#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:48:21 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257536 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705159.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_7705159 loop_ _publ_author_name 'He, Zhiyuan' 'Xue, Xiaolian' 'Liu, Yilan' 'Yu, Na' 'Krogman, Jeremy P.' _publ_section_title ; Aminolysis of bis[bis(trimethylsilyl)amido]-manganese, -iron, and -cobalt for the synthesis of mono- and bis-silylene complexes. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12586 _journal_page_last 12591 _journal_paper_doi 10.1039/d0dt00570c _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C30 H46 Cl4 Fe N4 Si2' _chemical_formula_sum 'C30 H46 Cl4 Fe N4 Si2' _chemical_formula_weight 716.54 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-12-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-02-14 deposited with the CCDC. 2020-08-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.599(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.4312(7) _cell_length_b 17.2983(12) _cell_length_c 19.8767(16) _cell_measurement_reflns_used 9982 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.407 _cell_measurement_theta_min 2.355 _cell_volume 3785.7(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.0551 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 65610 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.442 _diffrn_reflns_theta_min 2.128 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0777 before and 0.0641 after correction. The Ratio of minimum to maximum transmission is 0.8988. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.257 _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Diethyl Ether' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.359 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.106 _refine_ls_abs_structure_details ; Flack x determined using 4990 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.099(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 763 _refine_ls_number_reflns 15507 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0579 _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^)+(0.0998P)^2^+4.1885P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1535 _refine_ls_wR_factor_ref 0.1709 _reflns_Friedel_coverage 0.929 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 12310 _reflns_number_total 15507 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 7705159--7705168.cif.' _cod_database_code 7705159 _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. ; _shelx_estimated_absorpt_t_max 0.893 _shelx_estimated_absorpt_t_min 0.843 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C118(H118), C120(H120), C119(H119), C21(H21), C22(H22), C18(H18), C103(H103), C3(H3), C122(H122), C20(H20), C104(H104), C19(H19), C7(H7), C107(H107), C4(H4), C121(H121), C5(H5), C106(H106), C105(H105), C6(H6) 2.b Idealised Me refined as rotating group: C126(H12A,H12B,H12C), C110(H11D,H11E,H11F), C124(H12D,H12E,H12F), C30(H30A, H30B,H30C), C114(H11G,H11H,H11I), C24(H24A,H24B,H24C), C129(H12G,H12H,H12I), C125(H12J,H12K,H12L), C130(H13D,H13E,H13F), C111(H11J,H11K,H11L), C109(H10D, H10E,H10F), C10(H10A,H10B,H10C), C115(H11M,H11N,H11O), C113(H11P,H11Q,H11R), C26(H26A,H26B,H26C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C28(H28A,H28B, H28C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C9(H9A, H9B,H9C), C128(H12M,H12N,H12O), C14(H14A,H14B,H14C) ; _shelx_res_file ; TITL mo_hzy2181_0m_a.res in P2(1) mo_hzy2181_0m.res created by SHELXL-2018/3 at 15:34:27 on 16-Dec-2019 REM Old TITL mo_hzy2181_0m in P2(1) REM SHELXT solution in P2(1): R1 0.117, Rweak 0.019, Alpha 0.005 REM 0.396 for 10 systematic absences, Orientation as input REM Flack x = 0.146 ( 0.009 ) from 5163 Parsons' quotients REM Formula found by SHELXT: C60 N8 Si4 Cl8 Fe2 CELL 0.71073 11.4312 17.2983 19.8767 90 105.599 90 ZERR 4 0.0007 0.0012 0.0016 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl Fe N Si UNIT 120 184 16 4 16 8 L.S. 4 0 0 PLAN 20 SIZE 0.21 0.23 0.15 TEMP -123.15 list 4 fmap 2 53 acta REM REM REM WGHT 0.099800 4.188500 FVAR 0.38727 FE1 4 -0.167352 0.359129 0.500185 11.00000 0.02702 0.02347 = 0.03371 0.00083 0.00817 -0.00107 FE11 4 1.201711 0.653860 0.972486 11.00000 0.02395 0.02731 = 0.03232 -0.00437 0.00686 -0.00087 CL1 3 -0.020663 0.305471 0.456191 11.00000 0.02126 0.01858 = 0.03625 -0.00325 0.01534 0.00395 CL12 3 1.057742 0.716849 1.012145 11.00000 0.02120 0.03148 = 0.03411 -0.01009 0.01224 0.00775 CL11 3 1.353691 0.717135 0.942200 11.00000 0.03000 0.02786 = 0.05090 -0.00985 0.02170 -0.01198 CL2 3 -0.313981 0.287061 0.527336 11.00000 0.03607 0.03700 = 0.04685 0.00085 0.02240 -0.02370 CL14 3 1.169737 0.523859 0.803146 11.00000 0.03757 0.05318 = 0.04080 -0.01226 0.01668 0.00177 CL13 3 1.219435 0.487953 1.114949 11.00000 0.03702 0.05245 = 0.03856 0.00545 0.00984 -0.00877 CL3 3 -0.136771 0.483486 0.673778 11.00000 0.03927 0.04875 = 0.03688 -0.00605 0.01435 0.00948 CL4 3 -0.185888 0.528618 0.364004 11.00000 0.04053 0.04865 = 0.04577 0.01233 0.01326 -0.00723 SI1 6 -0.276908 0.452692 0.414113 11.00000 0.02574 0.02764 = 0.02908 0.00148 0.00640 0.00193 SI2 6 -0.054334 0.424700 0.606843 11.00000 0.02563 0.02662 = 0.03001 -0.00007 0.00666 0.00134 SI12 6 1.308605 0.564511 1.064310 11.00000 0.02434 0.03043 = 0.02915 -0.00224 