#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705238.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705238 loop_ _publ_author_name 'Melle, Philipp' 'S\'egaud, Nathalie' 'Albrecht, Martin' _publ_section_title ; Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12662 _journal_page_last 12673 _journal_paper_doi 10.1039/d0dt02482a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C38 H34 Co N10 O4, 2(F6 P)' _chemical_formula_sum 'C38 H34 Co F12 N10 O4 P2' _chemical_formula_weight 1043.62 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-02-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.1440(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.94056(17) _cell_length_b 21.9377(4) _cell_length_c 16.2425(2) _cell_measurement_reflns_used 28565 _cell_measurement_temperature 173.01(10) _cell_measurement_theta_max 27.5570 _cell_measurement_theta_min 1.9290 _cell_volume 4248.29(11) _computing_cell_refinement 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0965 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -10.00 103.00 1.00 25.00 -- 27.42 57.00 -30.00 113 2 \w -10.00 103.00 1.00 25.00 -- 27.42 57.00-180.00 113 3 \w 35.00 122.00 1.00 25.00 -- 27.42 178.00 -30.00 87 4 \w -54.00 83.00 1.00 25.00 -- 27.42 -38.00 90.00 137 5 \w -20.00 32.00 1.00 25.00 -- -23.50 -99.00-150.00 52 6 \w 35.00 122.00 1.00 25.00 -- 27.42 178.00-180.00 87 7 \w -10.00 103.00 1.00 25.00 -- 27.42 57.00-120.00 113 8 \w -20.00 82.00 1.00 25.00 -- 27.42 -99.00 -60.00 102 9 \w -49.00 65.00 1.00 25.00 -- 27.42 -57.00 -30.00 114 10 \w -10.00 103.00 1.00 25.00 -- 27.42 57.00 90.00 113 11 \w -16.00 104.00 1.00 25.00 -- 27.42 77.00 30.00 120 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0222114000 _diffrn_orient_matrix_UB_12 0.0077816000 _diffrn_orient_matrix_UB_13 0.0382125000 _diffrn_orient_matrix_UB_21 -0.0342123000 _diffrn_orient_matrix_UB_22 -0.0265042000 _diffrn_orient_matrix_UB_23 -0.0021626000 _diffrn_orient_matrix_UB_31 0.0432937000 _diffrn_orient_matrix_UB_32 -0.0168014000 _diffrn_orient_matrix_UB_33 0.0211814000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.944 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 73492 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.194 _diffrn_reflns_theta_min 1.561 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_T_max 0.89258 _exptl_absorpt_correction_T_min 0.89258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.632 _exptl_crystal_description block _exptl_crystal_F_000 2116 _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.348 _exptl_crystal_size_min 0.163 _refine_diff_density_max 1.172 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 727 _refine_ls_number_reflns 9855 _refine_ls_number_restraints 618 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0585 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+6.7788P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1509 _refine_ls_wR_factor_ref 0.1581 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8281 _reflns_number_total 9855 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 19ma017_pm293 _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_original_cell_volume 4248.28(12) _cod_database_code 7705238 _shelx_shelxl_version_number 2018/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.910 _shelx_estimated_absorpt_t_min 0.773 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints F3A \\sim P1 \\sim F2 \\sim F2A \\sim F6A \\sim F3 \\sim F5A \\sim F5 \\sim F6 \\sim F1A \\sim F1 \\sim F4 \\sim F4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 F9 \\sim P2 \\sim F10 \\sim F12 \\sim F8 \\sim F11 \\sim F7 \\sim F9A \\sim P2A \\sim F12A \\sim F10A \\sim F8A \\sim F11A \\sim F7A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 3. Rigid body (RIGU) restrains F6, P1, F4, F1A, F3A, F5A, F2, F3, F6A, F2A, F5, F1, F4A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 F10, P2, F9, F8, F7, F11, F12, F11A, F8A, P2A, F12A, F10A, F7A, F9A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(F8A)=Sof(P2A)=Sof(F10A)=Sof(F12A)=Sof(F11A)=Sof(F7A)=Sof(F9A)=1-FVAR(1) Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1) Sof(F4A)=Sof(F3A)=Sof(F5A)=Sof(F6A)=Sof(F1A)=Sof(F2A)=1-FVAR(2) Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F1)=Sof(F2)=FVAR(2) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37) 5.