#------------------------------------------------------------------------------ #$Date: 2016-03-05 10:48:12 +0200 (Sat, 05 Mar 2016) $ #$Revision: 177722 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/18/1541893.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_1541893 loop_ _publ_author_name 'Liu, Liu' 'Ruiz, David A.' 'Dahcheh, Fatme' 'Bertrand, Guy' 'Suter, Riccardo' 'Tondreau, Aaron M.' 'Gr\"utzmacher, Hansj\"org' _publ_section_title ; Isolation of Au-, Co-\h1PCO and Cu-\h2PCO complexes, conversion of an Ir--\h1PCO complex into a dimetalladiphosphene, and an interaction-free PCO anion ; _journal_issue 3 _journal_name_full 'Chem. Sci.' _journal_page_first 2335 _journal_paper_doi 10.1039/C5SC04504E _journal_volume 7 _journal_year 2016 _chemical_formula_moiety 'C34 H43 Co N3 O P, 2(C4 H8 O)' _chemical_formula_sum 'C42 H59 Co N3 O3 P' _chemical_formula_weight 743.82 _chemical_name_systematic iPr(PDI)Co(PCO) _chemical_properties_physical 'Air-sensitive, Heat-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2015-08-12 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2015-08-12 deposited with the CCDC. 2016-01-04 downloaded from the CCDC. ; _cell_angle_alpha 111.476(4) _cell_angle_beta 93.948(4) _cell_angle_gamma 104.766(4) _cell_formula_units_Z 2 _cell_length_a 10.1044(5) _cell_length_b 14.1614(7) _cell_length_c 15.8020(7) _cell_measurement_reflns_used 7587 _cell_measurement_temperature 105(2) _cell_measurement_theta_max 28.8370 _cell_measurement_theta_min 3.1910 _cell_volume 2001.36(19) _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 105(2) _diffrn_detector 'Oxford Diffraction Sapphire 3' _diffrn_detector_area_resol_mean 8.26 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; 1 omega -11.00 14.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -21.7904 -99.0000 -90.0000 25 2 omega -21.00 20.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -21.7904 -99.0000 60.0000 41 3 omega -98.00 -34.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -21.7904 -179.0000 -90.0000 64 4 omega 1.00 28.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 38.0000 90.0000 27 5 omega 21.00 67.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 57.0000 -120.0000 46 6 omega 41.00 94.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 38.0000 90.0000 53 7 omega -24.00 7.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 -57.0000 150.0000 31 8 omega -44.00 -4.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 -77.0000 150.0000 40 9 omega 13.00 52.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 -77.0000 150.0000 39 10 omega 6.00 88.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 57.0000 -60.0000 82 11 omega -52.00 5.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -21.7904 77.0000 -90.0000 57 12 omega -47.00 44.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 -57.0000 60.0000 91 13 omega 1.00 91.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 57.0000 30.0000 90 14 omega 34.00 98.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 179.0000 0.0000 64 15 omega 1.00 91.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 22.2592 57.0000 -180.0000 90 ; _diffrn_measurement_device 'kappa-stage diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S' _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_UB_11 -0.0329899000 _diffrn_orient_matrix_UB_12 -0.0357930000 _diffrn_orient_matrix_UB_13 0.0193599000 _diffrn_orient_matrix_UB_21 -0.0615107000 _diffrn_orient_matrix_UB_22 -0.0169284000 _diffrn_orient_matrix_UB_23 -0.0329665000 _diffrn_orient_matrix_UB_31 0.0239754000 _diffrn_orient_matrix_UB_32 -0.0402437000 _diffrn_orient_matrix_UB_33 -0.0307127000 _diffrn_radiation_monochromator 'focusing graphite' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_unetI/netI 0.0758 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 30723 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_min 2.788 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.234 _exptl_crystal_description block _exptl_crystal_F_000 796 _exptl_crystal_preparation 'Na(OCP) and (iPrPDI)CoCl in thf' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf hexanes' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.588 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 508 _refine_ls_number_reflns 8175 _refine_ls_number_restraints 70 _refine_ls_restrained_S_all 1.160 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0712 _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^)+(0.0380P)^2^+1.8930P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1356 _refine_ls_wR_factor_ref 0.1417 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7094 _reflns_number_total 8175 