data_MR258_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.50 H16.50 P0.50 Se0.50 Si' _chemical_formula_weight 273.83 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' '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' 'Se' 'Se' -0.0929 2.2259 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9355(3) _cell_length_b 14.2567(3) _cell_length_c 19.3825(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2745.48(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6977 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.34 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_F_000 1136 _exptl_transmission_factor_min 0.7497 _exptl_transmission_factor_max 0.8994 _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _exptl_absorpt_coefficient_mu 1.529 _shelx_estimated_absorpt_T_min 0.692 _shelx_estimated_absorpt_T_max 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'D8 Venture, Bruker Photon CMOS Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14832 _diffrn_reflns_av_unetI/netI 0.0933 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.303 _diffrn_reflns_theta_max 26.377 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 5564 _reflns_number_gt 4687 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.761 _reflns_Friedel_fraction_max 0.982 _reflns_Friedel_fraction_full 0.988 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'Microsoft Word' _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^)] 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_abs_structure_details ; Flack x determined using 1647 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.042(8) _chemical_absolute_configuration rm _refine_ls_number_reflns 5564 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.3922(5) 0.3917(3) 0.6458(3) 0.0118(11) Uani 1 1 d . . . . . C2 C 0.5052(5) 0.4605(3) 0.6290(3) 0.0129(11) Uani 1 1 d . . . . . C3 C 0.5005(5) 0.4902(3) 0.5550(3) 0.0137(11) Uani 1 1 d . . . . . C4 C 0.3934(5) 0.4638(3) 0.5158(3) 0.0092(11) Uani 1 1 d . . . . . C5 C 0.1877(5) 0.5022(3) 0.6062(3) 0.0114(11) Uani 1 1 d . . . . . C6 C 0.2671(5) 0.5448(3) 0.6569(3) 0.0127(11) Uani 1 1 d . . . . . C7 C 0.3886(5) 0.4895(3) 0.6778(3) 0.0139(11) Uani 1 1 d . . . . . H7 H 0.4122 0.4925 0.7279 0.017 Uiso 1 1 calc R U . . . C8 C 0.6426(5) 0.4495(3) 0.6603(3) 0.0128(11) Uani 1 1 d . . . . . C9 C 0.7301(5) 0.3823(3) 0.6347(3) 0.0169(12) Uani 1 1 d . . . . . H9 H 0.7029 0.3434 0.5974 0.020 Uiso 1 1 calc R U . . . C10 C 0.8575(6) 0.3715(4) 0.6633(3) 0.0228(14) Uani 1 1 d . . . . . H10 H 0.9173 0.3260 0.6448 0.027 Uiso 1 1 calc R U . . . C11 C 0.8981(6) 0.4259(4) 0.7179(3) 0.0257(14) Uani 1 1 d . . . . . H11 H 0.9841 0.4168 0.7382 0.031 Uiso 1 1 calc R U . . . C12 C 0.8121(6) 0.4942(4) 0.7431(3) 0.0266(14) Uani 1 1 d . . . . . H12 H 0.8399 0.5331 0.7802 0.032 Uiso 1 1 calc R U . . . C13 C 0.6860(6) 0.5059(4) 0.7144(3) 0.0197(13) Uani 1 1 d . . . . . H13 