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C38(H38A,H38B,H38C) ; _shelx_res_file ; TITL 19ma017_pm293_a.res in P2(1)/n 19ma017_pm293.res created by SHELXL-2018/1 at 10:07:11 on 07-Feb-2019 CELL 0.71073 11.940559 21.937684 16.242465 90 93.144 90 ZERR 4 0.000173 0.000403 0.000228 0 0.0013 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Co F N O P UNIT 152 136 4 48 40 16 8 SIMU F3A P1 F2 F2A F6A F3 F5A F5 F6 F1A F1 F4 F4A SIMU F9 P2 F10 F12 F8 F11 F7 F9A P2A F12A F10A F8A F11A F7A RIGU F6 P1 F4 F1A F3A F5A F2 F3 F6A F2A F5 F1 F4A RIGU F10 P2 F9 F8 F7 F11 F12 F11A F8A P2A F12A F10A F7A F9A L.S. 10 PLAN 20 SIZE 0.163 0.348 0.462 TEMP -100.14(10) BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.054900 6.778800 FVAR 1.87785 0.62199 0.51057 CO1 3 0.423845 0.192626 0.499548 11.00000 0.02812 0.03508 = 0.02490 0.00084 0.00052 0.00020 O1 6 0.444422 0.160328 0.371942 11.00000 0.04720 0.04224 = 0.02768 0.00067 0.00137 0.00786 O2 6 0.348847 0.256474 0.584328 11.00000 0.04295 0.04185 = 0.02879 -0.00081 0.00411 0.00444 O3 6 0.764881 0.207446 0.577553 11.00000 0.02660 0.04928 = 0.04978 -0.00165 0.00169 -0.00400 O4 6 0.282973 0.026636 0.571647 11.00000 0.04250 0.04281 = 0.05622 0.00523 0.00422 -0.01009 N1 5 0.466659 0.142105 0.119017 11.00000 0.05744 0.05103 = 0.02797 0.00317 0.00718 0.01607 N2 5 0.418100 0.193030 0.234971 11.00000 0.04466 0.04276 = 0.02581 0.00016 0.00234 0.00669 N3 5 0.356603 0.260298 0.425864 11.00000 0.02840 0.03809 = 0.02444 -0.00069 0.00037 -0.00122 N4 5 0.273949 0.355214 0.587294 11.00000 0.03776 0.04382 = 0.03500 -0.00892 0.00424 0.00046 N5 5 0.238191 0.418420 0.695597 11.00000 0.04113 0.04592 = 0.05314 -0.01548 0.00587 -0.00037 N6 5 0.623469 0.327554 0.585759 11.00000 0.05088 0.04276 = 0.04947 -0.00792 0.00804 -0.00425 N7 5 0.586801 0.231624 0.523248 11.00000 0.02963 0.03570 = 0.03264 0.00041 -0.00040 -0.00235 N8 5 0.513226 0.124315 0.555941 11.00000 0.02949 0.03410 = 0.02339 -0.00055 0.00286 -0.00015 N9 5 0.301567 0.124774 0.519791 11.00000 0.02792 0.04032 = 0.03339 0.00013 0.00139 -0.00328 N10 5 0.118313 0.137396 0.565727 11.00000 0.03576 0.04531 = 0.03684 -0.00244 0.00476 -0.00467 C1 1 0.472333 0.091807 0.071766 11.00000 0.08766 0.06776 = 0.03534 -0.00320 0.01518 0.02421 AFIX 43 H1 2 0.492244 0.095769 0.016189 11.00000 -1.20000 AFIX 0 C2 1 0.450183 0.035540 0.101909 11.00000 0.10845 0.05854 = 0.04761 -0.01207 0.01430 0.01456 AFIX 43 H2 2 0.454520 0.000506 0.067853 11.00000 -1.20000 AFIX 0 C3 1 0.421004 0.029966 0.183529 11.00000 0.08459 0.05071 = 0.04938 -0.00301 0.00940 0.00395 AFIX 43 H3 2 0.406239 -0.009011 0.206000 11.00000 -1.20000 AFIX 0 C4 1 0.413909 0.080995 0.230656 11.00000 0.06617 0.04461 = 0.03481 0.00014 0.00738 0.00172 AFIX 43 H4 2 0.394598 0.077135 0.286383 11.00000 -1.20000 AFIX 0 C5 1 0.434431 0.139108 0.198879 11.00000 0.04242 0.05051 = 0.02593 0.00252 0.00159 0.00807 C6 1 0.490442 0.202499 0.083587 11.00000 0.06782 0.05365 = 0.03514 0.01110 0.01456 0.01793 AFIX 137 H6A 2 0.422400 0.227536 0.082386 11.00000 -1.50000 H6B 2 0.514762 0.197385 0.027349 11.00000 -1.50000 H6C 2 0.549929 0.222615 0.117537 11.00000 -1.50000 AFIX 0 C7 1 0.413047 0.197917 0.316346 11.00000 0.03071 0.04131 = 0.02707 0.00117 0.00074 0.00192 C8 1 0.364481 0.257186 0.343852 11.00000 0.03263 0.04076 = 0.02571 0.00033 0.00051 0.00096 C9 1 0.329333 0.304584 0.292733 11.00000 0.04829 0.04957 = 0.02758 0.00542 0.00003 0.00441 AFIX 43 H9 2 0.335120 0.301794 0.234754 11.00000 -1.20000 AFIX 0 C10 1 0.285508 0.356220 0.327854 11.00000 0.06247 0.04983 = 0.04080 0.00922 0.00019 0.01322 AFIX 43 H10 2 0.260301 0.389360 0.294051 11.00000 -1.20000 AFIX 0 C11 1 0.278610 0.359284 0.412840 11.00000 0.05291 0.04509 = 0.03921 0.00154 0.00320 0.01170 AFIX 43 H11 2 0.249745 0.394571 0.438144 11.00000 -1.20000 AFIX 0 C12 1 0.314771 0.309734 0.459725 11.00000 0.03149 0.03829 = 0.03088 -0.00200 0.00187 0.00065 C13 1 0.312554 0.305555 0.552211 11.00000 0.02858 0.03982 = 0.03102 -0.00159 0.00129 -0.00210 C14 1 0.260454 0.360089 0.669013 11.00000 0.03264 0.04184 = 0.04389 -0.01216 0.00375 -0.00163 C15 1 0.260833 0.313125 0.728680 11.00000 0.05061 0.04973 = 0.04223 -0.01113 0.00830 -0.00168 AFIX 43 H15 2 0.277158 0.272402 0.713460 11.00000 -1.20000 AFIX 0 C16 1 0.237732 0.326292 0.808201 11.00000 0.05621 0.06867 = 0.04402 -0.00488 0.00585 -0.00573 AFIX 43 H16 2 0.236902 0.294119 0.847313 11.00000 -1.20000 AFIX 0 C17 1 0.215527 0.385042 0.833441 11.00000 0.04555 0.08008 = 0.05268 -0.03207 0.00396 0.00377 AFIX 43 H17 2 0.199021 0.393601 0.888816 11.00000 -1.20000 AFIX 0 C18 1 0.218232 0.431182 0.774802 11.00000 0.04233 0.06273 = 0.05864 -0.02667 0.00693 0.00114 AFIX 43 H18 2 0.205874 0.472205 0.790693 11.00000 -1.20000 AFIX 0 C19 1 0.244927 0.469046 0.636258 11.00000 0.07647 0.03928 = 0.07635 -0.01039 0.00519 0.00198 AFIX 137 H19A 2 0.321086 0.471321 0.616840 11.00000 -1.50000 H19B 2 0.226676 0.507455 