#------------------------------------------------------------------------------ #$Date: 2019-12-06 12:22:45 +0200 (Fri, 06 Dec 2019) $ #$Revision: 244935 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556438.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_1556438 loop_ _publ_author_name 'Muller, I.' 'Schneider, C.' 'Pietzonka, C.' 'Kraus, F.' 'Werncke, C.G.' _publ_section_title ; Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A Structural and Spectroscopic Study ; _journal_name_full Inorganics _journal_page_first 117 _journal_paper_doi 10.3390/inorganics7100117 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C22 H44 Co N4 Si4, 2(C10 H20 K0.5 O4)' _chemical_formula_sum 'C42 H84 Co K N4 O8 Si4' _chemical_formula_weight 983.52 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 77.712(2) _cell_angle_beta 80.199(2) _cell_angle_gamma 83.606(2) _cell_formula_units_Z 2 _cell_length_a 10.8097(5) _cell_length_b 13.2648(6) _cell_length_c 19.9051(10) _cell_measurement_reflns_used 9838 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 26.7563 _cell_measurement_theta_min 2.3772 _cell_volume 2739.7(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 89930 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.529 _diffrn_reflns_theta_min 2.119 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour 'clear dark green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.192 _exptl_crystal_description plate _exptl_crystal_F_000 1060 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.294 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.062 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 584 _refine_ls_number_reflns 12549 _refine_ls_number_restraints 57 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0420 _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^)+(0.0280P)^2^+1.5905P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.0830 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9015 _reflns_number_total 12549 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file K_18c6_Co4.cif _cod_data_source_block k(18c6)co8 _cod_database_code 1556438 _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 0.964 _shelx_estimated_absorpt_t_min 0.889 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains O100, C101, C102, C103, C104, O200, C201, C204 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3. Others Sof(H10E)=Sof(H10F)=Sof(H10I)=Sof(H10J)=Sof(O200)=Sof(C201)=Sof(H20A)= Sof(H20B)=Sof(C204)=Sof(H20C)=Sof(H20D)=1-FVAR(1) Sof(O100)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(H10D)=Sof(H10G)= Sof(H10H)=Sof(C104)=Sof(H10K)=Sof(H10L)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB), C6C(H6CA,H6CB), C8C(H8CA, H8CB), C16C(H16C,H16D), C2K(H2KA,H2KB), C3K(H3KA,H3KB), C5K(H5KA,H5KB), C6K(H6KA,H6KB), C8K(H8KA,H8KB), C16K(H16A,H16B), C301(H30A,H30B), C302(H30C, H30D), C303(H30E,H30F), C304(H30G,H30H), C101(H10A,H10B), C102(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C103(H10I,H10J), C104(H10K,H10L), C201(H20A, H20B), C204(H20C,H20D) 4.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10) 4.c Idealised Me refined as rotating group: C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A, H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F), C213(H21G,H21H,H21I), C221(H22A,H22B,H22C), C222(H22D, H22E,H22F), C223(H22G,H22H,H22I) ; _shelx_res_file ; TITL GW54_0m_a.res in P-1 k{18c6}co8.res created by SHELXL-2018/3 at 15:11:46 on 23-May-2019 REM Old TITL GW54_0m in P-1 REM SHELXT solution in P-1 REM R1 0.289, Rweak 0.101, Alpha 0.172, Orientation as input REM Formula found by SHELXT: C44 N2 O8 Si4 K Co REM ##### REM PART 0 CELL 0.71073 10.8097 13.2648 19.9051 77.712 80.199 83.606 ZERR 2 0.0005 0.0006 0.001 0.002 0.002 0.002 LATT 1 SFAC C H Co K N O Si UNIT 84 168 2 2 8 16 8 RIGU O100 > C204 L.S. 10 PLAN 10 SIZE 0.07 0.14 0.23 TEMP -173.15 BOND $H LIST 4 conf fmap 2 acta REM REM REM WGHT 0.028000 1.590500 FVAR 0.47275 0.69787 CO1 3 0.493210 0.549458 0.761103 11.00000 0.01459 0.01647 = 0.01371 -0.00213 -0.00495 -0.00124 K1 4 0.000000 1.000000 0.500000 10.50000 0.01942 0.02119 = 0.02071 0.00018 -0.00351 0.00171 K2 4 0.000000 1.000000 1.000000 10.50000 0.01984 0.01622 = 0.03336 -0.00102 -0.01075 -0.00145 N1 5 0.392994 0.573732 0.682770 11.00000 0.01789 0.02017 = 0.01479 -0.00237 -0.00488 -0.00012 N2 5 0.322525 0.525011 0.815536 11.00000 0.01793 0.01640 = 0.01653 -0.00163 -0.00412 -0.00281 C1 1 0.438704 0.586018 0.613796 11.00000 0.02180 0.02255 = 0.01788 -0.00212 -0.00433 -0.00093 AFIX 43 H1 2 0.525535 0.596663 0.599746 11.00000 -1.20000 AFIX 0 C2 1 0.368131 0.584096 0.563197 11.00000 0.03301 0.02804 = 0.01539 -0.00256 -0.00716 -0.00137 AFIX 43 H2 2 0.405154 0.593426 0.515678 11.00000 -1.20000 AFIX 0 C3 1 0.239623 0.567998 0.583189 11.00000 0.03275 0.02910 = 0.02344 -0.00469 -0.01578 -0.00130 AFIX 43 H3 2 0.187746 0.567334 0.549283 11.00000 -1.20000 AFIX 0 C4 1 0.190364 0.553270 0.652419 11.00000 0.02157 0.02402 = 0.02600 -0.00335 -0.01069 -0.00345 AFIX 43 H4 2 0.103880 0.541419 0.666633 11.00000 -1.20000 AFIX 0 C5 1 0.267037 0.555554 0.702812 11.00000 0.01735 0.01566 = 0.02137 -0.00200 -0.00675 -0.00177 C6 1 0.226332 0.536389 0.776379 11.00000 0.01820 0.01548 = 0.02099 -0.00333 -0.00584 -0.00124 C7 1 0.100263 0.532176 0.808374 11.00000 0.01676 0.02935 = 0.02946 -0.00584 -0.00527 -0.00317 AFIX 43 H7 2 0.035078 0.539369 0.780752 11.00000 -1.20000 AFIX 0 C8 1 0.071133 0.517769 0.879068 11.00000 0.01931 0.03377 = 0.02982 -0.00675 0.00453 -0.00464 AFIX 43 H8 2 -0.013897 0.514157 0.901046 11.00000 -1.20000 AFIX 0 C9 1 0.169578 0.508329 0.918963 11.00000 0.02765 0.02739 = 0.01927 -0.00477 0.00182 -0.00491 AFIX 43 H9 2 0.151896 0.499240 0.968196 11.00000 -1.20000 AFIX 0 C10 1 0.290158 0.512493 0.885576 11.00000 0.02563 0.01949 = 0.01676 -0.00383 -0.00450 -0.00317 AFIX 43 H10 2 0.355632 0.506270 0.912901 11.00000 -1.20000 AFIX 0 N11 5 0.614574 0.429468 0.742346 11.00000 0.01744 0.01670 = 0.01798 -0.00467 -0.00484 -0.00065 SI11 7 0.550565 0.314448 0.753862 11.00000 0.02128 0.01710 = 0.02244 -0.00425 -0.00341 -0.00331 C111 1 0.457157 0.306509 0.683659 11.00000 0.03596 0.02616 = 0.05172 -0.00910 -0.02070 -0.00606 AFIX 137 H11A 2 0.430261 0.236343 0.690922 11.00000 -1.50000 H11B 2 0.509702 0.322963 0.638107 11.00000 -1.50000 H11C 2 0.382926 0.356093 0.685432 11.00000 -1.50000 AFIX 0 C112 1 0.443706 0.280585 0.838627 11.00000 0.03902 0.01938 = 0.04389 -0.00229 0.01224 -0.00749 AFIX 137 H11D 2 0.428331 0.207154 0.847508 11.00000 -1.50000 H11E 2 0.363555 0.322789 0.836444 11.00000 -1.50000 H11F 2 0.483355 0.294105 0.876255 11.00000 -1.50000 AFIX 0 C113 1 0.671483 0.200488 0.754407 11.00000 0.03206 0.02014 = 0.02569 -0.00595 -0.00406 -0.00323 AFIX 137 H11G 2 0.628995 0.136900 0.760589 11.00000 -1.50000 H11H 2 0.719434 0.195410 0.792739 11.00000 -1.50000 H11I 2 0.728899 0.209891 0.710175 11.00000 -1.50000 AFIX 0 SI12 7 0.756594 0.452981 0.693159 11.00000 0.01759 0.01970 = 0.01747 -0.00442 -0.00238 -0.00181 C121 1 0.772862 0.421320 0.603832 11.00000 0.02914 0.03051 = 0.02137 -0.00794 -0.00073 -0.00302 AFIX 137 H12A 2 0.855806 0.438479 0.577869 11.00000 -1.50000 H12B 2 0.707074 0.461709 0.578939 11.00000 -1.50000 H12C 2 0.764152 0.347335 0.608315 11.00000 -1.50000 AFIX 0 C122 1 0.893455 0.378262 0.733514 11.00000 0.02083 0.02992 = 0.03633 -0.00536 -0.00592 -0.00296 AFIX 137 H12D 2 0.972495 0.397768 0.703698 11.00000 -1.50000 H12E 2 0.886604 0.303930 0.738348 11.00000 -1.50000 H12F 2 0.892398 0.394255 0.779469 11.00000 -1.50000 AFIX 0 C123 1 0.788780 0.592770 0.676109 11.00000 0.02606 0.02417 = 0.02558 -0.00464 0.00306 -0.00582 AFIX 137 H12G 2 0.870609 0.602702 0.646633 11.00000 -1.50000 H12H 2 0.789923 0.613683 0.720333 11.00000 -1.50000 H12I 2 0.722642 0.635044 0.652444 11.00000 -1.50000 AFIX 0 N21 5 0.544867 0.667356 0.796057 11.00000 0.01698 0.01926 = 0.01465 -0.00247 -0.00609 -0.00184 SI21 7 0.621073 0.639764 0.866141 11.00000 0.01828 0.02210 = 0.01346 -0.00152 -0.00675 -0.00191 C211 1 0.665995 0.498219 0.892341 11.00000 0.03453 0.02937 = 0.02055 0.00012 -0.01337 0.00311 AFIX 137 H21A 2 0.702934 0.485448 0.935343 11.00000 -1.50000 H21B 2 0.727654 0.475407 0.855364 11.00000 -1.50000 H21C 2 0.590929 0.459651 0.900040 11.00000 -1.50000 AFIX 0 C212 1 0.773647 0.703446 0.851433 11.00000 0.02369 0.04126 = 0.02146 -0.00610 -0.00874 -0.00482 AFIX 137 H21D 2 0.821501 0.673261 0.889505 11.00000 -1.50000 H21E 2 0.755487 0.777875 0.849925 11.00000 -1.50000 H21F 2 0.823197 0.692279 0.807228 11.00000 -1.50000 AFIX 0 C213 1 0.525254 0.677680 0.946729 11.00000 0.02738 0.03295 = 0.01820 -0.00476 -0.00302 -0.00702 AFIX 137 H21G 2 0.574254 0.658259 0.985305 11.00000 -1.50000 H21H 2 0.447584 0.641829 0.958832 11.00000 -1.50000 H21I 2 0.504160 0.752643 0.937904 11.00000 -1.50000 AFIX 0 SI22 7 0.473487 0.784513 0.764691 11.00000 0.01876 0.01752 = 0.01864 -0.00181 -0.00741 -0.00058 C221 1 0.510224 0.894512 0.803235 11.00000 0.03433 0.02100 = 0.03103 -0.00402 -0.00944 -0.00139 AFIX 137 H22A 2 0.483653 0.960710 0.774867 11.00000 -1.50000 H22B 2 0.601019 0.891052 0.804005 11.00000 -1.50000 H22C 2 0.465018 0.888711 0.850783 11.00000 -1.50000 AFIX 0 C222 1 0.297052 0.787950 0.781850 11.00000 0.02467 0.02481 = 0.02710 -0.00199 -0.00580 0.00281 AFIX 137 H22D 2 0.261448 0.857870 0.764109 11.00000 -1.50000 H22E 2 0.268817 0.769005 0.832029 11.00000 -1.50000 H22F 2 0.268755 0.738770 0.758374 11.00000 -1.50000 AFIX 0 C223 1 0.517668 0.825232 0.667659 11.00000 0.02554 0.02283 = 0.02215 0.00235 -0.00962 -0.00244 AFIX 137 H22G 2 0.474295 0.892834 0.651735 11.00000 -1.50000 H22H 2 0.492776 0.773973 0.644624 11.00000 -1.50000 H22I 2 0.608915 0.830067 0.656146 11.00000 -1.50000 AFIX 0 O1C 6 -0.011116 0.901352 0.638042 11.00000 0.02182 0.02042 = 0.02429 0.00068 -0.00402 -0.00074 C2C 1 -0.135782 0.886871 0.673465 11.00000 0.02557 0.03018 = 0.02365 0.00318 0.00199 -0.00290 AFIX 23 H2CA 2 -0.134543 0.863432 0.724023 11.00000 -1.20000 H2CB 2 -0.172104 0.833341 0.656571 11.00000 -1.20000 AFIX 0 C3C 1 -0.214113 0.987446 0.660068 11.00000 0.02711 0.03017 = 0.02273 -0.00673 -0.00004 -0.00029 AFIX 23 H3CA 2 -0.297425 0.981637 0.689698 11.00000 -1.20000 H3CB 2 -0.172225 1.042856 0.671644 11.00000 -1.20000 AFIX 0 O4C 6 -0.229580 1.012402 0.588775 11.00000 0.02370 0.02193 = 0.02266 -0.00409 -0.00290 0.00360 C5C 1 -0.309621 1.104688 0.573635 11.00000 0.02395 0.02508 = 0.03368 -0.00468 0.00051 0.00694 AFIX 23 H5CA 2 -0.274054 1.163277 0.585333 11.00000 -1.20000 H5CB 2 -0.394038 1.095890 0.601653 11.00000 -1.20000 AFIX 0 C6C 1 -0.319812 1.126255 0.498139 11.00000 0.01755 0.02993 = 0.03747 -0.00142 -0.00473 0.00287 AFIX 23 H6CA 2 -0.351164 1.066199 0.485877 11.00000 -1.20000 H6CB 2 -0.379566 1.187370 0.486861 11.00000 -1.20000 AFIX 0 O7C 6 -0.197961 1.145344 0.459955 11.00000 0.01942 0.02902 = 0.02428 -0.00038 -0.00781 0.00074 C8C 1 -0.198744 1.169608 0.386783 11.00000 0.02640 0.02736 = 0.02582 0.00020 -0.01194 0.00078 AFIX 23 H8CA 2 -0.258208 1.230675 0.374816 11.00000 -1.20000 H8CB 2 -0.226285 1.110565 0.371435 11.00000 -1.20000 AFIX 0 C16C 1 0.068587 0.807972 0.648896 11.00000 0.02482 0.02479 = 0.02591 0.00315 -0.00867 0.00303 AFIX 23 H16C 2 0.037213 0.754411 0.629659 11.00000 -1.20000 H16D 2 0.069083 0.781860 0.699300 11.00000 -1.20000 AFIX 0 O1K 6 0.038120 0.787668 1.021844 11.00000 0.03133 0.02034 = 0.03024 -0.00782 -0.01103 0.00143 C2K 1 -0.039151 0.739925 0.988464 11.00000 0.04092 0.02107 = 0.03492 -0.00710 -0.00925 -0.00751 AFIX 23 H2KA 2 -0.029470 0.663780 1.003721 11.00000 -1.20000 H2KB 2 -0.014180 0.757138 0.937388 11.00000 -1.20000 AFIX 0 C3K 1 -0.172881 0.779149 1.007721 11.00000 0.03648 0.02677 = 0.03225 -0.00459 -0.00587 -0.01506 AFIX 23 H3KA 2 -0.230207 0.740265 0.990780 11.00000 -1.20000 H3KB 2 -0.194577 0.769849 1.058913 11.00000 -1.20000 AFIX 0 O4K 6 -0.186113 0.886263 0.976539 11.00000 0.02138 0.02573 = 0.03663 -0.00221 -0.00568 -0.00679 C5K 1 -0.312000 0.930055 0.987211 11.00000 0.01726 0.04406 = 0.04084 -0.00630 -0.00610 -0.00819 AFIX 23 H5KA 2 -0.341759 0.925558 1.037549 11.00000 -1.20000 H5KB 2 -0.367828 0.891897 0.968665 11.00000 -1.20000 AFIX 0 C6K 1 -0.315125 1.040538 0.950417 11.00000 0.01938 0.04351 = 0.03553 -0.00533 -0.01236 -0.00123 AFIX 23 H6KA 2 -0.277933 1.045352 0.900931 11.00000 -1.20000 H6KB 2 -0.403238 1.070998 0.952533 11.00000 -1.20000 AFIX 0 O7K 6 -0.245153 1.095162 0.983256 11.00000 0.02445 0.03267 = 0.02811 -0.00509 -0.01098 0.00119 C8K 1 -0.238539 1.200842 0.948997 11.00000 0.03241 0.02753 = 0.03546 -0.00617 -0.01549 0.01206 AFIX 23 H8KA 2 -0.324422 1.235505 0.948290 11.00000 -1.20000 H8KB 2 -0.196345 1.205182 0.900369 11.00000 -1.20000 AFIX 0 C16K 1 0.165682 0.747253 1.012461 11.00000 0.03920 0.02717 = 0.04460 -0.01334 -0.01769 0.01429 AFIX 23 H16A 2 0.200704 0.760258 0.962369 11.00000 -1.20000 H16B 2 0.171450 0.671587 1.030437 11.00000 -1.20000 AFIX 0 O300 6 -0.115214 0.844199 0.471219 11.00000 0.04333 0.04292 = 0.11645 -0.04236 0.00193 -0.00809 C301 1 -0.243406 0.834134 0.470865 11.00000 0.04898 0.06408 = 0.07519 -0.02529 -0.00274 -0.00314 AFIX 23 H30A 2 -0.271776 0.878914 0.428900 11.00000 -1.20000 H30B 2 -0.295417 0.854576 0.512518 11.00000 -1.20000 AFIX 0 C302 1 -0.255597 0.723271 0.470970 11.00000 0.06341 0.06628 = 0.06910 -0.01179 -0.01387 -0.02878 AFIX 23 H30C 2 -0.288521 0.686095 0.518154 11.00000 -1.20000 H30D 2 -0.312851 0.716880 0.438469 11.00000 -1.20000 AFIX 0 C303 1 -0.127277 0.681957 0.448227 11.00000 0.07755 0.05619 = 0.14586 -0.05319 0.03793 -0.02865 AFIX 23 H30E 2 -0.107883 0.614210 0.478212 11.00000 -1.20000 H30F 2 -0.118514 0.672342 0.399617 11.00000 -1.20000 AFIX 0 C304 1 -0.042207 0.756346 0.453468 11.00000 0.05380 0.04362 = 0.09408 -0.03167 -0.00966 0.00179 AFIX 23 H30G 2 0.011313 0.725792 0.489548 11.00000 -1.20000 H30H 2 0.013202 0.775864 0.408508 11.00000 -1.20000 AFIX 0 PART 1 O100 6 0.035342 1.051380 0.858690 21.00000 0.07314 0.06291 = 0.03656 -0.01516 -0.00330 -0.02618 C101 1 0.126377 1.125648 0.827906 21.00000 0.06214 0.07303 = 0.05479 -0.01906 -0.01425 -0.03072 AFIX 23 H10A 2 0.197907 1.114417 0.854488 21.00000 -1.20000 H10B 2 0.087469 1.196901 0.827592 21.00000 -1.20000 AFIX 0 PART 0 C102 1 0.170545 1.109906 0.755169 11.00000 0.06390 0.06953 = 0.05432 -0.00958 -0.00787 -0.02365 PART 1 AFIX 23 H10C 2 0.243106 1.057513 0.752919 21.00000 -1.20000 H10D 2 0.193223 1.175392 0.723111 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H10E 2 0.167526 1.186372 0.742453 -21.00000 -1.20000 H10F 2 0.246588 1.081146 0.728011 -21.00000 -1.20000 AFIX 0 PART 0 C103 1 0.054380 1.072046 0.739993 11.00000 0.05295 0.05446 = 0.05609 -0.02333 -0.01675 0.00239 PART 1 AFIX 23 H10G 2 0.074698 1.033686 0.701437 21.00000 -1.20000 H10H 2 -0.008994 1.130152 0.728004 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H10I 2 -0.007490 1.130790 0.726797 -21.00000 -1.20000 H10J 2 0.075631 1.033401 0.701607 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C104 1 0.007023 0.999629 0.809583 21.00000 0.03332 0.05865 = 0.05121 -0.02596 0.00193 -0.00511 AFIX 23 H10K 2 -0.084585 0.992863 0.814847 21.00000 -1.20000 H10L 2 0.052294 0.930028 0.813211 21.00000 -1.20000 AFIX 0 PART 0 PART 2 O200 6 0.076960 1.010156 0.860705 -21.00000 0.04372 0.09760 = 0.04508 -0.03799 -0.00374 -0.00419 C201 1 0.174533 1.073126 0.834403 -21.00000 0.04875 0.09886 = 0.04882 -0.04545 -0.00845 -0.01527 AFIX 23 H20A 2 0.256169 1.034288 0.842267 -21.00000 -1.20000 H20B 2 0.164034 1.133290 0.857529 -21.00000 -1.20000 AFIX 0 C204 1 0.008334 1.010419 0.798689 -21.00000 0.04173 0.06841 = 0.05088 -0.02977 -0.01050 -0.01447 AFIX 23 H20C 2 0.013542 0.938891 0.790548 -21.00000 -1.20000 H20D 2 -0.081774 1.032365 0.811108 -21.00000 -1.20000 AFIX 0 HKLF 4 REM GW54_0m_a.res in P-1 REM wR2 = 0.0830, GooF = S = 1.017, Restrained GooF = 1.015 for all data REM R1 = 0.0420 for 9015 Fo > 4sig(Fo) and 0.0779 for all 12549 data REM 584 parameters refined using 57 restraints END WGHT 0.0280 1.5904 REM Highest difference peak 0.294, deepest hole -0.493, 1-sigma level 0.062 Q1 1 -0.0641 0.9010 0.6523 11.00000 0.05 0.29 Q2 1 0.7934 0.5245 0.6913 11.00000 0.05 0.29 Q3 1 0.6498 0.5589 0.8699 11.00000 0.05 0.29 Q4 1 0.3266 0.5562 0.6961 11.00000 0.05 0.28 Q5 1 0.5597 0.4111 0.7199 11.00000 0.05 0.28 Q6 1 0.7684 0.5246 0.6844 11.00000 0.05 0.28 Q7 1 0.5184 0.7228 0.7784 11.00000 0.05 0.28 Q8 1 0.1345 0.8121 0.6319 11.00000 0.05 0.27 Q9 1 0.6390 0.4473 0.7117 11.00000 0.05 0.27 Q10 1 0.1345 1.2140 0.8100 11.00000 0.05 0.26 ; _shelx_res_checksum 4934 _shelx_hkl_file ; -2 0 0 0.21720 3.53715 5 -2 0 0 4.07485 4.67021 5 -2 0 0 3.25040 3.38650 2 2 0 0 2.53584 2.28634 4 2 0 0 2.64753 4.55722 5 2 0 0 1.57323 3.40682 5 2 0 0 3.61833 3.49302 2 -3 0 0 995.140 18.3778 4 -3 0 0 955.508 22.3924 3 -3 0 0 945.611 22.1006 5 -3 0 0 957.443 21.0746 2 3 0 0 952.567 21.4297 2 3 0 0 976.401 18.5632 4 3 0 0 925.284 21.4441 5 -4 0 0 5680.70 97.4591 2 -4 0 0 5715.44 99.4211 3 -4 0 0 5543.24 93.5652 4 -4 0 0 5746.37 99.2971 5 -4 0 0 5523.18 98.1754 5 4 0 0 5729.04 94.1677 4 4 0 0 5544.59 98.3991 5 4 0 0 5840.20 98.3950 2 -5 0 0 62.7220 8.58004 5 -5 0 0 54.9200 7.67626 2 -5 0 0 45.9173 8.36460 3 -5 0 0 49.2110 5.20075 4 -5 0 0 44.8345 8.23728 5 5 0 0 46.6869 8.16339 5 5 0 0 54.3394 5.85977 4 5 0 0 61.1496 8.29116 2 5 0 0 71.8449 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8.57893 2 3 2 0 152.206 7.66665 4 3 2 0 161.706 9.11032 5 -4 -2 0 916.341 21.5130 2 -4 -2 0 868.960 20.0414 3 -4 -2 0 892.678 19.6605 3 -4 -2 0 894.712 19.9985 4 -4 -2 0 878.386 23.6541 5 4 2 0 867.478 19.8528 4 4 2 0 901.335 22.9276 5 4 2 0 845.696 21.1368 2 -5 -2 0 35.4215 5.86012 4 -5 -2 0 37.3650 7.44263 5 -5 -2 0 39.1312 6.92890 3 -5 -2 0 44.9809 7.24176 2 -5 -2 0 44.7211 6.59974 3 -5 -2 0 29.3292 7.98777 