data_sad_a _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H49 Cl N P Si' _chemical_formula_weight 542.23 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 8.9268(7) _cell_length_b 12.5462(9) _cell_length_c 14.7624(11) _cell_angle_alpha 76.497(2) _cell_angle_beta 79.230(2) _cell_angle_gamma 77.234(2) _cell_volume 1551.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.3635 _cell_measurement_theta_max 26.376 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_F_000 588 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.352 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.151 _exptl_absorpt_coefficient_mu 0.234 _shelx_estimated_absorpt_T_min 0.922 _shelx_estimated_absorpt_T_max 0.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6861 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS-2016/2' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'INCOATEC Microsource' _diffrn_measurement_device_type 'PHOTON 3C7' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 73540 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.991 _diffrn_reflns_theta_max 26.414 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6355 _reflns_number_gt 4909 _reflns_threshold_expression 'I > 2\s(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 'APEX3 v2019.11-0' _computing_cell_refinement 'SAINT V8.40B' _computing_data_reduction 'SAINT V8.40B' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'XP Version 5.1' _computing_publication_material 'XP Version 5.1' _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/[\s^2^(Fo^2^)+(0.0404P)^2^+0.3210P] where P=(Fo^2^+2Fc^2^)/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 6355 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cl1 Cl 0.41336(4) 0.50552(3) 0.67364(3) 0.01939(10) Uani 1 1 d . . . . . P1 P 0.69681(5) 0.15370(3) 0.82400(3) 0.01628(10) Uani 1 1 d . . . . . Si1 Si 0.61135(5) 0.42268(3) 0.74004(3) 0.01482(11) Uani 1 1 d . . . . . N1 N 0.70468(14) 0.62902(10) 0.74200(9) 0.0143(3) Uani 1 1 d . . . . . C1 C 0.70630(17) 0.31981(12) 0.65961(11) 0.0151(3) Uani 1 1 d . . . . . C2 C 0.73317(18) 0.35681(13) 0.56211(11) 0.0174(3) Uani 1 1 d . . . . . H2 H 0.706840 0.434275 0.536662 0.021 Uiso 1 1 calc R U . . . C3 C 0.79682(18) 0.28439(13) 0.50144(11) 0.0182(3) Uani 1 1 d . . . . . H3 H 0.812780 0.311816 0.435387 0.022 Uiso 1 1 calc R U . . . C4 C 0.83718(18) 0.17111(13) 0.53808(11) 0.0196(4) Uani 1 1 d . . . . . H4 H 0.883812 0.120866 0.497215 0.024 Uiso 1 1 calc R U . . . C5 C 0.80948(18) 0.13174(13) 0.63376(11) 0.0183(3) Uani 1 1 d . . . . . H5 H 0.836452 0.054022 0.658058 0.022 Uiso 1 1 calc R U . . . C6 C 0.74229(17) 0.20392(12) 0.69616(11) 0.0154(3) Uani 1 1 d . . . . . C7 C 0.84125(19) 0.02179(13) 0.84660(11) 0.0198(4) Uani 1 1 d . . . . . H7 H 0.836162 -0.026977 0.802906 0.024 Uiso 1 1 calc R U . . . C7A C 1.00305(19) 0.05049(14) 0.82945(13) 0.0259(4) Uani 1 1 