#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:33:31 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296663 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160173.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7160173
loop_
_publ_author_name
'Thunga, Sanjeeva'
'Singh, Neetika'
'Inapanuri, Madhu'
'Kokatla, Hari Prasad'
_publ_section_title
;
Rongalite induced metal-free C(sp2)-H functionalization of
indoles: direct access to 3-(sulfonylmethyl) indoles.
;
_journal_issue 44
_journal_name_full 'Organic & biomolecular chemistry'
_journal_page_first 8787
_journal_page_last 8792
_journal_paper_doi 10.1039/d4ob01356e
_journal_volume 22
_journal_year 2024
_chemical_formula_moiety '0.5(C25 H25 N O2 S)'
_chemical_formula_sum 'C12.5 H12.5 N0.5 O S0.5'
_chemical_formula_weight 201.77
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_Int_Tables_number 2
_atom_sites_solution_primary dual
_audit_creation_date 2019-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-02 deposited with the CCDC. 2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha 96.935(2)
_cell_angle_beta 104.121(2)
_cell_angle_gamma 102.127(2)
_cell_formula_units_Z 4
_cell_length_a 8.4532(2)
_cell_length_b 10.3709(2)
_cell_length_c 12.4478(3)
_cell_measurement_reflns_used 7200
_cell_measurement_temperature 93(2)
_cell_measurement_theta_max 79.1210
_cell_measurement_theta_min 5.5970
_cell_volume 1017.51(4)
_computing_cell_refinement 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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)'
_diffrn_ambient_temperature 93(2)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9650
_diffrn_measured_fraction_theta_max 0.9650
_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 -73.00 -48.00 0.50 1.00 -- 0.00 -19.00-150.00 50
2 \w 27.00 68.00 0.50 1.00 -- 0.00 37.00-180.00 82
3 \w -35.00 21.00 0.50 1.00 -- 0.00 -19.00-150.00 112
4 \w -75.00 17.00 0.50 1.00 -- 0.00 -37.00 150.00 184
5 \w -11.00 88.00 0.50 1.00 -- 0.00 37.00 120.00 198
6 \w 44.00 94.00 0.50 3.08 -- 107.20 -30.00 -90.00 100
7 \w 81.00 195.00 0.50 3.08 -- 107.20 15.00 30.00 228
8 \w 46.00 77.00 0.50 3.08 -- 107.20 -45.00 150.00 62
9 \w 28.00 140.00 0.50 3.08 -- 107.20 -82.00 120.00 224
10 \w 38.00 135.00 0.50 3.08 -- 107.20 -15.00 -30.00 194
11 \w 102.00 186.00 0.50 3.08 -- 107.20 15.00 -60.00 168
12 \w 39.00 140.00 0.50 3.08 -- 107.20 -82.00 -90.00 202
13 \w 92.00 196.00 0.50 3.08 -- 107.20 30.00 -30.00 208
14 \w 48.00 82.00 0.50 3.08 -- 107.20 -61.00 30.00 68
15 \w 46.00 100.00 0.50 3.08 -- 107.20 -82.00 -60.00 108
16 \w 81.00 117.00 0.50 3.08 -- 107.20 -45.00 150.00 72
17 \w 39.00 127.00 0.50 3.08 -- 107.20 -61.00 120.00 176
18 \w 92.00 136.00 0.50 3.08 -- 107.20 -82.00 0.00 88
19 \w 89.00 114.00 0.50 3.08 -- 107.20 -82.00-180.00 50
20 \w 43.00 110.00 0.50 3.08 -- 107.20 -82.00 30.00 134
21 \w 46.00 71.00 0.50 3.08 -- 107.20 -82.00 0.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0195809000
_diffrn_orient_matrix_UB_12 0.0035947000
_diffrn_orient_matrix_UB_13 0.1200925000
_diffrn_orient_matrix_UB_21 0.1702189000
_diffrn_orient_matrix_UB_22 0.1048807000
_diffrn_orient_matrix_UB_23 0.0468220000
_diffrn_orient_matrix_UB_31 -0.0910414000
_diffrn_orient_matrix_UB_32 0.1133908000
_diffrn_orient_matrix_UB_33 -0.0150395000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0274
_diffrn_reflns_av_unetI/netI 0.0331
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 10533
_diffrn_reflns_theta_full 79.7486
_diffrn_reflns_theta_max 79.75
_diffrn_reflns_theta_min 3.72
