#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:32:06 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270115 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708597.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_7708597 loop_ _publ_author_name 'Perez, Hiram' 'Di Santo, Alejandro' 'Piro, Oscar E.' 'Echeverr\'ia, Gustavo A.' 'Gonz\'alez M., Marlene' 'Ben Altabef, Aida' 'Gomila, Rosa Maria' 'Frontera, Antonio' 'Gil, Diego M.' _publ_section_title ; A novel 'main-part' isostructuralism in metal complexes with 1-methylimidazole: crystal structures, energy calculations and magnetic properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03159G _journal_year 2021 _chemical_formula_sum 'C16 H24 Co N14' _chemical_formula_weight 471.42 _chemical_name_systematic diazido-tetrakis(1-methylimidazole)cobalt(II) _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 mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-08-30 deposited with the CCDC. 2021-10-27 downloaded from the CCDC. ; _cell_angle_alpha 83.382(7) _cell_angle_beta 77.031(7) _cell_angle_gamma 73.001(7) _cell_formula_units_Z 1 _cell_length_a 7.9088(7) _cell_length_b 8.9979(8) _cell_length_c 9.1722(8) _cell_measurement_reflns_used 1263 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 24.7440 _cell_measurement_theta_min 4.4880 _cell_volume 607.41(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'ORTEP for Windows (Farrugia, 2012)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 297(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0604 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.818 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.818 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4539 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.818 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.816 _diffrn_reflns_theta_min 3.097 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.289 _exptl_crystal_description paralelepiped _exptl_crystal_F_000 245 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Methanol' _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.332 _exptl_crystal_size_min 0.088 _refine_diff_density_max 0.330 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 2600 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0442 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0138P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1051 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2149 _reflns_number_total 2600 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03159g2.cif _cod_data_source_block shelx _cod_database_code 7708597 _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_estimated_absorpt_t_min 0.762 _shelx_estimated_absorpt_t_max 0.938 _oxdiff_exptl_absorpt_empirical_full_min 0.880 _oxdiff_exptl_absorpt_empirical_full_max 1.249 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 0.71073 7.9088 8.9979 9.1722 83.382 77.031 73.001 ZERR 1.00 0.0007 0.0008 0.0008 0.007 0.007 0.007 LATT 