#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/91/4329104.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_4329104 loop_ _publ_author_name 'Mitsuaki Suzuki' 'Xing Lu' 'Satoru Sato' 'Hidefumi Nikawa' 'Naomi Mizorogi' 'Zdenek Slanina' 'Takahiro Tsuchiya' 'Shigeru Nagase' 'Takeshi Akasaka' _publ_section_title ; Where Does the Metal Cation Stay in Gd@C2v(9)-C82? A Single-Crystal X-ray Diffraction Study ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 5270 _journal_page_last 5273 _journal_paper_doi 10.1021/ic300186y _journal_volume 51 _journal_year 2012 _chemical_formula_moiety 'Gd C82, Ni N4 C36 H44, 1.4(C6 H6), 0.6(C H Cl3)' _chemical_formula_sum 'C127 H53 Cl1.8 Gd N4 Ni' _chemical_formula_weight 1914.50 _chemical_name_common Gd@C82/NiOEP/1.4benzene/0.6chloroform _chemical_name_systematic ; ? ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.998(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 25.3645(9) _cell_length_b 15.1820(6) _cell_length_c 19.7167(7) _cell_measurement_reflns_used 9929 _cell_measurement_temperature 90 _cell_measurement_theta_max 27.20 _cell_measurement_theta_min 2.51 _cell_volume 7563.7(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita, et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, et al., 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 90 _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 33392 _diffrn_reflns_theta_full 27.10 _diffrn_reflns_theta_max 27.10 _diffrn_reflns_theta_min 1.04 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_T_max 0.9065 _exptl_absorpt_correction_T_min 0.6829 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.681 _exptl_crystal_description plate _exptl_crystal_F_000 3862 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.091 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1025 _refine_ls_number_reflns 8660 _refine_ls_number_restraints 946 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0654 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+38.2145P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1745 _refine_ls_wR_factor_ref 0.1858 _reflns_number_gt 7175 _reflns_number_total 8660 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL Gd@C82/NiOEP/1.4benzene/0.6chloroform REM Yadorkari-X generated CELL 0.71073 25.3645 15.1820 19.7167 90.0000 94.9980 90.0000 ZERR 4.0 0.0009 0.0006 0.0007 0.0000 0.0020 0.0000 LATT 7 SYMM -X, +Y, -Z REM SPGR C2/m monoclinic SFAC C H N Cl Ni Gd UNIT 508 212 16 7.2 4 4 SIZE 0.33 0.23 0.08 TEMP -183.0 L.S. 10 FMAP 2 PLAN -25 ACTA CONF BOND $H MERG 2 EQIV $1 +X, -Y, +Z FREE C71 C71_$1 SIMU 0.01 0.01 C1 > C82 SADI 0.01 C47 C68 C75 C58 SADI 0.01 C54 C51 C65 C62 SADI 0.01 C20 C5 C2 C12 SADI 0.01 C63 C64 C53 C52 SADI 0.01 C72 C71 C79 C78 SADI 0.01 C11 C13 C19 C21 SADI 0.01 C19 C20 C20 C21 C11 C12 C12 C13 SADI 0.01 C51 C71 C54 C72 C78 C62 C79 C65 SADI 0.01 C51 C71 C79 C65 C78 C62 C72 C54 SADI 0.01 C77 C82 C82 C73 C80 C81 C81 C70 SADI 0.01 C73 C72 C71 C70 C80 C79 C78 C77 SADI 0.01 C64 C65 C51 C52 C53 C54 C63 C62 SADI 0.01 C50 C51 C66 C65 C62 C61 C54 C55 SADI 0.01 C13 C14 C19 C18 C22 C21 C10 C11 SADI 0.01 C41 C40 C32 C31 C30 C29 C42 C43 SADI 0.01 C40 C63 C53 C32 C43 C64 C52 C29 SADI 0.01 C41 C19 C13 C31 C30 C11 C21 C42 SADI 0.01 C77 C76 C73 C74 C69 C70 C67 C80 SADI 0.01 C61 C76 C66 C67 C69 C50 C74 C55 SADI 0.01 C74 C75 C75 C76 C67 C68 C68 C69 SADI 0.01 C56 C33 C28 C49 C60 C39 C45 C44 SADI 0.01 C39 C38 C44 C23 C34 C33 C27 C28 SADI 0.01 C23 C24 C38 C37 C35 C34 C26 C27 SADI 0.01 C18 C38 C22 C23 C14 C34 C10 C27 SADI 0.01 C37 C36 C36 C35 C26 C25 C25 C24 SADI 0.01 C33 C32 C39 C40 C29 C28 C43 C44 SADI 0.01 C4 C5 C5 C6 C1 C2 C2 C3 SADI 0.01 C1 C9 C6 C7 C4 C17 C3 C15 SADI 0.01 C45 C66 C61 C60 C49 C50 C55 C56 SADI 0.01 C79 C82 C78 C81 C71 C82 C72 C81 SADI 0.01 C7 C22 C18 C17 C9 C10 C14 C15 SADI 0.01 C79 C67 C78 C76 C74 C72 C71 C69 SADI 0.01 C6 C20 C20 C4 C1 C12 C12 C3 SADI 0.01 C66 C47 C47 C50 C55 C58 C58 C61 SADI 0.01 C17 C16 C16 C15 C9 C8 C8 C7 SADI 0.01 C24 C46 C59 C37 C35 C57 C26 C48 SADI 0.01 C62 C77 C54 C73 C65 C80 C70 C51 SADI 0.01 C57 C58 C58 C59 C46 C47 C47 C48 SADI 0.01 C60 C75 C75 C56 C49 C68 C68 C45 SADI 0.01 C60 C59 C57 C56 C49 C48 C46 C45 SADI 0.01 C61 C76 C66 C67 C74 C55 C69 C50 DFIX 1.38 0.02 C71 C72 C79 C78 DFIX 1.38 0.02 C12 C2 C5 C20 WGHT 0.093100 38.214500 FVAR 0.03975 PART -1 C1 1 0.297138 -0.218512 0.181760 10.50000 0.05576 0.04440 = 0.06231 -0.03783 -0.01892 0.00755 C2 1 0.349735 -0.232335 0.214459 10.50000 0.06275 0.04900 = 0.07467 -0.01667 0.00053 0.01344 C3 1 0.391275 -0.171394 0.200212 10.50000 0.04934 0.05038 = 0.07844 -0.00744 0.03026 0.00761 C4 1 0.374617 -0.100042 0.152761 10.50000 0.05993 0.08637 = 0.05425 -0.02104 0.02029 0.01202 C5 1 0.323105 -0.086070 0.118988 10.50000 0.09210 0.06325 = 0.04011 -0.01043 0.02056 0.00905 C6 1 0.281914 -0.148236 0.130951 10.50000 0.07902 0.05183 = 0.04127 -0.02203 -0.00218 -0.01063 C7 1 0.225608 -0.127015 0.138614 10.50000 0.07961 0.05783 = 0.05428 -0.02211 -0.03031 -0.00423 C8 1 0.207547 -0.182866 0.189670 10.50000 0.05610 0.05014 = 0.09246 -0.03064 -0.02495 -0.00713 C9 1 0.248861 -0.237347 0.218347 10.50000 0.06108 0.03462 = 0.08631 -0.02311 -0.02232 -0.00918 C10 1 0.250843 -0.260622 0.289516 10.50000 0.05968 0.02380 = 0.09331 -0.00054 -0.00731 -0.01613 C11 1 0.302528 -0.273397 0.319514 10.50000 0.06153 0.01417 = 0.06689 0.01156 -0.00580 -0.00993 C12 1 0.351266 -0.258477 0.280002 10.50000 0.06234 0.01637 = 0.04288 0.00077 -0.00647 0.01118 C13 1 0.393012 -0.225641 0.335626 10.50000 0.04335 0.02687 = 0.05331 0.01439 -0.01671 0.01406 C14 1 0.431296 -0.162713 0.323524 10.50000 0.03337 0.04984 = 0.07914 0.01027 -0.00847 0.01897 C15 1 0.430203 -0.133157 0.253257 10.50000 0.03792 0.06447 = 0.07814 0.00034 0.01934 0.02018 C16 1 0.437764 -0.045311 0.234040 10.50000 0.03111 0.07180 = 0.06244 -0.00550 0.02603 0.00911 C17 1 0.406142 -0.019816 0.175319 10.50000 0.04582 0.06157 = 0.05059 -0.00528 0.03272 -0.00047 C18 1 0.387672 0.068766 0.163546 10.50000 0.07816 0.07348 = 0.05575 0.00877 0.04400 -0.00479 C19 1 0.339872 0.078705 0.125394 10.50000 0.08716 0.05667 = 0.04002 0.00859 0.03618 -0.01056 C20 1 0.308716 -0.003921 0.104175 10.50000 0.11389 0.05492 = 0.03456 -0.00038 0.02883 0.00894 C21 1 0.251602 0.026585 0.105212 10.50000 0.09731 0.05268 = 0.01961 0.00407 -0.00350 0.01454 C22 1 0.213987 -0.035332 0.121348 10.50000 0.08937 0.06348 = 0.04484 -0.01304 -0.03595 0.00426 C23 1 0.172249 -0.008494 0.157358 10.50000 0.05289 0.07108 = 0.08749 -0.00150 -0.04518 0.00627 C24 1 0.149274 -0.061886 0.209751 10.50000 0.03323 0.06905 = 0.09773 0.00302 -0.02250 -0.00848 C25 1 0.167278 -0.146484 0.230684 10.50000 0.03962 0.05850 = 0.09887 -0.01836 -0.01401 -0.01708 C26 1 0.168557 -0.171830 0.299537 10.50000 0.05761 0.05914 = 0.10827 0.01051 0.01129 -0.03158 C27 1 0.211541 -0.228635 0.328386 10.50000 0.07641 0.04345 = 0.09536 0.01700 0.01251 -0.03285 C28 1 0.225351 -0.207234 0.399487 10.50000 0.09712 0.05402 = 0.09023 0.01986 0.04822 -0.01860 C29 1 0.278235 -0.213001 0.430484 10.50000 0.11361 0.03795 = 0.06098 0.01938 0.03567 -0.01723 C30 1 0.316754 -0.247999 0.389059 10.50000 0.07525 0.02280 = 0.06085 0.01657 0.00046 -0.01333 C31 1 0.370961 -0.219081 0.398684 10.50000 0.06270 0.02738 = 0.04381 0.00976 -0.03102 0.00217 C32 1 0.381946 -0.153039 0.449067 10.50000 0.09394 0.03132 = 0.03405 0.01175 -0.03395 -0.00328 C33 1 0.423305 -0.094156 0.437478 10.50000 0.06679 0.05078 = 0.06536 0.02559 -0.04701 -0.00517 C34 1 0.445547 -0.098923 0.372073 10.50000 0.02785 0.05345 = 0.08413 0.01080 -0.02779 0.00911 C35 1 0.459688 -0.010728 0.353273 10.50000 0.02512 0.08528 = 0.07568 -0.00561 -0.01134 0.00553 C36 1 0.454588 0.019444 0.286382 10.50000 0.02580 0.08421 = 0.06659 -0.00419 0.01419 -0.00214 C37 1 0.438801 0.105669 0.273507 10.50000 0.04612 0.07506 = 0.07654 0.00146 0.01525 -0.02296 C38 1 0.405706 0.130981 0.212910 10.50000 0.06698 0.07368 = 0.06823 0.01198 0.02599 -0.02503 C39 1 0.371177 0.204475 0.222445 10.50000 0.07493 0.05785 = 0.09998 0.01434 0.02754 -0.02616 C40 1 0.318587 0.210010 0.189885 10.50000 0.07051 0.04792 = 0.08881 0.01995 0.00876 -0.01194 C41 1 0.302524 0.147338 0.139674 10.50000 0.07671 0.04929 = 0.05763 0.02179 0.02218 0.00184 C42 1 0.249687 0.117055 0.128015 10.50000 0.06987 0.04080 = 0.02927 0.01620 -0.00070 0.00333 C43 1 0.209809 0.149700 0.168200 10.50000 