#------------------------------------------------------------------------------ #$Date: 2019-10-02 12:09:14 +0100 (Wed, 02 Oct 2019) $ #$Revision: 219027 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/03/4060390.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_4060390 loop_ _publ_author_name 'Mandal, Debaprasad' 'Gupta, B. D.' _publ_section_title ; Cobaloximes with Dimesitylglyoxime: Synthesis, Characterization, and Spectral Correlations with the Related Cobaloximes ; _journal_coden_ASTM ORGND7 _journal_issue 7 _journal_name_full Organometallics _journal_page_first 1501 _journal_page_last 1510 _journal_paper_doi 10.1021/om049096m _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C46 H53 Br1 Cl2 Co1 N5 O4' _chemical_formula_sum 'C46 H53 Br Cl2 Co N5 O4' _chemical_formula_weight 1899.35 _chemical_name_common 'Bromo cobalt(III) Mesitylglyoxime Pyridine' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.000(0) _cell_angle_beta 108.493(2) _cell_angle_gamma 90.000(0) _cell_formula_units_Z 8 _cell_length_a 27.579(17) _cell_length_b 9.116(5) _cell_length_c 36.610(2) _cell_measurement_temperature 100(2) _cell_volume 8729(7) _diffrn_ambient_temperature 100(2) _exptl_crystal_density_diffrn 1.445 _cod_duplicate_entry 4075673 _cod_depositor_comments ; Updated bibliographic information. Antanas Vaitkus, 2019-10-02 Marked entry as a duplicate of entry 4075673. Antanas Vaitkus, 2019-10-02 ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4060390 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24553(2) 0.15486(6) 0.632041(15) 0.00781(15) Uani 1 1 d . . . Br1 Br 0.27846(2) 0.38127(6) 0.621148(16) 0.02766(16) Uani 1 1 d . . . Cl1 Cl 0.17106(6) -0.23647(15) 0.51454(4) 0.0337(3) Uani 1 1 d . . . Cl2 Cl 0.18799(7) -0.1970(2) 0.44106(5) 0.0481(4) Uani 1 1 d . . . O1 O 0.25659(11) 0.2489(3) 0.70881(9) 0.0139(6) Uani 1 1 d . . . H1 H 0.2338 0.2754 0.6964 0.021 Uiso 1 1 d . . . O2 O 0.32011(11) 0.0115(3) 0.60576(8) 0.0124(6) Uani 1 1 d . . . H2 H 0.2991 0.0375 0.5870 0.019 Uiso 1 1 d . . . O3 O 0.23881(11) 0.0803(3) 0.55607(8) 0.0125(6) Uani 1 1 d . . . O4 O 0.17278(11) 0.2952(3) 0.65937(8) 0.0129(6) Uani 1 1 d . . . N1 N 0.27874(13) 0.1799(4) 0.68595(10) 0.0100(7) Uani 1 1 d . . . N2 N 0.30980(13) 0.0666(4) 0.63626(10) 0.0097(7) Uani 