1 SFAC C H N CO UNIT 16 24 14 1 MERG 2 SIZE 0.088 0.332 0.390 TEMP 24 REM Crystal shape/color: paralelepiped/violet CONF ABIN FMAP 2 PLAN -3 ACTA EQIV $1 -x+2, -y+1, -z+1 HTAB C14 N3_$1 EQIV $2 x, y, z+1 HTAB C13 N3_$2 L.S. 5 WGHT 0.044100 0.013800 FVAR 12.65993 C11 1 0.631208 0.380049 0.778758 11.00000 0.03247 0.03127 = 0.03148 -0.00505 -0.00340 -0.00858 C12 1 0.678554 0.603601 0.709298 11.00000 0.04619 0.03503 = 0.04320 0.00107 -0.01609 -0.01800 C13 1 0.742347 0.555325 0.835823 11.00000 0.04858 0.04470 = 0.04396 -0.00372 -0.01877 -0.01862 C14 1 0.761635 0.316560 1.011194 11.00000 0.05399 0.05589 = 0.03461 0.00536 -0.01483 -0.01141 AFIX 137 H14A 2 0.728414 0.221494 1.015344 11.00000 -1.50000 H14B 2 0.699068 0.371597 1.099945 11.00000 -1.50000 H14C 2 0.889460 0.293128 1.004837 11.00000 -1.50000 AFIX 0 C21 1 0.300520 0.806084 0.618615 11.00000 0.03494 0.03543 = 0.04753 -0.01110 -0.00744 -0.00664 C22 1 0.115337 0.682946 0.594676 11.00000 0.03314 0.03719 = 0.06568 -0.00843 -0.00816 -0.00791 C23 1 0.016219 0.819466 0.650241 11.00000 0.03392 0.04208 = 0.06543 -0.00803 -0.00409 0.00211 C24 1 0.088489 1.052237 0.726120 11.00000 0.07732 0.04711 = 0.09250 -0.03536 -0.02650 0.00804 AFIX 123 H24A 2 -0.040348 1.093199 0.751003 10.50000 -1.50000 H24B 2 0.137496 1.043099 0.814528 10.50000 -1.50000 H24C 2 0.138323 1.121106 0.652563 10.50000 -1.50000 H24D 2 0.197328 1.078403 0.727726 10.50000 -1.50000 H24E 2 0.019485 1.128503 0.664201 10.50000 -1.50000 H24F 2 0.018658 1.050496 0.826166 10.50000 -1.50000 AFIX 0 N1 3 0.626320 0.653979 0.401793 11.00000 0.04412 0.03239 = 0.03261 -0.00561 0.00132 -0.01788 N2 3 0.724239 0.638108 0.280552 11.00000 0.03724 0.03216 = 0.03950 -0.00155 -0.00558 -0.01540 N3 3 0.818385 0.631860 0.164620 11.00000 0.06578 0.07250 = 0.04740 -0.01156 0.01526 -0.03309 N11 3 0.606996 0.492696 0.673602 11.00000 0.03109 0.02918 = 0.02994 -0.00470 -0.00454 -0.00934 N12 3 0.712912 0.413077 0.879571 11.00000 0.03457 0.04359 = 0.02834 0.00021 -0.00847 -0.00843 N21 3 0.295107 0.673621 0.574941 11.00000 0.03083 0.02750 = 0.03022 -0.00321 -0.00413 -0.00696 N22 3 0.134369 0.898227 0.665344 11.00000 0.04510 0.03009 = 0.04721 -0.01159 -0.01038 0.00144 CO 4 0.500000 0.500000 0.500000 10.50000 0.02983 0.02554 = 0.02638 -0.00312 -0.00375 -0.00868 H11 2 0.597427 0.288265 0.788021 11.00000 0.02772 H12 2 0.676314 0.700235 0.647387 11.00000 0.04071 H13 2 0.791300 0.602630 0.891847 11.00000 0.05763 H21 2 0.404288 0.833863 0.621184 11.00000 0.04538 H22 2 0.080205 0.588554 0.569582 11.00000 0.04932 H23 2 -0.107308 0.874844 0.667479 11.00000 0.06209 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0442 for 2149 Fo > 4sig(Fo) and 0.0573 for all 2600 data REM 167 parameters refined using 0 restraints END WGHT 0.0417 0.0239 REM Highest difference peak 0.330, deepest hole -0.404, 1-sigma level 0.063 Q1 1 0.2135 0.6632 0.6016 11.00000 0.05 0.33 Q2 1 0.6143 0.5578 0.6971 11.00000 0.05 0.28 Q3 1 0.8969 0.5965 0.2439 11.00000 0.05 0.26 ; _shelx_res_checksum 50505 _shelx_hkl_file ; -10 -3 -4 10168.7 2083.53 2 -10 -3 -3 2171.10 1154.76 2 -10 -2 -5 6018.89 1695.53 2 -10 -2 -4 4558.23 1437.72 2 -10 -2 -3 1563.20 1082.25 2 -10 -2 -2-949.344 869.892 2 -10 -1 -5 5293.75 1575.33 2 -10 -1 -4 810.000 817.657 2 -10 -1 -3 2854.24 1170.27 2 -10 -1 -2 1170.22 939.006 2 -10 -1 -1 1184.41 968.885 2 -10 0 -3 442.140 460.313 2 -10 0 -2 1905.90 1168.15 2 -10 0 -1 6168.28 1728.44 2 -9 -7 1 4328.94 1378.28 4 -9 -6 -5 3520.65 1368.63 2 -9 -6 -4 4633.01 1485.06 2 -9 -6 -3 84.5275 388.199 2 -9 -6 -2 7941.17 1855.24 2 -9 -6 -1 3942.84 1349.18 2 -9 -6 1 17498.7 2479.89 4 -9 -5 -6 455.585 854.110 2 -9 -5 -5 5330.16 1627.08 2 -9 -5 -4 5290.88 1522.69 2 -9 -5 -3 809.258 899.746 2 -9 -5 -2 4452.25 1469.13 2 -9 -5 -1 10720.8 2206.65 2 -9 -5 0 2467.32 1164.20 2 -9 -4 -6 2387.32 1173.73 2 -9 -4 -5 7429.60 1784.50 2 -9 -4 -4 5282.74 1515.01 2 -9 -4 -3 824.226 761.929 2 -9 -4 -2 2933.50 1280.59 2 -9 -4 -1 13619.0 2336.26 2 -9 -4 0 1704.84 1142.04 2 -9 -3 -6 11159.6 2079.21 2 -9 -3 -5 6473.78 1639.86 2 -9 -3 -4 3841.24 1299.66 2 -9 -3 -3 1119.48 920.403 2 -9 -3 -2 775.993 812.419 2 -9 -3 -1 12393.7 2252.78 2 -9 -3 0 4501.04 1461.64 2 -9 -2 -6 8060.15 1722.32 2 -9 -2 -5 4387.23 1409.32 2 -9 -2 -4 7437.30 1700.34 2 -9 -2 -3 3479.46 1259.94 2 -9 -2 -2 5405.02 1546.51 2 -9 -2 -1 14827.2 2388.12 2 -9 -1 -5 9307.85 1862.46 2 -9 -1 -4 1819.41 946.436 2 -9 -1 -3 3687.67 1179.58 2 -9 -1 -2 189.043 732.334 2 -9 -1 -1 7609.39 1766.72 2 -9 0 -5 3054.21 977.000 2 -9 0 -4 782.496 823.999 2 -9 0 -3 8606.14 1745.86 2 -9 0 -2 5383.60 1412.50 2 -9 0 -1 3540.84 1247.14 2 -9 1 -3 2820.74 967.253 2 -9 1 -2 1289.67 759.656 2 -9 1 -1 221.603 592.782 2 -8 -9 -3 6829.34 1813.18 2 -8 -9 -2 5454.99 1625.90 2 -8 -9 -1 6495.51 1651.04 2 -8 -8 -5 3790.72 1227.48 2 -8 -8 -4 8336.00 1973.90 2 -8 -8 -3 11287.9 2215.03 2 -8 -8 -2 11054.0 2170.31 2 -8 -8 -1 2250.62 1101.27 2 -8 -8 0 9590.98 1929.99 4 -8 -8 0 8969.34 1905.77 2 -8 -8 1 5169.41 1467.38 4 -8 -8 1 6581.57 1701.54 2 -8 -8 2 1316.19 741.156 4 -8 -8 3-737.836 546.445 4 -8 -7 -5 7494.98 1737.90 2 -8 -7 -4 3495.10 1286.59 2 -8 -7 -3 6009.92 1641.41 2 -8 -7 -2 8039.36 1823.64 2 -8 -7 -1-60.2074 355.101 2 -8 -7 0 8130.93 1827.52 2 -8 -7 1 11760.8 2190.54 2 -8 -7 1 9112.44 1774.86 4 -8 -7 2 1154.01 730.331 4 -8 -7 2-771.756 587.146 2 -8 -7 3 89.5493 256.531 4 -8 -6 -5 1490.63 955.499 2 -8 -6 -4 2561.40 1098.91 2 -8 -6 -3 388.383 771.268 2 -8 -6 -2 14188.0 2367.09 2 -8 -6 -1-1226.33 894.771 2 -8 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4195.33 1175.38 2 -8 0 -2 751.554 663.797 2 -8 0 -1 5047.46 1312.13 2 -8 1 -5 813.173 563.900 2 -8 1 -4-380.799 529.309 2 -8 1 -3 15064.9 2021.94 2 -8 1 -2 660.120 579.975 2 -8 1 -1 9920.12 1708.96 2 -8 2 -2 3951.09 1070.92 2 -8 2 -1 5767.58 1272.37 2 -7 -11 -1 3796.86 1332.68 2 -7 -10 -3 2727.02 1114.40 2 -7 -10 -2 6231.63 1602.10 2 -7 -10 -1 1956.34 878.928 2 -7 -10 0-625.759 632.253 2 -7 -10 1 1878.92 851.188 2 -7 -10 2 1902.89 962.226 2 -7 -9 -4 8338.67 1798.78 2 -7 -9 -3 8582.66 1835.32 2 -7 -9 -2 2241.35 1033.86 2 -7 -9 -2 1035.67 783.954 4 -7 -9 -1 7326.70 1776.31 2 -7 -9 -1 9964.39 1911.41 4 -7 -9 0 5845.34 1597.43 2 -7 -9 0 7759.48 1779.54 4 -7 -9 1 6058.81 1660.86 4 -7 -9 1 8564.33 1817.92 2 -7 -9 2 4017.63 1222.43 2 -7 -9 2 3166.07 1143.38 4 -7 -9 3-490.324 585.303 2 -7 -8 -4 3364.45 1195.84 2 -7 -8 -3 24819.7 3019.34 2 -7 -8 -2 10898.1 1991.26 2 -7 -8 -1 16180.8 2434.27 2 -7 -8 0 23501.7 2905.41 4 -7 -8 0 21978.5 2816.27 2 -7 -8 1 6679.77 1680.06 4 -7 -8 1 6844.20 1629.10 2 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897.443 3 10 3 -1 5242.25 1366.68 3 0 0 0 0.00 0.00 0 TITL Co(1-MI)N3 in P1 REM P1 (#1 in standard setting) CELL 0.71073 7.908770 8.997875 9.172213 83.3817 77.0314 73.0008 ZERR 2.00 0.000686 0.000755 0.000794 0.0071 0.0074 0.0075 LATT -1 SFAC C H N Co UNIT 16.00 24.00 14.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 10805 _shelx_fab_file ; 10 3 4 -0.39 0.00 10 3 3 -0.21 0.00 10 2 5 0.00 0.00 10 2 4 -0.08 0.00 10 2 3 0.10 0.00 10 2 2 0.14 0.00 10 1 5 -0.09 0.00 10 1 4 0.01 0.00 10 1 3 0.24 0.00 10 1 2 0.04 0.00 10 1 1 -0.38 0.00 10 0 3 0.13 0.00 10 0 2 -0.09 0.00 10 0 1 -0.28 0.00 -9 -7 1 0.02 0.00 9 6 5 -0.53 0.00 9 6 4 -0.22 0.00 9 6 3 -0.20 0.00 9 6 2 -0.77 0.00 9 6 1 0.02 0.00 -9 -6 1 -0.10 0.00 9 5 6 0.09 0.00 9 5 5 -0.55 0.00 9 5 4 0.09 0.00 9 5 3 0.17 0.00 9 5 2 -0.83 0.00 9 5 1 0.07 0.00 9 5 0 0.29 0.00 9 4 6 0.25 0.00 9 4 5 -0.45 0.00 9 4 4 0.31 0.00 9 4 3 0.52 0.00 9 4 2 -0.61 0.00 9 4 1 0.34 0.00 9 4 0 0.72 0.00 9 3 6 0.36 0.00 9 3 5 -0.26 0.00 9 3 4 0.25 0.00 9 3 3 0.49 0.00 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0.22 0.00 -8 0 4 -0.10 0.00 -8 0 3 -0.61 0.00 -8 0 2 0.09 0.00 -8 0 1 0.19 0.00 8 0 0 -0.66 0.00 8 0 6 0.03 0.00 8 0 7 0.48 0.00 -8 -1 5 0.11 0.00 -8 -1 4 -0.03 0.00 -8 -1 3 -0.81 0.00 -8 -1 2 -0.05 0.00 -8 -1 1 -0.06 0.00 8 1 0 -1.00 0.00 8 1 6 -0.29 0.00 8 1 7 0.22 0.00 8 1 8 0.30 0.00 8 1 9 -0.26 0.00 -8 -2 5 0.21 0.00 -8 -2 4 0.03 0.00 -8 -2 3 -0.87 0.00 -8 -2 2 -0.14 0.00 -8 -2 1 -0.28 0.00 8 2 0 -1.22 0.00 8 2 6 -0.51 0.00 8 2 7 -0.06 0.00 8 2 8 0.23 0.00 8 2 9 -0.28 0.00 -8 -3 5 0.33 0.00 -8 -3 4 0.10 0.00 -8 -3 3 -0.64 0.00 -8 -3 2 -0.04 0.00 -8 -3 1 -0.26 0.00 8 3 0 -1.09 0.00 8 3 7 -0.19 0.00 8 3 8 0.19 0.00 8 3 9 -0.15 0.00 -8 -4 5 0.40 0.00 -8 -4 4 0.11 0.00 -8 -4 3 -0.25 0.00 -8 -4 1 -0.08 0.00 8 4 7 -0.19 0.00 8 4 8 0.17 0.00 8 4 9 0.05 0.00 -8 -5 5 0.35 0.00 -8 -5 4 0.06 0.00 -8 -5 3 0.08 0.00 -8 -5 1 0.07 0.00 8 5 6 -0.09 0.00 8 5 7 -0.11 0.00 8 5 8 0.12 0.00 8 5 9 0.14 0.00 -8 -6 4 0.05 0.00 -8 -6 3 0.28 0.00 8 6 6 0.11 0.00 8 6 7 0.01 0.00 8 6 8 0.06 0.00 8 6 9 0.11 0.00 8 7 6 0.19 0.00 8 7 7 0.10 0.00 8 7 8 0.03 0.00 8 8 6 0.13 0.00 8 8 7 0.08 0.00 8 9 5 0.39 0.00 8 9 6 0.07 0.00 9 -2 1 0.29 0.00 9 -2 2 0.03 0.00 9 -2 3 0.25 0.00 9 -2 4 0.49 0.00 9 -2 5 0.14 0.00 -9 1 3 0.03 0.00 -9 1 0 0.26 0.00 9 -1 4 0.44 0.00 -9 0 3 0.08 0.00 -9 0 1 -0.34 0.00 9 0 0 0.35 0.00 -9 -1 4 -0.15 0.00 -9 -1 2 -0.07 0.00 -9 -1 1 -0.19 0.00 9 1 0 0.66 0.00 -9 -2 2 0.13 0.00 -9 -2 1 0.06 0.00 9 2 0 1.02 0.00 -9 -3 3 0.59 0.00 -9 -3 2 0.19 0.00 -9 -3 1 0.15 0.00 -9 -4 1 0.03 0.00 10 1 0 -0.32 0.00 -10 -2 1 0.40 0.00 10 2 0 -0.44 0.00 -10 -3 1 0.35 0.00 1 0 0 -29.09 0.00 0 1 0 35.03 0.00 -9 2 0 0.27 0.00 10 3 0 -0.43 0.00 -8 4 0 -0.43 0.00 10 4 0 -0.26 0.00 -7 5 0 0.54 0.00 9 6 0 0.07 0.00 -6 7 0 -0.49 0.00 9 7 0 0.02 0.00 -5 8 0 0.59 0.00 -4 9 0 -0.40 0.00 -3 9 0 0.22 0.00 8 9 0 0.03 0.00 -2 10 0 -0.02 0.00 0 11 0 0.38 0.00 4 11 0 0.38 0.00 5 11 0 0.07 0.00 -5 -11 1 0.24 0.00 -4 -11 1 0.04 0.00 0 -11 1 -0.10 0.00 2 -10 1 0.26 0.00 3 -9 1 -0.56 0.00 4 -9 1 0.46 0.00 5 -8 1 -0.32 0.00 6 -7 1 0.17 0.00 -9 -5 1 -0.12 0.00 8 -4 1 -0.09 0.00 0 -1 1 16.33 0.00 0 0 1 17.26 0.00 -9 1 1 -0.29 0.00 10 2 1 -0.48 0.00 -8 3 1 0.01 0.00 10 3 1 -0.47 0.00 10 4 1 -0.31 0.00 -7 5 1 0.08 0.00 10 5 1 -0.11 0.00 -6 6 1 -0.33 0.00 9 7 1 0.13 0.00 -5 8 1 0.42 0.00 9 8 1 0.15 0.00 -3 9 1 0.54 0.00 -2 10 1 -0.59 0.00 0 11 1 -0.42 0.00 5 11 1 -0.47 0.00 6 11 1 0.53 0.00 -4 -11 2 0.74 0.00 -1 -11 2 0.11 0.00 -6 -10 2 0.36 0.00 1 -10 2 0.28 0.00 2 -10 2 -0.36 0.00 3 -9 2 0.09 0.00 5 -8 2 -0.25 0.00 6 -7 2 0.14 0.00 -9 -6 2 -0.06 0.00 -9 -5 2 -0.06 0.00 -9 -4 2 0.07 0.00 -9 0 2 -0.20 0.00 -8 3 2 -0.01 0.00 10 3 2 0.21 0.00 10 4 2 0.32 0.00 -7 5 2 -0.20 0.00 10 5 2 0.45 0.00 -6 6 2 0.21 0.00 10 6 2 0.44 0.00 -5 7 2 0.02 0.00 9 7 2 -0.42 0.00 9 8 2 -0.10 0.00 -2 10 2 -0.06 0.00 0 11 2 -0.73 0.00 5 11 2 0.43 0.00 6 11 2 -0.05 0.00 -5 -10 3 -0.37 0.00 1 -10 3 -0.35 0.00 3 -9 3 -0.01 0.00 -9 -4 3 0.38 0.00 -9 -2 3 0.52 0.00 -9 -1 3 0.28 0.00 -8 2 3 -0.48 0.00 -7 4 3 0.76 0.00 10 4 3 -0.38 0.00 10 5 3 -0.24 0.00 -6 6 3 -0.24 0.00 10 6 3 0.01 0.00 -5 7 3 0.16 0.00 9 7 3 -0.29 0.00 -4 8 3 -0.12 0.00 9 8 3 -0.17 0.00 -3 9 3 0.01 0.00 -2 10 3 -0.01 0.00 0 11 3 -0.24 0.00 5 11 3 0.82 0.00 6 11 3 -0.55 0.00 0 -10 4 -0.13 0.00 1 -10 4 -0.33 0.00 -5 -9 4 -0.06 0.00 2 -9 4 0.58 0.00 3 -9 4 -0.18 0.00 4 -8 4 0.11 0.00 -7 3 4 0.51 0.00 -7 4 4 0.32 0.00 10 4 4 -0.61 0.00 -6 5 4 -0.50 0.00 10 5 4 -0.49 0.00 -5 7 4 0.07 0.00 9 7 4 -0.35 0.00 -4 8 4 0.05 0.00 9 8 4 -0.24 0.00 8 9 4 0.24 0.00 7 10 4 -0.53 0.00 1 11 4 0.02 0.00 5 11 4 0.30 0.00 -2 -10 5 0.13 0.00 -1 -10 5 0.04 0.00 -5 -9 5 -0.27 0.00 1 -9 5 0.19 0.00 2 -9 5 0.01 0.00 -6 -8 5 0.17 0.00 3 -8 5 -0.03 0.00 4 -8 5 0.00 0.00 -7 -7 5 -0.31 0.00 -6 -7 5 0.20 0.00 5 -7 5 0.00 0.00 9 -1 5 0.23 0.00 -7 2 5 0.10 0.00 -7 3 5 0.02 0.00 10 3 5 0.05 0.00 -6 4 5 0.10 0.00 10 4 5 0.10 0.00 10 5 5 0.17 0.00 -5 6 5 -0.04 0.00 -4 7 5 0.07 0.00 9 7 5 -0.40 0.00 9 8 5 -0.24 0.00 0 10 5 -0.45 0.00 5 11 5 -0.13 0.00 -2 -9 6 0.02 0.00 -1 -9 6 -0.21 0.00 0 -9 6 0.00 0.00 1 -9 6 0.13 0.00 2 -8 6 -0.20 0.00 3 -8 6 0.06 0.00 -6 -7 6 -0.28 0.00 4 -7 6 -0.12 0.00 -7 -5 6 0.14 0.00 8 -3 6 0.14 0.00 8 -2 6 0.21 0.00 9 -1 6 0.05 0.00 9 0 6 0.09 0.00 -7 1 6 0.16 0.00 9 1 6 0.22 0.00 -6 3 6 -0.26 0.00 -5 5 6 -0.09 0.00 9 6 6 -0.05 0.00 9 7 6 -0.12 0.00 1 10 6 0.31 0.00 5 10 6 0.67 0.00 