# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhien Lin' _publ_contact_author_address ; ; _publ_contact_author_email zhienlin@scu.edu.cn _publ_author_name 'Zhien Lin' # Attachment '- 1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 884213' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H67 N4 O25.50 Zn4' _chemical_formula_weight 1225.42 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4178(3) _cell_length_b 15.4572(6) _cell_length_c 18.2451(9) _cell_angle_alpha 95.399(4) _cell_angle_beta 91.352(4) _cell_angle_gamma 90.312(3) _cell_volume 2643.39(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7342 _cell_measurement_theta_min 2.9651 _cell_measurement_theta_max 29.1618 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68168 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19853 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9311 _reflns_number_gt 6713 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.2204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9311 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 0.25341(6) 0.08870(4) 0.02975(3) 0.03124(18) Uani 1 1 d . . . Zn2 Zn 0.12112(6) 0.41788(4) 0.11214(3) 0.03432(18) Uani 1 1 d . . . Zn3 Zn 0.11070(7) 0.58318(4) 0.38737(4) 0.0415(2) Uani 1 1 d . . . Zn4 Zn 0.25004(6) 0.91445(4) 0.46921(3) 0.03361(18) Uani 1 1 d . . . O1 O 0.3124(4) 0.2117(2) 0.0059(2) 0.0401(9) Uani 1 1 d . . . O2 O 0.1666(4) 0.1604(2) 0.1192(2) 0.0394(9) Uani 1 1 d . . . O3 O 0.2669(4) 0.3497(2) 0.0449(2) 0.0447(10) Uani 1 1 d . . . O4 O 0.0973(4) 0.2960(2) 0.1480(2) 0.0406(9) Uani 1 1 d . . . O5 O -0.0218(3) 0.4709(2) 0.1895(2) 0.0418(9) Uani 1 1 d . . . O6 O 0.2610(3) 0.4696(2) 0.1965(2) 0.0374(9) Uani 1 1 d . . . O7 O -0.0278(3) 0.5306(2) 0.3046(2) 0.0448(10) Uani 1 1 d . . . O8 O 0.2567(3) 0.5368(3) 0.3090(2) 0.0448(10) Uani 1 1 d . . . O9 O 0.0869(4) 0.7047(2) 0.3519(2) 0.0504(10) Uani 1 1 d . . . O10 O 0.2532(4) 0.6543(2) 0.4606(2) 0.0507(11) Uani 1 1 d . . . O11 O 0.1588(4) 0.8413(2) 0.3804(2) 0.0440(10) Uani 1 1 d . . . O12 O 0.3038(4) 0.7910(2) 0.4969(2) 0.0474(10) Uani 1 1 d . . . O13 O 0.3622(3) 0.0238(2) -0.05982(19) 0.0340(8) Uani 1 1 d . . . O14 O 0.0542(3) 0.0975(2) -0.0319(2) 0.0364(9) Uani 1 1 d . . . O15 O 0.4439(3) 0.0542(2) 0.08214(19) 0.0365(9) Uani 1 1 d . . . O16 O 0.1500(3) -0.0261(2) 0.0508(2) 0.0349(8) Uani 1 1 d . . . O17 O -0.0398(4) 0.3984(2) 0.0283(2) 0.0412(9) Uani 1 1 d . . . O18 O 0.1385(4) 0.5323(2) 0.0609(2) 0.0412(9) Uani 1 1 d . . . O19 O -0.0467(4) 0.5989(2) 0.4684(2) 0.0449(10) Uani 1 1 d . . . O20 O 0.1349(4) 0.4685(2) 0.4402(2) 0.0464(10) Uani 1 1 d . . . O21 O 0.4340(4) 0.9485(3) 0.4175(2) 0.0432(10) Uani 1 1 d . . . O22 O 0.1469(3) 1.0286(2) 0.4512(2) 0.0402(9) Uani 1 1 d . . . O23 O 0.0548(3) 0.9006(2) 0.5281(2) 0.0383(9) Uani 1 1 d . . . O24 O 0.3688(3) 0.9734(2) 0.55984(19) 0.0356(8) Uani 1 1 d . . . N1 N 0.3345(5) -0.0101(3) -0.2219(3) 0.0492(13) Uani 1 1 d . . . H1A H 0.3651 -0.0153 -0.1754 0.059 Uiso 1 1 calc R . . H1B H 0.3464 -0.0621 -0.2476 0.059 Uiso 1 1 calc R . . N2 N -0.1445(4) 0.7571(3) 0.5458(3) 0.0402(11) Uani 1 1 d . . . H2A H -0.0862 0.8025 0.5411 0.048 Uiso 1 1 calc R . . H2B H -0.1040 0.7099 0.5226 0.048 Uiso 1 1 calc R . . N3 N -0.1220(4) 0.2459(3) -0.0655(2) 0.0363(11) Uani 1 1 d . . . H3A H -0.0669 0.2022 -0.0524 0.044 Uiso 1 1 calc R . . H3B H -0.0966 0.2937 -0.0359 0.044 Uiso 1 1 calc R . . N4 N 0.5528(5) 0.4482(4) 0.2220(4) 0.084(2) Uani 1 1 d . . . C1 C 0.2558(5) 0.2694(3) 0.0481(3) 0.0327(12) Uani 1 1 d . . . C2 C 0.1650(5) 0.2390(3) 0.1107(3) 0.0302(12) Uani 1 1 d . . . C3 C 0.0339(5) 0.5012(3) 0.2477(3) 0.0316(12) Uani 1 1 d . . . C4 C 0.1990(5) 0.5027(3) 0.2522(3) 0.0298(12) Uani 1 1 d . . . C5 C 0.1565(5) 0.7634(4) 0.3905(3) 0.0388(13) Uani 1 1 d . . . C6 C 0.2451(5) 0.7330(3) 0.4550(3) 0.0391(13) Uani 1 1 d . . . C7 C 0.5226(5) 0.0088(3) 0.0404(3) 0.0291(11) Uani 1 1 d . . . C8 C 0.0281(5) -0.0350(3) 0.0238(3) 0.0313(12) Uani 1 1 d . . . C9 C 0.0515(5) 0.5387(3) 0.0093(3) 0.0322(12) Uani 1 1 d . . . C10 C 0.0528(5) 0.4629(3) 0.4924(3) 0.0373(13) Uani 1 1 d . . . C11 C -0.0272(5) 0.9637(3) 0.5221(3) 0.0295(12) Uani 1 1 d . . . C12 C 0.4826(5) 1.0075(3) 0.5407(3) 0.0285(11) Uani 1 1 d . . . C13 C 0.1078(7) -0.0683(5) -0.1883(4) 0.070(2) Uani 1 1 d . . . H13A H 0.1490 -0.0749 -0.1405 0.105 Uiso 1 1 calc R . . H13B H 0.1224 -0.1203 -0.2202 0.105 Uiso 1 1 calc R . . H13C H 0.0078 -0.0579 -0.1839 0.105 Uiso 1 1 calc R . . C14 C 0.1772(6) 0.0077(4) -0.2201(3) 0.0509(16) Uani 1 1 d . . . H14A H 0.1622 0.0600 -0.1864 0.061 Uiso 1 1 calc R . . C15 C 0.1186(7) 0.0243(5) -0.2960(4) 0.069(2) Uani 1 1 d . . . H15A H 0.1683 0.0725 -0.3133 0.103 Uiso 1 1 calc R . . H15B H 0.0192 0.0374 -0.2929 0.103 Uiso 1 1 calc R . . H15C H 0.1312 -0.0266 -0.3296 0.103 Uiso 1 1 calc R . . C16 C 0.5796(7) 0.0200(5) -0.2480(4) 0.079(2) Uani 1 1 d . . . H16A H 0.5845 -0.0368 -0.2740 0.119 Uiso 1 1 calc R . . H16B H 0.6055 0.0167 -0.1971 0.119 Uiso 1 1 calc R . . H16C H 0.6438 0.0586 -0.2691 0.119 Uiso 1 1 calc R . . C17 C 0.4301(7) 0.0539(4) -0.2536(3) 0.0519(16) Uani 1 1 d . . . H17A H 0.4045 0.0553 -0.3059 0.062 Uiso 1 1 calc R . . C18 C 0.4133(9) 0.1417(5) -0.2165(5) 0.088(3) Uani 1 1 d . . . H18A H 0.3162 0.1594 -0.2216 0.131 Uiso 1 1 calc R . . H18B H 0.4741 0.1815 -0.2385 0.131 Uiso 1 1 calc R . . H18C H 0.4384 0.1415 -0.1653 0.131 Uiso 1 1 calc R . . C19 C -0.3774(7) 0.6974(5) 0.5084(6) 0.099(3) Uani 1 1 d . . . H19A H -0.4653 0.7072 0.4829 0.149 Uiso 1 1 calc R . . H19B H -0.3957 0.6893 0.5589 0.149 Uiso 