.5 . . ?
H10c C10 H10b 109.5 . . ?
H12a C12 C11 109.5 . . ?
H12b C12 C11 109.5 . . ?
H12b C12 H12a 109.5 . . ?
H12c C12 C11 109.5 . . ?
H12c C12 H12a 109.5 . . ?
H12c C12 H12b 109.5 . . ?
H13a C13 C11 109.5 . . ?
H13b C13 C11 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 C11 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?
H14a C14 C11 109.5 . . ?
H14b C14 C11 109.5 . . ?
H14b C14 H14a 109.5 . . ?
H14c C14 C11 109.5 . . ?
H14c C14 H14a 109.5 . . ?
H14c C14 H14b 109.5 . . ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -2 6074.09 107.23
0 0 2 5856.6 107.25
0 0 2 5760.37 107.93
0 0 3 0.83 0.47
0 0 -3 0.56 0.25
0 0 -3 1.5 0.48
0 0 3 0.68 0.32
0 0 -3 0.54 0.32
0 0 4 2445.55 47.36
0 0 -4 2465.75 47.37
0 0 -4 2307.82 48.92
0 0 -4 2279.21 48.37
0 0 -5 0.13 0.54
0 0 5 0.25 0.43
0 0 -5 0.21 0.59
0 0 -6 540.25 14.59
0 0 6 522.33 12.44
0 0 -6 542.65 13.82
0 0 7 -0.27 0.51
0 0 -7 1.12 0.82
0 0 -7 0.57 0.72
0 0 -7 0.08 0.72
0 0 -8 566.25 15.48
0 0 -8 587.82 13.93
0 0 -8 582.15 16.76
0 0 8 567.71 14.01
0 0 -9 0.18 0.89
0 0 -9 1.93 1.16
0 0 9 0.35 0.75
0 0 -9 0.32 0.96
0 0 10 315.5 9.3
0 0 -10 290.7 11.55
0 0 11 -0.44 0.82
0 0 -11 0.58 1.07
0 0 -12 12.15 2.43
0 0 -13 1.04 1.49
0 0 -14 4092.02 89.54
0 0 -15 1.59 1.76
0 0 -16 216.29 11.69
0 0 -17 0.45 1.8
0 0 -18 125.79 9.16
0 0 -19 1.99 1.9
0 0 -20 328.32 15.17
0 0 -20 350.25 16.61
0 0 -21 3.19 2.67
0 0 -21 0.54 1.97
0 0 -22 172.52 11.03
0 0 -22 157.72 11.17
0 -1 2 2698.43 51.09
0 -1 2 2629.63 51.61
0 1 -2 2679.94 51.58
0 1 -2 2600.82 51.73
0 1 -2 2593.75 51.54
0 -1 2 2586.06 51.44
0 -1 2 2668.06 51.57
0 -1 2 2606.96 51.65
0 1 -3 2765.03 53.53
0 1 3 2807.53 52.61
0 1 -3 2528.05 53.41
0 1 -3 2697.66 52.61
0 -1 3 2739.99 53.14
0 -1 3 2676.03 53.66
0 -1 3 2619.61 53.66
0 -1 -3 2732.36 52.46
0 1 -3 2568.77 53.55
0 -1 3 2768.74 52.75
0 1 -4 1589.15 32.11
0 1 4 1508.73 30.97
0 1 -4 1568.29 32.5
0 -1 4 1578.83 32.49
0 -1 4 1633.3 31.61
0 1 -4 1611.82 30.97
0 -1 -4 1552.13 30.85
0 -1 4 1572.26 32.38
0 1 -5 74.94 3.69
0 -1 -5 84.02 2.83
0 -1 5 71.89 3.62
0 -1 5 76.29 3.16
0 -1 5 84.41 3.22
0 1 -5 78.57 2.83
0 1 5 99.92 3.14
0 1 -5 74.14 3.44
0 -1 -6 4113.71 82.33
0 1 -6 4107.58 79.92
0 1 -6 4085 81.59
0 1 6 4039.3 80.17
0 -1 6 4202.26 80.7
0 1 -6 4043.05 82.4
0 -1 6 3952.17 82.23
0 -1 7 317.41 8.98
0 1 -7 328.74 9.75
0 1 -7 378.24 11
0 1 7 321.37 8.56
0 -1 -7 317.61 10.11
0 -1 7 298.44 10.27
0 1 -7 332.32 8.37
0 -1 -8 81.81 5.19
0 1 -8 79.31 4.3
0 1 8 79.11 3.6
0 1 -8 81.84 3.42
0 1 -8 69.95 4.53
0 -1 8 75.33 3.66
0 1 -9 934.45 22.56
0 -1 9 933.02 21.36
0 -1 -9 959.83 23.31
0 1 9 903.41 21.02
0 -1 -9 901.54 24.68
0 1 -9 935.64 20.51
0 1 -9 913.03 23.86
0 -1 -10 1179.78 31.06
0 1 10 1196.99 26.86
0 -1 10 1209.22 27.17
0 1 -10 1259.08 30.48
0 -1 11 2.55 1.04
0 1 -11 3.82 1.35
0 -1 -11 5.3 1.73
0 1 -12 175.18 9.01
0 -1 -12 189.41 9.78
0 -1 -13 20.81 3.35
0 1 -13 18.39 2.99
0 1 -14 12.43 2.7
0 -1 -14 11.01 2.79
0 1 -15 287.75 13.16
0 -1 -15 300.36 13.95
0 1 -16 10.17 2.77
0 -1 -16 4.89 2.25
0 1 -16 7.29 2.26
0 1 -17 71.79 6.58
0 -1 -17 70.91 6.83
0 1 -17 79.71 6.3
0 1 -18 175.66 9.96
0 1 -18 169.36 10.52
0 -1 -18 154.99 10.46
0 1 -19 40.87 5.32
0 1 -19 53.38 5.58
0 -1 -19 44.76 5.85
0 -1 -20 2.7 2.46
0 1 -20 2.99 2.46
0 1 -20 3.93 2.16
0 -1 -21 19.13 4.23
0 1 -21 17.66 3.89
0 -1 -22 95.43 8.29
0 1 -22 101.66 8.55
0 -1 -22 101.73 9.12
0 -1 -23 192.38 12.87
0 2 0 927.18 19.47
0 -2 0 936.96 19.4
0 2 0 927.58 18.87
0 -2 0 934.1 18.83
0 2 -1 41.9 1.61
0 2 1 38.13 1.83
0 2 1 40.98 1.68
0 -2 1 43.42 1.59
0 -2 -1 39.38 1.63
0 -2 1 37.83 1.78
0 2 -1 41.77 1.98
0 -2 1 41.85 1.92
0 2 -1 46.36 1.52
0 -2 -1 41.54 1.85
0 -2 1 43.92 1.46
0 2 -1 40.49 1.89
0 2 -2 6.94 0.76
0 -2 2 6.96 0.72
0 2 2 6.36 0.69
0 -2 -2 5.39 0.64
0 2 2 11.82 0.93