0.05313 0.04198 = 0.05379 0.00506 -0.01210 0.01914 C44 1 0.170162 0.084572 0.176036 10.50000 0.03230 0.04922 = 0.08099 0.01308 -0.03358 0.01306 C45 1 0.145434 0.086590 0.238895 10.50000 0.02139 0.05935 = 0.09722 0.00700 -0.01068 0.01832 C46 1 0.132975 -0.005938 0.261658 10.50000 0.02356 0.07175 = 0.10824 0.00388 0.00536 0.00875 C47 1 0.135474 -0.030516 0.328302 10.50000 0.05120 0.09743 = 0.09924 0.00202 0.03943 0.00684 C48 1 0.149885 -0.112367 0.347261 10.50000 0.06567 0.09115 = 0.10595 0.01024 0.03834 -0.02200 C49 1 0.187040 -0.140788 0.407162 10.50000 0.10537 0.07900 = 0.09247 0.02039 0.05190 -0.01399 C50 1 0.197193 -0.081516 0.455574 10.50000 0.13347 0.09173 = 0.08290 0.01591 0.05216 0.00360 C51 1 0.248455 -0.088194 0.493095 10.50000 0.14346 0.05851 = 0.03352 0.02369 0.04456 0.00320 C52 1 0.290502 -0.147557 0.480755 10.50000 0.14683 0.06088 = 0.04825 0.02103 0.02639 -0.01987 C53 1 0.344907 -0.119790 0.491460 10.50000 0.12091 0.06576 = 0.02909 0.01225 -0.00334 0.00216 C54 1 0.348170 -0.030192 0.515304 10.50000 0.10569 0.08873 = 0.02999 0.00380 -0.02149 -0.01613 C55 1 0.389530 0.023504 0.495826 10.50000 0.09268 0.07859 = 0.04662 0.00799 -0.04002 -0.01447 C56 1 0.426799 -0.007161 0.459998 10.50000 0.08793 0.08186 = 0.07091 0.00870 -0.04406 -0.00966 C57 1 0.448524 0.048480 0.405457 10.50000 0.04600 0.07461 = 0.07362 -0.01077 -0.02805 -0.01479 C58 1 0.433178 0.132055 0.391852 10.50000 0.07197 0.07416 = 0.08675 -0.02128 -0.01586 -0.02756 C59 1 0.427746 0.161785 0.328030 10.50000 0.06519 0.07195 = 0.09782 -0.00207 -0.00257 -0.04241 C60 1 0.387812 0.222523 0.291124 10.50000 0.08168 0.05839 = 0.12772 -0.00692 0.01959 -0.03588 C61 1 0.352432 0.255098 0.329211 10.50000 0.10623 0.05831 = 0.13963 -0.01613 -0.00420 -0.02164 C62 1 0.300169 0.268270 0.295310 10.50000 0.09001 0.02673 = 0.12114 -0.01262 -0.03039 0.00146 C63 1 0.279728 0.245147 0.228537 10.50000 0.07546 0.02503 = 0.08445 -0.00053 -0.00307 0.00652 C64 1 0.224718 0.214400 0.218705 10.50000 0.06257 0.02871 = 0.06534 0.00112 -0.00796 0.02083 C65 1 0.197382 0.215206 0.277893 10.50000 0.06038 0.04190 = 0.07473 -0.00266 -0.00652 0.03590 C66 1 0.157497 0.149251 0.285839 10.50000 0.04155 0.06719 = 0.08989 -0.00892 0.00059 0.03905 C67 1 0.160988 0.123459 0.360353 10.50000 0.07033 0.08729 = 0.08503 -0.01369 0.02519 0.03641 C68 1 0.151350 0.039569 0.382137 10.50000 0.08306 0.09808 = 0.09117 0.00905 0.04483 0.02601 C69 1 0.177421 0.010688 0.441599 10.50000 0.10800 0.09033 = 0.06870 -0.00311 0.04767 0.02476 C70 1 0.219903 0.061243 0.475791 10.50000 0.11340 0.10465 = 0.06304 0.00280 0.02071 0.04550 C71 1 0.256805 0.005830 0.508446 10.50000 0.14780 0.11890 = 0.06050 -0.00092 0.01807 0.01060 C72 1 0.305918 0.035601 0.519750 10.50000 0.10712 0.12038 = 0.02819 -0.02473 -0.01174 -0.01614 C73 1 0.320045 0.119795 0.498446 10.50000 0.09088 0.10103 = 0.04674 -0.04474 -0.02826 0.01872 C74 1 0.374088 0.118609 0.482564 10.50000 0.09290 0.07844 = 0.05864 -0.02134 -0.03159 -0.01932 C75 1 0.392296 0.172435 0.434145 10.50000 0.09632 0.07021 = 0.08547 -0.03236 -0.01563 -0.02168 C76 1 0.355563 0.227162 0.401876 10.50000 0.10907 0.05905 = 0.10474 -0.02993 -0.02586 -0.01171 C77 1 0.301166 0.236466 0.414712 10.50000 0.10896 0.05504 = 0.09289 -0.03957 -0.01155 0.01664 C78 1 0.270767 0.261642 0.355786 10.50000 0.09983 0.03678 = 0.09813 -0.02514 -0.01438 0.02545 C79 1 0.219971 0.236483 0.346868 10.50000 0.08680 0.04176 = 0.07844 -0.02516 -0.01821 0.04590 C80 1 0.198289 0.182963 0.395575 10.50000 0.08982 0.06874 = 0.07863 -0.02593 0.00219 0.05068 C81 1 0.227839 0.149694 0.454131 10.50000 0.09681 0.07789 = 0.05313 -0.02379 0.00607 0.05289 C82 1 0.283937 0.179488 0.464993 10.50000 0.11508 0.08109 = 0.06639 -0.03982 -0.00139 0.03087 PART -3 GD1 6 0.334960 -0.092067 0.256616 10.21000 0.06697 0.06413 = 0.11201 -0.05066 0.05974 -0.02240 PART -2 GD2 6 0.338091 -0.105762 0.277989 10.19000 0.01931 0.03575 = 0.04856 -0.02150 0.00005 0.01177 PART -4 GD3 6 0.357878 -0.079570 0.293752 10.07000 0.03985 0.06811 = 0.05012 -0.02245 -0.00712 0.02627 PART -5 GD4 6 0.373682 -0.018892 0.318895 10.03000 0.05834 PART 5 NI1 5 0.480618 0.000000 0.080804 10.50000 0.01274 0.01592 = 0.02264 0.00000 0.00018 0.00000 N1 3 0.423249 0.000000 0.007941 10.50000 0.01375 0.01791 = 0.02494 0.00000 0.00156 0.00000 N2 3 0.479382 0.129710 0.082165 11.00000 0.01518 0.01933 = 0.02623 0.00040 0.00132 0.00020 N3 3 0.535137 0.000000 0.157471 10.50000 0.01491 0.01961 = 0.02752 0.00000 0.00114 0.00000 C83 1 0.355038 0.044910 -0.071544 11.00000 0.01344 0.02653 = 0.02551 -0.00017 0.00263 0.00078 C84 1 0.397460 0.071672 -0.022657 11.00000 0.01358 0.02366 = 0.02463 0.00035 0.00235 0.00246 C85 1 0.409185 0.158380 -0.007483 11.00000 0.01653 0.02088 = 0.02642 0.00194 0.00182 0.00376 AFIX 43 H85 2 0.389782 0.202553 -0.033030 11.00000 -1.20000 AFIX 0 C86 1 0.447145 0.185165 0.042236 11.00000 0.01631 0.01968 = 0.02800 0.00120 0.00349 0.00197 C87 1 0.456771 0.276469 0.059916 11.00000 0.01867 0.02017 = 0.03333 0.00020 0.00437 -0.00013 C88 1 0.495544 0.276565 0.112188 11.00000 0.01932 0.01855 = 0.03527 -0.00035 0.00180 -0.00099 C89 1 0.509313 0.185309 0.125150 11.00000 0.01628 0.01948 = 0.02859 -0.00157 0.00268 -0.00148 C90 1 0.546639 0.158534 0.175880 11.00000 0.01490 0.02150 = 0.02954 -0.00203 0.00011 -0.00387 AFIX 43 H90 2 0.566075 0.202599 0.201507 11.00000 -1.20000 AFIX 0 C91 1 0.557448 0.071674 0.191646 11.00000 0.01470 0.02330 = 0.02763 -0.00033 0.00028 -0.00216 C92 1 0.316683 0.106370 -0.109189 11.00000 0.01801 0.03024 = 0.03099 0.00216 -0.00155 0.00299 AFIX 23 H92A 2 0.300428 0.076674 -0.150562 11.00000 -1.20000 H92B 2 0.335896 0.158900 -0.123734 11.00000 -1.20000 AFIX 0 C93 1 0.273036 0.135489 -0.064946 11.00000 0.02362 0.04340 = 0.05092 0.01051 0.00712 0.01359 AFIX 137 H93A 2 0.254095 0.083573 -0.050243 11.00000 -1.50000 H93B 2 0.248207 0.174393 -0.091406 11.00000 -1.50000 H93C 2 0.288907 0.167116 -0.024908 11.00000 -1.50000 AFIX 0 C94 1 0.427307 0.353006 0.026828 11.00000 0.02345 0.01934 = 0.04522 0.00164 -0.00157 0.00170 AFIX 23 H94A 2 0.423382 0.343709 -0.023055 11.00000 -1.20000 H94B 2 0.448388 0.407265 0.035949 11.00000 -1.20000 AFIX 0 C95 1 0.372405 0.366133 0.051993 11.00000 0.02966 0.02903 = 0.05978 -0.00089 0.00375 0.01121 AFIX 137 H95A 2 0.351747 0.311873 0.044776 11.00000 -1.50000 H95B 2 0.354216 0.414461 0.026667 11.00000 -1.50000 H95C 2 0.376121 0.380463 0.100639 11.00000 -1.50000 AFIX 0 C96 1 0.518901 0.353260 0.152417 11.00000 0.02765 0.02071 = 0.04671 -0.00245 -0.00541 -0.00171 AFIX 23 H96A 2 0.512483 0.407722 0.125338 11.00000 -1.20000 H96B 2 0.557668 0.344948 0.160212 11.00000 -1.20000 AFIX 0 C97 1 0.496117 0.364943 0.221171 11.00000 0.03979 0.03146 = 0.05488 -0.01683 -0.00129 0.00053 AFIX 137 H97A 2 0.458027 0.376423 0.213823 11.00000 -1.50000 H97B 2 0.513595 0.414714 0.245492 11.00000 -1.50000 H97C 2 0.502132 0.311178 0.248249 11.00000 -1.50000 AFIX 0 C98 1 0.621328 0.107009 0.298603 11.00000 0.02396 0.02979 = 0.04149 -0.00246 -0.01205 -0.00308 AFIX 23 H98A 2 0.637168 0.154927 0.273034 11.00000 -1.20000 H98B 2 0.650497 0.075466 0.324977 11.00000 -1.20000 AFIX 0 C99 1 0.584880 0.147376 0.348033 11.00000 0.03804 0.03633 = 0.03492 -0.00538 -0.01076 -0.00478 AFIX 137 H99A 2 0.555997 0.179061 0.322321 11.00000 -1.50000 H99B 2 0.605107 0.188434 0.378568 11.00000 -1.50000 H99C 2 0.570171 0.100511 0.374896 11.00000 -1.50000 AFIX 0 C100 1 0.593416 0.044385 0.249102 11.00000 0.01660 0.02734 = 0.03255 0.00052 -0.00350 -0.00077 PART 1 C101 1 0.271470 0.500000 0.266022 10.38000 0.04011 AFIX 43 H101 2 0.234576 0.500000 0.252618 10.38000 -1.20000 AFIX 0 C102 1 0.306657 0.500000 0.216934 10.38000 0.03660 AFIX 43 H102 2 0.293933 0.500000 0.170169 10.38000 -1.20000 AFIX 0 C103 1 0.360071 0.500000 0.235066 10.38000 0.03605 AFIX 43 H103 2 0.384519 0.500000 0.201202 10.38000 -1.20000 AFIX 0 C104 1 0.378661 0.500000 0.306591 10.38000 0.04953 AFIX 43 H104 2 0.415589 0.500000 0.319779 10.38000 -1.20000 AFIX 0 C105 1 0.342497 0.500000 0.356639 10.38000 0.04720 AFIX 43 H105 2 0.354067 0.500000 0.403780 10.38000 -1.20000 AFIX 0 C106 1 0.288373 0.500000 0.333833 10.38000 0.04037 AFIX 43 H106 2 0.262882 0.500000 0.366393 10.38000 -1.20000 PART -2 AFIX 0 C107 1 0.315660 0.520169 0.284828 10.12000 0.05326 AFIX 13 H107 2 0.316666 0.583770 0.271816 10.12000 -1.20000 AFIX 0 CL1 4 0.251765 0.510561 