1 1 calc R . . H19C H -0.3329 0.6464 0.4854 0.149 Uiso 1 1 calc R . . C20 C -0.2824(6) 0.7731(4) 0.5054(4) 0.0597(19) Uani 1 1 d . . . H20A H -0.3278 0.8246 0.5297 0.072 Uiso 1 1 calc R . . C21 C -0.2440(8) 0.7911(5) 0.4276(4) 0.083(3) Uani 1 1 d . . . H21A H -0.3289 0.8025 0.4001 0.125 Uiso 1 1 calc R . . H21B H -0.1970 0.7415 0.4039 0.125 Uiso 1 1 calc R . . H21C H -0.1819 0.8408 0.4298 0.125 Uiso 1 1 calc R . . C22 C -0.0014(8) 0.7259(5) 0.6521(4) 0.077(2) Uani 1 1 d . . . H22A H 0.0341 0.6758 0.6233 0.115 Uiso 1 1 calc R . . H22B H -0.0012 0.7152 0.7031 0.115 Uiso 1 1 calc R . . H22C H 0.0580 0.7753 0.6461 0.115 Uiso 1 1 calc R . . C23 C -0.1496(7) 0.7437(4) 0.6268(3) 0.0516(16) Uani 1 1 d . . . H23A H -0.2084 0.6923 0.6323 0.062 Uiso 1 1 calc R . . C24 C -0.2166(8) 0.8211(5) 0.6690(4) 0.078(2) Uani 1 1 d . . . H24A H -0.2199 0.8117 0.7202 0.117 Uiso 1 1 calc R . . H24B H -0.3113 0.8286 0.6501 0.117 Uiso 1 1 calc R . . H24C H -0.1612 0.8723 0.6636 0.117 Uiso 1 1 calc R . . C25 C -0.1276(11) 0.1845(5) -0.1944(4) 0.093(3) Uani 1 1 d . . . H25A H -0.1050 0.1950 -0.2439 0.140 Uiso 1 1 calc R . . H25B H -0.2278 0.1741 -0.1916 0.140 Uiso 1 1 calc R . . H25C H -0.0767 0.1345 -0.1808 0.140 Uiso 1 1 calc R . . C26 C -0.0859(7) 0.2621(4) -0.1429(3) 0.0497(16) Uani 1 1 d . . . H26A H -0.1416 0.3118 -0.1566 0.060 Uiso 1 1 calc R . . C27 C 0.0648(8) 0.2849(5) -0.1456(4) 0.079(2) Uani 1 1 d . . . H27A H 0.0850 0.3350 -0.1117 0.118 Uiso 1 1 calc R . . H27B H 0.0871 0.2975 -0.1946 0.118 Uiso 1 1 calc R . . H27C H 0.1213 0.2370 -0.1322 0.118 Uiso 1 1 calc R . . C28 C -0.3713(7) 0.2932(5) -0.0705(5) 0.088(3) Uani 1 1 d . . . H28A H -0.3665 0.2977 -0.1225 0.132 Uiso 1 1 calc R . . H28B H -0.3453 0.3479 -0.0442 0.132 Uiso 1 1 calc R . . H28C H -0.4663 0.2779 -0.0585 0.132 Uiso 1 1 calc R . . C29 C -0.2707(6) 0.2242(4) -0.0491(4) 0.0566(18) Uani 1 1 d . . . H29A H -0.2971 0.1687 -0.0765 0.068 Uiso 1 1 calc R . . C30 C -0.2763(8) 0.2147(4) 0.0322(4) 0.082(3) Uani 1 1 d . . . H30A H -0.2110 0.1706 0.0447 0.122 Uiso 1 1 calc R . . H30B H -0.3708 0.1985 0.0444 0.122 Uiso 1 1 calc R . . H30C H -0.2506 0.2690 0.0594 0.122 Uiso 1 1 calc R . . C31 C 0.4640(7) 0.3000(5) 0.2323(5) 0.086(3) Uani 1 1 d . . . H31A H 0.3703 0.3186 0.2195 0.129 Uiso 1 1 calc R . . H31B H 0.4783 0.3083 0.2848 0.129 Uiso 1 1 calc R . . H31C H 0.4744 0.2396 0.2158 0.129 Uiso 1 1 calc R . . C32 C 0.5714(7) 0.3522(4) 0.1962(5) 0.071(2) Uani 1 1 d . . . H32A H 0.5542 0.3441 0.1428 0.086 Uiso 1 1 calc R . . C33 C 0.7222(8) 0.3238(5) 0.2127(5) 0.097(3) Uani 1 1 d . . . H33A H 0.7325 0.2634 0.1961 0.145 Uiso 1 1 calc R . . H33B H 0.7413 0.3323 0.2649 0.145 Uiso 1 1 calc R . . H33C H 0.7880 0.3577 0.1878 0.145 Uiso 1 1 calc R . . C34 C 0.552(2) 0.4895(13) 0.0796(11) 0.092(6) Uiso 0.50 1 d P . . C34' C 0.610(2) 0.5096(15) 0.1135(16) 0.099(7) Uiso 0.50 1 d P . . C35 C 0.6255(15) 0.5112(10) 0.1548(12) 0.057(4) Uiso 0.50 1 d P . . C35' C 0.6355(15) 0.5153(10) 0.2013(11) 0.065(4) Uiso 0.50 1 d P . . C36 C 0.6068(18) 0.6001(12) 0.1922(11) 0.090(5) Uiso 0.50 1 d P . . C36' C 0.605(2) 0.6011(13) 0.2499(12) 0.102(6) Uiso 0.50 1 d P . . OW1 O 0.3635(5) -0.1486(3) -0.3354(3) 0.0708(13) Uani 1 1 d . . . OW2 O -0.3106(11) 0.4858(9) 0.3482(8) 0.136(6) Uani 0.50 1 d P . . 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 0.0277(3) 0.0260(3) 0.0400(4) 0.0028(3) 0.0020(2) 0.0012(2) Zn2 0.0363(3) 0.0272(3) 0.0386(4) -0.0008(3) -0.0021(3) 0.0011(2) Zn3 0.0458(4) 0.0336(4) 0.0434(4) -0.0064(3) 0.0053(3) -0.0082(3) Zn4 0.0307(3) 0.0304(3) 0.0393(4) 0.0018(3) -0.0015(3) -0.0062(2) O1 0.043(2) 0.0298(19) 0.048(3) 0.0006(18) 0.0183(18) -0.0005(16) O2 0.050(2) 0.0234(18) 0.047(3) 0.0102(18) 0.0147(18) 0.0023(16) O3 0.048(2) 0.031(2) 0.056(3) 0.0043(19) 0.0189(19) -0.0019(17) O4 0.052(2) 0.0312(19) 0.040(2) 0.0037(18) 0.0172(18) 0.0068(17) O5 0.0297(19) 0.045(2) 0.047(3) -0.012(2) -0.0084(17) -0.0009(16) O6 0.0253(18) 0.043(2) 0.041(2) -0.0056(19) -0.0020(16) 0.0018(15) O7 0.0295(19) 0.043(2) 0.057(3) -0.020(2) 0.0087(18) -0.0079(16) O8 0.0279(19) 0.062(3) 0.042(2) -0.009(2) -0.0041(17) -0.0096(17) O9 0.066(3) 0.041(2) 0.042(3) -0.001(2) -0.013(2) -0.0171(19) O10 0.048(2) 0.035(2) 0.067(3) 0.000(2) -0.017(2) -0.0013(18) O11 0.059(2) 0.032(2) 0.040(3) 0.0053(19) -0.0107(18) -0.0131(18) O12 0.043(2) 0.036(2) 0.060(3) -0.007(2) -0.0192(19) 0.0003(17) O13 0.0315(18) 0.042(2) 0.028(2) 0.0055(17) -0.0053(15) 0.0083(16) O14 0.0304(18) 0.0264(18) 0.054(3) 0.0151(18) -0.0058(16) -0.0043(15) O15 0.0329(19) 0.046(2) 0.029(2) -0.0053(18) -0.0005(15) 0.0096(16) O16 0.0301(19) 0.0276(18) 0.048(2) 0.0096(17) -0.0043(16) 0.0011(15) O17 0.053(2) 0.0238(19) 0.046(3) 0.0015(18) -0.0094(18) -0.0086(16) O18 0.048(2) 0.0281(19) 0.046(3) 0.0026(18) -0.0122(19) -0.0090(16) O19 0.051(2) 0.035(2) 0.049(3) 0.003(2) 0.0098(19) 0.0092(18) O20 0.054(2) 0.031(2) 0.055(3) 0.0020(19) 0.016(2) 0.0087(18) O21 0.039(2) 0.058(2) 0.030(2) -0.009(2) 0.0023(16) -0.0160(18) O22 0.0291(19) 0.041(2) 0.053(3) 0.0106(19) 0.0106(17) -0.0048(16) O23 0.037(2) 0.0283(19) 0.052(3) 0.0132(18) 0.0032(17) -0.0001(16) O24 0.0334(19) 0.044(2) 0.029(2) 0.0000(18) 0.0041(15) -0.0123(16) N1 0.058(3) 0.064(3) 0.025(3) 0.005(3) -0.003(2) -0.016(3) N2 0.039(2) 0.028(2) 0.053(3) 0.001(2) 0.003(2) -0.0030(19) N3 0.044(3) 0.020(2) 0.044(3) -0.001(2) -0.005(2) -0.0007(18) N4 0.038(3) 0.045(3) 0.171(7) 0.020(4) 0.000(4) 0.001(2) C1 0.025(2) 0.032(3) 0.040(3) -0.001(3) -0.001(2) -0.003(2) C2 0.026(2) 0.035(3) 0.031(3) 0.005(2) 0.000(2) -0.001(2) C3 0.024(3) 0.022(2) 