#------------------------------------------------------------------------------ #$Date: 2017-04-20 05:33:01 +0300 (Thu, 20 Apr 2017) $ #$Revision: 195612 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042722.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_7042722 loop_ _publ_author_name 'Armstrong, David' 'Taullaj, Fioralba' 'Singh, Kamalpreet' 'Mirabi, Bijan' 'Lough, Alan' 'Fekl, Ulrich Werner' _publ_section_title ; Adamantyl Metal Complexes: New Routes to Adamantyl Anions and New Transmetallations ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00428A _journal_year 2017 _chemical_formula_moiety 'C30 H38 N2 Zn' _chemical_formula_sum 'C30 H38 N2 Zn' _chemical_formula_weight 491.99 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-01-19 deposited with the CCDC. 2017-04-19 downloaded from the CCDC. ; _cell_angle_alpha 87.754(3) _cell_angle_beta 66.311(3) _cell_angle_gamma 78.315(3) _cell_formula_units_Z 2 _cell_length_a 10.5819(10) _cell_length_b 11.0816(10) _cell_length_c 11.7087(11) _cell_measurement_reflns_used 9949 _cell_measurement_temperature 147(2) _cell_measurement_theta_max 27.54 _cell_measurement_theta_min 2.22 _cell_volume 1229.9(2) _computing_cell_refinement APEX2 _computing_data_collection 'APEX2 (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 147(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 39635 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.648 _diffrn_reflns_theta_min 1.879 _diffrn_source 'sealed tube with Bruker Triumph monochromator' _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 19960' _exptl_crystal_density_diffrn 1.329 _exptl_crystal_description plate _exptl_crystal_F_000 524 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.361 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 5701 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0274 _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^)+(0.0237P)^2^+0.5884P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.0625 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4867 _reflns_number_total 5701 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00428a2.cif _cod_data_source_block d15142_a _cod_database_code 7042722 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.862 _shelx_estimated_absorpt_t_max 0.951 _shelx_res_file ; d15142_a.res created by SHELXL-2014/7 TITL mo_d15142_0m_a.res in P-1 REM Old TITL mo_d15142_0m in P1 REM SHELXT solution in P-1 REM R1 0.077, Rweak 0.008, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C30 N2 Zn CELL 0.71073 10.5819 11.0816 11.7087 87.754 66.311 78.315 ZERR 2.000 0.0010 0.0010 0.0011 0.003 0.003 0.003 LATT 1 SFAC C H N ZN UNIT 60 76 4 2 TEMP -126.140 SIZE 0.050 0.150 0.150 ACTA L.S. 5 BOND $H CONF HTAB FMAP 2 PLAN 20 WGHT 0.023700 0.588400 FVAR 0.61786 ZN1 4 0.646764 0.296858 0.656958 11.00000 0.01874 0.01695 = 