Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P. D. Beer' 'Andrew R. Cowley' 'David Curiel' 'Wallace Wong' _publ_contact_author_name 'Prof Paul Beer' _publ_contact_author_address ; Department of Chemistry University of Oxford Oxford OX13QR UNITED KINGDOM ; _publ_contact_author_email PAUL.BEER@CHEM.OX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Dinuclear Zinc(II) Dithiocarbamate Macrocycles: Ditopic Receptors for a Variety of Guest Molecules. ; data_receptor16_DABCO _database_code_depnum_ccdc_archive 'CCDC 252800' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _chemical_absolute_configuration ad _refine_special_details ; The diazabicyclononane bridge has been modelled as disordered over two positions related by an approximate centre of inversion. A common set of coordinates and anisotropic displacement parameters have been refined for the overlapping terminal N atoms (N3 and N8, N4 and N7) Similarity restraints were applied to the components of the anisotropic displacement parameters of directly-bonded pairs of disordered C and N atoms along the bonds ; #============================================================= _cell_length_a 21.7324(3) _cell_angle_alpha 90 _cell_length_b 7.2463(2) _cell_angle_beta 90 _cell_length_c 24.1595(4) _cell_angle_gamma 90 _cell_volume 3804.63(13) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y,z+1/2 x+1/2,-y,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C26 H52 N6 S8 Zn2 ' _chemical_formula_moiety ' C26 H52 N6 S8 Zn2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 836.03 _cell_measurement_reflns_used 27083 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1752. _exptl_absorpt_coefficient_mu 1.727 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.79 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 27083 _reflns_number_total 7927 # 8373 unique data including absences _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_min 5.158 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min 0 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min -31 _reflns_limit_l_max 31 _refine_diff_density_min -1.00 _refine_diff_density_max 1.48 _refine_ls_number_reflns 6946 _refine_ls_number_restraints 31 _refine_ls_number_parameters 435 #_refine_ls_R_factor_ref 0.0347 _refine_ls_wR_factor_ref 0.0365 _refine_ls_goodness_of_fit_ref 1.0987 #_reflns_number_all 7927 _refine_ls_R_factor_all 0.0425 _refine_ls_wR_factor_all 0.0438 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6946 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0365 _refine_ls_shift/su_max 0.018784 _refine_ls_abs_structure_Flack 0.486(10) _refine_ls_abs_structure_details 'Flack, 3512 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.496 0.0705 0.181 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group Zn1 Zn 0.571590(17) 0.55236(5) 0.24882(3) 0.0248 1.0000 Uani . . . . . S1 S 0.46307(4) 0.41730(12) 0.24114(5) 0.0305 1.0000 Uani . . . . . S2 S 0.50297(4) 0.77099(12) 0.28894(5) 0.0315 1.0000 Uani . . . . . C1 C 0.44325(16) 0.6268(5) 0.26920(15) 0.0266 1.0000 Uani . . . . . N1 N 0.38494(14) 0.6749(5) 0.27629(14) 0.0325 1.0000 Uani . . . . . C2 C 0.33429(18) 0.5524(6) 0.2589(2) 0.0404 1.0000 Uani . . . . . C3 C 0.3194(2) 0.5658(8) 0.1979(2) 0.0597 1.0000 Uani . . . . . C4 C 0.3664(2) 0.8488(6) 0.30342(18) 0.0409 1.0000 Uani . . . . . C5 C 0.3338(3) 0.9817(7) 0.2660(2) 0.0552 1.0000 Uani . . . . . S3 S 0.66461(5) 0.75861(13) 0.23221(5) 0.0345 1.0000 Uani . . . . . S4 S 0.60539(4) 0.48980(13) 0.15801(5) 0.0322 1.0000 Uani . . . . . C6 C 0.65885(15) 0.6635(5) 0.16722(15) 0.0246 1.0000 Uani . . . . . N2 N 0.69406(16) 0.7212(4) 0.12573(13) 0.0316 1.0000 Uani . . . . . C7 C 0.7371(2) 0.8771(6) 0.13338(18) 0.0447 1.0000 Uani . . . . . C8 C 0.7051(3) 1.0610(7) 0.1251(2) 0.0644 1.0000 Uani . . . . . C9 C 0.6901(2) 0.6492(6) 0.06891(16) 0.0383 1.0000 Uani . . . . . C10 C 0.7432(3) 0.5261(7) 0.0540(2) 0.0551 1.0000 Uani . . . . . N3 N 0.60816(13) 0.3728(4) 0.30995(12) 0.0226 0.520(8) Uani . U P . 1 C11 C 0.5605(4) 0.3305(17) 0.3535(4) 0.0577 0.520(8) Uani . U P . 1 C12 C 0.5886(4) 0.214(2) 0.4003(5) 0.0746 0.520(8) Uani . U P . 1 C13 C 0.6596(4) 0.4678(11) 0.3423(4) 0.0391 0.520(8) Uani . U P . 1 C14 C 0.6881(5) 0.3343(11) 0.3855(4) 0.0532 0.520(8) Uani . U P . 1 C15 C 0.6322(5) 0.2051(11) 0.2874(3) 0.0477 0.520(8) Uani . U P . 1 C16 C 0.6531(6) 0.0726(12) 0.3330(4) 0.0569 0.520(8) Uani . U P . 1 N4 N 0.65245(13) 0.1574(4) 0.38570(11) 0.0221 0.520(8) Uani . U P . 