0.00454 -0.00145 SI11 6 1.086333 0.583711 0.869189 11.00000 0.02515 0.03007 = 0.02727 -0.00380 0.00762 -0.00192 N3 5 0.090129 0.473838 0.610859 11.00000 0.02847 0.02583 = 0.03202 -0.00200 0.00626 0.00393 N101 5 1.450425 0.518005 1.061126 11.00000 0.02972 0.02917 = 0.02999 -0.00361 0.00837 -0.00081 N4 5 0.068707 0.368024 0.664129 11.00000 0.02826 0.02794 = 0.03582 0.00415 0.00598 0.00157 N104 5 0.945960 0.532691 0.867572 11.00000 0.02351 0.03113 = 0.02825 -0.00403 0.00580 -0.00052 N2 5 -0.407586 0.418840 0.345130 11.00000 0.02871 0.03358 = 0.03265 -0.00579 0.00787 0.00252 N1 5 -0.412623 0.504745 0.422483 11.00000 0.02576 0.02795 = 0.03767 -0.00090 0.00526 0.00377 N103 5 0.958752 0.635878 0.812501 11.00000 0.03032 0.03418 = 0.02988 0.00635 0.00863 -0.00092 N102 5 1.433050 0.606235 1.133693 11.00000 0.02922 0.03398 = 0.03173 -0.00633 0.00628 -0.00035 C16 1 0.150476 0.410377 0.643894 11.00000 0.02728 0.02887 = 0.02897 -0.00201 0.00707 0.00417 C118 1 0.723160 0.655372 0.877768 11.00000 0.03912 0.03712 = 0.02989 0.00239 0.00802 0.00259 AFIX 43 H118 2 0.786238 0.675866 0.914824 11.00000 -1.20000 AFIX 0 C120 1 0.509177 0.639596 0.819062 11.00000 0.03214 0.04194 = 0.04972 0.01778 0.01696 0.00819 AFIX 43 H120 2 0.426330 0.649159 0.816693 11.00000 -1.20000 AFIX 0 C117 1 0.751057 0.607821 0.826705 11.00000 0.02476 0.03514 = 0.02856 0.00587 0.00396 0.00095 C17 1 0.279608 0.390922 0.649195 11.00000 0.03226 0.02676 = 0.03644 0.00430 0.00967 0.00344 C27 1 0.125918 0.539468 0.573803 11.00000 0.03518 0.02478 = 0.03403 -0.00113 0.00685 0.00057 C119 1 0.600723 0.672252 0.873345 11.00000 0.04599 0.04238 = 0.04819 0.01211 0.02438 0.00793 AFIX 43 H119 2 0.580385 0.705306 0.906668 11.00000 -1.20000 AFIX 0 C21 1 0.492180 0.397183 0.708452 11.00000 0.03112 0.03911 = 0.05559 0.01430 -0.00263 -0.00164 AFIX 43 H21 2 0.556349 0.414173 0.746700 11.00000 -1.20000 AFIX 0 C116 1 0.880544 0.591817 0.833609 11.00000 0.02490 0.03224 = 0.01843 -0.00311 0.00167 -0.00487 C22 1 0.371721 0.415878 0.705765 11.00000 0.02873 0.04004 = 0.04409 -0.00115 0.00747 0.00003 AFIX 43 H22 2 0.353477 0.445159 0.742095 11.00000 -1.20000 AFIX 0 C1 1 -0.482799 0.457389 0.374265 11.00000 0.02683 0.02684 = 0.03152 0.00059 0.00938 -0.00035 C2 1 -0.616579 0.448716 0.358759 11.00000 0.02740 0.03818 = 0.03488 -0.00573 0.00993 -0.00240 C112 1 1.487166 0.461314 1.014707 11.00000 0.02973 0.03098 = 0.04390 -0.00701 0.01369 0.00257 C18 1 0.304255 0.347230 0.596735 11.00000 0.03463 0.04009 = 0.03161 0.00429 0.00679 0.00756 AFIX 43 H18 2 0.240121 0.330015 0.558570 11.00000 -1.20000 AFIX 0 C102 1 1.646473 0.586778 1.119913 11.00000 0.02863 0.03473 = 0.03390 -0.00386 0.00995 -0.00358 C103 1 1.684035 0.634877 1.073533 11.00000 0.04002 0.04756 = 0.03858 -0.00869 0.01460 -0.01110 AFIX 43 H103 2 1.625933 0.659091 1.036185 11.00000 -1.20000 AFIX 0 C127 1 0.941220 0.711269 0.772587 11.00000 0.04055 0.03499 = 0.03680 0.00702 0.00426 -0.00157 C101 1 1.514367 0.570416 1.106837 11.00000 0.02654 0.03122 = 0.02612 0.00459 0.00102 -0.00176 C3 1 -0.693393 0.487203 0.304278 11.00000 0.03421 0.05685 = 0.04664 0.00468 0.00866 0.00834 AFIX 43 H3 2 -0.661358 0.519254 0.274716 11.00000 -1.20000 AFIX 0 C123 1 0.914941 0.468257 0.908857 11.00000 0.02852 0.02883 = 0.03062 0.00148 0.00703 -0.00811 C108 1 1.445775 0.676497 1.178438 11.00000 0.03698 0.03659 = 0.03400 -0.00798 0.01045 -0.00416 C12 1 -0.430714 0.352613 0.296143 11.00000 0.03752 0.03899 = 0.03805 -0.00466 0.01054 0.00354 C126 1 1.025498 0.415148 0.926248 11.00000 0.04738 0.02947 = 0.06354 0.01285 0.01616 -0.00121 AFIX 137 H12A 2 1.038814 0.394699 0.882922 11.00000 -1.50000 H12B 2 1.011511 0.372232 0.955324 11.00000 -1.50000 H12C 2 1.097214 0.444384 0.951672 11.00000 -1.50000 AFIX 0 C23 1 0.078839 0.292571 0.700272 11.00000 0.03984 0.03672 = 0.03529 0.01078 0.01078 0.01121 C110 1 1.480134 0.747396 1.141993 11.00000 0.05705 0.04047 = 0.04432 -0.00876 0.00870 -0.00502 AFIX 137 H11D 2 1.560511 0.739557 1.134371 11.00000 -1.50000 H11E 2 1.481908 0.793165 1.171307 11.00000 -1.50000 H11F 2 1.420013 0.754924 1.096933 11.00000 -1.50000 AFIX 0 C122 1 0.659674 0.577892 0.772963 11.00000 0.03504 0.03875 = 0.03848 -0.00055 0.00300 -0.00085 AFIX 43 H122 2 0.679165 0.546348 0.738372 11.00000 -1.20000 AFIX 0 C20 1 0.517889 0.354147 0.655681 11.00000 0.02905 0.04393 = 0.05573 0.01835 0.01686 0.01183 AFIX 43 H20 2 0.599859 0.342254 0.657606 11.00000 -1.20000 AFIX 0 C124 1 0.890637 0.497863 0.976014 11.00000 0.04576 0.05029 = 0.03270 0.00523 0.01703 0.00271 AFIX 137 H12D 2 0.954303 0.534602 0.998700 11.00000 -1.50000 H12E 2 0.890490 0.454301 1.007513 11.00000 -1.50000 H12F 2 0.811482 0.523732 0.965032 11.00000 -1.50000 AFIX 0 C30 1 0.016786 0.592789 0.554537 11.00000 0.04996 0.03171 = 0.05261 0.00949 0.01680 0.00521 AFIX 137 H30A 2 -0.050781 0.566465 0.521609 11.00000 -1.50000 H30B 2 0.037796 0.639759 0.532796 11.00000 -1.50000 H30C 2 -0.007227 0.606624 0.596747 11.00000 -1.50000 AFIX 0 C104 1 1.808356 0.647153 1.082549 11.00000 0.05005 0.06843 = 0.04894 -0.02292 0.02634 -0.02238 AFIX 43 H104 2 1.835300 0.678741 1.050579 11.00000 -1.20000 AFIX 0 C19 1 0.425858 0.328309 0.600300 11.00000 0.04067 0.04307 = 0.05296 0.01427 0.02185 0.01293 AFIX 43 H19 2 0.444133 0.297881 0.564648 11.00000 -1.20000 AFIX 0 C114 1 1.498025 0.501863 0.947234 11.00000 0.05371 0.05098 = 0.03643 -0.00643 