d . . . . . H7AA H 1.027630 0.085623 0.763189 0.039 Uiso 1 1 calc R U . . . H7AB H 1.079507 -0.017852 0.844709 0.039 Uiso 1 1 calc R U . . . H7AC H 1.005890 0.102133 0.869441 0.039 Uiso 1 1 calc R U . . . C7B C 0.8038(2) -0.03863(14) 0.94861(12) 0.0269(4) Uani 1 1 d . . . . . H7BA H 0.706713 -0.066136 0.956281 0.040 Uiso 1 1 calc R U . . . H7BB H 0.792562 0.013230 0.990892 0.040 Uiso 1 1 calc R U . . . H7BC H 0.888171 -0.101638 0.963934 0.040 Uiso 1 1 calc R U . . . C8 C 0.51249(18) 0.10260(13) 0.83263(12) 0.0220(4) Uani 1 1 d . . . . . H8 H 0.493767 0.057455 0.897733 0.026 Uiso 1 1 calc R U . . . C8A C 0.5087(2) 0.02786(15) 0.76532(14) 0.0306(4) Uani 1 1 d . . . . . H8AA H 0.516124 0.071014 0.700622 0.046 Uiso 1 1 calc R U . . . H8AB H 0.411221 -0.000497 0.781518 0.046 Uiso 1 1 calc R U . . . H8AC H 0.596346 -0.034924 0.770593 0.046 Uiso 1 1 calc R U . . . C8B C 0.3775(2) 0.20200(15) 0.82433(14) 0.0298(4) Uani 1 1 d . . . . . H8BA H 0.390173 0.248470 0.761062 0.045 Uiso 1 1 calc R U . . . H8BB H 0.376327 0.246318 0.871108 0.045 Uiso 1 1 calc R U . . . H8BC H 0.279447 0.174851 0.835494 0.045 Uiso 1 1 calc R U . . . C9 C 0.74076(17) 0.52258(12) 0.72999(10) 0.0153(3) Uani 1 1 d . . . . . C10 C 0.91325(18) 0.47972(13) 0.73969(11) 0.0180(3) Uani 1 1 d . . . . . C10A C 0.9534(2) 0.36080(13) 0.79527(13) 0.0258(4) Uani 1 1 d . . . . . H10A H 0.936828 0.308200 0.760019 0.039 Uiso 1 1 calc R U . . . H10B H 0.886751 0.352926 0.856347 0.039 Uiso 1 1 calc R U . . . H10C H 1.062320 0.344928 0.805133 0.039 Uiso 1 1 calc R U . . . C10B C 1.00407(18) 0.48655(14) 0.63983(12) 0.0237(4) Uani 1 1 d . . . . . H10D H 0.977019 0.433095 0.609526 0.036 Uiso 1 1 calc R U . . . H10E H 1.115656 0.468759 0.643346 0.036 Uiso 1 1 calc R U . . . H10F H 0.977431 0.562171 0.602957 0.036 Uiso 1 1 calc R U . . . C11 C 0.95063(19) 0.56258(13) 0.79066(12) 0.0215(4) Uani 1 1 d . . . . . H11A H 0.946829 0.530728 0.858865 0.026 Uiso 1 1 calc R U . . . H11B H 1.055939 0.578537 0.765410 0.026 Uiso 1 1 calc R U . . . C12 C 0.82944(18) 0.66966(13) 0.77426(11) 0.0173(3) Uani 1 1 d . . . . . C12A C 0.88935(19) 0.76320(13) 0.69952(12) 0.0216(4) Uani 1 1 d . . . . . H12A H 0.932587 0.735856 0.641306 0.032 Uiso 1 1 calc R U . . . H12B H 0.970273 0.787589 0.722006 0.032 Uiso 1 1 calc R U . . . H12C H 0.803620 0.826185 0.687286 0.032 Uiso 1 1 calc R U . . . C12B C 0.77050(19) 0.71372(14) 0.86476(12) 0.0219(4) Uani 1 1 d . . . . . H12D H 0.855506 0.736300 0.884725 0.033 Uiso 1 1 calc R U . . . H12E H 0.731714 0.655037 0.914093 0.033 Uiso 1 1 calc R U . . . H12F H 0.686375 0.778178 0.853685 0.033 Uiso 1 1 calc R U . . . C13 C 0.55970(17) 0.70318(12) 0.72153(11) 0.0149(3) Uani 1 1 d . . . . . C14 C 0.55015(17) 0.76507(12) 0.62954(11) 0.0152(3) Uani 1 1 d . . . . . C15 C 0.41295(18) 0.84003(13) 0.61213(11) 0.0183(3) Uani 1 1 d . . . . . H15 H 0.405064 0.883866 0.550747 0.022 Uiso 1 1 