0.048(4) 0.001(2) 0.002(2) 0.001(2) C4 0.021(2) 0.027(3) 0.041(4) 0.003(2) -0.001(2) 0.000(2) C5 0.038(3) 0.044(3) 0.033(3) -0.003(3) 0.002(2) -0.005(3) C6 0.031(3) 0.027(3) 0.058(4) -0.005(3) 0.004(3) 0.000(2) C7 0.029(3) 0.028(3) 0.030(3) 0.003(2) -0.002(2) -0.005(2) C8 0.033(3) 0.023(2) 0.038(3) 0.004(2) 0.005(2) 0.000(2) C9 0.038(3) 0.024(3) 0.034(3) -0.002(2) 0.001(2) -0.002(2) C10 0.033(3) 0.031(3) 0.047(4) -0.003(3) 0.004(3) 0.001(2) C11 0.038(3) 0.025(3) 0.026(3) 0.008(2) -0.009(2) -0.008(2) C12 0.025(2) 0.026(2) 0.035(3) 0.004(2) 0.002(2) 0.000(2) C13 0.065(4) 0.090(5) 0.054(5) 0.001(4) 0.007(3) -0.031(4) C14 0.062(4) 0.058(4) 0.031(4) -0.002(3) 0.004(3) -0.004(3) C15 0.059(4) 0.104(6) 0.043(4) 0.005(4) -0.007(3) -0.006(4) C16 0.062(4) 0.115(7) 0.061(5) 0.017(5) -0.008(4) -0.021(4) C17 0.066(4) 0.058(4) 0.032(4) 0.011(3) -0.003(3) -0.018(3) C18 0.120(7) 0.058(5) 0.084(6) 0.001(5) 0.016(5) -0.035(4) C19 0.032(4) 0.079(5) 0.188(10) 0.027(6) -0.032(5) -0.010(3) C20 0.050(4) 0.043(4) 0.085(6) -0.001(4) -0.011(3) 0.016(3) C21 0.096(6) 0.072(5) 0.080(6) 0.006(5) -0.040(5) 0.004(4) C22 0.099(6) 0.068(5) 0.062(5) 0.005(4) -0.023(4) 0.002(4) C23 0.068(4) 0.038(3) 0.051(4) 0.011(3) 0.013(3) -0.007(3) C24 0.105(6) 0.062(5) 0.068(5) 0.002(4) 0.041(5) -0.002(4) C25 0.167(9) 0.068(5) 0.042(5) -0.005(4) -0.006(5) -0.014(5) C26 0.070(4) 0.036(3) 0.044(4) 0.008(3) -0.007(3) 0.004(3) C27 0.083(5) 0.072(5) 0.082(6) 0.006(4) 0.035(4) -0.008(4) C28 0.044(4) 0.059(5) 0.163(9) 0.022(5) 0.002(5) 0.006(3) C29 0.046(4) 0.032(3) 0.092(6) 0.006(3) 0.003(3) -0.003(3) C30 0.099(6) 0.050(4) 0.099(7) 0.013(4) 0.051(5) -0.002(4) C31 0.055(4) 0.074(5) 0.135(8) 0.045(5) -0.010(4) -0.006(4) C32 0.048(4) 0.060(4) 0.110(7) 0.026(5) 0.001(4) 0.002(3) C33 0.068(5) 0.080(6) 0.148(9) 0.035(6) 0.011(5) 0.022(4) OW1 0.092(3) 0.063(3) 0.058(3) 0.011(3) -0.006(3) -0.003(3) OW2 0.068(7) 0.171(13) 0.148(12) -0.095(11) -0.021(7) -0.013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.066(3) . ? Zn1 O2 2.071(4) . ? Zn1 O16 2.092(3) . ? Zn1 O15 2.108(3) . ? Zn1 O13 2.123(3) . ? Zn1 O14 2.176(3) . ? Zn2 O4 2.065(3) . ? Zn2 O18 2.084(4) . ? Zn2 O3 2.087(3) . ? Zn2 O5 2.087(4) . ? Zn2 O6 2.099(3) . ? Zn2 O17 2.127(4) . ? Zn3 O9 2.056(4) . ? Zn3 O7 2.075(4) . ? Zn3 O8 2.089(4) . ? Zn3 O10 2.101(4) . ? Zn3 O20 2.107(4) . ? Zn3 O19 2.117(4) . ? Zn4 O11 2.055(4) . ? Zn4 O22 2.068(3) . ? Zn4 O21 2.080(4) . ? Zn4 O12 2.081(4) . ? Zn4 O24 2.106(3) . ? Zn4 O23 2.171(3) . ? O1 C1 1.252(6) . ? O2 C2 1.239(6) . ? O3 C1 1.253(6) . ? O4 C2 1.248(6) . ? O5 C3 1.225(6) . ? O6 C4 1.253(6) . ? O7 C3 1.252(6) . ? O8 C4 1.230(6) . ? O9 C5 1.265(6) . ? O10 C6 1.234(6) . ? O11 C5 1.236(6) . ? O12 C6 1.240(6) . ? O13 C7 1.256(5) 2_655 ? O14 C8 1.257(6) 2 ? O15 C7 1.245(6) . ? O16 C8 1.240(6) . ? O17 C9 1.245(6) 2_565 ? O18 C9 1.245(6) . ? O19 C10 1.248(6) 2_566 ? O20 C10 1.249(6) . ? O21 C12 1.237(6) 2_676 ? O22 C11 1.240(6) 2_576 ? O23 C11 1.258(6) . ? O24 C12 1.263(6) . ? N1 C17 1.499(7) . ? N1 C14 1.510(7) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C20 1.512(7) . ? N2 C23 1.514(8) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C29 1.482(7) . ? N3 C26 1.504(7) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C35' 1.380(16) . ? N4 C32 1.526(9) . ? N4 C35 1.783(19) . ? C1 C2 1.550(7) . ? C3 C4 1.554(6) . ? C5 C6 1.538(8) . ? C7 O13 1.256(5) 2_655 ? C7 C7 1.525(10) 2_655 ? C8 O14 1.257(6) 2 ? C8 C8 1.539(10) 2 ? C9 O17 1.245(6) 2_565 ? C9 C9 1.544(9) 2_565 ? C10 O19 1.248(6) 2_566 ? C10 C10 1.531(10) 2_566 ? C11 O22 1.240(6) 2_576 ? C11 C11 1.537(9) 2_576 ? C12 O21 1.237(6) 2_676 ? C12 C12 1.524(10) 2_676 ? C13 C14 1.510(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.524(8) . ? C14 H14A 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.509(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.469(9) . ? C17 H17A 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.474(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.523(10) . ? C20 H20A 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.494(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.510(8) . ? C23 H23A 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.498(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.464(9) . ? C26 H26A 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.503(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.506(10) . ? C29 H29A 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.493(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.520(9) . ? C32 H32A 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C34' 0.85(3) . ? C34 C35 1.53(3) . ? C34' C35 0.76(2) . ? C34' C35' 1.61(3) . ? C34' C36 1.91(3) . ? C35 C35' 0.848(19) . ? C35 C36 1.49(2) . ? C35' C36 1.36(2) . ? C35' C36' 1.56(2) . ? C36 C36' 1.05(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 80.97(13) . . ? O1 Zn1 O16 167.84(13) . . ? O2 Zn1 O16 93.54(14) . . ? O1 Zn1 O15 98.42(14) . . ? O2 Zn1 O15 97.62(14) . . ? O16 Zn1 O15 93.04(13) . . ? O1 Zn1 O13 94.61(14) . . ? O2 Zn1 O13 173.83(14) . . ? O16 Zn1 O13 91.61(14) . . ? O15 Zn1 O13 78.68(13) . . ? O1 Zn1 O14 90.92(14) . . ? O2 Zn1 O14 89.88(14) . . ? O16 Zn1 O14 78.16(12) . . ? O15 Zn1 O14 168.81(13) . . ? O13 Zn1 O14 94.51(13) . . ? O4 Zn2 O18 171.78(15) . . ? O4 Zn2 O3 80.57(14) . . ? O18 Zn2 O3 94.70(15) . . ? O4 Zn2 O5 91.37(14) . . ? O18 Zn2 O5 93.64(15) . . ? O3 Zn2 O5 171.43(15) . . ? O4 Zn2 O6 97.51(15) . . ? O18 Zn2 O6 89.84(14) . . ? O3 Zn2 O6 99.03(15) . . ? O5 Zn2 O6 79.03(13) . . ? O4 Zn2 O17 94.54(14) . . ? O18 Zn2 O17 