0.01407 0.00022 -0.00665 -0.00503 N1 3 0.692738 0.282814 0.827426 11.00000 0.01694 0.01772 = 0.01494 0.00125 -0.00582 -0.00269 N2 3 0.611034 0.488550 0.728738 11.00000 0.01740 0.01790 = 0.01580 0.00064 -0.00753 -0.00346 C1 1 0.746246 0.175813 0.864139 11.00000 0.02092 0.01995 = 0.02110 0.00314 -0.00629 -0.00219 AFIX 43 H1A 2 0.740848 0.101132 0.830841 11.00000 -1.20000 AFIX 0 C2 1 0.808906 0.168863 0.948106 11.00000 0.01885 0.02944 = 0.02171 0.00953 -0.00708 -0.00018 AFIX 43 H2A 2 0.843750 0.091297 0.973460 11.00000 -1.20000 AFIX 0 C3 1 0.819678 0.277522 0.994350 11.00000 0.02001 0.04072 = 0.01814 0.00475 -0.01029 -0.00392 AFIX 43 H3A 2 0.862863 0.275745 1.051724 11.00000 -1.20000 AFIX 0 C4 1 0.766822 0.388858 0.956077 11.00000 0.01944 0.02984 = 0.01778 -0.00164 -0.00829 -0.00454 AFIX 43 H4A 2 0.774090 0.464445 0.986152 11.00000 -1.20000 AFIX 0 C5 1 0.702769 0.388584 0.872788 11.00000 0.01276 0.02059 = 0.01155 0.00069 -0.00237 -0.00303 C6 1 0.640573 0.503578 0.828340 11.00000 0.01233 0.01898 = 0.01399 0.00063 -0.00372 -0.00513 C7 1 0.612390 0.619386 0.885913 11.00000 0.01705 0.02287 = 0.01813 -0.00299 -0.00564 -0.00510 AFIX 43 H7A 2 0.633260 0.627923 0.956521 11.00000 -1.20000 AFIX 0 C8 1 0.553864 0.721459 0.839238 11.00000 0.01866 0.01787 = 0.02605 -0.00385 -0.00417 -0.00345 AFIX 43 H8A 2 0.535029 0.801225 0.876729 11.00000 -1.20000 AFIX 0 C9 1 0.522866 0.706477 0.737238 11.00000 0.01973 0.01854 = 0.02693 0.00363 -0.00779 -0.00037 AFIX 43 H9A 2 0.482109 0.775281 0.703579 11.00000 -1.20000 AFIX 0 C10 1 0.552847 0.588559 0.685603 11.00000 0.02308 0.02214 = 0.02086 0.00105 -0.01201 -0.00221 AFIX 43 H10A 2 0.531014 0.578005 0.615927 11.00000 -1.20000 AFIX 0 C11 1 0.846886 0.236246 0.533333 11.00000 0.02004 0.01843 = 0.01635 0.00311 -0.00928 -0.00275 AFIX 13 H11A 2 0.895766 0.179622 0.578303 11.00000 -1.20000 AFIX 0 C12 1 0.932598 0.338282 0.482153 11.00000 0.02150 0.02630 = 0.01864 -0.00113 -0.00979 -0.00798 AFIX 13 H12A 2 0.928454 0.387714 0.553675 11.00000 -1.20000 AFIX 0 C13 1 1.087360 0.282195 0.399763 11.00000 0.01976 0.04430 = 0.02542 0.00297 -0.01098 -0.00998 AFIX 23 H13A 2 1.140792 0.348827 0.368667 11.00000 -1.20000 H13B 2 1.130323 0.228183 0.449547 11.00000 -1.20000 AFIX 0 C14 1 1.094966 0.206911 0.288945 11.00000 0.01533 0.03724 = 0.02107 0.00026 -0.00411 -0.00194 AFIX 13 H14A 2 1.195579 0.169805 0.235843 11.00000 -1.20000 AFIX 0 C15 1 1.011629 0.104106 0.337542 11.00000 0.02595 0.02225 = 0.02253 -0.00171 -0.00762 0.00406 AFIX 23 H15A 2 1.054043 0.047489 0.386026 11.00000 -1.20000 H15B 2 1.015550 0.055965 0.266306 11.00000 -1.20000 AFIX 0 C16 1 0.857633 0.160743 0.420843 11.00000 0.02120 0.01451 = 0.01803 -0.00060 -0.00496 -0.00443 AFIX 13 H16A 2 0.803941 0.093200 0.451828 11.00000 -1.20000 AFIX 0 C17 1 0.870397 0.423432 0.403149 11.00000 0.02857 0.01736 = 0.02309 0.00299 -0.01076 -0.00941 