#------------------------------------------------------------------------------ #$Date: 2023-12-04 20:16:21 +0200 (Mon, 04 Dec 2023) $ #$Revision: 288017 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247821.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_7247821 loop_ _publ_author_name 'Ahmed, Naushad' 'Sahu, Prem Prakash' _publ_section_title ; Ferromagnetically coupled CoII2LnIII2 complexes (where LnIII = Ho, Er, Yb): experimental and theoretical investigations ; _journal_issue 47 _journal_name_full CrystEngComm _journal_page_first 6592 _journal_page_last 6601 _journal_paper_doi 10.1039/D3CE00827D _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'C66 H69 Co2 N4 O20 Yb2, 8(C H4 O), 3(N O3)' _chemical_formula_sum 'C74 H101 Co2 N7 O37 Yb2' _chemical_formula_weight 2144.55 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2022-08-30 _audit_creation_method ; Olex2 1.5-alpha (compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487) ; _audit_update_record ; 2023-10-16 deposited with the CCDC. 2023-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.400(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.7585(7) _cell_length_b 16.0409(5) _cell_length_c 19.8206(6) _cell_measurement_reflns_used 15117 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.4050 _cell_measurement_theta_min 1.8460 _cell_volume 8454.6(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5-alpha (Bourhis et al., 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_unetI/netI 0.0683 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 34693 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 1.856 _exptl_absorpt_coefficient_mu 2.672 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'Red Orange' _exptl_crystal_density_diffrn 1.685 _exptl_crystal_description Block _exptl_crystal_F_000 4336 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _refine_diff_density_max 1.108 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.142 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 608 _refine_ls_number_reflns 7455 _refine_ls_number_restraints 64 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0413 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+23.5288P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0946 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6042 _reflns_number_total 7455 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00827d2.cif _cod_data_source_block Co2Yb2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_ambient_temperature' value '100 (2)' was changed to '100(2)' -- the value was reformatted. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7247821 _shelx_shelxl_version_number 2018/3 _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. ; _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, All O(H) groups, All O(H,H) groups 2. Restrained distances O33-H33 0.85 with sigma of 0.01 O13-H13 0.85 with sigma of 0.01 C44-H33 1.887058 with sigma of 0.02 C24-H13 1.90588 with sigma of 0.02 O1-N2 \\sim O1A-N2A with sigma of 0.02 N2-O2 \\sim N2A-O2A with sigma of 0.02 N2-O4 \\sim N2A-O4A with sigma of 0.02 O4-O2 \\sim O4A-O2A with sigma of 0.04 O1-O4 \\sim O1A-O4A with sigma of 0.04 O1-O2 \\sim O1A-O2A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints O2A \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O1A \\sim O1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O4A \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4. Rigid body (RIGU) restrains O2A, N2A, O1A, O4A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O1, O4, O2, N2 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O2A)=Sof(O4A)=Sof(N2A)=Sof(O1A)=1-FVAR(1) Sof(O1)=Sof(N2)=Sof(O4)=Sof(O2)=FVAR(1) Fixed Sof: H52A(0.5) H52B(0.5) H52C(0.5) 6.a Rotating group: O3W(H3WA,H3WB) 6.b Secondary CH2 refined with riding coordinates: C24(H24A,H24B), C44(H44A,H44B) 6.c Aromatic/amide H refined with riding coordinates: C37(H37), C17(H17), C32(H32), C39(H39), C19(H19), C12(H12), C13(H13A), C14(H14), C34(H34), C22(H22), C33(H33A), C40(H40), C41(H41), C42(H42), C21(H21), C20(H20) 6.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C52(H52A,H52B,H52C), C72(H72A,H72B,H72C), C2S(H2SA,H2SB, H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C45(H45A,H45B,H45C), C1S(H1SA, H1SB,H1SC) 6.e Idealised tetrahedral OH refined as rotating group: O2S(H2S), O3S(H3S), O4S(H4S), O1S(H1S) ; _shelx_res_file ; TITL ms-ka-707-mecn-chcl3-3_mo_a.res in C2/c co2yb2.res created by SHELXL-2018/3 at 11:25:49 on 30-Aug-2022 CELL 0.71073 26.7585 16.0409 19.8206 90 96.4 90 ZERR 4 0.0007 0.0005 0.0006 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Co N O Yb UNIT 296 404 8 28 148 8 EQIV $1 1-X,+Y,1.5-Z DFIX 0.85 0.01 O33 H33 DFIX 0.85 0.01 O13 H13 DANG 1.887058 0.02 C44 H33 DANG 1.90588 0.02 C24 H13 SADI O1 N2 O1A N2A SADI N2 O2 N2A O2A SADI N2 O4 N2A O4A SADI 0.04 O4 O2 O4A O2A SADI 0.04 O1 O4 O1A O4A SADI 0.04 O1 O2 O1A O2A RIGU O2A N2A O1A O4A RIGU O1 O4 O2 N2 SIMU O2A O2 SIMU