# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H74 Mn4 N4 O26' _chemical_formula_weight 1462.97 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' Mn Mn 0.3368 0.7283 '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 8.792(4) _cell_length_b 11.024(5) _cell_length_c 16.479(7) _cell_angle_alpha 84.580(7) _cell_angle_beta 85.459(7) _cell_angle_gamma 78.893(7) _cell_volume 1557.0(11) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8435 _exptl_absorpt_correction_T_max 0.9171 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7729 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5443 _reflns_number_gt 3763 _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^)+(0.0843P)^2^+3.2767P] 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 5443 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1601 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Mn1 Mn 0.10030(10) 0.35995(7) 0.47994(5) 0.0229(2) Uani 1 1 d . . . Mn2 Mn -0.07490(11) 0.51103(8) 0.31982(5) 0.0315(3) Uani 1 1 d . . . O2 O 0.0826(5) 0.2189(3) 0.3993(2) 0.0352(10) Uani 1 1 d . . . C8 C 0.0020(6) 0.0036(5) 0.0842(3) 0.0224(12) Uani 1 1 d . . . O1 O -0.0455(6) 0.3229(4) 0.2952(3) 0.0533(13) Uani 1 1 d . . . C7 C 0.0155(6) 0.1090(5) 0.2112(3) 0.0245(12) Uani 1 1 d . . . H7 H 0.0200 0.1822 0.1789 0.029 Uiso 1 1 calc R . . C3 C 0.0133(6) -0.0015(5) 0.3436(3) 0.0227(11) Uani 1 1 d . . . H3 H 0.0223 -0.0050 0.3997 0.027 Uiso 1 1 calc R . . O6 O 0.5524(5) -0.1803(4) 0.0648(3) 0.0479(12) Uani 1 1 d . . . O3 O -0.0784(6) -0.2992(4) 0.3213(2) 0.0464(12) Uani 1 1 d . . . O7 O -0.0659(5) 0.5555(4) 0.1843(2) 0.0447(11) Uani 1 1 d . . . C9 C 0.1374(7) -0.0450(5) 0.0404(3) 0.0243(12) Uani 1 1 d . . . C13 C -0.1355(6) 0.0487(5) 0.0463(3) 0.0242(12) Uani 1 1 d . . . O5 O -0.5503(5) 0.1856(4) 0.0898(3) 0.0484(12) Uani 1 1 d . . . C6 C 0.0044(6) 0.0048(5) 0.1748(3) 0.0225(11) Uani 1 1 d . . . C5 C -0.0106(6) -0.1022(5) 0.2249(3) 0.0257(12) Uani 1 1 d . . . H5 H -0.0232 -0.1728 0.2013 0.031 Uiso 1 1 calc R . . C4 C -0.0073(6) -0.1054(5) 0.3078(3) 0.0210(11) Uani 1 1 d . . . C2 C 0.0204(6) 0.1079(5) 0.2955(3) 0.0241(12) Uani 1 1 d . . . C14 C -0.2770(7) 0.0973(5) 0.0902(3) 0.0294(13) Uani 1 1 d . . . H14 H -0.2773 0.1005 0.1464 0.035 Uiso 1 1 calc R . . C10 C 0.2797(7) -0.0899(5) 0.0774(3) 0.0295(13) Uani 1 1 d . . . H10 H 0.2823 -0.0875 0.1336 0.035 Uiso 1 1 calc R . . C15 C -0.4102(7) 0.1389(5) 0.0528(3) 0.0325(13) Uani 1 1 d . . . C1 C 0.0231(7) 0.2257(5) 0.3335(3) 0.0291(13) Uani 1 1 d . . . N1 N -0.1562(7) 0.5905(5) 0.0573(3) 0.0435(13) Uani 1 1 d . . . O8 O 0.3310(5) 0.2674(5) 0.5195(3) 0.0614(15) Uani 1 1 d . . . C11 C 0.4108(7) -0.1357(5) 0.0346(3) 0.0340(14) Uani 1 1 d . . . C17 C -0.1467(8) 0.5336(6) 0.1316(4) 0.0378(15) Uani 1 1 d . . . C18 C -0.2522(9) 0.4397(7) 0.1406(4) 0.0530(18) Uani 1 1 d . . . H18A H -0.1924 0.3560 0.1468 0.064 Uiso 1 1 calc R . . H18B H -0.3250 0.4531 0.1877 0.064 Uiso 1 1 calc R . . C12 C 0.5611(8) -0.1833(7) 0.1508(4) 0.0500(18) Uani 1 1 d . . . H12A H 0.6647 -0.2195 0.1651 0.075 Uiso 1 1 calc R . . H12B H 0.4897 -0.2320 0.1778 0.075 Uiso 1 1 calc R . . H12C H 0.5347 -0.1003 0.1675 0.075 Uiso 1 1 calc R . . C20 C -0.2609(10) 