# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email Catherine.Housecroft@unibas.ch _publ_contact_author_name 'Catherine Housecroft' loop_ _publ_author_name 'Catherine Housecroft' 'Edwin Constable' 'Guoqi Zhang' 'Jennifer Zampese' 'Markus Neuburger' 'Srboljub Vujovic' data_GQ214 _database_code_depnum_ccdc_archive 'CCDC 856244' #TrackingRef '- GQ214.cif' _audit_creation_date 11-02-09 _audit_creation_method CRYSTALS_ver_14.09 _oxford_structure_analysis_title 'gq214_123k_0ma in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 23.3334(7) _cell_length_b 10.3868(3) _cell_length_c 17.3827(6) _cell_angle_alpha 90 _cell_angle_beta 109.477(2) _cell_angle_gamma 90 _cell_volume 3971.8(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H26 Co2 N14 O2 S4 # Dc = 1.64 Fooo = 1732.00 Mu = 11.04 M = 980.87 # Found Formula = C40 H34 Co1 N12 O2 S2 # Dc = 1.40 FOOO = 1732.00 Mu = 5.90 M = 837.85 _chemical_formula_sum 'C40 H34 Co1 N12 O2 S2' _chemical_formula_moiety 'C38 H26 Co N12 S2, 2(C H4 O)' _chemical_compound_source ? _chemical_formula_weight 837.85 _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 3 _cell_measurement_theta_max 35 _cell_measurement_temperature 123 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_max 0.230 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.590 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 102487 _reflns_number_total 17451 _diffrn_reflns_av_R_equivalents 0.056 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17451 # Theoretical number of reflections is about 35025 _diffrn_reflns_theta_min 1.851 _diffrn_reflns_theta_max 35.018 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 35.018 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -37 _reflns_limit_h_max 35 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 1.41 _oxford_diffrn_Wilson_scale 691.40 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.82 _refine_diff_density_max 1.56 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 9242 _refine_ls_number_restraints 479 _refine_ls_number_parameters 678 _oxford_refine_ls_R_factor_ref 0.0548 _refine_ls_wR_factor_ref 0.0560 _refine_ls_goodness_of_fit_ref 1.0536 _refine_ls_shift/su_max 0.0057614 _refine_ls_shift/su_mean 0.0002323 # The values computed from all data _oxford_reflns_number_all 17423 _refine_ls_R_factor_all 0.1092 _refine_ls_wR_factor_all 0.1443 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12290 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_gt 0.0669 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.276 0.297 0.997E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co 0.249302(13) 0.72509(3) 0.248941(19) 0.0172 1.0000 Uani D U . . . . N1 N 0.20371(9) 0.8785(2) 0.18012(13) 0.0264 1.0000 Uani . . . . . . N2 N 0.29591(9) 0.5749(2) 0.32023(14) 0.0247 1.0000 Uani . . . . . . N3 N 0.30312(8) 0.70902(19) 0.16550(12) 0.0189 1.0000 Uani . . . . . . N4 N 0.49230(8) 0.62987(19) 0.09461(11) 0.0172 1.0000 Uani . . . . . . N5 N 0.68048(8) 0.35947(19) 0.17957(11) 0.0185 1.0000 Uani . . . . . . N6 N 0.52777(9) 0.8713(2) -0.14480(13) 0.0260 1.0000 Uani . . . . . . N7 N 0.46642(9) 1.0371(2) -0.19151(12) 0.0236 1.0000 Uani . . . . . . N11 N -0.02980(9) 0.5924(2) 0.65145(13) 0.0255 1.0000 Uani . . . . . . N12 N 0.03655(10) 0.4417(2) 0.71046(14) 0.0283 1.0000 Uani . . . . . . C1 C 0.19825(10) 0.9774(3) 0.14794(16) 0.0269 1.0000 Uani . . . . . . C2 C 0.30621(10) 0.5008(2) 0.37344(16) 0.0227 1.0000 Uani . . . . . . C3 C 0.31686(10) 0.8162(2) 0.13205(15) 0.0216 1.0000 Uani . . . . . . C4 C 0.36254(10) 0.8219(2) 0.09790(15) 0.0217 1.0000 Uani . . . . . . C5 C 0.39628(9) 0.7121(2) 0.09653(13) 0.0176 1.0000 Uani . . . . . . C6 C 0.38082(10) 0.5995(2) 0.12820(14) 0.0218 1.0000 Uani . . . . . . C7 C 0.33455(10) 0.6022(2) 0.16207(15) 0.0223 1.0000 Uani . . . . . . C8 C 0.44718(9) 0.7158(2) 0.06350(13) 0.0164 1.0000 Uani . . . . . . C9 C 0.44691(9) 0.8038(2) 0.00330(13) 0.0176 1.0000 Uani . . . . . . C10 C 0.49445(9) 0.8041(2) -0.02833(13) 0.0154 1.0000 Uani . . . . . . C11 C 0.54206(9) 0.7172(2) 0.00473(13) 0.0175 1.0000 Uani . . . . . . C12 C 0.53932(9) 0.6333(2) 0.06616(13) 0.0166 1.0000 Uani . . . . . . C13 C 0.62233(9) 0.3399(2) 0.17433(14) 0.0192 1.0000 Uani . . . . . . C14 C 0.57624(9) 0.4270(2) 0.13934(13) 0.0186 1.0000 Uani . . . . . . C15 C 0.58869(9) 0.5396(2) 0.10424(13) 0.0177 1.0000 Uani . . . . . . C16 C 0.64886(10) 0.5584(3) 0.10838(16) 0.0259 1.0000 Uani . . . . . . C17 C 0.69258(10) 0.4676(3) 0.14667(16) 0.0269 1.0000 Uani . . . . . . C18 C 0.49215(9) 0.8893(2) -0.09603(13) 0.0181 1.0000 Uani . . . . . . C19 C 0.51030(12) 0.9616(3) -0.20135(16) 0.0304 1.0000 Uani . . . . . . C20 C 0.45377(10) 0.9921(2) -0.12487(14) 0.0201 1.0000 Uani . . . . . . C28 C 0.01220(7) 0.66796(19) 0.54382(11) 0.0198 1.0000 Uani D U . . . . C36 C 0.01331(9) 0.5844(2) 0.61253(14) 0.0194 1.0000 Uani . . . . . . C37 C -0.01369(12) 0.5055(3) 0.70939(17) 0.0300 1.0000 Uani . . . . . . C38 C 0.05418(10) 0.4904(2) 0.64899(15) 0.0235 1.0000 Uani . . . . . . S1 S 0.18902(4) 1.11240(9) 0.09923(8) 0.0640 1.0000 Uani . . . . . . S2 S 0.32120(3) 0.40155(7) 0.44984(5) 0.0358 1.0000 Uani . . . . . . H1 H 0.4477 1.0980 -0.2238 0.0293 1.0000 Uiso R . . . . . H2 H 0.0561 0.3841 0.7460 0.0354 1.0000 Uiso R . . . . . H21 H 0.2947 0.8899 0.1322 0.0272 1.0000 Uiso R . . . . . H41 H 0.3702 0.8988 0.0756 0.0278 1.0000 Uiso R . . . . . H61 H 0.4014 0.5218 0.1274 0.0278 1.0000 Uiso R . . . . . H71 H 0.3244 0.5257 0.1838 0.0277 1.0000 Uiso R . . . . . H91 H 0.4146 0.8604 -0.0161 0.0219 1.0000 Uiso R . . . . . H111 H 0.5746 0.7142 -0.0150 0.0222 1.0000 Uiso R . . . . . H131 H 0.6133 0.2630 0.1956 0.0237 1.0000 Uiso R . . . . . H141 H 0.5368 0.4098 0.1394 0.0228 1.0000 Uiso R . . . . . H161 H 0.6596 0.6306 0.0863 0.0319 1.0000 Uiso R . . . . . H171 H 0.7324 0.4828 0.1511 0.0344 1.0000 Uiso R . . . . . H191 H 0.5261 0.9728 -0.2428 0.0368 1.0000 Uiso R . . . . . H201 H 0.4246 1.0266 -0.1047 0.0250 1.0000 Uiso R . . . . . H371 H -0.0343 0.4888 0.7461 0.0374 1.0000 Uiso R . . . . . H381 H 0.0874 0.4620 0.6360 0.0290 1.0000 Uiso R . . . . . N8 N 0.19139(9) 0.7438(3) 0.32732(12) 0.0206 0.757(3) Uani D U P 1 1 . N9 N 0.00771(11) 0.8175(3) 0.40856(18) 0.0205 0.757(3) Uani D U P 1 1 . N10 N -0.18256(10) 1.07734(19) 0.31863(10) 0.0207 0.757(3) Uani D U P 1 1 . C21 C 0.20537(10) 0.7017(3) 0.40442(13) 0.0220 0.757(3) Uani D U P 1 1 . C22 C 0.16272(9) 0.6983(4) 0.44464(15) 0.0249 0.757(3) Uani D U P 1 1 . C23 C 0.10337(9) 0.7378(3) 0.40472(13) 0.0203 0.757(3) Uani D U P 1 1 . C24 C 0.08929(10) 0.7794(3) 0.32503(13) 0.0234 0.757(3) Uani D U P 1 1 . C25 C 0.13382(9) 0.7783(3) 0.28688(14) 0.0232 0.757(3) Uani D U P 1 1 . C26 C 0.05499(10) 0.7396(3) 0.44277(16) 0.0196 0.757(3) Uani D U P 1 1 . C27 C 0.05855(12) 0.6617(3) 0.50996(18) 0.0190 0.757(3) Uani D U P 1 1 . C29 C -0.03614(12) 0.7520(3) 0.50948(19) 0.0217 0.757(3) Uani D U P 1 1 . C30 C -0.03649(11) 0.8244(3) 0.44141(16) 0.0198 0.757(3) Uani D U P 1 1 . C31 C -0.16090(11) 0.9921(2) 0.27726(13) 0.0223 0.757(3) Uani D U P 1 1 . C32 C -0.11343(11) 0.9085(3) 0.31619(12) 0.0206 0.757(3) Uani D U P 1 1 . C33 C -0.08876(11) 0.9100(3) 0.40057(12) 0.0204 0.757(3) Uani D U P 1 1 . C34 C -0.11422(11) 0.9897(3) 0.44405(13) 0.0237 0.757(3) Uani D U P 1 1 . C35 C -0.16152(11) 1.0730(3) 0.40050(11) 0.0233 0.757(3) Uani D U P 1 1 . H211 H 0.2450 0.6747 0.4329 0.0258 0.757(3) Uiso R . P 1 1 . H221 H 0.1746 0.6686 0.4979 0.0290 0.757(3) Uiso R . P 1 1 . H241 H 0.0499 0.8076 0.2956 0.0280 0.757(3) Uiso R . P 1 1 . H251 H 0.1227 0.8020 0.2308 0.0271 0.757(3) Uiso R . P 1 1 . H271 H 0.0917 0.6050 0.5311 0.0240 0.757(3) Uiso R . P 1 1 . H291 H -0.0675 0.7604 0.5306 0.0262 0.757(3) Uiso R . P 1 1 . H311 H -0.1785 0.9895 0.2199 0.0270 0.757(3) Uiso R . P 1 1 . H321 H -0.0993 0.8508 0.2852 0.0244 0.757(3) Uiso R . P 1 1 . H341 H -0.1008 0.9878 0.5004 0.0283 0.757(3) Uiso R . P 1 1 . H351 H -0.1778 1.1286 0.4299 0.0273 0.757(3) Uiso R . P 1 1 . N108 N 0.1947(3) 0.7523(6) 0.3312(4) 0.0222 0.243(3) Uani D U P 1 2 . N109 N 0.0120(3) 0.8363(7) 0.4188(5) 0.0267 0.243(3) Uani D U P 1 2 . N110 N -0.17344(19) 1.1104(6) 0.3343(3) 0.0220 0.243(3) Uani D U P 1 2 . C121 C 0.1891(3) 0.6541(6) 0.3785(4) 0.0251 0.243(3) Uani D U P 1 2 . C122 C 0.1453(3) 0.6505(6) 0.4169(4) 0.0235 0.243(3) Uani D U P 1 2 . C123 C 0.1065(2) 0.7542(6) 0.4101(4) 0.0230 0.243(3) Uani D U P 1 2 . C124 C 0.1126(3) 0.8566(5) 0.3627(4) 0.0228 0.243(3) Uani D U P 1 2 . C125 C 0.1578(3) 0.8539(6) 0.3254(4) 0.0237 0.243(3) Uani D U P 1 2 . C126 C 0.0579(2) 0.7532(6) 0.4479(4) 0.0234 0.243(3) Uani D U P 1 2 . C127 C 0.0588(3) 0.6668(8) 0.5102(5) 0.0215 0.243(3) Uani D U P 1 2 . C129 C -0.0345(3) 0.7571(7) 0.5118(5) 0.0243 0.243(3) Uani D U P 1 2 . C130 C -0.0340(2) 0.8400(6) 0.4483(4) 0.0265 0.243(3) Uani D U P 1 2 . C131 C -0.1161(2) 1.1289(5) 0.3360(4) 0.0235 0.243(3) Uani D U P 1 2 . C132 C -0.0687(2) 1.0458(5) 0.3757(4) 0.0242 0.243(3) Uani D U P 1 2 . C133 C -0.0828(2) 0.9360(5) 0.4112(4) 0.0282 0.243(3) Uani D U P 1 2 . C134 C -0.1428(2) 0.9140(6) 0.4041(5) 0.0323 0.243(3) Uani D U P 1 2 . C135 C -0.1891(2) 1.0023(6) 0.3647(4) 0.0327 0.243(3) Uani D U P 1 2 . H1211 H 0.2163 0.5857 0.3873 0.0331 0.243(3) Uiso R . P 1 2 . H1221 H 0.1422 0.5785 0.4472 0.0320 0.243(3) Uiso R . P 1 2 . H1241 H 0.0870 0.9273 0.3557 0.0320 0.243(3) Uiso R . P 1 2 . H1251 H 0.1617 0.9254 0.2949 0.0320 0.243(3) Uiso R . P 1 2 . H1271 H 0.0909 0.6085 0.5293 0.0270 0.243(3) Uiso R . P 1 2 . H1291 H -0.0663 0.7617 0.5325 0.0321 0.243(3) Uiso R . P 1 2 . H1311 H -0.1079 1.2001 0.3098 0.0350 0.243(3) Uiso R . P 1 2 . H1321 H -0.0290 1.0636 0.3781 0.0351 0.243(3) Uiso R . P 1 2 . H1341 H -0.1526 0.8394 0.4270 0.0451 0.243(3) Uiso R . P 1 2 . H1351 H -0.2296 0.9858 0.3591 0.0452 0.243(3) Uiso R . P 1 2 . C39 C 0.34484(15) 1.2685(3) -0.3171(3) 0.0487 1.0000 Uani . . . . . . O1 O 0.39965(9) 1.20387(19) -0.31140(13) 0.0324 1.0000 Uani . . . . . . H3 H 0.4221 1.2451 -0.3295 0.0510 1.0000 Uiso R . . . . . H391 H 0.3536 1.3536 -0.2943 0.0776 1.0000 Uiso R . . . . . H392 H 0.3240 1.2209 -0.2862 0.0769 1.0000 Uiso R . . . . . H393 H 0.3202 1.2720 -0.3733 0.0776 1.0000 Uiso R . . . . . O2 O 0.10347(10) 0.2870(2) 0.83686(14) 0.0436 1.0000 Uani D U . . . . H4 H 0.0803 0.2273 0.8380 0.0667 1.0000 Uiso R . . . . . C40 C 0.16785(11) 0.2719(5) 0.8805(3) 0.0549 0.789(8) Uani D U P 2 1 . H401 H 0.1831 0.3570 0.9107 0.0894 0.789(8) Uiso R . P 2 1 . H402 H 0.1740 0.1997 0.9189 0.0895 0.789(8) Uiso R . P 2 1 . H403 H 0.1874 0.2548 0.8386 0.0892 0.789(8) Uiso R . P 2 1 . C140 C 0.1511(6) 0.2204(16) 0.8164(12) 0.0532 0.211(8) Uani D U P 2 2 . H1401 H 0.1794 0.2829 0.8093 0.0740 0.211(8) Uiso R . P 2 2 . H1402 H 0.1721 0.1608 0.8587 0.0739 0.211(8) Uiso R . P 2 2 . H1403 H 0.1342 0.1739 0.7664 0.0739 0.211(8) Uiso R . P 2 2 . 