H 0.6280 0.5532 0.7319 0.024 Uiso 1 1 calc R U . . . C14 C 0.2256(6) 0.6293(3) 0.6857(3) 0.0191(13) Uani 1 1 d . . . . . H14 H 0.2803 0.6599 0.7190 0.023 Uiso 1 1 calc R U . . . C15 C 0.1047(6) 0.6684(4) 0.6658(3) 0.0201(13) Uani 1 1 d . . . . . H15 H 0.0748 0.7251 0.6864 0.024 Uiso 1 1 calc R U . . . C16 C 0.0266(6) 0.6250(4) 0.6158(3) 0.0243(14) Uani 1 1 d . . . . . H16 H -0.0561 0.6530 0.6022 0.029 Uiso 1 1 calc R U . . . C17 C 0.0670(5) 0.5414(3) 0.5853(3) 0.0167(12) Uani 1 1 d . . . . . H17 H 0.0132 0.5119 0.5510 0.020 Uiso 1 1 calc R U . . . C18 C 0.6130(5) 0.5489(3) 0.5270(3) 0.0143(11) Uani 1 1 d . . . . . C19 C 0.7027(5) 0.5121(4) 0.4791(3) 0.0196(13) Uani 1 1 d . . . . . H19 H 0.6981 0.4474 0.4676 0.023 Uiso 1 1 calc R U . . . C20 C 0.7981(6) 0.5681(4) 0.4482(3) 0.0312(16) Uani 1 1 d . . . . . H20 H 0.8601 0.5420 0.4162 0.037 Uiso 1 1 calc R U . . . C21 C 0.8031(6) 0.6625(4) 0.4641(4) 0.0397(17) Uani 1 1 d . . . . . H21 H 0.8674 0.7018 0.4421 0.048 Uiso 1 1 calc R U . . . C22 C 0.7158(7) 0.6997(4) 0.5112(3) 0.0353(17) Uani 1 1 d . . . . . H22 H 0.7197 0.7647 0.5219 0.042 Uiso 1 1 calc R U . . . C23 C 0.6217(6) 0.6432(3) 0.5436(3) 0.0224(13) Uani 1 1 d . . . . . H23 H 0.5630 0.6692 0.5773 0.027 Uiso 1 1 calc R U . . . C24 C 0.5065(7) 0.3047(4) 0.7782(3) 0.0292(15) Uani 1 1 d . . . . . H24A H 0.6001 0.3146 0.7640 0.044 Uiso 1 1 calc R U . . . H24B H 0.5015 0.2503 0.8090 0.044 Uiso 1 1 calc R U . . . H24C H 0.4737 0.3605 0.8025 0.044 Uiso 1 1 calc R U . . . C25 C 0.4713(6) 0.1850(3) 0.6492(3) 0.0253(15) Uani 1 1 d . . . . . H25A H 0.4169 0.1760 0.6076 0.038 Uiso 1 1 calc R U . . . H25B H 0.4700 0.1275 0.6768 0.038 Uiso 1 1 calc R U . . . H25C H 0.5642 0.1998 0.6361 0.038 Uiso 1 1 calc R U . . . C26 C 0.2248(6) 0.2585(4) 0.7299(3) 0.0261(14) Uani 1 1 d . . . . . H26A H 0.1695 0.2411 0.6900 0.039 Uiso 1 1 calc R U . . . H26B H 0.1871 0.3147 0.7517 0.039 Uiso 1 1 calc R U . . . H26C H 0.2255 0.2069 0.7632 0.039 Uiso 1 1 calc R U . . . C27 C 0.4088(6) 0.3931(4) 0.3701(3) 0.0239(14) Uani 1 1 d . . . . . H27A H 0.3919 0.4070 0.3214 0.036 Uiso 1 1 calc R U . . . H27B H 0.3580 0.3370 0.3836 0.036 Uiso 1 1 calc R U . . . H27C H 0.5052 0.3819 0.3771 0.036 Uiso 1 1 calc R U . . . C28 C 0.1696(6) 0.5116(3) 0.4148(3) 0.0204(12) Uani 1 1 d . . . . . H28A H 0.1457 0.5145 0.3658 0.031 Uiso 1 1 calc R U . . . H28B H 0.1440 0.5704 0.4374 0.031 Uiso 1 1 calc R U . . . H28C H 0.1220 0.4592 0.4367 0.031 Uiso 1 1 calc R U . . . C29 C 0.4359(6) 0.6041(4) 0.3947(3) 0.0227(14) Uani 1 1 d . . . . . H29A H 0.5330 0.5941 0.3901 0.034 Uiso 1 1 calc R U . . . H29B H 0.4191 0.6535 0.4288 0.034 Uiso 1 1 calc R U . . . H29C H 0.3984 0.6230 0.3501 0.034 Uiso 1 1 calc R U . . . Si1 Si 0.40066(15) 0.28324(10) 0.70071(7) 0.0167(3) Uani 1 1 d . . . . . Si2 Si 0.35451(15) 0.49365(9) 0.42353(8) 0.0125(3) Uani 1 1 d . . . . . P1 P 0.27683(14) 0.40221(8) 0.57200(7) 0.0108(3) Uani 1 1 d . . . . . Se1 Se 0.16666(6) 0.28791(3) 0.53387(3) 0.01944(14) Uani 1 1 d . . . . . 