Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Catherine E Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Edwin C. Constable' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Kate Harris' '' '' 'Markus Neuburger' '' '' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; A metallopolymer case-history:polymer, ring or ligand reaction? ; _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_name_full ? _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_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _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 will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_requested_journal 'Section E' # Attachment 'ethoxy.cif' data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 693545' _audit_creation_date 06-10-16 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '10161149 kh043_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.82930(10) _cell_length_b 21.7694(3) _cell_length_c 19.6786(2) _cell_angle_alpha 90 _cell_angle_beta 103.1996(7) _cell_angle_gamma 90 _cell_volume 4099.54(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C32 H26 Co1 F12 N6 O2 P2 # Dc = 1.42 Fooo = 2004.00 Mu = 5.87 M = 875.45 # Found Formula = C38 H36 Co1 F12 N8 O2 P2 # Dc = 1.60 FOOO = 2004.00 Mu = 5.98 M = 985.61 _chemical_formula_sum 'C38 H36 Co1 F12 N8 O2 P2' _chemical_formula_moiety 'C34 H30 Co N6 O2, 2(F6 P), 2(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 985.61 _cell_measurement_reflns_used 18612 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 0.598 # Sheldrick geometric approximatio 0.93 0.94 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction '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 173 _diffrn_reflns_number 37341 _reflns_number_total 9749 _diffrn_reflns_av_R_equivalents 0.075 # Number of reflections with Friedels Law is 9749 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9771 _diffrn_reflns_theta_min 3.002 _diffrn_reflns_theta_max 27.869 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.869 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.93 _refine_diff_density_max 0.89 _refine_ls_number_reflns 9705 _refine_ls_number_restraints 0 _refine_ls_number_parameters 568 #_refine_ls_R_factor_ref 0.0988 _refine_ls_wR_factor_ref 0.1515 _refine_ls_goodness_of_fit_ref 0.9868 #_reflns_number_all 9705 _refine_ls_R_factor_all 0.0988 _refine_ls_wR_factor_all 0.1515 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4599 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_gt 0.0917 _refine_ls_shift/su_max 0.000519 # 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 constr # 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: 4.58 5.67 1.42 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. 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--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # 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. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. 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. 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 0.52309(5) 0.23840(2) 0.39871(2) 0.0253 1.0000 Uani . . . . . . N1 N 0.6389(3) 0.16539(14) 0.36387(16) 0.0277 1.0000 Uani . . . . . . N2 N 0.4428(3) 0.23966(14) 0.30018(14) 0.0242 1.0000 Uani . . . . . . N3 N 0.3688(3) 0.31028(14) 0.39102(16) 0.0284 1.0000 Uani . . . . . . N4 N 0.6690(3) 0.30291(14) 0.39895(15) 0.0272 1.0000 Uani . . . . . . N5 N 0.6010(3) 0.24067(14) 0.49493(15) 0.0257 1.0000 Uani . . . . . . N6 N 0.4039(3) 0.17444(14) 0.43040(15) 0.0276 1.0000 Uani . . . . . . N7 N 0.5691(6) 0.4214(2) 0.5713(3) 0.0682 1.0000 Uani . . . . . . N8 N 0.4822(5) 0.4123(2) 0.2191(2) 0.0615 1.0000 Uani . . . . . . C1 C 0.7364(4) 0.12810(19) 0.4018(2) 0.0344 1.0000 Uani . . . . . . C2 C 0.8025(5) 0.0825(2) 0.3719(2) 0.0400 1.0000 Uani . . . . . . C3 C 0.7681(5) 0.0755(2) 0.3001(2) 0.0424 1.0000 Uani . . . . . . C4 C 0.6668(4) 0.11307(19) 0.2605(2) 0.0347 1.0000 Uani . . . . . . C5 C 0.6029(4) 0.15717(17) 0.29388(19) 0.0283 1.0000 Uani . . . . . . C6 C 0.4899(4) 0.19880(16) 0.25705(18) 0.0262 1.0000 Uani . . . . . . C7 C 0.4329(4) 0.19747(17) 0.18613(18) 0.0276 1.0000 Uani . . . . . . C8 C 0.3238(4) 0.23803(17) 0.15809(18) 0.0277 1.0000 Uani . . . . . . C9 C 0.2781(4) 0.27991(17) 0.20166(18) 0.0281 1.0000 Uani . . . . . . C10 C 0.3419(4) 0.27927(17) 0.27254(18) 0.0265 1.0000 Uani . . . . . . C11 C 0.3050(4) 0.32233(17) 0.32408(18) 0.0271 1.0000 Uani . . . . . . C12 C 0.2143(4) 0.37136(18) 0.3056(2) 0.0340 1.0000 Uani . . . . . . C13 C 0.1876(5) 0.4091(2) 0.3579(2) 0.0406 1.0000 Uani . . . . . . C14 C 0.2511(5) 0.3962(2) 0.4272(2) 0.0418 1.0000 Uani . . . . . . C15 C 0.3414(4) 0.34650(19) 0.4411(2) 0.0366 1.0000 Uani . . . . . . C16 C 0.6968(4) 0.33308(18) 0.3445(2) 0.0327 1.0000 Uani . . . . . . C17 C 0.7932(4) 0.38011(19) 0.3523(2) 0.0370 1.0000 Uani . . . . . . C18 C 0.8623(4) 0.39795(19) 0.4187(2) 0.0370 1.0000 Uani . . . . . . C19 C 0.8348(4) 0.36708(18) 0.4757(2) 0.0317 1.0000 Uani . . . . . . C20 C 0.7393(4) 0.31929(17) 0.46443(19) 0.0271 1.0000 Uani . . . . . . C21 C 0.7035(4) 0.28130(16) 0.51985(18) 0.0258 1.0000 Uani . . . . . . C22 C 0.7669(4) 0.28464(17) 0.59050(18) 0.0273 1.0000 Uani . . . . . . C23 C 0.7207(4) 0.24390(17) 0.63577(17) 0.0272 1.0000 Uani . . . . . . C24 C 0.6112(4) 0.20280(17) 