0.663266 11.00000 -1.50000 H19C 2 0.191494 0.461984 0.589259 11.00000 -1.50000 AFIX 0 C20 1 0.639799 0.388854 0.580656 11.00000 0.08393 0.04520 = 0.07883 -0.01501 0.01728 -0.01382 AFIX 43 H20 2 0.651980 0.412256 0.629541 11.00000 -1.20000 AFIX 0 C21 1 0.638736 0.416157 0.507127 11.00000 0.11295 0.04185 = 0.10118 0.00814 0.02327 -0.01043 AFIX 43 H21 2 0.648013 0.459107 0.504456 11.00000 -1.20000 AFIX 0 C22 1 0.624468 0.383300 0.435181 11.00000 0.08170 0.05634 = 0.07469 0.01856 0.01539 -0.00950 AFIX 43 H22 2 0.624314 0.402945 0.383051 11.00000 -1.20000 AFIX 0 C23 1 0.610539 0.321707 0.440721 11.00000 0.04671 0.04870 = 0.05596 0.01240 0.00854 -0.00528 AFIX 43 H23 2 0.601016 0.298277 0.391648 11.00000 -1.20000 AFIX 0 C24 1 0.609998 0.292445 0.516982 11.00000 0.02913 0.03944 = 0.04389 0.00075 0.00697 -0.00154 C25 1 0.616192 0.299885 0.667664 11.00000 0.07366 0.05932 = 0.04033 -0.00978 0.00026 0.00249 AFIX 137 H25A 2 0.553227 0.271192 0.666634 11.00000 -1.50000 H25B 2 0.604432 0.331878 0.708405 11.00000 -1.50000 H25C 2 0.686063 0.278130 0.682587 11.00000 -1.50000 AFIX 0 C26 1 0.666749 0.194408 0.556971 11.00000 0.02979 0.04083 = 0.02666 -0.00261 0.00380 0.00002 C27 1 0.624329 0.130577 0.569990 11.00000 0.02968 0.03886 = 0.02536 -0.00116 0.00219 0.00010 C28 1 0.690904 0.082425 0.596438 11.00000 0.03124 0.04674 = 0.03672 0.00232 0.00077 0.00521 AFIX 43 H28 2 0.769682 0.087256 0.605491 11.00000 -1.20000 AFIX 0 C29 1 0.640120 0.026743 0.609518 11.00000 0.04629 0.03958 = 0.04269 0.00574 0.00196 0.00938 AFIX 43 H29 2 0.684414 -0.007502 0.626288 11.00000 -1.20000 AFIX 0 C30 1 0.524591 0.020966 0.598136 11.00000 0.04568 0.03803 = 0.03641 0.00507 0.00132 -0.00341 AFIX 43 H30 2 0.488404 -0.016547 0.608852 11.00000 -1.20000 AFIX 0 C31 1 0.463497 0.071342 0.570745 11.00000 0.03517 0.03698 = 0.02629 -0.00097 0.00383 -0.00094 C32 1 0.338153 0.071718 0.554401 11.00000 0.03608 0.03974 = 0.03225 -0.00103 0.00458 -0.00393 C33 1 0.188643 0.132946 0.503051 11.00000 0.03004 0.04005 = 0.03721 -0.00413 0.00387 -0.00416 C34 1 0.144792 0.141944 0.423226 11.00000 0.03616 0.08171 = 0.03634 -0.00930 0.00162 0.00386 AFIX 43 H34 2 0.193078 0.140312 0.378699 11.00000 -1.20000 AFIX 0 C35 1 0.032628 0.153175 0.407596 11.00000 0.04276 0.11239 = 0.04370 -0.00641 -0.00641 0.00891 AFIX 43 H35 2 0.003223 0.159349 0.352693 11.00000 -1.20000 AFIX 0 C36 1 -0.037413 0.155409 0.473026 11.00000 0.03133 0.09116 = 0.05810 -0.01138 0.00015 0.00707 AFIX 43 H36 2 -0.115587 0.162281 0.463395 11.00000 -1.20000 AFIX 0 C37 1 0.007040 0.147699 0.550281 11.00000 0.03347 0.06235 = 0.05278 -0.00779 0.01152 -0.00128 AFIX 43 H37 2 -0.040672 0.149513 0.595137 11.00000 -1.20000 AFIX 0 C38 1 0.163767 0.135391 0.651461 11.00000 0.04969 0.07777 = 0.03447 0.00172 0.00620 0.00104 AFIX 137 H38A 2 0.184691 0.093401 0.666020 11.00000 -1.50000 H38B 2 0.106823 0.149818 0.688070 11.00000 -1.50000 H38C 2 0.230147 0.161615 0.657558 11.00000 -1.50000 AFIX 0 P1 7 0.042289 0.000740 0.258551 11.00000 0.05460 0.06035 = 0.07164 0.00318 0.00503 -0.00046 PART 1 F3 4 -0.005814 0.015740 0.344408 31.00000 0.09450 0.13950 = 0.09828 -0.02660 0.03282 0.00253 F4 4 0.083683 -0.061678 0.287609 31.00000 0.07367 0.09217 = 0.06810 0.03948 -0.00156 0.02998 F5 4 -0.080042 -0.030030 0.231391 31.00000 0.08347 0.07834 = 0.12926 0.03330 -0.03400 -0.02535 F6 4 0.077501 -0.011993 0.167155 31.00000 0.19210 0.05269 = 0.07025 0.02082 0.03251 0.01101 F1 4 -0.010678 0.065913 0.220569 31.00000 0.06469 0.06470 = 0.17641 0.03166 0.01378 0.00992 F2 4 0.152598 0.037365 0.276479 31.00000 0.05652 0.12160 = 0.11233 -0.00525 -0.01148 -0.00946 PART 0 PART -1 P2 7 -0.075310 0.354849 0.322747 21.00000 0.05781 0.04412 = 0.04859 -0.00492 -0.00446 0.00138 F7 4 -0.036360 0.301327 0.379348 21.00000 0.21589 0.06444 = 0.08959 0.02619 -0.05222 0.00766 F8 4 -0.129707 0.390609 0.393616 21.00000 0.09865 0.12600 = 0.06818 -0.02838 0.00639 0.01533 F9 4 -0.193256 0.324178 0.300549 21.00000 0.10223 0.09683 = 0.08147 0.00447 -0.01510 -0.04050 F10 4 -0.108016 0.409886 0.262581 21.00000 0.10263 0.08875 = 0.06634 0.02137 -0.00227 -0.00065 F11 4 -0.022847 0.324924 0.247935 21.00000 0.18849 0.13819 = 0.08972 -0.02776 0.05596 0.04937 F12 4 0.036645 0.390898 0.351451 21.00000 0.04282 0.09335 = 0.20472 0.01781 -0.01726 -0.00429 PART 0 PART -2 F8A 4 -0.127023 0.330374 0.385379 -21.00000 0.08817 0.25865 = 0.18711 0.05137 0.05182 -0.03190 P2A 7 -0.041613 0.349815 0.315315 -21.00000 0.06628 0.07270 = 0.04518 -0.00067 0.00097 -0.00284 F10A 4 -0.127569 0.406154 0.289622 -21.00000 0.12318 0.08060 = 0.18054 -0.03071 -0.01631 0.05194 F12A 4 0.016979 0.388656 0.378690 -21.00000 0.16200 0.17746 = 0.05427 -0.04329 -0.00876 -0.05458 F11A 4 0.046377 0.369617 0.256664 -21.00000 0.11733 0.17169 = 0.05258 0.04131 0.01709 0.00093 F7A 4 0.027519 0.297220 0.345704 -21.00000 0.13249 0.10377 = 0.20244 0.08234 0.01018 0.01888 F9A 4 -0.103693 0.310174 0.251002 -21.00000 0.19023 0.10297 = 0.18943 -0.06669 -0.08898 -0.00738 PART 0 PART 2 F4A 4 0.062697 -0.072783 0.275576 -31.00000 0.12286 0.06886 = 0.19287 0.03131 0.08521 0.02278 F3A 4 -0.077362 -0.007887 0.281686 -31.00000 0.05230 0.11783 = 0.12651 0.03413 0.01774 0.02140 F5A 4 0.021175 -0.011381 0.165971 -31.00000 0.09470 0.12184 = 0.07628 -0.02789 -0.01410 -0.00250 F6A 4 0.175715 0.005612 0.241339 -31.00000 0.05587 0.12037 = 0.10466 0.02732 0.00604 -0.02021 F1A 4 0.026726 0.068261 0.248716 -31.00000 0.17438 0.05661 = 0.07740 0.00773 0.03494 0.01221 F2A 4 0.078948 0.009058 0.356519 -31.00000 0.12145 0.13959 = 0.05868 0.01641 0.00032 0.00598 HKLF 4 REM 19ma017_pm293_a.res in P2(1)/n REM R1 = 0.0585 for 8281 Fo > 4sig(Fo) and 0.0702 for all 9855 data REM 727 parameters refined using 618 restraints END WGHT 0.0545 6.7940 REM Highest difference peak 1.172, deepest hole -0.745, 1-sigma level 0.072 Q1 1 -0.0780 0.0218 0.4858 11.00000 0.05 1.17 Q2 1 0.1992 0.3553 0.8760 11.00000 0.05 0.57 Q3 1 0.4518 0.2226 0.4838 11.00000 0.05 0.44 Q4 1 -0.0330 0.3829 0.2537 11.00000 0.05 0.44 Q5 1 0.2959 0.4621 0.8539 11.00000 0.05 0.43 Q6 1 -0.0343 0.2857 0.2865 11.00000 0.05 0.42 Q7 1 0.4492 0.1618 0.4815 11.00000 0.05 0.39 Q8 1 -0.0740 0.3162 0.2183 11.00000 0.05 0.39 Q9 1 0.2259 0.2756 0.7387 11.00000 0.05 0.38 Q10 1 0.3463 0.4664 0.6374 11.00000 0.05 0.37 Q11 1 0.0390 0.3401 0.3827 11.00000 0.05 0.34 Q12 1 -0.0634 -0.0081 0.3847 11.00000 0.05 0.34 Q13 1 0.5505 0.0363 0.1215 11.00000 0.05 0.32 Q14 1 0.2629 0.3187 0.5838 11.00000 0.05 0.32 Q15 1 -0.0616 0.3986 0.3817 11.00000 0.05 0.32 Q16 1 0.4841 0.0415 0.5630 11.00000 0.05 0.30 Q17 1 -0.1543 0.3515 0.2635 11.00000 0.05 0.28 Q18 1 0.2572 0.0619 0.2368 11.00000 0.05 0.28 Q19 1 0.0609 0.3823 0.2973 11.00000 0.05 0.28 Q20 1 -0.1049 0.3100 0.4120 11.00000 0.05 0.28 ; _shelx_res_checksum 11802 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.42385(3) 0.19263(2) 0.49955(2) 0.02940(11) Uani 1 1 d . . . . . O1 O 0.44442(19) 0.16033(10) 0.37194(12) 0.0391(5) Uani 1 1 d . . . . . O2 O 0.34885(18) 0.25647(10) 0.58433(12) 0.0378(5) Uani 1 1 d . . . . . O3 O 0.76488(17) 0.20745(11) 0.57755(14) 0.0419(5) Uani 1 1 d . . . . . O4 O 0.2830(2) 0.02664(11) 0.57165(15) 0.0471(6) Uani 1 1 d . . . . . N1 N 0.4667(3) 0.14211(14) 0.11902(16) 0.0453(7) Uani 1 1 d . . . . . N2 N 0.4181(2) 0.19303(12) 0.23497(15) 0.0377(6) Uani 1 1 d . . . . . N3 N 0.35660(19) 0.26030(11) 0.42586(14) 0.0303(5) Uani 1 1 d . . . . . N4 N 0.2739(2) 0.35521(13) 0.58729(16) 0.0388(6) Uani 1 1 d . . . . . N5 N 0.2382(2) 0.41842(14) 0.69560(19) 0.0466(7) Uani 1 1 d . . . . . N6 N 0.6235(3) 0.32755(14) 0.58576(19) 0.0475(7) Uani 1 1 d . . . . . N7 N 0.5868(2) 0.23162(12) 0.52325(15) 0.0327(5) Uani 1 1 d . . . . . N8 N 0.51323(19) 0.12432(11) 0.55594(13) 0.0289(5) Uani 1 1 d . . . . . N9 N 0.3016(2) 0.12477(12) 0.51979(15) 0.0339(5) Uani 1 1 d . . . . . N10 N 0.1183(2) 0.13740(13) 0.56573(16) 0.0392(6) Uani 1 1 d . . . . . C1 C 0.4723(4) 0.0918(2) 0.0718(2) 0.0632(11) Uani 1 1 d . . . . . H1 H 0.492244 0.095769 0.016189 0.076 Uiso 1 1 calc R . . . . C2 C 0.4502(5) 0.0355(2) 0.1019(3) 0.0712(13) Uani 1 1 d . . . . . H2 H 0.454520 0.000506 0.067853 0.085 Uiso 1 1 calc R . . . . C3 C 0.4210(4) 0.0300(2) 0.1835(2) 0.0614(10) Uani 1 1 d . . . . . H3 H 0.406239 -0.009011 0.206000 0.074 Uiso 1 1 calc R . . . . C4 C 0.4139(3) 0.08099(16) 0.2307(2) 0.0484(8) Uani 1 1 d . . . . . H4 H 0.394598 0.077135 0.286383 0.058 Uiso 1 1 calc R . . . . C5 C 0.4344(3) 0.13911(16) 0.19888(18) 0.0396(7) Uani 1 1 d . . . . . C6 C 0.4904(4) 0.20250(17) 0.0836(2) 0.0518(9) Uani 1 1 d . . . . . H6A H 0.422400 0.227536 0.082386 0.078 Uiso 1 1 calc GR . . . . H6B H 0.514762 0.197385 0.027349 0.078 Uiso 1 1 calc GR . . . . H6C H 0.549929 0.222615 0.117537 0.078 Uiso 1 1 calc GR . . . . C7 C 0.4130(2) 0.19792(14) 0.31635(17) 0.0331(6) Uani 1 1 d . . . . . C8 C 0.3645(2) 0.25719(14) 0.34385(17) 0.0331(6) Uani 1 1 d . . . . . C9 C 0.3293(3) 0.30458(16) 0.29273(19) 0.0419(7) Uani 1 1 d . . . . . H9 H 0.335120 0.301794 0.234754 0.050 Uiso 1 1 calc R . . . . C10 C 0.2855(3) 0.35622(18) 0.3279(2) 0.0511(9) Uani 1 1 d . . . . . H10 H 0.260301 0.389360 0.294051 0.061 Uiso 1 1 calc R . . . . C11 C 0.2786(3) 0.35928(16) 0.4128(2) 0.0457(8) Uani 1 1 d . . . . . H11 H 0.249745 0.394571 0.438144 0.055 