#------------------------------------------------------------------------------
#$Date: 2022-06-11 02:51:09 +0100 (Sat, 11 Jun 2022) $
#$Revision: 275970 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244114.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2244114
loop_
_publ_author_name
'Friedrich, Erik'
'Heinrich, Timo'
'Rosenberger, Lara'
'Krier, Mireille'
'Marek, Stephanie'
'Reggelin, Michael'
_publ_section_title
;
Synthesis and crystal structure of
rac-2-(1,3-dioxoisoindolin-2-yl)ethyl
4-methyl-N-phenyl-N'-(triisopropylsilyl)benzenesulfondiimidoate:
the first member of a new substance class
;
_journal_coeditor_code ZL5029
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022005904
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C32 H41 N3 O3 S Si'
_chemical_formula_moiety 'C32 H41 N3 O3 S Si'
_chemical_formula_sum 'C32 H41 N3 O3 S Si'
_chemical_formula_weight 575.83
_chemical_name_systematic
rac-2-[7-Methyl-4-(4-methylphenyl)-4-(phenylimino)-6,6-bis(propan-2-yl)-3-oxa-4\l^6^-thia-5-aza-6-silaoct-4-en-1-yl]-2,3-dihydro-1H-isoindole-1,3-dione
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 78.107(2)
_cell_angle_beta 87.922(2)
_cell_angle_gamma 89.512(2)
_cell_formula_units_Z 2
_cell_length_a 8.6752(2)
_cell_length_b 8.8765(2)
_cell_length_c 20.2299(6)
_cell_measurement_reflns_used 4930
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 72.0790
_cell_measurement_theta_min 4.4470
_cell_volume 1523.37(7)
_computing_cell_refinement 'CrysAlisPro (Rigaku, 2021)'
_computing_data_collection 'CrysAlisPro (Rigaku, 2021)'
_computing_data_reduction 'CrysAlisPro (Rigaku, 2021)'
_computing_molecular_graphics 'Mercury (Macrae et al., 2020)'
_computing_publication_material 'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL2018/1 (Sheldrick, 2015b)'
_computing_structure_solution 'SHELXT2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0465
_diffrn_reflns_av_unetI/netI 0.0383
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 28106
_diffrn_reflns_theta_full 67.079
_diffrn_reflns_theta_max 67.079
_diffrn_reflns_theta_min 4.470
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 1.612
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.555
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku, 2021)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.255
_exptl_crystal_description needle
_exptl_crystal_F_000 616
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.556
_refine_diff_density_min -0.379
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 368
_refine_ls_number_reflns 5410
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0518
_refine_ls_R_factor_gt 0.0408
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.4269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1030
_refine_ls_wR_factor_ref 0.1083
_reflns_number_gt 4426
_reflns_number_total 5410
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zl5029sup1.cif
_cod_data_source_block I
_cod_database_code 2244114
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.728
_shelx_estimated_absorpt_t_max 0.910
_shelx_hkl_file
;
-10 -2 -1 29.93 5.60
-10 -2 0 32.23 5.67
-10 -2 1 45.97 6.10
-10 -2 2 28.65 4.83
-10 -1 -7 6.99 3.95
-10 -1 -6 8.11 4.20
-10 -1 -5 49.14 7.40
-10 -1 -4 97.77 9.49
-10 -1 -3 28.04 5.15
-10 -1 -3 29.41 5.97
-10 -1 -2 4.21 4.18
-10 -1 -1 9.20 4.48
-10 -1 0 44.42 6.56
-10 -1 1 94.93 8.86
-10 -1 2 14.95 4.80
-10 -1 2 23.12 4.63
-10 -1 3 49.62 6.35
-10 -1 3 43.85 5.77
-10 -1 4 9.46 4.03
-10 -1 4 14.46 3.85
-10 0 -7 106.84 9.33
-10 0 -6 6.39 4.75
-10 0 -5 6.69 4.64
-10 0 -5 5.59 4.70
-10 0 -4 58.18 6.60
-10 0 -4 54.36 7.51
-10 0 -3 10.31 4.83
-10 0 -3 7.74 5.75
-10 0 -3 -6.06 5.67
-10 0 -2 186.58 12.30
-10 0 -2 167.44 12.82
-10 0 -2 180.42 14.01
-10 0 -1 9.30 4.68
-10 0 -1 8.02 5.89
-10 0 -1 13.85 4.46
-10 0 0 18.99 5.51
-10 0 0 20.53 4.70
-10 0 0 18.89 6.29
-10 0 1 109.14 9.22
-10 0 1 100.69 10.34
-10 0 2 36.79 5.95
-10 0 2 31.04 5.23
-10 0 2 20.10 6.05
-10 0 3 7.17 3.85
-10 0 3 6.21 4.43
-10 0 3 -0.62 4.17
-10 0 4 1.60 3.28
-10 0 4 11.31 4.31
-10 0 5 3.52 3.36
-10 0 5 4.42 4.28
-10 0 5 2.52 3.33
-10 1 -6 6.92 4.70
-10 1 -6 14.96 5.00
-10 1 -5 59.15 7.28
-10 1 -5 48.29 6.97
-10 1 -4 -0.91 3.48
-10 1 -4 7.65 4.71
-10 1 -4 9.79 4.79
-10 1 -3 2.52 3.58
-10 1 -3 1.47 4.98
-10 1 -3 -1.30 4.38
-10 1 -2 8.68 3.90
-10 1 -2 3.78 4.53
-10 1 -2 3.81 4.78
-10 1 -1 14.86 4.60
-10 1 -1 17.88 5.65
-10 1 -1 13.06 4.85
-10 1 0 42.75 6.08
-10 1 0 48.34 7.42
-10 1 0 48.34 6.23
-10 1 1 -1.21 4.64
-10 1 1 5.32 5.49
-10 1 2 1.22 4.22
-10 1 2 15.14 5.73
-10 1 3 22.96 5.49
-10 1 3 29.55 4.77
-10 1 3 20.49 5.67
-10 1 4 0.59 4.24
-10 1 4 3.07 3.46
-10 1 4 -0.58 4.06
-10 1 5 17.48 4.40
-10 1 5 24.77 5.03
-10 2 -3 -1.44 2.90
-10 2 -3 -4.49 4.57
-10 2 -3 2.91 4.03
-10 2 -2 38.02 4.86
-10 2 -2 39.20 6.45
-10 2 -2 27.74 5.48
-10 2 -1 21.73 4.33
-10 2 -1 7.00 5.08
-10 2 -1 6.93 4.21
-10 2 0 50.97 6.04
-10 2 0 63.96 7.90
-10 2 1 -0.52 3.74
-10 2 1 -0.71 4.71
-10 2 2 24.84 4.97
-10 2 2 33.40 6.30
-10 2 3 92.54 8.15
-10 2 3 90.67 9.17
-10 2 4 2.10 3.94
-10 2 4 10.91 4.56
-9 -5 -3 66.18 7.06
-9 -5 -2 5.33 3.67
-9 -5 -1 0.53 3.43
-9 -5 0 3.67 3.77
-9 -5 1 18.19 4.35
-9 -4 -3 0.66 4.09
-9 -4 -2 29.42 5.82
-9 -4 -1 -1.33 4.34
-9 -4 0 4.61 3.87
-9 -4 1 10.26 4.72
-9 -4 2 -0.61 3.75
-9 -4 3 9.19 4.11
-9 -4 4 3.11 3.62
-9 -4 5 141.14 9.50
-9 -3 -11 32.13 5.25
-9 -3 -10 105.64 9.10
-9 -3 -9 42.86 6.43
-9 -3 -3 44.53 7.07
-9 -3 -2 39.94 6.90
-9 -3 -2 38.93 6.81
-9 -3 -1 64.94 8.16
-9 -3 -1 63.25 8.19
-9 -3 0 53.21 6.63
-9 -3 0 50.46 7.19
-9 -3 0 49.02 7.35
-9 -3 1 4.94 4.63
-9 -3 1 0.63 4.45
-9 -3 1 8.14 4.65
-9 -3 2 114.15 9.30
-9 -3 2 142.16 9.97
-9 -3 2 109.57 9.91
-9 -3 2 112.32 10.01
-9 -3 3 16.07 4.29
-9 -3 3 9.12 4.67
-9 -3 3 8.99 3.88
-9 -3 3 4.08 4.72
-9 -3 4 54.48 6.26
-9 -3 4 59.06 6.48
-9 -3 4 57.94 6.28
-9 -3 4 43.33 6.48
-9 -3 5 47.87 5.62
-9 -3 5 37.20 5.24
-9 -3 5 36.28 5.58
-9 -3 6 4.82 3.16
-9 -3 6 -0.98 3.07
-9 -3 6 3.29 3.01
-9 -3 7 46.51 5.15
-9 -3 7 47.53 5.22
-9 -2 -12 40.65 5.21