0.60932(18) 0.0270 1.0000 Uani . . . . . . C25 C 0.5537(4) 0.20261(16) 0.53860(18) 0.0253 1.0000 Uani . . . . . . C26 C 0.4385(4) 0.16354(16) 0.50062(18) 0.0258 1.0000 Uani . . . . . . C27 C 0.3675(4) 0.12024(18) 0.5312(2) 0.0331 1.0000 Uani . . . . . . C28 C 0.2593(4) 0.08685(19) 0.4893(2) 0.0387 1.0000 Uani . . . . . . C29 C 0.2259(4) 0.09798(19) 0.4181(2) 0.0385 1.0000 Uani . . . . . . C30 C 0.2999(4) 0.14170(18) 0.39059(19) 0.0316 1.0000 Uani . . . . . . C31 C 0.1408(4) 0.26703(19) 0.06187(19) 0.0327 1.0000 Uani . . . . . . C32 C 0.0945(4) 0.2521(2) -0.0146(2) 0.0392 1.0000 Uani . . . . . . C33 C 0.9052(4) 0.2749(2) 0.73026(19) 0.0338 1.0000 Uani . . . . . . C34 C 0.9555(4) 0.2621(2) 0.8069(2) 0.0422 1.0000 Uani . . . . . . C35 C 0.5174(5) 0.4644(2) 0.5862(2) 0.0487 1.0000 Uani . . . . . . C36 C 0.4501(7) 0.5178(3) 0.6058(3) 0.0668 1.0000 Uani . . . . . . C37 C 0.5275(5) 0.4551(2) 0.1991(2) 0.0449 1.0000 Uani . . . . . . C38 C 0.5846(6) 0.5087(3) 0.1720(3) 0.0627 1.0000 Uani . . . . . . O1 O 0.2704(3) 0.23400(13) 0.08877(12) 0.0310 1.0000 Uani . . . . . . O2 O 0.7752(3) 0.24172(13) 0.70507(12) 0.0306 1.0000 Uani . . . . . . P1 P 0.09757(12) 0.07543(5) 0.16484(6) 0.0382 1.0000 Uani . . . . . . P2 P 0.93364(13) 0.08269(5) 0.61097(6) 0.0401 1.0000 Uani . . . . . . F1 F 0.0782(5) 0.04948(16) 0.08714(16) 0.0843 1.0000 Uani . . . . . . F2 F 0.1132(4) 0.10155(16) 0.24142(15) 0.0765 1.0000 Uani . . . . . . F3 F 0.0789(3) 0.14369(12) 0.13420(17) 0.0565 1.0000 Uani . . . . . . F4 F 0.1146(4) 0.00712(13) 0.19358(17) 0.0663 1.0000 Uani . . . . . . F5 F -0.0674(3) 0.07227(15) 0.15581(19) 0.0681 1.0000 Uani . . . . . . F6 F 0.2618(3) 0.07921(17) 0.1733(3) 0.0897 1.0000 Uani . . . . . . F11 F 0.9447(4) 0.0394(2) 0.5483(2) 0.1001 1.0000 Uani . . . . . . F12 F 0.9262(5) 0.1264(2) 0.6731(2) 0.1205 1.0000 Uani . . . . . . F13 F 0.9135(4) 0.14093(18) 0.5617(2) 0.1009 1.0000 Uani . . . . . . F14 F 0.9517(4) 0.02494(17) 0.6601(2) 0.0865 1.0000 Uani . . . . . . F15 F 0.7686(3) 0.07488(17) 0.5911(2) 0.0792 1.0000 Uani . . . . . . F16 F 1.1002(3) 0.09077(15) 0.62963(16) 0.0623 1.0000 Uani . . . . . . H11 H 0.7590 0.1343 0.4506 0.0405 1.0000 Uiso R . . . . . H21 H 0.8703 0.0567 0.4000 0.0488 1.0000 Uiso R . . . . . H31 H 0.8146 0.0455 0.2779 0.0510 1.0000 Uiso R . . . . . H41 H 0.6415 0.1096 0.2114 0.0421 1.0000 Uiso R . . . . . H71 H 0.4663 0.1690 0.1566 0.0333 1.0000 Uiso R . . . . . H91 H 0.2061 0.3087 0.1836 0.0340 1.0000 Uiso R . . . . . H121 H 0.1731 0.3784 0.2588 0.0402 1.0000 Uiso R . . . . . H131 H 0.1276 0.4431 0.3465 0.0505 1.0000 Uiso R . . . . . H141 H 0.2331 0.4206 0.4642 0.0503 1.0000 Uiso R . . . . . H151 H 0.3867 0.3365 0.4879 0.0449 1.0000 Uiso R . . . . . H161 H 0.6469 0.3212 0.2993 0.0412 1.0000 Uiso R . . . . . H171 H 0.8114 0.4002 0.3124 0.0453 1.0000 Uiso R . . . . . H181 H 0.9284 0.4303 0.4251 0.0442 1.0000 Uiso R . . . . . H191 H 0.8799 0.3778 0.5221 0.0397 1.0000 Uiso R . . . . . H221 H 0.8398 0.3139 0.6073 0.0333 1.0000 Uiso R . . . . . H241 H 0.5781 0.1758 0.6397 0.0323 1.0000 Uiso R . . . . . H271 H 0.3910 0.1144 0.5801 0.0411 1.0000 Uiso R . . . . . H281 H 0.2085 0.0571 0.5096 0.0463 1.0000 Uiso R . . . . . H291 H 0.1529 0.0762 0.3886 0.0460 1.0000 Uiso R . . . . . H301 H 0.2762 0.1502 0.3421 0.0370 1.0000 Uiso R . . . . . H311 H 0.1555 0.3120 0.0675 0.0378 1.0000 Uiso R . . . . . H312 H 0.0676 0.2534 0.0869 0.0381 1.0000 Uiso R . . . . . H321 H 0.0090 0.2750 -0.0335 0.0588 1.0000 Uiso R . . . . . H322 H 0.1675 0.2639 -0.0382 0.0592 1.0000 Uiso R . . . . . H323 H 0.0739 0.2082 -0.0214 0.0587 1.0000 Uiso R . . . . . H331 H 0.8870 0.3197 0.7225 0.0410 1.0000 Uiso R . . . . . H332 H 0.9757 0.2615 0.7045 0.0415 1.0000 Uiso R . . . . . H341 H 1.0417 0.2851 0.8237 0.0634 1.0000 Uiso R . . . . . H342 H 0.8850 0.2754 0.8320 0.0633 1.0000 Uiso R . . . . . H343 H 0.9733 0.2180 0.8145 0.0630 1.0000 Uiso R . . . . . H361 H 0.4305 0.5463 0.5674 0.1041 1.0000 Uiso R . . . . . H362 H 0.5113 0.5372 0.6452 0.1043 1.0000 Uiso R . . . . . H363 H 0.3651 0.5056 0.6180 0.1037 1.0000 Uiso R . . . . . H381 H 0.5886 0.5417 0.2046 0.0952 1.0000 Uiso R . . . . . H382 H 0.5231 0.5194 0.1277 0.0958 1.0000 Uiso R . . . . . H383 H 0.6764 0.4995 0.1665 0.0952 1.0000 Uiso 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 0.0263(2) 0.0261(2) 0.0223(2) 0.00031(19) 0.00288(17) -0.0008(2) N1 0.0246(15) 0.0310(16) 0.0273(15) 0.0027(12) 0.0051(12) 0.0001(12) N2 0.0185(13) 0.0342(16) 0.0187(13) 0.0043(11) 0.0018(10) -0.0068(12) N3 0.0284(16) 0.0284(16) 0.0270(15) -0.0017(12) 0.0037(12) -0.0010(12) N4 0.0299(16) 0.0248(14) 0.0263(14) 0.0012(12) 0.0052(12) 0.0032(12) N5 0.0277(15) 0.0240(14) 0.0247(14) 0.0003(11) 0.0044(11) -0.0011(12) N6 0.0274(15) 0.0277(15) 0.0261(15) -0.0024(12) 0.0029(12) 0.0025(12) N7 0.075(3) 0.065(3) 0.061(3) -0.006(2) 0.006(2) 0.019(3) N8 0.074(3) 0.058(3) 0.049(2) 0.008(2) 0.007(2) -0.012(2) C1 0.0299(19) 0.041(2) 0.0303(19) 0.0065(16) 0.0021(15) 0.0032(16) C2 0.039(2) 0.040(2) 0.039(2) 0.0072(18) 0.0027(18) 0.0090(18) C3 0.042(2) 0.043(2) 0.043(2) 0.0010(19) 0.0108(19) 0.0154(19) C4 0.037(2) 0.035(2) 0.0316(19) -0.0020(16) 0.0075(16) 0.0045(17) C5 0.0258(18) 0.0289(18) 0.0288(18) 0.0015(14) 0.0030(14) 0.0004(14) C6 0.0257(17) 0.0262(17) 0.0270(17) 0.0007(13) 0.0067(14) -0.0024(14) C7 0.0241(17) 0.0327(19) 0.0268(17) 