#------------------------------------------------------------------------------ #$Date: 2019-12-06 11:36:51 +0200 (Fri, 06 Dec 2019) $ #$Revision: 244930 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556433.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_1556433 loop_ _publ_author_name 'Yang, X.' 'Lunsford, A.' 'Darensbourg, M.Y.' _publ_section_title ; Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via the N2S2 Metallo-Ligand Strategy ; _journal_name_full Inorganics _journal_page_first 115 _journal_paper_doi 10.3390/inorganics7090115 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C10 H21 Al N2 S2' _chemical_formula_sum 'C10 H21 Al N2 S2' _chemical_formula_weight 260.39 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 94.767(7) _cell_angle_beta 98.204(7) _cell_angle_gamma 115.566(6) _cell_formula_units_Z 2 _cell_length_a 7.354(4) _cell_length_b 7.723(4) _cell_length_c 12.601(6) _cell_measurement_reflns_used 6296 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 50.99 _cell_measurement_theta_min 3.31 _cell_volume 630.5(6) _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker CMOS area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_unetI/netI 0.1270 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6296 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.495 _diffrn_reflns_theta_min 1.655 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.371 _exptl_crystal_description needle _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _exptl_transmission_factor_max 10 _exptl_transmission_factor_min -18 _refine_diff_density_max 0.633 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.104 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2333 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.250 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0733 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1248 _refine_ls_wR_factor_ref 0.1386 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1437 _reflns_number_total 2333 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file AlMeN2S2.cif _cod_data_source_block mo_AlMe_0m _cod_original_cell_volume 630.6(5) _cod_database_code 1556433 _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_estimated_absorpt_t_min 0.977 _shelx_estimated_absorpt_t_max 0.991 _shelx_res_file ; mo_AlMe_0m.res created by SHELXL-2014/7 TITL mo_AlMe_0m in P-1 CELL 0.71073 7.3543 7.7230 12.6006 94.767 98.204 115.566 ZERR 2.00 0.0035 0.0036 0.0060 0.007 0.007 0.006 LATT 1 SFAC C H N Al S UNIT 20 42 4 2 4 OMIT 3 -2 4 OMIT 1 0 0 OMIT -2 2 1 OMIT 0 -1 1 OMIT 1 2 5 OMIT -1 1 3 OMIT -1 1 1 OMIT -3 51 L.S. 4 ACTA BOND $H FMAP 2 PLAN 20 HTAB CONF SIZE 0.05 0.02 0.02 TEMP -173.000 WGHT 0.000000 EXTI 0.000548 FVAR 0.32335 S1 5 0.371700 -0.062499 0.796459 11.00000 0.02546 0.03618 = 0.05090 0.01524 0.00272 0.01898 S2 5 0.469855 0.266648 0.619924 11.00000 0.02398 0.04655 = 0.02956 0.01488 0.00129 0.02247 AL1 4 0.647866 0.206498 0.765829 11.00000 0.02119 0.02706 = 0.02237 0.00578 0.00136 0.01800 C4 1 1.081253 0.366793 0.768143 11.00000 0.02133 0.04209 = 0.02540 0.00111 0.00072 0.01602 