Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Mark Murrie' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Alan Ferguson' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Kyle W. Galloway' '' '' 'Suzanne M. Harte' '' '' 'Andrew Parkin' '' '' _publ_contact_author_name 'Mark Murrie' _publ_contact_author_address ; Department of Chemistry University of Glasgow University Avenue Glasgow G12 8QQ UNITED KINGDOM ; _publ_contact_author_email MARKM@CHEM.GLA.AC.UK _publ_section_title ; Tuning the structural motif by tuning the countercation size: from double salts to a 1D coordination polymer ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures have been sent by mail. ; _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' # Attachment 'murrie.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 294936' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.80 _oxford_structure_analysis_title 'ap75 in P 21/a' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.9580(5) _cell_length_b 14.1660(4) _cell_length_c 12.1050(4) _cell_angle_alpha 90 _cell_angle_beta 99.174(2) _cell_angle_gamma 90 _cell_volume 2532.18(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? 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' 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' 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' 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' 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' _cell_formula_units_Z 4 # Given Formula = C6 H12 Co1 N4 O6 S2 # Dc = 0.94 Fooo = 1236.00 Mu = 8.57 M = 359.25 # Found Formula = C8 H44 Co1 N2 O18 S2 # Dc = 1.52 FOOO = 1236.00 Mu = 9.19 M = 579.51 _chemical_formula_sum 'C8 H44 Co1 N2 O18 S2' _chemical_formula_moiety 'C8 H44 Co1 N2 O18 S2' _chemical_compound_source ? _chemical_formula_weight 579.51 _cell_measurement_reflns_used 13803 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 100 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.919 # Sheldrick geometric approximatio 0.58 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.91 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 100 _diffrn_reflns_number 30961 _reflns_number_total 5999 _diffrn_reflns_av_R_equivalents 0.085 # Number of reflections with Friedels Law is 5999 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6019 _diffrn_reflns_theta_min 1.379 _diffrn_reflns_theta_max 27.841 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.841 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.88 _oxford_diffrn_Wilson_scale 22.89 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.21 _refine_diff_density_max 0.99 _refine_ls_number_reflns 5999 _refine_ls_number_restraints 44 _refine_ls_number_parameters 417 #_refine_ls_R_factor_ref 0.0718 _refine_ls_wR_factor_ref 0.0651 _refine_ls_goodness_of_fit_ref 0.6573 #_reflns_number_all 5999 _refine_ls_R_factor_all 0.0718 _refine_ls_wR_factor_all 0.0651 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 3566 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_gt 0.0591 _refine_ls_shift/su_max 0.000723 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(F^2^) + 0.00 + 0.00P] where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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. Sheldrick, G.M. (1997). SHELXL-97. University of G\"ottingen, Germany. 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 0.80323(2) -0.11169(2) 0.11026(3) 0.0105 1.0000 Uani . . . . . . O1 O 0.69610(11) -0.03144(12) 0.03046(14) 0.0158 1.0000 Uani D . . . . . O2 O 0.80496(11) -0.20147(13) -0.03049(15) 0.0172 1.0000 Uani D . . . . . O3 O 0.71242(12) -0.20769(12) 0.15989(14) 0.0172 1.0000 Uani D . . . . . O4 O 0.79784(11) -0.03131(12) 0.25818(14) 0.0144 1.0000 Uani D . . . . . O5 O 0.91610(11) -0.17708(13) 0.19623(14) 0.0177 1.0000 Uani D . . . . . O6 O 0.88819(12) -0.02657(12) 0.03241(15) 0.0181 1.0000 Uani D . . . . . S1 S 0.60546(4) -0.14094(4) 0.40364(5) 0.0113 1.0000 Uani . . . . . . O11 O 0.62452(11) -0.14976(11) 0.52680(13) 0.0180 1.0000 Uani . . . . . . O12 O 0.64521(10) -0.05262(11) 0.36901(13) 0.0149 1.0000 Uani . . . . . . O13 O 0.64863(10) -0.22275(11) 0.35419(13) 0.0130 1.0000 Uani . . . . . . O14 O 0.50775(10) -0.14317(11) 0.36379(14) 0.0177 1.0000 Uani . . . . . . S2 S 1.03510(4) -0.22930(4) -0.03267(5) 0.0114 1.0000 Uani . . . . . . O21 O 1.11645(10) -0.25645(11) -0.07901(13) 0.0164 1.0000 Uani . . . . . . O22 O 1.00899(10) -0.13102(11) -0.06534(13) 0.0150 1.0000 Uani . . . . . . O23 O 0.95810(10) -0.29265(11) -0.07609(13) 0.0144 1.0000 Uani . . . . . . O24 O 1.05281(11) -0.23679(12) 0.09078(13) 0.0169 1.0000 Uani . . . . . . N3 N 1.12071(13) 0.01615(13) 0.34045(16) 0.0134 1.0000 Uani . . . . . . C31 C 1.13952(19) -0.06063(19) 0.2625(2) 0.0202 1.0000 Uani D . . . . . C32 C 1.02063(17) 0.0262(2) 0.3372(2) 0.0221 1.0000 Uani D . . . . . C33 C 1.15841(19) 0.10730(19) 0.3047(2) 0.0228 1.0000 Uani D . . . . . C34 C 1.16408(19) -0.0069(2) 0.4572(2) 0.0206 1.0000 Uani D . . . . . N4 N 0.37570(13) -0.27417(14) 0.56605(16) 0.0145 1.0000 Uani . . . . . . C41 C 0.33776(18) -0.2615(2) 0.4450(2) 0.0219 1.0000 Uani D . . . . . C42 C 0.46199(18) -0.3301(2) 0.5757(2) 0.0226 1.0000 Uani D . . . . . C43 C 0.3958(2) -0.1801(2) 0.6202(3) 0.0317 1.0000 Uani D . . . . . C44 C 0.3087(2) -0.3265(2) 0.6230(2) 0.0230 1.0000 Uani D . . . . . O51 O 0.59195(12) -0.40618(12) 0.34220(15) 0.0189 1.0000 Uani D . . . . . O52 O 0.37665(12) -0.00535(13) 0.33868(15) 0.0196 1.0000 Uani D . . . . . O53 O 0.58225(12) 0.02833(13) 0.16508(15) 0.0193 1.0000 Uani D . . . . . O54 O 1.17128(12) -0.34214(12) 0.24271(15) 0.0184 1.0000 Uani D . . . . . H11 H 0.6554(16) -0.015(2) 0.070(2) 0.050(3) 1.0000 Uiso D . . . . . H12 H 0.6619(18) -0.053(2) -0.0318(18) 0.050(3) 1.0000 Uiso D . . . . . H21 H 0.7541(15) -0.2294(19) -0.065(2) 0.050(3) 1.0000 Uiso D . . . . . H22 H 0.8476(16) -0.2380(18) -0.044(3) 0.050(3) 1.0000 Uiso D . . . . . H31 H 0.6878(19) -0.214(2) 0.2210(18) 0.050(3) 1.0000 Uiso D . . . . . H32 H 0.6821(18) -0.2520(17) 0.116(2) 0.050(3) 1.0000 Uiso D . . . . . H41 H 0.7516(15) -0.037(2) 0.293(2) 0.050(3) 1.0000 Uiso D . . . . . H42 H 0.805(2) 0.0301(12) 0.256(2) 0.050(3) 1.0000 Uiso D . . . . . H51 H 0.9616(15) -0.197(2) 0.165(2) 0.050(3) 1.0000 Uiso D . . . . . H52 H 0.929(2) -0.186(2) 0.2694(15) 0.050(3) 1.0000 Uiso D . . . . . H61 H 0.9141(19) 0.0287(14) 0.051(2) 0.050(3) 1.0000 Uiso D . . . . . H62 H 0.9277(17) -0.059(2) 0.002(2) 0.050(3) 1.0000 Uiso D . . . . . H311 H 1.1166(16) -0.1207(13) 0.2888(19) 0.025(2) 1.0000 Uiso D . . . . . H312 H 1.1076(15) -0.0460(17) 0.1880(15) 0.025(2) 1.0000 Uiso D . . . . . H313 H 1.2075(11) -0.0665(17) 0.269(2) 0.025(2) 1.0000 Uiso D . . . . . H321 H 1.0081(16) 0.0793(14) 0.3891(18) 0.025(2) 1.0000 Uiso D . . . . . H322 H 0.9982(16) -0.0361(13) 0.3614(19) 0.025(2) 1.0000 Uiso D . . . . . H323 H 0.9943(16) 0.0404(17) 0.2610(14) 0.025(2) 1.0000 Uiso D . . . . . H331 H 1.1497(16) 0.1551(15) 0.3592(17) 0.025(2) 1.0000 Uiso D . . . . . H332 H 1.2247(11) 0.0954(17) 0.3044(19) 0.025(2) 1.0000 Uiso D . . . . . H333 H 1.1241(15) 0.1216(17) 0.2317(15) 0.025(2) 1.0000 Uiso D . . . . . H341 H 1.1515(16) 0.0446(14) 0.5061(18) 0.025(2) 1.0000 Uiso D . . . . . H342 H 1.2302(11) -0.0062(17) 0.460(2) 0.025(2) 1.0000 Uiso D . . . . . H343 H 1.1412(16) -0.0689(13) 0.478(2) 0.025(2) 1.0000 Uiso D . . . . . H411 H 0.3809(15) -0.2209(15) 0.4095(19) 0.027(2) 1.0000 Uiso D . . . . . H412 H 0.3315(17) -0.3232(13) 0.4092(19) 0.027(2) 1.0000 Uiso D . . . . . H413 H 0.2813(13) -0.2246(16) 0.441(2) 0.027(2) 1.0000 Uiso D . . . . . H421 H 0.4862(16) -0.3378(17) 0.6571(14) 0.027(2) 1.0000 Uiso D . . . . . H422 H 0.4497(17) -0.3926(13) 0.5411(19) 0.027(2) 1.0000 Uiso D . . . . . H423 H 0.5063(14) -0.2954(16) 0.5382(19) 0.027(2) 