#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705245.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_7705245 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, 3(F6 P), 2(H2 O)' _chemical_formula_sum 'C38 H38 Co F18 N10 O6 P3' _chemical_formula_weight 1224.62 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2017-09-13 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.3165(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.05781(13) _cell_length_b 14.7905(2) _cell_length_c 24.4665(3) _cell_measurement_reflns_used 13124 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 27.4710 _cell_measurement_theta_min 1.6780 _cell_volume 4662.92(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 173.00(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 0.984 _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 -63.00 58.00 1.00 32.50 -- -23.50 70.00 97.00 121 2 \w 35.00 122.00 1.00 32.50 -- 27.42 178.00-150.00 87 3 \w -10.00 103.00 1.00 32.50 -- 27.42 57.00 -60.00 113 4 \w -49.00 65.00 1.00 32.50 -- 27.42 -57.00 0.00 114 5 \w 35.00 122.00 1.00 32.50 -- 27.42 178.00 -90.00 87 6 \w -44.00 25.00 1.00 32.50 -- 27.42 -70.00 -33.00 69 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0241485000 _diffrn_orient_matrix_UB_12 -0.0323790000 _diffrn_orient_matrix_UB_13 0.0151070000 _diffrn_orient_matrix_UB_21 0.0490119000 _diffrn_orient_matrix_UB_22 -0.0199381000 _diffrn_orient_matrix_UB_23 0.0095950000 _diffrn_orient_matrix_UB_31 0.0067004000 _diffrn_orient_matrix_UB_32 0.0292183000 _diffrn_orient_matrix_UB_33 0.0232977000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 39769 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.049 _diffrn_reflns_theta_min 1.580 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.744 _exptl_crystal_description needle _exptl_crystal_F_000 2472 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.281 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 699 _refine_ls_number_reflns 10068 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0584 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+5.2501P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1544 _refine_ls_wR_factor_ref 0.1661 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7551 _reflns_number_total 10068 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 17ma133_c2.res created by SHELXL-2014/7 TITL 17ma133_c2_a.res in P2(1)/c REM Old TITL 17MA133_C2 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.122, Rweak 0.010, Alpha 0.088, Orientation as input REM Formula found by SHELXT: C37 N11 O8 F16 P3 Co CELL 0.71073 13.057811 14.79048 24.466473 90 99.3165 90 ZERR 4 0.000134 0.000196 0.000277 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Co F N O P UNIT 152 152 4 72 40 24 12 EQIV $1 +X,0.5-Y,0.5+Z DFIX 1.97 H2Wa O43 DFIX 2.11 H2Wb O35_$1 DFIX 1.44 H2Wa H2Wb L.S. 40 PLAN 5 SIZE 0.3 0.05 0.05 BOND $H list 4 fmap 2 acta OMIT 0 54.1 REM REM REM WGHT 0.081300 5.250100 FVAR 1.48067 CO1 3 0.253288 0.190905 0.390944 11.00000 0.01519 0.01645 = 0.02029 0.00033 0.00412 0.00019 P2 7 0.187501 0.046285 0.636447 11.00000 0.02981 0.02911 = 0.02581 -0.00071 0.00237 0.00596 P1 7 0.222737 0.620487 0.472338 11.00000 0.03110 0.02980 = 0.03777 0.00065 0.00530 0.00157 P3 7 0.709528 0.376789 0.272217 11.00000 0.03895 0.03912 = 0.04029 0.00812 0.00507 0.00266 F12 4 0.141684 0.128786 0.667139 11.00000 0.06248 0.05968 = 0.07247 -0.03235 0.00139 0.01909 N8 5 0.265647 0.320799 0.374885 11.00000 0.02035 0.01615 = 0.02164 -0.00032 0.00487 -0.00058 N33 5 0.231143 0.166067 0.310878 11.00000 0.01858 0.01973 = 0.02229 -0.00231 0.00321 0.00108 O35 6 0.098867 0.163456 0.235238 11.00000 0.02641 0.03855 = 0.02218 -0.00409 0.00039 -0.00227 F7 4 0.164430 0.100197 0.580652 11.00000 0.09087 0.07591 = 0.04720 0.02583 0.02255 0.03542 F5 4 0.259451 0.717186 0.455432 11.00000 0.06636 0.04904 = 0.09209 0.02171 -0.00149 -0.02216 O43 6 0.099240 0.257243 0.514965 11.00000 0.02844 0.03273 = 0.02544 -0.00070 0.01116 0.00258 C31 1 0.311205 0.169910 0.278671 11.00000 0.02056 0.02348 = 0.01885 -0.00386 0.00175 0.00021 F6 4 0.184201 0.522647 0.488986 11.00000 0.05452 0.03283 = 0.04941 0.00451 0.00985 -0.00133 N27 5 0.474316 0.113368 0.263085 11.00000 0.02160 0.03538 = 0.02754 -0.00311 0.00591 0.00773 F1 4 0.188313 0.596991 0.408372 11.00000 0.07650 0.06152 = 0.04039 -0.00097 0.01342 -0.00952 N00G 5 0.231731 0.217484 0.466960 11.00000 0.01994 0.02240 = 0.02000 