0.0009(14) 0.0072(14) 0.0010(14) C8 0.0286(18) 0.0311(18) 0.0224(16) 0.0011(14) 0.0036(13) -0.0026(15) C9 0.0251(17) 0.0306(18) 0.0266(17) 0.0010(14) 0.0018(14) 0.0026(14) C10 0.0223(17) 0.0278(17) 0.0286(17) 0.0016(14) 0.0040(14) 0.0002(13) C11 0.0253(17) 0.0284(18) 0.0275(17) 0.0015(14) 0.0058(14) -0.0013(14) C12 0.037(2) 0.033(2) 0.0295(19) -0.0007(15) 0.0030(16) 0.0057(16) C13 0.040(2) 0.035(2) 0.048(2) -0.0050(18) 0.0114(19) 0.0065(18) C14 0.047(3) 0.042(2) 0.038(2) -0.0113(18) 0.0128(19) -0.0001(19) C15 0.043(2) 0.037(2) 0.0296(19) -0.0050(16) 0.0087(17) -0.0026(18) C16 0.037(2) 0.034(2) 0.0278(18) 0.0010(15) 0.0074(15) -0.0014(16) C17 0.040(2) 0.036(2) 0.037(2) 0.0080(17) 0.0128(17) -0.0015(17) C18 0.034(2) 0.032(2) 0.046(2) 0.0033(17) 0.0101(18) -0.0062(16) C19 0.0286(19) 0.034(2) 0.0314(19) -0.0008(15) 0.0039(15) -0.0033(15) C20 0.0250(17) 0.0265(17) 0.0293(17) 0.0019(14) 0.0050(14) 0.0004(14) C21 0.0245(17) 0.0247(17) 0.0278(17) 0.0010(13) 0.0048(14) 0.0005(13) C22 0.0281(18) 0.0273(17) 0.0259(17) -0.0016(14) 0.0052(14) -0.0030(14) C23 0.0282(18) 0.0327(19) 0.0199(15) -0.0042(13) 0.0039(13) -0.0006(15) C24 0.0298(18) 0.0270(17) 0.0241(16) 0.0018(13) 0.0058(14) 0.0009(14) C25 0.0240(17) 0.0246(17) 0.0272(17) -0.0006(13) 0.0059(13) 0.0018(13) C26 0.0239(17) 0.0251(17) 0.0275(17) -0.0002(13) 0.0040(13) -0.0001(13) C27 0.035(2) 0.033(2) 0.0322(19) -0.0002(15) 0.0087(16) -0.0059(16) C28 0.038(2) 0.036(2) 0.043(2) -0.0035(18) 0.0117(18) -0.0102(18) C29 0.035(2) 0.038(2) 0.042(2) -0.0119(18) 0.0050(17) -0.0095(17) C30 0.0311(19) 0.035(2) 0.0258(17) -0.0046(15) 0.0007(14) -0.0015(16) C31 0.032(2) 0.037(2) 0.0267(17) 0.0043(15) 0.0013(15) 0.0022(16) C32 0.038(2) 0.050(3) 0.0265(18) 0.0018(17) 0.0000(16) 0.0022(19) C33 0.0288(19) 0.044(2) 0.0262(17) -0.0020(16) 0.0010(14) -0.0045(16) C34 0.036(2) 0.057(3) 0.0293(19) 0.0016(19) -0.0001(16) -0.005(2) C35 0.052(3) 0.054(3) 0.039(2) 0.002(2) 0.007(2) 0.000(2) C36 0.080(4) 0.050(3) 0.081(4) -0.001(3) 0.041(3) 0.002(3) C37 0.053(3) 0.044(3) 0.036(2) -0.0041(19) 0.007(2) 0.002(2) C38 0.067(4) 0.049(3) 0.075(4) 0.002(3) 0.024(3) -0.003(3) O1 0.0293(13) 0.0402(15) 0.0215(12) 0.0004(11) 0.0014(10) 0.0044(12) O2 0.0298(13) 0.0393(15) 0.0214(12) -0.0005(10) 0.0029(10) -0.0060(11) P1 0.0398(6) 0.0284(5) 0.0435(6) 0.0002(4) 0.0033(5) 0.0037(4) P2 0.0455(6) 0.0312(5) 0.0407(6) -0.0025(4) 0.0034(5) -0.0036(5) F1 0.135(3) 0.069(2) 0.0453(18) -0.0085(16) 0.013(2) 0.033(2) F2 0.104(3) 0.068(2) 0.0426(16) -0.0159(15) -0.0144(17) 0.0229(19) F3 0.0596(18) 0.0340(14) 0.077(2) 0.0124(13) 0.0172(15) 0.0062(13) F4 0.094(2) 0.0317(14) 0.0657(19) 0.0066(13) 0.0021(17) 0.0050(15) F5 0.0419(16) 0.067(2) 0.090(2) 0.0089(18) 0.0044(16) -0.0053(15) F6 0.0406(18) 0.063(2) 0.165(4) 0.008(2) 0.023(2) 0.0101(16) F11 0.080(3) 0.127(4) 0.087(3) -0.068(3) 0.006(2) -0.004(2) F12 0.131(4) 0.125(4) 0.084(3) -0.056(3) -0.020(3) 0.067(3) F13 0.087(3) 0.088(3) 0.099(3) 0.054(2) -0.040(2) -0.041(2) F14 0.070(2) 0.074(2) 0.114(3) 0.052(2) 0.018(2) 0.0048(19) F15 0.0425(17) 0.075(2) 0.115(3) 0.015(2) 0.0075(18) 0.0038(16) F16 0.0493(17) 0.069(2) 0.0600(18) 0.0069(15) -0.0063(14) -0.0184(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.10822(3) 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 . N1 . 2.156(3) yes Co1 . N2 . 1.919(3) yes Co1 . N3 . 2.161(3) yes Co1 . N4 . 2.007(3) yes Co1 . N5 . 1.874(3) yes Co1 . N6 . 2.009(3) yes N1 . C1 . 1.345(5) yes N1 . C5 . 1.353(5) yes N2 . C6 . 1.380(5) yes N2 . C10 . 1.333(4) yes N3 . C11 . 1.349(4) yes N3 . C15 . 1.336(5) yes N4 . C16 . 1.337(5) yes N4 . C20 . 1.363(5) yes N5 . C21 . 1.347(4) yes N5 . C25 . 1.350(4) yes N6 . C26 . 1.366(4) yes N6 . C30 . 1.342(5) yes N7 . C35 . 1.136(7) yes N8 . C37 . 1.141(6) yes C1 . C2 . 1.388(6) yes C1 . H11 . 0.946 no C2 . C3 . 1.384(6) yes C2 . H21 . 0.948 no C3 . C4 . 1.383(6) yes C3 . H31 . 0.959 no C4 . C5 . 1.392(5) yes C4 . H41 . 0.943 no C5 . C6 . 1.488(5) yes C6 . C7 . 1.380(5) yes C7 . C8 . 1.401(5) yes C7 . H71 . 0.957 no C8 . C9 . 1.394(5) yes C8 . O1 . 1.348(4) yes C9 . C10 . 1.393(5) yes C9 . H91 . 0.952 no C10 . C11 . 1.486(5) yes C11 . C12 . 1.385(5) yes C12 . C13 . 1.389(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.392(6) yes C13 . H131 . 0.940 no C14 . C15 . 1.387(6) yes C14 . H141 . 0.949 no C15 . H151 . 0.952 no C16 . C17 . 1.379(6) yes C16 . H161 . 0.950 no C17 . C18 . 1.383(6) yes C17 . H171 . 0.950 no C18 . C19 . 1.386(5) yes C18 . H181 . 0.946 no C19 . C20 . 1.385(5) yes C19 . H191 . 0.948 no C20 . C21 . 1.474(5) yes C21 . C22 . 1.390(5) yes C22 . C23 . 1.404(5) yes C22 . H221 . 0.960 no C23 . C24 . 1.405(5) yes C23 . O2 . 1.347(4) yes C24 . C25 . 1.377(5) yes C24 . H241 . 0.947 no C25 . C26 . 1.476(5) yes C26 . C27 . 1.389(5) yes C27 . C28 . 1.392(5) yes C27 . H271 . 0.946 no C28 . C29 . 1.386(6) yes C28 . H281 . 0.959 no C29 . C30 . 1.381(6) yes C29 . H291 . 0.942 no C30 . H301 . 0.948 no C31 . C32 . 1.504(5) yes C31 . O1 . 1.453(4) yes C31 . H311 . 0.992 no C31 . H312 . 1.004 no C32 . H321 . 0.975 no C32 . H322 . 0.975 no C32 . H323 . 0.978 no C33 . C34 . 1.502(5) yes C33 . O2 . 1.452(4) yes C33 . H331 . 0.997 no C33 . H332 . 0.991 no C34 . H341 . 0.974 no C34 . H342 . 0.983 no C34 . H343 . 0.982 no C35 . C36 . 1.433(7) yes C36 . H361 . 0.962 no C36 . H362 . 0.965 no C36 . H363 . 