#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:33:31 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296663 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160172.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_7160172
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 'C17 H17 N O3 S'
_chemical_formula_sum 'C17 H17 N O3 S'
_chemical_formula_weight 315.40
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_Int_Tables_number 14
_atom_sites_solution_primary dual
_audit_creation_date 2019-12-05
_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 90
_cell_angle_beta 109.219(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.6272(2)
_cell_length_b 16.6924(2)
_cell_length_c 9.08710(10)
_cell_measurement_reflns_used 7031
_cell_measurement_temperature 93(2)
_cell_measurement_theta_max 79.1830
_cell_measurement_theta_min 5.8170
_cell_volume 1522.15(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 0.9711
_diffrn_measured_fraction_theta_max 0.9711
_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 54.00 82.00 0.50 5.00 -- 0.00 37.00 -90.00 56
2 \w -23.00 71.00 0.50 5.00 -- 0.00 57.00 150.00 188
3 \w -19.00 56.00 0.50 5.00 -- 0.00 37.00 30.00 150
4 \w 47.00 121.00 0.50 8.20 -- 107.20 -45.00 -30.00 148
5 \w 81.00 196.00 0.50 8.20 -- 107.20 82.00 90.00 230
6 \w 106.00 133.00 0.50 8.20 -- 107.20 15.00-120.00 54
7 \w 18.00 63.00 0.50 8.20 -- 107.20 -30.00 -60.00 90
8 \w 146.00 171.00 0.50 8.20 -- 107.20 15.00-120.00 50
9 \w 24.00 126.00 0.50 8.20 -- 107.20 -45.00 120.00 204
10 \w 70.00 119.00 0.50 8.20 -- 107.20 -30.00 -60.00 98
11 \w 72.00 127.00 0.50 8.20 -- 107.20 -77.00 -60.00 110
12 \w 50.00 123.00 0.50 8.20 -- 107.20 -15.00-120.00 146
13 \w 20.00 45.00 0.50 8.20 -- 107.20 -15.00-120.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0264572000
_diffrn_orient_matrix_UB_12 0.0786724000
_diffrn_orient_matrix_UB_13 0.0734068000
_diffrn_orient_matrix_UB_21 -0.1001917000
_diffrn_orient_matrix_UB_22 0.0254616000
_diffrn_orient_matrix_UB_23 -0.1581133000
_diffrn_orient_matrix_UB_31 -0.1133028000
_diffrn_orient_matrix_UB_32 -0.0409942000
_diffrn_orient_matrix_UB_33 0.0427094000
_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 0.0186
_diffrn_reflns_av_unetI/netI 0.0182
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 8378
_diffrn_reflns_theta_full 79.6459
_diffrn_reflns_theta_max 79.65
_diffrn_reflns_theta_min 4.41
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 1.996
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.84983
_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 'dark red'
_exptl_crystal_density_diffrn 1.3762
_exptl_crystal_description block
_exptl_crystal_F_000 667.3275
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.3256
_refine_diff_density_min -0.4873
_refine_diff_density_rms 0.0585
_refine_ls_d_res_high 0.7837
_refine_ls_d_res_low 10.0349
_refine_ls_goodness_of_fit_ref 1.0312
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_constraints 25
_refine_ls_number_parameters 209
_refine_ls_number_reflns 3221
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.0312
_refine_ls_R_factor_all 0.0371
_refine_ls_R_factor_gt 0.0364
_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^)+(0.0537P)^2^+0.9170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.0978
_reflns_Friedel_coverage 0.0
_reflns_limit_h_max 12
_reflns_limit_h_min -13
_reflns_limit_k_max 21
_reflns_limit_k_min 0
_reflns_limit_l_max 11
_reflns_limit_l_min 0
_reflns_number_gt 3123
_reflns_number_total 3221
_reflns_threshold_expression I>=2u(I)
_iucr_refine_instructions_details
;
TITL exp_522_001_a.res in P2(1)/c
REM Old TITL exp_522_001_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.078, Rweak 0.004, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C17 N O3 S
CELL 1.54184 10.6272 16.6924 9.0871 90 109.219 90
ZERR 4 0.0002 0.0002 0.0001 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O S