AFIX 23 H4A 2 1.119915 0.497103 0.808620 11.00000 -1.20000 H4B 2 1.196361 0.374392 0.733315 11.00000 -1.20000 AFIX 0 C2 1 0.912168 -0.007260 0.641141 11.00000 0.04942 0.04630 = 0.03769 0.01492 0.01362 0.03845 AFIX 43 H2 2 1.001811 -0.052205 0.615160 11.00000 -1.20000 AFIX 0 C3 1 0.872656 0.149073 0.598101 11.00000 0.03298 0.03431 = 0.02617 0.00441 0.00380 0.01918 AFIX 23 H3A 2 0.732203 0.090142 0.553070 11.00000 -1.20000 H3B 2 0.970727 0.209207 0.550297 11.00000 -1.20000 AFIX 0 C1 1 0.799590 -0.087362 0.728268 11.00000 0.03598 0.03297 = 0.04452 -0.00536 -0.00893 0.02252 AFIX 23 H1A 2 0.651895 -0.166633 0.695703 11.00000 -1.20000 H1B 2 0.851146 -0.174482 0.760210 11.00000 -1.20000 AFIX 0 N2 3 0.891895 0.304643 0.684007 11.00000 0.02079 0.02310 = 0.01815 0.00315 -0.00288 0.01309 C10 1 0.740655 0.420513 0.888317 11.00000 0.02729 0.03816 = 0.03165 0.00856 0.00318 0.02485 AFIX 137 H10A 2 0.795126 0.384812 0.954014 11.00000 -1.50000 H10B 2 0.624342 0.444777 0.900340 11.00000 -1.50000 H10C 2 0.848652 0.538405 0.871525 11.00000 -1.50000 AFIX 0 C7 1 0.514739 -0.164293 0.878612 11.00000 0.03591 0.04044 = 0.04116 0.01705 0.00949 0.02385 AFIX 23 H7A 2 0.458854 -0.194064 0.945433 11.00000 -1.20000 H7B 2 0.495566 -0.287722 0.837299 11.00000 -1.20000 AFIX 0 C8 1 0.889457 0.472213 0.634484 11.00000 0.02733 0.03624 = 0.03635 0.01511 0.00522 0.02245 AFIX 23 H8A 2 1.002527 0.522837 0.593883 11.00000 -1.20000 H8B 2 0.910932 0.577943 0.692341 11.00000 -1.20000 AFIX 0 C9 1 0.683474 0.407627 0.557586 11.00000 0.03397 0.03962 = 0.03476 0.01750 0.00269 0.02760 AFIX 23 H9A 2 0.678454 0.328198 0.490373 11.00000 -1.20000 H9B 2 0.670822 0.523647 0.537299 11.00000 -1.20000 AFIX 0 C6 1 0.741352 -0.026966 0.909600 11.00000 0.04113 0.04189 = 0.04812 0.01295 0.00443 0.03005 AFIX 23 H6A 2 0.764959 0.076688 0.969333 11.00000 -1.20000 H6B 2 0.817522 -0.098865 0.936176 11.00000 -1.20000 AFIX 0 C5 1 1.038013 0.213972 0.848301 11.00000 0.03690 0.05057 = 0.02743 -0.00786 -0.01264 0.03552 AFIX 23 H5A 2 1.131663 0.153005 0.846053 11.00000 -1.20000 H5B 2 1.062839 0.279657 0.923535 11.00000 -1.20000 AFIX 0 N1 3 0.820773 0.062726 0.815258 11.00000 0.02685 0.02820 = 0.03236 0.01263 0.00917 0.01795 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_AlMe_0m in P-1 REM R1 = 0.0733 for 1437 Fo > 4sig(Fo) and 0.1185 for all 2333 data REM 138 parameters refined using 0 restraints END WGHT 0.0644 0.4491 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C4 S2_$1 HTAB C3 S2 EQIV $2 -x+1, -y, -z+1 HTAB C3 S2_$2 HTAB C1 S1 EQIV $3 -x+1, -y+1, -z+1 HTAB C9 S2_$3 HTAB C5 S1_$1 REM Highest difference peak 0.633, deepest hole -0.437, 1-sigma level 0.104 Q1 1 1.0773 0.0541 0.6784 11.00000 0.05 0.63 Q2 1 1.1911 0.3124 0.8208 11.00000 0.05 0.62 Q3 1 0.8378 -0.1343 0.5791 11.00000 0.05 0.55 Q4 1 0.5080 0.4037 0.6615 11.00000 0.05 0.55 Q5 1 0.6645 -0.1647 0.8013 11.00000 0.05 0.55 Q6 1 0.6998 0.3328 0.8155 11.00000 0.05 0.54 Q7 1 0.4198 -0.0246 0.7208 11.00000 0.05 0.47 Q8 1 0.7985 -0.0325 0.6615 11.00000 0.05 0.43 Q9 1 0.3831 -0.2007 0.7607 11.00000 0.05 0.39 Q10 1 0.9474 0.0684 0.8429 11.00000 0.05 