1 Zn2 Zn 0.688501(18) -0.02087(5) 0.44729(4) 0.0260 1.0000 Uani . . . . . S5 S 0.79746(4) 0.09403(13) 0.45881(5) 0.0321 1.0000 Uani . . . . . S6 S 0.75491(5) -0.24442(14) 0.40417(6) 0.0394 1.0000 Uani . . . . . C17 C 0.81544(17) -0.1079(5) 0.42524(15) 0.0285 1.0000 Uani . . . . . N5 N 0.87343(15) -0.1571(5) 0.41694(14) 0.0334 1.0000 Uani . . . . . C18 C 0.92532(17) -0.0411(6) 0.4358(2) 0.0414 1.0000 Uani . . . . . C19 C 0.9431(3) -0.0751(8) 0.4949(3) 0.0637 1.0000 Uani . . . . . C20 C 0.8898(2) -0.3291(7) 0.3872(2) 0.0500 1.0000 Uani . . . . . C21 C 0.9160(3) -0.4778(7) 0.4225(3) 0.0703 1.0000 Uani . . . . . S7 S 0.59624(6) -0.23315(15) 0.46296(6) 0.0490 1.0000 Uani . . . . . S8 S 0.64739(4) 0.05811(15) 0.53496(5) 0.0353 1.0000 Uani . . . . . C22 C 0.59797(18) -0.1259(5) 0.52718(16) 0.0326 1.0000 Uani . . . . . N6 N 0.56214(18) -0.1828(5) 0.56831(15) 0.0406 1.0000 Uani . . . . . C23 C 0.5185(3) -0.3431(8) 0.5601(2) 0.0642 1.0000 Uani . . . . . C24 C 0.5481(4) -0.5200(9) 0.5736(3) 0.0856 1.0000 Uani . . . . . C25 C 0.5639(3) -0.0994(8) 0.62377(18) 0.0543 1.0000 Uani . . . . . C26 C 0.5058(4) -0.0054(11) 0.6384(3) 0.0812 1.0000 Uani . . . . . N7 N 0.65245(13) 0.1574(4) 0.38570(11) 0.0221 0.480(8) Uani . U P . 2 C27 C 0.7003(4) 0.2055(18) 0.3420(4) 0.0570 0.480(8) Uani . U P . 2 C28 C 0.6727(5) 0.328(2) 0.2968(5) 0.0747 0.480(8) Uani . U P . 2 C29 C 0.6031(5) 0.0594(13) 0.3530(4) 0.0457 0.480(8) Uani . U P . 2 C30 C 0.5742(5) 0.1928(13) 0.3094(5) 0.0555 0.480(8) Uani . U P . 2 C31 C 0.6277(6) 0.3187(13) 0.4073(4) 0.0466 0.480(8) Uani . U P . 2 C32 C 0.6039(7) 0.4557(14) 0.3615(4) 0.0586 0.480(8) Uani . U P . 2 N8 N 0.60816(13) 0.3728(4) 0.30995(12) 0.0226 0.480(8) Uani . U P . 2 H21 H 0.3462 0.4221 0.2674 0.0484 1.0000 Uiso . . . . . H22 H 0.2966 0.5858 0.2805 0.0484 1.0000 Uiso . . . . . H31 H 0.2848 0.4797 0.1889 0.0716 1.0000 Uiso . . . . . H32 H 0.3565 0.5314 0.1757 0.0716 1.0000 Uiso . . . . . H33 H 0.3069 0.6951 0.1888 0.0716 1.0000 Uiso . . . . . H41 H 0.4042 0.9105 0.3180 0.0490 1.0000 Uiso . . . . . H42 H 0.3383 0.8180 0.3349 0.0490 1.0000 Uiso . . . . . H51 H 0.3228 1.0955 0.2873 0.0663 1.0000 Uiso . . . . . H52 H 0.3614 1.0155 0.2345 0.0663 1.0000 Uiso . . . . . H53 H 0.2955 0.9230 0.2514 0.0663 1.0000 Uiso . . . . . H71 H 0.7713 0.8659 0.1059 0.0536 1.0000 Uiso . . . . . H72 H 0.7543 0.8721 0.1717 0.0536 1.0000 Uiso . . . . . H81 H 0.7353 1.1634 0.1306 0.0773 1.0000 Uiso . . . . . H82 H 0.6879 1.0673 0.0868 0.0773 1.0000 Uiso . . . . . H83 H 0.6709 1.0735 0.1526 0.0773 1.0000 Uiso . . . . . H91 H 0.6893 0.7558 0.0426 0.0460 1.0000 Uiso . . . . . H92 H 0.6511 0.5770 0.0652 0.0460 1.0000 Uiso . . . . . H101 H 0.7381 0.4813 0.0151 0.0662 1.0000 Uiso . . . . . H102 H 0.7825 0.5970 0.0572 0.0662 1.0000 Uiso . . . . . H103 H 0.7443 0.4181 0.0798 0.0662 1.0000 Uiso . . . . . H111 H 0.5446 0.4489 0.3693 0.0692 0.5203 Uiso . . . . 1 H112 H 0.5258 0.2604 0.3363 0.0692 0.5203 Uiso . . . . 1 H121 H 0.5896 0.2891 0.4351 0.0895 0.5203 Uiso . . . . 1 H122 H 0.5629 0.1017 0.4062 0.0895 0.5203 Uiso . . . . 1 H131 H 0.6924 0.5085 0.3159 0.0469 0.5203 Uiso . . . . 1 H132 H 0.6424 0.5778 0.3619 0.0469 0.5203 Uiso . . . . 1 H141 H 0.7320 0.3085 0.3755 0.0638 0.5203 Uiso . . . . 1 H142 H 0.6864 0.3919 0.4231 0.0638 0.5203 Uiso . . . . 1 H151 H 0.6682 0.2349 0.2632 0.0572 0.5203 Uiso . . . . 1 H152 H 0.5995 0.1438 0.2648 0.0572 0.5203 Uiso . . . . 1 H161 H 0.6959 0.0302 0.3247 0.0682 0.5203 Uiso . . . . 1 H162 H 0.6248 -0.0361 0.3337 0.0682 0.5203 Uiso . . . . 1 H181 H 0.9618 -0.0673 0.4117 0.0496 1.0000 Uiso . . . . . H182 H 0.9133 0.0915 0.4318 0.0496 1.0000 Uiso . . . . . H191 H 0.9783 0.0071 0.5051 0.0765 1.0000 Uiso . . . . . H192 H 0.9557 -0.2070 0.4995 0.0765 1.0000 Uiso . . . . . H193 H 0.9072 -0.0482 0.5195 0.0765 1.0000 Uiso . . . . . H201 H 0.9208 -0.2975 0.3581 0.0600 1.0000 Uiso . . . . . H202 H 0.8517 -0.3779 0.3692 0.0600 1.0000 Uiso . . . . . H211 H 0.9257 -0.5879 0.3991 0.0844 1.0000 Uiso . . . . . H212 H 0.9546 -0.4325 0.4405 0.0844 1.0000 Uiso . . . . . H213 H 0.8855 -0.5130 0.4516 0.0844 1.0000 Uiso . . . . . H231 H 0.4819 -0.3258 0.5845 0.0770 1.0000 Uiso . . . . . H232 H 0.5050 -0.3457 0.5205 0.0770 1.0000 Uiso . . . . . H241 H 0.5181 -0.6228 0.5677 0.1027 1.0000 Uiso . . . . . H242 H 0.5615 -0.5188 0.6132 0.1027 1.0000 Uiso . . . . . H243 H 0.5846 -0.5387 0.5491 0.1027 1.0000 Uiso . . . . . H251 H 0.5718 -0.1988 0.6516 0.0651 1.0000 Uiso . . . . . H252 H 0.5981 -0.0071 0.6250 0.0651 1.0000 Uiso . . . . . H261 H 0.5094 0.0487 0.6764 0.0974 1.0000 Uiso . . . . . H262 H 0.4712 -0.0964 0.6377 0.0974 1.0000 Uiso . . . . . H263 H 0.4975 0.0953 0.6111 0.0974 1.0000 Uiso . . . . . H271 H 0.7351 0.2727 0.3600 0.0684 0.4797 Uiso . . . . 2 H272 H 0.7159 0.0890 0.3249 0.0684 0.4797 Uiso . . . . 2 H281 H 0.6970 0.4443 0.2941 0.0897 0.4797 Uiso . . . . 2 H282 H 0.6743 0.2607 0.2607 0.0897 0.4797 Uiso . . . . 2 H291 H 0.6216 -0.0489 0.3335 0.0549 0.4797 Uiso . . . . 2 H292 H 0.5702 0.0157 0.3788 0.0549 0.4797 Uiso . . . . 2 H301 H 0.5772 0.1361 0.2718 0.0667 0.4797 Uiso . . . . 2 H302 H 0.5300 0.2147 0.3187 0.0667 0.4797 Uiso . . . . 2 H311 H 0.6601 0.3825 0.4295 0.0559 0.4797 Uiso . . . . 