-9 -2 -11 22.46 4.55
-9 -2 -10 129.47 10.29
-9 -2 -10 134.15 10.90
-9 -2 -9 8.23 4.76
-9 -2 -9 0.77 4.73
-9 -2 -8 86.62 9.00
-9 -2 -8 73.12 9.04
-9 -2 -7 56.38 8.49
-9 -2 -6 2.76 5.34
-9 -2 -5 -1.62 4.54
-9 -2 -5 11.19 5.96
-9 -2 -4 53.75 7.81
-9 -2 -4 52.28 8.29
-9 -2 -3 62.13 8.72
-9 -2 -3 45.98 8.36
-9 -2 -3 54.82 9.67
-9 -2 -2 551.88 28.37
-9 -2 -2 502.20 28.22
-9 -2 -2 524.15 29.63
-9 -2 -1 6.80 4.94
-9 -2 -1 6.20 4.16
-9 -2 -1 10.63 5.14
-9 -2 -1 4.06 6.25
-9 -2 -1 5.94 5.33
-9 -2 0 4.66 4.26
-9 -2 0 5.93 5.32
-9 -2 0 7.01 4.67
-9 -2 0 1.63 4.87
-9 -2 0 6.86 6.27
-9 -2 1 1.55 4.27
-9 -2 1 7.54 4.81
-9 -2 1 -3.08 5.34
-9 -2 1 4.80 4.79
-9 -2 2 28.57 5.96
-9 -2 2 32.76 6.61
-9 -2 2 27.41 5.81
-9 -2 2 19.45 5.78
-9 -2 3 31.98 6.12
-9 -2 3 41.90 6.31
-9 -2 3 40.86 7.28
-9 -2 3 29.78 6.02
-9 -2 4 40.87 6.28
-9 -2 4 26.54 6.19
-9 -2 4 31.33 6.13
-9 -2 4 34.13 6.18
-9 -2 4 44.55 6.48
-9 -2 5 7.23 4.74
-9 -2 5 -0.70 4.42
-9 -2 5 1.34 4.26
-9 -2 5 3.11 3.87
-9 -2 5 1.51 4.14
-9 -2 6 7.07 3.98
-9 -2 6 20.11 5.16
-9 -2 6 16.52 4.65
-9 -2 6 9.55 3.62
-9 -2 6 13.67 4.70
-9 -2 7 5.63 4.07
-9 -2 7 6.44 4.12
-9 -2 7 9.41 4.90
-9 -2 8 0.56 3.31
-9 -2 8 -0.58 3.65
-9 -2 8 4.86 3.45
-9 -2 9 3.90 3.12
-9 -2 9 -2.01 3.10
-9 -1 -12 26.15 4.81
-9 -1 -11 18.58 5.70
-9 -1 -10 2.91 4.61
-9 -1 -9 10.46 5.87
-9 -1 -8 5.22 5.05
-9 -1 -7 2.78 5.33
-9 -1 -7 -0.95 6.05
-9 -1 -6 0.80 4.81
-9 -1 -6 1.93 5.60
-9 -1 -6 -0.99 5.81
-9 -1 -5 4.16 4.89
-9 -1 -5 13.81 6.14
-9 -1 -5 7.17 6.38
-9 -1 -4 37.81 7.22
-9 -1 -4 22.11 7.73
-9 -1 -3 183.56 14.05
-9 -1 -3 170.28 14.59
-9 -1 -3 175.66 15.45
-9 -1 -2 159.88 13.28
-9 -1 -2 161.34 12.86
-9 -1 -2 142.83 14.28
-9 -1 -2 147.36 13.52
-9 -1 -1 268.59 17.94
-9 -1 -1 291.23 17.83
-9 -1 -1 257.51 19.26
-9 -1 -1 273.50 18.37
-9 -1 0 332.60 19.26
-9 -1 0 310.13 19.73
-9 -1 0 340.09 19.36
-9 -1 0 294.53 19.25
-9 -1 0 304.66 20.89
-9 -1 1 52.28 7.21
-9 -1 1 45.65 7.08
-9 -1 1 37.46 7.35
-9 -1 1 41.90 8.27
-9 -1 1 40.95 7.08
-9 -1 2 50.42 7.40
-9 -1 2 26.29 6.48
-9 -1 2 38.63 6.70
-9 -1 2 41.59 7.93
-9 -1 3 -0.88 4.49
-9 -1 3 -3.32 4.50
-9 -1 3 -5.94 5.61
-9 -1 3 -3.58 5.91
-9 -1 3 4.47 5.46
-9 -1 4 62.04 8.09
-9 -1 4 79.83 9.09
-9 -1 4 67.79 8.35
-9 -1 4 62.74 8.12
-9 -1 4 95.58 9.71
-9 -1 4 40.92 7.53
-9 -1 5 16.50 5.99
-9 -1 5 29.43 6.37
-9 -1 5 30.92 6.03
-9 -1 5 16.91 5.75
-9 -1 5 29.65 5.58
-9 -1 6 -0.76 4.15
-9 -1 6 -0.79 4.58
-9 -1 6 -4.09 5.18
-9 -1 7 4.36 4.13
-9 -1 7 4.80 4.49
-9 -1 7 -0.75 4.54
-9 -1 7 1.56 4.52
-9 -1 8 5.29 4.22
-9 -1 8 -2.80 4.56
-9 -1 8 -0.68 3.77
-9 -1 8 4.38 4.37
-9 -1 9 19.09 4.74
-9 -1 9 12.31 4.65
-9 -1 9 23.93 5.26
-9 -1 10 66.65 6.50
-9 -1 10 49.45 6.22
-9 -1 10 61.13 6.59
-9 0 -12 11.48 4.35
-9 0 -11 27.68 5.65
-9 0 -10 5.79 4.71
-9 0 -9 6.44 5.15
-9 0 -8 89.30 9.65
-9 0 -8 85.87 10.05
-9 0 -7 3.75 5.66
-9 0 -7 4.63 5.92
-9 0 -6 0.76 4.63
-9 0 -6 -0.98 5.46
-9 0 -6 11.70 6.50
-9 0 -5 225.85 15.36
-9 0 -5 224.98 16.95
-9 0 -5 233.50 17.23
-9 0 -4 1.69 5.11
-9 0 -4 2.08 6.76
-9 0 -4 -1.02 6.09
-9 0 -3 214.18 15.07
-9 0 -3 200.08 16.59
-9 0 -3 183.70 15.67
-9 0 -2 54.01 8.12
-9 0 -2 66.89 9.07
-9 0 -2 42.17 8.76
-9 0 -1 32.73 8.25
-9 0 -1 52.10 8.17
-9 0 0 15.08 5.66
-9 0 0 26.04 5.82
-9 0 0 16.18 6.17
-9 0 0 9.77 6.40
-9 0 1 8.46 5.28
-9 0 1 13.57 5.90
-9 0 1 15.61 5.75
-9 0 1 12.62 5.35
-9 0 1 12.77 6.32
-9 0 2 19.67 6.05
-9 0 2 12.30 6.04
-9 0 2 19.80 6.62
-9 0 2 18.14 5.94
-9 0 2 29.73 7.45
-9 0 3 54.65 8.22
-9 0 3 55.41 8.22
-9 0 3 67.73 9.01
-9 0 3 53.34 7.80
-9 0 3 58.20 7.85
-9 0 3 38.74 8.02
-9 0 4 8.61 4.99
-9 0 4 19.72 6.06
-9 0 4 22.76 5.75
-9 0 4 23.25 6.53
-9 0 4 24.23 5.81
-9 0 4 20.59 5.86
-9 0 5 199.90 14.27
-9 0 5 197.95 13.95
-9 0 5 179.02 13.69
-9 0 5 186.89 13.63
-9 0 5 183.83 14.31
-9 0 5 156.94 13.64
-9 0 6 68.64 8.22
-9 0 6 77.43 8.69
-9 0 6 67.00 8.78
-9 0 6 60.20 8.03
-9 0 6 65.61 8.37
-9 0 7 81.81 9.48
-9 0 7 74.98 8.77
-9 0 7 94.71 9.12
-9 0 7 94.76 9.14
-9 0 7 99.96 9.63
-9 0 8 38.23 6.35
-9 0 8 20.47 5.87
-9 0 8 35.78 6.34
-9 0 8 34.85 6.21
-9 0 8 43.32 6.11
-9 0 9 17.14 4.94
-9 0 9 16.68 4.81
-9 0 9 18.62 5.33
-9 0 9 19.39 5.06
-9 0 9 20.65 4.63
-9 0 10 49.11 6.30
-9 0 10 51.75 5.97
-9 0 10 41.50 6.17
-9 0 10 45.92 6.29
-9 1 -11 35.86 6.14
-9 1 -10 31.25 6.43
-9 1 -9 12.20 5.84
-9 1 -9 21.67 5.68
-9 1 -8 68.52 9.16
-9 1 -8 74.23 8.89
-9 1 -7 25.79 6.27
-9 1 -7 18.00 6.47
-9 1 -6 52.93 6.97
-9 1 -6 34.79 7.46
-9 1 -6 50.45 8.54
-9 1 -5 2.90 4.08
-9 1 -5 1.92 5.34
-9 1 -5 -0.99 5.68
-9 1 -4 26.65 6.85
-9 1 -4 27.29 6.13
-9 1 -4 24.97 6.89
-9 1 -4 31.15 7.48
-9 1 -3 37.92 7.44
-9 1 -3 24.70 6.27
-9 1 -3 30.07 7.30
-9 1 -3 47.41 8.98
-9 1 -2 32.42 6.83
-9 1 -2 13.72 5.39
-9 1 -2 13.78 6.11
-9 1 -2 27.43 7.61
-9 1 -1 11.06 5.58
-9 1 -1 11.50 5.91
-9 1 -1 8.28 5.21
-9 1 -1 5.36 5.96
-9 1 -1 11.42 5.76
-9 1 0 119.91 11.29
-9 1 0 114.16 11.19
-9 1 0 124.07 11.34
-9 1 0 104.98 10.28
-9 1 0 126.17 12.72
-9 1 1 66.26 8.46
-9 1 1 43.19 7.72
-9 1 1 54.70 7.65
-9 1 1 47.48 7.57
-9 1 1 36.79 7.72
-9 1 1 46.11 8.90
-9 1 1 27.26 6.99
-9 1 2 154.49 13.46
-9 1 2 183.72 13.81
-9 1 2 170.79 12.96
-9 1 2 164.65 13.80
-9 1 2 195.39 13.68
-9 1 2 147.69 14.42
-9 1 3 -4.06 5.50
-9 1 3 2.72 5.31
-9 1 3 4.23 4.59
-9 1 3 8.43 5.55
-9 1 3 -3.33 4.62
-9 1 3 -6.03 6.19
-9 1 4 17.52 6.09
-9 1 4 32.16 6.82
-9 1 4 16.79 5.62
-9 1 4 27.07 6.99
-9 1 4 27.12 6.01
-9 1 4 27.47 7.09
-9 1 5 128.77 11.36
-9 1 5 123.43 11.59
-9 1 5 125.68 10.98
-9 1 5 141.29 12.24
-9 1 5 120.80 10.61
-9 1 5 105.26 11.51
-9 1 6 107.70 10.08
-9 1 6 115.98 10.46
-9 1 6 102.66 10.67
-9 1 6 104.78 9.83
-9 1 6 89.46 9.37
-9 1 6 86.84 9.60
-9 1 7 59.32 7.38
-9 1 7 57.36 7.19
-9 1 7 54.15 8.27
-9 1 7 52.34 7.38
-9 1 7 63.06 8.02
-9 1 8 2.39 4.77
-9 1 8 -4.28 4.39
-9 1 8 0.74 4.36
-9 1 8 6.01 4.27
-9 1 8 3.82 4.34
-9 1 9 50.95 7.08
-9 1 9 56.79 6.94
-9 1 9 58.32 7.10
-9 1 9 37.16 6.45
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7 -5 10 -4.22 4.85
7 -5 11 148.50 11.06
7 -5 11 193.33 11.30
7 -4 -16 24.37 4.38
7 -4 -16 25.04 4.46
7 -4 -15 9.23 4.27
7 -4 -15 7.15 3.93