0.39 Q11 1 0.4483 0.4594 0.8613 11.00000 0.05 0.35 Q12 1 0.5948 0.0583 0.7209 11.00000 0.05 0.33 Q13 1 0.4555 0.0965 0.8282 11.00000 0.05 0.33 Q14 1 1.1688 0.0352 0.7367 11.00000 0.05 0.33 Q15 1 0.6030 0.3679 0.6006 11.00000 0.05 0.32 Q16 1 0.8544 -0.1711 0.8416 11.00000 0.05 0.30 Q17 1 0.5288 0.2965 0.5568 11.00000 0.05 0.30 Q18 1 0.7617 0.3592 0.4785 11.00000 0.05 0.30 Q19 1 0.5603 -0.1289 0.9373 11.00000 0.05 0.29 Q20 1 0.7612 -0.2496 0.7786 11.00000 0.05 0.29 ; _shelx_res_checksum 66174 _shelx_hkl_file ; -1 0 0 12.01 1.58 -1 0 0 15.29 1.75 -1 0 0 11.84 1.43 -1 0 0 15.27 1.48 -2 0 0 5.94 1.53 -2 0 0 5.09 1.49 -2 0 0 5.91 1.35 -3 0 0 3.76 1.67 -3 0 0 6.12 1.84 -3 0 0 6.43 1.62 3 0 0 2.34 1.23 -4 0 0 39.29 5.56 -4 0 0 44.60 4.89 -4 0 0 35.77 5.27 4 0 0 42.71 4.83 -5 0 0 12.66 3.56 -5 0 0 13.40 2.94 -5 0 0 10.87 3.20 5 0 0 16.51 3.24 -6 0 0 8.28 3.17 6 0 0 10.47 3.62 -7 0 0 49.94 8.45 7 0 0 41.71 7.44 -8 0 0 15.77 5.30 8 0 0 11.93 5.32 8 -1 0 2.91 3.59 -8 1 0 1.22 3.26 7 -1 0 3.27 2.67 -7 1 0 0.81 2.41 -7 1 0 0.67 2.50 6 -1 0 2.54 2.10 -6 1 0 8.06 3.27 -6 1 0 0.00 2.19 5 -1 0 281.37 18.01 -5 1 0 287.36 17.68 -5 1 0 276.18 18.21 -5 1 0 296.75 18.86 -4 1 0 100.58 7.70 -4 1 0 99.48 7.22 -4 1 0 100.78 7.87 -4 1 0 100.71 7.55 -3 1 0 2.20 1.18 -3 1 0 6.16 1.58 -3 1 0 0.02 0.91 -3 1 0 2.12 1.13 -2 1 0 8.03 1.74 -2 1 0 8.78 1.45 -2 1 0 9.52 1.71 -2 1 0 7.28 1.54 1 -1 0 266.53 14.79 -1 1 0 262.55 14.77 0 -1 0 183.98 10.14 0 -1 0 169.76 10.11 0 1 0 179.87 9.88 -1 -1 0 23.32 2.45 -2 -1 0 53.66 3.88 -2 -1 0 40.65 5.00 2 1 0 51.55 3.68 2 1 0 50.33 4.39 -3 -1 0 1.47 1.14 -3 -1 0 0.31 1.24 3 1 0 -0.06 0.73 3 1 0 0.56 1.42 -4 -1 0 2.32 1.79 -4 -1 0 4.98 1.86 4 1 0 0.27 1.03 4 1 0 3.20 2.09 -5 -1 0 8.48 3.26 5 1 0 16.55 3.90 -6 -1 0 30.39 6.30 6 1 0 20.00 5.09 -7 -1 0 27.40 6.41 7 1 0 24.05 5.99 8 -2 0 2.32 2.76 -8 2 0 3.91 3.13 7 -2 0 0.88 2.14 -7 2 0 5.37 3.12 -7 2 0 1.79 2.47 -6 2 0 84.50 9.66 -6 2 0 84.46 9.14 -6 2 0 83.12 9.33 -5 2 0 89.28 7.86 -5 2 0 90.75 8.00 -5 2 0 94.44 7.44 4 -2 0 10.35 2.43 -4 2 0 18.68 3.46 -4 2 0 14.01 2.97 3 -2 0 23.97 3.39 -3 2 0 23.66 3.64 -3 2 0 25.72 2.85 2 -2 0 120.16 6.84 2 -2 0 116.46 7.69 -2 2 0 117.45 7.66 1 -2 0 65.93 4.37 1 -2 0 72.57 5.02 -1 2 0 70.96 4.92 -1 2 0 71.36 4.82 0 -2 0 0.51 0.94 0 -2 0 1.32 0.94 0 2 0 1.16 0.73 0 2 0 -0.97 0.78 -1 -2 0 82.43 6.28 -1 -2 0 86.50 5.75 1 2 0 76.27 5.12 -2 -2 0 177.47 11.20 -2 -2 0 176.90 12.28 2 2 0 182.07 10.71 -3 -2 0 47.32 6.11 -3 -2 0 44.29 4.88 3 2 0 42.64 4.36 3 2 0 45.64 5.86 -4 -2 0 7.50 2.70 -4 -2 0 5.57 3.41 4 2 0 5.76 2.62 -5 -2 0 2.05 2.49 5 2 0 -0.59 2.14 -6 -2 0 2.47 2.87 6 2 0 0.97 2.85 -7 -2 0 -0.75 3.12 7 2 0 2.81 3.80 9 -3 0 8.74 4.13 -9 3 0 26.35 6.70 8 -3 0 3.71 2.92 -8 3 0 3.73 3.63 7 -3 0 7.52 2.85 -7 3 0 2.98 2.35 -7 3 0 8.06 3.30 6 -3 0 6.20 2.57 -6 3 0 4.83 2.50 -6 3 0 7.37 3.07 5 -3 0 9.08 2.69 -5 3 0 17.37 2.96 -5 3 0 13.65 3.14 4 -3 0 30.44 4.41 4 -3 0 41.99 4.00 -4 3 0 32.05 4.98 -4 3 0 38.53 4.94 3 -3 0 24.91 3.57 3 -3 0 26.92 2.13 -3 3 0 22.19 3.61 2 -3 0 37.10 2.76 -2 3 0 40.76 4.49 1 -3 0 22.66 2.79 1 -3 0 20.00 3.36 -1 3 0 20.51 2.81 0 -3 0 -0.48 