0.959 no C37 . C38 . 1.448(7) yes C38 . H381 . 0.957 no C38 . H382 . 0.967 no C38 . H383 . 0.954 no P1 . F1 . 1.600(3) yes P1 . F2 . 1.585(3) yes P1 . F3 . 1.598(3) yes P1 . F4 . 1.586(3) yes P1 . F5 . 1.592(3) yes P1 . F6 . 1.586(3) yes P2 . F11 . 1.575(3) yes P2 . F12 . 1.565(4) yes P2 . F13 . 1.581(3) yes P2 . F14 . 1.571(3) yes P2 . F15 . 1.589(3) yes P2 . F16 . 1.604(3) yes 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 N1 . Co1 . N2 . 79.31(12) yes N1 . Co1 . N3 . 157.65(11) yes N2 . Co1 . N3 . 78.38(12) yes N1 . Co1 . N4 . 95.03(12) yes N2 . Co1 . N4 . 96.97(12) yes N3 . Co1 . N4 . 89.05(12) yes N1 . Co1 . N5 . 102.55(12) yes N2 . Co1 . N5 . 177.67(13) yes N3 . Co1 . N5 . 99.79(12) yes N4 . Co1 . N5 . 81.51(12) yes N1 . Co1 . N6 . 88.60(12) yes N2 . Co1 . N6 . 100.89(12) yes N3 . Co1 . N6 . 94.23(12) yes N4 . Co1 . N6 . 162.14(12) yes N5 . Co1 . N6 . 80.63(12) yes Co1 . N1 . C1 . 129.0(3) yes Co1 . N1 . C5 . 112.8(2) yes C1 . N1 . C5 . 118.2(3) yes Co1 . N2 . C6 . 119.6(2) yes Co1 . N2 . C10 . 121.2(2) yes C6 . N2 . C10 . 119.2(3) yes Co1 . N3 . C11 . 111.8(2) yes Co1 . N3 . C15 . 129.2(3) yes C11 . N3 . C15 . 118.6(3) yes Co1 . N4 . C16 . 128.2(3) yes Co1 . N4 . C20 . 113.1(2) yes C16 . N4 . C20 . 118.5(3) yes Co1 . N5 . C21 . 119.0(2) yes Co1 . N5 . C25 . 120.4(2) yes C21 . N5 . C25 . 120.6(3) yes Co1 . N6 . C26 . 114.0(2) yes Co1 . N6 . C30 . 127.4(3) yes C26 . N6 . C30 . 118.6(3) yes N1 . C1 . C2 . 122.7(4) yes N1 . C1 . H11 . 116.8 no C2 . C1 . H11 . 120.6 no C1 . C2 . C3 . 118.9(4) yes C1 . C2 . H21 . 120.8 no C3 . C2 . H21 . 120.3 no C2 . C3 . C4 . 119.1(4) yes C2 . C3 . H31 . 120.7 no C4 . C3 . H31 . 120.2 no C3 . C4 . C5 . 119.1(4) yes C3 . C4 . H41 . 121.1 no C5 . C4 . H41 . 119.8 no C4 . C5 . N1 . 122.0(3) yes C4 . C5 . C6 . 123.9(3) yes N1 . C5 . C6 . 114.1(3) yes C5 . C6 . N2 . 114.3(3) yes C5 . C6 . C7 . 124.4(3) yes N2 . C6 . C7 . 121.3(3) yes C6 . C7 . C8 . 118.8(3) yes C6 . C7 . H71 . 120.7 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 119.7(3) yes C7 . C8 . O1 . 116.3(3) yes C9 . C8 . O1 . 124.0(3) yes C8 . C9 . C10 . 118.4(3) yes C8 . C9 . H91 . 121.2 no C10 . C9 . H91 . 120.5 no C9 . C10 . N2 . 122.6(3) yes C9 . C10 . C11 . 123.6(3) yes N2 . C10 . C11 . 113.8(3) yes C10 . C11 . N3 . 114.4(3) yes C10 . C11 . C12 . 123.3(3) yes N3 . C11 . C12 . 122.3(3) yes C11 . C12 . C13 . 118.7(4) yes C11 . C12 . H121 . 119.7 no C13 . C12 . H121 . 121.6 no C12 . C13 . C14 . 119.2(4) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 120.6 no C13 . C14 . C15 . 118.3(4) yes C13 . C14 . H141 . 121.1 no C15 . C14 . H141 . 120.6 no C14 . C15 . N3 . 122.9(4) yes C14 . C15 . H151 . 120.4 no N3 . C15 . H151 . 116.8 no N4 . C16 . C17 . 122.5(4) yes N4 . C16 . H161 . 117.4 no C17 . C16 . H161 . 120.1 no C16 . C17 . C18 . 119.3(4) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 118.9(4) yes C17 . C18 . H181 . 120.6 no C19 . C18 . H181 . 120.5 no C18 . C19 . C20 . 119.0(4) yes C18 . C19 . H191 . 121.7 no C20 . C19 . H191 . 119.3 no C19 . C20 . N4 . 121.8(3) yes C19 . C20 . C21 . 124.8(3) yes N4 . C20 . C21 . 113.4(3) yes C20 . C21 . N5 . 112.6(3) yes C20 . C21 . C22 . 125.7(3) yes N5 . C21 . C22 . 121.7(3) yes C21 . C22 . C23 . 117.8(3) yes C21 . C22 . H221 . 120.5 no C23 . C22 . H221 . 121.7 no C22 . C23 . C24 . 119.9(3) yes C22 . C23 . O2 . 123.6(3) yes C24 . C23 . O2 . 116.5(3) yes C23 . C24 . C25 . 118.6(3) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 121.0 no C24 . C25 . N5 . 121.3(3) yes C24 . C25 . C26 . 127.1(3) yes N5 . C25 . C26 . 111.5(3) yes C25 . C26 . N6 . 113.4(3) yes C25 . C26 . C27 . 125.1(3) yes N6 . C26 . C27 . 121.5(3) yes C26 . C27 . C28 . 119.3(4) yes C26 . C27 . H271 . 120.1 no C28 . C27 . H271 . 120.5 no C27 . C28 . C29 . 118.7(4) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.9 no C28 . C29 . C30 . 119.5(4) yes C28 . C29 . H291 . 120.5 no C30 . C29 . H291 . 120.0 no C29 . C30 . N6 . 122.4(4) yes C29 . C30 . H301 . 120.0 no N6 . C30 . H301 . 117.6 no C32 . C31 . O1 . 107.3(3) yes C32 . C31 . H311 . 109.2 no O1 . C31 . H311 . 110.8 no C32 . C31 . H312 . 109.8 no O1 . C31 . H312 . 110.0 no H311 . C31 . H312 . 109.7 no C31 . C32 . H321 . 108.1 no C31 . C32 . H322 . 109.4 no H321 . C32 . H322 . 110.2 no C31 . C32 . H323 . 110.7 no H321 . C32 . H323 . 108.3 no H322 . C32 . H323 . 110.1 no C34 . C33 . O2 . 108.3(3) yes C34 . C33 . H331 . 110.0 no O2 . C33 . H331 . 108.7 no C34 . C33 . H332 . 110.6 no O2 . C33 . H332 . 110.1 no H331 . C33 . H332 . 109.2 no C33 . C34 . H341 . 107.9 no C33 . C34 . H342 . 110.0 no H341 . C34 . H342 . 109.7 no C33 . C34 . H343 . 109.9 no H341 . C34 . H343 . 109.8 no H342 . C34 . H343 . 109.5 no N7 . C35 . C36 . 178.6(6) yes C35 . C36 . H361 . 109.5 no C35 . C36 . H362 . 109.3 no H361 . C36 . H362 . 109.0 no C35 . C36 . H363 . 108.9 no H361 . C36 . H363 . 110.3 no H362 . C36 . H363 . 109.7 no N8 . C37 . C38 . 178.6(5) yes C37 . C38 . H381 . 108.5 no C37 . C38 . H382 . 108.0 no H381 . C38 . H382 . 110.2 no C37 . C38 . H383 . 109.2 no H381 . C38 . H383 . 109.8 no H382 . C38 . H383 . 111.1 no C31 . O1 . C8 . 116.3(3) yes C33 . O2 . C23 . 116.3(3) yes F1 . P1 . F2 . 178.7(2) yes F1 . P1 . F3 . 89.39(18) yes F2 . P1 . F3 . 90.17(18) yes F1 . P1 . F4 . 89.41(18) yes F2 . P1 . F4 . 91.03(18) yes F3 . P1 . F4 . 178.74(18) yes F1 . P1 . F5 . 