7 -4 -14 46.72 6.44
7 -4 -14 40.72 6.16
7 -4 -13 5.60 4.55
7 -4 -13 2.13 3.98
7 -4 -12 -3.08 4.61
7 -4 -11 6.12 4.98
7 -4 -10 12.85 5.88
7 -4 -10 11.51 5.22
7 -4 -10 11.90 5.18
7 -4 -9 159.67 14.02
7 -4 -9 187.91 13.57
7 -4 -9 157.19 12.57
7 -4 -8 76.24 8.91
7 -4 -8 66.04 9.67
7 -4 -8 77.95 8.25
7 -4 -7 2.70 5.06
7 -4 -7 -3.21 4.25
7 -4 -6 109.96 11.20
7 -4 -6 107.18 11.69
7 -4 -6 101.37 9.84
7 -4 -5 1.91 5.18
7 -4 -5 1.06 6.13
7 -4 -5 13.44 5.37
7 -4 -4 123.33 11.65
7 -4 -4 106.46 11.47
7 -4 -4 109.86 10.98
7 -4 -3 62.99 8.99
7 -4 -3 40.07 8.50
7 -4 -3 64.47 8.67
7 -4 -2 19.27 6.41
7 -4 -2 18.17 6.43
7 -4 -1 58.25 9.09
7 -4 0 19.89 6.77
7 -4 1 7.86 5.46
7 -4 2 12.58 6.31
7 -4 4 21.24 6.89
7 -4 5 2.97 5.23
7 -4 6 20.22 6.51
7 -4 7 0.93 5.86
7 -4 7 1.92 4.66
7 -4 8 46.76 7.42
7 -4 9 113.26 10.64
7 -4 9 98.06 10.04
7 -4 10 156.01 12.35
7 -4 10 154.11 12.00
7 -4 11 246.95 15.17
7 -4 12 -1.78 4.08
7 -4 13 82.69 7.95
7 -4 13 90.88 7.53
7 -3 -16 6.68 3.67
7 -3 -16 6.57 3.38
7 -3 -15 -4.80 4.85
7 -3 -15 -0.59 3.70
7 -3 -14 243.15 15.57
7 -3 -14 283.73 15.91
7 -3 -13 159.31 12.07
7 -3 -13 166.07 12.25
7 -3 -12 35.47 6.54
7 -3 -12 25.92 6.55
7 -3 -12 33.69 5.88
7 -3 -11 35.66 7.41
7 -3 -11 46.99 7.56
7 -3 -10 0.98 5.26
7 -3 -10 4.15 4.77
7 -3 -10 6.10 5.16
7 -3 -9 -3.11 6.14
7 -3 -9 0.85 4.27
7 -3 -9 0.89 5.04
7 -3 -8 54.29 9.29
7 -3 -8 78.16 9.15
7 -3 -7 74.27 10.07
7 -3 -7 68.60 8.59
7 -3 -6 194.46 15.60
7 -3 -6 202.72 14.88
7 -3 -5 38.24 8.02
7 -3 -5 42.10 7.65
7 -3 -4 385.62 22.44
7 -3 -4 374.20 23.01
7 -3 -4 382.90 21.60
7 -3 -3 37.07 8.01
7 -3 -3 50.02 7.67
7 -3 -2 18.25 6.79
7 -3 -1 -5.01 6.00
7 -3 0 19.82 6.09
7 -3 1 107.81 11.36
7 -3 2 61.10 9.04
7 -3 3 164.76 13.90
7 -3 4 206.19 15.39
7 -3 6 10.76 5.69
7 -3 7 15.15 5.92
7 -3 8 108.19 10.77
7 -3 9 30.02 7.02
7 -3 10 -0.83 4.67
7 -3 10 -2.54 4.64
7 -3 11 98.88 9.47
7 -3 11 79.12 8.83
7 -3 12 22.52 5.39
7 -3 13 31.72 5.54
7 -3 14 7.61 3.83
7 -2 -17 14.67 3.65
7 -2 -17 13.21 3.87
7 -2 -16 1.58 3.51
7 -2 -16 1.49 3.18
7 -2 -16 0.58 3.51
7 -2 -15 34.53 5.83
7 -2 -15 51.79 6.17
7 -2 -14 50.61 7.14
7 -2 -14 47.22 6.53
7 -2 -13 -0.82 4.93
7 -2 -13 3.62 3.82
7 -2 -12 200.60 14.80
7 -2 -12 221.58 14.53
7 -2 -11 38.94 7.56
7 -2 -11 37.01 6.64
7 -2 -10 32.93 6.44
7 -2 -10 39.30 7.73
7 -2 -9 9.03 5.06
7 -2 -9 -0.92 5.17
7 -2 -8 7.50 4.74
7 -2 -7 258.87 16.73
7 -2 -6 159.99 12.75
7 -2 -5 223.95 15.53
7 -2 -4 2.70 4.99
7 -2 -3 205.60 15.69
7 -2 -2 12.65 5.23
7 -2 -1 184.36 14.52
7 -2 0 5.72 5.66
7 -2 1 268.91 18.19
7 -2 2 17.84 6.04
7 -2 3 183.03 14.26
7 -2 4 5.28 5.22
7 -2 7 35.06 6.84
7 -2 8 8.90 5.07
7 -2 9 35.23 6.75
7 -2 10 1.65 5.09
7 -2 11 6.47 5.26
7 -2 12 55.53 7.49
7 -2 13 1.33 4.52
7 -2 14 140.19 10.11
7 -1 -17 37.65 4.50
7 -1 -17 42.80 5.32
7 -1 -16 183.99 11.18
7 -1 -16 172.99 11.68
7 -1 -15 5.86 3.88
7 -1 -15 8.34 3.59
7 -1 -15 5.21 4.28
7 -1 -14 109.37 9.43
7 -1 -14 100.53 9.67
7 -1 -14 95.88 8.55
7 -1 -13 12.46 5.51
7 -1 -13 12.44 4.63
7 -1 -12 -1.80 5.60
7 -1 -12 2.82 3.86
7 -1 -11 12.16 5.79
7 -1 -11 14.22 4.85
7 -1 -10 97.69 10.64
7 -1 -9 30.04 6.25
7 -1 -9 42.18 7.59
7 -1 -9 32.14 6.20
7 -1 -8 57.26 7.55
7 -1 -7 24.75 5.63
7 -1 -6 56.86 7.40
7 -1 -5 5.64 4.83
7 -1 -5 5.87 5.62
7 -1 -4 663.83 32.23
7 -1 -4 667.24 33.47
7 -1 -3 161.35 13.63
7 -1 -2 709.21 34.86
7 -1 -1 115.15 11.29
7 -1 0 29.83 6.45
7 -1 1 309.06 19.54
7 -1 2 3.53 5.34
7 -1 2 1.88 4.97
7 -1 3 29.48 6.73
7 -1 4 5.85 5.16
7 -1 7 50.05 8.13
7 -1 8 35.80 6.63
7 -1 8 36.71 7.08
7 -1 9 -1.04 5.72
7 -1 12 2.92 4.20
7 0 -16 191.99 11.79
7 0 -15 16.18 3.92
7 0 -15 6.57 4.19
7 0 -14 68.59 6.98
7 0 -14 55.58 7.12
7 0 -13 -1.61 4.52
7 0 -13 -0.67 4.34
7 0 -13 -4.35 4.88
7 0 -12 3.49 5.11
7 0 -11 -6.48 5.97
7 0 -10 25.59 6.97
7 0 -9 90.32 10.35
7 0 -8 13.02 5.91
7 0 -4 95.22 10.52
7 0 -3 11.67 5.66
7 0 -2 176.60 14.21
7 0 -1 101.33 10.64
7 0 0 4.63 4.83
7 0 1 2.75 5.21
7 0 2 67.56 8.43
7 0 3 41.12 7.73
7 0 4 83.56 9.96
7 0 5 97.49 10.44
7 0 7 41.32 7.22
7 0 8 237.31 16.93
7 0 9 7.06 4.99
7 0 10 18.42 6.28
7 1 -16 70.75 6.12
7 1 -15 25.37 4.51
7 1 -14 4.01 4.00
7 1 -13 36.38 5.95
7 1 -13 22.24 4.92
7 1 -12 33.82 6.95
7 1 -12 40.34 6.20
7 1 -11 118.19 10.78
7 1 -11 95.15 9.25
7 1 -10 111.47 11.09
7 1 -9 428.81 24.05
7 1 -8 -1.84 5.72
7 1 -7 408.73 23.14
7 1 -6 146.67 12.28
7 1 -3 24.34 6.49
7 1 -2 5.93 5.36
7 1 -1 145.54 12.77
7 1 0 23.55 6.34
7 1 1 24.97 6.28
7 1 2 74.89 8.93
7 1 3 14.48 5.28
7 1 4 7.15 4.61
7 1 5 85.55 9.22
7 1 6 154.45 12.56
7 1 8 386.01 22.95
7 1 9 16.57 5.51
7 1 10 49.56 8.08
7 2 -11 93.69 9.34
7 2 -10 24.26 5.92
7 2 -9 314.61 19.12
7 2 -8 320.21 19.71
7 2 -7 113.75 10.86
7 2 -6 1.72 4.78
7 2 -5 -0.84 5.46
7 2 -4 260.23 16.62
7 2 1 27.64 6.33
7 2 2 18.63 5.39
7 2 3 20.08 5.62
7 2 4 2.68 3.85
7 2 5 310.55 18.93
7 2 8 3.95 4.81
7 2 8 6.47 4.76
7 2 9 77.80 9.35
7 2 10 2.89 5.35
7 3 -13 6.57 3.33
7 3 -12 80.38 7.49
7 3 -11 13.77 4.33
7 3 -10 175.51 12.25
7 3 -9 19.59 5.11
7 3 5 146.58 12.68
7 3 6 78.79 9.50
7 3 7 158.50 13.50
7 3 13 40.19 7.06
7 4 -12 10.05 3.50
7 4 -11 12.43 3.98
7 4 -11 6.81 4.63
7 4 -10 152.16 10.98
7 4 -9 6.02 4.09
7 4 11 18.85 5.71
7 4 12 8.40 4.67
7 4 17 57.07 5.44
7 5 -10 1.45 3.29
7 5 -9 1.11 3.44
7 5 -9 2.69 4.02
7 5 -8 12.58 4.75
7 5 2 23.42 5.89
7 5 3 70.32 8.24
7 5 4 -0.91 4.42
7 5 8 143.01 12.51
7 6 -5 106.75 10.00
7 6 -4 5.18 4.06
7 6 -3 -1.51 4.74
7 6 -2 7.91 4.29
7 6 -2 8.29 4.83
7 6 -1 -1.35 3.87
7 7 3 57.83 7.04
8 -6 -8 3.09 3.93
8 -6 -7 26.49 5.36
8 -6 -6 5.39 4.21
8 -6 -5 53.84 6.76
8 -6 -5 45.24 5.74
8 -6 -4 21.94 5.60
8 -6 -4 24.20 4.67
8 -6 -3 96.10 8.98
8 -6 -3 102.34 8.39
8 -6 -2 -2.45 4.70
8 -6 -2 8.40 3.67
8 -6 -1 5.95 4.20
8 -6 -1 8.50 4.18
8 -6 0 5.13 3.77
8 -6 0 0.61 3.56
8 -6 1 -0.54 3.52
8 -6 1 -1.20 3.10
8 -6 2 29.01 4.88
8 -6 2 23.60 4.89
8 -6 3 3.88 3.26
8 -6 3 1.14 3.55
8 -6 4 -2.71 3.73
8 -5 -11 4.56 3.30
8 -5 -11 -3.19 3.76
8 -5 -6 33.76 5.45
8 -5 -6 21.79 5.58
8 -5 -5 26.15 5.00
8 -5 -5 20.97 5.37
8 -5 -4 92.78 8.66
8 -5 -4 91.63 9.12
8 -5 -3 75.47 8.05
8 -5 -3 54.74 7.60
8 -5 -2 23.46 5.85