calc R U . . . C16 C 0.28822(18) 0.85159(13) 0.68274(12) 0.0195(4) Uani 1 1 d . . . . . H16 H 0.196503 0.904294 0.670125 0.023 Uiso 1 1 calc R U . . . C17 C 0.29727(18) 0.78656(13) 0.77136(11) 0.0186(3) Uani 1 1 d . . . . . H17 H 0.209569 0.793316 0.818706 0.022 Uiso 1 1 calc R U . . . C18 C 0.43174(18) 0.71105(12) 0.79346(11) 0.0162(3) Uani 1 1 d . . . . . C19 C 0.67617(18) 0.75034(13) 0.54560(11) 0.0185(3) Uani 1 1 d . . . . . H19 H 0.769317 0.698842 0.569587 0.022 Uiso 1 1 calc R U . . . C19A C 0.7251(2) 0.86070(14) 0.49238(12) 0.0254(4) Uani 1 1 d . . . . . H19A H 0.814739 0.845660 0.444465 0.038 Uiso 1 1 calc R U . . . H19B H 0.753016 0.897690 0.536740 0.038 Uiso 1 1 calc R U . . . H19C H 0.638760 0.909198 0.461960 0.038 Uiso 1 1 calc R U . . . C19B C 0.62168(19) 0.69729(14) 0.47740(11) 0.0219(4) Uani 1 1 d . . . . . H19D H 0.533450 0.748174 0.450623 0.033 Uiso 1 1 calc R U . . . H19E H 0.589908 0.626924 0.511142 0.033 Uiso 1 1 calc R U . . . H19F H 0.706701 0.682730 0.426676 0.033 Uiso 1 1 calc R U . . . C20 C 0.42914(19) 0.64014(13) 0.89233(11) 0.0190(3) Uani 1 1 d . . . . . H20 H 0.533542 0.591439 0.897204 0.023 Uiso 1 1 calc R U . . . C20A C 0.3951(2) 0.71240(15) 0.96752(12) 0.0254(4) Uani 1 1 d . . . . . H20A H 0.466675 0.765185 0.951919 0.038 Uiso 1 1 calc R U . . . H20B H 0.408987 0.664370 1.029203 0.038 Uiso 1 1 calc R U . . . H20C H 0.288052 0.753641 0.969329 0.038 Uiso 1 1 calc R U . . . C20B C 0.3076(2) 0.56514(14) 0.91381(12) 0.0242(4) Uani 1 1 d . . . . . H20D H 0.204782 0.611388 0.907190 0.036 Uiso 1 1 calc R U . . . H20E H 0.307629 0.521849 0.978319 0.036 Uiso 1 1 calc R U . . . H20F H 0.332646 0.514189 0.869653 0.036 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.01642(19) 0.01616(19) 0.0262(2) -0.00575(16) -0.00660(15) 0.00023(15) P1 0.0189(2) 0.0123(2) 0.0164(2) -0.00329(16) -0.00202(16) -0.00025(16) Si1 0.0146(2) 0.0109(2) 0.0188(2) -0.00400(17) -0.00278(17) -0.00057(16) N1 0.0136(6) 0.0109(6) 0.0189(7) -0.0041(5) -0.0036(5) -0.0009(5) C1 0.0122(7) 0.0129(7) 0.0210(8) -0.0049(6) -0.0030(6) -0.0018(6) C2 0.0169(8) 0.0126(8) 0.0216(9) -0.0018(6) -0.0024(6) -0.0026(6) C3 0.0173(8) 0.0206(8) 0.0157(8) -0.0025(6) -0.0002(6) -0.0039(7) C4 0.0185(8) 0.0192(8) 0.0214(9) -0.0092(7) -0.0005(7) -0.0006(7) C5 0.0195(8) 0.0126(8) 0.0225(9) -0.0044(6) -0.0040(7) -0.0007(6) C6 0.0139(8) 0.0138(8) 0.0189(8) -0.0045(6) -0.0031(6) -0.0013(6) C7 0.0261(9) 0.0117(8) 0.0214(9) -0.0052(6) -0.0064(7) 0.0014(7) C7A 0.0230(9) 0.0203(9) 0.0336(10) -0.0076(7) -0.0087(8) 0.0037(7) C7B 0.0390(11) 0.0174(9) 0.0224(9) -0.0031(7) -0.0083(8) 0.0009(8) C8 0.0195(8) 0.0177(8) 0.0249(9) 0.0022(7) -0.0019(7) -0.0034(7) C8A 0.0268(10) 0.0229(9) 0.0450(12) -0.0066(8) -0.0081(8) -0.0083(8) C8B 0.0193(9) 0.0230(9) 0.0435(12) -0.0030(8) -0.0032(8) -0.0012(7) C9 0.0161(8) 0.0132(8) 0.0148(8) -0.0023(6) -0.0011(6) -0.0007(6) C10 0.0142(8) 0.0137(8) 