1 1 d . . . N3 N 0.21366(13) 0.1367(4) 0.57839(10) 0.0100(7) Uani 1 1 d . . . N4 N 0.18175(13) 0.2411(4) 0.62827(10) 0.0107(7) Uani 1 1 d . . . N5 N 0.21993(12) -0.0414(4) 0.64081(10) 0.0087(6) Uani 1 1 d . . . C1 C 0.32434(15) 0.1257(4) 0.70027(12) 0.0101(8) Uani 1 1 d . . . C2 C 0.34229(15) 0.0532(4) 0.67060(12) 0.0101(8) Uani 1 1 d . . . C3 C 0.39044(15) -0.0319(5) 0.67895(12) 0.0112(8) Uani 1 1 d . . . C4 C 0.43839(15) 0.0375(5) 0.69197(12) 0.0132(8) Uani 1 1 d . . . C5 C 0.48248(16) -0.0475(6) 0.70083(13) 0.0181(9) Uani 1 1 d . . . H5 H 0.5149 -0.0009 0.7100 0.022 Uiso 1 1 calc R . . C6 C 0.48012(17) -0.2004(5) 0.69659(13) 0.0184(9) Uani 1 1 d . . . C7 C 0.43285(18) -0.2650(5) 0.68279(13) 0.0182(9) Uani 1 1 d . . . H7 H 0.4310 -0.3684 0.6794 0.022 Uiso 1 1 calc R . . C8 C 0.38772(16) -0.1855(5) 0.67355(12) 0.0137(8) Uani 1 1 d . . . C9 C 0.44418(17) 0.2018(5) 0.69637(14) 0.0176(9) Uani 1 1 d . . . H9A H 0.4137 0.2497 0.6790 0.026 Uiso 1 1 calc R . . H9B H 0.4744 0.2332 0.6899 0.026 Uiso 1 1 calc R . . H9C H 0.4481 0.2292 0.7230 0.026 Uiso 1 1 calc R . . C10 C 0.52849(19) -0.2910(7) 0.70794(16) 0.0289(12) Uani 1 1 d . . . H10A H 0.5500 -0.2611 0.6925 0.043 Uiso 1 1 calc R . . H10B H 0.5197 -0.3951 0.7034 0.043 Uiso 1 1 calc R . . H10C H 0.5471 -0.2756 0.7353 0.043 Uiso 1 1 calc R . . C11 C 0.33725(17) -0.2641(5) 0.65873(14) 0.0180(9) Uani 1 1 d . . . H11A H 0.3153 -0.2347 0.6739 0.027 Uiso 1 1 calc R . . H11B H 0.3430 -0.3702 0.6610 0.027 Uiso 1 1 calc R . . H11C H 0.3206 -0.2383 0.6316 0.027 Uiso 1 1 calc R . . C12 C 0.35508(15) 0.1406(5) 0.74132(12) 0.0125(8) Uani 1 1 d . . . C13 C 0.36296(15) 0.0191(5) 0.76628(13) 0.0128(8) Uani 1 1 d . . . C14 C 0.39242(16) 0.0354(5) 0.80427(13) 0.0140(8) Uani 1 1 d . . . H14 H 0.3972 -0.0463 0.8211 0.017 Uiso 1 1 calc R . . C15 C 0.41535(16) 0.1685(5) 0.81853(13) 0.0159(9) Uani 1 1 d . . . C16 C 0.40654(16) 0.2882(5) 0.79401(13) 0.0146(8) Uani 1 1 d . . . H16 H 0.4219 0.3796 0.8035 0.017 Uiso 1 1 calc R . . C17 C 0.37553(16) 0.2778(5) 0.75550(12) 0.0133(8) Uani 1 1 d . . . C18 C 0.33884(18) -0.1274(5) 0.75262(14) 0.0175(9) Uani 1 1 d . . . H18A H 0.3035 -0.1128 0.7360 0.026 Uiso 1 1 calc R . . H18B H 0.3389 -0.1873 0.7749 0.026 Uiso 1 1 calc R . . H18C H 0.3583 -0.1776 0.7381 0.026 Uiso 1 1 