data_1 _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2014). CrystalStructure. Version 4.1. Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SHELXS97 Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H15 P Se2' _chemical_formula_moiety 'C14 H15 P Se2' _chemical_formula_weight 372.17 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _symmetry_equiv_pos_site_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 7.3880(15) _cell_length_b 10.3745(19) _cell_length_c 10.8099(19) _cell_angle_alpha 107.355(8) _cell_angle_beta 107.255(8) _cell_angle_gamma 106.126(8) _cell_volume 691.6(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4347 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.47 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364.00 _exptl_absorpt_coefficient_mu 5.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.849 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.286 _diffrn_reflns_number 5346 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.246 _diffrn_reflns_theta_full 24.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2422 _reflns_number_gt 1928 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0652 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2422 _refine_ls_number_parameters 154 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.6478P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.51 _refine_diff_density_min -0.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'P' 'P' 0.1023 0.0942 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Se' 'Se' -0.0929 2.2259 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.42240(7) 0.87759(5) 0.31426(4) 0.02592(14) Uani 1 2 d . . . Se2 Se 0.86228(6) 0.95971(4) 0.26088(4) 0.02246(13) Uani 1 2 d . . . P1 P 0.73444(17) 0.87350(12) 0.39670(11) 0.0209(2) Uani 1 2 d . . . C1 C 0.3163(7) 0.7949(5) 0.1103(4) 0.0219(9) Uani 1 2 d . . . C2 C 0.1041(7) 0.7219(5) 0.0479(5) 0.0300(10) Uani 1 2 d . . . C3 C -0.0106(7) 0.6718(5) -0.0986(5) 0.0325(11) Uani 1 2 d . . . C4 C 0.0896(7) 0.6948(5) -0.1815(4) 0.0282(10) Uani 1 2 d . . . C5 C 0.3065(7) 0.7637(5) -0.1245(4) 0.0227(9) Uani 1 2 d . . . C6 C 0.4040(7) 0.7817(5) -0.2166(4) 0.0260(10) Uani 1 2 d . . . C7 C 0.6127(7) 0.8411(5) -0.1666(4) 0.0275(10) Uani 1 2 d . . . C8 C 0.7319(7) 0.8845(4) -0.0233(4) 0.0228(9) Uani 1 2 d . . . C9 C 0.6465(7) 0.8745(4) 0.0718(4) 0.0210(9) Uani 1 2 d . . . C10 C 0.4270(7) 0.8138(4) 0.0241(4) 0.0200(9) Uani 1 2 d . . . C11 C 0.6973(7) 0.6749(4) 0.3367(4) 0.0225(9) Uani 1 2 d . . . C12 C 0.5827(8) 0.6140(5) 0.4174(5) 0.0342(11) Uani 1 2 d . . . C13 C 0.5817(7) 0.5823(5) 0.1777(4) 0.0257(10) Uani 1 2 d . . . C14 C 0.9158(7) 0.6786(5) 0.3894(4) 0.0299(11) Uani 1 2 d . . . H2 H 0.03338 0.70504 0.10575 0.0360 Uiso 1 