8 -5 -2 16.83 5.73
8 -5 -2 23.03 5.64
8 -5 -1 3.10 4.10
8 -5 -1 12.01 5.21
8 -5 -1 4.63 4.63
8 -5 0 -0.78 4.29
8 -5 0 1.54 4.79
8 -5 0 -1.59 4.66
8 -5 1 32.06 6.24
8 -5 1 33.68 6.37
8 -5 1 30.83 6.08
8 -5 1 33.00 6.35
8 -5 2 -2.26 4.69
8 -5 2 -1.56 4.75
8 -5 2 -2.32 4.93
8 -5 2 2.66 4.05
8 -5 3 0.77 4.50
8 -5 3 5.29 4.39
8 -5 3 6.12 4.49
8 -5 4 55.47 7.57
8 -5 4 60.53 6.73
8 -5 4 68.75 8.12
8 -5 6 1.21 3.72
8 -5 7 153.06 10.72
8 -5 8 10.43 4.14
8 -4 -13 18.50 3.83
8 -4 -13 27.67 4.77
8 -4 -12 81.73 7.23
8 -4 -12 75.11 7.54
8 -4 -11 -1.17 3.65
8 -4 -9 30.77 5.92
8 -4 -8 28.98 5.82
8 -4 -7 158.17 12.21
8 -4 -6 4.64 5.45
8 -4 -6 18.20 5.25
8 -4 -5 202.19 13.34
8 -4 -5 201.25 15.86
8 -4 -5 212.32 14.50
8 -4 -4 -2.25 4.35
8 -4 -4 -1.89 5.37
8 -4 -4 0.86 4.91
8 -4 -3 3.97 4.20
8 -4 -3 -0.94 4.71
8 -4 -3 4.39 4.76
8 -4 -2 -1.67 4.68
8 -4 -2 -2.78 5.26
8 -4 -2 12.54 5.47
8 -4 -1 6.92 4.97
8 -4 -1 7.30 5.01
8 -4 -1 9.08 5.39
8 -4 0 10.71 5.86
8 -4 0 6.21 4.93
8 -4 1 38.34 7.22
8 -4 1 40.52 7.17
8 -4 2 10.98 5.70
8 -4 3 18.72 6.08
8 -4 4 5.34 4.90
8 -4 4 4.31 4.95
8 -4 5 223.88 15.39
8 -4 6 10.23 5.17
8 -4 7 125.17 10.52
8 -4 8 25.68 5.62
8 -4 9 21.45 4.87
8 -4 10 94.97 7.99
8 -3 -14 -1.54 3.14
8 -3 -14 3.20 3.12
8 -3 -13 102.66 7.90
8 -3 -13 111.78 8.79
8 -3 -12 1.64 3.50
8 -3 -11 29.02 5.38
8 -3 -10 72.15 7.64
8 -3 -9 2.84 4.08
8 -3 -9 2.34 4.06
8 -3 -8 170.83 12.75
8 -3 -8 189.95 13.44
8 -3 -7 57.10 8.84
8 -3 -7 58.89 7.49
8 -3 -6 6.04 5.46
8 -3 -6 2.46 4.27
8 -3 -5 14.21 6.64
8 -3 -5 22.26 5.97
8 -3 -4 -3.03 5.42
8 -3 -4 -5.31 5.20
8 -3 -3 36.05 7.65
8 -3 -3 37.51 7.39
8 -3 -2 7.39 4.46
8 -3 -2 6.91 5.74
8 -3 -2 15.97 5.69
8 -3 -1 14.58 6.49
8 -3 -1 9.51 4.93
8 -3 0 40.10 7.51
8 -3 1 7.48 5.49
8 -3 2 209.44 15.68
8 -3 3 9.51 6.04
8 -3 4 335.33 20.56
8 -3 5 47.65 7.66
8 -3 6 6.83 5.06
8 -3 7 128.11 11.22
8 -3 8 16.57 5.29
8 -3 9 52.89 7.34
8 -3 9 55.35 7.25
8 -3 10 3.15 3.99
8 -3 11 9.88 3.99
8 -2 -14 20.32 4.05
8 -2 -13 18.47 4.81
8 -2 -12 14.94 4.10
8 -2 -11 -2.34 3.50
8 -2 -10 12.25 4.25
8 -2 -10 14.39 5.44
8 -2 -9 4.83 4.41
8 -2 -9 0.93 5.18
8 -2 -9 6.63 5.16
8 -2 -8 -4.37 4.48
8 -2 -8 7.72 5.03
8 -2 -7 8.38 5.00
8 -2 -6 30.95 6.00
8 -2 -5 27.89 7.07
8 -2 -5 26.55 6.16
8 -2 -4 35.96 7.84
8 -2 -4 34.39 6.47
8 -2 -3 155.44 13.88
8 -2 -3 169.94 13.26
8 -2 -2 46.17 8.65
8 -2 -2 54.16 8.17
8 -2 -1 78.32 9.91
8 -2 0 214.79 15.99
8 -2 1 175.78 14.27
8 -2 2 128.57 11.79
8 -2 3 16.83 5.84
8 -2 6 14.01 5.67
8 -2 7 1.64 4.56
8 -2 8 4.61 4.27
8 -2 10 16.27 4.91
8 -2 11 26.15 5.08
8 -2 12 79.39 7.23
8 -1 -14 2.18 3.10
8 -1 -14 6.05 3.53
8 -1 -13 44.54 6.03
8 -1 -13 38.74 5.74
8 -1 -10 3.32 5.36
8 -1 -9 8.57 5.29
8 -1 -8 7.04 5.00
8 -1 -5 29.42 5.78
8 -1 -4 32.42 6.25
8 -1 -3 39.52 6.77
8 -1 -2 120.36 10.85
8 -1 0 89.87 10.37
8 -1 1 196.38 14.91
8 -1 2 33.86 7.25
8 -1 3 73.41 8.88
8 -1 7 3.98 4.63
8 0 -13 23.83 4.47
8 0 -13 24.17 4.06
8 0 -12 8.90 3.86
8 0 -12 11.12 3.90
8 0 -11 67.81 7.13
8 0 -10 132.54 11.41
8 0 -9 48.06 7.58
8 0 -8 144.53 12.32
8 0 -7 -0.89 5.88
8 1 -9 0.79 5.19
8 1 -8 127.13 11.38
8 1 -7 5.97 5.31
8 1 -6 285.07 17.92
8 1 -5 7.73 4.83
8 2 -7 -3.75 5.27
8 2 -6 51.83 7.40
8 2 -5 18.86 5.61
8 2 -4 -8.57 5.49
8 2 -3 55.77 7.43
8 5 -6 72.46 6.37
8 5 -3 -0.68 4.02
9 -5 -3 14.92 4.53
9 -5 -2 10.69 4.01
9 -5 -1 55.46 5.92
9 -5 0 11.32 3.90
9 -5 1 5.09 3.30
9 -4 -8 1.23 3.06
9 -4 0 5.43 3.74
9 -4 1 32.69 5.32
9 -4 1 40.02 5.43
9 -4 2 3.88 3.48
9 -4 2 -0.58 3.71
9 -4 3 57.79 6.66
9 -4 4 35.98 5.37
9 -4 5 36.00 5.58
9 -3 -2 304.87 17.48
9 -3 -1 95.40 9.12
9 -3 0 20.44 5.51
9 -3 1 121.81 10.42
9 -3 2 4.40 3.76
9 -3 2 3.01 4.18
9 -3 3 3.87 3.71
9 -3 3 9.35 4.56
9 -3 4 46.96 6.93
9 -2 -4 203.30 13.00
9 -2 -3 100.41 9.07
9 -2 -2 93.67 8.78
9 -2 -1 136.48 10.89
9 -2 0 137.90 11.01
9 -2 4 45.02 6.81
9 -2 5 10.28 4.36
9 -1 -11 7.44 3.47
9 -1 -2 136.39 12.40
9 -1 -1 41.72 7.04
9 -1 0 106.69 9.36
9 -1 1 20.53 5.10
9 -1 5 2.07 3.60
9 0 -10 47.23 5.31
9 0 -5 193.62 13.46
9 0 -1 5.88 5.08
9 0 0 13.01 5.40
9 1 -3 0.72 4.02
0 0 0 0.00 0.00
TITL exp_104257 in P1
REM P1 (#1 in standard setting)
CELL 1.54184 8.675168 8.876457 20.229937 78.1070 87.9216 89.5121
ZERR 4.00 0.000232 0.000241 0.000646 0.0025 0.0024 0.0022
LATT -1
SFAC C H N O Si S
UNIT 144.00 96.00 12.00 12.00 4.00 4.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.06 0.16 0.21
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 43930
_shelx_res_file
;
TITL exp_104257_a.res in P-1
exp_104257.res
created by SHELXL-2018/1 at 16:27:34 on 21-Apr-2022
REM Old TITL exp_104257 in P1
REM SHELXT solution in P-1
REM R1 0.116, Rweak 0.007, Alpha 0.053, Orientation as input
REM Formula found by SHELXT: C32 N3 O1 Si S
CELL 1.54184 8.6752 8.8765 20.2299 78.107 87.922 89.512
ZERR 2 0.0002 0.0002 0.0006 0.002 0.002 0.002
LATT 1
SFAC C H N O S Si
UNIT 64 82 6 6 2 2
L.S. 20 0 0
PLAN 9
SIZE 0.06 0.16 0.21
TEMP -173
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM
REM
REM
WGHT 0.057500 0.426900
FVAR 0.61308
S1 5 0.642420 0.369213 0.761797 11.00000 0.01866 0.01572 =
0.02224 -0.00441 0.00128 -0.00142
SI 6 0.822527 0.581766 0.830462 11.00000 0.01915 0.01613 =
0.02411 -0.00497 0.00010 -0.00130
O1 4 0.532738 0.431704 0.698426 11.00000 0.02098 0.02050 =
0.02315 -0.00607 -0.00091 0.00173
O2 4 0.371331 0.928266 0.671342 11.00000 0.03069 0.02738 =
0.02932 -0.00990 0.00140 0.00353
O3 4 0.618706 0.637449 0.538263 11.00000 0.03096 0.02482 =
0.03243 -0.00718 0.00342 0.00118
N1 3 0.758072 0.262075 0.737558 11.00000 0.02175 0.01649 =
0.02850 -0.00434 0.00279 -0.00091
N3 3 0.478578 0.750102 0.614757 11.00000 0.02159 0.01972 =
0.02477 -0.00480 -0.00038 -0.00073
N2 3 0.677665 0.502504 0.792487 11.00000 0.02003 0.01737 =
0.02845 -0.00789 -0.00085 -0.00090
C17 1 0.516932 0.238041 0.815608 11.00000 0.01730 0.01446 =
0.02498 -0.00284 0.00156 0.00009
C11 1 0.881232 0.308063 0.690290 11.00000 0.02000 0.02182 =
0.02583 -0.01246 0.00065 -0.00338
C4 1 0.659771 0.903847 0.547808 11.00000 0.02218 0.02425 =
0.02406 -0.00202 -0.00590 -0.00043