UNIT 68 68 4 12 4
L.S. 10
BOND $H
list 4
fmap 2
acta
WGHT 0.053746 0.917011
FVAR 0.636686
REM
REM
REM
S001 5 0.85845 0.69366 0.09160 11.00000 0.01995 0.01719 0.01816 =
0.00254 0.00718 0.00108
O002 4 0.88631 0.77853 0.10902 11.00000 0.02688 0.01887 0.03078 =
0.00408 0.01131 -0.00192
O003 4 0.87013 0.65452 -0.04512 11.00000 0.02846 0.02834 0.01921 =
0.00225 0.01092 0.00580
O004 4 0.65046 0.48727 0.56509 11.00000 0.02684 0.03059 0.02706 =
-0.00144 0.01344 -0.00317
N005 3 0.97634 0.42609 0.21921 11.00000 0.02260 0.02009 0.02309 =
-0.00209 0.00686 0.00369
C006 1 0.86937 0.51184 0.32792 11.00000 0.01821 0.01811 0.01664 =
0.00157 0.00266 0.00134
C007 1 0.64760 0.72553 0.18991 11.00000 0.02262 0.02058 0.02085 =
-0.00302 0.00547 -0.00084
AFIX 43
H007 2 0.70055 0.76583 0.24997 11.00000 -1.20000
AFIX 0
C008 1 0.69540 0.67725 0.09490 11.00000 0.02085 0.01701 0.01732 =
0.00191 0.00514 0.00059
C009 1 0.78775 0.53441 0.41506 11.00000 0.01957 0.01885 0.01959 =
-0.00015 0.00470 0.00129
AFIX 43
H009 2 0.77526 0.58803 0.43436 11.00000 -1.20000
AFIX 0
C00A 1 0.95166 0.55657 0.26022 11.00000 0.01831 0.02101 0.01684 =
0.00288 0.00404 0.00155
C00B 1 1.01523 0.50156 0.19698 11.00000 0.01926 0.02459 0.02008 =
0.00173 0.00487 0.00229
C00C 1 0.96806 0.64511 0.26175 11.00000 0.01878 0.02121 0.01980 =
0.00220 0.00456 0.00018
AFIX 23
H00a 2 1.05943 0.65747 0.27052 11.00000 -1.20000
H00c 2 0.95202 0.66665 0.35313 11.00000 -1.20000
AFIX 0
C00D 1 0.61695 0.61730 0.00367 11.00000 0.02688 0.01881 0.02063 =
-0.00174 0.00647 -0.00020
AFIX 43
H00D 2 0.65017 0.58491 -0.05831 11.00000 -1.20000
AFIX 0
C00E 1 0.82134 0.36994 0.35256 11.00000 0.02394 0.01732 0.02547 =
-0.00060 0.00364 -0.00013
AFIX 43
H00E 2 0.83129 0.31631 0.33090 11.00000 -1.20000
AFIX 0
C00F 1 0.88749 0.43024 0.30045 11.00000 0.01929 0.01961 0.01850 =
-0.00015 0.00265 0.00240
C00G 1 0.72666 0.47418 0.47109 11.00000 0.01913 0.02599 0.01865 =
0.00055 0.00548 -0.00021
C00H 1 0.51961 0.71248 0.19341 11.00000 0.02512 0.02681 0.02524 =
-0.00133 0.01030 0.00301
AFIX 43
H00H 2 0.48740 0.74391 0.25766 11.00000 -1.20000
AFIX 0
C00I 1 0.74078 0.39262 0.43722 11.00000 0.02241 0.02223 0.02497 =
0.00325 0.00524 -0.00425
AFIX 43
H00I 2 0.69502 0.35369 0.47259 11.00000 -1.20000
AFIX 0
C00J 1 0.43846 0.65297 0.10213 11.00000 0.02100 0.02616 0.02411 =
0.00565 0.00511 0.00102
C00K 1 0.48809 0.60642 0.00636 11.00000 0.02550 0.02161 0.02543 =
-0.00117 0.00346 -0.00459
AFIX 43
H00K 2 0.43410 0.56745 -0.05678 11.00000 -1.20000
AFIX 0
C00L 1 0.63149 0.56877 0.59917 11.00000 0.02604 0.03422 0.02808 =
-0.00797 0.01212 -0.00271
AFIX 137
H00f 2 0.59203 0.59761 0.50363 11.00000 -1.50000
H00g 2 0.57367 0.57133 0.66094 11.00000 -1.50000
H00j 2 0.71598 0.59230 0.65590 11.00000 -1.50000
AFIX 0
C00M 1 0.30000 0.63884 0.10801 11.00000 0.02525 0.04199 0.04011 =
0.00280 0.01209 -0.00343
AFIX 137
H00l 2 0.30563 0.61983 0.20969 11.00000 -1.50000
H00m 2 0.25068 0.68810 0.08680 11.00000 -1.50000
H00n 2 0.25557 0.59958 0.03129 11.00000 -1.50000
AFIX 0
H005 2 1.00763 0.38289 0.19985 11.00000 0.03706
H00B 2 1.08077 0.50941 0.14486 11.00000 0.02571
HKLF 4
END
Q2 1 0.777778 0.685185 0.1 11 0.05 0.33
REM The information below was added by Olex2.
REM
REM R1 = 0.0364 for 3123 Fo > 4sig(Fo) and 0.0371 for all 3221 data
REM 209 parameters refined using 0 restraints
REM Highest difference peak 0.3256, deepest hole -0.4873
REM Mean Shift 0.0000, Max Shift 0.0000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0371
REM R1_gt = 0.0364
REM wR_ref = 0.0978
REM GOOF = 1.0312
REM Shift_max = 0.0000
REM Shift_mean = 0.0000
REM Reflections_all = 3221
REM Reflections_gt = 3123
REM Parameters = 209
REM Hole = -0.4873
REM Peak = 0.3256
REM Flack = n/a
;
_cod_data_source_file d4ob01356e2.cif
_cod_data_source_block exp_522_001
_cod_depositor_comments
'Adding full bibliography for 7160172--7160173.cif.'
