#------------------------------------------------------------------------------ #$Date: 2019-06-05 03:19:39 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215692 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551206.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1551206 _journal_paper_doi 10.1039/C9SC01960J _chemical_formula_sum 'C18 H56 N4 Si6 Th' _chemical_formula_weight 729.24 _space_group_crystal_system trigonal _space_group_IT_number 167 _space_group_name_Hall '-R 3 2"c' _space_group_name_H-M_alt 'R -3 c :H' _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-04-18 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 18.497(6) _cell_length_b 18.497(6) _cell_length_c 16.973(4) _cell_measurement_reflns_used 895 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 17.4 _cell_measurement_theta_min 2.19 _cell_volume 5029(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_unetI/netI 0.0535 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8880 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.449 _diffrn_reflns_theta_max 24.449 _diffrn_reflns_theta_min 2.202 _exptl_absorpt_coefficient_mu 4.674 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_correction_T_min 0.6474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.445 _exptl_crystal_description block _exptl_crystal_F_000 2196 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.796 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.237 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.406 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 930 _refine_ls_number_restraints 47 _refine_ls_restrained_S_all 1.377 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0714 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+716.2777P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1843 _refine_ls_wR_factor_ref 0.1935 _reflns_Friedel_coverage 0.000 _reflns_number_gt 666 _reflns_number_total 930 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc01960j2.cif _cod_data_source_block complex_2 _cod_database_code 1551206 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_res_file ; SLS3149_0m_b.res created by SHELXL-2014/7 TITL SLS3149_01_b.res in R-3c CELL 0.71073 18.4974 18.4974 16.9728 90.000 90.000 120.000 ZERR 6.000 0.0055 0.0055 0.0043 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM Y, X, 1/2-Z SYMM X-Y, -Y, 1/2-Z SYMM -X, -X+Y, 1/2-Z SFAC C N Si Th H UNIT 108 24 36 6 336 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 sadi 0.01 N2 C1 N2 C2 N2 C3 N2_$1 C4 N2_$1 C5 N2_$1 C6 sadi 0.01 Si1 C1 Si1 C2 Si1 C3 Si2 C4 Si2 C5 Si2 C6 sadi 0.01 C1 C2 C1 C3 C2 C3 C4 C5 C4 C6 C5 C6 sadi 0.01 Th1 Si1 Th1 Si2 