#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:24:27 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195648 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042747.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_7042747 loop_ _publ_author_name 'Otero, Antonio' 'fernandez, juan' 'garces, andres' 'S\'ANCHEZ-BARBA MERLO, LUIS FERNANDO' 'lara, agustin' 'martinez-Ferrer, Jaime' 'Carrion, Maria Prado' 'Rodr\'iguez, Ana Mar\'ia' _publ_section_title ; Highly Thermally Stable and Robust Enantiopure NNN-Scorpionate Zirconium Initiators for the Controlled Ring-Opening Polymerization of rac-Lactide ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01050H _journal_year 2017 _chemical_absolute_configuration rm _chemical_formula_moiety 'C57 H71 F N5 S3 Zr, 0.5(C4 O)' _chemical_formula_sum 'C59 H75 F N5 O0.5 S3 Zr' _chemical_formula_weight 1068.64 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2017-04-18 deposited with the CCDC. 2017-04-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.641(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.9418(3) _cell_length_b 28.5201(8) _cell_length_c 10.9256(3) _cell_measurement_reflns_used 1166 _cell_measurement_temperature 240(2) _cell_measurement_theta_max 15.715 _cell_measurement_theta_min 2.217 _cell_volume 3022.77(15) _computing_cell_refinement 'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)' _computing_data_collection 'Bruker APEX' _computing_data_reduction 'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)' _computing_molecular_graphics 'WINGX v2014.1 (Farrugia, 2012)' _computing_publication_material 'WINGX v2014.1 (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 240(2) _diffrn_measured_fraction_theta_full 0.933 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device_type 'CCD area detector, APEX' _diffrn_measurement_method 'omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1104 _diffrn_reflns_av_unetI/netI 0.2036 _diffrn_reflns_Laue_measured_fraction_full 0.933 _diffrn_reflns_Laue_measured_fraction_max 0.961 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 15981 _diffrn_reflns_point_group_measured_fraction_full 0.935 _diffrn_reflns_point_group_measured_fraction_max 0.963 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 1.428 _exptl_absorpt_coefficient_mu 0.328 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.174 _exptl_crystal_description prism _exptl_crystal_F_000 1130 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.542 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.081 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.10(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 656 _refine_ls_number_reflns 9418 _refine_ls_number_restraints 93 _refine_ls_restrained_S_all 0.956 _refine_ls_R_factor_all 0.1801 _refine_ls_R_factor_gt 0.0835 _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^)+(0.0935P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1764 _refine_ls_wR_factor_ref 0.2288 _reflns_Friedel_coverage 0.960 _reflns_Friedel_fraction_full 0.936 _reflns_Friedel_fraction_max 0.964 _reflns_number_gt 4585 _reflns_number_total 9418 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01050h2.cif _cod_data_source_block 6 _cod_original_formula_sum 'C59 H75 F N5 O0.50 S3 Zr' _cod_database_code 7042747 _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_min 0.940 _shelx_estimated_absorpt_t_max 0.962 _shelxl_version_number 2013-4 _shelx_res_file ; TITL AGU23_3 in P2(1) CELL 0.71073 9.9418 28.5201 10.9256 90.000 102.641 90.000 ZERR 2.00 0.0003 0.0008 0.0003 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N F S ZR O UNIT 118 150 10 2 6 2 1 MERG 2 OMIT -2.00 50.00 TWIN DELU c35 > c37a SIMU c35 > c37a 0.02 0.04 0.8 DFIX 21 c34 c35 c34 c36 c34 c37 c34 c35a c34 c36a c34 c37a DFIX 21.63 c35 c36 c35 c37 c36 c37 c35a c36a c35a c37a c36a c37a DELU c45 > c47a SIMU c45 > c47a 0.02 0.04 0.8 DFIX 31 c44 c45 c44 c46 c44 c47 c44 c45a c44 c46a c44 c47a DFIX 31.63 c45 c46 c45 c47 c46 c47 c45a c46a c45a c47a c46a c47a DELU c55 > c57a SIMU c55 > c57a 0.02 0.04 0.8 DFIX 41 c54 c55 c54 c56 c54 c57 c54 c55a c54 c56a c54a c57a DFIX 41.63 c55 c56 c55 c57 c56 c57 c55a c56a c55a c57a c56a c57a simu 0.02 o1 > c204 delu 0.05 o1 > c204 sadi o1 c201 c201 c202 c202 c203 c203 c204 c204 o1 sadi 0.04 o1 c202 o1 c203 c201 c203 c202 c204 FMAP 2 PLAN 25 SIZE 0.120 0.150 0.190 ACTA L.S. 25 WGHT 0.093500 BASF 0.09567 FVAR 0.15284 1.50377 1.52686 1.48171 ZR1 6 0.610440 0.178481 0.795796 11.00000 0.03907 0.05372 = 0.04502 -0.00070 0.01380 0.00030 S1 5 0.387944 0.223349 0.772940 11.00000 0.06320 0.11026 = 0.06426 -0.01307 0.01177 0.03195 S2 5 0.630371 0.153873 1.017264 11.00000 0.04402 0.07160 = 0.04655 -0.00200 0.00940 -0.01073 S3 5 0.445633 0.118543 0.664801 11.00000 0.04273 0.07851 = 0.05112 -0.00951 0.01674 -0.00767 N1 3 0.771547 0.122082 0.768579 11.00000 0.04284 0.05534 = 0.04496 -0.00191 0.01366 -0.00438 N2 3 0.876502 0.135854 0.709579 