2 H312 H 0.5924 0.2855 0.4319 0.0559 0.4797 Uiso . . . . 2 H321 H 0.6295 0.5703 0.3620 0.0703 0.4797 Uiso . . . . 2 H322 H 0.5600 0.4884 0.3692 0.0703 0.4797 Uiso . . . . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02351(17) 0.02915(18) 0.02162(19) 0.00244(16) 0.00065(17) 0.00164(15) S1 0.0247(4) 0.0331(4) 0.0336(5) -0.0063(4) -0.0030(4) 0.0005(3) S2 0.0275(4) 0.0298(4) 0.0371(5) -0.0051(4) -0.0036(4) 0.0006(3) C1 0.0272(18) 0.0310(17) 0.0217(16) 0.0013(13) 0.0003(13) 0.0019(14) N1 0.0237(15) 0.0394(17) 0.0343(18) -0.0039(14) -0.0013(13) 0.0016(13) C2 0.0227(16) 0.048(2) 0.050(3) -0.0053(19) -0.0026(19) -0.0009(16) C3 0.046(3) 0.069(3) 0.064(4) -0.013(3) -0.027(2) 0.003(3) C4 0.034(2) 0.049(2) 0.040(2) -0.0106(18) 0.0023(17) 0.0118(18) C5 0.063(3) 0.040(2) 0.063(4) 0.002(2) 0.004(3) 0.008(2) S3 0.0400(5) 0.0392(5) 0.0243(4) -0.0026(3) 0.0015(4) -0.0166(4) S4 0.0325(4) 0.0387(5) 0.0255(5) -0.0036(4) 0.0007(4) -0.0134(4) C6 0.0205(16) 0.0281(16) 0.0252(17) 0.0046(13) -0.0007(13) -0.0017(13) N2 0.0364(18) 0.0343(16) 0.0242(15) 0.0030(12) -0.0016(13) -0.0081(13) C7 0.050(3) 0.048(2) 0.036(2) 0.0041(18) 0.0073(19) -0.026(2) C8 0.108(5) 0.042(3) 0.043(3) 0.006(2) 0.003(3) -0.029(3) C9 0.048(2) 0.048(2) 0.0186(17) 0.0018(16) 0.0022(17) -0.0114(19) C10 0.085(4) 0.046(3) 0.035(3) 0.0039(19) 0.014(3) 0.005(2) N3 0.0181(13) 0.0252(13) 0.0246(14) 0.0036(11) 0.0001(11) 0.0017(10) C11 0.021(3) 0.103(8) 0.050(5) 0.045(5) 0.011(3) 0.022(4) C12 0.028(3) 0.133(11) 0.063(6) 0.060(6) 0.016(4) 0.039(5) C13 0.041(4) 0.032(4) 0.044(5) 0.007(3) -0.025(3) -0.003(3) C14 0.066(6) 0.030(3) 0.063(6) 0.024(3) -0.034(5) -0.017(3) C15 0.092(8) 0.034(4) 0.017(3) -0.005(2) -0.015(4) 0.024(4) C16 0.115(10) 0.031(4) 0.024(3) 0.002(2) -0.017(4) 0.016(5) N4 0.0177(13) 0.0256(14) 0.0229(14) 0.0047(10) 0.0002(10) 0.0000(10) Zn2 0.02495(17) 0.02989(19) 0.02326(19) 0.00444(18) 0.00239(17) 0.00231(15) S5 0.0246(4) 0.0355(4) 0.0363(5) -0.0039(4) 0.0000(4) 0.0019(3) S6 0.0317(5) 0.0346(5) 0.0519(6) -0.0076(4) -0.0095(5) 0.0032(4) C17 0.0267(18) 0.0358(19) 0.0228(17) 0.0060(14) -0.0025(14) 0.0018(14) N5 0.0283(16) 0.0418(18) 0.0301(17) -0.0039(13) 0.0013(13) 0.0096(14) C18 0.0207(17) 0.048(2) 0.055(3) 0.0007(19) 0.0061(18) 0.0001(16) C19 0.058(3) 0.063(3) 0.070(4) 0.007(3) -0.027(3) -0.014(3) C20 0.039(2) 0.060(3) 0.051(3) -0.021(2) 0.002(2) 0.011(2) C21 0.096(5) 0.039(3) 0.075(4) -0.004(3) 0.029(3) 0.009(3) S7 0.0658(8) 0.0409(5) 0.0403(6) -0.0068(4) 0.0227(5) -0.0152(5) S8 0.0288(5) 0.0531(6) 0.0240(5) 0.0012(4) -0.0002(4) -0.0086(4) C22 0.034(2) 0.0346(19) 0.0289(19) 0.0084(15) 0.0047(16) 0.0039(15) N6 0.051(2) 0.0401(18) 0.0309(18) 0.0077(14) 0.0133(16) -0.0036(16) C23 0.076(4) 0.059(3) 0.058(3) 0.009(2) 0.040(3) -0.012(3) C24 0.121(6) 0.063(4) 0.073(5) 0.017(3) -0.005(4) -0.015(4) C25 0.063(3) 0.077(3) 0.022(2) 0.006(2) 0.009(2) -0.011(3) C26 0.099(5) 0.094(5) 0.051(4) -0.021(3) 0.014(3) 0.019(4) N7 0.0177(13) 0.0256(14) 0.0229(14) 0.0047(10) 0.0002(10) 0.0000(10) C27 0.023(4) 0.099(9) 0.049(6) 0.045(5) 0.012(3) 0.014(4) C28 0.032(3) 0.118(11) 0.075(7) 0.073(7) 0.031(5) 0.033(5) C29 0.052(5) 0.036(4) 0.049(6) 0.016(3) -0.029(4) -0.017(4) C30 0.060(6) 0.031(4) 0.076(8) 0.016(4) -0.047(6) -0.014(4) C31 0.072(8) 0.042(4) 0.026(4) -0.003(3) -0.009(4) 0.027(4) C32 0.100(10) 0.047(5) 0.029(3) -0.010(3) -0.028(5) 0.034(6) N8 0.0181(13) 0.0252(13) 0.0246(14) 0.0036(11) 0.0001(11) 0.0017(10) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . S1 . 2.5602(9) yes Zn1 . S2 . 2.3819(10) yes Zn1 . S3 . 2.5458(10) yes Zn1 . S4 . 2.3576(11) yes Zn1 . N3 . 2.123(3) yes Zn1 . N8 . 2.123(3) yes S1 . C1 . 1.717(4) yes S2 . C1 . 1.733(4) yes C1 . N1 . 1.326(5) yes N1 . C2 . 1.475(5) yes N1 . C4 . 1.477(5) yes C2 . C3 . 1.513(7) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . C5 . 1.499(7) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no S3 . C6 . 1.719(4) yes S4 . C6 . 1.727(3) yes C6 . N2 . 1.329(5) yes N2 . C7 . 1.478(5) yes N2 . C9 . 1.471(5) yes C7 . C8 . 1.516(8) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C9 . C10 . 1.503(7) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no N3 . C11 . 1.509(8) yes N3 . C13 . 1.528(8) yes N3 . C15 . 1.431(8) yes C11 . C12 . 1.536(12) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C12 . N4 . 1.489(9) yes C12 . H121 . 1.000 no C12 . H122 . 1.000 no C13 . C14 . 1.552(10) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . N4 . 1.498(8) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.531(11) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . N4 . 1.413(9) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no N4 . Zn2 . 2.121(3) yes Zn2 . S5 . 2.5255(10) yes Zn2 . S6 . 2.4066(11) yes Zn2 . S7 . 2.5553(12) yes Zn2 . S8 . 2.3690(11) yes Zn2 . N7 . 2.121(3) yes S5 . C17 . 1.718(4) yes S6 . C17 . 1.723(4) yes C17 . N5 . 1.325(5) yes N5 . C18 . 