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 0.00985(10) 0.02551(15) 0.01767(13) 0.00028(12) 0.00634(9) -0.00101(11) N1 0.0146(8) 0.0404(13) 0.0263(10) 0.0089(9) 0.0095(7) 0.0047(8) N2 0.0180(8) 0.0256(10) 0.0331(11) 0.0013(9) 0.0120(8) 0.0016(7) N3 0.0145(7) 0.0235(10) 0.0215(9) 0.0004(7) 0.0095(6) 0.0006(7) N4 0.0144(7) 0.0215(9) 0.0174(8) -0.0009(7) 0.0075(6) 0.0014(6) N5 0.0134(7) 0.0239(9) 0.0190(9) -0.0014(7) 0.0061(6) -0.0003(7) N6 0.0239(9) 0.0359(12) 0.0226(10) 0.0066(9) 0.0138(8) 0.0054(8) N7 0.0222(9) 0.0266(10) 0.0210(9) 0.0060(8) 0.0057(7) -0.0003(8) N11 0.0229(9) 0.0308(11) 0.0269(10) -0.0014(9) 0.0137(8) -0.0002(8) N12 0.0274(10) 0.0271(11) 0.0328(11) 0.0061(9) 0.0132(9) -0.0012(8) C1 0.0122(9) 0.0361(14) 0.0319(13) 0.0024(11) 0.0068(8) -0.0022(9) C2 0.0138(8) 0.0209(11) 0.0327(12) -0.0062(10) 0.0068(8) -0.0010(8) C3 0.0192(9) 0.0225(11) 0.0271(11) 0.0025(9) 0.0131(8) 0.0035(8) C4 0.0206(9) 0.0238(11) 0.0259(11) 0.0021(9) 0.0146(8) 0.0010(8) C5 0.0133(8) 0.0257(11) 0.0148(9) -0.0001(8) 0.0061(7) 0.0011(8) C6 0.0189(9) 0.0250(11) 0.0244(11) 0.0026(9) 0.0112(8) 0.0042(8) C7 0.0200(9) 0.0237(11) 0.0272(11) 0.0029(9) 0.0133(8) 0.0010(8) C8 0.0137(8) 0.0199(10) 0.0172(9) -0.0034(8) 0.0072(7) -0.0006(7) C9 0.0156(8) 0.0208(10) 0.0181(9) -0.0004(8) 0.0080(7) 0.0018(7) C10 0.0134(8) 0.0180(10) 0.0159(9) -0.0021(7) 0.0065(7) -0.0019(7) C11 0.0135(8) 0.0223(10) 0.0184(9) -0.0022(8) 0.0078(7) -0.0006(8) C12 0.0119(8) 0.0196(10) 0.0191(10) -0.0011(8) 0.0062(7) -0.0003(7) C13 0.0142(8) 0.0212(11) 0.0221(10) -0.0021(8) 0.0058(7) -0.0027(8) C14 0.0129(8) 0.0233(11) 0.0194(10) -0.0025(8) 0.0053(7) -0.0011(7) C15 0.0146(8) 0.0233(11) 0.0169(9) -0.0016(8) 0.0075(7) 0.0002(8) C16 0.0176(9) 0.0294(12) 0.0337(13) 0.0087(10) 0.0124(9) 0.0021(9) C17 0.0148(9) 0.0321(13) 0.0365(13) 0.0100(11) 0.0122(9) 0.0035(9) C18 0.0151(8) 0.0229(11) 0.0173(10) -0.0010(8) 0.0068(7) -0.0028(8) C19 0.0297(12) 0.0418(15) 0.0244(12) 0.0102(11) 0.0151(10) 0.0062(11) C20 0.0177(9) 0.0204(10) 0.0229(11) -0.0013(9) 0.0076(8) -0.0029(8) C28 0.0151(8) 0.0252(10) 0.0204(9) -0.0036(8) 0.0075(7) -0.0019(7) C36 0.0157(8) 0.0229(11) 0.0207(10) -0.0037(8) 0.0076(7) -0.0033(8) C37 0.0309(12) 0.0328(14) 0.0319(13) 0.0027(11) 0.0178(10) -0.0013(10) C38 0.0202(9) 0.0233(11) 0.0298(12) -0.0006(9) 0.0123(9) -0.0038(8) S1 0.0330(4) 0.0442(5) 0.1143(9) 0.0415(6) 0.0237(5) 0.0008(3) S2 0.0404(4) 0.0233(3) 0.0360(4) 0.0045(3) 0.0025(3) 0.0035(3) N8 0.0131(10) 0.0298(14) 0.0209(11) 0.0051(11) 0.0082(8) 0.0036(11) N9 0.0125(11) 0.0346(15) 0.0159(13) 0.0011(12) 0.0067(9) 0.0033(10) N10 0.0130(9) 0.0322(13) 0.0158(10) -0.0035(9) 0.0036(8) 0.0057(8) C21 0.0137(11) 0.0363(17) 0.0168(11) 0.0015(11) 0.0060(9) 0.0064(11) C22 0.0160(10) 0.0424(18) 0.0176(13) 0.0033(13) 0.0076(9) 0.0081(12) C23 0.0124(10) 0.0298(15) 0.0195(12) 0.0017(12) 0.0064(10) 0.0021(11) C24 0.0148(10) 0.0344(16) 0.0225(12) 0.0069(12) 0.0083(9) 0.0051(11) C25 0.0139(9) 0.0336(15) 0.0238(13) 0.0077(12) 0.0084(9) 0.0048(11) C26 0.0122(12) 0.0291(15) 0.0177(14) -0.0011(12) 0.0053(10) 0.0007(11) C27 0.0133(14) 0.0256(17) 0.0182(15) -0.0018(13) 0.0052(11) 0.0001(14) C29 0.0174(15) 0.0292(17) 0.0214(16) -0.0001(13) 0.0101(14) 0.0021(11) C30 0.0145(12) 0.0292(15) 0.0178(13) -0.0017(11) 0.0083(10) 0.0041(10) C31 0.0214(12) 0.0278(14) 0.0183(12) -0.0032(10) 0.0072(9) 0.0042(10) C32 0.0210(11) 0.0243(13) 0.0193(11) -0.0027(10) 0.0102(9) 0.0036(10) C33 0.0153(11) 0.0289(14) 0.0191(11) 0.0005(11) 0.0085(9) 0.0042(10) C34 0.0238(12) 0.0327(15) 0.0166(12) 0.0013(11) 0.0093(10) 0.0082(11) C35 0.0220(12) 0.0323(15) 0.0173(10) -0.0017(11) 0.0089(10) 0.0088(11) N108 0.013(3) 0.032(3) 0.025(3) 0.001(3) 0.0105(19) 0.003(3) N109 0.020(3) 0.035(4) 0.025(4) -0.005(3) 0.008(3) 0.008(3) N110 0.0149(19) 0.029(2) 0.023(2) -0.0061(16) 0.0077(15) 0.0097(15) C121 0.017(3) 0.031(4) 0.028(3) 0.002(3) 0.009(3) 0.002(3) C122 0.020(3) 0.026(3) 0.026(3) 0.002(3) 0.011(3) 0.002(3) C123 0.021(3) 0.027(3) 0.022(3) -0.001(3) 0.010(3) 0.004(3) C124 0.020(3) 0.027(3) 0.025(3) 0.000(3) 0.013(2) 0.004(3) C125 0.019(3) 0.029(3) 0.027(3) 0.003(3) 0.013(2) 0.004(3) C126 0.019(3) 0.031(4) 0.020(3) -0.005(3) 0.008(3) 0.005(3) C127 0.015(3) 0.029(4) 0.022(4) -0.006(3) 0.008(3) 0.003(4) C129 0.016(4) 0.032(4) 0.025(4) -0.006(3) 0.007(4) 0.003(2) C130 0.019(3) 0.036(4) 0.025(4) -0.004(3) 0.007(3) 0.004(3) C131 0.016(2) 0.030(3) 0.025(3) -0.002(3) 0.008(2) 0.004(2) C132 0.013(3) 0.033(3) 0.026(3) -0.002(3) 0.007(2) 0.003(2) C133 0.018(3) 0.037(3) 0.029(3) 0.002(3) 0.007(3) 0.003(2) C134 0.019(3) 0.039(4) 0.041(4) 0.012(3) 0.013(3) 0.008(3) C135 0.021(3) 0.039(3) 0.040(4) 0.007(3) 0.011(3) 0.011(3) C39 0.0373(15) 0.0404(17) 0.076(2) 0.0061(17) 0.0287(16) 0.0041(14) O1 0.0292(9) 0.0278(10) 0.0407(11) 0.0101(8) 0.0123(8) 0.0013(7) O2 0.0441(11) 0.0389(12) 0.0442(12) 0.0089(10) 0.0099(9) -0.0114(9) C40 0.0425(14) 0.062(3) 0.056(3) 0.007(2) 0.0111(17) -0.0132(19) C140 0.049(4) 0.052(5) 0.056(5) 0.005(4) 0.014(4) -0.007(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.05271(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . N5 3_655 2.1953(19) yes Co1 . N10 3_545 2.2228(10) yes Co1 . N1 . 2.063(2) yes Co1 . N2 . 2.062(2) yes Co1 . N3 . 2.2188(18) yes Co1 . N8 . 2.2242(10) yes Co1 . N5 3_655 2.1953(19) yes Co1 . N110 3_545 2.2225(11) yes Co1 . N1 . 2.063(2) yes Co1 . N2 . 2.062(2) yes Co1 . N3 . 2.2188(18) yes Co1 . N108 . 2.2278(11) yes N1 . C1 . 1.156(4) yes N2 . C2 . 1.165(3) yes N3 . C3 . 1.343(3) yes N3 . C7 . 1.342(3) yes N4 . C8 . 1.348(3) yes N4 . C12 . 1.346(3) yes N5 . C13 . 1.345(3) yes N5 . C17 . 1.333(3) yes N6 . C18 . 1.383(3) yes N6 . C19 . 1.321(3) yes N7 . C19 . 1.345(3) yes N7 . C20 . 1.369(3) yes N7 . H1 . 0.862 no N11 . C36 . 1.389(3) yes N11 . C37 . 1.311(4) yes N12 . C37 . 1.341(3) yes N12 . C38 . 1.364(3) yes N12 . H2 . 0.872 no C1 . S1 . 1.615(3) yes C2 . S2 . 1.624(3) yes C3 . C4 . 1.383(3) yes C3 . H21 . 0.925 no C4 . C5 . 1.390(3) yes C4 . H41 . 0.931 no C5 . C6 . 1.391(3) yes C5 . C8 . 1.482(3) yes C6 . C7 . 1.392(3) yes C6 . H61 . 0.941 no C7 . H71 . 0.944 no C8 . C9 . 1.388(3) yes C9 . C10 . 1.393(3) yes C9 . H91 . 0.926 no C10 . C11 . 1.398(3) yes C10 . C18 . 1.459(3) yes C11 . C12 . 1.396(3) yes C11 . H111 . 0.932 no C12 . C15 . 1.485(3) yes C13 . C14 . 1.382(3) yes C13 . H131 . 0.933 no C14 . C15 . 1.394(3) yes C14 . H141 . 0.937 no C15 . C16 . 1.395(3) yes C16 . C17 . 1.385(3) yes C16 . H161 . 0.915 no C17 . H171 . 0.920 no C18 . C20 . 1.376(3) yes C19 . H191 . 0.921 no C20 . H201 . 0.935 no C28 . C36 . 1.470(3) yes C28 . C27 . 1.3945(10) yes C28 . C29 . 1.3932(10) yes C28 . C36 . 1.470(3) yes C28 . C127 . 1.3955(11) yes C28 . C129 . 1.3957(11) yes C36 . C38 . 1.364(3) yes C37 . H371 . 0.935 no C38 . H381 . 0.925 no N8 . C21 . 1.3422(10) yes N8 . C25 . 1.3409(10) yes N9 . C26 . 1.3378(10) yes N9 . C30 . 1.3369(10) yes N10 . C31 . 1.3415(10) yes N10 . C35 . 1.3425(10) yes C21 . C22 . 1.3944(10) yes C21 . H211 . 0.935 no C22 . C23 . 1.3881(10) yes C22 . H221 . 0.926 no C23 . C24 . 1.3822(10) yes C23 . C26 . 1.4867(10) yes C24 . C25 . 1.4066(10) yes C24 . H241 . 0.938 no C25 . H251 . 0.953 no C26 . C27 . 1.4003(10) yes C27 . H271 . 0.944 no C29 . C30 . 1.3997(10) yes C29 . H291 . 0.926 no C30 . C33 . 1.4850(10) yes C31 . C32 . 1.3922(10) yes C31 . H311 . 0.944 no C32 . C33 . 1.3856(10) yes C32 . H321 . 0.936 no C33 . C34 . 1.3815(10) yes C34 . C35 . 1.4083(10) yes C34 . H341 . 0.924 no C35 . H351 . 0.931 no N108 . C121 . 1.3430(11) yes N108 . C125 . 1.3441(11) yes N109 . C126 . 1.3374(11) yes N109 . C130 . 1.3372(11) yes N110 . C131 . 1.3419(11) yes N110 . C135 . 1.3417(11) yes C121 . C122 . 1.3943(11) yes C121 . H1211 . 0.931 no C122 . C123 . 1.3866(11) yes C122 . H1221 . 0.932 no C123 . C124 . 1.3824(11) yes C123 . C126 . 1.4874(11) yes C124 . C125 . 1.4099(11) yes C124 . H1241 . 0.929 no C125 . H1251 . 0.934 no C126 . C127 . 1.4015(11) yes C127 . H1271 . 0.934 no C129 . C130 . 1.4018(11) yes C129 . H1291 . 0.929 no C130 . C133 . 1.4876(11) yes C131 . C132 . 1.3924(11) yes C131 . H1311 . 0.921 no C132 . C133 . 1.3871(11) yes C132 . H1321 . 0.931 no C133 . C134 . 1.3830(11) yes C134 . C135 . 1.4096(11) yes C134 . H1341 . 0.934 no C135 . H1351 . 0.932 no C39 . O1 . 