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04504e2.cif _cod_data_source_block mepdiirpco2 _cod_depositor_comments 'Adding full bibliography for 1541885--1541894.cif.' _cod_original_cell_volume 2001.36(18) _cod_database_code 1541893 _chemical_oxdiff_formula Co1P1C50H50N2 _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. ; _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C44-C43 = C42-C41 = C41-C40 = C40-C39 = C46-C45 = C46-C43 1.48721 with sigma of 0.001 O3-C42 = O3-C39 = O4-C44 = O4-C45 1.48721 with sigma of 0.001 3. Rigid body (RIGU) restrains C44, C43, C46, C45, O4 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O3, C39, C40, C41, C42 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)= Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(O4)=1-FVAR(1) Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)= Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(O3)=FVAR(1) 1(DFIX)=1(DFIX)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C19(H19), C16(H16), C31(H31), C28(H28) 5.b Secondary CH2 refined with riding coordinates: C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A, H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B) 5.c Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C14(H14), C13(H13), C12(H12), C26(H26), C25(H25), C24(H24) 5.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C33(H33A,H33B, H33C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C) ; _shelx_res_file ; exp_3173.res created by SHELXL-2014/7 TITL exp_3173_a.res in P-1 REM Old TITL exp_3173 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.171, Rweak 0.037, Alpha 0.103, Orientation as input REM Formula found by SHELXT: C42 N5 P Co CELL 0.71073 10.104442 14.161442 15.80201 111.4761 93.9479 104.7663 ZERR 2 0.000484 0.000673 0.00071 0.0044 0.004 0.0042 LATT 1 SFAC C H Co N O P UNIT 84 118 2 6 6 2 DFIX 31 0.001 C44 C43 C42 C41 C41 C40 C40 C39 C46 C45 C46 C43 DFIX 31 0.001 O3 C42 O3 C39 O4 C44 O4 C45 RIGU C44 C43 C46 C45 O4 RIGU O3 C39 C40 C41 C42 L.S. 50 0 0 PLAN 20 FREE C42 C39 BOND $H LIST 6 MORE -1 CONF fmap 2 53 acta 52 SHEL 999 0.8 REM REM REM WGHT 0.038000 1.893000 FVAR 0.47740 0.52298 1.48721 C34 1 0.918783 0.424970 0.748592 11.00000 0.01985 0.04859 = 0.02667 0.00997 0.00999 0.01638 C3 1 0.335697 0.332183 0.675746 11.00000 0.01870 0.01913 = 0.02244 0.01189 0.00977 0.00785 C4 1 0.191420 0.306159 0.657709 11.00000 0.02037 0.02382 = 0.02622 0.01152 0.01112 0.00780 AFIX 43 H4 2 0.143158 0.330878 0.705023 11.00000 -1.20000 AFIX 0 C5 1 0.120171 0.242482 0.567682 11.00000 0.01385 0.02485 = 0.03185 0.01223 0.00396 0.00519 AFIX 43 H5 2 0.023588 0.223664 0.555086 11.00000 -1.20000 AFIX 0 C6 1 0.191827 0.207116 0.497049 11.00000 0.01976 0.02129 = 0.02418 0.01071 0.00348 0.00521 AFIX 43 H6 2 0.144292 0.164776 0.436979 11.00000 -1.20000 AFIX 0 C7 1 0.336462 0.235899 0.517249 11.00000 0.01841 0.01488 = 0.02190 0.00867 0.00509 0.00675 C2 1 0.431336 0.396412 0.761678 11.00000 0.02112 0.02233 = 0.02157 0.01052 0.00781 0.00961 C1 1 0.381862 0.448520 0.849139 11.00000 0.02450 0.03357 = 0.02360 0.00680 0.00920 0.00927 AFIX 137 H1A 2 0.331223 0.395072 0.868479 11.00000 -1.50000 H1B 2 0.322202 0.487595 0.838545 11.00000 -1.50000 H1C 2 0.460432 0.496311 0.896482 11.00000 -1.50000 AFIX 0 C8 1 0.433915 0.213276 0.456183 11.00000 0.01925 0.01559 = 0.02027 0.00885 0.00493 0.00367 C9 1 0.387440 0.151047 0.354089 11.00000 0.02108 0.02592 = 0.02270 0.00853 0.00319 0.00383 AFIX 137 H9A 2 0.466339 0.157911 0.323779 11.00000 -1.50000 H9B 2 0.321163 0.177942 0.331221 11.00000 -1.50000 H9C 2 0.345030 0.077406 0.341834 11.00000 -1.50000 AFIX 0 C10 1 0.666151 0.460973 0.837543 11.00000 0.01774 0.02532 = 0.01780 0.00644 0.00806 0.00880 C15 1 0.732678 0.570104 0.863193 11.00000 0.01982 0.03001 = 0.02364 0.00931 0.01038 0.00786 C14 1 0.831742 0.622474 0.944124 11.00000 0.02463 0.02478 = 0.02813 0.00369 0.00576 0.00388 AFIX 43 H14 2 0.877576 0.694613 0.962681 11.00000 -1.20000 AFIX 0 C13 1 0.863958 0.570171 0.997775 11.00000 0.02558 0.04063 = 0.01975 0.00532 0.00301 0.01329 AFIX 43 H13 2 0.929911 0.607105 1.051871 11.00000 -1.20000 AFIX 0 C12 1 0.797574 0.462902 0.970456 11.00000 0.02906 0.03801 = 0.02115 0.01245 0.00877 0.01666 AFIX 43 H12 2 0.819399 0.428110 1.006738 11.00000 -1.20000 AFIX 0 C11 1 0.698092 0.405366 0.889295 11.00000 0.02602 0.03263 = 0.01787 0.00840 0.00708 0.01145 C19 1 0.628311 0.286844 0.859807 11.00000 0.03870 0.03198 = 0.02595 0.01433 0.00075 0.00885 AFIX 13 H19 2 0.567614 0.260768 0.799773 11.00000 -1.20000 AFIX 0 C20 1 0.537525 0.264817 0.927975 11.00000 0.04512 0.04562 = 0.06447 0.03178 0.01579 0.01207 AFIX 137 H20A 2 0.595080 0.286985 0.986879 11.00000 -1.50000 H20B 2 