AFIX 23 H17A 2 0.924609 0.489483 0.371525 11.00000 -1.20000 H17B 2 0.771431 0.462584 0.455175 11.00000 -1.20000 AFIX 0 C18 1 1.030556 0.291329 0.211186 11.00000 0.02519 0.03296 = 0.01724 0.00335 -0.00569 -0.01209 AFIX 23 H18A 2 1.035583 0.243232 0.139450 11.00000 -1.20000 H18B 2 1.084342 0.357461 0.178270 11.00000 -1.20000 AFIX 0 C19 1 0.793763 0.245319 0.342267 11.00000 0.01903 0.02133 = 0.01713 -0.00215 -0.00819 -0.00502 AFIX 23 H19A 2 0.797508 0.196726 0.271395 11.00000 -1.20000 H19B 2 0.693765 0.281596 0.394028 11.00000 -1.20000 AFIX 0 C20 1 0.876238 0.348480 0.292851 11.00000 0.02453 0.02076 = 0.01857 0.00398 -0.01166 -0.00567 AFIX 13 H20A 2 0.834072 0.403828 0.242215 11.00000 -1.20000 AFIX 0 C21 1 0.450819 0.287853 0.676454 11.00000 0.02179 0.01712 = 0.01514 0.00204 -0.00801 -0.00716 AFIX 13 H21A 2 0.420239 0.360396 0.633331 11.00000 -1.20000 AFIX 0 C22 1 0.442508 0.173501 0.611035 11.00000 0.02489 0.02470 = 0.01449 -0.00287 -0.00566 -0.01055 AFIX 13 H22A 2 0.515141 0.164481 0.523211 11.00000 -1.20000 AFIX 0 C23 1 0.295893 0.186118 0.609370 11.00000 0.03311 0.03561 = 0.02390 0.00349 -0.01566 -0.01879 AFIX 23 H23A 2 0.276442 0.259672 0.563621 11.00000 -1.20000 H23B 2 0.293069 0.112582 0.565784 11.00000 -1.20000 AFIX 0 C24 1 0.183533 0.198674 0.743575 11.00000 0.02188 0.03023 = 0.02900 0.00693 -0.01325 -0.01170 AFIX 13 H24A 2 0.088092 0.207664 0.742442 11.00000 -1.20000 AFIX 0 C25 1 0.213071 0.083839 0.813248 11.00000 0.02863 0.02322 = 0.02885 0.00417 -0.00854 -0.01285 AFIX 23 H25A 2 0.208727 0.009782 0.771440 11.00000 -1.20000 H25B 2 0.140627 0.091450 0.899924 11.00000 -1.20000 AFIX 0 C26 1 0.359662 0.070001 0.814709 11.00000 0.02625 0.01519 = 0.02780 0.00598 -0.00898 -0.00335 AFIX 13 H26A 2 0.379013 -0.005156 0.859972 11.00000 -1.20000 AFIX 0 C27 1 0.364400 0.184593 0.881243 11.00000 0.02016 0.02716 = 0.01496 0.00323 -0.00624 -0.00529 AFIX 23 H27A 2 0.292137 0.193261 0.968032 11.00000 -1.20000 H27B 2 0.457998 0.175631 0.884260 11.00000 -1.20000 AFIX 0 C28 1 0.336589 0.299496 0.810715 11.00000 0.02035 0.01634 = 0.01707 -0.00317 -0.00607 -0.00338 AFIX 13 H28A 2 0.339025 0.373893 0.854842 11.00000 -1.20000 AFIX 0 C29 1 0.188804 0.312150 0.811053 11.00000 0.02056 0.02109 = 0.02623 0.00379 -0.00768 -0.00140 AFIX 23 H29A 2 0.117318 0.319689 0.898133 11.00000 -1.20000 H29B 2 0.166986 0.387536 0.768579 11.00000 -1.20000 AFIX 0 C30 1 0.471495 0.057821 0.680177 11.00000 0.02718 0.01745 = 0.02994 -0.00615 -0.00618 -0.00337 AFIX 23 H30A 2 0.566372 0.047682 0.680730 11.00000 -1.20000 H30B 2 0.469037 -0.015980 0.636736 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_d15142_0m_a.res in P-1 REM R1 = 0.0274 for 4867 Fo > 4sig(Fo) and 0.0382 for all 5701 data REM 298 parameters refined using 0 restraints END WGHT 0.0235 0.5853 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.361, deepest hole -0.253, 1-sigma level 0.051 Q1 1 0.5166 0.2964 0.6858 11.00000 0.05 0.36 Q2 1 0.4027 0.2902 0.7419 11.00000 0.05 0.36 Q3 1 0.6260 0.4982 0.7794 11.00000 0.05 0.33 Q4 1 0.3669 0.1766 0.6209 11.00000 0.05 0.31 Q5 1 0.2659 0.2962 0.8154 11.00000 0.05 0.30 Q6 1 0.3642 0.1299 0.8458 11.00000 0.05 0.30 Q7 1 0.6575 0.4452 0.8607 11.00000 0.05 0.30 Q8 1 0.4624 0.2267 0.6464 11.00000 0.05 0.29 Q9 1 0.8313 0.2023 0.3764 11.00000 0.05 0.28 Q10 1 0.7126 0.3391 0.8372 11.00000 0.05 0.28 Q11 1 0.3643 0.2382 0.8336 11.00000 0.05 0.28 Q12 1 0.4621 0.1240 0.6504 11.00000 0.05 0.28 Q13 1 0.7145 0.3856 0.9283 11.00000 0.05 0.27 Q14 1 0.7730 0.2765 0.5916 11.00000 0.05 0.27 Q15 1 0.9269 0.1284 0.3811 11.00000 0.05 0.27 Q16 1 0.8458 0.2040 0.4849 11.00000 0.05 0.27 Q17 1 1.0600 0.2488 0.2544 11.00000 0.05 0.27 Q18 1 0.7581 0.3860 0.8937 11.00000 0.05 0.26 Q19 1 0.7977 0.1801 0.8917 11.00000 0.05 0.26 Q20 1 0.8719 0.3825 0.3436 11.00000 0.05 0.26 ; _shelx_res_checksum 59036 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 Zn1 Zn 0.64676(2) 0.29686(2) 0.65696(2) 0.01634(6) Uani 1 1 d . . N1 N 0.69274(13) 0.28281(11) 0.82743(11) 0.0169(3) Uani 1 1 d . . N2 N 0.61103(13) 0.48855(11) 0.72874(11) 0.0168(3) Uani 1 1 d . . C1 C 0.74625(17) 0.17581(14) 0.86414(15) 0.0217(3) Uani 1 1 d . . H1A H 0.7408 0.1011 0.8308 0.026 Uiso 1 1 calc R U C2 C 0.80891(17) 0.16886(16) 0.94811(15) 0.0247(4) Uani 1 1 d . . H2A H 0.8438 0.0913 0.9735 0.030 Uiso 1 1 calc R U C3 C 0.81968(17) 0.27752(16) 0.99435(15) 0.0259(4) Uani 1 1 d . . H3A H 0.8629 0.2757 1.0517 0.031 Uiso 1 1 calc R U C4 C 0.76682(16) 0.38886(15) 0.95608(14) 0.0221(3) Uani 1 1 d . . H4A H 0.7741 0.4644 0.9862 0.027 Uiso 1 1 calc R U C5 C 0.70277(15) 0.38858(13) 0.87279(13) 0.0158(3) Uani 1 1 d . . C6 C 0.64057(15) 0.50358(13) 0.82834(13) 0.0153(3) Uani 1 1 d . . C7 C 0.61239(16) 0.61939(14) 0.88591(15) 0.0195(3) Uani 1 1 d . . H7A H 0.6333 0.6279 0.9565 0.023 Uiso 1 1 calc R U C8 C 0.55386(16) 0.72146(14) 0.83924(15) 0.0223(3) Uani 1 1 d . . H8A H 0.5350 0.8012 0.8767 0.027 Uiso 1 1 calc R U C9 C 0.52287(17) 0.70648(14) 0.73724(16) 0.0229(3) Uani 1 1 d . . H9A H 0.4821 0.7753 0.7036 0.027 Uiso 1 1 calc R U C10 C 0.55285(17) 0.58856(14) 0.68560(15) 0.0214(3) Uani 1 1 d . . H10A H 0.5310 0.5780 0.6159 0.026 Uiso 1 1 calc R U C11 C 0.84689(16) 0.23625(14) 0.53333(14) 0.0179(3) Uani 1 1 d . . H11A H 0.8958 0.1796 0.5783 0.021 Uiso 1 1 calc R U C12 C 0.93260(17) 0.33828(15) 0.48215(15) 0.0210(3) Uani 1 1 d . . H12A H 0.9285 0.3877 0.5537 0.025 Uiso 1 1 calc R U C13 C 1.08736(18) 0.28219(17) 0.39976(16) 0.0287(4) Uani 1 1 d . . H13A H 1.1408 0.3488 0.3687 0.034 Uiso 1 1 calc R U H13B H 1.1303 0.2282 0.4495 0.034 Uiso 1 1 calc R U C14 C 1.09497(17) 0.20691(16) 0.28895(15) 0.0261(4) Uani 1 1 d . . H14A H 1.1956 0.1698 0.2358 0.031 Uiso 1 1 calc R U C15 C 1.01163(18) 0.10411(15) 