1.478(5) yes N5 . C20 . 1.482(5) yes C18 . C19 . 1.500(8) yes C18 . H181 . 1.000 no C18 . H182 . 1.000 no C19 . H191 . 1.000 no C19 . H192 . 1.000 no C19 . H193 . 1.000 no C20 . C21 . 1.489(8) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no S7 . C22 . 1.736(4) yes S8 . C22 . 1.722(4) yes C22 . N6 . 1.328(5) yes N6 . C23 . 1.512(7) yes N6 . C25 . 1.470(6) yes C23 . C24 . 1.470(9) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . C26 . 1.477(9) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no N7 . C27 . 1.522(9) yes N7 . C29 . 1.510(9) yes N7 . C31 . 1.389(9) yes C27 . C28 . 1.527(12) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . N8 . 1.474(9) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . C30 . 1.560(12) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C30 . N8 . 1.499(9) yes C30 . H301 . 1.000 no C30 . H302 . 1.000 no C31 . C32 . 1.573(12) yes C31 . H311 . 1.000 no C31 . H312 . 1.000 no C32 . N8 . 1.387(10) yes C32 . H321 . 1.000 no C32 . H322 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Zn1 . S2 . 72.96(3) yes S1 . Zn1 . S3 . 160.82(4) yes S2 . Zn1 . S3 . 99.84(4) yes S1 . Zn1 . S4 . 98.40(3) yes S2 . Zn1 . S4 . 134.56(4) yes S3 . Zn1 . S4 . 73.67(3) yes S1 . Zn1 . N3 . 99.26(8) yes S2 . Zn1 . N3 . 111.04(8) yes S3 . Zn1 . N3 . 99.92(8) yes S4 . Zn1 . N3 . 114.39(8) yes S1 . Zn1 . N8 . 99.26(8) yes S2 . Zn1 . N8 . 111.04(8) yes S3 . Zn1 . N8 . 99.92(8) yes S4 . Zn1 . N8 . 114.39(8) yes Zn1 . S1 . C1 . 82.22(13) yes Zn1 . S2 . C1 . 87.46(12) yes S1 . C1 . S2 . 117.0(2) yes S1 . C1 . N1 . 121.6(3) yes S2 . C1 . N1 . 121.4(3) yes C1 . N1 . C2 . 121.2(3) yes C1 . N1 . C4 . 122.9(3) yes C2 . N1 . C4 . 115.9(3) yes N1 . C2 . C3 . 113.5(4) yes N1 . C2 . H21 . 108.456 no C3 . C2 . H21 . 108.456 no N1 . C2 . H22 . 108.454 no C3 . C2 . H22 . 108.455 no H21 . C2 . H22 . 109.466 no C2 . C3 . H31 . 109.467 no C2 . C3 . H32 . 109.467 no H31 . C3 . H32 . 109.475 no C2 . C3 . H33 . 109.467 no H31 . C3 . H33 . 109.474 no H32 . C3 . H33 . 109.476 no N1 . C4 . C5 . 114.2(4) yes N1 . C4 . H41 . 108.276 no C5 . C4 . H41 . 108.277 no N1 . C4 . H42 . 108.276 no C5 . C4 . H42 . 108.275 no H41 . C4 . H42 . 109.467 no C4 . C5 . H51 . 109.465 no C4 . C5 . H52 . 109.464 no H51 . C5 . H52 . 109.476 no C4 . C5 . H53 . 109.467 no H51 . C5 . H53 . 109.478 no H52 . C5 . H53 . 109.477 no Zn1 . S3 . C6 . 81.42(12) yes Zn1 . S4 . C6 . 87.11(12) yes S3 . C6 . S4 . 117.3(2) yes S3 . C6 . N2 . 121.4(3) yes S4 . C6 . N2 . 121.3(3) yes C6 . N2 . C7 . 120.7(3) yes C6 . N2 . C9 . 123.9(3) yes C7 . N2 . C9 . 115.2(3) yes N2 . C7 . C8 . 111.4(4) yes N2 . C7 . H71 . 108.990 no C8 . C7 . H71 . 108.988 no N2 . C7 . H72 . 108.989 no C8 . C7 . H72 . 108.988 no H71 . C7 . H72 . 109.466 no C7 . C8 . H81 . 109.468 no C7 . C8 . H82 . 109.467 no H81 . C8 . H82 . 109.477 no C7 . C8 . H83 . 109.466 no H81 . C8 . H83 . 109.474 no H82 . C8 . H83 . 109.475 no N2 . C9 . C10 . 112.9(4) yes N2 . C9 . H91 . 108.610 no C10 . C9 . H91 . 108.610 no N2 . C9 . H92 . 108.608 no C10 . C9 . H92 . 108.609 no H91 . C9 . H92 . 109.466 no C9 . C10 . H101 . 109.464 no C9 . C10 . H102 . 109.466 no H101 . C10 . H102 . 109.476 no C9 . C10 . H103 . 109.467 no H101 . C10 . H103 . 109.475 no H102 . C10 . H103 . 109.479 no Zn1 . N3 . C11 . 110.7(3) yes Zn1 . N3 . C13 . 110.7(3) yes C11 . N3 . C13 . 103.7(6) yes Zn1 . N3 . C15 . 113.1(3) yes C11 . N3 . C15 . 110.2(7) yes C13 . N3 . C15 . 108.1(6) yes N3 . C11 . C12 . 110.6(6) yes N3 . C11 . H111 . 109.192 no C12 . C11 . H111 . 109.187 no N3 . C11 . H112 . 109.193 no C12 . C11 . H112 . 109.199 no H111 . C11 . H112 . 109.467 no C11 . C12 . N4 . 110.4(7) yes C11 . C12 . H121 . 109.258 no N4 . C12 . H121 . 109.256 no C11 . C12 . H122 . 109.241 no N4 . C12 . H122 . 109.239 no N3 . C13 . C14 . 110.8(6) yes N3 . C13 . H131 . 109.136 no C14 . C13 . H131 . 109.140 no N3 . C13 . H132 . 109.135 no C14 . C13 . H132 . 109.140 no H131 . C13 . H132 . 109.466 no C13 . C14 . N4 . 109.2(6) yes C13 . C14 . H141 . 109.542 no N4 . C14 . H141 . 109.545 no C13 . C14 . H142 . 109.541 no N4 . C14 . H142 . 109.544 no N7 . C14 . H142 . 109.544 no H141 . C14 . H142 . 109.467 no N3 . C15 . C16 . 111.4(6) yes N3 . C15 . H151 . 108.975 no C16 . C15 . H151 . 108.979 no N3 . C15 . H152 . 108.978 no C16 . C15 . H152 . 108.976 no H151 . C15 . H152 . 109.468 no C15 . C16 . N4 . 111.9(6) yes C15 . C16 . H161 . 108.848 no N4 . C16 . H161 . 108.848 no C15 . C16 . H162 . 108.856 no N4 . C16 . H162 . 108.858 no H161 . C16 . H162 . 109.468 no C12 . N4 . C14 . 104.2(8) yes C12 . N4 . C16 . 110.0(8) yes C14 . N4 . C16 . 111.4(7) yes C12 . N4 . Zn2 . 110.3(4) yes C14 . N4 . Zn2 . 109.4(4) yes C16 . N4 . Zn2 . 111.3(4) yes N4 . Zn2 . S5 . 102.88(8) yes N4 . Zn2 . S6 . 109.15(9) yes S5 . Zn2 . S6 . 72.98(3) yes N4 . Zn2 . S7 . 100.42(8) yes S5 . Zn2 . S7 . 156.61(4) yes S6 . Zn2 . S7 . 