5 5 2 0 32.3695 7.11925 2 5 2 0 32.3767 7.93177 5 5 2 0 37.5593 5.86588 4 5 2 0 30.1288 6.36626 5 -6 -2 0 410.826 16.4662 3 -6 -2 0 395.840 20.0145 5 -6 -2 0 398.962 14.3765 4 -6 -2 0 378.569 17.0410 3 -6 -2 0 401.342 16.9833 2 -6 -2 0 410.634 18.5119 5 6 2 0 417.689 18.9534 5 6 2 0 415.540 18.4128 5 6 2 0 404.941 14.6158 4 6 2 0 412.385 17.7428 2 -7 -2 0 3.81582 8.56892 5 -7 -2 0 9.19666 9.38109 5 -7 -2 0 2.96937 8.10804 3 -7 -2 0 7.31290 6.12187 4 -7 -2 0 11.9869 8.97015 3 -7 -2 0 9.80036 8.44891 2 7 2 0 2.41381 6.37755 4 7 2 0 12.7544 9.12818 5 7 2 0 7.86995 18.8982 5 7 2 0 10.5589 8.51885 2 -8 -2 0 438.835 17.3292 4 -8 -2 0 468.210 22.1131 3 -8 -2 0 424.349 22.8956 3 -8 -2 0 393.771 24.9285 5 -8 -2 0 436.895 21.7105 2 -8 -2 0 457.276 24.0717 5 8 2 0 481.940 25.1396 5 8 2 0 399.918 23.0506 2 8 2 0 414.048 18.3963 4 8 2 0 430.938 23.4721 5 -9 -2 0 3.81575 12.5505 3 -9 -2 0 10.5114 12.9659 3 -9 -2 0 10.1704 12.8123 5 -9 -2 0 3.33179 11.8085 2 -9 -2 0 -3.9328 8.75278 4 -9 -2 0 12.3383 13.3397 5 9 2 0 17.4246 9.85840 4 9 2 0 13.8218 13.7928 5 9 2 0 15.8321 15.0610 5 9 2 0 7.88663 13.7341 2 -10 -2 0 374.795 41.2947 5 -10 -2 0 291.946 26.3501 3 -10 -2 0 325.631 26.9953 2 -10 -2 0 291.076 28.0208 3 -10 -2 0 299.088 29.5555 5 -10 -2 0 328.083 20.3142 4 10 2 0 294.583 27.6644 5 10 2 0 293.487 29.0926 2 10 2 0 321.259 22.3032 4 -11 -2 0 33.0553 23.5265 5 -11 -2 0 32.5307 18.5977 2 -11 -2 0 51.7006 21.1426 5 -11 -2 0 30.1430 20.1403 3 -11 -2 0 8.05686 16.8722 3 -11 -2 0 47.9821 13.0964 4 11 2 0 26.7210 21.5114 5 11 2 0 23.6864 20.1337 5 11 2 0 31.7226 14.8165 4 11 2 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372.349 34.9267 5 10 -3 0 66.5398 11.1446 4 10 -3 0 77.5117 16.9361 5 10 -3 0 88.2261 21.2547 2 10 -3 0 91.1897 17.7727 5 -10 3 0 80.2152 8.13690 4 -10 3 0 80.0549 22.4373 3 -10 3 0 54.5035 23.6338 3 -10 3 0 80.6573 18.4489 5 -10 3 0 75.3343 18.5426 2 -10 3 0 88.3951 20.8035 5 9 -3 0 249.580 22.7312 5 9 -3 0 280.981 15.5183 4 9 -3 0 276.061 24.4371 5 9 -3 0 196.507 21.3219 2 -9 3 0 262.956 34.0513 3 -9 3 0 248.111 24.7403 2 -9 3 0 318.789 29.7566 3 -9 3 0 224.244 26.1504 5 -9 3 0 258.840 25.6197 5 -9 3 0 258.360 12.0313 4 8 -3 0 56.9827 8.54099 4 8 -3 0 64.0005 13.8799 5 8 -3 0 67.9182 15.2344 2 8 -3 0 64.6055 13.1681 5 -8 3 0 69.8970 13.2157 2 -8 3 0 35.1294 13.5625 5 -8 3 0 56.6614 15.0918 3 -8 3 0 42.5504 13.2035 5 -8 3 0 59.0081 18.1311 3 -8 3 0 79.7994 8.73066 4 7 -3 0 1594.36 43.3245 2 7 -3 0 1623.18 32.5754 4 7 -3 0 1643.53 40.9783 5 -7 3 0 1628.70 46.8373 3 -7 3 0 1610.48 40.8254 2 -7 3 0 1619.79 30.4879 4 -7 3 0 1634.84 40.1752 5 6 -3 0 135.574 9.74676 4 6 -3 0 132.645 13.2847 2 6 -3 0 130.537 13.8468 5 -6 3 0 153.227 13.8656 5 -6 3 0 142.715 14.6647 2 -6 3 0 129.929 17.8493 3 -6 3 0 144.998 7.59070 4 -6 3 0 137.495 13.3654 5 5 -3 0 240.421 10.0067 4 5 -3 0 255.710 15.9111 2 5 -3 0 252.401 13.8570 5 -5 3 0 236.612 14.9232 2 -5 3 0 252.438 13.8428 5 -5 3 0 258.292 8.86951 4 -5 3 0 246.974 13.0865 5 -5 3 0 232.852 18.4551 3 4 -3 0 1.77996 4.05543 4 4 -3 0 -7.8696 6.17052 2 4 -3 0 0.66672 5.24821 5 4 -3 0 -0.7931 4.69455 5 -4 3 0 -3.7208 5.49276 5 -4 3 0 1.24850 7.11978 3 -4 3 0 1.85944 3.62941 4 -4 3 0 8.26431 6.47622 2 -4 3 0 3.29645 4.98858 5 3 -3 0 1574.35 33.9552 2 3 -3 0 1597.63 28.7647 4 3 -3 0 1575.78 30.8326 5 -3 3 0 1581.77 36.9579 3 -3 3 0 1590.21 33.2365 2 -3 3 0 1565.88 30.5949 5 -3 3 0 1556.61 31.0875 5 -3 3 0 1562.84 28.8281 4 2 -3 0 4166.31 69.2904 5 2 -3 0 4147.69 72.9873 2 2 -3 0 4103.82 69.2793 5 -2 3 0 4148.30 72.5575 2 -2 3 0 4165.84 69.2893 5 -2 3 0 4189.94 69.5733 4 -2 3 0 4099.41 69.5548 5 -1 3 0 1136.60 23.7935 2 0 3 0 2024.57 36.4800 2 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48.3309 2 5 3 0 2430.13 48.2723 2 5 3 0 2453.36 50.5155 5 5 3 0 2398.91 46.4574 4 5 3 0 2470.57 50.7936 5 -6 -3 0 34.3934 6.64389 4 -6 -3 0 47.1509 7.05570 3 -6 -3 0 38.2510 7.44185 3 -6 -3 0 48.1981 9.61759 5 -6 -3 0 38.0313 8.30981 2 -6 -3 0 39.2116 9.84090 5 6 3 0 32.7024 8.35854 2 6 3 0 30.9889 7.58096 5 6 3 0 39.5906 6.90300 4 6 3 0 44.3307 9.47154 5 -7 -3 0 9.35683 8.36463 3 -7 -3 0 17.1504 7.88554 3 -7 -3 0 30.6577 10.1559 5 -7 -3 0 5.90816 8.64711 2 -7 -3 0 1.12000 9.69917 5 -7 -3 0 24.7770 7.44582 4 7 3 0 0.15326 10.1695 2 7 3 0 20.6835 10.2074 5 7 3 0 8.40208 9.69426 5 7 3 0 17.2165 7.19338 4 -8 -3 0 12.6067 11.0652 5 -8 -3 0 28.1714 10.1027 3 -8 -3 0 36.8253 11.3871 2 -8 -3 0 21.7082 9.68473 3 -8 -3 0 14.4322 8.66312 4 -8 -3 0 5.25898 11.7894 5 8 3 0 13.8949 10.6860 2 8 3 0 30.0418 8.93445 4 8 3 0 18.4880 9.87272 5 8 3 0 14.9648 10.9307 5 -9 -3 0 494.157 23.4187 3 -9 -3 0 477.370 28.0984 5 -9 -3 0 438.106 29.5016 5 -9 -3 0 498.661 26.7930 2 -9 -3 0 473.091 21.5929 4 -9 -3 0 480.664 24.6744 3 9 3 0 477.748 24.2457 4 9 3 0 514.843 29.4795 5 9 3 0 546.995 33.7548 5 9 3 0 468.579 27.6721 2 -10 -3 0 18.6273 15.8329 2 -10 -3 0 -14.388 12.5645 3 -10 -3 0 4.34550 18.2051 5 -10 -3 0 -5.0566 15.8733 5 -10 -3 0 -3.5519 10.7011 4 -10 -3 0 -19.714 14.4433 3 10 3 0 1.00858 16.4729 2 10 3 0 4.24596 15.0266 5 10 3 0 6.53503 11.9499 4 10 3 0 11.9429 14.6759 5 -11 -3 0 89.9135 15.1820 4 -11 -3 0 94.3282 18.6657 3 -11 -3 0 114.662 24.4884 5 -11 -3 0 100.799 21.1608 3 -11 -3 0 86.7990 22.3325 5 -11 -3 0 96.0832 20.9999 2 11 3 0 141.252 25.0018 2 11 3 0 88.5470 23.3746 5 11 3 0 148.532 23.5724 5 11 3 0 114.963 17.5039 4 -12 -3 0 193.690 26.8448 3 -12 -3 0 212.699 29.6186 5 -12 -3 0 153.283 22.8950 3 -12 -3 0 173.679 19.3256 4 -12 -3 0 139.227 26.5582 2 -12 -3 0 167.467 32.9245 5 12 3 0 205.704 30.4219 5 12 3 0 153.814 24.3862 5 12 3 0 147.281 20.9299 4 -13 -3 0 320.670 62.3271 5 -13 -3 0 300.918 46.0478 5 -13 -3 0 357.024 34.1450 4 -13 -3 0 368.933 43.3568 3 -13 -3 0 307.775 37.9733 3 -13 -3 0 342.285 35.1538 2 13 3 0 325.537 37.4355 5 13 3 0 369.453 40.5048 4 13 3 0 296.158 36.8751 5 13 -4 0 78.0613 28.9869 5 -13 4 0 48.8183 37.8205 3 12 -4 0 45.8288 23.4074 5 -12 4 0 -7.9698 24.5991 5 -12 4 0 51.9051 30.6412 3 -12 4 0 25.8732 23.9767 2 11 -4 0 44.8473 19.5948 5 11 -4 0 65.5456 23.1827 5 11 -4 0 51.2886 25.0233 2 -11 4 0 19.9462 20.0374 2 -11 4 0 30.1133 25.5687 5 -11 4 0 50.7980 26.5144 3 -11 4 0 86.8810 26.0444 5 -11 4 0 27.4333 29.7681 3 10 -4 0 34.0123 17.5817 5 10 -4 0 62.8358 22.8155 2 -10 4 0 73.3325 26.3488 3 -10 4 0 62.9871 22.9684 3 -10 4 0 44.7030 19.1707 2 -10 4 0 48.7389 20.4301 5 -10 4 0 57.5207 20.3855 5 9 -4 0 256.955 25.1218 5 9 -4 0 265.329 25.9201 2 9 -4 0 228.595 14.4528 4 -9 4 0 240.965 25.9618 5 -9 4 0 235.381 25.6425 2 -9 4 0 214.912 30.6889 3 -9 4 0 220.667 24.9150 5 -9 4 0 217.796 10.8753 4 -9 4 0 206.460 26.3885 3 8 -4 0 45.6008 15.3166 2 8 -4 0 35.0674 11.7156 5 8 -4 0 31.2554 7.61067 4 8 -4 0 13.1742 9.06887 5 -8 4 0 45.4918 15.7581 3 -8 4 0 65.0575 14.0498 2 -8 4 0 30.8545 12.3316 5 -8 4 0 38.1419 14.1564 5 -8 4 0 37.5635 5.55047 4 -8 4 0 28.9612 18.2733 3 7 -4 0 24.1853 9.86780 5 7 -4 0 39.1506 12.7780 2 7 -4 0 19.2401 11.0705 5 7 -4 0 36.3620 6.52550 4 -7 4 0 8.83839 12.7248 3 -7 4 0 11.0614 13.9862 3 -7 4 0 20.8702 10.1410 5 -7 4 0 43.7041 10.8705 2 -7 4 0 34.3662 5.21301 4 -7 4 0 23.8125 10.3403 5 6 -4 0 530.687 24.4029 2 6 -4 0 451.907 24.2178 5 6 -4 0 510.379 19.7620 5 6 -4 0 476.516 14.2786 4 -6 4 0 514.686 13.1538 4 -6 4 0 528.111 27.1963 3 -6 4 0 505.126 20.6044 5 -6 4 0 494.436 19.5134 5 -6 4 0 504.014 21.8092 2 5 -4 0 268.426 13.8362 5 5 -4 0 242.226 17.1246 2 5 -4 0 260.716 10.3299 4 5 -4 0 268.363 13.7414 5 -5 4 0 245.791 19.9117 3 -5 4 0 255.500 13.4751 5 -5 4 0 258.383 9.83173 4 -5 4 0 250.405 13.5791 5 -5 4 0 265.207 16.0112 2 4 -4 0 1664.93 33.9815 5 4 -4 0 1661.66 33.8003 5 4 -4 0 1646.30 38.2372 2 -4 4 0 1627.12 33.6077 5 -4 4 0 1617.15 31.0456 4 -4 4 0 1676.73 37.2289 2 -4 4 0 1651.98 42.0348 3 -4 4 0 1654.57 34.4395 5 3 -4 0 596.893 19.6717 2 3 -4 0 617.153 15.4725 5 3 -4 0 612.342 15.2053 5 -3 4 0 599.350 22.4720 3 -3 4 0 607.937 19.0184 2 -3 4 0 595.296 15.6533 5 -3 4 0 611.820 15.3103 4 -3 4 0 621.892 15.3399 5 2 -4 0 92.2918 5.77557 5 2 -4 0 103.029 10.6402 2 2 -4 0 82.2350 5.17113 5 -2 4 0 92.8956 11.5914 3 -2 4 0 92.7710 9.57008 2 -2 4 0 89.0106 5.57400 5 -2 4 0 88.0058 5.49819 5 -2 4 0 84.3620 7.34245 4 -1 4 0 8013.30 132.272 2 -1 4 0 7803.85 134.852 3 -1 4 0 7859.15 129.611 4 0 4 0 685.484 18.3408 3 0 4 0 682.890 15.8483 4 0 4 0 688.545 16.7106 2 -1 -4 0 2174.21 40.3987 2 -1 -4 0 2244.36 40.7141 4 -1 -4 0 2193.90 38.6733 5 -1 -4 0 2159.42 37.9856 5 1 4 0 2184.76 39.8323 2 1 4 0 2172.04 40.1239 4 1 4 0 2189.30 38.3959 5 1 4 0 2227.13 38.6837 5 1 4 0 2209.74 39.8059 3 -2 -4 0 613.974 16.0606 5 -2 -4 0 629.661 16.0825 2 -2 -4 0 639.428 15.4049 5 -2 -4 0 599.795 16.1720 4 2 4 0 630.686 16.1682 4 2 4 0 609.700 12.7187 3 2 4 0 641.343 16.0044 5 2 4 0 641.505 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253.329 26.8148 3 -11 -5 4 239.919 28.3521 2 -11 -5 4 169.896 24.6089 5 10 5 -4 53.7538 22.1658 