 
data_herges129
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C30 H42 N4 S Si2' 
_chemical_formula_weight          546.91

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.3629(4)
_cell_length_b                    15.4255(3)
_cell_length_c                    16.2296(4)
_cell_angle_alpha                 90
_cell_angle_beta                  94.777(2)
_cell_angle_gamma                 90
_cell_volume                      3333.78(14)
_cell_formula_units_Z             4
_cell_measurement_temperature     200(2)
_cell_measurement_reflns_used     32011 
_cell_measurement_theta_min       1.529 
_cell_measurement_theta_max       26.002 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             yellow 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.090          
_exptl_crystal_F_000              1176
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.06 
_exptl_absorpt_coefficient_mu     0.192
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.9228 
_exptl_absorpt_correction_T_max   0.9828 
_exptl_absorpt_process_details    'X-Red and X-Shape (STOE, 2008)'  
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       200(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type   'STOE IPDS-2' 
_diffrn_measurement_method        'Omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             32011
_diffrn_reflns_av_unetI/netI      0.0202
_diffrn_reflns_av_R_equivalents   0.0405
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.529
_diffrn_reflns_theta_max          26.002
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.990
_diffrn_measured_fraction_theta_full  0.989
_diffrn_reflns_Laue_measured_fraction_max    0.990
_diffrn_reflns_Laue_measured_fraction_full   0.989
_diffrn_reflns_point_group_measured_fraction_max   0.990
_diffrn_reflns_point_group_measured_fraction_full  0.989
_reflns_number_total              6482
_reflns_number_gt                 5702
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'X-AREA (STOE, 2008)'
_computing_cell_refinement        'X-AREA (STOE, 2008)'
_computing_data_reduction         'X-AREA (STOE, 2008)'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick,2015)' _computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0864P)²+1.1821P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6482
_refine_ls_number_parameters      346
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0662
_refine_ls_R_factor_gt            0.0599
_refine_ls_wR_factor_ref          0.1677
_refine_ls_wR_factor_gt           0.1623
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.051
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
C1 C 0.26558(16) 0.43213(13) 0.47343(11) 0.0517(4) Uani 1 1 d . . . . .
C2 C 0.18152(17) 0.47499(14) 0.43144(12) 0.0562(5) Uani 1 1 d . . . . .
C3 C 0.19115(17) 0.52210(14) 0.35760(12) 0.0580(5) Uani 1 1 d . . . . .
C4 C 0.28431(17) 0.52747(13) 0.32177(12) 0.0548(5) Uani 1 1 d . . . . .
C5 C 0.36509(16) 0.48604(13) 0.36327(12) 0.0531(5) Uani 1 1 d . . . . .
C6 C 0.35518(16) 0.43905(13) 0.43842(11) 0.0511(4) Uani 1 1 d . . . . .
N1 N 0.08932(15) 0.47718(15) 0.45703(12) 0.0710(6) Uani 1 1 d . . . . .
S1 S 0.02330(5) 0.53527(6) 0.39012(4) 0.0898(3) Uani 1 1 d . . . . .
N2 N 0.10479(16) 0.55889(16) 0.32712(12) 0.0759(6) Uani 1 1 d . . . . .
C7 C 0.46093(19) 0.48882(16) 0.33004(14) 0.0637(5) Uani 1 1 d . . . . .
N3 N 0.5373(2) 0.49005(18) 0.30316(16) 0.0891(7) Uani 1 1 d . . . . .
C8 C 0.44319(18) 0.39989(15) 0.47966(13) 0.0598(5) Uani 1 1 d . . . . .
N4 N 0.51293(17) 0.37005(16) 0.51378(14) 0.0797(6) Uani 1 1 d . . . . .
C9 C 0.25547(17) 0.38669(14) 0.54885(12) 0.0573(5) Uani 1 1 d . . . . .
C10 C 0.24668(18) 0.35019(15) 0.61246(13) 0.0616(5) Uani 1 1 d . . . . .