0 -2 2 8.58 0.86
0 2 -2 7.12 0.59
0 -2 2 7.11 0.63
0 -2 -2 7.05 0.73
0 2 -2 7.71 0.92
0 -2 3 52.38 2.23
0 -2 3 55.95 2.43
0 2 -3 51.71 2.14
0 2 -3 51.26 2.13
0 -2 3 48.24 1.98
0 2 3 43.18 1.98
0 -2 -3 44.17 1.95
0 2 3 45.7 2.15
0 -2 3 50.05 2.04
0 2 -3 52.24 2.51
0 -2 3 51.26 2.16
0 -2 3 46.7 2.22
0 -2 4 701.64 15.59
0 -2 4 757.78 16.66
0 2 -4 717.3 16.46
0 -2 4 736.9 16.8
0 2 -4 717.6 16.94
0 2 4 851.61 15.63
0 -2 4 716.18 16.32
0 -2 4 729.91 15.72
0 2 -4 754.33 15.9
0 -2 4 738.05 16.58
0 2 4 709.65 15.73
0 2 -4 745.8 16.52
0 -2 -4 710.83 15.56
0 -2 -4 750.28 15.02
0 2 -5 782.68 16.46
0 2 -5 761.49 17.56
0 2 -5 796.38 16.49
0 -2 5 764.79 17.98
0 -2 5 790.65 16.66
0 2 5 759.34 16.31
0 -2 5 807.15 18.17
0 -2 5 756.09 16.16
0 -2 -5 720.8 15.87
0 -2 5 744.88 17.22
0 2 -5 776.82 18.03
0 -2 -5 725.49 16.08
0 2 -5 784.22 17.83
0 2 6 110.84 3.41
0 2 -6 108.62 3.7
0 -2 6 107.27 3.87
0 2 -6 117.2 4.95
0 -2 6 101.83 4.69
0 2 -6 104.15 4.64
0 -2 6 109.73 3.28
0 2 -6 103.69 4.45
0 -2 -6 110.72 3.26
0 -2 -6 116.62 3.52
0 -2 6 113.57 4.93
0 2 6 136.35 4.03
0 -2 6 114.73 4.33
0 2 -6 113.32 3.52
0 -2 7 75.08 3.36
0 2 7 93.68 2.86
0 2 -7 77.06 4.09
0 2 7 71.73 3.16
0 2 -7 77.96 3.16
0 -2 7 80.04 4.32
0 -2 7 75.94 3.6
0 -2 -7 86.59 2.59
0 -2 7 81.09 4.39
0 2 -7 87.14 4.1
0 2 -7 82.56 2.83
0 2 -7 87.6 4.45
0 -2 7 78.99 2.57
0 2 -8 851.72 18.41
0 2 -8 902.82 21.42
0 2 -8 809.62 20.54
0 2 -8 879.95 20.45
0 -2 8 867.57 17.04
0 -2 8 870.69 21.6
0 -2 -8 880.18 17
0 -2 8 871.19 19.57
0 2 8 792.55 18.68
0 -2 9 106.73 5.85
0 2 -9 93.38 5.39
0 -2 -9 135.8 6.26
0 2 9 102.82 4.32
0 2 -9 112.52 5.24
0 2 -9 113.74 5.53
0 -2 9 96.63 4.54
0 2 -9 102.29 4.01
0 2 -10 1134.91 28.68
0 -2 10 1133.44 26.16
0 -2 -10 1119.66 30.15
0 2 -10 1130.97 27.84
0 2 -11 14.57 2.33
0 -2 -11 15.49 2.83
0 -2 11 13.29 2.34
0 2 -11 14.5 2.18
0 -2 -12 104.89 7.28
0 2 -12 109.38 6.67
0 2 -12 105.81 6.15
0 -2 -13 2.31 1.6
0 2 -13 10.14 2.23
0 2 -13 12.43 2.32
0 -2 -14 253.38 12.52
0 2 -14 237.77 10.49
0 2 -14 248.3 11.43
0 -2 -15 104.19 7.97
0 2 -15 99.18 7.09
0 2 -15 96.39 6.57
0 -2 -16 655.41 23.44
0 2 -16 656.77 21.03
0 2 -16 652.86 21.8
0 2 -17 113.04 7.72
0 -2 -17 107.7 8.63
0 2 -17 114.6 8.09
0 -2 -18 -0.52 2.14
0 2 -18 0.39 1.31
0 2 -18 -0.86 1.58
0 -2 -19 277.71 14.87
0 2 -19 275.11 13.46
0 2 -20 109.8 8.41
0 -2 -20 114.35 9.54
0 -2 -21 5.23 2.65
0 2 -21 10.06 3.09
0 2 -22 28.81 4.76
0 -2 -22 22.37 4.84
0 -3 0 0.29 0.28
0 -3 0 0.22 0.31
0 3 0 0.11 0.22
0 3 0 0.08 0.38
0 3 1 184.47 5.71
0 -3 1 194.46 5.83
0 -3 1 201.1 4.89
0 3 -1 186.89 5.77
0 -3 1 197.88 5.7
0 -3 1 188.61 5.01
0 -3 -1 176.08 5.04
0 3 -1 190.77 5.93
0 3 1 189.63 5.24
0 3 -1 208.96 5.25
0 -3 -1 187.45 5.61
0 3 -2 8498.77 177.81
0 3 2 9370.21 178.31
0 3 -2 8963.86 177.41
0 -3 2 9594.08 178.62
0 -3 -2 9178.2 178.06
0 -3 -2 9213.16 178.53
0 -3 2 9383.95 177.43
0 3 2 8817.84 178.65
0 -3 2 9530.21 177.78
0 3 -2 9269.11 178.8
0 3 -2 9604.86 179.29
0 -3 2 9999 179.14
0 -3 3 2691.56 52.54
0 -3 3 2668.52 52.99
0 -3 -3 2640.31 53
0 3 3 2672.69 53.35
0 -3 -3 2563.6 53.03
0 -3 3 2796.71 53.75
0 -3 3 2688.17 53.1
0 3 -3 2687.8 53.43
0 3 -3 2675.32 52.39
0 -3 3 2625.13 52.48
0 3 3 2657.86 53.2
0 3 -3 2540.44 53.97
0 -3 4 340.09 8.44
0 -3 4 312.06 8.22
0 3 -4 319.8 8.52
0 3 4 324.87 8.51
0 3 -4 331.75 8.27
0 -3 4 325.12 8.76
0 3 -4 275.21 8.94
0 3 4 329.21 8.68
0 -3 4 313.79 8.83
0 -3 4 316.57 8.44
0 -3 -4 351.97 8.36
0 -3 5 269.21 7.74
0 -3 5 261.72 7.99
0 3 5 268.41 7.85
0 -3 5 258.54 7.03
0 -3 5 261.68 7.11
0 -3 -5 257.89 7.05
0 3 -5 258.72 7.35
0 3 5 288.16 7.35
0 -3 5 276.34 7.99
0 3 -5 269.79 7.63
0 -3 5 264.59 7.63
0 -3 -5 270.79 5.99
0 3 -5 262.78 8.37
0 3 6 867.64 18.89
0 -3 -6 861.19 18.61
0 -3 6 864.55 20.11
0 3 -6 841.82 18.98
0 -3 6 850.16 18.57