0.01402 0.00730 AFIX 137 H11G 2 1.425483 0.533376 0.928010 11.00000 -1.50000 H11H 2 1.505328 0.462818 0.912869 11.00000 -1.50000 H11I 2 1.570139 0.535069 0.958102 11.00000 -1.50000 AFIX 0 C24 1 0.180327 0.295994 0.768629 11.00000 0.04930 0.04900 = 0.04837 0.01682 -0.00097 0.00139 AFIX 137 H24A 2 0.259345 0.296510 0.758157 11.00000 -1.50000 H24B 2 0.175124 0.250608 0.797193 11.00000 -1.50000 H24C 2 0.171423 0.343052 0.794258 11.00000 -1.50000 AFIX 0 C7 1 -0.662921 0.399077 0.401760 11.00000 0.04756 0.04678 = 0.04163 -0.01043 0.01968 -0.00748 AFIX 43 H7 2 -0.609696 0.370729 0.438389 11.00000 -1.20000 AFIX 0 C107 1 1.729530 0.554057 1.176145 11.00000 0.03092 0.05732 = 0.04085 -0.00068 0.00232 0.00560 AFIX 43 H107 2 1.703011 0.523087 1.208679 11.00000 -1.20000 AFIX 0 C129 1 0.908452 0.776471 0.815875 11.00000 0.10836 0.03626 = 0.07923 0.00965 0.04386 0.00802 AFIX 137 H12G 2 0.827596 0.767031 0.822277 11.00000 -1.50000 H12H 2 0.908398 0.825775 0.791582 11.00000 -1.50000 H12I 2 0.968305 0.778502 0.861580 11.00000 -1.50000 AFIX 0 C125 1 0.803910 0.422155 0.864487 11.00000 0.04272 0.04442 = 0.05040 -0.00753 0.00125 -0.01845 AFIX 137 H12J 2 0.730129 0.453292 0.858202 11.00000 -1.50000 H12K 2 0.795238 0.373942 0.888586 11.00000 -1.50000 H12L 2 0.816458 0.410206 0.818736 11.00000 -1.50000 AFIX 0 C130 1 0.841874 0.700481 0.704179 11.00000 0.06073 0.04926 = 0.05126 0.02189 -0.00388 -0.00112 AFIX 137 H13D 2 0.859244 0.654160 0.680159 11.00000 -1.50000 H13E 2 0.839708 0.745775 0.674253 11.00000 -1.50000 H13F 2 0.763063 0.694602 0.714327 11.00000 -1.50000 AFIX 0 C111 1 1.320911 0.688519 1.191105 11.00000 0.03651 0.04662 = 0.04560 -0.02010 0.00711 0.00618 AFIX 137 H11J 2 1.260276 0.696567 1.146320 11.00000 -1.50000 H11K 2 1.323291 0.733930 1.220924 11.00000 -1.50000 H11L 2 1.299125 0.642768 1.214192 11.00000 -1.50000 AFIX 0 C109 1 1.540113 0.660038 1.248441 11.00000 0.03658 0.05477 = 0.03260 -0.00927 -0.00257 0.00313 AFIX 137 H10D 2 1.526346 0.608276 1.264844 11.00000 -1.50000 H10E 2 1.532002 0.698543 1.283071 11.00000 -1.50000 H10F 2 1.622005 0.662824 1.241940 11.00000 -1.50000 AFIX 0 C4 1 -0.816567 0.479391 0.292488 11.00000 0.03028 0.09015 = 0.05776 -0.01372 0.00527 0.00539 AFIX 43 H4 2 -0.869562 0.506278 0.254711 11.00000 -1.20000 AFIX 0 C8 1 -0.440241 0.559392 0.472991 11.00000 0.04102 0.02899 = 0.04451 -0.00843 0.01421 0.00876 C10 1 -0.329326 0.607945 0.498576 11.00000 0.04985 0.04781 = 0.06242 -0.02173 0.02179 -0.00754 AFIX 137 H10A 2 -0.265205 0.577247 0.529837 11.00000 -1.50000 H10B 2 -0.348434 0.652663 0.523981 11.00000 -1.50000 H10C 2 -0.301465 0.625825 0.458719 11.00000 -1.50000 AFIX 0 C115 1 1.388672 0.400294 0.998478 11.00000 0.06381 0.04734 = 0.08027 -0.03208 0.02895 -0.01357 AFIX 137 H11M 2 1.385276 0.374492 1.041807 11.00000 -1.50000 H11N 2 1.406758 0.362146 0.966228 11.00000 -1.50000 H11O 2 1.310204 0.424732 0.976892 11.00000 -1.50000 AFIX 0 C121 1 0.538211 0.593991 0.769384 11.00000 0.03189 0.03835 = 0.05192 0.01257 0.00395 -0.00250 AFIX 43 H121 2 0.475420 0.573220 0.732327 11.00000 -1.20000 AFIX 0 C5 1 -0.864154 0.433231 0.334579 11.00000 0.03373 0.09687 = 0.07882 -0.04446 0.03523 -0.02097 AFIX 43 H5 2 -0.949737 0.429039 0.326209 11.00000 -1.20000 AFIX 0 C113 1 1.608817 0.422041 1.051434 11.00000 0.04941 0.03402 = 0.06284 -0.00274 0.01573 0.01222 AFIX 137 H11P 2 1.674071 0.460561 1.060758 11.00000 -1.50000 H11Q 2 1.626373 0.381353 1.021248 11.00000 -1.50000 H11R 2 1.603248 0.399274 1.095614 11.00000 -1.50000 AFIX 0 C26 1 -0.040484 0.281882 0.718196 11.00000 0.04879 0.05930 = 0.06833 0.03047 0.01686 0.00526 AFIX 137 H26A 2 -0.058240 0.328103 0.742210 11.00000 -1.50000 H26B 2 -0.035087 0.236835 0.748780 11.00000 -1.50000 H26C 2 -0.105518 0.273774 0.675224 11.00000 -1.50000 AFIX 0 C13 1 -0.309414 0.335063 0.283569 11.00000 0.05529 0.06568 = 0.05145 -0.02107 0.01056 0.00987 AFIX 137 H13A 2 -0.277479 0.381768 0.266925 11.00000 -1.50000 H13B 2 -0.318990 0.294217 0.248338 11.00000 -1.50000 H13C 2 -0.252764 0.317773 0.327255 11.00000 -1.50000 AFIX 0 C29 1 0.233804 0.581294 0.621798 11.00000 0.04832 0.03651 = 0.05347 0.00391 -0.00021 -0.01513 AFIX 137 H29A 2 0.214662 0.594948 0.665499 11.00000 -1.50000 H29B 2 0.251017 0.628424 0.598816 11.00000 -1.50000 H29C 2 0.305121 0.547411 0.631948 11.00000 -1.50000 AFIX 0 C106 1 1.854123 0.567184 1.184660 11.00000 0.03321 0.07287 = 0.05312 -0.01724 0.00079 0.00763 AFIX 43 H106 2 1.912376 0.544190 1.222698 11.00000 -1.20000 AFIX 0 C28 1 0.156297 0.510530 0.506610 11.00000 0.05286 0.04123 = 0.04148 0.00917 0.01851 0.00334 AFIX 137 H28A 2 0.226867 0.476068 0.519347 11.00000 -1.50000 H28B 2 0.174744 0.554855 0.480508 11.00000 -1.50000 H28C 2 0.086480 0.482378 0.477510 11.00000 -1.50000 AFIX 0 C105 1 1.891770 0.613099 1.138195 11.00000 0.02875 0.08162 = 0.04701 -0.02850 0.01216 -0.00563 AFIX 43 H105 2 1.976097 0.621589 1.144321 11.00000 -1.20000 AFIX 0 C6 1 -0.788145 0.392565 0.389351 11.00000 0.05046 0.06268 = 0.05464 -0.02937 0.03039 -0.02608 AFIX 43 H6 2 -0.821545 0.360421 0.418237 11.00000 -1.20000 AFIX 0 C15 1 -0.518767 0.375852 0.227094 11.00000 0.05624 0.07215 = 0.03916 -0.02151 -0.00085 0.00567 AFIX 137 H15A 2 -0.597690 0.388722 0.234744 11.00000 -1.50000 H15B 2 -0.528542 0.332811 0.193983 11.00000 -1.50000 H15C 2 -0.486780 0.420988 0.208084 11.00000 -1.50000 AFIX 0 C25 1 0.098306 0.227863 