0.33754(16) 0.0256(4) Uani 1 1 d . . H15A H 1.0540 0.0475 0.3860 0.031 Uiso 1 1 calc R U H15B H 1.0156 0.0560 0.2663 0.031 Uiso 1 1 calc R U C16 C 0.85763(16) 0.16074(13) 0.42084(14) 0.0187(3) Uani 1 1 d . . H16A H 0.8039 0.0932 0.4518 0.022 Uiso 1 1 calc R U C17 C 0.87040(18) 0.42343(14) 0.40315(15) 0.0222(3) Uani 1 1 d . . H17A H 0.9246 0.4895 0.3715 0.027 Uiso 1 1 calc R U H17B H 0.7714 0.4626 0.4552 0.027 Uiso 1 1 calc R U C18 C 1.03056(17) 0.29133(16) 0.21119(15) 0.0252(4) Uani 1 1 d . . H18A H 1.0356 0.2432 0.1395 0.030 Uiso 1 1 calc R U H18B H 1.0843 0.3575 0.1783 0.030 Uiso 1 1 calc R U C19 C 0.79376(16) 0.24532(14) 0.34227(14) 0.0186(3) Uani 1 1 d . . H19A H 0.7975 0.1967 0.2714 0.022 Uiso 1 1 calc R U H19B H 0.6938 0.2816 0.3940 0.022 Uiso 1 1 calc R U C20 C 0.87624(17) 0.34848(14) 0.29285(14) 0.0202(3) Uani 1 1 d . . H20A H 0.8341 0.4038 0.2422 0.024 Uiso 1 1 calc R U C21 C 0.45082(16) 0.28785(14) 0.67645(14) 0.0174(3) Uani 1 1 d . . H21A H 0.4202 0.3604 0.6333 0.021 Uiso 1 1 calc R U C22 C 0.44251(17) 0.17350(14) 0.61104(14) 0.0211(3) Uani 1 1 d . . H22A H 0.5151 0.1645 0.5232 0.025 Uiso 1 1 calc R U C23 C 0.29589(19) 0.18612(17) 0.60937(16) 0.0278(4) Uani 1 1 d . . H23A H 0.2764 0.2597 0.5636 0.033 Uiso 1 1 calc R U H23B H 0.2931 0.1126 0.5658 0.033 Uiso 1 1 calc R U C24 C 0.18353(18) 0.19867(15) 0.74357(16) 0.0252(4) Uani 1 1 d . . H24A H 0.0881 0.2077 0.7424 0.030 Uiso 1 1 calc R U C25 C 0.21307(18) 0.08384(15) 0.81325(17) 0.0268(4) Uani 1 1 d . . H25A H 0.2087 0.0098 0.7714 0.032 Uiso 1 1 calc R U H25B H 0.1406 0.0914 0.8999 0.032 Uiso 1 1 calc R U C26 C 0.35966(18) 0.07000(14) 0.81471(16) 0.0240(3) Uani 1 1 d . . H26A H 0.3790 -0.0052 0.8600 0.029 Uiso 1 1 calc R U C27 C 0.36440(17) 0.18459(15) 0.88124(15) 0.0210(3) Uani 1 1 d . . H27A H 0.2921 0.1933 0.9680 0.025 Uiso 1 1 calc R U H27B H 0.4580 0.1756 0.8843 0.025 Uiso 1 1 calc R U C28 C 0.33659(16) 0.29950(14) 0.81072(14) 0.0183(3) Uani 1 1 d . . H28A H 0.3390 0.3739 0.8548 0.022 Uiso 1 1 calc R U C29 C 0.18880(17) 0.31215(15) 0.81105(16) 0.0237(3) Uani 1 1 d . . H29A H 0.1173 0.3197 0.8981 0.028 Uiso 1 1 calc R U H29B H 0.1670 0.3875 0.7686 0.028 Uiso 1 1 calc R U C30 C 0.47150(18) 0.05782(14) 0.68018(16) 0.0266(4) Uani 1 1 d . . H30A H 0.5664 0.0477 0.6807 0.032 Uiso 1 1 calc R U H30B H 0.4690 -0.0160 0.6367 0.032 Uiso 1 1 calc R U 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 Zn1 0.01874(10) 0.01695(9) 0.01407(9) 0.00022(6) -0.00665(7) -0.00503(7) N1 0.0169(6) 0.0177(6) 0.0149(6) 0.0013(5) -0.0058(5) -0.0027(5) N2 0.0174(6) 0.0179(6) 0.0158(6) 0.0006(5) -0.0075(5) -0.0035(5) C1 0.0209(8) 0.0199(8) 0.0211(8) 0.0031(6) -0.0063(7) -0.0022(6) C2 0.0188(8) 0.0294(9) 0.0217(8) 0.0095(7) -0.0071(7) -0.0002(7) C3 0.0200(8) 0.0407(10) 0.0181(8) 0.0047(7) -0.0103(7) -0.0039(7) C4 0.0194(8) 0.0298(9) 0.0178(8) -0.0016(6) -0.0083(7) -0.0045(7) C5 