2 calc R . . H3 H -0.15704 0.62216 -0.13933 0.0390 Uiso 1 2 calc R . . H4 H 0.01164 0.66386 -0.28022 0.0338 Uiso 1 2 calc R . . H6 H 0.3219 0.7518 -0.3145 0.0312 Uiso 1 2 calc R . . H7 H 0.67732 0.85299 -0.22881 0.0330 Uiso 1 2 calc R . . H8 H 0.87828 0.9225 0.01005 0.0273 Uiso 1 2 calc R . . H12A H 0.66033 0.67559 0.5198 0.0410 Uiso 1 2 calc R . . H12B H 0.44445 0.61493 0.38609 0.0410 Uiso 1 2 calc R . . H12C H 0.57014 0.5127 0.39792 0.0410 Uiso 1 2 calc R . . H13A H 0.44212 0.58091 0.14541 0.0309 Uiso 1 2 calc R . . H13B H 0.65591 0.62477 0.12825 0.0309 Uiso 1 2 calc R . . H13C H 0.57224 0.48141 0.15657 0.0309 Uiso 1 2 calc R . . H14A H 0.98866 0.73879 0.49229 0.0359 Uiso 1 2 calc R . . H14B H 0.90749 0.57804 0.36903 0.0359 Uiso 1 2 calc R . . H14C H 0.99116 0.7214 0.34071 0.0359 Uiso 1 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Se1 0.0235(3) 0.0352(3) 0.0242(2) 0.0160(2) 0.0136(2) 0.01129(19) Se2 0.0174(3) 0.0236(3) 0.0237(2) 0.0055(2) 0.00734(18) 0.01006(18) P1 0.0196(6) 0.0228(6) 0.0198(5) 0.0089(5) 0.0081(5) 0.0079(5) C1 0.020(3) 0.023(2) 0.025(2) 0.013(2) 0.0090(19) 0.0101(18) C2 0.019(3) 0.036(3) 0.038(3) 0.014(2) 0.014(2) 0.014(2) C3 0.016(3) 0.032(3) 0.040(3) 0.010(2) 0.004(2) 0.010(2) C4 0.028(3) 0.027(3) 0.026(2) 0.017(2) 0.005(2) 0.0068(19) C5 0.022(3) 0.024(2) 0.025(2) 0.015(2) 0.0084(19) 0.0088(18) C6 0.033(3) 0.026(3) 0.020(2) 0.017(2) 0.009(2) 0.0076(18) C7 0.039(3) 0.028(3) 0.026(2) 0.019(2) 0.019(2) 0.015(2) C8 0.021(2) 0.021(2) 0.028(2) 0.008(2) 0.0124(19) 0.0113(19) C9 0.025(3) 0.020(2) 0.024(2) 0.013(2) 0.0103(19) 0.0113(18) C10 0.023(3) 0.016(2) 0.020(2) 0.010(2) 0.0069(18) 0.0056(17) C11 0.026(3) 0.022(2) 0.019(2) 0.010(2) 0.0091(18) 0.0083(18) C12 0.041(3) 0.033(3) 0.033(3) 0.013(2) 0.019(2) 0.018(2) C13 0.029(3) 0.019(2) 0.025(2) 0.008(2) 0.010(2) 0.0082(18) C14 0.032(3) 0.025(3) 0.029(2) 0.014(2) 0.007(2) 0.0097(19) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.1 (Rigaku, 2014)' _computing_molecular_graphics 'CrystalStructure 4.1' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Se1 P1 2.2291(15) yes . . Se1 C1 1.919(4) yes . . Se2 P1 2.2326(15) yes . . Se2 C9 1.925(4) yes . . P1 C11 1.878(5) yes . . C1 C2 1.377(6) yes . . C1 C10 1.431(7) yes . . C2 C3 1.402(6) yes . . C3 C4 1.352(8) yes . . C4 C5 1.405(6) yes . . C5 C6 1.417(8) yes . . C5 C10 1.428(5) yes . . C6 C7 1.352(7) yes . . C7 C8 1.390(6) yes . . C8 C9 1.369(7) yes . . C9 C10 1.427(6) yes . . C11 C12 1.532(8) yes . . C11 C13 1.514(5) yes . . C11 C14 1.529(7) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C4 H4 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C12 H12A 0.980 no . . C12 H12B 0.980 no . . C12 H12C 0.980 no . . C13 H13A 0.980 no . . C13 H13B 0.980 no . . C13 H13C 0.980 