O1A O1 SIMU O4A O4 L.S. 6 PLAN 2 TEMP -173(2) CONF FREE Yb1 C71_$1 FREE Co1 Yb1 FREE H3Wa Yb1 FREE H3Wb Yb1 BOND $H list 4 MORE -1 HTAB fmap 2 acta 52 OMIT -3 50 OMIT -1 1 1 OMIT -4 0 2 OMIT 1 1 0 REM REM REM WGHT 0.030100 23.528799 FVAR 0.11006 0.80827 YB1 6 0.443405 0.667954 0.654410 11.00000 0.01530 0.02476 = 0.02310 -0.00020 0.00122 0.00124 CO1 3 0.393147 0.819338 0.541963 11.00000 0.01485 0.02571 = 0.01953 -0.00077 0.00360 -0.00093 O11 5 0.385058 0.767518 0.633860 11.00000 0.01199 0.02797 = 0.02324 0.00375 0.00662 0.00511 O31 5 0.438897 0.716469 0.544255 11.00000 0.01668 0.03183 = 0.01833 -0.00130 0.00298 0.00472 O33 5 0.323693 0.760869 0.504590 11.00000 0.01850 0.02576 = 0.02838 0.00125 0.00073 -0.00493 H33 2 0.331616 0.712713 0.491863 11.00000 -1.50000 O12 5 0.359672 0.643098 0.704243 11.00000 0.01868 0.02435 = 0.02994 0.00648 0.00480 0.00098 O32 5 0.510715 0.613616 0.585509 11.00000 0.02523 0.04268 = 0.03255 0.00027 0.00608 0.01341 O13 5 0.461789 0.887518 0.563921 11.00000 0.01819 0.03532 = 0.02890 -0.00335 0.00155 -0.00551 H13 2 0.480909 0.858603 0.592036 11.00000 -1.50000 O72 5 0.498969 0.775794 0.843598 11.00000 0.01798 0.04224 = 0.02899 -0.00530 -0.00080 0.00631 O71 5 0.448317 0.713128 0.764249 11.00000 0.02465 0.02872 = 0.02735 -0.00464 0.00495 -0.00524 O51 5 0.467341 0.551630 0.710185 11.00000 0.02612 0.02615 = 0.03372 0.00242 -0.00033 0.00492 O3W 5 0.401833 0.565846 0.589552 11.00000 0.03186 0.02724 = 0.02863 0.00262 -0.00265 -0.00404 AFIX 7 H3WA 2 0.381722 0.540877 0.613142 11.00000 -1.50000 H3WB 2 0.382833 0.588386 0.557371 11.00000 -1.50000 AFIX 0 N31 4 0.397559 0.829279 0.439698 11.00000 0.01707 0.02872 = 0.02266 0.00077 0.00285 -0.00553 N11 4 0.358752 0.923660 0.575585 11.00000 0.02004 0.02150 = 0.02161 0.00160 0.00112 -0.00322 O2S 5 0.341522 0.447102 0.632581 11.00000 0.04768 0.04036 = 0.04271 0.00589 -0.00618 -0.01230 AFIX 147 H2S 2 0.352187 0.420302 0.667667 11.00000 -1.50000 AFIX 0 O3S 5 0.370565 0.359188 0.743935 11.00000 0.06436 0.05075 = 0.03730 0.00945 0.00776 0.00524 AFIX 147 H3S 2 0.383674 0.313080 0.736194 11.00000 -1.50000 AFIX 0 O4S 5 0.400593 0.205904 0.724315 11.00000 0.06895 0.05094 = 0.05488 -0.01462 0.00519 0.00547 AFIX 147 H4S 2 0.427815 0.179722 0.732057 11.00000 -1.50000 AFIX 0 C37 1 0.431883 0.795988 0.408497 11.00000 0.02408 0.03617 = 0.01736 -0.00035 0.00603 -0.01049 AFIX 43 H37 2 0.430875 0.807630 0.361370 11.00000 -1.20000 AFIX 0 C31 1 0.472096 0.742359 0.437824 11.00000 0.02305 0.03490 = 0.02095 -0.00147 0.00389 0.00333 O101 5 0.500000 0.150074 0.750000 10.50000 0.05533 0.04706 = 0.10345 0.00000 -0.01456 0.00000 C35 1 0.512683 0.649063 0.521802 11.00000 0.02064 0.03601 = 0.02372 -0.00663 0.00071 0.00189 C36 1 0.473336 0.703808 0.501612 11.00000 0.01575 0.03293 = 0.02673 -0.00626 0.00702 0.00004 N101 4 0.500000 0.071925 0.750000 10.50000 0.06327 0.03789 = 0.03446 0.00000 0.01923 0.00000 C38 1 0.359478 0.879364 0.402488 11.00000 0.02292 0.03474 = 0.01283 -0.00109 -0.00396 -0.00499 O102 5 0.460157 0.035487 0.751710 11.00000 0.09966 0.07282 = 0.09311 -0.01861 0.06119 -0.03176 C17 1 0.326637 0.924236 0.619820 11.00000 0.02026 0.02370 = 0.02693 -0.00529 -0.00150 0.00207 AFIX 43 H17 2 0.310315 0.975267 0.627950 11.00000 -1.20000 AFIX 0 C15 1 0.328532 0.711234 0.704146 11.00000 0.01410 0.02690 = 0.02328 -0.00055 -0.00084 -0.00175 C18 1 0.370239 1.000915 0.544449 11.00000 0.02740 0.02406 = 0.02112 -0.00316 0.00913 -0.00297 C23 1 0.421428 1.022800 0.547339 11.00000 0.02752 0.02862 = 0.03260 -0.00730 0.00881 -0.01015 C32 1 0.510397 0.723422 0.397133 11.00000 0.02971 0.05959 = 0.02289 0.00005 0.01021 0.00458 AFIX 43 H32 2 0.509472 0.747990 0.353400 11.00000 -1.20000 AFIX 0 C71 1 0.458954 0.774017 0.802994 11.00000 0.01754 0.03260 = 0.02330 -0.00027 0.01106 0.00189 C39 1 0.372340 0.942078 0.359019 11.00000 0.02160 0.04427 = 0.02342 0.00585 0.00159 -0.01236 AFIX 43 H39 2 0.406642 0.950300 0.352558 11.00000 -1.20000 AFIX 0 O1S 5 0.254779 0.392729 0.371869 11.00000 0.05812 0.04950 = 0.05952 -0.00756 0.00129 -0.00349 AFIX 147 H1S 2 0.272722 0.431842 0.389216 11.00000 -1.50000 AFIX 0 C25 1 0.353077 0.580439 0.755000 11.00000 0.02782 0.02473 = 0.04459 0.01318 0.00683 0.00140 AFIX 137 H25A 2 0.378252 0.536419 0.752899 11.00000 -1.50000 H25B 2 0.319311 0.556367 0.746328 11.00000 -1.50000 H25C 2 0.357201 0.606088 0.800153 11.00000 -1.50000 AFIX 0 C16 1 0.343581 0.778052 0.663747 11.00000 0.01151 0.02577 = 0.01899 0.00170 0.00192 -0.00092 C19 1 0.333173 1.050076 0.511212 11.00000 0.03280 0.02549 = 0.03034 0.00205 0.00532 -0.00086 AFIX 43 H19 2 0.298886 1.034036 0.509608 11.00000 -1.20000 AFIX 0 C12 1 0.272210 0.856783 0.694427 11.00000 0.01869 0.02835 = 0.03104 0.00203 0.00342 0.00371 AFIX 43 H12 2 0.253051 0.906760 0.692351 11.00000 -1.20000 AFIX 0 C24 1 0.461399 0.972254 0.587753 11.00000 0.02291 0.04435 = 0.03862 -0.01255 0.00441 -0.01036 AFIX 23 H24A 2 0.494660 0.997946 0.584318 11.00000 -1.20000 H24B 2 0.455392 0.972597 0.636142 11.00000 -1.20000 