0.00107 0.00444 0.00050 N00H 5 0.395656 0.361742 0.567132 11.00000 0.03636 0.02316 = 0.03026 -0.00273 -0.00200 -0.00087 O10 6 0.390278 0.424862 0.358229 11.00000 0.02965 0.02031 = 0.06005 0.00739 0.01368 -0.00365 F3 4 0.250900 0.642005 0.536775 11.00000 0.09248 0.06311 = 0.04747 -0.01255 0.00194 -0.02602 F13 4 0.644568 0.376339 0.212139 11.00000 0.11909 0.10666 = 0.03963 0.00887 -0.00965 0.00829 F11 4 0.230918 -0.037454 0.606820 11.00000 0.05958 0.04079 = 0.06626 -0.00999 0.01774 0.01497 F15 4 0.773377 0.379402 0.332083 11.00000 0.14938 0.07530 = 0.08162 -0.00354 -0.06114 0.00598 F17 4 0.663373 0.286816 0.289110 11.00000 0.11865 0.07751 = 0.09142 0.02673 -0.02601 -0.05408 C32 1 0.389509 0.106291 0.287568 11.00000 0.02396 0.02770 = 0.02240 -0.00086 0.00479 0.00078 AFIX 43 H32 2 0.383532 0.057632 0.310919 11.00000 -1.20000 AFIX 0 F2 4 0.108751 0.657933 0.473072 11.00000 0.04950 0.05352 = 0.08669 0.01339 0.02478 0.01935 F9 4 0.205835 -0.011622 0.692332 11.00000 0.06310 0.08316 = 0.04199 0.01860 0.01181 0.02319 AFIX 6 O1W 6 0.330786 0.601468 0.330072 11.00000 0.04264 0.03655 = 0.04878 0.00219 0.01670 -0.00413 H1WA 2 0.341927 0.546869 0.340103 11.00000 -1.50000 H1WB 2 0.286798 0.620350 0.349462 11.00000 -1.50000 AFIX 0 N19 5 0.285250 0.064567 0.409803 11.00000 0.01971 0.01766 = 0.02535 0.00110 0.00463 0.00153 C14 1 0.560107 0.127111 0.422123 11.00000 0.02037 0.02887 = 0.04323 -0.00325 0.00198 0.00197 AFIX 43 H14 2 0.599594 0.076094 0.433358 11.00000 -1.20000 AFIX 0 F8 4 0.072776 0.004725 0.624141 11.00000 0.03493 0.04475 = 0.11211 0.01033 -0.00125 0.00361 O18 6 0.425078 -0.031003 0.436748 11.00000 0.02771 0.02399 = 0.05560 0.00725 0.00272 0.00416 F14 4 0.626371 0.435554 0.291705 11.00000 0.17403 0.19533 = 0.07560 0.03414 0.05512 0.13556 C30 1 0.320169 0.238370 0.240990 11.00000 0.02800 0.02684 = 0.02918 -0.00027 0.00669 0.00496 AFIX 43 H30 2 0.267334 0.280742 0.232628 11.00000 -1.20000 AFIX 0 N22 5 0.115929 -0.134996 0.389948 11.00000 0.02366 0.01872 = 0.03736 0.00085 0.00210 -0.00238 F4 4 0.334496 0.581950 0.472002 11.00000 0.03983 0.10328 = 0.11503 0.04708 0.03091 0.02638 C17 1 0.386994 0.042512 0.421816 11.00000 0.02298 0.02254 = 0.02622 -0.00177 0.00464 0.00393 N2 5 0.027890 0.451393 0.376702 11.00000 0.02144 0.02121 = 0.03046 0.00101 0.00523 0.00349 C34 1 0.131734 0.167351 0.285236 11.00000 0.02016 0.01724 = 0.02878 -0.00230 0.00229 -0.00118 C36 1 0.058954 0.178036 0.326951 11.00000 0.02059 0.01734 = 0.02613 0.00127 0.00246 -0.00014 C014 1 0.312528 0.245927 0.509546 11.00000 0.02369 0.02317 = 0.01776 0.00265 0.00608 -0.00053 C7 1 0.113244 0.401089 0.392955 11.00000 0.02124 0.01720 = 0.02354 0.00226 0.00185 -0.00047 AFIX 43 H7 2 0.126616 0.379533 0.429116 11.00000 -1.20000 AFIX 0 F10 4 0.299712 0.086432 0.650913 11.00000 0.03937 0.04605 = 0.15295 -0.00225 -0.00641 -0.00609 AFIX 6 O2W 6 0.175476 0.344847 0.624233 11.00000 0.07918 0.04696 = 0.04298 -0.00089 0.01177 0.00032 H2WA 2 0.149528 0.306997 0.594633 11.00000 -1.50000 AFIX 0 C6 1 0.181611 0.380745 0.356937 11.00000 0.01986 0.01576 = 0.02538 -0.00019 0.00349 -0.00103 C019 1 0.391231 0.453428 0.590829 11.00000 0.06602 0.02388 = 0.05899 -0.01502 -0.01992 0.00182 AFIX 137 H01A 2 0.364725 0.495180 0.561937 11.00000 -1.50000 H01B 2 0.459664 0.471726 0.607616 11.00000 -1.50000 H01C 2 0.346433 0.452864 0.618308 11.00000 -1.50000 AFIX 0 C13 1 0.607243 0.207043 0.412117 11.00000 0.01811 0.03653 = 0.05419 -0.00500 0.00605 -0.00047 AFIX 43 H13 2 0.679239 0.210194 0.416467 11.00000 -1.20000 AFIX 0 C37 1 -0.047676 0.184906 0.315581 11.00000 0.01996 0.02784 = 0.02986 0.00464 0.00027 -0.00089 AFIX 43 H37 2 -0.083022 0.177142 0.279720 11.00000 -1.20000 AFIX 0 C4 1 0.074527 0.470550 0.288923 11.00000 0.04015 0.03194 = 0.03045 0.00987 0.00374 0.00909 AFIX 43 H4 2 0.061592 0.495821 0.253673 11.00000 -1.20000 AFIX 0 F18 4 0.763852 0.463143 0.251183 11.00000 0.09559 0.09247 = 0.16423 0.06502 -0.01052 -0.02957 C38 1 -0.101069 0.203713 0.358993 11.00000 0.01570 0.02635 = 0.04592 0.00763 0.00548 -0.00053 AFIX 43 H38 2 -0.173084 0.207800 0.352279 11.00000 -1.20000 AFIX 0 C01F 1 0.314555 0.332605 0.529889 11.00000 0.03011 0.02367 = 0.02735 0.00164 -0.00129 0.00337 AFIX 43 H01F 2 0.259599 0.371572 0.517911 11.00000 -1.20000 AFIX 0 C0AA 1 0.085665 -0.205731 0.347479 11.00000 0.04277 0.03175 = 0.05200 -0.01149 0.00248 -0.01054 AFIX 137 H0AA 2 0.031843 -0.182898 0.319472 11.00000 -1.50000 H0AB 2 0.060741 -0.257961 