0.489542 0.190012 0.905090 11.00000 -1.50000 H20C 2 0.470922 0.303617 0.934779 11.00000 -1.50000 AFIX 0 C21 1 0.735525 0.225889 0.847418 11.00000 0.05830 0.03398 = 0.04447 0.01801 0.01389 0.02078 AFIX 137 H21A 2 0.787907 0.237440 0.801788 11.00000 -1.50000 H21B 2 0.688577 0.151253 0.827522 11.00000 -1.50000 H21C 2 0.797386 0.250716 0.905168 11.00000 -1.50000 AFIX 0 C16 1 0.700326 0.629213 0.805893 11.00000 0.02492 0.02388 = 0.02933 0.01028 0.00245 0.00128 AFIX 13 H16 2 0.628938 0.578523 0.752253 11.00000 -1.20000 AFIX 0 C18 1 0.642746 0.718276 0.859589 11.00000 0.06965 0.06963 = 0.05067 0.03730 0.03045 0.04839 AFIX 137 H18A 2 0.561935 0.689622 0.881351 11.00000 -1.50000 H18B 2 0.617721 0.751049 0.819989 11.00000 -1.50000 H18C 2 0.712193 0.770442 0.911360 11.00000 -1.50000 AFIX 0 C17 1 0.828210 0.674380 0.770074 11.00000 0.05445 0.05669 = 0.06348 0.04198 0.03152 0.02660 AFIX 137 H17A 2 0.897814 0.727402 0.821335 11.00000 -1.50000 H17B 2 0.802103 0.705994 0.729765 11.00000 -1.50000 H17C 2 0.864904 0.618066 0.736660 11.00000 -1.50000 AFIX 0 C22 1 0.673158 0.242399 0.445140 11.00000 0.01418 0.02187 = 0.01583 0.00875 0.00388 0.00405 C27 1 0.714321 0.149964 0.420266 11.00000 0.01929 0.02154 = 0.01914 0.00804 0.00355 0.00484 C26 1 0.824849 0.145758 0.372411 11.00000 0.02296 0.02677 = 0.02273 0.00656 0.00837 0.00927 AFIX 43 H26 2 0.855199 0.085776 0.355546 11.00000 -1.20000 AFIX 0 C25 1 0.890360 0.229404 0.349500 11.00000 0.02026 0.03724 = 0.02415 0.01212 0.01262 0.00642 AFIX 43 H25 2 0.964177 0.225312 0.317678 11.00000 -1.20000 AFIX 0 C24 1 0.846133 0.318881 0.373882 11.00000 0.02379 0.02807 = 0.02244 0.01466 0.00820 0.00184 AFIX 43 H24 2 0.889954 0.374207 0.357473 11.00000 -1.20000 AFIX 0 C23 1 0.737398 0.327635 0.422460 11.00000 0.02049 0.02177 = 0.01550 0.00755 0.00050 0.00192 C31 1 0.691949 0.427289 0.451443 11.00000 0.02665 0.02368 = 0.03602 0.01692 0.00932 0.00722 AFIX 13 H31 2 0.635160 0.426049 0.499086 11.00000 -1.20000 AFIX 0 C32 1 0.601217 0.428358 0.371288 11.00000 0.05598 0.03499 = 0.06868 0.02198 -0.01864 0.01265 AFIX 137 H32A 2 0.654166 0.430072 0.323417 11.00000 -1.50000 H32B 2 0.569802 0.490209 0.392367 11.00000 -1.50000 H32C 2 0.522329 0.365468 0.347410 11.00000 -1.50000 AFIX 0 C33 1 0.813808 0.529188 0.493520 11.00000 0.04020 0.02072 = 0.05161 0.01345 0.00307 0.00667 AFIX 137 H33A 2 0.871921 0.526546 0.542776 11.00000 -1.50000 H33B 2 0.779274 0.589230 0.517406 11.00000 -1.50000 H33C 2 0.867041 0.536018 0.446900 11.00000 -1.50000 AFIX 0 C28 1 0.645515 0.057518 0.445279 11.00000 0.02235 0.02248 = 0.02887 0.01231 0.01271 0.00771 AFIX 13 H28 2 0.564886 0.072142 0.472477 11.00000 -1.20000 AFIX 0 C29 1 0.592415 -0.047877 0.360549 11.00000 0.03922 0.02402 = 0.03574 0.00897 0.01059 0.00319 AFIX 137 H29A 2 0.532343 -0.040435 0.315177 11.00000 -1.50000 H29B 2 0.541649 -0.102577 0.378478 11.00000 -1.50000 H29C 2 0.669914 -0.066792 0.334794 11.00000 -1.50000 AFIX 0 C30 1 0.743607 0.048819 0.517877 11.00000 0.03360 0.02972 = 0.03766 0.02094 0.00814 0.00808 AFIX 137 H30A 2 0.825955 0.037950 0.494235 11.00000 -1.50000 H30B 2 0.698019 -0.010217 0.532347 11.00000 -1.50000 H30C 2 0.768635 0.113246 0.572777 11.00000 -1.50000 AFIX 0 N2 4 0.407262 0.297116 0.606241 11.00000 0.01503 0.01729 = 0.01963 0.00904 0.00807 0.00524 N3 4 0.564384 0.253618 0.499432 11.00000 0.01865 0.01828 = 0.02022 0.01059 0.00766 0.00818 N1 4 0.562682 0.403096 0.753561 11.00000 0.01744 0.02015 = 0.01664 0.00704 0.00349 0.00525 O1 5 1.001333 0.470876 0.817124 11.00000 0.03008 0.09991 = 0.02682 0.00015 -0.00035 0.02378 P1 6 0.827177 0.357480 0.644459 11.00000 0.01745 0.04868 = 0.02066 0.00424 0.00514 0.01154 CO1 3 0.595049 0.332036 0.631257 11.00000 0.01330 0.01946 = 0.01574 0.00705 0.00523 0.00554 C35 1 -0.009416 -0.087479 0.279248 11.00000 0.06431 0.05439 = 0.04300 0.01897 0.01775 0.03417 AFIX 23 H35A 2 -0.055903 -0.081927 0.331790 11.00000 -1.20000 H35B 2 0.061443 -0.121862 0.282064 11.00000 -1.20000 AFIX 0 C36 1 -0.111458 -0.148667 0.190668 11.00000 0.06741 0.04008 = 0.05085 -0.00021 0.01778 -0.00028 AFIX 23 H36A 2 -0.201382 -0.137094 0.197586 11.00000 -1.20000 H36B 2 -0.122893 -0.224292 0.169216 11.00000 -1.20000 AFIX 0 C37 1 -0.044623 -0.103070 0.124780 11.00000 0.06118 0.04525 = 0.03722 0.00624 -0.00057 0.01303 AFIX 23 H37A 2 0.017432 -0.141328 0.094443 11.00000 -1.20000 H37B 2 -0.114452 -0.105170 0.078265 11.00000 -1.20000 AFIX 0 C38 1 0.033847 0.008868 0.188244 11.00000 0.08216 0.04657 = 0.03595 0.00874 0.01067 0.00725 AFIX 23 H38A 2 0.124145 0.029726 0.171642 11.00000 -1.20000 H38B 2 -0.016930 0.056751 0.183177 11.00000 -1.20000 AFIX 0 O2 5 0.050469 0.014758 0.279020 11.00000 0.03542 0.05163 = 0.02967 0.00039 