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 1.576
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.69174
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.3171
_exptl_crystal_description block
_exptl_crystal_F_000 429.8533
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.3287
_refine_diff_density_min -0.4861
_refine_diff_density_rms 0.0542
_refine_ls_d_res_high 0.7834
_refine_ls_d_res_low 11.8714
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref 1.0231
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_constraints 41
_refine_ls_number_parameters 267
_refine_ls_number_reflns 4274
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.0231
_refine_ls_R_factor_all 0.0411
_refine_ls_R_factor_gt 0.0390
_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^)+(0.0512P)^2^+0.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1050
_refine_ls_wR_factor_ref 0.1065
_reflns_Friedel_coverage 0.0
_reflns_limit_h_max 10
_reflns_limit_h_min -10
_reflns_limit_k_max 13
_reflns_limit_k_min -13
_reflns_limit_l_max 15
_reflns_limit_l_min 0
_reflns_number_gt 3973
_reflns_number_total 4274
_reflns_threshold_expression I>=2u(I)
_iucr_refine_instructions_details
;
TITL exp_538_23_a.res in P-1
REM Old TITL exp_538_23_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.090, Rweak 0.006, Alpha 0.051, Orientation as input
REM Formula found by SHELXT: C25 N O2 S
CELL 1.54184 8.4532 10.3709 12.4478 96.935 104.121 102.127
ZERR 4 0.0002 0.0002 0.0003 0.002 0.002 0.002
LATT 1
SFAC C H N O S
UNIT 50 50 2 4 2
L.S. 10
PLAN 20
BOND $H
FMAP 2
list 4
ABIN
ACTA
EXTI 0.001167
WGHT 0.051217 0.650038
FVAR 0.776799
REM
REM
REM
S001 5 0.51274 0.68738 0.78149 11.00000 0.02016 0.01649 0.01962 =
0.00269 0.00628 0.00694
O002 4 0.42647 0.62369 0.85519 11.00000 0.02544 0.02432 0.02509 =
0.00395 0.01207 0.00612
O003 4 0.44877 0.79276 0.73505 11.00000 0.02468 0.02010 0.02935 =
0.00400 0.00447 0.01094
N004 3 0.11964 0.35301 0.46904 11.00000 0.01749 0.02061 0.01956 =
0.00350 0.00405 0.00381
C005 1 0.34880 0.50598 0.58246 11.00000 0.02038 0.01736 0.01805 =
0.00358 0.00674 0.00792
C006 1 0.27691 0.27290 0.63542 11.00000 0.01705 0.01808 0.02184 =
0.00456 0.00649 0.00390
C007 1 0.24897 0.37706 0.56745 11.00000 0.01892 0.01919 0.01782 =
0.00283 0.00606 0.00660
C008 1 0.13507 0.46562 0.41976 11.00000 0.02120 0.02487 0.01881 =
0.00542 0.00807 0.00984
C009 1 0.73288 0.74662 0.85142 11.00000 0.02249 0.01825 0.01772 =
0.00133 0.00628 0.00711
C00A 1 0.82972 0.86103 0.82448 11.00000 0.02545 0.02002 0.01876 =
0.00201 0.00769 0.00622
C00B 1 0.28196 0.14592 0.58482 11.00000 0.02241 0.01857 0.02338 =
0.00173 0.00700 0.00394
AFIX 43
H00B 2 0.25767 0.12466 0.50684 11.00000 -1.20000
AFIX 0
C00C 1 0.27828 0.56332 0.48844 11.00000 0.02139 0.02055 0.01945 =
0.00513 0.00829 0.01006
C00D 1 0.81043 0.67081 0.92564 11.00000 0.02836 0.02217 0.01731 =
0.00275 0.00760 0.01029
C00E 1 0.30999 0.30123 0.75241 11.00000 0.02514 0.01819 0.02245 =
0.00362 0.00692 0.00743
AFIX 43
H00E 2 0.30613 0.38454 0.78736 11.00000 -1.20000
AFIX 0
C00F 1 1.00254 0.89814 0.87577 11.00000 0.02535 0.02305 0.02317 =
0.00136 0.00963 0.00439
AFIX 43
H00F 2 1.06694 0.97395 0.85979 11.00000 -1.20000
AFIX 0
C00G 1 0.35586 0.08134 0.76613 11.00000 0.02386 0.02023 0.03085 =
0.01031 0.00730 0.00669
AFIX 43
H00G 2 0.38268 0.01798 0.80962 11.00000 -1.20000
AFIX 0
C00H 1 0.32278 0.05185 0.64979 11.00000 0.02156 0.01585 0.03211 =
0.00255 0.00769 0.00431
AFIX 43
H00H 2 0.32803 -0.03128 0.61538 11.00000 -1.20000
AFIX 0