1.419(4) yes C39 . H391 . 0.962 no C39 . H392 . 0.970 no C39 . H393 . 0.955 no O1 . H3 . 0.816 no O2 . H4 . 0.827 no O2 . C40 . 1.4478(11) yes O2 . H4 . 0.827 no O2 . C140 . 1.4505(11) yes C40 . H401 . 1.028 no C40 . H402 . 0.982 no C40 . H403 . 0.996 no C140 . H1401 . 0.963 no C140 . H1402 . 0.961 no C140 . H1403 . 0.956 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 3_655 Co1 . N10 3_545 175.81(8) yes N5 3_655 Co1 . N1 . 88.87(8) yes N10 3_545 Co1 . N1 . 95.28(9) yes N5 3_655 Co1 . N2 . 89.78(8) yes N10 3_545 Co1 . N2 . 86.07(9) yes N1 . Co1 . N2 . 178.50(9) yes N5 3_655 Co1 . N3 . 86.54(7) yes N10 3_545 Co1 . N3 . 92.99(8) yes N1 . Co1 . N3 . 88.50(8) yes N2 . Co1 . N3 . 92.06(8) yes N5 3_655 Co1 . N8 . 95.11(10) yes N10 3_545 Co1 . N8 . 85.53(11) yes N1 . Co1 . N8 . 89.24(8) yes N2 . Co1 . N8 . 90.24(8) yes N3 . Co1 . N8 . 177.18(7) yes N5 3_655 Co1 . N110 3_545 172.56(19) yes N5 3_655 Co1 . N1 . 88.87(8) yes N110 3_545 Co1 . N1 . 83.79(19) yes N5 3_655 Co1 . N2 . 89.78(8) yes N110 3_545 Co1 . N2 . 97.57(19) yes N1 . Co1 . N2 . 178.50(9) yes N5 3_655 Co1 . N3 . 86.54(7) yes N110 3_545 Co1 . N3 . 92.03(17) yes N1 . Co1 . N3 . 88.50(8) yes N2 . Co1 . N3 . 92.06(8) yes N5 3_655 Co1 . N108 . 92.0(2) yes N110 3_545 Co1 . N108 . 89.1(3) yes N1 . Co1 . N108 . 88.82(16) yes N2 . Co1 . N108 . 90.58(16) yes N3 . Co1 . N108 . 176.98(17) yes Co1 . N1 . C1 . 156.85(18) yes Co1 . N2 . C2 . 154.79(19) yes Co1 . N3 . C3 . 119.30(15) yes Co1 . N3 . C7 . 121.88(15) yes C3 . N3 . C7 . 116.92(19) yes C8 . N4 . C12 . 117.30(19) yes Co1 3_645 N5 . C13 . 119.20(16) yes Co1 3_645 N5 . C17 . 123.64(14) yes C13 . N5 . C17 . 116.86(19) yes C18 . N6 . C19 . 105.1(2) yes C19 . N7 . C20 . 107.2(2) yes C19 . N7 . H1 . 126.0 no C20 . N7 . H1 . 126.6 no C36 . N11 . C37 . 105.3(2) yes C37 . N12 . C38 . 107.2(2) yes C37 . N12 . H2 . 126.7 no C38 . N12 . H2 . 125.9 no N1 . C1 . S1 . 177.5(3) yes N2 . C2 . S2 . 178.0(2) yes N3 . C3 . C4 . 123.4(2) yes N3 . C3 . H21 . 118.0 no C4 . C3 . H21 . 118.6 no C3 . C4 . C5 . 119.6(2) yes C3 . C4 . H41 . 119.8 no C5 . C4 . H41 . 120.6 no C4 . C5 . C6 . 117.39(19) yes C4 . C5 . C8 . 121.1(2) yes C6 . C5 . C8 . 121.5(2) yes C5 . C6 . C7 . 119.4(2) yes C5 . C6 . H61 . 120.9 no C7 . C6 . H61 . 119.7 no C6 . C7 . N3 . 123.3(2) yes C6 . C7 . H71 . 119.1 no N3 . C7 . H71 . 117.7 no C5 . C8 . N4 . 116.56(19) yes C5 . C8 . C9 . 120.41(19) yes N4 . C8 . C9 . 123.02(19) yes C8 . C9 . C10 . 119.67(19) yes C8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 120.8 no C9 . C10 . C11 . 117.7(2) yes C9 . C10 . C18 . 119.99(19) yes C11 . C10 . C18 . 122.26(18) yes C10 . C11 . C12 . 119.00(18) yes C10 . C11 . H111 . 120.2 no C12 . C11 . H111 . 120.8 no C11 . C12 . N4 . 123.24(19) yes C11 . C12 . C15 . 121.58(18) yes N4 . C12 . C15 . 115.18(19) yes N5 . C13 . C14 . 123.4(2) yes N5 . C13 . H131 . 117.3 no C14 . C13 . H131 . 119.3 no C13 . C14 . C15 . 119.80(19) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 120.5 no C12 . C15 . C14 . 120.08(18) yes C12 . C15 . C16 . 123.3(2) yes C14 . C15 . C16 . 116.6(2) yes C15 . C16 . C17 . 119.7(2) yes C15 . C16 . H161 . 120.4 no C17 . C16 . H161 . 119.9 no C16 . C17 . N5 . 123.5(2) yes C16 . C17 . H171 . 119.0 no N5 . C17 . H171 . 117.4 no C10 . C18 . N6 . 123.0(2) yes C10 . C18 . C20 . 127.50(19) yes N6 . C18 . C20 . 109.4(2) yes N7 . C19 . N6 . 112.2(2) yes N7 . C19 . H191 . 123.2 no N6 . C19 . H191 . 124.6 no C18 . C20 . N7 . 106.0(2) yes C18 . C20 . H201 . 128.8 no N7 . C20 . H201 . 125.2 no C36 . C28 . C27 . 120.61(17) yes C36 . C28 . C29 . 120.71(16) yes C27 . C28 . C29 . 118.65(19) yes C36 . C28 . C127 . 122.0(3) yes C36 . C28 . C129 . 121.1(3) yes C127 . C28 . C129 . 116.8(3) yes C28 . C36 . N11 . 122.72(19) yes C28 . C36 . C38 . 128.34(19) yes N11 . C36 . C38 . 108.9(2) yes N12 . C37 . N11 . 112.1(2) yes N12 . C37 . H371 . 123.0 no N11 . C37 . H371 . 124.9 no N12 . C38 . C36 . 106.4(2) yes N12 . C38 . H381 . 124.7 no C36 . C38 . H381 . 128.9 no Co1 . N8 . C21 . 126.03(13) yes Co1 . N8 . C25 . 114.16(12) yes C21 . N8 . C25 . 118.55(15) yes C26 . N9 . C30 . 118.79(18) yes Co1 3_555 N10 . C31 . 119.70(12) yes Co1 3_555 N10 . C35 . 121.81(12) yes C31 . N10 . C35 . 118.45(14) yes N8 . C21 . C22 . 122.17(18) yes N8 . C21 . H211 . 119.6 no C22 . C21 . H211 . 118.2 no C21 . C22 . C23 . 120.11(19) yes C21 . C22 . H221 . 119.0 no C23 . C22 . H221 . 120.9 no C22 . C23 . C24 . 117.24(17) yes C22 . C23 . C26 . 124.07(16) yes C24 . C23 . C26 . 118.69(16) yes C23 . C24 . C25 . 120.24(18) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 119.3 no C24 . C25 . N8 . 121.57(18) yes C24 . C25 . H251 . 119.1 no N8 . C25 . H251 . 119.3 no C23 . C26 . N9 . 116.47(17) yes C23 . C26 . C27 . 121.42(16) yes N9 . C26 . C27 . 122.10(17) yes C26 . C27 . C28 . 119.10(18) yes C26 . C27 . H271 . 119.8 no C28 . C27 . H271 . 121.0 no C28 . C29 . C30 . 118.33(18) yes C28 . C29 . H291 . 121.6 no C30 . C29 . H291 . 120.1 no C29 . C30 . N9 . 123.00(17) yes C29 . C30 . C33 . 119.88(16) yes N9 . C30 . C33 . 117.09(17) yes N10 . C31 . C32 . 122.14(18) yes N10 . C31 . H311 . 118.5 no C32 . C31 . H311 . 119.4 no C31 . C32 . C33 . 119.32(19) yes C31 . C32 . H321 . 119.7 no C33 . C32 . H321 . 121.0 no C30 . C33 . C32 . 118.96(17) yes C30 . C33 . C34 . 122.13(18) yes C32 . C33 . C34 . 118.90(17) yes C33 . C34 . C35 . 118.50(19) yes C33 . C34 . H341 . 120.7 no C35 . C34 . H341 . 120.8 no C34 . C35 . N10 . 122.29(18) yes C34 . C35 . H351 . 118.4 no N10 . C35 . H351 . 119.3 no Co1 . N108 . C121 . 119.3(3) yes Co1 . N108 . C125 . 122.7(3) yes C121 . N108 . C125 . 116.8(3) yes C126 . N109 . C130 . 121.2(3) yes Co1 3_555 N110 . C131 . 120.6(3) yes Co1 3_555 N110 . C135 . 116.2(3) yes C131 . N110 . C135 . 120.8(3) yes N108 . C121 . C122 . 123.3(3) yes N108 . C121 . H1211 . 118.7 no C122 . C121 . H1211 . 118.0 no C121 . C122 . C123 . 120.0(3) yes C121 . C122 . H1221 . 120.0 no C123 . C122 . H1221 . 120.0 no C122 . C123 . C124 . 117.0(3) yes C122 . C123 . C126 . 122.0(3) yes C124 . C123 . C126 . 121.0(3) yes C123 . C124 . C125 . 120.0(3) yes C123 . C124 . H1241 . 119.8 no C125 . C124 . H1241 . 120.2 no C124 . C125 . N108 . 122.7(3) yes C124 . C125 . H1251 . 118.3 no N108 . C125 . H1251 . 119.1 no C123 . C126 . N109 . 117.4(3) yes C123 . C126 . C127 . 122.0(3) yes N109 . C126 . C127 . 120.6(3) yes C126 . C127 . C28 . 120.4(3) yes C126 . C127 . H1271 . 119.5 no C28 . C127 . H1271 . 120.1 no C28 . C129 . C130 . 120.8(3) yes C28 . C129 . H1291 . 119.9 no C130 . C129 . H1291 . 119.3 no C129 . C130 . N109 . 120.1(3) yes C129 . C130 . C133 . 123.3(3) yes N109 . C130 . C133 . 116.6(3) yes N110 . C131 . C132 . 122.9(3) yes N110 . C131 . H1311 . 118.4 no C132 . C131 . H1311 . 118.7 no C131 . C132 . C133 . 117.6(3) yes C131 . C132 . H1321 . 120.8 no C133 . C132 . H1321 . 121.6 no C130 . C133 . C132 . 118.9(3) yes C130 . C133 . C134 . 122.2(3) yes C132 . C133 . C134 . 118.6(3) yes C133 . C134 . C135 . 121.7(3) yes C133 . C134 . H1341 . 119.0 no C135 . C134 . H1341 . 119.3 no C134 . C135 . N110 . 118.0(3) yes C134 . C135 . H1351 . 121.1 no N110 . C135 . H1351 . 120.9 no O1 . C39 . H391 . 110.1 no O1 . C39 . H392 . 109.0 no H391 . C39 . H392 . 108.5 no O1 . C39 . H393 . 108.1 no H391 . C39 . H393 . 111.0 no H392 . C39 . H393 . 110.1 no C39 . O1 . H3 . 113.8 no H4 . O2 . C40 . 118.5 no H4 . O2 . C140 . 101.9 no O2 . C40 . H401 . 107.2 no O2 . C40 . H402 . 109.2 no H401 . C40 . H402 . 111.3 no O2 . C40 . H403 . 106.5 no H401 . C40 . H403 . 111.2 no H402 . C40 . H403 . 111.1 no O2 . C140 . H1401 . 108.9 no O2 . C140 . H1402 . 110.9 no H1401 . C140 . H1402 . 109.7 no O2 . C140 . H1403 . 110.3 no H1401 . C140 . H1403 . 108.4 no H1402 . C140 . H1403 . 108.7 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N7 . H1 . O1 . 168 0.86 1.91 2.758(5) yes N12 . H2 . O2 . 169 0.87 1.89 2.750(5) yes C3 . H21 . C1 . 145 0.92 2.52 3.324(5) yes C6 . H61 . O1 4_565 134 0.94 2.58 3.304(5) yes C24 . H241 . C37 4_564 145 0.94 2.59 3.403(5) yes C31 . H311 . C121 3_555 130 0.94 2.37 3.067(5) yes C32 . H321 . O2 2_566 157 0.94 2.53 3.416(5) yes C32 . H321 . C140 2_566 123 0.94 1.92 2.555(5) yes C121 . H1211 . N2 . 122 0.93 2.50 3.098(5) yes C121 . H1211 . C2 . 148 0.93 2.36 3.190(5) yes C131 . H1311 . C25 3_555 140 0.92 1.78 2.560(5) yes O1 . H3 . N6 3_654 167 0.82 1.91 2.708(5) yes O2 . H4 . N11 3_546 176 0.83 1.88 2.705(5) yes C140 . H1403 . C31 2_566 132 0.96 2.06 2.796(5) yes C140 . H1403 . C32 2_566 174 0.96 1.60 2.555(5) yes # Attachment '- GQ228.CIF' data_gq228 _database_code_depnum_ccdc_archive 'CCDC 856245' #TrackingRef '- GQ228.