0.652546 11.00000 0.09362 0.02667 = 0.06264 0.00425 0.02779 0.00375 AFIX 137 H25A 2 0.031397 0.227696 0.609684 11.00000 -1.50000 H25B 2 0.100788 0.178114 0.676477 11.00000 -1.50000 H25C 2 0.175268 0.236110 0.640743 11.00000 -1.50000 AFIX 0 C11 1 -0.548542 0.609764 0.438694 11.00000 0.04972 0.04080 = 0.06555 -0.00526 0.00801 0.01555 AFIX 137 H11A 2 -0.534422 0.634960 0.397417 11.00000 -1.50000 H11B 2 -0.559436 0.649205 0.471885 11.00000 -1.50000 H11C 2 -0.621711 0.577658 0.424632 11.00000 -1.50000 AFIX 0 C9 1 -0.462058 0.514778 0.535227 11.00000 0.06209 0.06007 = 0.04005 -0.00871 0.01277 0.00655 AFIX 137 H9A 2 -0.533371 0.481394 0.519064 11.00000 -1.50000 H9B 2 -0.476016 0.551434 0.569857 11.00000 -1.50000 H9C 2 -0.390722 0.483010 0.556511 11.00000 -1.50000 AFIX 0 C128 1 1.060803 0.726100 0.756327 11.00000 0.04928 0.06604 = 0.07783 0.03053 0.02427 -0.00839 AFIX 137 H12M 2 1.122962 0.738271 0.799603 11.00000 -1.50000 H12N 2 1.052029 0.769750 0.723918 11.00000 -1.50000 H12O 2 1.085090 0.679913 0.734900 11.00000 -1.50000 AFIX 0 C14 1 -0.477434 0.282562 0.328915 11.00000 0.09238 0.03554 = 0.06686 -0.02062 0.03450 -0.01459 AFIX 137 H14A 2 -0.422434 0.272150 0.375112 11.00000 -1.50000 H14B 2 -0.480712 0.237230 0.298892 11.00000 -1.50000 H14C 2 -0.558928 0.293667 0.333626 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_hzy2181_0m_a.res in P2(1) REM wR2 = 0.1709, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0579 for 12310 Fo > 4sig(Fo) and 0.0806 for all 15507 data REM 763 parameters refined using 1 restraints END WGHT 0.0998 4.1885 REM Highest difference peak 1.359, deepest hole -0.676, 1-sigma level 0.106 Q1 1 -0.3350 0.3007 0.5223 11.00000 0.05 1.18 Q2 1 1.0184 0.7058 1.0824 11.00000 0.05 0.36 Q3 1 -0.8594 0.3622 0.4237 11.00000 0.05 0.33 Q4 1 1.0799 0.8257 0.7773 11.00000 0.05 0.32 Q5 1 1.9588 0.7114 1.0678 11.00000 0.05 0.30 Q6 1 1.4104 0.6832 1.2801 11.00000 0.05 0.30 Q7 1 1.6652 0.5243 1.2758 11.00000 0.05 0.29 Q8 1 1.5784 0.5737 1.2200 11.00000 0.05 0.29 Q9 1 0.0352 0.3646 0.7997 11.00000 0.05 0.29 Q10 1 0.4359 0.6664 0.7637 11.00000 0.05 0.29 Q11 1 -0.9261 0.4263 0.2120 11.00000 0.05 0.29 Q12 1 1.4985 0.7652 1.2436 11.00000 0.05 0.28 Q13 1 -0.0380 0.4797 0.6654 11.00000 0.05 0.27 Q14 1 -0.0237 0.3986 0.7763 11.00000 0.05 0.27 Q15 1 0.2056 0.2185 0.7043 11.00000 0.05 0.27 Q16 1 -0.2959 0.7216 0.4234 11.00000 0.05 0.27 Q17 1 -0.6610 0.3696 0.2777 11.00000 0.05 0.27 Q18 1 0.0584 0.1201 0.5799 11.00000 0.05 0.27 Q19 1 -0.2130 0.3447 0.7375 11.00000 0.05 0.27 Q20 1 0.1337 0.1802 0.7474 11.00000 0.05 0.27 ; _shelx_res_checksum 50233 _olex2_submission_special_instructions 'No special instructions were received' 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 Fe1 Fe -0.16735(10) 0.35913(6) 0.50019(6) 0.0281(3) Uani 1 1 d . . . . . Fe11 Fe 1.20171(9) 0.65386(6) 0.97249(6) 0.0280(3) Uani 1 1 d . . . . . Cl1 Cl -0.02066(15) 0.30547(9) 0.45619(10) 0.0239(4) Uani 1 1 d . . . . . Cl12 Cl 1.05774(15) 0.71685(11) 1.01215(10) 0.0280(4) Uani 1 1 d . . . . . Cl11 Cl 1.35369(17) 0.71713(11) 0.94220(11) 0.0342(4) Uani 1 1 d . . . . . Cl2 Cl -0.31398(18) 0.28706(12) 0.52734(12) 0.0378(5) Uani 1 1 d . . . . . Cl14 Cl 1.16974(19) 0.52386(14) 0.80315(12) 0.0427(5) Uani 1 1 d . . . . . Cl13 Cl 1.21944(19) 0.48795(14) 1.11495(12) 0.0427(5) Uani 1 1 d . . . . . Cl3 Cl -0.13677(19) 0.48349(14) 0.67378(11) 0.0408(5) Uani 1 1 d . . . . . Cl4 Cl -0.1859(2) 0.52862(14) 0.36400(12) 0.0447(5) Uani 1 1 d . . . . . Si1 Si -0.27691(19) 0.45269(12) 0.41411(12) 0.0277(5) Uani 1 1 d . . . . . Si2 Si -0.05433(19) 0.42470(12) 0.60684(12) 0.0276(5) Uani 1 1 d . . . . . Si12 Si 1.30860(19) 0.56451(13) 1.06431(12) 0.0285(5) Uani 1 1 d . . . . . Si11 Si 1.08633(19) 0.58371(12) 0.86919(12) 0.0274(5) Uani 1 1 d . . . . . N3 N 0.0901(6) 0.4738(4) 0.6109(3) 0.0291(14) Uani 1 1 d . . . . . N101 N 1.4504(6) 0.5180(4) 1.0611(3) 0.0296(14) Uani 1 1 d . . . . . N4 N 0.0687(6) 0.3680(4) 0.6641(4) 0.0312(15) Uani 1 1 d . . . . . N104 N 0.9460(5) 0.5327(4) 0.8676(3) 0.0279(14) Uani 1 1 d . . . . . N2 N -0.4076(6) 0.4188(4) 0.3451(4) 0.0317(15) Uani 1 1 d . . . . . N1 N -0.4126(6) 0.5047(4) 0.4225(4) 0.0311(15) Uani 1 1 d . . . . . N103 N 0.9588(6) 0.6359(4) 0.8125(4) 0.0314(15) Uani 1 1 d . . . . . N102 N 1.4331(6) 0.6062(4) 1.1337(4) 0.0320(15) Uani 1 1 d . . . . . C16 C 0.1505(7) 0.4104(5) 0.6439(4) 0.0285(17) Uani 1 1 d . . . . . C118 C 0.7232(8) 0.6554(5) 0.8778(4) 0.0356(18) Uani 1 1 d . . . . . H118 H 0.786238 0.675866 0.914824 0.043 Uiso 1 1 calc R . . . . C120 C 0.5092(8) 0.6396(5) 0.8191(5) 0.040(2) Uani 1 1 d . . . . . H120 H 0.426330 0.649159 0.816693 0.048 Uiso 1 1 calc R . . . . C117 C 0.7511(7) 0.6078(5) 0.8267(4) 0.0301(17) Uani 1 1 d . . . . . C17 C 0.2796(7) 0.3909(5) 0.6492(4) 0.0317(18) Uani 1 1 d . . . . . C27 C 0.1259(7) 0.5395(5) 0.5738(4) 0.0318(17) Uani 1 1 d . . . . . C119 C 0.6007(8) 0.6723(5) 0.8733(5) 0.043(2) Uani 1 1 d . . . . . H119 H 0.580385 0.705306 0.906668 0.052 Uiso 1 1 calc R . . . . C21 C 0.4922(8) 0.3972(5) 0.7085(6) 0.045(2) Uani 1 1 d . . . . . H21 H 0.556349 0.414173 0.746700 0.054 Uiso 1 1 calc R . . . . C116 C 0.8805(7) 0.5918(5) 0.8336(4) 0.0260(16) Uani 1 1 d . . . . . C22 C 0.3717(7) 0.4159(5) 0.7058(5) 0.0381(19) Uani 1 1 d . . . . . H22 H 0.353477 0.445159 0.742095 0.046 Uiso 1 1 calc R . . . . C1 C -0.4828(7) 0.4574(4) 