#------------------------------------------------------------------------------
#$Date: 2021-02-04 02:59:09 +0200 (Thu, 04 Feb 2021) $
#$Revision: 261483 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/56/4135618.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_4135618
loop_
_publ_author_name
'Zhu, Guohao'
'Gao, Wen-Chao'
'Jiang, Xuefeng'
_publ_section_title
;
 Rh(I)-Catalyzed Carbene Migration/Carbonylation/Cyclization:
 Straightforward Construction of Fully Substituted Aryne Precursors.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1334
_journal_page_last               1340
_journal_paper_doi               10.1021/jacs.0c13012
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C34 H36 N2 O6 S2 Si'
_chemical_formula_sum            'C34 H36 N2 O6 S2 Si'
_chemical_formula_weight         660.86
_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_date             2019-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                103.4620(10)
_cell_angle_beta                 90.2360(10)
_cell_angle_gamma                104.924(2)
_cell_formula_units_Z            2
_cell_length_a                   6.86330(10)
_cell_length_b                   11.6049(2)
_cell_length_c                   24.2941(4)
_cell_measurement_reflns_used    23018
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3670
_cell_measurement_theta_min      4.8080
_cell_volume                     1814.10(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      6.00  82.00   1.00    1.00    --    0.00  82.00 120.00   76
  2  ω    -12.00  30.00   1.00    1.00    --    0.00  38.00 150.00   42
  3  ω    -23.00  79.00   1.00    1.00    --    0.00  19.00 -60.00  102
  4  ω    -31.00  -6.00   1.00    1.00    --    0.00  82.00 120.00   25
  5  ω     58.00  84.00   1.00    1.00    --    0.00  57.00  90.00   26
  6  ω    -29.00  14.00   1.00    1.00    --    0.00  77.00-120.00   43
  7  ω     43.00  80.00   1.00    1.00    --    0.00  38.00   0.00   37
  8  ω    -14.00  22.00   1.00    1.00    --    0.00  38.00  30.00   36
  9  ω     20.00  62.00   1.00    1.00    --    0.00  77.00-120.00   42
 10  ω    -75.00 -32.00   1.00    1.00    --    0.00 -57.00 120.00   43
 11  ω     36.00  80.00   1.00    1.00    --    0.00  38.00 150.00   44
 12  ω    -19.00  27.00   1.00    1.00    --    0.00  38.00   0.00   46
 13  ω    -22.00  53.00   1.00    1.00    --    0.00  57.00  90.00   75
 14  ω     43.00  71.00   1.00    1.00    --    0.00  38.00  30.00   28
 15  ω     -9.00  20.00   1.00    1.00    --    0.00 -57.00 120.00   29
 16  ω     41.00 120.00   1.00    1.00    --   95.80 -61.00 -30.00   79
 17  ω     10.00  37.00   1.00    1.00    --   95.80 -61.00 -30.00   27
 18  ω     63.00  90.00   1.00    1.00    --   95.80  82.00   4.95   27
 19  ω    145.00 185.00   1.00    1.00    --   95.80  71.00  48.22   40
 20  ω     67.00  93.00   1.00    1.00    --   95.80  71.00  48.22   26
 21  ω     70.00 175.00   1.00    1.00    --   95.80  66.00-171.40  105
 22  ω    112.00 170.00   1.00    1.00    --   95.80  82.00-134.00   58
 23  ω     71.00  96.00   1.00    1.00    --   95.80  61.00   0.00   25
 24  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 -90.00   26
 25  ω     28.00  54.00   1.00    1.00    --   95.80 -82.00  90.00   26
 26  ω     58.00 116.00   1.00    1.00    --   95.80 -82.00  90.00   58
 27  ω     63.00  88.00   1.00    1.00    --   95.80  82.00 150.00   25
 28  ω    106.00 132.00   1.00    1.00    --   95.80  82.00 150.00   26
 29  ω      6.00 124.00   1.00    1.00    --   95.80 -82.00 -90.00  118
 30  ω     63.00  89.00   1.00    1.00    --   95.80  82.00-150.00   26
 31  ω     63.00  89.00   1.00    1.00    --   95.80  82.00  60.00   26