0.5490(7) 0.0067(4) 0.059(2) Uani 1 1 d . . . H20A H -0.2041 0.5080 -0.0392 0.071 Uiso 1 1 calc R . . H20B H -0.3377 0.6181 -0.0139 0.071 Uiso 1 1 calc R . . C21 C -0.0804(9) 0.6928(7) 0.0284(4) 0.0571(19) Uani 1 1 d . . . H21A H -0.1569 0.7674 0.0219 0.086 Uiso 1 1 calc R . . H21B H -0.0251 0.6764 -0.0232 0.086 Uiso 1 1 calc R . . H21C H -0.0088 0.7028 0.0672 0.086 Uiso 1 1 calc R . . N2 N 0.5756(8) 0.1568(7) 0.5242(5) 0.077(2) Uani 1 1 d . . . C16 C -0.5554(9) 0.1969(8) 0.1750(4) 0.061(2) Uani 1 1 d . . . H16A H -0.4798 0.2442 0.1864 0.092 Uiso 1 1 calc R . . H16B H -0.5328 0.1158 0.2032 0.092 Uiso 1 1 calc R . . H16C H -0.6571 0.2381 0.1931 0.092 Uiso 1 1 calc R . . C22 C 0.4435(9) 0.2081(7) 0.4898(5) 0.0564(19) Uani 1 1 d . . . C24 C 0.6321(12) 0.1190(16) 0.3870(7) 0.149(6) Uani 1 1 d . . . H24A H 0.6870 0.1700 0.3485 0.179 Uiso 1 1 calc R . . H24B H 0.6378 0.0394 0.3652 0.179 Uiso 1 1 calc R . . C19 C -0.3361(12) 0.4600(9) 0.0631(5) 0.085(3) Uani 1 1 d . . . H19A H -0.3281 0.3822 0.0386 0.102 Uiso 1 1 calc R . . H19B H -0.4451 0.4943 0.0743 0.102 Uiso 1 1 calc R . . C23 C 0.4690(11) 0.1802(10) 0.4010(5) 0.087(3) Uani 1 1 d . . . H23A H 0.4001 0.1263 0.3888 0.104 Uiso 1 1 calc R . . H23B H 0.4474 0.2565 0.3659 0.104 Uiso 1 1 calc R . . C25 C 0.7051(10) 0.1012(11) 0.4714(7) 0.100(4) Uani 1 1 d . . . H25A H 0.7394 0.0141 0.4881 0.120 Uiso 1 1 calc R . . H25B H 0.7919 0.1440 0.4705 0.120 Uiso 1 1 calc R . . O9 O 0.1692(5) 0.4680(4) 0.3589(2) 0.0388(10) Uani 1 1 d . . . C27 C 0.2889(8) 0.4978(7) 0.3245(5) 0.056(2) Uani 1 1 d . . . C28 C 0.2882(11) 0.5624(10) 0.2430(5) 0.090(3) Uani 1 1 d . . . H28A H 0.2508 0.5147 0.2057 0.136 Uiso 1 1 calc R . . H28B H 0.3918 0.5728 0.2250 0.136 Uiso 1 1 calc R . . H28C H 0.2216 0.6423 0.2445 0.136 Uiso 1 1 calc R . . C26 C 0.5930(14) 0.1662(12) 0.6122(7) 0.124(5) Uani 1 1 d . . . H26A H 0.6599 0.2238 0.6178 0.185 Uiso 1 1 calc R . . H26B H 0.6373 0.0861 0.6370 0.185 Uiso 1 1 calc R . . H26C H 0.4929 0.1946 0.6387 0.185 Uiso 1 1 calc R . . O11 O 0.1148(4) 0.5166(3) 0.5493(2) 0.0257(8) Uani 1 1 d . . . H11 H 0.2069 0.5532 0.5329 0.031 Uiso 1 1 calc R . . O1W O -0.3339(6) 0.5775(6) 0.3203(3) 0.0691(15) Uani 1 1 d . . . H1WA H -0.3624 0.6446 0.3465 0.104 Uiso 1 1 d R . . H1WB H -0.3828 0.5205 0.3445 0.104 Uiso 1 1 d R . . C1A C -0.0302(7) -0.2227(5) 0.3582(3) 0.0260(12) Uani 1 1 d . . . O4 O -0.0044(5) -0.2345(4) 0.4320(2) 0.0367(10) Uani 1 1 d . . . O10 O 0.4157(8) 0.4740(9) 0.3561(5) 0.134(3) Uani 1 1 d . . . O2W O 0.4088(17) 0.5659(15) 0.5039(9) 0.116(5) Uani 0.50 1 d P . . H2WA H 0.4321 0.5248 0.4621 0.139 Uiso 0.50 1 d PR . . H2WB H 0.4762 0.5392 0.5388 0.139 Uiso 0.50 1 d PR . . 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 0.0303(5) 0.0200(4) 0.0191(4) -0.0018(3) -0.0041(3) -0.0055(3) Mn2 0.0455(6) 0.0220(5) 0.0293(5) -0.0024(3) -0.0117(4) -0.0080(4) O2 0.062(3) 0.026(2) 0.020(2) -0.0047(16) -0.0119(19) -0.0106(19) C8 0.036(3) 0.020(3) 0.013(2) 0.001(2) -0.001(2) -0.011(2) O1 0.090(4) 0.026(2) 0.045(3) -0.005(2) -0.030(3) -0.001(2) C7 0.035(3) 0.018(3) 0.018(3) 0.004(2) -0.003(2) 0.000(2) C3 0.034(3) 0.021(3) 0.011(2) -0.003(2) 0.002(2) -0.002(2) O6 0.041(3) 0.063(3) 