0.297465 10.12000 0.03819 CL2 4 0.331318 0.470895 0.206529 10.12000 0.05198 CL3 4 0.359715 0.520270 0.349478 10.12000 0.05389 PART -3 C108 1 0.001788 0.094858 0.487810 10.18000 0.03876 AFIX 13 H108 2 0.002301 0.029007 0.486949 10.18000 -1.20000 AFIX 0 CL4 4 0.053749 0.125376 0.537651 10.18000 0.10420 CL5 4 -0.062479 0.126562 0.515550 10.18000 0.06782 CL6 4 -0.003315 0.128870 0.403568 10.18000 0.06479 PART -4 AFIX 66 C109 1 0.032327 0.125481 0.571827 10.32000 0.03032 AFIX 43 H109 2 0.050570 0.118458 0.615654 10.32000 -1.20000 AFIX 65 C110 1 0.060129 0.123246 0.514135 10.32000 0.03252 AFIX 43 H110 2 0.097373 0.114696 0.518531 10.32000 -1.20000 AFIX 65 C111 1 0.033437 0.133522 0.450010 10.32000 0.06185 AFIX 43 H111 2 0.052438 0.131994 0.410580 10.32000 -1.20000 AFIX 65 C112 1 -0.021057 0.146032 0.443577 10.32000 0.09295 AFIX 43 H112 2 -0.039299 0.153054 0.399750 10.32000 -1.20000 AFIX 65 C113 1 -0.048859 0.148266 0.501268 10.32000 0.10878 AFIX 43 H113 2 -0.086102 0.156816 0.496871 10.32000 -1.20000 AFIX 65 C114 1 -0.022167 0.137991 0.565394 10.32000 0.05953 AFIX 43 H114 2 -0.041169 0.139518 0.604823 10.32000 -1.20000 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0654 for 7175 Fo > 4sig(Fo) and 0.0778 for all 8660 data REM 1025 parameters refined using 946 restraints END WGHT 0.0932 38.2102 REM Highest difference peak 1.091, deepest hole -0.793, 1-sigma level 0.092 Q1 1 0.2833 -0.0797 0.5097 11.00000 0.05 1.09 Q2 1 0.3585 -0.1524 0.1696 11.00000 0.05 1.02 Q3 1 0.3121 0.0292 0.2191 11.00000 0.05 0.98 Q4 1 0.0794 0.1071 0.5014 11.00000 0.05 0.91 Q5 1 0.1696 -0.0753 0.4170 11.00000 0.05 0.83 Q6 1 0.3210 -0.2662 0.2615 11.00000 0.05 0.81 Q7 1 0.0472 0.1547 0.4657 11.00000 0.05 0.74 Q8 1 0.0092 0.1671 0.4200 11.00000 0.05 0.68 Q9 1 0.2987 0.0000 0.5253 10.50000 0.05 0.68 Q10 1 0.2816 -0.0700 0.1054 11.00000 0.05 0.65 Q11 1 0.3681 0.5000 0.3270 10.50000 0.05 0.63 Q12 1 0.3220 -0.1520 0.4857 11.00000 0.05 0.61 Q13 1 0.4109 -0.0743 0.4597 11.00000 0.05 0.61 Q14 1 0.1906 0.0000 0.1272 10.50000 0.05 0.57 Q15 1 0.3109 0.5000 0.3457 10.50000 0.05 0.57 Q16 1 0.4086 -0.1980 0.3556 11.00000 0.05 0.56 Q17 1 0.0084 0.1068 0.3869 11.00000 0.05 0.55 Q18 1 0.3672 -0.0335 0.1382 11.00000 0.05 0.54 Q19 1 0.1819 -0.0684 0.1417 11.00000 0.05 0.53 Q20 1 0.0374 0.1413 0.5480 11.00000 0.05 0.53 Q21 1 0.3083 -0.1753 0.1662 11.00000 0.05 0.52 Q22 1 -0.0210 0.1129 0.4064 11.00000 0.05 0.50 Q23 1 0.3874 0.5000 0.2865 10.50000 0.05 0.47 Q24 1 0.3869 -0.2306 0.3610 11.00000 0.05 0.47 Q25 1 0.2672 0.5000 0.3248 10.50000 0.05 0.45 ; _cod_data_source_file ic300186y_si_002.cif _cod_data_source_block k1 _cod_original_sg_symbol_H-M 'C 2/m' _cod_original_formula_sum 'C127 H53 Cl1.80 Gd N4 Ni' _cod_database_code 4329104 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2971(4) -0.2185(8) 0.1818(5) 0.056(3) Uani 0.50 1 d PDU A -1 C2 C 0.3497(4) -0.2323(8) 0.2145(5) 0.062(3) Uani 0.50 1 d PDU A -1 C3 C 0.3913(4) -0.1714(8) 0.2002(6) 0.058(2) Uani 0.50 1 d PDU A -1 C4 C 0.3746(4) -0.1000(8) 0.1528(7) 0.066(3) Uani 0.50 1 d PDU A -1 C5 C 0.3231(4) -0.0861(10) 0.1190(9) 0.064(3) Uani 0.50 1 d PDU A -1 C6 C 0.2819(6) -0.1482(10) 0.1310(7) 0.058(3) Uani 0.50 1 d PDU A -1 C7 C 0.2256(6) -0.1270(8) 0.1386(8) 0.066(3) Uani 0.50 1 d PDU A -1 C8 C 0.2075(5) -0.1829(9) 0.1897(8) 0.068(3) Uani 0.50 1 d PDU A -1 C9 C 0.2489(5) -0.2373(8) 0.2183(6) 0.062(3) Uani 0.50 1 d PDU A -1 C10 C 0.2508(4) -0.2606(6) 0.2895(5) 0.060(2) Uani 0.50 1 d PDU A -1 C11 C 0.3025(4) -0.2734(8) 0.3195(5) 0.048(2) Uani 0.50 1 d PDU A -1 C12 C 0.3513(3) -0.2585(5) 0.2800(4) 0.0412(17) Uani 0.50 1 d PDU A -1 C13 C 0.3930(3) -0.2256(5) 0.3356(4) 0.0424(18) Uani 0.50 1 d PDU A -1 C14 C 0.4313(8) -0.1627(12) 0.3235(6) 0.055(3) Uani 0.50 1 d PDU A -1 C15 C 0.4302(5) -0.1332(7) 0.2533(6) 0.059(3) Uani 0.50 1 d PDU A -1 C16 C 0.4378(3) -0.0453(6) 0.2340(5) 0.054(2) Uani 0.50 1 d PDU A -1 C17 C 0.4061(3) -0.0198(6) 0.1753(4) 0.051(3) Uani 0.50 1 d PDU A -1 C18 C 0.3877(5) 0.0688(7) 0.1635(6) 0.067(3) Uani 0.50 1 d PDU A -1 C19 C 0.3399(4) 0.0787(10) 0.1254(8) 0.059(3) Uani 0.50 1 d PDU A -1 C20 C 0.3087(3) -0.0039(11) 0.1042(3) 0.066(2) Uani 0.50 1 d PDU A -1 C21 C 0.2516(4) 0.0266(5) 0.1052(4) 0.057(2) Uani 0.50 1 d PDU A -1 C22 C 0.2140(4) -0.0353(6) 0.1213(5) 0.068(3) Uani 0.50 1 d PDU A -1 C23 C 0.1722(3) -0.0085(10) 0.1574(5) 0.073(2) Uani 0.50 1 d PDU A -1 C24 C 0.1493(5) -0.0619(7) 0.2098(7) 0.068(3) Uani 0.50 1 d PDU A -1 C25 C 0.1673(4) -0.1465(7) 0.2307(6) 0.067(2) Uani 0.50 1 d PDU A -1 C26 C 0.1686(6) -0.1718(10) 0.2995(7) 0.075(3) Uani 0.50 1 d PDU A -1 C27 C 0.2115(5) -0.2286(11) 0.3284(7) 0.071(3) Uani 0.50 1 d PDU A -1 C28 C 0.2254(5) -0.2072(8) 0.3995(7) 0.078(3) Uani 0.50 1 d PDU A -1 C29 C 0.2782(5) -0.2130(7) 0.4305(6) 0.069(3) Uani 0.50 1 d PDU A -1 C30 C 0.3168(5) -0.2480(7) 0.3891(5) 0.053(2) Uani 0.50 1 d PDU A -1 C31 C 0.3710(5) -0.2191(9) 0.3987(5) 0.047(2) Uani 0.50 1 d PDU A -1 C32 C 0.3819(5) -0.1530(7) 0.4491(5) 0.055(3) Uani 0.50 1 d PDU A -1 C33 C 0.4233(4) -0.0942(6) 0.4375(5) 0.064(2) Uani 0.50 1 d PDU A -1 C34 C 0.4455(4) -0.0989(7) 0.3721(6) 0.057(2) Uani 0.50 1 d PDU A -1 C35 C 0.4597(3) -0.0107(9) 0.3533(5) 0.063(2) Uani 0.50 1 d PDU A -1 C36 C 0.4546(3) 0.0194(7) 0.2864(5) 0.058(2) Uani 0.50 1 d PDU A -1 C37 C 0.4388(6) 0.1057(8) 0.2735(7) 0.065(3) Uani 0.50 1 d PDU A -1 C38 C 0.4057(5) 0.1310(9) 0.2129(6) 0.068(3) Uani 0.50 1 d PDU A -1 C39 C 0.3712(5) 0.2045(9) 0.2224(7) 0.076(3) Uani 0.50 1 d PDU A -1 C40 C 0.3186(5) 0.2100(9) 0.1899(7) 0.069(3) Uani 0.50 1 d PDU A -1 C41 C 0.3025(5) 0.1473(9) 0.1397(7) 0.060(3) Uani 0.50 1 d PDU A -1 C42 C 0.2497(6) 0.1171(6) 0.1280(5) 0.047(2) Uani 0.50 1 d PDU A -1 C43 C 0.2098(4) 0.1497(7) 0.1682(6) 0.051(2) Uani 0.50 1 d PDU A -1 C44 C 0.1702(3) 0.0846(6) 0.1760(5) 0.056(2) Uani 0.50 1 d PDU A -1 C45 C 0.1454(4) 0.0866(8) 0.2389(6) 0.060(2) Uani 0.50 1 d PDU A -1 C46 C 0.1330(3) -0.0059(11) 0.2617(5) 0.068(2) Uani 0.50 1 d PDU A -1 C47 C 0.1355(4) -0.0305(7) 0.3283(5) 0.081(3) Uani 0.50 1 d PDU A -1 C48 C 0.1499(7) -0.1124(10) 0.3473(8) 0.086(3) Uani 0.50 1 d PDU A -1 C49 C 0.1870(6) -0.1408(8) 0.4072(7) 0.090(3) Uani 0.50 1 d PDU A -1 C50 C 0.1972(6) -0.0815(9) 0.4556(7) 0.100(3) Uani 0.50 1 d PDU A -1 C51 C 0.2485(5) -0.0882(7) 0.4931(5) 0.076(3) Uani 0.50 1 d PDU A -1 C52 C 0.2905(6) -0.1476(8) 0.4808(7) 0.084(3) Uani 0.50 1 d PDU A -1 C53 C 0.3449(6) -0.1198(8) 0.4915(7) 0.072(3) Uani 0.50 1 d PDU A -1 C54 C 0.3482(5) -0.0302(6) 0.5153(5) 0.076(3) Uani 0.50 1 d PDU A -1 C55 C 0.3895(5) 0.0235(7) 0.4958(5) 0.075(3) Uani 0.50 1 d PDU A -1 C56 C 0.4268(4) -0.0072(10) 0.4600(5) 0.083(3) Uani 0.50 1 d PDU A -1 C57 C 0.4485(4) 0.0485(7) 0.4055(6) 0.067(2) Uani 0.50 1 d PDU A -1 C58 C 0.4332(5) 0.1321(7) 0.3919(6) 0.079(3) Uani 0.50 1 d PDU A -1 C59 C 0.4277(11) 0.1618(15) 0.3280(7) 0.079(4) Uani 0.50 1 d PDU A -1 C60 C 0.3878(5) 0.2225(9) 0.2911(7) 0.089(3) Uani 0.50 1 d PDU A -1 C61 C 0.3524(5) 0.2551(9) 0.3292(8) 0.102(3) Uani 0.50 1 d PDU A -1 C62 C 0.3002(5) 0.2683(11) 0.2953(6) 0.082(3) Uani 0.50 1 d PDU A -1 C63 C 0.2797(5) 0.2451(7) 0.2285(6) 0.062(2) Uani 0.50 1 d PDU A -1 C64 C 0.2247(5) 0.2144(7) 0.2187(5) 0.053(2) Uani 0.50 1 d PDU A -1 C65 C 0.1974(4) 0.2152(6) 0.2779(5) 0.060(2) Uani 0.50 1 d PDU A -1 C66 C 0.1575(5) 0.1493(8) 0.2858(6) 0.067(3) Uani 0.50 1 d PDU A -1 C67 C 0.1610(7) 0.1235(9) 0.3604(7) 0.080(3) Uani 0.50 1 d PDU A -1 C68 C 0.1513(5) 0.0396(7) 0.3821(6) 0.089(3) Uani 0.50 1 d PDU A -1 C69 C 0.1774(4) 0.0107(11) 0.4416(5) 0.087(3) Uani 0.50 1 d PDU A -1 C70 C 0.2199(6) 0.0612(8) 0.4758(8) 0.093(3) Uani 0.50 1 d PDU A -1 C71 C 0.2568(4) 0.0058(9) 0.5084(5) 0.109(3) Uani 0.50 1 d PDU A -1 C72 C 0.3059(4) 0.0356(8) 0.5198(5) 0.086(3) Uani 0.50 1 d PDU A -1 C73 C 0.3200(5) 0.1198(8) 0.4984(7) 0.082(3) Uani 0.50 1 d PDU A -1 C74 C 0.3741(5) 0.1186(8) 0.4826(7) 0.079(3) Uani 0.50 1 d PDU A -1 C75 C 0.3923(7) 0.1724(8) 0.4341(7) 0.085(4) Uani 0.50 1 d PDU A -1 C76 C 0.3556(6) 0.2272(14) 0.4019(9) 0.093(4) Uani 0.50 1 d PDU A -1 C77 C 0.3012(6) 0.2365(11) 0.4147(6) 0.087(3) Uani 0.50 1 d PDU A -1 C78 C 0.2708(4) 0.2616(7) 0.3558(6) 0.080(3) Uani 0.50 1 d PDU A -1 C79 C 0.2200(5) 0.2365(9) 0.3469(6) 0.070(3) Uani 0.50 1 d PDU A -1 C80 C 0.1983(5) 0.1830(9) 0.3956(6) 0.079(3) Uani 0.50 1 d PDU A -1 C81 C 0.2278(5) 0.1497(6) 0.4541(4) 0.076(3) Uani 0.50 1 d PDU A -1 C82 C 0.2839(6) 0.1795(7) 0.4650(6) 0.088(3) Uani 0.50 1 d PDU A -1 Gd1 Gd 0.33496(16) -0.0921(3) 0.25662(18) 0.0780(12) Uani 0.21 1 d P B -3 Gd2 Gd 0.33809(12) -0.1058(3) 0.27799(14) 0.0347(5) Uani 0.19 1 d P C -2 Gd3 Gd 0.3579(2) -0.0796(4) 0.2938(2) 0.0533(11) Uani 0.07 1 d P D -4 Gd4 Gd 0.3737(3) -0.0189(6) 0.3189(4) 0.058(2) Uiso 0.03 1 d P E -5 Ni1 Ni 0.48062(2) 0.0000 0.08080(3) 0.01718(16) Uani 1 2 d S . 