 32  ω     65.00 139.00   1.00    1.00    --   95.80  77.00-150.00   74
 33  ω     68.00 167.00   1.00    1.00    --   95.80  68.00 150.64   99
 34  ω     65.00  92.00   1.00    1.00    --   95.80  77.00  90.00   27
 35  ω     61.00 123.00   1.00    1.00    --   95.80 -82.00 -30.00   62
 36  ω     64.00  89.00   1.00    1.00    --   95.80  80.00-165.94   25
 37  ω     65.00  91.00   1.00    1.00    --   95.80  76.00 114.43   26
 38  ω     71.00 183.00   1.00    1.00    --   95.80  61.00 120.00  112
 39  ω      8.00 110.00   1.00    1.00    --   95.80 -61.00 150.00  102
 40  ω     65.00  91.00   1.00    1.00    --   95.80  77.00-180.00   26
 41  ω     63.00  95.00   1.00    1.00    --   95.80  82.00 -60.00   32
 42  ω     71.00  96.00   1.00    1.00    --   95.80  61.00 -60.00   25
 43  ω     12.00  51.00   1.00    1.00    --   95.80 -82.00 -30.00   39
 44  ω     63.00  88.00   1.00    1.00    --   95.80  82.00 -30.00   25
 45  ω     65.00  90.00   1.00    1.00    --   95.80  77.00   0.00   25
 46  ω     75.00 109.00   1.00    1.00    --   95.80  45.00 -60.00   34
 47  ω    119.00 148.00   1.00    1.00    --   95.80  45.00 -60.00   29
 48  ω     75.00 140.00   1.00    1.00    --   95.80  45.00 120.00   65
 49  ω     65.00  90.00   1.00    1.00    --   95.80  82.00 -90.00   25
 50  ω     77.00 116.00   1.00    1.00    --   95.80  45.00 -30.00   39
 51  ω     76.00 162.00   1.00    1.00    --   95.80  45.00  30.00   86
 52  ω     75.00 178.00   1.00    1.00    --   95.80  45.00  60.00  103
 53  ω    119.00 184.00   1.00    1.00    --   95.80  82.00-120.00   65
 54  ω    113.00 138.00   1.00    1.00    --   95.80  77.00 -60.00   25
 55  ω    133.00 159.00   1.00    1.00    --   95.80  69.00 -20.07   26
 56  ω     63.00  88.00   1.00    1.00    --   95.80  82.00-120.00   25
 57  ω     65.00 116.00   1.00    1.00    --   95.80  77.00  60.00   51
 58  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 120.00   26
 59  ω     65.00  90.00   1.00    1.00    --   95.80  77.00 -60.00   25
 60  ω     71.00 145.00   1.00    1.00    --   95.80  61.00-180.00   74
 61  ω     75.00 178.00   1.00    1.00    --   95.80  45.00   0.00  103
 62  ω     65.00  90.00   1.00    1.00    --   95.80  77.00  30.00   25
 63  ω     21.00 117.00   1.00    1.00    --   95.80 -82.00 150.00   96
 64  ω     68.00  93.00   1.00    1.00    --   95.80  69.00 -20.07   25
 65  ω     68.00  94.00   1.00    1.00    --   95.80  70.00-159.73   26
 66  ω     63.00  99.00   1.00    1.00    --   95.80  82.00-134.00   36
 67  ω     75.00 101.00   1.00    1.00    --   95.80  47.00 -75.73   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0067533000
_diffrn_orient_matrix_UB_12      -0.0649449000
_diffrn_orient_matrix_UB_13      0.0482533000
_diffrn_orient_matrix_UB_21      -0.0537996000
_diffrn_orient_matrix_UB_22      -0.1253530000
_diffrn_orient_matrix_UB_23      -0.0434904000
_diffrn_orient_matrix_UB_31      0.2264415000
_diffrn_orient_matrix_UB_32      0.0108544000
_diffrn_orient_matrix_UB_33      -0.0071897000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43298
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.471
_diffrn_reflns_theta_min         3.750
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0345
_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/[σ²(Fo²)+(0.0374P)²+0.9339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6762
_reflns_number_total             7293
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c13012_si_003.cif
_cod_data_source_block           exp_1010
_cod_database_code               4135618
_shelx_shelxl_version_number     2016/6
_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.