0.034(2) -0.008(2) -0.007(2) 0.006(2) O3 0.086(4) 0.028(2) 0.031(2) 0.0001(18) -0.006(2) -0.025(2) O7 0.055(3) 0.053(3) 0.030(2) -0.004(2) -0.008(2) -0.019(2) C9 0.039(3) 0.019(3) 0.015(3) 0.000(2) -0.003(2) -0.007(2) C13 0.038(3) 0.019(3) 0.017(3) -0.003(2) -0.004(2) -0.007(2) O5 0.042(3) 0.063(3) 0.035(2) -0.011(2) 0.006(2) 0.005(2) C6 0.031(3) 0.022(3) 0.015(3) -0.005(2) -0.006(2) -0.003(2) C5 0.039(3) 0.017(3) 0.021(3) -0.005(2) -0.001(2) -0.004(2) C4 0.029(3) 0.020(3) 0.013(2) -0.0018(19) 0.000(2) -0.003(2) C2 0.035(3) 0.019(3) 0.018(3) -0.005(2) -0.001(2) -0.004(2) C14 0.043(4) 0.029(3) 0.016(3) -0.005(2) 0.001(3) -0.007(3) C10 0.044(4) 0.029(3) 0.016(3) 0.000(2) -0.004(3) -0.006(3) C15 0.040(4) 0.031(3) 0.024(3) -0.002(2) 0.003(3) -0.003(3) C1 0.045(4) 0.025(3) 0.019(3) -0.003(2) -0.002(3) -0.009(3) N1 0.058(4) 0.042(3) 0.032(3) -0.001(2) -0.007(3) -0.011(3) O8 0.029(3) 0.061(3) 0.091(4) -0.027(3) -0.003(3) 0.010(2) C11 0.040(4) 0.034(3) 0.028(3) -0.001(3) -0.009(3) -0.004(3) C17 0.045(4) 0.038(3) 0.029(3) -0.006(3) -0.004(3) -0.002(3) C18 0.063(5) 0.049(4) 0.052(4) 0.003(3) -0.018(4) -0.021(4) C12 0.052(4) 0.060(5) 0.037(4) -0.009(3) -0.015(3) -0.002(4) C20 0.084(6) 0.055(5) 0.037(4) 0.000(3) -0.026(4) 0.000(4) C21 0.075(5) 0.046(4) 0.049(4) -0.001(3) 0.007(4) -0.013(4) N2 0.053(4) 0.089(5) 0.086(5) -0.029(4) -0.007(4) 0.010(4) C16 0.062(5) 0.075(5) 0.041(4) -0.009(4) 0.015(4) 0.000(4) C22 0.039(4) 0.057(5) 0.072(5) -0.006(4) -0.005(4) -0.005(4) C24 0.058(7) 0.281(19) 0.086(8) -0.046(10) 0.001(6) 0.037(9) C19 0.094(7) 0.100(7) 0.074(6) 0.013(5) -0.043(5) -0.044(6) C23 0.078(7) 0.112(8) 0.061(6) -0.019(5) 0.004(5) 0.010(6) C25 0.040(5) 0.127(9) 0.128(9) -0.040(7) 0.009(6) 0.006(5) O9 0.035(2) 0.043(2) 0.041(2) -0.0001(19) 0.002(2) -0.017(2) C27 0.036(4) 0.064(5) 0.070(5) 0.014(4) -0.013(4) -0.017(4) C28 0.069(6) 0.133(9) 0.068(6) 0.035(6) 0.006(5) -0.040(6) C26 0.121(10) 0.153(12) 0.095(8) -0.032(8) -0.059(8) 0.011(8) O11 0.032(2) 0.0217(19) 0.0243(19) -0.0038(15) -0.0028(16) -0.0057(16) O1W 0.047(3) 0.087(4) 0.073(4) -0.007(3) -0.001(3) -0.013(3) C1A 0.037(3) 0.020(3) 0.020(3) -0.001(2) 0.001(2) -0.006(2) O4 0.062(3) 0.032(2) 0.019(2) 0.0052(16) -0.0053(19) -0.017(2) O10 0.057(4) 0.197(9) 0.147(7) 0.082(6) -0.031(4) -0.057(5) O2W 0.112(12) 0.144(14) 0.109(11) -0.019(10) -0.027(10) -0.050(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 Mn1 O4 2.146(4) 2_556 ? Mn1 O11 2.165(4) 2_566 ? Mn1 O2 2.174(4) . ? Mn1 O11 2.188(3) . ? Mn1 O8 2.206(5) . ? Mn1 O9 2.323(4) . ? Mn2 O3 2.088(4) 1_565 ? Mn2 O1 2.114(4) . ? Mn2 O11 2.160(4) 2_566 ? Mn2 O9 2.239(4) . ? Mn2 O7 2.240(4) . ? Mn2 O1W 2.253(5) . ? O2 C1 1.231(6) . ? C8 C9 1.384(7) . ? C8 C13 1.389(7) . ? C8 C6 1.496(7) . ? O1 C1 1.263(7) . ? C7 C6 1.368(7) . ? C7 C2 1.392(7) . ? C7 H7 0.9300 . ? C3 C4 1.384(7) . ? C3 C2 1.389(7) . ? C3 H3 0.9300 . ? O6 C11 1.362(7) . ? O6 C12 1.423(7) . ? O3 C1A 1.240(6) . ? O3 Mn2 2.088(4) 1_545 ? O7 C17 1.233(7) . ? C9 C10 1.418(8) . ? C9 C13 1.434(7) 2 ? C13 C14 1.425(8) . ? C13 C9 1.434(7) 2 ? O5 C15 1.359(7) . ? O5 C16 1.418(8) . ? C6 C5 1.396(7) . ? C5 C4 1.367(7) . ? C5 H5 0.9300 . ? C4 C1A 1.508(7) . ? C2 C1 1.498(7) . ? C14 C15 1.348(8) . ? C14 