6 10 6 -0.37 0.00 -3 -8 7 0.15 0.00 -2 -8 7 -0.20 0.00 -1 -8 7 0.16 0.00 0 -8 7 -0.18 0.00 1 -8 7 0.22 0.00 2 -8 7 -0.20 0.00 3 -7 7 0.18 0.00 5 -6 7 -0.05 0.00 -6 -5 7 -0.28 0.00 8 -2 7 0.35 0.00 8 -1 7 0.53 0.00 9 0 7 -0.26 0.00 -6 1 7 -0.31 0.00 9 1 7 -0.09 0.00 -6 2 7 -0.29 0.00 9 2 7 0.15 0.00 9 3 7 0.29 0.00 -5 4 7 0.35 0.00 9 4 7 0.28 0.00 9 5 7 0.21 0.00 9 6 7 0.10 0.00 0 9 7 -0.20 0.00 7 9 7 0.20 0.00 2 10 7 0.22 0.00 5 10 7 0.53 0.00 -3 -7 8 0.08 0.00 -2 -7 8 -0.35 0.00 -1 -7 8 0.44 0.00 0 -7 8 -0.48 0.00 1 -7 8 0.35 0.00 2 -7 8 -0.42 0.00 3 -6 8 0.51 0.00 4 -6 8 -0.28 0.00 -5 -5 8 -0.17 0.00 -4 -5 8 0.17 0.00 -5 -4 8 -0.38 0.00 -5 -3 8 -0.43 0.00 8 -1 8 0.09 0.00 8 0 8 0.28 0.00 -5 1 8 -0.06 0.00 -5 2 8 -0.03 0.00 9 3 8 -0.15 0.00 -4 4 8 0.10 0.00 9 4 8 -0.09 0.00 1 9 8 0.70 0.00 2 9 8 -0.58 0.00 3 9 8 0.30 0.00 4 9 8 0.00 0.00 5 9 8 -0.08 0.00 6 9 8 -0.24 0.00 -2 -6 9 -0.05 0.00 -1 -6 9 0.16 0.00 0 -6 9 -0.13 0.00 1 -6 9 -0.08 0.00 2 -6 9 0.06 0.00 -3 -5 9 -0.40 0.00 3 -5 9 0.00 0.00 4 -5 9 -0.03 0.00 -4 -4 9 0.66 0.00 -3 -4 9 -0.81 0.00 -4 -3 9 0.83 0.00 -4 -2 9 0.69 0.00 -4 -1 9 0.38 0.00 7 -1 9 0.75 0.00 -4 0 9 0.23 0.00 7 0 9 0.82 0.00 -4 1 9 0.29 0.00 -4 2 9 0.34 0.00 7 7 9 0.19 0.00 1 8 9 0.03 0.00 2 8 9 -0.25 0.00 3 8 9 0.33 0.00 4 8 9 -0.15 0.00 5 8 9 -0.05 0.00 6 8 9 -0.12 0.00 -1 -5 10 -0.36 0.00 0 -5 10 0.51 0.00 1 -5 10 -0.49 0.00 2 -5 10 0.50 0.00 -2 -4 10 0.24 0.00 -1 -4 10 -0.53 0.00 0 -4 10 0.86 0.00 1 -4 10 -0.76 0.00 2 -4 10 0.70 0.00 3 -4 10 -0.74 0.00 -3 -3 10 0.01 0.00 -2 -3 10 0.23 0.00 -3 -2 10 0.22 0.00 -3 -1 10 0.46 0.00 -3 0 10 0.52 0.00 -3 1 10 0.31 0.00 7 1 10 -0.01 0.00 -3 2 10 0.05 0.00 7 5 10 -0.11 0.00 0 6 10 0.10 0.00 4 6 10 0.04 0.00 5 6 10 -0.21 0.00 6 6 10 0.11 0.00 2 7 10 0.29 0.00 3 7 10 -0.13 0.00 4 7 10 -0.04 0.00 5 7 10 -0.07 0.00 0 -3 11 0.05 0.00 1 -3 11 -0.04 0.00 2 -3 11 -0.24 0.00 -1 -2 11 0.40 0.00 2 -2 11 -0.56 0.00 3 -2 11 0.21 0.00 4 -2 11 0.29 0.00 -1 -1 11 0.55 0.00 -1 0 11 0.64 0.00 4 3 11 0.31 0.00 5 3 11 -0.39 0.00 6 3 11 0.39 0.00 2 4 11 0.33 0.00 3 4 11 -0.23 0.00 4 4 11 0.19 0.00 5 4 11 -0.31 0.00 2 5 11 0.26 0.00 3 5 11 -0.12 0.00 4 5 11 0.02 0.00 5 5 11 -0.17 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 70515) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 129 35 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 2.749 0 1 0 2.370 0 -1 1 3.378 0 0 1 2.282 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL shelxt_a.res in P-1 CELL 7.9088 8.9979 9.1722 83.38 77.03 73.00 SPGR P-1 # Solvent Accessible Volume = 133.7 # Electrons Found in S.A.V. = 34.6 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.433 0.995 0.312 ! 5.05 eA-3 C102 0.598 0.021-0.003 ! 3.86 eA-3 C103 0.448 0.023 0.081 ! 3.52 eA-3 Q104 0.942 0.968 0.226 ! 0.90 eA-3 Q105 0.402 0.717 0.211 ! 0.77 eA-3 Q106 0.867 0.897 0.343 ! 0.77 eA-3 Q107 0.437 0.539 0.468 ! 0.77 eA-3 Q108 0.879 0.311 0.464 ! 0.71 eA-3 Q109 0.715 0.236 0.028 ! 0.69 eA-3 Q110 0.753 0.691 0.120 ! 0.67 eA-3 Q111 0.185 0.386 0.110 ! 