;
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C19(H19),
 C20(H20), C23(H23), C24(H24), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_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 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.432
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.07993(5) 0.35480(3) 0.11787(2) 0.01994(9) Uani 1 1 d . . . . .
S2 S 0.70456(6) 1.00896(3) 0.36093(2) 0.02246(9) Uani 1 1 d . . . . .
Si1 Si 0.70183(6) 0.74923(3) 0.10773(2) 0.01731(9) Uani 1 1 d . . . . .
O1 O 0.02440(16) 0.35962(9) 0.06703(4) 0.0246(2) Uani 1 1 d . . . . .
O2 O -0.29302(16) 0.30269(9) 0.11329(5) 0.0262(2) Uani 1 1 d . . . . .
O3 O 0.88976(18) 1.06486(10) 0.33941(4) 0.0299(3) Uani 1 1 d . . . . .
O4 O 0.56895(19) 1.08012(10) 0.38298(5) 0.0313(3) Uani 1 1 d . . . . .
O5 O 0.29980(16) 0.82176(10) 0.34989(4) 0.0265(2) Uani 1 1 d . . . . .
O6 O 0.30645(17) 0.56632(10) 0.07985(4) 0.0252(2) Uani 1 1 d . . . . .
H6 H 0.209399 0.505575 0.071364 0.038 Uiso 1 1 calc GR . . . .
N1 N -0.04020(18) 0.50127(10) 0.15560(5) 0.0197(2) Uani 1 1 d . . . . .
N2 N 0.58459(19) 0.89827(11) 0.30569(5) 0.0211(3) Uani 1 1 d . . . . .
C1 C 0.1611(2) 0.58203(12) 0.17151(6) 0.0180(3) Uani 1 1 d . . . . .
C2 C 0.3183(2) 0.61509(12) 0.13611(6) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.4963(2) 0.70823(12) 0.15827(6) 0.0178(3) Uani 1 1 d . . . . .
C4 C 0.5036(2) 0.76704(12) 0.21592(6) 0.0176(3) Uani 1 1 d . . . . .
C5 C 0.6728(2) 0.86990(13) 0.25068(6) 0.0204(3) Uani 1 1 d . . . . .
H5A H 0.793582 0.842802 0.254321 0.024 Uiso 1 1 calc R . . . .
H5B H 0.705235 0.940425 0.234138 0.024 Uiso 1 1 calc R . . . .
C6 C 0.3941(2) 0.81944(13) 0.30761(6) 0.0205(3) Uani 1 1 d . . . . .
C7 C 0.3452(2) 0.73875(13) 0.25036(6) 0.0187(3) Uani 1 1 d . . . . .
C8 C 0.1698(2) 0.64615(12) 0.22826(6) 0.0178(3) Uani 1 1 d . . . . .
C9 C -0.0283(2) 0.60808(13) 0.24961(6) 0.0197(3) Uani 1 1 d . . . . .
C10 C -0.1087(2) 0.64578(14) 0.30154(6) 0.0234(3) Uani 1 1 d . . . . .
H10 H -0.026812 0.702235 0.331687 0.028 Uiso 1 1 calc R . . . .
C11 C -0.3116(2) 0.59773(14) 0.30725(7) 0.0274(3) Uani 1 1 d . . . . .
H11 H -0.366259 0.621450 0.341693 0.033 Uiso 1 1 calc R . . . .
C12 C -0.4360(2) 0.51380(14) 0.26185(7) 0.0271(3) Uani 1 1 d . . . . .
H12 H -0.572368 0.482753 0.266556 0.033 Uiso 1 1 calc R . . . .