H14 0.9300 . ? C10 C11 1.340(8) . ? C10 H10 0.9300 . ? C15 C11 1.444(8) 2 ? N1 C17 1.324(8) . ? N1 C21 1.442(9) . ? N1 C20 1.452(9) . ? O8 C22 1.175(8) . ? C11 C15 1.444(8) 2 ? C17 C18 1.507(9) . ? C18 C19 1.503(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C20 C19 1.497(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N2 C22 1.335(10) . ? N2 C25 1.451(10) . ? N2 C26 1.484(12) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C22 C23 1.513(11) . ? C24 C23 1.474(12) . ? C24 C25 1.557(14) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? O9 C27 1.241(8) . ? C27 O10 1.240(9) . ? C27 C28 1.460(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O11 Mn2 2.160(4) 2_566 ? O11 Mn1 2.165(4) 2_566 ? O11 H11 0.9800 . ? O1W H1WA 0.8766 . ? O1W H1WB 0.8766 . ? C1A O4 1.244(6) . ? O4 Mn1 2.146(4) 2_556 ? O2W H2WA 0.8500 . ? O2W H2WB 0.8501 . ? 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 O11 97.88(16) 2_556 2_566 ? O4 Mn1 O2 81.63(15) 2_556 . ? O11 Mn1 O2 96.72(15) 2_566 . ? O4 Mn1 O11 103.87(14) 2_556 . ? O11 Mn1 O11 79.61(15) 2_566 . ? O2 Mn1 O11 173.69(14) . . ? O4 Mn1 O8 87.15(19) 2_556 . ? O11 Mn1 O8 168.43(16) 2_566 . ? O2 Mn1 O8 94.31(17) . . ? O11 Mn1 O8 89.08(16) . . ? O4 Mn1 O9 163.44(15) 2_556 . ? O11 Mn1 O9 77.08(14) 2_566 . ? O2 Mn1 O9 83.30(15) . . ? O11 Mn1 O9 90.85(14) . . ? O8 Mn1 O9 100.83(18) . . ? O3 Mn2 O1 168.30(19) 1_565 . ? O3 Mn2 O11 93.74(14) 1_565 2_566 ? O1 Mn2 O11 97.10(16) . 2_566 ? O3 Mn2 O9 90.57(17) 1_565 . ? O1 Mn2 O9 87.18(18) . . ? O11 Mn2 O9 79.02(15) 2_566 . ? O3 Mn2 O7 83.10(16) 1_565 . ? O1 Mn2 O7 86.68(17) . . ? O11 Mn2 O7 172.22(16) 2_566 . ? O9 Mn2 O7 108.04(16) . . ? O3 Mn2 O1W 81.7(2) 1_565 . ? O1 Mn2 O1W 103.6(2) . . ? O11 Mn2 O1W 84.86(17) 2_566 . ? O9 Mn2 O1W 161.62(18) . . ? O7 Mn2 O1W 87.65(18) . . ? C1 O2 Mn1 131.7(4) . . ? C9 C8 C13 121.5(5) . . ? C9 C8 C6 118.8(5) . . ? C13 C8 C6 119.6(5) . . ? C1 O1 Mn2 130.7(4) . . ? C6 C7 C2 121.6(5) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C11 O6 C12 116.9(5) . . ? C1A O3 Mn2 142.5(4) . 1_545 ? C17 O7 Mn2 131.3(4) . . ? C8 C9 C10 122.7(5) . . ? C8 C9 C13 119.2(5) . 2 ? C10 C9 C13 118.1(5) . 2 ? C8 C13 C14 122.7(5) . . ? C8 C13 C9 119.2(5) . 2 ? C14 C13 C9 118.1(5) . 2 ? C15 O5 C16 117.1(5) . . ? C7 C6 C5 118.2(5) . . ? C7 C6 C8 122.3(5) . . ? C5 C6 C8 119.5(4) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 C1A 118.4(4) . . ? C3 C4 C1A 121.7(4) . . ? C3 C2 C7 119.1(4) . . ? C3 C2 C1 120.9(4) . . ? C7 C2 C1 119.9(5) . . ? C15 C14 C13 122.1(5) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C11 C10 C9 122.4(5) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C14 C15 O5 126.1(5) . . ? C14 C15 C11 119.4(5) . 2 ? O5 C15 C11 114.5(5) . 2 ? O2 C1 O1 126.6(5) . . ? O2 C1 C2 118.5(5) . . ? O1 C1 C2 114.8(5) . . ? C17 N1 C21 124.4(6) . . ? C17 N1 C20 114.7(6) . . ? C21 N1 C20 120.7(6) . . ? C22 O8 Mn1 136.6(6) . . ? C10 C11 O6 126.5(5) . . ? C10 C11 C15 119.8(5) . 2 ? O6 C11 C15 113.7(5) . 2 ? O7 C17 N1 125.1(6) . . ? O7 C17 C18 126.4(6) . . ? N1 C17 C18 108.5(6) . . ? C19 C18 C17 104.9(6) . . ? C19 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? C19 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.8 . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C20 C19 104.0(6) . . ? N1 C20 H20A 110.9 . . ? C19 C20 H20A 110.9 . . ? N1 C20 H20B 110.9 . . ? C19 C20 H20B 110.9 . . ? H20A C20 H20B 109.0 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 N2 C25 117.6(8) . . ? C22 N2 C26 120.9(8) . . ? C25 N2 C26 121.3(8) . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O8 C22 N2 128.5(8) . . ? O8 C22 C23 125.5(8) . . ? N2 C22 C23 105.9(7) . . ? C23 C24 C25 106.6(8) . . ? C23 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? C23 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C20 C19 C18 107.0(6) . . ? C20 C19 H19A 110.3 . . ? C18 C19 H19A 110.3 . . ? C20 C19 H19B 110.3 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C24 C23 C22 107.8(8) . . ? C24 C23 H23A 110.1 . . ? C22 C23 H23A 110.1 . . ? C24 C23 H23B 110.1 . . ? C22 C23 H23B 110.1 . . ? H23A C23 H23B 108.5 . . ? N2 C25 C24 101.9(7) . . ? N2 C25 H25A 111.4 . . ? C24 C25 H25A 111.4 . . ? N2 C25 H25B 111.4 . . ? C24 C25 H25B 111.4 . . ? H25A C25 H25B 109.3 . . ? C27 O9 Mn2 129.8(5) . . ? C27 O9 Mn1 137.3(5) . . ? Mn2 O9 Mn1 92.86(15) . . ? O10 C27 O9 122.8(7) . . ? O10 C27 C28 115.9(7) . . ? O9 C27 C28 121.4(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Mn2 O11 Mn1 99.72(15) 2_566 2_566 ? Mn2 O11 Mn1 116.08(16) 2_566 . ? Mn1 O11 Mn1 100.39(15) 2_566 . ? Mn2 O11 H11 113.0 2_566 . ? Mn1 O11 H11 113.0 2_566 . ? Mn1 O11 H11 113.0 . . ? Mn2 O1W H1WA 111.0 . . ? Mn2 O1W H1WB 110.5 . . ? H1WA O1W H1WB 107.9 . . ? O3 C1A O4 125.3(5) . . ? O3 C1A C4 115.3(5) . . ? O4 C1A C4 119.3(5) . . ? C1A O4 Mn1 123.7(4) . 2_556 ? H2WA O2W H2WB 108.9 . . ? 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 O11 H11 O2W 0.98 1.83 2.774(15) 160.6 . O2W H2WA O10 0.85 1.91 2.717(18) 158.5 . O1W H1WB O10 0.88 1.93 2.671(8) 141.7 1_455 O2W H2WB O10 0.85 2.02 2.830(16) 158.6 2_666 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.844 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 967536' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 N0 Ni2 O22' _chemical_formula_weight 920.10 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' Ni Ni 0.3393 1.1124 '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 11.080(3) _cell_length_b 16.583(4) _cell_length_c 16.600(4) _cell_angle_alpha 68.533(5) _cell_angle_beta 89.208(4) _cell_angle_gamma 89.167(4) _cell_volume 2837.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8992 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13700 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9855 _reflns_number_gt 6077 _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^)+(0.0921P)^2^+0.0000P] 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 9855 _refine_ls_number_parameters 476 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.003 _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 Ni1 Ni 0.64014(4) 1.00459(3) 0.49658(3) 0.02245(17) Uani 1 1 d . . . Ni2 Ni 0.49827(4) 0.81226(3) 0.50446(4) 0.02963(18) Uani 1 1 d . . . O8 O 0.3568(3) 0.90845(18) 0.62862(19) 0.0363(8) Uani 1 1 d . . . O3W O 0.6522(3) 0.9169(2) 0.6274(2) 0.0418(8) Uani 1 1 d . . . H3WA H 0.7270 0.9070 0.6429 0.063 Uiso 1 1 d R . . H3WB H 