78.75(13) . . ? O3 Zn2 O17 90.95(15) . . ? O5 Zn2 O17 92.59(14) . . ? O6 Zn2 O17 165.45(13) . . ? O9 Zn3 O7 90.74(15) . . ? O9 Zn3 O8 96.97(16) . . ? O7 Zn3 O8 80.13(14) . . ? O9 Zn3 O10 80.09(15) . . ? O7 Zn3 O10 170.41(16) . . ? O8 Zn3 O10 98.08(15) . . ? O9 Zn3 O20 171.18(16) . . ? O7 Zn3 O20 96.08(16) . . ? O8 Zn3 O20 89.73(15) . . ? O10 Zn3 O20 93.33(16) . . ? O9 Zn3 O19 95.45(16) . . ? O7 Zn3 O19 94.71(15) . . ? O8 Zn3 O19 166.60(15) . . ? O10 Zn3 O19 88.99(16) . . ? O20 Zn3 O19 78.46(14) . . ? O11 Zn4 O22 95.89(15) . . ? O11 Zn4 O21 96.89(15) . . ? O22 Zn4 O21 93.92(14) . . ? O11 Zn4 O12 80.71(15) . . ? O22 Zn4 O12 165.44(14) . . ? O21 Zn4 O12 100.53(16) . . ? O11 Zn4 O24 170.62(14) . . ? O22 Zn4 O24 92.99(15) . . ? O21 Zn4 O24 79.46(13) . . ? O12 Zn4 O24 91.41(14) . . ? O11 Zn4 O23 88.71(15) . . ? O22 Zn4 O23 78.46(13) . . ? O21 Zn4 O23 171.01(14) . . ? O12 Zn4 O23 87.29(14) . . ? O24 Zn4 O23 96.04(14) . . ? C1 O1 Zn1 111.6(3) . . ? C2 O2 Zn1 111.5(3) . . ? C1 O3 Zn2 111.5(3) . . ? C2 O4 Zn2 112.8(3) . . ? C3 O5 Zn2 114.2(3) . . ? C4 O6 Zn2 113.3(3) . . ? C3 O7 Zn3 113.2(3) . . ? C4 O8 Zn3 112.6(3) . . ? C5 O9 Zn3 113.6(4) . . ? C6 O10 Zn3 111.6(4) . . ? C5 O11 Zn4 111.1(4) . . ? C6 O12 Zn4 111.9(3) . . ? C7 O13 Zn1 112.9(3) 2_655 . ? C8 O14 Zn1 112.1(3) 2 . ? C7 O15 Zn1 113.0(3) . . ? C8 O16 Zn1 114.7(3) . . ? C9 O17 Zn2 112.7(3) 2_565 . ? C9 O18 Zn2 114.6(3) . . ? C10 O19 Zn3 113.3(3) 2_566 . ? C10 O20 Zn3 113.9(3) . . ? C12 O21 Zn4 112.8(3) 2_676 . ? C11 O22 Zn4 115.0(3) 2_576 . ? C11 O23 Zn4 111.9(3) . . ? C12 O24 Zn4 112.3(3) . . ? C17 N1 C14 118.6(5) . . ? C17 N1 H1A 107.7 . . ? C14 N1 H1A 107.7 . . ? C17 N1 H1B 107.7 . . ? C14 N1 H1B 107.7 . . ? H1A N1 H1B 107.1 . . ? C20 N2 C23 118.3(5) . . ? C20 N2 H2A 107.7 . . ? C23 N2 H2A 107.7 . . ? C20 N2 H2B 107.7 . . ? C23 N2 H2B 107.7 . . ? H2A N2 H2B 107.1 . . ? C29 N3 C26 119.0(5) . . ? C29 N3 H3A 107.6 . . ? C26 N3 H3A 107.6 . . ? C29 N3 H3B 107.6 . . ? C26 N3 H3B 107.6 . . ? H3A N3 H3B 107.0 . . ? C35' N4 C32 125.3(8) . . ? C35' N4 C35 27.5(8) . . ? C32 N4 C35 108.4(8) . . ? O1 C1 O3 126.0(5) . . ? O1 C1 C2 117.2(4) . . ? O3 C1 C2 116.8(5) . . ? O2 C2 O4 126.2(5) . . ? O2 C2 C1 116.9(4) . . ? O4 C2 C1 117.0(4) . . ? O5 C3 O7 127.0(4) . . ? O5 C3 C4 117.0(5) . . ? O7 C3 C4 116.0(5) . . ? O8 C4 O6 126.0(4) . . ? O8 C4 C3 117.8(4) . . ? O6 C4 C3 116.2(5) . . ? O11 C5 O9 125.6(5) . . ? O11 C5 C6 118.5(5) . . ? O9 C5 C6 115.8(5) . . ? O10 C6 O12 125.6(6) . . ? O10 C6 C5 118.2(5) . . ? O12 C6 C5 116.2(5) . . ? O15 C7 O13 124.9(5) . 2_655 ? O15 C7 C7 118.3(5) . 2_655 ? O13 C7 C7 116.8(5) 2_655 2_655 ? O16 C8 O14 125.0(5) . 2 ? O16 C8 C8 118.2(5) . 2 ? O14 C8 C8 116.7(5) 2 2 ? O17 C9 O18 126.2(5) 2_565 . ? O17 C9 C9 117.4(6) 2_565 2_565 ? O18 C9 C9 116.5(6) . 2_565 ? O19 C10 O20 125.6(5) 2_566 . ? O19 C10 C10 117.4(6) 2_566 2_566 ? O20 C10 C10 116.9(6) . 2_566 ? O22 C11 O23 125.4(5) 2_576 . ? O22 C11 C11 118.2(5) 2_576 2_576 ? O23 C11 C11 116.4(6) . 2_576 ? O21 C12 O24 125.1(5) 2_676 . ? O21 C12 C12 118.6(5) 2_676 2_676 ? O24 C12 C12 116.3(5) . 2_676 ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C13 107.0(5) . . ? N1 C14 C15 111.2(5) . . ? C13 C14 C15 113.7(6) . . ? N1 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N1 111.2(6) . . ? C18 C17 C16 113.3(6) . . ? N1 C17 C16 107.0(5) . . ? C18 C17 H17A 108.4 . . ? N1 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C20 N2 109.1(5) . . ? C19 C20 C21 114.0(7) . . ? N2 C20 C21 106.7(5) . . ? C19 C20 H20A 109.0 . . ? N2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C22 C23 C24 113.9(6) . . ? C22 C23 N2 107.2(5) . . ? C24 C23 N2 110.3(5) . . ? C22 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? N2 C23 H23A 108.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C25 113.3(6) . . ? C27 C26 N3 109.4(5) . . ? C25 C26 N3 109.6(5) . . ? C27 C26 H26A 108.1 . . ? C25 C26 H26A 108.1 . . ? N3 C26 H26A 108.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C28 111.3(5) . . ? N3 C29 C30 107.4(5) . . ? C28 C29 C30 110.9(6) . . ? N3 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C31 C32 C33 111.8(6) . . ? C31 C32 N4 109.0(6) . . ? C33 C32 N4 110.4(6) . . ? C31 C32 H32A 108.5 . . ? C33 C32 H32A 108.5 . . ? N4 C32 H32A 108.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34' C34 C35 18(2) . . ? C35 C34' C34 143(4) . . ? C35 C34' C35' 2.7(18) . . ? C34 C34' C35' 142(3) . . ? C35 C34' C36 46(2) . . ? C34 C34' C36 136(3) . . ? C35' C34' C36 44.6(10) . . ? C34' C35 C35' 175(3) . . ? C34' C35 C36 112(3) . . ? C35' C35 C36 64.8(17) . . ? C34' C35 C34 20(2) . . ? C35' C35 C34 158(2) . . ? C36 C35 C34 118.0(15) . . ? C34' C35 N4 130(3) . . ? C35' C35 N4 48.8(15) . . ? C36 C35 N4 99.9(14) . . ? C34 C35 N4 111.0(11) . . ? C35 C35' C36 81.0(19) . . ? C35 C35' N4 104(2) . . ? C36 C35' N4 132.5(14) . . ? C35 C35' C36' 122(2) . . ? C36 C35' C36' 41.6(10) . . ? N4 C35' C36' 110.6(14) . . ? C35 C35' C34' 2.4(16) . . ? C36 C35' C34' 79.5(14) . . ? N4 C35' C34' 103.3(13) . . ? C36' C35' C34' 120.4(15) . . ? C36' C36 C35' 79.1(19) . . ? C36' C36 C35 113(2) . . ? C35' C36 C35 34.2(9) . . ? C36' C36 C34' 134(2) . . ? C35' C36 C34' 55.9(12) . . ? C35 C36 C34' 21.7(9) . . ? C36 C36' C35' 59.4(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O13 0.90 2.14 2.960(6) 151.1 . N2 H2A O23 0.90 2.05 2.944(6) 176.6 . N2 H2B O19 0.90 1.98 2.873(5) 170.8 . N3 H3A O14 0.90 2.04 2.940(5) 174.9 . N3 H3B O17 0.90 1.97 2.871(5) 179.6 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.331 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.095 