0.0271(9) -0.0057(7) -0.0057(7) -0.0003(6) C10A 0.0209(9) 0.0163(8) 0.0410(11) -0.0053(8) -0.0140(8) 0.0023(7) C10B 0.0153(8) 0.0224(9) 0.0346(10) -0.0129(8) -0.0006(7) -0.0010(7) C11 0.0188(8) 0.0172(8) 0.0307(10) -0.0081(7) -0.0092(7) 0.0007(7) C12 0.0158(8) 0.0140(8) 0.0239(9) -0.0068(6) -0.0056(6) -0.0009(6) C12A 0.0197(8) 0.0186(8) 0.0287(9) -0.0069(7) -0.0034(7) -0.0059(7) C12B 0.0232(9) 0.0196(8) 0.0258(9) -0.0075(7) -0.0065(7) -0.0044(7) C13 0.0156(8) 0.0099(7) 0.0206(8) -0.0062(6) -0.0050(6) 0.0000(6) C14 0.0169(8) 0.0101(7) 0.0203(8) -0.0049(6) -0.0032(6) -0.0032(6) C15 0.0217(8) 0.0124(8) 0.0211(9) -0.0025(6) -0.0071(7) -0.0011(6) C16 0.0179(8) 0.0133(8) 0.0273(9) -0.0069(7) -0.0065(7) 0.0028(6) C17 0.0171(8) 0.0169(8) 0.0221(9) -0.0088(7) -0.0009(6) -0.0005(6) C18 0.0184(8) 0.0119(7) 0.0203(8) -0.0067(6) -0.0042(6) -0.0018(6) C19 0.0182(8) 0.0157(8) 0.0198(8) -0.0020(6) -0.0023(6) -0.0012(6) C19A 0.0265(9) 0.0218(9) 0.0259(10) 0.0007(7) -0.0027(7) -0.0069(7) C19B 0.0235(9) 0.0209(9) 0.0196(9) -0.0053(7) -0.0005(7) -0.0016(7) C20 0.0189(8) 0.0181(8) 0.0185(8) -0.0045(7) -0.0016(6) -0.0004(6) C20A 0.0268(9) 0.0278(9) 0.0217(9) -0.0089(7) -0.0023(7) -0.0016(8) C20B 0.0251(9) 0.0224(9) 0.0232(9) -0.0036(7) 0.0009(7) -0.0050(7) _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 Cl1 Si1 2.1272(6) . ? P1 C6 1.8425(16) . ? P1 C7 1.8635(16) . ? P1 C8 1.8667(17) . ? Si1 C9 1.8484(16) . ? Si1 C1 1.9104(15) . ? N1 C9 1.3481(19) . ? N1 C13 1.4542(18) . ? N1 C12 1.513(2) . ? C1 C2 1.398(2) . ? C1 C6 1.414(2) . ? C2 C3 1.383(2) . ? C3 C4 1.389(2) . ? C4 C5 1.378(2) . ? C5 C6 1.404(2) . ? C7 C7A 1.527(2) . ? C7 C7B 1.531(2) . ? C8 C8A 1.526(2) . ? C8 C8B 1.530(2) . ? C9 C10 1.537(2) . ? C10 C10A 1.526(2) . ? C10 C10B 1.537(2) . ? C10 C11 1.540(2) . ? C11 C12 1.529(2) . ? C12 C12B 1.523(2) . ? C12 C12A 1.527(2) . ? C13 C14 1.406(2) . ? C13 C18 1.410(2) . ? C14 C15 1.395(2) . ? C14 C19 1.526(2) . ? C15 C16 1.383(2) . ? C16 C17 1.377(2) . ? C17 C18 1.394(2) . ? C18 C20 1.521(2) . ? C19 C19B 1.527(2) . ? C19 C19A 1.535(2) . ? C20 C20B 1.532(2) . ? C20 C20A 1.539(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 C6 P1 C7 102.94(7) . . ? C6 P1 C8 101.87(7) . . ? C7 P1 C8 102.79(7) . . ? C9 Si1 C1 108.83(7) . . ? C9 Si1 Cl1 109.36(5) . . ? C1 Si1 Cl1 100.39(5) . . ? C9 N1 C13 123.33(13) . . ? C9 N1 C12 115.46(12) . . ? C13 N1 C12 121.14(11) . . ? C2 C1 C6 118.19(14) . . ? C2 C1 Si1 120.51(11) . . ? C6 C1 Si1 121.18(12) . . ? C3 C2 C1 122.18(14) . . ? C2 C3 C4 119.31(15) . . ? C5 C4 C3 119.92(15) . . ? C4 C5 C6 121.46(14) . . ? C5 C6 C1 118.88(14) . . ? C5 C6 P1 122.65(12) . . ? C1 C6 P1 118.46(11) . . ? C7A C7 C7B 110.32(14) . . ? C7A C7 P1 108.68(11) . . ? C7B C7 P1 109.09(11) . . ? C8A C8 C8B 110.14(15) . . ? C8A C8 P1 117.18(12) . . ? C8B C8 P1 109.42(12) . . ? N1 C9 C10 107.74(13) . . ? N1 C9 Si1 129.35(11) . . ? C10 C9 Si1 