0.6194 0.8681 0.6329 0.063 Uiso 1 1 d R . . C6 C 0.1082(4) 0.7217(3) 0.4872(3) 0.0310(11) Uani 1 1 d . . . H6 H 0.1812 0.6935 0.4867 0.037 Uiso 1 1 calc R . . C10 C 0.0379(4) 0.5204(3) 0.5712(3) 0.0317(11) Uani 1 1 d . . . C9 C 0.0021(4) 0.5857(3) 0.4964(3) 0.0288(10) Uani 1 1 d . . . C11 C 0.0351(4) 0.4310(3) 0.5761(3) 0.0344(11) Uani 1 1 d . . . O2W O 0.4963(3) 0.6774(2) 0.5397(3) 0.0696(12) Uani 1 1 d . . . H2WA H 0.4980 0.6408 0.5913 0.104 Uiso 1 1 d R . . H2WB H 0.4935 0.6508 0.5047 0.104 Uiso 1 1 d R . . C24 C 0.4081(4) 0.8361(3) 0.6668(3) 0.0319(11) Uani 1 1 d . . . C18 C 0.3951(4) 0.7973(3) 0.7630(3) 0.0343(11) Uani 1 1 d . . . C27 C 0.5785(5) 0.5569(3) 0.9398(3) 0.0469(13) Uani 1 1 d . . . C23 C 0.4254(4) 0.7110(3) 0.8084(3) 0.0399(12) Uani 1 1 d . . . H23 H 0.4480 0.6761 0.7777 0.048 Uiso 1 1 calc R . . C26 C 0.4606(5) 0.5837(3) 0.9492(3) 0.0449(13) Uani 1 1 d . . . O11 O 0.8573(4) 0.6283(3) 0.8065(3) 0.1065(19) Uani 1 1 d . . . C5 C 0.0004(4) 0.6774(3) 0.4921(3) 0.0276(10) Uani 1 1 d . . . C12 C 0.0696(5) 0.3654(3) 0.6554(4) 0.0537(15) Uani 1 1 d . . . H12 H 0.0660 0.3079 0.6599 0.064 Uiso 1 1 calc R . . C15 C 0.0788(4) 0.5352(3) 0.6457(3) 0.0384(12) Uani 1 1 d . . . H15 H 0.0823 0.5919 0.6438 0.046 Uiso 1 1 calc R . . O6 O 0.1570(4) 0.4790(3) 0.7915(2) 0.0704(12) Uani 1 1 d . . . C32 C 0.6187(5) 0.4728(3) 0.9918(3) 0.0446(13) Uani 1 1 d . . . O12 O 0.9335(4) 0.4819(3) 0.9100(3) 0.0807(14) Uani 1 1 d . . . C22 C 0.4229(5) 0.6754(3) 0.8977(3) 0.0445(13) Uani 1 1 d . . . C19 C 0.3590(5) 0.8485(3) 0.8089(4) 0.0568(16) Uani 1 1 d . . . H19 H 0.3394 0.9065 0.7790 0.068 Uiso 1 1 calc R . . O2 O 0.3189(3) 0.80585(19) 0.4853(2) 0.0491(9) Uani 1 1 d U . . C14 C 0.1126(5) 0.4705(4) 0.7185(4) 0.0534(14) Uani 1 1 d . . . O5 O 0.1335(6) 0.3228(3) 0.8029(3) 0.126(2) Uani 1 1 d U . . C21 C 0.3870(6) 0.7296(4) 0.9420(4) 0.0619(17) Uani 1 1 d . . . H21 H 0.3868 0.7076 1.0022 0.074 Uiso 1 1 calc R . . C13 C 0.1070(6) 0.3821(3) 0.7241(4) 0.0687(18) Uani 1 1 d . . . C31 C 0.7410(5) 0.4470(3) 0.9833(3) 0.0518(14) Uani 1 1 d . . . H31 H 0.7685 0.3927 1.0194 0.062 Uiso 1 1 calc R . . C28 C 0.6636(5) 0.6118(4) 0.8781(4) 0.0609(16) Uani 1 1 d . . . H28 H 0.6407 0.6683 0.8449 0.073 Uiso 1 1 calc R . . C25 C 0.3126(11) 0.8673(5) 0.9505(6) 0.131(4) Uani 1 1 d . . . C29 C 0.7754(6) 0.5837(4) 0.8673(4) 0.0627(16) Uani 1 1 d . . . C30 C 0.8172(6) 0.5009(4) 0.9231(4) 0.0607(16) Uani 1 1 d . . . C33 C 0.8088(8) 0.7050(5) 0.7350(5) 0.133(4) Uani 1 1 d . . . H33A H 0.8672 0.7242 0.6888 0.200 Uiso 1 1 calc R . . H33B H 0.7921 0.7508 0.7561 0.200 Uiso 1 1 calc R . . H33C H 0.7357 0.6896 0.7140 0.200 Uiso 1 1 calc R . . O10 O 0.2831(7) 0.9470(4) 0.9065(4) 0.150(3) Uani 1 1 d . . . H10 H 0.2625 0.9711 0.9397 0.226 Uiso 1 1 calc R . . C16 C 0.1679(7) 0.5656(4) 0.7888(4) 0.078(2) Uani 1 1 d . . . H16A H 0.2200 0.5975 0.7415 0.117 Uiso 1 1 calc R . . H16B H 0.2014 0.5647 0.8421 0.117 Uiso 1 1 calc R . . H16C H 0.0897 0.5929 0.7808 0.117 Uiso 1 1 calc R . . O9 O 0.3009(9) 0.8341(4) 1.0290(4) 0.191(4) Uani 1 1 d . . . C34 C 0.9753(6) 0.3968(5) 0.9630(5) 0.092(2) Uani 1 1 d . . . H34A H 1.0607 0.3924 0.9548 0.139 Uiso 1 1 calc R . . H34B H 0.9347 0.3543 0.9468 