C30 1 0.867138 0.777312 0.777091 11.00000 0.02735 0.01920 =
0.02957 -0.00792 -0.00169 -0.00597
AFIX 13
H30 2 0.941234 0.829050 0.801923 11.00000 -1.20000
AFIX 0
C16 1 1.008876 0.210431 0.694742 11.00000 0.02422 0.02374 =
0.03002 -0.01114 -0.00122 0.00108
AFIX 43
H16 2 1.013655 0.123095 0.730762 11.00000 -1.20000
AFIX 0
C9 1 0.585006 0.992583 0.588213 11.00000 0.02651 0.02473 =
0.02293 -0.00397 -0.00669 -0.00263
C20 1 0.330110 0.024352 0.901489 11.00000 0.02035 0.01876 =
0.03443 -0.00148 0.00518 -0.00006
C18 1 0.512868 0.234182 0.883891 11.00000 0.02317 0.01888 =
0.02639 -0.00563 0.00084 -0.00159
AFIX 43
H18 2 0.573253 0.304358 0.901627 11.00000 -1.20000
AFIX 0
C3 1 0.590107 0.747285 0.563548 11.00000 0.02129 0.02306 =
0.02296 -0.00345 -0.00296 0.00079
C21 1 0.336014 0.030399 0.832085 11.00000 0.02234 0.01926 =
0.03954 -0.00777 -0.00167 -0.00334
AFIX 43
H21 2 0.275146 -0.039010 0.814108 11.00000 -1.20000
AFIX 0
C10 1 0.465384 0.895469 0.630899 11.00000 0.02486 0.02275 =
0.02348 -0.00609 -0.00658 0.00110
C12 1 0.878355 0.437948 0.638147 11.00000 0.02261 0.02257 =
0.02853 -0.00975 0.00016 -0.00119
AFIX 43
H12 2 0.792938 0.506435 0.634980 11.00000 -1.20000
AFIX 0
C22 1 0.429262 0.136051 0.788776 11.00000 0.02601 0.02299 =
0.02589 -0.00759 0.00086 -0.00164
AFIX 43
H22 2 0.433214 0.138741 0.741556 11.00000 -1.20000
AFIX 0
C1 1 0.403273 0.530910 0.707668 11.00000 0.01876 0.02395 =
0.02644 -0.00543 0.00254 0.00103
AFIX 23
H1A 2 0.429808 0.598387 0.738910 11.00000 -1.20000
H1B 2 0.312386 0.468228 0.727047 11.00000 -1.20000
AFIX 0
C19 1 0.419986 0.127113 0.926862 11.00000 0.02806 0.02294 =
0.02475 -0.00317 0.00369 0.00180
AFIX 43
H19 2 0.417784 0.123993 0.974110 11.00000 -1.20000
AFIX 0
C24 1 0.999048 0.455630 0.836412 11.00000 0.02175 0.02395 =
0.02827 -0.00765 -0.00077 0.00003
AFIX 13
H24 2 1.024122 0.441481 0.789435 11.00000 -1.20000
AFIX 0
C2 1 0.368093 0.626402 0.639326 11.00000 0.01944 0.02300 =
0.02874 -0.00416 0.00099 -0.00341
AFIX 23
H2A 2 0.366244 0.558188 0.606327 11.00000 -1.20000
H2B 2 0.263929 0.671795 0.641762 11.00000 -1.20000
AFIX 0
C13 1 0.999895 0.467422 0.590884 11.00000 0.03106 0.02554 =
0.02842 -0.01002 0.00474 -0.00907
AFIX 43
H13 2 0.997509 0.556827 0.555804 11.00000 -1.20000
AFIX 0
C27 1 0.742146 0.596960 0.917165 11.00000 0.02305 0.02514 =
0.02650 -0.00738 -0.00008 0.00039
AFIX 13
H27 2 0.750357 0.492007 0.946548 11.00000 -1.20000
AFIX 0
C8 1 0.621620 1.146166 0.583210 11.00000 0.04022 0.02672 =
0.02920 -0.00677 -0.00732 -0.00266
AFIX 43
H8 2 0.570588 1.207038 0.610828 11.00000 -1.20000
AFIX 0
C28 1 0.570806 0.642910 0.919039 11.00000 0.02558 0.03212 =
0.03289 -0.01306 0.00392 -0.00042
AFIX 137
H28A 2 0.558879 0.749867 0.894987 11.00000 -1.50000
H28B 2 0.533930 0.632856 0.966109 11.00000 -1.50000
H28C 2 0.510518 0.575262 0.897214 11.00000 -1.50000
AFIX 0
C25 1 0.972129 0.293344 0.879416 11.00000 0.02632 0.02480 =
0.03763 -0.00550 -0.00679 0.00439
AFIX 137
H25A 2 0.947197 0.300481 0.926309 11.00000 -1.50000
H25B 2 1.065707 0.231402 0.877778 11.00000 -1.50000
H25C 2 0.886315 0.244644 0.861586 11.00000 -1.50000
AFIX 0
C5 1 0.774988 0.963574 0.501171 11.00000 0.02415 0.03042 =
0.02737 0.00081 -0.00351 -0.00121
AFIX 43
H5 2 0.826384 0.902115 0.473913 11.00000 -1.20000
AFIX 0
C15 1 1.129095 0.240551 0.646632 11.00000 0.02107 0.03274 =
0.04090 -0.01827 0.00145 0.00009
AFIX 43
H15 2 1.215207 0.172932 0.649736 11.00000 -1.20000
AFIX 0
C14 1 1.124574 0.368281 0.594172 11.00000 0.02407 0.03497 =
0.03646 -0.01934 0.00850 -0.01036
AFIX 43
H14 2 1.206057 0.387532 0.560883 11.00000 -1.20000
AFIX 0
C7 1 0.736976 1.207136 0.535693 11.00000 0.04193 0.02838 =
0.03185 -0.00140 -0.01112 -0.01369
AFIX 43
H7 2 0.764486 1.312400 0.530483 11.00000 -1.20000
AFIX 0
C23 1 0.228434 -0.090125 0.948462 11.00000 0.03009 0.02886 =
0.04405 0.00075 0.00865 -0.00603
AFIX 137
H23A 2 0.120046 -0.067014 0.938481 11.00000 -1.50000
H23B 2 0.246165 -0.083527 0.995349 11.00000 -1.50000
H23C 2 0.252958 -0.194293 0.942108 11.00000 -1.50000
AFIX 0
C26 1 1.143480 0.527304 0.859378 11.00000 0.02194 0.03567 =
0.04354 -0.01113 -0.00111 0.00017
AFIX 137
H26A 2 1.161285 0.629633 0.830942 11.00000 -1.50000
H26B 2 1.233053 0.461466 0.855196 11.00000 -1.50000
H26C 2 1.128079 0.536457 0.906621 11.00000 -1.50000
AFIX 0
C29 1 0.837426 0.705552 0.949954 11.00000 0.02929 0.05207 =
0.03685 -0.02544 0.00089 -0.00352
AFIX 137
H29A 2 0.945592 0.672665 0.951077 11.00000 -1.50000
H29B 2 0.797407 0.702220 0.996161 11.00000 -1.50000
H29C 2 0.829942 0.810909 0.923502 11.00000 -1.50000
AFIX 0
C6 1 0.812557 1.117910 0.495842 11.00000 0.02969 0.03527 =
0.02902 0.00111 -0.00534 -0.01022
AFIX 43
H6 2 0.891433 1.162922 0.464320 11.00000 -1.20000
AFIX 0
C31 1 0.721784 0.877148 0.766546 11.00000 0.03717 0.02067 =
0.06504 0.00748 -0.00837 -0.00188
AFIX 137
H31A 2 0.639953 0.820185 0.750234 11.00000 -1.50000
H31B 2 0.744630 0.971775 0.733154 11.00000 -1.50000
H31C 2 0.687716 0.903397 0.809501 11.00000 -1.50000
AFIX 0
C32 1 0.943137 0.767733 0.708925 11.00000 0.07891 0.02656 =
0.03779 -0.00448 0.01903 -0.00979
AFIX 137
H32A 2 1.035816 0.703364 0.716090 11.00000 -1.50000
H32B 2 0.971724 0.871329 0.684381 11.00000 -1.50000
H32C 2 0.870715 0.722351 0.682492 11.00000 -1.50000
AFIX 0
HKLF 4
REM exp_104257_a.res in P-1
REM R1 = 0.0408 for 4426 Fo > 4sig(Fo) and 0.0518 for all 5410 data
REM 368 parameters refined using 0 restraints
END
WGHT 0.0575 0.4269
REM Highest difference peak 0.556, deepest hole -0.379, 1-sigma level 0.051
Q1 1 0.7814 0.5845 0.8780 11.00000 0.05 0.56
Q2 1 0.7079 0.3585 0.7187 11.00000 0.05 0.32
Q3 1 0.9267 0.5167 0.8418 11.00000 0.05 0.29
Q4 1 0.5909 0.4023 0.7176 11.00000 0.05 0.28
Q5 1 0.4827 0.2662 0.8427 11.00000 0.05 0.24
Q6 1 0.2875 0.0578 0.8639 11.00000 0.05 0.23
Q7 1 0.3559 0.1130 0.8194 11.00000 0.05 0.21
Q8 1 0.9390 0.4411 0.6149 11.00000 0.05 0.21
Q9 1 0.5649 0.2045 0.8420 11.00000 0.05 0.20
;
_shelx_res_checksum 76433
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.64242(5) 0.36921(5) 0.76180(2) 0.01884(13) Uani d 1 . .