C13 C -0.3594(2) 0.47610(14) 0.20993(7) 0.0254(3) Uani 1 1 d . . . . .
H13 H -0.442590 0.421325 0.179576 0.030 Uiso 1 1 calc R . . . .
C14 C -0.1544(2) 0.52291(13) 0.20479(6) 0.0207(3) Uani 1 1 d . . . . .
C15 C 0.0381(2) 0.28155(12) 0.15821(6) 0.0202(3) Uani 1 1 d . . . . .
C16 C -0.0404(3) 0.26187(14) 0.20888(7) 0.0279(3) Uani 1 1 d . . . . .
H16 H -0.154189 0.287091 0.221272 0.034 Uiso 1 1 calc R . . . .
C17 C 0.0534(3) 0.20416(15) 0.24061(7) 0.0307(4) Uani 1 1 d . . . . .
H17 H 0.002854 0.191830 0.274850 0.037 Uiso 1 1 calc R . . . .
C18 C 0.2215(2) 0.16433(14) 0.22223(7) 0.0281(3) Uani 1 1 d . . . . .
C19 C 0.2955(2) 0.18446(14) 0.17132(7) 0.0289(3) Uani 1 1 d . . . . .
H19 H 0.407929 0.158041 0.158576 0.035 Uiso 1 1 calc R . . . .
C20 C 0.2056(2) 0.24310(13) 0.13896(7) 0.0252(3) Uani 1 1 d . . . . .
H20 H 0.257118 0.256326 0.104942 0.030 Uiso 1 1 calc R . . . .
C21 C 0.3224(3) 0.10067(19) 0.25695(9) 0.0431(5) Uani 1 1 d . . . . .
H21A H 0.252732 0.095206 0.290817 0.065 Uiso 1 1 calc GR . . . .
H21B H 0.460577 0.146849 0.266977 0.065 Uiso 1 1 calc GR . . . .
H21C H 0.317894 0.019533 0.235094 0.065 Uiso 1 1 calc GR . . . .
C22 C 0.7574(2) 0.93407(13) 0.41167(6) 0.0220(3) Uani 1 1 d . . . . .
C23 C 0.9418(2) 0.90637(14) 0.41285(6) 0.0266(3) Uani 1 1 d . . . . .
H23 H 1.037779 0.928976 0.387698 0.032 Uiso 1 1 calc R . . . .
C24 C 0.9805(3) 0.84444(15) 0.45216(7) 0.0309(4) Uani 1 1 d . . . . .
H24 H 1.102983 0.824182 0.452724 0.037 Uiso 1 1 calc R . . . .
C25 C 0.8413(3) 0.81191(15) 0.49068(7) 0.0317(4) Uani 1 1 d . . . . .
C26 C 0.6600(3) 0.84408(17) 0.48959(7) 0.0353(4) Uani 1 1 d . . . . .
H26 H 0.566539 0.824725 0.515859 0.042 Uiso 1 1 calc R . . . .
C27 C 0.6156(3) 0.90440(16) 0.45015(7) 0.0298(3) Uani 1 1 d . . . . .
H27 H 0.493103 0.924604 0.449501 0.036 Uiso 1 1 calc R . . . .
C28 C 0.8843(3) 0.74255(18) 0.53249(8) 0.0449(5) Uani 1 1 d . . . . .
H28A H 0.812646 0.657354 0.519545 0.067 Uiso 1 1 calc GR . . . .
H28B H 0.840810 0.775838 0.568862 0.067 Uiso 1 1 calc GR . . . .
H28C H 1.026749 0.750227 0.535719 0.067 Uiso 1 1 calc GR . . . .
C29 C 0.7364(2) 0.60904(13) 0.05699(6) 0.0244(3) Uani 1 1 d . . . . .
H29A H 0.711563 0.542072 0.075205 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.872155 0.625121 0.045286 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.643086 0.587902 0.024387 0.037 Uiso 1 1 calc GR . . . .
C30 C 0.9506(2) 0.82771(14) 0.14925(6) 0.0238(3) Uani 1 1 d . . . . .