120.03(11) . . ? C10A C10 C9 115.62(13) . . ? C10A C10 C10B 108.70(13) . . ? C9 C10 C10B 107.48(13) . . ? C10A C10 C11 109.99(13) . . ? C9 C10 C11 103.25(12) . . ? C10B C10 C11 111.76(14) . . ? C12 C11 C10 107.67(13) . . ? N1 C12 C12B 111.92(13) . . ? N1 C12 C12A 111.17(13) . . ? C12B C12 C12A 107.82(13) . . ? N1 C12 C11 101.27(12) . . ? C12B C12 C11 111.18(13) . . ? C12A C12 C11 113.47(13) . . ? C14 C13 C18 121.37(13) . . ? C14 C13 N1 118.87(13) . . ? C18 C13 N1 119.76(13) . . ? C15 C14 C13 118.17(14) . . ? C15 C14 C19 117.43(14) . . ? C13 C14 C19 124.27(13) . . ? C16 C15 C14 121.10(15) . . ? C17 C16 C15 119.86(14) . . ? C16 C17 C18 121.75(15) . . ? C17 C18 C13 117.63(14) . . ? C17 C18 C20 118.00(14) . . ? C13 C18 C20 124.34(13) . . ? C14 C19 C19B 110.46(13) . . ? C14 C19 C19A 112.66(13) . . ? C19B C19 C19A 109.18(13) . . ? C18 C20 C20B 111.65(13) . . ? C18 C20 C20A 111.73(13) . . ? C20B C20 C20A 108.44(13) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.7(2) . . . . ? Si1 C1 C2 C3 -177.79(12) . . . . ? C1 C2 C3 C4 -0.7(2) . . . . ? C2 C3 C4 C5 1.9(2) . . . . ? C3 C4 C5 C6 -0.7(2) . . . . ? C4 C5 C6 C1 -1.7(2) . . . . ? C4 C5 C6 P1 177.63(12) . . . . ? C2 C1 C6 C5 2.8(2) . . . . ? Si1 C1 C6 C5 178.87(11) . . . . ? C2 C1 C6 P1 -176.55(11) . . . . ? Si1 C1 C6 P1 -0.45(18) . . . . ? C7 P1 C6 C5 27.50(15) . . . . ? C8 P1 C6 C5 -78.79(14) . . . . ? C7 P1 C6 C1 -153.21(12) . . . . ? C8 P1 C6 C1 100.51(13) . . . . ? C6 P1 C7 C7A 67.31(12) . . . . ? C8 P1 C7 C7A 172.90(11) . . . . ? C6 P1 C7 C7B -172.36(12) . . . . ? C8 P1 C7 C7B -66.77(13) . . . . ? C6 P1 C8 C8A 47.63(14) . . . . ? C7 P1 C8 C8A -58.78(14) . . . . ? C6 P1 C8 C8B -78.63(13) . . . . ? C7 P1 C8 C8B 174.96(12) . . . . ? C13 N1 C9 C10 168.83(13) . . . . ? C12 N1 C9 C10 -8.31(17) . . . . ? C13 N1 C9 Si1 -30.8(2) . . . . ? C12 N1 C9 Si1 152.04(12) . . . . ? C1 Si1 C9 N1 151.84(14) . . . . ? Cl1 Si1 C9 N1 43.07(15) . . . . ? C1 Si1 C9 C10 -49.87(13) . . . . ? Cl1 Si1 C9 C10 -158.64(10) . . . . ? N1 C9 C10 C10A 138.46(14) . . . . ? Si1 C9 C10 C10A -24.06(19) . . . . ? N1 C9 C10 C10B -99.96(14) . . . . ? Si1 C9 C10 C10B 97.52(14) . . . . ? N1 C9 C10 C11 18.30(16) . . . . ? Si1 C9 C10 C11 -144.22(12) . . . . ? C10A C10 C11 C12 -145.68(14) . . . . ? C9 C10 C11 C12 -21.75(17) . . . . ? C10B C10 C11 C12 93.48(15) . . . . ? C9 N1 C12 C12B -123.99(14) . . . . ? C13 N1 C12 C12B 58.81(18) . . . . ? C9 N1 C12 C12A 115.36(14) . . . . ? C13 N1 C12 C12A -61.84(17) . . . . ? C9 N1 C12 C11 -5.48(17) . . . . ? C13 N1 C12 C11 177.32(13) . . . . ? C10 C11 C12 N1 16.89(16) . . . . ? C10 C11 C12 C12B 135.94(14) . . . . ? C10 C11 C12 C12A -102.31(16) . . . . ? C9 N1 C13 C14 -87.02(18) . . . . ? C12 N1 C13 C14 89.95(17) . . . . ? C9 N1 C13 C18 92.45(18) . . . . ? C12 N1 C13 C18 -90.58(17) . . . . ? C18 C13 C14 C15 3.7(2) . . . . ? N1 C13 C14 C15 -176.81(13) . . . . ? C18 C13 C14 C19 -172.07(14) . . . . ? N1 