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 C1 0.014(3) 0.013(2) 0.009(3) 0.000(2) 0.000(2) 0.003(2) C2 0.012(3) 0.014(2) 0.013(3) -0.003(2) -0.001(2) 0.003(2) C3 0.016(3) 0.010(2) 0.015(3) 0.000(2) 0.001(2) 0.002(2) C4 0.006(2) 0.011(2) 0.010(3) -0.0008(19) 0.000(2) 0.001(2) C5 0.011(3) 0.012(2) 0.011(3) 0.003(2) 0.003(2) 0.000(2) C6 0.011(3) 0.014(2) 0.013(3) 0.005(2) 0.004(2) 0.002(2) C7 0.019(3) 0.014(2) 0.009(3) -0.002(2) -0.002(2) 0.000(2) C8 0.017(3) 0.013(2) 0.008(3) 0.001(2) -0.005(2) 0.004(2) C9 0.018(3) 0.017(3) 0.016(3) -0.002(2) -0.004(3) 0.000(2) C10 0.019(3) 0.018(3) 0.032(4) 0.004(2) -0.001(3) 0.009(2) C11 0.017(3) 0.031(3) 0.028(4) 0.007(3) -0.012(3) 0.001(3) C12 0.024(4) 0.030(3) 0.026(4) -0.006(3) -0.010(3) -0.004(3) C13 0.020(3) 0.018(2) 0.021(3) -0.007(2) -0.004(3) 0.002(2) C14 0.023(3) 0.016(3) 0.018(3) 0.000(2) 0.002(3) -0.001(3) C15 0.022(3) 0.015(2) 0.024(3) 0.000(2) 0.004(3) 0.007(2) C16 0.014(3) 0.028(3) 0.030(4) 0.013(3) 0.003(3) 0.009(3) C17 0.016(3) 0.017(3) 0.017(3) 0.005(2) 0.002(2) -0.001(2) C18 0.010(2) 0.017(2) 0.016(3) 0.002(2) -0.004(2) 0.002(2) C19 0.014(3) 0.024(3) 0.021(3) 0.002(2) -0.001(2) 0.000(2) C20 0.018(3) 0.047(4) 0.028(4) 0.005(3) 0.006(3) -0.002(3) C21 0.024(4) 0.043(3) 0.051(5) 0.016(4) -0.007(4) -0.021(3) C22 0.036(4) 0.020(3) 0.050(5) 0.006(3) -0.013(3) -0.014(3) C23 0.026(3) 0.020(3) 0.021(3) -0.003(2) -0.005(3) -0.002(2) C24 0.045(4) 0.026(3) 0.016(3) 0.005(3) 0.003(3) 0.015(3) C25 0.046(4) 0.011(2) 0.019(3) 0.004(2) 0.016(3) 0.011(3) C26 0.033(3) 0.021(3) 0.025(4) 0.004(2) 0.013(3) 0.002(3) C27 0.033(4) 0.026(3) 0.012(3) -0.006(2) -0.003(3) 0.004(3) C28 0.021(3) 0.022(3) 0.018(3) 0.000(2) -0.009(3) -0.001(3) C29 0.024(3) 0.026(3) 0.018(3) 0.011(3) -0.002(3) 0.000(3) Si1 0.0261(8) 0.0125(6) 0.0115(8) 0.0026(6) 0.0069(7) 0.0076(7) Si2 0.0145(8) 0.0134(6) 0.0095(7) -0.0009(6) -0.0034(6) 0.0012(6) P1 0.0120(7) 0.0092(6) 0.0113(7) -0.0019(5) 0.0006(6) -0.0014(5) Se1 0.0215(3) 0.0156(2) 0.0212(3) -0.0052(2) 0.0012(3) -0.0083(2) _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 C2 1.526(7) . ? C1 C7 1.526(6) . ? C1 P1 1.839(5) . ? C1 Si1 1.880(5) . ? C2 C3 1.496(7) . ? C2 C8 1.501(7) . ? C2 C7 1.552(7) . ? C3 C4 1.361(7) . ? C3 C18 1.498(7) . ? C4 P1 1.817(5) . ? C4 Si2 1.877(5) . ? C5 C17 1.383(7) . ? C5 C6 1.398(7) . ? C5 P1 1.805(5) . ? C6 C14 1.390(7) . ? C6 C7 1.499(7) . ? C7 H7 1.0000 . ? C8 C9 1.386(7) . ? C8 C13 1.389(7) . ? C9 C10 1.390(7) . ? C9 H9 0.9500 . ? C10 C11 1.372(8) . ? C10 H10 0.9500 . ? C11 C12 1.384(8) . ? C11 H11 0.9500 . ? C12 C13 1.381(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.380(7) . ? C14 H14 0.9500 . ? C15 C16 1.386(8) . ? C15 H15 0.9500 . ? C16 C17 1.391(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.385(7) . ? C18 C19 1.391(7) . ? C19 C20 