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H30 Co N8 S2, 0.67(C2 H4 Cl2), C H4 O, H2 O' _chemical_formula_sum 'C50.33 H38.67 Cl1.33 Co N8 O2 S2' _chemical_formula_weight 957.90 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc 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' _cell_length_a 28.199(6) _cell_length_b 10.371(2) _cell_length_c 32.295(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.51(3) _cell_angle_gamma 90.00 _cell_volume 9184(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 78106 _cell_measurement_theta_min 4.20 _cell_measurement_theta_max 64.72 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3939 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8195 _exptl_absorpt_correction_T_max 0.9710 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81174 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10540 _reflns_number_gt 9902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+19.5346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10540 _refine_ls_number_parameters 615 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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 0.884909(9) 0.40887(2) 0.636923(7) 0.01951(8) Uani 1 1 d . . . N1 N 0.87993(6) 0.34491(16) 0.57129(5) 0.0225(3) Uani 1 1 d . . . N2 N 0.92743(6) 0.29072(16) 0.43376(5) 0.0239(3) Uani 1 1 d . . . N3 N 1.04854(6) 0.48799(16) 0.36442(5) 0.0245(3) Uani 1 1 d . . . C1 C 0.87567(7) 0.22003(19) 0.56043(6) 0.0257(4) Uani 1 1 d . . . H1A H 0.8704 0.1596 0.5810 0.031 Uiso 1 1 calc R . . C2 C 0.87856(7) 0.17431(19) 0.52082(6) 0.0255(4) Uani 1 1 d . . . H2A H 0.8737 0.0854 0.5141 0.031 Uiso 1 1 calc R . . C3 C 0.88864(7) 0.26044(19) 0.49095(6) 0.0225(4) Uani 1 1 d . . . C4 C 0.89297(7) 0.39014(19) 0.50201(6) 0.0247(4) Uani 1 1 d . . . H4A H 0.8997 0.4522 0.4825 0.030 Uiso 1 1 calc R . . C5 C 0.88743(7) 0.42817(19) 0.54164(6) 0.0243(4) Uani 1 1 d . . . H5A H 0.8890 0.5176 0.5482 0.029 Uiso 1 1 calc R . . C6 C 0.89577(7) 0.21898(18) 0.44876(6) 0.0225(4) Uani 1 1 d . . . C7 C 0.87035(7) 0.11591(19) 0.42645(6) 0.0236(4) Uani 1 1 d . . . H7A H 0.8493 0.0650 0.4389 0.028 Uiso 1 1 calc R . . C8 C 0.87608(7) 0.08808(18) 0.38557(6) 0.0229(4) Uani 1 1 d . . . C9 C 0.91001(7) 0.1619(2) 0.37045(6) 0.0253(4) Uani 1 1 d . . . H9A H 0.9156 0.1457 0.3430 0.030 Uiso 1 1 calc R . . C10 C 0.93552(7) 0.25912(19) 0.39590(6) 0.0236(4) Uani 1 1 d . . . C11 C 1.01895(7) 0.53354(19) 0.38807(6) 0.0248(4) Uani 1 1 d . . . H11A H 1.0234 0.6199 0.3981 0.030 Uiso 1 1 calc R . . C12 C 0.98244(7) 0.46176(19) 0.39861(6) 0.0245(4) Uani 1 1 d . . . H12A H 0.9635 0.4969 0.4166 0.029 Uiso 1 1 calc R . . C13 C 0.97350(7) 0.33755(19) 0.38267(6) 0.0241(4) Uani 1 1 d . . . C14 C 1.00227(8) 0.2920(2) 0.35635(7) 0.0325(5) Uani 1 1 d . . . H14A H 0.9965 0.2090 0.3437 0.039 Uiso 1 1 calc R . . C15 C 1.03954(8) 0.3692(2) 0.34868(7) 0.0317(4) Uani 1 1 d . . . H15A H 1.0596 0.3358 0.3314 0.038 Uiso 1 1 calc R . . C16 C 0.84624(7) -0.01205(18) 0.35861(6) 0.0226(4) Uani 1 1 d . . . C17 C 0.80471(8) -0.0644(2) 0.36888(7) 0.0302(4) Uani 1 1 d . . . H17A H 0.7960 -0.0375 0.3942 0.036 Uiso 1 1 calc R . . C18 C 0.77617(8) -0.1545(2) 0.34287(7) 0.0310(4) Uani 1 1 d . . . H18A H 0.7484 -0.1896 0.3507 0.037 Uiso 1 1 calc R . . C19 C 0.78785(7) -0.19436(19) 0.30522(7) 0.0269(4) Uani 1 1 d . . . C20 C 0.82978(7) -0.14453(19) 0.29512(6) 0.0274(4) Uani 1 1 d . . . H20A H 0.8387 -0.1722 0.2699 0.033 Uiso 1 1 calc R . . C21 C 0.85845(7) -0.05536(19) 0.32139(6) 0.0248(4) Uani 1 1 d . . . H21A H 0.8869 -0.0229 0.3141 0.030 Uiso 1 1 calc R . . C22 C 0.75764(8) -0.2833(2) 0.27676(7) 0.0335(4) Uani 1 1 d . . . C23 C 0.73327(10) -0.3524(3) 0.25150(9) 0.0489(6) Uani 1 1 d . . . H23 H 0.7136 -0.4081 0.2311 0.059 Uiso 1 1 calc R . . N4 N 0.88733(6) 0.46505(16) 0.70218(5) 0.0240(3) Uani 1 1 d . . . N5 N 0.82014(6) 0.55980(17) 0.82895(5) 0.0254(3) Uani 1 1 d . . . N6 N 0.68135(6) 0.80179(17) 0.86326(5) 0.0245(3) Uani 1 1 d . . . C24 C 0.91864(7) 0.4162(2) 0.73600(6) 0.0283(4) Uani 1 1 d . . . H24A H 0.9474 0.3757 0.7318 0.034 Uiso 1 1 calc R . . C25 C 0.91150(7) 0.4214(2) 0.77714(6) 0.0288(4) Uani 1 1 d . . . H25A H 0.9349 0.3852 0.8002 0.035 Uiso 1 1 calc R . . C26 C 0.86985(7) 0.47979(19) 0.78415(6) 0.0235(4) Uani 1 1 d . . . C27 C 0.83862(8) 0.5368(2) 0.74934(7) 0.0324(5) Uani 1 1 d . . . H27A H 0.8105 0.5821 0.7529 0.039 Uiso 1 1 calc R . . C28 C 0.84852(8) 0.5274(2) 0.70955(7) 0.0319(4) Uani 1 1 d . . . H28A H 0.8267 0.5672 0.6862 0.038 Uiso 1 1 calc R . . C29 C 0.85639(7) 0.47908(19) 0.82602(6) 0.0228(4) Uani 1 1 d . . . C30 C 0.87788(7) 0.39588(18) 0.85881(6) 0.0229(4) Uani 1 1 d . . . H30A H 0.9030 0.3389 0.8553 0.027 Uiso 1 1 calc R . . C31 C 0.86248(7) 0.39618(18) 0.89683(6) 0.0227(4) Uani 1 1 d . . . C32 C 0.82522(7) 0.4825(2) 0.89978(6) 0.0251(4) Uani 1 1 d . . . H32A H 0.8138 0.4875 0.9252 0.030 Uiso 1 1 calc R . . C33 C 0.80518(7) 0.5606(2) 0.86532(6) 0.0246(4) Uani 1 1 d . . . C34 C 0.71825(7) 0.7961(2) 0.89781(6) 0.0254(4) Uani 1 1 d . . . H34A H 0.7164 0.8475 0.9217 0.030 Uiso 1 1 calc R . . C35 C 0.75892(7) 0.7193(2) 0.90054(6) 0.0258(4) Uani 1 1 d . . . H35A H 0.7837 0.7162 0.9261 0.031 Uiso 1 1 calc R . . C36 C 0.76323(7) 0.6468(2) 0.86548(6) 0.0251(4) Uani 1 1 d . . . C37 C 0.72599(8) 0.6566(2) 0.82903(7) 0.0365(5) Uani 1 1 d . . . H37A H 0.7280 0.6113 0.8039 0.044 Uiso 1 1 calc R . . C38 C 0.68600(8) 0.7328(2) 0.82947(7) 0.0366(5) Uani 1 1 d . . . H38A H 0.6604 0.7364 0.8044 0.044 Uiso 1 1 calc R . . C39 C 0.88493(7) 0.31120(18) 0.93303(6) 0.0238(4) Uani 1 1 d . . . C40 C 0.86102(8) 0.2840(2) 0.96533(7) 0.0289(4) Uani 1 1 d . . . H40A H 0.8288 0.3152 0.9630 0.035 Uiso 1 1 calc R . . C41 C 0.88344(8) 0.2123(2) 1.00059(7) 0.0327(4) Uani 1 1 d . . . H41A H 0.8665 0.1948 1.0222 0.039 Uiso 1 1 calc R . . C42 C 0.93058(8) 0.1657(2) 1.00477(7) 0.0315(4) Uani 1 1 d . . . C43 C 0.95413(8) 0.1884(2) 0.97198(8) 0.0370(5) Uani 1 1 d . . . H43A H 0.9860 0.1551 0.9740 0.044 Uiso 1 1 calc R . . C44 C 0.93132(8) 0.2590(2) 0.93665(7) 0.0318(4) Uani 1 1 d . . . H44A H 0.9476 0.2723 0.9143 0.038 Uiso 1 1 calc R . . C45 C 0.95425(9) 0.0939(2) 1.04188(8) 0.0382(5) Uani 1 1 d . . . C46 C 0.97312(11) 0.0343(3) 1.07245(9) 0.0485(6) Uani 1 1 d . . . H46 H 0.9883 -0.0137 1.0970 0.058 Uiso 1 1 calc R . . N50 N 0.84361(6) 0.56839(17) 0.61241(5) 0.0271(3) Uani 1 1 d . . . C50 C 0.81801(8) 0.6406(2) 0.59107(7) 0.0293(4) Uani 1 1 d . . . S50 S 0.78178(3) 0.74321(8) 0.56059(3) 0.05382(19) Uani 1 1 d . . . N60 N 0.92834(6) 0.24766(17) 0.65815(5) 0.0274(3) Uani 1 1 d . . . C60 C 0.96577(7) 0.19749(19) 0.66478(6) 0.0272(4) Uani 1 1 d . . . S60 S 1.01957(2) 0.13083(7) 0.67292(2) 0.04859(17) Uani 1 1 d . . . O100 O 0.71960(8) 0.4882(2) 0.52508(7) 0.0534(5) Uani 1 1 d . . . H100 H 0.7320 0.5594 0.5341 0.080 Uiso 1 1 calc R . . C100 C 0.74082(12) 0.4435(3) 0.49256(10) 0.0539(7) Uani 1 1 d . . . H10A H 0.7265 0.4892 0.4660 0.081 Uiso 1 1 calc R . . H10B H 0.7347 0.3508 0.4885 0.081 Uiso 1 1 calc R . . H10C H 0.7760 0.4593 0.5005 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.93300(15) 0.7848(2) 0.75320(7) 0.0878(7) Uani 0.67 1 d P A 1 Cl2 Cl 0.86047(10) 0.8857(2) 0.66064(7) 0.1168(7) Uani 0.67 1 d P A 1 C101 C 0.9350(3) 0.9271(6) 0.7258(2) 0.0835(19) Uani 0.67 1 d P A 1 H10D H 0.9521 0.9932 0.7460 0.100 Uiso 0.67 1 calc PR A 1 H10E H 0.9541 0.9130 0.7041 0.100 Uiso 0.67 1 calc PR A 1 C102 C 0.8887(3) 0.9736(7) 0.7057(2) 0.0896(19) Uani 0.67 1 d P A 1 H10F H 0.8918 1.0645 0.6973 0.108 Uiso 0.67 1 calc PR A 1 H10G H 0.8676 0.9720 0.7263 0.108 Uiso 0.67 1 calc PR A 1 O200 O 0.8790(6) 0.9283(8) 0.6290(3) 0.141(5) Uani 0.33 1 d PU B 2 O201 O 0.8370(4) 0.8828(9) 0.6951(5) 0.115(4) Uani 0.33 1 d P C 2 O202 O 0.9245(8) 0.8291(10) 0.7461(5) 0.093(5) Uani 0.33 1 d P D 2 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 0.01890(13) 0.02349(14) 0.01798(13) 0.00086(9) 0.00806(9) -0.00134(9) N1 0.0247(7) 0.0257(8) 0.0190(7) -0.0006(6) 0.0090(6) -0.0028(6) N2 0.0235(7) 0.0274(8) 0.0229(7) -0.0017(6) 0.0094(6) -0.0028(6) N3 0.0228(7) 0.0280(8) 0.0256(8) -0.0018(6) 0.0115(6) -0.0047(6) C1 0.0310(10) 0.0252(9) 0.0231(9) 0.0020(7) 0.0107(7) -0.0039(7) C2 0.0303(9) 0.0233(9) 0.0251(9) -0.0009(7) 0.0108(7) -0.0035(7) C3 0.0208(8) 0.0274(9) 0.0204(8) -0.0004(7) 0.0071(7) -0.0010(7) C4 0.0292(9) 0.0262(9) 0.0206(8) 0.0018(7) 0.0095(7) -0.0018(7) C5 0.0287(9) 0.0239(9) 0.0217(9) 0.0005(7) 0.0087(7) -0.0017(7) C6 0.0223(8) 0.0260(9) 0.0207(8) 0.0006(7) 0.0082(7) -0.0002(7) C7 0.0229(8) 0.0268(9) 0.0232(9) 0.0003(7) 0.0096(7) -0.0027(7) C8 0.0213(8) 0.0259(9) 0.0224(9) -0.0009(7) 0.0065(7) -0.0005(7) C9 0.0254(9) 0.0312(10) 0.0217(8) -0.0030(7) 0.0105(7) -0.0039(7) C10 0.0222(8) 0.0276(9) 0.0228(8) -0.0014(7) 0.0091(7) -0.0024(7) C11 0.0222(8) 0.0260(9) 0.0278(9) -0.0021(7) 0.0091(7) -0.0017(7) C12 0.0215(8) 0.0282(9) 0.0262(9) -0.0020(7) 0.0103(7) -0.0001(7) C13 0.0230(8) 0.0294(9) 0.0216(8) -0.0015(7) 0.0088(7) -0.0040(7) C14 0.0378(11) 0.0313(10) 0.0350(11) -0.0110(8) 0.0217(9) -0.0104(9) C15 0.0347(10) 0.0335(10) 0.0331(10) -0.0090(8) 0.0207(9) -0.0082(9) C16 0.0224(8) 0.0241(8) 0.0217(8) -0.0005(7) 0.0057(7) 0.0000(7) C17 0.0292(10) 0.0341(10) 0.0299(10) -0.0057(8) 0.0120(8) -0.0059(8) C18 0.0248(9) 0.0331(10) 0.0363(11) -0.0028(9) 0.0093(8) -0.0053(8) C19 0.0259(9) 0.0215(9) 0.0305(10) -0.0010(7) 0.0008(8) 0.0014(7) C20 0.0305(10) 0.0264(9) 0.0253(9) -0.0026(7) 0.0066(8) 0.0023(8) C21 0.0241(9) 0.0259(9) 0.0253(9) -0.0009(7) 0.0080(7) 0.0002(7) C22 0.0336(11) 0.0274(10) 0.0373(11) -0.0013(9) 0.0034(9) -0.0006(8) C23 0.0503(15) 0.0403(13) 0.0504(15) -0.0111(11) 0.0002(12) -0.0116(11) N4 0.0230(7) 0.0306(8) 0.0204(7) -0.0019(6) 0.0092(6) 0.0006(6) N5 0.0235(8) 0.0331(8) 0.0211(7) -0.0015(6) 0.0081(6) 0.0055(7) N6 0.0216(7) 0.0323(8) 0.0207(7) -0.0030(6) 0.0074(6) 0.0053(6) C24 0.0206(9) 0.0427(11) 0.0230(9) -0.0033(8) 0.0079(7) 0.0056(8) C25 0.0218(9) 0.0439(12) 0.0211(9) -0.0016(8) 0.0057(7) 0.0073(8) C26 0.0226(8) 0.0276(9) 0.0217(8) -0.0027(7) 0.0079(7) 0.0021(7) C27 0.0316(10) 0.0427(12) 0.0256(10) 0.0036(8) 0.0124(8) 0.0155(9) C28 0.0337(10) 0.0398(11) 0.0247(9) 0.0051(8) 0.0118(8) 0.0138(9) C29 0.0201(8) 0.0286(9) 0.0207(8) -0.0036(7) 0.0069(7) 0.0010(7) C30 0.0201(8) 0.0260(9) 0.0232(9) -0.0046(7) 0.0067(7) 0.0021(7) C31 0.0202(8) 0.0260(9) 0.0224(9) -0.0029(7) 0.0055(7) -0.0012(7) C32 0.0242(9) 0.0321(10) 0.0205(8) -0.0024(7) 0.0082(7) 0.0031(7) C33 0.0216(8) 0.0310(9) 0.0222(9) -0.0036(7) 0.0072(7) 0.0033(7) C34 0.0237(9) 0.0318(10) 