0 3 -6 869.58 20
0 -3 -6 871.14 17.74
0 3 -6 875.62 20.92
0 -3 6 880.34 20.08
0 3 6 871.39 20.04
0 -3 6 845.56 20.54
0 -3 6 865.02 19.73
0 -3 6 864.91 18.95
0 -3 7 455.68 11.25
0 -3 -7 466.98 10.27
0 3 7 427.93 11.27
0 3 -7 457.44 13.07
0 3 7 460.84 10.92
0 -3 7 469.31 12.72
0 3 -7 443.18 12.13
0 -3 7 475.85 13.13
0 -3 -7 442.66 10.51
0 3 -7 448.37 11.03
0 -3 7 478.05 12.11
0 -3 7 448 10.56
0 3 -7 431.3 12.35
0 3 -8 226.61 7.78
0 3 -8 220.34 8.09
0 3 8 235.79 6.4
0 3 -8 229 6.48
0 -3 8 230.44 6.96
0 -3 8 230.94 8.61
0 -3 8 227.9 7.47
0 3 -8 231.29 8.52
0 -3 -8 230.95 5.99
0 -3 8 241.42 8.44
0 3 8 192.78 6.64
0 -3 9 129.59 6.46
0 3 -9 121.89 5.92
0 3 -9 115.44 5.96
0 3 -9 119.39 4.08
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10 6 -2 89.83 8.78
10 6 -2 96.17 7.17
10 -6 2 82.26 7.89
10 -6 1 74.92 6.9
10 6 -1 70.76 6.23
10 6 0 98.04 7.9
10 -6 0 102.51 7.97
10 6 0 107.12 7.57
10 6 1 62.92 6.31
10 6 1 69.77 6.09
10 6 2 83.07 7.24
10 6 2 89.04 6.96
10 6 3 38.34 5.15
10 6 3 36.17 4.5
10 6 4 8.9 3.02
10 6 4 9.47 2.73
10 6 5 117.54 8.9
10 6 5 123.24 8.01
-10 6 -5 125.15 9.23
-10 6 -6 20.79 4.32
10 6 6 15.04 3.53
10 6 6 19.51 3.5
-10 6 -7 3.91 2.42
10 6 7 2.48 2.19
10 6 7 0.72 1.64
10 6 8 55.28 6.52
-10 6 -8 55.51 6.43
10 6 9 92.77 8.54
10 7 -7 61.69 7.69
10 7 -7 73.25 6.49
10 -7 7 50.7 7.2
10 7 -6 53.98 7.17
10 7 -6 69.79 6.37
10 -7 6 60.91 7.48
10 7 -5 8.72 3.91
10 7 -5 15.41 3.21
10 -7 5 5.31 3.85
10 7 -4 13.2 4.22
10 7 -4 18.09 3.54
10 -7 4 17.1 4.37
10 7 -3 27 4.02
10 -7 3 29.25 5.31
10 7 -2 143.61 8.97
10 -7 2 140.15 10.2
10 7 -1 94.9 7.35
10 7 0 190.07 10.46
10 7 1 110.22 7.76
10 7 2 137.45 8.67
10 7 3 33.59 4.55
10 7 4 17.5 3.46
10 7 5 6.83 2.69
10 7 6 69.5 6.1
-10 7 -6 56.16 6.52
10 8 -7 18.69 3.68
10 8 -6 43.1 6.17
10 8 -6 40.88 5.16
10 8 -5 3.33 3.07
10 8 -5 2.52 2.18
10 -8 5 0.54 3.36
10 8 -4 115.35 8.33
10 -8 4 102.76 9.07
10 8 -3 63.82 6.14
10 -8 3 60.7 7.1
10 8 -2 59.94 5.98
10 -8 2 61.96 6.96
10 8 -1 85.82 7.18
10 8 0 170.05 10.03
10 8 1 79.43 6.83
10 8 2 69.04 6.37
10 8 3 68.75 6.34
10 8 4 112.48 8.02
10 8 5 1.61 1.84
10 8 6 46.58 5.38
10 -9 3 26.64 5.24
10 -9 2 2.01 3.04
11 0 0 1 1.92
11 0 -1 44.82 5.9
11 0 1 46.02 5.95
11 0 2 86.21 7.91
11 0 3 0.52 2.51
11 0 4 11.03 3.59
11 0 -4 17.6 3.41
11 0 5 45.58 5.06
11 0 5 40.88 5.71
11 0 6 41.94 4.84
11 0 -6 49.9 5.38
11 0 -7 1.17 1.97
11 1 -7 24.39 3.99
11 1 -6 9.34 2.79
11 -1 5 54.11 6.47
11 1 -5 62.86 5.96
11 -1 4 97.66 8.52
11 1 -4 101.41 7.61
11 -1 3 86.86 8.09
11 1 -3 83.87 6.94
11 -1 2 97.81 8.41
11 1 -2 96.55 7.41
11 1 -1 2.51 2.29
11 -1 1 5.56 2.44
11 1 -1 5.85 2.44
11 1 0 12.5 3.46
11 -1 0 6.02 2.83
11 1 0 13.59 2.88
11 -1 -1 3.53 2.43
11 1 1 8.59 3.35
11 1 1 5.02 2.42
11 1 2 94.1 8.25
11 1 2 98.7 7.31
11 1 3 85.24 7.97
11 1 3 100.24 7.33
11 1 4 72.4 7.35
11 1 4 82.42 6.75
11 1 5 41.4 5.96
11 1 5 52.2 5.42
11 1 6 4.07 1.92
11 2 -7 61.54 6.12
11 2 -6 422.39 16.68
11 -2 5 64.68 7.11
11 2 -5 53.08 7.64
11 2 -5 73.94 6.49
11 -2 4 28.79 5.08
11 2 -4 36.02 4.66
11 -2 3 5.71 2.81
11 2 -3 10.17 2.87
11 -2 2 133.36 9.78
11 2 -2 136.59 8.82
11 2 -1 33.58 4.93
11 -2 1 30.31 4.81
11 2 -1 31.09 4.46
11 2 0 196.98 12.01
11 -2 0 185.77 11.68
11 2 0 199.66 10.68
11 -2 -1 38.25 5.26
11 2 1 34.22 4.96
11 2 1 35.04 4.65
11 2 2 134.97 9.84
11 2 2 142.11 8.84
11 2 3 7.77 3.14
11 2 3 11.42 2.7
11 2 4 29.83 5
11 2 4 26.44 4.1
11 2 5 63.11 7.09
11 2 5 65.51 6.05
11 2 6 395.89 15.67
11 3 -7 6.3 2.69
11 3 -6 43.89 5.14
11 3 -5 9.6 4.67
11 -3 5 8.44 3.03
11 3 -5 8.72 2.91
11 3 -4 4.75 3.82
11 -3 4 6.26 3
11 3 -4 5.94 2.55
11 -3 3 152.51 10.69
11 3 -3 148.79 12.01
11 3 -3 173.1 9.99
11 -3 2 16.54 3.73
11 3 -2 21.61 4.02
11 -3 1 26.56 4.7
11 3 -1 36.01 4.64
11 3 0 88.42 7.89
11 -3 0 89.34 8.08
11 3 0 105.65 7.68