1.0000 Uiso D . . . . . H431 H 0.3419(13) -0.1410(16) 0.611(2) 0.027(2) 1.0000 Uiso D . . . . . H432 H 0.4230(16) -0.1905(17) 0.6982(15) 0.027(2) 1.0000 Uiso D . . . . . H433 H 0.4391(15) -0.1423(16) 0.5844(19) 0.027(2) 1.0000 Uiso D . . . . . H441 H 0.2570(13) -0.2860(16) 0.621(2) 0.027(2) 1.0000 Uiso D . . . . . H442 H 0.3401(16) -0.3386(17) 0.7013(15) 0.027(2) 1.0000 Uiso D . . . . . H443 H 0.2959(16) -0.3890(13) 0.5845(19) 0.027(2) 1.0000 Uiso D . . . . . H511 H 0.6049(19) -0.3452(13) 0.336(2) 0.045(3) 1.0000 Uiso D . . . . . H512 H 0.6028(19) -0.432(2) 0.2807(18) 0.045(3) 1.0000 Uiso D . . . . . H521 H 0.4227(15) -0.0433(17) 0.353(2) 0.045(3) 1.0000 Uiso D . . . . . H522 H 0.385(2) 0.0339(17) 0.3933(19) 0.045(3) 1.0000 Uiso D . . . . . H531 H 0.5938(19) 0.0044(19) 0.2308(16) 0.045(3) 1.0000 Uiso D . . . . . H532 H 0.5272(13) 0.051(2) 0.159(2) 0.045(3) 1.0000 Uiso D . . . . . H541 H 1.1383(18) -0.3129(19) 0.1858(19) 0.045(3) 1.0000 Uiso D . . . . . H542 H 1.1562(19) -0.318(2) 0.3021(18) 0.045(3) 1.0000 Uiso 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 Co1 0.00927(16) 0.01176(17) 0.01104(17) -0.00032(15) 0.00291(12) -0.00061(14) O1 0.0147(10) 0.0194(10) 0.0139(10) -0.0007(8) 0.0037(7) 0.0053(8) O2 0.0105(9) 0.0225(10) 0.0188(10) -0.0096(8) 0.0029(8) -0.0031(8) O3 0.0205(10) 0.0179(10) 0.0153(10) -0.0041(8) 0.0094(8) -0.0081(8) O4 0.0163(9) 0.0144(9) 0.0134(9) -0.0021(8) 0.0049(7) -0.0003(8) O5 0.0146(9) 0.0281(11) 0.0105(9) -0.0006(8) 0.0026(8) 0.0059(8) O6 0.0190(10) 0.0127(10) 0.0254(11) -0.0034(8) 0.0123(8) -0.0043(8) S1 0.0114(3) 0.0126(3) 0.0103(3) 0.0008(3) 0.0032(2) 0.0013(2) O11 0.0272(10) 0.0171(9) 0.0102(9) 0.0021(8) 0.0039(8) 0.0058(8) O12 0.0165(9) 0.0132(9) 0.0156(9) 0.0018(7) 0.0045(7) -0.0018(7) O13 0.0133(9) 0.0133(9) 0.0131(9) -0.0005(7) 0.0045(7) 0.0038(7) O14 0.0096(8) 0.0188(9) 0.0243(10) 0.0013(8) 0.0017(7) 0.0018(7) S2 0.0107(3) 0.0120(3) 0.0119(3) -0.0010(3) 0.0032(2) 0.0003(2) O21 0.0118(9) 0.0188(10) 0.0203(10) -0.0009(8) 0.0079(7) 0.0036(7) O22 0.0151(9) 0.0107(9) 0.0200(9) 0.0005(7) 0.0055(7) 0.0008(7) O23 0.0147(9) 0.0134(9) 0.0155(9) -0.0023(7) 0.0038(7) -0.0045(7) O24 0.0160(9) 0.0234(10) 0.0110(9) -0.0016(8) 0.0014(7) 0.0045(8) N3 0.0132(11) 0.0125(11) 0.0140(11) -0.0002(9) 0.0006(9) -0.0004(9) C31 0.0275(16) 0.0148(14) 0.0193(15) -0.0037(12) 0.0070(12) 0.0027(12) C32 0.0118(14) 0.0308(17) 0.0230(16) -0.0019(14) 0.0010(12) 0.0041(12) C33 0.0256(15) 0.0136(14) 0.0281(16) 0.0044(13) 0.0010(13) -0.0057(13) C34 0.0268(16) 0.0203(15) 0.0129(14) 0.0012(12) -0.0019(12) -0.0018(13) N4 0.0174(11) 0.0122(11) 0.0145(11) -0.0013(9) 0.0042(9) -0.0009(9) C41 0.0170(14) 0.0286(17) 0.0188(15) 0.0073(13) -0.0005(12) 0.0002(13) C42 0.0144(14) 0.0290(17) 0.0235(16) 0.0050(13) -0.0001(12) 0.0037(12) C43 0.041(2) 0.0192(16) 0.0357(19) -0.0118(15) 0.0088(16) -0.0062(14) C44 0.0260(16) 0.0219(15) 0.0239(16) 0.0020(13) 0.0124(13) -0.0026(13) O51 0.0191(10) 0.0201(11) 0.0173(10) -0.0007(8) 0.0027(8) -0.0058(8) O52 0.0183(10) 0.0214(11) 0.0186(10) -0.0037(8) 0.0013(8) 0.0054(8) O53 0.0159(10) 0.0276(11) 0.0155(10) 0.0066(8) 0.0055(8) 0.0081(8) O54 0.0200(10) 0.0193(11) 0.0162(10) 0.0007(8) 0.0036(8) 0.0052(8) _refine_ls_extinction_coef 51(7) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _oxford_refine_ls_scale 0.19067(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 . O1 . 2.0735(17) yes Co1 . O2 . 2.1296(17) yes Co1 . O3 . 2.0774(17) yes Co1 . O4 . 2.1343(17) yes Co1 . O5 . 2.0569(17) yes Co1 . O6 . 2.0829(17) yes O1 . H11 . 0.865(17) no O1 . H12 . 0.894(17) no O2 . H21 . 0.901(16) no O2 . H22 . 0.858(17) no O3 . H31 . 0.882(17) no O3 . H32 . 0.898(16) no O4 . H41 . 0.870(17) no O4 . H42 . 0.877(17) no O5 . H51 . 0.879(17) no O5 . H52 . 0.884(17) no O6 . H61 . 0.886(17) no O6 . H62 . 0.869(17) no S1 . O11 . 1.4778(16) yes S1 . O12 . 1.4744(17) yes S1 . O13 . 1.4973(16) yes S1 . O14 . 1.4646(16) yes S2 . O21 . 1.4701(16) yes S2 . O22 . 1.4826(16) yes S2 . O23 . 1.4882(16) yes S2 . O24 . 1.4793(16) yes N3 . C31 . 1.496(3) yes N3 . C32 . 1.498(3) yes N3 . C33 . 1.500(3) yes N3 . C34 . 1.494(3) yes C31 . H311 . 0.989(16) no C31 . H312 . 0.973(15) no C31 . H313 . 1.010(16) no C32 . H321 . 1.016(16) no C32 . H322 . 1.004(16) no C32 . H323 . 0.965(15) no C33 . H331 . 0.969(16) no C33 . H332 . 1.007(15) no C33 . H333 . 0.970(15) no C34 . H341 . 0.976(16) no C34 . H342 . 0.984(16) no C34 . H343 . 0.991(16) no N4 . C41 . 1.496(3) yes N4 . C42 . 1.503(3) yes N4 . C43 . 1.494(3) yes N4 . C44 . 1.500(3) yes C41 . H411 . 1.010(16) no C41 . H412 . 0.974(16) no C41 . H413 . 0.988(16) no C42 . H421 . 1.001(16) no C42 . H422 . 0.985(16) no C42 . H423 . 0.990(16) no C43 . H431 . 0.969(16) no C43 . H432 . 0.978(16) no C43 . H433 . 0.993(16) no C44 . H441 . 0.960(16) no C44 . H442 . 1.003(15) no C44 . H443 . 1.005(16) no O51 . H511 . 0.891(16) no O51 . H512 . 0.868(17) no O52 . H521 . 0.869(16) no O52 . H522 . 0.858(16) no O53 . H531 . 0.857(16) no O53 . H532 . 0.873(16) no O54 . H541 . 0.884(16) no O54 . H542 . 0.858(17) 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 O1 . Co1 . O2 . 93.54(7) yes O1 . Co1 . O3 . 90.07(7) yes O2 . Co1 . O3 . 86.12(7) yes O1 . Co1 . O4 . 88.20(7) yes O2 . Co1 . O4 . 175.36(7) yes O3 . Co1 . O4 . 89.58(7) yes O1 . Co1 . O5 . 173.50(7) yes O2 . Co1 . O5 . 91.27(7) yes O3 . Co1 . O5 . 94.62(7) yes O4 . Co1 . O5 . 87.34(7) yes O1 . Co1 . O6 . 87.36(7) yes O2 . Co1 . O6 . 84.13(7) yes O3 . Co1 . O6 . 169.73(7) yes O4 . Co1 . O6 . 100.26(7) yes O5 . Co1 . O6 . 88.79(7) yes Co1 . O1 . H11 . 116.8(20) no Co1 . O1 . H12 . 120.1(20) no H11 . O1 . H12 . 102(3) no Co1 . O2 . H21 . 121.4(19) no Co1 . O2 . H22 . 128(2) no H21 . O2 . H22 . 104(3) no Co1 . O3 . H31 . 133.5(20) no Co1 . O3 . H32 . 125.2(20) no H31 . O3 . H32 . 101(3) no Co1 . O4 . H41 . 120.2(20) no Co1 . O4 . H42 . 119(2) no H41 . O4 . H42 . 102(3) no Co1 . O5 . H51 . 123.6(20) no Co1 . O5 . H52 . 126.7(20) no H51 . O5 . H52 . 110(3) no Co1 . O6 . H61 . 132(2) no Co1 . O6 . H62 . 113(2) no H61 . O6 . H62 . 106(3) no O11 . S1 . O12 . 109.69(10) yes O11 . S1 . O13 . 108.16(9) yes O12 . S1 . O13 . 108.90(9) yes O11 . S1 . O14 . 110.63(10) yes O12 . S1 . O14 . 110.56(9) yes O13 . S1 . O14 . 108.84(9) yes O21 . S2 . O22 . 110.04(10) yes O21 . S2 . O23 . 110.40(10) yes O22 . S2 . O23 . 108.42(9) yes O21 . S2 . O24 . 109.93(9) yes O22 . S2 . O24 . 109.51(10) yes O23 . S2 . O24 . 108.51(10) yes C31 . N3 . C32 . 109.9(2) yes C31 . N3 . C33 . 109.1(2) yes C32 . N3 . C33 . 109.3(2) yes C31 . N3 . C34 . 109.9(2) yes C32 . N3 . C34 . 109.1(2) yes C33 . N3 . C34 . 109.53(19) yes N3 . C31 . H311 . 108.3(15) no N3 . C31 . H312 . 108.4(15) no H311 . C31 . H312 . 110(2) no N3 . C31 . H313 . 107.3(14) no H311 . C31 . H313 . 107.4(20) no H312 . C31 . H313 . 116(2) no N3 . C32 . H321 . 109.6(14) no N3 . C32 . H322 . 106.7(14) no H321 . C32 . H322 . 111.5(19) no N3 . C32 . H323 . 107.4(15) no H321 . C32 . H323 . 110.5(20) no H322 . C32 . H323 . 111(2) no N3 . C33 . H331 . 107.9(15) no N3 . C33 . H332 . 105.9(14) no H331 . C33 . H332 . 111.1(20) no N3 . C33 . H333 . 105.8(15) no H331 . C33 . H333 . 111(2) no H332 . C33 . H333 . 114(2) no N3 . C34 . H341 . 108.3(14) no N3 . C34 . H342 . 108.1(15) no H341 . C34 . H342 . 105.2(20) no N3 . C34 . H343 . 108.8(14) no H341 . C34 . H343 . 113(2) no H342 . C34 . H343 . 113(2) no C41 . N4 . C42 . 109.0(2) yes C41 . N4 . C43 . 109.9(2) yes C42 . N4 . C43 . 109.0(2) yes C41 . N4 . C44 . 109.4(2) yes C42 . N4 . C44 . 109.4(2) yes C43 . N4 . C44 . 109.9(2) yes N4 . C41 . H411 . 108.5(14) no N4 . C41 . H412 . 108.8(15) no H411 . C41 . H412 . 110(2) no N4 . C41 . H413 . 107.4(15) no H411 . C41 . H413 . 106.2(20) no H412 . C41 . H413 . 116(2) no N4 . C42 . H421 . 107.8(15) no N4 . C42 . H422 . 