no . . C14 H14A 0.980 no . . C14 H14B 0.980 no . . C14 H14C 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 P1 Se1 C1 107.40(16) yes . . . P1 Se2 C9 108.58(15) yes . . . Se1 P1 Se2 98.87(6) yes . . . Se1 P1 C11 107.36(14) yes . . . Se2 P1 C11 106.74(17) yes . . . Se1 C1 C2 111.6(4) yes . . . Se1 C1 C10 128.0(3) yes . . . C2 C1 C10 120.0(4) yes . . . C1 C2 C3 121.8(5) yes . . . C2 C3 C4 119.3(4) yes . . . C3 C4 C5 121.4(4) yes . . . C4 C5 C6 119.1(4) yes . . . C4 C5 C10 120.4(5) yes . . . C6 C5 C10 120.5(4) yes . . . C5 C6 C7 120.7(4) yes . . . C6 C7 C8 119.4(5) yes . . . C7 C8 C9 122.6(4) yes . . . Se2 C9 C8 109.8(3) yes . . . Se2 C9 C10 130.1(4) yes . . . C8 C9 C10 120.0(4) yes . . . C1 C10 C5 117.0(4) yes . . . C1 C10 C9 126.2(4) yes . . . C5 C10 C9 116.8(4) yes . . . P1 C11 C12 105.2(3) yes . . . P1 C11 C13 115.4(4) yes . . . P1 C11 C14 105.1(3) yes . . . C12 C11 C13 111.0(3) yes . . . C12 C11 C14 109.4(4) yes . . . C13 C11 C14 110.4(4) yes . . . C1 C2 H2 119.091 no . . . C3 C2 H2 119.094 no . . . C2 C3 H3 120.362 no . . . C4 C3 H3 120.358 no . . . C3 C4 H4 119.313 no . . . C5 C4 H4 119.313 no . . . C5 C6 H6 119.674 no . . . C7 C6 H6 119.675 no . . . C6 C7 H7 120.317 no . . . C8 C7 H7 120.323 no . . . C7 C8 H8 118.694 no . . . C9 C8 H8 118.696 no . . . C11 C12 H12A 109.469 no . . . C11 C12 H12B 109.467 no . . . C11 C12 H12C 109.469 no . . . H12A C12 H12B 109.474 no . . . H12A C12 H12C 109.475 no . . . H12B C12 H12C 109.473 no . . . C11 C13 H13A 109.472 no . . . C11 C13 H13B 109.469 no . . . C11 C13 H13C 109.475 no . . . H13A C13 H13B 109.467 no . . . H13A C13 H13C 109.471 no . . . H13B C13 H13C 109.473 no . . . C11 C14 H14A 109.475 no . . . C11 C14 H14B 109.470 no . . . C11 C14 H14C 109.469 no . . . H14A C14 H14B 109.474 no . . . H14A C14 H14C 109.473 no . . . H14B C14 H14C 109.467 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 P1 Se1 C1 C2 148.1(3) no . . . . P1 Se1 C1 C10 -38.6(4) no . . . . C1 Se1 P1 Se2 45.43(15) no . . . . C1 Se1 P1 C11 -65.31(16) no . . . . P1 Se2 C9 C8 -160.1(2) no . . . . P1 Se2 C9 C10 22.9(4) no . . . . C9 Se2 P1 Se1 -39.65(17) no . . . . C9 Se2 P1 C11 71.59(17) no . . . . Se1 P1 C11 C12 -67.3(2) no . . . . Se1 P1 C11 C13 55.4(3) no . . . . Se1 P1 C11 C14 177.23(18) no . . . . Se2 P1 C11 C12 -172.51(15) no . . . . Se2 P1 C11 C13 -49.8(3) no . . . . Se2 P1 C11 C14 72.0(2) no . . . . Se1 C1 C2 C3 170.3(3) no . . . . Se1 C1 C10 C5 -168.4(3) no . . . . Se1 C1 C10 C9 13.3(7) no . . . . C2 C1 C10 C5 4.4(7) no . . . . C2 C1 C10 C9 -173.9(4) no . . . . C10 C1 C2 C3 -3.6(8) no . . . . C1 C2 C3 C4 0.3(8) no . . . . C2 C3 C4 C5 2.1(8) no . . . . C3 C4 C5 C6 178.4(4) no . . . . C3 C4 C5 C10 -1.2(7) no . . . . C4 C5 C6 C7 -176.8(4) no . . . . C4 C5 C10 C1 -2.0(7) no . . . . C4 C5 C10 C9 176.4(4) no . . . . C6 C5 C10 C1 178.4(4) no . . . . C6 C5 C10 C9 -3.2(7) no . . . . C10 C5 C6 C7 2.7(7) no . . . . C5 C6 C7 C8 0.1(7) no . . . . C6 C7 C8 C9 -2.4(7) no . . . . C7 C8 C9 Se2 -175.5(4) no . . . . C7 C8 C9 C10 1.8(7) no . . . . Se2 C9 C10 C1 -4.2(7) no . . . . Se2 C9 C10 C5 177.6(3) no . . . . C8 C9 C10 C1 179.2(4) no . . . . C8 C9 C10 C5 1.0(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Se1 C9 3.488(5) no . . Se1 C12 3.599(6) no . . Se2 C1 3.529(4) no . . Se2 C13 3.567(4) no . . C1 C4 2.789(6) no . . C1 C13 3.428(8) no . . C2 C5 2.770(8) no . . C3 C10 2.833(6) no . . C5 C8 2.756(6) no . . C6 C9 2.792(6) no . . C7 C10 2.833(8) no . . C9 C13 3.510(7) no . . C10 C13 3.551(7) no . . Se2 P1 3.5135(12) no . 2_776 P1 Se2 3.5135(12) no . 2_776 P1 P1 3.5857(15) no . 2_776 C1 C7 3.500(7) no . 2_675 C3 C8 3.366(8) no . 1_455 C5 C9 3.524(7) no . 2_675 C7 C1 3.500(7) no . 2_675 C7 C10 3.583(7) no . 2_675 C8 C3 3.366(8) no . 1_655 C9 C5 3.524(7) no . 2_675 C10 C7 3.583(7) no . 2_675 C12 C12 3.535(8) no . 2_666 C13 C13 3.365(6) no . 2_665 Se1 H2 2.7271 no . . Se1 H12B 3.0804 no . . Se1 H13A 3.1435 no . . Se2 H8 2.6657 no . . Se2 H13B 3.0402 no . . Se2 H14C 3.1396 no . . P1 H12A 2.7792 no . . P1 H12B 2.8770 no . . P1 H13A 3.0358 no . . P1 H13B 3.0197 no . . P1 H14A 2.7779 no . . P1 H14C 2.8683 no . . C1 H3 3.2803 no . . C1 H13A 2.7153 no . . C1 H13B 3.4380 no . . C2 H4 3.2360 no . . C2 H13A 3.2976 no . . C4 H2 3.2273 no . . C4 H6 2.6023 no . . C5 H3 3.2633 no . . C5 H7 3.2685 no . . C6 H4 2.5917 no . . C6 H8 3.2162 no . . C8 H6 3.2282 no . . C8 H13B 3.5488 no . . C9 H7 3.2702 no . . C9 H13A 3.4347 no . . C9 H13B 2.8477 no . . C10 H2 3.2865 no . . C10 H4 3.3114 no . . C10 H6 3.3237 no . . C10 H8 3.2752 no . . C10 H13A 3.0860 no . . C10 H13B 3.1631 no . . C12 H13A 2.6885 no . . C12 H13B 3.3542 no . . C12 H13C 2.7102 no . . C12 H14A 2.6650 no . . C12 H14B 2.7008 no . . C12 H14C 3.3466 no . . C13 H12A 3.3508 no . . C13 H12B 2.7034 no . . C13 H12C 2.7034 no . . C13 H14A 3.3420 no . . C13 H14B 2.6896 no . . C13 H14C 2.6897 no . . C14 H12A 2.6684 no . . C14 H12B 3.3461 no . . C14 H12C 2.6988 no . . C14 H13A 3.3449 no . . C14 H13B 2.6862 no . . C14 H13C 2.6862 no . . H2 H3 2.3442 no . . H2 H13A 3.5613 no . . H3 H4 2.2977 no . . H4 H6 2.4016 no . . H6 H7 2.3023 no . . H7 H8 2.3263 no . . H12A H13A 3.5807 no . . H12A H13C 3.5966 no . . H12A H14A 2.4623 no . . H12A H14B 2.9703 no . . H12A H14C 3.5579 no . . H12B H13A 2.5132 no . . H12B H13B 3.5894 no . . H12B H13C 3.0053 no . . H12B H14A 3.5562 no . . H12B H14B 3.5976 no . . H12C H13A 2.9730 no . . H12C H13B 3.6000 no . . H12C H13C 2.5365 no . . H12C H14A 2.9623 no . . H12C H14B 2.5334 no . . H12C H14C 3.5978 no . . H13A H14B 3.5825 no . . H13A H14C 3.5826 no . . H13B H14A 3.5773 no . . H13B H14B 2.9745 no . . H13B H14C 2.5074 no . . H13C H14A 3.5773 no . . H13C H14B 2.5074 no . . H13C H14C 2.9746 no . . Se1 H7 3.3895 no . 