11 3 1 33.93 4.94
11 3 1 35.31 4.78
11 3 2 19.98 4
11 3 2 20.45 3.66
11 3 3 165.99 11.15
11 3 3 184.17 10.21
11 3 4 5.73 2.64
11 3 4 8.78 2.77
11 3 5 6.87 3.09
11 3 5 11 3.03
11 3 6 42.76 4.97
-11 3 -7 8.89 2.98
11 -4 5 2.1 2.25
11 4 -5 -1.21 2.13
11 -4 4 53.34 6.54
11 4 -4 50.53 7.52
11 4 -4 62.92 6.18
11 4 -3 19.94 5.15
11 -4 3 15.3 3.79
11 4 -3 18.77 3.63
11 -4 2 17.52 3.99
11 4 -2 11.55 3.18
11 -4 1 13.45 3.66
11 4 -1 15.47 3.41
11 4 0 76.39 7.38
11 -4 0 72.25 7.33
11 4 0 62.36 6.09
11 4 1 23.32 4.43
11 4 1 12.96 3.12
11 4 2 10.48 3.36
11 4 2 11.73 3
11 4 3 17.3 3.99
11 4 3 20.21 3.66
11 4 4 56.44 6.5
11 4 4 50.63 5.43
-11 4 -5 -0.47 2.2
11 4 5 -1.54 2.12
11 -5 4 100.12 8.61
11 5 -4 79.93 9.21
11 5 -3 18.4 5.15
11 -5 3 28.11 4.79
11 5 -2 3.87 3.42
11 -5 2 -0.99 2.51
11 -5 1 20.65 4.12
11 5 0 43.61 5.69
11 -5 0 27.99 4.78
11 5 1 17.17 3.89
11 5 2 2.48 2.39
11 5 3 33.11 5.09
11 5 4 104.33 8.8
11 6 -3 19.97 5.57
11 6 0 0.97 2.28
11 6 1 98.98 8.52
11 6 2 14.18 3.71
11 6 3 15.21 3.73
_iucr_refine_fcf_details
;
data_AKS95_CCDC1
_computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)'
_shelx_refln_list_code 4
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2
_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'
_symmetry_space_group_name_H-M 'P 21 21 21'
_symmetry_space_group_name_Hall ' P 2ac 2ab'
_symmetry_Int_Tables_number 19
_cell_length_a 9.2225(2)
_cell_length_b 15.1104(3)
_cell_length_c 18.1484(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2529.08(9)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_F_squared_weight
_refln_observed_status
-11 -5 -3 78.875 64.737 12.777 43.689 o
-11 -5 -2 4.258 2.808 6.395 215.554 o
-11 -5 -1 37.831 54.343 10.842 64.280 o
-11 -4 -4 153.388 149.591 10.148 42.021 o
-11 -4 -3 46.450 47.109 6.148 138.948 o
-11 -4 -2 36.129 38.105 7.855 110.387 o
-11 -4 -1 42.026 38.425 6.566 136.207 o
-11 -3 -5 20.792 23.233 5.038 244.079 o
-11 -3 -4 12.128 15.086 4.557 328.064 o
-11 -3 -3 418.593 421.807 19.901 10.485 o
-11 -3 -2 51.277 50.590 7.196 110.709 o
-11 -3 -1 98.701 84.364 12.434 42.273 o
-11 -2 -6 1022.990 1111.570 43.896 2.249 o
-11 -2 -5 177.683 174.021 13.836 27.741 o
-11 -2 -4 84.580 87.140 9.513 62.523 o
-11 -2 -3 27.598 21.321 5.869 187.428 o
-11 -2 -2 374.600 355.692 17.237 13.283 o
-11 -2 -1 72.357 83.313 7.172 91.081 o
-11 -1 -6 13.897 24.579 7.342 144.865 o
-11 -1 -5 146.008 155.704 11.536 37.402 o
-11 -1 -4 229.792 262.586 14.936 21.054 o
-11 -1 -3 208.894 224.118 13.862 24.597 o
-11 -1 -2 236.293 255.544 14.631 21.370 o
-11 -1 -1 15.972 12.091 3.626 429.938 o
-10 -9 -3 80.521 70.107 13.790 38.411 o
-10 -9 -2 2.659 5.290 8.000 140.487 o
-10 -8 -5 3.054 5.840 4.135 479.845 o
-10 -8 -4 304.930 289.344 16.566 16.244 o
-10 -8 -3 174.518 164.538 12.222 32.356 o
-10 -8 -2 160.448 160.041 11.936 34.544 o
-10 -8 -1 261.328 225.847 18.895 15.836 o
-10 -7 -7 178.138 168.893 15.531 24.240 o
-10 -7 -6 152.400 165.746 11.092 37.776 o
-10 -7 -5 25.080 29.305 7.763 122.123 o
-10 -7 -4 51.550 43.752 6.064 137.810 o
-10 -7 -3 85.552 73.322 8.435 73.714 o
-10 -7 -2 348.215 374.012 17.726 13.309 o
-10 -7 -1 280.008 249.742 19.343 14.733 o
-10 -6 -8 128.471 119.055 18.264 21.780 o
-10 -6 -7 10.808 8.659 5.737 239.951 o
-10 -6 -6 52.464 48.797 7.566 103.767 o
-10 -6 -5 282.217 284.985 11.556 22.805 o
-10 -6 -4 25.425 16.961 4.117 307.382 o
-10 -6 -3 92.419 90.712 6.782 85.095 o
-10 -6 -2 225.971 239.319 10.308 29.837 o
-10 -6 -1 186.719 191.286 12.169 30.540 o
-10 -5 -9 184.123 166.312 18.711 18.739 o
-10 -5 -8 82.840 98.003 10.728 53.019 o
-10 -5 -7 390.125 400.883 24.124 9.043 o
-10 -5 -6 227.292 222.216 11.608 27.810 o
-10 -5 -5 298.223 296.741 13.383 19.620 o
-10 -5 -4 61.655 54.158 6.227 121.173 o