C00I 1 1.08272 0.82675 0.94974 11.00000 0.02322 0.02985 0.02078 =
-0.00252 0.00564 0.00745
C00J 1 0.03750 0.48646 0.31813 11.00000 0.02356 0.03682 0.01994 =
0.00712 0.00611 0.01151
AFIX 43
H00J 2 -0.05827 0.42217 0.27468 11.00000 -1.20000
AFIX 0
C00K 1 0.98420 0.71462 0.97349 11.00000 0.02712 0.02755 0.01926 =
0.00348 0.00379 0.01279
AFIX 43
H00K 2 1.03644 0.66657 1.02356 11.00000 -1.20000
AFIX 0
C00L 1 0.32904 0.68460 0.45267 11.00000 0.02629 0.02280 0.02496 =
0.00825 0.01135 0.01089
AFIX 43
H00L 2 0.42358 0.75002 0.49624 11.00000 -1.20000
AFIX 0
C00M 1 0.51513 0.56488 0.66679 11.00000 0.02058 0.01638 0.02052 =
0.00321 0.00697 0.00714
AFIX 23
H00a 2 0.59388 0.60658 0.62850 11.00000 -1.20000
H00c 2 0.55664 0.49288 0.69756 11.00000 -1.20000
AFIX 0
C00N 1 0.76170 0.94597 0.74266 11.00000 0.03051 0.02576 0.02896 =
0.01130 0.01098 0.00708
AFIX 137
H00d 2 0.69964 0.88963 0.67145 11.00000 -1.50000
H00i 2 0.68868 0.99108 0.77186 11.00000 -1.50000
H00m 2 0.85359 1.01111 0.73274 11.00000 -1.50000
AFIX 0
C00O 1 -0.02058 0.23410 0.42641 11.00000 0.01858 0.02518 0.02391 =
0.00032 0.00366 0.00317
AFIX 137
H00n 2 0.00254 0.17575 0.36940 11.00000 -1.50000
H00o 2 -0.03477 0.18787 0.48706 11.00000 -1.50000
H00p 2 -0.12178 0.26044 0.39472 11.00000 -1.50000
AFIX 0
C00P 1 0.23540 0.70474 0.35119 11.00000 0.03470 0.03161 0.02818 =
0.01547 0.01500 0.01689
AFIX 43
H00q 2 0.26881 0.78411 0.32588 11.00000 -1.20000
AFIX 0
C00Q 1 0.34875 0.20566 0.81720 11.00000 0.02924 0.02446 0.02361 =
0.00857 0.00802 0.00888
AFIX 43
H00r 2 0.36995 0.22531 0.89504 11.00000 -1.20000
AFIX 0
C00R 1 0.09055 0.60747 0.28547 11.00000 0.03213 0.04261 0.02274 =
0.01442 0.00949 0.01936
AFIX 43
H00s 2 0.02888 0.62489 0.21841 11.00000 -1.20000
AFIX 0
C00S 1 0.72094 0.54423 0.95606 11.00000 0.03300 0.02400 0.02691 =
0.00968 0.00751 0.01051
AFIX 137
H00t 2 0.63731 0.56341 0.99133 11.00000 -1.50000
H00u 2 0.66759 0.47775 0.88904 11.00000 -1.50000
H00v 2 0.80105 0.51107 1.00714 11.00000 -1.50000
AFIX 0
C00T 1 1.27069 0.86635 0.99857 11.00000 0.02470 0.04271 0.03054 =
-0.00244 0.00330 0.00844
AFIX 137
H00w 2 1.32280 0.83241 0.94460 11.00000 -1.50000
H00x 2 1.30903 0.96235 1.01658 11.00000 -1.50000
H00y 2 1.30035 0.82960 1.06571 11.00000 -1.50000
AFIX 0
HKLF 4
END
Q1 1 0.518519 0.611111 0.725 11 0.05 0.33
Q2 1 0.62963 0.722222 0.825 11 0.05 0.33
REM The information below was added by Olex2.
REM
REM R1 = 0.0390 for 3973 Fo > 4sig(Fo) and 0.0411 for all 4274 data
REM 267 parameters refined using 0 restraints
REM Highest difference peak 0.3287, deepest hole -0.4861
REM Mean Shift 0.0000, Max Shift 0.0000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0411
REM R1_gt = 0.0390
REM wR_ref = 0.1065
REM GOOF = 1.0231
REM Shift_max = 0.0000
REM Shift_mean = 0.0000
REM Reflections_all = 4274
REM Reflections_gt = 3973
REM Parameters = 267
REM Hole = -0.4861
REM Peak = 0.3287
REM Flack = n/a
;
_cod_data_source_file d4ob01356e2.cif
_cod_data_source_block exp_538_23
_cod_depositor_comments
'Adding full bibliography for 7160172--7160173.cif.'
_cod_database_code 7160173
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 71.98
_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 Secondary CH2 refined with riding coordinates:
C00M(H00a,H00c)
2.b Aromatic/amide H refined with riding coordinates:
C00K(H00K), C00F(H00F), C00L(H00L), C00P(H00q), C00R(H00s), C00J(H00J),
C00E(H00E), C00Q(H00r), C00G(H00G), C00H(H00H), C00B(H00B)
2.c Idealised Me refined as rotating group:
C00N(H00d,H00i,H00m), C00O(H00n,H00o,H00p), C00S(H00t,H00u,H00v), C00T(H00w,