2_675 Se1 H14C 3.2874 no . 1_455 Se2 H2 3.4439 no . 1_655 Se2 H6 3.5834 no . 2_675 Se2 H7 3.5910 no . 2_775 Se2 H14A 3.0790 no . 2_776 P1 H14A 3.5912 no . 2_776 C1 H7 3.4738 no . 2_675 C2 H8 3.0518 no . 1_455 C2 H14C 3.5054 no . 1_455 C3 H7 3.5906 no . 1_455 C3 H8 2.9591 no . 1_455 C3 H12B 3.4725 no . 2_565 C3 H13A 3.3020 no . 2_565 C4 H13C 3.4772 no . 2_665 C4 H14A 3.5763 no . 1_454 C4 H14B 2.9602 no . 2_665 C5 H13C 2.8831 no . 2_665 C5 H14B 3.2974 no . 2_665 C6 H12C 3.1909 no . 2_665 C6 H13C 3.0265 no . 2_665 C6 H14A 3.4917 no . 1_454 C6 H14B 3.3542 no . 2_665 C7 H3 3.2226 no . 1_655 C7 H8 3.4126 no . 2_775 C7 H12A 3.4833 no . 1_554 C7 H12C 3.3636 no . 2_665 C7 H13C 3.2918 no . 2_665 C8 H2 3.5187 no . 1_655 C8 H3 3.0770 no . 1_655 C8 H8 2.9509 no . 2_775 C8 H13C 3.4074 no . 2_665 C9 H13C 3.3498 no . 2_665 C10 H13C 3.1055 no . 2_665 C12 H3 3.2630 no . 2_565 C12 H4 3.5959 no . 1_656 C12 H12A 3.4143 no . 2_666 C12 H12C 3.0115 no . 2_666 C13 H3 3.0857 no . 2_565 C13 H13A 3.3226 no . 2_665 C13 H13B 2.9761 no . 2_665 C13 H13C 3.2414 no . 2_665 C14 H2 3.4904 no . 1_655 C14 H4 3.4878 no . 1_656 C14 H6 3.3781 no . 1_656 H2 Se2 3.4439 no . 1_455 H2 C8 3.5187 no . 1_455 H2 C14 3.4904 no . 1_455 H2 H8 3.0981 no . 1_455 H2 H13A 3.5015 no . 2_565 H2 H13B 2.7862 no . 1_455 H2 H14C 2.6114 no . 1_455 H3 C7 3.2226 no . 1_455 H3 C8 3.0770 no . 1_455 H3 C12 3.2630 no . 2_565 H3 C13 3.0857 no . 2_565 H3 H7 3.2366 no . 1_455 H3 H8 2.9464 no . 1_455 H3 H12B 2.7383 no . 2_565 H3 H12C 3.0528 no . 2_565 H3 H13A 2.4998 no . 2_565 H3 H13B 3.5528 no . 1_455 H3 H13C 2.8826 no . 2_565 H4 C12 3.5959 no . 1_454 H4 C14 3.4878 no . 1_454 H4 H12A 2.9032 no . 1_454 H4 H12B 3.3694 no . 2_565 H4 H12C 3.5178 no . 1_454 H4 H14A 2.7652 no . 1_454 H4 H14B 3.4111 no . 1_454 H4 H14B 2.7042 no . 2_665 H6 Se2 3.5834 no . 2_675 H6 C14 3.3781 no . 1_454 H6 H12C 3.0241 no . 2_665 H6 H13C 3.4790 no . 2_665 H6 H14A 2.6530 no . 1_454 H6 H14B 3.3716 no . 1_454 H6 H14B 3.1483 no . 2_665 H7 Se1 3.3895 no . 2_675 H7 Se2 3.5910 no . 2_775 H7 C1 3.4738 no . 2_675 H7 C3 3.5906 no . 1_655 H7 H3 3.2366 no . 1_655 H7 H8 3.1075 no . 2_775 H7 H12A 2.7337 no . 1_554 H7 H12C 3.3323 no . 2_665 H8 C2 3.0518 no . 1_655 H8 C3 2.9591 no . 1_655 H8 C7 3.4126 no . 2_775 H8 C8 2.9509 no . 2_775 H8 H2 3.0981 no . 1_655 H8 H3 2.9464 no . 1_655 H8 H7 3.1075 no . 2_775 H8 H8 2.1683 no . 2_775 H12A C7 3.4833 no . 1_556 H12A C12 3.4143 no . 2_666 H12A H4 2.9032 no . 1_656 H12A H7 2.7337 no . 1_556 H12A H12A 3.5697 no . 2_666 H12A H12B 3.4233 no . 2_666 H12A H12C 2.7556 no . 