89.0(2) yes F2 . P1 . F5 . 89.8(2) yes F3 . P1 . F5 . 88.38(17) yes F4 . P1 . F5 . 91.22(19) yes F1 . P1 . F6 . 90.9(2) yes F2 . P1 . F6 . 90.3(2) yes F3 . P1 . F6 . 91.02(18) yes F4 . P1 . F6 . 89.4(2) yes F5 . P1 . F6 . 179.4(2) yes F11 . P2 . F12 . 178.6(3) yes F11 . P2 . F13 . 91.2(3) yes F12 . P2 . F13 . 88.3(3) yes F11 . P2 . F14 . 89.1(3) yes F12 . P2 . F14 . 91.4(3) yes F13 . P2 . F14 . 179.3(2) yes F11 . P2 . F15 . 89.6(2) yes F12 . P2 . F15 . 91.7(2) yes F13 . P2 . F15 . 87.5(2) yes F14 . P2 . F15 . 91.8(2) yes F11 . P2 . F16 . 89.7(2) yes F12 . P2 . F16 . 89.0(2) yes F13 . P2 . F16 . 91.76(19) yes F14 . P2 . F16 . 88.91(18) yes F15 . P2 . F16 . 179.0(2) yes # Attachment 'methoxy_solvate.cif' data_kh034_173k _database_code_depnum_ccdc_archive 'CCDC 693546' _audit_creation_date 08-06-26 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '6261045 kh034_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 30.2955(4) _cell_length_b 12.46980(10) _cell_length_c 19.6441(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7421.12(14) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n ' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y+1/2,z x+1/2,y+1/2,-z 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C34 H28 Co1 F12 N6 O3 P2 # Dc = 1.64 Fooo = 3704.00 Mu = 6.55 M = 917.49 # Found Formula = C34 H29 Co1 F12 N7 O2 P2 # Dc = 1.64 FOOO = 3704.00 Mu = 6.53 M = 916.51 _chemical_formula_sum 'C34 H29 Co1 F12 N7 O2 P2' _chemical_formula_moiety 'C32 H26 Co N6 O2, 2(F6 P), C2 H3 N' _chemical_compound_source ? _chemical_formula_weight 916.51 _cell_measurement_reflns_used 9679 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 0.653 # Sheldrick geometric approximatio 0.86 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction '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 173 _diffrn_reflns_number 34884 _reflns_number_total 8864 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 8864 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8854 _diffrn_reflns_theta_min 1.344 _diffrn_reflns_theta_max 27.881 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.881 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 39 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.48 _refine_diff_density_max 0.56 _refine_ls_number_reflns 5265 _refine_ls_number_restraints 0 _refine_ls_number_parameters 524 #_refine_ls_R_factor_ref 0.0373 _refine_ls_wR_factor_ref 0.0432 _refine_ls_goodness_of_fit_ref 1.0935 #_reflns_number_all 8806 _refine_ls_R_factor_all 0.0696 _refine_ls_wR_factor_all 0.0740 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.4\s(I) _reflns_number_gt 5265 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_gt 0.0432 _refine_ls_shift/su_max 0.001597 # 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 constr # 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: 0.455 0.363 0.211 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. 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--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # 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. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. 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. 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 0.355016(10) 0.49424(2) 0.502868(16) 0.0262 1.0000 Uani . . . . . . N1 N 0.29302(7) 0.55354(16) 0.53410(10) 0.0284 1.0000 Uani . . . . . . N2 N 0.35984(6) 0.48052(16) 0.59955(10) 0.0265 1.0000 Uani . . . . . . N3 N 0.41919(7) 0.42815(17) 0.51099(10) 0.0301 1.0000 Uani . . . . . . N4 N 0.37813(7) 0.64845(17) 0.49353(10) 0.0299 1.0000 Uani . . . . . . N5 N 0.35328(6) 0.50967(16) 0.40649(10) 0.0273 1.0000 Uani . . . . . . N6 N 0.32981(7) 0.34614(16) 0.47587(10) 0.0275 1.0000 Uani . . . . . . N7 N 0.4331(2) 0.1103(4) 0.5133(2) 0.1206 1.0000 Uani . . . . . . C1 C 0.25996(8) 0.5903(2) 0.49559(13) 0.0332 1.0000 Uani . . . . . . C2 C 0.22107(9) 0.6307(2) 0.52256(14) 0.0368 1.0000 Uani . . . . . . C3 C 0.21632(9) 0.6325(2) 0.59283(15) 0.0379 1.0000 Uani . . . . . . C4 C 0.25007(9) 0.5944(2) 0.63357(13) 0.0338 1.0000 Uani . . . . . . C5 C 0.28822(8) 0.55599(19) 0.60277(12) 0.0275 1.0000 Uani . . . . . . C6 C 0.32671(8) 0.51392(18) 0.64072(12) 0.0275 1.0000 Uani . . . . . . C7 C 0.32997(8) 0.5079(2) 0.71069(12) 0.0310 1.0000 Uani . . . . . . C8 C 0.36827(9) 0.4642(2) 0.73918(12) 0.0319 1.0000 Uani . . . . . . C9 C 0.40264(9) 0.4308(2) 0.69700(13) 0.0328 1.0000 Uani . . . . . . C10 C 0.39742(8) 0.4414(2) 0.62713(12) 0.0283 1.0000 Uani . . . . . . C11 C 0.43140(8) 0.4122(2) 0.57659(12) 0.0299 1.0000 Uani . . . . . . C12 C 0.47250(9) 0.3717(2) 0.59357(14) 0.0384 1.0000 Uani . . . . . . C13 C 0.50145(10) 0.3457(3) 0.54191(15) 0.0436 1.0000 Uani . . . . . . C14 C 0.48918(10) 0.3612(3) 0.47520(15) 0.0445 1.0000 Uani . . . . . . C15 C 0.44790(9) 0.4027(2) 0.46166(13) 0.0364 1.0000 Uani . . . . . . C16 C 0.38966(8) 0.7158(2) 0.54353(14) 0.0351 1.0000 Uani . . . . . . C17 C 0.40097(10) 0.8215(2) 0.53172(16) 0.0429 1.0000 Uani . . . . . . C18 C 0.40001(10) 0.8598(2) 0.46539(17) 0.0437 1.0000 Uani . . . . . . C19 C 0.38859(9) 0.7911(2) 0.41308(14) 0.0361 1.0000 Uani . . . . . . C20 C 0.37840(8) 0.6853(2) 0.42841(13) 0.0295 1.0000 Uani . . . . . . C21 C 0.36730(8) 0.6024(2) 0.37743(13) 0.0294 1.0000 Uani . . . . . . C22 C 0.37152(9) 0.6123(2) 0.30807(13) 