sadi 0.01 N2_$1 Si2 N2 Si1 eqiv $1 x-y+1/3, x-1/3, -z+2/3 eadp C4 C5 C6 eadp C1 C2 FREE C2 C5 FREE Si1 Si2 FREE C3 C6 FREE Si2 C3 FREE C4 C3 FREE N2 C6 TEMP -173.020 WGHT 0.000100 716.277710 FVAR 0.13918 MOLE 1 SI1 3 0.576663 0.140439 0.432391 10.50000 0.02559 0.01324 = 0.03232 -0.00314 -0.00751 0.01489 SI2 3 0.657154 0.142559 0.368704 10.50000 0.00891 0.01888 = 0.01767 -0.00210 -0.00201 0.00510 PART 1 C1 1 0.494611 0.104897 0.512741 10.50000 0.02443 0.03164 = 0.02109 0.02143 0.00456 0.01195 C2 1 0.681122 0.204624 0.483422 10.50000 0.02443 0.03164 = 0.02109 0.02143 0.00456 0.01195 C3 1 0.574507 0.042695 0.395131 10.50000 0.02924 0.01606 = 0.02448 -0.00647 0.00315 -0.00389 PART 2 C5 1 0.725478 0.157549 0.457611 10.50000 0.02831 0.00647 = 0.04002 0.00126 0.01858 -0.00046 C4 1 0.639536 0.043907 0.318269 10.50000 0.02831 0.00647 = 0.04002 0.00126 0.01858 -0.00046 AFIX 137 H4A 5 0.632752 0.048250 0.261508 10.50000 -1.50000 H4B 5 0.589077 -0.004046 0.339542 10.50000 -1.50000 H4C 5 0.687646 0.036380 0.327614 10.50000 -1.50000 AFIX 0 C6 1 0.552012 0.119158 0.409216 10.50000 0.02831 0.00647 = 0.04002 0.00126 0.01858 -0.00046 PART 0 TH1 4 0.666667 0.333333 0.333333 10.16670 0.01351 0.01351 = 0.02633 0.00000 0.00000 0.00676 N1 2 0.666667 0.333333 0.465080 10.16670 0.02934 0.02934 = 0.05630 0.00000 0.00000 0.01467 N2 2 0.561023 0.194449 0.359090 10.50000 0.00755 0.01325 = 0.02451 0.00086 0.00427 0.00062 HKLF 4 REM SLS3149_01_b.res in R-3c REM R1 = 0.0714 for 666 Fo > 4sig(Fo) and 0.1010 for all 930 data REM 70 parameters refined using 47 restraints END WGHT 0.0000 715.7992 REM Highest difference peak 0.796, deepest hole -1.627, 1-sigma level 0.237 Q1 1 0.6792 0.2480 0.4711 11.00000 0.05 0.80 Q2 1 0.7164 -0.0473 0.2965 11.00000 0.05 0.68 Q3 1 0.6499 0.1920 0.4236 11.00000 0.05 0.66 Q4 1 0.5975 0.2069 0.3716 11.00000 0.05 0.65 Q5 1 0.6249 0.1447 0.3828 11.00000 0.05 0.64 Q6 1 0.7033 0.0164 0.3863 11.00000 0.05 0.64 Q7 1 0.4624 0.0814 0.4612 11.00000 0.05 0.63 Q8 1 0.6396 0.1119 0.3416 11.00000 0.05 0.62 Q9 1 0.6567 0.0649 0.3372 11.00000 0.05 0.62 Q10 1 0.6550 -0.0391 0.3363 11.00000 0.05 0.62 Q11 1 0.5449 0.0187 0.3799 11.00000 0.05 0.62 Q12 1 0.5597 0.1388 0.3814 11.00000 0.05 0.60 Q13 1 0.4367 0.0501 0.5185 11.00000 0.05 0.59 Q14 1 0.7542 0.2393 0.4951 11.00000 0.05 0.59 Q15 1 0.7295 0.1927 0.4834 11.00000 0.05 0.57 Q16 1 0.6134 0.0210 0.3867 11.00000 0.05 0.57 Q17 1 0.6536 0.2581 0.5398 11.00000 0.05 0.55 Q18 1 0.6468 0.0787 0.3777 11.00000 0.05 0.55 Q19 1 0.6038 0.0099 0.4656 11.00000 0.05 0.55 Q20 1 0.5350 0.0935 0.4928 11.00000 0.05 0.54 ; _shelx_res_checksum 73350 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' 