11.00000 0.03891 0.04273 = 0.06782 -0.00559 0.02307 -0.00215 N3 3 0.636912 0.202436 0.589180 11.00000 0.05798 0.04300 = 0.05816 -0.00107 0.01786 0.00675 N4 3 0.768026 0.195022 0.566078 11.00000 0.03538 0.05058 = 0.04373 -0.00209 0.00743 -0.00281 N5 3 0.793525 0.218351 0.840682 11.00000 0.04135 0.04440 = 0.05654 -0.01941 0.00973 0.00012 F1 4 0.919982 0.312275 1.297674 11.00000 0.20702 0.11928 = 0.06234 -0.04641 0.04537 -0.05385 C1 1 0.962956 0.100671 0.704636 11.00000 0.04198 0.05081 = 0.05001 -0.00263 0.01576 0.01650 C2 1 0.911782 0.062241 0.757700 11.00000 0.04261 0.05440 = 0.05730 0.00765 0.00848 0.01037 AFIX 43 H2 2 0.947978 0.032046 0.764378 11.00000 -1.20000 AFIX 0 C3 1 0.796446 0.077273 0.798974 11.00000 0.05880 0.03545 = 0.05615 0.00897 0.00960 0.01563 C4 1 1.087792 0.105639 0.648767 11.00000 0.05989 0.07074 = 0.10602 0.02310 0.04505 0.02064 AFIX 137 H4A 2 1.058973 0.111593 0.560420 11.00000 -1.50000 H4B 2 1.140720 0.077215 0.661943 11.00000 -1.50000 H4C 2 1.143321 0.131277 0.688299 11.00000 -1.50000 AFIX 0 C5 1 0.707714 0.048828 0.864257 11.00000 0.05955 0.05831 = 0.05553 0.00817 -0.00260 -0.00370 AFIX 137 H5A 2 0.722919 0.058338 0.950484 11.00000 -1.50000 H5B 2 0.730437 0.016241 0.859957 11.00000 -1.50000 H5C 2 0.612623 0.053578 0.824388 11.00000 -1.50000 AFIX 0 C6 1 0.769930 0.201563 0.443602 11.00000 0.08355 0.03672 = 0.05019 -0.00677 0.02433 0.00115 C7 1 0.637825 0.213156 0.389888 11.00000 0.08287 0.06100 = 0.04560 0.01354 0.00916 0.00143 AFIX 43 H7 2 0.605697 0.219766 0.305170 11.00000 -1.20000 AFIX 0 C8 1 0.557021 0.213790 0.479082 11.00000 0.05456 0.08445 = 0.04361 0.02020 -0.00404 0.00608 C9 1 0.893111 0.195179 0.389706 11.00000 0.08953 0.07787 = 0.06931 0.01057 0.05137 0.01737 AFIX 137 H9A 2 0.956780 0.220365 0.416605 11.00000 -1.50000 H9B 2 0.865802 0.195168 0.299813 11.00000 -1.50000 H9C 2 0.936564 0.165866 0.417780 11.00000 -1.50000 AFIX 0 C10 1 0.407177 0.222928 0.463894 11.00000 0.07136 0.13711 = 0.06142 0.02411 0.01929 0.01631 AFIX 137 H10A 2 0.363154 0.195577 0.488219 11.00000 -1.50000 H10B 2 0.367601 0.230211 0.377754 11.00000 -1.50000 H10C 2 0.393936 0.248903 0.515893 11.00000 -1.50000 AFIX 0 C11 1 0.882373 0.184488 0.665358 11.00000 0.05042 0.03226 = 0.05285 0.00436 0.02799 0.00193 AFIX 13 H11 2 0.964420 0.186448 0.629616 11.00000 -1.20000 AFIX 0 C12 1 0.903857 0.219775 0.772767 11.00000 0.02456 0.06137 = 0.04794 -0.01077 0.00626 -0.00879 AFIX 13 H12 2 0.989812 0.211551 0.831838 11.00000 -1.20000 AFIX 0 C13 1 0.922564 0.268022 0.720524 11.00000 0.04448 0.04066 = 0.05832 -0.00847 0.01200 -0.01155 C14 1 1.040076 0.279091 0.688504 11.00000 0.05059 0.04842 = 0.07742 0.00107 0.01729 -0.00471 AFIX 43 H14 2 1.111499 0.257412 0.698107 11.00000 -1.20000 AFIX 0 C15 1 1.056555 0.328122 0.635435 11.00000 0.07897 0.06450 = 0.11079 0.00843 0.03694 -0.01725 AFIX 43 H15 2 1.136140 0.339381 0.614019 11.00000 -1.20000 AFIX 0 C16 1 0.925163 0.354988 0.623455 11.00000 0.10576 0.04907 = 0.10185 0.01684 0.02475 -0.02340 AFIX 13 H16 2 0.924976 0.385972 0.584639 11.00000 -1.20000 AFIX 0 C17 1 0.803129 0.322691 0.561651 11.00000 0.10172 0.06333 = 0.08448 0.01829 0.00907 0.00253 AFIX 23 H17A 2 0.825891 0.299560 0.504313 11.00000 -1.20000 H17B 2 0.718731 0.339257 0.524925 11.00000 -1.20000 AFIX 0 C18 1 0.810053 0.304263 0.695793 11.00000 0.04029 0.06617 = 0.07155 -0.00616 0.00583 -0.00625 AFIX 13 H18 2 0.722126 0.295113 0.715436 11.00000 -1.20000 AFIX 0 C19 1 0.868175 0.354049 0.744919 11.00000 0.06304 0.04505 = 0.09472 -0.01287 0.00052 -0.00281 C20 1 0.971447 0.356482 0.866753 11.00000 0.11657 0.06718 = 0.11037 -0.03351 0.03538 -0.01900 AFIX 137 H20A 2 1.039719 0.332510 0.868940 11.00000 -1.50000 H20B 2 0.925807 0.351821 0.934674 11.00000 -1.50000 H20C 2 1.015164 0.386680 0.874922 11.00000 -1.50000 AFIX 0 C21 1 0.747534 0.389025 0.742539 11.00000 0.13513 0.06257 = 0.14679 -0.00132 0.02500 0.02330 AFIX 137 H21A 2 0.783495 0.420285 0.756210 11.00000 -1.50000 H21B 2 0.700359 0.380950 0.807454 11.00000 -1.50000 H21C 2 0.684308 0.387420 0.662483 11.00000 -1.50000 AFIX 0 C22 1 0.829416 0.241787 0.955708 11.00000 0.05079 0.04142 = 0.05913 -0.00472 0.02774 -0.01205 C23 1 0.733184 0.271823 0.993793 11.00000 0.05738 0.05248 = 0.07248 -0.02466 0.02166 -0.01645 AFIX 43 H23 2 0.648137 0.276922 0.939894 11.00000 -1.20000 AFIX 0 C24 1 0.762200 0.293510 1.107829 11.00000 0.07950 0.07477 = 0.08272 -0.01892 0.03369 0.00004 AFIX 43 H24 2 0.694766 0.311170 1.133584 11.00000 -1.20000 AFIX 0 C25 1 0.885765 0.289456 1.181571 11.00000 0.11245 0.07886 = 0.04372 -0.01987 0.02880 -0.04341 C26 1 0.987873 0.260950 1.154847 11.00000 0.08232 0.08058 = 0.07701 -0.02364 0.01054 -0.03487 AFIX 43 H26 2 1.073383 0.258128 1.209650 11.00000 -1.20000 AFIX 0 C27 1 0.956434 0.236771 1.042241 11.00000 0.06631 0.06828 = 0.05577 -0.01504 0.01968 -0.01170 AFIX 43 H27 2 1.021822 0.216390 1.022941 11.00000 -1.20000 AFIX 0 C28 1 0.382725 0.263037 0.894842 11.00000 0.05121 0.07974 = 0.04490 -0.01614 0.01636 0.00676 C29 1 0.394100 0.310897 0.874588 11.00000 0.11104 0.08857 = 0.07622 -0.01619 0.03473 -0.00164 AFIX 43 H29 2 0.409777 0.321067 0.798042 11.00000 -1.20000 AFIX 0 C30 1 0.382941 0.343456 0.963771 11.00000 0.10280 0.06726 = 0.07291 0.02516 0.02180 0.01536 AFIX 43 H30 2 0.387023 0.375092 0.944272 11.00000 -1.20000 AFIX 0 C31 1 0.365478 0.330869 1.084187 11.00000 0.04315 0.05441 = 0.09635 -0.00184 0.01351 0.00863 C32 1 0.353221 0.282268 1.100843 11.00000 0.08493 0.04287 = 0.08060 -0.00408 0.03868 0.00133 AFIX 43 H32 2 0.338599 0.271261 1.176998 11.00000 -1.20000 AFIX 0 C33 1 0.362281 0.249979 1.006801 11.00000 0.06383 0.05549 = 0.07258 0.00397 0.02345 0.01044 AFIX 43 H33 2 0.353761 0.218210 1.022735 11.00000 -1.20000 AFIX 0 C34 1 0.355560 0.365966 1.192815 11.00000 0.07629 0.04007 = 0.08932 -0.01001 0.01717 -0.00876 PART 1 C35 1 0.483979 0.361045 1.291999 10.70000 0.07539 AFIX 33 H35A 2 0.562170 0.369032 1.257909 10.70000 -1.50000 H35B 2 0.492685 0.329250 1.321519 10.70000 -1.50000 H35C 2 0.479853 0.381683 1.360494 10.70000 -1.50000 AFIX 0 C36 1 0.233803 0.353442 1.245975 10.70000 0.08011 AFIX 33 H36A 2 0.150902 0.356992 1.182385 10.70000 -1.50000 H36B 2 0.230332 0.373787 1.315217 10.70000 -1.50000 H36C 2 0.242041 0.321511 1.274436 10.70000 -1.50000 AFIX 0 C37 1 0.338399 0.415191 1.142198 10.70000 0.09390 AFIX 33 H37A 2 0.418405 0.423911 1.111693 10.70000 -1.50000 H37B 2 0.327570 0.436313 1.207778 10.70000 -1.50000 H37C 2 0.258276 0.416753 1.074833 10.70000 -1.50000 AFIX 0 PART 2 C35A 1 0.482248 0.396530 1.218604 10.30000 0.14135 AFIX 33 H35D 2 0.478112 0.417724 1.285945 10.30000 -1.50000 H35E 2 0.486430 0.414120 1.144614 10.30000 -1.50000 H35F 2 0.562919 0.377220 1.241685 10.30000 -1.50000 AFIX 0 C36A 1 0.344468 0.342350 1.314601 10.30000 0.14070 AFIX 33 H36D 2 0.255967 0.327553 1.304324 10.30000 -1.50000 H36E 2 0.354740 0.365386 1.380060 10.30000 -1.50000 H36F 2 0.415675 0.319162 1.336502 10.30000 -1.50000 AFIX 0 C37A 1 0.230617 0.397857 1.154305 10.30000 0.13148 AFIX 33 H37D 2 0.149371 0.379117 1.127007 10.30000 -1.50000 H37E 2 0.242998 0.417876 1.086992 10.30000 -1.50000 H37F 2 0.220710 0.416685 1.224635 10.30000 -1.50000 AFIX 0 PART 0 C38 1 0.480994 0.129489 1.057327 11.00000 0.04262 0.06262 = 0.02288 0.00721 -0.00509 0.00331 C39 1 0.360217 0.118417 0.976784 11.00000 0.07140 0.15821 = 0.04759 0.02073 0.02060 -0.03213 AFIX 43 H39 2 0.354795 0.121781 0.891174 11.00000 -1.20000 AFIX 0 C40 1 0.247804 0.102782 1.015008 11.00000 0.03992 0.13154 = 0.03777 0.00487 0.00211 -0.01649 AFIX 43 H40 2 0.166253 0.097669 0.956055 11.00000 -1.20000 AFIX 0 C41 1 0.252218 0.094171 1.141859 11.00000 0.04229 0.06320 = 0.04555 0.00210 0.01136 0.00518 C42 1 0.375149 0.105217 1.223793 11.00000 0.05043 0.13047 = 0.04049 0.00833 0.00517 -0.03019 AFIX 43 H42 2 0.383224 0.101455 1.309649 11.00000 -1.20000 AFIX 0 C43 1 0.484321 0.121530 1.179928 11.00000 0.07154 0.09568 = 0.05439 -0.00251 0.01145 -0.02727 AFIX 43 H43 2 0.566101 0.127564 1.237746 11.00000 -1.20000 AFIX 0 C44 1 0.124801 0.074921 1.184491 11.00000 0.03441 0.08086 = 0.05292 0.00237 0.01049 0.00215 PART 1 C45 1 0.080797 0.027227 1.122012 10.60000 0.05442 AFIX 33 H45A 2 0.000881 0.015982 1.148805 10.60000 -1.50000 H45B 2 0.154707 0.005116 1.145832 10.60000 -1.50000 H45C 2 0.059405 0.030885 1.032496 10.60000 -1.50000 AFIX 0 C46 1 0.148982 0.068441 1.326153 10.60000 0.06669 AFIX 33 H46A 2 0.066412 0.056744 1.347307 10.60000 -1.50000 H46B 2 0.173123 0.098019 1.367009 10.60000 -1.50000 H46C 2 0.222638 0.046478 1.353341 10.60000 -1.50000 AFIX 0 C47 1 0.001355 0.108160 1.138894 10.60000 0.04867 AFIX 33 H47A 2 -0.078180 0.096148 1.164894 10.60000 -1.50000 H47B 2 -0.017743 0.110252 1.049049 10.60000 -1.50000 H47C 2 0.023259 0.138741 1.174399 10.60000 -1.50000 AFIX 0 PART 2 C45A 1 0.156144 0.023380 1.215839 10.40000 0.14839 AFIX 33 H45D 2 0.079039 0.009228 1.241337 10.40000 -1.50000 H45E 2 0.236464 0.021027 1.282795 10.40000 -1.50000 H45F 2 0.172650 0.007460 1.143108 10.40000 -1.50000 AFIX 0 C46A 1 0.119243 0.100189 1.308330 10.40000 0.09239 AFIX 33 H46D 2 0.040649 0.089364 1.337981 10.40000 -1.50000 H46E 2 0.111838 0.133391 1.293982 10.40000 -1.50000 H46F 2 0.201789 0.093518 1.369996 10.40000 -1.50000 AFIX 0 C47A 1 -0.015469 0.079516 1.095439 10.40000 0.21883 AFIX 33 H47D 2 -0.084819 0.066009 1.133454 10.40000 -1.50000 H47E 2 -0.014309 0.063375 1.018571 10.40000 -1.50000 H47F 2 -0.035789 0.112063 1.078100 10.40000 -1.50000 AFIX 0 PART 0 C48 1 0.512445 0.077996 0.571910 11.00000 0.04836 0.05567 = 0.03496 -0.00467 0.00819 -0.00261 C49 1 0.613520 0.088896 0.506121 11.00000 0.05262 0.07808 = 0.04381 -0.00797 0.01785 -0.01179 AFIX 43 H49 2 0.648981 0.119172 0.510348 11.00000 -1.20000 AFIX 0 C50 1 0.661622 0.055982 0.435474 11.00000 0.05238 0.08636 = 0.05588 -0.02630 0.01626 -0.03081 AFIX 43 H50 2 0.729159 0.064681 0.392941 11.00000 -1.20000 AFIX 0 C51 1 0.614642 0.010837 0.424723 11.00000 