Si Si 0.82253(6) 0.58177(6) 0.83046(3) 0.01969(14) Uani d 1 . .
O O1 0.53274(15) 0.43170(15) 0.69843(7) 0.0213(3) Uani d 1 . .
O O2 0.37133(16) 0.92827(16) 0.67134(7) 0.0286(3) Uani d 1 . .
O O3 0.61871(16) 0.63745(16) 0.53826(7) 0.0293(3) Uani d 1 . .
N N1 0.75807(18) 0.26207(18) 0.73756(9) 0.0224(4) Uani d 1 . .
N N3 0.47858(18) 0.75010(18) 0.61476(8) 0.0220(4) Uani d 1 . .
N N2 0.67766(18) 0.50250(18) 0.79249(8) 0.0215(4) Uani d 1 . .
C C17 0.5169(2) 0.2380(2) 0.81561(10) 0.0191(4) Uani d 1 . .
C C11 0.8812(2) 0.3081(2) 0.69029(10) 0.0215(4) Uani d 1 . .
C C4 0.6598(2) 0.9038(2) 0.54781(10) 0.0238(4) Uani d 1 . .
C C30 0.8671(2) 0.7773(2) 0.77709(11) 0.0249(5) Uani d 1 . .
H H30 0.941234 0.829050 0.801923 0.030 Uiso calc 1 . .
C C16 1.0089(2) 0.2104(2) 0.69474(11) 0.0252(5) Uani d 1 . .
H H16 1.013655 0.123095 0.730762 0.030 Uiso calc 1 . .
C C9 0.5850(2) 0.9926(2) 0.58821(10) 0.0247(4) Uani d 1 . .
C C20 0.3301(2) 0.0244(2) 0.90149(11) 0.0252(5) Uani d 1 . .
C C18 0.5129(2) 0.2342(2) 0.88389(10) 0.0227(4) Uani d 1 . .
H H18 0.573253 0.304358 0.901627 0.027 Uiso calc 1 . .
C C3 0.5901(2) 0.7473(2) 0.56355(10) 0.0226(4) Uani d 1 . .
C C21 0.3360(2) 0.0304(2) 0.83209(11) 0.0268(5) Uani d 1 . .
H H21 0.275146 -0.039010 0.814108 0.032 Uiso calc 1 . .
C C10 0.4654(2) 0.8955(2) 0.63090(10) 0.0234(4) Uani d 1 . .
C C12 0.8784(2) 0.4379(2) 0.63815(10) 0.0239(4) Uani d 1 . .
H H12 0.792938 0.506435 0.634980 0.029 Uiso calc 1 . .
C C22 0.4293(2) 0.1361(2) 0.78878(11) 0.0246(4) Uani d 1 . .
H H22 0.433214 0.138741 0.741556 0.030 Uiso calc 1 . .
C C1 0.4033(2) 0.5309(2) 0.70767(10) 0.0231(4) Uani d 1 . .
H H1A 0.429808 0.598387 0.738910 0.028 Uiso calc 1 . .
H H1B 0.312386 0.468228 0.727047 0.028 Uiso calc 1 . .
C C19 0.4200(2) 0.1271(2) 0.92686(11) 0.0256(5) Uani d 1 . .
H H19 0.417784 0.123993 0.974110 0.031 Uiso calc 1 . .
C C24 0.9990(2) 0.4556(2) 0.83641(11) 0.0243(4) Uani d 1 . .
H H24 1.024122 0.441481 0.789435 0.029 Uiso calc 1 . .
C C2 0.3681(2) 0.6264(2) 0.63933(11) 0.0239(4) Uani d 1 . .
H H2A 0.366244 0.558188 0.606327 0.029 Uiso calc 1 . .
H H2B 0.263929 0.671795 0.641762 0.029 Uiso calc 1 . .
C C13 0.9999(2) 0.4674(2) 0.59088(11) 0.0278(5) Uani d 1 . .
H H13 0.997509 0.556827 0.555804 0.033 Uiso calc 1 . .
C C27 0.7421(2) 0.5970(2) 0.91717(11) 0.0246(4) Uani d 1 . .
H H27 0.750357 0.492007 0.946548 0.030 Uiso calc 1 . .
C C8 0.6216(3) 1.1462(2) 0.58321(11) 0.0317(5) Uani d 1 . .
H H8 0.570588 1.207038 0.610828 0.038 Uiso calc 1 . .
C C28 0.5708(2) 0.6429(3) 0.91904(12) 0.0294(5) Uani d 1 . .
H H28A 0.558879 0.749867 0.894987 0.044 Uiso calc 1 . .
H H28B 0.533930 0.632856 0.966109 0.044 Uiso calc 1 . .
H H28C 0.510518 0.575262 0.897214 0.044 Uiso calc 1 . .
C C25 0.9721(2) 0.2933(2) 0.87942(12) 0.0296(5) Uani d 1 . .
H H25A 0.947197 0.300481 0.926309 0.044 Uiso calc 1 . .
H H25B 1.065707 0.231402 0.877778 0.044 Uiso calc 1 . .
H H25C 0.886315 0.244644 0.861586 0.044 Uiso calc 1 . .
C C5 0.7750(2) 0.9636(2) 0.50117(11) 0.0282(5) Uani d 1 . .
H H5 0.826384 0.902115 0.473913 0.034 Uiso calc 1 . .
C C15 1.1291(2) 0.2406(3) 0.64663(12) 0.0301(5) Uani d 1 . .
H H15 1.215207 0.172932 0.649736 0.036 Uiso calc 1 . .
C C14 1.1246(2) 0.3683(3) 0.59417(12) 0.0303(5) Uani d 1 . .
H H14 1.206057 0.387532 0.560883 0.036 Uiso calc 1 . .
C C7 0.7370(3) 1.2071(3) 0.53569(11) 0.0344(5) Uani d 1 . .
H H7 0.764486 1.312400 0.530483 0.041 Uiso calc 1 . .
C C23 0.2284(3) -0.0901(3) 0.94846(12) 0.0357(6) Uani d 1 . .
H H23A 0.120046 -0.067014 0.938481 0.054 Uiso calc 1 . .
H H23B 0.246165 -0.083527 0.995349 0.054 Uiso calc 1 . .
H H23C 0.252958 -0.194293 0.942108 0.054 Uiso calc 1 . .
C C26 1.1435(2) 0.5273(3) 0.85938(12) 0.0333(5) Uani d 1 . .
H H26A 1.161285 0.629633 0.830942 0.050 Uiso calc 1 . .
H H26B 1.233053 0.461466 0.855196 0.050 Uiso calc 1 . .
H H26C 1.128079 0.536457 0.906621 0.050 Uiso calc 1 . .
C C29 0.8374(3) 0.7056(3) 0.94995(12) 0.0371(6) Uani d 1 . .
H H29A 0.945592 0.672665 0.951077 0.056 Uiso calc 1 . .
H H29B 0.797407 0.702220 0.996161 0.056 Uiso calc 1 . .
H H29C 0.829942 0.810909 0.923502 0.056 Uiso calc 1 . .
C C6 0.8126(3) 1.1179(3) 0.49584(11) 0.0323(5) Uani d 1 . .
H H6 0.891433 1.162922 0.464320 0.039 Uiso calc 1 . .
C C31 0.7218(3) 0.8771(3) 0.76655(14) 0.0431(6) Uani d 1 . .
H H31A 0.639953 0.820185 0.750234 0.065 Uiso calc 1 . .
H H31B 0.744630 0.971775 0.733154 0.065 Uiso calc 1 . .