2 10 5 -4 21.6327 15.2485 5 10 5 -4 43.3013 14.4863 4 10 5 -4 41.9425 20.4772 5 -10 -5 4 -19.964 22.5954 5 -10 -5 4 20.5011 17.8674 5 -10 -5 4 41.4820 13.6634 3 -10 -5 4 101.639 18.2012 3 -10 -5 4 80.4307 19.9101 2 9 5 -4 38.6051 17.4169 5 9 5 -4 29.6431 12.5886 4 9 5 -4 17.5006 14.5621 5 9 5 -4 6.73296 15.2747 2 -9 -5 4 62.5841 16.6469 2 -9 -5 4 19.2359 17.6463 5 -9 -5 4 29.2034 11.1538 3 -9 -5 4 39.6367 17.5976 5 8 5 -4 52.4664 11.5832 4 8 5 -4 48.1262 13.7337 2 8 5 -4 34.9108 15.0300 5 8 5 -4 38.8676 16.0086 5 -8 -5 4 26.9399 14.0332 5 -8 -5 4 57.3309 16.4600 3 -8 -5 4 51.3158 15.8495 2 -8 -5 4 52.5542 9.98181 3 -8 -5 4 35.0247 12.7802 5 7 5 -4 607.075 27.8490 5 7 5 -4 591.653 28.9043 5 7 5 -4 569.172 22.9280 4 7 5 -4 611.799 26.5952 2 -7 -5 4 605.396 29.5063 5 -7 -5 4 570.119 26.6975 2 -7 -5 4 567.623 27.2036 5 6 5 -4 79.8210 11.7985 4 6 5 -4 114.850 12.6962 2 6 5 -4 93.5464 13.4982 5 6 5 -4 90.8470 13.6606 5 -6 -5 4 76.6330 13.2596 5 -6 -5 4 74.1028 12.8800 2 -6 -5 4 78.7361 8.81184 3 -6 -5 4 66.1380 13.5714 5 5 5 -4 720.258 22.5805 4 5 5 -4 685.612 24.2243 2 5 5 -4 748.675 26.3044 5 5 5 -4 702.359 17.2769 3 5 5 -4 728.332 24.3538 5 -5 -5 4 710.440 24.8716 5 -5 -5 4 696.734 18.6247 3 -5 -5 4 727.922 25.8320 5 -5 -5 4 715.630 25.2133 2 4 5 -4 39.1929 7.52041 5 4 5 -4 50.0698 9.04290 2 4 5 -4 49.2938 7.97600 4 4 5 -4 44.9371 5.69034 3 4 5 -4 40.8202 8.92598 5 -4 -5 4 42.9190 8.54329 5 -4 -5 4 38.5301 9.70097 2 -4 -5 4 52.3043 6.96644 3 3 5 -4 662.262 20.8751 5 3 5 -4 647.131 18.0080 3 3 5 -4 674.957 19.5784 5 3 5 -4 654.081 20.9452 2 3 5 -4 637.035 19.7000 4 -3 -5 4 693.621 22.3906 2 -3 -5 4 661.849 18.2886 3 -3 -5 4 633.065 20.4466 5 -3 -5 4 688.973 20.2336 5 2 5 -4 585.519 17.7220 5 2 5 -4 612.533 17.0541 5 2 5 -4 612.917 19.4949 2 2 5 -4 616.135 18.9158 4 2 5 -4 486.647 19.0594 3 -2 -5 4 593.870 17.5913 5 -2 -5 4 601.411 20.5483 2 -2 -5 4 624.100 18.4206 3 -2 -5 4 595.360 17.3739 5 1 5 -4 260.419 14.9048 4 1 5 -4 278.234 10.4252 5 1 5 -4 253.123 15.1099 3 1 5 -4 270.790 11.4348 5 1 5 -4 286.091 14.3787 2 -1 -5 4 269.202 15.4823 2 -1 -5 4 270.284 11.5029 5 -1 -5 4 274.227 10.7268 5 -1 -5 4 273.041 14.6194 3 0 5 -4 62.0087 6.56609 5 0 5 -4 71.7417 8.00349 5 0 5 -4 65.7986 9.70293 3 0 5 -4 72.1232 8.98832 2 0 5 -4 54.8694 8.17074 4 0 -5 4 61.9115 6.43326 5 0 -5 4 71.8674 7.49180 5 0 -5 4 69.5937 9.62812 3 0 -5 4 49.0990 8.56841 2 -1 5 -4 704.688 21.5536 4 -1 5 -4 679.397 15.4679 5 -1 5 -4 660.853 21.5832 2 -1 5 -4 695.557 24.0839 3 -1 5 -4 692.768 15.8649 5 1 -5 4 701.707 24.1367 3 -2 5 -4 587.159 14.9147 5 -2 5 -4 581.750 24.0721 3 -2 5 -4 602.561 22.3091 2 -2 5 -4 580.136 20.2224 4 2 -5 4 619.621 23.9175 3 2 -5 4 599.103 13.9943 5 2 -5 4 602.092 13.4816 5 -3 5 -4 1040.63 23.4939 5 -3 5 -4 1060.01 33.5185 3 -3 5 -4 1071.94 22.6051 5 -3 5 -4 1011.18 27.3771 4 -3 5 -4 1116.03 30.6800 2 3 -5 4 1043.69 26.7603 4 3 -5 4 1036.60 22.6163 5 3 -5 4 1039.11 22.0457 5 -4 5 -4 126.210 16.3421 3 -4 5 -4 109.798 10.5766 5 -4 5 -4 89.3354 12.0832 2 -4 5 -4 127.870 9.71538 5 -4 5 -4 104.216 10.4625 4 4 -5 4 120.633 10.5422 5 4 -5 4 104.502 9.10519 5 4 -5 4 117.362 10.8771 4 -5 5 -4 4.72931 7.73418 4 -5 5 -4 1.86457 9.63526 2 -5 5 -4 5.34074 6.08244 5 5 -5 4 7.74299 7.28978 5 5 -5 4 8.55496 7.98789 4 5 -5 4 9.55994 6.35922 5 5 -5 4 -16.136 10.2375 2 -6 5 -4 791.448 29.7505 2 -6 5 -4 771.702 24.2552 4 -6 5 -4 799.603 25.5498 5 -6 5 -4 809.320 24.0416 5 -6 5 -4 806.333 36.4273 3 6 -5 4 793.407 24.4043 4 6 -5 4 787.791 32.4247 2 6 -5 4 746.311 23.5596 5 6 -5 4 822.411 25.2829 5 -7 5 -4 7.69812 9.43573 5 -7 5 -4 0.82352 15.4537 3 -7 5 -4 14.1052 9.19332 4 -7 5 -4 10.0778 12.0353 2 -7 5 -4 16.2570 10.7187 5 7 -5 4 15.0146 13.2137 2 7 -5 4 14.2550 9.52229 5 7 -5 4 12.9579 9.83256 4 -8 5 -4 109.379 16.0275 5 -8 5 -4 102.558 14.0692 5 -8 5 -4 101.397 11.5872 4 -8 5 -4 50.6729 14.8047 2 -8 5 -4 99.6342 20.7998 3 8 -5 4 77.5743 13.3611 4 8 -5 4 103.999 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11.4831 5 2 -3 5 275.485 16.7919 3 -3 3 -5 356.809 13.2281 5 -3 3 -5 364.119 17.3295 2 -3 3 -5 338.719 18.9923 3 -3 3 -5 368.352 14.0123 5 -3 3 -5 371.232 16.0575 4 3 -3 5 355.864 19.7044 3 3 -3 5 359.365 13.9133 5 3 -3 5 372.442 15.5937 4 3 -3 5 353.782 13.1381 5 -4 3 -5 1960.62 44.5606 2 -4 3 -5 1979.37 41.8092 4 -4 3 -5 1971.38 41.3491 5 -4 3 -5 2061.01 40.7375 5 -4 3 -5 2010.15 49.1936 3 4 -3 5 2003.62 48.5709 3 4 -3 5 1993.31 41.2329 5 4 -3 5 1975.48 45.1898 2 4 -3 5 2000.87 42.0073 4 4 -3 5 2001.85 40.5489 5 -5 3 -5 446.615 16.8771 5 -5 3 -5 411.463 17.5578 5 -5 3 -5 420.463 23.8520 3 -5 3 -5 441.876 17.5429 4 -5 3 -5 430.954 20.5408 2 5 -3 5 388.827 22.5915 5 5 -3 5 400.455 21.0619 2 5 -3 5 430.543 18.1960 4 5 -3 5 395.275 16.6534 5 -6 3 -5 247.123 22.9169 3 -6 3 -5 249.842 16.9378 5 -6 3 -5 288.979 16.0109 4 -6 3 -5 258.994 18.9319 2 -6 3 -5 254.165 15.2914 5 6 -3 5 240.037 17.4114 5 6 -3 5 256.561 16.4613 4 6 -3 5 216.040 29.8518 2 6 -3 5 239.155 15.3569 5 -7 3 -5 246.820 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15.1473 2 -6 10 12 19.5820 27.9123 3 5 -10 -12 -12.542 21.2759 5 5 -10 -12 30.7817 28.3237 3 5 -10 -12 -8.1611 14.6846 5 -5 10 12 -19.505 22.7286 3 -5 10 12 -1.4070 12.5009 2 -5 10 12 8.41934 23.9569 5 -5 10 12 1.31601 20.3588 5 4 -10 -12 11.7448 14.9234 5 4 -10 -12 12.8827 19.0784 5 4 -10 -12 46.6527 16.4483 2 4 -10 -12 26.5347 22.7640 3 -4 10 12 18.3308 22.9814 3 -4 10 12 47.3317 17.2814 5 -4 10 12 47.6452 21.1162 5 -4 10 12 11.5362 10.5588 2 3 -10 -12 -4.2140 16.5865 5 3 -10 -12 10.2538 8.04606 4 3 -10 -12 -26.125 13.5468 5 3 -10 -12 5.60170 12.3549 2 3 -10 -12 21.5375 22.4589 3 -3 10 12 -2.1811 14.0931 5 -3 10 12 -2.8502 18.3185 5 -3 10 12 2.60935 18.7029 3 -3 10 12 11.0091 10.8807 4 -3 10 12 11.9973 8.54777 2 2 -10 -12 -10.300 15.7890 5 2 -10 -12 -4.5463 16.7826 3 2 -10 -12 0.04461 8.32808 4 2 -10 -12 1.05871 12.7311 5 -2 10 12 -0.9495 16.3299 5 -2 10 12 1.83402 18.9155 3 -2 10 12 7.56163 13.3337 5 -2 10 12 15.3487 11.3747 4 1 -10 -12 28.7540 19.6494 3 1 -10 -12 31.4381 10.2771 4 1 -10 -12 31.8574 14.5881 5 1 -10 -12 36.7139 16.7254 5 -1 10 12 25.0897 13.4378 5 -1 10 12 29.6832 17.2082 5 -1 10 12 36.0341 12.6543 4 0 -10 -12 386.225 26.6978 5 0 -10 -12 350.620 19.7078 4 0 -10 -12 374.603 33.7576 3 0 -10 -12 386.594 25.7238 5 0 10 12 339.558 26.1977 5 0 10 12 348.209 31.8105 3 0 10 12 363.555 23.1794 4 0 10 12 365.764 29.0335 5 -1 -10 -12 13.4143 10.5831 4 -1 -10 -12 21.9962 14.1525 5 -1 -10 -12 26.2386 14.7482 5 -1 -10 -12 -8.9762 16.4303 3 1 10 12 20.0619 13.1748 5 1 10 12 19.0073 16.0697 3 1 10 12 9.17485 13.4990 5 1 10 12 14.3956 12.6625 4 -2 -10 -12 4.30358 14.9972 3 -2 -10 -12 27.4000 25.6856 5 -2 -10 -12 4.55499 10.1961 4 -2 -10 -12 -7.8302 15.5142 5 2 10 12 15.5365 14.0647 5 2 10 12 -2.0902 13.8561 5 2 10 12 -7.8473 11.4021 4 2 10 12 -3.2877 16.3116 3 -3 -10 -12 325.940 21.8027 4 -3 -10 -12 289.332 27.6501 3 -3 -10 -12 328.070 31.5447 5 3 10 12 281.212 32.4950 3 3 10 12 312.241 27.6089 5 3 10 12 334.399 26.5684 5 3 10 12 314.365 25.1947 4 -4 -10 -12 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1 -3 -25 -30.589 40.8074 5 -1 3 25 8.42136 33.5527 5 0 -3 -25 45.9985 25.9281 2 0 -3 -25 33.5612 30.0134 4 0 -3 -25 47.0390 40.1916 5 0 -3 -25 -8.9424 61.8488 5 0 3 25 46.1574 41.5621 5 0 3 25 104.417 41.1063 3 -1 -3 -25 30.0158 34.8120 5 -1 -3 -25 51.2071 30.0710 4 -1 -3 -25 46.7395 39.4838 5 -1 -3 -25 -4.3030 23.8691 2 1 3 25 5.05606 35.8713 5 1 3 25 50.6469 38.3632 3 -2 -3 -25 -15.537 38.8615 5 -2 -3 -25 4.77654 23.0981 2 -2 -3 -25 16.4714 36.8840 5 -2 -3 -25 -32.330 28.8822 2 -2 -3 -25 -14.263 28.6117 4 2 3 25 8.98221 39.1649 3 2 3 25 -65.796 34.2104 5 -3 -3 -25 21.3461 36.2944 5 -3 -3 -25 12.6084 30.6062 4 -3 -3 -25 30.3316 29.1020 2 -3 -3 -25 40.0743 24.5341 2 -3 -3 -25 44.9751 39.9916 5 3 3 25 57.0469 36.7410 3 3 3 25 29.3112 35.8709 5 -4 -3 -25 55.9248 30.6369 2 -4 -3 -25 -55.572 33.3471 5 -4 -3 -25 -18.856 28.7642 4 -4 -3 -25 16.3659 25.0473 2 -4 -3 -25 24.2777 38.3506 5 4 3 25 78.7218 40.0835 3 4 3 25 -18.750 34.4137 5 -5 -3 -25 -24.891 44.2958 5 -5 -3 -25 32.1273 30.7099 5 -5 -3 -25 -8.3007 41.1092 4 -5 -3 -25 77.3286 25.8232 2 -5 -3 -25 -15.612 29.8947 2 5 3 25 24.9220 35.1264 5 1 -4 -25 6.25073 39.3976 5 1 -4 -25 87.6546 30.0208 4 -1 4 25 -3.7651 38.0465 5 0 -4 -25 4.06467 41.7352 5 0 -4 -25 6.27518 28.9569 4 0 -4 -25 5.07145 25.4940 5 0 4 25 -9.7448 31.7867 5 0 4 25 23.5949 52.3003 3 -1 -4 -25 52.6611 34.9729 5 -1 -4 -25 32.1302 29.3129 2 -1 -4 -25 55.4740 37.7843 5 -1 -4 -25 38.4867 30.6715 4 1 4 25 9.28832 35.1923 5 1 4 25 -13.662 35.1029 3 -2 -4 -25 -16.029 39.9605 5 -2 -4 -25 23.2980 28.9787 4 -2 -4 -25 -15.128 24.8045 2 2 4 25 8.31927 30.5068 5 2 4 25 62.3638 39.0150 3 -3 -4 -25 -0.6308 36.8016 5 -3 -4 -25 88.4182 31.8528 2 -3 -4 -25 19.5367 29.2612 4 -3 -4 -25 150.526 40.7223 5 3 4 25 83.5562 38.4169 3 3 4 25 76.0648 38.9987 5 -4 -4 -25 -56.386 27.8559 4 -4 -4 -25 -24.326 37.4869 5 -4 -4 -25 22.5444 33.1415 2 -4 -4 -25 -41.252 38.5270 5 4 4 25 44.4764 37.1024 3 4 4 25 -18.611 36.1378 5 -5 -4 -25 -5.1679 37.3551 5 -5 -4 -25 -103.42 47.5891 5 -5 -4 -25 -3.2938 27.7133 2 -5 -4 -25 -21.182 26.4371 4 5 4 25 83.8802 43.3301 3 5 4 25 50.3423 38.6790 5 0 -5 -25 14.7825 29.4117 4 0 -5 -25 78.9624 44.6641 5 0 5 25 42.3147 33.4755 5 -1 -5 -25 165.597 29.1777 2 -1 -5 -25 192.376 30.9320 4 -1 -5 -25 223.874 44.9510 5 1 5 25 195.896 40.2784 5 1 5 25 150.261 45.9273 3 1 5 25 118.886 42.8465 5 -2 -5 -25 -11.726 33.1168 5 -2 -5 -25 86.6403 39.5965 5 -2 -5 -25 6.15457 24.7477 2 -2 -5 -25 46.6836 28.1985 4 2 5 25 16.8629 38.2213 5 2 5 25 -8.2029 36.7561 5 2 5 25 7.32273 35.8608 3 -3 -5 -25 -18.630 39.3374 5 -3 -5 -25 26.1787 44.2234 5 -3 -5 -25 25.9364 24.1484 2 -3 -5 -25 25.5470 28.9935 4 3 5 25 -4.1607 33.6934 5 3 5 25 63.6262 39.5905 3 -4 -5 -25 -48.881 38.3541 5 -4 -5 -25 51.2114 41.4069 5 -4 -5 -25 53.6309 26.0988 2 -4 -5 -25 1.64211 29.5200 4 4 5 25 18.0086 36.8923 3 4 5 25 12.7749 33.5219 5 -5 -5 -25 34.5924 28.5025 4 -5 -5 -25 -2.6662 39.1659 5 -5 -5 -25 -69.387 31.7482 5 5 5 25 23.6093 39.9367 5 5 5 25 82.7761 43.0709 3 0 -6 -25 27.4027 26.8120 4 0 -6 -25 0.33448 41.0560 5 0 6 25 -27.026 42.4063 5 0 6 25 59.9086 45.2925 5 -1 -6 -25 30.4475 43.7010 5 -1 -6 -25 34.4993 27.8458 4 1 6 25 32.1964 41.9411 5 1 6 25 30.4025 38.2199 5 -2 -6 -25 32.9951 28.8590 4 -2 -6 -25 105.552 41.9820 5 2 6 25 7.57413 34.4286 5 2 6 25 51.1395 41.0908 5 2 6 25 89.3815 39.6522 3 -3 -6 -25 42.7200 41.6069 5 -3 -6 -25 1.77914 28.8026 4 3 6 25 -50.148 35.9689 5 3 6 25 -34.417 36.2371 5 3 6 25 29.7198 35.1571 3 -4 -6 -25 47.2953 29.9012 4 -4 -6 -25 74.4172 41.0915 5 4 6 25 107.686 40.3335 3 4 6 25 20.9087 37.2149 5 -5 -6 -25 -34.100 41.6610 5 -5 -6 -25 79.1692 29.3730 4 5 6 25 20.2422 41.7043 3 5 6 25 9.49622 40.0983 5 -1 -7 -25 5.07263 27.0355 4 -1 -7 -25 -13.128 42.3978 5 1 7 25 11.4225 44.3829 5 1 7 25 38.3826 35.4781 5 -2 -7 -25 17.9160 27.7953 4 -2 -7 -25 -23.201 38.9865 5 2 7 25 32.0604 43.8505 5 2 7 25 56.5208 43.1953 5 -3 -7 -25 74.1583 44.4936 5 -3 -7 -25 31.7896 30.4919 4 3 7 25 96.7670 65.6869 5 3 7 25 89.4713 42.9790 5 -4 -7 -25 8.29980 29.5122 4 -4 -7 -25 43.9155 39.4509 5 4 7 25 74.5083 46.7620 3 4 7 25 -28.269 39.7320 5 4 7 25 89.5023 39.1746 5 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7042 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71075 10.820 13.268 19.919 77.688 80.205 83.603 ) ; _shelx_hkl_checksum 90450 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.49321(2) 0.54946(2) 0.76110(2) 0.01471(7) Uani 1 1 d . . . . . K1 K 0.000000 1.000000 0.500000 0.02129(14) Uani 1 2 d S T P . . K2 K 0.000000 1.000000 1.000000 0.02292(14) Uani 1 2 d S T P . . N1 N 0.39299(15) 0.57373(12) 0.68277(8) 0.0176(4) Uani 1 1 d . . . . . N2 N 0.32253(15) 0.52501(12) 0.81554(8) 0.0169(3) Uani 1 1 d . . . . . C1 C 0.43870(19) 0.58602(15) 0.61380(10) 0.0209(4) Uani 1 1 d . . . . . H1 H 0.525535 0.596663 0.599746 0.025 Uiso 1 1 calc R . . . . C2 C 0.3681(2) 0.58410(16) 0.56320(11) 0.0254(5) Uani 1 1 d . . . . . H2 H 0.405154 0.593426 0.515678 0.030 Uiso 1 1 calc R . . . . C3 C 0.2396(2) 0.56800(17) 0.58319(11) 0.0272(5) Uani 1 1 d . . . . . H3 H 0.187746 0.567334 0.549283 0.033 Uiso 1 1 calc R . . . . C4 C 0.19036(19) 0.55327(16) 0.65242(11) 0.0231(5) Uani 1 1 d . . . . . H4 H 0.103880 0.541419 0.666633 0.028 Uiso 1 1 calc R . . . . C5 C 0.26704(18) 0.55555(15) 0.70281(10) 0.0179(4) Uani 1 1 d . . . . . C6 C 0.22633(18) 0.53639(15) 0.77638(10) 0.0179(4) Uani 1 1 d . . . . . C7 C 0.10026(19) 0.53218(16) 0.80837(11) 0.0249(5) Uani 1 1 d . . . . . H7 H 0.035078 0.539369 0.780752 0.030 Uiso 1 1 calc R . . . . C8 C 0.0711(2) 0.51777(17) 0.87907(12) 0.0284(5) Uani 1 1 d . . . . . H8 H -0.013897 0.514157 0.901046 0.034 Uiso 1 1 calc R . . . . C9 C 0.1696(2) 0.50833(16) 0.91896(11) 0.0252(5) Uani 1 1 d . . . . . H9 H 0.151896 0.499240 0.968196 0.030 Uiso 1 1 calc R . . . . C10 C 0.29016(19) 0.51249(15) 0.88558(10) 0.0203(4) Uani 1 1 d . . . . . H10 H 0.355632 0.506270 0.912901 0.024 Uiso 1 1 calc R . . . . N11 N 0.61457(15) 0.42947(12) 0.74235(8) 0.0170(3) Uani 1 1 d . . . . . Si11 Si 0.55056(5) 0.31445(4) 0.75386(3) 0.02007(13) Uani 1 1 d . . . . . C111 C 0.4572(2) 0.30651(18) 0.68366(13) 0.0358(6) Uani 1 1 d . . . . . H11A H 0.430261 0.236343 0.690922 0.054 Uiso 1 1 calc GR . . . . H11B H 0.509702 0.322963 0.638107 0.054 Uiso 1 1 calc GR . . . . H11C H 0.382926 0.356093 0.685432 0.054 Uiso 1 1 calc GR . . . . C112 C 0.4437(2) 0.28059(17) 0.83863(13) 0.0365(6) Uani 1 1 d . . . . . H11D H 0.428331 0.207154 0.847508 0.055 Uiso 1 1 calc GR . . . . H11E H 0.363555 0.322789 0.836444 0.055 Uiso 1 1 calc GR . . . . H11F H 0.483355 0.294105 0.876255 0.055 Uiso 1 1 calc GR . . . . C113 C 0.6715(2) 0.20049(16) 0.75441(11) 0.0257(5) Uani 1 1 d . . . . . H11G H 0.628995 0.136900 0.760589 0.039 Uiso 1 1 calc GR . . . . H11H H 0.719434 0.195410 0.792739 0.039 Uiso 1 1 calc GR . . . . H11I H 0.728899 0.209891 0.710175 0.039 Uiso 1 1 calc GR . . . . Si12 Si 0.75659(5) 0.45298(4) 0.69316(3) 0.01815(12) Uani 1 1 d . . . . . C121 C 0.7729(2) 0.42132(17) 0.60383(11) 0.0269(5) Uani 1 1 d . . . . . H12A H 0.855806 0.438479 0.577869 0.040 Uiso 1 1 calc GR . . . . H12B H 0.707074 0.461709 0.578939 0.040 Uiso 1 1 calc GR . . . . H12C H 0.764152 0.347335 0.608315 0.040 Uiso 1 1 calc GR . . . . C122 C 0.89346(19) 0.37826(17) 0.73351(12) 0.0289(5) Uani 1 1 d . . . . . H12D H 0.972495 0.397768 0.703698 0.043 Uiso 1 1 calc GR . . . . H12E H 0.886604 0.303930 0.738348 0.043 Uiso 1 1 calc GR . . . . H12F H 0.892398 0.394255 0.779469 0.043 Uiso 1 1 calc GR . . . . C123 C 0.7888(2) 0.59277(16) 0.67611(11) 0.0258(5) Uani 1 1 d . . . . . H12G H 0.870609 0.602702 0.646633 0.039 Uiso 1 1 calc GR . . . . H12H H 0.789923 0.613683 0.720333 0.039 Uiso 1 1 calc GR . . . . H12I H 0.722642 0.635044 0.652444 0.039 Uiso 1 1 calc GR . . . . N21 N 0.54487(14) 0.66736(12) 0.79606(8) 0.0166(3) Uani 1 1 d . . . . . Si21 Si 0.62107(5) 0.63976(4) 0.86614(3) 0.01770(12) Uani 1 1 d . . . . . C211 C 0.6660(2) 0.49822(17) 0.89234(11) 0.0282(5) Uani 1 1 d . . . . . H21A H 0.702934 0.485448 0.935343 0.042 Uiso 1 1 calc GR . . . . H21B H 0.727654 0.475407 0.855364 0.042 Uiso 1 1 calc GR . . . . H21C H 0.590929 0.459651 0.900040 0.042 Uiso 1 1 calc GR . . . . C212 C 0.77365(19) 0.70345(18) 0.85143(11) 0.0280(5) Uani 1 1 d . . . . . H21D H 0.821501 0.673261 0.889505 0.042 Uiso 1 1 calc GR . . . . H21E H 0.755487 0.777875 0.849925 0.042 Uiso 1 1 calc GR . . . . H21F H 0.823197 0.692279 0.807228 0.042 Uiso 1 1 calc GR . . . . C213 C 0.5253(2) 0.67768(17) 0.94673(11) 0.0259(5) Uani 1 1 d . . . . . H21G H 0.574254 0.658259 0.985305 0.039 Uiso 1 1 calc GR . . . . H21H H 0.447584 0.641829 0.958832 0.039 Uiso 1 1 calc GR . . . . H21I H 0.504160 0.752643 0.937904 0.039 Uiso 1 1 calc GR . . . . Si22 Si 0.47349(5) 0.78451(4) 0.76469(3) 0.01809(12) Uani 1 1 d . . . . . C221 C 0.5102(2) 0.89451(16) 0.80323(12) 0.0285(5) Uani 1 1 d . . . . . H22A H 0.483653 0.960710 0.774867 0.043 Uiso 1 1 calc GR . . . . H22B H 0.601019 0.891052 0.804005 0.043 Uiso 1 1 calc GR . . . . H22C H 0.465018 0.888711 0.850783 0.043 Uiso 1 1 calc GR . . . . C222 C 0.29705(19) 0.78795(17) 0.78185(11) 0.0261(5) Uani 1 1 d . . . . . H22D H 0.261448 0.857870 0.764109 0.039 Uiso 1 1 calc GR . . . . H22E H 0.268817 0.769005 0.832029 0.039 Uiso 1 1 calc GR . . . . H22F H 0.268755 0.738770 0.758374 0.039 Uiso 1 1 calc GR . . . . C223 C 0.5177(2) 0.82523(16) 0.66766(11) 0.0238(5) Uani 1 1 d . . . . . H22G H 0.474295 0.892834 0.651735 0.036 Uiso 1 1 calc GR . . . . H22H H 0.492776 0.773973 0.644624 0.036 Uiso 1 1 calc GR . . . . H22I H 0.608915 0.830067 0.656146 0.036 Uiso 1 1 calc GR . . . . O1C O -0.01112(13) 0.90135(10) 0.63804(7) 0.0229(3) Uani 1 1 d . . . . . C2C C -0.1358(2) 0.88687(17) 0.67346(11) 0.0284(5) Uani 1 1 d . . . . . H2CA H -0.134543 0.863432 0.724023 0.034 Uiso 1 1 calc R . . . . H2CB H -0.172104 0.833341 0.656571 0.034 Uiso 1 1 calc R . . . . C3C C -0.2141(2) 0.98745(17) 0.66007(11) 0.0270(5) Uani 1 1 d . . . . . H3CA H -0.297425 0.981637 0.689698 0.032 Uiso 1 1 calc R . . . . H3CB H -0.172225 1.042856 0.671644 0.032 Uiso 1 1 calc R . . . . O4C O -0.22958(13) 1.01240(11) 0.58877(7) 0.0233(3) Uani 1 1 d . . . . . C5C C -0.3096(2) 1.10469(17) 0.57363(12) 0.0290(5) Uani 1 1 d . . . . . H5CA H -0.274054 1.163277 0.585333 0.035 Uiso 1 1 calc R . . . . H5CB H -0.394038 1.095890 0.601653 0.035 Uiso 1 1 calc R . . . . C6C C -0.31981(19) 1.12625(18) 0.49814(12) 0.0294(5) Uani 1 1 d . . . . . H6CA H -0.351164 1.066199 0.485877 0.035 Uiso 1 1 calc R . . . . H6CB H -0.379566 1.187370 0.486861 0.035 Uiso 1 1 calc R . . . . O7C O -0.19796(13) 1.14534(11) 0.45996(7) 0.0246(3) Uani 1 1 d . . . . . C8C C -0.1987(2) 1.16961(17) 