5 N1 N 0.42325(13) 0.0000 0.00794(19) 0.0189(7) Uani 1 2 d S . 5 N2 N 0.47938(9) 0.12971(18) 0.08216(13) 0.0203(5) Uani 1 1 d . . 5 N3 N 0.53514(14) 0.0000 0.15747(19) 0.0207(7) Uani 1 2 d S . 5 C83 C 0.35504(11) 0.0449(2) -0.07154(16) 0.0218(6) Uani 1 1 d . . 5 C84 C 0.39746(11) 0.0717(2) -0.02266(15) 0.0206(6) Uani 1 1 d . . 5 C85 C 0.40918(11) 0.1584(2) -0.00748(16) 0.0213(6) Uani 1 1 d . . 5 H85 H 0.3898 0.2026 -0.0330 0.026 Uiso 1 1 calc R . 5 C86 C 0.44715(11) 0.1852(2) 0.04224(16) 0.0212(6) Uani 1 1 d . . 5 C87 C 0.45677(12) 0.2765(2) 0.05992(17) 0.0239(6) Uani 1 1 d . . 5 C88 C 0.49554(12) 0.2766(2) 0.11219(17) 0.0244(7) Uani 1 1 d . . 5 C89 C 0.50931(11) 0.1853(2) 0.12515(16) 0.0214(6) Uani 1 1 d . . 5 C90 C 0.54664(11) 0.1585(2) 0.17588(16) 0.0221(6) Uani 1 1 d . . 5 H90 H 0.5661 0.2026 0.2015 0.027 Uiso 1 1 calc R . 5 C91 C 0.55745(11) 0.0717(2) 0.19165(16) 0.0220(6) Uani 1 1 d . . 5 C92 C 0.31668(12) 0.1064(2) -0.10919(17) 0.0266(7) Uani 1 1 d . . 5 H92A H 0.3004 0.0767 -0.1506 0.032 Uiso 1 1 calc R . 5 H92B H 0.3359 0.1589 -0.1237 0.032 Uiso 1 1 calc R . 5 C93 C 0.27304(14) 0.1355(3) -0.0649(2) 0.0391(9) Uani 1 1 d . . 5 H93A H 0.2541 0.0836 -0.0502 0.059 Uiso 1 1 calc R . 5 H93B H 0.2482 0.1744 -0.0914 0.059 Uiso 1 1 calc R . 5 H93C H 0.2889 0.1671 -0.0249 0.059 Uiso 1 1 calc R . 5 C94 C 0.42731(13) 0.3530(2) 0.02683(19) 0.0296(7) Uani 1 1 d . . 5 H94A H 0.4234 0.3437 -0.0231 0.036 Uiso 1 1 calc R . 5 H94B H 0.4484 0.4073 0.0359 0.036 Uiso 1 1 calc R . 5 C95 C 0.37240(15) 0.3661(3) 0.0520(2) 0.0395(9) Uani 1 1 d . . 5 H95A H 0.3517 0.3119 0.0448 0.059 Uiso 1 1 calc R . 5 H95B H 0.3542 0.4145 0.0267 0.059 Uiso 1 1 calc R . 5 H95C H 0.3761 0.3805 0.1006 0.059 Uiso 1 1 calc R . 5 C96 C 0.51890(14) 0.3533(2) 0.1524(2) 0.0322(8) Uani 1 1 d . . 5 H96A H 0.5125 0.4077 0.1253 0.039 Uiso 1 1 calc R . 5 H96B H 0.5577 0.3449 0.1602 0.039 Uiso 1 1 calc R . 5 C97 C 0.49612(16) 0.3649(3) 0.2212(2) 0.0424(10) Uani 1 1 d . . 5 H97A H 0.4580 0.3764 0.2138 0.064 Uiso 1 1 calc R . 5 H97B H 0.5136 0.4147 0.2455 0.064 Uiso 1 1 calc R . 5 H97C H 0.5021 0.3112 0.2482 0.064 Uiso 1 1 calc R . 5 C98 C 0.62133(14) 0.1070(2) 0.29860(19) 0.0326(8) Uani 1 1 d . . 5 H98A H 0.6372 0.1549 0.2730 0.039 Uiso 1 1 calc R . 5 H98B H 0.6505 0.0755 0.3250 0.039 Uiso 1 1 calc R . 5 C99 C 0.58488(15) 0.1474(3) 0.34803(19) 0.0372(9) Uani 1 1 d . . 5 H99A H 0.5560 0.1791 0.3223 0.056 Uiso 1 1 calc R . 5 H99B H 0.6051 0.1884 0.3786 0.056 Uiso 1 1 calc R . 5 H99C H 0.5702 0.1005 0.3749 0.056 Uiso 1 1 calc R . 5 C100 C 0.59342(12) 0.0444(2) 0.24910(17) 0.0258(7) Uani 1 1 d . . 5 C101 C 0.2715(3) 0.5000 0.2660(4) 0.0401(17) Uiso 0.38 2 d SP F 1 H101 H 0.2346 0.5000 0.2526 0.048 Uiso 0.38 2 calc SPR F 1 C102 C 0.3067(3) 0.5000 0.2169(4) 0.0366(16) Uiso 0.38 2 d SP F 1 H102 H 0.2939 0.5000 0.1702 0.044 Uiso 0.38 2 calc SPR F 1 C103 C 0.3601(3) 0.5000 0.2351(4) 0.0360(15) Uiso 0.38 2 d SP F 1 H103 H 0.3845 0.5000 0.2012 0.043 Uiso 0.38 2 calc SPR F 1 C104 C 0.3787(4) 0.5000 0.3066(5) 0.050(2) Uiso 0.38 2 d SP F 1 H104 H 0.4156 0.5000 0.3198 0.059 Uiso 0.38 2 calc SPR F 1 C105 C 0.3425(4) 0.5000 0.3566(5) 0.047(2) Uiso 0.38 2 d SP F 1 H105 H 0.3541 0.5000 0.4038 0.057 Uiso 0.38 2 calc SPR F 1 C106 C 0.2884(3) 0.5000 0.3338(4) 0.0404(17) Uiso 0.38 2 d SP F 1 H106 H 0.2629 0.5000 0.3664 0.048 Uiso 0.38 2 calc SPR F 1 C107 C 0.3157(14) 0.520(3) 0.2848(18) 0.053(10) Uiso 0.12 1 d P G -2 H107 H 0.3167 0.5838 0.2718 0.064 Uiso 0.12 1 calc PR G -2 Cl1 Cl 0.2518(3) 0.5106(8) 0.2975(3) 0.0382(18) Uiso 0.12 1 d P G -2 Cl2 Cl 0.3313(4) 0.4709(6) 0.2065(5) 0.052(2) Uiso 0.12 1 d P G -2 Cl3 Cl 0.3597(4) 0.5203(7) 0.3495(5) 0.054(3) Uiso 0.12 1 d P G -2 C108 C 0.0018(12) 0.0949(13) 0.4878(11) 0.039(5) Uiso 0.18 1 d P H -3 H108 H 0.0023 0.0290 0.4869 0.047 Uiso 0.18 1 calc PR H -3 Cl4 Cl 0.0537(6) 0.1254(10) 0.5377(9) 0.104(4) Uiso 0.18 1 d P H -3 Cl5 Cl -0.0625(4) 0.1266(6) 0.5156(5) 0.068(2) Uiso 0.18 1 d P H -3 Cl6 Cl -0.0033(4) 0.1289(6) 0.4036(4) 0.0648(18) Uiso 0.18 1 d P H -3 C109 C 0.0323(4) 0.1255(7) 0.5718(5) 0.030(2) Uiso 0.32 1 d PG I -4 H109 H 0.0506 0.1185 0.6157 0.036 Uiso 0.32 1 calc PR I -4 C110 C 0.0601(4) 0.1232(8) 0.5141(7) 0.033(3) Uiso 0.32 1 d PG I -4 H110 H 0.0974 0.1147 0.5185 0.039 Uiso 0.32 1 calc PR I -4 C111 C 0.0334(6) 0.1335(11) 0.4500(6) 0.062(5) Uiso 0.32 1 d PG I -4 H111 H 0.0524 0.1320 0.4106 0.074 Uiso 0.32 1 calc PR I -4 C112 C -0.0211(6) 0.1460(11) 0.4436(6) 0.093(7) Uiso 0.32 1 d PG I -4 H112 H -0.0393 0.1531 0.3997 0.112 Uiso 0.32 1 calc PR I -4 C113 C -0.0489(4) 0.1483(11) 0.5013(8) 0.109(11) Uiso 0.32 1 d PG I -4 H113 H -0.0861 0.1568 0.4969 0.131 Uiso 0.32 1 calc PR I -4 C114 C -0.0222(4) 0.1380(10) 0.5654(7) 0.060(5) Uiso 0.32 1 d PG I -4 H114 H -0.0412 0.1395 0.6048 0.071 Uiso 0.32 1 calc PR I -4 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 C1 0.056(5) 0.044(5) 0.062(5) -0.038(4) -0.019(4) 0.008(4) C2 0.063(5) 0.049(5) 0.075(5) -0.017(4) 0.001(5) 0.013(4) C3 0.049(5) 0.050(5) 0.078(5) -0.007(5) 0.030(4) 0.008(4) C4 0.060(5) 0.086(6) 0.054(5) -0.021(5) 0.020(4) 0.012(5) C5 0.092(6) 0.063(6) 0.040(5) -0.010(5) 0.021(5) 0.009(6) C6 0.079(6) 0.052(5) 0.041(4) -0.022(4) -0.002(5) -0.011(5) C7 0.080(6) 0.058(5) 0.054(6) -0.022(5) -0.030(5) -0.004(5) C8 0.056(5) 0.050(6) 0.092(6) -0.031(5) -0.025(5) -0.007(5) C9 0.061(5) 0.035(5) 0.086(6) -0.023(4) -0.022(5) -0.009(5) C10 0.060(5) 0.024(4) 0.093(5) -0.001(4) -0.007(4) -0.016(4) C11 0.062(5) 0.014(4) 0.067(5) 0.012(4) -0.006(4) -0.010(3) C12 0.062(4) 0.016(3) 0.043(4) 0.001(3) -0.006(4) 0.011(3) C13 0.043(4) 0.027(3) 0.053(4) 0.014(3) -0.017(3) 0.014(3) C14 0.033(5) 0.050(5) 0.079(5) 0.010(5) -0.008(4) 0.019(5) C15 0.038(4) 0.064(5) 0.078(6) 0.000(5) 0.019(4) 0.020(4) C16 0.031(3) 0.072(5) 0.062(4) -0.005(4) 0.026(3) 0.009(4) C17 0.046(4) 0.062(7) 0.051(4) -0.005(4) 0.033(3) 0.000(4) C18 0.078(6) 0.073(6) 0.056(5) 0.009(5) 0.044(5) -0.005(5) C19 0.087(6) 0.057(5) 0.040(5) 0.009(5) 0.036(5) -0.011(5) C20 0.114(5) 0.055(4) 0.035(3) 0.000(7) 0.029(3) 0.009(7) C21 0.097(5) 0.053(5) 0.020(3) 0.004(3) -0.004(4) 0.015(4) C22 0.089(5) 0.063(5) 0.045(4) -0.013(4) -0.036(4) 0.004(4) C23 0.053(4) 0.071(5) 0.087(5) -0.001(6) -0.045(4) 0.006(6) C24 0.033(4) 0.069(6) 0.098(6) 0.003(5) -0.023(5) -0.008(4) C25 0.040(4) 0.058(5) 0.099(6) -0.018(5) -0.014(4) -0.017(4) C26 0.058(6) 0.059(6) 0.108(7) 0.011(5) 0.011(5) -0.032(5) C27 0.076(6) 0.043(5) 0.095(6) 0.017(6) 0.013(5) -0.033(5) C28 0.097(6) 0.054(5) 0.090(6) 0.020(5) 0.048(5) -0.019(5) C29 0.114(6) 0.038(5) 0.061(5) 0.019(4) 0.036(5) -0.017(5) C30 0.075(5) 0.023(4) 0.061(5) 0.017(4) 0.000(4) -0.013(4) C31 0.063(5) 0.027(4) 0.044(4) 0.010(4) -0.031(4) 0.002(4) C32 0.094(6) 0.031(4) 0.034(4) 0.012(4) -0.034(4) -0.003(5) C33 0.067(5) 0.051(4) 0.065(5) 0.026(4) -0.047(4) -0.005(4) C34 0.028(4) 0.053(5) 0.084(5) 0.011(5) -0.028(4) 0.009(4) C35 0.025(3) 0.085(6) 0.076(4) -0.006(6) -0.011(3) 0.006(5) C36 0.026(3) 0.084(7) 0.067(4) -0.004(4) 0.014(3) -0.002(4) C37 0.046(5) 0.075(6) 0.077(6) 0.001(5) 0.015(5) -0.023(5) C38 0.067(6) 0.074(6) 0.068(5) 0.012(5) 0.026(5) -0.025(5) C39 0.075(6) 0.058(6) 0.100(6) 0.014(5) 0.028(5) -0.026(5) C40 0.071(6) 0.048(5) 0.089(6) 0.020(5) 0.009(5) -0.012(5) C41 0.077(6) 0.049(5) 0.058(6) 0.022(5) 0.022(5) 0.002(5) C42 0.070(6) 0.041(4) 0.029(4) 0.016(3) -0.001(4) 0.003(4) C43 0.053(4) 0.042(5) 0.054(5) 0.005(4) -0.012(4) 0.019(4) C44 0.032(4) 0.049(4) 0.081(5) 0.013(4) -0.034(4) 0.013(3) C45 0.021(3) 0.059(5) 0.097(6) 0.007(5) -0.011(4) 0.018(4) C46 0.024(3) 0.072(5) 0.108(5) 0.004(7) 0.005(3) 0.009(6) C47 0.051(4) 0.097(6) 0.099(6) 0.002(5) 0.039(5) 0.007(4) C48 0.066(6) 0.091(6) 0.106(7) 0.010(6) 0.038(5) -0.022(5) C49 0.105(6) 0.079(6) 0.092(6) 0.020(5) 0.052(5) -0.014(6) C50 0.133(7) 0.092(6) 0.083(6) 0.016(5) 0.052(6) 0.004(6) C51 0.143(7) 0.059(5) 0.034(4) 0.024(4) 0.045(5) 0.003(5) C52 