0.3743(4) 0.0281(16) Uani 1 1 d . . . . . C2 C -0.6166(7) 0.4487(5) 0.3588(4) 0.0332(18) Uani 1 1 d . . . . . C112 C 1.4872(7) 0.4613(5) 1.0147(5) 0.0341(18) Uani 1 1 d . . . . . C18 C 0.3043(8) 0.3472(5) 0.5967(4) 0.0359(19) Uani 1 1 d . . . . . H18 H 0.240121 0.330015 0.558570 0.043 Uiso 1 1 calc R . . . . C102 C 1.6465(7) 0.5868(5) 1.1199(4) 0.0321(18) Uani 1 1 d . . . . . C103 C 1.6840(8) 0.6349(5) 1.0735(5) 0.041(2) Uani 1 1 d . . . . . H103 H 1.625933 0.659091 1.036185 0.050 Uiso 1 1 calc R . . . . C127 C 0.9412(8) 0.7113(5) 0.7726(5) 0.039(2) Uani 1 1 d . . . . . C101 C 1.5144(7) 0.5704(5) 1.1068(4) 0.0291(16) Uani 1 1 d . . . . . C3 C -0.6934(8) 0.4872(6) 0.3043(5) 0.046(2) Uani 1 1 d . . . . . H3 H -0.661358 0.519254 0.274716 0.056 Uiso 1 1 calc R . . . . C123 C 0.9149(7) 0.4683(5) 0.9089(4) 0.0295(17) Uani 1 1 d . . . . . C108 C 1.4458(8) 0.6765(5) 1.1784(5) 0.0357(19) Uani 1 1 d . . . . . C12 C -0.4307(8) 0.3526(5) 0.2961(5) 0.0381(19) Uani 1 1 d . . . . . C126 C 1.0255(9) 0.4151(5) 0.9262(6) 0.047(2) Uani 1 1 d . . . . . H12A H 1.038814 0.394699 0.882922 0.070 Uiso 1 1 calc GR . . . . H12B H 1.011511 0.372232 0.955324 0.070 Uiso 1 1 calc GR . . . . H12C H 1.097214 0.444384 0.951672 0.070 Uiso 1 1 calc GR . . . . C23 C 0.0788(8) 0.2926(5) 0.7003(5) 0.037(2) Uani 1 1 d . . . . . C110 C 1.4801(9) 0.7474(6) 1.1420(5) 0.048(2) Uani 1 1 d . . . . . H11D H 1.560511 0.739557 1.134371 0.072 Uiso 1 1 calc GR . . . . H11E H 1.481908 0.793165 1.171307 0.072 Uiso 1 1 calc GR . . . . H11F H 1.420013 0.754924 1.096933 0.072 Uiso 1 1 calc GR . . . . C122 C 0.6597(8) 0.5779(5) 0.7730(5) 0.039(2) Uani 1 1 d . . . . . H122 H 0.679165 0.546348 0.738372 0.047 Uiso 1 1 calc R . . . . C20 C 0.5179(8) 0.3541(6) 0.6557(5) 0.042(2) Uani 1 1 d . . . . . H20 H 0.599859 0.342254 0.657606 0.050 Uiso 1 1 calc R . . . . C124 C 0.8906(8) 0.4979(6) 0.9760(5) 0.042(2) Uani 1 1 d . . . . . H12D H 0.954303 0.534602 0.998700 0.062 Uiso 1 1 calc GR . . . . H12E H 0.890490 0.454301 1.007513 0.062 Uiso 1 1 calc GR . . . . H12F H 0.811482 0.523732 0.965032 0.062 Uiso 1 1 calc GR . . . . C30 C 0.0168(9) 0.5928(5) 0.5545(5) 0.044(2) Uani 1 1 d . . . . . H30A H -0.050781 0.566465 0.521609 0.066 Uiso 1 1 calc GR . . . . H30B H 0.037796 0.639759 0.532796 0.066 Uiso 1 1 calc GR . . . . H30C H -0.007227 0.606624 0.596747 0.066 Uiso 1 1 calc GR . . . . C104 C 1.8084(9) 0.6472(7) 1.0825(5) 0.053(3) Uani 1 1 d . . . . . H104 H 1.835300 0.678741 1.050579 0.064 Uiso 1 1 calc R . . . . C19 C 0.4259(8) 0.3283(6) 0.6003(5) 0.044(2) Uani 1 1 d . . . . . H19 H 0.444133 0.297881 0.564648 0.053 Uiso 1 1 calc R . . . . C114 C 1.4980(9) 0.5019(6) 0.9472(5) 0.047(2) Uani 1 1 d . . . . . H11G H 1.425483 0.533376 0.928010 0.070 Uiso 1 1 calc GR . . . . H11H H 1.505328 0.462818 0.912869 0.070 Uiso 1 1 calc GR . . . . H11I H 1.570139 0.535069 0.958102 0.070 Uiso 1 1 calc GR . . . . C24 C 0.1803(9) 0.2960(6) 0.7686(5) 0.052(3) Uani 1 1 d . . . . . H24A H 0.259345 0.296510 0.758157 0.077 Uiso 1 1 calc GR . . . . H24B H 0.175124 0.250608 0.797193 0.077 Uiso 1 1 calc GR . . . . H24C H 0.171423 0.343052 0.794258 0.077 Uiso 1 1 calc GR . . . . C7 C -0.6629(9) 0.3991(6) 0.4018(5) 0.044(2) Uani 1 1 d . . . . . H7 H -0.609696 0.370729 0.438389 0.053 Uiso 1 1 calc R . . . . C107 C 1.7295(8) 0.5541(6) 1.1761(5) 0.044(2) Uani 1 1 d . . . . . H107 H 1.703011 0.523087 1.208679 0.053 Uiso 1 1 calc R . . . . C129 C 0.9085(13) 0.7765(7) 0.8159(7) 0.071(4) Uani 1 1 d . . . . . H12G H 0.827596 0.767031 0.822277 0.107 Uiso 1 1 calc GR . . . . H12H H 0.908398 0.825775 0.791582 0.107 Uiso 1 1 calc GR . . . . H12I H 0.968305 0.778502 0.861580 0.107 Uiso 1 1 calc GR . . . . C125 C 0.8039(8) 0.4222(6) 0.8645(5) 0.048(2) Uani 1 1 d . . . . . H12J H 0.730129 0.453292 0.858202 0.072 Uiso 1 1 calc GR . . . . H12K H 0.795238 0.373942 0.888586 0.072 Uiso 1 1 calc GR . . . . H12L H 0.816458 0.410206 0.818736 0.072 Uiso 1 1 calc GR . . . . C130 C 0.8419(10) 0.7005(6) 0.7042(5) 0.057(3) Uani 1 1 d . . . . . H13D H 0.859244 0.654160 0.680159 0.086 Uiso 1 1 calc GR . . . . H13E H 0.839708 0.745775 0.674253 0.086 Uiso 1 1 calc GR . . . . H13F H 0.763063 0.694602 0.714327 0.086 Uiso 1 1 calc GR . . . . C111 C 1.3209(8) 0.6885(6) 1.1911(5) 0.044(2) Uani 1 1 d . . . . . H11J H 1.260276 0.696567 1.146320 0.066 Uiso 1 1 calc GR . . . . H11K H 1.323291 0.733930 1.220924 0.066 Uiso 1 1 calc GR . . . . H11L H 1.299125 0.642768 1.214192 0.066 Uiso 1 1 calc GR . . . . C109 C 1.5401(8) 0.6600(6) 1.2484(5) 0.044(2) Uani 1 1 d . . . . . H10D H 1.526346 0.608276 1.264844 0.065 Uiso 1 1 calc GR . . . . H10E H 1.532002 0.698543 1.283071 0.065 Uiso 1 1 calc GR . . . . H10F H 1.622005 0.662824 1.241940 0.065 Uiso 1 1 calc GR . . . . C4 C -0.8166(8) 0.4794(8) 0.2925(6) 0.061(3) Uani 1 1 d . . . . . H4 H -0.869562 0.506278 0.254711 0.073 Uiso 1 1 calc R . . . . C8 C -0.4402(8) 0.5594(5) 0.4730(5) 0.0376(19) Uani 1 1 d . . . . . C10 C -0.3293(9) 0.6079(6) 0.4986(6) 0.052(3) Uani 1 1 d . . . . . H10A H -0.265205 0.577247 0.529837 0.078 Uiso 1 1 calc GR . . . . H10B H -0.348434 0.652663 0.523981 0.078 Uiso 1 1 calc GR . . . . H10C H -0.301465 0.625825 0.458719 0.078 Uiso 1 1 calc GR . . . . C115 C 1.3887(10) 0.4003(6) 0.9985(7) 0.062(3) Uani 1 1 d . . . . . H11M H 1.385276 0.374492 1.041807 0.093 Uiso 1 1 calc GR . . . . H11N H 1.406758 