0.67 eA-3 Q112 0.311 0.298 0.368 ! 0.64 eA-3 Q113 0.601 0.168 0.384 ! 0.64 eA-3 Q114 0.900 0.291 0.007 ! 0.62 eA-3 Q115 0.929 0.398 0.437 ! 0.62 eA-3 Q116 0.936 0.124 0.324 ! 0.59 eA-3 Q117 0.686 0.624 0.430 ! 0.56 eA-3 Q118 0.882 0.587 0.226 ! 0.55 eA-3 Q119 0.117 0.116 0.334 ! 0.52 eA-3 Q120 0.560 0.690 0.372 ! 0.50 eA-3 ) ; _shelx_fab_checksum 39820 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 C11 C 0.6312(3) 0.3800(3) 0.7788(3) 0.0320(6) Uani 1 1 d . . . . . C12 C 0.6786(4) 0.6036(3) 0.7093(3) 0.0391(6) Uani 1 1 d . . . . . C13 C 0.7423(4) 0.5553(4) 0.8358(3) 0.0428(7) Uani 1 1 d . . . . . C14 C 0.7616(4) 0.3166(4) 1.0112(3) 0.0486(7) Uani 1 1 d . . . . . H14A H 0.7284 0.2215 1.0153 0.073 Uiso 1 1 calc R U . . . H14B H 0.6991 0.3716 1.0999 0.073 Uiso 1 1 calc R U . . . H14C H 0.8895 0.2931 1.0048 0.073 Uiso 1 1 calc R U . . . C21 C 0.3005(4) 0.8061(3) 0.6186(3) 0.0394(7) Uani 1 1 d . . . . . C22 C 0.1153(3) 0.6829(4) 0.5947(4) 0.0455(7) Uani 1 1 d . . . . . C23 C 0.0162(4) 0.8195(4) 0.6502(4) 0.0504(8) Uani 1 1 d . . . . . C24 C 0.0885(5) 1.0522(4) 0.7261(5) 0.0736(11) Uani 1 1 d . . . . . H24A H -0.0403 1.0932 0.7510 0.110 Uiso 0.5 1 calc R U P . . H24B H 0.1375 1.0431 0.8145 0.110 Uiso 0.5 1 calc R U P . . H24C H 0.1383 1.1211 0.6526 0.110 Uiso 0.5 1 calc R U P . . H24D H 0.1973 1.0784 0.7277 0.110 Uiso 0.5 1 calc R U P . . H24E H 0.0195 1.1285 0.6642 0.110 Uiso 0.5 1 calc R U P . . H24F H 0.0187 1.0505 0.8262 0.110 Uiso 0.5 1 calc R U P . . N1 N 0.6263(3) 0.6540(2) 0.4018(2) 0.0359(5) Uani 1 1 d . . . . . N2 N 0.7242(3) 0.6381(2) 0.2806(3) 0.0354(5) Uani 1 1 d . . . . . N3 N 0.8184(4) 0.6319(3) 0.1646(3) 0.0625(8) Uani 1 1 d . . . . . N11 N 0.6070(2) 0.4927(2) 0.6736(2) 0.0298(5) Uani 1 1 d . . . . . N12 N 0.7129(3) 0.4131(3) 0.8796(2) 0.0358(5) Uani 1 1 d . . . . . N21 N 0.2951(2) 0.6736(2) 0.5749(2) 0.0299(5) Uani 1 1 d . . . . . N22 N 0.1344(3) 0.8982(3) 0.6653(3) 0.0424(6) Uani 1 1 d . . . . . Co Co 0.5000 0.5000 0.5000 0.02719(16) Uani 1 2 d S . P . . H11 H 0.597(3) 0.288(3) 0.788(3) 0.028(6) Uiso 1 1 d . . . . . H12 H 0.676(3) 0.700(3) 0.647(3) 0.041(7) Uiso 1 1 d . . . . . H13 H 0.791(4) 0.603(4) 0.892(4) 0.058(9) Uiso 1 1 d . . . . . H21 H 0.404(4) 0.834(3) 0.621(3) 0.045(8) Uiso 1 1 d . . . . . H22 H 0.080(3) 0.589(4) 0.570(3) 0.049(8) Uiso 1 1 d . . . . . H23 H -0.107(4) 0.875(4) 0.667(4) 0.062(9) Uiso 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 C11 0.0325(13) 0.0313(15) 0.0315(14) -0.0050(12) -0.0034(11) -0.0086(11) C12 0.0462(15) 0.0350(16) 0.0432(17) 0.0011(13) -0.0161(13) -0.0180(13) C13 0.0486(16) 0.0447(18) 0.0440(17) -0.0037(14) -0.0188(13) -0.0186(14) C14 0.0540(17) 0.056(2) 0.0346(16) 0.0054(14) -0.0148(14) -0.0114(15) C21 0.0349(14) 0.0354(16) 0.0475(17) -0.0111(13) -0.0074(12) -0.0066(12) C22 0.0331(14) 0.0372(16) 0.066(2) -0.0084(15) -0.0082(13) -0.0079(13) C23 0.0339(15) 0.0421(18) 0.065(2) -0.0080(16) -0.0041(14) 0.0021(14) C24 0.077(2) 0.047(2) 0.092(3) -0.035(2) -0.027(2) 