_cod_database_code 7160172
_reflns_odcompleteness_completeness 99.84
_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:
C00C(H00a,H00c)
2.b Aromatic/amide H refined with riding coordinates:
C007(H007), C009(H009), C00D(H00D), C00E(H00E), C00H(H00H), C00I(H00I),
C00K(H00K)
2.c Idealised Me refined as rotating group:
C00L(H00f,H00g,H00j), C00M(H00l,H00m,H00n)
;
_iucr_refine_fcf_details
;
data_exp_522_001_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+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
_cell_length_a 10.6272(2)
_cell_length_b 16.6924(2)
_cell_length_c 9.08710(10)
_cell_angle_alpha 90
_cell_angle_beta 109.219(2)
_cell_angle_gamma 90
_cell_volume 1522.15(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
-13 0 4 29.094 23.016 1.258 33.092 o
-13 0 6 119.352 108.666 2.689 6.204 o
-13 1 3 8.398 7.154 0.765 116.670 o
-13 1 4 197.068 178.913 20.488 1.348 o
-13 1 5 1.867 1.065 0.302 602.957 o
-13 1 6 56.586 36.474 4.342 13.148 o
-13 2 3 52.906 48.129 1.875 16.223 o
-13 2 4 55.706 40.785 11.631 4.987 o
-13 2 5 14.228 17.120 1.061 60.027 o
-13 2 6 131.554 126.033 3.010 5.344 o
-13 3 4 98.344 116.042 3.108 6.907 o
-13 3 5 200.382 185.633 4.144 3.076 o
-13 4 6 0.844 1.357 0.296 924.205 o
-13 5 4 1.618 0.715 0.370 699.370 o
-13 5 5 125.745 110.640 2.566 5.922 o
-12 0 2 235.807 223.229 4.169 2.453 o
-12 0 4 128.410 150.455 4.539 4.759 o
-12 0 6 221.786 241.582 5.921 2.388 o
-12 0 8 311.799 317.389 6.143 1.548 o
-12 1 1 8.738 7.475 0.839 110.647 o
-12 1 2 196.409 195.732 3.800 3.089 o
-12 1 3 12.842 12.785 0.699 74.183 o
-12 1 4 26.946 26.604 1.280 33.323 o
-12 1 5 23.539 29.902 1.323 34.722 o
-12 1 6 672.316 796.674 16.651 0.393 o
-12 1 7 129.351 161.848 2.965 4.862 o
-12 1 8 314.450 309.182 4.237 1.607 o
-12 2 1 250.420 270.247 5.970 2.042 o
-12 2 2 27.799 30.591 1.022 31.699 o
-12 2 3 0.121 0.573 0.341 2580.760 o
-12 2 4 308.393 314.111 4.884 1.609 o
-12 2 5 154.167 176.858 3.433 4.005 o
-12 2 6 0.130 0.244 0.427 2806.590 o
-12 2 7 465.445 487.176 8.239 0.823 o
-12 2 8 288.617 242.298 4.613 1.937 o
-12 3 1 238.882 255.051 5.748 2.198 o
-12 3 2 149.527 158.400 3.148 4.351 o
-12 3 3 459.705 456.724 8.276 0.860 o
-12 3 4 7.985 5.479 0.509 135.551 o
-12 3 5 36.384 39.260 1.240 23.708 o
-12 3 6 21.076 21.561 1.307 41.970 o
-12 3 7 91.551 95.863 2.590 8.070 o
-12 3 8 0.988 3.996 0.493 453.636 o
-12 4 1 632.358 654.662 11.940 0.494 o
-12 4 2 62.486 60.611 2.418 12.819 o
-12 4 3 10.833 15.813 1.283 69.641 o
-12 4 4 19.801 18.567 1.418 45.204 o
-12 4 5 405.684 396.030 6.759 1.069 o
-12 4 6 6.223 5.129 0.470 165.815 o
-12 4 7 368.355 400.524 7.746 1.147 o
-12 5 1 531.858 598.047 10.978 0.623 o
-12 5 2 65.853 70.614 5.094 9.351 o
-12 5 3 219.480 236.039 9.337 2.146 o
-12 5 4 311.096 312.794 4.878 1.599 o
-12 5 5 152.921 178.768 3.158 4.042 o
-12 5 6 41.518 39.451 6.093 11.889 o
-12 5 7 42.062 37.028 1.480 21.482 o
-12 6 1 81.559 88.314 2.689 9.042 o
-12 6 2 36.204 43.565 1.924 21.712 o
-12 6 3 57.727 57.205 2.344 13.913 o
-12 6 4 7.405 8.641 0.680 120.896 o
-12 6 5 202.600 197.534 5.390 2.861 o
-12 6 6 6.444 6.045 0.481 153.862 o
-12 6 7 29.265 25.113 0.987 32.786 o
-12 7 1 69.430 79.113 2.344 10.803 o