0.362146 0.966228 0.093 Uiso 1 1 calc GR . . . . H11O H 1.310204 0.424732 0.976892 0.093 Uiso 1 1 calc GR . . . . C121 C 0.5382(8) 0.5940(5) 0.7694(5) 0.042(2) Uani 1 1 d . . . . . H121 H 0.475420 0.573220 0.732327 0.051 Uiso 1 1 calc R . . . . C5 C -0.8642(10) 0.4332(8) 0.3346(7) 0.066(4) Uani 1 1 d . . . . . H5 H -0.949737 0.429039 0.326209 0.079 Uiso 1 1 calc R . . . . C113 C 1.6088(9) 0.4220(6) 1.0514(6) 0.049(2) Uani 1 1 d . . . . . H11P H 1.674071 0.460561 1.060758 0.073 Uiso 1 1 calc GR . . . . H11Q H 1.626373 0.381353 1.021248 0.073 Uiso 1 1 calc GR . . . . H11R H 1.603248 0.399274 1.095614 0.073 Uiso 1 1 calc GR . . . . C26 C -0.0405(9) 0.2819(7) 0.7182(6) 0.059(3) Uani 1 1 d . . . . . H26A H -0.058240 0.328103 0.742210 0.088 Uiso 1 1 calc GR . . . . H26B H -0.035087 0.236835 0.748780 0.088 Uiso 1 1 calc GR . . . . H26C H -0.105518 0.273774 0.675224 0.088 Uiso 1 1 calc GR . . . . C13 C -0.3094(9) 0.3351(7) 0.2836(6) 0.058(3) Uani 1 1 d . . . . . H13A H -0.277479 0.381768 0.266925 0.087 Uiso 1 1 calc GR . . . . H13B H -0.318990 0.294217 0.248338 0.087 Uiso 1 1 calc GR . . . . H13C H -0.252764 0.317773 0.327255 0.087 Uiso 1 1 calc GR . . . . C29 C 0.2338(9) 0.5813(6) 0.6218(5) 0.049(2) Uani 1 1 d . . . . . H29A H 0.214662 0.594948 0.665499 0.073 Uiso 1 1 calc GR . . . . H29B H 0.251017 0.628424 0.598816 0.073 Uiso 1 1 calc GR . . . . H29C H 0.305121 0.547411 0.631948 0.073 Uiso 1 1 calc GR . . . . C106 C 1.8541(9) 0.5672(7) 1.1847(6) 0.055(3) Uani 1 1 d . . . . . H106 H 1.912376 0.544190 1.222698 0.066 Uiso 1 1 calc R . . . . C28 C 0.1563(9) 0.5105(6) 0.5066(5) 0.044(2) Uani 1 1 d . . . . . H28A H 0.226867 0.476068 0.519347 0.066 Uiso 1 1 calc GR . . . . H28B H 0.174744 0.554855 0.480508 0.066 Uiso 1 1 calc GR . . . . H28C H 0.086480 0.482378 0.477510 0.066 Uiso 1 1 calc GR . . . . C105 C 1.8918(8) 0.6131(7) 1.1382(5) 0.052(3) Uani 1 1 d . . . . . H105 H 1.976097 0.621589 1.144321 0.062 Uiso 1 1 calc R . . . . C6 C -0.7881(9) 0.3926(7) 0.3894(6) 0.053(3) Uani 1 1 d . . . . . H6 H -0.821545 0.360421 0.418237 0.063 Uiso 1 1 calc R . . . . C15 C -0.5188(10) 0.3759(7) 0.2271(5) 0.058(3) Uani 1 1 d . . . . . H15A H -0.597690 0.388722 0.234744 0.088 Uiso 1 1 calc GR . . . . H15B H -0.528542 0.332811 0.193983 0.088 Uiso 1 1 calc GR . . . . H15C H -0.486780 0.420988 0.208084 0.088 Uiso 1 1 calc GR . . . . C25 C 0.0983(12) 0.2279(6) 0.6525(6) 0.060(3) Uani 1 1 d . . . . . H25A H 0.031397 0.227696 0.609684 0.090 Uiso 1 1 calc GR . . . . H25B H 0.100788 0.178114 0.676477 0.090 Uiso 1 1 calc GR . . . . H25C H 0.175268 0.236110 0.640743 0.090 Uiso 1 1 calc GR . . . . C11 C -0.5485(9) 0.6098(6) 0.4387(6) 0.053(3) Uani 1 1 d . . . . . H11A H -0.534422 0.634960 0.397417 0.080 Uiso 1 1 calc GR . . . . H11B H -0.559436 0.649205 0.471885 0.080 Uiso 1 1 calc GR . . . . H11C H -0.621711 0.577658 0.424632 0.080 Uiso 1 1 calc GR . . . . C9 C -0.4621(10) 0.5148(7) 0.5352(5) 0.054(3) Uani 1 1 d . . . . . H9A H -0.533371 0.481394 0.519064 0.081 Uiso 1 1 calc GR . . . . H9B H -0.476016 0.551434 0.569857 0.081 Uiso 1 1 calc GR . . . . H9C H -0.390722 0.483010 0.556511 0.081 Uiso 1 1 calc GR . . . . C128 C 1.0608(9) 0.7261(7) 0.7563(7) 0.063(3) Uani 1 1 d . . . . . H12M H 1.122962 0.738271 0.799603 0.094 Uiso 1 1 calc GR . . . . H12N H 1.052029 0.769750 0.723918 0.094 Uiso 1 1 calc GR . . . . H12O H 1.085090 0.679913 0.734900 0.094 Uiso 1 1 calc GR . . . . C14 C -0.4774(12) 0.2826(6) 0.3289(6) 0.062(3) Uani 1 1 d . . . . . H14A H -0.422434 0.272150 0.375112 0.094 Uiso 1 1 calc GR . . . . H14B H -0.480712 0.237230 0.298892 0.094 Uiso 1 1 calc GR . . . . H14C H -0.558928 0.293667 0.333626 0.094 Uiso 1 1 calc GR . . . . 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 Fe1 0.0270(6) 0.0235(5) 0.0337(6) 0.0008(5) 0.0082(5) -0.0011(4) Fe11 0.0240(5) 0.0273(6) 0.0323(6) -0.0044(5) 0.0069(4) -0.0009(4) Cl1 0.0213(8) 0.0186(8) 0.0362(10) -0.0033(7) 0.0153(7) 0.0039(6) Cl12 0.0212(8) 0.0315(9) 0.0341(10) -0.0101(8) 0.0122(7) 0.0077(7) Cl11 0.0300(9) 0.0279(9) 0.0509(12) -0.0098(9) 0.0217(9) -0.0120(8) Cl2 0.0361(10) 0.0370(11) 0.0468(12) 0.0009(9) 0.0224(9) -0.0237(8) Cl14 0.0376(11) 0.0532(13) 0.0408(12) -0.0123(10) 0.0167(9) 0.0018(9) Cl13 0.0370(11) 0.0524(13) 0.0386(12) 0.0055(10) 0.0098(9) -0.0088(9) Cl3 0.0393(11) 0.0487(12) 0.0369(12) -0.0060(10) 0.0144(9) 0.0095(9) Cl4 0.0405(11) 0.0486(13) 0.0458(13) 0.0123(11) 0.0133(10) -0.0072(10) Si1 0.0257(10) 0.0276(11) 0.0291(12) 0.0015(9) 0.0064(9) 0.0019(8) Si2 0.0256(10) 0.0266(11) 0.0300(12) -0.0001(9) 0.0067(9) 0.0013(8) Si12 0.0243(10) 0.0304(11) 0.0292(12) -0.0022(9) 0.0045(8) -0.0015(8) Si11 0.0252(10) 0.0301(11) 0.0273(11) -0.0038(9) 0.0076(8) -0.0019(8) N3 0.028(3) 0.026(3) 0.032(4) -0.002(3) 0.006(3) 0.004(3) N101 0.030(3) 0.029(3) 0.030(4) -0.004(3) 0.008(3) -0.001(3) N4 0.028(3) 0.028(3) 0.036(4) 0.004(3) 0.006(3) 0.002(3) N104 0.024(3) 0.031(3) 0.028(3) -0.004(3) 0.006(3) -0.001(3) N2 0.029(3) 0.034(4) 0.033(4) -0.006(3) 0.008(3) 0.003(3) N1 0.026(3) 0.028(3) 0.038(4) -0.001(3) 0.005(3) 0.004(3) N103 0.030(3) 0.034(4) 0.030(4) 0.006(3) 0.009(3) -0.001(3) N102 0.029(3) 0.034(4) 0.032(4) -0.006(3) 0.006(3) 0.000(3) C16 0.027(4) 0.029(4) 0.029(4) -0.002(3) 0.007(3) 0.004(3) C118 0.039(5) 0.037(5) 0.030(4) 0.002(4) 0.008(4) 0.003(4) C120 0.032(4) 0.042(5) 0.050(5) 0.018(4) 0.017(4) 0.008(4) C117 