0.0080(18) N1 0.0441(12) 0.0324(12) 0.0326(12) -0.0056(10) 0.0013(10) -0.0179(10) N2 0.0372(12) 0.0322(12) 0.0395(14) -0.0016(10) -0.0056(10) -0.0154(10) N3 0.0658(17) 0.072(2) 0.0474(17) -0.0116(15) 0.0153(14) -0.0331(15) N11 0.0311(10) 0.0292(11) 0.0299(11) -0.0047(10) -0.0045(9) -0.0093(9) N12 0.0346(11) 0.0436(14) 0.0283(12) 0.0002(10) -0.0085(9) -0.0084(10) N21 0.0308(11) 0.0275(12) 0.0302(11) -0.0032(9) -0.0041(9) -0.0070(9) N22 0.0451(13) 0.0301(13) 0.0472(15) -0.0116(11) -0.0104(11) 0.0014(10) Co 0.0298(3) 0.0255(3) 0.0264(3) -0.0031(2) -0.00375(19) -0.0087(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' Co Co 0.3494 0.9721 '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 _geom_angle_publ_flag N11 C11 N12 111.3(2) . . ? C13 C12 N11 109.1(3) . . ? C12 C13 N12 107.0(2) . . ? N21 C21 N22 111.3(2) . . ? C23 C22 N21 109.7(3) . . ? C22 C23 N22 106.8(2) . . ? N2 N1 Co 122.94(16) . . ? N3 N2 N1 175.9(3) . . ? C11 N11 C12 105.6(2) . . ? C11 N11 Co 127.58(17) . . ? C12 N11 Co 126.81(19) . . ? C11 N12 C13 106.9(2) . . ? C11 N12 C14 127.0(2) . . ? C13 N12 C14 126.1(2) . . ? C21 N21 C22 105.4(2) . . ? C21 N21 Co 127.16(17) . . ? C22 N21 Co 127.40(18) . . ? C21 N22 C23 106.9(2) . . ? C21 N22 C24 126.4(2) . . ? C23 N22 C24 126.7(2) . . ? N11 Co N11 180.0 . 2_666 ? N11 Co N21 88.06(8) . 2_666 ? N11 Co N21 91.94(8) 2_666 2_666 ? N11 Co N21 91.94(8) . . ? N11 Co N21 88.06(8) 2_666 . ? N21 Co N21 180.0 2_666 . ? N11 Co N1 88.64(9) . . ? N11 Co N1 91.36(9) 2_666 . ? N21 Co N1 92.33(8) 2_666 . ? N21 Co N1 87.67(8) . . ? N11 Co N1 91.36(9) . 2_666 ? N11 Co N1 88.64(9) 2_666 2_666 ? N21 Co N1 87.67(8) 2_666 2_666 ? N21 Co N1 92.33(8) . 2_666 ? N1 Co N1 180.0 . 2_666 ? 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 C11 N11 1.318(3) . ? C11 N12 1.343(3) . ? C12 C13 1.345(4) . ? C12 N11 1.383(3) . ? C13 N12 1.367(4) . ? C14 N12 1.460(3) . ? C21 N21 1.315(3) . ? C21 N22 1.338(3) . ? C22 C23 1.336(4) . ? C22 N21 1.371(3) . ? C23 N22 1.365(4) . ? C24 N22 1.468(4) . ? N1 N2 1.201(3) . ? N1 Co 1.961(2) . ? N2 N3 1.150(3) . ? N11 Co 1.9504(19) . ? N21 Co 1.9510(18) . ? Co N11 1.9504(19) 2_666 ? Co N21 1.9510(18) 2_666 ? Co N1 1.961(2) 2_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C14 H14C N3 0.96 2.70 3.489(4) 140.3 2_766 C13 H13 N3 0.91(3) 2.61(3) 3.386(4) 144(3) 1_556 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 N11 C12 C13 N12 0.6(3) . . . . ? N21 C22 C23 N22 0.3(4) . . . . ? N12 C11 N11 C12 0.3(3) . . . . ? N12 C11 N11 Co 178.57(14) . . . . ? C13 C12 N11 C11 -0.6(3) . . . . ? C13 C12 N11 Co -178.82(17) . . . . ? N11 C11 N12 C13 0.0(3) . . . . ? N11 C11 N12 C14 180.0(2) . . . . ? C12 C13 N12 C11 -0.4(3) . . . . ? C12 C13 N12 C14 179.6(2) . . . . ? N22 C21 N21 C22 0.2(3) . . . . ? N22 C21 N21 Co -179.17(18) . . . . ? C23 C22 N21 C21 -0.3(4) . . . . ? C23 C22 N21 Co 179.1(2) . . . . ? N21 C21 N22 C23 -0.1(3) . . . . ? N21 C21 N22 C24 178.0(3) . . . . ? C22 C23 N22 C21 -0.1(4) . . . . ? C22 C23 N22 C24 -178.2(3) . . . . ?