calc R . . C19 C 0.4478(2) 0.1808(6) 0.86008(14) 0.0244(10) Uani 1 1 d . . . H19A H 0.4730 0.1011 0.8664 0.037 Uiso 1 1 calc R . . H19B H 0.4260 0.1740 0.8766 0.037 Uiso 1 1 calc R . . H19C H 0.4656 0.2754 0.8643 0.037 Uiso 1 1 calc R . . C20 C 0.36409(18) 0.4157(5) 0.73125(13) 0.0185(9) Uani 1 1 d . . . H20A H 0.3567 0.3898 0.7040 0.028 Uiso 1 1 calc R . . H20B H 0.3938 0.4812 0.7392 0.028 Uiso 1 1 calc R . . H20C H 0.3344 0.4655 0.7348 0.028 Uiso 1 1 calc R . . C21 C 0.16647(15) 0.1827(4) 0.56428(12) 0.0106(8) Uani 1 1 d . . . C22 C 0.14684(16) 0.2411(4) 0.59438(12) 0.0113(8) Uani 1 1 d . . . C23 C 0.13918(16) 0.1742(5) 0.52228(12) 0.0126(8) Uani 1 1 d . . . C24 C 0.09859(16) 0.0754(5) 0.50742(13) 0.0162(9) Uani 1 1 d . . . C25 C 0.07809(18) 0.0594(6) 0.46756(13) 0.0220(10) Uani 1 1 d . . . H25 H 0.0504 -0.0064 0.4574 0.026 Uiso 1 1 calc R . . C26 C 0.09684(19) 0.1364(6) 0.44233(14) 0.0241(10) Uani 1 1 d . . . C27 C 0.13676(18) 0.2356(5) 0.45779(14) 0.0202(10) Uani 1 1 d . . . H27 H 0.1497 0.2903 0.4408 0.024 Uiso 1 1 calc R . . C28 C 0.15791(16) 0.2564(5) 0.49692(13) 0.0143(8) Uani 1 1 d . . . C29 C 0.07782(18) -0.0178(6) 0.53316(14) 0.0217(10) Uani 1 1 d . . . H29A H 0.1063 -0.0580 0.5542 0.033 Uiso 1 1 calc R . . H29B H 0.0575 -0.0983 0.5181 0.033 Uiso 1 1 calc R . . H29C H 0.0562 0.0426 0.5439 0.033 Uiso 1 1 calc R . . C30 C 0.0775(2) 0.1107(8) 0.39953(15) 0.0377(14) Uani 1 1 d . . . H30A H 0.0701 0.2051 0.3861 0.057 Uiso 1 1 calc R . . H30B H 0.0462 0.0516 0.3930 0.057 Uiso 1 1 calc R . . H30C H 0.1036 0.0586 0.3916 0.057 Uiso 1 1 calc R . . C31 C 0.20036(18) 0.3670(5) 0.51102(15) 0.0195(9) Uani 1 1 d . . . H31A H 0.2155 0.3586 0.5390 0.029 Uiso 1 1 calc R . . H31B H 0.1866 0.4661 0.5044 0.029 Uiso 1 1 calc R . . H31C H 0.2266 0.3483 0.4988 0.029 Uiso 1 1 calc R . . C32 C 0.09337(16) 0.2894(4) 0.58766(12) 0.0106(8) Uani 1 1 d . . . C33 C 0.06349(16) 0.2121(5) 0.60663(12) 0.0130(8) Uani 1 1 d . . . C34 C 0.01348(16) 0.2565(5) 0.60097(13) 0.0149(8) Uani 1 1 d . . . H34 H -0.0064 0.2049 0.6138 0.018 Uiso 1 1 calc R . . C35 C -0.00868(17) 0.3742(5) 0.57717(14) 0.0180(9) Uani 1 1 d . . . C36 C 0.02121(17) 0.4472(5) 0.55863(13) 0.0161(9) Uani 1 1 d . . . H36 H 0.0065 0.5260 0.5418 0.019 Uiso 1 1 calc R . . C37 C 0.07169(16) 0.4092(5) 