0.364570 11.00000 -1.50000 H0AC 2 0.144813 -0.222143 0.330893 11.00000 -1.50000 AFIX 0 C28 1 0.484581 0.181580 0.227898 11.00000 0.03016 0.03792 = 0.03020 -0.00361 0.01212 -0.00361 AFIX 43 H28 2 0.544263 0.186193 0.211863 11.00000 -1.20000 AFIX 0 C01I 1 0.477857 0.308486 0.584424 11.00000 0.03058 0.03637 = 0.02534 0.00030 -0.00128 0.00190 AFIX 43 H01I 2 0.534613 0.331127 0.608408 11.00000 -1.20000 AFIX 0 C29 1 0.407310 0.243767 0.215873 11.00000 0.03848 0.03420 = 0.02935 0.00493 0.01375 -0.00090 AFIX 43 H29 2 0.413254 0.289878 0.190734 11.00000 -1.20000 AFIX 0 C3 1 0.006788 0.486040 0.325482 11.00000 0.02821 0.03086 = 0.03599 0.00729 -0.00001 0.00426 AFIX 43 H3 2 -0.052939 0.520138 0.314803 11.00000 -1.20000 AFIX 0 C11 1 0.440722 0.276679 0.390148 11.00000 0.01977 0.02190 = 0.02789 -0.00283 0.00598 -0.00357 C42 1 0.132222 0.228731 0.473724 11.00000 0.02165 0.01764 = 0.02327 0.00441 0.00634 0.00014 C15 1 0.453128 0.123721 0.415231 11.00000 0.02294 0.02147 = 0.02293 -0.00005 0.00229 0.00311 F16 4 0.798796 0.323287 0.253147 11.00000 0.15388 0.23177 = 0.13677 0.10974 0.10160 0.13973 C01P 1 0.393969 0.188604 0.530098 11.00000 0.03197 0.02155 = 0.02697 -0.00336 0.00311 0.00436 AFIX 43 H01P 2 0.392029 0.128300 0.519213 11.00000 -1.20000 AFIX 0 C9 1 0.362722 0.350233 0.372484 11.00000 0.02089 0.02087 = 0.02745 -0.00228 0.00745 -0.00230 C40 1 0.059626 0.207196 0.421252 11.00000 0.02000 0.01788 = 0.02558 0.00501 0.00715 0.00241 C5 1 0.161350 0.417880 0.304175 11.00000 0.03412 0.02590 = 0.02691 0.00212 0.01076 0.00196 AFIX 43 H5 2 0.206470 0.407160 0.279122 11.00000 -1.20000 AFIX 0 C25 1 0.173511 -0.005906 0.468522 11.00000 0.03757 0.02519 = 0.02898 0.00051 0.00791 -0.00148 AFIX 43 H25 2 0.193151 0.037604 0.495636 11.00000 -1.20000 AFIX 0 C01U 1 0.477734 0.220763 0.566597 11.00000 0.03060 0.03254 = 0.03032 -0.00029 -0.00001 0.00974 AFIX 43 H01U 2 0.533715 0.183100 0.578997 11.00000 -1.20000 AFIX 0 C21 1 0.182585 -0.069523 0.380271 11.00000 0.02398 0.02462 = 0.02649 0.00088 0.00677 0.00194 AFIX 43 H21 2 0.208098 -0.068838 0.346921 11.00000 -1.20000 AFIX 0 C26 1 0.557867 0.045166 0.275363 11.00000 0.03126 0.05866 = 0.04286 0.00710 0.00827 0.02117 AFIX 137 H26A 2 0.551657 0.014633 0.309297 11.00000 -1.50000 H26B 2 0.624143 0.074620 0.279048 11.00000 -1.50000 H26C 2 0.551978 0.002019 0.245706 11.00000 -1.50000 AFIX 0 C12 1 0.547754 0.283670 0.395443 11.00000 0.02247 0.02405 = 0.05065 -0.00433 0.01071 -0.00560 AFIX 43 H12 2 0.579061 0.337834 0.388104 11.00000 -1.20000 AFIX 0 C20 1 0.213331 -0.003506 0.419366 11.00000 0.02076 0.01599 = 0.02699 0.00627 0.00331 0.00368 C39 1 -0.047728 0.216453 0.412329 11.00000 0.02025 0.02273 = 0.03673 0.00615 0.01209 0.00141 AFIX 43 H39 2 -0.082922 0.230803 0.441320 11.00000 -1.20000 AFIX 0 C23 1 0.076554 -0.137514 0.437202 11.00000 0.02492 0.02502 = 0.04238 0.00921 0.00848 -0.00091 AFIX 43 H23 2 0.030203 -0.182908 0.442991 11.00000 -1.20000 AFIX 0 C1 1 -0.043031 0.469964 0.417131 11.00000 0.02843 0.03646 = 0.03928 -0.00049 0.01385 0.00553 AFIX 137 H1A 2 -0.023573 0.433154 0.449462 11.00000 -1.50000 H1B 2 -0.113034 0.456112 0.400586 11.00000 -1.50000 H1C 2 -0.038303 0.532625 0.427465 11.00000 -1.50000 AFIX 0 C24 1 0.104826 -0.072927 0.477011 11.00000 0.03741 0.02969 = 0.03343 0.00567 0.01616 0.00381 AFIX 43 H24 2 0.077483 -0.074467 0.509814 11.00000 -1.20000 AFIX 0 N41 5 0.109068 0.187204 0.379115 11.00000 0.01757 0.01629 = 0.02286 0.00316 0.00580 -0.00249 N16 5 0.397530 0.198225 0.400571 11.00000 0.01663 0.02072 = 0.02110 -0.00059 0.00419 0.00165 H2WB 2 0.143555 0.322992 0.653920 11.00000 0.13160 HKLF 4 REM 17ma133_c2_a.res in P2(1)/c REM R1 = 0.0584 for 7551 Fo > 4sig(Fo) and 0.0816 for all 10068 data REM 699 parameters refined using 3 restraints END WGHT 0.0813 5.2501 REM Highest difference peak 1.281, deepest hole -0.795, 1-sigma level 0.091 Q1 1 0.2574 0.0550 0.6961 11.00000 0.05 1.28 Q2 1 0.7237 0.4847 0.2886 11.00000 0.05 1.16 Q3 1 0.7216 0.2755 0.2571 11.00000 0.05 1.06 Q4 1 0.1059 0.0223 0.6667 11.00000 0.05 1.02 Q5 1 0.5897 0.3519 0.2851 11.00000 0.05 1.01 REM The information below was added by Olex2. REM REM R1 = 0.0584 for 7551 Fo > 4sig(Fo) and 0.0816 for all 41264 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.28, deepest hole -0.79 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0816 REM R1_gt = 0.0584 REM wR_ref = 0.1661 REM GOOF = 1.102 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 