2_666 H12B C3 3.4725 no . 2_565 H12B H3 2.7383 no . 2_565 H12B H4 3.3694 no . 2_565 H12B H12A 3.4233 no . 2_666 H12B H12C 3.0217 no . 2_666 H12C C6 3.1909 no . 2_665 H12C C7 3.3636 no . 2_665 H12C C12 3.0115 no . 2_666 H12C H3 3.0528 no . 2_565 H12C H4 3.5178 no . 1_656 H12C H6 3.0241 no . 2_665 H12C H7 3.3323 no . 2_665 H12C H12A 2.7556 no . 2_666 H12C H12B 3.0217 no . 2_666 H12C H12C 2.7507 no . 2_666 H13A C3 3.3020 no . 2_565 H13A C13 3.3226 no . 2_665 H13A H2 3.5015 no . 2_565 H13A H3 2.4998 no . 2_565 H13A H13A 3.5605 no . 2_665 H13A H13B 2.8167 no . 2_665 H13A H13C 3.0956 no . 2_665 H13B C13 2.9761 no . 2_665 H13B H2 2.7862 no . 1_655 H13B H3 3.5528 no . 1_655 H13B H13A 2.8167 no . 2_665 H13B H13B 2.8831 no . 2_665 H13B H13C 2.7204 no . 2_665 H13C C4 3.4772 no . 2_665 H13C C5 2.8831 no . 2_665 H13C C6 3.0265 no . 2_665 H13C C7 3.2918 no . 2_665 H13C C8 3.4074 no . 2_665 H13C C9 3.3498 no . 2_665 H13C C10 3.1055 no . 2_665 H13C C13 3.2414 no . 2_665 H13C H3 2.8826 no . 2_565 H13C H6 3.4790 no . 2_665 H13C H13A 3.0956 no . 2_665 H13C H13B 2.7204 no . 2_665 H13C H13C 3.4074 no . 2_665 H14A Se2 3.0790 no . 2_776 H14A P1 3.5912 no . 2_776 H14A C4 3.5763 no . 1_656 H14A C6 3.4917 no . 1_656 H14A H4 2.7652 no . 1_656 H14A H6 2.6530 no . 1_656 H14B C4 2.9602 no . 2_665 H14B C5 3.2974 no . 2_665 H14B C6 3.3542 no . 2_665 H14B H4 3.4111 no . 1_656 H14B H4 2.7042 no . 2_665 H14B H6 3.3716 no . 1_656 H14B H6 3.1483 no . 2_665 H14C Se1 3.2874 no . 1_655 H14C C2 3.5054 no . 1_655 H14C H2 2.6114 no . 1_655 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL PSC21-1-FS CELL 0.71075 7.38800 10.37450 10.80990 107.35500 107.25500 106.12600 ZERR 2 0.00152 0.00187 0.00187 0.00760 0.00750 0.00750 LATT 1 SFAC C H P SE UNIT 28 30 2 4 SHEL 99999.000000 0.840885 OMIT 0 0 1 OMIT 0 -6 9 L.S. 10 FMAP 2 PLAN -10 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -148.0 ACTA SIZE 0.120 0.060 0.030 WGHT 0.026700 0.647800 FVAR 1.43669 SE1 4 0.422396 0.877595 0.314264 11.00000 0.02349 0.03519 = 0.02423 0.01129 0.01357 0.01601 SE2 4 0.862284 0.959712 0.260878 11.00000 0.01737 0.02364 = 0.02369 0.01006 0.00734 0.00552 P1 3 0.734436 0.873502 0.396699 11.00000 0.01957 0.02281 = 0.01979 0.00788 0.00806 0.00890 C1 1 0.316344 0.794860 0.110338 11.00000 0.02011 0.02316 = 0.02515 0.01014 0.00896 0.01268 C2 1 0.104088 0.721896 0.047924 11.00000 0.01905 0.03554 = 0.03815 0.01406 0.01372 0.01387 AFIX 43 H2 2 0.033377 0.705043 0.105754 11.00000 -1.20000 AFIX 0 C3 1 -0.010571 0.671782 -0.098641 11.00000 0.01628 0.03227 = 0.03959 0.00995 0.00398 0.01033 AFIX 43 H3 2 -0.157036 0.622157 -0.139329 11.00000 -1.20000 AFIX 0 C4 1 0.089575 0.694849 -0.181451 11.00000 0.02750 0.02745 = 0.02570 0.00681 0.00498 0.01662 AFIX 43 H4 2 0.011636 0.663861 -0.280218 11.00000 -1.20000 AFIX 0 C5 1 0.306491 0.763687 -0.124473 11.00000 0.02185 0.02371 = 0.02455 0.00875 0.00839 0.01451 C6 1 0.403983 0.781708 -0.216621 11.00000 0.03283 0.02614 = 0.01980 0.00755 0.00931 0.01669 AFIX 43 H6 2 0.321902 0.751800 -0.314501 11.00000 -1.20000 AFIX 0 C7 1 0.612727 0.841063 -0.166605 11.00000 0.03879 0.02809 = 0.02632 0.01474 0.01880 0.01859 AFIX 43 H7 2 0.677324 0.852990 -0.228813 11.00000 -1.20000 AFIX 0 C8 1 0.731860 0.884456 -0.023271 11.00000 0.02097 0.02136 = 0.02839 0.01131 0.01240 0.00842 AFIX 43 H8 2 0.878275 0.922505 0.010052 11.00000 -1.20000 AFIX 0 C9 1 0.646534 0.874530 0.071787 11.00000 0.02452 0.01960 = 0.02380 0.01125 0.01032 0.01266 C10 1 0.426969 0.813820 0.024119 11.00000 0.02253 0.01574 = 0.02022 0.00563 0.00688 0.00988 C11 1 0.697318 0.674862 0.336652 11.00000 0.02569 0.02216 = 0.01948 0.00835 0.00908 0.01004 C12 1 0.582740 0.614043 0.417389 11.00000 0.04133 0.03288 = 0.03343 0.01827 0.01895 0.01339 AFIX 33 H12A 2 0.660329 0.675590 0.519802 11.00000 -1.20000 H12B 2 0.444451 0.614931 0.386095 11.00000 -1.20000 H12C 2 0.570139 0.512698 0.397921 11.00000 -1.20000 AFIX 0 C13 1 0.581695 0.582323 0.177696 11.00000 0.02894 0.01938 = 0.02539 0.00821 0.00973 0.00779 AFIX 33 H13A 2 0.442121 0.580912 0.145410 11.00000 -1.20000 H13B 2 0.655906 0.624767 0.128247 11.00000 -1.20000 H13C 2 0.572237 0.481407 0.156569 11.00000 -1.20000 AFIX 0 C14 1 0.915761 0.678608 0.389407 11.00000 0.03190 0.02524 = 0.02895 0.00973 0.00738 0.01384 AFIX 33 H14A 2 0.988663 0.738793 0.492291 11.00000 -1.20000 H14B 2 0.907490 0.578036 0.369034 11.00000 -1.20000 H14C 2 0.991159 0.721396 0.340713 11.00000 -1.20000 AFIX 0 HKLF 4 REM PSC21-1-FS REM R1 = 0.0326 for 1928 Fo > 4sig(Fo) and 0.0481 for all 2422 data REM 154 parameters refined using 0 restraints END WGHT 0.0248 0.1883 REM Instructions for potential hydrogen bonds HTAB C12 Se1 HTAB C13 Se1 HTAB C13 Se2 EQIV $1 -x+2, -y+2, -z+1 HTAB C14 Se2_$1 HTAB C14 Se2 REM Highest difference peak 0.506, deepest hole -0.656, 1-sigma level 0.107 Q1 1 0.3110 1.0378 0.2256 11.00000 0.05 0.51 Q2 1 0.8310 0.9577 0.3257 11.00000 0.05 0.48 Q3 1 0.2593 0.7726 0.1601 11.00000 0.05 0.46 Q4 1 0.3496 0.7533 0.2663 11.00000 0.05 0.45 Q5 1 0.3692 0.7578 0.3165 11.00000 0.05 0.42 Q6 1 0.3762 0.8342 -0.3234 11.00000 0.05 0.41 Q7 1 0.5676 0.7376 -0.3656 11.00000 0.05 0.39 Q8 1 0.7983 0.8656 0.2135 11.00000 0.05 0.38 Q9 1 0.9038 1.0643 0.3210 11.00000 0.05 0.38 Q10 1 0.2161 0.7333 0.0489 11.00000 0.05 0.38 ; _shelx_res_checksum 19927 _shelx_hkl_file ; 0 0 1 -12.55 6.49 0 0 1 0.64 8.40 0 0 -1 -16.21 11.35 0 -1 026918.14 981.83 0 1 -111182.49 324.64 0 1 -111392.43 316.44 0 -1 111644.31 330.68 -1 0 1 5230.69 146.05 1 0 -1 5210.53 158.08 -1 0 1 5229.37 