AFIX 0 C11 1 0.314260 0.851137 0.657608 11.00000 0.01737 0.02961 = 0.02112 -0.00271 0.00345 -0.00242 C13 1 0.258326 0.791260 0.733383 11.00000 0.02592 0.03445 = 0.03794 0.00243 0.01502 0.00317 AFIX 43 H13A 2 0.229451 0.796076 0.756990 11.00000 -1.20000 AFIX 0 C52 1 0.500000 0.422092 0.750000 10.50000 0.03834 0.02052 = 0.06684 0.00000 -0.00557 0.00000 PART -1 AFIX 137 H52A 2 0.468023 0.401727 0.763424 10.50000 -1.50000 H52B 2 0.527760 0.401727 0.782212 10.50000 -1.50000 H52C 2 0.504217 0.401727 0.704363 10.50000 -1.50000 AFIX 0 PART 0 C14 1 0.286290 0.718606 0.738185 11.00000 0.02420 0.03137 = 0.02176 0.00694 0.00499 -0.00626 AFIX 43 H14 2 0.276487 0.673584 0.764935 11.00000 -1.20000 AFIX 0 C34 1 0.550394 0.632418 0.481125 11.00000 0.02677 0.05618 = 0.03175 -0.00874 0.00587 0.01336 AFIX 43 H34 2 0.576939 0.595135 0.496006 11.00000 -1.20000 AFIX 0 C22 1 0.432996 1.095971 0.515020 11.00000 0.03723 0.03484 = 0.05191 -0.00253 0.01553 -0.00872 AFIX 43 H22 2 0.467242 1.111669 0.515178 11.00000 -1.20000 AFIX 0 C43 1 0.309081 0.867395 0.412878 11.00000 0.01725 0.02493 = 0.02456 -0.00046 -0.00076 -0.00595 C51 1 0.500000 0.515206 0.750000 10.50000 0.03053 0.01971 = 0.03143 0.00000 0.00778 0.00000 C33 1 0.548743 0.670817 0.418789 11.00000 0.02840 0.06819 = 0.03366 -0.00364 0.00989 0.01521 AFIX 43 H33A 2 0.574594 0.660493 0.390669 11.00000 -1.20000 AFIX 0 C44 1 0.289107 0.798125 0.453581 11.00000 0.01729 0.04619 = 0.04199 0.01633 0.00073 -0.00062 AFIX 23 H44A 2 0.260436 0.820225 0.475634 11.00000 -1.20000 H44B 2 0.275808 0.753856 0.421698 11.00000 -1.20000 AFIX 0 C40 1 0.336047 0.992348 0.325263 11.00000 0.03193 0.03987 = 0.03173 0.01395 -0.00504 -0.01007 AFIX 43 H40 2 0.345250 1.033862 0.294773 11.00000 -1.20000 AFIX 0 C41 1 0.285918 0.982252 0.335871 11.00000 0.03161 0.03984 = 0.03462 0.00312 -0.01149 0.00001 AFIX 43 H41 2 0.260673 1.017471 0.313694 11.00000 -1.20000 AFIX 0 C72 1 0.425035 0.846600 0.800455 11.00000 0.03242 0.04180 = 0.04846 -0.00636 -0.01006 0.01335 AFIX 137 H72A 2 0.429925 0.876353 0.843874 11.00000 -1.50000 H72B 2 0.390080 0.827661 0.791959 11.00000 -1.50000 H72C 2 0.432543 0.884056 0.763845 11.00000 -1.50000 AFIX 0 C42 1 0.273469 0.920022 0.379285 11.00000 0.01857 0.03672 = 0.02914 0.00513 -0.00175 -0.00430 AFIX 43 H42 2 0.239186 0.913052 0.386372 11.00000 -1.20000 AFIX 0 C2S 1 0.311894 0.394289 0.587388 11.00000 0.05178 0.04800 = 0.05604 -0.00480 -0.00402 -0.01467 AFIX 137 H2SA 2 0.302546 0.423660 0.544481 11.00000 -1.50000 H2SB 2 0.281410 0.378380 0.607422 11.00000 -1.50000 H2SC 2 0.331146 0.344140 0.578869 11.00000 -1.50000 AFIX 0 C21 1 0.395972 1.146557 0.482625 11.00000 0.07016 0.02513 = 0.04527 -0.00115 0.02094 -0.00950 AFIX 43 H21 2 0.404941 1.197216 0.462257 11.00000 -1.20000 AFIX 0 C20 1 0.346275 1.123931 0.479742 11.00000 0.05696 0.03297 = 0.04067 0.00669 0.01137 0.00864 AFIX 43 H20 2 0.320936 1.158136 0.456557 11.00000 -1.20000 AFIX 0 C3S 1 0.368430 0.367626 0.811495 11.00000 0.05166 0.05292 = 0.07240 0.00758 0.00226 0.00101 AFIX 137 H3SA 2 0.347669 0.416077 0.819829 11.00000 -1.50000 H3SB 2 0.402459 0.375571 0.834475 11.00000 -1.50000 H3SC 2 0.353615 0.317340 0.829099 11.00000 -1.50000 AFIX 0 C4S 1 0.365257 0.156199 0.684404 11.00000 0.08597 0.06782 = 0.05796 -0.01247 0.00143 -0.01530 AFIX 137 H4SA 2 0.370202 0.162316 0.636402 11.00000 -1.50000 H4SB 2 0.331163 0.174078 0.691234 11.00000 -1.50000 H4SC 2 0.369849 0.097663 0.697840 11.00000 -1.50000 AFIX 0 C45 1 0.543599 0.542930 0.600770 11.00000 0.07961 0.10421 = 0.06954 0.04064 0.03834 0.06948 AFIX 137 H45A 2 0.535853 0.516726 0.643043 11.00000 -1.50000 H45B 2 0.578658 0.561759 0.605979 11.00000 -1.50000 H45C 2 0.538565 0.502413 0.563628 11.00000 -1.50000 AFIX 0 C1S 1 0.265780 0.318526 0.409867 11.00000 0.10951 0.05778 = 0.04914 -0.00847 0.00376 -0.00690 AFIX 137 H1SA 2 0.252720 0.270323 0.383086 11.00000 -1.50000 H1SB 2 0.249931 0.321088 0.452072 11.00000 -1.50000 H1SC 2 0.302272 0.313017 0.420637 11.00000 -1.50000 AFIX 0 PART 1 O1 5 0.356075 0.609061 0.465626 21.00000 0.03150 0.03369 = 0.04410 -0.00431 -0.01514 -0.00437 N2 4 0.323367 0.551614 0.449224 21.00000 0.02946 0.03277 = 0.03280 -0.00799 0.00186 0.00133 O4 5 0.337359 0.484802 0.431863 21.00000 0.05534 0.03508 = 0.10837 -0.02349 0.02566 -0.00140 O2 5 0.278705 0.567989 0.449902 21.00000 0.02232 0.06349 = 0.09245 -0.00231 -0.00199 0.00580 PART 2 O2A 5 0.317538 0.572901 0.471888 -21.00000 0.13153 0.14034 = 0.08553 0.02112 0.06882 0.01759 O4A 5 0.333319 0.523428 0.372958 -21.00000 0.08789 0.07540 = 0.08228 -0.01391 0.01567 0.01387 N2A 4 0.336538 0.573937 0.418264 -21.00000 0.03681 0.05965 = 0.05945 0.00594 0.01626 0.00274 O1A 5 0.354481 0.645676 0.406150 -21.00000 0.09256 0.06348 = 0.14154 0.00525 0.05840 -0.01071 HKLF 4 REM ms-ka-707-mecn-chcl3-3_mo_a.res in C2/c REM wR2 = 0.0946, GooF = S = 1.045, Restrained GooF = 1.042 for all data REM R1 = 0.0413 for 6042 Fo > 4sig(Fo) and 0.0561 for all 7455 data REM 608 parameters refined using 64 restraints