Si1 Si 0.23626(5) 0.29087(4) 0.71037(4) 0.0619(2) Uani 1 1 d . . . . .
C11 C 0.3372(2) 0.20593(19) 0.71534(16) 0.0791(7) Uani 1 1 d . . . . .
H11 H 0.3289 0.1701 0.7657 0.095 Uiso 1 1 calc R U . . .
C12 C 0.3294(3) 0.1447(2) 0.6421(2) 0.1083(11) Uani 1 1 d . . . . .
H12A H 0.3378 0.1774 0.5914 0.162 Uiso 1 1 calc R U . . .
H12B H 0.2634 0.1167 0.6378 0.162 Uiso 1 1 calc R U . . .
H12C H 0.3820 0.1005 0.6497 0.162 Uiso 1 1 calc R U . . .
C13 C 0.4417(2) 0.2459(3) 0.7262(2) 0.1031(11) Uani 1 1 d . . . . .
H13A H 0.4923 0.1998 0.7293 0.155 Uiso 1 1 calc R U . . .
H13B H 0.4484 0.2801 0.7773 0.155 Uiso 1 1 calc R U . . .
H13C H 0.4517 0.2837 0.6790 0.155 Uiso 1 1 calc R U . . .
C14 C 0.2599(2) 0.3734(2) 0.79551(14) 0.0774(7) Uani 1 1 d . . . . .
H14 H 0.3291 0.3966 0.7911 0.093 Uiso 1 1 calc R U . . .
C15 C 0.2592(3) 0.3319(3) 0.88211(17) 0.1050(11) Uani 1 1 d . . . . .
H15A H 0.2774 0.3757 0.9245 0.158 Uiso 1 1 calc R U . . .
H15B H 0.3079 0.2843 0.8872 0.158 Uiso 1 1 calc R U . . .
H15C H 0.1920 0.3094 0.8896 0.158 Uiso 1 1 calc R U . . .
C16 C 0.1888(3) 0.4502(2) 0.7863(2) 0.0988(10) Uani 1 1 d . . . . .
H16A H 0.1202 0.4307 0.7933 0.148 Uiso 1 1 calc R U . . .
H16B H 0.1913 0.4757 0.7312 0.148 Uiso 1 1 calc R U . . .
H16C H 0.2089 0.4937 0.8284 0.148 Uiso 1 1 calc R U . . .
C17 C 0.1050(2) 0.2475(2) 0.70740(19) 0.0876(8) Uani 1 1 d . . . . .
H17 H 0.0629 0.2949 0.7284 0.105 Uiso 1 1 calc R U . . .
C18 C 0.0968(3) 0.1703(3) 0.7665(3) 0.1332(16) Uani 1 1 d . . . . .
H18A H 0.0258 0.1558 0.7701 0.200 Uiso 1 1 calc R U . . .
H18B H 0.1272 0.1858 0.8216 0.200 Uiso 1 1 calc R U . . .
H18C H 0.1319 0.1202 0.7457 0.200 Uiso 1 1 calc R U . . .
C19 C 0.0582(4) 0.2243(3) 0.6233(3) 0.1322(16) Uani 1 1 d . . . . .
H19A H 0.0946 0.1754 0.6013 0.198 Uiso 1 1 calc R U . . .
H19B H 0.0614 0.2743 0.5863 0.198 Uiso 1 1 calc R U . . .
H19C H -0.0122 0.2079 0.6271 0.198 Uiso 1 1 calc R U . . .
C20 C 0.29051(18) 0.57301(15) 0.24610(13) 0.0610(5) Uani 1 1 d . . . . .
C21 C 0.28798(19) 0.61106(16) 0.18219(14) 0.0649(6) Uani 1 1 d . . . . .
Si2 Si 0.27375(5) 0.67191(5) 0.08434(4) 0.0633(2) Uani 1 1 d . . . . .
C22 C 0.1429(2) 0.6503(3) 0.03973(18) 0.0958(10) Uani 1 1 d . . . . .