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 Si1 Si 0.5767(7) 0.1404(5) 0.4324(6) 0.021(2) Uani 0.5 1 d D . P . . Si2 Si 0.6572(5) 0.1426(5) 0.3687(5) 0.016(2) Uani 0.5 1 d D . P . . C1 C 0.4946(15) 0.1049(16) 0.5127(12) 0.027(6) Uani 0.5 1 d D . P A 1 C2 C 0.6811(14) 0.2046(16) 0.4834(14) 0.027(6) Uani 0.5 1 d D . P A 1 C3 C 0.5745(17) 0.0427(13) 0.3951(16) 0.030(10) Uani 0.5 1 d D . P A 1 C5 C 0.7255(15) 0.1575(16) 0.4576(13) 0.029(6) Uani 0.5 1 d D . P A 2 C4 C 0.6395(16) 0.0439(12) 0.3183(16) 0.029(6) Uani 0.5 1 d D . P A 2 H4A H 0.6328 0.0483 0.2615 0.044 Uiso 0.5 1 calc R U P A 2 H4B H 0.5891 -0.0040 0.3395 0.044 Uiso 0.5 1 calc R U P A 2 H4C H 0.6876 0.0364 0.3276 0.044 Uiso 0.5 1 calc R U P A 2 C6 C 0.5520(13) 0.1192(17) 0.4092(16) 0.029(6) Uani 0.5 1 d D . P A 2 Th1 Th 0.6667 0.3333 0.3333 0.0178(5) Uani 1 6 d DS T P A . N1 N 0.6667 0.3333 0.465(3) 0.038(13) Uani 0.5001 3 d S T P . . N2 N 0.5610(10) 0.1944(12) 0.3591(7) 0.017(6) Uani 0.5 1 d D . P A . 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 Si1 0.026(7) 0.013(5) 0.032(5) -0.003(4) -0.008(6) 0.015(6) Si2 0.009(5) 0.019(5) 0.018(4) -0.002(4) -0.002(4) 0.005(4) C1 0.024(14) 0.032(16) 0.021(14) 0.021(12) 0.005(12) 0.012(13) C2 0.024(14) 0.032(16) 0.021(14) 0.021(12) 0.005(12) 0.012(13) C3 0.03(2) 0.02(2) 0.02(2) -0.006(16) 0.003(18) -0.004(18) C5 0.028(14) 0.006(10) 0.040(15) 0.001(10) 0.019(12) 0.000(10) C4 0.028(14) 0.006(10) 0.040(15) 0.001(10) 0.019(12) 0.000(10) C6 0.028(14) 0.006(10) 0.040(15) 0.001(10) 0.019(12) 0.000(10) Th1 0.0135(5) 0.0135(5) 0.0263(8) 0.000 0.000 0.0068(3) N1 0.029(17) 0.029(17) 0.06(3) 0.000 0.000 0.015(9) N2 0.008(14) 0.013(15) 0.025(17) 0.001(13) 0.004(12) 0.001(12) 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' 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' Th Th -7.2400 8.8979 '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' 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 C6 Si1 N2 66(4) . . N2 Si1 C1 112.7(7) . . N2 Si1 C3 112.7(7) . . C1 Si1 C3 106.1(7) . . N2 Si1 C2 112.6(7) . . C1 Si1 C2 106.1(7) . . C3 Si1 C2 106.1(7) . . C6 Si1 Th1 100(3) . . N2 Si1 Th1 36.1(5) . . C1 Si1 Th1 125.9(8) . . C3 Si1 Th1 125.5(8) . . C2 Si1 Th1 76.5(8) . . N2 Si2 C4 113.0(7) 33_545 . N2 Si2 C6 112.2(7) 33_545 . C4 Si2 C6 106.4(7) . . N2 Si2 C5 112.3(7) 33_545 . C4 Si2 C5 106.4(7) . . C6 Si2 C5 106.1(7) . . N2 Si2 C2 100.2(8) 33_545 . N2 Si2 Th1 37.0(6) 33_545 . C4 Si2 Th1 142.6(8) . . C6 Si2 Th1 79.7(9) . . C5 Si2 Th1 107.2(8) . . C2 Si2 Th1 74.3(7) . . Si1 C2 Si2 52.4(6) . . Si2 C4 H4A 109.5 . . Si2 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . Si2 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . Si1 C6 Si2 74(2) . . N1 Th1 N1 180.0 . 