0.147(7) 0.061(6) 0.048(5) 0.021(5) 0.026(5) -0.020(6) C53 0.121(7) 0.066(5) 0.029(4) 0.012(4) -0.003(6) 0.002(6) C54 0.106(6) 0.089(6) 0.030(4) 0.004(4) -0.021(5) -0.016(5) C55 0.093(6) 0.079(6) 0.047(4) 0.008(4) -0.040(4) -0.014(5) C56 0.088(5) 0.082(5) 0.071(5) 0.009(6) -0.044(4) -0.010(6) C57 0.046(4) 0.075(5) 0.074(5) -0.011(5) -0.028(4) -0.015(4) C58 0.072(6) 0.074(6) 0.087(6) -0.021(6) -0.016(5) -0.028(5) C59 0.065(6) 0.072(6) 0.098(7) -0.002(6) -0.003(6) -0.042(6) C60 0.082(6) 0.058(5) 0.128(7) -0.007(6) 0.020(6) -0.036(5) C61 0.106(7) 0.058(5) 0.140(7) -0.016(6) -0.004(6) -0.022(6) C62 0.090(6) 0.027(5) 0.121(7) -0.013(6) -0.030(6) 0.001(5) C63 0.075(6) 0.025(4) 0.084(6) -0.001(4) -0.003(5) 0.007(4) C64 0.063(5) 0.029(4) 0.065(5) 0.001(4) -0.008(5) 0.021(4) C65 0.060(5) 0.042(4) 0.075(5) -0.003(4) -0.007(4) 0.036(4) C66 0.042(5) 0.067(6) 0.090(6) -0.009(5) 0.001(5) 0.039(4) C67 0.070(6) 0.087(6) 0.085(6) -0.014(6) 0.025(5) 0.036(5) C68 0.083(6) 0.098(6) 0.091(6) 0.009(5) 0.045(5) 0.026(5) C69 0.108(6) 0.090(7) 0.069(5) -0.003(6) 0.048(4) 0.025(6) C70 0.113(7) 0.105(7) 0.063(6) 0.003(6) 0.021(5) 0.046(6) C71 0.148(7) 0.119(6) 0.061(4) -0.001(7) 0.018(5) 0.011(7) C72 0.107(6) 0.120(7) 0.028(4) -0.025(4) -0.012(5) -0.016(5) C73 0.091(6) 0.101(6) 0.047(5) -0.045(5) -0.028(5) 0.019(6) C74 0.093(6) 0.078(6) 0.059(6) -0.021(5) -0.032(5) -0.019(6) C75 0.096(6) 0.070(6) 0.085(7) -0.032(6) -0.016(6) -0.022(6) C76 0.109(7) 0.059(6) 0.105(7) -0.030(6) -0.026(7) -0.012(6) C77 0.109(7) 0.055(6) 0.093(7) -0.040(6) -0.012(6) 0.017(6) C78 0.100(6) 0.037(4) 0.098(6) -0.025(5) -0.014(5) 0.025(5) C79 0.087(6) 0.042(5) 0.078(6) -0.025(5) -0.018(5) 0.046(5) C80 0.090(6) 0.069(6) 0.079(6) -0.026(5) 0.002(5) 0.051(5) C81 0.097(6) 0.078(6) 0.053(5) -0.024(4) 0.006(5) 0.053(5) C82 0.115(6) 0.081(7) 0.066(6) -0.040(5) -0.001(6) 0.031(6) Gd1 0.067(2) 0.0641(19) 0.112(3) -0.0507(18) 0.060(2) -0.0224(13) Gd2 0.0193(7) 0.0358(10) 0.0486(13) -0.0215(8) 0.0001(9) 0.0118(8) Gd3 0.040(2) 0.068(3) 0.050(2) -0.022(2) -0.0071(19) 0.026(2) Ni1 0.0127(3) 0.0159(3) 0.0226(3) 0.000 0.00018(19) 0.000 N1 0.0137(16) 0.0179(18) 0.0249(18) 0.000 0.0016(13) 0.000 N2 0.0152(11) 0.0193(13) 0.0262(13) 0.0004(10) 0.0013(9) 0.0002(10) N3 0.0149(16) 0.0196(18) 0.0275(19) 0.000 0.0011(14) 0.000 C83 0.0134(13) 0.0265(16) 0.0255(15) -0.0002(13) 0.0026(11) 0.0008(12) C84 0.0136(13) 0.0237(16) 0.0246(15) 0.0003(12) 0.0024(11) 0.0025(11) C85 0.0165(13) 0.0209(15) 0.0264(15) 0.0019(12) 0.0018(11) 0.0038(11) C86 0.0163(13) 0.0197(15) 0.0280(15) 0.0012(12) 0.0035(11) 0.0020(11) C87 0.0187(14) 0.0202(15) 0.0333(17) 0.0002(13) 0.0044(12) -0.0001(12) C88 0.0193(14) 0.0186(15) 0.0353(17) -0.0004(13) 0.0018(12) -0.0010(12) C89 0.0163(13) 0.0195(15) 0.0286(15) -0.0016(12) 0.0027(11) -0.0015(11) C90 0.0149(13) 0.0215(15) 0.0295(16) -0.0020(13) 0.0001(11) -0.0039(11) C91 0.0147(13) 0.0233(16) 0.0276(15) -0.0003(13) 0.0003(11) -0.0022(11) C92 0.0180(14) 0.0302(18) 0.0310(16) 0.0022(14) -0.0016(12) 0.0030(13) C93 0.0236(16) 0.043(2) 0.051(2) 0.0105(19) 0.0071(15) 0.0136(16) C94 0.0235(16) 0.0193(16) 0.045(2) 0.0016(14) -0.0016(14) 0.0017(13) C95 0.0297(18) 0.0290(19) 0.060(3) -0.0009(18) 0.0038(17) 0.0112(15) C96 0.0276(17) 0.0207(17) 0.047(2) -0.0025(15) -0.0054(15) -0.0017(13) C97 0.040(2) 0.031(2) 0.055(2) -0.0168(18) -0.0013(18) 0.0005(17) C98 0.0240(16) 0.0298(18) 0.041(2) -0.0025(15) -0.0120(14) -0.0031(14) C99 0.0380(19) 0.036(2) 0.0349(19) -0.0054(16) -0.0108(15) -0.0048(16) C100 0.0166(14) 0.0273(17) 0.0325(17) 0.0005(14) -0.0035(12) -0.0008(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 C2 C1 C6 125.3(10) . . C2 C1 C9 121.2(10) . . C6 C1 C9 106.5(9) . . C12 C2 C1 114.7(8) . . C12 C2 C3 114.4(7) . . C1 C2 C3 118.7(10) . . C2 C3 C4 114.9(9) . . C2 C3 C15 124.1(9) . . C4 C3 C15 107.2(9) . . C5 C4 C3 127.3(11) . . C5 C4 C17 117.3(10) . . C3 C4 C17 107.0(8) . . C20 C5 C4 117.7(8) . . C20 C5 C6 117.5(9) . . C4 C5 C6 118.2(12) . . C5 C6 C7 126.3(12) . . C5 C6 C1 115.4(11) . . C7 C6 C1 106.4(9) . . C8 C7 C22 131.6(14) . . C8 C7 C6 108.3(10) . . C22 C7 C6 111.1(14) . . C9 C8 C7 111.0(12) . . C9 C8 C25 121.9(13) . . C7 C8 C25 116.7(13) . . C8 C9 C10 119.6(12) . . C8 C9 C1 107.7(10) . . C10 C9 C1 123.6(10) . . C27 C10 C11 120.1(11) . . C27 C10 C9 118.8(10) . . C11 C10 C9 113.3(9) . . C10 C11 C30 120.8(10) . . C10 C11 C12 122.0(8) . . C30 C11 C12 107.3(7) . . C2 C12 C11 124.9(7) . . C2 C12 C13 123.2(7) . . C11 C12 C13 102.7(7) . . C14 C13 C31 115.9(10) . . C14 C13 C12 123.0(9) . . C31 C13 C12 110.5(7) . . C34 C14 C13 120.2(12) . . C34 C14 C15 115.1(12) . . C13 C14 C15 114.7(10) . . C16 C15 C14 123.9(12) . . C16 C15 C3 106.1(9) . . C14 C15 C3 120.3(10) . . C15 C16 C17 113.7(10) . . C15 C16 C36 119.1(9) . . C17 C16 C36 120.5(8) . . C16 C17 C18 123.1(9) . . C16 C17 C4 105.8(8) . . C18 C17 C4 123.6(9) . . C19 C18 C38 121.5(11) . . C19 C18 C17 116.7(11) . . C38 C18 C17 115.8(10) . . C18 C19 C41 122.0(12) . . C18 C19 C20 118.1(11) . . C41 C19 C20 108.2(9) . . C5 C20 C19 126.1(7) . . C5 C20 C21 121.8(9) . . C19 C20 C21 102.6(9) . . C22 C21 C42 121.8(9) . . C22 C21 C20 117.9(9) . . C42 C21 C20 110.5(9) . . C23 C22 C21 119.1(10) . . C23 C22 C7 108.0(12) . . C21 C22 C7 124.6(11) . . C22 C23 C44 117.3(10) . . C22 C23 C24 124.3(12) . . C44 C23 C24 109.3(10) . . C25 C24 C46 116.1(13) . . C25 C24 C23 124.6(12) . . C46 C24 C23 109.5(10) . . C26 C25 C24 120.6(13) . . C26 C25 C8 118.1(11) . . C24 C25 C8 113.9(11) . . C25 C26 C48 119.1(13) . . C25 C26 C27 119.3(12) . . C48 C26 C27 113.5(12) . . C10 C27 C28 118.9(12) . . C10 C27 C26 122.3(12) . . C28 C27 C26 110.6(11) . . C49 C28 C29 128.7(13) . . C49 C28 C27 98.8(11) . . C29 C28 C27 122.6(11) . . C52 C29 C28 113.4(12) . . C52 C29 C30 122.7(11) . . C28 C29 C30 116.2(10) . . C29 C30 C11 121.1(10) . . C29 C30 C31 120.2(9) . . C11 C30 C31 111.4(8) . . C13 C31 C32 126.7(10) . . C13 C31 C30 108.0(7) . . C32 C31 C30 115.7(10) . . C53 C32 C33 114.4(10) . . C53 C32 C31 124.7(10) . . C33 C32 C31 115.9(11) . . C56 C33 C32 125.2(11) . . C56 C33 C34 108.1(9) . . C32 C33 C34 117.6(10) . . C14 C34 C35 121.8(11) . . C14 C34 C33 123.3(11) . . C35 C34 C33 107.8(9) . . C36 C35 C57 118.2(12) . . C36 C35 C34 123.0(10) . . C57 C35 C34 109.5(10) . . C37 C36 C35 119.1(11) . . C37 C36 C16 116.4(9) . . C35 C36 C16 116.4(9) . . C36 C37 C59 120.1(12) . . C36 C37 C38 122.6(11) . . C59 C37 C38 109.1(12) . . C18 C38 C39 116.5(11) . . C18 C38 C37 121.5(12) . . C39 C38 C37 114.4(11) . . C60 C39 C40 127.5(13) . . C60 C39 C38 98.1(11) . . C40 C39 C38 122.7(12) . . C63 C40 C41 117.7(11) . . C63 C40 C39 116.7(12) . . C41 C40 C39 118.5(11) . . C40 C41 C42 123.0(11) . . C40 C41 C19 117.9(12) . . C42 C41 C19 111.1(9) . . C41 C42 C43 120.2(10) . . C41 C42 C21 107.6(9) . . C43 C42 C21 123.1(11) . . C64 C43 C42 118.0(10) . . C64 C43 C44 123.2(11) . . C42 C43 C44 111.1(11) . . C43 C44 C45 116.3(10) . . C43 C44 C23 126.9(9) . . C45 C44 C23 105.4(8) . . C66 C45 C44 121.2(11) . . C66 C45 C46 119.5(11) . . C44 C45 C46 110.7(9) . . C47 C46 C24 122.7(14) . . C47 C46 C45 123.1(12) . . C24 C46 C45 105.1(10) . . C48 C47 C46 120.8(14) . . C48 C47 C68 113.7(10) . . C46 C47 C68 117.7(10) . . C47 C48 C26 120.4(14) . . C47 C48 C49 128.4(14) . . C26 C48 C49 96.6(12) . . C50 C49 C28 118.0(14) . . C50 C49 C48 116.1(11) . . C28 C49 C48 120.5(13) . . C49 C50 C51 115.7(13) . . C49 C50 C69 117.4(11) . . C51 C50 C69 115.5(11) . . C52 C51 C50 127.4(12) . . C52 C51 C71 123.3(11) . . C50 C51 C71 98.3(9) . . C29 C52 C51 116.0(12) . . C29 C52 C53 117.1(10) . . C51 C52 C53 120.6(10) . . C32 C53 C54 120.8(12) . . C32 C53 C52 119.3(10) . . C54 C53 C52 110.6(10) . . C55 C54 C53 118.8(10) . . C55 C54 C72 100.8(8) . . C53 C54 C72 129.7(10) . . C56 C55 C54 122.0(11) . . C56 C55 C74 115.7(11) . . C54 C55 C74 114.3(10) . . C55 C56 C33 118.6(11) . . C55 C56 C57 120.6(12) . . C33 C56 C57 108.7(10) . . C58 C57 C35 121.8(13) . . C58 C57 C56 123.5(12) . . C35 C57 C56 105.8(10) . . C59 C58 C57 120.7(16) . . C59 C58 C75 111.3(12) . . C57 C58 C75 118.1(11) . . C58 C59 C37 120.1(15) . . C58 C59 C60 132.2(16) . . C37 C59 C60 99.8(13) . . C61 C60 C39 117.3(14) . . C61 C60 C59 114.6(13) . . C39 C60 C59 118.5(13) . . C60 C61 C62 115.6(14) . . C60 C61 C76 117.4(13) . . C62 C61 C76 117.0(12) . . C63 C62 C61 130.0(13) . . C63 C62 C78 124.7(11) . . C61 C62 C78 