0.0218(8) -0.0062(7) 0.0077(7) 0.0011(7) C35 0.0222(9) 0.0343(10) 0.0212(8) -0.0034(7) 0.0059(7) 0.0021(7) C36 0.0236(9) 0.0315(10) 0.0218(8) -0.0007(7) 0.0086(7) 0.0053(7) C37 0.0344(11) 0.0509(13) 0.0234(9) -0.0095(9) 0.0050(8) 0.0166(10) C38 0.0330(11) 0.0525(14) 0.0219(9) -0.0096(9) 0.0018(8) 0.0167(10) C39 0.0249(9) 0.0238(9) 0.0232(8) -0.0018(7) 0.0065(7) 0.0001(7) C40 0.0270(9) 0.0323(10) 0.0293(10) 0.0011(8) 0.0107(8) 0.0026(8) C41 0.0381(11) 0.0341(11) 0.0286(10) 0.0030(8) 0.0131(9) 0.0000(9) C42 0.0347(10) 0.0261(9) 0.0325(10) 0.0031(8) 0.0053(8) -0.0014(8) C43 0.0310(10) 0.0374(12) 0.0444(12) 0.0108(10) 0.0125(9) 0.0086(9) C44 0.0297(10) 0.0330(10) 0.0362(11) 0.0071(9) 0.0148(9) 0.0057(8) C45 0.0406(12) 0.0334(11) 0.0383(12) 0.0043(9) 0.0048(10) -0.0021(9) C46 0.0536(15) 0.0419(13) 0.0431(14) 0.0114(11) -0.0024(12) -0.0015(12) N50 0.0286(8) 0.0277(8) 0.0268(8) 0.0034(7) 0.0101(7) 0.0034(7) C50 0.0278(9) 0.0330(10) 0.0312(10) 0.0028(8) 0.0151(8) 0.0000(8) S50 0.0402(3) 0.0562(4) 0.0652(4) 0.0303(3) 0.0126(3) 0.0149(3) N60 0.0284(8) 0.0287(8) 0.0261(8) 0.0013(6) 0.0084(7) 0.0021(7) C60 0.0296(10) 0.0263(9) 0.0250(9) -0.0048(7) 0.0048(7) -0.0005(8) S60 0.0305(3) 0.0489(4) 0.0601(4) -0.0132(3) -0.0021(3) 0.0107(3) O100 0.0486(11) 0.0643(13) 0.0498(11) 0.0064(10) 0.0166(9) -0.0056(9) C100 0.0598(17) 0.0554(16) 0.0498(16) 0.0113(13) 0.0193(13) 0.0081(14) Cl1 0.1386(19) 0.0735(16) 0.0427(7) -0.0036(9) 0.0038(9) -0.0106(16) Cl2 0.1382(18) 0.1069(15) 0.0972(14) -0.0261(12) 0.0112(13) 0.0210(13) C101 0.113(5) 0.063(3) 0.085(4) -0.011(3) 0.046(4) -0.023(3) C102 0.100(5) 0.074(4) 0.106(5) -0.006(4) 0.045(4) -0.007(4) O200 0.317(14) 0.055(4) 0.066(5) -0.020(4) 0.073(7) -0.114(7) O201 0.132(9) 0.056(5) 0.187(12) 0.006(6) 0.098(9) 0.013(5) O202 0.139(12) 0.037(6) 0.093(10) -0.007(5) 0.005(8) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N50 2.0712(18) . ? Co1 N60 2.0911(18) . ? Co1 N3 2.1695(16) 5_766 ? Co1 N4 2.1723(16) . ? Co1 N6 2.1723(16) 4_646 ? Co1 N1 2.1940(16) . ? N1 C1 1.340(3) . ? N1 C5 1.342(2) . ? N2 C10 1.336(2) . ? N2 C6 1.337(2) . ? N3 C15 1.334(3) . ? N3 C11 1.342(2) . ? N3 Co1 2.1695(16) 5_766 ? C1 C2 1.384(3) . ? C1 H1A 0.9500 . ? C2 C3 1.392(3) . ? C2 H2A 0.9500 . ? C3 C4 1.390(3) . ? C3 C6 1.487(2) . ? C4 C5 1.383(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.391(3) . ? C7 C8 1.397(3) . ? C7 H7A 0.9500 . ? C8 C9 1.399(3) . ? C8 C16 1.484(3) . ? C9 C10 1.391(3) . ? C9 H9A 0.9500 . ? C10 C13 1.485(3) . ? C11 C12 1.376(3) . ? C11 H11A 0.9500 . ? C12 C13 1.388(3) . ? C12 H12A 0.9500 . ? C13 C14 1.388(3) . ? C14 C15 1.389(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.399(3) . ? C16 C21 1.399(3) . ? C17 C18 1.382(3) . ? C17 H17A 0.9500 . ? C18 C19 1.395(3) . ? C18 H18A 0.9500 . ? C19 C20 1.397(3) . ? C19 C22 1.434(3) . ? C20 C21 1.381(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.179(3) . ? C23 H23 0.9500 . ? N4 C24 1.334(3) . ? N4 C28 1.339(3) . ? N5 C33 1.338(2) . ? N5 C29 1.342(2) . ? N6 C38 1.337(3) . ? N6 C34 1.337(3) . ? N6 Co1 2.1723(16) 4_656 ? C24 C25 1.391(3) . ? C24 H24A 0.9500 . ? C25 C26 1.387(3) . ? C25 H25A 0.9500 . ? C26 C27 1.388(3) . ? C26 C29 1.488(3) . ? C27 C28 1.381(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.390(3) . ? C30 C31 1.395(3) . ? C30 H30A 0.9500 . ? C31 C32 1.401(3) . ? C31 C39 1.483(3) . ? C32 C33 1.386(3) . ? C32 H32A 0.9500 . ? C33 C36 1.484(3) . ? C34 C35 1.382(3) . ? C34 H34A 0.9500 . ? C35 C36 1.388(3) . ? C35 H35A 0.9500 . ? C36 C37 1.386(3) . ? C37 C38 1.379(3) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.395(3) . ? C39 C40 1.397(3) . ? C40 C41 1.383(3) . ? C40 H40A 0.9500 . ? C41 C42 1.391(3) . ? C41 H41A 0.9500 . ? C42 C43 1.395(3) . ? C42 C45 1.436(3) . ? C43 C44 1.382(3) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.181(4) . ? C46 H46 0.9500 . ? N50 C50 1.151(3) . ? C50 S50 1.635(2) . ? N60 C60 1.151(3) . ? C60 S60 1.631(2) . ? O100 C100 1.403(4) . ? O100 H100 0.8400 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? Cl1 C101 1.727(7) . ? Cl2 C102 1.744(8) . ? C101 C102 1.402(10) . ? C101 H10D 0.9900 . ? C101 H10E 0.9900 . ? C102 H10F 0.9900 . ? C102 H10G 0.9900 . ? 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 N50 Co1 N60 176.33(7) . . ? N50 Co1 N3 90.59(7) . 5_766 ? N60 Co1 N3 87.58(7) . 5_766 ? N50 Co1 N4 92.52(7) . . ? N60 Co1 N4 90.76(7) . . ? N3 Co1 N4 93.21(7) 5_766 . ? N50 Co1 N6 90.05(7) . 4_646 ? N60 Co1 N6 91.70(7) . 4_646 ? N3 Co1 N6 178.25(6) 5_766 4_646 ? N4 Co1 N6 88.38(7) . 4_646 ? N50 Co1 N1 88.22(7) . . ? N60 Co1 N1 88.58(7) . . ? N3 Co1 N1 89.43(6) 5_766 . ? N4 Co1 N1 177.25(6) . . ? N6 Co1 N1 88.97(6) 4_646 . ? C1 N1 C5 117.04(16) . . ? C1 N1 Co1 121.78(12) . . ? C5 N1 Co1 120.63(13) . . ? C10 N2 C6 117.80(17) . . ? C15 N3 C11 116.99(17) . . ? C15 N3 Co1 122.41(13) . 5_766 ? C11 N3 Co1 119.58(13) . 5_766 ? N1 C1 C2 123.50(18) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.09(18) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 117.58(17) . . ? C4 C3 C6 119.53(17) . . ? C2 C3 C6 122.88(18) . . ? C5 C4 C3 119.46(17) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 123.20(18) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? N2 C6 C7 123.17(17) . . ? N2 C6 C3 114.58(17) . . ? C7 C6 C3 122.23(16) . . ? C6 C7 C8 119.27(17) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C7 C8 C9 117.14(17) . . ? C7 C8 C16 121.62(17) . . ? C9 C8 C16 121.20(17) . . ? C10 C9 C8 119.46(17) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? N2 C10 C9 122.92(17) . . ? N2 C10 C13 114.70(17) . . ? C9 C10 C13 122.37(17) . . ? N3 C11 C12 123.44(18) . . ? N3 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 119.45(17) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 117.47(17) . . ? C14 C13 C10 123.64(18) . . ? C12 C13 C10 118.84(17) . . ? C13 C14 C15 119.22(19) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? N3 C15 C14 123.28(19) . . ? N3 C15 H15A 118.4 . . ? C14 C15 H15A 118.4 . . ? C17 C16 C21 117.82(18) . . ? C17 C16 C8 121.56(17) . . ? C21 C16 C8 120.61(17) . . ? C18 C17 C16 121.26(19) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 120.49(19) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C20 118.63(18) . . ? C18 C19 C22 121.6(2) . . ? C20 C19 C22 119.80(19) . . ? C21 C20 C19 120.67(18) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C16 121.08(18) . . ? C20 C21 H21A 119.5 . . ? C16 C21 H21A 119.5 . . ? C23 C22 C19 176.3(3) . . ? C22 C23 H23 180.0 . . ? C24 N4 C28 116.74(16) . . ? C24 N4 Co1 123.87(13) . . ? C28 N4 Co1 117.41(14) . . ? C33 N5 C29 117.87(17) . . ? C38 N6 C34 116.85(17) . . ? C38 N6 Co1 121.32(14) . 4_656 ? C34 N6 Co1 121.73(13) . 4_656 ? N4 C24 C25 123.49(18) . . ? N4 C24 H24A 118.3 . . ? C25 C24 H24A 118.3 . . ? C26 C25 C24 119.35(19) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 117.10(18) . . ? C25 C26 C29 123.50(18) . . ? C27 C26 C29 119.34(17) . . ? C28 C27 C26 119.71(18) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? N4 C28 C27 123.42(19) . . ? N4 C28 H28A 118.3 . . ? C27 C28 H28A 118.3 . . ? N5 C29 C30 122.50(17) . . ? N5 C29 C26 114.92(17) . . ? C30 C29 C26 122.49(17) . . ? C29 C30 C31 119.94(17) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C32 117.02(18) . . ? C30 C31 C39 121.96(17) . . ? C32 C31 C39 121.01(17) . . ? C33 C32 C31 119.37(17) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? N5 C33 C32 123.28(18) . . ? N5 C33 C36 114.97(17) . . ? C32 C33 C36 121.67(17) . . ? N6 C34 C35 123.43(17) . . ? N6 C34 H34A 118.3 . . ? C35 C34 H34A 118.3 . . ? C34 C35 C36 119.33(18) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? C37 C36 C35 117.35(18) . . ? C37 C36 C33 119.19(17) . . ? C35 C36 C33 123.46(18) . . ? C38 C37 C36 119.49(19) . . ? C38 C37 H37A 120.3 . . ? C36 C37 H37A 120.3 . . ? N6 C38 C37 123.5(2) . . ? N6 C38 H38A 118.3 . . ? C37 C38 H38A 118.3 . . ? C44 C39 C40 117.77(19) . . ? C44 C39 C31 121.05(18) . . ? C40 C39 C31 121.15(17) . . ? C41 C40 C39 121.06(19) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C40 C41 C42 120.6(2) . . ? C40 C41 H41A 119.7 . . ? C42 C41 H41A 119.7 . . ? C41 C42 C43 118.8(2) . . ? C41 C42 C45 120.6(2) . . ? C43 C42 C45 120.7(2) . . ? C44 C43 C42 120.2(2) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C43 C44 C39 121.4(2) . . ? C43 C44 H44A 119.3 . . ? C39 C44 H44A 119.3 . . ? C46 C45 C42 179.1(3) . . ? C45 C46 H46 180.0 . . ? C50 N50 Co1 165.19(18) . . ? N50 C50 S50 179.7(2) . . ? C60 N60 Co1 149.74(17) . . ? N60 C60 S60 177.6(2) . . ? C100 O100 H100 109.5 . . ? O100 C100 H10A 109.5 . . ? O100 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 Cl1 113.2(5) . . ? C102 C101 H10D 108.9 . . ? Cl1 C101 H10D 108.9 . . ? C102 C101 H10E 108.9 . . ? Cl1 C101 H10E 108.9 . . ? H10D C101 H10E 107.8 . . ? C101 C102 Cl2 113.7(5) . . ? C101 C102 H10F 108.8 . . ? Cl2 C102 H10F 108.8 . . ? C101 C102 H10G 108.8 . . ? Cl2 C102 H10G 108.8 . . ? H10F C102 H10G 107.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.535 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.066 # Attachment '- GQ229.CIF' data_gq229 _database_code_depnum_ccdc_archive 'CCDC 856246' #TrackingRef '- GQ229.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 Co N6 O2 S2' _chemical_formula_sum 'C27 H28 Co N6 O2 S2' _chemical_formula_weight 591.62 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.3014(8) _cell_length_b 14.3112(7) _cell_length_c 26.2091(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5364.