0.56384(12) 0.0126(8) Uani 1 1 d . . . C38 C 0.08423(17) 0.0827(5) 0.63214(14) 0.0174(9) Uani 1 1 d . . . H38A H 0.1014 0.0162 0.6192 0.026 Uiso 1 1 calc R . . H38B H 0.0561 0.0309 0.6375 0.026 Uiso 1 1 calc R . . H38C H 0.1087 0.1166 0.6564 0.026 Uiso 1 1 calc R . . C39 C -0.06263(18) 0.4211(7) 0.57218(17) 0.0293(12) Uani 1 1 d . . . H39A H -0.0661 0.5266 0.5668 0.044 Uiso 1 1 calc R . . H39B H -0.0708 0.4000 0.5958 0.044 Uiso 1 1 calc R . . H39C H -0.0862 0.3672 0.5506 0.044 Uiso 1 1 calc R . . C40 C 0.10209(17) 0.4991(5) 0.54447(14) 0.0186(9) Uani 1 1 d . . . H40A H 0.1386 0.4814 0.5571 0.028 Uiso 1 1 calc R . . H40B H 0.0946 0.6034 0.5464 0.028 Uiso 1 1 calc R . . H40C H 0.0928 0.4712 0.5173 0.028 Uiso 1 1 calc R . . C41 C 0.21276(15) -0.0766(5) 0.67424(13) 0.0145(8) Uani 1 1 d . . . H41 H 0.2150 -0.0015 0.6927 0.017 Uiso 1 1 calc R . . C42 C 0.20212(17) -0.2188(5) 0.68288(14) 0.0183(9) Uani 1 1 d . . . H42 H 0.1977 -0.2406 0.7070 0.022 Uiso 1 1 calc R . . C43 C 0.19808(17) -0.3288(5) 0.65584(15) 0.0199(9) Uani 1 1 d . . . H43 H 0.1912 -0.4272 0.6612 0.024 Uiso 1 1 calc R . . C44 C 0.20437(17) -0.2917(5) 0.62092(14) 0.0181(9) Uani 1 1 d . . . H44 H 0.2012 -0.3642 0.6017 0.022 Uiso 1 1 calc R . . C45 C 0.21531(16) -0.1478(5) 0.61439(13) 0.0139(8) Uani 1 1 d . . . H45 H 0.2197 -0.1232 0.5904 0.017 Uiso 1 1 calc R . . C46 C 0.1983(2) -0.1252(6) 0.48756(16) 0.0282(11) Uani 1 1 d . . . H46A H 0.2355 -0.1167 0.5009 0.034 Uiso 1 1 calc R . . H46B H 0.1833 -0.0256 0.4855 0.034 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0075(3) 0.0082(3) 0.0082(3) -0.00005(19) 0.0032(2) 0.00012(18) Br1 0.0292(3) 0.0217(3) 0.0308(3) 0.0007(2) 0.0078(2) -0.00143(19) Cl1 0.0405(8) 0.0294(7) 0.0333(7) 0.0017(6) 0.0150(6) -0.0030(5) Cl2 0.0529(10) 0.0638(11) 0.0307(8) -0.0119(7) 0.0178(7) -0.0041(8) O1 0.0123(14) 0.0187(15) 0.0112(15) -0.0023(12) 0.0046(12) 0.0056(11) O2 0.0104(13) 0.0196(15) 0.0075(14) -0.0014(11) 0.0032(11) 0.0039(11) O3 0.0105(14) 0.0182(15) 0.0106(14) -0.0009(12) 0.0059(11) 0.0031(11) O4 0.0148(14) 0.0168(15) 0.0088(14) -0.0033(11) 0.0061(11) 0.0037(11) N1 0.0124(16) 0.0077(15) 0.0114(16) -0.0027(13) 0.0059(13) -0.0015(12) N2 0.0094(15) 0.0105(16) 0.0114(17) -0.0014(13) 0.0065(13) -0.0020(12) N3 0.0116(16) 0.0100(16) 0.0101(17) 