C13 C14 C19 7.4(2) . . . . ? C13 C14 C15 C16 -1.4(2) . . . . ? C19 C14 C15 C16 174.67(15) . . . . ? C14 C15 C16 C17 -1.5(2) . . . . ? C15 C16 C17 C18 2.2(2) . . . . ? C16 C17 C18 C13 0.0(2) . . . . ? C16 C17 C18 C20 -178.07(15) . . . . ? C14 C13 C18 C17 -3.0(2) . . . . ? N1 C13 C18 C17 177.51(13) . . . . ? C14 C13 C18 C20 174.92(14) . . . . ? N1 C13 C18 C20 -4.5(2) . . . . ? C15 C14 C19 C19B -65.91(18) . . . . ? C13 C14 C19 C19B 109.92(17) . . . . ? C15 C14 C19 C19A 56.49(19) . . . . ? C13 C14 C19 C19A -127.68(16) . . . . ? C17 C18 C20 C20B 61.49(19) . . . . ? C13 C18 C20 C20B -116.45(17) . . . . ? C17 C18 C20 C20A -60.15(19) . . . . ? C13 C18 C20 C20A 121.90(16) . . . . ? _refine_diff_density_max 0.266 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.047 _shelx_res_file ; TITL sad_a.res in P-1 sad_a.res created by SHELXL-2018/3 at 14:33:01 on 13-May-2022 REM Old TITL sad in P-1 REM SHELXT solution in P-1: R1 0.113, Rweak 0.032, Alpha 0.058 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 N P Cl2 CELL 0.71073 8.9268 12.5462 14.7624 76.497 79.230 77.234 ZERR 2.000 0.0007 0.0009 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H N SI P CL UNIT 64 98 2 2 2 2 TEMP -173.150 SIZE 0.151 0.153 0.352 OMIT 0 1 0 L.S. 20 ACTA BOND CONF LIST 4 FMAP 2 PLAN 20 WGHT 0.040400 0.321000 FVAR 0.78196 CL1 6 0.413357 0.505519 0.673641 11.00000 0.01642 0.01616 = 0.02623 -0.00575 -0.00660 0.00023 P1 5 0.696812 0.153703 0.824000 11.00000 0.01888 0.01227 = 0.01642 -0.00329 -0.00202 -0.00025 SI1 4 0.611353 0.422676 0.740037 11.00000 0.01459 0.01088 = 0.01880 -0.00400 -0.00278 -0.00057 N1 3 0.704684 0.629015 0.741997 11.00000 0.01357 0.01090 = 0.01888 -0.00406 -0.00362 -0.00086 C1 1 0.706297 0.319809 0.659611 11.00000 0.01222 0.01293 = 0.02096 -0.00489 -0.00299 -0.00175 C2 1 0.733170 0.356808 0.562106 11.00000 0.01687 0.01264 = 0.02158 -0.00176 -0.00242 -0.00259 AFIX 43 H2 2 0.706840 0.434275 0.536662 11.00000 -1.20000 AFIX 0 C3 1 0.796819 0.284390 0.501437 11.00000 0.01731 0.02056 = 0.01565 -0.00253 -0.00021 -0.00394 AFIX 43 H3 2 0.812780 0.311816 0.435387 11.00000 -1.20000 AFIX 0 C4 1 0.837175 0.171114 0.538083 11.00000 0.01847 0.01922 = 0.02142 -0.00923 -0.00051 -0.00057 AFIX 43 H4 2 0.883812 0.120866 0.497215 11.00000 -1.20000 AFIX 0 C5 1 0.809485 0.131737 0.633759 11.00000 0.01955 0.01262 = 0.02252 -0.00440 -0.00400 -0.00071 AFIX 43 H5 2 0.836452 0.054022 0.658058 11.00000 -1.20000 AFIX 0 C6 1 0.742286 0.203918 0.696161 11.00000 0.01391 0.01384 = 0.01886 -0.00451 -0.00307 -0.00131 C7 1 0.841252 0.021787 0.846601 11.00000 0.02608 0.01174 = 0.02144 -0.00525 -0.00643 0.00135 AFIX 13 H7 2 0.836162 -0.026977 0.802906 11.00000 -1.20000 AFIX 0 C7A 1 1.003054 0.050493 0.829450 11.00000 0.02299 0.02032 = 0.03360 -0.00758 -0.00868 0.00367 AFIX 137 H7AA 2 1.027630 0.085623 0.763189 11.00000 -1.50000 H7AB 2 1.079507 -0.017852 0.844709 11.00000 -1.50000 H7AC 2 1.005890 0.102133 0.869441 11.00000 -1.50000 AFIX 0 C7B 1 0.803804 -0.038626 0.948608 11.00000 0.03901 0.01744 = 0.02240 -0.00307 -0.00829 0.00086 AFIX 137 H7BA 2 0.706713 -0.066136 0.956281 11.00000 -1.50000 H7BB 2 0.792562 0.013230 0.990892 11.00000 -1.50000 H7BC 2 0.888171 -0.101638 0.963934 11.00000 -1.50000 AFIX 0 C8 1 0.512486 0.102604 0.832632 11.00000 0.01955 0.01769 = 0.02490 0.00217 -0.00189 -0.00343 AFIX 13 H8 2 0.493767 0.057455 0.897733 11.00000 -1.20000 AFIX 0 C8A 1 0.508706 0.027861 0.765318 11.00000 0.02677 0.02293 = 0.04497 -0.00662 -0.00809 -0.00828 AFIX 137 H8AA 2 0.516124 0.071014 0.700622 11.00000 -1.50000 H8AB 2 0.411221 -0.000497 0.781518 11.00000 -1.50000 H8AC 2 0.596346 -0.034924 0.770593 11.00000 -1.50000 AFIX 0 C8B 1 0.377467 0.201998 0.824327 11.00000 0.01927 0.02297 = 0.04348 -0.00304 -0.00322 -0.00119 AFIX 137 H8BA 2 0.390173 0.248470 0.761062 11.00000 -1.50000 H8BB 2 0.376327 0.246318 0.871108 11.00000 -1.50000 H8BC 2 0.279447 0.174851 0.835494 11.00000 -1.50000 AFIX 0 C9 1 0.740759 0.522582 0.729989 11.00000 0.01610 0.01316 = 0.01483 -0.00230 -0.00112 -0.00067 C10 1 0.913254 0.479715 0.739692 11.00000 0.01423 0.01366 = 0.02708 -0.00573 -0.00572 -0.00025 C10A 1 0.953378 0.360803 0.795270 11.00000 0.02095 0.01626 = 0.04101 -0.00527 -0.01397 0.00233 AFIX 137 H10A 2 0.936828 0.308200 0.760019 11.00000 -1.50000 H10B 2 0.886751 0.352926 0.856347 11.00000 -1.50000 H10C 2 1.062320 0.344928 0.805133 11.00000 -1.50000 AFIX 0 C10B 1 1.004069 0.486555 0.639831 11.00000 0.01530 0.02245 = 0.03456 -0.01286 -0.00063 -0.00099 AFIX 137 H10D 2 0.977019 0.433095 0.609526 11.00000 -1.50000 H10E 2 1.115656 0.468759 0.643346 11.00000 -1.50000 H10F 2 0.977431 0.562171 0.602957 11.00000 -1.50000 AFIX 0 C11 1 0.950629 0.562583 0.790655 11.00000 0.01879 0.01717 = 0.03068 -0.00808 -0.00919 0.00070 AFIX 23 H11A 2 0.946829 0.530728 0.858865 11.00000 -1.20000 H11B 2 1.055939 0.578537 0.765410 11.00000 -1.20000 AFIX 0 C12 1 0.829443 0.669664 0.774260 11.00000 0.01576 0.01402 = 0.02387 -0.00677 -0.00557 -0.00092 C12A 1 0.889347 0.763204 0.699518 11.00000 0.01972 0.01856 = 0.02868 -0.00687 -0.00338 -0.00586 AFIX 137 H12A 2 0.932587 0.735856 0.641306 11.00000 -1.50000 H12B 2 0.970273 0.787589 0.722006 11.00000 -1.50000 H12C 2 0.803620 0.826185 0.687286 11.00000 -1.50000 AFIX 0 C12B 1 0.770503 0.713724 0.864762 11.00000 0.02319 0.01956 = 0.02584 -0.00751 -0.00648 -0.00443 AFIX 137 H12D 2 0.855506 0.736300 0.884725 11.00000 -1.50000 H12E 2 0.731714 0.655037 0.914093 11.00000 -1.50000 H12F 2 0.686375 0.778178 0.853685 11.00000 -1.50000 AFIX 0 C13 1 0.559703 0.703184 0.721529 11.00000 0.01556 0.00995 = 0.02058 -0.00623 -0.00503 -0.00002 C14 1 0.550152 0.765073 0.629537 11.00000 0.01692 0.01008 = 0.02027 -0.00495 -0.00323 -0.00320 C15 1 0.412950 0.840032 0.612129 11.00000 0.02173 0.01242 = 0.02111 -0.00254 -0.00705 -0.00115 