H22 H 0.1328 0.6849 -0.0124 0.115 Uiso 1 1 calc R U . . .
C23 C 0.1272(4) 0.5561(4) 0.0158(3) 0.152(2) Uani 1 1 d . . . . .
H23A H 0.1285 0.5204 0.0658 0.228 Uiso 1 1 calc R U . . .
H23B H 0.1808 0.5374 -0.0179 0.228 Uiso 1 1 calc R U . . .
H23C H 0.0620 0.5495 -0.0161 0.228 Uiso 1 1 calc R U . . .
C24 C 0.0640(3) 0.6795(4) 0.0949(3) 0.1355(18) Uani 1 1 d . . . . .
H24A H -0.0025 0.6621 0.0705 0.203 Uiso 1 1 calc R U . . .
H24B H 0.0665 0.7427 0.1007 0.203 Uiso 1 1 calc R U . . .
H24C H 0.0767 0.6526 0.1495 0.203 Uiso 1 1 calc R U . . .
C25 C 0.3004(2) 0.78839(19) 0.1120(2) 0.0848(8) Uani 1 1 d . . . . .
H25 H 0.3749 0.7957 0.1126 0.102 Uiso 1 1 calc R U . . .
C26 C 0.2727(3) 0.8141(2) 0.1971(2) 0.1131(12) Uani 1 1 d . . . . .
H26A H 0.2957 0.8735 0.2093 0.170 Uiso 1 1 calc R U . . .
H26B H 0.3049 0.7745 0.2384 0.170 Uiso 1 1 calc R U . . .
H26C H 0.1997 0.8112 0.1988 0.170 Uiso 1 1 calc R U . . .
C27 C 0.2543(3) 0.8513(3) 0.0465(3) 0.1311(16) Uani 1 1 d . . . . .
H27A H 0.1815 0.8539 0.0498 0.197 Uiso 1 1 calc R U . . .
H27B H 0.2687 0.8311 -0.0085 0.197 Uiso 1 1 calc R U . . .
H27C H 0.2832 0.9091 0.0564 0.197 Uiso 1 1 calc R U . . .
C28 C 0.3658(3) 0.6206(3) 0.01611(17) 0.0945(9) Uani 1 1 d . . . . .
H28 H 0.3463 0.5582 0.0107 0.113 Uiso 1 1 calc R U . . .
C29 C 0.3548(3) 0.6583(3) -0.07241(18) 0.1181(14) Uani 1 1 d . . . . .
H29A H 0.3755 0.7193 -0.0709 0.177 Uiso 1 1 calc R U . . .
H29B H 0.2846 0.6541 -0.0948 0.177 Uiso 1 1 calc R U . . .
H29C H 0.3973 0.6256 -0.1077 0.177 Uiso 1 1 calc R U . . .
C30 C 0.4707(3) 0.6215(3) 0.0523(2) 0.1133(12) Uani 1 1 d . . . . .
H30A H 0.5129 0.5891 0.0164 0.170 Uiso 1 1 calc R U . . .
H30B H 0.4745 0.5944 0.1071 0.170 Uiso 1 1 calc R U . . .
H30C H 0.4945 0.6815 0.0575 0.170 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C6 1.372(3) . ?
C1 C9 1.427(3) . ?
C1 C2 1.427(3) . ?
C2 N1 1.333(3) . ?
C2 C3 1.416(3) . ?
C3 N2 1.343(3) . ?
C3 C4 1.420(3) . ?
C4 C5 1.381(3) . ?
C4 C20 1.423(3) . ?
C5 C7 1.431(3) . ?
C5 C6 1.434(3) . ?
C6 C8 1.437(3) . ?
N1 S1 1.6127(19) . ?
S1 N2 1.597(2) . ?
C7 N3 1.143(3) . ?
C8 N4 1.141(3) . ?
C9 C10 1.190(3) . ?
C10 Si1 1.849(2) . ?