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 884214' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Co2 N2 O14' _chemical_formula_weight 622.35 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 15.5337(4) _cell_length_b 9.8251(3) _cell_length_c 16.7644(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2558.59(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2172 _cell_measurement_theta_min 2.8846 _cell_measurement_theta_max 28.8982 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90580 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4788 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1169 _reflns_number_gt 996 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+4.0204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1169 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Co1 Co 0.32548(4) 0.0000 0.5000 0.0278(3) Uani 1 2 d S . . O1 O 0.42871(14) 0.0712(2) 0.56907(12) 0.0331(6) Uani 1 1 d . . . O2 O 0.32958(13) 0.1852(2) 0.43690(14) 0.0345(6) Uani 1 1 d . . . O3 O 0.26897(14) 0.3909(2) 0.43926(13) 0.0337(6) Uani 1 1 d . . . C1 C 0.5000 0.0404(4) 0.5399(2) 0.0229(9) Uani 1 2 d S . . C2 C 0.27839(19) 0.2732(3) 0.46417(18) 0.0262(7) Uani 1 1 d . . . N1 N 0.0221(3) 0.2163(5) 0.3017(3) 0.0267(14) Uani 0.50 1 d P . . C3 C 0.1391(5) 0.0484(8) 0.2706(5) 0.051(2) Uani 0.50 1 d P . . C4 C 0.1241(2) 0.1722(4) 0.3088(2) 0.0472(9) Uani 1 1 d . . . C5 C 0.1677(4) 0.3007(8) 0.2746(5) 0.0431(18) Uani 0.50 1 d P . . C6 C -0.0412(4) 0.1100(7) 0.3284(4) 0.0359(15) Uani 0.50 1 d P . . C7 C -0.0314(5) 0.0801(7) 0.4177(4) 0.0445(18) Uani 0.50 1 d P . . OW1 O 0.5000 0.2508(4) 0.3638(2) 0.0478(9) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0203(4) 0.0246(4) 0.0385(5) -0.0030(2) 0.000 0.000 O1 0.0255(11) 0.0352(12) 0.0387(13) -0.0127(10) 0.0047(9) -0.0002(10) O2 0.0303(13) 0.0317(12) 0.0415(14) 0.0011(10) 0.0112(9) 0.0064(9) O3 0.0303(12) 0.0268(11) 0.0440(13) 0.0059(9) 0.0090(10) 0.0019(10) C1 0.026(2) 0.0164(19) 0.026(2) -0.0030(17) 0.000 0.000 C2 0.0190(14) 0.0300(16) 0.0297(17) -0.0024(12) -0.0004(12) -0.0007(13) N1 0.019(4) 0.028(2) 0.034(3) 0.0019(19) 0.0008(17) -0.0006(19) C3 0.045(5) 0.046(4) 0.062(5) 0.002(4) 0.010(4) 0.020(4) C4 0.0330(19) 0.059(2) 0.049(2) 0.0032(17) -0.0050(16) -0.0082(18) C5 0.030(4) 0.053(4) 0.046(4) -0.008(4) -0.004(3) -0.012(3) C6 0.032(3) 0.033(4) 0.042(4) -0.001(3) 0.001(3) -0.007(3) C7 0.052(4) 0.048(4) 0.033(3) 0.013(3) 0.004(3) -0.005(3) OW1 0.055(2) 0.052(2) 0.036(2) 0.0024(16) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.083(2) 16_545 ? Co1 O3 2.083(2) 13_556 ? Co1 O1 2.098(2) . ? Co1 O1 2.098(2) 4_556 ? Co1 O2 2.106(2) . ? Co1 O2 2.106(2) 4_556 ? O1 C1 1.248(3) . ? O2 C2 1.261(4) . ? O3 C2 1.238(4) . ? O3 Co1 2.083(2) 13_556 ? C1 O1 1.248(3) 12_655 ? C1 C1 1.555(8) 9_656 ? C2 C2 1.559(6) 13_556 ? N1 N1 0.685(8) 12 ? N1 C6 1.176(8) 12 ? N1 C6 1.503(8) . ? N1 C4 1.648(5) . ? C3 C4 1.395(9) . ? C3 C6 1.902(10) 12 ? C4 C6 1.463(8) 12 ? C4 C5 1.544(9) . ? C6 N1 1.176(8) 12 ? C6 C6 1.281(14) 12 ? C6 C4 1.463(8) 12 ? C6 C7 1.534(9) . ? C6 C7 1.897(10) 12 ? C6 C3 1.902(10) 12 ? C7 C7 0.974(15) 12 ? C7 C6 1.897(10) 12 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O3 90.42(13) 16_545 13_556 ? O3 Co1 O1 168.48(8) 16_545 . ? O3 Co1 O1 95.57(9) 13_556 . ? O3 Co1 O1 95.57(9) 16_545 4_556 ? O3 Co1 O1 168.48(8) 13_556 4_556 ? O1 Co1 O1 80.31(11) . 4_556 ? O3 Co1 O2 102.72(8) 16_545 . ? O3 Co1 O2 79.77(8) 13_556 . ? O1 Co1 O2 88.05(9) . . ? O1 Co1 O2 89.30(8) 4_556 . ? O3 Co1 O2 79.77(8) 16_545 4_556 ? O3 Co1 O2 102.72(8) 13_556 4_556 ? O1 Co1 O2 89.30(8) . 4_556 ? O1 Co1 O2 88.05(9) 4_556 4_556 ? O2 Co1 O2 176.54(12) . 4_556 ? C1 O1 Co1 112.4(2) . . ? C2 O2 Co1 113.05(19) . . ? C2 O3 Co1 113.50(19) . 13_556 ? O1 C1 O1 125.1(4) 12_655 . ? O1 C1 C1 117.46(18) 12_655 9_656 ? O1 C1 C1 117.46(18) . 9_656 ? O3 C2 O2 126.4(3) . . ? O3 C2 C2 117.8(3) . 13_556 ? O2 C2 C2 115.8(3) . 13_556 ? N1 N1 C6 104.7(4) 12 12 ? N1 N1 C6 49.2(3) 12 . ? C6 N1 C6 55.5(6) 12 . ? N1 N1 C4 164.2(2) 12 . ? C6 N1 C4 59.7(4) 12 . ? C6 N1 C4 115.1(4) . . ? C4 C3 C6 49.8(3) . 12 ? C3 C4 C6 83.4(5) . 12 ? C3 C4 C5 118.0(5) . . ? C6 C4 C5 144.3(5) 12 . ? C3 C4 N1 110.9(4) . . ? C6 C4 N1 43.9(3) 12 . ? C5 C4 N1 100.4(4) . . ? N1 C6 C6 75.3(4) 12 12 ? N1 C6 C4 76.4(5) 12 12 ? C6 C6 C4 151.7(3) 12 12 ? N1 C6 N1 26.2(3) 12 . ? C6 C6 N1 49.2(3) 12 . ? C4 C6 N1 102.6(5) 12 . ? N1 C6 C7 121.1(6) 12 . ? C6 C6 C7 84.3(4) 12 . ? C4 C6 C7 112.8(5) 12 . ? N1 C6 C7 111.0(5) . . ? N1 C6 C7 106.7(5) 12 12 ? C6 C6 C7 53.5(3) 12 12 ? C4 C6 C7 139.9(5) 12 12 ? N1 C6 C7 87.4(4) . 12 ? C7 C6 C7 30.7(5) . 12 ? N1 C6 C3 106.9(5) 12 12 ? C6 C6 C3 143.1(3) 12 12 ? C4 C6 C3 46.7(4) 12 12 ? N1 C6 C3 126.3(5) . 12 ? C7 C6 C3 121.1(5) . 12 ? C7 C6 C3 145.9(5) 12 12 ? C7 C7 C6 95.7(4) 12 . ? C7 C7 C6 53.5(3) 12 12 ? C6 C7 C6 42.2(5) . 12 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.579 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.088 # Attachment '- 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 884215' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H22 Mn2 N2 O17 P2' _chemical_formula_weight 602.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.6900(6) _cell_length_b 14.4331(8) _cell_length_c 29.8442(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4173.