0.00463 -0.00018 PART 1 C39 1 0.643702 0.158757 0.130691 21.00000 0.02735 0.05429 = 0.02361 -0.00036 0.00441 0.02045 AFIX 23 H39A 2 0.569902 0.163073 0.090957 21.00000 -1.20000 H39B 2 0.653731 0.210823 0.193042 21.00000 -1.20000 AFIX 0 C40 1 0.776855 0.175042 0.095435 21.00000 0.04595 0.09282 = 0.05020 0.03746 0.01898 0.03079 AFIX 23 H40A 2 0.782094 0.221968 0.063059 21.00000 -1.20000 H40B 2 0.855514 0.206124 0.146017 21.00000 -1.20000 AFIX 0 C41 1 0.776974 0.067677 0.031338 21.00000 0.06040 0.08616 = 0.03897 0.02402 0.00832 0.03575 AFIX 23 H41A 2 0.747329 0.057018 -0.032055 21.00000 -1.20000 H41B 2 0.870079 0.061179 0.037413 21.00000 -1.20000 AFIX 0 C42 1 0.679951 -0.013402 0.054995 21.00000 0.05823 0.04185 = 0.03792 0.00434 0.01165 0.02629 AFIX 23 H42A 2 0.729857 -0.052144 0.077496 21.00000 -1.20000 H42B 2 0.609819 -0.063598 0.001612 21.00000 -1.20000 AFIX 0 O3 5 0.615665 0.049527 0.128665 21.00000 0.13568 0.09728 = 0.10727 0.04137 0.05924 0.04459 PART 0 PART 2 C43 1 0.683880 0.042166 0.089750 -21.00000 0.07733 0.09175 = 0.05277 0.02888 0.01824 0.03531 AFIX 23 H43A 2 0.743603 0.038208 0.138302 -21.00000 -1.20000 H43B 2 0.599018 -0.017220 0.068082 -21.00000 -1.20000 AFIX 0 C44 1 0.756339 0.053354 0.013613 -21.00000 0.08951 0.08660 = 0.04835 0.01502 0.01392 0.03303 AFIX 23 H44A 2 0.690017 0.040348 -0.039805 -21.00000 -1.20000 H44B 2 0.810275 0.003812 -0.004681 -21.00000 -1.20000 AFIX 0 C45 1 0.780542 0.233144 0.119707 -21.00000 0.10730 0.08302 = 0.05106 0.02105 0.01165 0.04243 AFIX 23 H45A 2 0.754529 0.283197 0.098483 -21.00000 -1.20000 H45B 2 0.837863 0.270985 0.180814 -21.00000 -1.20000 AFIX 0 C46 1 0.657436 0.147040 0.116678 -21.00000 0.10478 0.09626 = 0.06290 0.03163 0.02169 0.04022 AFIX 23 H46A 2 0.580192 0.140684 0.072858 -21.00000 -1.20000 H46B 2 0.630760 0.166421 0.177101 -21.00000 -1.20000 AFIX 0 O4 5 0.848757 0.165191 0.052839 -21.00000 0.10709 0.08203 = 0.07154 0.00840 0.02847 0.02280 HKLF 4 REM exp_3173_a.res in P-1 REM R1 = 0.0712 for 7094 Fo > 4sig(Fo) and 0.0852 for all 8175 data REM 508 parameters refined using 70 restraints END WGHT 0.0382 1.8584 REM Highest difference peak 0.588, deepest hole -0.518, 1-sigma level 0.070 Q1 1 0.5586 0.2611 0.5829 11.00000 0.05 0.59 Q2 1 0.6926 0.3283 0.6339 11.00000 0.05 0.54 Q3 1 0.4195 -0.0577 0.2751 11.00000 0.05 0.50 Q4 1 0.5149 0.3553 0.6447 11.00000 0.05 0.50 Q5 1 0.5972 0.3867 0.5955 11.00000 0.05 0.47 Q6 1 -0.1435 -0.0970 0.1483 11.00000 0.05 0.47 Q7 1 0.5748 0.2766 0.6630 11.00000 0.05 0.43 Q8 1 0.6380 0.3945 0.6907 11.00000 0.05 0.42 Q9 1 0.7372 0.3808 0.6455 11.00000 0.05 0.42 Q10 1 0.7150 0.3785 0.4421 11.00000 0.05 0.37 Q11 1 0.6226 -0.0018 0.0436 11.00000 0.05 0.35 Q12 1 0.5824 0.5867 0.5344 11.00000 0.05 0.31 Q13 1 0.6950 0.2801 0.4209 11.00000 0.05 0.31 Q14 1 0.5582 0.4004 0.6805 11.00000 0.05 0.30 Q15 1 0.7125 0.0177 0.0403 11.00000 0.05 0.30 Q16 1 0.6907 0.0606 0.2026 11.00000 0.05 0.29 Q17 1 0.7143 0.6053 0.8408 11.00000 0.05 0.29 Q18 1 0.6861 0.1051 0.4343 11.00000 0.05 0.28 Q19 1 0.8715 0.3746 0.6986 11.00000 0.05 0.27 Q20 1 0.4029 0.1954 0.3256 11.00000 0.05 0.27 ; _shelx_res_checksum 57416 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C34 C 0.9188(4) 0.4250(3) 0.7486(3) 0.0317(8) Uani 1 1 d . . . . . C3 C 0.3357(3) 0.3322(2) 0.6757(2) 0.0183(7) Uani 1 1 d . . . . . C4 C 0.1914(3) 0.3062(2) 0.6577(2) 0.0224(7) Uani 1 1 d . . . . . H4 H 0.1432 0.3309 0.7050 0.027 Uiso 1 1 calc R . . . . C5 C 0.1202(3) 0.2425(2) 0.5677(2) 0.0234(7) Uani 1 1 d . . . . . H5 H 0.0236 0.2237 0.5551 0.028 Uiso 1 1 calc R . . . . C6 C 0.1918(3) 0.2071(2) 0.4970(2) 0.0215(7) Uani 1 1 d . . . . . H6 H 0.1443 0.1648 0.4370 0.026 Uiso 1 1 calc R . . . . C7 C 0.3365(3) 0.2359(2) 0.5172(2) 0.0176(6) Uani 1 1 d . . . . . C2 C 0.4313(3) 0.3964(2) 0.7617(2) 0.0203(7) Uani 1 1 d . . . . . C1 C 0.3819(3) 0.4485(3) 0.8491(2) 0.0282(8) Uani 1 1 d . . . . . H1A H 0.3312 0.3951 0.8685 0.042 Uiso 1 1 calc GR . . . . H1B H 0.3222 0.4876 0.8385 0.042 Uiso 1 1 calc GR . . . . H1C H 0.4604 0.4963 0.8965 0.042 Uiso 1 1 calc GR . . . . C8 C 0.4339(3) 0.2133(2) 0.4562(2) 0.0181(6) Uani 1 1 d . . . . . C9 C 0.3874(3) 0.1510(3) 0.3541(2) 0.0243(7) Uani 1 1 d . . . . . H9A H 0.4663 0.1579 0.3238 0.036 Uiso 1 1 calc GR . . . . H9B H 0.3212 0.1779 0.3312 0.036 Uiso 1 1 calc GR . . . . H9C H 0.3450 0.0774 0.3418 0.036 Uiso 1 1 calc GR . . . . C10 C 0.6662(3) 0.4610(2) 0.8375(2) 0.0202(7) Uani 1 1 d . . . . . C15 C 0.7327(3) 0.5701(3) 0.8632(2) 0.0245(7) Uani 1 1 d . . . . . C14 C 0.8317(3) 0.6225(3) 0.9441(2) 0.0286(8) Uani 1 1 d . . . . . H14 H 0.8776 0.6946 0.9627 0.034 Uiso 1 1 calc R . . . . C13 C 0.8640(4) 0.5702(3) 0.9978(2) 0.0301(8) Uani 1 1 d . . . . . H13 H 0.9299 0.6071 1.0519 0.036 Uiso 1 1 calc R . . . . C12 C 0.7976(3) 0.4629(3) 0.9705(2) 0.0277(8) Uani 1 1 d . . . . . H12 H 0.8194 0.4281 1.0067 0.033 Uiso 1 1 calc R . . . . C11 C 0.6981(3) 0.4054(3) 0.8893(2) 0.0253(7) Uani 1 1 d . . . . . C19 C 0.6283(4) 0.2868(3) 0.8598(3) 0.0320(8) Uani 1 1 d . . . . . H19 H 0.5676 0.2608 0.7998 0.038 Uiso 1 1 calc R . . . . C20 C 0.5375(4) 0.2648(3) 0.9280(3) 0.0488(11) Uani 1 1 d . . . . . H20A H 0.5951 0.2870 0.9869 0.073 Uiso 1 1 calc GR . . . . H20B H 0.4895 0.1900 0.9051 0.073 Uiso 1 1 calc GR . . . . H20C H 0.4709 0.3036 0.9348 0.073 Uiso 1 1 calc GR . . . . C21 C 0.7355(4) 0.2259(3) 0.8474(3) 0.0432(10) Uani 1 1 d . . . . . H21A H 0.7879 0.2374 0.8018 0.065 Uiso 1 1 calc GR . . . . H21B H 0.6886 0.1513 0.8275 0.065 Uiso 1 1 calc GR . . . . H21C H 0.7974 0.2507 0.9052 0.065 Uiso 1 1 calc GR . . . . C16 C 0.7003(3) 0.6292(3) 0.8059(2) 0.0275(8) Uani 1 1 d . . . . . H16 H 0.6289 0.5785 0.7523 0.033 Uiso 1 1 calc R . . . . C18 C 0.6427(5) 0.7183(4) 0.8596(3) 0.0527(12) Uani 1 1 d . . . . . H18A H 0.5619 0.6896 0.8814 0.079 Uiso 1 1 calc GR . . . . H18B H 0.6177 0.7510 0.8200 0.079 Uiso 1 1 calc GR . . . . H18C H 0.7122 0.7704 0.9114 0.079 Uiso 1 1 calc GR . . . . C17 C 0.8282(5) 0.6744(3) 0.7701(3) 0.0497(12) Uani 1 1 d . . . . . H17A H 0.8978 0.7274 0.8213 0.075 Uiso 1 1 calc GR . . . . H17B H 0.8021 0.7060 0.7298 0.075 Uiso 1 1 calc GR . . . . H17C H 0.8649 0.6181 0.7367 0.075 Uiso 1 1 calc GR . . . . C22 C 0.6732(3) 0.2424(2) 0.4451(2) 0.0171(6) Uani 1 1 d . . . . . C27 C 0.7143(3) 0.1500(2) 0.4203(2) 0.0203(7) Uani 1 1 d . . . . . C26 C 0.8248(3) 0.1458(3) 0.3724(2) 0.0246(7) Uani 1 1 d . . . . . H26 H 0.8552 0.0858 0.3555 0.029 Uiso 1 1 calc R . . . . C25 C 0.8904(3) 0.2294(3) 0.3495(2) 0.0272(8) Uani 1 1 d . . . . . H25 H 0.9642 0.2253 0.3177 0.033 Uiso 1 1 calc R . . . . C24 C 0.8461(3) 0.3189(3) 0.3739(2) 0.0244(7) Uani 1 1 d . . . . . H24 H 0.8900 0.3742 0.3575 0.029 Uiso 1 1 calc R . . . . C23 C 0.7374(3) 0.3276(2) 0.4225(2) 0.0203(7) Uani 1 1 d . . . . . C31 C 0.6919(3) 0.4273(3) 0.4514(3) 0.0271(8) Uani 1 1 d . . . . . H31 H 0.6352 0.4260 0.4991 0.033 Uiso 1 1 calc R . . . . C32 C 0.6012(5) 0.4284(3) 0.3713(3) 0.0546(13) Uani 1 1 d . . . . . H32A H 0.6542 0.4301 0.3234 0.082 Uiso 1 1 calc GR . . . . H32B H 0.5698 0.4902 0.3924 0.082 Uiso 1 1 calc GR . . . . H32C H 0.5223 0.3655 0.3474 0.082 Uiso 1 1 calc GR . . . . C33 C 0.8138(4) 0.5292(3) 0.4935(3) 0.0386(10) Uani 1 1 d . . . . . H33A H 0.8719 0.5265 0.5428 0.058 Uiso 1 1 calc GR . . . . H33B H 0.7793 0.5892 0.5174 0.058 Uiso 1 1 calc GR . . . . H33C H 0.8670 0.5360 0.4469 0.058 Uiso 1 1 calc GR . . . . C28 C 0.6455(3) 0.0575(2) 0.4453(2) 0.0233(7) Uani 1 1 d . . . . . H28 H 0.5649 0.0721 0.4725 0.028 Uiso 1 1 calc R . . . . C29 C 0.5924(4) -0.0479(3) 0.3605(3) 0.0349(9) Uani 1 1 d . . . . . H29A H 0.5323 -0.0404 0.3152 0.052 Uiso 1 1 calc GR . . . . H29B H 0.5416 -0.1026 0.3785 0.052 Uiso 1 1 calc GR . . . . H29C H 0.6699 -0.0668 0.3348 0.052 Uiso 1 1 calc GR . . . . C30 C 0.7436(4) 0.0488(3) 0.5179(3) 0.0316(8) Uani 1 1 d . . . . . H30A H 0.8260 0.0379 0.4942 0.047 Uiso 1 1 calc GR . . . . H30B H 0.6980 -0.0102 0.5323 0.047 Uiso 1 1 calc GR . . . . H30C H 0.7686 0.1132 0.5728 0.047 Uiso 1 1 calc GR . . . . N2 N 0.4073(2) 0.29712(19) 0.60624(17) 0.0165(5) Uani 1 1 d . . . . . N3 N 0.5644(3) 0.25362(19) 0.49943(18) 0.0174(6) Uani 1 1 d . . . . . N1 N 0.5627(3) 0.40310(19) 0.75356(17) 0.0182(6) Uani 1 1 d . . . . . O1 O 1.0013(3) 0.4709(3) 0.81712(19) 0.0592(9) Uani 1 1 d . . . . . P1 P 0.82718(9) 0.35748(8) 0.64446(6) 0.0314(2) Uani 1 1 d . . . . . Co1 Co 0.59505(4) 0.33204(3) 0.63126(3) 0.01589(12) Uani 1 1 d . . . . . C35 C -0.0094(5) -0.0875(3) 0.2792(3) 0.0503(11) Uani 1 1 d . . . . . H35A H -0.0559 -0.0819 0.3318 0.060 Uiso 1 1 calc R . . . . H35B H 0.0614 -0.1219 0.2821 0.060 Uiso 1 1 calc R . . . . C36 C -0.1115(5) -0.1487(4) 0.1907(3) 0.0612(14) Uani 1 1 d . . . . . H36A H -0.2014 -0.1371 0.1976 0.073 Uiso 1 1 calc R . . . . H36B H -0.1229 -0.2243 0.1692 0.073 Uiso 1 1 calc R . . . . C37 C -0.0446(5) -0.1031(3) 0.1248(3) 0.0520(12) Uani 1 1 d . . . . . H37A H 0.0174 -0.1413 0.0944 0.062 Uiso 1 1 calc R . . . . H37B H -0.1145 -0.1052 0.0783 0.062 Uiso 1 1 calc R . . . . C38 C 0.0338(6) 0.0089(4) 0.1882(3) 0.0596(13) Uani 1 1 d . . . . . H38A H 0.1241 0.0297 0.1716 0.072 Uiso 1 1 calc R . . . . H38B H -0.0169 0.0568 0.1832 0.072 Uiso 1 1 calc R . . . . O2 O 0.0505(3) 0.0148(2) 0.27902(18) 0.0464(7) Uani 1 1 d . . . . . C39 C 0.6437(9) 0.1588(6) 0.1307(9) 0.038(3) Uani 0.523(8) 1 d D U P A 1 H39A H 0.5699 0.1631 0.0910 0.046 Uiso 0.523(8) 1 calc R . P A 1 H39B