-10 -5 -3 44.972 47.429 5.909 146.614 o
-10 -5 -2 137.576 119.845 7.547 59.871 o
-10 -5 -1 10.337 12.764 3.460 506.481 o
-10 -4 -10 26.093 25.000 8.421 107.686 o
-10 -4 -9 126.068 114.588 25.527 12.511 o
-10 -4 -8 67.218 65.992 13.171 42.746 o
-10 -4 -7 221.283 228.984 12.324 26.612 o
-10 -4 -6 6.406 7.453 3.827 502.658 o
-10 -4 -5 365.284 370.937 14.845 14.968 o
-10 -4 -4 100.939 103.798 14.495 32.937 o
-10 -4 -3 221.187 240.064 11.764 27.324 o
-10 -4 -2 323.467 330.562 15.874 15.809 o
-10 -4 -1 120.197 96.445 7.158 70.479 o
-10 -3 -10 1.596 9.444 5.108 325.854 o
-10 -3 -9 138.838 160.561 13.574 31.325 o
-10 -3 -8 8.081 4.650 5.134 306.323 o
-10 -3 -7 850.382 781.726 31.211 3.817 o
-10 -3 -6 34.541 32.999 5.329 189.751 o
-10 -3 -5 241.012 266.039 14.324 21.393 o
-10 -3 -4 94.820 110.123 8.190 67.792 o
-10 -3 -3 106.654 124.887 9.841 52.210 o
-10 -3 -2 309.457 324.774 15.743 16.392 o
-10 -3 -1 592.706 586.737 22.854 6.833 o
-10 -2 -10 67.333 83.634 10.408 59.354 o
-10 -2 -9 147.372 145.210 16.961 23.179 o
-10 -2 -8 11.908 10.556 5.586 245.791 o
-10 -2 -7 850.376 894.801 24.193 4.305 o
-10 -2 -6 149.617 118.566 8.674 51.411 o
-10 -2 -5 636.118 652.754 44.830 3.128 o
-10 -2 -4 261.108 298.755 15.119 18.971 o
-10 -2 -3 105.810 119.932 9.652 53.922 o
-10 -2 -2 263.891 280.244 20.948 13.374 o
-10 -2 -1 151.073 157.209 9.019 46.362 o
-10 -1 -10 292.698 287.741 18.099 15.158 o
-10 -1 -9 10.265 8.463 5.895 230.471 o
-10 -1 -8 365.076 381.656 17.385 13.116 o
-10 -1 -7 178.557 208.070 21.408 15.097 o
-10 -1 -6 150.457 150.596 9.622 44.442 o
-10 -1 -5 144.512 158.938 11.035 39.176 o
-10 -1 -4 181.972 212.389 12.792 28.667 o
-10 -1 -3 111.492 106.770 9.230 56.727 o
-10 -1 -2 289.775 290.630 40.119 4.898 o
-10 -1 -1 227.602 231.693 10.941 28.756 o
-9 -11 -5 135.172 145.687 16.264 25.119 o
-9 -11 -4 21.532 23.968 6.221 179.099 o
-9 -11 -3 8.938 2.498 4.790 346.427 o
-9 -11 -2 48.801 49.557 9.461 77.200 o
-9 -11 -1 9.866 9.182 5.033 301.059 o
-9 -10 -7 137.004 137.661 15.395 27.252 o
-9 -10 -6 241.285 264.518 15.661 19.598 o
-9 -10 -5 158.276 193.181 13.193 29.918 o
-9 -10 -4 50.645 48.619 14.092 40.334 o
-9 -10 -3 130.163 143.909 11.426 40.072 o
-9 -10 -2 471.148 473.804 20.291 9.300 o
-9 -10 -1 45.968 27.547 10.658 67.226 o
-9 -9 -9 234.327 219.583 20.737 14.637 o
-9 -9 -8 305.773 328.945 18.164 14.348 o
-9 -9 -7 1.255 -0.884 3.905 589.906 o
-9 -9 -6 384.821 380.986 15.131 14.156 o
-9 -9 -5 33.130 40.699 7.082 129.342 o
-9 -9 -4 9.579 9.362 4.876 317.946 o
-9 -9 -3 0.637 2.379 4.518 439.592 o
-9 -9 -2 132.843 116.110 10.208 46.819 o
-9 -9 -1 128.888 116.385 10.032 48.255 o
-9 -8 -10 156.803 151.108 17.843 21.126 o
-9 -8 -9 181.952 164.780 27.803 10.124 o
-9 -8 -8 107.318 105.662 11.418 45.027 o
-9 -8 -7 27.440 25.062 4.978 228.813 o
-9 -8 -6 26.057 29.193 6.840 147.596 o
-9 -8 -5 287.102 265.609 12.337 22.031 o
-9 -8 -4 71.023 68.637 6.902 99.079 o
-9 -8 -3 7.294 18.636 5.187 279.249 o
-9 -8 -2 21.696 18.525 5.776 204.296 o
-9 -8 -1 31.219 14.952 6.500 161.345 o
-9 -7 -11 74.631 59.264 12.527 45.819 o
-9 -7 -10 37.665 32.480 7.675 114.999 o
-9 -7 -9 63.793 71.287 9.512 69.465 o
-9 -7 -8 2.255 -0.845 3.421 739.170 o
-9 -7 -7 227.087 208.116 11.164 29.205 o
-9 -7 -6 28.822 27.329 5.068 218.239 o
-9 -7 -5 711.030 696.739 20.596 6.017 o
-9 -7 -4 37.438 38.778 5.454 175.776 o
-9 -7 -3 31.989 32.780 5.149 202.303 o
-9 -7 -2 173.876 149.004 17.405 21.347 o
-9 -7 -1 124.214 98.489 8.865 57.277 o
-9 -6 -11 5.888 4.369 8.658 118.864 o
-9 -6 -10 401.434 447.876 34.066 5.639 o
-9 -6 -9 245.428 233.062 15.074 20.824 o
-9 -6 -8 188.791 192.693 12.706 29.065 o
-9 -6 -7 246.585 250.077 10.411 27.717 o
-9 -6 -6 88.062 94.713 6.574 88.383 o
-9 -6 -5 151.170 159.840 8.354 48.961 o
-9 -6 -4 781.542 690.171 21.766 5.421 o