H H31C 0.687716 0.903397 0.809501 0.065 Uiso calc 1 . .
C C32 0.9431(3) 0.7677(3) 0.70892(13) 0.0485(7) Uani d 1 . .
H H32A 1.035816 0.703364 0.716090 0.073 Uiso calc 1 . .
H H32B 0.971724 0.871329 0.684381 0.073 Uiso calc 1 . .
H H32C 0.870715 0.722351 0.682492 0.073 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.0187(2) 0.0157(2) 0.0222(3) -0.00142(18) 0.00128(19) -0.00441(18)
Si 0.0192(3) 0.0161(3) 0.0241(3) -0.0013(2) 0.0001(2) -0.0050(2)
O1 0.0210(7) 0.0205(7) 0.0231(8) 0.0017(5) -0.0009(6) -0.0061(6)
O2 0.0307(8) 0.0274(8) 0.0293(8) 0.0035(6) 0.0014(7) -0.0099(6)
O3 0.0310(8) 0.0248(8) 0.0324(9) 0.0012(6) 0.0034(7) -0.0072(7)
N1 0.0217(8) 0.0165(8) 0.0285(10) -0.0009(7) 0.0028(7) -0.0043(7)
N3 0.0216(8) 0.0197(8) 0.0248(9) -0.0007(7) -0.0004(7) -0.0048(7)
N2 0.0200(8) 0.0174(8) 0.0284(10) -0.0009(7) -0.0009(7) -0.0079(7)
C17 0.0173(9) 0.0145(9) 0.0250(11) 0.0001(7) 0.0016(8) -0.0028(8)
C11 0.0200(10) 0.0218(10) 0.0258(11) -0.0034(8) 0.0006(8) -0.0125(8)
C4 0.0222(10) 0.0243(10) 0.0241(11) -0.0004(8) -0.0059(8) -0.0020(8)
C30 0.0274(11) 0.0192(10) 0.0296(12) -0.0060(8) -0.0017(9) -0.0079(9)
C16 0.0242(11) 0.0237(10) 0.0300(12) 0.0011(8) -0.0012(9) -0.0111(9)
C9 0.0265(11) 0.0247(10) 0.0229(11) -0.0026(9) -0.0067(9) -0.0040(9)
C20 0.0204(10) 0.0188(10) 0.0344(13) -0.0001(8) 0.0052(9) -0.0015(9)
C18 0.0232(10) 0.0189(9) 0.0264(11) -0.0016(8) 0.0008(8) -0.0056(8)
C3 0.0213(10) 0.0231(10) 0.0230(11) 0.0008(8) -0.0030(8) -0.0035(9)
C21 0.0223(10) 0.0193(10) 0.0395(13) -0.0033(8) -0.0017(9) -0.0078(9)
C10 0.0249(10) 0.0228(10) 0.0235(11) 0.0011(8) -0.0066(9) -0.0061(8)
C12 0.0226(10) 0.0226(10) 0.0285(12) -0.0012(8) 0.0002(9) -0.0097(9)
C22 0.0260(11) 0.0230(10) 0.0259(11) -0.0016(8) 0.0009(9) -0.0076(9)
C1 0.0188(10) 0.0239(10) 0.0264(11) 0.0010(8) 0.0025(8) -0.0054(9)
C19 0.0281(11) 0.0229(10) 0.0248(11) 0.0018(9) 0.0037(9) -0.0032(9)
C24 0.0218(10) 0.0239(10) 0.0283(12) 0.0000(8) -0.0008(9) -0.0076(9)
C2 0.0194(10) 0.0230(10) 0.0287(12) -0.0034(8) 0.0010(8) -0.0042(9)
C13 0.0311(11) 0.0255(11) 0.0284(12) -0.0091(9) 0.0047(9) -0.0100(9)
C27 0.0231(10) 0.0251(10) 0.0265(11) 0.0004(8) -0.0001(8) -0.0074(9)
C8 0.0402(13) 0.0267(11) 0.0292(12) -0.0027(10) -0.0073(10) -0.0068(9)
C28 0.0256(11) 0.0321(11) 0.0329(13) -0.0004(9) 0.0039(9) -0.0131(10)
C25 0.0263(11) 0.0248(11) 0.0376(13) 0.0044(9) -0.0068(9) -0.0055(10)
C5 0.0242(11) 0.0304(11) 0.0274(12) -0.0012(9) -0.0035(9) 0.0008(9)
C15 0.0211(11) 0.0327(12) 0.0409(14) 0.0001(9) 0.0015(9) -0.0183(10)
C14 0.0241(11) 0.0350(12) 0.0365(13) -0.0104(9) 0.0085(9) -0.0193(10)
C7 0.0419(13) 0.0284(11) 0.0319(13) -0.0137(10) -0.0111(11) -0.0014(10)
C23 0.0301(12) 0.0289(12) 0.0441(15) -0.0060(10) 0.0086(10) 0.0008(10)
C26 0.0219(11) 0.0357(12) 0.0435(14) 0.0002(9) -0.0011(10) -0.0111(11)
C29 0.0293(12) 0.0521(15) 0.0368(14) -0.0035(11) 0.0009(10) -0.0254(12)
C6 0.0297(12) 0.0353(12) 0.0290(12) -0.0102(10) -0.0053(10) 0.0011(10)
C31 0.0372(13) 0.0207(11) 0.0650(18) -0.0019(10) -0.0084(12) 0.0075(11)
C32 0.0789(19) 0.0266(12) 0.0378(15) -0.0098(13) 0.0190(14) -0.0045(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 6 5 0.0920
4 -4 -3 0.0830
-5 -2 -3 0.0784
5 2 3 0.0784
0 -1 12 0.0226
0 1 -12 0.0383
1 -2 -13 0.0487
1 2 12 0.0381
-5 0 7 0.0779
-3 -1 -11 0.0561
2 1 -11 0.0581
1 -6 -4 0.0883
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 S1 C17 . . 101.13(8) ?
N1 S1 O1 . . 105.93(8) y
N1 S1 C17 . . 101.98(9) y
N2 S1 O1 . . 107.27(8) y
N2 S1 N1 . . 126.60(9) y
N2 S1 C17 . . 111.06(9) ?
N2 Si C30 . . 107.57(9) ?
N2 Si C24 . . 110.09(9) ?
S1 N2 Si . . 142.24(11) y
N2 Si C27 . . 105.99(9) y
C30 Si C24 . . 110.30(9) ?
C30 Si C27 . . 111.23(9) ?
C24 Si C27 . . 111.50(9) ?
C1 O1 S1 . . 118.87(12) ?
C11 N1 S1 . . 125.44(14) ?
C3 N3 C10 . . 112.05(16) ?
C3 N3 C2 . . 123.98(16) ?
C10 N3 C2 . . 122.95(16) ?
C18 C17 S1 . . 119.20(15) ?
C18 C17 C22 . . 120.93(18) ?
C22 C17 S1 . . 119.81(15) ?
C16 C11 N1 . . 116.63(18) ?
C12 C11 N1 . . 124.22(17) ?
C12 C11 C16 . . 119.04(19) ?
C9 C4 C3 . . 108.23(18) ?
C5 C4 C9 . . 121.8(2) ?
C5 C4 C3 . . 129.93(19) ?
Si C30 H30 . . 107.8 ?
C31 C30 Si . . 111.13(14) ?
C31 C30 H30 . . 107.8 ?
C32 C30 Si . . 112.26(14) ?
C32 C30 H30 . . 107.8 ?
C32 C30 C31 . . 110.0(2) ?
C11 C16 H16 . . 119.9 ?
C15 C16 C11 . . 120.2(2) ?
C15 C16 H16 . . 119.9 ?
C4 C9 C10 . . 108.12(18) ?
C8 C9 C4 . . 121.5(2) ?
C8 C9 C10 . . 130.3(2) ?
C21 C20 C23 . . 121.1(2) ?
C19 C20 C21 . . 118.59(18) ?
C19 C20 C23 . . 120.3(2) ?
C17 C18 H18 . . 120.2 ?
C17 C18 C19 . . 119.65(19) ?
C19 C18 H18 . . 120.2 ?
O3 C3 N3 . . 125.02(18) ?
O3 C3 C4 . . 129.27(19) ?
N3 C3 C4 . . 105.70(16) ?
C20 C21 H21 . . 119.4 ?
C22 C21 C20 . . 121.12(19) ?
C22 C21 H21 . . 119.4 ?
O2 C10 N3 . . 124.20(19) ?
O2 C10 C9 . . 129.97(19) ?
N3 C10 C9 . . 105.82(17) ?
C11 C12 H12 . . 119.9 ?
C13 C12 C11 . . 120.15(19) ?
C13 C12 H12 . . 119.9 ?
C17 C22 H22 . . 120.5 ?
C21 C22 C17 . . 118.94(19) ?
C21 C22 H22 . . 120.5 ?
O1 C1 H1A . . 110.2 ?
O1 C1 H1B . . 110.2 ?
O1 C1 C2 . . 107.48(15) ?
H1A C1 H1B . . 108.5 ?
C2 C1 H1A . . 110.2 ?
C2 C1 H1B . . 110.2 ?
C20 C19 H19 . . 119.6 ?
C18 C19 C20 . . 120.8(2) ?
C18 C19 H19 . . 119.6 ?
Si C24 H24 . . 106.0 ?
C25 C24 Si . . 113.53(14) ?
C25 C24 H24 . . 106.0 ?
C25 C24 C26 . . 110.03(18) ?
C26 C24 Si . . 114.45(14) ?
C26 C24 H24 . . 106.0 ?
N3 C2 C1 . . 113.82(17) ?
N3 C2 H2A . . 108.8 ?
N3 C2 H2B . . 108.8 ?
C1 C2 H2A . . 108.8 ?
C1 C2 H2B . . 108.8 ?
H2A C2 H2B . . 107.7 ?
C12 C13 H13 . . 119.6 ?
C14 C13 C12 . . 120.8(2) ?
C14 C13 H13 . . 119.6 ?
Si C27 H27 . . 106.6 ?
C28 C27 Si . . 114.45(15) ?
C28 C27 H27 . . 106.6 ?
C29 C27 Si . . 112.48(14) ?