0.0013(13) 0.0058(13) -0.0006(12) N4 0.0147(17) 0.0104(16) 0.0087(16) 0.0002(13) 0.0059(13) 0.0014(13) N5 0.0076(15) 0.0079(15) 0.0089(16) 0.0026(12) 0.0002(12) 0.0024(11) C1 0.0115(18) 0.0079(18) 0.012(2) -0.0003(14) 0.0049(15) -0.0003(14) C2 0.0121(18) 0.0092(18) 0.0109(19) -0.0020(15) 0.0061(15) -0.0021(14) C3 0.0074(18) 0.016(2) 0.0091(19) 0.0002(15) 0.0015(14) 0.0014(15) C4 0.0106(19) 0.020(2) 0.0086(19) 0.0000(16) 0.0028(15) -0.0018(16) C5 0.0091(19) 0.031(3) 0.015(2) 0.0033(19) 0.0047(16) 0.0015(17) C6 0.015(2) 0.027(2) 0.013(2) 0.0032(18) 0.0061(17) 0.0076(18) C7 0.022(2) 0.021(2) 0.013(2) 0.0018(17) 0.0077(18) 0.0075(18) C8 0.014(2) 0.017(2) 0.011(2) 0.0005(16) 0.0039(16) 0.0020(16) C9 0.014(2) 0.021(2) 0.019(2) 0.0004(18) 0.0071(17) -0.0033(16) C10 0.018(2) 0.040(3) 0.029(3) 0.008(2) 0.009(2) 0.014(2) C11 0.021(2) 0.011(2) 0.020(2) -0.0038(17) 0.0033(18) 0.0016(16) C12 0.0088(18) 0.016(2) 0.013(2) -0.0009(16) 0.0045(15) -0.0007(15) C13 0.0087(18) 0.015(2) 0.017(2) 0.0010(16) 0.0070(16) 0.0023(15) C14 0.0123(19) 0.017(2) 0.015(2) 0.0046(16) 0.0071(16) 0.0060(15) C15 0.0124(19) 0.020(2) 0.014(2) 0.0010(17) 0.0036(16) 0.0025(16) C16 0.0131(19) 0.015(2) 0.015(2) -0.0039(16) 0.0039(16) -0.0024(15) C17 0.015(2) 0.013(2) 0.012(2) -0.0011(16) 0.0059(16) -0.0006(15) C18 0.021(2) 0.014(2) 0.018(2) 0.0036(17) 0.0065(18) -0.0026(16) C19 0.027(3) 0.028(3) 0.012(2) -0.0012(19) -0.0017(19) -0.001(2) C20 0.023(2) 0.016(2) 0.014(2) -0.0002(17) 0.0023(18) -0.0015(17) C21 0.0136(19) 0.0090(18) 0.0112(19) 0.0030(15) 0.0067(15) -0.0006(14) C22 0.0152(19) 0.0095(18) 0.011(2) 0.0035(15) 0.0074(16) -0.0005(15) C23 0.0150(19) 0.016(2) 0.0079(19) 0.0035(15) 0.0048(15) 0.0045(15) C24 0.0109(19) 0.021(2) 0.017(2) 0.0042(18) 0.0054(16) 0.0038(16) C25 0.015(2) 0.035(3) 0.013(2) -0.003(2) 0.0011(17) 0.0012(19) C26 0.023(2) 0.034(3) 0.013(2) 0.002(2) 0.0032(19) 0.008(2) C27 0.024(2) 0.024(2) 0.015(2) 0.0098(18) 0.0095(19) 0.0099(18) C28 0.015(2) 0.014(2) 0.016(2) 0.0065(16) 0.0082(17) 0.0061(16) C29 0.017(2) 0.028(3) 0.021(2) 0.001(2) 0.0068(18) -0.0096(18) C30 0.033(3) 0.066(4) 0.009(2) 0.003(3) 0.000(2) 0.006(3) C31 0.019(2) 0.019(2) 0.025(3) 0.0065(18) 0.0136(19) -0.0003(17) C32 0.0131(19) 0.0109(18) 0.0075(18) 0.0019(15) 0.0029(15) 0.0011(15) C33 0.0115(19) 