END WGHT 0.0301 23.5130 REM Instructions for potential hydrogen bonds HTAB O33 O1 HTAB O33 O2A HTAB O33 N2A HTAB O33 O1A HTAB O13 O72_$1 HTAB O3W O2S HTAB O3W O1 HTAB O3W N2 HTAB O3W O2A HTAB O2S O3S HTAB O3S O4S HTAB O4S O101 HTAB O4S N101 HTAB O4S O102 EQIV $2 x, -y+1, z-1/2 HTAB C39 O102_$2 HTAB O1S N2 HTAB O1S O4 HTAB O1S O2 HTAB O1S O4A HTAB C25 O51 EQIV $3 x, y+1, z HTAB C24 O102_$3 EQIV $4 x, -y+1, z+1/2 HTAB C14 O1S_$4 EQIV $5 -x+1/2, -y+3/2, -z+1 HTAB C44 O2_$5 HTAB C72 O102_$3 HTAB C3S O4A_$4 HTAB C3S N2A_$4 HTAB C45 O51 EQIV $6 -x+1, -y+1, -z+1 HTAB C45 O4_$6 REM Highest difference peak 1.108, deepest hole -0.864, 1-sigma level 0.142 Q1 1 0.3307 0.6615 0.4654 11.00000 0.05 1.11 Q2 1 0.4933 0.6677 0.7007 11.00000 0.05 0.93 ; _shelx_res_checksum 22987 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Yb1 Yb 0.44340(2) 0.66795(2) 0.65441(2) 0.02112(9) Uani 1 1 d . . . . . Co1 Co 0.39315(3) 0.81934(4) 0.54196(3) 0.01990(17) Uani 1 1 d . . . . . O11 O 0.38506(12) 0.7675(2) 0.63386(17) 0.0207(8) Uani 1 1 d . . . . . O31 O 0.43890(12) 0.7165(2) 0.54425(16) 0.0222(8) Uani 1 1 d . . . . . O33 O 0.32369(13) 0.7609(2) 0.50459(18) 0.0244(8) Uani 1 1 d D . . . . H33 H 0.3316(17) 0.7127(15) 0.4919(17) 0.037 Uiso 1 1 d D U . . . O12 O 0.35967(13) 0.6431(2) 0.70424(17) 0.0242(8) Uani 1 1 d . . . . . O32 O 0.51072(14) 0.6136(2) 0.58551(19) 0.0333(10) Uani 1 1 d . . . . . O13 O 0.46179(13) 0.8875(2) 0.56392(18) 0.0275(9) Uani 1 1 d D . . . . H13 H 0.4809(18) 0.8586(16) 0.5920(18) 0.041 Uiso 1 1 d D U . . . O72 O 0.49897(13) 0.7758(2) 0.84360(18) 0.0300(9) Uani 1 1 d . . . . . O71 O 0.44832(13) 0.7131(2) 0.76425(18) 0.0268(9) Uani 1 1 d . . . . . O51 O 0.46734(14) 0.5516(2) 0.71019(18) 0.0289(9) Uani 1 1 d . . . . . O3W O 0.40183(14) 0.5658(2) 0.58955(18) 0.0297(9) Uani 1 1 d . . . . . H3WA H 0.381722 0.540877 0.613142 0.045 Uiso 1 1 d R U . . . H3WB H 0.382833 0.588386 0.557371 0.045 Uiso 1 1 d R U . . . N31 N 0.39756(16) 0.8293(3) 0.4397(2) 0.0228(10) Uani 1 1 d . . . . . N11 N 0.35875(15) 0.9237(3) 0.5756(2) 0.0211(10) Uani 1 1 d . . . . . O2S O 0.34152(17) 0.4471(3) 0.6326(2) 0.0444(11) Uani 1 1 d . . . . . H2S H 0.352187 0.420302 0.667667 0.067 Uiso 1 1 calc R U . . . O3S O 0.37057(19) 0.3592(3) 0.7439(2) 0.0506(12) Uani 1 1 d . . . . . H3S H 0.383674 0.313080 0.736194 0.076 Uiso 1 1 calc R U . . . O4S O 0.4006(2) 0.2059(3) 0.7243(3) 0.0584(13) Uani 1 1 d . . . . . H4S H 0.427815 0.179722 0.732057 0.088 Uiso 1 1 calc R U . . . C37 C 0.4319(2) 0.7960(3) 0.4085(3) 0.0256(12) Uani 1 1 d . . . . . H37 H 0.430875 0.807630 0.361370 0.031 Uiso 1 1 calc R U . . . C31 C 0.4721(2) 0.7424(3) 0.4378(3) 0.0262(12) Uani 1 1 d . . . . . O101 O 0.500000 0.1501(5) 0.750000 0.070(2) Uani 1 2 d S T P . . C35 C 0.5127(2) 0.6491(3) 0.5218(3) 0.0269(13) Uani 1 1 d . . . . . C36 C 0.47334(19) 0.7038(3) 0.5016(3) 0.0248(12) Uani 1 1 d . . . . . N101 N 0.500000 0.0719(5) 0.750000 0.044(2) Uani 1 2 d S T P . . C38 C 0.3595(2) 0.8794(3) 0.4025(2) 0.0239(12) Uani 1 1 d . . . . . O102 O 0.4602(2) 0.0355(3) 0.7517(3) 0.085(2) Uani 1 1 d . . . . . C17 C 0.32664(19) 0.9242(3) 0.6198(3) 0.0239(12) Uani 1 1 d . . . . . H17 H 0.310315 0.975267 0.627950 0.029 Uiso 1 1 calc R U . . . C15 C 0.32853(18) 0.7112(3) 0.7041(3) 0.0216(12) Uani 1 1 d . . . . . C18 C 0.3702(2) 1.0009(3) 0.5444(3) 0.0237(12) Uani 1 1 d . . . . . C23 C 0.4214(2) 1.0228(3) 0.5473(3) 0.0292(13) Uani 1 1 d . . . . . C32 C 0.5104(2) 0.7234(4) 0.3971(3) 0.0369(15) Uani 1 1 d . . . . . H32 H 0.509472 0.747990 0.353400 0.044 Uiso 1 1 calc R U . . . C71 C 0.45895(19) 0.7740(3) 0.8030(3) 0.0238(12) Uani 1 1 d . . . . . C39 C 0.3723(2) 0.9421(4) 0.3590(3) 0.0298(13) Uani 1 1 d . . . . . H39 H 0.406642 0.950300 0.352558 0.036 Uiso 1 1 calc R U . . . O1S O 0.25478(19) 0.3927(3) 0.3719(2) 0.0561(13) Uani 1 1 d . . . . . H1S H 0.272722 0.431842 0.389216 0.084 Uiso 1 1 calc R U . . . C25 C 0.3531(2) 0.5804(3) 0.7550(3) 0.0322(14) Uani 1 1 d . . . . . H25A H 0.378252 0.536419 0.752899 0.048 Uiso 1 1 calc R U . . . H25B H 0.319311 0.556367 0.746328 0.048 Uiso 1 1 calc R U . . . H25C H 0.357201 0.606088 0.800153 0.048 Uiso 1 1 calc R U . . . C16 C 0.34358(18) 0.7781(3) 0.6637(2) 0.0187(11) Uani 1 1 d . . . . . C19 C 0.3332(2) 1.0501(3) 0.5112(3) 0.0294(13) Uani 1 1 d . . . . . H19 H 0.298886 1.034036 0.509608 0.035 Uiso 1 1 calc R U . . . C12 C 0.2722(2) 0.8568(3) 0.6944(3) 0.0260(12) Uani 1 1 d . . . . . H12 H 0.253051 0.906760 0.692351 0.031 Uiso 1 1 calc R U . . . C24 C 0.4614(2) 0.9723(4) 0.5878(3) 0.0352(15) Uani 1 1 d D . . . . H24A H 0.494660 0.997946 0.584318 0.042 Uiso 1 1 calc R U . . . H24B H 0.455392 0.972597 0.636142 0.042 Uiso 1 1 calc R U . . . C11 C 0.31426(19) 0.8511(3) 0.6576(3) 0.0226(12) Uani 1 1 d . . . . . C13 C 0.2583(2) 0.7913(4) 0.7334(3) 0.0319(14) Uani 1 1 d . . . . . H13A H 0.229451 0.796076 0.756990 0.038 Uiso 1 1 calc R U . . . C52 C 0.500000 0.4221(5) 0.750000 0.043(2) Uani 1 2 d S T P . . H52A H 0.468023 0.401727 0.763424 