97.2(9) . . C40 C63 C62 112.4(11) . . C40 C63 C64 120.8(9) . . C62 C63 C64 117.9(10) . . C65 C64 C43 117.7(11) . . C65 C64 C63 114.7(10) . . C43 C64 C63 120.2(9) . . C64 C65 C66 119.0(10) . . C64 C65 C79 126.2(10) . . C66 C65 C79 105.9(9) . . C45 C66 C65 122.5(11) . . C45 C66 C67 118.4(11) . . C65 C66 C67 107.6(10) . . C68 C67 C80 123.9(14) . . C68 C67 C66 123.1(12) . . C80 C67 C66 106.6(10) . . C69 C68 C67 118.7(16) . . C69 C68 C47 116.7(10) . . C67 C68 C47 118.1(9) . . C68 C69 C70 121.1(14) . . C68 C69 C50 125.7(12) . . C70 C69 C50 100.7(10) . . C71 C70 C81 127.4(13) . . C71 C70 C69 110.1(10) . . C81 C70 C69 118.7(13) . . C72 C71 C70 117.5(11) . . C72 C71 C51 118.8(10) . . C70 C71 C51 114.7(9) . . C71 C72 C73 121.4(10) . . C71 C72 C54 115.9(10) . . C73 C72 C54 113.2(8) . . C72 C73 C82 123.6(12) . . C72 C73 C74 109.2(9) . . C82 C73 C74 120.0(14) . . C75 C74 C73 122.2(14) . . C75 C74 C55 126.4(13) . . C73 C74 C55 102.3(10) . . C76 C75 C74 115.5(17) . . C76 C75 C58 117.5(12) . . C74 C75 C58 115.6(11) . . C75 C76 C77 127.4(17) . . C75 C76 C61 126.8(15) . . C77 C76 C61 99.8(11) . . C78 C77 C82 124.8(13) . . C78 C77 C76 110.6(10) . . C82 C77 C76 115.2(14) . . C79 C78 C77 119.2(10) . . C79 C78 C62 117.7(10) . . C77 C78 C62 114.5(8) . . C78 C79 C80 120.2(10) . . C78 C79 C65 118.6(11) . . C80 C79 C65 111.2(8) . . C79 C80 C81 123.6(12) . . C79 C80 C67 108.2(9) . . C81 C80 C67 116.6(13) . . C80 C81 C70 120.1(13) . . C80 C81 C82 116.1(10) . . C70 C81 C82 113.6(10) . . C73 C82 C77 119.6(16) . . C73 C82 C81 116.4(11) . . C77 C82 C81 115.8(10) . . N1 Ni1 N3 176.82(15) . . N1 Ni1 N2 89.90(7) . 6 N3 Ni1 N2 90.03(7) . 6 N1 Ni1 N2 89.90(7) . . N3 Ni1 N2 90.03(7) . . N2 Ni1 N2 177.50(15) 6 . C84 N1 C84 104.0(3) 6 . C84 N1 Ni1 127.98(17) 6 . C84 N1 Ni1 127.98(17) . . C86 N2 C89 104.2(3) . . C86 N2 Ni1 127.9(2) . . C89 N2 Ni1 127.8(2) . . C91 N3 C91 104.6(4) . 6 C91 N3 Ni1 127.66(18) . . C91 N3 Ni1 127.66(18) 6 . C83 C83 C84 106.40(18) 6 . C83 C83 C92 128.55(18) 6 . C84 C83 C92 124.9(3) . . C85 C84 N1 125.0(3) . . C85 C84 C83 123.4(3) . . N1 C84 C83 111.6(3) . . C86 C85 C84 124.2(3) . . C86 C85 H85 117.9 . . C84 C85 H85 117.9 . . N2 C86 C85 124.9(3) . . N2 C86 C87 111.7(3) . . C85 C86 C87 123.3(3) . . C88 C87 C86 106.2(3) . . C88 C87 C94 128.9(3) . . C86 C87 C94 124.8(3) . . C87 C88 C89 106.3(3) . . C87 C88 C96 128.8(3) . . C89 C88 C96 124.9(3) . . N2 C89 C90 125.0(3) . . N2 C89 C88 111.5(3) . . C90 C89 C88 123.5(3) . . C91 C90 C89 123.9(3) . . C91 C90 H90 118.1 . . C89 C90 H90 118.1 . . N3 C91 C90 125.6(3) . . N3 C91 C100 111.1(3) . . C90 C91 C100 123.3(3) . . C83 C92 C93 111.6(3) . . C83 C92 H92A 109.3 . . C93 C92 H92A 109.3 . . C83 C92 H92B 109.3 . . C93 C92 H92B 109.3 . . H92A C92 H92B 108.0 . . C87 C94 C95 113.1(3) . . C87 C94 H94A 109.0 . . C95 C94 H94A 109.0 . . C87 C94 H94B 109.0 . . C95 C94 H94B 109.0 . . H94A C94 H94B 107.8 . . C88 C96 C97 113.3(3) . . C88 C96 H96A 108.9 . . C97 C96 H96A 108.9 . . C88 C96 H96B 108.9 . . C97 C96 H96B 108.9 . . H96A C96 H96B 107.7 . . C100 C98 C99 113.1(3) . . C100 C98 H98A 109.0 . . C99 C98 H98A 109.0 . . C100 C98 H98B 109.0 . . C99 C98 H98B 109.0 . . H98A C98 H98B 107.8 . . C100 C100 C91 106.58(19) 6 . C100 C100 C98 129.47(19) 6 . C91 C100 C98 123.9(3) . . C106 C101 C102 121.4(8) . . C106 C101 H101 119.3 . . C102 C101 H101 119.3 . . C103 C102 C101 120.3(7) . . C103 C102 H102 119.8 . . C101 C102 H102 119.8 . . C102 C103 C104 119.0(7) . . C102 C103 H103 120.5 . . C104 C103 H103 120.5 . . C105 C104 C103 120.5(8) . . C105 C104 H104 119.8 . . C103 C104 H104 119.8 . . C104 C105 C106 117.0(9) . . C104 C105 H105 121.5 . . C106 C105 H105 121.5 . . C101 C106 C105 121.8(8) . . C101 C106 H106 119.1 . . C105 C106 H106 119.1 . . Cl3 C107 Cl1 120(2) . . Cl3 C107 Cl2 119(2) . . Cl1 C107 Cl2 113(2) . . Cl3 C107 H107 99.8 . . Cl1 C107 H107 99.8 . . Cl2 C107 H107 99.8 . . Cl4 C108 Cl6 118.6(16) . . Cl4 C108 Cl5 115.9(13) . . Cl6 C108 Cl5 102.4(14) . . Cl4 C108 H108 106.4 . . Cl6 C108 H108 106.4 . . Cl5 C108 H108 106.4 . . C110 C109 C114 120.0 . . C110 C109 H109 120.0 . . C114 C109 H109 120.0 . . C111 C110 C109 120.0 . . C111 C110 H110 120.0 . . C109 C110 H110 120.0 . . C110 C111 C112 120.0 . . C110 C111 H111 120.0 . . C112 C111 H111 120.0 . . C113 C112 C111 120.0 . . C113 C112 H112 120.0 . . C111 C112 H112 120.0 . . C112 C113 C114 120.0 . . C112 C113 H113 120.0 . . C114 C113 H113 120.0 . . C113 C114 C109 120.0 . . C113 C114 H114 120.0 . . C109 C114 H114 120.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.446(10) . C1 C6 1.491(18) . C1 C9 1.502(12) . C2 C12 1.349(11) . C2 C3 1.448(10) . C3 C4 1.469(17) . C3 C15 1.492(12) . C4 C5 1.430(10) . C4 C17 1.503(11) . C5 C20 1.325(12) . C5 C6 1.443(10) . C6 C7 1.485(12) . C7 C8 1.422(11) . C7 C22 1.457(12) . C8 C9 1.414(11) . C8 C25 1.465(18) . C9 C10 1.444(11) . C10 C27 1.396(12) . C10 C11 1.404(10) . C11 C30 1.440(10) . C11 C12 1.534(10) . C12 C13 1.540(9) . C13 C14 1.397(11) . C13 C31 1.411(10) . C14 C34 1.387(12) . C14 C15 1.454(12) . C15 C16 1.404(10) . C16 C17 1.404(10) . C16 C36 1.462(14) . C17 C18 1.436(12) . C18 C19 1.378(11) . C18 C38 1.404(12) . C19 C41 1.452(11) . C19 C20 1.522(10) . C20 C21 1.523(10) . C21 C22 1.396(10) . C21 C42 1.447(10) . C22 C23 1.386(11) . C23 C44 1.462(13) . C23 C24 1.473(13) . C24 C25 1.413(10) . C24 C46 1.419(13) . C25 C26 1.409(11) . C26 C48 1.415(13) . C26 C27 1.466(13) . C27 C28 1.452(13) . C28 C49 1.418(13) . C28 C29 1.427(12) . C29 C52 1.419(12) . C29 C30 1.429(11) . C30 C31 1.440(15) . C31 C32 1.422(10) . C32 C53 1.405(12) . C32 C33 1.412(11) . C33 C56 1.394(13) . C33 C34 1.454(12) . C34 C35 1.443(13) . C35 C36 1.392(10) . C35 C57 1.413(12) . C36 C37 1.386(11) . C37 C59 1.419(13) . C37 C38 1.451(13) . C38 C39 1.441(13) . C39 C60 1.410(13) . C39 C40 1.432(12) . C40 C63 1.403(11) . C40 C41 1.408(12) . C41 C42 1.417(18) . C42 C43 1.427(11) . C43 C64 1.426(11) . C43 C44 1.428(11) . C44 C45 1.437(13) . C45 C66 1.344(13) . C45 C46 1.516(15) . C46 C47 1.362(10) . C47 C48 1.339(12) . C47 C68 1.532(16) . C48 C49 1.508(14) . C49 C50 1.321(13) . C50 C51 1.442(12) . C50 C69 1.504(15) . C51 C52 1.433(12) . C51 C71 1.471(13) . C52 C53 1.441(16) . C53 C54 1.439(11) . C54 C55 1.408(11) . C54 C72 1.473(12) . C55 C56 1.314(12) . C55 C74 1.513(14) . C56 C57 1.509(14) . C57 C58 1.347(11) . C58 C59 1.333(12) . C58 C75 1.516(17) . C59 C60 1.509(15) . C60 C61 1.316(13) . C61 C62 1.446(12) . C61 C76 1.490(15) . C62 C63 1.416(12) . C62 C78 1.464(12) . C63 C64 1.468(15) . C64 C65 1.408(11) . C65 C66 1.442(12) . C65 C79 1.465(11) . C66 C67 1.516(14) . C67 C68 1.373(12) . C67 C80 1.442(14) . C68 C69 1.367(12) . C69 C70 1.442(14) . C70 C71 1.376(13) . C70 C81 1.429(12) . C71 C72 1.326(12) . C72 C73 1.402(13) . C73 C82 1.411(12) . C73 C74 1.433(14) . C74 C75 1.367(13) . C75 C76 1.364(13) . C76 C77 1.431(14) . C77 C78 1.391(13) . C77 C82 1.413(13) . C78 C79 1.341(12) . C79 C80 1.406(13) . C80 C81 1.414(12) . C81 C82 1.49(2) . Ni1 N1 1.954(4) . Ni1 N3 1.958(4) . Ni1 N2 1.970(3) 6 Ni1 N2 1.970(3) . N1 C84 1.381(4) 6 N1 C84 1.381(4) . N2 C86 1.373(4) . N2 C89 1.377(4) . N3 C91 1.375(4) . N3 C91 1.375(4) 6 C83 C83 1.364(7) 6 C83 C84 1.439(4) . C83 C92 1.497(4) . C84 C85 1.377(5) . C85 C86 1.374(4) . C85 H85 0.9500 . C86 C87 1.445(4) . C87 C88 1.361(5) . C87 C94 1.500(5) . C88 C89 1.446(4) . C88 C96 1.501(5) . C89 C90 1.377(4) . C90 C91 1.377(5) . C90 H90 0.9500 . C91 C100 1.452(4) . C92 C93 1.533(5) . C92 H92A 0.9900 . C92 H92B 0.9900 . C93 H93A 0.9800 . C93 H93B 0.9800 . C93 H93C 0.9800 . C94 C95 1.532(5) . C94 H94A 0.9900 . C94 H94B 0.9900 . C95 H95A 0.9800 . C95 H95B 0.9800 . C95 H95C 0.9800 . C96 C97 1.530(6) . C96 H96A 0.9900 . C96 H96B 0.9900 . C97 H97A 0.9800 . C97 H97B 0.9800 . C97 H97C 0.9800 . C98 C100 1.496(5) . C98 C99 1.529(6) . C98 H98A 0.9900 . C98 H98B 0.9900 . C99 H99A 0.9800 . C99 H99B 0.9800 . C99 H99C 0.9800 . C100 C100 1.348(7) 6 C101 C106 1.368(11) . C101 C102 1.373(12) . C101 H101 0.9500 . C102 C103 1.371(11) . C102 H102 0.9500 . C103 C104 1.448(11) . C103 H103 0.9500 . C104 C105 1.405(14) . C104 H104 0.9500 . C105 C106 1.407(13) . C105 H105 0.9500 . C106 H106 0.9500 . C107 Cl3 1.62(4) . C107 Cl1 1.67(4) . C107 Cl2 1.79(4) . C107 H107 1.0000 . C108 Cl4 1.64(3) . C108 Cl6 1.73(2) . C108 Cl5 1.83(3) . C108 H108 1.0000 . C109 C110 1.3900 . C109 C114 1.3900 . C109 H109 0.9500 . C110 C111 1.3900 . C110 H110 0.9500 . C111 C112 1.3900 . C111 H111 0.9500 . C112 C113 1.3900 . C112 H112 0.9500 . C113 C114 1.3900 . C113 H113 0.9500 . C114 H114 0.9500 . 