0.04705 0.06868 = 0.05921 -0.01886 0.01110 -0.00712 C52 1 0.517775 0.000285 0.490753 11.00000 0.09623 0.07847 = 0.08853 -0.01482 0.05171 -0.03759 AFIX 43 H52 2 0.483580 -0.030167 0.486177 11.00000 -1.20000 AFIX 0 C53 1 0.467601 0.031955 0.563700 11.00000 0.06199 0.06957 = 0.05624 -0.00692 0.01941 -0.02775 AFIX 43 H53 2 0.402662 0.022415 0.608222 11.00000 -1.20000 AFIX 0 C54 1 0.667675 -0.025448 0.337706 11.00000 0.08553 0.07421 = 0.11235 -0.02151 0.04256 -0.02037 PART 1 C55 1 0.792289 -0.014476 0.293002 10.50000 0.10170 AFIX 137 H55A 2 0.809843 -0.039051 0.238512 10.50000 -1.50000 H55B 2 0.869064 -0.011808 0.363293 10.50000 -1.50000 H55C 2 0.779811 0.014640 0.247838 10.50000 -1.50000 AFIX 0 C56 1 0.548949 -0.025379 0.223531 10.50000 0.10756 AFIX 137 H56A 2 0.526395 -0.057072 0.197237 10.50000 -1.50000 H56B 2 0.575288 -0.008352 0.156678 10.50000 -1.50000 H56C 2 0.470089 -0.010670 0.244481 10.50000 -1.50000 AFIX 0 C57 1 0.674550 -0.073096 0.392637 10.50000 0.06872 AFIX 137 H57A 2 0.716161 -0.071497 0.480535 10.50000 -1.50000 H57B 2 0.728830 -0.092992 0.351478 10.50000 -1.50000 H57C 2 0.583117 -0.085684 0.381502 10.50000 -1.50000 AFIX 0 PART 2 C55A 1 0.823615 -0.028115 0.395796 10.50000 0.10266 AFIX 137 H55D 2 0.837692 -0.040666 0.479166 10.50000 -1.50000 H55E 2 0.862837 0.002739 0.399014 10.50000 -1.50000 H55F 2 0.867325 -0.048076 0.345346 10.50000 -1.50000 AFIX 0 C56A 1 0.660732 -0.006423 0.209628 10.50000 0.12634 AFIX 137 H56D 2 0.715818 0.021466 0.215264 10.50000 -1.50000 H56E 2 0.566805 0.000940 0.171026 10.50000 -1.50000 H56F 2 0.695095 -0.029404 0.159981 10.50000 -1.50000 AFIX 0 C57A 1 0.614207 -0.072210 0.333797 10.50000 0.10411 AFIX 137 H57D 2 0.664705 -0.092106 0.288963 10.50000 -1.50000 H57E 2 0.518612 -0.072100 0.292041 10.50000 -1.50000 H57F 2 0.623482 -0.083755 0.417770 10.50000 -1.50000 AFIX 0 PART 0 O1 7 1.196288 -0.010555 0.726786 10.50000 0.08694 0.08242 = 0.10621 0.04016 0.04579 0.01271 C202 1 1.245530 -0.048065 0.897565 10.50000 0.10563 0.08208 = 0.10322 0.01032 0.03769 0.01540 AFIX 23 H20D 2 1.317764 -0.071421 0.919150 10.50000 -1.20000 H20E 2 1.225938 -0.035491 0.974300 10.50000 -1.20000 AFIX 0 C201 1 1.282296 -0.014972 0.830801 10.50000 0.09110 0.07122 = 0.11790 0.01525 0.04113 0.01347 AFIX 23 H20F 2 1.288794 0.014352 0.876698 10.50000 -1.20000 H20G 2 1.372583 -0.022043 0.815387 10.50000 -1.20000 AFIX 0 C203 1 1.135824 -0.066199 0.828030 10.50000 0.11560 0.07317 = 0.12774 0.03089 0.02789 -0.00043 AFIX 23 H20H 2 1.053164 -0.054176 0.850437 10.50000 -1.20000 H20I 2 1.136709 -0.100121 0.834609 10.50000 -1.20000 AFIX 0 C204 1 1.143911 -0.052645 0.715337 10.50000 0.13670 0.10782 = 0.12216 0.01392 0.00708 0.02520 AFIX 23 H20J 2 1.202445 -0.073776 0.680747 10.50000 -1.20000 H20K 2 1.053141 -0.052312 0.660031 10.50000 -1.20000 AFIX 0 HKLF 4 REM AGU23_3 in P2(1) REM R1 = 0.0835 for 4585 Fo > 4sig(Fo) and 0.1801 for all 9418 data REM 656 parameters refined using 93 restraints END WGHT 0.0856 0.0000 REM Highest difference peak 0.542, deepest hole -0.363, 1-sigma level 0.081 Q1 1 1.1699 -0.0388 0.6359 11.00000 0.05 0.54 Q2 1 1.1372 -0.0618 0.8798 11.00000 0.05 0.49 Q3 1 1.1162 -0.0793 0.7233 11.00000 0.05 0.44 Q4 1 1.1081 -0.0700 0.8587 11.00000 0.05 0.44 Q5 1 1.0546 -0.0590 0.7139 11.00000 0.05 0.42 Q6 1 1.1434 0.4223 0.8814 11.00000 0.05 0.40 Q7 1 1.2211 -0.0262 0.7776 11.00000 0.05 0.40 Q8 1 1.1953 0.0066 0.7497 11.00000 0.05 0.39 Q9 1 1.2496 0.0067 0.8215 11.00000 0.05 0.37 Q10 1 0.1983 0.0440 1.3294 11.00000 0.05 0.37 Q11 1 1.2783 -0.0284 0.7243 11.00000 0.05 0.35 Q12 1 0.8709 -0.0618 0.2683 11.00000 0.05 0.35 Q13 1 0.7448 -0.0019 0.2464 11.00000 0.05 0.32 Q14 1 0.2686 0.2009 0.6403 11.00000 0.05 0.31 Q15 1 1.0070 0.4224 0.8688 11.00000 0.05 0.31 Q16 1 1.2233 0.3569 0.7192 11.00000 0.05 0.31 Q17 1 0.5280 0.1561 0.6575 11.00000 0.05 0.31 Q18 1 1.0316 -0.0594 0.6404 11.00000 0.05 0.30 Q19 1 1.1958 0.3528 0.7379 11.00000 0.05 0.30 Q20 1 1.2284 -0.0246 0.8536 11.00000 0.05 0.30 Q21 1 1.0935 0.3282 0.5362 11.00000 0.05 0.29 Q22 1 1.3252 -0.0279 0.9090 11.00000 0.05 0.29 Q23 1 0.2135 0.3798 0.8676 11.00000 0.05 0.29 Q24 1 0.7561 -0.0542 0.5128 11.00000 0.05 0.29 Q25 1 1.1684 0.2292 0.6153 11.00000 0.05 0.29 ; _shelx_res_checksum 17113 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Zr1 Zr 0.61044(14) 0.17848(6) 0.79580(14) 0.0452(4) Uani 1 1 d . . . . . S1 S 0.3879(5) 0.2233(2) 0.7729(5) 0.0796(17) Uani 1 1 d . . . . . S2 S 0.6304(4) 0.15387(16) 1.0173(4) 0.0541(12) Uani 1 1 d . . . . . S3 S 0.4456(4) 0.11854(17) 0.6648(4) 0.0565(13) Uani 1 1 d . . . . . N1 N 0.7715(13) 0.1221(5) 0.7686(12) 0.047(4) Uani 1 1 d . . . . . N2 N 0.8765(13) 0.1359(5) 0.7096(13) 0.048(4) Uani 1 1 d . . . . . N3 N 0.6369(15) 0.2024(4) 0.5892(15) 0.052(4) Uani 1 1 d . . . . . N4 N 0.7680(13) 0.1950(4) 0.5661(13) 0.043(4) Uani 1 1 d . . . . . N5 N 0.7935(13) 0.2184(4) 0.8407(13) 0.048(4) Uani 1 1 d . . . . . F1 F 0.9200(17) 0.3123(5) 1.2977(11) 0.127(6) Uani 