-12 7 2 108.790 105.101 19.217 1.883 o
-12 7 3 206.801 205.115 3.236 2.927 o
-12 7 4 11.441 13.037 0.732 79.117 o
-12 7 5 13.888 13.078 0.662 70.108 o
-12 7 6 234.463 181.274 2.642 2.764 o
-12 8 2 195.431 176.935 35.005 0.628 o
-12 8 3 1.257 0.641 0.221 928.540 o
-12 8 4 354.670 329.242 34.277 0.513 o
-12 8 5 0.707 1.423 0.345 954.086 o
-12 9 3 78.907 86.242 2.368 9.502 o
-12 9 4 6.307 7.697 0.641 139.783 o
-12 9 5 0.907 1.085 0.296 966.541 o
-11 0 2 24.258 30.451 1.468 33.358 o
-11 0 4 17.475 20.796 1.949 43.223 o
-11 0 6 1006.580 1141.850 20.968 0.205 o
-11 0 8 13.607 15.665 1.307 61.261 o
-11 1 1 569.696 582.335 5.985 0.624 o
-11 1 2 7.804 10.179 0.642 110.925 o
-11 1 3 49.435 48.387 1.550 17.357 o
-11 1 4 196.538 199.509 3.590 3.077 o
-11 1 5 45.428 56.226 2.119 16.737 o
-11 1 6 56.524 58.455 2.076 14.263 o
-11 1 7 6.368 7.755 0.837 132.962 o
-11 1 8 388.074 451.129 6.471 1.048 o
-11 1 9 16.946 25.458 1.233 45.389 o
-11 2 1 533.240 568.178 5.818 0.678 o
-11 2 2 821.659 849.201 9.473 0.332 o
-11 2 3 75.862 78.837 2.000 10.310 o
-11 2 4 74.720 78.633 1.994 10.442 o
-11 2 5 27.835 22.812 1.048 34.872 o
-11 2 6 202.594 227.324 6.266 2.614 o
-11 2 7 522.602 569.431 11.471 0.646 o
-11 2 8 37.330 46.994 2.097 20.370 o
-11 2 9 14.278 14.472 0.643 66.654 o
-11 3 1 213.149 216.848 2.889 2.795 o
-11 3 2 838.204 870.232 11.434 0.316 o
-11 3 3 872.188 916.534 11.722 0.293 o
-11 3 4 80.913 89.657 2.529 9.113 o
-11 3 5 301.846 295.450 10.842 1.448 o
-11 3 6 32.839 34.493 2.615 23.202 o
-11 3 7 85.572 101.793 2.502 8.308 o
-11 3 8 156.028 173.601 3.129 4.034 o
-11 3 9 19.069 15.837 0.913 51.667 o
-11 4 1 5.001 5.681 0.671 177.320 o
-11 4 2 139.092 128.469 2.808 5.094 o
-11 4 3 85.331 90.434 1.935 8.952 o
-11 4 4 295.928 289.852 5.427 1.721 o
-11 4 5 26.168 28.616 1.147 33.510 o
-11 4 6 59.763 57.401 1.518 14.207 o
-11 4 7 86.633 75.061 2.023 9.458 o
-11 4 8 11.258 11.076 0.802 83.720 o
-11 4 9 128.957 105.015 2.442 5.929 o
-11 5 1 19.800 25.472 1.236 41.437 o
-11 5 2 250.882 254.821 3.767 2.199 o
-11 5 3 241.404 242.077 5.637 2.237 o
-11 5 4 158.956 147.093 2.571 4.326 o
-11 5 5 267.447 286.901 3.752 1.958 o
-11 5 6 15.051 21.428 0.893 54.241 o
-11 5 7 44.697 41.992 2.590 18.008 o
-11 5 8 97.123 105.928 2.960 7.292 o
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8 15 1 229.657 167.674 3.552 2.856 o
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9 0 2 285.071 305.277 7.869 1.640 o
9 0 4 25.005 25.774 1.492 34.653 o
9 1 0 1380.330 1348.560 12.417 0.138 o
9 1 1 58.236 62.572 1.416 14.082 o
9 1 2 0.524 0.958 0.459 1144.780 o
9 1 3 101.980 109.082 2.834 6.982 o
9 1 4 25.508 28.541 1.005 34.495 o
9 1 5 2.629 2.427 0.544 354.237 o
9 2 0 2.340 2.471 0.418 396.963 o
9 2 1 481.759 497.894 4.997 0.816 o
9 2 2 492.911 498.140 6.335 0.786 o
9 2 3 32.212 36.809 1.764 25.273 o
9 2 4 18.729 19.834 1.924 42.383 o
9 2 5 39.611 35.428 4.292 16.360 o
9 3 0 282.032 287.591 3.395 1.870 o
9 3 1 330.966 337.342 4.239 1.466 o
9 3 2 68.130 70.734 2.233 11.508 o
9 3 3 38.283 45.119 2.442 19.699 o
9 3 4 77.353 71.029 1.789 10.658 o
9 3 5 1.165 0.641 0.370 900.468 o
9 4 0 471.797 480.320 6.131 0.840 o
9 4 1 290.316 293.885 5.256 1.746 o
9 4 2 36.489 33.739 1.247 24.948 o