H00x,H00y)
;
_iucr_refine_fcf_details
;
data_exp_538_23_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,-y,-z
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
_cell_length_a 8.4532(2)
_cell_length_b 10.3709(2)
_cell_length_c 12.4478(3)
_cell_angle_alpha 96.935(2)
_cell_angle_beta 104.121(2)
_cell_angle_gamma 102.127(2)
_cell_volume 1017.51(4)
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
-10 -2 6 1.453 2.784 0.696 409.059 o
-10 -1 1 0.857 1.375 0.663 635.471 o
-10 -1 2 49.227 39.575 2.519 16.894 o
-10 -1 3 31.958 36.824 2.569 22.505 o
-10 -1 4 330.512 294.821 12.048 1.142 o
-10 -1 5 187.103 171.144 5.176 3.049 o
-10 -1 6 30.858 22.009 5.212 14.917 o
-10 -1 7 43.345 31.305 2.072 20.825 o
-10 -1 8 172.269 70.399 3.331 4.672 o
-10 0 2 90.801 103.610 5.237 6.254 o
-10 0 3 40.877 38.497 2.884 18.305 o
-10 0 4 41.342 46.783 3.215 16.321 o
-10 0 5 9.119 9.415 0.995 98.039 o
-10 0 6 4.399 3.423 0.676 224.300 o
-10 0 7 101.712 65.577 10.068 3.908 o
-10 0 8 19.508 13.954 1.326 50.259 o
-10 1 1 9.872 9.115 1.044 93.106 o
-10 1 2 260.017 236.246 16.920 1.145 o
-10 1 3 1.248 1.574 0.621 554.809 o
-10 1 4 18.866 22.986 2.204 37.001 o
-10 1 5 17.331 16.964 1.306 51.676 o
-10 1 6 17.620 15.340 1.765 47.658 o
-10 1 7 11.925 11.185 1.036 78.285 o
-10 1 8 72.438 50.661 2.834 11.476 o
-10 1 9 1.820 0.729 0.464 604.853 o
-10 2 1 244.383 251.519 6.737 1.932 o
-10 2 2 0.218 0.449 0.597 1289.230 o
-10 2 3 5.289 4.249 0.637 191.822 o
-10 2 4 285.767 231.369 19.754 0.939 o
-10 2 5 27.407 19.469 1.351 36.167 o
-10 2 6 150.658 140.339 21.362 1.160 o
-10 2 7 61.291 46.412 2.502 13.794 o
-10 2 8 0.416 -0.050 0.530 1530.050 o
-10 3 1 172.331 165.900 5.174 3.310 o
-10 3 2 118.240 127.916 4.281 5.194 o
-10 3 3 0.082 0.131 0.672 1369.570 o
-10 3 4 38.822 42.989 2.701 18.746 o
-10 3 5 20.311 20.782 2.478 34.383 o
-10 3 6 25.191 20.791 6.405 12.193 o
-10 3 7 10.089 9.595 1.226 85.992 o
-10 3 8 5.457 3.745 0.646 193.159 o
-10 4 1 5.306 6.493 0.813 158.641 o
-10 4 2 16.508 15.838 1.219 55.325 o
-10 4 3 36.609 40.400 2.560 20.216 o
-10 4 4 44.490 43.397 2.059 18.572 o
-10 4 5 139.640 154.205 6.728 3.641 o
-10 4 6 6.111 4.095 1.019 151.834 o
-10 4 7 76.897 77.658 3.861 8.755 o
-10 5 1 21.754 19.191 1.525 41.410 o
-10 5 2 98.880 107.037 3.644 6.638 o
-10 5 3 19.675 21.120 1.906 39.679 o
-10 5 4 97.447 109.266 3.936 6.518 o
-10 5 5 51.661 51.871 2.933 14.341 o
-10 5 6 64.053 59.686 4.325 10.136 o
-10 5 7 7.579 6.463 0.928 124.296 o
-10 6 1 36.929 37.785 2.320 21.270 o
-10 6 2 170.752 147.294 6.281 3.285 o
-10 6 3 2.793 4.010 0.961 233.104 o
-10 6 4 133.630 133.713 4.224 4.659 o
-10 6 5 33.492 31.385 2.859 21.862 o
-10 6 6 129.988 86.822 3.812 5.663 o
-10 7 1 95.290 62.875 2.950 8.577 o
-10 7 2 140.619 101.240 4.475 4.853 o
-10 7 3 145.370 103.494 4.591 4.653 o
-10 7 4 1.610 1.160 0.530 571.402 o
-10 7 5 5.615 4.392 0.646 182.319 o
-9 -4 1 13.463 8.684 0.812 80.766 o
-9 -4 2 25.653 25.204 1.201 35.805 o
-9 -4 3 102.009 101.963 3.361 6.734 o
-9 -4 4 24.456 26.697 1.413 35.236 o
-9 -4 5 13.319 16.791 1.132 62.828 o
-9 -4 6 7.767 5.733 0.903 127.134 o
-9 -4 7 43.196 31.466 5.262 12.332 o
-9 -4 8 3.060 1.325 0.514 373.026 o
-9 -3 1 87.184 112.675 5.187 6.244 o
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8 3 3 17.444 18.511 1.624 46.963 o
8 3 4 4.819 3.464 0.580 218.972 o
8 4 0 36.684 38.020 4.284 15.320 o
8 4 1 25.677 23.321 3.894 21.420 o
8 4 3 15.921 11.965 0.945 64.538 o
8 5 0 43.294 45.954 8.336 6.836 o
8 5 1 243.948 218.622 8.667 1.890 o
9 -8 0 2.348 2.304 0.795 326.461 o