110.0(15) no H421 . C42 . H422 . 110(2) no N4 . C42 . H423 . 109.4(15) no H421 . C42 . H423 . 110.0(20) no H422 . C42 . H423 . 110(2) no N4 . C43 . H431 . 110.9(15) no N4 . C43 . H432 . 108.2(15) no H431 . C43 . H432 . 114(2) no N4 . C43 . H433 . 112.8(15) no H431 . C43 . H433 . 103(2) no H432 . C43 . H433 . 108(2) no N4 . C44 . H441 . 106.7(15) no N4 . C44 . H442 . 105.7(15) no H441 . C44 . H442 . 112(2) no N4 . C44 . H443 . 108.2(15) no H441 . C44 . H443 . 115(2) no H442 . C44 . H443 . 108.3(20) no H511 . O51 . H512 . 105(3) no H521 . O52 . H522 . 103(3) no H531 . O53 . H532 . 106(3) no H541 . O54 . H542 . 106(3) no data_2 _database_code_depnum_ccdc_archive 'CCDC 294937' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.80 _oxford_structure_analysis_title 'ap81 in P 21/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 6.9495(2) _cell_length_b 16.0265(5) _cell_length_c 14.7693(5) _cell_angle_alpha 90 _cell_angle_beta 101.867(2) _cell_angle_gamma 90 _cell_volume 1609.79(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-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' 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' 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' 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' 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' _cell_formula_units_Z 2 # Given Formula = C40 H24 Co12 N10 O12 S2 # Dc = 3.32 Fooo = 746.00 Mu = 62.42 M = 804.01 # Found Formula = C16 H60 Co1 N2 O18 S2 # Dc = 1.43 FOOO = 746.00 Mu = 7.35 M = 345.86 _chemical_formula_sum 'C16 H60 Co1 N2 O18 S2' _chemical_formula_moiety 'C16 H60 Co1 N2 O18 S2' _chemical_compound_source ? _chemical_formula_weight 691.72 _cell_measurement_reflns_used 11646 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour 'pale pink' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.55 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 0.735 # Sheldrick geometric approximatio 0.88 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 100 _diffrn_reflns_number 23078 _reflns_number_total 3812 _diffrn_reflns_av_R_equivalents 0.058 # Number of reflections with Friedels Law is 3812 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3839 _diffrn_reflns_theta_min 1.897 _diffrn_reflns_theta_max 27.873 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.873 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -9 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 1.13 _oxford_diffrn_Wilson_scale 90.23 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.98 _refine_diff_density_max 0.86 _refine_ls_number_reflns 3812 _refine_ls_number_restraints 76 _refine_ls_number_parameters 274 #_refine_ls_R_factor_ref 0.0805 _refine_ls_wR_factor_ref 0.0849 _refine_ls_goodness_of_fit_ref 0.8407 #_reflns_number_all 3812 _refine_ls_R_factor_all 0.0805 _refine_ls_wR_factor_all 0.0849 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 2408 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_gt 0.0774 _refine_ls_shift/su_max 0.000323 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refxyz # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(F^2^) + 0.00 + 0.00P] where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Because the data were collected with molybdenum radiation, there were no measurable anomalous differences, as a consequence of which it was admissible to merge Friedel pairs of reflections. All hydrogen atoms were found in difference density syntheses. Hydrogen atoms were placed geometrically after each cycle. Hydrogen atoms were placed geometrically after each cycle, the preferred orientations of those groups whose conformations could not be assigned unambiguously having been previously identified by examination of a difference Fourier map. Hydrogen atoms were seen in a difference density synthesis. Those attached to carbon atoms were repositioned geometrically. Hydrogen were initially refined with soft restraints on the bonds to regularise their geometry (bond lengths to accepted values, angles either set by symmetry or to accepted values, and U[iso] dependent upon the adjacent bonded atom), after which they were refined with riding constraints only. donated by Bill Clegg: The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93-98, O---N in the range 0.86-0.89 and O---H = 0.82 \%A) and isotropic adps (U(H) in the range 1.2-1.5 times U~equiv~ of the adjacent atom), after which they were refined with riding constraints. . ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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. Sheldrick, G.M. (1997). SHELXL-97. University of G\"ottingen, Germany. 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 0.0000 0.0000 1.0000 0.0105 1.0000 Uani S . . . . . O1 O -0.0625(3) -0.01936(12) 0.85700(13) 0.0164 1.0000 Uani D . . . . . O2 O 0.2206(3) 0.08471(12) 0.98083(12) 0.0139 1.0000 Uani D . . . . . O3 O 0.2199(3) -0.09287(12) 1.01895(13) 0.0136 1.0000 Uani D . . . . . S1 S 0.41879(10) -0.04004(4) 0.81146(4) 0.0117 1.0000 Uani . . . . . . O11 O 0.4413(3) -0.10509(11) 0.88502(12) 0.0142 1.0000 Uani . . . . . . O12 O 0.2196(2) -0.04594(12) 0.75351(12) 0.0159 1.0000 Uani . . . . . . O13 O 0.4467(3) 0.04381(12) 0.85596(12) 0.0153 1.0000 Uani . . . . . . O14 O 0.5702(3) -0.05265(12) 0.75584(12) 0.0153 1.0000 Uani . . . . . . N3 N 0.6053(3) 0.21579(14) 0.68428(15) 0.0152 1.0000 Uani D . . . . . C31 C 0.7687(4) 0.16238(18) 0.7395(2) 0.0181 1.0000 Uani D . . . . . C32 C 0.9492(5) 0.2091(2) 0.7877(2) 0.0305 1.0000 Uani D . . . . . C33 C 0.6722(4) 0.25884(18) 0.60451(19) 0.0178 1.0000 Uani D . . . . . C34 C 0.7173(4) 0.2013(2) 0.5303(2) 0.0221 1.0000 Uani D . . . . . C35 C 0.4338(4) 0.15727(18) 0.6487(2) 0.0169 1.0000 Uani D . . . . . C36 C 0.2598(4) 0.1970(2) 0.5846(2) 0.0239 1.0000 Uani D . . . . . C37 C 0.5470(4) 0.28494(18) 0.7437(2) 0.0192 1.0000 Uani D . . . . . C38 C 0.4944(5) 0.2572(2) 0.8330(2) 0.0231 1.0000 Uani D . . . . . O21 O -0.0207(3) 0.01370(15) 0.59082(16) 0.0290 1.0000 Uani D . . . . . O22 O 0.6084(4) -0.04783(19) 0.57131(16) 0.0439 1.0000 Uani D . . . . . H311 H 0.715(3) 0.1327(12) 0.7856(13) 0.0222 1.0000 Uiso D . . . . . H312 H 0.805(3) 0.1227(12) 0.6957(13) 0.0225 1.0000 Uiso D . . . . . H321 H 1.044(3) 0.1687(14) 0.8182(16) 0.0359 1.0000 Uiso D . . . . . H322 H 0.921(4) 0.2472(14) 0.8352(15) 0.0362 1.0000 Uiso D . . . . . H323 H 1.011(3) 0.2419(14) 0.7466(15) 0.0358 1.0000 Uiso D . . . . . H331 H 0.786(3) 0.2925(12) 0.6306(13) 0.0220 1.0000 Uiso D . . . . . H332 H 0.567(3) 0.2970(12) 0.5770(13) 0.0212 1.0000 Uiso D . . . . . H341 H 0.766(3) 0.2379(14) 0.4871(15) 0.0276 1.0000 Uiso D . . . . . H342 H 0.818(3) 0.1595(13) 0.5535(16) 0.0267 1.0000 Uiso D . . . . . H343 H 0.605(3) 0.1721(14) 0.4956(15) 0.0270 1.0000 Uiso D . . . . . H351 H 0.393(3) 0.1337(12) 0.7023(12) 0.0201 1.0000 Uiso D . . . . . H352 H 0.486(3) 0.1128(12) 0.6149(13) 0.0201 1.0000 Uiso D . . . . . H361 H 0.161(3) 0.1535(13) 0.5680(16) 0.0292 1.0000 Uiso D . . . . . H362 H 0.202(3) 0.2435(13) 0.6125(16) 0.0291 1.0000 Uiso D . . . . . H363 H 0.294(4) 0.2166(14) 0.5275(13) 0.0282 1.0000 Uiso D . . . . . H371 H 0.657(3) 0.3218(12) 0.7576(13) 0.0229 1.0000 Uiso D . . . . . H372 H 0.433(3) 0.3150(13) 0.7066(13) 0.0223 1.0000 Uiso D . . . . . H381 H 0.449(3) 0.3033(13) 0.8652(16) 0.0279 1.0000 Uiso D . . . . . H382 H 0.607(3) 0.2339(14) 0.8727(15) 0.0276 1.0000 Uiso D . . . . . H383 H 0.389(3) 0.2161(13) 0.8228(17) 0.0279 1.0000 Uiso D . . . . . H21 H 0.308(4) 0.097(2) 1.0254(17) 0.0400 1.0000 Uiso D . . . . . H32 H 0.263(5) -0.098(2) 0.9725(16) 0.0400 1.0000 Uiso D . . . . . H31 H 0.309(4) -0.081(2) 1.0618(17) 0.0400 1.0000 Uiso D . . . . . H22 H 0.270(4) 0.070(2) 0.9392(17) 0.0400 1.0000 Uiso D . . . . . H12 H 0.018(4) -0.024(2) 0.825(2) 0.0400 1.0000 Uiso