0.139 Uiso 1 1 calc R . . H34C H 0.9584 0.3869 1.0227 0.139 Uiso 1 1 calc R . . C20 C 0.3516(6) 0.8153(4) 0.8983(4) 0.0658(18) Uani 1 1 d . . . C17 C 0.1176(12) 0.2343(6) 0.8154(6) 0.169(4) Uani 1 1 d U . . H17A H 0.1743 0.2179 0.7798 0.254 Uiso 1 1 calc R . . H17B H 0.0369 0.2259 0.7999 0.254 Uiso 1 1 calc R . . H17C H 0.1308 0.1992 0.8751 0.254 Uiso 1 1 calc R . . C4 C -0.1082(4) 0.7204(3) 0.4938(3) 0.0328(11) Uani 1 1 d . . . H4 H -0.1806 0.6916 0.4973 0.039 Uiso 1 1 calc R . . C3 C -0.1104(3) 0.8055(2) 0.4902(3) 0.0232(9) Uani 1 1 d . . . C2 C -0.0006(3) 0.8482(2) 0.4850(3) 0.0265(10) Uani 1 1 d . . . H2 H -0.0012 0.9051 0.4829 0.032 Uiso 1 1 calc R . . C1 C 0.1089(3) 0.8073(2) 0.4831(3) 0.0264(10) Uani 1 1 d . . . O7 O 0.4701(3) 0.79492(19) 0.6316(2) 0.0434(8) Uani 1 1 d . . . O13 O 0.5024(2) 0.93993(15) 0.46513(17) 0.0198(6) Uani 1 1 d . . . H13 H 0.5001 0.9615 0.4017 0.024 Uiso 1 1 calc R . . O1 O 0.2233(2) 0.92800(17) 0.4754(2) 0.0354(8) Uani 1 1 d . . . C8 C -0.2290(3) 0.8482(3) 0.4929(3) 0.0247(9) Uani 1 1 d . . . O3 O -0.2301(2) 0.93023(17) 0.4661(2) 0.0327(7) Uani 1 1 d . . . O4 O -0.3171(2) 0.79949(18) 0.5240(2) 0.0419(8) Uani 1 1 d . . . C7 C 0.2259(4) 0.8506(3) 0.4820(3) 0.0319(11) Uani 1 1 d . . . O1W O 0.5247(4) 0.8171(3) 0.3765(3) 0.0948(15) Uani 1 1 d . . . H1WA H 0.5426 0.7740 0.3622 0.142 Uiso 1 1 d R . . H1WB H 0.5191 0.8627 0.3312 0.142 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 Ni1 0.0121(3) 0.0138(3) 0.0399(4) -0.0079(2) -0.0008(2) -0.00012(19) Ni2 0.0143(3) 0.0182(3) 0.0584(4) -0.0164(3) 0.0022(2) -0.0005(2) O8 0.0274(17) 0.0280(17) 0.043(2) -0.0006(15) 0.0052(14) 0.0045(13) O3W 0.0336(19) 0.0373(19) 0.051(2) -0.0111(16) -0.0073(15) -0.0001(14) C6 0.019(2) 0.021(2) 0.060(3) -0.023(2) 0.001(2) 0.0015(17) C10 0.024(2) 0.024(2) 0.054(3) -0.023(2) -0.004(2) -0.0026(18) C9 0.020(2) 0.016(2) 0.054(3) -0.017(2) -0.003(2) 0.0012(16) C11 0.025(2) 0.018(2) 0.064(3) -0.018(2) -0.004(2) 0.0013(18) O2W 0.061(3) 0.032(2) 0.114(4) -0.025(2) 0.005(3) 0.0030(18) C24 0.027(2) 0.017(2) 0.046(3) -0.005(2) 0.000(2) 0.0027(18) C18 0.036(3) 0.025(2) 0.032(3) 0.001(2) -0.008(2) 0.0009(19) C27 0.059(4) 0.040(3) 0.031(3) 0.000(2) -0.012(2) 0.000(3) C23 0.049(3) 0.027(3) 0.037(3) -0.003(2) -0.003(2) 0.002(2) C26 0.057(3) 0.041(3) 0.029(3) -0.003(2) -0.004(2) 0.007(3) O11 0.087(4) 0.079(3) 0.096(4) 0.035(3) 0.029(3) 0.015(3) C5 0.019(2) 0.022(2) 0.051(3) -0.023(2) -0.0012(19) 0.0008(17) C12 0.079(4) 0.027(3) 0.056(4) -0.015(3) -0.011(3) -0.001(3) C15 0.035(3) 0.028(3) 0.059(3) -0.025(3) -0.002(2) -0.002(2) O6 0.104(4) 0.061(3) 0.052(3) -0.027(2) -0.019(2) -0.002(2) C32 0.055(3) 0.039(3) 0.031(3) -0.002(2) -0.010(2) 0.006(2) O12 0.065(3) 0.067(3) 0.082(3) 0.004(2) 0.009(2) 0.023(2) C22 0.057(3) 0.032(3) 0.041(3) -0.008(2) -0.012(2) 0.006(2) C19 0.088(5) 0.024(3) 0.051(4) -0.004(3) -0.019(3) 0.009(3) O2 0.0174(15) 0.0305(16) 0.104(2) -0.0307(16) -0.0047(15) 0.0035(12) C14 0.060(4) 0.054(4) 0.053(4) -0.027(3) -0.009(3) -0.005(3) O5 0.233(7) 0.051(3) 0.084(4) -0.009(3) -0.069(4) 0.004(4) C21 0.097(5) 0.052(4) 0.033(3) -0.012(3) -0.013(3) 0.011(3) C13 0.101(5) 0.032(3) 0.067(4) -0.010(3) -0.029(4) 0.005(3) C31 0.071(4) 