1.376(7) . ? C19 H19 0.9500 . ? C20 C21 1.382(8) . ? C20 H20 0.9500 . ? C21 C22 1.367(9) . ? C21 H21 0.9500 . ? C22 C23 1.384(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 Si1 1.860(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 Si1 1.857(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 Si1 1.870(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si2 1.849(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si2 1.862(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si2 1.855(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 Se1 2.0975(13) . ? 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 C2 C1 C7 61.1(3) . . ? C2 C1 P1 103.9(3) . . ? C7 C1 P1 103.2(3) . . ? C2 C1 Si1 128.0(4) . . ? C7 C1 Si1 121.5(4) . . ? P1 C1 Si1 122.4(3) . . ? C3 C2 C8 116.4(5) . . ? C3 C2 C1 111.3(4) . . ? C8 C2 C1 121.1(4) . . ? C3 C2 C7 119.1(4) . . ? C8 C2 C7 117.4(4) . . ? C1 C2 C7 59.4(3) . . ? C4 C3 C2 118.8(5) . . ? C4 C3 C18 122.4(5) . . ? C2 C3 C18 118.8(4) . . ? C3 C4 P1 107.2(4) . . ? C3 C4 Si2 129.1(4) . . ? P1 C4 Si2 123.3(3) . . ? C17 C5 C6 121.3(5) . . ? C17 C5 P1 129.5(4) . . ? C6 C5 P1 108.9(4) . . ? C14 C6 C5 119.4(5) . . ? C14 C6 C7 125.8(5) . . ? C5 C6 C7 114.6(4) . . ? C6 C7 C1 112.9(4) . . ? C6 C7 C2 125.2(4) . . ? C1 C7 C2 59.4(3) . . ? C6 C7 H7 115.4 . . ? C1 C7 H7 115.4 . . ? C2 C7 H7 115.4 . . ? C9 C8 C13 118.3(5) . . ? C9 C8 C2 119.9(5) . . ? C13 C8 C2 121.8(5) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.2(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.1(5) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? C15 C14 C6 119.7(5) . . ? C15 C14 H14 120.1 . . ? C6 C14 H14 120.1 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 121.2(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C5 C17 C16 118.1(5) . . ? C5 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C23 C18 C19 118.8(5) . . ? C23 C18 C3 120.4(5) . . ? C19 C18 C3 120.6(4) . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.5(6) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.3(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 120.1(6) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 Si1 C24 110.2(3) . . ? C25 Si1 C26 111.9(3) . . ? C24 Si1 C26 108.4(3) . . ? C25 Si1 C1 109.5(2) . . ? C24 Si1 C1 110.4(2) . . ? C26 Si1 C1 106.5(2) . . ? C27 Si2 C29 111.3(3) . . ? C27 Si2 C28 110.1(3) . . ? C29 Si2 C28 106.6(2) . . ? C27 Si2 C4 107.3(2) . . ? C29 Si2 C4 112.9(2) . . ? C28 Si2 C4 108.7(2) . . ? C5 P1 C4 98.7(2) . . ? C5 P1 C1 94.8(2) . . ? C4 P1 C1 96.2(2) . . ? C5 P1 Se1 119.14(17) . . ? C4 P1 Se1 119.79(16) . . ? C1 P1 Se1 122.43(16) . . ? 