H30A H 0.949789 0.909271 0.169326 0.036 Uiso 1 1 calc GR . . . .
H30B H 1.057418 0.832094 0.123795 0.036 Uiso 1 1 calc GR . . . .
H30C H 0.971943 0.781926 0.175882 0.036 Uiso 1 1 calc GR . . . .
C31 C 0.6366(2) 0.85980(13) 0.06842(6) 0.0221(3) Uani 1 1 d . . . . .
C32 C 0.8176(3) 0.90526(16) 0.03479(7) 0.0348(4) Uani 1 1 d . . . . .
H32A H 0.933132 0.949535 0.060606 0.052 Uiso 1 1 calc GR . . . .
H32B H 0.785362 0.958517 0.013357 0.052 Uiso 1 1 calc GR . . . .
H32C H 0.847569 0.836139 0.009405 0.052 Uiso 1 1 calc GR . . . .
C33 C 0.5971(3) 0.97062(14) 0.11075(7) 0.0314(4) Uani 1 1 d . . . . .
H33A H 0.483680 0.943179 0.131847 0.047 Uiso 1 1 calc GR . . . .
H33B H 0.568408 1.026933 0.090542 0.047 Uiso 1 1 calc GR . . . .
H33C H 0.714457 1.011134 0.136355 0.047 Uiso 1 1 calc GR . . . .
C34 C 0.4491(3) 0.79889(16) 0.02724(7) 0.0349(4) Uani 1 1 d . . . . .
H34A H 0.471957 0.729848 0.000066 0.052 Uiso 1 1 calc GR . . . .
H34B H 0.423213 0.857219 0.007852 0.052 Uiso 1 1 calc GR . . . .
H34C H 0.334739 0.771417 0.048008 0.052 Uiso 1 1 calc GR . . . .
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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 N1 106.42(6) . . ?
O1 S1 C15 108.26(7) . . ?
O2 S1 O1 118.98(6) . . ?
O2 S1 N1 106.15(6) . . ?
O2 S1 C15 109.94(7) . . ?
N1 S1 C15 106.35(6) . . ?
O3 S2 N2 103.80(6) . . ?
O3 S2 C22 109.13(7) . . ?
O4 S2 O3 120.26(7) . . ?
O4 S2 N2 107.96(7) . . ?
O4 S2 C22 108.84(7) . . ?
N2 S2 C22 105.88(7) . . ?
C29 Si1 C3 111.59(6) . . ?
C29 Si1 C30 106.74(7) . . ?
C29 Si1 C31 111.05(7) . . ?
C30 Si1 C3 109.77(6) . . ?
C30 Si1 C31 108.09(7) . . ?
C31 Si1 C3 109.50(6) . . ?
C2 O6 H6 109.5 . . ?
C1 N1 S1 122.05(9) . . ?
C14 N1 S1 117.20(9) . . ?
C14 N1 C1 105.99(11) . . ?
C5 N2 S2 123.30(10) . . ?
C6 N2 S2 123.47(10) . . ?
C6 N2 C5 113.17(11) . . ?
C2 C1 N1 128.60(12) . . ?
C8 C1 N1 108.93(12) . . ?
C8 C1 C2 121.35(13) . . ?
O6 C2 C1 123.51(13) . . ?
O6 C2 C3 115.72(12) . . ?
C3 C2 C1 120.69(12) . . ?
C2 C3 Si1 118.42(10) . . ?
C4 C3 Si1 125.18(11) . . ?
C4 C3 C2 116.35(12) . . ?
C3 C4 C5 127.92(13) . . ?
C7 C4 C3 123.17(13) . . ?
C7 C4 C5 108.89(12) . . ?
N2 C5 C4 102.07(11) . . ?
N2 C5 H5A 111.4 . . ?
N2 C5 H5B 111.4 . . ?
C4 C5 H5A 111.4 . . ?
C4 C5 H5B 111.4 . . ?
H5A C5 H5B 109.2 . . ?
O5 C6 N2 124.04(13) . . ?
O5 C6 C7 130.60(14) . . ?