-9 -6 -3 215.961 214.253 11.403 29.297 o
-9 -6 -2 86.959 75.524 5.830 103.100 o
-9 -6 -1 361.864 325.930 11.314 18.565 o
-9 -5 -12 116.812 118.375 11.282 43.712 o
-9 -5 -11 45.532 47.677 7.748 104.546 o
-9 -5 -10 53.145 51.504 7.853 97.868 o
-9 -5 -9 7.915 4.082 4.435 396.150 o
-9 -5 -8 259.705 276.835 12.285 23.178 o
-9 -5 -7 21.242 18.496 4.018 331.616 o
-9 -5 -6 361.731 341.025 12.074 17.660 o
-9 -5 -5 98.052 85.582 6.909 82.496 o
-9 -5 -4 129.208 134.089 7.496 60.473 o
-9 -5 -3 489.894 463.854 13.851 11.666 o
-9 -5 -2 7.960 5.290 2.910 745.268 o
-9 -5 -1 603.397 626.945 15.033 8.370 o
-9 -4 -12 237.769 232.215 23.027 12.501 o
-9 -4 -11 35.890 41.220 7.376 120.004 o
-9 -4 -10 82.627 77.579 9.332 65.615 o
-9 -4 -9 356.578 345.574 29.461 7.451 o
-9 -4 -8 117.610 113.711 8.125 61.851 o
-9 -4 -7 388.932 414.846 19.391 11.228 o
-9 -4 -6 321.911 327.532 13.373 18.171 o
-9 -4 -5 43.204 30.908 5.834 160.301 o
-9 -4 -4 0.645 7.700 2.984 876.834 o
-9 -4 -3 181.011 184.988 8.599 41.580 o
-9 -4 -2 462.319 448.834 15.072 11.808 o
-9 -4 -1 13.344 10.781 2.536 684.260 o
-9 -3 -13 25.583 24.237 10.316 76.471 o
-9 -3 -12 37.214 42.027 11.816 56.784 o
-9 -3 -11 77.042 63.705 14.145 37.404 o
-9 -3 -10 82.205 74.263 9.550 64.240 o
-9 -3 -9 35.264 36.035 7.079 129.574 o
-9 -3 -8 488.506 537.495 17.534 9.684 o
-9 -3 -7 31.154 22.101 4.158 272.957 o
-9 -3 -6 1123.750 1059.560 30.744 2.789 o
-9 -3 -5 275.905 271.551 12.055 22.808 o
-9 -3 -4 39.451 42.139 5.212 178.998 o
-9 -3 -3 104.502 97.747 8.327 65.763 o
-9 -3 -2 227.632 247.968 10.815 28.409 o
-9 -3 -1 91.143 99.042 6.781 83.879 o
-9 -2 -13 17.693 17.997 5.473 230.383 o
-9 -2 -12 35.296 44.211 11.605 58.689 o
-9 -2 -11 324.600 321.080 18.163 14.031 o
-9 -2 -10 29.143 22.477 8.184 111.823 o
-9 -2 -9 31.890 28.756 9.158 90.631 o
-9 -2 -8 65.982 64.939 6.366 111.687 o
-9 -2 -7 10.048 7.793 3.239 588.622 o
-9 -2 -6 56.578 50.374 5.590 141.230 o
-9 -2 -5 66.901 78.209 15.264 33.194 o
-9 -2 -4 103.482 104.553 16.658 26.446 o
-9 -2 -3 1304.930 1280.530 33.173 2.173 o
-9 -2 -2 281.569 307.054 12.086 21.627 o
-9 -2 -1 1221.600 1216.240 26.427 2.619 o
-9 -1 -14 239.364 252.578 34.869 6.450 o
-9 -1 -13 214.539 219.418 18.369 17.665 o
-9 -1 -12 107.223 94.062 9.865 54.706 o
-9 -1 -11 194.861 186.709 15.341 23.460 o
-9 -1 -10 273.758 262.864 15.914 18.227 o
-9 -1 -9 54.665 52.074 10.695 62.512 o
-9 -1 -8 160.330 162.017 9.450 42.966 o
-9 -1 -7 253.555 297.081 17.052 17.061 o
-9 -1 -6 167.791 180.088 11.204 35.197 o
-9 -1 -5 809.252 878.281 40.132 3.011 o
-9 -1 -4 344.917 377.981 24.948 9.239 o
-9 -1 -3 213.857 203.530 17.974 18.405 o
-9 -1 -2 33.447 58.260 6.773 129.781 o
-9 -1 -1 522.630 543.460 21.078 8.096 o
-8 -13 -4 70.769 72.870 12.421 46.080 o
-8 -13 -3 117.953 111.898 10.740 46.610 o
-8 -13 -2 24.706 35.432 7.049 139.485 o
-8 -13 -1 8.548 8.702 5.474 266.238 o
-8 -12 -7 33.958 35.369 9.079 89.861 o
-8 -12 -6 146.745 143.553 11.637 37.575 o
-8 -12 -5 136.779 122.463 11.079 41.957 o
-8 -12 -4 16.429 12.784 6.369 188.057 o
-8 -12 -3 0.803 2.474 4.605 421.985 o
-8 -12 -2 261.043 262.185 15.217 19.502 o
-8 -12 -1 41.612 25.988 5.999 159.841 o
-8 -11 -9 158.693 160.766 16.737 22.884 o
-8 -11 -8 23.196 18.588 5.870 196.870 o
-8 -11 -7 244.514 230.683 14.487 21.757 o
-8 -11 -6 5.376 1.729 4.542 403.890 o
-8 -11 -5 384.414 468.464 20.361 10.417 o
-8 -11 -4 166.659 174.992 12.486 31.836 o
-8 -11 -3 267.518 257.620 14.719 19.974 o
-8 -11 -2 72.097 65.650 9.671 66.570 o
-8 -11 -1 139.329 133.115 11.632 38.874 o
-8 -10 -11 153.333 117.113 10.644 42.082 o
-8 -10 -10 3.115 5.417 5.108 328.035 o
-8 -10 -9 136.813 119.123 11.061 42.225 o
-8 -10 -8 334.301 349.615 14.073 16.761 o
-8 -10 -7 521.189 503.798 16.976 9.662 o