0.96 0 -3 0 0.25 0.92 0 3 0 -0.16 0.95 0 3 0 0.58 0.89 -1 -3 0 29.85 4.42 -1 -3 0 25.09 3.59 1 3 0 32.18 3.31 1 3 0 27.70 4.20 -2 -3 0 11.45 2.51 -2 -3 0 13.21 3.49 2 3 0 18.76 3.58 2 3 0 13.26 2.14 -3 -3 0 1.36 1.44 -3 -3 0 -0.41 1.43 3 3 0 0.12 1.11 -4 -3 0 3.39 2.49 4 3 0 1.91 2.07 -5 -3 0 0.35 2.16 5 3 0 -1.63 2.12 -6 -3 0 2.62 3.12 6 3 0 6.31 3.55 9 -4 0 3.50 3.33 -8 4 0 4.83 3.43 -8 4 0 3.95 3.46 7 -4 0 -0.08 1.95 -7 4 0 1.10 2.33 -7 4 0 0.96 2.34 6 -4 0 12.94 3.47 -6 4 0 6.50 2.85 -6 4 0 9.11 3.33 5 -4 0 -0.60 1.38 -5 4 0 0.25 1.46 -5 4 0 -0.92 1.63 4 -4 0 9.34 1.68 4 -4 0 13.31 3.24 -4 4 0 14.03 3.29 -4 4 0 8.58 2.60 3 -4 0 22.81 4.06 3 -4 0 21.73 2.18 -3 4 0 18.35 3.49 -3 4 0 16.13 3.28 2 -4 0 33.49 4.44 2 -4 0 20.53 2.75 -2 4 0 29.52 4.15 -2 4 0 30.30 4.24 1 -4 0 1.75 1.48 1 -4 0 3.21 1.35 -1 4 0 1.60 1.51 -1 4 0 5.05 1.70 0 -4 0 26.30 4.00 0 -4 0 23.15 3.85 0 4 0 24.27 3.13 0 4 0 21.86 3.81 -1 -4 0 18.57 3.35 -1 -4 0 15.99 3.56 1 4 0 25.13 4.31 1 4 0 13.72 2.37 -2 -4 0 22.26 4.57 -2 -4 0 17.55 3.47 2 4 0 14.77 3.67 -3 -4 0 2.82 2.33 3 4 0 3.80 2.54 -4 -4 0 0.04 2.46 4 4 0 0.43 2.09 -5 -4 0 6.91 3.55 5 4 0 1.49 2.65 -9 5 0 2.73 3.38 8 -5 0 1.22 2.63 -8 5 0 2.05 3.39 -8 5 0 3.96 3.39 7 -5 0 4.26 2.92 -7 5 0 2.86 2.89 -7 5 0 3.20 2.40 6 -5 0 26.11 5.24 -6 5 0 33.87 5.96 -6 5 0 39.71 6.52 5 -5 0 37.14 5.94 -5 5 0 34.86 5.62 4 -5 0 6.21 2.63 -4 5 0 4.44 2.21 -4 5 0 8.51 2.83 3 -5 0 51.30 6.79 -3 5 0 52.99 6.49 -3 5 0 59.92 6.95 2 -5 0 0.99 1.46 2 -5 0 0.10 0.97 -2 5 0 3.37 1.93 -2 5 0 -0.30 1.31 1 -5 0 23.38 4.21 1 -5 0 16.54 3.32 -1 5 0 20.27 3.52 -1 5 0 17.33 3.83 0 -5 0 3.43 1.81 0 -5 0 2.14 1.83 0 5 0 4.40 1.78 0 5 0 2.28 2.23 -1 -5 0 5.11 2.17 -1 -5 0 8.63 3.21 1 5 0 3.81 2.61 -2 -5 0 16.57 4.41 -2 -5 0 16.87 3.77 2 5 0 15.44 4.03 -3 -5 0 17.99 4.53 3 5 0 23.32 5.34 -4 -5 0 0.37 2.96 4 5 0 4.81 3.47 -9 6 0 1.98 3.67 8 -6 0 11.33 4.47 -8 6 0 11.29 4.51 7 -6 0 9.30 3.99 -7 6 0 10.63 3.87 -7 6 0 10.25 4.28 6 -6 0 38.68 6.71 -6 6 0 37.74 6.90 -6 6 0 40.36 6.62 5 -6 0 6.17 2.87 -5 6 0 2.97 2.37 -5 6 0 8.69 3.39 4 -6 0 1.80 1.60 -4 6 0 0.07 1.89 -4 6 0 0.34 1.72 3 -6 0 2.13 2.08 -3 6 0 5.63 2.68 -3 6 0 1.48 1.78 2 -6 0 116.21 9.40 -2 6 0 96.89 8.38 -2 6 0 95.47 8.71 1 -6 0 0.61 1.57 1 -6 0 3.46 2.22 -1 6 0 4.76 2.63 -1 6 0 2.87 1.90 0 -6 0 18.07 4.20 0 -6 0 8.08 3.08 0 6 0 9.27 3.20 -1 -6 0 32.25 5.82 -1 -6 0 33.21 5.47 1 6 0 27.13 5.81 -2 -6 0 41.21 6.93 2 6 0 29.27 6.31 -3 -6 0 -1.72 2.06 3 6 0 1.63 2.72 8 -7 0 10.53 4.63 -8 7 0 8.56 4.79 7 -7 0 10.15 3.89 -7 7 0 17.85 5.27 6 -7 0 5.84 3.54 -6 7 0 6.98 3.44 -6 7 0 10.97 4.51 5 -7 0 26.98 6.29 -5 7 0 28.26 5.52 -5 7 0 30.66 6.47 4 -7 0 52.55 7.90 -4 7 0 53.58 7.47 -4 7 0 63.30 8.34 3 -7 0 87.97 11.00 -3 7 0 119.03 9.88 -3 7 0 106.91 11.34 2 -7 0 6.04 2.84 -2 7 0 8.57 3.17 -2 7 0 7.46 3.37 1 -7 0 1.35 2.07 -1 7 0 1.57 2.48 0 -7 0 6.73 2.98 0 -7 0 3.36 2.75 0 7 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4.38 4.50 3 -5 13 8.95 4.25 3 4 -13 8.68 4.30 -3 -4 13 5.19 4.47 2 4 -13 6.27 3.39 -2 -4 13 5.23 3.71 1 4 -13 22.10 5.24 -1 -4 13 16.98 5.14 0 4 -13 4.75 3.67 0 -4 13 2.64 2.51 -1 4 -13 7.53 4.03 1 -4 13 3.04 3.16 -2 4 -13 2.52 3.96 2 -4 13 0.67 2.83 -3 4 -13 -0.17 3.71 3 -4 13 0.10 3.28 -4 4 -13 10.20 5.37 4 -4 13 13.70 5.17 4 3 -13 3.44 3.16 -4 -3 13 -1.61 3.17 3 3 -13 -0.80 2.32 -3 -3 13 2.04 3.12 2 3 -13 1.69 2.27 -2 -3 13 1.59 2.66 1 3 -13 0.10 1.93 -1 -3 13 1.91 2.61 0 3 -13 10.32 3.38 0 -3 13 4.27 2.77 -1 3 -13 11.19 4.60 1 -3 13 10.25 3.70 -2 3 -13 3.29 3.29 2 -3 13 0.36 3.35 -3 3 -13 3.77 4.36 3 -3 13 4.04 4.14 -4 3 -13 37.39 8.42 4 -3 13 20.22 6.33 5 2 -13 2.56 3.16 -5 -2 13 1.17 3.43 4 2 -13 4.67 3.63 -4 -2 13 8.40 4.68 3 2 -13 9.50 4.09 -3 -2 13 4.01 3.38 2 2 -13 8.63 3.71 -2 -2 13 7.40 3.62 1 2 -13 19.96 5.13 -1 -2 13 14.80 4.52 0 2 -13 92.41 11.03 0 -2 13 97.43 11.30 -1 2 -13 17.79 4.59 1 -2 13 11.25 4.49 -2 2 -13 -1.63 1.94 -2 2 -13 3.15 3.40 2 -2 13 3.35 3.41 -3 2 -13 3.11 3.52 3 -2 13 -2.07 2.85 -4 2 -13 13.19 5.72 4 -2 13 1.88 4.01 5 1 -13 31.81 6.92 -5 -1 13 21.51 6.31 4 1 -13 24.57 5.82 -4 -1 13 27.75 6.76 3 1 -13 0.29 2.08 -3 -1 13 -0.81 2.12 2 1 -13 8.06 3.41 -2 -1 13 1.20 2.31 1 1 -13 4.61 3.02 -1 -1 13 5.26 3.09 -1 -1 13 6.85 3.09 0 1 -13 6.05 2.74 0 -1 13 8.20 3.66 -1 1 -13 9.84 3.68 1 -1 13 4.54 3.60 -2 1 -13 1.32 2.89 2 -1 13 1.97 3.19 -3 1 -13 3.91 3.63 -3 1 -13 -2.48 3.54 3 -1 13 1.88 3.61 6 0 -13 2.06 3.23 -6 0 13 0.78 3.09 5 0 -13 6.48 3.35 -5 0 13 12.91 5.19 4 0 -13 0.05 1.82 -4 0 13 2.64 2.84 3 0 -13 2.19 2.11 -3 0 13 -0.67 1.99 -3 0 13 1.95 3.67 2 0 -13 1.26 2.17 -2 0 13 0.38 2.29 -2 0 13 1.06 2.22 1 0 -13 -0.80 1.78 -1 0 13 -0.59 2.38 0 0 -13 9.32 3.77 0 0 13 2.82 2.68 -1 0 -13 10.41 4.37 1 0 13 4.52 3.58 -2 0 -13 12.59 4.07 2 0 13 19.73 6.17 -3 0 -13 0.24 3.66 3 0 13 3.61 4.12 6 -1 -13 2.16 2.80 -6 1 13 3.15 3.89 5 -1 -13 4.18 3.37 -5 1 13 7.96 4.50 4 -1 -13 1.96 2.04 -4 1 13 5.76 3.48 -4 1 13 4.26 2.93 3 -1 -13 10.09 4.09 -3 1 13 1.93 2.51 -3 1 13 4.50 3.01 2 -1 -13 -0.56 2.14 -2 1 13 -0.61 2.59 1 -1 -13 4.69 3.33 -1 1 13 7.36 3.39 0 -1 -13 -1.47 1.98 0 1 13 -0.49 2.55 -1 -1 -13 3.31 3.42 1 1 13 -0.34 2.53 -2 -1 -13 6.77 4.28 2 1 13 -2.40 2.72 6 -2 -13 -1.01 2.95 -6 2 13 5.59 4.42 5 -2 -13 2.06 2.94 -5 2 13 0.87 2.42 -5 2 13 -0.87 2.55 4 -2 -13 1.26 2.21 -4 2 13 -1.43 2.09 -4 2 13 4.16 3.16 3 -2 -13 3.15 2.86 -3 2 13 2.56 2.62 -3 2 13 4.02 2.91 2 -2 -13 3.85 3.20 -2 2 13 -1.36 2.38 1 -2 -13 -2.26 1.75 -1 2 13 -2.88 2.51 0 -2 -13 14.89 5.79 0 2 13 8.74 3.97 -1 -2 -13 -1.27 2.64 1 2 13 3.73 3.16 6 -3 -13 2.72 3.15 -6 3 13 -1.08 2.93 -6 3 13 0.09 2.84 5 -3 -13 10.27 4.06 -5 3 13 7.87 3.81 -5 3 13 10.06 4.19 4 -3 -13 12.69 4.73 -4 3 13 6.02 3.52 -4 3 13 6.03 3.40 3 -3 -13 16.41 5.30 -3 3 13 6.34 3.66 2 -3 -13 1.58 2.89 -2 3 13 -1.47 2.30 1 -3 -13 3.05 3.14 -1 3 13 -0.43 3.29 0 -3 -13 2.01 2.82 0 3 13 -2.60 2.75 5 -4 -13 1.95 3.22 -5 4 13 -1.54 2.55 -5 4 13 -0.52 2.54 4 -4 -13 2.94 3.15 -4 4 13 0.90 2.88 3 -4 -13 -1.53 2.57 -3 4 13 -0.70 2.78 2 -4 -13 18.85 5.96 -2 4 13 23.37 5.86 1 -4 -13 0.63 3.35 -1 4 13 -0.43 2.63 0 -5 14 0.11 2.73 -1 5 -14 3.63 3.91 1 -5 14 -0.63 4.98 -2 5 -14 5.43 4.97 2 4 -14 1.82 2.67 -2 -4 14 3.31 3.64 -1 -4 14 9.57 4.24 0 -4 14 0.40 2.42 -2 4 -14 -0.40 3.77 2 -4 14 -2.26 2.69 -3 4 -14 -0.26 4.33 3 -4 14 4.58 4.20 3 3 -14 -3.76 2.22 -3 -3 14 -2.00 2.70 2 3 -14 -0.90 2.52 -2 -3 14 0.05 2.58 1 3 -14 5.56 3.34 -1 -3 14 3.82 3.42 0 3 -14 0.26 2.27 1 -3 14 11.03 4.24 2 -3 14 3.76 3.40 -3 3 -14 4.92 4.65 3 -3 14 3.22 3.36 4 2 -14 3.98 3.51 -4 -2 14 5.24 4.33 3 2 -14 1.80 2.95 -3 -2 14 0.84 2.73 2 2 -14 2.80 3.00 -2 -2 14 -0.49 2.21 1 2 -14 2.95 2.71 -1 -2 14 -4.03 1.79 0 2 -14 6.89 3.38 0 -2 14 2.97 3.13 -1 2 -14 -1.15 2.42 1 -2 14 0.61 2.77 2 -2 14 7.55 4.26 3 -2 14 5.48 4.33 -5 -1 14 1.75 3.95 4 1 -14 -2.82 2.11 -4 -1 14 3.00 3.30 3 1 -14 4.24 3.07 -3 -1 14 -1.44 1.82 2 1 -14 39.39 6.98 -2 -1 14 15.58 4.65 1 1 -14 8.31 3.94 -1 -1 14 11.77 4.31 0 1 -14 31.19 6.61 0 -1 14 25.45 5.72 -1 1 -14 7.43 3.53 1 -1 14 6.09 3.66 -2 1 -14 0.77 2.98 2 -1 14 -0.19 3.08 5 0 -14 6.55 3.87 -5 0 14 2.84 3.80 4 0 -14 3.98 3.20 -4 0 14 2.92 3.43 3 0 -14 1.68 2.39 -3 0 14 3.70 3.16 2 0 -14 10.27 4.11 -2 0 14 7.48 3.42 -2 0 14 3.51 4.37 1 0 -14 10.69 4.37 -1 0 14 12.83 4.33 0 0 -14 8.96 4.29 0 0 14 1.36 2.58 -1 0 -14 2.82 3.73 1 0 14 -0.31 3.20 -2 0 -14 10.68 5.06 2 0 14 12.01 5.25 5 -1 -14 -0.17 2.18 -5 1 14 -1.70 2.50 4 -1 -14 1.33 2.46 -4 1 14 1.83 3.08 3 -1 -14 1.45 2.59 -3 1 14 6.53 3.28 -3 1 14 4.67 3.28 2 -1 -14 0.91 2.58 -2 1 14 -0.55 2.82 1 -1 -14 5.93 3.40 -1 1 14 7.16 3.64 0 -1 -14 27.99 6.64 0 1 14 33.15 7.03 -1 -1 -14 19.73 5.80 1 1 14 13.37 5.29 5 -2 -14 2.49 3.35 -5 2 14 4.42 3.22 4 -2 -14 13.79 4.99 -4 2 14 9.65 4.14 -4 2 14 5.73 3.58 3 -2 -14 10.20 4.11 -3 2 14 7.96 4.03 2 -2 -14 -2.04 2.16 -2 2 14 5.48 3.94 1 -2 -14 6.72 3.74 -1 2 14 4.36 3.55 0 -2 -14 9.55 4.41 0 2 14 8.70 4.11 5 -3 -14 4.01 3.80 -5 3 14 8.03 3.92 -5 3 14 5.31 3.50 4 -3 -14 10.34 4.27 -4 3 14 13.34 4.68 3 -3 -14 0.59 3.06 -3 3 14 2.59 3.32 2 -3 -14 -0.28 2.27 -2 3 14 2.56 3.00 1 -3 -14 0.48 2.71 -1 3 14 -2.01 3.02 2 3 -15 36.65 7.58 -2 -3 15 25.99 6.64 -1 -3 15 0.06 2.66 1 -3 15 -2.51 3.44 3 2 -15 -0.74 2.50 -3 -2 15 2.18 3.55 2 2 -15 -0.71 2.35 -2 -2 15 0.79 2.75 1 2 -15 8.12 4.07 0 2 -15 -1.57 2.33 0 -2 15 4.98 3.40 -1 2 -15 1.86 3.14 1 -2 15 4.60 3.66 3 1 -15 2.94 3.08 -3 -1 15 0.63 2.67 2 1 -15 4.07 3.29 -2 -1 15 1.20 3.11 1 1 -15 6.75 3.64 -1 -1 15 2.91 2.96 0 1 -15 29.79 6.48 0 -1 15 12.53 4.72 -1 1 -15 4.18 3.85 1 -1 15 4.03 4.09 4 0 -15 2.29 3.34 -4 0 15 5.25 3.82 3 0 -15 0.90 2.82 -3 0 15 0.90 2.87 2 0 -15 1.82 2.70 -2 0 15 -0.65 2.74 1 0 -15 3.20 3.48 -1 0 15 3.48 3.80 0 0 -15 1.48 2.91 0 0 15 1.94 3.11 -1 0 -15 4.28 3.70 1 0 15 0.31 3.22 4 -1 -15 0.24 3.08 -4 1 15 -0.71 2.78 3 -1 -15 -0.51 2.40 -3 1 15 1.12 2.60 2 -1 -15 -0.24 2.84 -2 1 15 4.03 3.54 1 -1 -15 15.40 5.28 -1 1 15 -0.46 3.58 0 -1 -15 2.69 3.15 0 1 15 2.60 3.40 -4 2 15 0.84 2.87 3 -2 -15 5.83 3.82 -3 2 15 1.68 3.08 2 -2 -15 3.53 3.75 -2 2 15 8.59 4.54 1 -2 -15 6.44 4.29 -1 2 15 6.44 4.51 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 25501 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 S1 S 0.3717(2) -0.0625(2) 0.79646(13) 0.0357(5) Uani 1 1 d . . . . . S2 S 0.4699(2) 0.2666(2) 0.61992(11) 0.0308(4) Uani 1 1 d . . . . . Al1 Al 0.6479(2) 0.2065(2) 0.76583(12) 