Uiso 1 1 calc R . . . . C12 C 0.3148(2) 0.30973(14) 0.45973(18) 0.0335(6) Uani 1 1 d . . . . . C13 C 0.3126(2) 0.30556(14) 0.55221(18) 0.0332(6) Uani 1 1 d . . . . . C14 C 0.2605(3) 0.36009(15) 0.6690(2) 0.0394(7) Uani 1 1 d . . . . . C15 C 0.2608(3) 0.31312(17) 0.7287(2) 0.0473(8) Uani 1 1 d . . . . . H15 H 0.277158 0.272402 0.713460 0.057 Uiso 1 1 calc R . . . . C16 C 0.2377(3) 0.3263(2) 0.8082(2) 0.0562(9) Uani 1 1 d . . . . . H16 H 0.236902 0.294119 0.847313 0.067 Uiso 1 1 calc R . . . . C17 C 0.2155(3) 0.3850(2) 0.8334(3) 0.0594(11) Uani 1 1 d . . . . . H17 H 0.199021 0.393601 0.888816 0.071 Uiso 1 1 calc R . . . . C18 C 0.2182(3) 0.4312(2) 0.7748(2) 0.0544(10) Uani 1 1 d . . . . . H18 H 0.205874 0.472205 0.790693 0.065 Uiso 1 1 calc R . . . . C19 C 0.2449(4) 0.46905(18) 0.6363(3) 0.0640(11) Uani 1 1 d . . . . . H19A H 0.321086 0.471321 0.616840 0.096 Uiso 1 1 calc GR . . . . H19B H 0.226676 0.507455 0.663266 0.096 Uiso 1 1 calc GR . . . . H19C H 0.191494 0.461984 0.589259 0.096 Uiso 1 1 calc GR . . . . C20 C 0.6398(4) 0.38885(19) 0.5807(3) 0.0688(12) Uani 1 1 d . . . . . H20 H 0.651980 0.412256 0.629541 0.083 Uiso 1 1 calc R . . . . C21 C 0.6387(5) 0.4162(2) 0.5071(4) 0.0847(16) Uani 1 1 d . . . . . H21 H 0.648013 0.459107 0.504456 0.102 Uiso 1 1 calc R . . . . C22 C 0.6245(4) 0.3833(2) 0.4352(3) 0.0705(12) Uani 1 1 d . . . . . H22 H 0.624314 0.402945 0.383051 0.085 Uiso 1 1 calc R . . . . C23 C 0.6105(3) 0.32171(17) 0.4407(2) 0.0502(9) Uani 1 1 d . . . . . H23 H 0.601016 0.298277 0.391648 0.060 Uiso 1 1 calc R . . . . C24 C 0.6100(3) 0.29244(15) 0.5170(2) 0.0373(7) Uani 1 1 d . . . . . C25 C 0.6162(4) 0.29989(19) 0.6677(2) 0.0579(10) Uani 1 1 d . . . . . H25A H 0.553227 0.271192 0.666634 0.087 Uiso 1 1 calc GR . . . . H25B H 0.604432 0.331878 0.708405 0.087 Uiso 1 1 calc GR . . . . H25C H 0.686063 0.278130 0.682587 0.087 Uiso 1 1 calc GR . . . . C26 C 0.6667(2) 0.19441(14) 0.55697(17) 0.0323(6) Uani 1 1 d . . . . . C27 C 0.6243(2) 0.13058(14) 0.56999(17) 0.0313(6) Uani 1 1 d . . . . . C28 C 0.6909(3) 0.08243(15) 0.59644(19) 0.0383(7) Uani 1 1 d . . . . . H28 H 0.769682 0.087256 0.605491 0.046 Uiso 1 1 calc R . . . . C29 C 0.6401(3) 0.02674(16) 0.6095(2) 0.0429(7) Uani 1 1 d . . . . . H29 H 0.684414 -0.007502 0.626288 0.051 Uiso 1 1 calc R . . . . C30 C 0.5246(3) 0.02097(15) 0.59814(19) 0.0401(7) Uani 1 1 d . . . . . H30 H 0.488404 -0.016547 0.608852 0.048 Uiso 1 1 calc R . . . . C31 C 0.4635(2) 0.07134(14) 0.57075(17) 0.0327(6) Uani 1 1 d . . . . . C32 C 0.3382(3) 0.07172(15) 0.55440(18) 0.0359(6) Uani 1 1 d . . . . . C33 C 0.1886(2) 0.13295(14) 0.50305(19) 0.0357(6) Uani 1 1 d . . . . . C34 C 0.1448(3) 0.1419(2) 0.4232(2) 0.0514(9) Uani 1 1 d . . . . . H34 H 0.193078 0.140312 0.378699 0.062 Uiso 1 1 calc R . . . . C35 C 0.0326(3) 0.1532(2) 0.4076(2) 0.0666(12) Uani 1 1 d . . . . . H35 H 0.003223 0.159349 0.352693 0.080 Uiso 1 1 calc R . . . . C36 C -0.0374(3) 0.1554(2) 0.4730(3) 0.0603(11) Uani 1 1 d . . . . . H36 H -0.115587 0.162281 0.463395 0.072 Uiso 1 1 calc R . . . . C37 C 0.0070(3) 0.14770(18) 0.5503(2) 0.0492(8) Uani 1 1 d . . . . . H37 H -0.040672 0.149513 0.595137 0.059 Uiso 1 1 calc R . . . . C38 C 0.1638(3) 0.1354(2) 0.6515(2) 0.0538(9) Uani 1 1 d . . . . . H38A H 0.184691 0.093401 0.666020 0.081 Uiso 1 1 calc GR . . . . H38B H 0.106823 0.149818 0.688070 0.081 Uiso 1 1 calc GR . . . . H38C H 0.230147 0.161615 0.657558 0.081 Uiso 1 1 calc GR . . . . P1 P 0.04229(10) 0.00074(6) 0.25855(8) 0.0621(3) Uani 1 1 d . U . . . F3 F -0.0058(9) 0.0157(4) 0.3444(5) 0.110(3) Uani 0.511(13) 1 d . U P A 1 F4 F 0.0837(11) -0.0617(6) 0.2876(7) 0.078(3) Uani 0.511(13) 1 d . U P A 1 F5 F -0.0800(7) -0.0300(4) 0.2314(8) 0.098(3) Uani 0.511(13) 1 d . U P A 1 F6 F 0.0775(13) -0.0120(4) 0.1672(6) 0.104(4) Uani 0.511(13) 1 d . U P A 1 F1 F -0.0107(8) 0.0659(6) 0.2206(10) 0.102(4) Uani 0.511(13) 1 d . U P A 1 F2 F 0.1526(7) 0.0374(5) 0.2765(6) 0.097(3) Uani 0.511(13) 1 d . U P A 1 P2 P -0.0753(4) 0.3548(3) 0.3227(4) 0.0504(9) Uani 0.622(8) 1 d . U P B -1 F7 F -0.0364(11) 0.3013(3) 0.3793(5) 0.126(3) Uani 0.622(8) 1 d . U P B -1 F8 F -0.1297(5) 0.3906(3) 0.3936(3) 0.098(2) Uani 0.622(8) 1 d . U P B -1 F9 F -0.1933(5) 0.3242(3) 0.3005(4) 0.094(2) Uani 0.622(8) 1 d . U P B -1 F10 F -0.1080(10) 0.4099(5) 0.2626(5) 0.086(2) Uani 0.622(8) 1 d . U P B -1 F11 F -0.0228(10) 0.3249(5) 0.2479(5) 0.137(3) Uani 0.622(8) 1 d . U P B -1 F12 F 0.0366(6) 0.3909(4) 0.3515(7) 0.115(3) Uani 0.622(8) 1 d . U P B -1 F8A F -0.1270(11) 0.3304(11) 0.3854(11) 0.176(7) Uani 0.378(8) 1 d . U P B -2 P2A P -0.0416(8) 0.3498(6) 0.3153(7) 0.0615(19) Uani 