9 -8 1 103.086 77.774 3.530 7.245 o
9 -7 0 248.135 234.091 21.900 0.890 o
9 -7 1 115.195 123.534 5.535 4.910 o
9 -7 2 1.528 2.097 1.342 241.372 o
9 -7 3 6.661 6.629 1.110 124.527 o
9 -6 0 1.352 1.765 0.704 480.364 o
9 -6 1 10.320 8.565 1.154 89.301 o
9 -6 2 142.964 144.858 6.596 3.699 o
9 -6 3 20.701 20.675 2.353 35.118 o
9 -6 4 6.039 5.353 0.911 150.393 o
9 -5 0 41.064 50.765 2.521 17.527 o
9 -5 1 275.806 287.657 23.889 0.737 o
9 -5 2 208.925 230.429 14.915 1.455 o
9 -5 3 94.221 110.974 3.796 6.700 o
9 -5 4 3.984 3.828 0.696 229.234 o
9 -4 0 1.014 1.822 1.000 384.195 o
9 -4 1 109.795 123.138 4.471 5.497 o
9 -4 2 1.910 1.297 0.651 458.350 o
9 -4 3 13.774 15.297 0.990 65.401 o
9 -4 4 193.130 205.613 27.759 0.706 o
9 -3 0 99.671 94.909 5.502 5.922 o
9 -3 1 293.290 285.855 12.661 1.237 o
9 -3 2 120.297 127.388 3.626 5.337 o
9 -3 3 169.352 205.657 7.698 2.680 o
9 -3 4 0.098 0.514 0.804 882.604 o
9 -2 0 53.389 57.023 2.934 13.602 o
9 -2 1 217.333 242.696 7.913 2.058 o
9 -2 2 0.226 1.641 1.375 300.961 o
9 -2 3 52.162 64.954 3.447 12.410 o
9 -2 4 29.806 31.850 1.564 28.593 o
9 -1 0 199.173 224.240 10.076 2.021 o
9 -1 1 15.176 16.472 1.806 50.278 o
9 -1 2 169.155 203.333 6.518 2.879 o
9 -1 3 0.517 1.790 1.243 327.155 o
9 -1 4 47.923 52.219 2.734 15.371 o
9 0 0 6.867 9.418 1.012 113.962 o
9 0 1 159.356 167.595 5.286 3.492 o
9 0 2 0.156 1.094 0.845 692.781 o
9 0 3 19.430 24.593 1.773 39.093 o
9 0 4 14.966 15.628 1.094 60.507 o
9 1 0 22.336 23.839 1.424 38.722 o
9 1 1 53.648 56.071 2.220 14.681 o
9 1 2 25.649 22.598 4.400 19.108 o
9 1 3 11.819 12.595 0.994 76.586 o
9 2 0 95.210 91.394 15.230 2.234 o
9 2 1 44.179 36.693 5.195 12.043 o
9 3 0 7.019 6.181 0.845 135.449 o
10 -6 0 83.387 71.824 3.430 8.822 o
10 -5 0 9.245 9.761 1.193 90.809 o
10 -5 1 115.068 109.294 4.789 5.430 o
10 -4 0 133.447 100.660 4.425 5.096 o
10 -4 1 33.084 31.819 2.038 25.059 o
10 -4 2 13.911 9.496 0.845 76.720 o
10 -3 0 328.764 313.037 30.742 0.494 o
10 -3 2 7.485 3.613 0.580 158.230 o
10 -2 0 2.172 2.137 0.424 442.391 o
10 -2 1 2.266 1.061 0.580 453.576 o
10 -1 0 115.686 94.871 3.006 6.378 o
10 -1 1 0.226 0.066 0.315 3341.810 o
;
_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 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.699
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
S001 S 0.51274(4) 0.68738(3) 0.78149(3) 0.01830(12) Uani 1.000000 .
O002 O 0.42647(14) 0.62369(11) 0.85519(9) 0.0241(2) Uani 1.000000 .
O003 O 0.44877(14) 0.79276(11) 0.73505(10) 0.0245(2) Uani 1.000000 .
N004 N 0.11964(16) 0.35301(13) 0.46904(11) 0.0196(3) Uani 1.000000 .
C005 C 0.34880(18) 0.50598(14) 0.58246(12) 0.0178(3) Uani 1.000000 .
C006 C 0.27691(18) 0.27290(14) 0.63542(13) 0.0188(3) Uani 1.000000 .
C007 C 0.24897(18) 0.37706(14) 0.56745(12) 0.0182(3) Uani 1.000000 .
C008 C 0.13507(19) 0.46562(15) 0.41976(13) 0.0204(3) Uani 1.000000 .
C009 C 0.73288(19) 0.74662(15) 0.85142(12) 0.0192(3) Uani 1.000000 .
C00A C 0.8297(2) 0.86103(15) 0.82448(13) 0.0212(3) Uani 1.000000 .
C00B C 0.28196(19) 0.14592(15) 0.58482(13) 0.0217(3) Uani 1.000000 .
C00C C 0.27828(19) 0.56332(15) 0.48844(12) 0.0191(3) Uani 1.000000 .
C00D C 0.8104(2) 0.67081(15) 0.92564(13) 0.0218(3) Uani 1.000000 .
C00E C 0.3100(2) 0.30123(15) 0.75241(13) 0.0216(3) Uani 1.000000 .
C00F C 1.0025(2) 0.89814(16) 0.87577(13) 0.0238(3) Uani 1.000000 .
C00G C 0.3559(2) 0.08134(16) 0.76613(14) 0.0243(3) Uani 1.000000 .
C00H C 0.32278(19) 0.05185(15) 0.64979(14) 0.0233(3) Uani 1.000000 .
C00I C 1.0827(2) 0.82675(17) 0.94974(13) 0.0252(3) Uani 1.000000 .