9 4 3 76.498 77.545 1.832 10.384 o
9 4 4 93.318 90.756 2.843 8.028 o
9 4 5 7.533 7.672 0.888 119.389 o
9 5 0 265.987 267.063 5.234 1.980 o
9 5 1 21.649 21.096 1.043 42.704 o
9 5 2 18.223 19.778 0.851 49.873 o
9 5 3 354.081 370.349 18.748 0.895 o
9 5 4 28.815 26.318 1.203 32.135 o
9 5 5 74.071 54.789 1.850 11.997 o
9 6 0 58.664 68.460 2.393 12.825 o
9 6 1 387.756 408.340 10.842 1.016 o
9 6 2 30.857 31.992 1.219 28.646 o
9 6 3 59.410 57.578 1.554 14.231 o
9 6 4 288.055 270.735 15.862 1.274 o
9 7 0 210.264 214.551 5.316 2.683 o
9 7 1 28.588 31.009 1.236 30.465 o
9 7 2 117.935 126.388 2.453 5.941 o
9 7 3 116.108 112.762 3.018 6.179 o
9 7 4 19.761 17.969 1.455 45.480 o
9 8 0 0.052 0.350 0.506 2389.150 o
9 8 1 44.874 52.689 1.556 17.987 o
9 8 2 438.972 443.356 8.731 0.907 o
9 8 3 0.087 0.711 0.295 2637.060 o
9 9 0 17.271 15.288 1.172 54.237 o
9 9 1 62.184 61.653 2.006 13.110 o
9 9 2 77.057 72.182 1.626 10.694 o
9 9 3 4.198 3.431 0.432 245.353 o
9 10 0 28.420 30.460 2.553 26.474 o
9 10 1 17.450 17.515 1.406 49.988 o
9 10 2 39.761 36.104 2.183 21.257 o
9 10 3 1.766 2.689 0.518 432.469 o
9 11 0 20.291 24.570 1.677 39.176 o
9 11 1 11.415 13.223 1.110 74.492 o
9 11 2 9.292 7.305 0.605 111.099 o
9 12 0 211.093 212.081 16.368 1.597 o
9 12 1 1.257 1.471 0.293 721.042 o
9 12 2 304.568 251.116 43.232 0.398 o
9 13 0 545.414 494.781 57.429 0.206 o
9 13 1 60.196 47.834 8.622 6.999 o
9 14 0 216.685 210.573 4.564 2.691 o
9 14 1 182.971 139.058 2.936 3.855 o
10 0 0 291.621 289.486 7.573 1.660 o
10 0 2 3.756 4.095 0.962 208.970 o
10 0 4 227.914 211.585 5.156 2.527 o
10 1 0 281.020 301.363 4.356 1.808 o
10 1 1 217.637 220.167 3.423 2.697 o
10 1 2 291.758 308.879 5.224 1.698 o
10 1 3 1.355 1.737 0.479 591.462 o
10 1 4 1.932 3.150 0.962 305.904 o
10 2 0 50.249 53.935 1.245 16.731 o
10 2 1 106.753 111.580 2.262 6.819 o
10 2 2 196.332 209.006 3.967 2.988 o
10 2 3 1.893 1.840 0.491 478.746 o
10 2 4 22.265 15.961 1.061 45.397 o
10 3 0 26.909 27.317 0.892 34.061 o
10 3 1 258.707 272.051 4.064 2.061 o
10 3 2 13.898 15.553 0.990 63.626 o
10 3 3 4.354 5.499 1.073 169.780 o
10 3 4 84.863 76.597 2.615 9.289 o
10 4 0 47.194 47.728 1.424 18.167 o
10 4 1 200.577 201.812 3.207 3.032 o
10 4 2 56.834 59.033 2.418 13.838 o
10 4 3 660.133 649.001 32.304 0.327 o
10 4 4 128.195 83.381 2.541 6.404 o
10 5 0 140.853 146.930 4.314 4.524 o
10 5 1 373.474 384.908 8.585 1.136 o
10 5 2 110.538 108.420 3.577 6.362 o
10 5 3 87.993 90.366 2.960 8.356 o
10 6 0 106.194 109.097 2.868 6.758 o
10 6 1 272.622 277.242 25.372 0.849 o
10 6 2 92.101 92.212 4.601 7.250 o
10 6 3 50.113 55.654 3.355 14.149 o
10 7 0 182.425 177.357 6.204 3.161 o
10 7 1 48.175 49.789 1.708 17.335 o
10 7 2 152.688 158.839 2.939 4.296 o
10 7 3 254.693 202.985 54.444 0.282 o
10 8 0 140.261 144.278 5.563 4.315 o
10 8 1 54.703 59.274 2.171 14.430 o
10 8 2 4.036 3.477 0.599 240.036 o
10 9 0 157.732 158.778 3.235 4.146 o
10 9 1 23.584 27.876 1.150 36.205 o
10 9 2 401.625 367.393 6.907 1.116 o
10 10 0 63.547 66.485 1.822 12.665 o
10 10 1 381.994 393.636 11.792 1.023 o
10 11 0 342.933 334.810 8.819 1.303 o
10 11 1 123.336 93.594 2.270 6.450 o
10 12 0 3.301 2.738 0.395 310.588 o
10 12 1 29.401 21.857 0.962 34.111 o