0.0211(4) Uani 1 1 d . . . . . C4 C 1.0813(8) 0.3668(8) 0.7681(4) 0.0297(14) Uani 1 1 d . . . . . H4A H 1.1199 0.4971 0.8086 0.036 Uiso 1 1 calc R U . . . H4B H 1.1964 0.3744 0.7333 0.036 Uiso 1 1 calc R U . . . C2 C 0.9122(9) -0.0073(8) 0.6411(4) 0.0372(15) Uani 1 1 d . . . . . H2 H 1.0018 -0.0522 0.6152 0.045 Uiso 1 1 calc R U . . . C3 C 0.8727(8) 0.1491(7) 0.5981(4) 0.0299(14) Uani 1 1 d . . . . . H3A H 0.7322 0.0901 0.5531 0.036 Uiso 1 1 calc R U . . . H3B H 0.9707 0.2092 0.5503 0.036 Uiso 1 1 calc R U . . . C1 C 0.7996(8) -0.0874(8) 0.7283(4) 0.0379(15) Uani 1 1 d . . . . . H1A H 0.6519 -0.1666 0.6957 0.045 Uiso 1 1 calc R U . . . H1B H 0.8511 -0.1745 0.7602 0.045 Uiso 1 1 calc R U . . . N2 N 0.8919(6) 0.3046(5) 0.6840(3) 0.0203(10) Uani 1 1 d . . . . . C10 C 0.7407(8) 0.4205(7) 0.8883(4) 0.0288(13) Uani 1 1 d . . . . . H10A H 0.7951 0.3848 0.9540 0.043 Uiso 1 1 calc R U . . . H10B H 0.6243 0.4448 0.9003 0.043 Uiso 1 1 calc R U . . . H10C H 0.8487 0.5384 0.8715 0.043 Uiso 1 1 calc R U . . . C7 C 0.5147(8) -0.1643(8) 0.8786(5) 0.0359(15) Uani 1 1 d . . . . . H7A H 0.4589 -0.1941 0.9454 0.043 Uiso 1 1 calc R U . . . H7B H 0.4956 -0.2877 0.8373 0.043 Uiso 1 1 calc R U . . . C8 C 0.8895(8) 0.4722(7) 0.6345(4) 0.0299(14) Uani 1 1 d . . . . . H8A H 1.0025 0.5228 0.5939 0.036 Uiso 1 1 calc R U . . . H8B H 0.9109 0.5779 0.6923 0.036 Uiso 1 1 calc R U . . . C9 C 0.6835(8) 0.4076(8) 0.5576(4) 0.0318(14) Uani 1 1 d . . . . . H9A H 0.6785 0.3282 0.4904 0.038 Uiso 1 1 calc R U . . . H9B H 0.6708 0.5236 0.5373 0.038 Uiso 1 1 calc R U . . . C6 C 0.7414(9) -0.0270(8) 0.9096(5) 0.0397(16) Uani 1 1 d . . . . . H6A H 0.7650 0.0767 0.9693 0.048 Uiso 1 1 calc R U . . . H6B H 0.8175 -0.0989 0.9362 0.048 Uiso 1 1 calc R U . . . C5 C 1.0380(8) 0.2140(8) 0.8483(4) 0.0355(15) Uani 1 1 d . . . . . H5A H 1.1317 0.1530 0.8461 0.043 Uiso 1 1 calc R U . . . H5B H 1.0628 0.2797 0.9235 0.043 Uiso 1 1 calc R U . . . N1 N 0.8208(6) 0.0627(6) 0.8153(3) 0.0262(11) 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 S1 0.0255(8) 0.0362(9) 0.0509(10) 0.0152(8) 0.0027(7) 0.0190(7) S2 0.0240(8) 0.0465(10) 0.0296(9) 0.0149(7) 0.0013(7) 0.0225(8) Al1 0.0212(9) 0.0271(9) 0.0224(9) 0.0058(7) 0.0014(7) 0.0180(8) C4 0.021(3) 0.042(4) 0.025(3) 0.001(3) 0.001(3) 0.016(3) C2 0.049(4) 0.046(4) 0.038(4) 0.015(3) 0.014(3) 0.038(3) C3 0.033(3) 0.034(3) 0.026(3) 0.004(3) 0.004(3) 0.019(3) C1 0.036(4) 0.033(4) 0.045(4) -0.005(3) -0.009(3) 0.023(3) N2 0.021(2) 0.023(2) 0.018(2) 0.003(2) -0.0029(19) 0.013(2) C10 0.027(3) 0.038(3) 0.032(3) 0.009(3) 0.003(3) 0.025(3) C7 0.036(4) 0.040(4) 0.041(4) 0.017(3) 0.009(3) 0.024(3) C8 0.027(3) 0.036(4) 0.036(3) 0.015(3) 0.005(3) 0.022(3) C9 0.034(3) 0.040(4) 0.035(3) 0.017(3) 0.003(3) 0.028(3) C6 0.041(4) 0.042(4) 0.048(4) 0.013(3) 0.004(3) 0.030(3) C5 0.037(4) 0.051(4) 0.027(3) -0.008(3) -0.013(3) 0.036(3) N1 0.027(3) 0.028(3) 0.032(3) 0.013(2) 0.009(2) 0.018(2) 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C7 S1 Al1 98.15(19) . . C9 S2 Al1 99.04(17) . . C10 Al1 N2 102.2(2) . . C10 Al1 N1 102.2(2) . . N2 Al1 N1 74.85(17) . . C10 Al1 S2 