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6545 _cell_measurement_theta_min 2.8707 _cell_measurement_theta_max 29.2003 _exptl_crystal_description rod _exptl_crystal_colour light-pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67198 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15127 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3680 _reflns_number_gt 3115 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+4.6541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3680 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.13053(4) 0.23551(4) 0.700512(15) 0.02466(14) Uani 1 1 d . . . Mn2 Mn 0.24975(4) 0.45728(4) 0.546064(15) 0.02920(15) Uani 1 1 d . . . P1 P 0.06314(8) 0.29612(7) 0.59580(3) 0.0264(2) Uani 1 1 d . . . P2 P 0.28638(8) 0.53050(7) 0.65278(3) 0.0294(2) Uani 1 1 d . . . O1 O 0.3254(3) 0.5029(3) 0.60690(8) 0.0786(12) Uani 1 1 d . . . O2 O 0.3939(2) 0.49025(19) 0.68610(8) 0.0440(7) Uani 1 1 d . . . H1 H 0.3713 0.4375 0.6932 0.066 Uiso 1 1 calc R . . O3 O 0.1427(2) 0.49169(18) 0.66564(8) 0.0390(6) Uani 1 1 d . . . H2 H 0.1363 0.4379 0.6570 0.058 Uiso 1 1 calc R . . O4 O 0.2817(3) 0.6326(2) 0.65879(10) 0.0603(9) Uani 1 1 d . . . O5 O 0.1881(2) 0.3217(2) 0.56932(8) 0.0402(6) Uani 1 1 d . . . O6 O 0.0759(2) 0.32026(17) 0.64442(7) 0.0315(5) Uani 1 1 d . . . O7 O -0.0689(2) 0.34434(19) 0.57759(8) 0.0410(6) Uani 1 1 d . . . H3 H -0.0496 0.3968 0.5691 0.061 Uiso 1 1 calc R . . O8 O 0.0284(2) 0.19072(19) 0.58922(8) 0.0431(7) Uani 1 1 d . . . H4 H 0.0741 0.1597 0.6068 0.065 Uiso 1 1 calc R . . O9 O 0.4461(2) 0.39624(19) 0.52473(8) 0.0417(7) Uani 1 1 d . . . O10 O 0.6449(2) 0.4318(2) 0.49199(8) 0.0405(7) Uani 1 1 d . . . O11 O 0.1305(2) 0.42305(18) 0.48493(7) 0.0338(6) Uani 1 1 d . . . O12 O -0.0680(2) 0.45352(18) 0.45081(7) 0.0312(6) Uani 1 1 d . . . O13 O -0.0729(2) 0.17063(17) 0.70349(7) 0.0308(6) Uani 1 1 d . . . O14 O 0.0157(2) 0.31810(18) 0.75027(8) 0.0373(6) Uani 1 1 d . . . O15 O -0.2684(2) 0.1722(2) 0.74166(8) 0.0439(7) Uani 1 1 d . . . O16 O -0.1780(2) 0.31753(17) 0.78965(7) 0.0328(6) Uani 1 1 d . . . N1 N -0.5559(4) 0.2255(3) 0.58343(17) 0.0941(18) Uani 1 1 d . . . H5 H -0.6285 0.2630 0.5818 0.141 Uiso 1 1 calc R . . H6 H -0.5845 0.1676 0.5879 0.141 Uiso 1 1 calc R . . H7 H -0.5084 0.2284 0.5579 0.141 Uiso 1 1 calc R . . N2 N -0.2439(3) 0.0468(2) 0.65545(9) 0.0347(7) Uani 1 1 d . . . H2B H -0.1819 0.0851 0.6689 0.042 Uiso 1 1 calc R . . C1 C 0.5260(3) 0.4502(3) 0.50465(10) 0.0318(8) Uani 1 1 d . . . C2 C 0.0187(3) 0.4642(2) 0.48163(9) 0.0241(7) Uani 1 1 d . . . C3 C -0.1511(3) 0.2020(2) 0.73337(10) 0.0258(7) Uani 1 1 d . . . C4 C -0.0986(3) 0.2865(2) 0.76006(10) 0.0252(7) Uani 1 1 d . . . C5 C -0.4702(5) 0.2531(3) 0.61948(14) 0.0550(12) Uani 1 1 d . . . H8 H -0.5234 0.2508 0.6470 0.066 Uiso 1 1 calc R . . H9 H -0.4420 0.3168 0.6148 0.066 Uiso 1 1 calc R . . C6 C -0.3431(4) 0.1939(3) 0.62498(15) 0.0530(11) Uani 1 1 d . . . H10 H -0.3023 0.1834 0.5957 0.064 Uiso 1 1 calc R . . H11 H -0.2763 0.2273 0.6430 0.064 Uiso 1 1 calc R . . C7 C -0.3719(3) 0.1018(3) 0.64670(12) 0.0367(9) Uani 1 1 d . . . H12 H -0.4196 0.1121 0.6748 0.044 Uiso 1 1 calc R . . H13 H -0.4326 0.0661 0.6274 0.044 Uiso 1 1 calc R . . C8 C -0.2720(5) -0.0306(3) 0.68683(15) 0.0567(12) Uani 1 1 d . . . H14 H -0.3133 -0.0067 0.7137 0.085 Uiso 1 1 calc R . . H15 H -0.1871 -0.0613 0.6941 0.085 Uiso 1 1 calc R . . H16 H -0.3340 -0.0739 0.6730 0.085 Uiso 1 1 calc R . . C9 C -0.1801(4) 0.0122(3) 0.61348(13) 0.0503(11) Uani 1 1 d . . . H17 H -0.0977 -0.0218 0.6205 0.076 Uiso 1 1 calc R . . H18 H -0.1573 0.0637 0.5945 0.076 Uiso 1 1 calc R . . H19 H -0.2439 -0.0277 0.5982 0.076 Uiso 1 1 calc R . . OW1 O -0.2346(4) 0.2758(2) 0.52024(12) 0.0901(13) Uani 1 1 d . . . H20 H -0.3029 0.2201 0.5096 0.108 Uiso 1 1 d R . . H21 H -0.2805 0.3247 0.5075 0.108 Uiso 1 1 d R . . 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 Mn1 0.0195(2) 0.0266(3) 0.0279(3) 0.0027(2) -0.00005(17) -0.0014(2) Mn2 0.0228(2) 0.0393(4) 0.0255(3) -0.0010(2) 0.00197(18) 0.0017(2) P1 0.0248(4) 0.0241(5) 0.0304(4) 0.0014(4) -0.0045(3) 0.0017(3) P2 0.0303(4) 0.0304(6) 0.0276(4) 0.0031(4) -0.0059(3) -0.0097(4) O1 0.0385(14) 0.163(4) 0.0344(14) -0.0246(19) 0.0011(11) -0.0265(19) O2 0.0408(13) 0.0328(17) 0.0584(16) 0.0171(13) -0.0143(12) -0.0077(12) O3 0.0299(11) 0.0261(16) 0.0610(16) -0.0048(13) 0.0071(11) -0.0021(11) O4 0.0724(19) 0.0257(17) 0.083(2) 0.0154(16) -0.0431(16) -0.0154(14) O5 0.0340(12) 0.0455(18) 0.0411(13) 0.0072(13) 0.0058(10) 0.0092(12) O6 0.0392(12) 0.0254(15) 0.0299(11) 0.0016(11) -0.0041(9) -0.0019(11) O7 0.0352(12) 0.0290(16) 0.0586(16) 0.0028(13) -0.0126(11) 0.0068(11) O8 0.0511(14) 0.0265(16) 0.0515(15) -0.0012(13) -0.0208(12) 0.0021(12) O9 0.0327(12) 0.0423(18) 0.0500(14) 0.0133(13) 0.0134(11) 0.0069(12) O10 0.0249(11) 0.0468(19) 0.0498(14) 0.0095(13) 0.0092(10) 0.0092(11) O11 0.0324(12) 0.0415(17) 0.0274(11) -0.0076(11) -0.0004(9) 0.0076(11) O12 0.0296(11) 0.0365(16) 0.0276(11) -0.0105(11) -0.0019(9) 0.0002(10) O13 0.0235(10) 0.0340(16) 0.0350(12) -0.0129(11) 0.0050(9) -0.0050(10) O14 0.0295(11) 0.0389(17) 0.0436(13) -0.0152(12) 0.0079(10) -0.0121(11) O15 0.0284(12) 0.051(2) 0.0529(15) -0.0253(14) 0.0129(10) -0.0159(12) O16 0.0283(11) 0.0288(15) 0.0414(13) -0.0144(11) 0.0077(10) -0.0049(10) N1 0.068(2) 0.038(3) 0.176(5) -0.031(3) -0.070(3) 0.018(2) N2 0.0322(14) 0.0301(19) 0.0418(16) -0.0027(14) -0.0088(12) -0.0076(13) C1 0.0271(16) 0.044(3) 0.0241(15) 0.0032(16) -0.0004(13) 0.0029(15) C2 0.0244(15) 0.028(2) 0.0198(14) 0.0003(14) 0.0041(11) -0.0029(14) C3 0.0227(14) 0.026(2) 0.0286(16) -0.0031(15) -0.0004(12) -0.0005(14) C4 0.0236(15) 0.022(2) 0.0305(17) -0.0018(15) -0.0028(12) 0.0008(13) C5 0.079(3) 0.038(3) 0.049(2) -0.010(2) -0.016(2) 0.014(2) C6 