10 13 0 58.606 49.288 1.505 15.209 o
11 0 0 277.570 310.902 7.203 1.693 o
11 0 2 21.982 23.238 1.357 39.602 o
11 1 0 66.654 65.913 1.953 12.186 o
11 1 1 62.968 69.748 1.900 12.465 o
11 1 2 70.517 77.146 1.796 11.078 o
11 1 3 124.265 85.380 7.882 4.720 o
11 2 0 235.427 253.025 4.352 2.311 o
11 2 1 116.631 120.534 2.812 6.041 o
11 2 2 20.351 20.919 1.332 43.236 o
11 3 0 4.098 4.559 0.451 227.187 o
11 3 1 296.246 308.152 4.686 1.693 o
11 3 2 19.257 23.435 1.357 42.883 o
11 3 3 17.419 12.063 0.863 59.780 o
11 4 0 6.421 4.925 0.610 159.856 o
11 4 1 16.130 17.959 1.357 52.432 o
11 4 2 14.371 13.118 0.691 68.220 o
11 5 0 56.022 57.522 1.728 14.737 o
11 5 1 181.137 184.646 4.712 3.307 o
11 5 2 12.263 10.114 1.061 78.007 o
11 6 0 161.249 150.843 10.595 2.870 o
11 6 2 92.496 69.683 27.382 1.112 o
11 7 0 10.581 11.274 1.036 83.335 o
11 7 1 10.731 8.730 3.047 50.194 o
11 7 2 72.623 60.439 1.677 11.907 o
11 8 0 423.744 449.040 6.130 0.970 o
11 8 1 75.984 71.219 2.146 10.627 o
11 9 0 250.662 238.837 8.992 1.954 o
11 9 1 97.786 75.339 1.899 8.582 o
11 10 0 51.191 48.453 1.233 17.182 o
12 0 0 708.023 718.801 12.433 0.416 o
12 1 0 404.502 382.445 48.881 0.294 o
12 1 1 8.984 10.460 0.715 99.758 o
12 2 0 0.282 0.567 0.469 1668.570 o
12 2 1 0.294 0.839 0.345 1696.910 o
12 3 0 58.160 51.361 1.924 14.751 o
12 3 1 238.408 174.930 2.948 2.742 o
12 4 0 0.431 0.173 0.419 1916.130 o
12 4 1 336.597 243.938 69.097 0.177 o
12 5 0 0.083 0.247 0.395 3348.040 o
12 5 1 362.480 296.520 5.328 1.397 o
12 6 0 35.275 37.373 1.431 24.341 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 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.781
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2
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 0.85845(3) 0.693659(19) 0.09160(4) 0.01821(11) Uani 1.000000 .
O002 O 0.88631(10) 0.77853(6) 0.10902(12) 0.0251(2) Uani 1.000000 .
O003 O 0.87013(10) 0.65452(6) -0.04512(11) 0.0246(2) Uani 1.000000 .
O004 O 0.65046(11) 0.48727(7) 0.56509(12) 0.0270(2) Uani 1.000000 .
N005 N 0.97634(12) 0.42609(8) 0.21921(14) 0.0221(3) Uani 1.000000 .
C006 C 0.86937(13) 0.51184(8) 0.32792(15) 0.0184(3) Uani 1.000000 .
C007 C 0.64760(14) 0.72553(9) 0.18991(16) 0.0218(3) Uani 1.000000 .
H007 H 0.70055(14) 0.76583(9) 0.24997(16) 0.0261(3) Uiso 1.000000 R
C008 C 0.69540(14) 0.67725(8) 0.09490(15) 0.0187(3) Uani 1.000000 .
C009 C 0.78775(13) 0.53441(8) 0.41506(16) 0.0198(3) Uani 1.000000 .
H009 H 0.77526(13) 0.58803(8) 0.43436(16) 0.0237(3) Uiso 1.000000 R
C00A C 0.95166(13) 0.55657(8) 0.26022(15) 0.0192(3) Uani 1.000000 .
C00B C 1.01523(14) 0.50156(9) 0.19698(16) 0.0217(3) Uani 1.000000 .
C00C C 0.96806(14) 0.64511(8) 0.26175(16) 0.0204(3) Uani 1.000000 .
H00a H 1.05943(14) 0.65747(8) 0.27052(16) 0.0244(3) Uiso 1.000000 R
H00c H 0.95202(14) 0.66665(8) 0.35313(16) 0.0244(3) Uiso 1.000000 R
C00D C 0.61695(15) 0.61730(8) 0.00367(16) 0.0224(3) Uani 1.000000 .
H00D H 0.65017(15) 0.58491(8) -0.05831(16) 0.0269(4) Uiso 1.000000 R
C00E C 0.82134(14) 0.36994(9) 0.35256(17) 0.0233(3) Uani 1.000000 .
H00E H 0.83129(14) 0.31631(9) 0.33090(17) 0.0280(4) Uiso 1.000000 R
C00F C 0.88749(14) 0.43024(8) 0.30045(16) 0.0200(3) Uani 1.000000 .