0.0128(7) 0.0206(7) 0.0116(7) 0.0007(6) -0.0024(6) -0.0030(6) C6 0.0123(7) 0.0190(7) 0.0140(7) 0.0006(6) -0.0037(6) -0.0051(6) C7 0.0171(8) 0.0229(8) 0.0181(8) -0.0030(6) -0.0056(6) -0.0051(6) C8 0.0187(8) 0.0179(8) 0.0260(9) -0.0039(6) -0.0042(7) -0.0035(6) C9 0.0197(8) 0.0185(8) 0.0269(9) 0.0036(6) -0.0078(7) -0.0004(6) C10 0.0231(8) 0.0221(8) 0.0209(8) 0.0010(6) -0.0120(7) -0.0022(6) C11 0.0200(8) 0.0184(7) 0.0163(7) 0.0031(6) -0.0093(6) -0.0027(6) C12 0.0215(8) 0.0263(8) 0.0186(8) -0.0011(6) -0.0098(7) -0.0080(6) C13 0.0198(9) 0.0443(11) 0.0254(9) 0.0030(8) -0.0110(7) -0.0100(8) C14 0.0153(8) 0.0372(10) 0.0211(8) 0.0003(7) -0.0041(7) -0.0019(7) C15 0.0259(9) 0.0223(8) 0.0225(8) -0.0017(7) -0.0076(7) 0.0041(7) C16 0.0212(8) 0.0145(7) 0.0180(8) -0.0006(6) -0.0050(6) -0.0044(6) C17 0.0286(9) 0.0174(7) 0.0231(8) 0.0030(6) -0.0108(7) -0.0094(6) C18 0.0252(9) 0.0330(9) 0.0172(8) 0.0033(7) -0.0057(7) -0.0121(7) C19 0.0190(8) 0.0213(8) 0.0171(8) -0.0022(6) -0.0082(6) -0.0050(6) C20 0.0245(8) 0.0208(8) 0.0186(8) 0.0040(6) -0.0117(7) -0.0057(6) C21 0.0218(8) 0.0171(7) 0.0151(7) 0.0020(6) -0.0080(6) -0.0072(6) C22 0.0249(8) 0.0247(8) 0.0145(8) -0.0029(6) -0.0057(7) -0.0106(7) C23 0.0331(10) 0.0356(10) 0.0239(9) 0.0035(7) -0.0157(8) -0.0188(8) C24 0.0219(8) 0.0302(9) 0.0290(9) 0.0069(7) -0.0132(7) -0.0117(7) C25 0.0286(9) 0.0232(8) 0.0289(9) 0.0042(7) -0.0085(8) -0.0128(7) C26 0.0263(9) 0.0152(7) 0.0278(9) 0.0060(6) -0.0090(7) -0.0034(6) C27 0.0202(8) 0.0272(8) 0.0150(7) 0.0032(6) -0.0062(6) -0.0053(6) C28 0.0203(8) 0.0163(7) 0.0171(8) -0.0032(6) -0.0061(6) -0.0034(6) C29 0.0206(8) 0.0211(8) 0.0262(9) 0.0038(7) -0.0077(7) -0.0014(6) C30 0.0272(9) 0.0174(8) 0.0299(9) -0.0061(7) -0.0062(8) -0.0034(7) 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' Zn Zn 0.2839 1.4301 '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 C21 Zn1 C11 137.88(6) C21 Zn1 N2 100.82(5) C11 Zn1 N2 112.18(5) C21 Zn1 N1 118.00(5) C11 Zn1 N1 96.59(5) N2 Zn1 N1 73.48(4) C1 N1 C5 118.42(13) C1 N1 Zn1 122.98(10) C5 N1 Zn1 116.07(9) C10 N2 C6 118.20(13) C10 N2 Zn1 124.36(10) C6 N2 Zn1 117.25(9) N1 C1 C2 123.15(15) N1 C1 H1A 118.4 C2 C1 H1A 118.4 C1 C2 C3 118.41(15) C1 C2 H2A 120.8 C3 C2 H2A 120.8 C2 C3 C4 119.22(15) C2 C3 H3A 120.4 C4 C3 H3A 120.4 C3 C4 C5 119.08(15) C3 C4 H4A 120.5 C5 C4 H4A 120.5 N1 C5 C4 121.69(14) N1 C5 C6 115.40(13) C4 C5 C6 122.91(14) N2 C6 C7 121.68(14) N2 C6 C5 115.45(12) C7 C6 C5 122.86(13) C8 C7 C6 119.25(14) C8 C7 H7A 120.4 C6 C7 H7A 120.4 C7 C8 C9 119.30(14) C7 C8 H8A 120.4 C9 C8 H8A 120.4 C10 C9 C8 118.18(15) C10 C9 H9A 120.9 C8 C9 H9A 120.9 N2 C10 C9 123.39(15) N2 C10 H10A 118.3 C9 C10 H10A 118.3 C16 C11 C12 107.79(12) C16 C11 Zn1 113.32(10) C12 C11 Zn1 114.76(10) C16 C11 H11A 106.8 C12 C11 H11A 106.8 Zn1 C11 H11A 106.8 C17 C12 C13 108.38(13) C17 C12 C11 109.88(12) C13 C12 C11 