H 0.6537 0.2108 0.1930 0.046 Uiso 0.523(8) 1 calc R . P A 1 C40 C 0.7769(9) 0.1750(8) 0.0954(7) 0.058(3) Uani 0.523(8) 1 d D U P A 1 H40A H 0.7821 0.2220 0.0631 0.069 Uiso 0.523(8) 1 calc R . P A 1 H40B H 0.8555 0.2061 0.1460 0.069 Uiso 0.523(8) 1 calc R . P A 1 C41 C 0.7770(19) 0.0677(7) 0.0313(10) 0.059(4) Uani 0.523(8) 1 d D U P A 1 H41A H 0.7473 0.0570 -0.0321 0.071 Uiso 0.523(8) 1 calc R . P A 1 H41B H 0.8701 0.0612 0.0374 0.071 Uiso 0.523(8) 1 calc R . P A 1 C42 C 0.6800(9) -0.0134(6) 0.0550(6) 0.047(3) Uani 0.523(8) 1 d D U P A 1 H42A H 0.7299 -0.0521 0.0775 0.056 Uiso 0.523(8) 1 calc R . P A 1 H42B H 0.6098 -0.0636 0.0016 0.056 Uiso 0.523(8) 1 calc R . P A 1 O3 O 0.6157(10) 0.0495(6) 0.1287(6) 0.109(4) Uani 0.523(8) 1 d D U P A 1 C43 C 0.6839(13) 0.0422(10) 0.0897(8) 0.072(4) Uani 0.477(8) 1 d D U P A 2 H43A H 0.7436 0.0382 0.1383 0.086 Uiso 0.477(8) 1 calc R . P A 2 H43B H 0.5990 -0.0172 0.0681 0.086 Uiso 0.477(8) 1 calc R . P A 2 C44 C 0.756(2) 0.0534(9) 0.0136(10) 0.077(6) Uani 0.477(8) 1 d D U P A 2 H44A H 0.6900 0.0403 -0.0398 0.092 Uiso 0.477(8) 1 calc R . P A 2 H44B H 0.8103 0.0038 -0.0047 0.092 Uiso 0.477(8) 1 calc R . P A 2 C45 C 0.7805(12) 0.2331(9) 0.1197(8) 0.080(4) Uani 0.477(8) 1 d D U P A 2 H45A H 0.7545 0.2832 0.0985 0.095 Uiso 0.477(8) 1 calc R . P A 2 H45B H 0.8379 0.2710 0.1808 0.095 Uiso 0.477(8) 1 calc R . P A 2 C46 C 0.6574(16) 0.1470(9) 0.1167(15) 0.086(6) Uani 0.477(8) 1 d D U P A 2 H46A H 0.5802 0.1407 0.0729 0.103 Uiso 0.477(8) 1 calc R . P A 2 H46B H 0.6308 0.1664 0.1771 0.103 Uiso 0.477(8) 1 calc R . P A 2 O4 O 0.8488(10) 0.1652(7) 0.0528(6) 0.094(3) Uani 0.477(8) 1 d 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 C34 0.0198(17) 0.049(2) 0.027(2) 0.0100(17) 0.0100(16) 0.0164(16) C3 0.0187(15) 0.0191(16) 0.0224(17) 0.0119(13) 0.0098(13) 0.0078(13) C4 0.0204(16) 0.0238(17) 0.0262(18) 0.0115(14) 0.0111(14) 0.0078(13) C5 0.0139(15) 0.0248(17) 0.0319(19) 0.0122(15) 0.0040(14) 0.0052(13) C6 0.0198(16) 0.0213(17) 0.0242(18) 0.0107(14) 0.0035(14) 0.0052(13) C7 0.0184(15) 0.0149(15) 0.0219(17) 0.0087(13) 0.0051(13) 0.0067(12) C2 0.0211(16) 0.0223(17) 0.0216(17) 0.0105(13) 0.0078(14) 0.0096(13) C1 0.0245(18) 0.034(2) 0.0236(19) 0.0068(15) 0.0092(15) 0.0093(15) C8 0.0193(15) 0.0156(15) 0.0203(17) 0.0088(13) 0.0049(13) 0.0037(12) C9 0.0211(17) 0.0259(18) 0.0227(18) 0.0085(14) 0.0032(14) 0.0038(14) C10 0.0177(15) 0.0253(17) 0.0178(16) 0.0064(13) 0.0081(13) 0.0088(13) C15 0.0198(16) 0.0300(19) 0.0236(18) 0.0093(14) 0.0104(14) 0.0079(14) C14 0.0246(18) 0.0248(18) 0.0281(19) 0.0037(15) 0.0058(15) 0.0039(14) C13 0.0256(18) 0.041(2) 0.0197(18) 0.0053(16) 0.0030(15) 0.0133(16) C12 0.0291(19) 0.038(2) 0.0212(18) 0.0125(15) 0.0088(15) 0.0167(16) C11 0.0260(17) 0.0326(19) 0.0179(17) 0.0084(14) 0.0071(14) 0.0114(15) C19 0.039(2) 0.032(2) 0.0259(19) 0.0143(16) 0.0007(17) 0.0088(17) C20 0.045(2) 0.046(3) 0.064(3) 0.032(2) 0.016(2) 0.012(2) C21 0.058(3) 0.034(2) 0.044(3) 0.0180(19) 0.014(2) 0.021(2) C16 0.0249(17) 0.0239(18) 0.0293(19) 0.0103(15) 0.0024(15) 0.0013(14) C18 0.070(3) 0.070(3) 0.051(3) 0.037(2) 0.030(2) 0.048(3) C17 0.054(3) 0.057(3) 0.063(3) 0.042(2) 0.032(2) 0.027(2) C22 0.0142(14) 0.0219(16) 0.0158(16) 0.0087(13) 0.0039(12) 0.0041(12) C27 0.0193(16) 0.0215(17) 0.0191(17) 0.0080(13) 0.0036(13) 0.0048(13) C26 0.0230(17) 0.0268(18) 0.0227(18) 0.0066(14) 0.0084(14) 0.0093(14) C25 0.0203(17) 0.037(2) 0.0242(18) 0.0121(15) 0.0126(15) 0.0064(15) C24 0.0238(17) 0.0281(18) 0.0224(18) 0.0147(14) 0.0082(14) 0.0018(14) C23 0.0205(16) 0.0218(17) 0.0155(16) 0.0075(13) 0.0005(13) 0.0019(13) C31 0.0266(18) 0.0237(18) 0.036(2) 0.0169(15) 0.0093(16) 0.0072(14) C32 0.056(3) 0.035(2) 0.069(3) 0.022(2) -0.019(2) 0.013(2) C33 0.040(2) 0.0207(19) 0.052(3) 0.0135(17) 0.0031(19) 0.0067(16) C28 0.0223(16) 0.0225(17) 0.0289(19) 0.0123(14) 0.0127(15) 0.0077(14) C29 0.039(2) 0.0240(19) 0.036(2) 0.0090(16) 0.0106(18) 0.0032(16) C30 0.034(2) 0.030(2) 0.038(2) 0.0209(17) 0.0081(17) 0.0081(16) N2 0.0150(12) 0.0173(13) 0.0196(14) 0.0090(11) 0.0081(11) 0.0052(10) N3 0.0187(13) 0.0183(13) 0.0202(14) 0.0106(11) 0.0077(11) 0.0082(11) N1 0.0174(13) 0.0202(14) 0.0166(14) 0.0070(11) 0.0035(11) 0.0052(11) O1 0.0301(15) 0.100(3) 0.0268(16) 0.0001(16) -0.0004(13) 0.0238(16) P1 0.0174(4) 0.0487(6) 0.0207(5) 0.0042(4) 0.0051(4) 0.0115(4) Co1 0.0133(2) 0.0195(2) 0.0157(2) 0.00705(17) 0.00523(16) 0.00554(16) C35 0.064(3) 0.054(3) 0.043(3) 0.019(2) 0.018(2) 0.034(2) C36 0.067(3) 0.040(3) 0.051(3) 0.000(2) 0.018(3) 0.000(2) C37 0.061(3) 0.045(3) 0.037(2) 0.006(2) -0.001(2) 0.013(2) C38 0.082(4) 0.047(3) 0.036(3) 0.009(2) 0.011(2) 0.007(2) O2 0.0354(15) 0.0516(18) 0.0297(15) 0.0004(13) 0.0046(13) -0.0002(13) C39 