C00G C 0.72666(14) 0.47418(9) 0.47109(16) 0.0214(3) Uani 1.000000 .
C00H C 0.51961(15) 0.71248(9) 0.19341(18) 0.0252(3) Uani 1.000000 .
H00H H 0.48740(15) 0.74391(9) 0.25766(18) 0.0303(4) Uiso 1.000000 R
C00I C 0.74078(14) 0.39262(9) 0.43722(17) 0.0238(3) Uani 1.000000 .
H00I H 0.69502(14) 0.35369(9) 0.47259(17) 0.0286(4) Uiso 1.000000 R
C00J C 0.43846(14) 0.65297(9) 0.10213(17) 0.0243(3) Uani 1.000000 .
C00K C 0.48809(15) 0.60642(9) 0.00636(18) 0.0254(3) Uani 1.000000 .
H00K H 0.43410(15) 0.56745(9) -0.05678(18) 0.0305(4) Uiso 1.000000 R
C00L C 0.63149(16) 0.56877(10) 0.59917(18) 0.0287(3) Uani 1.000000 .
H00f H 0.5920(12) 0.5976(2) 0.50363(19) 0.0430(5) Uiso 1.000000 GR
H00g H 0.5737(10) 0.57133(11) 0.6609(13) 0.0430(5) Uiso 1.000000 GR
H00j H 0.7160(2) 0.5923(2) 0.6559(13) 0.0430(5) Uiso 1.000000 GR
C00M C 0.30000(16) 0.63884(12) 0.1080(2) 0.0355(4) Uani 1.000000 .
H00l H 0.30563(17) 0.6198(8) 0.2097(6) 0.0532(6) Uiso 1.000000 GR
H00m H 0.2507(5) 0.6881(2) 0.0868(17) 0.0532(6) Uiso 1.000000 GR
H00n H 0.2556(5) 0.5996(6) 0.0313(12) 0.0532(6) Uiso 1.000000 GR
H005 H 1.008(2) 0.3829(14) 0.200(2) 0.037(5) Uiso 1.000000 .
H00B H 1.0808(18) 0.5094(11) 0.145(2) 0.026(4) Uiso 1.000000 .
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 0.01995(19) 0.01719(18) 0.01816(18) 0.00108(11) 0.00718(13) 0.00254(11)
O002 0.0269(5) 0.0189(5) 0.0308(6) -0.0019(4) 0.0113(4) 0.0041(4)
O003 0.0285(5) 0.0283(5) 0.0192(5) 0.0058(4) 0.0109(4) 0.0022(4)
O004 0.0268(5) 0.0306(6) 0.0271(5) -0.0032(4) 0.0134(4) -0.0014(4)
N005 0.0226(6) 0.0201(6) 0.0231(6) 0.0037(5) 0.0069(5) -0.0021(5)
C006 0.0182(6) 0.0181(6) 0.0166(6) 0.0013(5) 0.0027(5) 0.0016(5)
C007 0.0226(7) 0.0206(7) 0.0208(6) -0.0008(5) 0.0055(5) -0.0030(5)
C008 0.0209(6) 0.0170(6) 0.0173(6) 0.0006(5) 0.0051(5) 0.0019(5)
C009 0.0196(6) 0.0188(6) 0.0196(6) 0.0013(5) 0.0047(5) -0.0002(5)
C00A 0.0183(6) 0.0210(7) 0.0168(6) 0.0016(5) 0.0040(5) 0.0029(5)
C00B 0.0193(6) 0.0246(7) 0.0201(6) 0.0023(5) 0.0049(5) 0.0017(5)
C00C 0.0188(6) 0.0212(7) 0.0198(6) 0.0002(5) 0.0046(5) 0.0022(5)
C00D 0.0269(7) 0.0188(6) 0.0206(6) -0.0002(5) 0.0065(5) -0.0017(5)
C00E 0.0239(7) 0.0173(6) 0.0255(7) -0.0001(5) 0.0036(6) -0.0006(5)
C00F 0.0193(6) 0.0196(7) 0.0185(6) 0.0024(5) 0.0027(5) -0.0001(5)
C00G 0.0191(6) 0.0260(7) 0.0187(6) -0.0002(5) 0.0055(5) 0.0005(5)
C00H 0.0251(7) 0.0268(7) 0.0252(7) 0.0030(6) 0.0103(6) -0.0013(6)
C00I 0.0224(7) 0.0222(7) 0.0250(7) -0.0042(5) 0.0052(6) 0.0033(6)
C00J 0.0210(7) 0.0262(7) 0.0241(7) 0.0010(6) 0.0051(6) 0.0057(6)
C00K 0.0255(7) 0.0216(7) 0.0254(7) -0.0046(6) 0.0035(6) -0.0012(6)
C00L 0.0260(7) 0.0342(8) 0.0281(7) -0.0027(6) 0.0121(6) -0.0080(6)
C00M 0.0253(8) 0.0420(10) 0.0401(9) -0.0034(7) 0.0121(7) 0.0028(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 117.71(6) . . ?
C008 S001 O002 108.49(6) . . ?