1 1 d . . . . . C1 C 0.9630(17) 0.1007(6) 0.7046(17) 0.047(5) Uani 1 1 d . . . . . C2 C 0.9118(17) 0.0622(6) 0.7577(17) 0.052(5) Uani 1 1 d . . . . . H2 H 0.9480 0.0320 0.7644 0.062 Uiso 1 1 calc R U . . . C3 C 0.7964(17) 0.0773(6) 0.7990(16) 0.051(4) Uani 1 1 d . . . . . C4 C 1.0878(17) 0.1056(7) 0.6488(19) 0.075(6) Uani 1 1 d . . . . . H4A H 1.0590 0.1116 0.5604 0.112 Uiso 1 1 calc R U . . . H4B H 1.1407 0.0772 0.6619 0.112 Uiso 1 1 calc R U . . . H4C H 1.1433 0.1313 0.6883 0.112 Uiso 1 1 calc R U . . . C5 C 0.7077(17) 0.0488(6) 0.8643(17) 0.060(5) Uani 1 1 d . . . . . H5A H 0.7229 0.0583 0.9505 0.090 Uiso 1 1 calc R U . . . H5B H 0.7304 0.0162 0.8600 0.090 Uiso 1 1 calc R U . . . H5C H 0.6126 0.0536 0.8244 0.090 Uiso 1 1 calc R U . . . C6 C 0.770(2) 0.2016(6) 0.4436(18) 0.055(5) Uani 1 1 d . . . . . C7 C 0.638(2) 0.2132(6) 0.3899(18) 0.064(5) Uani 1 1 d . . . . . H7 H 0.6057 0.2198 0.3052 0.077 Uiso 1 1 calc R U . . . C8 C 0.5570(19) 0.2138(7) 0.4791(19) 0.063(5) Uani 1 1 d . . . . . C9 C 0.8931(19) 0.1952(6) 0.3897(17) 0.074(6) Uani 1 1 d . . . . . H9A H 0.9568 0.2204 0.4166 0.111 Uiso 1 1 calc R U . . . H9B H 0.8658 0.1952 0.2998 0.111 Uiso 1 1 calc R U . . . H9C H 0.9366 0.1659 0.4178 0.111 Uiso 1 1 calc R U . . . C10 C 0.407(2) 0.2229(9) 0.4639(19) 0.089(7) Uani 1 1 d . . . . . H10A H 0.3632 0.1956 0.4882 0.134 Uiso 1 1 calc R U . . . H10B H 0.3676 0.2302 0.3778 0.134 Uiso 1 1 calc R U . . . H10C H 0.3939 0.2489 0.5159 0.134 Uiso 1 1 calc R U . . . C11 C 0.8824(15) 0.1845(6) 0.6654(14) 0.043(4) Uani 1 1 d . . . . . H11 H 0.9644 0.1864 0.6296 0.051 Uiso 1 1 calc R U . . . C12 C 0.9039(16) 0.2198(6) 0.7728(16) 0.045(5) Uani 1 1 d . . . . . H12 H 0.9898 0.2116 0.8318 0.054 Uiso 1 1 calc R U . . . C13 C 0.9226(17) 0.2680(6) 0.7205(17) 0.048(5) Uani 1 1 d . . . . . C14 C 1.0401(18) 0.2791(6) 0.6885(17) 0.058(5) Uani 1 1 d . . . . . H14 H 1.1115 0.2574 0.6981 0.070 Uiso 1 1 calc R U . . . C15 C 1.057(2) 0.3281(7) 0.635(2) 0.082(7) Uani 1 1 d . . . . . H15 H 1.1361 0.3394 0.6140 0.099 Uiso 1 1 calc R U . . . C16 C 0.925(2) 0.3550(7) 0.623(2) 0.085(7) Uani 1 1 d . . . . . H16 H 0.9250 0.3860 0.5846 0.102 Uiso 1 1 calc R U . . . C17 C 0.803(2) 0.3227(7) 0.562(2) 0.085(7) Uani 1 1 d . . . . . H17A H 0.8259 0.2996 0.5043 0.102 Uiso 1 1 calc R U . . . H17B H 0.7187 0.3393 0.5249 0.102 Uiso 1 1 calc R U . . . C18 C 0.8101(18) 0.3043(6) 0.6958(18) 0.060(5) Uani 1 1 d . . . . . H18 H 0.7221 0.2951 0.7154 0.072 Uiso 1 1 calc R U . . . C19 C 0.868(2) 0.3540(6) 0.745(2) 0.070(6) Uani 1 1 d . . . . . C20 C 0.971(2) 0.3565(7) 0.867(2) 0.096(8) Uani 1 1 d . . . . . H20A H 1.0397 0.3325 0.8689 0.145 Uiso 1 1 calc R U . . . H20B H 0.9258 0.3518 0.9347 0.145 Uiso 1 1 calc R U . . . H20C H 1.0152 0.3867 0.8749 0.145 Uiso 1 1 calc R U . . . C21 C 0.748(3) 0.3890(7) 0.743(3) 0.116(9) Uani 1 1 d . . . . . H21A H 0.7835 0.4203 0.7562 0.174 Uiso 1 1 calc R U . . . H21B H 0.7004 0.3810 0.8075 0.174 Uiso 1 1 calc R U . . . H21C H 0.6843 0.3874 0.6625 0.174 Uiso 1 1 calc R U . . . C22 C 0.8294(18) 0.2418(5) 0.9557(18) 0.048(5) Uani 1 1 d . . . . . C23 C 0.7332(18) 0.2718(6) 0.9938(19) 0.060(5) Uani 1 1 d . . . . . H23 H 0.6481 0.2769 0.9399 0.072 Uiso 1 1 calc R U . . . C24 C 0.762(3) 0.2935(7) 1.108(2) 0.077(6) Uani 1 1 d . . . . . H24 H 0.6948 0.3112 1.1336 0.092 Uiso 1 1 calc R U . . . C25 C 0.886(3) 0.2895(8) 1.182(2) 0.077(7) Uani 1 1 d . . . . . C26 C 0.988(2) 0.2609(8) 1.155(2) 0.081(7) Uani 1 1 d . . . . . H26 H 1.0734 0.2581 1.2097 0.097 Uiso 1 1 calc R U . . . C27 C 0.956(2) 0.2368(6) 1.0422(18) 0.062(5) Uani 1 1 d . . . . . H27 H 1.0218 0.2164 1.0229 0.075 Uiso 1 1 calc R U . . . C28 C 0.3827(17) 0.2630(7) 0.8948(17) 0.058(5) Uani 1 1 d . . . . . C29 C 0.394(2) 0.3109(8) 0.875(2) 0.090(7) Uani 1 1 d . . . . . H29 H 0.4098 0.3211 0.7980 0.108 Uiso 1 1 calc R U . . . C30 C 0.383(2) 0.3435(8) 0.964(2) 0.081(6) Uani 1 1 d . . . . . H30 H 0.3870 0.3751 0.9443 0.097 Uiso 1 1 calc R U . . . C31 C 0.3655(17) 0.3309(6) 1.084(2) 0.065(5) Uani 1 1 d . . . . . C32 C 0.3532(19) 0.2823(6) 1.1008(19) 0.066(6) Uani 1 1 d . . . . . H32 H 0.3386 0.2713 1.1770 0.080 Uiso 1 1 calc R U . . . C33 C 0.3623(19) 0.2500(7) 1.0068(19) 0.063(6) Uani 1 1 d . . . . . H33 H 0.3538 0.2182 1.0227 0.075 Uiso 1 1 calc R U . . . C34 C 0.3556(17) 0.3660(5) 1.1928(18) 0.069(6) Uani 1 1 d D . . . . C35 C 0.484(2) 0.3610(9) 1.292(2) 0.075(8) Uiso 0.7 1 d D . P A 1 H35A H 0.5622 0.3690 1.2579 0.113 Uiso 0.7 1 calc R U P A 1 H35B H 0.4927 0.3292 1.3215 0.113 Uiso 0.7 1 calc R U P A 1 H35C H 0.4799 0.3817 1.3605 0.113 Uiso 0.7 1 calc R U P A 1 C36 C 0.234(3) 0.3534(10) 1.246(3) 0.080(8) Uiso 0.7 1 d D . P A 1 H36A H 0.1509 0.3570 1.1824 0.120 Uiso 0.7 1 calc R U P A 1 H36B H 0.2303 0.3738 1.3152 0.120 Uiso 0.7 1 calc R U P A 1 H36C H 0.2420 0.3215 1.2744 0.120 Uiso 0.7 1 calc R U P A 1 C37 C 0.338(3) 0.4152(9) 1.142(3) 0.094(10) Uiso 0.7 1 d D . P A 1 H37A H 0.4184 0.4239 1.1117 0.141 Uiso 