D . . . . . H11 H -0.170(3) -0.033(2) 0.828(2) 0.0400 1.0000 Uiso D . . . . . H211 H 0.072(4) -0.001(2) 0.6282(19) 0.0400 1.0000 Uiso D . . . . . H221 H 0.573(5) -0.052(2) 0.6187(15) 0.0400 1.0000 Uiso D . . . . . H213 H 0.009(11) -0.002(5) 0.545(3) 0.0400 0.5000 Uiso D . . . . . H212 H -0.088(9) -0.027(3) 0.580(5) 0.0400 0.5000 Uiso D . . . . . H222 H 0.556(10) -0.033(4) 0.521(2) 0.0400 0.5000 Uiso D . . . . . H223 H 0.708(6) -0.021(4) 0.575(5) 0.0400 0.5000 Uiso 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 Co1 0.0080(2) 0.0121(3) 0.0118(3) 0.0000(2) 0.0028(2) 0.0006(2) O1 0.0084(10) 0.0281(13) 0.0130(10) -0.0035(8) 0.0033(8) -0.0014(9) O2 0.0117(10) 0.0184(11) 0.0119(10) -0.0014(9) 0.0033(8) -0.0015(9) O3 0.0119(10) 0.0153(11) 0.0143(10) -0.0001(9) 0.0041(8) 0.0024(8) S1 0.0090(3) 0.0154(4) 0.0110(3) 0.0005(3) 0.0027(3) -0.0002(3) O11 0.0123(10) 0.0164(11) 0.0143(9) 0.0036(8) 0.0039(8) 0.0005(8) O12 0.0069(9) 0.0275(12) 0.0121(9) -0.0003(9) -0.0005(7) -0.0003(9) O13 0.0145(10) 0.0152(11) 0.0170(10) -0.0018(9) 0.0049(8) -0.0004(9) O14 0.0095(9) 0.0250(12) 0.0123(9) -0.0008(8) 0.0045(8) -0.0005(8) N3 0.0138(12) 0.0138(13) 0.0188(12) 0.0064(10) 0.0053(10) 0.0009(10) C31 0.0180(15) 0.0151(16) 0.0214(15) 0.0093(12) 0.0043(12) 0.0042(13) C32 0.0197(19) 0.035(2) 0.0353(19) 0.0129(16) 0.0018(15) -0.0010(15) C33 0.0160(15) 0.0173(16) 0.0214(15) 0.0098(13) 0.0070(12) 0.0006(13) C34 0.0159(16) 0.0253(19) 0.0265(17) 0.0106(14) 0.0075(13) 0.0016(13) C35 0.0150(15) 0.0142(16) 0.0226(15) 0.0042(13) 0.0064(12) -0.0017(12) C36 0.0142(16) 0.027(2) 0.0298(18) 0.0057(14) 0.0033(14) -0.0013(14) C37 0.0215(17) 0.0133(16) 0.0234(16) 0.0016(13) 0.0062(13) -0.0023(13) C38 0.0269(18) 0.0192(17) 0.0246(17) 0.0009(14) 0.0082(14) -0.0007(14) O21 0.0228(13) 0.0323(16) 0.0280(13) 0.0100(11) -0.0040(10) -0.0005(11) O22 0.0364(16) 0.081(2) 0.0184(12) -0.0145(14) 0.0145(12) -0.0307(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2739(2) 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 . O3 2_557 2.1101(19) yes Co1 . O2 2_557 2.1100(19) yes Co1 . O1 2_557 2.0901(18) yes Co1 . O1 . 2.0901(18) yes Co1 . O2 . 2.1100(19) yes Co1 . O3 . 2.1101(19) yes O1 . H12 . 0.802(17) no O1 . H11 . 0.811(17) no O2 . H21 . 0.822(17) no O2 . H22 . 0.800(17) no O3 . H32 . 0.808(17) no O3 . H31 . 0.813(17) no S1 . O11 . 1.4905(18) yes S1 . O12 . 1.4731(17) yes S1 . O13 . 1.4910(19) yes S1 . O14 . 1.4757(18) yes N3 . C31 . 1.518(3) yes N3 . C33 . 1.518(3) yes N3 . C35 . 1.523(3) yes N3 . C37 . 1.519(3) yes C31 . C32 . 1.508(4) yes C31 . H311 . 0.969(16) no C31 . H312 . 0.975(16) no C32 . H321 . 0.965(17) no C32 . H322 . 0.979(17) no C32 . H323 . 0.967(17) no C33 . C34 . 1.514(4) yes C33 . H331 . 0.971(16) no C33 . H332 . 0.975(16) no C34 . H341 . 0.978(17) no C34 . H342 . 0.980(17) no C34 . H343 . 0.961(16) no C35 . C36 . 1.514(4) yes C35 . H351 . 0.970(16) no C35 . H352 . 0.981(16) no C36 . H361 . 0.974(17) no C36 . H362 . 0.979(17) no C36 . H363 . 0.976(16) no C37 . C38 . 1.506(4) yes C37 . H371 . 0.956(16) no C37 . H372 . 0.990(16) no C38 . H381 . 0.965(17) no C38 . H382 . 0.953(16) no C38 . H383 . 0.971(17) no O21 . H211 . 0.793(17) no O21 . H213 . 0.787(19) no O21 . H212 . 0.801(19) no O22 . H221 . 0.790(17) no O22 . H222 . 0.789(19) no O22 . H223 . 0.802(19) 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 O3 2_557 Co1 . O2 2_557 86.87(7) yes O3 2_557 Co1 . O1 2_557 91.36(7) yes O2 2_557 Co1 . O1 2_557 88.03(7) yes O3 2_557 Co1 . O1 . 88.64(7) yes O2 2_557 Co1 . O1 . 91.97(7) yes O1 2_557 Co1 . O1 . 179.995 yes O3 2_557 Co1 . O2 . 93.13(7) yes O2 2_557 Co1 . O2 . 179.995 yes O1 2_557 Co1 . O2 . 91.97(7) yes O1 . Co1 . O2 . 88.03(7) yes O3 2_557 Co1 . O3 . 179.995 yes O2 2_557 Co1 . O3 . 93.13(7) yes O1 2_557 Co1 . O3 . 88.64(7) yes O1 . Co1 . O3 . 91.36(7) yes O2 . Co1 . O3 . 86.87(7) yes Co1 . O1 . H12 . 125(2) no Co1 . O1 . H11 . 124(2) no H12 . O1 . H11 . 110(3) no Co1 . O2 . H21 . 119(2) no Co1 . O2 . H22 . 111(2) no H21 . O2 . H22 . 109(3) no Co1 . O3 . H32 . 110(2) no Co1 . O3 . H31 . 110(2) no H32 . O3 . H31 . 109(3) no O11 . S1 . O12 . 108.89(11) yes O11 . S1 . O13 . 108.94(11) yes O12 . S1 . O13 . 109.61(11) yes O11 . S1 . O14 . 109.27(11) yes O12 . S1 . O14 . 111.10(10) yes O13 . S1 . O14 . 109.00(11) yes C31 . N3 . C33 . 111.0(2) yes C31 . N3 . C35 . 106.5(2) yes C33 . N3 . C35 . 110.8(2) yes C31 . N3 . C37 . 111.1(2) yes C33 . N3 . C37 . 106.1(2) yes C35 . N3 . C37 . 111.4(2) yes N3 . C31 . C32 . 115.5(2) yes N3 . C31 . H311 . 107.4(12) no C32 . C31 . H311 . 108.5(12) no N3 . C31 . H312 . 106.0(12) no C32 . C31 . H312 . 109.6(12) no H311 . C31 . H312 . 109.6(14) no C31 . C32 . H321 . 107.8(16) no C31 . C32 . H322 . 112.3(16) no H321 . C32 . H322 . 107.5(15) no C31 . C32 . H323 . 114.0(15) no H321 . C32 . H323 . 108.2(15) no H322 . C32 . H323 . 106.8(16) no N3 . C33 . C34 . 115.3(2) yes N3 . C33 . H331 . 107.5(12) no C34 . C33 . H331 . 110.6(12) no N3 . C33 . H332 . 106.6(12) no C34 . C33 . H332 . 109.3(12) no H331 . C33 . H332 . 107.3(14) no C33 . C34 . H341 . 105.0(15) no C33 . C34 . H342 . 113.8(15) no H341 . C34 . H342 . 108.5(15) no C33 . C34 . H343 . 114.7(15) no H341 . C34 . H343 . 107.2(15) no H342 . C34 . H343 . 107.3(15) no N3 . C35 . C36 . 115.1(2) yes N3 . C35 . H351 . 107.3(12) no C36 . C35 . H351 . 110.1(12) no N3 . C35 . H352 . 106.1(12) no C36 . C35 . H352 . 108.5(11) no H351 . C35 . H352 . 109.5(14) no C35 . C36 . H361 . 106.8(15) no C35 . C36 . H362 . 113.8(15) no H361 . C36 . H362 . 108.6(15) no C35 . C36 . H363 . 111.7(15) no H361 . C36 . H363 . 107.5(15) no H362 . C36 . H363 . 108.3(15) no N3 . C37 . C38 . 115.6(2) yes N3 . C37 . H371 . 106.1(12) no C38 . C37 . H371 . 108.8(12) no N3 . C37 . H372 . 108.2(12) no C38 . C37 . H372 . 108.5(12) no H371 . C37 . H372 . 109.4(14) no C37 . C38 . H381 . 111.6(15) no C37 . C38 . H382 . 109.8(15) no H381 . C38 . H382 . 107.8(15) no C37 . C38 . H383 . 112.0(15) no H381 . C38 . H383 . 106.5(15) no H382 . C38 . H383 . 108.9(15) no H211 . O21 . H213 . 101(6) no H211 . O21 . H212 . 104(5) no H213 . O21 . H212 . 79(7) no H221 . O22 . H222 . 133(6) no H221 . O22 . H223 . 113(5) no H222 . O22 . H223 . 98(7) no data_3 _database_code_depnum_ccdc_archive 'CCDC 294938' _audit_creation_date 05-11-10 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title 'import in P 21/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.2597(4) _cell_length_b 23.4134(6) _cell_length_c 16.9043(3) _cell_angle_alpha 90 _cell_angle_beta 101.7390(10) _cell_angle_gamma 90 _cell_volume 5913.3(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-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' 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' 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' 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 8 # Given Formula = C55 H115 Co2.50 N2.50 O17.50 # Dc = 1.39 Fooo = 2424.00 Mu = 7.68 M = 1238.86 # Found Formula = C44 H98 Co2 N2 O22 # Dc = 1.26 FOOO = 2424.00 Mu = 6.32 M = 1125.13 _chemical_formula_sum 'C22 H49 Co1 N1 O11' _chemical_formula_moiety 'C22 H49 Co1 N1 O11' _chemical_compound_source ? _chemical_formula_weight 562.57 _cell_measurement_reflns_used 53433 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 100 _exptl_crystal_description rod _exptl_crystal_colour 'pale pink' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.632 # Sheldrick geometric approximatio 0.88 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _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 100 _diffrn_reflns_number 67294 _reflns_number_total 13430 _diffrn_reflns_av_R_equivalents 0.069 # Number of reflections with Friedels Law is 13430 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13554 _diffrn_reflns_theta_min 1.507 