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 C7 C1 C2 C3 -112.1(5) . . . . ? P1 C1 C2 C3 -14.5(5) . . . . ? Si1 C1 C2 C3 138.9(4) . . . . ? C7 C1 C2 C8 105.5(5) . . . . ? P1 C1 C2 C8 -156.9(4) . . . . ? Si1 C1 C2 C8 -3.5(7) . . . . ? P1 C1 C2 C7 97.6(4) . . . . ? Si1 C1 C2 C7 -109.0(5) . . . . ? C8 C2 C3 C4 152.1(4) . . . . ? C1 C2 C3 C4 7.8(6) . . . . ? C7 C2 C3 C4 -58.2(6) . . . . ? C8 C2 C3 C18 -28.8(6) . . . . ? C1 C2 C3 C18 -173.1(4) . . . . ? C7 C2 C3 C18 121.0(5) . . . . ? C2 C3 C4 P1 3.6(5) . . . . ? C18 C3 C4 P1 -175.5(4) . . . . ? C2 C3 C4 Si2 177.2(4) . . . . ? C18 C3 C4 Si2 -2.0(7) . . . . ? C17 C5 C6 C14 -1.5(7) . . . . ? P1 C5 C6 C14 173.3(4) . . . . ? C17 C5 C6 C7 175.1(5) . . . . ? P1 C5 C6 C7 -10.1(5) . . . . ? C14 C6 C7 C1 169.3(5) . . . . ? C5 C6 C7 C1 -7.0(6) . . . . ? C14 C6 C7 C2 -122.9(6) . . . . ? C5 C6 C7 C2 60.7(6) . . . . ? C2 C1 C7 C6 118.5(5) . . . . ? P1 C1 C7 C6 19.7(5) . . . . ? Si1 C1 C7 C6 -122.3(4) . . . . ? P1 C1 C7 C2 -98.8(4) . . . . ? Si1 C1 C7 C2 119.2(5) . . . . ? C3 C2 C7 C6 1.1(7) . . . . ? C8 C2 C7 C6 150.5(5) . . . . ? C1 C2 C7 C6 -97.8(5) . . . . ? C3 C2 C7 C1 98.9(5) . . . . ? C8 C2 C7 C1 -111.7(5) . . . . ? C3 C2 C8 C9 -63.3(6) . . . . ? C1 C2 C8 C9 77.3(7) . . . . ? C7 C2 C8 C9 146.5(5) . . . . ? C3 C2 C8 C13 116.1(5) . . . . ? C1 C2 C8 C13 -103.3(6) . . . . ? C7 C2 C8 C13 -34.1(7) . . . . ? C13 C8 C9 C10 0.6(8) . . . . ? C2 C8 C9 C10 -180.0(5) . . . . ? C8 C9 C10 C11 1.1(8) . . . . ? C9 C10 C11 C12 -2.1(9) . . . . ? C10 C11 C12 C13 1.4(9) . . . . ? C11 C12 C13 C8 0.4(9) . . . . ? C9 C8 C13 C12 -1.4(8) . . . . ? C2 C8 C13 C12 179.2(5) . . . . ? C5 C6 C14 C15 2.2(7) . . . . ? C7 C6 C14 C15 -174.0(5) . . . . ? C6 C14 C15 C16 -1.8(8) . . . . ? C14 C15 C16 C17 0.7(8) . . . . ? C6 C5 C17 C16 0.4(8) . . . . ? P1 C5 C17 C16 -173.3(4) . . . . ? C15 C16 C17 C5 0.1(8) . . . . ? C4 C3 C18 C23 104.0(6) . . . . ? C2 C3 C18 C23 -75.1(6) . . . . ? C4 C3 C18 C19 -70.1(6) . . . . ? C2 C3 C18 C19 110.8(6) . . . . ? C23 C18 C19 C20 -0.5(8) . . . . ? C3 C18 C19 C20 173.7(5) . . . . ? C18 C19 C20 C21 -1.2(9) . . . . ? C19 C20 C21 C22 1.4(10) . . . . ? C20 C21 C22 C23 0.0(10) . . . . ? C21 C22 C23 C18 -1.7(9) . . . . ? C19 C18 C23 C22 1.9(8) . . . . ? C3 C18 C23 C22 -172.2(5) . . . . ? C2 C1 Si1 C25 -81.2(5) . . . . ? C7 C1 Si1 C25 -157.3(4) . . . . ? P1 C1 Si1 C25 67.9(4) . . . . ? C2 C1 Si1 C24 40.2(5) . . . . ? C7 C1 Si1 C24 -35.9(5) . . . . ? P1 C1 Si1 C24 -170.7(3) . . . . ? C2 C1 Si1 C26 157.6(5) . . . . ? C7 C1 Si1 C26 81.5(5) . . . . ? P1 C1 Si1 C26 -53.3(4) . . . . ? C3 C4 Si2 C27 98.6(5) . . . . ? P1 C4 Si2 C27 -88.8(3) . . . . ? C3 C4 Si2 C29 -24.3(5) . . . . ? P1 C4 Si2 C29 148.3(3) . . . . ? C3 C4 Si2 C28 -142.4(4) . . . . ? P1 C4 Si2 C28 30.2(3) . . . . ? C17 C5 P1 C4 96.4(5) . . . . ? C6 C5 P1 C4 -77.8(4) . . . . ? C17 C5 P1 C1 -166.5(5) . . . . ? C6 C5 P1 C1 19.2(4) . . . . ? C17 C5 P1 Se1 -34.9(5) . . . . ? C6 C5 P1 Se1 150.8(3) . . . . ? C3 C4 P1 C5 84.9(4) . . . . ? Si2 C4 P1 C5 -89.1(3) . . . . ? C3 C4 P1 C1 -11.0(4) . . . . ? Si2 C4 P1 C1 175.0(3) . . . . ? C3 C4 P1 Se1 -144.2(3) . . . . ? Si2 C4 P1 Se1 41.8(3) . . . . ? C2 C1 P1 C5 -84.8(4) . . . . ? C7 C1 P1 