109.41(16) . . N2 Al1 S2 85.21(12) . . N1 Al1 S2 145.51(15) . . C10 Al1 S1 109.84(17) . . N2 Al1 S1 145.26(13) . . N1 Al1 S1 85.40(14) . . S2 Al1 S1 96.23(8) . . N2 C4 C5 108.6(4) . . N2 C4 H4A 110.0 . . C5 C4 H4A 110.0 . . N2 C4 H4B 110.0 . . C5 C4 H4B 110.0 . . H4A C4 H4B 108.3 . . C3 C2 C1 114.2(5) . . C3 C2 H2 122.9 . . C1 C2 H2 122.9 . . C2 C3 N2 114.0(4) . . C2 C3 H3A 108.8 . . N2 C3 H3A 108.8 . . C2 C3 H3B 108.8 . . N2 C3 H3B 108.8 . . H3A C3 H3B 107.7 . . N1 C1 C2 113.5(5) . . N1 C1 H1A 108.9 . . C2 C1 H1A 108.9 . . N1 C1 H1B 108.9 . . C2 C1 H1B 108.9 . . H1A C1 H1B 107.7 . . C3 N2 C4 110.7(4) . . C3 N2 C8 110.2(4) . . C4 N2 C8 111.2(4) . . C3 N2 Al1 111.7(3) . . C4 N2 Al1 105.9(3) . . C8 N2 Al1 106.9(3) . . Al1 C10 H10A 109.5 . . Al1 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . Al1 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C6 C7 S1 112.1(4) . . C6 C7 H7A 109.2 . . S1 C7 H7A 109.2 . . C6 C7 H7B 109.2 . . S1 C7 H7B 109.2 . . H7A C7 H7B 107.9 . . N2 C8 C9 109.8(4) . . N2 C8 H8A 109.7 . . C9 C8 H8A 109.7 . . N2 C8 H8B 109.7 . . C9 C8 H8B 109.7 . . H8A C8 H8B 108.2 . . C8 C9 S2 111.4(4) . . C8 C9 H9A 109.4 . . S2 C9 H9A 109.4 . . C8 C9 H9B 109.4 . . S2 C9 H9B 109.4 . . H9A C9 H9B 108.0 . . N1 C6 C7 111.2(5) . . N1 C6 H6A 109.4 . . C7 C6 H6A 109.4 . . N1 C6 H6B 109.4 . . C7 C6 H6B 109.4 . . H6A C6 H6B 108.0 . . N1 C5 C4 109.0(4) . . N1 C5 H5A 109.9 . . C4 C5 H5A 109.9 . . N1 C5 H5B 109.9 . . C4 C5 H5B 109.9 . . H5A C5 H5B 108.3 . . C1 N1 C5 110.8(4) . . C1 N1 C6 110.4(4) . . C5 N1 C6 111.3(4) . . C1 N1 Al1 111.9(3) . . C5 N1 Al1 106.5(3) . . C6 N1 Al1 105.9(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 S1 C7 1.826(5) . S1 Al1 2.303(2) . S2 C9 1.813(5) . S2 Al1 2.300(2) . Al1 C10 1.970(5) . Al1 N2 2.084(4) . Al1 N1 2.085(4) . C4 N2 1.487(6) . C4 C5 1.575(7) . C4 H4A 0.9900 . C4 H4B 0.9900 . C2 C3 1.484(7) . C2 C1 1.484(7) . C2 H2 0.9500 . C3 N2 1.493(6) . C3 H3A 0.9900 . C3 H3B 0.9900 . C1 N1 1.468(6) . C1 H1A 0.9900 . C1 H1B 0.9900 . N2 C8 1.488(6) . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C7 C6 1.508(7) . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 C9 1.527(6) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 H9A 0.9900 . C9 H9B 0.9900 . C6 N1 1.490(6) . C6 H6A 0.9900 . C6 H6B 0.9900 . C5 N1 1.486(6) . C5 H5A 0.9900 . C5 H5B 0.9900 . 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 C1 C2 C3 N2 48.8(6) . . . . C3 C2 C1 N1 -49.6(6) . . . . C2 C3 N2 C4 45.8(6) . . . . C2 C3 N2 C8 169.3(4) . . . . C2 C3 N2 Al1 -72.0(5) . . . . C5 C4 N2 C3 -79.9(5) . . . . C5 C4 N2 C8 157.1(4) . . . . C5 C4 N2 Al1 41.3(4) . . . . Al1 S1 C7 C6 9.2(4) . . . . C3 N2 C8 C9 62.9(5) . . . . C4 N2 C8 C9 -174.0(4) . . . . Al1 N2 C8 C9 -58.7(4) . . . . N2 C8 C9 S2 47.0(5) . . . . Al1 S2 C9 C8 -13.6(4) . . . . S1 C7 C6 N1 -44.0(6) . . . . N2 C4 C5 N1 -1.9(5) . . . . C2 C1 N1 C5 -44.7(6) . . . . C2 C1 N1 C6 -168.5(4) . . . . C2 C1 N1 Al1 74.0(5) . . . . C4 C5 N1 C1 83.5(5) . . . . C4 C5 N1 C6 -153.3(4) . . . . C4 C5 N1 Al1 -38.4(4) . . . . C7 C6 N1 C1 -62.7(6) . . . . C7 C6 N1 C5 173.8(4) . . . . C7 C6 N1 Al1 58.5(5) . . . .