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.928 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 1.23 _oxford_diffrn_Wilson_scale 66.90 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.41 _refine_diff_density_max 2.47 _refine_ls_number_reflns 13430 _refine_ls_number_restraints 18 _refine_ls_number_parameters 674 #_refine_ls_R_factor_ref 0.1341 _refine_ls_wR_factor_ref 0.1520 _refine_ls_goodness_of_fit_ref 0.8225 #_reflns_number_all 13430 _refine_ls_R_factor_all 0.1341 _refine_ls_wR_factor_all 0.1520 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 6106 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_gt 0.1338 _refine_ls_shift/su_max 0.000876 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.597E-01 0.00 0.00 0.00 0.00 0.333 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 atoms attached 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 0.5000 0.0000 0.5000 0.0154 1.0000 Uani S . . . . . O2 O 0.63156(18) -0.02507(13) 0.52597(15) 0.0216 1.0000 Uani . . . . . . C3 C 0.6843(3) -0.03421(19) 0.4771(2) 0.0232 1.0000 Uani . . . . . . C4 C 0.7839(3) -0.0408(2) 0.5152(2) 0.0254 1.0000 Uani . . . . . . C5 C 0.8066(3) -0.02431(19) 0.6051(2) 0.0207 1.0000 Uani . . . . . . O6 O 0.75279(18) -0.05875(12) 0.64808(16) 0.0178 1.0000 Uani D . . . . . Co7 Co 0.74558(4) -0.00975(2) 0.75209(3) 0.0152 1.0000 Uani . . . . . . O8 O 0.76054(18) -0.07554(12) 0.83972(16) 0.0167 1.0000 Uani D . . . . . C9 C 0.7037(3) -0.05883(18) 0.8954(2) 0.0174 1.0000 Uani . . . . . . C10 C 0.7398(3) -0.08722(18) 0.9775(2) 0.0182 1.0000 Uani . . . . . . C11 C 0.8370(3) -0.07210(18) 1.0138(2) 0.0169 1.0000 Uani . . . . . . O12 O 0.87973(18) -0.04545(12) 0.96715(15) 0.0190 1.0000 Uani . . . . . . Co13 Co 1.0000 0.0000 1.0000 0.0164 1.0000 Uani S . . . . . O14 O 0.95614(19) 0.05711(13) 0.90064(17) 0.0203 1.0000 Uani D . . . . . O15 O 1.0588(2) -0.04858(13) 0.92383(17) 0.0221 1.0000 Uani D . . . . . O16 O 0.86955(18) -0.08770(12) 1.08365(16) 0.0208 1.0000 Uani . . . . . . C17 C 0.7054(3) 0.00682(18) 0.9056(2) 0.0169 1.0000 Uani . . . . . . O18 O 0.73230(18) 0.03613(11) 0.85072(15) 0.0172 1.0000 Uani . . . . . . O19 O 0.68149(19) 0.02713(12) 0.96525(15) 0.0211 1.0000 Uani . . . . . . C20 C 0.6094(3) -0.08042(18) 0.8565(2) 0.0194 1.0000 Uani . . . . . . C21 C 0.5734(3) -0.06979(18) 0.7660(2) 0.0178 1.0000 Uani . . . . . . O22 O 0.61188(18) -0.03136(12) 0.73032(16) 0.0184 1.0000 Uani . . . . . . O23 O 0.50790(18) -0.09713(12) 0.73216(16) 0.0207 1.0000 Uani . . . . . . O24 O 0.74511(19) 0.05344(12) 0.66954(16) 0.0209 1.0000 Uani . . . . . . C25 C 0.7878(3) 0.03989(19) 0.6149(2) 0.0207 1.0000 Uani . . . . . . O26 O 0.8138(2) 0.07382(14) 0.56873(18) 0.0335 1.0000 Uani . . . . . . O27 O 0.88425(18) -0.01090(12) 0.77323(16) 0.0208 1.0000 Uani . . . . . . C28 C 0.9312(3) -0.03943(19) 0.7325(2) 0.0194 1.0000 Uani . . . . . . C29 C 0.9035(3) -0.0400(2) 0.6406(2) 0.0243 1.0000 Uani . . . . . . O30 O 0.99983(19) -0.06607(13) 0.76339(16) 0.0248 1.0000 Uani . . . . . . O31 O 0.66066(19) -0.03965(14) 0.40228(16) 0.0310 1.0000 Uani . . . . . . O32 O 0.51717(19) 0.04098(13) 0.61547(16) 0.0190 1.0000 Uani D . . . . . O33 O 0.4685(2) -0.07394(13) 0.55957(16) 0.0229 1.0000 Uani D . . . . . N34 N -0.2649(2) 0.03834(14) 0.22703(18) 0.0176 1.0000 Uani . . . . . . C35 C -0.1862(3) -0.00160(18) 0.2268(2) 0.0210 1.0000 Uani . . . . . . C36 C -0.1586(3) -0.03798(18) 0.3020(2) 0.0226 1.0000 Uani . . . . . . C37 C -0.0875(3) -0.08136(18) 0.2901(2) 0.0227 1.0000 Uani . . . . . . C38 C -0.0550(3) -0.1177(2) 0.3656(3) 0.0361 1.0000 Uani . . . . . . C39 C -0.2711(3) 0.07738(18) 0.1539(2) 0.0208 1.0000 Uani . . . . . . C40 C -0.3499(3) 0.11918(19) 0.1407(2) 0.0248 1.0000 Uani . . . . . . C41 C -0.3346(3) 0.16881(19) 0.0878(3) 0.0323 1.0000 Uani . . . . . . C42 C -0.4114(4) 0.2113(2) 0.0759(3) 0.0392 1.0000 Uani . . . . . . C43 C -0.3508(3) 0.00468(18) 0.2240(2) 0.0207 1.0000 Uani . . . . . . C44 C -0.3793(3) -0.03583(19) 0.1526(3) 0.0262 1.0000 Uani . . . . . . C45 C -0.4612(3) -0.0692(2) 0.1627(3) 0.0335 1.0000 Uani . . . . . . C46 C -0.4924(4) -0.1112(2) 0.0938(3) 0.0431 1.0000 Uani . . . . . . C47 C -0.2502(3) 0.07273(18) 0.3045(2) 0.0199 1.0000 Uani . . . . . . C48 C -0.1701(3) 0.11381(18) 0.3165(2) 0.0229 1.0000 Uani . . . . . . C49 C -0.1430(3) 0.1310(2) 0.4059(2) 0.0278 1.0000 Uani . . . . . . C50 C -0.0678(3) 0.1745(2) 0.4200(3) 0.0357 1.0000 Uani . . . . . . N51 N 0.4685(2) 0.25429(15) 0.3812(2) 0.0276 1.0000 Uani . . . . . . C52 C 0.4145(3) 0.28601(18) 0.3086(2) 0.0254 1.0000 Uani . . . . . . C53 C 0.3955(3) 0.25094(19) 0.2301(3) 0.0352 1.0000 Uani . . . . . . C54 C 0.3362(3) 0.28372(19) 0.1620(3) 0.0312 1.0000 Uani . . . . . . C55 C 0.3218(3) 0.2513(2) 0.0833(3) 0.0418 1.0000 Uani . . . . . . C56 C 0.5545(3) 0.23046(19) 0.3636(3) 0.0279 1.0000 Uani . . . . . . C57 C 0.6124(3) 0.27493(19) 0.3335(3) 0.0270 1.0000 Uani . . . . . . C58 C 0.7019(3) 0.2490(2) 0.3236(3) 0.0365 1.0000 Uani . . . . . . C59 C 0.7604(3) 0.2911(2) 0.2899(3) 0.0477 1.0000 Uani . . . . . . C60 C 0.4886(3) 0.29739(19) 0.4506(3) 0.0283 1.0000 Uani . . . . . . C61 C 0.5509(4) 0.2760(2) 0.5265(3) 0.0380 1.0000 Uani . . . . . . C62 C 0.5484(4) 0.3149(2) 0.5997(3) 0.0417 1.0000 Uani . . . . . . C63 C 0.4659(5) 0.3022(4) 0.6349(5) 0.103(3) 1.0000 Uiso . . . . . . C64 C 0.4142(4) 0.2039(2) 0.4040(3) 0.0387 1.0000 Uani . . . . . . C65 C 0.3185(4) 0.2167(2) 0.4179(3) 0.0467 1.0000 Uani . . . . . . C66 C 0.2445(5) 0.2093(4) 0.3410(5) 0.099(3) 1.0000 Uiso . . . . . . O68 O 0.6645(2) 0.14299(14) 0.51511(19) 0.0297 1.0000 Uani D . . . . . O69 O 0.3198(2) 0.38398(14) 0.47691(19) 0.0261 1.0000 Uani D . . . . . O70 O 0.7166(3) 0.14267(15) 0.77361(19) 0.0361 1.0000 Uani D . . . . . O71 O 0.5705(2) 0.15604(14) 0.6410(2) 0.0359 1.0000 Uani D . . . . . H41 H 0.8017 -0.0815 0.5095 0.0500 1.0000 Uiso R . . . . . H42 H 0.8189 -0.0155 0.4854 0.0500 1.0000 Uiso R . . . . . H101 H 0.7017 -0.0748 1.0161 0.0500 1.0000 Uiso R . . . . . H102 H 0.7355 -0.1296 0.9704 0.0500 1.0000 Uiso R . . . . . H201 H 0.6087 -0.1226 0.8652 0.0500 1.0000 Uiso R . . . . . H202 H 0.5668 -0.0616 0.8861 0.0500 1.0000 Uiso R . . . . . H291 H 0.9423 -0.0119 0.6194 0.0500 1.0000 Uiso R . . . . . H292 H 0.9148 -0.0792 0.6214 0.0500 1.0000 Uiso R . . . . . H351 H -0.2025 -0.0279 0.1794 0.0269 1.0000 Uiso R . . . . . H352 H -0.1337 0.0223 0.2204 0.0500 1.0000 Uiso R . . . . . H361 H -0.2123 -0.0584 0.3135 0.0500 1.0000 Uiso R . . . . . H362 H -0.1330 -0.0128 0.3487 0.0500 1.0000 Uiso R . . . . . H371 H -0.1143 -0.1074 0.2447 0.0500 1.0000 Uiso R . . . . . H372 H -0.0352 -0.0608 0.2761 0.0500 1.0000 Uiso R . . . . . H381 H -0.0092 -0.1459 0.3558 0.0500 1.0000 Uiso R . . . . . H382 H -0.1070 -0.1385 0.3798 0.0500 1.0000 Uiso R . . . . . H383 H -0.0279 -0.0919 0.4112 0.0500 1.0000 Uiso R . . . . . H391 H -0.2147 0.1002 0.1610 0.0500 1.0000 Uiso R . . . . . H392 H -0.2768 0.0529 0.1046 0.0500 1.0000 Uiso R . . . . . H401 H -0.3574 0.1342 0.1943 0.0500 1.0000 Uiso R . . . . . H402 H -0.4055 0.0985 0.1142 0.0500 1.0000 Uiso R . . . . . H411 H -0.2776 0.1883 0.1135 0.0500 1.0000 Uiso R . . . . . H412 H -0.3292 0.1537 0.0337 0.0500 1.0000 Uiso R . . . . . H421 H -0.3989 0.2434 0.0408 0.0500 1.0000 Uiso R . . . . . H422 H -0.4169 0.2267 0.1299 0.0500 1.0000 Uiso R . . . . . H423 H -0.4685 0.1921 0.0501 0.0500 1.0000 Uiso R . . . . . H431 H -0.4004 0.0328 0.2227 0.0500 1.0000 Uiso R . . . . . H432 H -0.3435 -0.0187 0.2744 0.0500 1.0000 Uiso R . . . . . H441 H -0.3931 -0.0132 0.1014 0.0500 1.0000 Uiso R . . . . . H442 H -0.3293 -0.0630 0.1503 0.0500 1.0000 Uiso R . . . . . H451 H -0.5108 -0.0416 0.1642 0.0500 1.0000 Uiso R . . . . . H452 H -0.4470 -0.0907 0.2149 0.0500 1.0000 Uiso R . . . . . H461 H -0.5467 -0.1320 0.1030 0.0500 1.0000 Uiso