0.7 1 calc R U P A 1 H37B H 0.3276 0.4363 1.2078 0.141 Uiso 0.7 1 calc R U P A 1 H37C H 0.2583 0.4168 1.0748 0.141 Uiso 0.7 1 calc R U P A 1 C35A C 0.482(5) 0.397(2) 1.219(8) 0.14(3) Uiso 0.3 1 d D . P A 2 H35D H 0.4781 0.4177 1.2859 0.212 Uiso 0.3 1 calc R U P A 2 H35E H 0.4864 0.4141 1.1446 0.212 Uiso 0.3 1 calc R U P A 2 H35F H 0.5629 0.3772 1.2417 0.212 Uiso 0.3 1 calc R U P A 2 C36A C 0.344(8) 0.342(3) 1.315(5) 0.14(4) Uiso 0.3 1 d D . P A 2 H36D H 0.2560 0.3276 1.3043 0.211 Uiso 0.3 1 calc R U P A 2 H36E H 0.3547 0.3654 1.3801 0.211 Uiso 0.3 1 calc R U P A 2 H36F H 0.4157 0.3192 1.3365 0.211 Uiso 0.3 1 calc R U P A 2 C37A C 0.231(5) 0.398(2) 1.154(7) 0.13(3) Uiso 0.3 1 d D . P A 2 H37D H 0.1494 0.3791 1.1270 0.197 Uiso 0.3 1 calc R U P A 2 H37E H 0.2430 0.4179 1.0870 0.197 Uiso 0.3 1 calc R U P A 2 H37F H 0.2207 0.4167 1.2246 0.197 Uiso 0.3 1 calc R U P A 2 C38 C 0.4810(17) 0.1295(6) 1.0573(15) 0.045(4) Uani 1 1 d . . . . . C39 C 0.360(2) 0.1184(9) 0.977(2) 0.091(8) Uani 1 1 d . . . . . H39 H 0.3548 0.1218 0.8912 0.109 Uiso 1 1 calc R U . . . C40 C 0.2478(17) 0.1028(7) 1.0150(17) 0.071(6) Uani 1 1 d . . . . . H40 H 0.1663 0.0977 0.9561 0.085 Uiso 1 1 calc R U . . . C41 C 0.2522(16) 0.0942(6) 1.1419(16) 0.050(4) Uani 1 1 d . . . . . C42 C 0.3751(18) 0.1052(8) 1.2238(18) 0.075(6) Uani 1 1 d . . . . . H42 H 0.3832 0.1015 1.3096 0.089 Uiso 1 1 calc R U . . . C43 C 0.484(2) 0.1215(7) 1.1799(18) 0.074(6) Uani 1 1 d . . . . . H43 H 0.5661 0.1276 1.2377 0.089 Uiso 1 1 calc R U . . . C44 C 0.1248(15) 0.0749(6) 1.1845(15) 0.056(5) Uani 1 1 d D . . . . C45 C 0.081(3) 0.0272(8) 1.122(2) 0.054(7) Uiso 0.6 1 d D . P B 1 H45A H 0.0009 0.0160 1.1488 0.082 Uiso 0.6 1 calc R U P B 1 H45B H 0.1547 0.0051 1.1458 0.082 Uiso 0.6 1 calc R U P B 1 H45C H 0.0594 0.0309 1.0325 0.082 Uiso 0.6 1 calc R U P B 1 C46 C 0.149(3) 0.0684(10) 1.326(2) 0.067(9) Uiso 0.6 1 d D . P B 1 H46A H 0.0664 0.0567 1.3473 0.100 Uiso 0.6 1 calc R U P B 1 H46B H 0.1731 0.0980 1.3670 0.100 Uiso 0.6 1 calc R U P B 1 H46C H 0.2226 0.0465 1.3533 0.100 Uiso 0.6 1 calc R U P B 1 C47 C 0.001(2) 0.1082(9) 1.139(3) 0.049(8) Uiso 0.6 1 d D . P B 1 H47A H -0.0782 0.0961 1.1649 0.073 Uiso 0.6 1 calc R U P B 1 H47B H -0.0177 0.1103 1.0490 0.073 Uiso 0.6 1 calc R U P B 1 H47C H 0.0233 0.1387 1.1744 0.073 Uiso 0.6 1 calc R U P B 1 C45A C 0.156(7) 0.0234(12) 1.216(6) 0.15(3) Uiso 0.4 1 d D . P B 2 H45D H 0.0790 0.0092 1.2413 0.223 Uiso 0.4 1 calc R U P B 2 H45E H 0.2365 0.0210 1.2828 0.223 Uiso 0.4 1 calc R U P B 2 H45F H 0.1726 0.0075 1.1431 0.223 Uiso 0.4 1 calc R U P B 2 C46A C 0.119(5) 0.1002(18) 1.308(4) 0.092(17) Uiso 0.4 1 d D . P B 2 H46D H 0.0406 0.0894 1.3380 0.139 Uiso 0.4 1 calc R U P B 2 H46E H 0.1118 0.1334 1.2940 0.139 Uiso 0.4 1 calc R U P B 2 H46F H 0.2018 0.0935 1.3700 0.139 Uiso 0.4 1 calc R U P B 2 C47A C -0.015(5) 0.080(3) 1.095(5) 0.22(5) Uiso 0.4 1 d D . P B 2 H47D H -0.0848 0.0660 1.1335 0.328 Uiso 0.4 1 calc R U P B 2 H47E H -0.0143 0.0634 1.0186 0.328 Uiso 0.4 1 calc R U P B 2 H47F H -0.0358 0.1121 1.0781 0.328 Uiso 0.4 1 calc R U P B 2 C48 C 0.5124(16) 0.0780(6) 0.5719(15) 0.046(4) Uani 1 1 d . . . . . C49 C 0.6135(16) 0.0889(7) 0.5061(16) 0.057(5) Uani 1 1 d . . . . . H49 H 0.6490 0.1192 0.5103 0.068 Uiso 1 1 calc R U . . . C50 C 0.6616(18) 0.0560(7) 0.4355(17) 0.064(6) Uani 1 1 d . . . . . H50 H 0.7292 0.0647 0.3929 0.077 Uiso 1 1 calc R U . . . C51 C 0.6146(17) 0.0108(7) 0.4247(17) 0.058(5) Uani 1 1 d . . . . . C52 C 0.518(2) 0.0003(7) 0.491(2) 0.083(7) Uani 1 1 d . . . . . H52 H 0.4836 -0.0302 0.4862 0.099 Uiso 1 1 calc R U . . . C53 C 0.4676(18) 0.0320(6) 0.5637(17) 0.062(5) Uani 1 1 d . . . . . H53 H 0.4027 0.0224 0.6082 0.074 Uiso 1 1 calc R U . . . C54 C 0.668(2) -0.0254(7) 0.338(2) 0.087(7) Uani 1 1 d D . . . . C55 C 0.792(4) -0.0145(15) 0.293(4) 0.102(15) Uiso 0.5 1 d D . P C 1 H55A H 0.8098 -0.0391 0.2385 0.153 Uiso 0.5 1 calc R U P C 1 H55B H 0.8691 -0.0118 0.3633 0.153 Uiso 0.5 1 calc R U P C 1 H55C H 0.7798 0.0146 0.2478 0.153 Uiso 0.5 1 calc R U P C 1 C56 C 0.549(4) -0.0254(15) 0.224(4) 0.108(17) Uiso 0.5 1 d D . P C 1 H56A H 0.5264 -0.0571 0.1972 0.161 Uiso 0.5 1 calc R U P C 1 H56B H 0.5753 -0.0084 0.1567 0.161 Uiso 0.5 1 calc R U P C 1 H56C H 0.4701 -0.0107 0.2445 0.161 Uiso 0.5 1 calc R U P C 1 C57 C 0.675(4) -0.0731(11) 0.393(4) 0.069(11) Uiso 0.5 1 d D U P C 1 H57A H 0.7162 -0.0715 0.4805 0.103 Uiso 0.5 1 calc R U P C 1 H57B H 0.7288 -0.0930 0.3515 0.103 Uiso 0.5 1 calc R U P C 1 H57C H 0.5831 -0.0857 0.3815 0.103 Uiso 0.5 1 calc R U P C 1 C55A C 0.824(3) -0.0281(15) 0.396(4) 0.103(16) Uiso 0.5 1 d D . P C 2 H55D H 0.8377 -0.0407 0.4792 0.154 Uiso 0.5 1 calc R U P C 2 H55E H 0.8628 0.0027 0.3990 0.154 Uiso 0.5 1 calc R U P C 2 H55F H 0.8673 -0.0481 0.3453 0.154 Uiso 0.5 1 calc R U P C 2 C56A C 0.661(5) -0.0064(18) 0.210(4) 0.126(19) Uiso 0.5 1 d D . P C 2 H56D H 0.7158 0.0215 0.2153 0.190 Uiso 0.5 1 calc R U P C 2 H56E H 0.5668 0.0009 0.1710 0.190 