41264 REM Reflections_gt = 7551 REM Parameters = n/a REM Hole = -0.79 REM Peak = 1.28 REM Flack = n/a ; _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 17MA133_PM107-H2O _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_original_cell_volume 4662.91(10) _cod_database_code 7705245 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C38H34Co1F12N10O4P2 _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 0.971 _shelx_estimated_absorpt_t_min 0.840 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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, All O(H) groups, All O(H,H) groups 2. Restrained distances H2WA-O43 1.97 with sigma of 0.02 H2WB-O35_$1 2.11 with sigma of 0.02 H2WA-H2WB 1.44 with sigma of 0.02 3.a Free rotating group: O1W(H1WA,H1WB), O2W(H2WA) 3.b Aromatic/amide H refined with riding coordinates: C32(H32), C14(H14), C30(H30), C7(H7), C13(H13), C37(H37), C4(H4), C38(H38), C01F(H01F), C28(H28), C01I(H01I), C29(H29), C3(H3), C01P(H01P), C5(H5), C25(H25), C01U(H01U), C21(H21), C12(H12), C39(H39), C23(H23), C24(H24) 3.c Idealised Me refined as rotating group: C019(H01A,H01B,H01C), C0AA(H0AA,H0AB,H0AC), C26(H26A,H26B,H26C), C1(H1A,H1B, H1C) ; _olex2_date_sample_data_collection 2017-09-12 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.624 _oxdiff_exptl_absorpt_empirical_full_min 0.661 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.25329(3) 0.19091(3) 0.39094(2) 0.01717(12) Uani 1 1 d . . . . . P2 P 0.18750(7) 0.04628(7) 0.63645(4) 0.0285(2) Uani 1 1 d . . . . . P1 P 0.22274(8) 0.62049(7) 0.47234(4) 0.0329(2) Uani 1 1 d . . . . . P3 P 0.70953(8) 0.37679(8) 0.27222(4) 0.0396(3) Uani 1 1 d . . . . . F12 F 0.1417(2) 0.1288(2) 0.66714(12) 0.0659(8) Uani 1 1 d . . . . . N8 N 0.2656(2) 0.32080(18) 0.37488(11) 0.0192(5) Uani 1 1 d . . . . . N33 N 0.23114(19) 0.16607(19) 0.31088(11) 0.0202(6) Uani 1 1 d . . . . . O35 O 0.09887(18) 0.16346(18) 0.23524(9) 0.0294(6) Uani 1 1 d D . . . . F7 F 0.1644(3) 0.1002(2) 0.58065(11) 0.0701(9) Uani 1 1 d . . . . . F5 F 0.2595(2) 0.7172(2) 0.45543(14) 0.0708(9) Uani 1 1 d . . . . . O43 O 0.09924(18) 0.25724(17) 0.51497(9) 0.0281(5) Uani 1 1 d D . . . . C31 C 0.3112(2) 0.1699(2) 0.27867(12) 0.0211(7) Uani 1 1 d . . . . . F6 F 0.18420(19) 0.52265(16) 0.48899(10) 0.0454(6) Uani 1 1 d . . . . . N27 N 0.4743(2) 0.1134(2) 0.26309(12) 0.0280(7) Uani 1 1 d . . . . . F1 F 0.1883(2) 0.5970(2) 0.40837(10) 0.0590(7) Uani 1 1 d . . . . . N00G N 0.2317(2) 0.21748(19) 0.46696(10) 0.0206(6) Uani 1 1 d . . . . . N00H N 0.3957(2) 0.3617(2) 0.56713(12) 0.0307(7) Uani 1 1 d . . . . . O10 O 0.39028(19) 0.42486(17) 0.35823(12) 0.0360(6) Uani 1 1 d . . . . . F3 F 0.2509(3) 0.6420(2) 0.53678(11) 0.0687(9) Uani 1 1 d . . . . . F13 F 0.6446(3) 0.3763(3) 0.21214(12) 0.0910(12) Uani 1 1 d . . . . . F11 F 0.2309(2) -0.03745(18) 0.60682(11) 0.0547(7) Uani 1 1 d . . . . . F15 F 0.7734(4) 0.3794(3) 0.33208(16) 0.1109(16) Uani 1 1 d . . . . . F17 F 0.6634(3) 0.2868(3) 0.28911(16) 0.1006(14) Uani 1 1 d . . . . . C32 C 0.3895(2) 0.1063(2) 0.28757(13) 0.0246(7) Uani 1 1 d . . . . . H32 H 0.3835 0.0576 0.3109 0.029 Uiso 1 1 calc R . . . . F2 F 0.1088(2) 0.6579(2) 0.47307(13) 0.0617(8) Uani 1 1 d . . . . . F9 F 0.2058(2) -0.0116(2) 0.69233(10) 0.0624(8) Uani 1 1 d . . . . . O1W O 0.3308(2) 0.6015(2) 0.33007(12) 0.0416(7) Uani 1 1 d . . . . . H1WA H 0.3419 0.5469 0.3401 0.062 Uiso 1 1 d G . . . . H1WB H 0.2868 0.6204 0.3495 0.062 Uiso 1 1 d G . . . . N19 N 0.2852(2) 0.06457(19) 0.40980(11) 0.0208(6) Uani 1 1 d . . . . . C14 C 0.5601(3) 0.1271(3) 0.42212(16) 0.0312(8) Uani 1 1 d . . . . . H14 H 0.5996 0.0761 0.4334 0.037 Uiso 1 1 calc R . . . . F8 F 0.0728(2) 0.00473(19) 0.62414(14) 0.0654(8) Uani 1 1 d . . . . . O18 O 0.42508(19) -0.03100(18) 0.43675(12) 0.0362(6) Uani 1 1 d . . . . . F14 F 0.6264(4) 0.4356(4) 0.29170(16) 0.144(2) Uani 1 1 d . . . . . C30 C 0.3202(3) 0.2384(3) 0.24099(14) 0.0278(8) Uani 1 1 d . . . . . H30 H 0.2673 0.2807 0.2326 0.033 Uiso 1 1 calc R . . . . N22 N 0.1159(2) -0.1350(2) 0.38995(12) 0.0269(6) Uani 1 1 d . . . . . F4 F 0.3345(2) 0.5819(3) 0.47200(15) 0.0840(11) Uani 1 1 d . . . . . C17 C 0.3870(2) 0.0425(2) 0.42182(13) 0.0238(7) Uani 1 1 d . . . . . N2 N 0.0279(2) 0.4514(2) 0.37670(12) 0.0243(6) Uani 1 1 d . . . . . C34 C 0.1317(2) 0.1674(2) 0.28524(13) 0.0222(7) Uani 1 1 d . . . . . C36 C 0.0590(2) 0.1780(2) 0.32695(13) 0.0215(7) Uani 1 1 d . . . . . C014 C 0.3125(2) 0.2459(2) 0.50955(12) 