110.91(13) C17 C12 H12A 109.2 C13 C12 H12A 109.2 C11 C12 H12A 109.2 C14 C13 C12 109.63(13) C14 C13 H13A 109.7 C12 C13 H13A 109.7 C14 C13 H13B 109.7 C12 C13 H13B 109.7 H13A C13 H13B 108.2 C18 C14 C15 109.00(14) C18 C14 C13 109.49(14) C15 C14 C13 109.57(14) C18 C14 H14A 109.6 C15 C14 H14A 109.6 C13 C14 H14A 109.6 C14 C15 C16 109.69(13) C14 C15 H15A 109.7 C16 C15 H15A 109.7 C14 C15 H15B 109.7 C16 C15 H15B 109.7 H15A C15 H15B 108.2 C15 C16 C19 108.49(12) C15 C16 C11 111.36(13) C19 C16 C11 109.36(12) C15 C16 H16A 109.2 C19 C16 H16A 109.2 C11 C16 H16A 109.2 C12 C17 C20 109.70(13) C12 C17 H17A 109.7 C20 C17 H17A 109.7 C12 C17 H17B 109.7 C20 C17 H17B 109.7 H17A C17 H17B 108.2 C14 C18 C20 109.55(13) C14 C18 H18A 109.8 C20 C18 H18A 109.8 C14 C18 H18B 109.8 C20 C18 H18B 109.8 H18A C18 H18B 108.2 C20 C19 C16 109.75(12) C20 C19 H19A 109.7 C16 C19 H19A 109.7 C20 C19 H19B 109.7 C16 C19 H19B 109.7 H19A C19 H19B 108.2 C19 C20 C18 109.29(13) C19 C20 C17 109.52(12) C18 C20 C17 109.09(13) C19 C20 H20A 109.6 C18 C20 H20A 109.6 C17 C20 H20A 109.6 C28 C21 C22 107.62(12) C28 C21 Zn1 116.73(10) C22 C21 Zn1 114.52(11) C28 C21 H21A 105.7 C22 C21 H21A 105.7 Zn1 C21 H21A 105.7 C30 C22 C23 108.83(13) C30 C22 C21 109.70(13) C23 C22 C21 110.89(13) C30 C22 H22A 109.1 C23 C22 H22A 109.1 C21 C22 H22A 109.1 C24 C23 C22 109.70(13) C24 C23 H23A 109.7 C22 C23 H23A 109.7 C24 C23 H23B 109.7 C22 C23 H23B 109.7 H23A C23 H23B 108.2 C25 C24 C29 108.75(13) C25 C24 C23 109.46(14) C29 C24 C23 109.60(13) C25 C24 H24A 109.7 C29 C24 H24A 109.7 C23 C24 H24A 109.7 C24 C25 C26 109.63(13) C24 C25 H25A 109.7 C26 C25 H25A 109.7 C24 C25 H25B 109.7 C26 C25 H25B 109.7 H25A C25 H25B 108.2 C30 C26 C25 109.51(14) C30 C26 C27 109.34(13) C25 C26 C27 109.23(13) C30 C26 H26A 109.6 C25 C26 H26A 109.6 C27 C26 H26A 109.6 C28 C27 C26 109.49(13) C28 C27 H27A 109.8 C26 C27 H27A 109.8 C28 C27 H27B 109.8 C26 C27 H27B 109.8 H27A C27 H27B 108.2 C27 C28 C29 108.21(12) C27 C28 C21 110.00(12) C29 C28 C21 111.21(13) C27 C28 H28A 109.1 C29 C28 H28A 109.1 C21 C28 H28A 109.1 C24 C29 C28 109.71(13) C24 C29 H29A 109.7 C28 C29 H29A 109.7 C24 C29 H29B 109.7 C28 C29 H29B 109.7 H29A C29 H29B 108.2 C22 C30 C26 109.60(13) C22 C30 H30A 109.8 C26 C30 H30A 109.8 C22 C30 H30B 109.8 C26 C30 H30B 109.8 H30A C30 H30B 108.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zn1 C21 2.0157(15) Zn1 C11 2.0169(16) Zn1 N2 2.2183(12) Zn1 N1 2.2293(12) N1 C1 1.3398(19) N1 C5 1.3460(19) N2 C10 1.3387(19) N2 C6 1.3471(19) C1 C2 1.382(2) C1 H1A 0.9500 C2 C3 1.383(2) C2 H2A 0.9500 C3 C4 1.384(2) C3 H3A 0.9500 C4 C5 1.394(2) C4 H4A 0.9500 C5 C6 1.487(2) C6 C7 1.393(2) C7 C8 1.379(2) C7 H7A 0.9500 C8 C9 1.383(2) C8 H8A 0.9500 C9 C10 1.383(2) C9 H9A 0.9500 C10 H10A 0.9500 C11 C16 1.541(2) C11 C12 1.545(2) C11 H11A 1.0000 C12 C17 1.532(2) C12 C13 1.538(2) C12 H12A 1.0000 C13 C14 1.536(2) C13 H13A 0.9900 C13 H13B 