C5 -21.7(4) . . . . ? Si1 C1 P1 C5 119.9(3) . . . . ? C2 C1 P1 C4 14.5(4) . . . . ? C7 C1 P1 C4 77.6(3) . . . . ? Si1 C1 P1 C4 -140.8(3) . . . . ? C2 C1 P1 Se1 146.0(3) . . . . ? C7 C1 P1 Se1 -151.0(3) . . . . ? Si1 C1 P1 Se1 -9.4(4) . . . . ? _refine_diff_density_max 1.078 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.085 _shelx_res_file ; MR258_a.res created by SHELXL-2014/7 TITL MR258_a.res in P2(1)2(1)2(1) REM Old TITL MR258 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.083, Rweak 0.040, Alpha 0.004, Orientation as input REM Flack x = 0.108 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C29 Si2 P Br CELL 0.71073 9.9355 14.2567 19.3825 90.000 90.000 90.000 ZERR 8.000 0.0003 0.0003 0.0006 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C Si P Se H UNIT 116 8 4 4 132 TEMP -173.160 SIZE 0.18 0.20 0.26 L.S. 30 BOND $H acta conf LIST 6 FMAP 2 PLAN 20 WGHT 0.000000 FVAR 0.57733 C1 1 0.392152 0.391749 0.645789 11.00000 0.01373 0.01273 = 0.00882 -0.00048 -0.00005 0.00311 C2 1 0.505199 0.460468 0.629006 11.00000 0.01230 0.01392 = 0.01253 -0.00260 -0.00050 0.00320 C3 1 0.500518 0.490168 0.554998 11.00000 0.01608 0.01038 = 0.01475 0.00021 0.00113 0.00166 C4 1 0.393364 0.463841 0.515754 11.00000 0.00642 0.01097 = 0.01015 -0.00082 -0.00041 0.00135 C5 1 0.187651 0.502237 0.606184 11.00000 0.01081 0.01215 = 0.01124 0.00280 0.00293 -0.00008 C6 1 0.267074 0.544811 0.656856 11.00000 0.01130 0.01383 = 0.01288 0.00454 0.00376 0.00211 C7 1 0.388635 0.489482 0.677828 11.00000 0.01937 0.01389 = 0.00855 -0.00227 -0.00207 -0.00003 AFIX 13 H7 5 0.412175 0.492503 0.727941 11.00000 -1.20000 AFIX 0 C8 1 0.642555 0.449516 0.660264 11.00000 0.01719 0.01279 = 0.00844 0.00066 -0.00518 0.00388 C9 1 0.730120 0.382326 0.634684 11.00000 0.01764 0.01697 = 0.01605 -0.00188 -0.00376 0.00032 AFIX 43 H9 5 0.702934 0.343417 0.597414 11.00000 -1.20000 AFIX 0 C10 1 0.857538 0.371537 0.663258 11.00000 0.01902 0.01757 = 0.03178 0.00408 -0.00136 0.00898 AFIX 43 H10 5 0.917269 0.325992 0.644751 11.00000 -1.20000 AFIX 0 C11 1 0.898058 0.425900 0.717883 11.00000 0.01728 0.03141 = 0.02831 0.00696 -0.01188 0.00069 AFIX 43 H11 5 0.984116 0.416771 0.738161 11.00000 -1.20000 AFIX 0 C12 1 0.812117 0.494154 0.743076 11.00000 0.02445 0.02992 = 0.02554 -0.00555 -0.00962 -0.00373 AFIX 43 H12 5 0.839924 0.533071 0.780221 11.00000 -1.20000 AFIX 0 C13 1 0.685984 0.505854 0.714355 11.00000 0.02001 0.01787 = 0.02120 -0.00681 -0.00354 0.00190 AFIX 43 H13 5 0.627998 0.553186 0.731869 11.00000 -1.20000 AFIX 0 C14 1 0.225620 0.629253 0.685698 11.00000 0.02261 0.01615 = 0.01849 -0.00048 0.00221 -0.00063 AFIX 43 H14 5 0.280338 0.659919 0.718967 11.00000 -1.20000 AFIX 0 C15 1 0.104678 0.668355 0.665815 11.00000 0.02153 0.01488 = 0.02376 -0.00017 0.00378 0.00705 AFIX 43 H15 5 0.074835 0.725124 0.686423 11.00000 -1.20000 AFIX 0 C16 1 0.026568 0.625027 0.615837 11.00000 0.01435 0.02819 = 