0.0212(7) Uani 1 1 d . . . . . C7 C 0.1132(2) 0.4011(2) 0.39295(13) 0.0209(7) Uani 1 1 d . . . . . H7 H 0.1266 0.3795 0.4291 0.025 Uiso 1 1 calc R . . . . F10 F 0.2997(2) 0.0864(2) 0.65091(17) 0.0819(11) Uani 1 1 d . . . . . O2W O 0.1755(3) 0.3448(2) 0.62423(14) 0.0562(8) Uani 1 1 d . . . . . H2WA H 0.1495 0.3070 0.5946 0.084 Uiso 1 1 d DG . . . . C6 C 0.1816(2) 0.3807(2) 0.35694(13) 0.0204(6) Uani 1 1 d . . . . . C019 C 0.3912(4) 0.4534(3) 0.5908(2) 0.0530(13) Uani 1 1 d . . . . . H01A H 0.3647 0.4952 0.5619 0.079 Uiso 1 1 calc GR . . . . H01B H 0.4597 0.4717 0.6076 0.079 Uiso 1 1 calc GR . . . . H01C H 0.3464 0.4529 0.6183 0.079 Uiso 1 1 calc GR . . . . C13 C 0.6072(3) 0.2070(3) 0.41212(17) 0.0363(9) Uani 1 1 d . . . . . H13 H 0.6792 0.2102 0.4165 0.044 Uiso 1 1 calc R . . . . C37 C -0.0477(2) 0.1849(2) 0.31558(14) 0.0263(7) Uani 1 1 d . . . . . H37 H -0.0830 0.1771 0.2797 0.032 Uiso 1 1 calc R . . . . C4 C 0.0745(3) 0.4706(3) 0.28892(15) 0.0344(9) Uani 1 1 d . . . . . H4 H 0.0616 0.4958 0.2537 0.041 Uiso 1 1 calc R . . . . F18 F 0.7639(3) 0.4631(3) 0.2512(2) 0.1209(17) Uani 1 1 d . . . . . C38 C -0.1011(3) 0.2037(2) 0.35899(16) 0.0293(8) Uani 1 1 d . . . . . H38 H -0.1731 0.2078 0.3523 0.035 Uiso 1 1 calc R . . . . C01F C 0.3146(3) 0.3326(3) 0.52989(14) 0.0277(7) Uani 1 1 d . . . . . H01F H 0.2596 0.3716 0.5179 0.033 Uiso 1 1 calc R . . . . C0AA C 0.0857(3) -0.2057(3) 0.34748(18) 0.0427(10) Uani 1 1 d . . . . . H0AA H 0.0318 -0.1829 0.3195 0.064 Uiso 1 1 calc GR . . . . H0AB H 0.0607 -0.2580 0.3646 0.064 Uiso 1 1 calc GR . . . . H0AC H 0.1448 -0.2221 0.3309 0.064 Uiso 1 1 calc GR . . . . C28 C 0.4846(3) 0.1816(3) 0.22790(15) 0.0320(8) Uani 1 1 d . . . . . H28 H 0.5443 0.1862 0.2119 0.038 Uiso 1 1 calc R . . . . C01I C 0.4779(3) 0.3085(3) 0.58442(14) 0.0314(8) Uani 1 1 d . . . . . H01I H 0.5346 0.3311 0.6084 0.038 Uiso 1 1 calc R . . . . C29 C 0.4073(3) 0.2438(3) 0.21587(15) 0.0331(8) Uani 1 1 d . . . . . H29 H 0.4133 0.2899 0.1907 0.040 Uiso 1 1 calc R . . . . C3 C 0.0068(3) 0.4860(3) 0.32548(15) 0.0323(8) Uani 1 1 d . . . . . H3 H -0.0529 0.5201 0.3148 0.039 Uiso 1 1 calc R . . . . C11 C 0.4407(2) 0.2767(2) 0.39015(13) 0.0230(7) Uani 1 1 d . . . . . C42 C 0.1322(2) 0.2287(2) 0.47372(13) 0.0206(6) Uani 1 1 d . . . . . C15 C 0.4531(2) 0.1237(2) 0.41523(13) 0.0226(7) Uani 1 1 d . . . . . F16 F 0.7988(4) 0.3233(4) 0.2531(2) 0.165(3) Uani 1 1 d . . . . . C01P C 0.3940(3) 0.1886(2) 0.53010(14) 0.0270(7) Uani 1 1 d . . . . . H01P H 0.3920 0.1283 0.5192 0.032 Uiso 1 1 calc R . . . . C9 C 0.3627(2) 0.3502(2) 0.37248(13) 0.0227(7) Uani 1 1 d . . . . . C40 C 0.0596(2) 0.2072(2) 0.42125(13) 0.0208(7) Uani 1 1 d . . . . . C5 C 0.1614(3) 0.4179(2) 0.30418(14) 0.0283(8) Uani 1 1 d . . . . . H5 H 0.2065 0.4072 0.2791 0.034 Uiso 1 1 calc R . . . . C25 C 0.1735(3) -0.0059(3) 0.46852(15) 0.0303(8) Uani 1 1 d . . . . . H25 H 0.1932 0.0376 0.4956 0.036 Uiso 1 1 calc R . . . . C01U C 0.4777(3) 0.2208(3) 0.56660(15) 0.0317(8) Uani 1 1 d . . . . . H01U H 0.5337 0.1831 0.5790 0.038 Uiso 1 1 calc R . . . . C21 C 0.1826(2) -0.0695(2) 0.38027(14) 0.0247(7) Uani 1 1 d . . . . . H21 H 0.2081 -0.0688 0.3469 0.030 Uiso 1 1 calc R . . . . C26 C 0.5579(3) 0.0452(3) 0.27536(17) 0.0440(11) Uani 1 1 d . . . . . H26A H 0.5517 0.0146 0.3093 0.066 Uiso 1 1 calc GR . . . . H26B H 0.6241 0.0746 0.2790 0.066 Uiso 1 1 calc GR . . . . H26C H 0.5520 0.0020 0.2457 0.066 Uiso 1 1 calc GR . . . . C12 C 0.5478(3) 0.2837(3) 0.39544(16) 0.0319(8) Uani 1 1 d . . . . . H12 H 0.5791 0.3378 0.3881 0.038 Uiso 1 1 calc R . . . . C20 C 0.2133(2) -0.0035(2) 0.41937(13) 0.0213(7) Uani 1 1 d . . . . . C39 C -0.0477(2) 0.2165(2) 0.41233(15) 0.0257(7) Uani 1 1 d . . . . . H39 H -0.0829 0.2308 0.4413 0.031 Uiso 1 1 calc R . . . . C23 C 0.0766(3) -0.1375(3) 0.43720(15) 0.0304(8) Uani 1 1 d . . . . . H23 H 0.0302 -0.1829 0.4430 0.037 Uiso 1 1 calc R . . . . C1 C -0.0430(3) 0.4700(3) 0.41713(16) 0.0338(8) Uani 1 1 d . . . . . H1A H -0.0236 0.4332 0.4495 0.051 Uiso 1 1 calc GR . . . . H1B H -0.1130 0.4561 0.4006 0.051 Uiso 1 1 calc GR . . . . H1C H -0.0383 0.5326 0.4275 0.051 Uiso 1 1 calc GR . . . . C24 C 0.1048(3) -0.0729(3) 0.47701(15) 0.0324(8) Uani 1 1 d . . . . . H24 H 0.0775 -0.0745 0.5098 0.039 Uiso 1 1 calc R . . . . N41 N 0.10907(19) 0.18720(18) 0.37911(11) 0.0186(5) Uani 1 1 d . . . . . N16 N 0.39753(19) 0.19823(18) 0.40057(10) 0.0194(6) Uani 1 1 d . . . . . H2WB H 0.144(6) 0.323(5) 