0.027(4) 0.054(5) 0.024(5) 0.000(4) 0.004(4) 0.020(4) C40 0.046(5) 0.093(6) 0.050(6) 0.037(5) 0.019(4) 0.031(5) C41 0.060(7) 0.086(7) 0.039(6) 0.024(5) 0.008(5) 0.036(5) C42 0.058(5) 0.042(5) 0.038(5) 0.004(4) 0.012(4) 0.026(4) O3 0.136(8) 0.097(6) 0.107(7) 0.041(5) 0.059(6) 0.045(5) C43 0.077(8) 0.092(8) 0.053(7) 0.029(6) 0.018(6) 0.035(6) C44 0.090(11) 0.087(7) 0.048(8) 0.015(5) 0.014(7) 0.033(6) C45 0.107(9) 0.083(7) 0.051(7) 0.021(6) 0.012(6) 0.042(6) C46 0.105(10) 0.096(8) 0.063(11) 0.032(7) 0.022(8) 0.040(7) O4 0.107(7) 0.082(6) 0.072(6) 0.008(4) 0.028(5) 0.023(5) 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' 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 O1 C34 P1 169.9(3) C4 C3 C2 129.3(3) N2 C3 C4 120.7(3) N2 C3 C2 110.0(3) C3 C4 H4 120.5 C3 C4 C5 119.1(3) C5 C4 H4 120.5 C4 C5 H5 119.7 C6 C5 C4 120.6(3) C6 C5 H5 119.7 C5 C6 H6 120.5 C5 C6 C7 118.9(3) C7 C6 H6 120.5 C6 C7 C8 129.5(3) N2 C7 C6 120.8(3) N2 C7 C8 109.7(3) C3 C2 C1 121.5(3) N1 C2 C3 113.0(3) N1 C2 C1 125.5(3) C2 C1 H1A 109.5 C2 C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C7 C8 C9 121.9(3) N3 C8 C7 113.1(3) N3 C8 C9 125.1(3) C8 C9 H9A 109.5 C8 C9 H9B 109.5 C8 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C15 C10 N1 119.1(3) C11 C10 C15 122.4(3) C11 C10 N1 118.5(3) C10 C15 C16 122.2(3) C14 C15 C10 117.2(3) C14 C15 C16 120.6(3) C15 C14 H14 119.1 C13 C14 C15 121.9(3) C13 C14 H14 119.1 C14 C13 H13 120.2 C12 C13 C14 119.6(3) C12 C13 H13 120.2 C13 C12 H12 119.3 C13 C12 C11 121.4(3) C11 C12 H12 119.3 C10 C11 C12 117.6(3) C10 C11 C19 122.0(3) C12 C11 C19 120.4(3) C11 C19 H19 107.7 C11 C19 C20 111.5(3) C11 C19 C21 111.2(3) C20 C19 H19 107.7 C20 C19 C21 110.7(3) C21 C19 H19 107.7 C19 C20 H20A 109.5 C19 C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C19 C21 H21A 109.5 C19 C21 H21B 109.5 C19 C21 H21C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C15 C16 H16 107.9 C15 C16 C18 111.7(3) C15 C16 C17 111.7(3) C18 C16 H16 107.9 C18 C16 C17 109.6(3) C17 C16 H16 107.9 C16 C18 H18A 109.5 C16 C18 H18B 109.5 C16 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C16 C17 H17A 109.5 C16 C17 H17B 109.5 C16 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C27 C22 N3 119.8(3) C23 C22 C27 122.4(3) C23 C22 N3 117.7(3) C22 C27 C28 122.6(3) C26 C27 C22 117.4(3) C26 C27 C28 119.9(3) C27 C26 H26 119.4 C25 C26 C27 121.1(3) C25 C26 H26 119.4 C26 C25 H25 120.0 C24 C25 C26 120.1(3) C24 C25 H25 120.0 C25 C24 H24 119.4 C25 C24 C23 121.1(3) C23 C24 H24 119.4 C22 C23 C31 121.3(3) C24 C23 C22 117.8(3) C24 C23 C31 120.9(3) C23 C31 H31 107.4 C23 C31 C32 111.3(3) C23 C31 C33 112.9(3) C32 C31 H31 107.4 C32 C31 C33 110.3(3) C33 C31 H31 107.4 C31 C32 H32A 109.5 C31 C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32B 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C31 C33 H33A 109.5 C31 C33 H33B 109.5 C31 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C27 C28 H28 107.6 C27 C28 C29 112.2(3) C27 C28 C30 111.0(3) C29 C28 H28 107.6 C30 C28 H28 107.6 C30 C28 C29 110.7(3) C28 C29 H29A 109.5 C28 C29 H29B 109.5 C28 C29 H29C 109.5 H29A C29 H29B 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C28 C30 H30A 109.5 C28 C30 H30B 109.5 C28 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C3 N2 C7 119.9(3) C3 N2 Co1 120.0(2) C7 N2 Co1 120.1(2) C8 N3 C22 118.6(3) C8 N3 Co1 116.5(2) C22 N3 Co1 124.9(2) C2 N1 C10 117.0(3) C2 N1 Co1 116.1(2) C10 N1 Co1 126.87(19) C34 P1 Co1 116.23(12) N2 Co1 N3 80.66(11) N2 Co1 N1 81.00(11) N2 Co1 P1 172.39(8) N3 Co1 P1 92.22(8) N1 Co1 N3 161.54(11) N1 Co1 P1 106.20(8) H35A C35 H35B 108.8 C36 C35 H35A 110.7 C36 C35 H35B 110.7 O2 C35 H35A 110.7 O2 C35 H35B 110.7 O2 C35 C36 105.3(4) C35 C36 H36A 111.2 C35 C36 H36B 111.2 C35 C36 C37 103.0(4) H36A C36 H36B 109.1 C37 C36 H36A 111.2 C37 C36 H36B 111.2 C36 C37 H37A 111.3 C36 C37 H37B 111.3 H37A C37 H37B 109.2 C38 C37 C36 102.4(4) C38 C37 H37A 111.3 C38 C37 H37B 111.3 C37 C38 H38A 110.0 C37 C38 H38B 110.0 H38A C38 H38B 108.4 O2 C38 C37 108.5(4) O2 C38 H38A 110.0 O2 C38 H38B 110.0 C38 O2 C35 109.9(3) H39A C39 H39B 109.1 C40 C39 H39A 111.2 C40 C39 H39B 111.2 C40 C39 O3 102.9(7) O3 C39 H39A 111.2 O3 C39 H39B 111.2 C39 C40 H40A 110.6 C39 C40 H40B 110.6 H40A C40 H40B 108.7 C41 C40 C39 105.9(9) C41 C40 H40A 110.6 C41 C40 H40B 110.6 C40 C41 H41A 110.0 C40 C41 H41B 110.0 H41A C41 H41B 108.4 C42 C41 C40 108.5(8) C42 C41 H41A 110.0 C42 C41 H41B 110.0 C41 C42 H42A 110.9 C41 C42 H42B 110.9 C41 C42 O3 104.2(7) H42A C42 H42B 108.9 O3 C42 H42A 110.9 O3 C42 H42B 110.9 C42 O3 C39 109.3(7) H43A C43 H43B 110.3 C44 C43 H43A 112.9 C44 C43 H43B 112.9 C44 C43 C46 94.0(12) C46 C43 H43A 112.9 C46 C43 H43B 112.9 C43 C44 H44A 110.8 C43 C44 H44B 