0.9900 C14 C18 1.530(2) C14 C15 1.534(2) C14 H14A 1.0000 C15 C16 1.535(2) C15 H15A 0.9900 C15 H15B 0.9900 C16 C19 1.535(2) C16 H16A 1.0000 C17 C20 1.536(2) C17 H17A 0.9900 C17 H17B 0.9900 C18 C20 1.535(2) C18 H18A 0.9900 C18 H18B 0.9900 C19 C20 1.533(2) C19 H19A 0.9900 C19 H19B 0.9900 C20 H20A 1.0000 C21 C28 1.541(2) C21 C22 1.541(2) C21 H21A 1.0000 C22 C30 1.534(2) C22 C23 1.537(2) C22 H22A 1.0000 C23 C24 1.533(2) C23 H23A 0.9900 C23 H23B 0.9900 C24 C25 1.531(2) C24 C29 1.533(2) C24 H24A 1.0000 C25 C26 1.535(2) C25 H25A 0.9900 C25 H25B 0.9900 C26 C30 1.534(2) C26 C27 1.535(2) C26 H26A 1.0000 C27 C28 1.533(2) C27 H27A 0.9900 C27 H27B 0.9900 C28 C29 1.540(2) C28 H28A 1.0000 C29 H29A 0.9900 C29 H29B 0.9900 C30 H30A 0.9900 C30 H30B 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 C5 N1 C1 C2 1.2(2) Zn1 N1 C1 C2 162.49(12) N1 C1 C2 C3 -1.5(2) C1 C2 C3 C4 0.5(2) C2 C3 C4 C5 0.6(2) C1 N1 C5 C4 0.0(2) Zn1 N1 C5 C4 -162.56(11) C1 N1 C5 C6 -179.76(13) Zn1 N1 C5 C6 17.71(16) C3 C4 C5 N1 -0.9(2) C3 C4 C5 C6 178.81(14) C10 N2 C6 C7 -0.2(2) Zn1 N2 C6 C7 -175.37(11) C10 N2 C6 C5 179.00(13) Zn1 N2 C6 C5 3.79(16) N1 C5 C6 N2 -14.29(19) C4 C5 C6 N2 165.98(14) N1 C5 C6 C7 164.85(14) C4 C5 C6 C7 -14.9(2) N2 C6 C7 C8 -0.6(2) C5 C6 C7 C8 -179.65(14) C6 C7 C8 C9 0.8(2) C7 C8 C9 C10 -0.3(2) C6 N2 C10 C9 0.7(2) Zn1 N2 C10 C9 175.51(12) C8 C9 C10 N2 -0.4(2) C16 C11 C12 C17 61.15(16) Zn1 C11 C12 C17 -66.13(14) C16 C11 C12 C13 -58.66(16) Zn1 C11 C12 C13 174.06(10) C17 C12 C13 C14 -60.65(17) C11 C12 C13 C14 60.05(17) C12 C13 C14 C18 60.30(18) C12 C13 C14 C15 -59.20(18) C18 C14 C15 C16 -60.99(17) C13 C14 C15 C16 58.81(17) C14 C15 C16 C19 60.83(16) C14 C15 C16 C11 -59.58(17) C12 C11 C16 C15 58.51(16) Zn1 C11 C16 C15 -173.38(10) C12 C11 C16 C19 -61.38(15) Zn1 C11 C16 C19 66.73(14) C13 C12 C17 C20 61.09(16) C11 C12 C17 C20 -60.24(17) C15 C14 C18 C20 60.21(17) C13 C14 C18 C20 -59.64(17) C15 C16 C19 C20 -60.41(16) C11 C16 C19 C20 61.23(16) C16 C19 C20 C18 60.21(16) C16 C19 C20 C17 -59.25(16) C14 C18 C20 C19 -59.93(17) C14 C18 C20 C17 59.79(17) C12 C17 C20 C19 58.66(17) C12 C17 C20 C18 -60.92(16) C28 C21 C22 C30 -61.09(16) Zn1 C21 C22 C30 70.48(14) C28 C21 C22 C23 59.15(16) Zn1 C21 C22 C23 -169.28(10) C30 C22 C23 C24 60.41(17) C21 C22 C23 C24 -60.35(17) C22 C23 C24 C25 -60.16(17) C22 C23 C24 C29 59.03(18) C29 C24 C25 C26 -60.18(18) C23 C24 C25 C26 59.53(17) C24 C25 C26 C30 -59.58(17) C24 C25 C26 C27 60.13(18) C30 C26 C27 C28 59.15(17) C25 C26 C27 C28 -60.67(16) C26 C27 C28 C29 60.91(16) C26 C27 C28 C21 -60.76(16) C22 C21 C28 C27 61.05(16) Zn1 C21 C28 C27 -69.30(14) C22 C21 C28 C29 -58.81(16) Zn1 C21 C28 C29 170.84(10) C25 C24 C29 C28 61.11(17) C23 C24 C29 C28 -58.51(17) C27 C28 C29 C24 -61.40(16) C21 C28 C29 C24 59.52(16) C23 C22 C30 C26 -60.37(17) C21 C22 C30 C26 61.11(17) C25 C26 C30 C22 60.20(17) C27 C26 C30 C22 -59.44(17)