97.44(4) yes N4 . Zn2 . S8 . 109.93(8) yes S5 . Zn2 . S8 . 100.10(4) yes S6 . Zn2 . S8 . 140.87(4) yes S7 . Zn2 . S8 . 73.57(4) yes S5 . Zn2 . N7 . 102.88(8) yes S6 . Zn2 . N7 . 109.15(9) yes S7 . Zn2 . N7 . 100.42(8) yes S8 . Zn2 . N7 . 109.93(8) yes Zn2 . S5 . C17 . 83.13(13) yes Zn2 . S6 . C17 . 86.76(13) yes S5 . C17 . S6 . 117.1(2) yes S5 . C17 . N5 . 121.1(3) yes S6 . C17 . N5 . 121.8(3) yes C17 . N5 . C18 . 121.7(3) yes C17 . N5 . C20 . 121.9(4) yes C18 . N5 . C20 . 116.4(3) yes N5 . C18 . C19 . 113.3(4) yes N5 . C18 . H181 . 108.500 no C19 . C18 . H181 . 108.500 no N5 . C18 . H182 . 108.500 no C19 . C18 . H182 . 108.500 no H181 . C18 . H182 . 109.468 no C18 . C19 . H191 . 109.468 no C18 . C19 . H192 . 109.466 no H191 . C19 . H192 . 109.477 no C18 . C19 . H193 . 109.466 no H191 . C19 . H193 . 109.477 no H192 . C19 . H193 . 109.474 no N5 . C20 . C21 . 115.0(4) yes N5 . C20 . H201 . 108.073 no C21 . C20 . H201 . 108.075 no N5 . C20 . H202 . 108.073 no C21 . C20 . H202 . 108.072 no H201 . C20 . H202 . 109.467 no C20 . C21 . H211 . 109.468 no C20 . C21 . H212 . 109.467 no H211 . C21 . H212 . 109.473 no C20 . C21 . H213 . 109.470 no H211 . C21 . H213 . 109.476 no H212 . C21 . H213 . 109.474 no Zn2 . S7 . C22 . 81.13(13) yes Zn2 . S8 . C22 . 87.17(14) yes S7 . C22 . S8 . 117.2(2) yes S7 . C22 . N6 . 121.1(3) yes S8 . C22 . N6 . 121.6(3) yes C22 . N6 . C23 . 120.5(4) yes C22 . N6 . C25 . 122.6(4) yes C23 . N6 . C25 . 116.9(4) yes N6 . C23 . C24 . 111.5(6) yes N6 . C23 . H231 . 108.955 no C24 . C23 . H231 . 108.957 no N6 . C23 . H232 . 108.956 no C24 . C23 . H232 . 108.956 no H231 . C23 . H232 . 109.467 no C23 . C24 . H241 . 109.465 no C23 . C24 . H242 . 109.464 no H241 . C24 . H242 . 109.477 no C23 . C24 . H243 . 109.465 no H241 . C24 . H243 . 109.480 no H242 . C24 . H243 . 109.477 no N6 . C25 . C26 . 112.7(5) yes N6 . C25 . H251 . 108.654 no C26 . C25 . H251 . 108.651 no N6 . C25 . H252 . 108.653 no C26 . C25 . H252 . 108.647 no H251 . C25 . H252 . 109.467 no C25 . C26 . H261 . 109.474 no C25 . C26 . H262 . 109.464 no H261 . C26 . H262 . 109.473 no C25 . C26 . H263 . 109.470 no H261 . C26 . H263 . 109.479 no H262 . C26 . H263 . 109.467 no Zn2 . N7 . C27 . 112.0(4) yes Zn2 . N7 . C29 . 110.1(4) yes C27 . N7 . C29 . 103.3(7) yes Zn2 . N7 . C31 . 113.1(4) yes C27 . N7 . C31 . 109.4(7) yes C29 . N7 . C31 . 108.5(7) yes N7 . C27 . C28 . 111.1(6) yes N7 . C27 . H271 . 109.063 no C28 . C27 . H271 . 109.065 no N7 . C27 . H272 . 109.068 no C28 . C27 . H272 . 109.067 no H271 . C27 . H272 . 109.468 no C27 . C28 . N8 . 110.4(7) yes C27 . C28 . H281 . 109.236 no N8 . C28 . H281 . 109.235 no N3 . C28 . H282 . 109.240 no C27 . C28 . H282 . 109.238 no N8 . C28 . H282 . 109.240 no H281 . C28 . H282 . 109.467 no N7 . C29 . C30 . 110.3(6) yes N7 . C29 . H291 . 109.257 no C30 . C29 . H291 . 109.259 no N7 . C29 . H292 . 109.262 no C30 . C29 . H292 . 109.255 no H291 . C29 . H292 . 109.467 no C29 . C30 . N8 . 109.6(6) yes C29 . C30 . H301 . 109.438 no N8 . C30 . H301 . 109.436 no C29 . C30 . H302 . 109.447 no N8 . C30 . H302 . 109.449 no H301 . C30 . H302 . 109.466 no N7 . C31 . C32 . 113.2(7) yes N7 . C31 . H311 . 108.524 no C32 . C31 . H311 . 108.524 no N7 . C31 . H312 . 108.520 no C32 . C31 . H312 . 108.517 no H311 . C31 . H312 . 109.465 no C31 . C32 . N8 . 109.6(7) yes C31 . C32 . H321 . 109.429 no N8 . C32 . H321 . 109.431 no C31 . C32 . H322 . 109.436 no N8 . C32 . H322 . 109.436 no H321 . C32 . H322 . 109.466 no Zn1 . N8 . C28 . 110.0(4) yes Zn1 . N8 . C30 . 110.1(4) yes C28 . N8 . C30 . 105.8(8) yes Zn1 . N8 . C32 . 109.5(4) yes C28 . N8 . C32 . 110.7(9) yes C30 . N8 . C32 . 110.6(8) yes #===END data_receptor12_DABCO _database_code_depnum_ccdc_archive 'CCDC 252801' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_special_details ; The diazabicyclononane bridge is disordered over two positions related by a centre of inversion. The coordinates and adps of the terminal N atoms have been constrained to be related by this symmetry element The structure contains a small void centred on the point 0, 0.5, 0.5 and the largest residual electron density peak of a difference Fourier map occurs within this region. However, no clearly-defined atomic positions are present and accordingly no attempt to model disordered solvent in this void has been made ; #============================================================= _cell_length_a 11.6711(4) _cell_angle_alpha 110.2029(15) _cell_length_b 11.9793(4) _cell_angle_beta 100.1626(15) _cell_length_c 12.4675(4) _cell_angle_gamma 115.6632(17) _cell_volume 1360.59(9) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C50 H68 N6 S8 Zn2 ' _chemical_formula_moiety ' C50 H68 N6 S8 Zn2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1140.42 _cell_measurement_reflns_used 16123 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 