C29 C27 H27 . . 106.6 ?
C29 C27 C28 . . 109.50(17) ?
C9 C8 H8 . . 121.6 ?
C9 C8 C7 . . 116.8(2) ?
C7 C8 H8 . . 121.6 ?
C27 C28 H28A . . 109.5 ?
C27 C28 H28B . . 109.5 ?
C27 C28 H28C . . 109.5 ?
H28A C28 H28B . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
C24 C25 H25A . . 109.5 ?
C24 C25 H25B . . 109.5 ?
C24 C25 H25C . . 109.5 ?
H25A C25 H25B . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C4 C5 H5 . . 121.5 ?
C4 C5 C6 . . 117.0(2) ?
C6 C5 H5 . . 121.5 ?
C16 C15 H15 . . 119.7 ?
C14 C15 C16 . . 120.6(2) ?
C14 C15 H15 . . 119.7 ?
C13 C14 C15 . . 119.2(2) ?
C13 C14 H14 . . 120.4 ?
C15 C14 H14 . . 120.4 ?
C8 C7 H7 . . 119.2 ?
C6 C7 C8 . . 121.6(2) ?
C6 C7 H7 . . 119.2 ?
C20 C23 H23A . . 109.5 ?
C20 C23 H23B . . 109.5 ?
C20 C23 H23C . . 109.5 ?
H23A C23 H23B . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C24 C26 H26A . . 109.5 ?
C24 C26 H26B . . 109.5 ?
C24 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C27 C29 H29A . . 109.5 ?
C27 C29 H29B . . 109.5 ?
C27 C29 H29C . . 109.5 ?
H29A C29 H29B . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C5 C6 H6 . . 119.4 ?
C7 C6 C5 . . 121.2(2) ?
C7 C6 H6 . . 119.4 ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31B . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32B . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 N1 . 1.5139(16) y
S1 N2 . 1.4838(16) y
S1 O1 . 1.6257(14) y
S1 C17 . 1.7718(19) y
Si N2 . 1.7240(17) y
Si C30 . 1.881(2) ?
Si C24 . 1.882(2) ?
Si C27 . 1.894(2) ?
O1 C1 . 1.452(2) ?
O2 C10 . 1.211(2) ?
O3 C3 . 1.211(2) ?
N1 C11 . 1.412(2) y
N3 C3 . 1.396(2) ?
N3 C10 . 1.398(2) ?
N3 C2 . 1.459(2) ?
C17 C18 . 1.374(3) ?
C17 C22 . 1.392(3) ?
C11 C16 . 1.394(3) ?
C11 C12 . 1.394(3) ?
C4 C9 . 1.388(3) ?
C4 C3 . 1.489(3) ?
C4 C5 . 1.380(3) ?
C30 H30 . 1.0000 ?
C30 C31 . 1.531(3) ?
C30 C32 . 1.525(3) ?
C16 H16 . 0.9500 ?
C16 C15 . 1.389(3) ?
C9 C10 . 1.486(3) ?
C9 C8 . 1.385(3) ?
C20 C21 . 1.393(3) ?
C20 C19 . 1.392(3) ?
C20 C23 . 1.507(3) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.389(3) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.387(3) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.387(3) ?
C22 H22 . 0.9500 ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C1 C2 . 1.505(3) ?
C19 H19 . 0.9500 ?
C24 H24 . 1.0000 ?
C24 C25 . 1.537(3) ?
C24 C26 . 1.539(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C13 H13 . 0.9500 ?
C13 C14 . 1.383(3) ?
C27 H27 . 1.0000 ?
C27 C28 . 1.539(3) ?
C27 C29 . 1.539(3) ?
C8 H8 . 0.9500 ?
C8 C7 . 1.394(3) ?
C28 H28A . 0.9800 ?
C28 H28B . 0.9800 ?
C28 H28C . 0.9800 ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C5 H5 . 0.9500 ?
C5 C6 . 1.392(3) ?
C15 H15 . 0.9500 ?
C15 C14 . 1.386(3) ?
C14 H14 . 0.9500 ?
C7 H7 . 0.9500 ?
C7 C6 . 1.387(3) ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C26 H26A . 0.9800 ?
C26 H26B . 0.9800 ?
C26 H26C . 0.9800 ?
C29 H29A . 0.9800 ?
C29 H29B . 0.9800 ?
C29 H29C . 0.9800 ?
C6 H6 . 0.9500 ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C15 H15 O2 1_645 0.95 2.52 3.429(3) 160
C22 H22 O2 1_545 0.95 2.639 3.348(3) 132
C14 H14 O3 2_766 0.95 2.52 3.429(3) 161
C31 H31B N1 1_565 0.98 2.60 3.361(3) 135
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S1 O1 C1 C2 . . . . 154.80(13) ?
S1 N1 C11 C16 . . . . 153.82(16) ?
S1 N1 C11 C12 . . . . -30.1(3) ?
S1 C17 C18 C19 . . . . -177.16(14) ?
S1 C17 C22 C21 . . . . 177.63(15) ?
O1 S1 N1 C11 . . . . 71.56(18) ?
O1 S1 N2 Si . . . . -143.37(17) ?
O1 S1 C17 C18 . . . . -138.15(15) ?
O1 S1 C17 C22 . . . . 44.69(16) ?
O1 C1 C2 N3 . . . . -74.8(2) ?
N1 S1 O1 C1 . . . . 176.34(13) ?
N1 S1 N2 Si . . . . -17.3(2) ?
N1 S1 C17 C18 . . . . 112.72(16) ?
N1 S1 C17 C22 . . . . -64.45(17) ?
N1 C11 C16 C15 . . . . 174.52(18) ?
N1 C11 C12 C13 . . . . -174.88(18) ?
N2 S1 O1 C1 . . . . -46.09(15) ?
N2 S1 N1 C11 . . . . -55.1(2) ?
N2 S1 C17 C18 . . . . -24.57(18) ?
N2 S1 C17 C22 . . . . 158.26(15) ?
N2 Si C30 C31 . . . . 55.01(18) ?
N2 Si C30 C32 . . . . -68.60(19) ?
N2 Si C24 C25 . . . . -61.52(17) ?
N2 Si C24 C26 . . . . 171.01(15) ?
N2 Si C27 C28 . . . . -38.05(17) ?
N2 Si C27 C29 . . . . -163.87(15) ?
C17 S1 O1 C1 . . . . 70.31(14) ?
C17 S1 N1 C11 . . . . 176.97(17) ?
C17 S1 N2 Si . . . . 106.97(18) ?
C17 C18 C19 C20 . . . . -0.5(3) ?
C11 C16 C15 C14 . . . . 0.6(3) ?
C11 C12 C13 C14 . . . . 0.7(3) ?
C4 C9 C10 O2 . . . . -177.3(2) ?
C4 C9 C10 N3 . . . . 1.7(2) ?
C4 C9 C8 C7 . . . . 0.0(3) ?
C4 C5 C6 C7 . . . . -0.1(3) ?
C30 Si N2 S1 . . . . 119.40(18) ?
C30 Si C24 C25 . . . . 179.92(15) ?
C30 Si C24 C26 . . . . 52.46(18) ?
C30 Si C27 C28 . . . . 78.57(17) ?
C30 Si C27 C29 . . . . -47.24(18) ?
C16 C11 C12 C13 . . . . 1.1(3) ?
C16 C15 C14 C13 . . . . 1.2(3) ?
C9 C4 C3 O3 . . . . 177.6(2) ?
C9 C4 C3 N3 . . . . -1.7(2) ?
C9 C4 C5 C6 . . . . -0.5(3) ?
C9 C8 C7 C6 . . . . -0.7(3) ?
C20 C21 C22 C17 . . . . -0.5(3) ?
C18 C17 C22 C21 . . . . 0.5(3) ?
C3 N3 C10 O2 . . . . 176.21(19) ?
C3 N3 C10 C9 . . . . -2.9(2) ?
C3 N3 C2 C1 . . . . 105.9(2) ?
C3 C4 C9 C10 . . . . 0.0(2) ?
C3 C4 C9 C8 . . . . -177.80(19) ?
C3 C4 C5 C6 . . . . 177.5(2) ?
C21 C20 C19 C18 . . . . 0.4(3) ?
C10 N3 C3 O3 . . . . -176.40(19) ?
C10 N3 C3 C4 . . . . 2.9(2) ?
C10 N3 C2 C1 . . . . -86.5(2) ?
C10 C9 C8 C7 . . . . -177.2(2) ?
C12 C11 C16 C15 . . . . -1.8(3) ?
C12 C13 C14 C15 . . . . -1.8(3) ?
C22 C17 C18 C19 . . . . 0.0(3) ?
C19 C20 C21 C22 . . . . 0.1(3) ?
C24 Si N2 S1 . . . . -0.8(2) ?
C24 Si C30 C31 . . . . 175.10(16) ?
C24 Si C30 C32 . . . . 51.5(2) ?
C24 Si C27 C28 . . . . -157.85(14) ?
C24 Si C27 C29 . . . . 76.34(17) ?
C2 N3 C3 O3 . . . . -7.7(3) ?
C2 N3 C3 C4 . . . . 171.58(17) ?
C2 N3 C10 O2 . . . . 7.4(3) ?
C2 N3 C10 C9 . . . . -171.74(17) ?
C27 Si N2 S1 . . . . -121.54(18) ?
C27 Si C30 C31 . . . . -60.64(18) ?
C27 Si C30 C32 . . . . 175.74(17) ?
C27 Si C24 C25 . . . . 55.82(18) ?
C27 Si C24 C26 . . . . -71.65(18) ?
C8 C9 C10 O2 . . . . 0.2(4) ?
C8 C9 C10 N3 . . . . 179.2(2) ?
C8 C7 C6 C5 . . . . 0.7(3) ?
C5 C4 C9 C10 . . . . 178.36(18) ?
C5 C4 C9 C8 . . . . 0.6(3) ?
C5 C4 C3 O3 . . . . -0.7(4) ?
C5 C4 C3 N3 . . . . -179.9(2) ?
C23 C20 C21 C22 . . . . 179.82(19) ?
C23 C20 C19 C18 . . . . -179.31(18) ?
_cod_database_fobs_code 2244114