R . . . . . H462 H -0.5072 -0.0901 0.0413 0.0500 1.0000 Uiso R . . . . . H463 H -0.4434 -0.1392 0.0921 0.0500 1.0000 Uiso R . . . . . H471 H -0.3053 0.0959 0.3045 0.0500 1.0000 Uiso R . . . . . H472 H -0.2408 0.0454 0.3510 0.0500 1.0000 Uiso R . . . . . H481 H -0.1867 0.1488 0.2829 0.0500 1.0000 Uiso R . . . . . H482 H -0.1187 0.0943 0.2994 0.0500 1.0000 Uiso R . . . . . H491 H -0.1961 0.1479 0.4235 0.0500 1.0000 Uiso R . . . . . H492 H -0.1231 0.0960 0.4388 0.0500 1.0000 Uiso R . . . . . H501 H -0.0519 0.1846 0.4787 0.0500 1.0000 Uiso R . . . . . H502 H -0.0874 0.2096 0.3876 0.0500 1.0000 Uiso R . . . . . H503 H -0.0144 0.1577 0.4028 0.0500 1.0000 Uiso R . . . . . H521 H 0.4493 0.3207 0.2991 0.0500 1.0000 Uiso R . . . . . H522 H 0.3560 0.2980 0.3212 0.0500 1.0000 Uiso R . . . . . H531 H 0.4533 0.2416 0.2138 0.0500 1.0000 Uiso R . . . . . H532 H 0.3645 0.2147 0.2398 0.0500 1.0000 Uiso R . . . . . H541 H 0.3653 0.3212 0.1552 0.0500 1.0000 Uiso R . . . . . H542 H 0.2769 0.2906 0.1767 0.0500 1.0000 Uiso R . . . . . H551 H 0.2827 0.2739 0.0397 0.0500 1.0000 Uiso R . . . . . H552 H 0.3810 0.2445 0.0683 0.0500 1.0000 Uiso R . . . . . H553 H 0.2926 0.2139 0.0899 0.0500 1.0000 Uiso R . . . . . H561 H 0.5893 0.2132 0.4144 0.0500 1.0000 Uiso R . . . . . H562 H 0.5392 0.2002 0.3213 0.0500 1.0000 Uiso R . . . . . H571 H 0.6245 0.3070 0.3734 0.0500 1.0000 Uiso R . . . . . H572 H 0.5806 0.2900 0.2800 0.0500 1.0000 Uiso R . . . . . H581 H 0.7350 0.2360 0.3778 0.0500 1.0000 Uiso R . . . . . H582 H 0.6893 0.2155 0.2864 0.0500 1.0000 Uiso R . . . . . H591 H 0.8178 0.2724 0.2847 0.0500 1.0000 Uiso R . . . . . H592 H 0.7736 0.3247 0.3270 0.0500 1.0000 Uiso R . . . . . H593 H 0.7278 0.3042 0.2356 0.0500 1.0000 Uiso R . . . . . H601 H 0.5157 0.3323 0.4312 0.0500 1.0000 Uiso R . . . . . H602 H 0.4305 0.3077 0.4656 0.0500 1.0000 Uiso R . . . . . H611 H 0.6133 0.2751 0.5166 0.0500 1.0000 Uiso R . . . . . H612 H 0.5327 0.2367 0.5394 0.0500 1.0000 Uiso R . . . . . H621 H 0.6035 0.3091 0.6424 0.0500 1.0000 Uiso R . . . . . H622 H 0.5456 0.3555 0.5810 0.0500 1.0000 Uiso R . . . . . H631 H 0.4648 0.3284 0.6815 0.0500 1.0000 Uiso R . . . . . H632 H 0.4684 0.2617 0.6539 0.0500 1.0000 Uiso R . . . . . H633 H 0.4105 0.3082 0.5925 0.0500 1.0000 Uiso R . . . . . H641 H 0.4495 0.1859 0.4541 0.0500 1.0000 Uiso R . . . . . H642 H 0.4069 0.1759 0.3584 0.0500 1.0000 Uiso R . . . . . H651 H 0.3178 0.2576 0.4347 0.0500 1.0000 Uiso R . . . . . H652 H 0.3061 0.1917 0.4624 0.0500 1.0000 Uiso R . . . . . H21 H 0.274(2) 0.4052(18) 0.473(3) 0.0500 1.0000 Uiso D . . . . . H43 H 0.7141(17) 0.126(2) 0.528(3) 0.0500 1.0000 Uiso D . . . . . H51 H 0.350(3) 0.400(2) 0.446(2) 0.0500 1.0000 Uiso D . . . . . H94 H 0.636(3) 0.150(2) 0.552(2) 0.0500 1.0000 Uiso D . . . . . H28 H 0.709(3) 0.148(2) 0.8216(12) 0.0500 1.0000 Uiso D . . . . . H30 H 0.485(3) -0.069(2) 0.6102(6) 0.0500 1.0000 Uiso D . . . . . H36 H 0.548(3) 0.0228(19) 0.655(2) 0.0500 1.0000 Uiso D . . . . . H46 H 0.4169(15) -0.084(2) 0.534(3) 0.0500 1.0000 Uiso D . . . . . H49 H 0.4625(10) 0.040(2) 0.619(3) 0.0500 1.0000 Uiso D . . . . . H62 H 0.735(3) 0.1236(19) 0.738(2) 0.0500 1.0000 Uiso D . . . . . C671 C 0.1549(6) 0.2193(5) 0.3721(6) 0.156(4) 1.0000 Uiso . . . . . . H661 H 0.2508 0.2388 0.2998 0.0500 1.0000 Uiso R . . . . . H662 H 0.2474 0.1704 0.3173 0.0500 1.0000 Uiso R . . . . . H672 H 0.1028 0.2153 0.3258 0.0500 1.0000 Uiso R . . . . . H673 H 0.1541 0.2582 0.3963 0.0500 1.0000 Uiso R . . . . . H674 H 0.1507 0.1898 0.4139 0.0500 1.0000 Uiso R . . . . . H6 H 1.033(3) -0.053(2) 0.8748(10) 0.0500 1.0000 Uiso D . . . . . H13 H 0.936(3) 0.0390(19) 0.8571(17) 0.0500 1.0000 Uiso D . . . . . H14 H 1.095(3) -0.0724(16) 0.951(3) 0.0500 1.0000 Uiso D . . . . . H19 H 0.557(3) 0.1209(6) 0.641(3) 0.0500 1.0000 Uiso D . . . . . H31 H 1.0087(14) 0.070(2) 0.903(3) 0.0500 1.0000 Uiso D . . . . . H70 H 0.610(3) 0.156(2) 0.6846(17) 0.0500 1.0000 Uiso D . . . . . H100 H 0.6973(8) -0.057(2) 0.627(3) 0.0500 1.0000 Uiso D . . . . . H200 H 0.8117(15) -0.063(2) 0.862(3) 0.0500 1.0000 Uiso 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 Co1 0.0113(4) 0.0217(5) 0.0122(4) 0.0009(3) 0.0000(3) 0.0005(4) O2 0.0151(16) 0.041(2) 0.0092(14) 0.0008(13) 0.0025(12) 0.0053(14) C3 0.020(2) 0.034(3) 0.015(2) 0.0027(19) 0.0013(19) 0.000(2) C4 0.015(2) 0.048(3) 0.013(2) 0.002(2) 0.0034(18) 0.005(2) C5 0.010(2) 0.035(3) 0.017(2) 0.0067(19) 0.0024(18) 0.0007(19) O6 0.0106(15) 0.0285(18) 0.0143(15) 0.0009(12) 0.0023(12) -0.0007(13) Co7 0.0120(3) 0.0230(3) 0.0101(3) 0.0006(3) 0.0010(2) 0.0004(3) O8 0.0147(15) 0.0221(17) 0.0139(15) -0.0007(12) 0.0039(12) 0.0002(13) C9 0.017(2) 0.022(2) 0.012(2) -0.0013(17) 0.0008(17) 0.0001(18) C10 0.020(2) 0.022(2) 0.012(2) 0.0028(17) 0.0002(18) -0.0024(19) C11 0.019(2) 0.021(2) 0.009(2) -0.0006(17) 0.0012(17) -0.0017(19) O12 0.0163(15) 0.0268(18) 0.0120(14) 0.0015(12) -0.0020(12) -0.0069(13) Co13 0.0137(4) 0.0215(5) 0.0123(4) 0.0004(3) -0.0011(3) 0.0001(4) O14 0.0178(17) 0.0226(18) 0.0182(16) 0.0007(13) -0.0016(14) -0.0016(14) O15 0.0194(17) 0.0282(19) 0.0169(16) 0.0003(14) -0.0007(13) 0.0049(14) O16 0.0215(16) 0.0247(17) 0.0138(15) 0.0030(12) -0.0019(13) 0.0001(13) C17 0.0080(19) 0.021(2) 0.018(2) 0.0016(18) -0.0061(16) 0.0023(18) O18 0.0189(16) 0.0205(17) 0.0123(14) -0.0002(12) 0.0031(12) -0.0016(13) O19 0.0242(17) 0.0282(18) 0.0119(14) -0.0041(12) 0.0062(13) 0.0008(14) C20 0.016(2) 0.023(2) 0.018(2) 0.0038(18) 0.0007(18) -0.0012(19) C21 0.014(2) 0.022(2) 0.017(2) -0.0013(18) 0.0025(18) 0.0033(19) O22 0.0105(15) 0.0255(17) 0.0176(15) 0.0018(12) -0.0006(12) -0.0016(13) O23 0.0156(16) 0.0280(18) 0.0163(15) -0.0032(13) -0.0020(12) -0.0038(13) O24 0.0180(16) 0.0260(17) 0.0185(15) 0.0040(13) 0.0033(13) 0.0002(13) C25 0.012(2) 0.036(3) 0.014(2) 0.006(2) 0.0012(18) 0.001(2) O26 0.0322(19) 0.041(2) 0.0308(18) 0.0192(16) 0.0140(16) 0.0032(16) O27 0.0108(14) 0.0337(19) 0.0171(15) -0.0018(13) 0.0011(12) 0.0004(13) C28 0.011(2) 0.030(3) 0.017(2) 0.0017(19) 0.0005(18) -0.0025(19) C29 0.013(2) 0.038(3) 0.022(2) 0.000(2) 0.0027(18) 0.004(2) O30 0.0141(16) 0.040(2) 0.0183(15) -0.0011(14) -0.0015(13) 0.0054(14) O31 0.0186(17) 0.061(2) 0.0125(15) 0.0025(15) 0.0016(13) 0.0069(16) O32 0.0183(17) 0.0252(18) 0.0123(15) -0.0001(12) 0.0004(13) 0.0028(14) O33 0.0258(18) 0.0292(18) 0.0111(15) 0.0015(13) -0.0025(14) -0.0031(15) N34 0.0158(19) 0.023(2) 0.0137(17) 0.0000(14) 0.0036(15) 0.0008(15) C35 0.019(2) 0.022(2) 0.022(2) -0.0001(19) 0.0057(18) 0.003(2) C36 0.027(3) 0.025(3) 0.017(2) 0.0038(18) 0.0089(19) 0.007(2) C37 0.021(2) 0.025(3) 0.022(2) 0.0016(19) 0.0038(19) 0.002(2) C38 0.030(3) 0.040(3) 0.037(3) 0.012(2) 0.003(2) 0.014(2) C39 0.019(2) 0.025(3) 0.019(2) 0.0052(18) 0.0069(19) 0.0034(19) C40 0.026(3) 0.031(3) 0.019(2) 0.0025(19) 0.008(2) 0.006(2) C41 0.033(3) 0.026(3) 0.037(3) 0.011(2) 0.008(2) 0.008(2) C42 0.052(4) 0.032(3) 0.034(3) 0.005(2) 0.010(3) 0.012(3) C43 0.013(2) 0.027(3) 0.022(2) 0.0016(19) 0.0042(17) -0.0029(19) C44 0.023(3) 0.029(3) 0.025(2) -0.001(2) 0.002(2) 0.001(2) C45 0.024(3) 0.037(3) 0.039(3) -0.008(2) 0.005(2) -0.003(2) C46 0.036(3) 0.042(3) 0.049(3) -0.013(3) 0.003(3) -0.003(3) C47 0.019(2) 0.025(2) 0.016(2) -0.0015(18) 0.0054(18) 0.0040(19) C48 0.023(3) 0.023(3) 0.023(2) 0.0004(19) 0.006(2) 0.003(2) C49 0.032(3) 0.034(3) 0.018(2) 0.001(2) 0.004(2) -0.002(2) C50 0.037(3) 0.033(3) 0.034(3) -0.002(2) -0.001(2) -0.002(2) N51 0.027(2) 0.021(2) 0.035(2) 0.0045(17) 0.0051(17) 0.0024(18) C52 0.024(3) 0.022(3) 0.028(3) 0.0094(19) -0.002(2) 0.000(2) C53 0.037(3) 0.024(3) 0.039(3) 0.001(2) -0.005(2) 0.005(2) C54 0.023(3) 0.023(3) 0.042(3) 0.000(2) -0.007(2) 0.006(2) C55 0.044(3) 0.055(4) 0.023(3) -0.009(2) -0.002(2) 0.019(3) C56 0.023(3) 0.029(3) 0.029(3) -0.001(2) -0.001(2) 0.008(2) C57 0.024(3) 0.026(3) 0.031(3) -0.002(2) 0.004(2) 0.006(2) C58 0.026(3) 0.040(3) 0.043(3) -0.001(2) 0.005(2) 0.011(2) C59 0.028(3) 0.057(4) 0.061(4) 0.011(3) 0.015(3) 0.004(3) C60 0.029(3) 0.025(3) 0.031(3) 0.002(2) 0.007(2) 0.005(2) C61 0.042(3) 0.036(3) 0.033(3) 0.000(2) 0.003(2) 0.014(3) C62 0.049(4) 0.038(3) 0.043(3) 0.000(2) 0.020(3) 0.000(3) C64 0.048(4) 0.025(3) 0.044(3) 0.013(2) 0.011(3) -0.005(2) C65 0.042(3) 0.057(4) 0.044(3) 0.000(3) 0.013(3) -0.013(3) O68 0.025(2) 0.029(2) 0.0314(19) 0.0020(15) -0.0032(16) -0.0041(15) O69 0.0215(19) 0.029(2) 0.0271(18) 0.0028(14) 0.0025(15) 0.0007(15) O70 0.048(2) 0.034(2) 0.0258(19) -0.0033(16) 0.0052(18) -0.0009(17) O71 0.044(2) 0.0264(19) 0.035(2) 0.0003(17) 0.0049(17) -0.0025(18) _refine_ls_extinction_coef 40(40) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _oxford_refine_ls_scale 0.13271(6) 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 . O32 2_656 2.143(3) yes Co1 . O33 2_656 2.107(3) yes Co1 . O2 2_656 2.052(3) yes Co1 . O2 . 