C00J C 0.0375(2) 0.48646(18) 0.31813(13) 0.0260(3) Uani 1.000000 .
C00K C 0.9842(2) 0.71462(16) 0.97349(13) 0.0243(3) Uani 1.000000 .
C00L C 0.3290(2) 0.68460(16) 0.45267(13) 0.0228(3) Uani 1.000000 .
C00M C 0.51513(18) 0.56488(14) 0.66679(12) 0.0185(3) Uani 1.000000 .
C00N C 0.7617(2) 0.94597(17) 0.74266(14) 0.0273(3) Uani 1.000000 .
C00O C -0.02058(19) 0.23410(16) 0.42641(14) 0.0237(3) Uani 1.000000 .
C00P C 0.2354(2) 0.70474(18) 0.35119(14) 0.0281(4) Uani 1.000000 .
C00Q C 0.3487(2) 0.20566(16) 0.81720(14) 0.0249(3) Uani 1.000000 .
C00R C 0.0906(2) 0.60747(19) 0.28547(14) 0.0298(4) Uani 1.000000 .
C00S C 0.7209(2) 0.54423(16) 0.95606(14) 0.0271(3) Uani 1.000000 .
C00T C 1.2707(2) 0.8664(2) 0.99857(16) 0.0342(4) Uani 1.000000 .
H00K H 1.0364(2) 0.66657(16) 1.02356(13) 0.0291(4) Uiso 1.000000 R
H00F H 1.0669(2) 0.97395(16) 0.85979(13) 0.0286(4) Uiso 1.000000 R
H00L H 0.4236(2) 0.75002(16) 0.49624(13) 0.0274(4) Uiso 1.000000 R
H00q H 0.2688(2) 0.78411(18) 0.32588(14) 0.0338(4) Uiso 1.000000 R
H00s H 0.0289(2) 0.62489(19) 0.21841(14) 0.0358(4) Uiso 1.000000 R
H00J H -0.0583(2) 0.42217(18) 0.27468(13) 0.0312(4) Uiso 1.000000 R
H00E H 0.3061(2) 0.38454(15) 0.78736(13) 0.0259(4) Uiso 1.000000 R
H00r H 0.3699(2) 0.22531(16) 0.89504(14) 0.0299(4) Uiso 1.000000 R
H00G H 0.3827(2) 0.01798(16) 0.80962(14) 0.0292(4) Uiso 1.000000 R
H00H H 0.32803(19) -0.03128(15) 0.61538(14) 0.0280(4) Uiso 1.000000 R
H00B H 0.25767(19) 0.12466(15) 0.50684(13) 0.0260(4) Uiso 1.000000 R
H00a H 0.59388(18) 0.60658(14) 0.62850(12) 0.0223(3) Uiso 1.000000 R
H00c H 0.55664(18) 0.49288(14) 0.69756(12) 0.0223(3) Uiso 1.000000 R
H00d H 0.6996(14) 0.8896(2) 0.6714(4) 0.0410(5) Uiso 1.000000 GR
H00i H 0.6887(14) 0.9911(11) 0.7719(5) 0.0410(5) Uiso 1.000000 GR
H00m H 0.8536(2) 1.0111(9) 0.7327(9) 0.0410(5) Uiso 1.000000 GR
H00n H 0.0025(7) 0.1757(6) 0.3694(8) 0.0355(5) Uiso 1.000000 GR
H00o H -0.0348(10) 0.1879(7) 0.4871(2) 0.0355(5) Uiso 1.000000 GR
H00p H -0.1218(4) 0.26044(19) 0.3947(10) 0.0355(5) Uiso 1.000000 GR
H00t H 0.6373(12) 0.5634(3) 0.9913(10) 0.0407(5) Uiso 1.000000 GR
H00u H 0.6676(14) 0.4777(5) 0.8890(2) 0.0407(5) Uiso 1.000000 GR
H00v H 0.8010(3) 0.5111(8) 1.0071(9) 0.0407(5) Uiso 1.000000 GR
H00w H 1.3228(2) 0.8324(13) 0.9446(5) 0.0514(6) Uiso 1.000000 GR
H00x H 1.3090(3) 0.9624(2) 1.0166(12) 0.0514(6) Uiso 1.000000 GR
H00y H 1.3004(3) 0.8296(13) 1.0657(7) 0.0514(6) 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
S001 0.02016(19) 0.01649(18) 0.01962(19) 0.00694(13) 0.00628(14) 0.00269(13)
O002 0.0254(6) 0.0243(5) 0.0251(6) 0.0061(4) 0.0121(4) 0.0040(4)
O003 0.0247(6) 0.0201(5) 0.0293(6) 0.0109(4) 0.0045(4) 0.0040(4)
N004 0.0175(6) 0.0206(6) 0.0196(6) 0.0038(5) 0.0040(5) 0.0035(5)
C005 0.0204(7) 0.0174(7) 0.0181(7) 0.0079(5) 0.0067(5) 0.0036(5)
C006 0.0170(7) 0.0181(7) 0.0218(7) 0.0039(5) 0.0065(5) 0.0046(5)
C007 0.0189(7) 0.0192(7) 0.0178(7) 0.0066(5) 0.0061(5) 0.0028(5)
C008 0.0212(7) 0.0249(7) 0.0188(7) 0.0098(6) 0.0081(6) 0.0054(6)
C009 0.0225(7) 0.0183(7) 0.0177(7) 0.0071(6) 0.0063(6) 0.0013(5)