169.94 1 0 -1 5404.70 161.76 1 -1 0 5.08 15.07 1 -1 0 -9.75 28.53 1 -1 0 2.54 17.42 1 0 0 4118.76 117.72 -1 0 0 4333.02 154.93 1 -1 -115186.38 523.00 -1 1 115353.24 503.34 1 -1 -115720.27 519.32 -1 1 115212.97 512.20 0 1 1 6163.41 220.33 0 1 1 5865.93 180.45 0 -1 -1 5897.12 226.39 -1 1 -1 956.45 59.81 1 -1 1 836.69 64.45 1 1 -1 2284.71 119.00 -1 -1 1 2167.63 117.10 1 1 -1 2392.36 123.47 -1 -1 1 2215.06 92.90 0 1 -2 442.42 20.98 0 -1 2 418.99 27.04 0 -1 2 442.79 56.88 0 1 -2 543.13 57.54 0 -2 121632.41 731.93 0 -2 124135.05 925.72 0 2 -124479.47 940.59 1 0 -2 2016.61 87.67 -1 0 2 2085.52 112.84 -1 0 2 1958.52 77.23 1 0 -2 1993.18 80.01 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2160.25 111.74 1 2 -1 2209.95 88.45 -1 -2 1 2407.99 133.72 1 -2 2 8920.99 272.05 1 -2 2 8918.14 289.41 1 2 -221299.33 802.44 1 2 -221293.15 760.62 -1 -2 220734.60 758.52 -1 -2 220375.12 721.13 0 2 1 3948.44 157.35 0 -2 -1 3950.71 186.94 2 0 -117008.69 655.32 -2 0 116928.10 585.40 2 0 -116347.94 619.54 2 -1 0 358.63 48.89 -2 1 0 337.88 44.85 -1 -1 3 79.64 30.83 1 1 -3 107.26 32.61 -1 -1 3 127.40 37.85 1 1 -3 78.59 34.70 -1 -1 -1 633.93 51.08 1 1 1 684.83 81.76 0 -1 3 3702.43 154.45 0 -1 3 3650.06 173.28 0 1 -3 3875.20 137.67 1 0 -3 518.19 72.18 1 0 -3 630.21 47.24 -1 0 3 562.79 78.67 1 0 -3 580.28 48.38 2 0 -2 927.32 84.59 2 0 -2 923.40 65.16 -2 0 2 700.50 69.79 -2 0 2 831.55 74.32 1 -3 128652.82 1146.56 -1 3 -129787.14 1139.29 2 -2 010509.85 377.59 2 -2 011476.43 414.13 2 -2 011415.96 414.12 2 -1 -2 3159.68 148.03 -2 1 2 3329.76 125.79 2 -1 -2 3227.32 147.67 -2 1 2 3180.14 113.50 0 3 -125940.65 1007.93 0 -3 126332.94 1063.04 0 -2 3 3035.12 93.52 0 2 -3 3131.61 127.17 0 2 -3 3184.29 102.51 0 -2 3 3188.80 110.31 1 -3 064933.00 2908.36 -1 3 063313.36 3025.50 -1 3 064091.99 2879.66 1 -3 066322.58 3200.90 1 -3 062877.55 3006.73 2 -2 -1 6608.67 224.96 2 -2 -1 6668.81 252.62 2 -2 -1 6468.07 224.19 -2 2 1 6005.06 223.08 2 0 0 361.42 50.94 -2 0 0 346.45 46.12 0 -3 2 569.44 44.68 0 3 -2 680.77 38.50 0 3 -2 637.28 76.75 0 -3 2 731.28 75.77 1 0 2 785.83 65.25 -1 0 -2 760.81 55.49 1 2 0 454.18 77.74 -1 -2 0 181.61 68.99 0 0 -3 7884.71 264.99 0 0 3 7479.98 267.38 0 0 3 7553.56 262.60 0 0 -3 7940.41 294.45 0 0 -3 8174.59 225.00 -1 2 2 837.35 90.78 -1 2 2 879.06 83.49 -1 2 2 876.29 74.11 1 -2 -2 825.63 64.64 1 -2 -2 1054.17 97.54 1 -2 -2 759.21 73.77 -1 -2 3 6104.57 197.36 1 2 -3 5931.72 209.59 -1 -2 3 5888.37 217.90 1 -3 211001.28 339.15 1 -3 210862.61 355.13 -1 3 -211142.54 376.10 2 1 -2 5278.52 214.27 -2 -1 2 5300.26 204.57 2 1 -2 5025.04 176.21 -2 -1 2 5045.91 226.72 -2 2 -1 505.44 43.23 2 -2 1 495.41 66.45 -2 1 -1 9476.27 323.90 2 -1 1 9051.75 328.99 0 3 0 149.56 70.87 0 -3 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