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 112582 _cell_measurement_theta_min 4.21 _cell_measurement_theta_max 67.57 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_T_max 0.9288 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 139949 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6116 _reflns_number_gt 5980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+6.4988P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6116 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.250399(18) 0.030639(19) 0.259544(9) 0.01915(8) Uani 1 1 d . . . N1 N 0.19254(11) -0.02322(12) 0.33010(6) 0.0200(3) Uani 1 1 d . . . N2 N 0.21749(11) -0.09284(12) 0.50751(6) 0.0198(3) Uani 1 1 d . . . N3 N 0.19274(11) -0.08065(12) 0.68799(6) 0.0221(3) Uani 1 1 d . . . C1 C 0.24409(13) -0.03646(14) 0.37251(7) 0.0201(4) Uani 1 1 d . . . H1A H 0.3080 -0.0183 0.3718 0.024 Uiso 1 1 calc R . . C2 C 0.20927(13) -0.07507(13) 0.41712(7) 0.0188(4) Uani 1 1 d . . . C3 C 0.11481(14) -0.10079(15) 0.41750(8) 0.0243(4) Uani 1 1 d . . . H3A H 0.0877 -0.1272 0.4473 0.029 Uiso 1 1 calc R . . C4 C 0.06135(14) -0.08754(16) 0.37427(8) 0.0265(4) Uani 1 1 d . . . H4A H -0.0029 -0.1045 0.3740 0.032 Uiso 1 1 calc R . . C5 C 0.10228(14) -0.04928(15) 0.33140(7) 0.0233(4) Uani 1 1 d . . . H5A H 0.0652 -0.0410 0.3017 0.028 Uiso 1 1 calc R . . C6 C 0.26682(13) -0.08848(13) 0.46379(7) 0.0189(4) Uani 1 1 d . . . C7 C 0.36349(13) -0.09748(14) 0.46212(7) 0.0202(4) Uani 1 1 d . . . H7A H 0.3954 -0.0930 0.4304 0.024 Uiso 1 1 calc R . . C8 C 0.41391(13) -0.11307(13) 0.50706(7) 0.0196(4) Uani 1 1 d . . . C9 C 0.36221(14) -0.11665(14) 0.55216(7) 0.0217(4) Uani 1 1 d . . . H9A H 0.3930 -0.1264 0.5838 0.026 Uiso 1 1 calc R . . C10 C 0.26578(13) -0.10595(14) 0.55071(7) 0.0198(4) Uani 1 1 d . . . C11 C 0.24319(13) -0.08033(14) 0.64469(7) 0.0210(4) Uani 1 1 d . . . H11A H 0.3062 -0.0595 0.6463 0.025 Uiso 1 1 calc R . . C12 C 0.20817(13) -0.10879(14) 0.59792(7) 0.0198(4) Uani 1 1 d . . . C13 C 0.11537(14) -0.13850(15) 0.59608(7) 0.0246(4) Uani 1 1 d . . . H13A H 0.0884 -0.1581 0.5647 0.030 Uiso 1 1 calc R . . C14 C 0.06317(14) -0.13909(16) 0.64038(8) 0.0268(4) Uani 1 1 d . . . H14A H -0.0001 -0.1593 0.6399 0.032 Uiso 1 1 calc R . . C15 C 0.10406(14) -0.11004(15) 0.68528(8) 0.0247(4) Uani 1 1 d . . . H15A H 0.0677 -0.1109 0.7156 0.030 Uiso 1 1 calc R . . C16 C 0.51673(13) -0.12659(14) 0.50703(7) 0.0217(4) Uani 1 1 d . . . C17 C 0.56948(15) -0.12009(18) 0.46267(8) 0.0325(5) Uani 1 1 d . . . H17A H 0.5383 -0.1078 0.4314 0.039 Uiso 1 1 calc R . . C18 C 0.66534(15) -0.13083(18) 0.46223(9) 0.0331(5) Uani 1 1 d . . . H18A H 0.6981 -0.1254 0.4308 0.040 Uiso 1 1 calc R . . C19 C 0.71530(14) -0.14948(15) 0.50693(9) 0.0262(4) Uani 1 1 d . . . C20 C 0.66294(15) -0.15524(18) 0.55200(9) 0.0321(5) Uani 1 1 d . . . H20A H 0.6940 -0.1670 0.5834 0.039 Uiso 1 1 calc R . . C21 C 0.56671(15) -0.14406(17) 0.55168(8) 0.0309(5) Uani 1 1 d . . . H21A H 0.5336 -0.1485 0.5830 0.037 Uiso 1 1 calc R . . N4 N 0.81051(13) -0.16154(16) 0.50674(8) 0.0365(5) Uani 1 1 d . . . C22 C 0.86406(16) -0.1412(2) 0.46068(12) 0.0455(7) Uani 1 1 d . . . H22A H 0.8374 -0.1757 0.4318 0.068 Uiso 1 1 calc R . . H22B H 0.9293 -0.1602 0.4657 0.068 Uiso 1 1 calc R . . H22C H 0.8615 -0.0740 0.4536 0.068 Uiso 1 1 calc R . . C23 C 0.86285(17) -0.1667(2) 0.55424(11) 0.0421(6) Uani 1 1 d . . . H23A H 0.8657 -0.1045 0.5699 0.063 Uiso 1 1 calc R . . H23B H 0.9264 -0.1888 0.5472 0.063 Uiso 1 1 calc R . . H23C H 0.8317 -0.2101 0.5776 0.063 Uiso 1 1 calc R . . N30 N 0.12392(12) 0.09380(13) 0.24169(7) 0.0258(4) Uani 1 1 d . . . C30 C 0.07545(13) 0.14259(14) 0.21837(7) 0.0219(4) Uani 1 1 d . . . S30 S 0.00984(4) 0.21306(4) 0.18495(2) 0.03162(13) Uani 1 1 d . . . N40 N 0.37812(12) -0.02914(14) 0.27603(7) 0.0271(4) Uani 1 1 d . . . C40 C 0.43453(14) -0.07244(15) 0.29667(8) 0.0245(4) Uani 1 1 d . . . S40 S 0.51017(4) -0.13674(6) 0.32728(3) 0.04599(19) Uani 1 1 d . . . O50 O 0.20612(11) -0.09122(11) 0.22126(6) 0.0274(3) Uani 1 1 d . . . H50 H 0.153(2) -0.0947(19) 0.2120(10) 0.033 Uiso 1 1 d . . . C50 C 0.26252(17) -0.14947(18) 0.18931(9) 0.0365(5) Uani 1 1 d . . . H50A H 0.2661 -0.1222 0.1551 0.055 Uiso 1 1 calc R . . H50B H 0.2346 -0.2119 0.1872 0.055 Uiso 1 1 calc R . . H50C H 0.3256 -0.1542 0.2037 0.055 Uiso 1 1 calc R . . O60 O 0.29730(11) 0.14843(12) 0.30033(7) 0.0332(4) Uani 1 1 d . . . H60 H 0.352(2) 0.157(2) 0.3029(11) 0.040 Uiso 1 1 d . . . C60 C 0.2491(2) 0.23211(18) 0.31205(10) 0.0406(6) Uani 1 1 d . . . H60A H 0.2616 0.2788 0.2855 0.061 Uiso 1 1 calc R . . H60B H 0.2705 0.2559 0.3451 0.061 Uiso 1 1 calc R . . H60C H 0.1817 0.2196 0.3136 0.061 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 0.01513(12) 0.02743(14) 0.01488(13) 0.00182(9) -0.00113(9) 0.00317(10) N1 0.0188(7) 0.0254(8) 0.0157(7) -0.0001(6) 0.0000(6) 0.0015(6) N2 0.0180(7) 0.0248(8) 0.0165(7) -0.0011(6) 0.0006(6) -0.0014(6) N3 0.0175(7) 0.0323(9) 0.0164(7) -0.0023(6) 0.0010(6) 0.0010(7) C1 0.0172(8) 0.0254(9) 0.0177(8) -0.0014(7) 0.0000(7) 0.0009(7) C2 0.0186(8) 0.0217(9) 0.0161(8) -0.0016(7) -0.0002(7) 0.0010(7) C3 0.0201(9) 0.0320(10) 0.0208(9) 0.0013(8) 0.0026(7) -0.0030(8) C4 0.0180(9) 0.0367(11) 0.0248(10) 0.0005(8) -0.0010(8) -0.0039(8) C5 0.0198(9) 0.0317(10) 0.0185(9) -0.0006(8) -0.0025(7) 0.0012(8) C6 0.0201(9) 0.0204(8) 0.0163(8) 0.0006(7) 0.0001(7) -0.0002(7) C7 0.0197(9) 0.0236(9) 0.0173(8) 0.0007(7) 0.0029(7) -0.0006(7) C8 0.0181(8) 0.0212(9) 0.0193(9) -0.0007(7) 0.0014(7) -0.0004(7) C9 0.0204(9) 0.0292(10) 0.0156(8) -0.0013(7) -0.0018(7) 0.0004(8) C10 0.0191(9) 0.0237(9) 0.0167(8) -0.0013(7) 0.0006(7) -0.0004(7) C11 0.0151(8) 0.0297(10) 0.0182(8) -0.0011(7) 0.0008(7) 0.0008(7) C12 0.0168(8) 0.0254(9) 0.0173(9) 0.0010(7) 0.0002(7) 0.0015(7) C13 0.0197(9) 0.0357(11) 0.0185(9) -0.0004(8) -0.0010(7) -0.0035(8) C14 0.0170(9) 0.0381(11) 0.0254(10) 0.0015(9) 0.0013(8) -0.0034(8) C15 0.0182(9) 0.0366(11) 0.0194(9) 0.0004(8) 0.0047(7) -0.0006(8) C16 0.0171(9) 0.0255(9) 0.0224(9) -0.0006(7) 0.0009(7) 0.0000(7) C17 0.0239(10) 0.0528(14) 0.0208(10) -0.0006(9) -0.0001(8) 0.0036(10) C18 0.0218(10) 0.0520(14) 0.0255(10) 0.0009(10) 0.0067(8) 0.0035(10) C19 0.0180(9) 0.0250(10) 0.0358(11) 0.0025(8) 0.0011(8) 0.0021(8) C20 0.0215(10) 0.0452(13) 0.0297(11) 0.0097(10) -0.0022(8) 0.0029(9) C21 0.0224(10) 0.0466(13) 0.0238(10) 0.0081(9) 0.0022(8) 0.0018(9) N4 0.0172(8) 0.0490(12) 0.0431(11) 0.0086(10) 0.0025(8) 0.0045(8) C22 0.0201(10) 0.0544(16) 0.0620(17) 0.0129(13) 0.0139(11) 0.0067(11) C23 0.0224(11) 0.0482(15) 0.0557(16) -0.0080(12) -0.0103(11) 0.0083(10) N30 0.0182(8) 0.0345(9) 0.0248(9) 0.0040(7) 0.0003(7) 0.0046(7) C30 0.0154(8) 0.0296(10) 0.0205(9) 0.0011(8) 0.0023(7) -0.0007(7) S30 0.0223(2) 0.0373(3) 0.0352(3) 0.0127(2) -0.0054(2) 0.0026(2) N40 0.0189(8) 0.0394(10) 0.0230(8) 0.0035(7) -0.0007(7) 0.0063(7) C40 0.0191(9) 0.0341(11) 0.0203(9) 0.0023(8) 0.0035(7) 0.0015(8) S40 0.0275(3) 0.0685(5) 0.0420(3) 0.0279(3) 0.0030(2) 0.0171(3) O50 0.0210(7) 0.0344(8) 0.0270(7) -0.0071(6) -0.0005(6) 0.0034(6) C50 0.0357(12) 0.0407(13) 0.0332(12) -0.0102(10) 0.0011(10) 0.0102(10) O60 0.0206(7) 0.0335(8) 0.0455(10) -0.0118(7) 0.0002(7) -0.0006(6) C60 0.0494(15) 0.0344(12) 0.0380(13) -0.0050(10) -0.0085(12) 0.0101(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N40 2.0627(17) . ? Co1 N30 2.0755(17) . ? Co1 O60 2.1057(16) . ? Co1 O50 2.1093(16) . ? Co1 N3 2.1658(16) 2_554 ? Co1 N1 2.1677(16) . ? N1 C5 1.344(3) . ? N1 C1 1.347(2) . ? N2 C10 1.339(2) . ? N2 C6 1.347(2) . ? N3 C15 1.338(3) . ? N3 C11 1.345(2) . ? N3 Co1 2.1658(16) 2 ? C1 C2 1.386(3) . ? C1 H1A 0.9500 . ? C2 C3 1.400(3) . ? C2 C6 1.487(2) . ? C3 C4 1.380(3) . ? C3 H3A 0.9500 . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.389(3) . ? C7 C8 1.399(3) . ? C7 H7A 0.9500 . ? C8 C9 1.395(3) . ? C8 C16 1.483(3) . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C12 1.487(3) . ? C11 C12 1.385(3) . ? C11 H11A 0.9500 . ? C12 C13 1.394(3) . ? C13 C14 1.380(3) . ? C13 H13A 0.9500 . ? C14 C15 1.378(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.389(3) . ? C16 C21 1.394(3) . ? C17 C18 1.380(3) . ? C17 H17A 0.9500 . ? C18 C19 1.398(3) . ? C18 H18A 0.9500 . ? C19 N4 1.373(3) . ? C19 C20 1.401(3) . ? C20 C21 1.386(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? N4 C23 1.455(3) . ? N4 C22 1.459(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N30 C30 1.158(3) . ? C30 S30 1.632(2) . ? N40 C40 1.152(3) . ? C40 S40 1.631(2) . ? O50 C50 1.431(3) . ? O50 H50 0.80(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O60 C60 1.416(3) . ? O60 H60 0.80(3) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 N40 Co1 N30 178.30(7) . . ? N40 Co1 O60 86.77(7) . . ? N30 Co1 O60 92.48(7) . . ? N40 Co1 O50 91.29(7) . . ? N30 Co1 O50 89.50(7) . . ? O60 Co1 O50 177.41(7) . . ? N40 Co1 N3 89.20(7) . 2_554 ? N30 Co1 N3 89.32(7) . 2_554 ? O60 Co1 N3 93.18(7) . 2_554 ? O50 Co1 N3 88.51(6) . 2_554 ? N40 Co1 N1 90.68(7) . . ? N30 Co1 N1 90.83(6) . . ? O60 Co1 N1 88.46(7) . . ? O50 Co1 N1 89.84(6) . . ? N3 Co1 N1 178.35(7) 2_554 . ? C5 N1 C1 117.76(17) . . ? C5 N1 Co1 119.14(13) . . ? C1 N1 Co1 123.02(13) . . ? C10 N2 C6 117.09(16) . . ? C15 N3 C11 117.70(17) . . ? C15 N3 Co1 120.38(13) . 2 ? C11 N3 Co1 121.88(13) . 