2.052(3) yes Co1 . O32 . 2.143(3) yes Co1 . O33 . 2.107(3) yes O2 . C3 . 1.284(5) yes C3 . C4 . 1.533(6) yes C3 . O31 . 1.249(5) yes C4 . C5 . 1.538(5) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . O6 . 1.447(5) yes C5 . C25 . 1.546(6) yes C5 . C29 . 1.523(5) yes O6 . Co7 . 2.121(3) yes O6 . H100 . 0.849(5) no Co7 . O8 . 2.117(3) yes Co7 . O18 . 2.028(3) yes Co7 . O22 . 2.061(3) yes Co7 . O24 . 2.033(3) yes Co7 . O27 . 2.073(3) yes O8 . C9 . 1.457(5) yes O8 . H200 . 0.850(5) no C9 . C10 . 1.537(5) yes C9 . C17 . 1.547(6) yes C9 . C20 . 1.541(5) yes C10 . C11 . 1.527(5) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C11 . O12 . 1.283(5) yes C11 . O16 . 1.240(4) yes O12 . Co13 . 2.096(3) yes Co13 . O14 2_757 2.145(3) yes Co13 . O15 2_757 2.056(3) yes Co13 . O14 . 2.145(3) yes Co13 . O15 . 2.056(3) yes O14 . H13 . 0.849(5) no O14 . H31 . 0.850(5) no O15 . H6 . 0.849(5) no O15 . H14 . 0.850(5) no C17 . O18 . 1.286(5) yes C17 . O19 . 1.236(5) yes C20 . C21 . 1.537(5) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C21 . O22 . 1.289(5) yes C21 . O23 . 1.226(5) yes O24 . C25 . 1.273(5) yes C25 . O26 . 1.235(5) yes O27 . C28 . 1.279(5) yes C28 . C29 . 1.526(5) yes C28 . O30 . 1.239(5) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no O32 . H36 . 0.850(5) no O32 . H49 . 0.849(5) no O33 . H30 . 0.848(5) no O33 . H46 . 0.849(5) no N34 . C35 . 1.523(5) yes N34 . C39 . 1.525(5) yes N34 . C43 . 1.522(5) yes N34 . C47 . 1.515(5) yes C35 . C36 . 1.517(5) yes C35 . H351 . 1.000 no C35 . H352 . 1.000 no C36 . C37 . 1.530(6) yes C36 . H361 . 1.000 no C36 . H362 . 1.000 no C37 . C38 . 1.530(6) yes C37 . H371 . 1.000 no C37 . H372 . 1.000 no C38 . H381 . 1.000 no C38 . H382 . 1.000 no C38 . H383 . 1.000 no C39 . C40 . 1.531(6) yes C39 . H391 . 1.000 no C39 . H392 . 1.000 no C40 . C41 . 1.513(6) yes C40 . H401 . 1.000 no C40 . H402 . 1.000 no C41 . C42 . 1.520(6) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C42 . H421 . 1.000 no C42 . H422 . 1.000 no C42 . H423 . 1.000 no C43 . C44 . 1.527(5) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C44 . C45 . 1.514(6) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C45 . C46 . 1.525(6) yes C45 . H451 . 1.000 no C45 . H452 . 1.000 no C46 . H461 . 1.000 no C46 . H462 . 1.000 no C46 . H463 . 1.000 no C47 . C48 . 1.536(6) yes C47 . H471 . 1.000 no C47 . H472 . 1.000 no C48 . C49 . 1.538(5) yes C48 . H481 . 1.000 no C48 . H482 . 1.000 no C49 . C50 . 1.516(6) yes C49 . H491 . 1.000 no C49 . H492 . 1.000 no C50 . H501 . 1.000 no C50 . H502 . 1.000 no C50 . H503 . 1.000 no N51 . C52 . 1.524(5) yes N51 . C56 . 1.510(5) yes N51 . C60 . 1.531(5) yes N51 . C64 . 1.535(6) yes C52 . C53 . 1.538(6) yes C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . C54 . 1.519(6) yes C53 . H531 . 1.000 no C53 . H532 . 1.000 no C54 . C55 . 1.508(6) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no C55 . H551 . 1.000 no C55 . H552 . 1.000 no C55 . H553 . 1.000 no C56 . C57 . 1.519(6) yes C56 . H561 . 1.000 no C56 . H562 . 1.000 no C57 . C58 . 1.534(6) yes C57 . H571 . 1.000 no C57 . H572 . 1.000 no C58 . C59 . 1.516(7) yes C58 . H581 . 1.000 no C58 . H582 . 1.000 no C59 . H591 . 1.000 no C59 . H592 . 1.000 no C59 . H593 . 1.000 no C60 . C61 . 1.518(6) yes C60 . H601 . 1.000 no C60 . H602 . 1.000 no C61 . C62 . 1.544(6) yes C61 . H611 . 1.000 no C61 . H612 . 1.000 no C62 . C63 . 1.527(8) yes C62 . H621 . 1.000 no C62 . H622 . 1.000 no C63 . H631 . 1.000 no C63 . H632 . 1.000 no C63 . H633 . 1.000 no C64 . C65 . 1.556(7) yes C64 . H641 . 1.000 no C64 . H642 . 1.000 no C65 . C66 . 1.549(8) yes C65 . H651 . 1.000 no C65 . H652 . 1.000 no C66 . C671 . 1.580(11) yes C66 . H661 . 1.000 no C66 . H662 . 1.000 no O68 . H43 . 0.849(5) no O68 . H94 . 0.849(5) no O69 . H21 . 0.850(5) no O69 . H51 . 0.850(5) no O70 . H28 . 0.852(5) no O70 . H62 . 0.849(5) no O71 . H19 . 0.850(5) no O71 . H70 . 0.850(5) no C671 . H672 . 1.000 no C671 . H673 . 1.000 no C671 . H674 . 1.000 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 O32 2_656 Co1 . O33 2_656 85.99(11) yes O32 2_656 Co1 . O2 2_656 90.01(11) yes O33 2_656 Co1 . O2 2_656 88.33(12) yes O32 2_656 Co1 . O2 . 89.99(11) yes O33 2_656 Co1 . O2 . 91.67(12) yes O2 2_656 Co1 . O2 . 179.994 yes O32 2_656 Co1 . O32 . 179.995 yes O33 2_656 Co1 . O32 . 94.01(11) yes O2 2_656 Co1 . O32 . 89.99(11) yes O2 . Co1 . O32 . 90.01(11) yes O32 2_656 Co1 . O33 . 94.01(11) yes O33 2_656 Co1 . O33 . 179.995 yes O2 2_656 Co1 . O33 . 91.67(12) yes O2 . Co1 . O33 . 88.33(12) yes O32 . Co1 . O33 . 85.99(11) yes Co1 . O2 . C3 . 128.7(3) yes O2 . C3 . C4 . 116.4(3) yes O2 . C3 . O31 . 125.4(4) yes C4 . C3 . O31 . 118.2(4) yes C3 . C4 . C5 . 113.2(3) yes C3 . C4 . H41 . 108.738 no C5 . C4 . H41 . 108.872 no C3 . C4 . H42 . 108.297 no C5 . C4 . H42 . 108.198 no H41 . C4 . H42 . 109.466 no C4 . C5 . O6 . 108.6(3) yes C4 . C5 . C25 . 110.0(3) yes O6 . C5 . C25 . 110.6(3) yes C4 . C5 . C29 . 109.5(3) yes O6 . C5 . C29 . 105.8(3) yes C25 . C5 . C29 . 112.2(3) yes C5 . O6 . Co7 . 104.2(2) yes C5 . O6 . H100 . 113(3) no Co7 . O6 . H100 . 96(3) no O6 . Co7 . O8 . 99.78(11) yes O6 . Co7 . O18 . 177.22(11) yes O8 . Co7 . O18 . 79.91(11) yes O6 . Co7 . O22 . 86.31(11) yes O8 . Co7 . O22 . 84.73(11) yes O18 . Co7 . O22 . 90.92(11) yes O6 . Co7 . O24 . 79.52(11) yes O8 . Co7 . O24 . 174.12(11) yes O18 . Co7 . O24 . 101.07(11) yes O22 . Co7 . O24 . 101.01(11) yes O6 . Co7 . O27 . 84.98(11) yes O8 . Co7 . O27 . 84.78(11) yes O18 . Co7 . O27 . 97.73(11) yes O22 . Co7 . O27 . 165.03(12) yes O24 . Co7 . O27 . 89.35(11) yes Co7 . O8 . C9 . 105.2(2) yes Co7 . O8 . H200 . 91(3) no C9 . O8 . H200 . 103(3) no O8 . C9 . C10 . 108.5(3) yes O8 . C9 . C17 . 109.9(3) yes C10 . C9 . C17 . 109.5(3) yes O8 . C9 . C20 . 105.2(3) yes C10 . C9 . C20 . 112.1(3) yes C17 . C9 . C20 . 111.5(3) yes C9 . C10 . C11 . 113.7(3) yes C9 . C10 . H101 . 108.306 no C11 . C10 . H101 . 108.501 no C9 . C10 . H102 . 108.528 no C11 . C10 . H102 . 108.251 no H101 . C10 . H102 . 109.467 no C10 . C11 . O12 . 116.1(3) yes C10 . C11 . O16 . 118.8(4) yes O12 . C11 . O16 . 125.0(4) yes C11 . O12 . Co13 . 127.7(2) yes O14 2_757 Co13 . O12 . 90.45(10) yes O14 2_757 Co13 . O12 2_757 89.55(10) yes O12 . Co13 . O12 2_757 179.995 yes O14 2_757 Co13 . O15 2_757 87.75(11) yes O12 . Co13 . O15 2_757 88.66(11) yes O12 2_757 Co13 . O15 2_757 91.34(11) yes O14 2_757 Co13 . O14 . 179.995 yes O12 . Co13 . O14 . 89.55(10) yes O12 2_757 Co13 . O14 . 90.45(10) yes O15 2_757 Co13 . O14 . 92.25(11) yes O14 2_757 Co13 . O15 . 92.25(11) yes O12 . Co13 . O15 . 91.34(11) yes O12 2_757 Co13 . O15 . 88.66(11) yes O15 2_757 Co13 . O15 . 179.994 yes O14 . Co13 . O15 . 87.75(11) yes Co13 . O14 . H13 . 112(3) no Co13 . O14 . H31 . 93(3) no H13 . O14 . H31 . 112(5) no Co13 . O15 . H6 . 