0.03022 0.01271 0.00348 0.00856 AFIX 43 H16 5 -0.056051 0.652994 0.602214 11.00000 -1.20000 AFIX 0 C17 1 0.066961 0.541361 0.585279 11.00000 0.01625 0.01737 = 0.01658 0.00462 0.00186 -0.00083 AFIX 43 H17 5 0.013183 0.511923 0.551022 11.00000 -1.20000 AFIX 0 C18 1 0.612968 0.548944 0.527007 11.00000 0.01022 0.01704 = 0.01552 0.00250 -0.00424 0.00182 C19 1 0.702709 0.512069 0.479099 11.00000 0.01415 0.02391 = 0.02065 0.00191 -0.00071 -0.00005 AFIX 43 H19 5 0.698106 0.447389 0.467550 11.00000 -1.20000 AFIX 0 C20 1 0.798124 0.568053 0.448191 11.00000 0.01827 0.04705 = 0.02826 0.00537 0.00593 -0.00191 AFIX 43 H20 5 0.860126 0.541966 0.416191 11.00000 -1.20000 AFIX 0 C21 1 0.803051 0.662509 0.464059 11.00000 0.02445 0.04341 = 0.05111 0.01617 -0.00683 -0.02106 AFIX 43 H21 5 0.867351 0.701755 0.442091 11.00000 -1.20000 AFIX 0 C22 1 0.715772 0.699697 0.511240 11.00000 0.03560 0.02010 = 0.05007 0.00563 -0.01318 -0.01431 AFIX 43 H22 5 0.719732 0.764690 0.521862 11.00000 -1.20000 AFIX 0 C23 1 0.621693 0.643246 0.543618 11.00000 0.02575 0.02001 = 0.02133 -0.00286 -0.00529 -0.00174 AFIX 43 H23 5 0.563020 0.669204 0.577280 11.00000 -1.20000 AFIX 0 C24 1 0.506532 0.304682 0.778247 11.00000 0.04503 0.02613 = 0.01640 0.00503 0.00276 0.01536 AFIX 137 H24A 5 0.600121 0.314591 0.764042 11.00000 -1.50000 H24B 5 0.501528 0.250273 0.809039 11.00000 -1.50000 H24C 5 0.473737 0.360485 0.802519 11.00000 -1.50000 AFIX 0 C25 1 0.471263 0.185035 0.649233 11.00000 0.04628 0.01088 = 0.01882 0.00386 0.01551 0.01130 AFIX 137 H25A 5 0.416917 0.176046 0.607560 11.00000 -1.50000 H25B 5 0.469985 0.127453 0.676839 11.00000 -1.50000 H25C 5 0.564152 0.199777 0.636130 11.00000 -1.50000 AFIX 0 C26 1 0.224761 0.258547 0.729853 11.00000 0.03304 0.02063 = 0.02454 0.00386 0.01268 0.00190 AFIX 137 H26A 5 0.169483 0.241111 0.689990 11.00000 -1.50000 H26B 5 0.187090 0.314733 0.751660 11.00000 -1.50000 H26C 5 0.225534 0.206857 0.763180 11.00000 -1.50000 AFIX 0 C27 1 0.408791 0.393087 0.370133 11.00000 0.03320 0.02635 = 0.01212 -0.00581 -0.00310 0.00450 AFIX 137 H27A 5 0.391946 0.406981 0.321374 11.00000 -1.50000 H27B 5 0.358046 0.337047 0.383576 11.00000 -1.50000 H27C 5 0.505152 0.381922 0.377141 11.00000 -1.50000 AFIX 0 C28 1 0.169642 0.511569 0.414837 11.00000 0.02101 0.02177 = 0.01832 -0.00037 -0.00885 -0.00059 AFIX 137 H28A 5 0.145667 0.514503 0.365839 11.00000 -1.50000 H28B 5 0.144005 0.570411 0.437431 11.00000 -1.50000 H28C 5 0.121957 0.459221 0.436663 11.00000 -1.50000 AFIX 0 C29 1 0.435862 0.604074 0.394749 11.00000 0.02384 0.02594 = 0.01840 0.01128 -0.00171 -0.00022 AFIX 137 H29A 5 0.533037 0.594090 0.390138 11.00000 -1.50000 H29B 5 0.419097 0.653497 0.428824 11.00000 -1.50000 H29C 5 0.398417 0.622957 0.350083 11.00000 -1.50000 AFIX 0 SI1 2 0.400658 0.283238 0.700709 11.00000 0.02610 0.01252 = 0.01146 0.00258 0.00690 0.00763 SI2 2 0.354514 0.493654 0.423533 11.00000 0.01446 0.01345 = 