-8 -10 -6 113.750 100.291 7.843 66.607 o
-8 -10 -5 17.502 25.081 5.861 201.604 o
-8 -10 -4 280.332 247.607 14.174 20.362 o
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;
_iucr_refine_instructions_details
;
TITL aks95_a.res in P2(1)2(1)2(1)
REM Old TITL AKS95 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.089, Rweak 0.028, Alpha 0.003, Orientation as input
REM Flack x = 0.086 ( 0.020 ) from Parsons' quotients
REM Formula found by SHELXT: C24 N3 O5 S
CELL 0.71073 9.2225 15.1104 18.1484 90 90 90
ZERR 4 0.0002 0.0003 0.0004 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 100 128 8 20 4
L.S. 10
PLAN 20
SIZE 0.2 0.15 0.1
BOND $H
FMAP 2
list 4
ACTA
SHEL 999 0.8
WGHT 0.038167 0.551274
FVAR 0.616435
REM
REM
REM
S1 5 0.68374 0.66571 0.17588 11.00000 0.01458 0.01441 0.01535 =
0.00000 -0.00003 0.00097
O1 4 0.83340 0.44803 0.21805 11.00000 0.01573 0.01530 0.03291 =
0.00444 0.00086 0.00263
O3 4 0.78737 0.71388 0.13187 11.00000 0.01981 0.02062 0.01960 =
0.00168 0.00416 -0.00014
O2 4 0.95018 0.57998 0.22375 11.00000 0.01867 0.02117 0.03893 =
0.00210 -0.00571 -0.00211
O5 4 0.29986 0.99972 0.09605 11.00000 0.03308 0.03017 0.02360 =
0.00030 -0.00359 0.01605
O4 4 0.48788 0.92640 0.04754 11.00000 0.04009 0.04154 0.01702 =
0.00864 0.00605 0.02336
N1 3 0.70549 0.56618 0.19239 11.00000 0.01593 0.01409 0.02092 =
-0.00086 -0.00013 0.00030
N2 3 0.52526 0.69277 0.06092 11.00000 0.02843 0.02568 0.01925 =
0.00231 -0.00638 -0.00165
C6 1 0.58433 0.81083 0.25438 11.00000 0.01432 0.01616 0.01820 =
0.00187 0.00063 -0.00181
C9 1 0.40213 0.95047 0.10299 11.00000 0.02344 0.01518 0.02047 =
-0.00033 -0.00205 0.00249
C5 1 0.54692 0.85106 0.32093 11.00000 0.01768 0.01472 0.02001 =
0.00019 0.00240 0.00195
AFIX 43
H5 2 0.50246 0.90629 0.31977 11.00000 -1.20000
AFIX 0
C7 1 0.55109 0.85386 0.18349 11.00000 0.01794 0.01478 0.01564 =
-0.00088 0.00065 -0.00112
AFIX 43
H7 2 0.60966 0.84100 0.14318 11.00000 -1.20000
AFIX 0
C21 1 0.84204 0.53661 0.21294 11.00000 0.01817 0.01681 0.01660 =
-0.00091 0.00205 0.00244
C1 1 0.64966 0.72637 0.25805 11.00000 0.01370 0.01610 0.01728 =
-0.00156 0.00090 -0.00033
C15 1 0.50951 0.66608 0.13007 11.00000 0.01860 0.01303 0.02120 =
-0.00139 -0.00421 0.00173
C16 1 0.37929 0.64417 0.16444 11.00000 0.01920 0.01454 0.02546 =
-0.00363 -0.00128 0.00010
C8 1 0.44222 0.90985 0.17420 11.00000 0.02216 0.02120 0.01553 =
-0.00039 0.00126 0.00389
AFIX 43
H8 2 0.38718 0.92465 0.21533 11.00000 -1.20000
AFIX 0
C4 1 0.57365 0.81162 0.38927 11.00000 0.01590 0.02039 0.01722 =
0.00049 0.00249 0.00005
C2 1 0.67796 0.68643 0.32493 11.00000 0.01957 0.01492 0.01916 =
0.00207 -0.00083 0.00154
AFIX 43
H2 2 0.72118 0.63086 0.32645 11.00000 -1.20000
AFIX 0
C20 1 0.36369 0.61144 0.24225 11.00000 0.02151 0.02990 0.02721 =
0.00332 0.00083 -0.00263
AFIX 137
H20a 2 0.43921 0.56956 0.25272 11.00000 -1.50000
H20b 2 0.37090 0.66047 0.27569 11.00000 -1.50000
H20c 2 0.27099 0.58339 0.24803 11.00000 -1.50000
AFIX 0
C3 1 0.64173 0.72947 0.38980 11.00000 0.02325 0.02101 0.01580 =
0.00318 -0.00004 0.00097
AFIX 43
H3 2 0.66340 0.70285 0.43467 11.00000 -1.20000
AFIX 0
C22 1 0.96156 0.39361 0.23763 11.00000 0.01970 0.02269 0.03301 =
0.00728 0.00268 0.00891
C17 1 0.25573 0.65607 0.12066 11.00000 0.02013 0.02476 0.03594 =
-0.00433 -0.00634 0.00184
AFIX 43
H17 2 0.16449 0.64427 0.14015 11.00000 -1.20000
AFIX 0
C18 1 0.26823 0.68508 0.04902 11.00000 0.03047 0.02856 0.03670 =
-0.00143 -0.01562 0.00243
AFIX 43
H18 2 0.18610 0.69355 0.02014 11.00000 -1.20000
AFIX 0
C11 1 0.53013 0.86052 0.45997 11.00000 0.03306 0.02416 0.01728 =
0.00006 0.00596 0.00328
C19 1 0.40442 0.70136 0.02078 11.00000 0.03788 0.03304 0.02516 =
0.00477 -0.01294 -0.00159
AFIX 43
H19 2 0.41260 0.71903 -0.02813 11.00000 -1.20000
AFIX 0