1.228 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.93 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 16123 _reflns_number_total 6073 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_min 5.121 _diffrn_reflns_theta_max 27.410 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.410 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.54 _refine_diff_density_max 1.62 _refine_ls_number_reflns 4191 _refine_ls_number_restraints 0 _refine_ls_number_parameters 325 #_refine_ls_R_factor_ref 0.0441 _refine_ls_wR_factor_ref 0.0509 _refine_ls_goodness_of_fit_ref 1.0956 #_reflns_number_all 6073 _refine_ls_R_factor_all 0.0706 _refine_ls_wR_factor_all 0.0585 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4191 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_gt 0.0509 _refine_ls_shift/su_max 0.003839 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.18 0.382 0.817 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_disorder_group Zn1 Zn 0.17620(4) 0.19475(4) 0.34593(3) 0.0283 1.0000 Uani . S1 S 0.16159(9) 0.14266(9) 0.13256(7) 0.0342 1.0000 Uani . S2 S 0.02525(8) 0.26143(10) 0.26628(8) 0.0362 1.0000 Uani . C1 C 0.0741(3) 0.2274(3) 0.1411(3) 0.0269 1.0000 Uani . N1 N 0.0455(3) 0.2667(3) 0.0568(2) 0.0282 1.0000 Uani . C2 C 0.0894(3) 0.2401(3) -0.0493(3) 0.0303 1.0000 Uani . C3 C 0.1991(3) 0.3755(3) -0.0404(3) 0.0283 1.0000 Uani . C4 C 0.3190(3) 0.4710(3) 0.0628(3) 0.0302 1.0000 Uani . C5 C 0.4255(3) 0.5929(3) 0.0684(3) 0.0270 1.0000 Uani . C6 C 0.5504(3) 0.6921(3) 0.1739(3) 0.0292 1.0000 Uani . C7 C 0.6531(3) 0.8087(3) 0.1777(3) 0.0279 1.0000 Uani . C8 C 0.6340(3) 0.8295(4) 0.0723(3) 0.0320 1.0000 Uani . C9 C 0.5148(4) 0.7353(4) -0.0317(3) 0.0347 1.0000 Uani . C10 C 0.4071(3) 0.6154(3) -0.0361(3) 0.0294 1.0000 Uani . C11 C 0.2822(4) 0.5159(4) -0.1418(3) 0.0352 1.0000 Uani . C12 C 0.1813(3) 0.4001(4) -0.1433(3) 0.0344 1.0000 Uani . C13 C 0.7881(3) 0.9126(3) 0.2889(3) 0.0305 1.0000 Uani . C14 C -0.0262(3) 0.3422(4) 0.0627(3) 0.0342 1.0000 Uani . C15 C -0.1693(4) 0.2538(4) -0.0409(3) 0.0364 1.0000 Uani . C16 C -0.2704(4) 0.1268(4) -0.0336(4) 0.0445 1.0000 Uani . C17 C -0.4075(4) 0.0352(5) -0.1447(4) 0.0578 1.0000 Uani . S3 S 0.21656(10) 0.02254(9) 0.37052(8) 0.0379 1.0000 Uani . S4 S 0.13026(8) 0.18682(9) 0.53198(8) 0.0312 1.0000 Uani . C18 C 0.1955(3) 0.0805(3) 0.5088(3) 0.0261 1.0000 Uani . N2 N 0.2318(3) 0.0456(3) 0.5939(2) 0.0295 1.0000 Uani . C19 C 0.2888(4) -0.0446(4) 0.5727(3) 0.0413 1.0000 Uani . C20 C 0.1802(5) -0.1998(5) 0.5049(5) 0.0557 1.0000 Uani . C21 C 0.2437(7) -0.2885(6) 0.4637(6) 0.0811 1.0000 Uani . C22 C 0.2894(8) -0.2795(7) 0.3556(6) 0.0908 1.0000 Uani . N3 N 0.3786(3) 0.3846(3) 0.4423(2) 0.0273 0.5000 Uani -1 C23 C 0.4812(7) 0.3619(7) 0.4948(8) 0.0427 0.5000 Uani -1 C24 C 0.6245(7) 0.5000(7) 0.5655(9) 0.0498 0.5000 Uani -1 C25 C 0.3784(7) 0.4973(7) 0.5524(7) 0.0359 0.5000 Uani -1 C26 C 0.5215(7) 0.6335(7) 0.6174(7) 0.0437 0.5000 Uani -1 C27 C 0.4151(8) 0.4472(9) 0.3619(7) 0.0478 0.5000 Uani -1 C28 C 0.5596(8) 0.5801(9) 0.4285(7) 0.0572 0.5000 Uani -1 N4 N 0.6214(3) 0.6154(3) 0.5577(2) 0.0273 0.5000 Uani -1 H21 H 0.0074 0.1902 -0.1277 0.0318 1.0000 Uiso . H22 H 0.1274 0.1793 -0.0508 0.0318 1.0000 Uiso . H41 H 0.3315 0.4542 0.1360 0.0335 1.0000 Uiso . H61 H 0.5638 0.6764 0.2477 0.0335 1.0000 Uiso . H81 H 0.7084 0.9140 0.0737 0.0400 1.0000 Uiso . H91 H 0.5039 0.7516 -0.1054 0.0425 1.0000 Uiso . H111 H 0.2679 0.5306 -0.2161 0.0421 1.0000 Uiso . H121 H 0.0936 0.3319 -0.2183 0.0362 1.0000 Uiso . H131 H 0.8395 0.9986 0.2800 0.0340 1.0000 Uiso . H132 H 0.8434 0.8683 0.2911 0.0340 1.0000 Uiso . H141 H 0.0307 0.4287 0.0563 0.0396 1.0000 Uiso . H142 H -0.0364 0.3699 0.1442 0.0396 1.0000 Uiso . H151 H -0.2074 0.3150 -0.0364 0.0454 1.0000 Uiso . H152 H -0.1595 0.2203 -0.1222 0.0454 1.0000 Uiso . H161 H -0.2876 0.1599 0.0437 0.0508 1.0000 Uiso . H162 H -0.2296 0.0692 -0.0310 0.0508 1.0000 Uiso . H171 H -0.4713 -0.0473 -0.1366 0.0593 1.0000 Uiso . H172 H -0.4494 0.0918 -0.1478 0.0593 1.0000 Uiso . H173 H -0.3915 0.0011 -0.2226 0.0593 1.0000 Uiso . H191 H 0.3487 -0.0217 0.6548 0.0518 1.0000 Uiso . H192 H 0.3456 -0.0236 0.5227 0.0518 1.0000 Uiso . H201 H 0.1351 -0.2255 0.5610 0.0679 1.0000 Uiso . H202 H 0.1097 -0.2206 0.4301 0.0679 1.0000 Uiso . H211 H 0.3260 -0.2540 0.5360 0.1022 1.0000 Uiso . H212 H 0.1737 -0.3891 0.4361 0.1022 1.0000 Uiso . H221 H 0.3296 -0.3387 0.3328 0.1188 1.0000 Uiso . H222 H 0.3602 -0.1795 0.3823 0.1188 1.0000 Uiso . H223 H 0.2078 -0.3146 0.2823 0.1188 1.0000 Uiso . H231 H 0.4551 0.3256 0.5534 0.0396 0.5000 Uiso -1 H232 H 0.4855 0.2909 0.4267 0.0396 0.5000 Uiso -1 H241 H 0.6571 0.5235 0.6546 0.0489 0.5000 Uiso -1 H242 H 0.6900 0.4856 0.5293 0.0489 0.5000 Uiso -1 H251 H 0.3562 0.4620 0.6125 0.0336 0.5000 Uiso -1 H252 H 0.3078 0.5163 0.5204 0.0336 0.5000 Uiso -1 H261 H 0.5593 0.6590 0.7066 0.0390 0.5000 