0.0351 1.0000 Uani . . . . . . C23 C 0.36144(9) 0.5235(2) 0.26731(12) 0.0365 1.0000 Uani . . . . . . C24 C 0.34655(9) 0.4283(2) 0.29681(13) 0.0328 1.0000 Uani . . . . . . C25 C 0.34274(8) 0.4248(2) 0.36732(12) 0.0280 1.0000 Uani . . . . . . C26 C 0.32773(8) 0.33096(19) 0.40738(11) 0.0268 1.0000 Uani . . . . . . C27 C 0.31269(9) 0.2361(2) 0.37917(12) 0.0327 1.0000 Uani . . . . . . C28 C 0.29911(9) 0.1541(2) 0.42193(14) 0.0369 1.0000 Uani . . . . . . C29 C 0.30091(10) 0.1692(2) 0.49135(13) 0.0369 1.0000 Uani . . . . . . C30 C 0.31667(9) 0.2662(2) 0.51645(12) 0.0327 1.0000 Uani . . . . . . C31 C 0.40674(11) 0.4041(3) 0.83733(15) 0.0503 1.0000 Uani . . . . . . C32 C 0.35881(12) 0.4459(3) 0.15651(14) 0.0535 1.0000 Uani . . . . . . C33 C 0.4553(2) 0.0775(5) 0.5562(3) 0.0954 1.0000 Uani . . . . . . C34 C 0.4810(2) 0.0333(6) 0.6097(3) 0.1347 1.0000 Uani . . . . . . O1 O 0.36915(7) 0.45713(18) 0.80764(9) 0.0421 1.0000 Uani . . . . . . O2 O 0.36705(8) 0.53740(17) 0.19961(9) 0.0470 1.0000 Uani . . . . . . P1 P 0.47934(4) 0.71924(10) 0.72516(5) 0.0691 1.0000 Uani . . . . . . P2 P 0.2500 0.7500 0.31565(5) 0.0316 1.0000 Uani S T . . . . P3 P 0.2500 0.2500 0.19540(4) 0.0281 1.0000 Uani S T . . . . F1 F 0.45725(9) 0.6709(4) 0.78936(13) 0.1250 1.0000 Uani . . . . . . F2 F 0.50139(16) 0.7737(3) 0.66027(15) 0.1542 1.0000 Uani . . . . . . F3 F 0.52648(8) 0.7111(3) 0.75998(16) 0.1051 1.0000 Uani . . . . . . F4 F 0.43211(13) 0.7310(3) 0.69117(16) 0.1342 1.0000 Uani . . . . . . F5 F 0.47432(13) 0.8352(3) 0.75724(17) 0.1375 1.0000 Uani . . . . . . F6 F 0.48443(11) 0.6079(2) 0.69100(16) 0.1112 1.0000 Uani . . . . . . F7 F 0.28706(5) 0.75838(14) 0.37360(8) 0.0448 1.0000 Uani . . . . . . F8 F 0.24522(6) 0.87824(13) 0.31571(8) 0.0460 1.0000 Uani . . . . . . F9 F 0.21275(6) 0.74193(15) 0.25805(8) 0.0454 1.0000 Uani . . . . . . F10 F 0.25356(5) 0.34042(13) 0.25283(7) 0.0403 1.0000 Uani . . . . . . F11 F 0.30289(5) 0.23727(12) 0.19543(8) 0.0364 1.0000 Uani . . . . . . F12 F 0.25368(5) 0.34000(12) 0.13751(7) 0.0378 1.0000 Uani . . . . . . H11 H 0.2645 0.5894 0.4479 0.0391 1.0000 Uiso R . . . . . H21 H 0.1980 0.6566 0.4946 0.0434 1.0000 Uiso R . . . . . H31 H 0.1904 0.6598 0.6127 0.0450 1.0000 Uiso R . . . . . H41 H 0.2472 0.5953 0.6805 0.0404 1.0000 Uiso R . . . . . H71 H 0.3073 0.5314 0.7387 0.0373 1.0000 Uiso R . . . . . H91 H 0.4285 0.4024 0.7155 0.0386 1.0000 Uiso R . . . . . H121 H 0.4803 0.3609 0.6389 0.0452 1.0000 Uiso R . . . . . H131 H 0.5295 0.3167 0.5521 0.0513 1.0000 Uiso R . . . . . H141 H 0.5076 0.3438 0.4396 0.0517 1.0000 Uiso R . . . . . H151 H 0.4396 0.4136 0.4167 0.0420 1.0000 Uiso R . . . . . H161 H 0.3903 0.6873 0.5884 0.0429 1.0000 Uiso R . . . . . H171 H 0.4095 0.8663 0.5682 0.0502 1.0000 Uiso R . . . . . H181 H 0.4064 0.9308 0.4560 0.0512 1.0000 Uiso R . . . . . H191 H 0.3881 0.8160 0.3686 0.0429 1.0000 Uiso R . . . . . H221 H 0.3814 0.6746 0.2887 0.0420 1.0000 Uiso R . . . . . H241 H 0.3386 0.3676 0.2704 0.0395 1.0000 Uiso R . . . . . H271 H 0.3117 0.2275 0.3319 0.0378 1.0000 Uiso R . . . . . H281 H 0.2889 0.0894 0.4044 0.0428 1.0000 Uiso R . . . . . H291 H 0.2914 0.1151 0.5210 0.0419 1.0000 Uiso R . . . . . H301 H 0.3182 0.2774 0.5635 0.0392 1.0000 Uiso R . . . . . H311 H 0.4020 0.3997 0.8869 0.0755 1.0000 Uiso R . . . . . H312 H 0.4334 0.4444 0.8280 0.0755 1.0000 Uiso R . . . . . H313 H 0.4097 0.3319 0.8183 0.0754 1.0000 Uiso R . . . . . H321 H 0.3616 0.4695 0.1098 0.0869 1.0000 Uiso R . . . . . H322 H 0.3820 0.3897 0.1634 0.0858 1.0000 Uiso R . . . . . H323 H 0.3290 0.4167 0.1640 0.0865 1.0000 Uiso R . . . . . H341 H 0.4998 0.0881 0.6286 0.2012 1.0000 Uiso R . . . . . H342 H 0.4983 -0.0243 0.5897 0.2013 1.0000 Uiso R . . . . . H343 H 0.4612 0.0051 0.6444 0.2011 1.0000 Uiso 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 0.02649(15) 0.02675(15) 0.02524(15) -0.00169(13) 0.00108(13) -0.00115(13) N1 0.0325(11) 0.0262(10) 0.0264(10) -0.0009(8) 0.0027(8) -0.0031(9) N2 0.0269(10) 0.0269(10) 0.0258(9) -0.0015(8) 0.0013(8) -0.0018(8) N3 0.0310(11) 0.0332(10) 0.0261(10) -0.0021(8) -0.0022(8) 0.0008(9) N4 0.0280(10) 0.0322(10) 0.0296(10) -0.0003(9) -0.0001(8) 0.0024(8) N5 0.0262(9) 0.0272(10) 0.0285(9) 0.0000(8) -0.0007(8) -0.0020(8) N6 0.0277(10) 0.0320(11) 0.0229(9) -0.0024(8) 0.0000(8) 0.0004(9) N7 0.185(5) 0.106(3) 0.072(3) 0.006(2) -0.028(3) -0.070(4) C1 0.0389(14) 0.0293(12) 0.0315(12) 0.0037(11) -0.0010(11) -0.0046(10) C2 0.0358(14) 0.0334(14) 0.0411(14) 0.0063(11) -0.0049(11) 0.0007(11) C3 0.0339(14) 0.0379(15) 0.0419(15) -0.0003(12) 0.0035(12) 0.0062(11) C4 0.0361(13) 0.0343(13) 0.0311(12) -0.0018(10) 0.0041(11) 0.0027(11) C5 0.0314(12) 0.0251(12) 0.0260(11) -0.0027(9) 0.0031(9) -0.0025(9) C6 0.0300(12) 0.0236(11) 0.0290(11) -0.0027(9) 0.0056(9) -0.0007(10) C7 0.0326(12) 0.0334(13) 0.0268(11) -0.0030(10) 0.0056(9) 0.0000(11) C8 0.0369(14) 0.0356(13) 0.0233(11) -0.0005(10) 0.0016(10) -0.0048(11) C9 0.0329(13) 0.0377(14) 0.0278(12) -0.0002(10) -0.0021(10) -0.0014(11) C10 0.0272(12) 0.0289(12) 0.0287(12) -0.0011(9) 0.0003(9) -0.0019(10) C11 0.0307(12) 0.0334(13) 0.0255(11) -0.0008(10) 0.0004(10) 0.0001(10) C12 0.0342(14) 0.0507(17) 0.0304(13) 0.0015(12) -0.0011(11) 0.0060(12) C13 0.0315(13) 0.0558(18) 0.0434(16) -0.0018(13) 0.0038(12) 0.0118(13) C14 0.0424(16) 0.0553(18) 0.0356(14) -0.0085(13) 0.0106(12) 0.0059(14) C15 