C23 1 1.07328 0.40077 0.17725 11.00000 0.02557 0.02916 0.03569 =
0.00679 0.00568 0.01117
AFIX 137
H23a 2 1.02924 0.38668 0.13078 11.00000 -1.50000
H23b 2 1.11065 0.46004 0.17571 11.00000 -1.50000
H23c 2 1.15109 0.36016 0.18682 11.00000 -1.50000
AFIX 0
C25 1 1.02055 0.41989 0.31249 11.00000 0.03618 0.04601 0.03087 =
0.00991 -0.00191 0.01492
AFIX 137
H25a 2 1.06248 0.47793 0.30952 11.00000 -1.50000
H25b 2 0.94315 0.42015 0.34786 11.00000 -1.50000
H25c 2 1.09338 0.37822 0.32750 11.00000 -1.50000
AFIX 0
C24 1 0.89702 0.30097 0.23903 11.00000 0.03397 0.02153 0.06750 =
0.01426 0.00637 0.00666
AFIX 137
H24a 2 0.82185 0.29827 0.27556 11.00000 -1.50000
H24b 2 0.85702 0.28730 0.19154 11.00000 -1.50000
H24c 2 0.97144 0.25890 0.25088 11.00000 -1.50000
AFIX 0
C10 1 0.44473 0.96079 -0.02344 11.00000 0.07126 0.06762 0.01970 =
0.01375 0.00782 0.03925
AFIX 137
H10a 2 0.51283 0.94193 -0.06024 11.00000 -1.50000
H10b 2 0.34995 0.93901 -0.03565 11.00000 -1.50000
H10c 2 0.44276 1.02427 -0.02159 11.00000 -1.50000
AFIX 0
C12 1 0.53361 0.80073 0.52722 11.00000 0.07734 0.04824 0.02068 =
0.00609 0.01451 0.02691
AFIX 137
H12a 2 0.47197 0.75049 0.51902 11.00000 -1.50000
H12b 2 0.63113 0.78096 0.53567 11.00000 -1.50000
H12c 2 0.49993 0.83295 0.56948 11.00000 -1.50000
AFIX 0
C13 1 0.37419 0.89446 0.45278 11.00000 0.05630 0.07001 0.02698 =
0.00042 0.01112 0.03480
AFIX 137
H13a 2 0.37043 0.94007 0.41601 11.00000 -1.50000
H13b 2 0.31176 0.84655 0.43860 11.00000 -1.50000
H13c 2 0.34268 0.91801 0.49923 11.00000 -1.50000
AFIX 0
C14 1 0.63131 0.93868 0.47095 11.00000 0.09232 0.06556 0.04356 =
-0.03338 0.02636 -0.04011
AFIX 137
H14a 2 0.72779 0.91752 0.48012 11.00000 -1.50000
H14b 2 0.63116 0.97479 0.42743 11.00000 -1.50000
H14c 2 0.59897 0.97314 0.51224 11.00000 -1.50000
AFIX 0
HKLF 4
END
Q1 1 0.7 0.895833 0.5 11 0.05 0.36
Q2 1 0.466667 0.9375 0.45 11 0.05 0.24
Q3 1 0.6 0.666667 0.15 11 0.05 0.23
Q4 1 0.7 0.708333 0.216667 11 0.05 0.18
Q5 1 0.7 0.604167 0.183333 11 0.05 0.17
Q6 1 0.566667 0.833333 0.283333 11 0.05 0.16
Q7 1 0.566667 0.833333 0.216667 11 0.05 0.16
Q8 1 0.633333 0.770833 0.25 11 0.05 0.15
Q9 1 0.633333 0.708333 0.3 11 0.05 0.14
Q10 1 0.533333 0.833333 0.566667 11 0.05 0.14
Q11 1 0.666667 0.541667 0.2 11 0.05 0.14
Q12 1 0.433333 0.916667 0.133333 11 0.05 0.14
Q13 1 0.4 0.625 0.2 11 0.05 0.14
Q14 1 0.433333 0.645833 0.15 11 0.05 0.13
Q15 1 0.966667 0.416667 0.283333 11 0.05 0.13
Q16 1 0.533333 0.833333 0.416667 11 0.05 0.12
Q17 1 0.3 0.645833 0.15 11 0.05 0.12
Q18 1 0.266667 0.666667 0.083333 11 0.05 0.12
Q19 1 0.633333 0.770833 0.383333 11 0.05 0.12
Q20 1 0.533333 0.916667 0.183333 11 0.05 0.12
REM The information below was added by Olex2.
REM
REM R1 = 0.0298 for 4889 Fo > 4sig(Fo) and 0.0313 for all 5105 data
REM 306 parameters refined using 0 restraints
REM Highest difference peak 0.3602, deepest hole -0.2472
REM Mean Shift 0.0000, Max Shift 0.0000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0313
REM R1_gt = 0.0298
REM wR_ref = 0.0749
REM GOOF = 1.0345
REM Shift_max = 0.0000
REM Shift_mean = 0.0000
REM Reflections_all = 5105
REM Reflections_gt = 4889
REM Parameters = 306
REM Hole = -0.2472
REM Peak = 0.3602
REM Flack = 0.04(5)
;
loop_
_atom_type.symbol
_atom_type.scat_dispersion_real
_atom_type.scat_dispersion_imag
_atom_type.scat_Cromer_Mann_a1
_atom_type.scat_Cromer_Mann_a2
_atom_type.scat_Cromer_Mann_a3
_atom_type.scat_Cromer_Mann_a4
_atom_type.scat_Cromer_Mann_b1
_atom_type.scat_Cromer_Mann_b2
_atom_type.scat_Cromer_Mann_b3
_atom_type.scat_Cromer_Mann_b4
_atom_type.scat_Cromer_Mann_c
_atom_type.scat_source
_atom_type.scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 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 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.741