Uiso -1 H262 H 0.5128 0.7107 0.6111 0.0390 0.5000 Uiso -1 H271 H 0.3472 0.4721 0.3364 0.0419 0.5000 Uiso -1 H272 H 0.4118 0.3772 0.2868 0.0419 0.5000 Uiso -1 H281 H 0.5538 0.6603 0.4268 0.0457 0.5000 Uiso -1 H282 H 0.6193 0.5644 0.3845 0.0457 0.5000 Uiso -1 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 0.02085(18) 0.02272(19) 0.02518(19) 0.00802(14) 0.00172(13) 0.00459(14) S1 0.0354(4) 0.0314(4) 0.0253(4) 0.0061(3) 0.0021(3) 0.0192(4) S2 0.0291(4) 0.0480(5) 0.0344(4) 0.0223(4) 0.0126(3) 0.0206(4) C1 0.0174(12) 0.0173(13) 0.0252(14) 0.0051(11) -0.0007(11) 0.0006(11) N1 0.0249(12) 0.0250(12) 0.0246(12) 0.0069(10) 0.0055(10) 0.0107(11) C2 0.0287(15) 0.0269(15) 0.0240(14) 0.0081(12) 0.0051(12) 0.0112(13) C3 0.0282(15) 0.0260(15) 0.0227(14) 0.0060(12) 0.0070(12) 0.0136(13) C4 0.0298(15) 0.0288(15) 0.0253(15) 0.0105(12) 0.0060(12) 0.0141(13) C5 0.0290(15) 0.0299(15) 0.0237(14) 0.0110(12) 0.0111(12) 0.0179(13) C6 0.0293(15) 0.0297(15) 0.0248(14) 0.0122(12) 0.0086(12) 0.0141(13) C7 0.0259(14) 0.0297(15) 0.0275(15) 0.0112(12) 0.0101(12) 0.0162(13) C8 0.0337(16) 0.0337(16) 0.0326(16) 0.0180(14) 0.0169(14) 0.0179(14) C9 0.0364(17) 0.0401(18) 0.0298(16) 0.0200(14) 0.0123(14) 0.0197(15) C10 0.0307(16) 0.0346(16) 0.0227(14) 0.0118(13) 0.0110(12) 0.0184(14) C11 0.0387(18) 0.0417(18) 0.0249(15) 0.0163(14) 0.0090(14) 0.0221(16) C12 0.0331(16) 0.0348(17) 0.0226(15) 0.0069(13) 0.0031(13) 0.0164(14) C13 0.0278(15) 0.0313(16) 0.0260(15) 0.0120(13) 0.0087(12) 0.0127(13) C14 0.0330(16) 0.0325(16) 0.0335(17) 0.0125(14) 0.0104(14) 0.0182(14) C15 0.0354(17) 0.0432(19) 0.0349(17) 0.0180(15) 0.0117(14) 0.0256(16) C16 0.0324(18) 0.043(2) 0.051(2) 0.0189(17) 0.0094(16) 0.0206(16) C17 0.035(2) 0.056(3) 0.057(3) 0.011(2) 0.0069(19) 0.022(2) S3 0.0518(5) 0.0272(4) 0.0265(4) 0.0089(3) 0.0144(4) 0.0182(4) S4 0.0270(4) 0.0316(4) 0.0338(4) 0.0165(3) 0.0119(3) 0.0141(3) C18 0.0190(13) 0.0180(13) 0.0240(14) 0.0054(11) 0.0026(11) 0.0024(11) N2 0.0266(13) 0.0258(12) 0.0259(13) 0.0094(10) 0.0064(10) 0.0098(11) C19 0.051(2) 0.042(2) 0.0365(18) 0.0172(16) 0.0136(16) 0.0315(18) C20 0.063(3) 0.043(2) 0.064(3) 0.023(2) 0.022(2) 0.033(2) C21 0.107(5) 0.067(3) 0.081(4) 0.029(3) 0.028(3) 0.064(4) C22 0.129(6) 0.087(4) 0.081(4) 0.029(3) 0.048(4) 0.082(4) N3 0.0230(12) 0.0222(12) 0.0236(12) 0.0087(10) 0.0026(10) 0.0063(10) C23 0.020(3) 0.019(3) 0.060(5) 0.010(3) -0.003(3) 0.002(3) C24 0.021(3) 0.022(3) 0.079(6) 0.011(4) 0.000(3) 0.009(3) C25 0.023(3) 0.020(3) 0.040(4) 0.002(3) 0.010(3) 0.004(3) C26 0.022(3) 0.029(3) 0.047(4) -0.004(3) 0.012(3) 0.005(3) C27 0.031(4) 0.042(4) 0.032(4) 0.018(3) -0.003(3) -0.004(3) C28 0.040(4) 0.049(5) 0.025(3) 0.018(3) -0.009(3) -0.012(4) N4 0.0230(12) 0.0222(12) 0.0236(12) 0.0087(10) 0.0026(10) 0.0063(10) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . S1 . 2.4691(9) yes Zn1 . S2 . 2.4244(9) yes Zn1 . S3 . 2.4081(10) yes Zn1 . S4 . 2.4948(9) yes Zn1 . N3 . 2.157(2) yes Zn1 . N4 2_666 2.157(2) yes S1 . C1 . 1.716(3) yes S2 . C1 . 1.733(3) yes C1 . N1 . 1.339(4) yes N1 . C2 . 1.484(4) yes N1 . C14 . 1.468(4) yes C2 . C3 . 1.520(4) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.372(4) yes C3 . C12 . 1.413(5) yes C4 . C5 . 1.418(4) yes C4 . H41 . 1.000 no C5 . C6 . 1.418(4) yes C5 . C10 . 1.417(4) yes C6 . C7 . 1.370(5) yes C6 . H61 . 1.000 no C7 . C8 . 1.418(5) yes C7 . C13 . 1.515(4) yes C8 . C9 . 1.372(5) yes C8 . H81 . 1.000 no C9 . C10 . 1.416(5) yes C9 . H91 . 1.000 no C10 . C11 . 1.419(4) yes C11 . C12 . 1.368(5) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . N2 2_666 1.468(4) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . C15 . 1.530(5) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.515(5) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . C17 . 1.526(5) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no S3 . C18 . 1.728(3) yes S4 . C18 . 1.717(3) yes C18 . N2 . 1.334(4) yes N2 . C19 . 1.473(5) yes C19 . C20 . 1.508(6) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C20 . C21 . 1.543(7) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C21 . C22 . 1.554(10) yes C21 . H211 . 1.000 no C21 . H212 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no N3 . C23 . 1.436(8) yes N3 . C25 . 1.558(7) yes N3 . C27 . 1.464(8) yes C23 . C24 . 1.545(9) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . N4 . 1.434(8) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . C26 . 1.535(9) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . N4 . 1.541(7) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . C28 . 1.528(9) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . N4 . 1.465(7) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Zn1 . S2 . 73.60(3) yes S1 . Zn1 . S3 . 101.96(3) yes S2 . Zn1 . S3 . 151.56(4) yes S1 . Zn1 . S4 . 164.69(3) yes S2 . Zn1 . S4 . 103.06(3) yes S3 . Zn1 . S4 . 73.63(3) yes S1 . Zn1 . N3 . 