0.064 Uiso 0.5 1 calc R U P A -1 H52B H 0.527760 0.401727 0.782212 0.064 Uiso 0.5 1 calc R U P A -1 H52C H 0.504217 0.401727 0.704363 0.064 Uiso 0.5 1 calc R U P A -1 C14 C 0.2863(2) 0.7186(3) 0.7382(3) 0.0256(12) Uani 1 1 d . . . . . H14 H 0.276487 0.673584 0.764935 0.031 Uiso 1 1 calc R U . . . C34 C 0.5504(2) 0.6324(4) 0.4811(3) 0.0380(15) Uani 1 1 d . . . . . H34 H 0.576939 0.595135 0.496006 0.046 Uiso 1 1 calc R U . . . C22 C 0.4330(2) 1.0960(4) 0.5150(3) 0.0405(16) Uani 1 1 d . . . . . H22 H 0.467242 1.111669 0.515178 0.049 Uiso 1 1 calc R U . . . C43 C 0.30908(19) 0.8674(3) 0.4129(3) 0.0225(12) Uani 1 1 d . . . . . C51 C 0.500000 0.5152(5) 0.750000 0.0269(18) Uani 1 2 d S T P . . C33 C 0.5487(2) 0.6708(4) 0.4188(3) 0.0429(17) Uani 1 1 d . . . . . H33A H 0.574594 0.660493 0.390669 0.052 Uiso 1 1 calc R U . . . C44 C 0.2891(2) 0.7981(4) 0.4536(3) 0.0354(15) Uani 1 1 d D . . . . H44A H 0.260436 0.820225 0.475634 0.042 Uiso 1 1 calc R U . . . H44B H 0.275808 0.753856 0.421698 0.042 Uiso 1 1 calc R U . . . C40 C 0.3360(2) 0.9923(4) 0.3253(3) 0.0352(14) Uani 1 1 d . . . . . H40 H 0.345250 1.033862 0.294773 0.042 Uiso 1 1 calc R U . . . C41 C 0.2859(2) 0.9823(4) 0.3359(3) 0.0365(14) Uani 1 1 d . . . . . H41 H 0.260673 1.017471 0.313694 0.044 Uiso 1 1 calc R U . . . C72 C 0.4250(2) 0.8466(4) 0.8005(3) 0.0420(16) Uani 1 1 d . . . . . H72A H 0.429925 0.876353 0.843874 0.063 Uiso 1 1 calc R U . . . H72B H 0.390080 0.827661 0.791959 0.063 Uiso 1 1 calc R U . . . H72C H 0.432543 0.884056 0.763845 0.063 Uiso 1 1 calc R U . . . C42 C 0.2735(2) 0.9200(3) 0.3793(3) 0.0285(13) Uani 1 1 d . . . . . H42 H 0.239186 0.913052 0.386372 0.034 Uiso 1 1 calc R U . . . C2S C 0.3119(3) 0.3943(4) 0.5874(4) 0.0527(18) Uani 1 1 d . . . . . H2SA H 0.302546 0.423660 0.544481 0.079 Uiso 1 1 calc R U . . . H2SB H 0.281410 0.378380 0.607422 0.079 Uiso 1 1 calc R U . . . H2SC H 0.331146 0.344140 0.578869 0.079 Uiso 1 1 calc R U . . . C21 C 0.3960(3) 1.1466(4) 0.4826(3) 0.0458(18) Uani 1 1 d . . . . . H21 H 0.404941 1.197216 0.462257 0.055 Uiso 1 1 calc R U . . . C20 C 0.3463(3) 1.1239(4) 0.4797(3) 0.0431(17) Uani 1 1 d . . . . . H20 H 0.320936 1.158136 0.456557 0.052 Uiso 1 1 calc R U . . . C3S C 0.3684(3) 0.3676(5) 0.8115(4) 0.059(2) Uani 1 1 d . . . . . H3SA H 0.347669 0.416077 0.819829 0.089 Uiso 1 1 calc R U . . . H3SB H 0.402459 0.375571 0.834475 0.089 Uiso 1 1 calc R U . . . H3SC H 0.353615 0.317340 0.829099 0.089 Uiso 1 1 calc R U . . . C4S C 0.3653(3) 0.1562(5) 0.6844(4) 0.071(2) Uani 1 1 d . . . . . H4SA H 0.370202 0.162316 0.636402 0.107 Uiso 1 1 calc R U . . . H4SB H 0.331163 0.174078 0.691234 0.107 Uiso 1 1 calc R U . . . H4SC H 0.369849 0.097663 0.697840 0.107 Uiso 1 1 calc R U . . . C45 C 0.5436(3) 0.5429(5) 0.6008(4) 0.082(3) Uani 1 1 d . . . . . H45A H 0.535853 0.516726 0.643043 0.123 Uiso 1 1 calc R U . . . H45B H 0.578658 0.561759 0.605979 0.123 Uiso 1 1 calc R U . . . H45C H 0.538565 0.502413 0.563628 0.123 Uiso 1 1 calc R U . . . C1S C 0.2658(4) 0.3185(5) 0.4099(4) 0.073(3) Uani 1 1 d . . . . . H1SA H 0.252720 0.270323 0.383086 0.109 Uiso 1 1 calc R U . . . H1SB H 0.249931 0.321088 0.452072 0.109 Uiso 1 1 calc R U . . . H1SC H 0.302272 0.313017 0.420637 0.109 Uiso 1 1 calc R U . . . O1 O 0.3561(2) 0.6091(3) 0.4656(3) 0.0379(16) Uani 0.808(9) 1 d D U P B 1 N2 N 0.3234(3) 0.5516(5) 0.4492(4) 0.0318(19) Uani 0.808(9) 1 d D . P B 1 O4 O 0.3374(2) 0.4848(4) 0.4319(4) 0.065(2) Uani 0.808(9) 1 d D U P B 1 O2 O 0.2787(2) 0.5680(4) 0.4499(4) 0.060(2) Uani 0.808(9) 1 d D U P B 1 O2A O 0.318(2) 0.573(3) 0.4719(19) 0.115(18) Uani 0.192(9) 1 d D U P B 2 O4A O 0.3333(12) 0.5234(18) 0.3730(16) 0.081(10) Uani 0.192(9) 1 d D U P B 2 N2A N 0.3365(12) 0.5739(17) 0.4183(16) 0.051(8) Uani 0.192(9) 1 d D . P B 2 O1A O 0.3545(13) 0.6457(16) 0.4062(19) 0.096(12) Uani 0.192(9) 1 d D U P B 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 Yb1 0.01530(13) 0.02476(14) 0.02310(15) -0.00020(10) 0.00122(10) 0.00124(9) Co1 0.0148(4) 0.0257(4) 0.0195(4) -0.0008(3) 0.0036(3) -0.0009(3) O11 0.0120(18) 0.028(2) 0.0232(19) 0.0037(16) 0.0066(15) 0.0051(15) O31 0.0167(19) 0.032(2) 0.0183(19) -0.0013(16) 0.0030(16) 0.0047(16) O33 0.0185(19) 0.026(2) 0.028(2) 0.0013(17) 0.0007(16) -0.0049(16) O12 0.0187(19) 0.024(2) 0.030(2) 0.0065(16) 0.0048(16) 0.0010(15) O32 0.025(2) 0.043(3) 0.033(2) 0.0003(19) 0.0061(18) 0.0134(18) O13 0.018(2) 0.035(2) 0.029(2) -0.0034(18) 0.0016(17) -0.0055(17) O72 0.018(2) 0.042(2) 0.029(2) -0.0053(18) -0.0008(17) 0.0063(17) O71 0.025(2) 0.029(2) 0.027(2) -0.0046(17) 0.0049(17) -0.0052(17) O51 0.026(2) 0.026(2) 0.034(2) 0.0024(17) -0.0003(18) 0.0049(17) O3W 0.032(2) 0.027(2) 0.029(2) 0.0026(17) -0.0027(18) -0.0040(17) N31 0.017(2) 0.029(3) 0.023(2) 0.001(2) 0.003(2) -0.0055(19) N11 0.020(2) 0.021(2) 0.022(2) 0.0016(19) 0.001(2) -0.0032(18) O2S 0.048(3) 0.040(3) 0.043(3) 0.006(2) -0.006(2) -0.012(2) O3S 0.064(3) 0.051(3) 0.037(3) 0.009(2) 0.008(2) 0.005(3) O4S 0.069(4) 0.051(3) 0.055(3) -0.015(3) 