0.6539(14) 0.13(3) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0152(2) 0.0164(2) 0.0203(2) 0.00033(16) 0.00412(15) 0.00019(16) P2 0.0298(5) 0.0291(5) 0.0258(4) -0.0007(4) 0.0024(3) 0.0060(4) P1 0.0311(5) 0.0298(6) 0.0378(5) 0.0006(4) 0.0053(4) 0.0016(4) P3 0.0390(6) 0.0391(6) 0.0403(6) 0.0081(5) 0.0051(4) 0.0027(5) F12 0.0625(18) 0.0597(19) 0.0725(19) -0.0324(15) 0.0014(14) 0.0191(14) N8 0.0204(13) 0.0162(14) 0.0216(13) -0.0003(10) 0.0049(10) -0.0006(11) N33 0.0186(12) 0.0197(14) 0.0223(13) -0.0023(11) 0.0032(10) 0.0011(11) O35 0.0264(12) 0.0386(15) 0.0222(12) -0.0041(10) 0.0004(9) -0.0023(11) F7 0.091(2) 0.076(2) 0.0472(15) 0.0258(15) 0.0225(14) 0.0354(18) F5 0.0664(19) 0.0490(18) 0.092(2) 0.0217(16) -0.0015(16) -0.0222(15) O43 0.0284(12) 0.0327(15) 0.0254(12) -0.0007(10) 0.0112(9) 0.0026(11) C31 0.0206(15) 0.0235(18) 0.0189(15) -0.0039(13) 0.0018(12) 0.0002(13) F6 0.0545(15) 0.0328(14) 0.0494(14) 0.0045(11) 0.0099(11) -0.0013(11) N27 0.0216(14) 0.0354(18) 0.0275(15) -0.0031(13) 0.0059(11) 0.0077(13) F1 0.0765(19) 0.0615(19) 0.0404(14) -0.0010(13) 0.0134(13) -0.0095(15) N00G 0.0199(13) 0.0224(15) 0.0200(13) 0.0011(11) 0.0044(10) 0.0005(11) N00H 0.0364(16) 0.0232(17) 0.0303(15) -0.0027(12) -0.0020(12) -0.0009(13) O10 0.0296(13) 0.0203(14) 0.0601(17) 0.0074(12) 0.0137(12) -0.0036(11) F3 0.092(2) 0.063(2) 0.0475(16) -0.0125(14) 0.0019(14) -0.0260(17) F13 0.119(3) 0.107(3) 0.0396(16) 0.0089(17) -0.0097(17) 0.008(2) F11 0.0596(16) 0.0408(16) 0.0663(17) -0.0100(12) 0.0177(13) 0.0150(13) F15 0.149(4) 0.075(3) 0.082(2) -0.0035(19) -0.061(2) 0.006(2) F17 0.119(3) 0.078(3) 0.091(3) 0.027(2) -0.026(2) -0.054(2) C32 0.0240(16) 0.0277(19) 0.0224(16) -0.0009(14) 0.0048(12) 0.0008(14) F2 0.0495(15) 0.0535(18) 0.087(2) 0.0134(15) 0.0248(14) 0.0193(14) F9 0.0631(17) 0.083(2) 0.0420(14) 0.0186(14) 0.0118(12) 0.0232(16) O1W 0.0426(16) 0.0365(17) 0.0488(17) 0.0022(14) 0.0167(13) -0.0041(13) N19 0.0197(12) 0.0177(14) 0.0253(13) 0.0011(11) 0.0046(10) 0.0015(11) C14 0.0204(16) 0.029(2) 0.043(2) -0.0032(16) 0.0020(14) 0.0020(15) F8 0.0349(13) 0.0447(17) 0.112(2) 0.0103(16) -0.0013(14) 0.0036(12) O18 0.0277(13) 0.0240(15) 0.0556(17) 0.0073(12) 0.0027(11) 0.0042(11) F14 0.174(4) 0.195(5) 0.076(3) 0.034(3) 0.055(3) 0.136(4) C30 0.0280(17) 0.027(2) 0.0292(17) -0.0003(15) 0.0067(13) 0.0050(15) N22 0.0237(14) 0.0187(16) 0.0374(16) 0.0008(12) 0.0021(12) -0.0024(12) F4 0.0398(15) 0.103(3) 0.115(3) 0.047(2) 0.0309(16) 0.0264(16) C17 0.0230(15) 0.0225(19) 0.0262(16) -0.0018(14) 0.0046(12) 0.0039(14) N2 0.0214(13) 0.0212(15) 0.0305(15) 0.0010(12) 0.0052(11) 0.0035(12) C34 0.0202(15) 0.0172(17) 0.0288(17) -0.0023(13) 0.0023(12) -0.0012(13) C36 0.0206(15) 0.0173(17) 0.0261(16) 0.0013(13) 0.0025(12) -0.0001(13) C014 0.0237(15) 0.0232(18) 0.0178(14) 0.0027(13) 0.0061(12) -0.0005(13) C7 0.0212(15) 0.0172(17) 0.0235(15) 0.0023(13) 0.0019(12) -0.0005(13) F10 0.0394(15) 0.0461(19) 0.153(3) -0.0023(19) -0.0064(17) -0.0061(13) O2W 0.079(2) 0.047(2) 0.0430(18) -0.0009(15) 0.0118(17) 0.0003(18) C6 0.0199(14) 0.0158(16) 0.0254(16) -0.0002(13) 0.0035(12) -0.0010(12) C019 0.066(3) 0.024(2) 0.059(3) -0.015(2) -0.020(2) 0.002(2) C13 0.0181(16) 0.037(2) 0.054(2) -0.0050(18) 0.0061(15) -0.0005(15) C37 0.0200(15) 0.028(2) 0.0299(17) 0.0046(14) 0.0003(13) -0.0009(14) C4 0.040(2) 0.032(2) 0.0304(18) 0.0099(16) 0.0037(15) 0.0091(17) F18 0.096(3) 0.092(3) 0.164(4) 0.065(3) -0.011(3) -0.030(2) C38 0.0157(15) 0.026(2) 0.046(2) 0.0076(16) 0.0055(14) -0.0005(14) C01F 0.0301(17) 0.0237(19) 0.0274(17) 0.0016(14) -0.0013(14) 0.0034(15) C0AA 0.043(2) 0.032(2) 0.052(2) -0.0115(19) 0.0025(19) -0.0105(18) C28 0.0302(18) 0.038(2) 0.0302(18) -0.0036(16) 0.0121(14) -0.0036(16) C01I 0.0306(18) 0.036(2) 0.0253(17) 0.0003(15) -0.0013(14) 0.0019(16) C29 0.038(2) 0.034(2) 0.0293(18) 0.0049(16) 0.0137(15) -0.0009(17) C3 0.0282(18) 0.031(2) 0.0360(19) 0.0073(16) 0.0000(14) 0.0043(16) C11 0.0198(15) 0.0219(18) 0.0279(16) -0.0028(14) 0.0060(12) -0.0036(13) C42 0.0217(15) 0.0176(17) 0.0233(15) 0.0044(13) 0.0063(12) 0.0001(13) C15 0.0229(15) 0.0215(18) 0.0229(15) -0.0001(13) 0.0023(12) 0.0031(13) F16 0.154(4) 0.232(6) 0.137(4) 0.110(4) 0.102(3) 0.140(4) C01P 0.0320(18) 0.0216(18) 0.0270(17) -0.0034(14) 0.0031(14) 0.0044(15) C9 0.0209(15) 0.0209(18) 0.0274(16) -0.0023(14) 0.0074(12) -0.0023(13) C40 0.0200(15) 0.0179(17) 0.0256(16) 0.0050(13) 0.0072(12) 0.0024(13) C5 0.0341(18) 0.026(2) 0.0269(17) 0.0021(14) 0.0108(14) 