0.38678(11) 0.0266(5) Uani 1 1 d . . . . . H8CA H -0.258208 1.230675 0.374816 0.032 Uiso 1 1 calc R . . . . H8CB H -0.226285 1.110565 0.371435 0.032 Uiso 1 1 calc R . . . . C16C C 0.06859(19) 0.80797(16) 0.64890(11) 0.0262(5) Uani 1 1 d . . . . . H16C H 0.037213 0.754411 0.629659 0.031 Uiso 1 1 calc R . . . . H16D H 0.069083 0.781860 0.699300 0.031 Uiso 1 1 calc R . . . . O1K O 0.03812(14) 0.78767(11) 1.02184(8) 0.0264(3) Uani 1 1 d . . . . . C2K C -0.0392(2) 0.73993(17) 0.98846(13) 0.0313(5) Uani 1 1 d . . . . . H2KA H -0.029470 0.663780 1.003721 0.038 Uiso 1 1 calc R . . . . H2KB H -0.014180 0.757138 0.937388 0.038 Uiso 1 1 calc R . . . . C3K C -0.1729(2) 0.77915(17) 1.00772(12) 0.0310(5) Uani 1 1 d . . . . . H3KA H -0.230207 0.740265 0.990780 0.037 Uiso 1 1 calc R . . . . H3KB H -0.194577 0.769849 1.058913 0.037 Uiso 1 1 calc R . . . . O4K O -0.18611(13) 0.88626(11) 0.97654(8) 0.0280(3) Uani 1 1 d . . . . . C5K C -0.3120(2) 0.93006(18) 0.98721(13) 0.0337(6) Uani 1 1 d . . . . . H5KA H -0.341759 0.925558 1.037549 0.040 Uiso 1 1 calc R . . . . H5KB H -0.367828 0.891897 0.968665 0.040 Uiso 1 1 calc R . . . . C6K C -0.3151(2) 1.04054(18) 0.95042(13) 0.0323(5) Uani 1 1 d . . . . . H6KA H -0.277933 1.045352 0.900931 0.039 Uiso 1 1 calc R . . . . H6KB H -0.403238 1.070998 0.952533 0.039 Uiso 1 1 calc R . . . . O7K O -0.24515(13) 1.09516(12) 0.98326(8) 0.0280(3) Uani 1 1 d . . . . . C8K C -0.2385(2) 1.20084(17) 0.94900(12) 0.0317(5) Uani 1 1 d . . . . . H8KA H -0.324422 1.235505 0.948290 0.038 Uiso 1 1 calc R . . . . H8KB H -0.196345 1.205182 0.900369 0.038 Uiso 1 1 calc R . . . . C16K C 0.1657(2) 0.74725(18) 1.01246(14) 0.0360(6) Uani 1 1 d . . . . . H16A H 0.200704 0.760258 0.962369 0.043 Uiso 1 1 calc R . . . . H16B H 0.171450 0.671587 1.030437 0.043 Uiso 1 1 calc R . . . . O300 O -0.11521(18) 0.84420(15) 0.47122(13) 0.0649(6) Uani 1 1 d . . . . . C301 C -0.2434(3) 0.8341(2) 0.47087(18) 0.0619(9) Uani 1 1 d . . . . . H30A H -0.271776 0.878914 0.428900 0.074 Uiso 1 1 calc R . . . . H30B H -0.295417 0.854576 0.512518 0.074 Uiso 1 1 calc R . . . . C302 C -0.2556(3) 0.7233(2) 0.47097(18) 0.0642(9) Uani 1 1 d . . . . . H30C H -0.288521 0.686095 0.518154 0.077 Uiso 1 1 calc R . . . . H30D H -0.312851 0.716880 0.438469 0.077 Uiso 1 1 calc R . . . . C303 C -0.1273(3) 0.6820(3) 0.4482(2) 0.0929(14) Uani 1 1 d . . . . . H30E H -0.107883 0.614210 0.478212 0.112 Uiso 1 1 calc R . . . . H30F H -0.118514 0.672342 0.399617 0.112 Uiso 1 1 calc R . . . . C304 C -0.0422(3) 0.7563(2) 0.45347(19) 0.0617(9) Uani 1 1 d . . . . . H30G H 0.011313 0.725792 0.489548 0.074 Uiso 1 1 calc R . . . . H30H H 0.013202 0.775864 0.408508 0.074 Uiso 1 1 calc R . . . . O100 O 0.0353(9) 1.0514(5) 0.8587(3) 0.0557(16) Uani 0.698(18) 1 d . U . A 1 C101 C 0.1264(9) 1.1256(7) 0.8279(3) 0.060(2) Uani 0.698(18) 1 d . U . A 1 H10A H 0.197907 1.114417 0.854488 0.072 Uiso 0.698(18) 1 calc R . . A 1 H10B H 0.087469 1.196901 0.827592 0.072 Uiso 0.698(18) 1 calc R . . A 1 C102 C 0.1705(3) 1.1099(3) 0.75517(16) 0.0617(8) Uani 1 1 d . U . . . H10C H 0.243106 1.057513 0.752919 0.074 Uiso 0.698(18) 1 calc R . . A 1 H10D H 0.193223 1.175392 0.723111 0.074 Uiso 0.698(18) 1 calc R . . A 1 H10E H 0.167526 1.186372 0.742453 0.074 Uiso 0.302(18) 1 calc R . . A 2 H10F H 0.246588 1.081146 0.728011 0.074 Uiso 0.302(18) 1 calc R . . A 2 C103 C 0.0544(3) 1.0720(2) 0.73999(16) 0.0521(7) Uani 1 1 d . U . . . H10G H 0.074698 1.033686 0.701437 0.063 Uiso 0.698(18) 1 calc R . . A 1 H10H H -0.008994 1.130152 0.728004 0.063 Uiso 0.698(18) 1 calc R . . A 1 H10I H -0.007490 1.130790 0.726797 0.063 Uiso 0.302(18) 1 calc R . . A 2 H10J H 0.075631 1.033401 0.701607 0.063 Uiso 0.302(18) 1 calc R . . A 2 C104 C 0.0070(16) 0.9996(12) 0.8096(7) 0.046(2) Uani 0.698(18) 1 d . U . A 1 H10K H -0.084585 0.992863 0.814847 0.056 Uiso 0.698(18) 1 calc R . . A 1 H10L H 0.052294 0.930028 0.813211 0.056 Uiso 0.698(18) 1 calc R . . A 1 O200 O 0.0770(13) 1.0102(18) 0.8607(8) 0.059(3) Uani 0.302(18) 1 d . U . A 2 C201 C 0.1745(16) 1.073(2) 0.8344(7) 0.060(4) Uani 0.302(18) 1 d . U . A 2 H20A H 0.256169 1.034288 0.842267 0.072 Uiso 0.302(18) 1 calc R . . A 2 H20B H 0.164034 1.133290 0.857529 0.072 Uiso 0.302(18) 1 calc R . . A 2 C204 C 0.008(4) 1.010(3) 0.7987(19) 0.050(6) Uani 0.302(18) 1 d . U . A 2 H20C H 0.013542 0.938891 0.790548 0.060 Uiso 0.302(18) 1 calc R . . A 2 H20D H -0.081774 1.032365 0.811108 0.060 Uiso 0.302(18) 1 calc R . . A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01459(13) 0.01647(14) 0.01371(14) -0.00213(10) -0.00495(10) -0.00124(10) K1 0.0194(3) 0.0212(3) 0.0207(3) 0.0002(3) -0.0035(3) 0.0017(2) K2 0.0198(3) 0.0162(3) 0.0334(4) -0.0010(3) -0.0108(3) -0.0015(2) N1 0.0179(8) 0.0202(9) 0.0148(8) -0.0024(7) -0.0049(7) -0.0001(7) N2 0.0179(8) 0.0164(9) 0.0165(9) -0.0016(7) -0.0041(7) -0.0028(7) C1 0.0218(11) 0.0225(11) 0.0179(10) -0.0021(9) -0.0043(8) -0.0009(8) C2 0.0330(12) 0.0280(12) 0.0154(11) -0.0026(9) -0.0072(9) -0.0014(9) C3 0.0327(12) 0.0291(12) 0.0234(12) -0.0047(10) -0.0158(10) -0.0013(10) C4 0.0216(11) 0.0240(11) 0.0260(12) -0.0033(9) -0.0107(9) -0.0034(9) C5 0.0173(10) 0.0157(10) 0.0214(11) -0.0020(8) -0.0068(8) -0.0018(8) C6 0.0182(10) 0.0155(10) 0.0210(11) -0.0033(8) -0.0058(8) -0.0012(8) C7 0.0168(10) 0.0294(12) 0.0295(12) -0.0058(10) -0.0053(9) -0.0032(9) C8 0.0193(11) 0.0338(13) 0.0298(13) -0.0067(10) 0.0045(9) -0.0046(9) C9 0.0276(12) 0.0274(12) 0.0193(11) -0.0048(9) 0.0018(9) -0.0049(9) C10 0.0256(11) 0.0195(11) 0.0168(10) -0.0038(8) -0.0045(8) -0.0032(8) N11 0.0174(8) 0.0167(9) 0.0180(9) -0.0047(7) -0.0048(7) -0.0007(7) Si11 0.0213(3) 0.0171(3) 0.0224(3) -0.0042(2) -0.0034(2) -0.0033(2) C111 0.0360(13) 0.0262(13) 0.0517(16) -0.0091(11) -0.0207(12) -0.0061(10) C112 0.0390(14) 0.0194(12) 0.0439(15) -0.0023(11) 0.0122(11) -0.0075(10) C113 0.0321(12) 0.0201(11) 0.0257(12) -0.0060(9) -0.0041(9) -0.0032(9) Si12 0.0176(3) 0.0197(3) 0.0175(3) -0.0044(2) -0.0024(2) -0.0018(2) C121 0.0291(12) 0.0305(12) 0.0214(11) -0.0079(9) -0.0007(9) -0.0030(9) C122 0.0208(11) 0.0299(13) 0.0363(13) -0.0054(10) -0.0059(10) -0.0030(9) C123 0.0261(11) 0.0242(12) 0.0256(12) -0.0046(9) 0.0031(9) -0.0058(9) N21 0.0170(8) 0.0193(9) 0.0146(8) -0.0025(7) -0.0061(7) -0.0018(7) Si21 0.0183(3) 0.0221(3) 0.0135(3) -0.0015(2) -0.0068(2) -0.0019(2) C211 0.0345(13) 0.0294(12) 0.0206(11) 0.0001(9) -0.0134(10) 0.0031(10) C212 0.0237(11) 0.0413(14) 0.0215(11) -0.0061(10) -0.0087(9) -0.0048(10) C213 0.0274(12) 0.0330(13) 0.0182(11) -0.0048(9) -0.0030(9) -0.0070(9) Si22 0.0188(3) 0.0175(3) 0.0186(3) -0.0018(2) -0.0074(2) -0.0006(2) C221 0.0343(13) 0.0210(12) 0.0310(13) -0.0040(10) -0.0094(10) -0.0014(9) C222 0.0247(11) 0.0248(12) 0.0271(12) -0.0020(9) -0.0058(9) 0.0028(9) C223 0.0255(11) 0.0228(11) 0.0222(11) 0.0023(9) -0.0096(9) -0.0024(9) O1C 0.0218(7) 0.0204(8) 0.0243(8) 0.0007(6) -0.0040(6) -0.0007(6) C2C 0.0256(12) 0.0302(13) 0.0236(12) 0.0032(10) 0.0020(9) -0.0029(9) C3C 0.0271(12) 0.0302(12) 0.0227(12) -0.0067(10) 0.0000(9) -0.0003(9) O4C 0.0237(8) 0.0219(8) 0.0227(8) -0.0041(6) -0.0029(6) 0.0036(6) C5C 0.0239(11) 0.0251(12) 0.0337(13) -0.0047(10) 0.0005(10) 0.0069(9) C6C 0.0175(11) 0.0299(13) 0.0375(14) -0.0014(10) -0.0047(9) 0.0029(9) O7C 0.0194(7) 0.0290(8) 0.0243(8) -0.0004(6) -0.0078(6) 0.0007(6) C8C 0.0264(12) 0.0274(12) 0.0258(12) 0.0002(9) -0.0119(9) 0.0008(9) C16C 0.0248(11) 0.0248(12) 0.0259(12) 0.0032(9) -0.0087(9) 0.0030(9) O1K 0.0313(8) 0.0203(8) 0.0302(9) -0.0078(7) -0.0110(7) 0.0014(6) C2K 0.0409(14) 0.0211(12) 0.0349(13) -0.0071(10) -0.0092(11) -0.0075(10) C3K 0.0365(13) 0.0268(12) 0.0323(13) -0.0046(10) -0.0059(10) -0.0151(10) O4K 0.0214(8) 0.0257(8) 0.0366(9) -0.0022(7) -0.0057(7) -0.0068(6) C5K 0.0173(11) 0.0441(15) 0.0408(14) -0.0063(12) -0.0061(10) -0.0082(10) C6K 0.0194(11) 0.0435(15) 0.0355(14) -0.0053(11) -0.0124(10) -0.0012(10) O7K 0.0245(8) 0.0327(9) 0.0281(8) -0.0051(7) -0.0110(7) 0.0012(7) C8K 0.0324(13) 0.0275(13) 0.0355(14) -0.0062(10) -0.0155(11) 0.0121(10) C16K 0.0392(14) 0.0272(13) 0.0446(15) -0.0133(11) -0.0177(12) 0.0143(10) O300 0.0433(12) 0.0429(12) 0.1164(19) -0.0424(12) 0.0019(12) -0.0081(9) C301 0.0490(19) 0.064(2) 0.075(2) -0.0253(18) -0.0027(16) -0.0031(15) C302 0.063(2) 0.066(2) 0.069(2) -0.0118(17) -0.0139(17) -0.0288(17) C303 0.078(3) 0.056(2) 0.146(4) -0.053(2) 0.038(3) -0.0286(19) C304 0.0538(19) 0.0436(18) 0.094(3) -0.0317(17) -0.0097(18) 0.0018(14) O100 0.073(4) 0.063(3) 0.0366(18) -0.015(2) -0.003(2) -0.026(3) C101 0.062(5) 0.073(4) 0.055(3) -0.019(3) -0.014(3) -0.031(3) C102 0.064(2) 0.070(2) 0.0543(19) -0.0096(16) -0.0079(16) -0.0237(17) C103 0.0530(18) 0.0545(19) 0.0561(19) -0.0233(15) -0.0167(15) 0.0024(14) C104 0.033(4) 0.059(5) 0.051(5) -0.026(4) 0.002(4) -0.005(4) O200 0.044(6) 0.098(11) 0.045(4) -0.038(6) -0.004(4) -0.004(5) C201 0.049(7) 0.099(13) 0.049(5) -0.045(7) -0.008(5) -0.015(7) C204 0.042(11) 0.068(13) 0.051(8) -0.030(6) -0.010(7) -0.014(9) 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' K K 0.2009 0.2494 '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' 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 N1 Co1 N11 102.83(6) . . N1 Co1 N21 121.61(6) . . N2 Co1 N1 80.63(6) . . N2 Co1 N11 120.18(6) . . N2 Co1 N21 103.38(6) . . N11 Co1 N21 121.91(6) . . O1C K1 O1C 180.00(5) 2_576 . O1C K1 O4C 61.47(4) . . O1C K1 O4C 118.53(4) . 