110.8 C43 C44 O4 104.8(9) H44A C44 H44B 108.9 O4 C44 H44A 110.8 O4 C44 H44B 110.8 H45A C45 H45B 109.8 C46 C45 H45A 112.2 C46 C45 H45B 112.2 O4 C45 H45A 112.2 O4 C45 H45B 112.2 O4 C45 C46 97.8(10) C43 C46 H46A 109.0 C43 C46 H46B 109.0 C45 C46 C43 112.9(11) C45 C46 H46A 109.0 C45 C46 H46B 109.0 H46A C46 H46B 107.8 C45 O4 C44 108.9(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C34 O1 1.173(4) C34 P1 1.633(4) C3 C4 1.391(4) C3 C2 1.439(4) C3 N2 1.367(4) C4 H4 0.9300 C4 C5 1.394(5) C5 H5 0.9300 C5 C6 1.381(4) C6 H6 0.9300 C6 C7 1.393(4) C7 C8 1.438(4) C7 N2 1.376(4) C2 C1 1.497(4) C2 N1 1.325(4) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C8 C9 1.498(4) C8 N3 1.318(4) C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C10 C15 1.407(4) C10 C11 1.399(5) C10 N1 1.450(4) C15 C14 1.392(5) C15 C16 1.510(5) C14 H14 0.9300 C14 C13 1.385(5) C13 H13 0.9300 C13 C12 1.380(5) C12 H12 0.9300 C12 C11 1.400(5) C11 C19 1.520(5) C19 H19 0.9800 C19 C20 1.528(5) C19 C21 1.529(5) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C16 H16 0.9800 C16 C18 1.519(5) C16 C17 1.531(5) C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C22 C27 1.402(4) C22 C23 1.399(4) C22 N3 1.445(4) C27 C26 1.393(4) C27 C28 1.519(4) C26 H26 0.9300 C26 C25 1.386(5) C25 H25 0.9300 C25 C24 1.382(5) C24 H24 0.9300 C24 C23 1.388(4) C23 C31 1.516(4) C31 H31 0.9800 C31 C32 1.519(5) C31 C33 1.523(5) C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C28 H28 0.9800 C28 C29 1.529(5) C28 C30 1.524(5) C29 H29A 0.9600 C29 H29B 0.9600 C29 H29C 0.9600 C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 N2 Co1 1.810(2) N3 Co1 1.926(3) N1 Co1 1.920(3) P1 Co1 2.2631(9) C35 H35A 0.9700 C35 H35B 0.9700 C35 C36 1.494(6) C35 O2 1.421(5) C36 H36A 0.9700 C36 H36B 0.9700 C36 C37 1.524(6) C37 H37A 0.9700 C37 H37B 0.9700 C37 C38 1.494(6) C38 H38A 0.9700 C38 H38B 0.9700 C38 O2 1.402(5) C39 H39A 0.9700 C39 H39B 0.9700 C39 C40 1.488(4) C39 O3 1.488(4) C40 H40A 0.9700 C40 H40B 0.9700 C40 C41 1.487(4) C41 H41A 0.9700 C41 H41B 0.9700 C41 C42 1.487(4) C42 H42A 0.9700 C42 H42B 0.9700 C42 O3 1.487(4) C43 H43A 0.9700 C43 H43B 0.9700 C43 C44 1.487(4) C43 C46 1.488(4) C44 H44A 0.9700 C44 H44B 0.9700 C44 O4 1.487(4) C45 H45A 0.9700 C45 H45B 0.9700 C45 C46 1.487(4) C45 O4 1.487(4) C46 H46A 0.9700 C46 H46B 0.9700 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C3 C4 C5 C6 -1.0(5) C3 C2 N1 C10 -176.5(3) C3 C2 N1 Co1 2.3(3) C3 N2 Co1 N3 -177.7(2) C3 N2 Co1 N1 0.2(2) C4 C3 C2 C1 -1.0(5) C4 C3 C2 N1 179.1(3) C4 C3 N2 C7 0.4(4) C4 C3 N2 Co1 179.9(2) C4 C5 C6 C7 0.1(5) C5 C6 C7 C8 -177.2(3) C5 C6 C7 N2 1.0(4) C6 C7 C8 C9 0.5(5) C6 C7 C8 N3 179.8(3) C6 C7 N2 C3 -1.3(4) C6 C7 N2 Co1 179.1(2) C7 C8 N3 C22 -176.1(2) C7 C8 N3 Co1 -0.1(3) C7 N2 Co1 N3 1.9(2) C7 N2 Co1 N1 179.7(2) C2 C3 C4 C5 179.6(3) C2 C3 N2 C7 -178.6(3) C2 C3 N2 Co1 1.0(3) C1 C2 N1 C10 3.6(5) C1 C2 N1 Co1 -177.6(3) C8 C7 N2 C3 177.2(2) C8 C7 N2 Co1 -2.3(3) C9 C8 N3 C22 3.2(4) C9 C8 N3 Co1 179.2(2) C10 C15 C14 C13 -0.2(5) C10 C15 C16 C18 118.6(4) C10 C15 C16 C17 -118.2(4) C10 C11 C19 C20 -114.1(4) C10 C11 C19 C21 121.8(4) C15 C10 C11 C12 1.7(5) C15 C10 C11 C19 -178.4(3) C15 C10 N1 C2 -92.5(3) C15 C10 N1 Co1 88.9(3) C15 C14 C13 C12 0.6(5) C14 C15 C16 C18 -61.9(4) C14 C15 C16 C17 61.3(4) C14 C13 C12 C11 0.1(5) C13 C12 C11 C10 -1.2(5) C13 C12 C11 C19 178.9(3) C12 C11 C19 C20 65.8(4) C12 C11 C19 C21 -58.3(4) C11 C10 C15 C14 -1.0(4) C11 C10 C15 C16 178.5(3) C11 C10 N1 C2 88.7(3) C11 C10 N1 Co1 -89.9(3) C16 C15 C14 C13 -179.7(3) C22 C27 C26 C25 -0.7(5) C22 C27 C28 C29 125.3(3) C22 C27 C28 C30 -110.2(3) C22 C23 C31 C32 -102.0(4) C22 C23 C31 C33 133.3(3) C27 C22 C23 C24 -0.3(5) C27 C22 C23 C31 -179.1(3) C27 C22 N3 C8 -85.9(4) C27 C22 N3 Co1 98.5(3) C27 C26 C25 C24 -0.2(5) C26 C27 C28 C29 -56.1(4) C26 C27 C28 C30 68.4(4) C26 C25 C24 C23 0.9(5) C25 C24 C23 C22 -0.6(5) C25 C24 C23 C31 178.2(3) C24 C23 C31 C32 79.2(4) C24 C23 C31 C33 -45.5(4) C23 C22 C27 C26 0.9(5) C23 C22 C27 C28 179.6(3) C23 C22 N3 C8 96.6(3) C23 C22 N3 Co1 -79.0(3) C28 C27 C26 C25 -179.4(3) N2 C3 C4 C5 0.8(5) N2 C3 C2 C1 177.9(3) N2 C3 C2 N1 -2.1(4) N2 C7 C8 C9 -177.9(3) N2 C7 C8 N3 1.4(4) N3 C22 C27 C26 -176.5(3) N3 C22 C27 C28 2.2(5) N3 C22 C23 C24 177.2(3) N3 C22 C23 C31 -1.7(4) N1 C10 C15 C14 -179.7(3) N1 C10 C15 C16 -0.2(4) N1 C10 C11 C12 -179.6(3) N1 C10 C11 C19 0.3(4) C35 C36 C37 C38 -30.4(5) C36 C35 O2 C38 -21.5(5) C36 C37 C38 O2 18.5(5) C37 C38 O2 C35 1.5(5) O2 C35 C36 C37 32.2(4) C39 C40 C41 C42 -22.0(17) C40 C39 O3 C42 -28.0(12) C40 C41 C42 O3 4.6(17) C41 C42 O3 C39 14.7(14) O3 C39 C40 C41 29.9(14) C43 C44 O4 C45 -33(2) C44 C43 C46 C45 -44.0(19) C46 C43 C44 O4 43.0(19) C46 C45 O4 C44 4.8(17) O4 C45 C46 C43 25.6(18)