C00A 0.0255(8) 0.0200(7) 0.0188(7) 0.0062(6) 0.0077(6) 0.0020(6)
C00B 0.0224(7) 0.0186(7) 0.0234(7) 0.0039(6) 0.0070(6) 0.0017(6)
C00C 0.0214(7) 0.0206(7) 0.0194(7) 0.0101(6) 0.0083(6) 0.0051(6)
C00D 0.0284(8) 0.0222(7) 0.0173(7) 0.0103(6) 0.0076(6) 0.0027(6)
C00E 0.0251(8) 0.0182(7) 0.0224(7) 0.0074(6) 0.0069(6) 0.0036(6)
C00F 0.0254(8) 0.0230(7) 0.0232(7) 0.0044(6) 0.0096(6) 0.0014(6)
C00G 0.0239(8) 0.0202(7) 0.0308(8) 0.0067(6) 0.0073(6) 0.0103(6)
C00H 0.0216(7) 0.0158(7) 0.0321(8) 0.0043(6) 0.0077(6) 0.0026(6)
C00I 0.0232(8) 0.0298(8) 0.0208(7) 0.0074(6) 0.0056(6) -0.0025(6)
C00J 0.0236(8) 0.0368(9) 0.0199(7) 0.0115(7) 0.0061(6) 0.0071(6)
C00K 0.0271(8) 0.0275(8) 0.0193(7) 0.0128(6) 0.0038(6) 0.0035(6)
C00L 0.0263(8) 0.0228(7) 0.0250(8) 0.0109(6) 0.0114(6) 0.0083(6)
C00M 0.0206(7) 0.0164(6) 0.0205(7) 0.0071(5) 0.0070(6) 0.0032(5)
C00N 0.0305(8) 0.0258(8) 0.0290(8) 0.0071(7) 0.0110(7) 0.0113(7)
C00O 0.0186(7) 0.0252(8) 0.0239(7) 0.0032(6) 0.0037(6) 0.0003(6)
C00P 0.0347(9) 0.0316(8) 0.0282(8) 0.0169(7) 0.0150(7) 0.0155(7)
C00Q 0.0292(8) 0.0245(8) 0.0236(8) 0.0089(6) 0.0080(6) 0.0086(6)
C00R 0.0321(9) 0.0426(10) 0.0227(8) 0.0194(8) 0.0095(7) 0.0144(7)
C00S 0.0330(9) 0.0240(8) 0.0269(8) 0.0105(7) 0.0075(7) 0.0097(6)
C00T 0.0247(8) 0.0427(10) 0.0305(9) 0.0084(7) 0.0033(7) -0.0024(8)
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 0.01920 0.00962 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 0.33537 0.55136 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 0.05239 0.03377 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 0.03256 0.01839 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'
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
O003 S001 O002 116.15(7) . . ?
C009 S001 O002 109.76(7) . . ?
C009 S001 O003 110.24(7) . . ?
C00M S001 O002 110.50(7) . . ?
C00M S001 O003 108.20(7) . . ?
C00M S001 C009 100.89(7) . . ?
C008 N004 C007 109.01(12) . . ?
C00O N004 C007 126.95(13) . . ?
C00O N004 C008 123.85(13) . . ?
C00C C005 C007 106.93(13) . . ?
C00M C005 C007 126.66(13) . . ?
C00M C005 C00C 125.45(13) . . ?
C00B C006 C007 120.68(13) . . ?
C00E C006 C007 120.65(13) . . ?
C00E C006 C00B 118.54(14) . . ?
C005 C007 N004 109.10(13) . . ?
C006 C007 N004 122.62(13) . . ?
C006 C007 C005 128.05(13) . . ?
C00C C008 N004 107.94(13) . . ?
C00J C008 N004 129.49(15) . . ?
C00J C008 C00C 122.52(14) . . ?
C00A C009 S001 120.02(11) . . ?
C00D C009 S001 118.84(11) . . ?
C00D C009 C00A 120.89(14) . . ?
C00F C00A C009 117.89(14) . . ?
C00N C00A C009 125.50(14) . . ?
C00N C00A C00F 116.60(14) . . ?
C00H C00B C006 120.71(14) . . ?
H00B C00B C006 119.65(9) . . ?
H00B C00B C00H 119.65(9) . . ?
C008 C00C C005 107.02(13) . . ?
C00L C00C C005 133.53(15) . . ?
C00L C00C C008 119.29(14) . . ?
C00K C00D C009 117.67(14) . . ?
C00S C00D C009 125.32(14) . . ?
C00S C00D C00K 117.01(14) . . ?
C00Q C00E C006 120.50(14) . . ?
H00E C00E C006 119.75(9) . . ?
H00E C00E C00Q 119.75(9) . . ?
C00I C00F C00A 122.77(15) . . ?
H00F C00F C00A 118.62(9) . . ?
H00F C00F C00I 118.62(9) . . ?