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_4 C6 C1 C2 C12 143.6(11) . . C9 C1 C2 C12 -3.2(15) . . C6 C1 C2 C3 3.2(17) . . C9 C1 C2 C3 -143.6(11) . . C12 C2 C3 C4 -140.3(10) . . C1 C2 C3 C4 0.2(15) . . C12 C2 C3 C15 -5.2(16) . . C1 C2 C3 C15 135.2(11) . . C2 C3 C4 C5 -1.4(18) . . C15 C3 C4 C5 -143.6(14) . . C2 C3 C4 C17 145.5(10) . . C15 C3 C4 C17 3.2(12) . . C3 C4 C5 C20 150.2(13) . . C17 C4 C5 C20 6(2) . . C3 C4 C5 C6 -1(2) . . C17 C4 C5 C6 -144.7(14) . . C20 C5 C6 C7 -10(2) . . C4 C5 C6 C7 141.2(14) . . C20 C5 C6 C1 -147.2(14) . . C4 C5 C6 C1 4(2) . . C2 C1 C6 C5 -5.3(17) . . C9 C1 C6 C5 145.5(12) . . C2 C1 C6 C7 -150.6(11) . . C9 C1 C6 C7 0.2(11) . . C5 C6 C7 C8 -141.9(14) . . C1 C6 C7 C8 -1.5(13) . . C5 C6 C7 C22 9.5(19) . . C1 C6 C7 C22 149.9(10) . . C22 C7 C8 C9 -140.9(13) . . C6 C7 C8 C9 2.4(14) . . C22 C7 C8 C25 4.7(19) . . C6 C7 C8 C25 148.1(10) . . C7 C8 C9 C10 145.7(10) . . C25 C8 C9 C10 2.1(17) . . C7 C8 C9 C1 -2.3(13) . . C25 C8 C9 C1 -145.9(11) . . C2 C1 C9 C8 153.5(11) . . C6 C1 C9 C8 1.2(12) . . C2 C1 C9 C10 7.0(17) . . C6 C1 C9 C10 -145.2(11) . . C8 C9 C10 C27 0.1(16) . . C1 C9 C10 C27 142.8(13) . . C8 C9 C10 C11 -149.3(11) . . C1 C9 C10 C11 -6.6(15) . . C27 C10 C11 C30 -4.5(16) . . C9 C10 C11 C30 144.5(10) . . C27 C10 C11 C12 -145.8(12) . . C9 C10 C11 C12 3.2(14) . . C1 C2 C12 C11 -0.1(15) . . C3 C2 C12 C11 142.0(10) . . C1 C2 C12 C13 -141.2(9) . . C3 C2 C12 C13 0.9(14) . . C10 C11 C12 C2 0.0(16) . . C30 C11 C12 C2 -145.7(10) . . C10 C11 C12 C13 147.5(10) . . C30 C11 C12 C13 1.7(10) . . C2 C12 C13 C14 3.2(17) . . C11 C12 C13 C14 -145.0(14) . . C2 C12 C13 C31 146.2(10) . . C11 C12 C13 C31 -2.0(10) . . C31 C13 C14 C34 0(2) . . C12 C13 C14 C34 141.3(13) . . C31 C13 C14 C15 -143.8(14) . . C12 C13 C14 C15 -3(2) . . C34 C14 C15 C16 -6(2) . . C13 C14 C15 C16 139.8(13) . . C34 C14 C15 C3 -147.3(12) . . C13 C14 C15 C3 -2(2) . . C2 C3 C15 C16 -141.5(11) . . C4 C3 C15 C16 -3.6(12) . . C2 C3 C15 C14 6(2) . . C4 C3 C15 C14 143.8(14) . . C14 C15 C16 C17 -143.2(14) . . C3 C15 C16 C17 2.7(12) . . C14 C15 C16 C36 8.4(18) . . C3 C15 C16 C36 154.3(8) . . C15 C16 C17 C18 149.8(10) . . C36 C16 C17 C18 -1.3(13) . . C15 C16 C17 C4 -0.7(11) . . C36 C16 C17 C4 -151.8(9) . . C5 C4 C17 C16 149.1(12) . . C3 C4 C17 C16 -1.6(11) . . C5 C4 C17 C18 -1.3(16) . . C3 C4 C17 C18 -151.9(11) . . C16 C17 C18 C19 -149.8(10) . . C4 C17 C18 C19 -4.5(15) . . C16 C17 C18 C38 3.6(16) . . C4 C17 C18 C38 148.9(12) . . C38 C18 C19 C41 -8(2) . . C17 C18 C19 C41 143.8(12) . . C38 C18 C19 C20 -146.8(11) . . C17 C18 C19 C20 5.0(18) . . C4 C5 C20 C19 -6.0(16) . . C6 C5 C20 C19 145.2(14) . . C4 C5 C20 C21 -146.3(12) . . C6 C5 C20 C21 4.9(19) . . C18 C19 C20 C5 0.1(13) . . C41 C19 C20 C5 -143.9(15) . . C18 C19 C20 C21 146.3(11) . . C41 C19 C20 C21 2.3(13) . . C5 C20 C21 C22 -1.0(14) . . C19 C20 C21 C22 -149.1(10) . . C5 C20 C21 C42 145.5(12) . . C19 C20 C21 C42 -2.5(10) . . C42 C21 C22 C23 3.2(14) . . C20 C21 C22 C23 145.8(8) . . C42 C21 C22 C7 -141.4(9) . . C20 C21 C22 C7 1.2(14) . . C8 C7 C22 C23 -10.2(17) . . C6 C7 C22 C23 -152.8(10) . . C8 C7 C22 C21 137.6(14) . . C6 C7 C22 C21 -5.0(16) . . C21 C22 C23 C44 0.4(12) . . C7 C22 C23 C44 150.2(8) . . C21 C22 C23 C24 -143.0(11) . . C7 C22 C23 C24 6.8(13) . . C22 C23 C24 C25 1.0(17) . . C44 C23 C24 C25 -144.9(11) . . C22 C23 C24 C46 145.3(10) . . C44 C23 C24 C46 -0.5(10) . . C46 C24 C25 C26 -0.1(16) . . C23 C24 C25 C26 142.2(13) . . C46 C24 C25 C8 -149.4(10) . . C23 C24 C25 C8 -7.1(16) . . C9 C8 C25 C26 -4.1(17) . . C7 C8 C25 C26 -145.8(12) . . C9 C8 C25 C24 146.1(12) . . C7 C8 C25 C24 4.4(15) . . C24 C25 C26 C48 2(2) . . C8 C25 C26 C48 150.1(14) . . C24 C25 C26 C27 -144.3(14) . . C8 C25 C26 C27 3.7(19) . . C11 C10 C27 C28 1.3(19) . . C9 C10 C27 C28 -146.0(12) . . C11 C10 C27 C26 146.9(14) . . C9 C10 C27 C26 0(2) . . C25 C26 C27 C10 -2(2) . . C48 C26 C27 C10 -149.8(15) . . C25 C26 C27 C28 146.5(13) . . C48 C26 C27 C28 -2(2) . . C10 C27 C28 C49 151.6(13) . . C26 C27 C28 C49 2.3(16) . . C10 C27 C28 C29 4(2) . . C26 C27 C28 C29 -145.8(13) . . C49 C28 C29 C52 7.5(18) . . C27 C28 C29 C52 145.5(13) . . C49 C28 C29 C30 -142.9(13) . . C27 C28 C29 C30 -4.9(18) . . C52 C29 C30 C11 -145.7(12) . . C28 C29 C30 C11 1.6(15) . . C52 C29 C30 C31 1.9(16) . . C28 C29 C30 C31 149.2(11) . . C10 C11 C30 C29 3.0(16) . . C12 C11 C30 C29 149.3(9) . . C10 C11 C30 C31 -147.2(10) . . C12 C11 C30 C31 -1.0(13) . . C14 C13 C31 C32 3.2(19) . . C12 C13 C31 C32 -142.7(12) . . C14 C13 C31 C30 147.4(13) . . C12 C13 C31 C30 1.5(12) . . C29 C30 C31 C13 -150.8(10) . . C11 C30 C31 C13 -0.3(13) . . C29 C30 C31 C32 -2.2(16) . . C11 C30 C31 C32 148.3(11) . . C13 C31 C32 C53 146.1(12) . . C30 C31 C32 C53 4.2(18) . . C13 C31 C32 C33 -7.4(18) . . C30 C31 C32 C33 -149.2(10) . . C53 C32 C33 C56 -5.3(15) . . C31 C32 C33 C56 150.9(10) . . C53 C32 C33 C34 -148.2(11) . . C31 C32 C33 C34 8.0(15) . . C13 C14 C34 C35 -145.5(14) . . C15 C14 C34 C35 -2(2) . . C13 C14 C34 C33 1(2) . . C15 C14 C34 C33 145.0(13) . . C56 C33 C34 C14 -154.4(13) . . C32 C33 C34 C14 -5.6(17) . . C56 C33 C34 C35 -3.6(10) . . C32 C33 C34 C35 145.1(9) . . C14 C34 C35 C36 7.2(16) . . C33 C34 C35 C36 -144.1(9) . . C14 C34 C35 C57 153.0(13) . . C33 C34 C35 C57 1.7(9) . . C57 C35 C36 C37 -0.1(14) . . C34 C35 C36 C37 142.9(11) . . C57 C35 C36 C16 -147.6(8) . . C34 C35 C36 C16 -4.6(12) . . C15 C16 C36 C37 -151.3(8) . . C17 C16 C36 C37 -1.6(12) . . C15 C16 C36 C35 -2.8(12) . . C17 C16 C36 C35 146.8(8) . . C35 C36 C37 C59 0(2) . . C16 C36 C37 C59 147.2(17) . . C35 C36 C37 C38 -145.3(11) . . C16 C36 C37 C38 2.3(16) . . C19 C18 C38 C39 1.2(17) . . C17 C18 C38 C39 -150.8(11) . . C19 C18 C38 C37 149.1(13) . . C17 C18 C38 C37 -2.9(17) . . C36 C37 C38 C18 0.0(19) . . C59 C37 C38 C18 -148.2(16) . . C36 C37 C38 C39 148.5(12) . . C59 C37 C38 C39 0.3(18) . . C18 C38 C39 C60 152.5(11) . . C37 C38 C39 C60 2.4(13) . . C18 C38 C39 C40 7.2(17) . . C37 C38 C39 C40 -142.9(13) . . C60 C39 C40 C63 7(2) . . C38 C39 C40 C63 141.3(13) . . C60 C39 C40 C41 -143.5(14) . . C38 C39 C40 C41 -8.8(19) . . C63 C40 C41 C42 -1.7(19) . . C39 C40 C41 C42 148.0(13) . . C63 C40 C41 C19 -147.8(13) . . C39 C40 C41 C19 2.0(18) . . C18 C19 C41 C40 6(2) . . C20 C19 C41 C40 148.5(12) . . C18 C19 C41 C42 -143.7(13) . . C20 C19 C41 C42 -1.4(15) . . C40 C41 C42 C43 -0.3(18) . . C19 C41 C42 C43 147.7(11) . . C40 C41 C42 C21 -148.3(12) . . C19 C41 C42 C21 -0.2(13) . . C22 C21 C42 C41 146.8(10) . . C20 C21 C42 C41 1.8(11) . . C22 C21 C42 C43 0.0(16) . . C20 C21 C42 C43 -145.0(11) . . C41 C42 C43 C64 1.4(15) . . C21 C42 C43 C64 144.2(11) . . C41 C42 C43 C44 -149.0(10) . . C21 C42 C43 C44 -6.1(15) . . C64 C43 C44 C45 -0.4(14) . . C42 C43 C44 C45 148.2(9) . . C64 C43 C44 C23 -138.3(11) . . C42 C43 C44 C23 10.3(14) . . C22 C23 C44 C43 -7.8(14) . . C24 C23 C44 C43 140.7(10) . . C22 C23 C44 C45 -149.2(8) . . C24 C23 C44 C45 -0.7(10) . . C43 C44 C45 C66 3.1(14) . . C23 C44 C45 C66 149.3(10) . . C43 C44 C45 C46 -144.6(8) . . C23 C44 C45 C46 1.6(9) . . C25 C24 C46 C47 1.5(16) . . C23 C24 C46 C47 -146.2(10) . . C25 C24 C46 C45 149.1(11) . . C23 C24 C46 C45 1.4(9) . . C66 C45 C46 C47 -2.8(14) . . C44 C45 C46 C47 145.5(9) . . C66 C45 C46 C24 -150.2(12) . . C44 C45 C46 C24 -1.9(9) . . C24 C46 C47 C48 -5.2(19) . . C45 C46 C47 C48 -147.0(14) . . C24 C46 C47 C68 142.2(12) . . C45 C46 C47 C68 0.4(14) . . C46 C47 C48 C26 7(2) . . C68 C47 C48 C26 -141.4(15) . . C46 C47 C48 C49 136.6(16) . . C68 C47 C48 C49 -12(2) . . C25 C26 C48 C47 -6(3) . . C27 C26 C48 C47 142.6(15) . . C25 C26 C48 C49 -148.1(13) . . C27 C26 C48 C49 0.2(18) . . C29 C28 C49 C50 -10(2) . . C27 C28 C49 C50 -155.5(13) . . C29 C28 C49 C48 142.7(14) . . C27 C28 C49 C48 -2.5(17) . . C47 C48 C49 C50 17(2) . . C26 C48 C49 C50 155.1(14) . . C47 C48 C49 C28 -136.3(17) . . C26 C48 C49 C28 1.5(18) . . C28 C49 C50 C51 3.7(19) . . C48 C49 C50 C51 -150.6(12) . . C28 C49 C50 C69 145.6(12) . . C48 C49 C50 C69 -9(2) . . C49 C50 C51 C52 4.6(19) . . C69 C50 C51 C52 -138.1(12) . . C49 C50 C51 C71 148.8(12) . . C69 C50 C51 C71 6.1(13) . . C28 C29 C52 C51 1.1(15) . . C30 C29 C52 C51 149.2(11) . . C28 C29 C52 C53 -151.2(11) . . C30 C29 C52 C53 -3.1(18) . . C50 C51 