0.005(3) 0.005(3) C37 0.024(3) 0.036(3) 0.017(3) 0.000(2) 0.006(2) -0.010(2) C31 0.023(3) 0.035(3) 0.021(3) -0.001(2) 0.004(2) 0.003(2) O101 0.055(5) 0.047(5) 0.103(6) 0.000 -0.015(4) 0.000 C35 0.021(3) 0.036(3) 0.024(3) -0.007(3) 0.001(2) 0.002(2) C36 0.016(3) 0.033(3) 0.027(3) -0.006(2) 0.007(2) 0.000(2) N101 0.063(6) 0.038(5) 0.034(4) 0.000 0.019(4) 0.000 C38 0.023(3) 0.035(3) 0.013(3) -0.001(2) -0.004(2) -0.005(2) O102 0.100(5) 0.073(4) 0.093(4) -0.019(3) 0.061(4) -0.032(4) C17 0.020(3) 0.024(3) 0.027(3) -0.005(2) -0.002(2) 0.002(2) C15 0.014(3) 0.027(3) 0.023(3) -0.001(2) -0.001(2) -0.002(2) C18 0.027(3) 0.024(3) 0.021(3) -0.003(2) 0.009(2) -0.003(2) C23 0.028(3) 0.029(3) 0.033(3) -0.007(3) 0.009(3) -0.010(2) C32 0.030(3) 0.060(4) 0.023(3) 0.000(3) 0.010(3) 0.005(3) C71 0.018(3) 0.033(3) 0.023(3) 0.000(2) 0.011(2) 0.002(2) C39 0.022(3) 0.044(4) 0.023(3) 0.006(3) 0.002(2) -0.012(3) O1S 0.058(3) 0.050(3) 0.060(3) -0.008(3) 0.001(3) -0.003(3) C25 0.028(3) 0.025(3) 0.045(4) 0.013(3) 0.007(3) 0.001(2) C16 0.012(2) 0.026(3) 0.019(3) 0.002(2) 0.002(2) -0.001(2) C19 0.033(3) 0.025(3) 0.030(3) 0.002(3) 0.005(3) -0.001(3) C12 0.019(3) 0.028(3) 0.031(3) 0.002(3) 0.003(2) 0.004(2) C24 0.023(3) 0.044(4) 0.039(4) -0.013(3) 0.004(3) -0.010(3) C11 0.017(3) 0.030(3) 0.021(3) -0.003(2) 0.003(2) -0.002(2) C13 0.026(3) 0.034(3) 0.038(4) 0.002(3) 0.015(3) 0.003(3) C52 0.038(5) 0.021(4) 0.067(6) 0.000 -0.006(5) 0.000 C14 0.024(3) 0.031(3) 0.022(3) 0.007(2) 0.005(2) -0.006(2) C34 0.027(3) 0.056(4) 0.032(3) -0.009(3) 0.006(3) 0.013(3) C22 0.037(4) 0.035(4) 0.052(4) -0.003(3) 0.016(3) -0.009(3) C43 0.017(3) 0.025(3) 0.025(3) 0.000(2) -0.001(2) -0.006(2) C51 0.031(5) 0.020(4) 0.031(5) 0.000 0.008(4) 0.000 C33 0.028(3) 0.068(5) 0.034(4) -0.004(3) 0.010(3) 0.015(3) C44 0.017(3) 0.046(4) 0.042(4) 0.016(3) 0.001(3) -0.001(3) C40 0.032(3) 0.040(4) 0.032(3) 0.014(3) -0.005(3) -0.010(3) C41 0.032(3) 0.040(4) 0.035(3) 0.003(3) -0.011(3) 0.000(3) C72 0.032(4) 0.042(4) 0.048(4) -0.006(3) -0.010(3) 0.013(3) C42 0.019(3) 0.037(3) 0.029(3) 0.005(3) -0.002(2) -0.004(2) C2S 0.052(5) 0.048(4) 0.056(4) -0.005(4) -0.004(4) -0.015(4) C21 0.070(5) 0.025(3) 0.045(4) -0.001(3) 0.021(4) -0.009(3) C20 0.057(5) 0.033(4) 0.041(4) 0.007(3) 0.011(3) 0.009(3) C3S 0.052(5) 0.053(5) 0.072(6) 0.008(4) 0.002(4) 0.001(4) C4S 0.086(7) 0.068(6) 0.058(5) -0.012(4) 0.001(5) -0.015(5) C45 0.080(6) 0.104(7) 0.070(5) 0.041(5) 0.038(5) 0.069(5) C1S 0.110(8) 0.058(5) 0.049(5) -0.008(4) 0.004(5) -0.007(5) O1 0.031(3) 0.034(3) 0.044(4) -0.004(3) -0.015(3) -0.004(2) N2 0.029(4) 0.033(3) 0.033(5) -0.008(3) 0.002(4) 0.001(3) O4 0.055(4) 0.035(3) 0.108(6) -0.023(4) 0.026(4) -0.001(3) O2 0.022(3) 0.063(4) 0.092(5) -0.002(4) -0.002(3) 0.006(3) O2A 0.13(4) 0.14(3) 0.09(2) 0.02(2) 0.07(2) 0.02(3) O4A 0.09(2) 0.075(18) 0.082(19) -0.014(15) 0.016(18) 0.014(16) N2A 0.037(18) 0.060(15) 0.059(18) 0.006(12) 0.016(15) 0.003(13) O1A 0.09(2) 0.063(15) 0.14(3) 0.005(15) 0.06(2) -0.011(14) 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' Yb Yb -0.3850 5.5486 '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 O11 Yb1 O31 68.01(11) . . ? O11 Yb1 O12 64.01(11) . . ? O11 Yb1 O32 132.12(12) . . ? O11 Yb1 O72 85.40(13) . 2_656 ? O11 Yb1 O71 84.95(13) . . ? O11 Yb1 O3W 97.05(13) . . ? O11 Yb1 H3WA 95.4 . . ? O11 Yb1 H3WB 81.7 . . ? O31 Yb1 O12 117.29(11) . . ? O31 Yb1 O32 64.62(12) . . ? O31 Yb1 O72 74.26(13) . 2_656 ? O31 Yb1 H3WA 90.1 . . ? O31 Yb1 H3WB 61.4 . . ? O12 Yb1 H3WA 58.0 . . ? O12 Yb1 H3WB 73.8 . . ? O32 Yb1 O12 148.62(12) . . ? O32 Yb1 H3WA 91.4 . . ? O32 Yb1 H3WB 81.9 . . ? O72 Yb1 O12 135.62(12) 2_656 . ? O72 Yb1 O32 75.76(13) 2_656 . ? O72 Yb1 H3WA 162.9 2_656 . ? O72 Yb1 H3WB 135.5 2_656 . ? O71 Yb1 O31 141.80(13) . . ? O71 Yb1 O12 69.15(12) . . ? O71 Yb1 O32 130.85(13) . . ? O71 Yb1 O72 77.24(12) . 2_656 ? O71 Yb1 O3W 137.22(12) . . ? O71 Yb1 H3WA 119.9 . . ? O71 Yb1 H3WB 142.8 . . ? O51 Yb1 O11 147.61(12) . . ? O51 Yb1 O31 137.23(12) . . ? O51 Yb1 O12 83.94(12) . . ? O51 Yb1 O32 78.28(12) . . ? O51 Yb1 O72 117.62(14) . 2_656 ? O51 Yb1 O71 79.04(13) . . ? O51 Yb1 O3W 76.96(14) . . ? O51 Yb1 H3WA 69.4 . . ? O51 Yb1 H3WB 94.3 . . ? O3W Yb1 O31 74.90(13) . . ? O3W Yb1 O12 73.51(12) . . ? O3W Yb1 O32 77.38(13) . . ? O3W Yb1 O72 145.52(13) . 2_656 ? O3W Yb1 H3WA 17.4 . . ? O3W Yb1 H3WB 17.3 . . ? H3WA Yb1 H3WB 28.9 . . ? O11 Co1 O31 76.97(13) . . ? O11 Co1 O33 87.47(14) . . ? O11 Co1 O13 101.60(14) . . ? O11 Co1 N31 160.10(15) . . ? O11 Co1 N11 86.92(14) . . ? O31 Co1 O33 98.52(14) . . ? O31 Co1 O13 84.84(14) . . ? O31 Co1 N11 159.17(15) . . ? O33 Co1 O13 170.85(14) . . ? N31 Co1 O31 89.11(15) . . ? N31 Co1 O33 80.52(15) . . ? N31 Co1 O13 91.07(15) . . ? N31 Co1 N11 109.53(17) . . ? N11 Co1 O33 93.79(15) . . ? N11 Co1 O13 85.60(15) . . ? Co1 O11 Yb1 108.21(13) . . ? C16 O11 Yb1 127.7(3) . . ? C16 O11 Co1 121.7(3) . . ? Co1 O31 Yb1 105.08(13) . . ? C36 O31 Yb1 125.5(3) . . ? C36 O31 Co1 124.1(3) . . ? Co1 O33 H33 105(3) . . ? C44 O33 Co1 122.2(3) . . ? C44 O33 H33 110(2) . . ? C15 O12 Yb1 115.4(3) . . ? C15 O12 C25 115.6(4) . . ? C25 O12 Yb1 123.5(3) . . ? C35 O32 Yb1 116.7(3) . . ? C35 O32 C45 115.2(4) . . ? C45 O32 Yb1 127.6(3) . . ? Co1 O13 H13 107(3) . . ? C24 O13 Co1 120.8(3) . . ? C24 O13 H13 109(2) . . ? C71 O72 Yb1 120.6(3) . 