C00Q C00G C00H 119.73(14) . . ?
H00G C00G C00H 120.13(9) . . ?
H00G C00G C00Q 120.13(9) . . ?
C00G C00H C00B 120.20(14) . . ?
H00H C00H C00B 119.90(9) . . ?
H00H C00H C00G 119.90(9) . . ?
C00K C00I C00F 117.78(15) . . ?
C00T C00I C00F 120.95(16) . . ?
C00T C00I C00K 121.22(16) . . ?
C00R C00J C008 116.73(16) . . ?
H00J C00J C008 121.64(10) . . ?
H00J C00J C00R 121.64(10) . . ?
C00I C00K C00D 122.97(15) . . ?
H00K C00K C00D 118.51(9) . . ?
H00K C00K C00I 118.51(9) . . ?
C00P C00L C00C 118.51(16) . . ?
H00L C00L C00C 120.75(9) . . ?
H00L C00L C00P 120.75(10) . . ?
C005 C00M S001 114.77(10) . . ?
H00a C00M S001 108.57(5) . . ?
H00a C00M C005 108.57(8) . . ?
H00c C00M S001 108.57(5) . . ?
H00c C00M C005 108.57(8) . . ?
H00c C00M H00a 107.6 . . ?
H00d C00N C00A 109.5 . . ?
H00i C00N C00A 109.5 . . ?
H00i C00N H00d 109.5 . . ?
H00m C00N C00A 109.5 . . ?
H00m C00N H00d 109.5 . . ?
H00m C00N H00i 109.5 . . ?
H00n C00O N004 109.5 . . ?
H00o C00O N004 109.5 . . ?
H00o C00O H00n 109.5 . . ?
H00p C00O N004 109.5 . . ?
H00p C00O H00n 109.5 . . ?
H00p C00O H00o 109.5 . . ?
C00R C00P C00L 121.26(15) . . ?
H00q C00P C00L 119.37(10) . . ?
H00q C00P C00R 119.37(9) . . ?
C00G C00Q C00E 120.30(15) . . ?
H00r C00Q C00E 119.85(9) . . ?
H00r C00Q C00G 119.85(9) . . ?
C00P C00R C00J 121.65(15) . . ?
H00s C00R C00J 119.17(10) . . ?
H00s C00R C00P 119.17(9) . . ?
H00t C00S C00D 109.5 . . ?
H00u C00S C00D 109.5 . . ?
H00u C00S H00t 109.5 . . ?
H00v C00S C00D 109.5 . . ?
H00v C00S H00t 109.5 . . ?
H00v C00S H00u 109.5 . . ?
H00w C00T C00I 109.5 . . ?
H00x C00T C00I 109.5 . . ?
H00x C00T H00w 109.5 . . ?
H00y C00T C00I 109.5 . . ?
H00y C00T H00w 109.5 . . ?
H00y C00T H00x 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S001 O002 1.4422(11) . ?
S001 O003 1.4385(11) . ?
S001 C009 1.7884(15) . ?
S001 C00M 1.7999(15) . ?
N004 C007 1.3842(19) . ?
N004 C008 1.3803(19) . ?
N004 C00O 1.4589(19) . ?
C005 C007 1.387(2) . ?
C005 C00C 1.434(2) . ?
C005 C00M 1.489(2) . ?
C006 C007 1.473(2) . ?
C006 C00B 1.403(2) . ?
C006 C00E 1.396(2) . ?
C008 C00C 1.412(2) . ?
C008 C00J 1.400(2) . ?
C009 C00A 1.419(2) . ?
C009 C00D 1.413(2) . ?
C00A C00F 1.393(2) . ?
C00A C00N 1.513(2) . ?
C00B C00H 1.386(2) . ?
C00B H00B 0.9300 . ?
C00C C00L 1.402(2) . ?
C00D C00K 1.395(2) . ?
C00D C00S 1.510(2) . ?
C00E C00Q 1.393(2) . ?
C00E H00E 0.9300 . ?
C00F C00I 1.388(2) . ?
C00F H00F 0.9300 . ?
C00G C00H 1.389(2) . ?
C00G C00Q 1.387(2) . ?
C00G H00G 0.9300 . ?
C00H H00H 0.9300 . ?
C00I C00K 1.389(2) . ?
C00I C00T 1.502(2) . ?
C00J C00R 1.385(2) . ?
C00J H00J 0.9300 . ?
C00K H00K 0.9300 . ?
C00L C00P 1.382(2) . ?
C00L H00L 0.9300 . ?
C00M H00a 0.9700 . ?
C00M H00c 0.9700 . ?
C00N H00d 0.9600 . ?
C00N H00i 0.9600 . ?
C00N H00m 0.9600 . ?
C00O H00n 0.9600 . ?
C00O H00o 0.9600 . ?
C00O H00p 0.9600 . ?
C00P C00R 1.407(3) . ?
C00P H00q 0.9300 . ?
C00Q H00r 0.9300 . ?
C00R H00s 0.9300 . ?
C00S H00t 0.9600 . ?
C00S H00u 0.9600 . ?
C00S H00v 0.9600 . ?
C00T H00w 0.9600 . ?
C00T H00x 0.9600 . ?
C00T H00y 0.9600 . ?