0.025(4) 0.035(4) 0.029(4) 0.006(3) 0.004(3) 0.001(3) C17 0.032(4) 0.027(4) 0.036(5) 0.004(3) 0.010(4) 0.003(3) C27 0.035(4) 0.025(4) 0.034(4) -0.001(3) 0.007(3) 0.001(3) C119 0.046(5) 0.042(5) 0.048(6) 0.012(4) 0.024(4) 0.008(4) C21 0.031(4) 0.039(5) 0.056(6) 0.014(4) -0.003(4) -0.002(4) C116 0.025(4) 0.032(4) 0.018(4) -0.003(3) 0.002(3) -0.005(3) C22 0.029(4) 0.040(5) 0.044(5) -0.001(4) 0.007(4) 0.000(3) C1 0.027(4) 0.027(4) 0.032(4) 0.001(3) 0.009(3) 0.000(3) C2 0.027(4) 0.038(4) 0.035(4) -0.006(4) 0.010(3) -0.002(3) C112 0.030(4) 0.031(4) 0.044(5) -0.007(4) 0.014(4) 0.003(3) C18 0.035(4) 0.040(5) 0.032(5) 0.004(4) 0.007(3) 0.008(4) C102 0.029(4) 0.035(4) 0.034(4) -0.004(4) 0.010(3) -0.004(3) C103 0.040(5) 0.048(5) 0.039(5) -0.009(4) 0.015(4) -0.011(4) C127 0.041(5) 0.035(5) 0.037(5) 0.007(4) 0.004(4) -0.002(4) C101 0.027(4) 0.031(4) 0.026(4) 0.005(3) 0.001(3) -0.002(3) C3 0.034(5) 0.057(6) 0.047(6) 0.005(5) 0.009(4) 0.008(4) C123 0.029(4) 0.029(4) 0.031(4) 0.001(3) 0.007(3) -0.008(3) C108 0.037(4) 0.037(5) 0.034(5) -0.008(4) 0.010(4) -0.004(3) C12 0.038(4) 0.039(5) 0.038(5) -0.005(4) 0.011(4) 0.004(4) C126 0.047(5) 0.029(4) 0.064(7) 0.013(4) 0.016(5) -0.001(4) C23 0.040(5) 0.037(5) 0.035(5) 0.011(4) 0.011(4) 0.011(4) C110 0.057(6) 0.040(5) 0.044(6) -0.009(4) 0.009(5) -0.005(4) C122 0.035(4) 0.039(5) 0.038(5) -0.001(4) 0.003(4) -0.001(4) C20 0.029(4) 0.044(5) 0.056(6) 0.018(5) 0.017(4) 0.012(4) C124 0.046(5) 0.050(5) 0.033(5) 0.005(4) 0.017(4) 0.003(4) C30 0.050(5) 0.032(5) 0.053(6) 0.009(4) 0.017(4) 0.005(4) C104 0.050(6) 0.068(7) 0.049(6) -0.023(5) 0.026(5) -0.022(5) C19 0.041(5) 0.043(5) 0.053(6) 0.014(4) 0.022(4) 0.013(4) C114 0.054(6) 0.051(6) 0.036(5) -0.006(4) 0.014(4) 0.007(5) C24 0.049(6) 0.049(6) 0.048(6) 0.017(5) -0.001(4) 0.001(4) C7 0.048(5) 0.047(5) 0.042(5) -0.010(4) 0.020(4) -0.007(4) C107 0.031(4) 0.057(6) 0.041(5) -0.001(4) 0.002(4) 0.006(4) C129 0.108(10) 0.036(6) 0.079(9) 0.010(6) 0.044(8) 0.008(6) C125 0.043(5) 0.044(5) 0.050(6) -0.008(5) 0.001(4) -0.018(4) C130 0.061(6) 0.049(6) 0.051(6) 0.022(5) -0.004(5) -0.001(5) C111 0.037(5) 0.047(5) 0.046(5) -0.020(4) 0.007(4) 0.006(4) C109 0.037(5) 0.055(6) 0.033(5) -0.009(4) -0.003(4) 0.003(4) C4 0.030(5) 0.090(9) 0.058(7) -0.014(6) 0.005(4) 0.005(5) C8 0.041(5) 0.029(4) 0.045(5) -0.008(4) 0.014(4) 0.009(4) C10 0.050(6) 0.048(6) 0.062(7) -0.022(5) 0.022(5) -0.008(4) C115 0.064(7) 0.047(6) 0.080(8) -0.032(6) 0.029(6) -0.014(5) C121 0.032(4) 0.038(5) 0.052(6) 0.013(4) 0.004(4) -0.003(4) C5 0.034(5) 0.097(9) 0.079(8) -0.044(7) 0.035(6) -0.021(6) C113 0.049(5) 0.034(5) 0.063(7) -0.003(5) 0.016(5) 0.012(4) C26 0.049(6) 0.059(7) 0.068(8) 0.030(6) 0.017(5) 0.005(5) C13 0.055(6) 0.066(7) 0.051(6) -0.021(5) 0.011(5) 0.010(5) C29 0.048(5) 0.037(5) 0.053(6) 0.004(4) 0.000(5) -0.015(4) C106 0.033(5) 0.073(7) 0.053(6) -0.017(6) 0.001(4) 0.008(5) C28 0.053(6) 0.041(5) 0.041(5) 0.009(4) 0.019(4) 0.003(4) C105 0.029(5) 0.082(8) 0.047(6) -0.029(6) 0.012(4) -0.006(5) C6 0.050(6) 0.063(6) 0.055(6) -0.029(5) 0.030(5) -0.026(5) C15 0.056(6) 0.072(8) 0.039(6) -0.022(5) -0.001(5) 0.006(5) C25 0.094(8) 0.027(5) 0.063(7) 0.004(5) 0.028(6) 0.004(5) C11 0.050(6) 0.041(5) 0.066(7) -0.005(5) 0.008(5) 0.016(4) C9 0.062(6) 0.060(7) 0.040(6) -0.009(5) 0.013(5) 0.007(5) C128 0.049(6) 0.066(7) 0.078(8) 0.031(6) 0.024(5) -0.008(5) C14 0.092(8) 0.036(5) 0.067(7) -0.021(5) 0.034(7) -0.015(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Si Si 0.0817 0.0704 '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 Cl1 Fe1 Si1 106.97(8) . . ? Cl1 Fe1 Si2 104.43(8) . . ? Cl2 Fe1 Cl1 122.21(8) . . ? Cl2 Fe1 Si1 104.98(9) . . ? Cl2 Fe1 Si2 107.50(9) . . ? Si1 Fe1 Si2 110.60(8) . . ? Cl12 Fe11 Si12 107.75(9) . . ? Cl12 Fe11 Si11 104.52(8) . . ? Cl11 Fe11 Cl12 122.42(8) . . ? Cl11 Fe11 Si12 103.76(8) . . ? Cl11 Fe11 Si11 107.19(9) . . ? Si11 Fe11 Si12 111.14(8) . . ? Cl4 Si1 Fe1 121.59(11) . . ? Cl4 Si1 C1 114.4(2) . . ? N2 Si1 Fe1 118.3(2) . . ? N2 Si1 Cl4 104.8(3) . . ? N2 Si1 N1 71.7(3) . . ? N2 Si1 C1 36.0(3) . . ? N1 Si1 Fe1 123.2(2) . . ? N1 Si1 Cl4 106.0(2) . . ? N1 Si1 C1 36.4(3) . . ? C1 Si1 Fe1 123.7(2) . . ? Cl3 Si2 Fe1 123.66(12) . . ? Cl3 Si2 C16 116.7(2) . . ? N3 Si2 Fe1 120.7(2) . . ? N3 Si2 Cl3 107.5(2) . . ? N3 Si2 C16 37.0(3) . . ? N4 Si2 Fe1 115.3(2) . . ? N4 Si2 Cl3 105.4(2) . . ? N4 Si2 N3 72.0(3) . . ? N4 Si2 C16 35.9(3) . . ? C16 Si2 Fe1 119.3(2) . . ? Cl13 Si12 Fe11 123.27(11) . . ? Cl13 Si12 C101 116.0(2) . . ? N101 Si12 Fe11 121.4(2) . . ? N101 Si12 Cl13 106.9(2) . . ? N101 Si12 N102 71.6(3) . . ? N101 Si12 C101 36.4(3) . . ? N102 Si12 Fe11 116.1(2) . . ? N102 Si12 Cl13 105.5(3) . . ? N102 Si12 C101 36.1(3) . . ? C101 Si12 Fe11 120.4(2) . . ? Cl14 Si11 Fe11 122.61(11) . . ? Cl14 Si11 C116 116.3(2) . . ? N104 Si11 Fe11 121.9(2) . . ? N104 Si11 Cl14 107.3(2) . . ? N104 Si11 N103 71.0(3) . . ? N104 Si11 C116 36.1(3) . . ? N103 Si11 Fe11 115.8(2) . . ? N103 Si11 Cl14 106.3(3) . . ? N103 Si11 C116 35.7(3) . . ? C116 Si11 Fe11 120.7(2) . . ? C16 N3 Si2 88.9(5) . . ? C16 N3 C27 133.5(7) . . ? C27 N3 Si2 134.6(5) . . ? C112 N101 Si12 135.7(5) . . ? C101 N101 Si12 90.3(5) . . ? C101 N101 C112 132.1(7) . . ? C16 N4 Si2 90.1(5) . . ? C16 N4 C23 131.5(7) . . ? C23 N4 Si2 136.0(6) . . ? C116 N104 Si11 90.5(5) . . ? C116 N104 C123 132.0(6) . . ? C123 N104 Si11 134.0(5) . . ? C1 N2 Si1 