2_656 ? C71 O71 Yb1 144.6(3) . . ? C51 O51 Yb1 147.6(4) . . ? Yb1 O3W H3WA 109.0 . . ? Yb1 O3W H3WB 109.2 . . ? H3WA O3W H3WB 104.5 . . ? C37 N31 Co1 124.7(4) . . ? C37 N31 C38 119.5(4) . . ? C38 N31 Co1 115.8(3) . . ? C17 N11 Co1 125.5(3) . . ? C17 N11 C18 118.4(4) . . ? C18 N11 Co1 116.0(3) . . ? C2S O2S H2S 109.5 . . ? C3S O3S H3S 109.5 . . ? C4S O4S H4S 109.5 . . ? N31 C37 H37 116.7 . . ? N31 C37 C31 126.5(5) . . ? C31 C37 H37 116.7 . . ? C36 C31 C37 124.4(4) . . ? C36 C31 C32 118.4(5) . . ? C32 C31 C37 117.0(5) . . ? O32 C35 C36 114.5(4) . . ? C34 C35 O32 123.6(5) . . ? C34 C35 C36 122.0(5) . . ? O31 C36 C31 123.7(5) . . ? O31 C36 C35 117.8(5) . . ? C35 C36 C31 118.5(4) . . ? O102 N101 O101 118.6(4) 2_656 . ? O102 N101 O101 118.6(4) . . ? O102 N101 O102 122.7(9) 2_656 . ? C39 C38 N31 120.8(5) . . ? C39 C38 C43 119.9(5) . . ? C43 C38 N31 119.2(4) . . ? N11 C17 H17 118.3 . . ? N11 C17 C11 123.5(5) . . ? C11 C17 H17 118.3 . . ? O12 C15 C16 113.0(4) . . ? O12 C15 C14 126.5(4) . . ? C14 C15 C16 120.5(5) . . ? C23 C18 N11 116.9(5) . . ? C19 C18 N11 121.6(5) . . ? C19 C18 C23 121.5(5) . . ? C18 C23 C24 121.3(5) . . ? C22 C23 C18 117.2(6) . . ? C22 C23 C24 121.4(5) . . ? C31 C32 H32 119.2 . . ? C33 C32 C31 121.7(5) . . ? C33 C32 H32 119.2 . . ? O72 C71 Yb1 39.2(2) . 2_656 ? O72 C71 C72 118.6(5) . . ? O71 C71 Yb1 82.5(3) . 2_656 ? O71 C71 O72 121.6(5) . . ? O71 C71 C72 119.8(5) . . ? C72 C71 Yb1 157.6(4) . 2_656 ? C38 C39 H39 119.5 . . ? C40 C39 C38 120.9(5) . . ? C40 C39 H39 119.5 . . ? C1S O1S H1S 109.5 . . ? O12 C25 H25A 109.5 . . ? O12 C25 H25B 109.5 . . ? O12 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C16 C15 117.3(4) . . ? O11 C16 C11 123.6(4) . . ? C11 C16 C15 119.1(4) . . ? C18 C19 H19 120.2 . . ? C18 C19 C20 119.7(6) . . ? C20 C19 H19 120.2 . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C13 C12 C11 121.4(5) . . ? O13 C24 C23 111.5(5) . . ? O13 C24 H24A 109.3 . . ? O13 C24 H24B 109.3 . . ? C23 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C16 C11 C17 124.1(4) . . ? C16 C11 C12 118.5(5) . . ? C12 C11 C17 117.2(5) . . ? C12 C13 H13A 119.9 . . ? C12 C13 C14 120.2(5) . . ? C14 C13 H13A 119.9 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? C15 C14 H14 119.9 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C35 C34 H34 120.6 . . ? C33 C34 C35 118.9(6) . . ? C33 C34 H34 120.6 . . ? C23 C22 H22 119.2 . . ? C21 C22 C23 121.7(6) . . ? C21 C22 H22 119.1 . . ? C38 C43 C44 125.8(5) . . ? C42 C43 C38 117.9(5) . . ? C42 C43 C44 116.1(5) . . ? O51 C51 O51 124.5(7) 2_656 . ? O51 C51 C52 117.8(4) 2_656 . ? O51 C51 C52 117.8(4) . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? O33 C44 C43 116.7(5) . . ? O33 C44 H44A 108.1 . . ? O33 C44 H44B 108.1 . . ? C43 C44 H44A 108.1 . . ? C43 C44 H44B 108.1 . . ? H44A C44 H44B 107.3 . . ? C39 C40 H40 120.1 . . ? C39 C40 C41 119.9(5) . . ? C41 C40 H40 120.1 . . ? C40 C41 H41 120.6 . . ? C42 C41 C40 118.8(5) . . ? C42 C41 H41 120.6 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72B 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C43 C42 H42 118.7 . . ? C41 C42 C43 122.6(5) . . ? C41 C42 H42 118.7 . . ? O2S C2S H2SA 109.5 . . ? O2S C2S H2SB 109.5 . . ? O2S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C22 C21 H21 119.8 . . ? C20 C21 C22 120.3(6) . . ? C20 C21 H21 119.8 . . ? C19 C20 H20 120.2 . . ? C21 C20 C19 119.6(6) . . ? C21 C20 H20 120.2 . . ? O3S C3S H3SA 109.5 . . ? O3S C3S H3SB 109.5 . . ? O3S C3S H3SC 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O4S C4S H4SA 109.5 . . ? O4S C4S H4SB 109.5 . . ? O4S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? O32 C45 H45A 109.5 . . ? O32 C45 H45B 109.5 . . ? O32 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O4 N2 O1 119.2(8) . . ? O4 N2 O2 122.1(8) . . ? O2 N2 O1 118.7(7) . . ? O2A N2A O1A 112(3) . . ? O4A N2A O2A 129(3) . . ? O4A N2A O1A 117(3) . . ? 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 Yb1 O11 2.239(3) . ? Yb1 O31 2.308(3) . ? Yb1 O12 2.578(3) . ? Yb1 O32 2.533(3) . ? Yb1 O72 2.315(4) 2_656 ? Yb1 O71 2.284(3) . ? Yb1 O51 2.226(4) . ? Yb1 O3W 2.292(4) . ? Yb1 H3WA 2.6921 . ? Yb1 H3WB 2.6945 . ? Co1 O11 2.036(3) . ? Co1 O31 2.052(3) . ? Co1 O33 2.139(4) . ? Co1 O13 2.140(4) . ? Co1 N31 2.050(4) . ? Co1 N11 2.056(4) . ? O11 C16 1.326(5) . ? O31 C36 1.334(6) . ? O33 H33 0.847(10) . ? O33 C44 1.424(7) . ? O12 C15 1.374(6) . ? O12 C25 1.447(6) . ? O32 C35 1.391(6) . ? O32 C45 1.446(7) . ? O13 H13 0.851(10) . ? O13 C24 1.439(7) . ? O72 C71 1.266(6) . ? O71 C71 1.255(6) . ? O51 C51 1.255(5) . ? O3W H3WA 0.8513 . ? O3W H3WB 0.8507 . ? N31 C37 1.280(6) . ? N31 C38 1.435(7) . ? N11 C17 1.294(6) . ? N11 C18 1.433(6) . ? O2S H2S 