2_576 O1C K1 O4C 118.53(4) 2_576 . O1C K1 O4C 61.47(4) 2_576 2_576 O1C K1 O7C 119.18(4) 2_576 2_576 O1C K1 O7C 119.19(4) . . O1C K1 O7C 60.82(4) 2_576 . O1C K1 O7C 60.81(4) . 2_576 O4C K1 O4C 180.0 . 2_576 O4C K1 O7C 59.24(4) . . O4C K1 O7C 120.76(4) 2_576 . O4C K1 O7C 120.76(4) . 2_576 O4C K1 O7C 59.24(4) 2_576 2_576 O7C K1 O7C 180.0 2_576 . O300 K1 O1C 89.01(6) . 2_576 O300 K1 O1C 89.01(6) 2_576 . O300 K1 O1C 90.99(6) . . O300 K1 O1C 90.99(6) 2_576 2_576 O300 K1 O4C 79.79(5) 2_576 2_576 O300 K1 O4C 100.21(5) . 2_576 O300 K1 O4C 79.79(5) . . O300 K1 O4C 100.21(5) 2_576 . O300 K1 O7C 88.93(5) 2_576 . O300 K1 O7C 88.93(5) . 2_576 O300 K1 O7C 91.07(5) 2_576 2_576 O300 K1 O7C 91.07(5) . . O300 K1 O300 180.0 2_576 . O1K K2 O1K 179.999(13) 2_577 . O1K K2 O4K 119.02(4) . 2_577 O1K K2 O4K 60.98(4) 2_577 2_577 O1K K2 O4K 60.98(4) . . O1K K2 O4K 119.02(4) 2_577 . O1K K2 O7K 119.07(4) 2_577 2_577 O1K K2 O7K 119.07(4) . . O1K K2 O7K 60.93(4) . 2_577 O1K K2 O7K 60.93(4) 2_577 . O1K K2 C201 78.3(4) . 2_577 O1K K2 C201 101.7(4) . . O1K K2 C201 101.7(4) 2_577 2_577 O1K K2 C201 78.3(4) 2_577 . O4K K2 O4K 180.00(6) . 2_577 O4K K2 O7K 120.55(4) . 2_577 O4K K2 O7K 59.45(4) 2_577 2_577 O4K K2 O7K 59.44(4) . . O4K K2 O7K 120.56(4) 2_577 . O4K K2 C201 76.4(2) 2_577 . O4K K2 C201 103.6(2) 2_577 2_577 O4K K2 C201 76.4(2) . 2_577 O4K K2 C201 103.6(2) . . O7K K2 O7K 180.00(6) 2_577 . O7K K2 C201 103.2(4) 2_577 2_577 O7K K2 C201 76.8(4) . 2_577 O7K K2 C201 103.2(4) . . O7K K2 C201 76.8(4) 2_577 . O100 K2 O1K 78.49(16) . 2_577 O100 K2 O1K 101.51(16) 2_577 2_577 O100 K2 O1K 101.51(16) . . O100 K2 O1K 78.49(16) 2_577 . O100 K2 O4K 81.94(14) . . O100 K2 O4K 98.06(14) . 2_577 O100 K2 O4K 98.06(14) 2_577 . O100 K2 O4K 81.94(14) 2_577 2_577 O100 K2 O7K 82.0(2) . . O100 K2 O7K 98.0(2) . 2_577 O100 K2 O7K 98.0(2) 2_577 . O100 K2 O7K 82.0(2) 2_577 2_577 O100 K2 O100 180.0 . 2_577 O100 K2 O200 166.0(3) . 2_577 O100 K2 O200 14.0(3) 2_577 2_577 O100 K2 C201 155.3(2) . 2_577 O100 K2 C201 24.7(2) 2_577 2_577 O200 K2 O1K 89.7(5) . . O200 K2 O1K 90.3(5) 2_577 . O200 K2 O4K 97.6(3) 2_577 . O200 K2 O4K 82.4(3) . . O200 K2 O7K 94.3(4) . . O200 K2 O7K 85.7(4) 2_577 . O200 K2 O200 180.0 2_577 . O200 K2 C201 21.3(4) 2_577 2_577 O200 K2 C201 21.3(4) . . O200 K2 C201 158.7(4) . 2_577 O200 K2 C201 158.7(4) 2_577 . C201 K2 C201 180.0 . 2_577 C1 N1 Co1 126.88(13) . . C1 N1 C5 117.24(16) . . C5 N1 Co1 114.57(12) . . C6 N2 Co1 115.22(13) . . C10 N2 Co1 126.71(13) . . C10 N2 C6 117.44(17) . . N1 C1 H1 117.8 . . N1 C1 C2 124.45(19) . . C2 C1 H1 117.8 . . C1 C2 H2 120.8 . . C1 C2 C3 118.45(19) . . C3 C2 H2 120.8 . . C2 C3 H3 120.5 . . C4 C3 C2 118.91(19) . . C4 C3 H3 120.5 . . C3 C4 H4 119.7 . . C3 C4 C5 120.60(19) . . C5 C4 H4 119.7 . . N1 C5 C4 120.31(18) . . N1 C5 C6 114.71(16) . . C4 C5 C6 124.94(18) . . N2 C6 C5 114.27(17) . . N2 C6 C7 120.86(18) . . C7 C6 C5 124.84(18) . . C6 C7 H7 119.9 . . C8 C7 C6 120.17(19) . . C8 C7 H7 119.9 . . C7 C8 H8 120.6 . . C7 C8 C9 118.86(19) . . C9 C8 H8 120.6 . . C8 C9 H9 120.6 . . C10 C9 C8 118.7(2) . . C10 C9 H9 120.6 . . N2 C10 C9 123.89(19) . . N2 C10 H10 118.1 . . C9 C10 H10 118.1 . . Si11 N11 Co1 115.63(8) . . Si12 N11 Co1 118.99(9) . . Si12 N11 Si11 122.25(10) . . N11 Si11 C111 113.79(9) . . N11 Si11 C112 113.85(9) . . N11 Si11 C113 113.37(9) . . C111 Si11 C113 104.42(10) . . C112 Si11 C111 106.44(12) . . C112 Si11 C113 103.99(10) . . Si11 C111 H11A 109.5 . . Si11 C111 H11B 109.5 . . Si11 C111 H11C 109.5 . . H11A C111 H11B 109.5 . . H11A C111 H11C 109.5 . . H11B C111 H11C 109.5 . . Si11 C112 H11D 109.5 . . Si11 C112 H11E 109.5 . . Si11 C112 H11F 109.5 . . H11D C112 H11E 109.5 . . H11D C112 H11F 109.5 . . H11E C112 H11F 109.5 . . Si11 C113 H11G 109.5 . . Si11 C113 H11H 109.5 . . Si11 C113 H11I 109.5 . . H11G C113 H11H 109.5 . . H11G C113 H11I 109.5 . . H11H C113 H11I 109.5 . . N11 Si12 C121 113.75(9) . . N11 Si12 C122 113.60(9) . . N11 Si12 C123 112.54(9) . . C122 Si12 C121 105.66(10) . . C123 Si12 C121 104.42(10) . . C123 Si12 C122 106.07(10) . . Si12 C121 H12A 109.5 . . Si12 C121 H12B 109.5 . . Si12 C121 H12C 109.5 . . H12A C121 H12B 109.5 . . H12A C121 H12C 109.5 . . H12B C121 H12C 109.5 . . Si12 C122 H12D 109.5 . . Si12 C122 H12E 109.5 . . Si12 C122 H12F 109.5 . . H12D C122 H12E 109.5 . . H12D C122 H12F 109.5 . . H12E C122 H12F 109.5 . . Si12 C123 H12G 109.5 . . Si12 C123 H12H 109.5 . . Si12 C123 H12I 109.5 . . H12G C123 H12H 109.5 . . H12G C123 H12I 109.5 . . H12H C123 H12I 109.5 . . Si21 N21 Co1 118.45(9) . . Si21 N21 Si22 125.32(10) . . Si22 N21 Co1 114.22(8) . . N21 Si21 C211 112.52(9) . . N21 Si21 C212 113.54(9) . . N21 Si21 C213 113.86(9) . . C211 Si21 C212 104.84(10) . . C211 Si21 C213 104.96(10) . . C212 Si21 C213 106.30(10) . . Si21 C211 H21A 109.5 . . Si21 C211 H21B 109.5 . . Si21 C211 H21C 109.5 . . H21A C211 H21B 109.5 . . H21A C211 H21C 109.5 . . H21B C211 H21C 109.5 . . Si21 C212 H21D 109.5 . . Si21 C212 H21E 109.5 . . Si21 C212 H21F 109.5 . . H21D C212 H21E 109.5 . . H21D C212 H21F 109.5 . . H21E C212 H21F 109.5 . . Si21 C213 H21G 109.5 . . Si21 C213 H21H 109.5 . . Si21 C213 H21I 109.5 . . H21G C213 H21H 109.5 . . H21G C213 H21I 109.5 . . H21H C213 H21I 109.5 . . N21 Si22 C221 114.68(9) . . N21 Si22 C222 113.29(9) . . N21 Si22 C223 112.13(9) . . C222 Si22 C221 103.83(10) . . C222 Si22 C223 106.14(10) . . C223 Si22 C221 105.99(10) . . Si22 C221 H22A 109.5 . . Si22 C221 H22B 109.5 . . Si22 C221 H22C 109.5 . . H22A C221 H22B 109.5 . . H22A C221 H22C 109.5 . . H22B C221 H22C 109.5 . . Si22 C222 H22D 109.5 . . Si22 C222 H22E 109.5 . . Si22 C222 H22F 109.5 . . H22D C222 H22E 109.5 . . H22D C222 H22F 109.5 . . H22E C222 H22F 109.5 . . Si22 C223 H22G 109.5 . . Si22 C223 H22H 109.5 . . Si22 C223 H22I 109.5 . . H22G C223 H22H 109.5 . . H22G C223 H22I 109.5 . . H22H C223 H22I 109.5 . . C2C O1C K1 113.88(11) . . C2C O1C C16C 111.50(15) . . C16C O1C K1 114.15(11) . . O1C C2C H2CA 109.9 . . O1C C2C H2CB 109.9 . . O1C C2C C3C 108.75(17) . . H2CA C2C H2CB 108.3 . . C3C C2C H2CA 109.9 . . C3C C2C H2CB 109.9 . . C2C C3C H3CA 109.9 . . C2C C3C H3CB 109.9 . . H3CA C3C H3CB 108.3 . . O4C C3C C2C 109.09(17) . . O4C C3C H3CA 109.9 . . O4C C3C H3CB 109.9 . . C3C O4C K1 112.27(11) . . C3C O4C C5C 111.70(16) . . C5C O4C K1 116.44(12) . . O4C C5C H5CA 110.0 . . O4C C5C H5CB 110.0 . . O4C C5C C6C 108.47(17) . . H5CA C5C H5CB 108.4 . . C6C C5C H5CA 110.0 . . C6C C5C H5CB 110.0 . . C5C C6C H6CA 110.1 . . C5C C6C H6CB 110.1 . . H6CA C6C H6CB 108.4 . . O7C C6C C5C 108.08(17) . . O7C C6C H6CA 110.1 . . O7C C6C H6CB 110.1 . . C6C O7C K1 116.00(12) . . C6C O7C C8C 112.25(15) . . C8C O7C K1 113.50(11) . . O7C C8C H8CA 110.0 . . O7C C8C H8CB 110.0 . . O7C C8C C16C 108.61(17) . 2_576 H8CA C8C H8CB 108.3 . . C16C C8C H8CA 110.0 2_576 . C16C C8C H8CB 110.0 2_576 . O1C C16C C8C 108.40(17) . 2_576 O1C C16C H16C 110.0 . . O1C C16C H16D 110.0 . . C8C C16C H16C 110.0 2_576 . C8C C16C H16D 110.0 2_576 . H16C C16C H16D 108.4 . . C2K O1K K2 114.35(12) . . C16K O1K K2 115.66(13) . . C16K O1K C2K 112.22(16) . . O1K C2K H2KA 110.1 . . O1K C2K H2KB 110.1 . . O1K C2K C3K 108.08(18) . . H2KA C2K H2KB 108.4 . . C3K C2K H2KA 110.1 . . C3K C2K H2KB 110.1 . . C2K C3K H3KA 110.1 . . C2K C3K H3KB 110.1 . . H3KA C3K H3KB 108.4 . . O4K C3K C2K 108.07(18) . . O4K C3K H3KA 110.1 . . O4K C3K H3KB 110.1 . . C3K O4K K2 113.28(12) . . C5K O4K K2 116.47(12) . . C5K O4K C3K 112.97(16) . . O4K C5K H5KA 110.1 . . O4K C5K H5KB 110.1 . . O4K C5K C6K 108.22(18) . . H5KA C5K H5KB 108.4 . . C6K C5K H5KA 110.1 . . C6K C5K H5KB 110.1 . . C5K C6K H6KA 110.0 . . C5K C6K H6KB 110.0 . . H6KA C6K H6KB 108.4 . . O7K C6K C5K 108.47(18) . . O7K C6K H6KA 110.0 . . O7K C6K H6KB 110.0 . . C6K O7K K2 113.76(12) . . C6K O7K C8K 111.98(16) . . C8K O7K K2 110.54(12) . . O7K C8K H8KA 110.0 . . O7K C8K H8KB 110.0 . . O7K C8K C16K 108.42(18) . 2_577 H8KA C8K H8KB 108.4 . . C16K C8K H8KA 110.0 2_577 . C16K C8K H8KB 110.0 2_577 . O1K C16K C8K 108.48(18) . 