0.378(8) 1 d . U P B -2 F10A F -0.1276(19) 0.4062(9) 0.2896(13) 0.129(6) Uani 0.378(8) 1 d . U P B -2 F12A F 0.0170(16) 0.3887(10) 0.3787(8) 0.132(6) Uani 0.378(8) 1 d . U P B -2 F11A F 0.0464(10) 0.3696(7) 0.2567(6) 0.113(4) Uani 0.378(8) 1 d . U P B -2 F7A F 0.0275(13) 0.2972(7) 0.3457(13) 0.146(6) Uani 0.378(8) 1 d . U P B -2 F9A F -0.1037(18) 0.3102(7) 0.2510(13) 0.165(7) Uani 0.378(8) 1 d . U P B -2 F4A F 0.0627(16) -0.0728(7) 0.2756(11) 0.125(5) Uani 0.489(13) 1 d . U P A 2 F3A F -0.0774(7) -0.0079(5) 0.2817(7) 0.098(4) Uani 0.489(13) 1 d . U P A 2 F5A F 0.0212(9) -0.0114(6) 0.1660(7) 0.098(3) Uani 0.489(13) 1 d . U P A 2 F6A F 0.1757(6) 0.0056(6) 0.2413(7) 0.094(3) Uani 0.489(13) 1 d . U P A 2 F1A F 0.0267(14) 0.0683(6) 0.2487(7) 0.102(4) Uani 0.489(13) 1 d . U P A 2 F2A F 0.0789(11) 0.0091(4) 0.3565(4) 0.107(4) Uani 0.489(13) 1 d . U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0281(2) 0.0351(2) 0.02490(19) 0.00084(15) 0.00052(14) 0.00020(15) O1 0.0472(13) 0.0422(12) 0.0277(10) 0.0007(9) 0.0014(9) 0.0079(10) O2 0.0429(12) 0.0418(12) 0.0288(10) -0.0008(9) 0.0041(9) 0.0044(10) O3 0.0266(10) 0.0493(13) 0.0498(13) -0.0017(10) 0.0017(9) -0.0040(9) O4 0.0425(13) 0.0428(13) 0.0562(14) 0.0052(11) 0.0042(11) -0.0101(10) N1 0.0574(17) 0.0510(17) 0.0280(13) 0.0032(12) 0.0072(12) 0.0161(14) N2 0.0447(15) 0.0428(14) 0.0258(12) 0.0002(10) 0.0023(10) 0.0067(12) N3 0.0284(12) 0.0381(13) 0.0244(11) -0.0007(9) 0.0004(9) -0.0012(10) N4 0.0378(14) 0.0438(15) 0.0350(13) -0.0089(11) 0.0042(11) 0.0005(11) N5 0.0411(15) 0.0459(16) 0.0531(17) -0.0155(13) 0.0059(13) -0.0004(12) N6 0.0509(17) 0.0428(16) 0.0495(17) -0.0079(13) 0.0080(13) -0.0042(13) N7 0.0296(12) 0.0357(13) 0.0326(12) 0.0004(10) -0.0004(9) -0.0024(10) N8 0.0295(11) 0.0341(12) 0.0234(11) -0.0005(9) 0.0029(9) -0.0001(9) N9 0.0279(12) 0.0403(14) 0.0334(12) 0.0001(10) 0.0014(9) -0.0033(10) N10 0.0358(13) 0.0453(15) 0.0368(13) -0.0024(11) 0.0048(11) -0.0047(11) C1 0.088(3) 0.068(3) 0.0353(18) -0.0032(18) 0.0152(19) 0.024(2) C2 0.108(4) 0.059(3) 0.048(2) -0.0121(19) 0.014(2) 0.015(2) C3 0.085(3) 0.051(2) 0.049(2) -0.0030(17) 0.009(2) 0.004(2) C4 0.066(2) 0.0446(19) 0.0348(16) 0.0001(14) 0.0074(15) 0.0017(17) C5 0.0424(17) 0.0505(19) 0.0259(14) 0.0025(13) 0.0016(12) 0.0081(14) C6 0.068(2) 0.054(2) 0.0351(17) 0.0111(15) 0.0146(16) 0.0179(18) C7 0.0307(14) 0.0413(16) 0.0271(13) 0.0012(12) 0.0007(11) 0.0019(12) C8 0.0326(14) 0.0408(16) 0.0257(13) 0.0003(11) 0.0005(11) 0.0010(12) C9 0.0483(18) 0.0496(19) 0.0276(14) 0.0054(13) 0.0000(13) 0.0044(15) C10 0.062(2) 0.050(2) 0.0408(18) 0.0092(15) 0.0002(16) 0.0132(17) C11 0.053(2) 0.0451(19) 0.0392(17) 0.0015(14) 0.0032(14) 0.0117(15) C12 0.0315(14) 0.0383(16) 0.0309(14) -0.0020(12) 0.0019(11) 0.0007(12) C13 0.0286(13) 0.0398(16) 0.0310(14) -0.0016(12) 0.0013(11) -0.0021(12) C14 0.0326(15) 0.0418(17) 0.0439(17) -0.0122(14) 0.0038(13) -0.0016(13) C15 0.051(2) 0.050(2) 0.0422(18) -0.0111(15) 0.0083(15) -0.0017(16) C16 0.056(2) 0.069(3) 0.0440(19) -0.0049(18) 0.0058(17) -0.0057(19) C17 0.046(2) 0.080(3) 0.053(2) -0.032(2) 0.0040(16) 0.0038(19) C18 0.0423(19) 0.063(2) 0.059(2) -0.0267(19) 0.0069(16) 0.0011(17) C19 0.076(3) 0.039(2) 0.076(3) -0.0104(19) 0.005(2) 0.0020(19) C20 0.084(3) 0.045(2) 0.079(3) -0.015(2) 0.017(2) -0.014(2) C21 0.113(4) 0.042(2) 0.101(4) 0.008(2) 0.023(3) -0.010(3) C22 0.082(3) 0.056(3) 0.075(3) 0.019(2) 0.015(2) -0.009(2) C23 0.0467(19) 0.049(2) 0.056(2) 0.0124(16) 0.0085(16) -0.0053(15) C24 0.0291(14) 0.0394(16) 0.0439(17) 0.0007(13) 0.0070(12) -0.0015(12) C25 0.074(3) 0.059(2) 0.0403(19) -0.0098(17) 0.0003(18) 0.002(2) C26 0.0298(14) 0.0408(16) 0.0267(13) -0.0026(11) 0.0038(10) 0.0000(12) C27 0.0297(14) 0.0389(16) 0.0254(13) -0.0012(11) 0.0022(10) 0.0001(11) C28 0.0312(15) 0.0467(18) 0.0367(15) 0.0023(13) 0.0008(12) 0.0052(13) C29 0.0463(18) 0.0396(17) 0.0427(17) 0.0057(14) 0.0020(14) 0.0094(14) C30 0.0457(18) 0.0380(16) 0.0364(16) 0.0051(13) 0.0013(13) -0.0034(14) C31 0.0352(15) 0.0370(15) 0.0263(13) -0.0010(11) 0.0038(11) -0.0009(12) C32 0.0361(15) 0.0397(16) 0.0323(14) -0.0010(12) 0.0046(12) -0.0039(13) C33 0.0300(14) 0.0400(16) 0.0372(15) -0.0041(13) 0.0039(12) -0.0042(12) C34 0.0362(17) 0.082(3) 0.0363(17) -0.0093(17) 0.0016(13) 0.0039(17) C35 0.043(2) 0.112(4) 0.044(2) -0.006(2) -0.0064(16) 0.009(2) C36 0.0313(17) 0.091(3) 0.058(2) -0.011(2) 0.0002(16) 0.0071(18) C37 0.0335(16) 0.062(2) 0.053(2) -0.0078(17) 0.0115(14) -0.0013(15) C38 0.050(2) 0.078(3) 0.0345(17) 0.0017(17) 0.0062(15) 0.0010(19) P1 0.0546(6) 0.0604(7) 0.0716(7) 0.0032(5) 0.0050(5) -0.0005(5) F3 0.095(7) 0.139(6) 0.098(5) -0.027(4) 