0.044(2) 0.047(3) 0.068(3) 0.012(2) -0.0220(19) -0.012(2) C7 0.0300(16) 0.040(3) 0.0403(19) 0.0024(18) -0.0014(14) -0.0034(16) C8 0.070(3) 0.040(3) 0.060(3) 0.012(2) -0.011(2) -0.008(2) C9 0.0404(19) 0.050(3) 0.060(2) -0.019(2) -0.0039(18) -0.003(2) OW1 0.141(3) 0.033(2) 0.096(3) -0.0064(19) -0.074(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.116(3) 8_655 ? Mn1 O6 2.140(2) . ? Mn1 O13 2.184(2) . ? Mn1 O15 2.185(2) 6_657 ? Mn1 O14 2.205(2) . ? Mn1 O16 2.220(2) 6_657 ? Mn2 O1 2.066(3) . ? Mn2 O5 2.161(3) . ? Mn2 O12 2.184(2) 5_566 ? Mn2 O9 2.191(2) . ? Mn2 O10 2.213(3) 5_666 ? Mn2 O11 2.215(2) . ? P1 O5 1.492(2) . ? P1 O6 1.497(2) . ? P1 O7 1.555(2) . ? P1 O8 1.570(3) . ? P2 O1 1.475(3) . ? P2 O4 1.486(3) . ? P2 O3 1.549(2) . ? P2 O2 1.553(2) . ? O2 H1 0.8200 . ? O3 H2 0.8200 . ? O4 Mn1 2.116(3) 8_665 ? O7 H3 0.8200 . ? O8 H4 0.8200 . ? O9 C1 1.252(4) . ? O10 C1 1.242(4) . ? O10 Mn2 2.213(3) 5_666 ? O11 C2 1.240(4) . ? O12 C2 1.255(3) . ? O12 Mn2 2.184(2) 5_566 ? O13 C3 1.255(4) . ? O14 C4 1.233(4) . ? O15 C3 1.240(4) . ? O15 Mn1 2.185(2) 6_557 ? O16 C4 1.253(4) . ? O16 Mn1 2.220(2) 6_557 ? N1 C5 1.416(5) . ? N1 H5 0.8900 . ? N1 H6 0.8900 . ? N1 H7 0.8900 . ? N2 C8 1.483(5) . ? N2 C9 1.483(5) . ? N2 C7 1.496(4) . ? N2 H2B 0.9100 . ? C1 C1 1.547(7) 5_666 ? C2 C2 1.549(6) 5_566 ? C3 C4 1.544(5) . ? C5 C6 1.508(6) . ? C5 H8 0.9700 . ? C5 H9 0.9700 . ? C6 C7 1.506(6) . ? C6 H10 0.9700 . ? C6 H11 0.9700 . ? C7 H12 0.9700 . ? C7 H13 0.9700 . ? C8 H14 0.9600 . ? C8 H15 0.9600 . ? C8 H16 0.9600 . ? C9 H17 0.9600 . ? C9 H18 0.9600 . ? C9 H19 0.9600 . ? OW1 H20 1.0885 . ? OW1 H21 0.9168 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O6 92.30(10) 8_655 . ? O4 Mn1 O13 94.91(10) 8_655 . ? O6 Mn1 O13 93.08(9) . . ? O4 Mn1 O15 89.49(12) 8_655 6_657 ? O6 Mn1 O15 165.49(9) . 6_657 ? O13 Mn1 O15 101.11(9) . 6_657 ? O4 Mn1 O14 168.00(10) 8_655 . ? O6 Mn1 O14 95.34(9) . . ? O13 Mn1 O14 75.47(8) . . ? O15 Mn1 O14 85.43(10) 6_657 . ? O4 Mn1 O16 96.67(11) 8_655 6_657 ? O6 Mn1 O16 90.32(8) . 6_657 ? O13 Mn1 O16 167.79(9) . 6_657 ? O15 Mn1 O16 75.18(8) 6_657 6_657 ? O14 Mn1 O16 92.54(9) . 6_657 ? O1 Mn2 O5 96.01(13) . . ? O1 Mn2 O12 93.49(11) . 5_566 ? O5 Mn2 O12 107.28(9) . 5_566 ? O1 Mn2 O9 94.32(11) . . ? O5 Mn2 O9 88.24(9) . . ? O12 Mn2 O9 161.77(9) 5_566 . ? O1 Mn2 O10 93.24(12) . 5_666 ? O5 Mn2 O10 161.43(9) . 5_666 ? O12 Mn2 O10 88.14(9) 5_566 5_666 ? O9 Mn2 O10 75.00(9) . 5_666 ? O1 Mn2 O11 168.52(11) . . ? O5 Mn2 O11 85.32(10) . . ? O12 Mn2 O11 75.28(8) 5_566 . ? O9 Mn2 O11 97.12(9) . . ? O10 Mn2 O11 88.82(9) 5_666 . ? O5 P1 O6 112.87(14) . . ? O5 P1 O7 111.85(14) . . ? O6 P1 O7 107.60(14) . . ? O5 P1 O8 110.32(15) . . ? O6 P1 O8 111.36(14) . . ? O7 P1 O8 102.33(14) . . ? O1 P2 O4 112.8(2) . . ? O1 P2 O3 111.28(15) . . ? O4 P2 O3 107.56(17) . . ? O1 P2 O2 108.73(18) . . ? O4 P2 O2 108.32(15) . . ? O3 P2 O2 108.00(14) . . ? P2 O1 Mn2 144.16(16) . . ? P2 O2 H1 109.5 . . ? P2 O3 H2 109.5 . . ? P2 O4 Mn1 139.03(16) . 8_665 ? P1 O5 Mn2 128.22(15) . . ? P1 O6 Mn1 130.21(15) . . ? P1 O7 H3 109.5 . . ? P1 O8 H4 109.5 . . ? C1 O9 Mn2 115.2(2) . . ? C1 O10 Mn2 115.4(2) . 5_666 ? C2 O11 Mn2 114.48(19) . . ? C2 O12 Mn2 115.8(2) . 5_566 ? C3 O13 Mn1 114.8(2) . . ? C4 O14 Mn1 114.4(2) . . ? C3 O15 Mn1 115.0(2) . 6_557 ? C4 O16 Mn1 114.6(2) . 6_557 ? C5 N1 H5 109.5 . . ? C5 N1 H6 109.5 . . ? H5 N1 H6 109.5 . . ? C5 N1 H7 109.5 . . ? H5 N1 H7 109.5 . . ? H6 N1 H7 109.5 . . ? C8 N2 C9 110.9(3) . . ? C8 N2 C7 110.9(3) . . ? C9 N2 C7 112.1(3) . . ? C8 N2 H2B 107.5 . . ? C9 N2 H2B 107.5 . . ? C7 N2 H2B 107.5 . . ? O10 C1 O9 125.9(4) . . ? O10 C1 C1 116.5(4) . 5_666 ? O9 C1 C1 117.6(3) . 5_666 ? O11 C2 O12 125.7(3) . . ? O11 C2 C2 117.9(3) . 5_566 ? O12 C2 C2 116.4(3) . 5_566 ? O15 C3 O13 124.8(3) . . ? O15 C3 C4 118.3(3) . . ? O13 C3 C4 116.9(3) . . ? O14 C4 O16 125.9(3) . . ? O14 C4 C3 117.8(3) . . ? O16 C4 C3 116.3(3) . . ? N1 C5 C6 113.7(4) . . ? N1 C5 H8 108.8 . . ? C6 C5 H8 108.8 . . ? N1 C5 H9 108.8 . . ? C6 C5 H9 108.8 . . ? H8 C5 H9 107.7 . . ? C7 C6 C5 113.3(3) . . ? C7 C6 H10 108.9 . . ? C5 C6 H10 108.9 . . ? C7 C6 H11 108.9 . . ? C5 C6 H11 108.9 . . ? H10 C6 H11 107.7 . . ? N2 C7 C6 113.0(3) . . ? N2 C7 H12 109.0 . . ? C6 C7 H12 109.0 . . ? N2 C7 H13 109.0 . . ? C6 C7 H13 109.0 . . ? H12 C7 H13 107.8 . . ? N2 C8 H14 109.5 . . ? N2 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? N2 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? N2 C9 H17 109.5 . . ? N2 C9 H18 109.5 . . ? H17 C9 H18 109.5 . . ? N2 C9 H19 109.5 . . ? H17 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? H20 OW1 H21 98.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H1 O16 0.82 1.87 2.688(4) 178.9 6_657 O3 H2 O6 0.82 1.84 2.635(4) 164.7 . O8 H4 O4 0.82 2.12 2.898(4) 157.4 8_655 N1 H5 O5 0.89 2.00 2.874(4) 165.8 1_455 N1 H6 O12 0.89 2.10 2.781(5) 132.4 4_456 N2 H2B O13 0.91 1.92 2.828(4) 171.4 . OW1 H20 O11 1.09 2.17 3.158(4) 149.6 4_456 OW1 H21 O10 0.92 1.77 2.672(4) 168.5 1_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.071 # Attachment '- 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 884216' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12.80 N2 O7.40 Zn' _chemical_formula_weight 320.77 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.884(3) _cell_length_b 12.146(2) _cell_length_c 16.327(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.50(3) _cell_angle_gamma 90.00 _cell_volume 2505.