0.0385(14) 0.0463(16) 0.0245(12) -0.0057(11) 0.0012(10) 0.0012(12) C16 0.0317(13) 0.0418(15) 0.0319(13) -0.0060(11) -0.0002(10) 0.0017(11) C17 0.0415(16) 0.0400(16) 0.0473(16) -0.0140(13) -0.0018(13) -0.0041(13) C18 0.0422(16) 0.0330(14) 0.0558(18) -0.0029(13) 0.0029(14) -0.0073(12) C19 0.0363(14) 0.0324(13) 0.0397(14) 0.0035(11) 0.0006(11) -0.0041(11) C20 0.0260(12) 0.0305(13) 0.0321(12) 0.0011(10) -0.0004(10) 0.0000(10) C21 0.0273(12) 0.0302(12) 0.0306(12) 0.0021(10) -0.0010(10) -0.0017(10) C22 0.0389(14) 0.0342(13) 0.0323(13) 0.0054(11) -0.0016(11) -0.0085(11) C23 0.0413(15) 0.0459(16) 0.0224(11) 0.0036(11) -0.0015(11) -0.0102(12) C24 0.0366(14) 0.0368(14) 0.0250(12) 0.0004(10) -0.0013(10) -0.0049(11) C25 0.0270(12) 0.0298(12) 0.0273(11) 0.0002(9) -0.0034(9) -0.0015(9) C26 0.0278(12) 0.0292(12) 0.0235(11) 0.0004(9) 0.0011(9) 0.0008(10) C27 0.0407(14) 0.0342(13) 0.0231(11) -0.0011(10) -0.0004(10) -0.0019(11) C28 0.0442(15) 0.0298(13) 0.0366(14) -0.0012(11) 0.0027(12) -0.0070(11) C29 0.0457(15) 0.0332(13) 0.0320(13) 0.0059(11) 0.0049(12) -0.0038(11) C30 0.0362(13) 0.0385(14) 0.0234(11) 0.0008(10) 0.0037(10) 0.0004(11) C31 0.0508(18) 0.072(2) 0.0282(13) 0.0043(14) -0.0062(13) 0.0058(16) C32 0.080(2) 0.0563(19) 0.0241(13) -0.0015(12) 0.0032(14) -0.0248(18) C33 0.113(4) 0.101(4) 0.072(3) -0.015(3) -0.001(3) -0.054(3) C34 0.097(4) 0.192(7) 0.116(5) -0.036(5) -0.034(4) -0.025(4) O1 0.0478(11) 0.0565(13) 0.0219(9) 0.0006(8) 0.0010(8) 0.0044(10) O2 0.0671(14) 0.0493(12) 0.0245(9) 0.0040(8) -0.0007(9) -0.0240(11) P1 0.0830(7) 0.0861(7) 0.0382(4) -0.0175(5) 0.0028(5) -0.0181(6) P2 0.0338(5) 0.0353(5) 0.0256(4) 0.0000 0.0000 -0.0006(4) P3 0.0327(4) 0.0272(4) 0.0245(4) 0.0000 0.0000 -0.0014(4) F1 0.0643(15) 0.253(4) 0.0580(14) 0.045(2) 0.0156(12) 0.007(2) F2 0.264(5) 0.128(3) 0.0702(18) -0.0131(18) 0.030(2) -0.113(3) F3 0.0585(15) 0.132(2) 0.125(2) -0.038(2) 0.0082(15) -0.0084(15) F4 0.154(3) 0.145(3) 0.104(2) -0.014(2) -0.084(2) 0.000(2) F5 0.175(3) 0.126(3) 0.112(2) -0.069(2) -0.061(2) 0.031(2) F6 0.132(2) 0.0785(18) 0.123(2) -0.0382(17) 0.042(2) -0.0383(17) F7 0.0419(9) 0.0561(10) 0.0365(8) -0.0057(8) -0.0101(7) 0.0007(8) F8 0.0570(11) 0.0358(9) 0.0453(9) -0.0002(7) 0.0023(8) 0.0013(8) F9 0.0449(9) 0.0543(10) 0.0368(8) -0.0045(8) -0.0106(7) 0.0015(8) F10 0.0451(9) 0.0415(8) 0.0342(7) -0.0121(7) -0.0016(7) -0.0009(7) F11 0.0338(8) 0.0372(8) 0.0383(8) -0.0012(7) 0.0006(6) -0.0003(6) F12 0.0460(9) 0.0337(8) 0.0337(7) 0.0078(6) 0.0017(7) -0.0016(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12121(16) 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 . N1 . 2.110(2) yes Co1 . N2 . 1.913(2) yes Co1 . N3 . 2.118(2) yes Co1 . N4 . 2.055(2) yes Co1 . N5 . 1.904(2) yes Co1 . N6 . 2.068(2) yes N1 . C1 . 1.337(3) yes N1 . C5 . 1.357(3) yes N2 . C6 . 1.354(3) yes N2 . C10 . 1.352(3) yes N3 . C11 . 1.355(3) yes N3 . C15 . 1.340(3) yes N4 . C16 . 1.339(3) yes N4 . C20 . 1.360(3) yes N5 . C21 . 1.358(3) yes N5 . C25 . 1.347(3) yes N6 . C26 . 1.360(3) yes N6 . C30 . 1.337(3) yes N7 . C33 . 1.153(7) yes C1 . C2 . 1.386(4) yes C1 . H11 . 0.947 no C2 . C3 . 1.388(4) yes C2 . H21 . 0.946 no C3 . C4 . 1.383(4) yes C3 . H31 . 0.940 no C4 . C5 . 1.390(4) yes C4 . H41 . 0.925 no C5 . C6 . 1.480(3) yes C6 . C7 . 1.380(3) yes C7 . C8 . 1.399(4) yes C7 . H71 . 0.927 no C8 . C9 . 1.394(4) yes C8 . O1 . 1.348(3) yes C9 . C10 . 1.388(3) yes C9 . H91 . 0.933 no C10 . C11 . 1.476(3) yes C11 . C12 . 1.385(4) yes C12 . C13 . 1.380(4) yes C12 . H121 . 0.931 no C13 . C14 . 1.376(4) yes C13 . H131 . 0.946 no C14 . C15 . 1.379(4) yes C14 . H141 . 0.922 no C15 . H151 . 0.929 no C16 . C17 . 1.381(4) yes C16 . H161 . 0.950 no C17 . C18 . 1.388(4) yes C17 . H171 . 0.944 no C18 . C19 . 1.382(4) yes C18 . H181 . 0.924 no C19 . C20 . 1.387(4) yes C19 . H191 . 0.927 no C20 . C21 . 1.478(3) yes C21 . C22 . 1.374(4) yes C22 . C23 . 1.401(4) yes C22 . H221 . 0.915 no C23 . C24 . 1.395(4) yes C23 . O2 . 1.352(3) yes C24 . C25 . 1.391(3) yes C24 . H241 . 0.949 no C25 . C26 . 1.482(3) yes C26 . C27 . 1.383(3) yes C27 . C28 . 1.386(4) yes C27 . H271 . 0.935 no C28 . C29 . 1.378(4) yes C28 . H281 . 0.930 no C29 . C30 . 1.391(4) yes C29 . H291 . 0.935 no C30 . H301 . 0.936 no C31 . O1 . 1.440(4) yes C31 . H311 . 0.986 no C31 . H312 . 0.969 no C31 . H313 . 0.979 no C32 . O2 . 1.443(4) yes C32 . H321 . 0.968 no C32 . H322 . 1.002 no C32 . H323 . 0.986 no C33 . C34 . 1.420(9) yes C34 . H341 . 0.963 no C34 . H342 . 0.974 no C34 . H343 . 0.973 no P1 . F1 . 1.550(3) yes P1 . F2 . 1.591(3) yes P1 . F3 . 1.587(3) yes P1 . F4 . 1.586(3) yes P1 . F5 . 1.585(3) yes P1 . F6 . 1.550(3) yes P2 . F8 7_565 1.6056(16) yes P2 . F7 7_565 1.6022(16) yes P2 . F9 7_565 1.6014(17) yes P2 . F7 . 1.6022(16) yes P2 . F8 . 1.6056(16) yes P2 . F9 . 1.6014(17) yes P3 . F11 7_555 1.6100(15) yes P3 . F12 7_555 1.6017(15) yes P3 . F10 7_555 1.5987(15) yes P3 . F10 . 1.5987(15) yes P3 . F11 . 1.6100(15) yes P3 . F12 . 1.6017(15) yes 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 N1 . Co1 . N2 . 79.08(8) yes N1 . Co1 . N3 . 158.72(8) yes N2 . Co1 . N3 . 79.64(8) yes N1 . Co1 . N4 . 90.07(8) yes N2 . Co1 . N4 . 98.41(8) yes N3 . Co1 . N4 . 93.33(8) yes N1 . Co1 . N5 . 103.25(8) yes N2 . Co1 . N5 . 177.12(9) yes N3 . Co1 . N5 . 98.02(8) yes N4 . Co1 . N5 . 79.98(8) yes N1 . Co1 . N6 . 