2 ? N1 C1 C2 123.75(17) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 117.23(17) . . ? C1 C2 C6 123.14(17) . . ? C3 C2 C6 119.63(17) . . ? C4 C3 C2 119.51(18) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 119.21(18) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 122.54(18) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? N2 C6 C7 122.94(17) . . ? N2 C6 C2 114.57(16) . . ? C7 C6 C2 122.48(17) . . ? C6 C7 C8 120.08(17) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 116.49(17) . . ? C9 C8 C16 121.40(17) . . ? C7 C8 C16 122.10(17) . . ? C10 C9 C8 119.95(18) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C10 C9 123.43(17) . . ? N2 C10 C12 114.93(16) . . ? C9 C10 C12 121.64(17) . . ? N3 C11 C12 123.48(18) . . ? N3 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 117.67(17) . . ? C11 C12 C10 121.86(17) . . ? C13 C12 C10 120.45(17) . . ? C14 C13 C12 119.17(18) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C15 C14 C13 119.14(18) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? N3 C15 C14 122.84(18) . . ? N3 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C17 C16 C21 115.86(19) . . ? C17 C16 C8 122.01(18) . . ? C21 C16 C8 122.10(18) . . ? C18 C17 C16 122.6(2) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 C19 121.5(2) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? N4 C19 C18 121.9(2) . . ? N4 C19 C20 121.7(2) . . ? C18 C19 C20 116.41(19) . . ? C21 C20 C19 121.3(2) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C16 122.4(2) . . ? C20 C21 H21A 118.8 . . ? C16 C21 H21A 118.8 . . ? C19 N4 C23 120.9(2) . . ? C19 N4 C22 119.9(2) . . ? C23 N4 C22 116.6(2) . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C30 N30 Co1 154.56(16) . . ? N30 C30 S30 178.32(19) . . ? C40 N40 Co1 160.31(17) . . ? N40 C40 S40 177.1(2) . . ? C50 O50 Co1 126.22(14) . . ? C50 O50 H50 109(2) . . ? Co1 O50 H50 119(2) . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C60 O60 Co1 129.20(15) . . ? C60 O60 H60 110(2) . . ? Co1 O60 H60 118(2) . . ? O60 C60 H60A 109.5 . . ? O60 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O60 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.926 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.054 # Attachment '- GQ234.CIF' data_gq234moved _database_code_depnum_ccdc_archive 'CCDC 856247' #TrackingRef '- GQ234.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H30 Co N8 S2), 5(H2 O)' _chemical_formula_sum 'C88 H70 Co2 N16 O5 S4' _chemical_formula_weight 1677.72 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc 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' _cell_length_a 24.608(2) _cell_length_b 10.6168(10) _cell_length_c 17.7748(16) _cell_angle_alpha 90.00 _cell_angle_beta 116.118(6) _cell_angle_gamma 90.00 _cell_volume 4169.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42276 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 65.85 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9158 _exptl_absorpt_correction_T_max 0.9461 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45214 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3715 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+13.7151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3715 _refine_ls_number_parameters 274 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 1.0000 0.0000 0.5000 0.0304(2) Uani 1 2 d S . . N1 N 0.92967(11) 0.1279(3) 0.49767(18) 0.0362(6) Uani 1 1 d . . . N2 N 0.74009(11) 0.3794(2) 0.40370(17) 0.0324(6) Uani 1 1 d . . . N3 N 0.55590(11) 0.4671(3) 0.13756(17) 0.0316(6) Uani 1 1 d . . . C1 C 0.94206(19) 0.2333(5) 0.5403(4) 0.091(2) Uani 1 1 d . . . H1A H 0.9833 0.2517 0.5755 0.109 Uiso 1 1 calc R . . C2 C 0.89895(19) 0.3195(5) 0.5372(4) 0.091(2) Uani 1 1 d . . . H2A H 0.9109 0.3939 0.5703 0.110 Uiso 1 1 calc R . . C3 C 0.83866(14) 0.2972(3) 0.4862(2) 0.0346(7) Uani 1 1 d . . . C4 C 0.82610(14) 0.1888(3) 0.4405(2) 0.0343(7) Uani 1 1 d . . . H4A H 0.7854 0.1696 0.4028 0.041 Uiso 1 1 calc R . . C5 C 0.87156(14) 0.1071(3) 0.4482(2) 0.0348(7) Uani 1 1 d . . . H5A H 0.8608 0.0315 0.4163 0.042 Uiso 1 1 calc R . . C6 C 0.78929(13) 0.3861(3) 0.4773(2) 0.0335(7) Uani 1 1 d . . . C7 C 0.79452(14) 0.4690(3) 0.5397(2) 0.0350(7) Uani 1 1 d . . . H7A H 0.8306 0.4711 0.5907 0.042 Uiso 1 1 calc R . . C8 C 0.74672(14) 0.5500(3) 0.5281(2) 0.0325(7) Uani 1 1 d . . . C9 C 0.69619(14) 0.5434(3) 0.4509(2) 0.0332(7) Uani 1 1 d . . . H9A H 0.6625 0.5967 0.4395 0.040 Uiso 1 1 calc R . . C10 C 0.69484(13) 0.4602(3) 0.3909(2) 0.0314(7) Uani 1 1 d . . . C11 C 0.59765(16) 0.3764(3) 0.1662(2) 0.0430(8) Uani 1 1 d . . . H11A H 0.5972 0.3136 0.1279 0.052 Uiso 1 1 calc R . . C12 C 0.64101(16) 0.3686(3) 0.2473(2) 0.0430(8) Uani 1 1 d . . . H12A H 0.6692 0.3010 0.2641 0.052 Uiso 1 1 calc R . . C13 C 0.64386(13) 0.4585(3) 0.3048(2) 0.0309(7) Uani 1 1 d . . . C14 C 0.59970(17) 0.5495(4) 0.2767(2) 0.0483(9) Uani 1 1 d . . . H14A H 0.5984 0.6118 0.3142 0.058 Uiso 1 1 calc R . . C15 C 0.55745(17) 0.5503(4) 0.1946(2) 0.0477(9) Uani 1 1 d . . . H15A H 0.5274 0.6142 0.1772 0.057 Uiso 1 1 calc R . . C16 C 0.74983(14) 0.6393(3) 0.5936(2) 0.0354(7) Uani 1 1 d . . . C17 C 0.79251(19) 0.6264(5) 0.6758(2) 0.0591(12) Uani 1 1 d . . . H17A H 0.8197 0.5571 0.6913 0.071 Uiso 1 1 calc R . . C18 C 0.7962(2) 0.7132(6) 0.7360(3) 0.0717(15) Uani 1 1 d . . . H18A H 0.8264 0.7037 0.7920 0.086 Uiso 1 1 calc R . . C19 C 0.75662(19) 0.8129(4) 0.7155(2) 0.0527(10) Uani 1 1 d . . . H19A H 0.7596 0.8728 0.7569 0.063 Uiso 1 1 calc R . . C20 C 0.71291(18) 0.8248(4) 0.6348(2) 0.0461(9) Uani 1 1 d . . . H20A H 0.6848 0.8923 0.6203 0.055 Uiso 1 1 calc R . . C21 C 0.70953(15) 0.7395(3) 0.5746(2) 0.0378(7) Uani 1 1 d . . . H21A H 0.6790 0.7492 0.5188 0.045 Uiso 1 1 calc R . . S100 S 1.06783(5) 0.33589(10) 0.38464(7) 0.0533(3) Uani 1 1 d . . . N100 N 1.04293(12) 0.1504(3) 0.47530(18) 0.0361(6) Uani 1 1 d . . . C100 C 1.05327(13) 0.2301(3) 0.4392(2) 0.0329(7) Uani 1 1 d . . . O200 O 0.9276(5) 0.4861(14) 0.8605(13) 0.199(10) Uani 0.50 1 d P A 1 O300 O 0.9397(5) 0.4957(15) 0.7996(14) 0.202(9) Uani 0.50 1 d PD B 2 O400 O 1.0000 0.308(3) 0.7500 0.31(2) Uani 0.50 2 d SPD C 3 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 0.0169(3) 0.0267(3) 0.0354(4) 0.0008(2) 0.0005(2) -0.0009(2) N1 0.0212(13) 0.0320(14) 0.0415(15) -0.0001(12) 0.0012(11) 0.0020(11) N2 0.0208(12) 0.0303(14) 0.0375(14) 0.0067(11) 0.0048(11) 0.0019(10) N3 0.0208(12) 0.0315(13) 0.0343(14) 0.0028(11) 0.0046(11) 0.0021(10) C1 0.0253(19) 0.065(3) 0.122(4) -0.053(3) -0.024(2) 0.0134(19) C2 0.031(2) 0.059(3) 0.126(5) -0.053(3) -0.018(2) 0.012(2) C3 0.0227(15) 0.0316(16) 0.0380(17) 0.0058(14) 0.0029(13) 0.0003(13) C4 0.0194(14) 0.0452(19) 0.0339(16) 0.0008(14) 0.0077(12) -0.0036(13) C5 0.0223(15) 0.0416(18) 0.0379(17) -0.0034(14) 0.0108(13) -0.0046(13) C6 0.0209(14) 0.0296(16) 0.0404(17) 0.0061(13) 0.0048(13) -0.0016(12) C7 0.0215(15) 0.0364(17) 0.0366(17) 0.0058(14) 0.0032(13) -0.0021(13) C8 0.0236(15) 0.0359(17) 0.0339(16) 0.0044(14) 0.0088(13) -0.0038(13) C9 0.0210(15) 0.0363(17) 0.0359(17) 0.0070(14) 0.0068(13) 0.0029(13) C10 0.0198(14) 0.0338(16) 0.0327(16) 0.0053(13) 0.0043(12) -0.0008(12) C11 0.0351(18) 0.0380(18) 0.0390(18) -0.0019(15) 0.0009(15) 0.0121(15) C12 0.0315(17) 0.0406(19) 0.0408(18) 0.0013(15) 0.0010(15) 0.0138(14) C13 0.0186(14) 0.0329(16) 0.0342(16) 0.0053(13) 0.0054(12) 0.0004(12) C14 0.043(2) 0.051(2) 0.0359(18) -0.0047(17) 0.0035(16) 0.0210(17) C15 0.0374(19) 0.053(2) 0.0395(19) 0.0033(17) 0.0046(16) 0.0253(17) C16 0.0250(15) 0.0439(19) 0.0361(17) 0.0031(14) 0.0123(13) -0.0055(14) C17 0.043(2) 0.083(3) 0.040(2) -0.005(2) 0.0075(17) 0.021(2) C18 0.055(3) 0.109(4) 0.038(2) -0.014(2) 0.0079(19) 0.021(3) C19 0.051(2) 0.071(3) 0.043(2) -0.0087(19) 0.0263(18) -0.003(2) C20 0.047(2) 0.047(2) 0.052(2) 0.0059(17) 0.0279(18) 0.0013(17) C21 0.0315(16) 0.0408(18) 0.0388(18) 0.0045(15) 0.0134(14) -0.0028(14) S100 0.0533(6) 0.0454(6) 0.0633(6) 0.0077(5) 0.0277(5) -0.0040(4) N100 0.0255(13) 0.0319(14) 0.0388(15) 0.0009(12) 0.0031(12) -0.0055(11) C100 0.0210(14) 0.0326(17) 0.0358(16) -0.0078(14) 0.0040(13) 0.0020(12) O200 0.090(8) 0.189(14) 0.34(2) 0.175(15) 0.113(12) 0.050(8) O300 0.053(6) 0.209(17) 0.30(2) 0.036(15) 0.041(10) -0.033(7) O400 0.17(2) 0.67(7) 0.067(10) 0.000 0.039(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N100 2.065(3) 5_756 ? Co1 N100 2.065(3) . ? Co1 N1 2.186(3) . ? Co1 N1 2.186(3) 5_756 ? Co1 N3 2.243(3) 8_556 ? Co1 N3 2.243(3) 4_645 ? N1 C1 1.309(5) . ? N1 C5 1.326(4) . ? N2 C6 1.337(4) . ? N2 C10 1.343(4) . ? N3 C15 1.332(5) . ? N3 C11 1.334(4) . ? N3 Co1 2.243(3) 4_655 ? C1 C2 1.384(6) . ? C1 H1A 0.9500 . ? C2 C3 1.377(5) . ? C2 H2A 0.9500 . ? C3 C4 1.364(5) . ? C3 C6 1.490(5) . ? C4 C5 1.374(5) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.377(5) . ? C7 C8 1.397(5) . ? C7 H7A 0.9500 . ? C8 C9 1.391(4) . ? C8 C16 1.477(5) . ? C9 C10 1.373(5) . ? C9 H9A 0.9500 . ? C10 C13 1.492(4) . ? C11 C12 1.368(5) . ? C11 H11A 0.9500 . ? C12 C13 1.377(5) . ? C12 H12A 0.9500 . ? C13 C14 1.373(5) . ? C14 C15 1.370(5) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.380(5) . ? C16 C21 1.391(5) . ? C17 C18 1.384(6) . ? C17 H17A 0.9500 . ? C18 C19 1.375(7) . ? C18 H18A 0.9500 . ? C19 C20 1.368(6) . ? C19 H19A 0.9500 . ? C20 C21 1.376(5) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? S100 C100 1.624(4) . ? N100 C100 1.156(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 N100 Co1 N100 180.00(16) 5_756 . ? N100 Co1 N1 90.53(11) 5_756 . ? N100 Co1 N1 89.47(11) . . ? N100 Co1 N1 89.47(11) 5_756 5_756 ? N100 Co1 N1 90.53(11) . 5_756 ? N1 Co1 N1 180.00(16) . 5_756 ? N100 Co1 N3 90.82(10) 5_756 8_556 ? N100 Co1 N3 89.18(10) . 8_556 ? N1 Co1 N3 91.39(10) . 8_556 ? N1 Co1 N3 88.61(10) 5_756 8_556 ? N100 Co1 N3 89.18(10) 5_756 4_645 ? N100 Co1 N3 90.82(10) . 4_645 ? N1 Co1 N3 88.61(10) . 4_645 ? N1 Co1 N3 91.39(10) 5_756 4_645 ? N3 Co1 N3 180.000(1) 8_556 4_645 ? C1 N1 C5 115.7(3) . . ? C1 N1 Co1 122.6(2) . . ? C5 N1 Co1 121.5(2) . . ? C6 N2 C10 117.3(3) . . ? C15 N3 C11 115.4(3) . . ? C15 N3 Co1 121.6(2) . 