0.00948 -0.00085 -0.00342 0.00118 P1 3 0.276829 0.402205 0.571998 11.00000 0.01196 0.00921 = 0.01125 -0.00191 0.00061 -0.00142 SE1 4 0.166665 0.287908 0.533871 11.00000 0.02151 0.01565 = 0.02116 -0.00524 0.00120 -0.00826 HKLF 4 REM MR258_a.res in P2(1)2(1)2(1) REM R1 = 0.0436 for 4687 Fo > 4sig(Fo) and 0.0585 for all 5564 data REM 304 parameters refined using 0 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 1.078, deepest hole -0.484, 1-sigma level 0.085 Q1 1 0.1574 0.3264 0.4978 11.00000 0.05 1.08 Q2 1 0.2599 0.2815 0.5330 11.00000 0.05 0.40 Q3 1 0.0747 0.2814 0.5452 11.00000 0.05 0.37 Q4 1 0.6774 0.3519 0.6655 11.00000 0.05 0.37 Q5 1 0.3216 0.2488 0.7087 11.00000 0.05 0.36 Q6 1 0.3234 0.4406 0.5390 11.00000 0.05 0.36 Q7 1 0.6375 0.3817 0.5095 11.00000 0.05 0.34 Q8 1 0.2131 0.3423 0.5626 11.00000 0.05 0.34 Q9 1 0.7260 0.4787 0.7628 11.00000 0.05 0.32 Q10 1 0.3980 0.1228 0.6389 11.00000 0.05 0.32 Q11 1 0.5178 0.6220 0.3841 11.00000 0.05 0.32 Q12 1 0.2626 0.5229 0.4062 11.00000 0.05 0.32 Q13 1 0.3567 0.3986 0.6065 11.00000 0.05 0.31 Q14 1 0.0726 0.4975 0.6343 11.00000 0.05 0.31 Q15 1 0.3991 0.6005 0.5429 11.00000 0.05 0.30 Q16 1 0.2158 0.6698 0.6372 11.00000 0.05 0.30 Q17 1 0.0896 0.2617 0.5150 11.00000 0.05 0.30 Q18 1 0.6608 0.4643 0.7026 11.00000 0.05 0.30 Q19 1 0.4107 0.2373 0.6630 11.00000 0.05 0.29 Q20 1 0.6432 0.1750 0.5648 11.00000 0.05 0.29 ; _shelx_res_checksum 28515 _shelx_hkl_file ; -2 0 0 6346.77 384.56 2 0 0 6321.27 385.06 3 0 0 -2.20 7.00 -3 0 0 -2.30 6.80 4 0 0 2683.63 174.88 -4 0 0 2834.92 173.48 -5 0 0 9.40 11.30 5 0 0 18.70 15.00 6 0 0 1227.88 91.49 -6 0 0 1281.27 86.99 7 0 0 -22.40 20.60 8 0 0 79.69 30.80 10 0 0 185.48 50.49 11 0 0 69.69 55.09 12 0 0 113.29 70.69 1 1 0 2560.94 155.78 1 -1 0 2627.54 158.68 -1 1 0 2536.75 158.68 2 -1 0 217.98 20.40 2 1 0 214.68 17.30 -2 1 0 253.67 20.60 -2 -1 0 233.38 16.30 3 1 0 1089.09 71.59 -3 1 0 1084.59 73.69 3 -1 0 1107.39 74.69 -3 -1 0 1120.49 70.09 -4 -1 0 6379.26 392.46 4 -1 0 6534.05 397.86 -4 1 0 6512.55 396.56 4 1 0 6353.56 395.06 5 1 0 29.40 14.40 -5 1 0 2.80 13.30 5 -1 0 16.20 15.50 -5 -1 0 23.40 10.10 -6 1 0 271.67 34.00 6 1 0 269.87 35.70 6 -1 0 297.47 39.30 7 1 0 171.68 32.50 7 -1 0 126.79 30.00 8 1 0 2339.67 165.18 8 -1 0 2451.55 168.78 9 -1 0 101.99 41.20 9 1 0 167.68 41.30 10 -1 0 1199.48 113.19 10 1 0 1242.78 110.09 11 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83.09 -1 -1 -24 48.10 81.09 1 -1 24 114.29 75.09 1 -1 -24 -92.19 76.59 -1 1 -24 79.89 84.79 0 -2 -24 8.00 78.89 0 2 -24 8.90 72.59 1 2 -24 665.43 109.99 -1 -2 -24 514.75 107.09 1 -2 -24 367.36 101.69 -1 2 -24 520.85 102.89 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95836 #============================================================================== _publ_requested_journal '??????' _publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END====================================================