93.37(8) yes N2 . Co1 . N6 . 101.71(8) yes N3 . Co1 . N6 . 90.62(8) yes N4 . Co1 . N6 . 159.87(8) yes N5 . Co1 . N6 . 79.92(8) yes Co1 . N1 . C1 . 128.53(17) yes Co1 . N1 . C5 . 113.10(16) yes C1 . N1 . C5 . 118.3(2) yes Co1 . N2 . C6 . 120.58(16) yes Co1 . N2 . C10 . 119.64(16) yes C6 . N2 . C10 . 119.7(2) yes Co1 . N3 . C11 . 112.30(16) yes Co1 . N3 . C15 . 129.31(17) yes C11 . N3 . C15 . 118.4(2) yes Co1 . N4 . C16 . 127.64(18) yes Co1 . N4 . C20 . 113.75(16) yes C16 . N4 . C20 . 118.4(2) yes Co1 . N5 . C21 . 119.70(16) yes Co1 . N5 . C25 . 119.69(16) yes C21 . N5 . C25 . 120.2(2) yes Co1 . N6 . C26 . 113.27(16) yes Co1 . N6 . C30 . 128.52(16) yes C26 . N6 . C30 . 118.2(2) yes N1 . C1 . C2 . 123.0(2) yes N1 . C1 . H11 . 116.6 no C2 . C1 . H11 . 120.3 no C1 . C2 . C3 . 118.3(3) yes C1 . C2 . H21 . 122.0 no C3 . C2 . H21 . 119.7 no C2 . C3 . C4 . 119.6(3) yes C2 . C3 . H31 . 120.4 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 118.8(2) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 121.0 no C4 . C5 . N1 . 122.0(2) yes C4 . C5 . C6 . 123.9(2) yes N1 . C5 . C6 . 114.1(2) yes C5 . C6 . N2 . 113.1(2) yes C5 . C6 . C7 . 125.3(2) yes N2 . C6 . C7 . 121.7(2) yes C6 . C7 . C8 . 118.6(2) yes C6 . C7 . H71 . 121.4 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 119.9(2) yes C7 . C8 . O1 . 116.2(2) yes C9 . C8 . O1 . 124.0(2) yes C8 . C9 . C10 . 118.3(2) yes C8 . C9 . H91 . 120.6 no C10 . C9 . H91 . 121.1 no C9 . C10 . N2 . 121.8(2) yes C9 . C10 . C11 . 124.2(2) yes N2 . C10 . C11 . 114.0(2) yes C10 . C11 . N3 . 114.4(2) yes C10 . C11 . C12 . 123.7(2) yes N3 . C11 . C12 . 121.9(2) yes C11 . C12 . C13 . 118.7(3) yes C11 . C12 . H121 . 120.7 no C13 . C12 . H121 . 120.6 no C12 . C13 . C14 . 119.7(3) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 119.9 no C13 . C14 . C15 . 118.8(3) yes C13 . C14 . H141 . 121.8 no C15 . C14 . H141 . 119.4 no C14 . C15 . N3 . 122.5(2) yes C14 . C15 . H151 . 119.0 no N3 . C15 . H151 . 118.4 no N4 . C16 . C17 . 122.7(3) yes N4 . C16 . H161 . 116.8 no C17 . C16 . H161 . 120.5 no C16 . C17 . C18 . 118.7(3) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.9 no C17 . C18 . C19 . 119.3(3) yes C17 . C18 . H181 . 120.9 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 118.9(3) yes C18 . C19 . H191 . 119.8 no C20 . C19 . H191 . 121.3 no C19 . C20 . N4 . 121.8(2) yes C19 . C20 . C21 . 124.6(2) yes N4 . C20 . C21 . 113.5(2) yes C20 . C21 . N5 . 112.5(2) yes C20 . C21 . C22 . 126.0(2) yes N5 . C21 . C22 . 121.5(2) yes C21 . C22 . C23 . 118.4(2) yes C21 . C22 . H221 . 121.2 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 120.4(2) yes C22 . C23 . O2 . 115.7(2) yes C24 . C23 . O2 . 124.0(2) yes C23 . C24 . C25 . 117.9(2) yes C23 . C24 . H241 . 122.3 no C25 . C24 . H241 . 119.9 no C24 . C25 . N5 . 121.6(2) yes C24 . C25 . C26 . 125.4(2) yes N5 . C25 . C26 . 112.9(2) yes C25 . C26 . N6 . 113.7(2) yes C25 . C26 . C27 . 124.3(2) yes N6 . C26 . C27 . 122.0(2) yes C26 . C27 . C28 . 119.1(2) yes C26 . C27 . H271 . 120.5 no C28 . C27 . H271 . 120.4 no C27 . C28 . C29 . 119.2(2) yes C27 . C28 . H281 . 121.0 no C29 . C28 . H281 . 119.8 no C28 . C29 . C30 . 118.9(2) yes C28 . C29 . H291 . 120.4 no C30 . C29 . H291 . 120.8 no C29 . C30 . N6 . 122.6(2) yes C29 . C30 . H301 . 119.8 no N6 . C30 . H301 . 117.5 no O1 . C31 . H311 . 108.1 no O1 . C31 . H312 . 110.2 no H311 . C31 . H312 . 109.7 no O1 . C31 . H313 . 109.9 no H311 . C31 . H313 . 109.8 no H312 . C31 . H313 . 109.2 no O2 . C32 . H321 . 107.5 no O2 . C32 . H322 . 110.7 no H321 . C32 . H322 . 106.1 no O2 . C32 . H323 . 111.3 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 111.4 no N7 . C33 . C34 . 177.2(6) yes C33 . C34 . H341 . 109.5 no C33 . C34 . H342 . 106.4 no H341 . C34 . H342 . 111.2 no C33 . C34 . H343 . 108.8 no H341 . C34 . H343 . 110.5 no H342 . C34 . H343 . 110.3 no C31 . O1 . C8 . 116.7(2) yes C32 . O2 . C23 . 117.0(2) yes F1 . P1 . F2 . 177.6(2) yes F1 . P1 . F3 . 90.74(16) yes F2 . P1 . F3 . 89.7(2) yes F1 . P1 . F4 . 89.35(19) yes F2 . P1 . F4 . 90.1(2) yes F3 . P1 . F4 . 178.28(19) yes F1 . P1 . F5 . 89.4(2) yes F2 . P1 . F5 . 88.2(2) yes F3 . P1 . F5 . 88.48(17) yes F4 . P1 . F5 . 89.81(19) yes F1 . P1 . F6 . 92.7(2) yes F2 . P1 . F6 . 89.67(18) yes F3 . P1 . F6 . 92.28(19) yes F4 . P1 . F6 . 89.43(19) yes F5 . P1 . F6 . 177.8(2) yes F8 7_565 P2 . F7 7_565 89.87(9) yes F8 7_565 P2 . F9 7_565 89.98(9) yes F7 7_565 P2 . F9 7_565 179.65(9) yes F8 7_565 P2 . F7 . 90.07(9) yes F7 7_565 P2 . F7 . 89.46(13) yes F9 7_565 P2 . F7 . 90.24(9) yes F8 7_565 P2 . F8 . 179.92(14) yes F7 7_565 P2 . F8 . 90.07(9) yes F9 7_565 P2 . F8 . 90.08(9) yes F7 . P2 . F8 . 89.87(9) yes F8 7_565 P2 . F9 . 90.08(9) yes F7 7_565 P2 . F9 . 90.24(9) yes F9 7_565 P2 . F9 . 90.07(13) yes F7 . P2 . F9 . 179.65(9) yes F8 . P2 . F9 . 89.98(9) yes F11 7_555 P3 . F12 7_555 90.00(8) yes F11 7_555 P3 . F10 7_555 90.12(8) yes F12 7_555 P3 . F10 7_555 90.12(8) yes F11 7_555 P3 . F10 . 89.85(8) yes F12 7_555 P3 . F10 . 179.62(9) yes F10 7_555 P3 . F10 . 90.23(12) yes F11 7_555 P3 . F11 . 179.95(12) yes F12 7_555 P3 . F11 . 90.03(8) yes F10 7_555 P3 . F11 . 89.85(8) yes F10 . P3 . F11 . 90.12(8) yes F11 7_555 P3 . F12 . 90.03(8) yes F12 7_555 P3 . F12 . 89.53(12) yes F10 7_555 P3 . F12 . 179.62(9) yes F10 . P3 . F12 . 90.12(8) yes F11 . P3 . F12 . 90.00(8) yes