31_655 N1 Th1 N2 100.7(3) . 32 N1 Th1 N2 79.3(3) 31_655 32 N1 Th1 N2 100.7(3) . 31_655 N1 Th1 N2 79.3(3) 31_655 31_655 N2 Th1 N2 116.66(19) 32 31_655 N1 Th1 N2 79.3(3) . 2_655 N1 Th1 N2 100.7(3) 31_655 2_655 N2 Th1 N2 180.0 32 2_655 N2 Th1 N2 63.34(19) 31_655 2_655 N1 Th1 N2 79.3(3) . 3_665 N1 Th1 N2 100.7(3) 31_655 3_665 N2 Th1 N2 63.34(19) 32 3_665 N2 Th1 N2 63.34(19) 31_655 3_665 N2 Th1 N2 116.66(19) 2_655 3_665 N1 Th1 N2 100.7(3) . 33_545 N1 Th1 N2 79.3(3) 31_655 33_545 N2 Th1 N2 116.66(19) 32 33_545 N2 Th1 N2 116.66(19) 31_655 33_545 N2 Th1 N2 63.34(19) 2_655 33_545 N2 Th1 N2 180.0 3_665 33_545 N1 Th1 N2 79.3(3) . . N1 Th1 N2 100.7(3) 31_655 . N2 Th1 N2 63.34(19) 32 . N2 Th1 N2 180.0 31_655 . N2 Th1 N2 116.66(19) 2_655 . N2 Th1 N2 116.66(19) 3_665 . N2 Th1 N2 63.34(19) 33_545 . N1 Th1 Si2 99.89(15) . 31_655 N1 Th1 Si2 80.12(15) 31_655 31_655 N2 Th1 Si2 74.4(4) 32 31_655 N2 Th1 Si2 43.5(4) 31_655 31_655 N2 Th1 Si2 105.6(4) 2_655 31_655 N2 Th1 Si2 25.86(19) 3_665 31_655 N2 Th1 Si2 154.14(19) 33_545 31_655 N2 Th1 Si2 136.5(4) . 31_655 N1 Th1 Si2 80.11(15) . . N1 Th1 Si2 99.88(15) 31_655 . N2 Th1 Si2 105.6(4) 32 . N2 Th1 Si2 136.5(4) 31_655 . N2 Th1 Si2 74.4(4) 2_655 . N2 Th1 Si2 154.14(19) 3_665 . N2 Th1 Si2 25.86(19) 33_545 . N2 Th1 Si2 43.5(4) . . Si2 Th1 Si2 180.0 31_655 . N1 Th1 Si2 80.11(15) . 2_655 N1 Th1 Si2 99.89(15) 31_655 2_655 N2 Th1 Si2 136.5(4) 32 2_655 N2 Th1 Si2 25.86(19) 31_655 2_655 N2 Th1 Si2 43.5(4) 2_655 2_655 N2 Th1 Si2 74.4(4) 3_665 2_655 N2 Th1 Si2 105.6(4) 33_545 2_655 N2 Th1 Si2 154.14(19) . 2_655 Si2 Th1 Si2 62.88(9) 31_655 2_655 Si2 Th1 Si2 117.11(9) . 2_655 N1 Th1 Si2 99.89(15) . 32 N1 Th1 Si2 80.11(15) 31_655 32 N2 Th1 Si2 43.5(4) 32 32 N2 Th1 Si2 154.14(19) 31_655 32 N2 Th1 Si2 136.5(4) 2_655 32 N2 Th1 Si2 105.6(4) 3_665 32 N2 Th1 Si2 74.4(4) 33_545 32 N2 Th1 Si2 25.86(19) . 32 Si2 Th1 Si2 117.12(9) 31_655 32 Si2 Th1 Si2 62.89(9) . 32 Si2 Th1 Si2 180.0 2_655 32 Si1 N2 Si2 124.0(11) . 32 Si1 N2 Th1 118.7(6) . . Si2 N2 Th1 117.2(6) 32 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 C6 0.58(3) . Si1 N2 1.708(12) . Si1 C1 1.897(18) . Si1 C3 1.897(17) . Si1 C2 1.897(18) . Si1 Th1 3.520(8) . Si2 N2 1.714(12) 33_545 Si2 C4 1.891(17) . Si2 C6 1.898(18) . Si2 C5 1.898(18) . Si2 C2 2.19(3) . Si2 Th1 3.496(8) . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . Th1 N1 2.24(6) . Th1 N1 2.24(6) 31_655 Th1 N2 2.364(19) 32 Th1 N2 2.364(19) 31_655 Th1 N2 2.364(19) 2_655 Th1 N2 2.364(19) 3_665 Th1 N2 2.364(19) 33_545 Th1 N2 2.364(19) . Th1 Si2 3.496(8) 31_655 Th1 Si2 3.496(8) 2_655 Th1 Si2 3.496(8) 32 N2 Si2 1.714(12) 32