0.0020(15) C25 0.0376(19) 0.025(2) 0.0290(18) 0.0005(15) 0.0079(14) -0.0015(16) C01U 0.0306(18) 0.033(2) 0.0303(18) -0.0003(15) 0.0000(14) 0.0097(16) C21 0.0240(16) 0.0246(19) 0.0265(16) 0.0009(14) 0.0068(13) 0.0019(14) C26 0.031(2) 0.059(3) 0.043(2) 0.007(2) 0.0083(16) 0.021(2) C12 0.0225(17) 0.024(2) 0.051(2) -0.0043(16) 0.0107(15) -0.0056(15) C20 0.0208(15) 0.0160(17) 0.0270(16) 0.0063(13) 0.0033(12) 0.0037(13) C39 0.0203(15) 0.0227(19) 0.0367(18) 0.0062(15) 0.0121(13) 0.0014(14) C23 0.0249(17) 0.025(2) 0.042(2) 0.0092(16) 0.0085(15) -0.0009(15) C1 0.0284(18) 0.036(2) 0.039(2) -0.0005(17) 0.0139(15) 0.0055(16) C24 0.0374(19) 0.030(2) 0.0334(19) 0.0057(16) 0.0162(15) 0.0038(16) N41 0.0176(12) 0.0163(14) 0.0229(13) 0.0032(11) 0.0058(10) -0.0025(10) N16 0.0166(12) 0.0207(15) 0.0211(13) -0.0006(11) 0.0042(10) 0.0016(11) 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 N33 Co1 N8 89.26(11) . . ? N00G Co1 N8 91.29(11) . . ? N00G Co1 N33 163.52(11) . . ? N19 Co1 N8 163.19(11) . . ? N19 Co1 N33 92.75(11) . . ? N19 Co1 N00G 91.47(11) . . ? N41 Co1 N8 96.38(11) . . ? N41 Co1 N33 81.82(11) . . ? N41 Co1 N00G 81.75(11) . . ? N41 Co1 N19 100.42(11) . . ? N41 Co1 N16 177.66(12) . . ? N16 Co1 N8 81.66(11) . . ? N16 Co1 N33 96.85(11) . . ? N16 Co1 N00G 99.52(11) . . ? N16 Co1 N19 81.53(11) . . ? F12 P2 F8 88.37(16) . . ? F7 P2 F12 89.26(17) . . ? F7 P2 F11 91.82(16) . . ? F7 P2 F9 177.10(19) . . ? F7 P2 F8 89.40(18) . . ? F11 P2 F12 178.36(18) . . ? F11 P2 F9 87.56(15) . . ? F11 P2 F8 90.40(16) . . ? F9 P2 F12 91.31(17) . . ? F9 P2 F8 87.77(16) . . ? F10 P2 F12 90.69(18) . . ? F10 P2 F7 92.6(2) . . ? F10 P2 F11 90.50(17) . . ? F10 P2 F9 90.27(18) . . ? F10 P2 F8 177.8(2) . . ? F5 P1 F6 179.30(17) . . ? F5 P1 F1 89.41(17) . . ? F5 P1 F3 92.69(17) . . ? F5 P1 F2 90.68(17) . . ? F1 P1 F6 90.14(15) . . ? F3 P1 F6 87.74(15) . . ? F3 P1 F1 176.79(17) . . ? F2 P1 F6 88.78(15) . . ? F2 P1 F1 88.36(16) . . ? F2 P1 F3 89.18(18) . . ? F4 P1 F5 90.32(18) . . ? F4 P1 F6 90.22(17) . . ? F4 P1 F1 91.74(19) . . ? F4 P1 F3 90.7(2) . . ? F4 P1 F2 179.00(19) . . ? F13 P3 F18 84.4(2) . . ? F15 P3 F13 178.8(2) . . ? F15 P3 F18 94.9(2) . . ? F17 P3 F13 94.1(2) . . ? F17 P3 F15 86.7(2) . . ? F17 P3 F18 174.1(3) . . ? F14 P3 F13 89.5(2) . . ? F14 P3 F15 89.5(3) . . ? F14 P3 F17 94.5(3) . . ? F14 P3 F18 91.2(3) . . ? F14 P3 F16 175.9(4) . . ? F16 P3 F13 92.0(3) . . ? F16 P3 F15 88.9(3) . . ? F16 P3 F17 89.2(3) . . ? F16 P3 F18 85.1(3) . . ? C6 N8 Co1 125.7(2) . . ? C9 N8 Co1 115.5(2) . . ? C9 N8 C6 117.9(3) . . ? C31 N33 Co1 123.1(2) . . ? C34 N33 Co1 115.9(2) . . ? C34 N33 C31 119.0(3) . . ? C32 C31 N33 118.8(3) . . ? C32 C31 C30 117.5(3) . . ? C30 C31 N33 123.5(3) . . ? C32 N27 C28 121.1(3) . . ? C32 N27 C26 119.3(3) . . ? C28 N27 C26 119.6(3) . . ? C014 N00G Co1 123.4(2) . . ? C42 N00G Co1 115.5(2) . . ? C42 N00G C014 119.3(3) . . ? C01F N00H C019 118.7(3) . . ? C01I N00H C019 119.6(3) . . ? C01I N00H C01F 121.6(3) . . ? C31 C32 H32 119.4 . . ? N27 C32 C31 121.2(3) . . ? N27 C32 H32 119.4 . . ? H1WA O1W H1WB 104.5 . . ? C17 N19 Co1 116.5(2) . . ? C17 N19 C20 116.4(3) . . ? C20 N19 Co1 126.5(2) . . ? C13 C14 H14 120.5 . . ? C13 C14 C15 118.9(3) . . ? C15 C14 H14 120.5 . . ? C31 C30 H30 119.9 . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30 119.9 . . ? C21 N22 C0AA 119.4(3) . . ? C23 N22 C0AA 119.3(3) . . ? C23 N22 C21 121.4(3) . . ? N19 C17 C15 110.2(3) . . ? O18 C17 N19 127.9(3) . . ? O18 C17 C15 121.9(3) . . ? C7 N2 C1 118.8(3) . . ? C3 N2 C7 121.5(3) . . ? C3 N2 C1 119.7(3) . . ? N33 C34 C36 110.5(3) . . ? O35 C34 N33 128.1(3) . . ? O35 C34 C36 121.3(3) . . ? C37 C36 C34 126.6(3) . . ? N41 C36 C34 112.9(3) . . ? N41 C36 C37 120.3(3) . . ? C01F C014 N00G 120.7(3) . . ? C01F C014 C01P 118.0(3) . . ? C01P C014 N00G 121.2(3) . . ? N2 C7 H7 119.3 . . ? N2 C7 C6 121.4(3) . . ? C6 C7 H7 119.3 . . ? H2WA O2W H2WB 103.9 . . ? C7 C6 N8 118.9(3) . . ? C7 C6 C5 117.4(3) . . ? C5 C6 N8 123.7(3) . . ? N00H C019 H01A 109.5 . . ? N00H C019 H01B 109.5 . . ? N00H C019 H01C 109.5 . . ? H01A C019 H01B 109.5 . . ? H01A C019 H01C 109.5 . . ? H01B C019 H01C 109.5 . . ? C14 C13 H13 119.8 . . ? C14 C13 C12 120.4(3) . . ? C12 C13 H13 119.8 . . ? C36 C37 H37 120.8 . . ? C36 C37 C38 118.4(3) . . ? C38 C37 H37 120.8 . . ? C3 C4 H4 119.8 . . ? C3 C4 C5 120.4(3) . . ? C5 C4 H4 119.8 . . ? C37 C38 H38 119.7 . . ? C39 C38 C37 120.5(3) . . ? C39 C38 H38 119.7 . . ? N00H C01F C014 120.6(3) . . ? N00H