0.8400 . ? O2S C2S 1.411(7) . ? O3S H3S 0.8400 . ? O3S C3S 1.353(8) . ? O4S H4S 0.8400 . ? O4S C4S 1.410(9) . ? C37 H37 0.9500 . ? C37 C31 1.448(8) . ? C31 C36 1.405(7) . ? C31 C32 1.406(7) . ? O101 N101 1.254(9) . ? C35 C36 1.395(7) . ? C35 C34 1.386(7) . ? N101 O102 1.220(6) 2_656 ? N101 O102 1.220(6) . ? C38 C39 1.392(7) . ? C38 C43 1.400(7) . ? C17 H17 0.9500 . ? C17 C11 1.449(7) . ? C15 C16 1.423(7) . ? C15 C14 1.384(7) . ? C18 C23 1.409(7) . ? C18 C19 1.376(8) . ? C23 C24 1.501(8) . ? C23 C22 1.389(8) . ? C32 H32 0.9500 . ? C32 C33 1.361(8) . ? C71 C72 1.474(7) . ? C39 H39 0.9500 . ? C39 C40 1.377(8) . ? O1S H1S 0.8400 . ? O1S C1S 1.422(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C16 C11 1.408(7) . ? C19 H19 0.9500 . ? C19 C20 1.402(8) . ? C12 H12 0.9500 . ? C12 C11 1.411(7) . ? C12 C13 1.379(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C13 H13A 0.9500 . ? C13 C14 1.383(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C52 C51 1.494(10) . ? C14 H14 0.9500 . ? C34 H34 0.9500 . ? C34 C33 1.377(8) . ? C22 H22 0.9500 . ? C22 C21 1.382(9) . ? C43 C44 1.506(7) . ? C43 C42 1.387(7) . ? C33 H33A 0.9500 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C40 H40 0.9500 . ? C40 C41 1.390(8) . ? C41 H41 0.9500 . ? C41 C42 1.383(7) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C42 H42 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C21 H21 0.9500 . ? C21 C20 1.373(9) . ? C20 H20 0.9500 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? O1 N2 1.287(9) . ? N2 O4 1.198(8) . ? N2 O2 1.225(10) . ? O2A N2A 1.23(2) . ? O4A N2A 1.205(18) . ? N2A O1A 1.28(2) . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Yb1 O11 C16 C15 -13.1(6) . . . . ? Yb1 O11 C16 C11 166.8(4) . . . . ? Yb1 O31 C36 C31 -172.3(4) . . . . ? Yb1 O31 C36 C35 7.8(7) . . . . ? Yb1 O12 C15 C16 12.4(5) . . . . ? Yb1 O12 C15 C14 -167.8(4) . . . . ? Yb1 O32 C35 C36 -6.7(6) . . . . ? Yb1 O32 C35 C34 173.0(5) . . . . ? Yb1 O72 C71 O71 2.4(6) 2_656 . . . ? Yb1 O72 C71 C72 -176.0(4) 2_656 . . . ? Yb1 O71 C71 Yb1 -105.0(5) . . . 2_656 ? Yb1 O71 C71 O72 -106.5(6) . . . . ? Yb1 O71 C71 C72 71.9(7) . . . . ? Yb1 O51 C51 O51 20.2(4) . . . 2_656 ? Yb1 O51 C51 C52 -159.8(4) . . . . ? Co1 O11 C16 C15 147.2(4) . . . . ? Co1 O11 C16 C11 -33.0(6) . . . . ? Co1 O31 C36 C31 -21.8(7) . . . . ? Co1 O31 C36 C35 158.3(4) . . . . ? Co1 O33 C44 C43 16.9(7) . . . . ? Co1 O13 C24 C23 -45.1(5) . . . . ? Co1 N31 C37 C31 3.3(8) . . . . ? Co1 N31 C38 C39 129.4(4) . . . . ? Co1 N31 C38 C43 -47.4(6) . . . . ? Co1 N11 C17 C11 6.8(7) . . . . ? Co1 N11 C18 C23 -55.8(5) . . . . ? Co1 N11 C18 C19 122.0(4) . . . . ? O11 C16 C11 C17 -2.0(8) . . . . ? O11 C16 C11 C12 -177.0(5) . . . . ? O12 C15 C16 O11 -1.8(7) . . . . ? O12 C15 C16 C11 178.4(4) . . . . ? O12 C15 C14 C13 -179.9(5) . . . . ? O32 C35 C36 O31 0.2(7) . . . . ? O32 C35 C36 C31 -179.8(5) . . . . ? O32 C35 C34 C33 179.9(6) . . . . ? N31 C37 C31 C36 14.7(9) . . . . ? N31 C37 C31 C32 -170.0(5) . . . . ? N31 C38 C39 C40 -177.5(5) . . . . ? N31 C38 C43 C44 -8.5(8) . . . . ? N31 C38 C43 C42 176.2(5) . . . . ? N11 C17 C11 C16 16.5(8) . . . . ? N11 C17 C11 C12 -168.5(5) . . . . ? N11 C18 C23 C24 -6.6(7) . . . . ? N11 C18 C23 C22 177.6(5) . . . . ? N11 C18 C19 C20 -178.1(5) . . . . ? C37 N31 C38 C39 -49.1(7) . . . . ? C37 N31 C38 C43 134.1(5) . . . . ? C37 C31 C36 O31 -4.3(9) . . . . ? C37 C31 C36 C35 175.7(5) . . . . ? C37 C31 C32 C33 -177.2(6) . . . . ? C31 C32 C33 C34 1.8(10) . . . . ? C35 C34 C33 C32 -0.8(10) . . . . ? C36 C31 C32 C33 -1.6(9) . . . . ? C36 C35 C34 C33 -0.3(9) . . . . ? C38 N31 C37 C31 -178.4(5) . . . . ? C38 C39 C40 C41 1.8(9) . . . . ? C38 C43 C44 O33 24.1(8) . . . . ? C38 C43 C42 C41 0.8(8) . . . . ? C17 N11 C18 C23 126.9(5) . . . . ? C17 N11 C18 C19 -55.3(7) . . . . ? C15 C16 C11 C17 177.9(5) . . . . ? C15 C16 C11 C12 2.9(8) . . . . ? C18 N11 C17 C11 -176.2(5) . . . . ? C18 C23 C24 O13 60.2(6) . . . . ? C18 C23 C22 C21 1.5(9) . . . . ? C18 C19 C20 C21 -0.2(9) . . . . ? C23 C18 C19 C20 -0.4(8) . . . . ? C23 C22 C21 C20 -2.1(10) . . . . ? C32 C31 C36 O31 -179.5(5) . . . . ? C32 C31 C36 C35 0.5(8) . . . . ? C39 C38 C43 C44 174.7(5) . . . . ? C39 C38 C43 C42 -0.6(8) . . . . ? C39 C40 C41 C42 -1.5(9) . . . . ? C25 O12 C15 C16 167.4(4) . . . . ? C25 O12 C15 C14 -12.8(7) . . . . ? C16 C15 C14 C13 -0.2(8) . . . . ? C19 C18 C23 C24 175.6(5) . . . . ? C19 C18 C23 C22 -0.2(8) . . . . ? C12 C13 C14 C15 0.3(9) . . . . ? C24 C23 C22 C21 -174.4(5) . . . . ? C11 C12 C13 C14 1.3(9) . . . . ? C13 C12 C11 C17 -178.2(5) . . . . ? C13 C12 C11 C16 -2.9(8) . . . . ? C14 C15 C16 O11 178.4(5) . . . . ? C14 C15 C16 C11 -1.4(8) . . . . ? C34 C35 C36 O31 -179.6(5) . . . . ? C34 C35 C36 C31 0.5(9) . . . . ? C22 C23 C24 O13 -124.2(5) . . . . ? C22 C21 C20 C19 1.4(9) . . . . ? C43 C38 C39 C40 -0.7(8) . . . . ? C44 C43 C42 C41 -174.9(5) . . . . ? C40 C41 C42 C43 0.2(9) . . . . ? C42 C43 C44 O33 -160.5(5) . . . . ? C45 O32 C35 C36 166.0(6) . . . . ? C45 O32 C35 C34 -14.2(9) . . . . ?