2_577 O1K C16K H16A 110.0 . . O1K C16K H16B 110.0 . . C8K C16K H16A 110.0 2_577 . C8K C16K H16B 110.0 2_577 . H16A C16K H16B 108.4 . . C301 O300 K1 130.49(16) . . C304 O300 K1 119.65(16) . . C304 O300 C301 109.9(2) . . O300 C301 H30A 110.3 . . O300 C301 H30B 110.3 . . O300 C301 C302 106.9(2) . . H30A C301 H30B 108.6 . . C302 C301 H30A 110.3 . . C302 C301 H30B 110.3 . . C301 C302 H30C 110.8 . . C301 C302 H30D 110.8 . . H30C C302 H30D 108.9 . . C303 C302 C301 104.7(3) . . C303 C302 H30C 110.8 . . C303 C302 H30D 110.8 . . C302 C303 H30E 110.3 . . C302 C303 H30F 110.3 . . H30E C303 H30F 108.5 . . C304 C303 C302 107.2(3) . . C304 C303 H30E 110.3 . . C304 C303 H30F 110.3 . . O300 C304 C303 108.1(3) . . O300 C304 H30G 110.1 . . O300 C304 H30H 110.1 . . C303 C304 H30G 110.1 . . C303 C304 H30H 110.1 . . H30G C304 H30H 108.4 . . C101 O100 K2 115.7(4) . . C104 O100 K2 130.4(7) . . C104 O100 C101 111.4(7) . . O100 C101 H10A 110.4 . . O100 C101 H10B 110.4 . . O100 C101 C102 106.5(4) . . H10A C101 H10B 108.6 . . C102 C101 H10A 110.4 . . C102 C101 H10B 110.4 . . C101 C102 H10C 111.7 . . C101 C102 H10D 111.7 . . C101 C102 C103 100.2(4) . . H10C C102 H10D 109.5 . . H10E C102 H10F 108.5 . . C103 C102 H10C 111.7 . . C103 C102 H10D 111.7 . . C103 C102 H10E 110.2 . . C103 C102 H10F 110.2 . . C103 C102 C201 107.3(6) . . C201 C102 H10E 110.2 . . C201 C102 H10F 110.2 . . C102 C103 H10G 111.2 . . C102 C103 H10H 111.2 . . C102 C103 H10I 110.7 . . C102 C103 H10J 110.7 . . C102 C103 C104 102.7(7) . . H10G C103 H10H 109.1 . . H10I C103 H10J 108.8 . . C104 C103 H10G 111.2 . . C104 C103 H10H 111.2 . . C204 C103 C102 105.3(17) . . C204 C103 H10I 110.7 . . C204 C103 H10J 110.7 . . O100 C104 C103 102.1(10) . . O100 C104 H10K 111.3 . . O100 C104 H10L 111.3 . . C103 C104 H10K 111.3 . . C103 C104 H10L 111.3 . . H10K C104 H10L 109.2 . . C201 O200 K2 112.7(9) . . C201 O200 C204 105.7(18) . . C204 O200 K2 134.0(17) . . K2 C201 H20A 99.7 . . K2 C201 H20B 72.3 . . C102 C201 K2 146.3(8) . . C102 C201 H20A 110.3 . . C102 C201 H20B 110.3 . . O200 C201 K2 46.0(7) . . O200 C201 C102 107.0(10) . . O200 C201 H20A 110.3 . . O200 C201 H20B 110.3 . . H20A C201 H20B 108.6 . . C103 C204 O200 114(3) . . C103 C204 H20C 108.7 . . C103 C204 H20D 108.7 . . O200 C204 H20C 108.7 . . O200 C204 H20D 108.7 . . H20C C204 H20D 107.6 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 N1 1.9980(16) . Co1 N2 1.9966(16) . Co1 N11 2.0037(16) . Co1 N21 2.0079(16) . K1 O1C 2.7693(14) 2_576 K1 O1C 2.7693(14) . K1 O4C 2.8015(14) 2_576 K1 O4C 2.8015(14) . K1 O7C 2.8177(14) 2_576 K1 O7C 2.8177(14) . K1 O300 2.7332(18) 2_576 K1 O300 2.7332(18) . K2 O1K 2.7519(14) . K2 O1K 2.7518(14) 2_577 K2 O4K 2.7995(14) . K2 O4K 2.7996(14) 2_577 K2 O7K 2.8467(14) . K2 O7K 2.8467(14) 2_577 K2 O100 2.720(6) 2_577 K2 O100 2.720(6) . K2 O200 2.735(13) 2_577 K2 O200 2.735(13) . K2 C201 3.506(14) . K2 C201 3.506(14) 2_577 N1 C1 1.359(2) . N1 C5 1.385(2) . N2 C6 1.379(2) . N2 C10 1.357(2) . C1 H1 0.9500 . C1 C2 1.369(3) . C2 H2 0.9500 . C2 C3 1.405(3) . C3 H3 0.9500 . C3 C4 1.371(3) . C4 H4 0.9500 . C4 C5 1.413(3) . C5 C6 1.432(3) . C6 C7 1.404(3) . C7 H7 0.9500 . C7 C8 1.365(3) . C8 H8 0.9500 . C8 C9 1.412(3) . C9 H9 0.9500 . C9 C10 1.360(3) . C10 H10 0.9500 . N11 Si11 1.7004(16) . N11 Si12 1.6964(16) . Si11 C111 1.884(2) . Si11 C112 1.874(2) . Si11 C113 1.885(2) . C111 H11A 0.9800 . C111 H11B 0.9800 . C111 H11C 0.9800 . C112 H11D 0.9800 . C112 H11E 0.9800 . C112 H11F 0.9800 . C113 H11G 0.9800 . C113 H11H 0.9800 . C113 H11I 0.9800 . Si12 C121 1.888(2) . Si12 C122 1.886(2) . Si12 C123 1.874(2) . C121 H12A 0.9800 . C121 H12B 0.9800 . C121 H12C 0.9800 . C122 H12D 0.9800 . C122 H12E 0.9800 . C122 H12F 0.9800 . C123 H12G 0.9800 . C123 H12H 0.9800 . C123 H12I 0.9800 . N21 Si21 1.6928(16) . N21 Si22 1.6983(16) . Si21 C211 1.871(2) . Si21 C212 1.887(2) . Si21 C213 1.887(2) . C211 H21A 0.9800 . C211 H21B 0.9800 . C211 H21C 0.9800 . C212 H21D 0.9800 . C212 H21E 0.9800 . C212 H21F 0.9800 . C213 H21G 0.9800 . C213 H21H 0.9800 . C213 H21I 0.9800 . Si22 C221 1.893(2) . Si22 C222 1.877(2) . Si22 C223 1.884(2) . C221 H22A 0.9800 . C221 H22B 0.9800 . C221 H22C 0.9800 . C222 H22D 0.9800 . C222 H22E 0.9800 . C222 H22F 0.9800 . C223 H22G 0.9800 . C223 H22H 0.9800 . C223 H22I 0.9800 . O1C C2C 1.424(2) . O1C C16C 1.427(2) . C2C H2CA 0.9900 . C2C H2CB 0.9900 . C2C C3C 1.497(3) . C3C H3CA 0.9900 . C3C H3CB 0.9900 . C3C O4C 1.421(2) . O4C C5C 1.426(2) . C5C H5CA 0.9900 . C5C H5CB 0.9900 . C5C C6C 1.489(3) . C6C H6CA 0.9900 . C6C H6CB 0.9900 . C6C O7C 1.424(2) . O7C C8C 1.424(2) . C8C H8CA 0.9900 . C8C H8CB 0.9900 . C8C C16C 1.495(3) 2_576 C16C H16C 0.9900 . C16C H16D 0.9900 . O1K C2K 1.423(2) . O1K C16K 1.419(3) . C2K H2KA 0.9900 . C2K H2KB 0.9900 . C2K C3K 1.495(3) . C3K H3KA 0.9900 . C3K H3KB 0.9900 . C3K O4K 1.426(3) . O4K C5K 1.419(3) . C5K H5KA 0.9900 . C5K H5KB 0.9900 . C5K C6K 1.492(3) . C6K H6KA 0.9900 . C6K H6KB 0.9900 . C6K O7K 1.420(3) . O7K C8K 1.426(3) . C8K H8KA 0.9900 . C8K H8KB 0.9900 . C8K C16K 1.495(3) 2_577 C16K H16A 0.9900 . C16K H16B 0.9900 . O300 C301 1.408(3) . O300 C304 1.408(3) . C301 H30A 0.9900 . C301 H30B 0.9900 . C301 C302 1.491(4) . C302 H30C 0.9900 . C302 H30D 0.9900 . C302 C303 1.467(5) . C303 H30E 0.9900 . C303 H30F 0.9900 . C303 C304 1.452(4) . C304 H30G 0.9900 . C304 H30H 0.9900 . O100 C101 1.438(8) . O100 C104 1.398(18) . C101 H10A 0.9900 . C101 H10B 0.9900 . C101 C102 1.496(7) . C102 H10C 0.9900 . C102 H10D 0.9900 . C102 H10E 0.9900 . C102 H10F 0.9900 . C102 C103 1.501(4) . C102 C201 1.555(17) . C103 H10G 0.9900 . C103 H10H 0.9900 . C103 H10I 0.9900 . C103 H10J 0.9900 . C103 C104 1.551(15) . C103 C204 1.33(4) . C104 H10K 0.9900 . C104 H10L 0.9900 . O200 C201 1.381(19) . O200 C204 1.54(4) . C201 H20A 0.9900 . C201 H20B 0.9900 . C204 H20C 0.9900 . C204 H20D 0.9900 . 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 Co1 N1 C1 C2 167.82(16) . . . . Co1 N1 C5 C4 -169.66(15) . . . . Co1 N1 C5 C6 8.2(2) . . . . Co1 N2 C6 C5 4.9(2) . . . . Co1 N2 C6 C7 -173.20(15) . . . . Co1 N2 C10 C9 171.86(15) . . . . Co1 N11 Si11 C111 73.27(13) . . . . Co1 N11 Si11 C112 -48.95(13) . . . . Co1 N11 Si11 C113 -167.58(9) . . . . Co1 N11 Si12 C121 -108.47(11) . . . . Co1 N11 Si12 C122 130.59(10) . . . . Co1 N11 Si12 C123 10.03(13) . . . . Co1 N21 Si21 C211 8.46(13) . . . . Co1 N21 Si21 C212 127.35(11) . . . . Co1 N21 Si21 C213 -110.83(11) . . . . Co1 N21 Si22 C221 174.86(10) . . . . Co1 N21 Si22 C222 55.90(12) . . . . Co1 N21 Si22 C223 -64.21(11) . . . . K1 O1C C2C C3C -49.2(2) . . . . K1 O1C C16C C8C 51.96(19) . . . 2_576 K1 O4C C5C C6C 48.5(2) . . . . K1 O7C C8C C16C -47.99(19) . . . 2_576 K1 O300 C301 C302 -164.6(2) . . . . K1 O300 C304 C303 174.0(3) . . . . K2 O1K C2K C3K -51.8(2) . . . . K2 O1K C16K C8K 48.2(2) . . . 2_577 K2 O4K C5K C6K 48.3(2) . . . . K2 O7K C8K C16K -53.07(19) . . . 2_577 K2 O100 C101 C102 156.7(7) . . . . K2 O100 C104 C103 -179.1(6) . . . . K2 O200 C201 C102 -156.1(14) . . . . K2 O200 C204 C103 143(2) . . . . N1 C1 C2 C3 -0.3(3) . . . . N1 C5 C6 N2 -8.5(2) . . . . N1 C5 C6 C7 169.50(18) . . . . N2 C6 C7 C8 0.7(3) . . . . C1 N1 C5 C4 -1.8(3) . . . . C1 N1 C5 C6 176.02(17) . . . . C1 C2 C3 C4 -1.0(3) . . . . C2 C3 C4 C5 0.8(3) . . . . C3 C4 C5 N1 0.6(3) . . . . C3 C4 C5 C6 -176.96(19) . . . . C4 C5 C6 N2 169.19(18) . . . . C4 C5 C6 C7 -12.8(3) . . . . C5 N1 C1 C2 1.7(3) . . . . C5 C6 C7 C8 -177.2(2) . . . . C6 N2 C10 C9 1.5(3) . . . . C6 C7 C8 C9 0.6(3) . . . . C7 C8 C9 C10 -0.9(3) . . . . C8 C9 C10 N2 -0.2(3) . . . . C10 N2 C6 C5 176.36(17) . . . . C10 N2 C6 C7 -1.7(3) . . . . Si11 N11 Si12 C121 50.61(14) . . . . Si11 N11 Si12 C122 -70.33(14) . . . . Si11 N11 Si12 C123 169.12(11) . . . . Si12 N11 Si11 C111 -86.47(14) . . . . Si12 N11 Si11 C112 151.31(12) . . . . Si12 N11 Si11 C113 32.68(15) . . . . Si21 N21 Si22 C221 11.31(15) . . . . Si21 N21 Si22 C222 -107.64(13) . . . . Si21 N21 Si22 C223 132.25(12) . . . . Si22 N21 Si21 C211 171.37(12) . . . . Si22 N21 Si21 C212 -69.75(14) . . . . Si22 N21 Si21 C213 52.08(15) . . . . O1C C2C C3C O4C 67.8(2) . . . . C2C O1C C16C C8C -177.24(17) . . . 2_576 C2C C3C O4C K1 -50.45(19) . . . . C2C C3C O4C C5C 176.64(17) . . . . C3C O4C C5C C6C 179.31(17) . . . . O4C C5C C6C O7C -63.6(2) . . . . C5C C6C O7C K1 48.8(2) . . . . C5C C6C O7C C8C -178.43(17) . . . . C6C O7C C8C C16C 178.03(17) . . . 2_576 C16C O1C C2C C3C 179.89(17) . . . . O1K C2K C3K O4K 67.6(2) . . . . C2K O1K C16K C8K -178.18(18) . . . 2_577 C2K C3K O4K K2 -49.11(19) . . . . C2K C3K O4K C5K 175.70(18) . . . . C3K O4K C5K C6K -178.01(18) . . . . O4K C5K C6K O7K -65.9(2) . . . . C5K C6K O7K K2 51.0(2) . . . . C5K C6K O7K C8K 177.24(18) . . . . C6K O7K C8K C16K 178.96(18) . . . 2_577 C16K O1K C2K C3K 173.94(19) . . . . O300 C301 C302 C303 -18.3(4) . . . . C301 O300 C304 C303 -5.9(4) . . . . C301 C302 C303 C304 14.7(5) . . . . C302 C303 C304 O300 -6.1(5) . . . . C304 O300 C301 C302 15.2(4) . . . . O100 C101 C102 C103 30.0(5) . . . . C101 O100 C104 C103 -18.0(12) . . . . C101 C102 C103 C104 -40.0(8) . . . . C102 C103 C104 O100 36.6(11) . . . . C102 C103 C204 O200 7(3) . . . . C103 C102 C201 K2 -26(2) . . . . C103 C102 C201 O200 6.0(12) . . . . C104 O100 C101 C102 -7.4(9) . . . . C201 C102 C103 C204 -8(2) . . . . C201 O200 C204 C103 -3(3) . . . . C204 O200 C201 K2 154(2) . . . . C204 O200 C201 C102 -2(2) . . . .