Si1 C17 1.874(3) . ?
Si1 C11 1.878(3) . ?
Si1 C14 1.886(3) . ?
C11 C12 1.515(5) . ?
C11 C13 1.523(5) . ?
C14 C16 1.519(4) . ?
C14 C15 1.545(4) . ?
C17 C19 1.497(5) . ?
C17 C18 1.538(4) . ?
C20 C21 1.190(3) . ?
C21 Si2 1.841(2) . ?
Si2 C22 1.866(3) . ?
Si2 C25 1.879(3) . ?
Si2 C28 1.895(3) . ?
C22 C24 1.509(5) . ?
C22 C23 1.514(6) . ?
C25 C26 1.513(5) . ?
C25 C27 1.530(4) . ?
C28 C30 1.474(5) . ?
C28 C29 1.546(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
C6 C1 C9 122.81(19) . . ?
C6 C1 C2 116.48(17) . . ?
C9 C1 C2 120.69(19) . . ?
N1 C2 C3 113.70(19) . . ?
N1 C2 C1 125.05(19) . . ?
C3 C2 C1 121.2(2) . . ?
N2 C3 C2 113.1(2) . . ?
N2 C3 C4 125.48(19) . . ?
C2 C3 C4 121.40(19) . . ?
C5 C4 C3 116.73(18) . . ?
C5 C4 C20 123.4(2) . . ?
C3 C4 C20 119.9(2) . . ?
C4 C5 C7 119.36(19) . . ?
C4 C5 C6 121.66(19) . . ?
C7 C5 C6 118.97(19) . . ?
C1 C6 C5 122.49(18) . . ?
C1 C6 C8 118.89(18) . . ?
C5 C6 C8 118.59(19) . . ?
C2 N1 S1 105.80(15) . . ?
N2 S1 N1 101.18(10) . . ?
C3 N2 S1 106.18(15) . . ?
N3 C7 C5 179.2(3) . . ?
N4 C8 C6 178.5(2) . . ?
C10 C9 C1 178.8(2) . . ?
C9 C10 Si1 178.1(2) . . ?
C10 Si1 C17 106.98(12) . . ?
C10 Si1 C11 106.08(11) . . ?
C17 Si1 C11 114.80(15) . . ?
C10 Si1 C14 106.01(12) . . ?
C17 Si1 C14 111.05(14) . . ?
C11 Si1 C14 111.31(13) . . ?
C12 C11 C13 110.2(3) . . ?
C12 C11 Si1 113.5(2) . . ?
C13 C11 Si1 111.8(2) . . ?
C16 C14 C15 111.2(3) . . ?
C16 C14 Si1 112.91(19) . . ?
C15 C14 Si1 112.0(2) . . ?
C19 C17 C18 109.8(3) . . ?
C19 C17 Si1 115.3(3) . . ?
C18 C17 Si1 112.1(2) . . ?
C21 C20 C4 175.1(3) . . ?
C20 C21 Si2 175.5(2) . . ?
C21 Si2 C22 105.65(12) . . ?
C21 Si2 C25 106.13(12) . . ?
C22 Si2 C25 114.63(17) . . ?
C21 Si2 C28 105.41(13) . . ?
C22 Si2 C28 109.35(16) . . ?
C25 Si2 C28 114.78(15) . . ?
C24 C22 C23 110.5(3) . . ?
C24 C22 Si2 113.3(3) . . ?
C23 C22 Si2 112.2(3) . . ?
C26 C25 C27 110.6(3) . . ?
C26 C25 Si2 114.4(2) . . ?
C27 C25 Si2 112.5(3) . . ?
C30 C28 C29 112.4(3) . . ?
C30 C28 Si2 113.9(2) . . ?
C29 C28 Si2 111.7(3) . . ?
 
_refine_diff_density_max    0.585
_refine_diff_density_min   -0.423
_refine_diff_density_rms    0.039

_shelxl_version_number 2014-3