N2 C6 C7 105.36(12) . . ?
C4 C7 C6 110.35(13) . . ?
C4 C7 C8 120.22(13) . . ?
C8 C7 C6 129.42(13) . . ?
C1 C8 C9 108.11(12) . . ?
C7 C8 C1 118.06(13) . . ?
C7 C8 C9 133.30(13) . . ?
C10 C9 C8 132.91(14) . . ?
C10 C9 C14 119.61(14) . . ?
C14 C9 C8 107.32(12) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 C9 118.89(15) . . ?
C11 C10 H10 120.6 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.81(15) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.13(15) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 121.1 . . ?
C12 C13 C14 117.78(15) . . ?
C14 C13 H13 121.1 . . ?
C9 C14 N1 109.58(12) . . ?
C13 C14 N1 128.57(14) . . ?
C13 C14 C9 121.76(14) . . ?
C16 C15 S1 119.16(12) . . ?
C20 C15 S1 119.76(11) . . ?
C20 C15 C16 121.07(14) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 118.97(15) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.4 . . ?
C16 C17 C18 121.17(15) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C21 120.87(16) . . ?
C19 C18 C17 118.54(14) . . ?
C19 C18 C21 120.60(16) . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.48(15) . . ?
C20 C19 H19 119.3 . . ?
C15 C20 C19 118.76(14) . . ?
C15 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 S2 119.08(11) . . ?
C23 C22 C27 121.18(14) . . ?
C27 C22 S2 119.73(12) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 118.75(15) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 119.2 . . ?
C23 C24 C25 121.57(16) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C26 118.40(15) . . ?
C24 C25 C28 120.89(17) . . ?
C26 C25 C28 120.71(17) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 C25 121.35(16) . . ?
C27 C26 H26 119.3 . . ?
C22 C27 H27 120.6 . . ?
C26 C27 C22 118.71(16) . . ?
C26 C27 H27 120.6 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 Si1 108.24(11) . . ?
C33 C31 Si1 110.19(10) . . ?
C33 C31 C32 108.84(13) . . ?
C34 C31 Si1 112.22(10) . . ?
C34 C31 C32 108.94(13) . . ?
C34 C31 C33 108.35(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.4353(11) . ?
S1 O2 1.4243(11) . ?
S1 N1 1.6845(12) . ?
S1 C15 1.7536(15) . ?
S2 O3 1.4313(12) . ?
S2 O4 1.4244(12) . ?
S2 N2 1.6652(12) . ?
S2 C22 1.7502(15) . ?
Si1 C3 1.9140(14) . ?
Si1 C29 1.8681(15) . ?
Si1 C30 1.8760(16) . ?
Si1 C31 1.9033(15) . ?
O5 C6 1.2150(17) . ?
O6 H6 0.8200 . ?
O6 C2 1.3455(17) . ?
N1 C1 1.4482(18) . ?
N1 C14 1.4403(18) . ?
N2 C5 1.4714(17) . ?
N2 C6 1.3973(19) . ?
C1 C2 1.4137(19) . ?
C1 C8 1.3990(19) . ?
C2 C3 1.4122(19) . ?
C3 C4 1.4024(19) . ?
C4 C5 1.5148(19) . ?
C4 C7 1.3934(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.4668(19) . ?
C7 C8 1.397(2) . ?
C8 C9 1.4547(19) . ?
C9 C10 1.400(2) . ?
C9 C14 1.401(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.381(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.399(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(2) . ?
C15 C16 1.389(2) . ?
C15 C20 1.383(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.384(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.389(2) . ?
C18 C19 1.386(2) . ?
C18 C21 1.512(2) . ?
C19 H19 0.9300 . ?
C19 C20 1.387(2) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.386(2) . ?
C22 C27 1.387(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.384(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.385(2) . ?
C25 C26 1.390(3) . ?
C25 C28 1.506(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.386(2) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.537(2) . ?
C31 C33 1.533(2) . ?
C31 C34 1.532(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.551 0.500 0.500 304.4 95.4 ?