C008 S001 O003 107.90(6) . . ?
C00C S001 O002 107.27(6) . . ?
C00C S001 O003 108.76(6) . . ?
C00C S001 C008 106.14(6) . . ?
C00L O004 C00G 116.20(12) . . ?
C00F N005 C00B 109.13(12) . . ?
H005 N005 C00B 127.2(15) . . ?
H005 N005 C00F 123.1(14) . . ?
C00A C006 C009 132.79(13) . . ?
C00F C006 C009 120.31(13) . . ?
C00F C006 C00A 106.81(12) . . ?
C008 C007 H007 120.55(8) . . ?
C00H C007 H007 120.55(9) . . ?
C00H C007 C008 118.90(13) . . ?
C007 C008 S001 118.77(11) . . ?
C00D C008 S001 120.11(11) . . ?
C00D C008 C007 121.13(13) . . ?
H009 C009 C006 121.15(8) . . ?
C00G C009 C006 117.70(13) . . ?
C00G C009 H009 121.15(8) . . ?
C00B C00A C006 106.56(12) . . ?
C00C C00A C006 126.84(12) . . ?
C00C C00A C00B 126.58(13) . . ?
C00A C00B N005 109.97(12) . . ?
H00B C00B N005 119.9(11) . . ?
H00B C00B C00A 130.1(11) . . ?
C00A C00C S001 113.57(10) . . ?
H00a C00C S001 108.85(5) . . ?
H00a C00C C00A 108.85(7) . . ?
H00c C00C S001 108.85(5) . . ?
H00c C00C C00A 108.85(7) . . ?
H00c C00C H00a 107.7 . . ?
H00D C00D C008 120.49(8) . . ?
C00K C00D C008 119.01(13) . . ?
C00K C00D H00D 120.49(9) . . ?
C00F C00E H00E 121.13(8) . . ?
C00I C00E H00E 121.13(9) . . ?
C00I C00E C00F 117.74(13) . . ?
C006 C00F N005 107.52(12) . . ?
C00E C00F N005 130.94(13) . . ?
C00E C00F C006 121.54(13) . . ?
C009 C00G O004 123.91(13) . . ?
C00I C00G O004 114.50(12) . . ?
C00I C00G C009 121.58(13) . . ?
H00H C00H C007 119.45(9) . . ?
C00J C00H C007 121.10(14) . . ?
C00J C00H H00H 119.45(9) . . ?
C00G C00I C00E 121.03(13) . . ?
H00I C00I C00E 119.49(9) . . ?
H00I C00I C00G 119.49(8) . . ?
C00K C00J C00H 118.77(13) . . ?
C00M C00J C00H 120.62(14) . . ?
C00M C00J C00K 120.61(14) . . ?
C00J C00K C00D 121.07(14) . . ?
H00K C00K C00D 119.47(9) . . ?
H00K C00K C00J 119.47(9) . . ?
H00f C00L O004 109.5 . . ?
H00g C00L O004 109.5 . . ?
H00g C00L H00f 109.5 . . ?
H00j C00L O004 109.5 . . ?
H00j C00L H00f 109.5 . . ?
H00j C00L H00g 109.5 . . ?
H00l C00M C00J 109.5 . . ?
H00m C00M C00J 109.5 . . ?
H00m C00M H00l 109.5 . . ?
H00n C00M C00J 109.5 . . ?
H00n C00M H00l 109.5 . . ?
H00n C00M H00m 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 1.4453(11) . ?
S001 O003 1.4447(10) . ?
S001 C008 1.7642(14) . ?
S001 C00C 1.7941(14) . ?
O004 C00G 1.3742(17) . ?
O004 C00L 1.4242(19) . ?
N005 C00B 1.3616(19) . ?
N005 C00F 1.3785(18) . ?
N005 H005 0.84(2) . ?
C006 C009 1.4048(19) . ?
C006 C00A 1.4335(19) . ?
C006 C00F 1.4094(19) . ?
C007 H007 0.9300 . ?
C007 C008 1.3934(19) . ?
C007 C00H 1.388(2) . ?
C008 C00D 1.3889(19) . ?
C009 H009 0.9300 . ?
C009 C00G 1.3817(19) . ?
C00A C00B 1.373(2) . ?
C00A C00C 1.4876(19) . ?
C00B H00B 0.972(18) . ?
C00C H00a 0.9700 . ?
C00C H00c 0.9700 . ?
C00D H00D 0.9300 . ?
C00D C00K 1.390(2) . ?
C00E H00E 0.9300 . ?
C00E C00F 1.397(2) . ?
C00E C00I 1.379(2) . ?
C00G C00I 1.415(2) . ?
C00H H00H 0.9300 . ?
C00H C00J 1.396(2) . ?
C00I H00I 0.9300 . ?
C00J C00K 1.393(2) . ?
C00J C00M 1.508(2) . ?
C00K H00K 0.9300 . ?
C00L H00f 0.9600 . ?
C00L H00g 0.9600 . ?
C00L H00j 0.9600 . ?
C00M H00l 0.9600 . ?
C00M H00m 0.9600 . ?
C00M H00n 0.9600 . ?