AFIX 43 H15 2 0.405064 0.883866 0.550747 11.00000 -1.20000 AFIX 0 C16 1 0.288224 0.851593 0.682742 11.00000 0.01786 0.01329 = 0.02731 -0.00695 -0.00650 0.00281 AFIX 43 H16 2 0.196503 0.904294 0.670125 11.00000 -1.20000 AFIX 0 C17 1 0.297273 0.786563 0.771358 11.00000 0.01710 0.01692 = 0.02214 -0.00884 -0.00087 -0.00048 AFIX 43 H17 2 0.209569 0.793316 0.818706 11.00000 -1.20000 AFIX 0 C18 1 0.431743 0.711052 0.793463 11.00000 0.01835 0.01190 = 0.02033 -0.00669 -0.00417 -0.00182 C19 1 0.676172 0.750344 0.545604 11.00000 0.01824 0.01567 = 0.01975 -0.00198 -0.00226 -0.00117 AFIX 13 H19 2 0.769317 0.698842 0.569587 11.00000 -1.20000 AFIX 0 C19A 1 0.725093 0.860697 0.492382 11.00000 0.02648 0.02177 = 0.02591 0.00065 -0.00266 -0.00694 AFIX 137 H19A 2 0.814739 0.845660 0.444465 11.00000 -1.50000 H19B 2 0.753016 0.897690 0.536740 11.00000 -1.50000 H19C 2 0.638760 0.909198 0.461960 11.00000 -1.50000 AFIX 0 C19B 1 0.621676 0.697290 0.477401 11.00000 0.02347 0.02094 = 0.01964 -0.00527 -0.00046 -0.00156 AFIX 137 H19D 2 0.533450 0.748174 0.450623 11.00000 -1.50000 H19E 2 0.589908 0.626924 0.511142 11.00000 -1.50000 H19F 2 0.706701 0.682730 0.426676 11.00000 -1.50000 AFIX 0 C20 1 0.429138 0.640142 0.892332 11.00000 0.01891 0.01815 = 0.01854 -0.00454 -0.00164 -0.00043 AFIX 13 H20 2 0.533542 0.591439 0.897204 11.00000 -1.20000 AFIX 0 C20A 1 0.395124 0.712395 0.967523 11.00000 0.02681 0.02775 = 0.02165 -0.00885 -0.00233 -0.00160 AFIX 137 H20A 2 0.466675 0.765185 0.951919 11.00000 -1.50000 H20B 2 0.408987 0.664370 1.029203 11.00000 -1.50000 H20C 2 0.288052 0.753641 0.969329 11.00000 -1.50000 AFIX 0 C20B 1 0.307604 0.565137 0.913808 11.00000 0.02513 0.02241 = 0.02316 -0.00355 0.00086 -0.00505 AFIX 137 H20D 2 0.204782 0.611388 0.907190 11.00000 -1.50000 H20E 2 0.307629 0.521849 0.978319 11.00000 -1.50000 H20F 2 0.332646 0.514189 0.869653 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in P-1 REM wR2 = 0.0852, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0340 for 4909 Fo > 4sig(Fo) and 0.0522 for all 6355 data REM 337 parameters refined using 0 restraints END WGHT 0.0404 0.3210 REM Highest difference peak 0.266, deepest hole -0.305, 1-sigma level 0.047 Q1 1 0.7351 0.1788 0.7531 11.00000 0.05 0.27 Q2 1 0.4411 0.6833 0.8429 11.00000 0.05 0.24 Q3 1 0.6815 0.4985 0.7009 11.00000 0.05 0.24 Q4 1 0.6103 0.7579 0.5901 11.00000 0.05 0.24 Q5 1 0.7145 0.2578 0.6730 11.00000 0.05 0.23 Q6 1 0.9339 0.5215 0.7569 11.00000 0.05 0.22 Q7 1 0.6478 0.7176 0.5148 11.00000 0.05 0.21 Q8 1 0.4142 0.6741 0.9237 11.00000 0.05 0.21 Q9 1 0.7750 0.1725 0.6628 11.00000 0.05 0.21 Q10 1 0.8238 -0.0034 0.8978 11.00000 0.05 0.20 Q11 1 0.6320 0.6626 0.7351 11.00000 0.05 0.20 Q12 1 0.9494 0.4869 0.6944 11.00000 0.05 0.20 Q13 1 0.5924 0.1140 0.8244 11.00000 0.05 0.20 Q14 1 0.8248 0.4945 0.7300 11.00000 0.05 0.19 Q15 1 0.5712 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