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72437 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9114 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2197 _reflns_number_gt 1855 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+2.8353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2197 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 0.42955(3) 0.20855(3) 0.47951(3) 0.04322(18) Uani 1 1 d . . . O1 O 0.46661(18) 0.08792(17) 0.40780(15) 0.0435(5) Uani 1 1 d . . . O2 O 0.5127(2) -0.08829(18) 0.42142(15) 0.0495(6) Uani 1 1 d . . . O3 O 0.3775(2) 0.29959(18) 0.56128(17) 0.0490(6) Uani 1 1 d . . . O4 O 0.22838(19) 0.3385(2) 0.57417(17) 0.0519(6) Uani 1 1 d . . . O5 O 0.56533(18) 0.30080(19) 0.51829(17) 0.0533(7) Uani 1 1 d . . . O6 O 0.3887(2) 0.3257(2) 0.36883(17) 0.0559(6) Uani 1 1 d . . . O7 O 0.6266(2) 0.4591(2) 0.4910(2) 0.0712(8) Uani 1 1 d . . . N1 N 0.4466(3) 0.4917(3) 0.3445(2) 0.0630(9) Uani 1 1 d . . . H1A H 0.4977 0.5384 0.3639 0.076 Uiso 1 1 calc R . . N2 N 0.2309(2) 0.5722(3) 0.3352(2) 0.0618(9) Uani 1 1 d . . . H2A H 0.2829 0.5589 0.3908 0.074 Uiso 1 1 calc R . . C1 C 0.4939(2) -0.0003(3) 0.4510(2) 0.0364(7) Uani 1 1 d . . . C2 C 0.2804(3) 0.2898(2) 0.5392(2) 0.0407(8) Uani 1 1 d . . . C3 C 0.5593(3) 0.3858(3) 0.4733(3) 0.0498(9) Uani 1 1 d . . . C4 C 0.4563(3) 0.3995(3) 0.3896(3) 0.0495(9) Uani 1 1 d . . . C5 C 0.3531(4) 0.5181(4) 0.2631(3) 0.0738(13) Uani 1 1 d . . . H5A H 0.3119 0.4515 0.2411 0.089 Uiso 1 1 calc R . . H5B H 0.3757 0.5429 0.2174 0.089 Uiso 1 1 calc R . . C6 C 0.2832(3) 0.6046(4) 0.2756(3) 0.0674(12) Uani 1 1 d . . . H6A H 0.3254 0.6700 0.3003 0.081 Uiso 1 1 calc R . . H6B H 0.2289 0.6239 0.2169 0.081 Uiso 1 1 calc R . . C7 C 0.1680(4) 0.6677(5) 0.3436(4) 0.101(2) Uani 1 1 d . . . H7A H 0.1340 0.6481 0.3821 0.152 Uiso 1 1 calc R . . H7B H 0.1154 0.6872 0.2852 0.152 Uiso 1 1 calc R . . H7C H 0.2142 0.7293 0.3690 0.152 Uiso 1 1 calc R . . C8 C 0.1655(3) 0.4704(4) 0.3059(4) 0.0870(15) Uani 1 1 d . . . H8A H 0.1352 0.4539 0.3477 0.130 Uiso 1 1 calc R . . H8B H 0.2093 0.4101 0.3041 0.130 Uiso 1 1 calc R . . H8C H 0.1100 0.4816 0.2471 0.130 Uiso 1 1 calc R . . OW1 O 0.5000 0.2960(10) 0.7500 0.101(4) Uani 0.50 2 d SP . . OW2 O 0.2817(16) 0.8984(17) 0.4190(15) 0.080(6) Uani 0.15 1 d P . . 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 0.0541(3) 0.0318(2) 0.0440(3) 0.00306(15) 0.0204(2) 0.00919(16) O1 0.0602(14) 0.0349(12) 0.0420(13) 0.0097(10) 0.0279(12) 0.0129(10) O2 0.0735(16) 0.0397(13) 0.0389(13) 0.0042(10) 0.0270(12) 0.0180(11) O3 0.0540(15) 0.0428(14) 0.0469(15) -0.0093(10) 0.0178(12) 0.0066(10) O4 0.0609(15) 0.0469(14) 0.0522(15) -0.0167(12) 0.0279(13) 0.0047(12) O5 0.0497(14) 0.0405(15) 0.0616(18) 0.0123(11) 0.0148(14) 0.0061(10) O6 0.0615(16) 0.0458(14) 0.0482(15) 0.0096(12) 0.0107(13) 0.0063(13) O7 0.0589(16) 0.0564(17) 0.092(2) 0.0176(15) 0.0249(16) -0.0051(14) N1 0.067(2) 0.058(2) 0.077(2) 0.0305(17) 0.0426(19) 0.0207(16) N2 0.0411(16) 0.082(2) 0.064(2) 0.0304(18) 0.0235(16) 0.0122(16) C1 0.0412(16) 0.0353(17) 0.0368(18) 0.0034(13) 0.0202(14) 0.0063(13) C2 0.057(2) 0.0276(16) 0.0360(18) 0.0035(13) 0.0176(17) 0.0095(14) C3 0.0492(19) 0.042(2) 0.061(2) 0.0076(18) 0.0259(18) 0.0107(17) C4 0.058(2) 0.043(2) 0.054(2) 0.0107(17) 0.0299(19) 0.0146(17) C5 0.087(3) 0.081(3) 0.066(3) 0.040(2) 0.044(3) 0.036(2) C6 0.063(2) 0.079(3) 0.069(3) 0.041(2) 0.036(2) 0.025(2) C7 0.079(3) 0.117(4) 0.133(5) 0.055(4) 0.068(4) 0.045(3) C8 0.056(2) 0.111(4) 0.081(3) 0.036(3) 0.016(2) -0.004(3) OW1 0.059(5) 0.194(12) 0.029(4) 0.000 -0.003(4) 0.000 OW2 0.064(12) 0.075(13) 0.089(16) 0.003(11) 0.020(11) 0.005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.054(2) . ? Zn1 O1 2.069(2) . ? Zn1 O4 2.075(3) 7_556 ? Zn1 O2 2.078(2) 5_656 ? Zn1 O3 2.080(2) . ? Zn1 O6 2.182(2) . ? O1 C1 1.252(4) . ? O2 C1 1.244(4) . ? O2 Zn1 2.078(2) 5_656 ? O3 C2 1.249(4) . ? O4 C2 1.241(4) . ? O4 Zn1 2.075(3) 7_556 ? O5 C3 1.249(4) . ? O6 C4 1.240(4) . ? O7 C3 1.235(4) . ? N1 C4 1.316(5) . ? N1 C5 1.456(5) . ? N1 H1A 0.8600 . ? N2 C6 1.490(5) . ? N2 C8 1.491(6) . ? N2 C7 1.493(6) . ? N2 H2A 0.9100 . ? C1 C1 1.537(6) 5_656 ? C2 C2 1.545(6) 7_556 ? C3 C4 1.522(5) . ? C5 C6 1.500(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O1 98.56(10) . . ? O5 Zn1 O4 162.53(10) . 7_556 ? O1 Zn1 O4 91.91(9) . 7_556 ? O5 Zn1 O2 97.75(10) . 5_656 ? O1 Zn1 O2 80.58(9) . 5_656 ? O4 Zn1 O2 97.73(11) 7_556 5_656 ? O5 Zn1 O3 91.77(10) . . ? O1 Zn1 O3 166.80(9) . . ? O4 Zn1 O3 80.21(9) 7_556 . ? O2 Zn1 O3 89.93(9) 5_656 . ? O5 Zn1 O6 77.85(10) . . ? O1 Zn1 O6 91.89(10) . . ? O4 Zn1 O6 87.91(11) 7_556 . ? O2 Zn1 O6 170.70(10) 5_656 . ? O3 Zn1 O6 98.34(10) . . ? C1 O1 Zn1 112.04(19) . . ? C1 O2 Zn1 112.2(2) . 5_656 ? C2 O3 Zn1 112.6(2) . . ? C2 O4 Zn1 112.9(2) . 7_556 ? C3 O5 Zn1 116.1(2) . . ? C4 O6 Zn1 109.7(2) . . ? C4 N1 C5 123.0(4) . . ? C4 N1 H1A 118.5 . . ? C5 N1 H1A 118.5 . . ? C6 N2 C8 114.0(4) . . ? C6 N2 C7 108.5(3) . . ? C8 N2 C7 111.9(4) . . ? C6 N2 H2A 107.4 . . ? C8 N2 H2A 107.4 . . ? C7 N2 H2A 107.4 . . ? O2 C1 O1 125.4(3) . . ? O2 C1 C1 117.2(3) . 5_656 ? O1 C1 C1 117.3(3) . 5_656 ? O4 C2 O3 125.9(3) . . ? O4 C2 C2 117.2(4) . 7_556 ? O3 C2 C2 116.9(4) . 7_556 ? O7 C3 O5 126.7(4) . . ? O7 C3 C4 117.9(3) . . ? O5 C3 C4 115.3(3) . . ? O6 C4 N1 124.9(4) . . ? O6 C4 C3 119.3(3) . . ? N1 C4 C3 115.9(3) . . ? N1 C5 C6 114.4(4) . . ? N1 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? N1 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N2 C6 C5 114.9(3) . . ? N2 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N2 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.730 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.070