0.016(2) 0.012(2) 0.0000(16) 0.0040(16) -0.0008(15) C34 0.014(2) 0.019(2) 0.014(2) 0.0005(17) 0.0065(17) -0.0007(16) C35 0.012(2) 0.023(2) 0.018(2) -0.0009(18) 0.0019(17) 0.0047(16) C36 0.016(2) 0.016(2) 0.015(2) 0.0005(17) 0.0020(17) 0.0034(16) C37 0.0124(19) 0.0116(19) 0.012(2) 0.0017(16) 0.0019(16) -0.0005(15) C38 0.015(2) 0.020(2) 0.021(2) 0.0099(18) 0.0105(18) 0.0052(17) C39 0.011(2) 0.041(3) 0.034(3) 0.003(2) 0.003(2) 0.008(2) C40 0.019(2) 0.015(2) 0.021(2) 0.0077(18) 0.0064(18) 0.0021(17) C41 0.0103(19) 0.019(2) 0.014(2) 0.0022(17) 0.0032(16) 0.0001(16) C42 0.015(2) 0.021(2) 0.021(2) 0.0075(18) 0.0080(18) 0.0008(17) C43 0.015(2) 0.014(2) 0.031(3) 0.0034(19) 0.0075(19) -0.0032(16) C44 0.014(2) 0.015(2) 0.022(2) -0.0014(18) -0.0001(17) -0.0030(16) C45 0.0108(19) 0.016(2) 0.013(2) 0.0005(16) 0.0009(16) -0.0017(15) C46 0.027(3) 0.032(3) 0.028(3) -0.007(2) 0.011(2) -0.001(2) 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 Co1 N3 1.888(4) . yes Co1 N4 1.891(3) . yes Co1 N2 1.908(3) . yes Co1 N1 1.908(4) . yes Co1 N5 1.986(4) . yes Co1 Br1 2.3396(12) . yes Cl1 C46 1.744(6) . ? Cl2 C46 1.761(6) . ? O1 N1 1.339(4) . ? O2 N2 1.335(4) . ? O3 N3 1.331(4) . ? O4 N4 1.334(4) . ? N1 C1 1.297(5) . yes N2 C2 1.298(5) . yes N3 C21 1.307(5) . yes N4 C22 1.307(5) . yes N5 C41 1.339(5) . ? N5 C45 1.347(6) . ? C1 C12 1.479(6) . ? C1 C2 1.484(6) . yes C2 C3 1.484(5) . ? C3 C4 1.406(6) . ? C3 C8 1.413(6) . ? C4 C5 1.390(6) . ? C4 C9 1.509(6) . ? C5 C6 1.402(7) . ? C6 C7 1.373(7) . ? C6 C10 1.511(6) . ? C7 C8 1.386(6) . ? C8 C11 1.505(6) . ? C12 C17 1.402(6) . ? C12 C13 1.408(6) . ? C13 C14 1.378(6) . ? C13 C18 1.505(6) . ? C14 C15 1.391(6) . ? C15 C16 1.385(6) . ? C15 C19 1.505(6) . ? C16 C17 1.401(6) . ? C17 C20 1.513(6) . ? C21 C22 1.473(6) . yes C21 C23 1.484(6) . ? C22 C32 1.483(6) . ? C23 C24 1.405(6) . ? C23 C28 1.412(6) . ? C24 C25 1.395(6) . ? C24 C29 1.510(6) . ? C25 C26 1.384(7) . ? C26 C27 1.398(7) . ? C26 C30 1.505(7) . ? C27 C28 1.378(7) . ? C28 C31 1.507(6) . ? C32 C37 1.407(6) . ? C32 C33 1.422(6) . ? C33 C34 1.388(6) . ? C33 C38 1.501(6) . ? C34 C35 1.395(6) . ? C35 C36 1.392(7) . ? C35 C39 1.502(6) . ? C36 C37 1.388(6) . ? C37 C40 1.501(6) . ? C41 C42 1.388(6) . ? C42 C43 1.388(7) . ? C43 C44 1.385(7) . ? C44 C45 1.384(6) . ?