90.4(5) . . ? C1 N2 C12 130.5(7) . . ? C12 N2 Si1 134.9(6) . . ? C1 N1 Si1 89.6(5) . . ? C1 N1 C8 132.7(7) . . ? C8 N1 Si1 135.7(6) . . ? C116 N103 Si11 90.9(5) . . ? C116 N103 C127 131.0(7) . . ? C127 N103 Si11 136.2(6) . . ? C101 N102 Si12 90.0(5) . . ? C101 N102 C108 130.3(7) . . ? C108 N102 Si12 134.3(5) . . ? N3 C16 Si2 54.1(4) . . ? N3 C16 C17 125.3(7) . . ? N4 C16 Si2 54.0(4) . . ? N4 C16 N3 106.4(6) . . ? N4 C16 C17 128.1(7) . . ? C17 C16 Si2 164.4(6) . . ? C117 C118 C119 119.3(8) . . ? C121 C120 C119 120.6(8) . . ? C118 C117 C116 117.3(7) . . ? C122 C117 C118 120.4(8) . . ? C122 C117 C116 122.3(8) . . ? C22 C17 C16 120.6(8) . . ? C18 C17 C16 118.1(8) . . ? C18 C17 C22 121.3(8) . . ? N3 C27 C30 106.0(7) . . ? N3 C27 C29 109.9(7) . . ? N3 C27 C28 109.8(7) . . ? C30 C27 C29 110.0(8) . . ? C30 C27 C28 109.8(7) . . ? C29 C27 C28 111.2(8) . . ? C120 C119 C118 119.2(9) . . ? C20 C21 C22 120.2(9) . . ? N104 C116 Si11 53.4(4) . . ? N104 C116 C117 126.9(7) . . ? N103 C116 Si11 53.4(4) . . ? N103 C116 N104 105.4(6) . . ? N103 C116 C117 127.4(7) . . ? C117 C116 Si11 165.8(6) . . ? C17 C22 C21 118.9(9) . . ? N2 C1 Si1 53.6(4) . . ? N2 C1 N1 106.4(7) . . ? N2 C1 C2 127.3(7) . . ? N1 C1 Si1 54.0(4) . . ? N1 C1 C2 126.3(7) . . ? C2 C1 Si1 168.8(6) . . ? C3 C2 C1 121.4(8) . . ? C3 C2 C7 120.6(8) . . ? C7 C2 C1 118.0(8) . . ? N101 C112 C114 110.0(7) . . ? N101 C112 C115 106.0(7) . . ? N101 C112 C113 111.5(7) . . ? C115 C112 C114 111.1(8) . . ? C115 C112 C113 108.5(8) . . ? C113 C112 C114 109.7(7) . . ? C17 C18 C19 119.3(9) . . ? C103 C102 C101 118.5(8) . . ? C107 C102 C103 121.0(8) . . ? C107 C102 C101 120.6(8) . . ? C102 C103 C104 119.3(10) . . ? N103 C127 C129 111.1(8) . . ? N103 C127 C130 108.8(7) . . ? C129 C127 C130 110.8(9) . . ? C128 C127 N103 105.0(8) . . ? C128 C127 C129 111.7(9) . . ? C128 C127 C130 109.2(9) . . ? N101 C101 Si12 53.3(4) . . ? N101 C101 C102 125.8(7) . . ? N102 C101 Si12 54.0(4) . . ? N102 C101 N101 105.7(7) . . ? N102 C101 C102 128.4(7) . . ? C102 C101 Si12 166.2(6) . . ? C2 C3 C4 119.9(10) . . ? N104 C123 C126 105.7(6) . . ? N104 C123 C124 111.1(7) . . ? N104 C123 C125 110.6(7) . . ? C126 C123 C125 108.6(8) . . ? C124 C123 C126 109.8(7) . . ? C124 C123 C125 110.8(7) . . ? N102 C108 C110 111.6(7) . . ? N102 C108 C111 105.3(7) . . ? N102 C108 C109 108.7(7) . . ? C110 C108 C111 109.8(8) . . ? C110 C108 C109 111.7(8) . . ? C111 C108 C109 109.5(7) . . ? N2 C12 C13 104.8(7) . . ? N2 C12 C15 110.3(8) . . ? N2 C12 C14 110.6(7) . . ? C13 C12 C15 108.6(8) . . ? C13 C12 C14 110.6(9) . . ? C15 C12 C14 111.7(9) . . ? N4 C23 C24 109.8(8) . . ? N4 C23 C26 105.4(7) . . ? N4 C23 C25 110.6(7) . . ? C26 C23 C24 108.2(8) . . ? C26 C23 C25 110.5(9) . . ? C25 C23 C24 112.2(8) . . ? C117 C122 C121 120.0(9) . . ? C19 C20 C21 120.6(8) . . ? C105 C104 C103 119.7(10) . . ? C20 C19 C18 119.7(9) . . ? C6 C7 C2 118.6(10) . . ? C102 C107 C106 119.0(10) . . ? C5 C4 C3 120.7(11) . . ? N1 C8 C10 106.0(7) . . ? N1 C8 C11 111.1(8) . . ? N1 C8 C9 109.7(7) . . ? C10 C8 C11 110.2(8) . . ? C10 C8 C9 108.4(8) . . ? C11 C8 C9 111.2(8) . . ? C120 C121 C122 120.4(9) . . ? C4 C5 C6 120.4(9) . . ? C105 C106 C107 120.2(10) . . ? C106 C105 C104 120.8(9) . . ? C5 C6 C7 119.7(10) . . ? 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 Fe1 Cl1 2.2862(18) . ? Fe1 Cl2 2.2674(19) . ? Fe1 Si1 2.442(2) . ? Fe1 Si2 2.445(2) . ? Fe11 Cl12 2.2836(19) . ? Fe11 Cl11 2.267(2) . ? Fe11 Si12 2.452(2) . ? Fe11 Si11 2.444(2) . ? Cl14 Si11 2.092(3) . ? Cl13 Si12 2.088(3) . ? Cl3 Si2 2.090(3) . ? Cl4 Si1 2.087(3) . ? Si1 N2 1.831(7) . ? Si1 N1 1.840(7) . ? Si1 C1 2.274(8) . ? Si2 N3 1.840(7) . ? Si2 N4 1.837(7) . ? Si2 C16 2.271(8) . ? Si12 N101 1.826(7) . ? Si12 N102 1.842(7) . ? Si12 C101 2.278(8) . ? Si11 N104 1.824(7) . ? Si11 N103 1.824(7) . ? Si11 C116 2.271(8) . ? N3 C16 1.367(10) . ? N3 C27 1.470(10) . ? N101 C112 1.482(10) . ? N101 C101 1.351(10) . ? N4 C16 1.332(11) . ? N4 C23 1.479(11) . ? N104 C116 1.338(10) . ? N104 C123 1.483(10) . ? N2 C1 1.337(10) . ? N2 C12 1.481(11) . ? N1 C1 1.349(10) . ? N1 C8 1.474(10) . ? N103 C116 1.326(10) . ? N103 C127 1.512(11) . ? N102 C101 1.342(11) . ? N102 C108 1.490(10) . ? C16 C17 1.490(11) . ? C118 C117 1.408(12) . ? C118 C119 1.409(12) . ? C120 C119 1.404(14) . ? C120 C121 1.373(14) . ? C117 C116 1.476(10) . ? C117 C122 1.378(11) . ? C17 C22 1.387(12) . ? C17 C18 1.377(12) . ? C27 C30 1.516(12) . ? C27 C29 1.524(12) . ? C27 C28 1.551(12) . ? C21 C22 1.401(12) . ? C21 C20 1.381(14) . ? C1 C2 1.484(11) . ? C2 C3 1.370(13) . ? C2 C7 1.411(13) . ? C112 C114 1.548(13) . ? C112 C115 1.513(13) . ? C112 C113 1.543(12) . ? C18 C19 1.411(12) . ? C102 C103 1.393(12) . ? C102 C101 1.489(11) . ? C102 C107 1.379(12) . ? C103 C104 1.400(13) . ? C127 C129 1.525(15) . ? C127 C130 1.531(13) . ? C127 C128 1.509(13) . ? C3 C4 1.371(13) . ? C123 C126 1.525(12) . ? C123 C124 1.523(12) . ? C123 C125 1.556(11) . ? C108 C110 1.528(13) . ? C108 C111 1.529(12) . ? C108 C109 1.540(12) . ? C12 C13 1.505(13) . ? C12 C15 1.522(13) . ? C12 C14 1.538(14) . ? C23 C24 1.532(13) . ? C23 C26 1.511(13) . ? C23 C25 1.522(14) . ? C122 C121 1.399(12) . ? C20 C19 1.377(14) . ? C104 C105 1.383(15) . ? C7 C6 1.390(13) . ? C107 C106 1.407(13) . ? C4 C5 1.370(17) . ? C8 C10 1.492(12) . ? C8 C11 1.517(12) . ? C8 C9 1.534(14) . ? C5 C6 1.388(17) . ? C106 C105 1.372(16) . ?