Uiso 0.5 1 calc R U P C 2 H56F H 0.6951 -0.0294 0.1600 0.190 Uiso 0.5 1 calc R U P C 2 C57A C 0.614(4) -0.0722(14) 0.334(4) 0.104(17) Uiso 0.5 1 d D U P C 2 H57D H 0.6647 -0.0921 0.2890 0.156 Uiso 0.5 1 calc R U P C 2 H57E H 0.5186 -0.0721 0.2920 0.156 Uiso 0.5 1 calc R U P C 2 H57F H 0.6235 -0.0838 0.4178 0.156 Uiso 0.5 1 calc R U P C 2 O1 O 1.196(3) -0.0106(10) 0.727(3) 0.088(8) Uani 0.5 1 d D U P . . C202 C 1.246(4) -0.0481(14) 0.898(3) 0.095(10) Uani 0.5 1 d D U P . . H20D H 1.3178 -0.0714 0.9192 0.114 Uiso 0.5 1 calc R U P . . H20E H 1.2259 -0.0355 0.9743 0.114 Uiso 0.5 1 calc R U P . . C201 C 1.282(4) -0.0150(14) 0.831(4) 0.091(10) Uani 0.5 1 d D U P . . H20F H 1.2888 0.0144 0.8767 0.109 Uiso 0.5 1 calc R U P . . H20G H 1.3726 -0.0220 0.8154 0.109 Uiso 0.5 1 calc R U P . . C203 C 1.136(4) -0.0662(14) 0.828(4) 0.105(11) Uani 0.5 1 d D U P . . H20H H 1.0532 -0.0542 0.8504 0.126 Uiso 0.5 1 calc R U P . . H20I H 1.1367 -0.1001 0.8346 0.126 Uiso 0.5 1 calc R U P . . C204 C 1.144(5) -0.0526(14) 0.715(4) 0.125(12) Uani 0.5 1 d D U P . . H20J H 1.2024 -0.0738 0.6807 0.151 Uiso 0.5 1 calc R U P . . H20K H 1.0531 -0.0523 0.6600 0.151 Uiso 0.5 1 calc R U P . . 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 Zr1 0.0391(8) 0.0537(9) 0.0450(10) -0.0007(10) 0.0138(7) 0.0003(9) S1 0.063(3) 0.110(5) 0.064(4) -0.013(3) 0.012(3) 0.032(3) S2 0.044(3) 0.072(3) 0.047(3) -0.002(2) 0.009(2) -0.011(2) S3 0.043(3) 0.079(3) 0.051(3) -0.010(2) 0.017(2) -0.008(2) N1 0.043(8) 0.055(9) 0.045(9) -0.002(7) 0.014(8) -0.004(7) N2 0.039(8) 0.043(8) 0.068(11) -0.006(7) 0.023(8) -0.002(6) N3 0.058(9) 0.043(8) 0.058(11) -0.001(7) 0.018(9) 0.007(7) N4 0.035(8) 0.051(9) 0.044(9) -0.002(6) 0.007(8) -0.003(6) N5 0.041(8) 0.044(8) 0.057(10) -0.019(7) 0.010(8) 0.000(6) F1 0.207(16) 0.119(11) 0.062(9) -0.046(8) 0.045(10) -0.054(10) C1 0.042(10) 0.051(11) 0.050(12) -0.003(9) 0.016(9) 0.017(9) C2 0.043(11) 0.054(11) 0.057(12) 0.008(10) 0.008(10) 0.010(9) C3 0.059(11) 0.035(10) 0.056(12) 0.009(9) 0.010(10) 0.016(8) C4 0.060(12) 0.071(14) 0.106(18) 0.023(12) 0.045(13) 0.021(10) C5 0.060(12) 0.058(12) 0.056(13) 0.008(10) -0.003(11) -0.004(9) C6 0.084(15) 0.037(9) 0.050(13) -0.007(8) 0.024(13) 0.001(9) C7 0.083(15) 0.061(12) 0.046(13) 0.014(10) 0.009(12) 0.001(11) C8 0.055(12) 0.084(14) 0.044(13) 0.020(11) -0.004(12) 0.006(10) C9 0.090(14) 0.078(14) 0.069(13) 0.011(10) 0.051(12) 0.017(10) C10 0.071(15) 0.14(2) 0.061(15) 0.024(14) 0.019(13) 0.016(13) C11 0.050(9) 0.032(10) 0.053(11) 0.004(9) 0.028(9) 0.002(8) C12 0.025(9) 0.061(12) 0.048(12) -0.011(9) 0.006(9) -0.009(8) C13 0.044(11) 0.041(10) 0.058(13) -0.008(9) 0.012(10) -0.012(8) C14 0.051(11) 0.048(11) 0.077(15) 0.001(10) 0.017(11) -0.005(9) C15 0.079(15) 0.065(14) 0.111(19) 0.008(12) 0.037(15) -0.017(11) C16 0.106(18) 0.049(12) 0.102(18) 0.017(12) 0.025(16) -0.023(12) C17 0.102(17) 0.063(14) 0.084(17) 0.018(12) 0.009(15) 0.003(12) C18 0.040(11) 0.066(13) 0.072(15) -0.006(11) 0.006(11) -0.006(9) C19 0.063(13) 0.045(11) 0.095(17) -0.013(11) 0.001(14) -0.003(9) C20 0.12(2) 0.067(15) 0.11(2) -0.034(13) 0.035(18) -0.019(13) C21 0.14(2) 0.063(15) 0.15(2) -0.001(15) 0.03(2) 0.023(14) C22 0.051(11) 0.041(10) 0.059(13) -0.005(9) 0.028(11) -0.012(8) C23 0.057(11) 0.052(11) 0.072(14) -0.025(10) 0.022(11) -0.016(9) C24 0.079(16) 0.075(15) 0.083(18) -0.019(13) 0.034(16) 0.000(12) C25 0.11(2) 0.079(15) 0.044(14) -0.020(11) 0.029(15) -0.043(15) C26 0.082(16) 0.081(16) 0.077(17) -0.024(13) 0.011(14) -0.035(13) C27 0.066(14) 0.068(13) 0.056(14) -0.015(10) 0.020(12) -0.012(10) C28 0.051(11) 0.080(14) 0.045(12) -0.016(10) 0.016(10) 0.007(10) C29 0.111(19) 0.089(18) 0.076(16) -0.016(14) 0.035(15) -0.002(14) C30 0.103(17) 0.067(14) 0.073(16) 0.025(12) 0.022(14) 0.015(12) C31 0.043(11) 0.054(12) 0.096(17) -0.002(11) 0.014(11) 0.009(8) C32 0.085(14) 0.043(11) 0.081(15) -0.004(10) 0.039(13) 0.001(10) C33 0.064(13) 0.055(12) 0.073(15) 0.004(11) 0.023(12) 0.010(10) C34 0.076(14) 0.040(10) 0.089(16) -0.010(10) 0.017(13) -0.009(9) C38 0.043(10) 0.063(11) 0.023(10) 0.007(8) -0.005(9) 0.003(8) C39 0.071(16) 0.16(2) 0.048(15) 0.021(15) 0.021(14) -0.032(15) C40 0.040(11) 0.132(19) 0.038(13) 0.005(11) 0.002(10) -0.016(11) C41 0.042(11) 0.063(11) 0.046(12) 0.002(9) 0.011(10) 0.005(8) C42 0.050(12) 0.130(19) 0.040(13) 0.008(11) 0.005(11) -0.030(12) C43 0.072(14) 0.096(15) 0.054(14) -0.003(11) 0.011(12) -0.027(12) C44 0.034(10) 0.081(13) 0.053(12) 0.002(10) 0.010(9) 0.002(8) C48 0.048(10) 0.056(11) 0.035(10) -0.005(8) 0.008(9) -0.003(8) C49 0.053(11) 0.078(13) 0.044(11) -0.008(10) 0.018(10) -0.012(9) C50 0.052(11) 0.086(15) 0.056(13) -0.026(11) 0.016(11) -0.031(10) C51 0.047(11) 0.069(13) 0.059(13) -0.019(10) 0.011(10) -0.007(9) C52 0.096(16) 0.078(15) 0.089(16) -0.015(12) 0.052(14) -0.038(12) C53 0.062(12) 0.070(13) 0.056(13) -0.007(10) 0.019(11) -0.028(10) C54 0.086(16) 0.074(15) 0.112(19) -0.022(13) 0.043(15) -0.020(11) O1 0.087(18) 0.082(16) 0.11(2) 