121(3) no Co13 . O15 . H14 . 110(3) no H6 . O15 . H14 . 124(5) no C9 . C17 . O18 . 116.8(4) yes C9 . C17 . O19 . 118.2(4) yes O18 . C17 . O19 . 125.0(4) yes Co7 . O18 . C17 . 114.2(3) yes C9 . C20 . C21 . 119.1(3) yes C9 . C20 . H201 . 107.382 no C21 . C20 . H201 . 107.112 no C9 . C20 . H202 . 106.682 no C21 . C20 . H202 . 106.914 no H201 . C20 . H202 . 109.466 no C20 . C21 . O22 . 118.3(3) yes C20 . C21 . O23 . 118.2(4) yes O22 . C21 . O23 . 123.5(4) yes Co7 . O22 . C21 . 128.0(2) yes Co7 . O24 . C25 . 112.7(3) yes C5 . C25 . O24 . 117.0(4) yes C5 . C25 . O26 . 117.8(4) yes O24 . C25 . O26 . 125.2(4) yes Co7 . O27 . C28 . 125.3(2) yes O27 . C28 . C29 . 118.9(4) yes O27 . C28 . O30 . 123.7(4) yes C29 . C28 . O30 . 117.4(4) yes C28 . C29 . C5 . 116.4(3) yes C28 . C29 . H291 . 107.322 no C5 . C29 . H291 . 107.419 no C28 . C29 . H292 . 107.906 no C5 . C29 . H292 . 108.158 no H291 . C29 . H292 . 109.467 no Co1 . O32 . H36 . 116(3) no Co1 . O32 . H49 . 97(3) no H36 . O32 . H49 . 109(5) no Co1 . O33 . H30 . 109(3) no Co1 . O33 . H46 . 105(3) no H30 . O33 . H46 . 127(5) no C35 . N34 . C39 . 106.5(3) yes C35 . N34 . C43 . 110.9(3) yes C39 . N34 . C43 . 111.9(3) yes C35 . N34 . C47 . 110.5(3) yes C39 . N34 . C47 . 110.9(3) yes C43 . N34 . C47 . 106.2(3) yes N34 . C35 . C36 . 115.2(3) yes N34 . C35 . H351 . 108.205 no C36 . C35 . H351 . 107.811 no N34 . C35 . H352 . 107.798 no C36 . C35 . H352 . 108.251 no H351 . C35 . H352 . 109.467 no C35 . C36 . C37 . 110.2(3) yes C35 . C36 . H361 . 109.441 no C37 . C36 . H361 . 109.848 no C35 . C36 . H362 . 109.123 no C37 . C36 . H362 . 108.707 no H361 . C36 . H362 . 109.467 no C36 . C37 . C38 . 112.2(4) yes C36 . C37 . H371 . 108.300 no C38 . C37 . H371 . 108.330 no C36 . C37 . H372 . 109.399 no C38 . C37 . H372 . 109.102 no H371 . C37 . H372 . 109.467 no C37 . C38 . H381 . 110.291 no C37 . C38 . H382 . 109.440 no H381 . C38 . H382 . 109.476 no C37 . C38 . H383 . 108.666 no H381 . C38 . H383 . 109.476 no H382 . C38 . H383 . 109.476 no N34 . C39 . C40 . 114.7(3) yes N34 . C39 . H391 . 108.289 no C40 . C39 . H391 . 107.846 no N34 . C39 . H392 . 108.254 no C40 . C39 . H392 . 108.187 no H391 . C39 . H392 . 109.467 no C39 . C40 . C41 . 111.4(4) yes C39 . C40 . H401 . 108.923 no C41 . C40 . H401 . 108.968 no C39 . C40 . H402 . 109.052 no C41 . C40 . H402 . 108.967 no H401 . C40 . H402 . 109.467 no C40 . C41 . C42 . 111.9(4) yes C40 . C41 . H411 . 108.665 no C42 . C41 . H411 . 109.691 no C40 . C41 . H412 . 108.719 no C42 . C41 . H412 . 108.336 no H411 . C41 . H412 . 109.467 no C41 . C42 . H421 . 109.659 no C41 . C42 . H422 . 108.690 no H421 . C42 . H422 . 109.476 no C41 . C42 . H423 . 110.048 no H421 . C42 . H423 . 109.476 no H422 . C42 . H423 . 109.476 no N34 . C43 . C44 . 116.9(3) yes N34 . C43 . H431 . 107.556 no C44 . C43 . H431 . 107.448 no N34 . C43 . H432 . 107.980 no C44 . C43 . H432 . 107.368 no H431 . C43 . H432 . 109.467 no C43 . C44 . C45 . 109.8(4) yes C43 . C44 . H441 . 109.293 no C45 . C44 . H441 . 109.779 no C43 . C44 . H442 . 109.282 no C45 . C44 . H442 . 109.187 no H441 . C44 . H442 . 109.467 no C44 . C45 . C46 . 112.5(4) yes C44 . C45 . H451 . 108.373 no C46 . C45 . H451 . 108.361 no C44 . C45 . H452 . 108.951 no C46 . C45 . H452 . 109.138 no H451 . C45 . H452 . 109.467 no C45 . C46 . H461 . 109.576 no C45 . C46 . H462 . 109.801 no H461 . C46 . H462 . 109.475 no C45 . C46 . H463 . 109.022 no H461 . C46 . H463 . 109.476 no H462 . C46 . H463 . 109.476 no N34 . C47 . C48 . 114.8(3) yes N34 . C47 . H471 . 108.166 no C48 . C47 . H471 . 107.876 no N34 . C47 . H472 . 108.187 no C48 . C47 . H472 . 108.236 no H471 . C47 . H472 . 109.467 no C47 . C48 . C49 . 109.9(3) yes C47 . C48 . H481 . 109.663 no C49 . C48 . H481 . 109.307 no C47 . C48 . H482 . 109.085 no C49 . C48 . H482 . 109.393 no H481 . C48 . H482 . 109.467 no C48 . C49 . C50 . 111.9(4) yes C48 . C49 . H491 . 108.869 no C50 . C49 . H491 . 108.587 no C48 . C49 . H492 . 108.825 no C50 . C49 . H492 . 109.125 no H491 . C49 . H492 . 109.467 no C49 . C50 . H501 . 109.834 no C49 . C50 . H502 . 109.552 no H501 . C50 . H502 . 109.476 no C49 . C50 . H503 . 109.013 no H501 . C50 . H503 . 109.476 no H502 . C50 . H503 . 109.476 no C52 . N51 . C56 . 111.7(3) yes C52 . N51 . C60 . 106.7(3) yes C56 . N51 . C60 . 110.3(3) yes C52 . N51 . C64 . 110.3(3) yes C56 . N51 . C64 . 107.4(3) yes C60 . N51 . C64 . 110.4(4) yes N51 . C52 . C53 . 114.3(3) yes N51 . C52 . H521 . 107.952 no C53 . C52 . H521 . 107.891 no N51 . C52 . H522 . 108.923 no C53 . C52 . H522 . 108.271 no H521 . C52 . H522 . 109.467 no C52 . C53 . C54 . 111.3(4) yes C52 . C53 . H531 . 109.355 no C54 . C53 . H531 . 108.863 no C52 . C53 . H532 . 108.871 no C54 . C53 . H532 . 108.953 no H531 . C53 . H532 . 109.467 no C53 . C54 . C55 . 111.8(4) yes C53 . C54 . H541 . 108.709 no C55 . C54 . H541 . 109.200 no C53 . C54 . H542 . 108.759 no C55 . C54 . H542 . 108.833 no H541 . C54 . H542 . 109.467 no C54 . C55 . H551 . 110.039 no C54 . C55 . H552 . 108.996 no H551 . C55 . H552 . 109.476 no C54 . C55 . H553 . 109.364 no H551 . C55 . H553 . 109.476 no H552 . C55 . H553 . 109.476 no N51 . C56 . C57 . 113.6(4) yes N51 . C56 . H561 . 108.196 no C57 . C56 . H561 . 108.760 no N51 . C56 . H562 . 108.472 no C57 . C56 . H562 . 108.252 no H561 . C56 . H562 . 109.467 no C56 . C57 . C58 . 110.9(4) yes C56 . C57 . H571 . 109.192 no C58 . C57 . H571 . 108.841 no C56 . C57 . H572 . 109.672 no C58 . C57 . H572 . 108.721 no H571 . C57 . H572 . 109.467 no C57 . C58 . C59 . 112.9(4) yes C57 . C58 . H581 . 108.458 no C59 . C58 . H581 . 108.444 no C57 . C58 . H582 . 108.469 no C59 . C58 . H582 . 109.050 no H581 . C58 . H582 . 109.467 no C58 . C59 . H591 . 109.977 no C58 . C59 . H592 . 109.515 no H591 . C59 . H592 . 109.476 no C58 . C59 . H593 . 108.906 no H591 . C59 . H593 . 109.476 no H592 . C59 . H593 . 109.476 no N51 . C60 . C61 . 115.1(4) yes N51 . C60 . H601 . 108.641 no C61 . C60 . H601 . 108.366 no N51 . C60 . H602 . 107.703 no C61 . C60 . H602 . 107.453 no H601 . C60 . H602 . 109.466 no C60 . C61 . C62 . 111.7(4) yes C60 . C61 . H611 . 108.675 no C62 . C61 . H611 . 109.086 no C60 . C61 . H612 . 109.460 no C62 . C61 . H612 . 108.404 no H611 . C61 . H612 . 109.467 no C61 . C62 . C63 . 110.8(5) yes C61 . C62 . H621 . 110.036 no C63 . C62 . H621 . 109.421 no C61 . C62 . H622 . 108.186 no C63 . C62 . H622 . 108.906 no H621 . C62 . H622 . 109.467 no C62 . C63 . H631 . 109.570 no C62 . C63 . H632 . 109.157 no H631 . C63 . H632 . 109.476 no C62 . C63 . H633 . 109.673 no H631 . C63 . H633 . 109.476 no H632 . C63 . H633 . 109.476 no N51 . C64 . C65 . 117.4(4) yes N51 . C64 . H641 . 108.173 no C65 . C64 . H641 . 108.218 no N51 . C64 . H642 . 107.041 no C65 . C64 . H642 . 106.338 no H641 . C64 . H642 . 109.467 no C64 . C65 . C66 . 113.4(5) yes C64 . C65 . H651 . 106.940 no C66 . C65 . H651 . 107.309 no C64 . C65 . H652 . 109.121 no C66 . C65 . H652 . 110.495 no H651 . C65 . H652 . 109.467 no C65 . C66 . C671 . 103.7(6) yes C65 . C66 . H661 . 110.572 no C671 . C66 . H661 . 109.966 no C65 . C66 . H662 . 110.760 no C671 . C66 . H662 . 112.311 no H661 . C66 . H662 . 109.467 no H43 . O68 . H94 . 118(5) no H21 . O69 . H51 . 104(5) no H28 . O70 . H62 . 152(5) no H19 . O71 . H70 . 97(5) no C66 . C671 . H672 . 109.241 no C66 . C671 . H673 . 110.736 no H672 . C671 . H673 . 109.476 no C66 . C671 . H674 . 108.415 no H672 . C671 . H674 . 109.476 no H673 . C671 . H674 . 109.476 no # start Validation Reply Form _vrf_PLAT220_3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.07 Ratio RESPONSE: The large value for Ueq is in a molecule that is present as a counterion - the terminal C of an n-butyl chain. Although non-solvent, we can expect large values of Ueq for such atoms. ; # end Validation Reply Form