C52 C29 -7.1(18) . . C71 C51 C52 C29 -143.2(11) . . C50 C51 C52 C53 144.2(13) . . C71 C51 C52 C53 8.0(18) . . C33 C32 C53 C54 4.8(17) . . C31 C32 C53 C54 -149.0(12) . . C33 C32 C53 C52 148.2(11) . . C31 C32 C53 C52 -6(2) . . C29 C52 C53 C32 4.7(18) . . C51 C52 C53 C32 -146.2(12) . . C29 C52 C53 C54 151.6(11) . . C51 C52 C53 C54 0.6(17) . . C32 C53 C54 C55 -0.5(17) . . C52 C53 C54 C55 -146.9(10) . . C32 C53 C54 C72 136.6(14) . . C52 C53 C54 C72 -9.7(17) . . C53 C54 C55 C56 -4.0(15) . . C72 C54 C55 C56 -151.8(9) . . C53 C54 C55 C74 143.3(9) . . C72 C54 C55 C74 -4.5(11) . . C54 C55 C56 C33 3.8(14) . . C74 C55 C56 C33 -143.2(9) . . C54 C55 C56 C57 142.1(10) . . C74 C55 C56 C57 -4.9(13) . . C32 C33 C56 C55 1.1(14) . . C34 C33 C56 C55 146.9(9) . . C32 C33 C56 C57 -141.7(10) . . C34 C33 C56 C57 4.1(10) . . C36 C35 C57 C58 0.2(15) . . C34 C35 C57 C58 -147.5(10) . . C36 C35 C57 C56 148.3(8) . . C34 C35 C57 C56 0.7(9) . . C55 C56 C57 C58 2.6(15) . . C33 C56 C57 C58 144.5(10) . . C55 C56 C57 C35 -144.9(9) . . C33 C56 C57 C35 -3.0(10) . . C35 C57 C58 C59 0(2) . . C56 C57 C58 C59 -142.2(18) . . C35 C57 C58 C75 143.1(12) . . C56 C57 C58 C75 0.6(17) . . C57 C58 C59 C37 -1(3) . . C75 C58 C59 C37 -146(2) . . C57 C58 C59 C60 141(2) . . C75 C58 C59 C60 -4(3) . . C36 C37 C59 C58 1(3) . . C38 C37 C59 C58 150(2) . . C36 C37 C59 C60 -151.8(13) . . C38 C37 C59 C60 -3(2) . . C40 C39 C60 C61 -6(2) . . C38 C39 C60 C61 -148.9(12) . . C40 C39 C60 C59 138.5(18) . . C38 C39 C60 C59 -4.4(18) . . C58 C59 C60 C61 3(4) . . C37 C59 C60 C61 150.2(15) . . C58 C59 C60 C39 -143(2) . . C37 C59 C60 C39 5(2) . . C39 C60 C61 C62 0.1(19) . . C59 C60 C61 C62 -145.7(16) . . C39 C60 C61 C76 144.7(14) . . C59 C60 C61 C76 -1(2) . . C60 C61 C62 C63 6(2) . . C76 C61 C62 C63 -139.1(17) . . C60 C61 C62 C78 154.2(12) . . C76 C61 C62 C78 9.5(18) . . C41 C40 C63 C62 149.3(13) . . C39 C40 C63 C62 -0.9(17) . . C41 C40 C63 C64 2.6(18) . . C39 C40 C63 C64 -147.6(11) . . C61 C62 C63 C40 -5(2) . . C78 C62 C63 C40 -146.1(14) . . C61 C62 C63 C64 142.7(14) . . C78 C62 C63 C64 2(2) . . C42 C43 C64 C65 -148.8(10) . . C44 C43 C64 C65 -2.3(15) . . C42 C43 C64 C63 -0.4(15) . . C44 C43 C64 C63 146.1(10) . . C40 C63 C64 C65 147.7(11) . . C62 C63 C64 C65 2.7(15) . . C40 C63 C64 C43 -1.6(16) . . C62 C63 C64 C43 -146.6(11) . . C43 C64 C65 C66 2.4(14) . . C63 C64 C65 C66 -147.7(10) . . C43 C64 C65 C79 144.8(12) . . C63 C64 C65 C79 -5.3(15) . . C44 C45 C66 C65 -3.1(17) . . C46 C45 C66 C65 141.9(10) . . C44 C45 C66 C67 -141.8(12) . . C46 C45 C66 C67 3.2(18) . . C64 C65 C66 C45 0.2(16) . . C79 C65 C66 C45 -149.0(12) . . C64 C65 C66 C67 142.7(11) . . C79 C65 C66 C67 -6.6(13) . . C45 C66 C67 C68 -1(2) . . C65 C66 C67 C68 -145.6(14) . . C45 C66 C67 C80 151.4(11) . . C65 C66 C67 C80 7.1(16) . . C80 C67 C68 C69 2(2) . . C66 C67 C68 C69 149.8(13) . . C80 C67 C68 C47 -149.1(13) . . C66 C67 C68 C47 -1(2) . . C48 C47 C68 C69 -0.3(17) . . C46 C47 C68 C69 -149.9(10) . . C48 C47 C68 C67 151.1(10) . . C46 C47 C68 C67 1.4(17) . . C67 C68 C69 C70 -9.2(19) . . C47 C68 C69 C70 141.9(12) . . C67 C68 C69 C50 -143.8(15) . . C47 C68 C69 C50 7.4(18) . . C49 C50 C69 C68 -2(2) . . C51 C50 C69 C68 139.6(12) . . C49 C50 C69 C70 -144.0(15) . . C51 C50 C69 C70 -2.0(13) . . C68 C69 C70 C71 -147.5(12) . . C50 C69 C70 C71 -3.6(13) . . C68 C69 C70 C81 11.9(19) . . C50 C69 C70 C81 155.9(14) . . C81 C70 C71 C72 -2(2) . . C69 C70 C71 C72 154.9(11) . . C81 C70 C71 C51 -149.0(13) . . C69 C70 C71 C51 8.2(15) . . C52 C51 C71 C72 -8.6(15) . . C50 C51 C71 C72 -154.8(10) . . C52 C51 C71 C70 137.7(13) . . C50 C51 C71 C70 -8.5(13) . . C70 C71 C72 C73 -0.9(17) . . C51 C71 C72 C73 144.4(11) . . C70 C71 C72 C54 -145.0(11) . . C51 C71 C72 C54 0.3(13) . . C55 C54 C72 C71 152.2(9) . . C53 C54 C72 C71 9.6(16) . . C55 C54 C72 C73 5.1(11) . . C53 C54 C72 C73 -137.5(10) . . C71 C72 C73 C82 1.2(19) . . C54 C72 C73 C82 146.1(12) . . C71 C72 C73 C74 -149.0(11) . . C54 C72 C73 C74 -4.0(14) . . C72 C73 C74 C75 149.7(13) . . C82 C73 C74 C75 -2(2) . . C72 C73 C74 C55 1.0(13) . . C82 C73 C74 C55 -150.4(12) . . C56 C55 C74 C75 5.0(17) . . C54 C55 C74 C75 -144.5(13) . . C56 C55 C74 C73 151.9(10) . . C54 C55 C74 C73 2.4(13) . . C73 C74 C75 C76 0(2) . . C55 C74 C75 C76 140.7(15) . . C73 C74 C75 C58 -142.9(13) . . C55 C74 C75 C58 -2(2) . . C59 C58 C75 C76 3(2) . . C57 C58 C75 C76 -142.8(15) . . C59 C58 C75 C74 145.4(17) . . C57 C58 C75 C74 -0.7(19) . . C74 C75 C76 C77 2(3) . . C58 C75 C76 C77 144.4(17) . . C74 C75 C76 C61 -144.8(17) . . C58 C75 C76 C61 -3(3) . . C60 C61 C76 C75 2(3) . . C62 C61 C76 C75 145.8(19) . . C60 C61 C76 C77 -152.4(14) . . C62 C61 C76 C77 -8(2) . . C75 C76 C77 C78 -150.9(19) . . C61 C76 C77 C78 3.0(19) . . C75 C76 C77 C82 -3(3) . . C61 C76 C77 C82 151.3(14) . . C82 C77 C78 C79 5(2) . . C76 C77 C78 C79 149.9(15) . . C82 C77 C78 C62 -141.8(15) . . C76 C77 C78 C62 2.8(19) . . C63 C62 C78 C79 -4(2) . . C61 C62 C78 C79 -154.8(11) . . C63 C62 C78 C77 143.8(14) . . C61 C62 C78 C77 -7.2(15) . . C77 C78 C79 C80 -2.0(19) . . C62 C78 C79 C80 144.1(13) . . C77 C78 C79 C65 -144.6(12) . . C62 C78 C79 C65 1.4(17) . . C64 C65 C79 C78 3.2(18) . . C66 C65 C79 C78 149.6(11) . . C64 C65 C79 C80 -142.5(11) . . C66 C65 C79 C80 3.8(14) . . C78 C79 C80 C81 -3(2) . . C65 C79 C80 C81 142.4(11) . . C78 C79 C80 C67 -144.4(14) . . C65 C79 C80 C67 0.7(16) . . C68 C67 C80 C79 147.7(15) . . C66 C67 C80 C79 -4.8(17) . . C68 C67 C80 C81 3(2) . . C66 C67 C80 C81 -149.5(12) . . C79 C80 C81 C70 -139.0(14) . . C67 C80 C81 C70 -0.2(18) . . C79 C80 C81 C82 4.1(17) . . C67 C80 C81 C82 142.9(12) . . C71 C70 C81 C80 148.6(14) . . C69 C70 C81 C80 -6.9(19) . . C71 C70 C81 C82 4.7(19) . . C69 C70 C81 C82 -150.8(11) . . C72 C73 C82 C77 -145.6(14) . . C74 C73 C82 C77 1(2) . . C72 C73 C82 C81 1.5(19) . . C74 C73 C82 C81 148.6(12) . . C78 C77 C82 C73 143.7(14) . . C76 C77 C82 C73 0(2) . . C78 C77 C82 C81 -4(2) . . C76 C77 C82 C81 -146.9(13) . . C80 C81 C82 C73 -149.4(12) . . C70 C81 C82 C73 -3.9(16) . . C80 C81 C82 C77 -1.0(16) . . C70 C81 C82 C77 144.4(13) . . N3 Ni1 N1 C84 -88.3(3) . 6 N2 Ni1 N1 C84 0.4(3) 6 6 N2 Ni1 N1 C84 -177.1(3) . 6 N3 Ni1 N1 C84 88.3(3) . . N2 Ni1 N1 C84 177.1(3) 6 . N2 Ni1 N1 C84 -0.4(3) . . N1 Ni1 N2 C86 -0.2(3) . . N3 Ni1 N2 C86 -177.0(3) . . N2 Ni1 N2 C86 -86(4) 6 . N1 Ni1 N2 C89 177.1(3) . . N3 Ni1 N2 C89 0.3(3) . . N2 Ni1 N2 C89 92(4) 6 . N1 Ni1 N3 C91 -88.0(3) . . N2 Ni1 N3 C91 -176.7(3) 6 . N2 Ni1 N3 C91 0.8(3) . . N1 Ni1 N3 C91 88.0(3) . 6 N2 Ni1 N3 C91 -0.8(3) 6 6 N2 Ni1 N3 C91 176.7(3) . 6 C84 N1 C84 C85 179.03(19) 6 . Ni1 N1 C84 C85 1.7(5) . . C84 N1 C84 C83 0.9(4) 6 . Ni1 N1 C84 C83 -176.4(2) . . C83 C83 C84 C85 -178.7(3) 6 . C92 C83 C84 C85 -3.4(5) . . C83 C83 C84 N1 -0.6(3) 6 . C92 C83 C84 N1 174.7(3) . . N1 C84 C85 C86 -2.5(5) . . C83 C84 C85 C86 175.4(3) . . C89 N2 C86 C85 -178.3(3) . . Ni1 N2 C86 C85 -0.5(4) . . C89 N2 C86 C87 0.1(3) . . Ni1 N2 C86 C87 177.9(2) . . C84 C85 C86 N2 1.8(5) . . C84 C85 C86 C87 -176.4(3) . . N2 C86 C87 C88 -0.4(4) . . C85 C86 C87 C88 178.0(3) . . N2 C86 C87 C94 -178.7(3) . . C85 C86 C87 C94 -0.2(5) . . C86 C87 C88 C89 0.5(4) . . C94 C87 C88 C89 178.7(3) . . C86 C87 C88 C96 -176.7(3) . . C94 C87 C88 C96 1.5(6) . . C86 N2 C89 C90 178.2(3) . . Ni1 N2 C89 C90 0.4(4) . . C86 N2 C89 C88 0.2(3) . . Ni1 N2 C89 C88 -177.6(2) . . C87 C88 C89 N2 -0.5(4) . . C96 C88 C89 N2 176.8(3) . . C87 C88 C89 C90 -178.5(3) . . C96 C88 C89 C90 -1.2(5) . . N2 C89 C90 C91 -2.4(5) . . C88 C89 C90 C91 175.4(3) . . C91 N3 C91 C90 -179.5(2) 6 . Ni1 N3 C91 C90 -2.8(5) . . C91 N3 C91 C100 -1.3(5) 6 . Ni1 N3 C91 C100 175.3(3) . . C89 C90 C91 N3 3.7(5) . . C89 C90 C91 C100 -174.3(3) . . C83 C83 C92 C93 94.7(3) 6 . C84 C83 C92 C93 -79.6(4) . . C88 C87 C94 C95 -100.1(4) . . C86 C87 C94 C95 77.7(4) . . C87 C88 C96 C97 99.6(4) . . C89 C88 C96 C97 -77.1(4) . . N3 C91 C100 C100 0.8(3) . 6 C90 C91 C100 C100 179.0(3) . 6 N3 C91 C100 C98 -176.2(3) . . C90 C91 C100 C98 2.0(5) . . C99 C98 C100 C100 -102.3(3) . 6 C99 C98 C100 C91 74.1(4) . . C106 C101 C102 C103 0.0 . . C101 C102 C103 C104 0.0 . . C102 C103 C104 C105 0.000(1) . . C103 C104 C105 C106 0.000(1) . . C102 C101 C106 C105 0.000(1) . . C104 C105 C106 C101 0.000(1) . . C114 C109 C110 C111 0.0 . . C109 C110 C111 C112 0.0 . . C110 C111 C112 C113 0.0 . . C111 C112 C113 C114 0.0 . . C112 C113 C114 C109 0.0 . . C110 C109 C114 C113 0.0 . .