C01F H01F 119.7 . . ? C014 C01F H01F 119.7 . . ? N22 C0AA H0AA 109.5 . . ? N22 C0AA H0AB 109.5 . . ? N22 C0AA H0AC 109.5 . . ? H0AA C0AA H0AB 109.5 . . ? H0AA C0AA H0AC 109.5 . . ? H0AB C0AA H0AC 109.5 . . ? N27 C28 H28 120.1 . . ? N27 C28 C29 119.8(3) . . ? C29 C28 H28 120.1 . . ? N00H C01I H01I 120.1 . . ? N00H C01I C01U 119.7(3) . . ? C01U C01I H01I 120.1 . . ? C30 C29 H29 120.0 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29 120.0 . . ? N2 C3 C4 119.2(3) . . ? N2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C12 C11 C9 126.7(3) . . ? N16 C11 C9 113.4(3) . . ? N16 C11 C12 119.9(3) . . ? O43 C42 N00G 127.9(3) . . ? O43 C42 C40 121.1(3) . . ? N00G C42 C40 110.9(3) . . ? C14 C15 C17 127.1(3) . . ? N16 C15 C14 119.9(3) . . ? N16 C15 C17 113.0(3) . . ? C014 C01P H01P 119.9 . . ? C01U C01P C014 120.3(3) . . ? C01U C01P H01P 119.9 . . ? N8 C9 C11 110.5(3) . . ? O10 C9 N8 128.5(3) . . ? O10 C9 C11 121.0(3) . . ? C39 C40 C42 126.5(3) . . ? N41 C40 C42 113.0(3) . . ? N41 C40 C39 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C20 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C24 C25 C20 119.7(3) . . ? C01I C01U C01P 119.5(3) . . ? C01I C01U H01U 120.2 . . ? C01P C01U H01U 120.2 . . ? N22 C21 H21 119.7 . . ? N22 C21 C20 120.7(3) . . ? C20 C21 H21 119.7 . . ? N27 C26 H26A 109.5 . . ? N27 C26 H26B 109.5 . . ? N27 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C13 C12 H12 120.9 . . ? C11 C12 C13 118.1(3) . . ? C11 C12 H12 120.9 . . ? C25 C20 N19 120.8(3) . . ? C21 C20 N19 120.8(3) . . ? C21 C20 C25 118.4(3) . . ? C38 C39 C40 118.3(3) . . ? C38 C39 H39 120.9 . . ? C40 C39 H39 120.9 . . ? N22 C23 H23 120.1 . . ? N22 C23 C24 119.8(3) . . ? C24 C23 H23 120.1 . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C25 C24 H24 119.9 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 119.9 . . ? C36 N41 Co1 118.4(2) . . ? C40 N41 Co1 118.5(2) . . ? C40 N41 C36 122.3(3) . . ? C11 N16 Co1 118.5(2) . . ? C11 N16 C15 122.8(3) . . ? C15 N16 Co1 118.7(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N8 1.973(3) . ? Co1 N33 1.968(3) . ? Co1 N00G 1.965(3) . ? Co1 N19 1.954(3) . ? Co1 N41 1.859(3) . ? Co1 N16 1.863(3) . ? P2 F12 1.599(3) . ? P2 F7 1.567(3) . ? P2 F11 1.586(3) . ? P2 F9 1.598(3) . ? P2 F8 1.602(3) . ? P2 F10 1.567(3) . ? P1 F5 1.585(3) . ? P1 F6 1.606(3) . ? P1 F1 1.595(3) . ? P1 F3 1.592(3) . ? P1 F2 1.591(3) . ? P1 F4 1.568(3) . ? P3 F13 1.574(3) . ? P3 F15 1.564(3) . ? P3 F17 1.545(3) . ? P3 F14 1.526(4) . ? P3 F18 1.587(4) . ? P3 F16 1.542(4) . ? N8 C6 1.424(4) . ? N8 C9 1.351(4) . ? N33 C31 1.408(4) . ? N33 C34 1.347(4) . ? O35 C34 1.230(4) . ? O43 C42 1.234(4) . ? C31 C32 1.381(5) . ? C31 C30 1.387(5) . ? N27 C32 1.346(4) . ? N27 C28 1.347(5) . ? N27 C26 1.481(5) . ? N00G C014 1.421(4) . ? N00G C42 1.346(4) . ? N00H C019 1.480(5) . ? N00H C01F 1.351(4) . ? N00H C01I 1.343(5) . ? O10 C9 1.229(4) . ? C32 H32 0.9300 . ? O1W H1WA 0.8497 . ? O1W H1WB 0.8492 . ? N19 C17 1.353(4) . ? N19 C20 1.422(4) . ? C14 H14 0.9300 . ? C14 C13 1.373(5) . ? C14 C15 1.381(4) . ? O18 C17 1.226(4) . ? C30 H30 0.9300 . ? C30 C29 1.380(5) . ? N22 C0AA 1.482(5) . ? N22 C21 1.348(4) . ? N22 C23 1.340(5) . ? C17 C15 1.503(5) . ? N2 C7 1.346(4) . ? N2 C3 1.341(4) . ? N2 C1 1.486(4) . ? C34 C36 1.511(4) . ? C36 C37 1.379(4) . ? C36 N41 1.344(4) . ? C014 C01F 1.374(5) . ? C014 C01P 1.389(5) . ? C7 H7 0.9300 . ? C7 C6 1.385(4) . ? O2W H2WA 0.9345 . ? O2W H2WB 0.95(4) . ? C6 C5 1.388(5) . ? C019 H01A 0.9600 . ? C019 H01B 0.9600 . ? C019 H01C 0.9600 . ? C13 H13 0.9300 . ? C13 C12 1.397(5) . ? C37 H37 0.9300 . ? C37 C38 1.390(5) . ? C4 H4 0.9300 . ? C4 C3 1.375(5) . ? C4 C5 1.376(5) . ? C38 H38 0.9300 . ? C38 C39 1.389(5) . ? C01F H01F 0.9300 . ? C0AA H0AA 0.9600 . ? C0AA H0AB 0.9600 . ? C0AA H0AC 0.9600 . ? C28 H28 0.9300 . ? C28 C29 1.362(5) . ? C01I H01I 0.9300 . ? C01I C01U 1.369(5) . ? C29 H29 0.9300 . ? C3 H3 0.9300 . ? C11 C9 1.505(5) . ? C11 C12 1.386(4) . ? C11 N16 1.333(4) . ? C42 C40 1.501(4) . ? C15 N16 1.336(4) . ? C01P H01P 0.9300 . ? C01P C01U 1.380(5) . ? C40 C39 1.390(4) . ? C40 N41 1.335(4) . ? C5 H5 0.9300 . ? C25 H25 0.9300 . ? C25 C20 1.386(5) . ? C25 C24 1.375(5) . ? C01U H01U 0.9300 . ? C21 H21 0.9300 . ? C21 C20 1.380(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C12 H12 0.9300 . ? C39 H39 0.9300 . ? C23 H23 0.9300 . ? C23 C24 1.372(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C24 H24 0.9300 . ?