0.040(17) 0.046(16) 0.013(14) C202 0.11(2) 0.08(2) 0.10(2) 0.010(19) 0.04(2) 0.015(19) C201 0.09(2) 0.071(19) 0.12(3) 0.015(19) 0.041(19) 0.013(17) C203 0.12(2) 0.07(2) 0.13(3) 0.03(2) 0.03(2) 0.000(19) C204 0.14(2) 0.11(2) 0.12(2) 0.01(2) 0.01(2) 0.03(2) 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N5 Zr1 N1 79.6(5) N5 Zr1 N3 78.5(5) N1 Zr1 N3 81.9(4) N5 Zr1 S2 92.6(4) N1 Zr1 S2 91.1(3) N3 Zr1 S2 169.5(4) N5 Zr1 S1 116.3(4) N1 Zr1 S1 161.6(4) N3 Zr1 S1 92.1(4) S2 Zr1 S1 96.96(17) N5 Zr1 S3 153.9(4) N1 Zr1 S3 80.9(3) N3 Zr1 S3 81.7(3) S2 Zr1 S3 105.02(15) S1 Zr1 S3 81.03(17) C28 S1 Zr1 115.0(6) C38 S2 Zr1 117.2(6) C48 S3 Zr1 118.8(6) C3 N1 N2 105.6(12) C3 N1 Zr1 136.5(10) N2 N1 Zr1 117.9(10) C1 N2 N1 111.2(13) C1 N2 C11 128.6(12) N1 N2 C11 120.2(12) C8 N3 N4 105.7(13) C8 N3 Zr1 138.2(11) N4 N3 Zr1 114.9(11) C6 N4 N3 111.9(15) C6 N4 C11 126.9(14) N3 N4 C11 121.1(12) C22 N5 C12 111.9(12) C22 N5 Zr1 120.2(9) C12 N5 Zr1 127.2(10) N2 C1 C2 106.2(13) N2 C1 C4 122.9(15) C2 C1 C4 130.9(15) C3 C2 C1 107.2(15) N1 C3 C2 109.7(14) N1 C3 C5 123.0(14) C2 C3 C5 127.2(15) C7 C6 N4 103.8(15) C7 C6 C9 131.6(18) N4 C6 C9 124.5(18) C6 C7 C8 110.6(17) N3 C8 C7 108.0(16) N3 C8 C10 122.0(17) C7 C8 C10 130.0(19) N4 C11 N2 111.5(13) N4 C11 C12 113.7(13) N2 C11 C12 112.2(13) N5 C12 C13 112.7(13) N5 C12 C11 112.3(12) C13 C12 C11 108.5(13) C14 C13 C18 116.9(16) C14 C13 C12 120.1(16) C18 C13 C12 122.9(14) C13 C14 C15 119.2(16) C16 C15 C14 109.6(15) C15 C16 C17 108.6(17) C15 C16 C19 113.0(18) C17 C16 C19 88.0(15) C16 C17 C18 85.5(16) C13 C18 C17 106.3(15) C13 C18 C19 110.7(15) C17 C18 C19 87.3(15) C20 C19 C21 111.2(19) C20 C19 C16 116.9(17) C21 C19 C16 113(2) C20 C19 C18 118.2(17) C21 C19 C18 110.3(17) C16 C19 C18 84.3(14) N5 C22 C27 124.7(15) N5 C22 C23 119.9(17) C27 C22 C23 115.4(16) C24 C23 C22 121.5(19) C25 C24 C23 120.1(19) C24 C25 C26 123.5(19) C24 C25 F1 121(2) C26 C25 F1 115(2) C25 C26 C27 117(2) C26 C27 C22 122.7(19) C33 C28 C29 116.9(18) C33 C28 S1 123.4(16) C29 C28 S1 119.6(15) C28 C29 C30 122(2) C29 C30 C31 122(2) C32 C31 C30 113.8(18) C32 C31 C34 120.5(18) C30 C31 C34 125.7(17) C31 C32 C33 122.2(18) C28 C33 C32 122.5(18) C35 C34 C36 109.4(16) C35 C34 C37 111.4(16) C36 C34 C37 109.2(16) C35A C34 C36A 108(2) C35A C34 C37A 108(2) C36A C34 C37A 107(2) C35 C34 C31 107.7(16) C36 C34 C31 109.3(16) C35A C34 C31 109(3) C37 C34 C31 109.7(18) C36A C34 C31 114(4) C37A C34 C31 111(3) C39 C38 C43 115.4(16) C39 C38 S2 126.7(13) C43 C38 S2 117.9(14) C38 C39 C40 123.3(19) C39 C40 C41 121.0(18) C40 C41 C42 115.6(15) C40 C41 C44 120.8(16) C42 C41 C44 123.6(15) C43 C42 C41 120.6(17) C42 C43 C38 123.9(19) C45A C44 C47A 110(2) C45A C44 C41 106(3) C47A C44 C41 118(3) C46 C44 C41 113.1(16) C45A C44 C46A 107(2) C47A C44 C46A 108(2) C41 C44 C46A 107(2) C46 C44 C45 108.0(15) C41 C44 C45 110.6(15) C46 C44 C47 109.8(15) C41 C44 C47 109.3(15) C45 C44 C47 105.7(15) C53 C48 C49 115.9(15) C53 C48 S3 120.2(12) C49 C48 S3 123.8(13) C50 C49 C48 121.3(17) C51 C50 C49 122.7(16) C50 C51 C52 115.6(16) C50 C51 C54 121.3(15) C52 C51 C54 123.1(17) C53 C52 C51 123.7(18) C52 C53 C48 120.7(16) C55 C54 C57 111(2) C57A C54 C56A 112(2) C55 C54 C56 107(2) C57 C54 C56 107.0(19) C57A C54 C55A 107(2) C56A C54 C55A 103.9(19) C57A C54 C51 117(2) C55 C54 C51 119(2) C57 C54 C51 111(2) C56A C54 C51 112(3) C56 C54 C51 101(2) C55A C54 C51 103(2) C201 O1 C204 100(3) C203 C202 C201 105(2) O1 C201 C202 111(2) C202 C203 C204 103(2) O1 C204 C203 107(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zr1 N5 2.111(13) Zr1 N1 2.334(13) Zr1 N3 2.427(15) Zr1 S2 2.485(5) Zr1 S1 2.520(5) Zr1 S3 2.575(5) S1 C28 1.757(17) S2 C38 1.779(16) S3 C48 1.762(16) N1 C3 1.330(19) N1 N2 1.397(16) N2 C1 1.330(19) N2 C11 1.47(2) N3 C8 1.33(2) N3 N4 1.397(16) N4 C6 1.36(2) N4 C11 1.421(19) N5 C22 1.40(2) N5 C12 1.453(18) F1 C25 1.40(2) C1 C2 1.39(2) C1 C4 1.50(2) C2 C3 1.39(2) C3 C5 1.49(2) C6 C7 1.36(2) C6 C9 1.48(2) C7 C8 1.39(2) C8 C10 1.49(2) C11 C12 1.53(2) C12 C13 1.52(2) C13 C14 1.33(2) C13 C18 1.50(2) C14 C15 1.54(2) C15 C16 1.50(3) C16 C17 1.55(3) C16 C19 1.55(3) C17 C18 1.54(3) C18 C19 1.58(2) C19 C20 1.49(3) C19 C21 1.56(3) C22 C27 1.41(2) C22 C23 1.41(2) C23 C24 1.36(3) C24 C25 1.32(3) C25 C26 1.38(3) C26 C27 1.39(3) C28 C33 1.34(2) C28 C29 1.39(3) C29 C30 1.37(3) C30 C31 1.41(3) C31 C32 1.41(2) C31 C34 1.57(2) C32 C33 1.40(2) C34 C35 1.49(2) C34 C36 1.50(2) C34 C35A 1.51(3) C34 C37 1.50(2) C34 C36A 1.52(3) C34 C37A 1.52(3) C38 C39 1.36(3) C38 C43 1.35(2) C39 C40 1.35(2) C40 C41 1.40(2) C41 C42 1.38(2) C41 C44 1.54(2) C42 C43 1.36(2) C44 C45A 1.53(3) C44 C47A 1.52(3) C44 C46 1.52(2) C44 C46A 1.54(3) C44 C45 1.54(2) C44 C47 1.54(2) C48 C53 1.38(2) C48 C49 1.39(2) C49 C50 1.37(2) C50 C51 1.37(2) C51 C52 1.36(2) C51 C54 1.57(2) C52 C53 1.37(2) C54 C57A 1.43(4) C54 C55 1.46(3) C54 C57 1.48(2) C54 C56A 1.49(3) C54 C56 1.52(3) C54 C55A 1.54(3) O1 C201 1.27(3) O1 C204 1.30(3) C202 C203 1.29(3) C202 C201 1.29(3) C203 C204 1.31(3)