4_655 ? C11 N3 Co1 121.9(2) . 4_655 ? N1 C1 C2 124.3(4) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C4 C3 C2 115.7(3) . . ? C4 C3 C6 120.7(3) . . ? C2 C3 C6 123.6(3) . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? N2 C6 C7 123.0(3) . . ? N2 C6 C3 114.6(3) . . ? C7 C6 C3 122.4(3) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 116.3(3) . . ? C9 C8 C16 121.6(3) . . ? C7 C8 C16 122.1(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N2 C10 C9 123.0(3) . . ? N2 C10 C13 115.2(3) . . ? C9 C10 C13 121.8(3) . . ? N3 C11 C12 124.0(3) . . ? N3 C11 H11A 118.0 . . ? C12 C11 H11A 118.0 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 116.4(3) . . ? C14 C13 C10 122.5(3) . . ? C12 C13 C10 121.0(3) . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C15 C14 124.1(3) . . ? N3 C15 H15A 118.0 . . ? C14 C15 H15A 118.0 . . ? C17 C16 C21 117.5(3) . . ? C17 C16 C8 121.5(3) . . ? C21 C16 C8 121.0(3) . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C21 120.3(4) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C20 C21 C16 121.5(3) . . ? C20 C21 H21A 119.3 . . ? C16 C21 H21A 119.3 . . ? C100 N100 Co1 160.4(2) . . ? N100 C100 S100 176.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.789 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.082 # Attachment '- SV12.CIF' data_sv12 _database_code_depnum_ccdc_archive 'CCDC 856248' #TrackingRef '- SV12.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H13 N5, C H Cl3' _chemical_formula_sum 'C19 H14 Cl3 N5' _chemical_formula_weight 418.70 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0576(8) _cell_length_b 21.727(3) _cell_length_c 12.0929(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.978(8) _cell_angle_gamma 90.00 _cell_volume 1799.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6135 _cell_measurement_theta_min 6.42 _cell_measurement_theta_max 64.87 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9793 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29140 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.25 _reflns_number_total 4014 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.1589P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4014 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 N1 N -0.0807(2) 0.22123(6) 0.71750(13) 0.0293(3) Uani 1 1 d . . . N2 N 0.05533(19) 0.44339(6) 0.81478(11) 0.0177(3) Uani 1 1 d . . . N3 N 0.4148(2) 0.57327(6) 1.13924(11) 0.0228(3) Uani 1 1 d . . . C1 C -0.1320(3) 0.25384(8) 0.62224(16) 0.0333(4) Uani 1 1 d . . . H1A H -0.1730 0.2320 0.5525 0.040 Uiso 1 1 calc R . . C2 C -0.1301(3) 0.31750(7) 0.61737(15) 0.0285(4) Uani 1 1 d . . . H2A H -0.1697 0.3382 0.5463 0.034 Uiso 1 1 calc R . . C3 C -0.0696(2) 0.35053(7) 0.71768(13) 0.0189(3) Uani 1 1 d . . . C4 C -0.0175(3) 0.31698(7) 0.81796(14) 0.0240(3) Uani 1 1 d . . . H4A H 0.0235 0.3375 0.8891 0.029 Uiso 1 1 calc R . . C5 C -0.0258(3) 0.25340(7) 0.81358(15) 0.0276(4) Uani 1 1 d . . . H5A H 0.0097 0.2314 0.8834 0.033 Uiso 1 1 calc R . . C6 C -0.0544(2) 0.41878(7) 0.71902(13) 0.0176(3) Uani 1 1 d . . . C7 C -0.1489(2) 0.45418(7) 0.62665(12) 0.0186(3) Uani 1 1 d . . . H7A H -0.2280 0.4351 0.5608 0.022 Uiso 1 1 calc R . . C8 C -0.1270(2) 0.51797(7) 0.63132(12) 0.0167(3) Uani 1 1 d . . . C9 C -0.0114(2) 0.54337(6) 0.73075(12) 0.0170(3) Uani 1 1 d . . . H9A H 0.0081 0.5866 0.7374 0.020 Uiso 1 1 calc R . . C10 C 0.0749(2) 0.50449(7) 0.82019(12) 0.0163(3) Uani 1 1 d . . . C11 C 0.3683(2) 0.51396(7) 1.12298(13) 0.0223(3) Uani 1 1 d . . . H11A H 0.4115 0.4865 1.1851 0.027 Uiso 1 1 calc R . . C12 C 0.2613(2) 0.49000(7) 1.02161(13) 0.0201(3) Uani 1 1 d . . . H12A H 0.2339 0.4472 1.0146 0.024 Uiso 1 1 calc R . . C13 C 0.1940(2) 0.52922(7) 0.92967(12) 0.0165(3) Uani 1 1 d . . . C14 C 0.2422(3) 0.59082(7) 0.94544(13) 0.0249(3) Uani 1 1 d . . . H14A H 0.2002 0.6195 0.8851 0.030 Uiso 1 1 calc R . . C15 C 0.3523(3) 0.61011(8) 1.05017(14) 0.0287(4) Uani 1 1 d . . . H15A H 0.3855 0.6525 1.0591 0.034 Uiso 1 1 calc R . . C16 C -0.2200(2) 0.55677(7) 0.53528(12) 0.0175(3) Uani 1 1 d . . . C17 C -0.3220(2) 0.53959(7) 0.42910(13) 0.0226(3) Uani 1 1 d . . . H17A H -0.3497 0.4987 0.4021 0.027 Uiso 1 1 calc R . . C18 C -0.3067(3) 0.63889(8) 0.43998(14) 0.0279(4) Uani 1 1 d . . . H18A H -0.3245 0.6810 0.4191 0.033 Uiso 1 1 calc R . . N4 N -0.2109(2) 0.62000(6) 0.54127(12) 0.0272(3) Uani 1 1 d . . . N5 N -0.3764(2) 0.59223(6) 0.36941(11) 0.0224(3) Uani 1 1 d . . . H5B H -0.4441 0.5951 0.2982 0.027 Uiso 1 1 calc R . . C100 C 0.6046(3) 0.67595(7) 0.73463(15) 0.0273(3) Uani 1 1 d . . . H10A H 0.7197 0.6630 0.7057 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.41177(8) 0.62372(2) 0.68538(4) 0.03813(13) Uani 1 1 d . . . Cl2 Cl 0.53402(8) 0.74998(2) 0.68461(5) 0.04433(15) Uani 1 1 d . . . Cl3 Cl 0.67049(9) 0.67624(2) 0.88429(4) 0.04517(15) 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 N1 0.0395(8) 0.0163(6) 0.0315(8) -0.0021(6) 0.0071(6) -0.0018(6) N2 0.0203(6) 0.0149(6) 0.0158(6) -0.0002(5) 0.0003(5) 0.0005(5) N3 0.0252(7) 0.0252(7) 0.0143(6) -0.0014(5) -0.0022(5) 0.0008(5) C1 0.0494(11) 0.0193(8) 0.0271(9) -0.0066(7) 0.0011(8) -0.0045(7) C2 0.0419(10) 0.0186(7) 0.0206(8) -0.0015(6) -0.0009(7) -0.0019(7) C3 0.0204(7) 0.0144(7) 0.0205(7) -0.0014(6) 0.0019(6) -0.0004(5) C4 0.0308(8) 0.0174(7) 0.0212(7) -0.0016(6) 0.0012(6) 0.0009(6) C5 0.0369(9) 0.0184(7) 0.0260(8) 0.0034(6) 0.0048(7) 0.0024(7) C6 0.0193(7) 0.0151(7) 0.0173(7) -0.0014(5) 0.0024(5) 0.0003(5) C7 0.0213(7) 0.0176(7) 0.0142(6) -0.0033(5) -0.0011(5) -0.0017(6) C8 0.0179(7) 0.0167(7) 0.0140(6) -0.0001(5) 0.0012(5) 0.0010(5) C9 0.0209(7) 0.0137(6) 0.0149(7) -0.0002(5) 0.0011(5) -0.0004(5) C10 0.0172(6) 0.0161(6) 0.0143(6) -0.0012(5) 0.0011(5) -0.0004(5) C11 0.0240(8) 0.0252(8) 0.0150(7) 0.0046(6) -0.0008(6) 0.0015(6) C12 0.0232(7) 0.0174(7) 0.0175(7) 0.0033(6) 0.0006(6) -0.0001(6) C13 0.0179(7) 0.0170(7) 0.0128(6) -0.0008(5) 0.0005(5) 0.0013(5) C14 0.0373(9) 0.0169(7) 0.0146(7) 0.0014(5) -0.0052(6) -0.0011(6) C15 0.0420(10) 0.0176(7) 0.0202(8) -0.0024(6) -0.0048(7) -0.0029(7) C16 0.0208(7) 0.0160(7) 0.0139(7) -0.0010(5) 0.0007(6) -0.0010(5) C17 0.0284(8) 0.0187(7) 0.0167(7) -0.0015(6) -0.0023(6) -0.0002(6) C18 0.0403(10) 0.0187(7) 0.0192(8) 0.0032(6) -0.0036(7) -0.0013(7) N4 0.0424(8) 0.0162(6) 0.0168(6) 0.0007(5) -0.0050(6) -0.0020(6) N5 0.0264(7) 0.0230(6) 0.0131(6) 0.0009(5) -0.0043(5) -0.0005(5) C100 0.0335(9) 0.0188(7) 0.0264(8) 0.0034(6) 0.0007(7) 0.0017(6) Cl1 0.0446(3) 0.0275(2) 0.0382(3) -0.00528(18) 0.0019(2) -0.00756(18) Cl2 0.0462(3) 0.0243(2) 0.0570(3) 0.0166(2) 0.0018(2) 0.00519(19) Cl3 0.0577(3) 0.0440(3) 0.0275(2) 0.00524(19) -0.0021(2) -0.0124(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 C1 1.326(2) . ? N1 C5 1.331(2) . ? N2 C10 1.3346(19) . ? N2 C6 1.3392(19) . ? N3 C15 1.329(2) . ? N3 C11 1.333(2) . ? C1 C2 1.384(2) . ? C1 H1A 0.9500 . ? C2 C3 1.385(2) . ? C2 H2A 0.9500 . ? C3 C4 1.386(2) . ? C3 C6 1.486(2) . ? C4 C5 1.383(2) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.387(2) . ? C7 C8 1.394(2) . ? C7 H7A 0.9500 . ? C8 C9 1.394(2) . ? C8 C16 1.457(2) . ? C9 C10 1.392(2) . ? C9 H9A 0.9500 . ? C10 C13 1.4868(19) . ? C11 C12 1.377(2) . ? C11 H11A 0.9500 . ? C12 C13 1.390(2) . ? C12 H12A 0.9500 . ? C13 C14 1.383(2) . ? C14 C15 1.381(2) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.364(2) . ? C16 N4 1.3764(19) . ? C17 N5 1.357(2) . ? C17 H17A 0.9500 . ? C18 N4 1.313(2) . ? C18 N5 1.340(2) . ? C18 H18A 0.9500 . ? N5 H5B 0.8800 . ? C100 Cl2 1.7480(17) . ? C100 Cl3 1.7565(18) . ? C100 Cl1 1.7615(18) . ? C100 H10A 1.0000 . ? 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 C1 N1 C5 116.02(14) . . ? C10 N2 C6 118.10(13) . . ? C15 N3 C11 116.17(14) . . ? N1 C1 C2 124.56(16) . . ? N1 C1 H1A 117.7 . . ? C2 C1 H1A 117.7 . . ? C1 C2 C3 118.98(16) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C2 C3 C4 117.00(14) . . ? C2 C3 C6 122.18(14) . . ? C4 C3 C6 120.79(14) . . ? C5 C4 C3 119.47(15) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 123.96(16) . . ? N1 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? N2 C6 C7 122.69(14) . . ? N2 C6 C3 115.65(13) . . ? C7 C6 C3 121.66(13) . . ? C6 C7 C8 119.43(13) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 117.70(13) . . ? C9 C8 C16 121.05(13) . . ? C7 C8 C16 121.25(13) . . ? C10 C9 C8 119.03(13) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? N2 C10 C9 123.03(13) . . ? N2 C10 C13 115.64(13) . . ? C9 C10 C13 121.32(13) . . ? N3 C11 C12 124.01(14) . . ? N3 C11 H11A 118.0 . . ? C12 C11 H11A 118.0 . . ? C11 C12 C13 119.22(14) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 117.25(14) . . ? C14 C13 C10 122.68(13) . . ? C12 C13 C10 120.07(13) . . ? C15 C14 C13 119.03(14) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? N3 C15 C14 124.31(15) . . ? N3 C15 H15A 117.8 . . ? C14 C15 H15A 117.8 . . ? C17 C16 N4 109.27(13) . . ? C17 C16 C8 128.75(14) . . ? N4 C16 C8 121.96(13) . . ? N5 C17 C16 106.68(13) . . ? N5 C17 H17A 126.7 . . ? C16 C17 H17A 126.7 . . ? N4 C18 N5 112.62(14) . . ? N4 C18 H18A 123.7 . . ? N5 C18 H18A 123.7 . . ? C18 N4 C16 104.82(13) . . ? C18 N5 C17 106.60(13) . . ? C18 N5 H5B 126.7 . . ? C17 N5 H5B 126.7 . . ? Cl2 C100 Cl3 109.62(9) . . ? Cl2 C100 Cl1 110.09(10) . . ? Cl3 C100 Cl1 109.96(10) . . ? Cl2 C100 H10A 109.1 . . ? Cl3 C100 H10A 109.1 . . ? Cl1 C100 H10A 109.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.507 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.050