0.033(5) 0.003(5) F4 0.074(5) 0.092(7) 0.068(4) 0.039(4) -0.002(4) 0.030(4) F5 0.083(4) 0.078(5) 0.129(7) 0.033(5) -0.034(5) -0.025(4) F6 0.192(11) 0.053(4) 0.070(4) 0.021(3) 0.033(6) 0.011(5) F1 0.065(4) 0.065(4) 0.176(12) 0.032(7) 0.014(5) 0.010(3) F2 0.057(4) 0.122(6) 0.112(6) -0.005(5) -0.011(4) -0.009(4) P2 0.058(2) 0.0441(12) 0.0486(17) -0.0049(10) -0.0045(17) 0.0014(16) F7 0.216(10) 0.064(3) 0.090(4) 0.026(3) -0.052(5) 0.008(5) F8 0.099(4) 0.126(5) 0.068(3) -0.028(3) 0.006(3) 0.015(3) F9 0.102(4) 0.097(4) 0.081(4) 0.004(3) -0.015(3) -0.040(3) F10 0.103(5) 0.089(4) 0.066(3) 0.021(3) -0.002(3) -0.001(4) F11 0.188(9) 0.138(8) 0.090(4) -0.028(4) 0.056(6) 0.049(7) F12 0.043(3) 0.093(4) 0.205(10) 0.018(5) -0.017(4) -0.004(3) F8A 0.088(8) 0.259(18) 0.187(12) 0.051(12) 0.052(8) -0.032(9) P2A 0.066(5) 0.073(4) 0.045(2) -0.001(2) 0.001(3) -0.003(3) F10A 0.123(10) 0.081(9) 0.181(16) -0.031(8) -0.016(10) 0.052(8) F12A 0.162(12) 0.177(11) 0.054(5) -0.043(6) -0.009(6) -0.055(9) F11A 0.117(7) 0.172(11) 0.053(5) 0.041(6) 0.017(5) 0.001(7) F7A 0.132(10) 0.104(7) 0.202(15) 0.082(8) 0.010(8) 0.019(7) F9A 0.190(15) 0.103(8) 0.189(12) -0.067(9) -0.089(11) -0.007(9) F4A 0.123(10) 0.069(5) 0.193(12) 0.031(6) 0.085(9) 0.023(5) F3A 0.052(4) 0.118(7) 0.127(8) 0.034(6) 0.018(4) 0.021(4) F5A 0.095(6) 0.122(7) 0.076(5) -0.028(4) -0.014(4) -0.003(5) F6A 0.056(4) 0.120(7) 0.105(6) 0.027(5) 0.006(3) -0.020(4) F1A 0.174(12) 0.057(4) 0.077(5) 0.008(4) 0.035(6) 0.012(6) F2A 0.121(8) 0.140(6) 0.059(4) 0.016(4) 0.000(4) 0.006(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O1 149.60(8) . . ? N3 Co1 O1 75.21(9) . . ? N3 Co1 O2 75.08(9) . . ? N3 Co1 N7 97.99(10) . . ? N3 Co1 N9 110.40(10) . . ? N7 Co1 O1 98.60(9) . . ? N7 Co1 O2 91.74(9) . . ? N8 Co1 O1 95.94(8) . . ? N8 Co1 O2 114.31(8) . . ? N8 Co1 N3 168.84(9) . . ? N8 Co1 N7 76.33(10) . . ? N8 Co1 N9 76.20(10) . . ? N9 Co1 O1 91.90(9) . . ? N9 Co1 O2 92.44(9) . . ? N9 Co1 N7 151.42(10) . . ? C7 O1 Co1 114.56(19) . . ? C13 O2 Co1 115.37(18) . . ? C1 N1 C5 121.6(3) . . ? C1 N1 C6 119.7(3) . . ? C5 N1 C6 118.7(3) . . ? C7 N2 C5 121.4(3) . . ? C8 N3 Co1 119.8(2) . . ? C12 N3 Co1 119.74(19) . . ? C12 N3 C8 120.1(3) . . ? C13 N4 C14 123.5(3) . . ? C14 N5 C19 118.4(3) . . ? C18 N5 C14 122.5(3) . . ? C18 N5 C19 119.0(3) . . ? C20 N6 C25 118.6(3) . . ? C24 N6 C20 121.4(3) . . ? C24 N6 C25 120.0(3) . . ? C24 N7 Co1 124.2(2) . . ? C26 N7 Co1 116.6(2) . . ? C26 N7 C24 118.6(3) . . ? C27 N8 Co1 119.5(2) . . ? C31 N8 Co1 119.80(19) . . ? C31 N8 C27 120.3(3) . . ? C32 N9 Co1 117.25(19) . . ? C32 N9 C33 119.0(3) . . ? C33 N9 Co1 123.7(2) . . ? C33 N10 C38 119.8(3) . . ? C37 N10 C33 120.8(3) . . ? C37 N10 C38 119.2(3) . . ? N1 C1 H1 119.3 . . ? N1 C1 C2 121.4(3) . . ? C2 C1 H1 119.3 . . ? C1 C2 H2 120.5 . . ? C1 C2 C3 119.1(4) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3 120.4 . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3 120.4 . . ? C3 C4 H4 119.2 . . ? C3 C4 C5 121.5(3) . . ? C5 C4 H4 119.2 . . ? N1 C5 C4 117.0(3) . . ? N2 C5 N1 115.2(3) . . ? N2 C5 C4 127.5(3) . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 N2 129.0(3) . . ? O1 C7 C8 117.2(2) . . ? N2 C7 C8 113.9(3) . . ? N3 C8 C7 112.9(3) . . ? N3 C8 C9 121.5(3) . . ? C9 C8 C7 125.6(3) . . ? C8 C9 H9 120.7 . . ? C8 C9 C10 118.5(3) . . ? C10 C9 H9 120.7 . . ? C9 C10 H10 120.2 . . ? C9 C10 C11 119.6(3) . . ? C11 C10 H10 120.2 . . ? C10 C11 H11 120.8 . . ? C12 C11 C10 118.4(3) . . ? C12 C11 H11 120.8 . . ? N3 C12 C11 121.9(3) . . ? N3 C12 C13 113.0(3) . . ? C11 C12 C13 125.1(3) . . ? O2 C13 N4 130.1(3) . . ? O2 C13 C12 116.1(3) . . ? N4 C13 C12 113.9(3) . . ? N4 C14 N5 114.6(3) . . ? N4 C14 C15 128.3(3) . . ? N5 C14 C15 117.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 119.0 . . ? C15 C16 C17 122.0(4) . . ? C17 C16 H16 119.0 . . ? C16 C17 H17 121.2 . . ? C16 C17 C18 117.6(4) . . ? C18 C17 H17 121.2 . . ? N5 C18 C17 120.9(4) . . ? N5 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 H20 119.9 . . ? C21 C20 N6 120.2(4) . . ? C21 C20 H20 119.9 . . ? C20 C21 H21 119.4 . . ? C20 C21 C22 121.3(4) . . ? C22 C21 H21 119.4 . . ? C21 C22 H22 120.9 . . ? C23 C22 C21 118.2(4) . . ? C23 C22 H22 120.9 . . ? C22 C23 H23 119.3 . . ? C22 C23 C24 121.4(4) . . ? C24 C23 H23 119.3 . . ? N6 C24 N7 120.5(3) . . ? N6 C24 C23 117.6(3) . . ? N7 C24 C23 121.7(3) . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O3 C26 N7 127.6(3) . . ? O3 C26 C27 119.9(3) . . ? N7 C26 C27 112.5(2) . . ? N8 C27 C26 114.1(3) . . ? N8 C27 C28 121.6(3) . . ? C28 C27 C26 124.3(3) . . ? C27 C28 H28 120.8 . . ? C27 C28 C29 118.3(3) . . ? C29 C28 H28 120.8 . . ? C28 C29 H29 120.0 . . ? C28 C29 C30 120.0(3) . . ? C30 C29 H29 120.0 . . ? C29 C30 H30 120.9 . . ? C31 C30 C29 118.2(3) . . ? C31 C30 H30 120.9 . . ? N8 C31 C30 121.5(3) . . ? N8 C31 C32 114.3(3) . . ? C30 C31 C32 124.2(3) . . ? O4 C32 N9 128.4(3) . . ? O4 C32 C31 119.7(3) . . ? N9 C32 C31 111.9(3) . . ? N9 C33 C34 121.4(3) . . ? N10 C33 N9 120.1(3) . . ? N10 C33 C34 118.3(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.5 . . ? C34 C35 H35 120.4 . . ? C34 C35 C36 119.2(4) . . ? C36 C35 H35 120.4 . . ? C35 C36 H36 120.5 . . ? C37 C36 C35 119.1(3) . . ? C37 C36 H36 120.5 . . ? N10 C37 H37 119.2 . . ? C36 C37 N10 121.7(3) . . ? C36 C37 H37 119.2 . . ? N10 C38 H38A 109.5 . . ? N10 C38 H38B 109.5 . . ? N10 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F3 P1 F5 87.8(5) . . ? F3 P1 F6 173.5(6) . . ? F3 P1 F1 89.9(6) . . ? F4 P1 F3 92.4(6) . . ? F4 P1 F5 89.0(6) . . ? F4 P1 F6 91.9(6) . . ? F4 P1 F1 174.9(7) . . ? F4 P1 F2 98.6(6) . . ? F5 P1 F1 86.5(5) . . ? F6 P1 F5 87.4(5) . . ? F6 P1 F1 85.4(6) . . ? F2 P1 F3 94.2(5) . . ? F2 P1 F5 172.1(4) . . ? F2 P1 F6 90.1(5) . . ? F2 P1 F1 85.8(5) . . ? F3A P1 F4A 88.2(7) . . ? F3A P1 F5A 96.6(5) . . ? F3A P1 F6A 174.2(5) . . ? F3A P1 F2A 88.8(5) . . ? F5A P1 F4A 90.6(8) . . ? F5A P1 F6A 87.3(5) . . ? F5A P1 F2A 173.1(5) . . ? F6A P1 F4A 87.5(7) . . ? F6A P1 F2A 87.0(5) . . ? F1A P1 F4A 176.3(8) . . ? F1A P1 F3A 92.1(6) . . ? F1A P1 F5A 93.1(6) . . ? F1A P1 F6A 91.9(6) . . ? F1A P1 F2A 91.1(5) . . ? F2A P1 F4A 85.2(7) . . ? F7 P2 F8 93.8(5) . . ? F7 P2 F9 92.7(6) . . ? F7 P2 F10 176.6(7) . . ? F7 P2 F12 89.0(6) . . ? F8 P2 F9 88.9(4) . . ? F8 P2 F10 88.5(5) . . ? F8 P2 F12 84.9(5) . . ? F9 P2 F10 89.8(6) . . ? F9 P2 F12 173.7(6) . . ? F10 P2 F12 88.7(6) . . ? F11 P2 F7 91.3(6) . . ? F11 P2 F8 174.7(6) . . ? F11 P2 F9 92.0(6) . . ? F11 P2 F10 86.3(6) . . ? F11 P2 F12 94.1(7) . . ? F8A P2A F10A 88.2(12) . . ? F12A P2A F8A 87.4(11) . . ? F12A P2A F10A 90.5(13) . . ? F12A P2A F11A 87.4(10) . . ? F12A P2A F7A 89.0(13) . . ? F12A P2A F9A 179.0(14) . . ? F11A P2A F8A 174.4(11) . . ? F11A P2A F10A 94.0(11) . . ? F11A P2A F9A 93.5(12) . . ? F7A P2A F8A 85.5(11) . . ? F7A P2A F10A 173.7(12) . . ? F7A P2A F11A 92.3(8) . . ? F7A P2A F9A 91.4(12) . . ? F9A P2A F8A 91.7(13) . . ? F9A P2A F10A 88.9(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.217(2) . ? Co1 O2 2.190(2) . ? Co1 N3 2.043(2) . ? Co1 N7 2.141(2) . ? Co1 N8 2.029(2) . ? Co1 N9 2.123(2) . ? O1 C7 1.264(4) . ? O2 C13 1.263(4) . ? O3 C26 1.234(4) . ? O4 C32 1.229(4) . ? N1 C1 1.348(5) . ? N1 C5 1.375(4) . ? N1 C6 1.478(5) . ? N2 C5 1.339(4) . ? N2 C7 1.331(4) . ? N3 C8 1.342(4) . ? N3 C12 1.326(4) . ? N4 C13 1.324(4) . ? N4 C14 1.350(4) . ? N5 C14 1.381(4) . ? N5 C18 1.351(5) . ? N5 C19 1.476(5) . ? N6 C20 1.362(5) . ? N6 C24 1.359(4) . ? N6 C25 1.469(5) . ? N7 C24 1.368(4) . ? N7 C26 1.349(4) . ? N8 C27 1.341(4) . ? N8 C31 1.333(4) . ? N9 C32 1.355(4) . ? N9 C33 1.373(4) . ? N10 C33 1.358(4) . ? N10 C37 1.358(4) . ? N10 C38 1.467(4) . ? C1 H1 0.9500 . ? C1 C2 1.359(6) . ? C2 H2 0.9500 . ? C2 C3 1.394(6) . ? C3 H3 0.9500 . ? C3 C4 1.361(5) . ? C4 H4 0.9500 . ? C4 C5 1.402(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.502(4) . ? C8 C9 1.381(4) . ? C9 H9 0.9500 . ? C9 C10 1.384(5) . ? C10 H10 0.9500 . ? C10 C11 1.389(5) . ? C11 H11 0.9500 . ? C11 C12 1.383(4) . ? C12 C13 1.507(4) . ? C14 C15 1.414(5) . ? C15 H15 0.9500 . ? C15 C16 1.366(5) . ? C16 H16 0.9500 . ? C16 C17 1.383(6) . ? C17 H17 0.9500 . ? C17 C18 1.391(6) . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20 0.9500 . ? C20 C21 1.336(7) . ? C21 H21 0.9500 . ? C21 C22 1.376(7) . ? C22 H22 0.9500 . ? C22 C23 1.365(6) . ? C23 H23 0.9500 . ? C23 C24 1.395(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.508(4) . ? C27 C28 1.377(4) . ? C28 H28 0.9500 . ? C28 C29 1.385(5) . ? C29 H29 0.9500 . ? C29 C30 1.388(5) . ? C30 H30 0.9500 . ? C30 C31 1.384(4) . ? C31 C32 1.506(4) . ? C33 C34 1.386(5) . ? C34 H34 0.9500 . ? C34 C35 1.372(5) . ? C35 H35 0.9500 . ? C35 C36 1.389(6) . ? C36 H36 0.9500 . ? C36 C37 1.346(5) . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? P1 F3 1.572(7) . ? P1 F4 1.522(11) . ? P1 F5 1.647(7) . ? P1 F6 1.590(10) . ? P1 F1 1.668(11) . ? P1 F2 1.557(7) . ? P1 F4A 1.652(15) . ? P1 F3A 1.509(7) . ? P1 F5A 1.534(11) . ? P1 F6A 1.636(8) . ? P1 F1A 1.500(13) . ? P1 F2A 1.637(7) . ? P2 F7 1.547(9) . ? P2 F8 1.563(7) . ? P2 F9 1.584(7) . ? P2 F10 1.589(11) . ? P2 F11 1.544(7) . ? P2 F12 1.600(9) . ? F8A P2A 1.626(15) . ? P2A F10A 1.646(19) . ? P2A F12A 1.482(18) . ? P2A F11A 1.520(13) . ? P2A F7A 1.487(17) . ? P2A F9A 1.521(16) . ?