97.77(7) yes S2 . Zn1 . N3 . 105.34(7) yes S3 . Zn1 . N3 . 103.09(7) yes S4 . Zn1 . N3 . 97.52(7) yes S1 . Zn1 . N4 2_666 97.77(7) yes S2 . Zn1 . N4 2_666 105.34(7) yes S3 . Zn1 . N4 2_666 103.09(7) yes S4 . Zn1 . N4 2_666 97.52(7) yes Zn1 . S1 . C1 . 83.71(11) yes Zn1 . S2 . C1 . 84.76(11) yes S1 . C1 . S2 . 116.42(18) yes S1 . C1 . N1 . 122.4(2) yes S2 . C1 . N1 . 121.2(2) yes C1 . N1 . C2 . 121.4(3) yes C1 . N1 . C14 . 123.8(3) yes C2 . N1 . C14 . 114.8(3) yes N1 . C2 . C3 . 112.2(2) yes N1 . C2 . H21 . 108.795 no C3 . C2 . H21 . 108.795 no N1 . C2 . H22 . 108.795 no C3 . C2 . H22 . 108.795 no H21 . C2 . H22 . 109.467 no C2 . C3 . C4 . 121.5(3) yes C2 . C3 . C12 . 119.4(3) yes C4 . C3 . C12 . 119.0(3) yes C3 . C4 . C5 . 121.7(3) yes C3 . C4 . H41 . 119.130 no C5 . C4 . H41 . 119.130 no C4 . C5 . C6 . 122.5(3) yes C4 . C5 . C10 . 118.7(3) yes C6 . C5 . C10 . 118.9(3) yes C5 . C6 . C7 . 121.9(3) yes C5 . C6 . H61 . 119.061 no C7 . C6 . H61 . 119.061 no C6 . C7 . C8 . 118.8(3) yes C6 . C7 . C13 . 122.0(3) yes C8 . C7 . C13 . 119.2(3) yes C7 . C8 . C9 . 120.9(3) yes C7 . C8 . H81 . 119.534 no C9 . C8 . H81 . 119.534 no C8 . C9 . C10 . 120.8(3) yes C8 . C9 . H91 . 119.600 no C10 . C9 . H91 . 119.601 no C5 . C10 . C9 . 118.7(3) yes C5 . C10 . C11 . 118.8(3) yes C9 . C10 . C11 . 122.4(3) yes C10 . C11 . C12 . 120.8(3) yes C10 . C11 . H111 . 119.610 no C12 . C11 . H111 . 119.610 no C3 . C12 . C11 . 121.0(3) yes C3 . C12 . H121 . 119.518 no C11 . C12 . H121 . 119.518 no C7 . C13 . N2 2_666 112.4(3) yes C7 . C13 . H131 . 108.727 no N2 2_666 C13 . H131 . 108.727 no C7 . C13 . H132 . 108.727 no N2 2_666 C13 . H132 . 108.727 no H131 . C13 . H132 . 109.467 no N1 . C14 . C15 . 113.0(3) yes N1 . C14 . H141 . 108.591 no C15 . C14 . H141 . 108.591 no N1 . C14 . H142 . 108.592 no C15 . C14 . H142 . 108.591 no H141 . C14 . H142 . 109.467 no C14 . C15 . C16 . 113.8(3) yes C14 . C15 . H151 . 108.387 no C16 . C15 . H151 . 108.387 no C14 . C15 . H152 . 108.387 no C16 . C15 . H152 . 108.387 no H151 . C15 . H152 . 109.467 no C15 . C16 . C17 . 111.8(4) yes C15 . C16 . H161 . 108.878 no C17 . C16 . H161 . 108.878 no C15 . C16 . H162 . 108.878 no C17 . C16 . H162 . 108.879 no H161 . C16 . H162 . 109.467 no C16 . C17 . H171 . 109.466 no C16 . C17 . H172 . 109.467 no H171 . C17 . H172 . 109.476 no C16 . C17 . H173 . 109.466 no H171 . C17 . H173 . 109.475 no H172 . C17 . H173 . 109.476 no Zn1 . S3 . C18 . 85.09(11) yes Zn1 . S4 . C18 . 82.63(11) yes S3 . C18 . S4 . 117.07(18) yes S3 . C18 . N2 . 120.6(2) yes S4 . C18 . N2 . 122.3(2) yes C13 2_666 N2 . C18 . 123.1(3) yes C13 2_666 N2 . C19 . 115.4(3) yes C18 . N2 . C19 . 121.4(3) yes N2 . C19 . C20 . 113.6(3) yes N2 . C19 . H191 . 108.443 no C20 . C19 . H191 . 108.443 no N2 . C19 . H192 . 108.443 no C20 . C19 . H192 . 108.443 no H191 . C19 . H192 . 109.467 no C19 . C20 . C21 . 111.2(4) yes C19 . C20 . H201 . 109.048 no C21 . C20 . H201 . 109.047 no C19 . C20 . H202 . 109.048 no C21 . C20 . H202 . 109.047 no H201 . C20 . H202 . 109.466 no C20 . C21 . C22 . 112.9(5) yes C20 . C21 . H211 . 108.612 no C22 . C21 . H211 . 108.613 no C20 . C21 . H212 . 108.612 no C22 . C21 . H212 . 108.612 no H211 . C21 . H212 . 109.467 no C21 . C22 . H221 . 109.468 no C21 . C22 . H222 . 109.466 no H221 . C22 . H222 . 109.473 no C21 . C22 . H223 . 109.469 no H221 . C22 . H223 . 109.477 no H222 . C22 . H223 . 109.475 no Zn1 . N3 . C23 . 112.1(3) yes Zn1 . N3 . C25 . 109.6(3) yes C23 . N3 . C25 . 106.6(5) yes Zn1 . N3 . C27 . 110.9(3) yes C23 . N3 . C27 . 112.0(5) yes C25 . N3 . C27 . 105.3(5) yes N3 . C23 . C24 . 111.1(5) yes N3 . C23 . H231 . 109.064 no C24 . C23 . H231 . 109.066 no N3 . C23 . H232 . 109.063 no C24 . C23 . H232 . 109.063 no H231 . C23 . H232 . 109.467 no C23 . C24 . N4 . 112.1(6) yes C23 . C24 . H241 . 108.805 no N4 . C24 . H241 . 108.805 no C23 . C24 . H242 . 108.808 no N4 . C24 . H242 . 108.808 no H241 . C24 . H242 . 109.467 no N3 . C25 . C26 . 109.1(5) yes N3 . C25 . H251 . 109.570 no C26 . C25 . H251 . 109.571 no N3 . C25 . H252 . 109.571 no C26 . C25 . H252 . 109.571 no N4 2_666 C25 . H252 . 109.571 no C25 . C26 . N4 . 111.2(5) yes C25 . C26 . H261 . 109.040 no N4 . C26 . H261 . 109.040 no C25 . C26 . H262 . 109.040 no N4 . C26 . H262 . 109.041 no H261 . C26 . H262 . 109.466 no N3 . C27 . C28 . 111.2(5) yes N3 . C27 . H271 . 109.034 no C28 . C27 . H271 . 109.033 no N3 . C27 . H272 . 109.032 no C28 . C27 . H272 . 109.033 no H271 . C27 . H272 . 109.467 no C27 . C28 . N4 . 111.8(6) yes C27 . C28 . H281 . 108.894 no N4 . C28 . H281 . 108.894 no C27 . C28 . H282 . 108.893 no N4 . C28 . H282 . 108.892 no H281 . C28 . H282 . 109.467 no Zn1 2_666 N4 . C24 . 111.1(3) yes Zn1 2_666 N4 . C26 . 110.7(3) yes C24 . N4 . C26 . 105.9(5) yes Zn1 2_666 N4 . C28 . 112.2(3) yes C24 . N4 . C28 . 111.0(6) yes C26 . N4 . C28 . 105.5(6) yes #===END