0.040(3) 0.035(3) -0.003(3) -0.006(3) 0.009(3) C28 0.061(4) 0.049(3) 0.050(4) 0.007(3) -0.010(3) 0.006(3) C25 0.273(13) 0.060(5) 0.068(6) -0.033(5) -0.037(7) 0.061(6) C29 0.063(4) 0.047(3) 0.054(4) 0.008(3) 0.004(3) 0.008(3) C30 0.061(4) 0.057(4) 0.052(4) -0.006(3) -0.006(3) 0.008(3) C33 0.134(8) 0.080(6) 0.112(7) 0.050(5) 0.038(6) 0.018(5) O10 0.274(9) 0.095(4) 0.101(5) -0.058(4) -0.026(5) 0.061(5) C16 0.100(6) 0.081(5) 0.072(5) -0.051(4) -0.016(4) -0.004(4) O9 0.415(13) 0.098(5) 0.062(4) -0.036(4) -0.006(5) 0.086(6) C34 0.068(5) 0.095(6) 0.092(6) -0.010(4) 0.006(4) 0.030(4) C20 0.112(6) 0.043(3) 0.043(4) -0.017(3) -0.011(3) 0.009(3) C17 0.280(10) 0.078(5) 0.119(6) 0.002(5) -0.090(6) -0.010(6) C4 0.019(2) 0.020(2) 0.067(3) -0.025(2) -0.001(2) -0.0026(17) C3 0.011(2) 0.023(2) 0.041(3) -0.019(2) -0.0012(17) -0.0002(16) C2 0.017(2) 0.015(2) 0.050(3) -0.014(2) 0.0012(19) -0.0026(16) C1 0.014(2) 0.018(2) 0.048(3) -0.015(2) 0.0010(18) 0.0006(16) O7 0.041(2) 0.0239(17) 0.051(2) 0.0029(16) 0.0061(16) 0.0034(14) O13 0.0125(13) 0.0178(14) 0.0276(16) -0.0063(12) 0.0003(11) -0.0028(10) O1 0.0194(16) 0.0200(16) 0.071(2) -0.0213(16) -0.0057(14) -0.0021(12) C8 0.014(2) 0.026(2) 0.032(3) -0.009(2) 0.0017(17) -0.0032(17) O3 0.0183(15) 0.0143(15) 0.063(2) -0.0109(14) 0.0014(14) 0.0056(11) O4 0.0132(16) 0.0210(16) 0.086(3) -0.0128(16) 0.0046(15) -0.0010(12) C7 0.018(2) 0.030(3) 0.055(3) -0.023(2) 0.001(2) -0.0030(18) O1W 0.111(4) 0.083(3) 0.110(4) -0.059(3) 0.009(3) 0.004(3) _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 Ni1 O13 2.025(2) 2_676 ? Ni1 O1 2.050(3) 2_676 ? Ni1 O8 2.051(3) 2_676 ? Ni1 O3 2.056(3) 1_655 ? Ni1 O13 2.057(2) . ? Ni1 O3W 2.130(3) . ? Ni2 O13 1.975(2) . ? Ni2 O2 2.027(3) . ? Ni2 O7 2.044(3) . ? Ni2 O4 2.071(3) 1_655 ? Ni2 O2W 2.094(3) . ? Ni2 O1W 2.112(5) . ? O8 C24 1.265(5) . ? O8 Ni1 2.051(3) 2_676 ? O3W H3WA 0.8665 . ? O3W H3WB 0.8659 . ? C6 C1 1.396(5) . ? C6 C5 1.398(6) . ? C6 H6 0.9300 . ? C10 C9 1.374(6) . ? C10 C15 1.427(6) . ? C10 C11 1.456(5) . ? C9 C11 1.398(6) 2_566 ? C9 C5 1.496(5) . ? C11 C9 1.398(6) 2_566 ? C11 C12 1.420(6) . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8503 . ? C24 O7 1.243(5) . ? C24 C18 1.492(6) . ? C18 C19 1.385(7) . ? C18 C23 1.390(6) . ? C27 C26 1.399(7) . ? C27 C32 1.414(6) . ? C27 C28 1.443(8) . ? C23 C22 1.381(6) . ? C23 H23 0.9300 . ? C26 C32 1.392(7) 2_667 ? C26 C22 1.502(6) . ? O11 C29 1.354(7) . ? O11 C33 1.487(7) . ? C5 C4 1.395(5) . ? C12 C13 1.341(7) . ? C12 H12 0.9300 . ? C15 C14 1.344(7) . ? C15 H15 0.9300 . ? O6 C14 1.370(6) . ? O6 C16 1.427(7) . ? C32 C26 1.392(7) 2_667 ? C32 C31 1.435(7) . ? O12 C30 1.355(7) . ? O12 C34 1.436(7) . ? C22 C21 1.403(7) . ? C19 C20 1.383(7) . ? C19 H19 0.9300 . ? O2 C7 1.251(5) . ? C14 C13 1.436(7) . ? O5 C13 1.351(7) . ? O5 C17 1.419(9) . ? C21 C20 1.391(7) . ? C21 H21 0.9300 . ? C31 C30 1.363(8) . ? C31 H31 0.9300 . ? C28 C29 1.351(8) . ? C28 H28 0.9300 . ? C25 O9 1.221(9) . ? C25 O10 1.293(8) . ? C25 C20 1.487(9) . ? C29 C30 1.421(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O10 H10 0.8200 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C4 C3 1.390(5) . ? C4 H4 0.9300 . ? C3 C2 1.402(5) . ? C3 C8 1.491(5) . ? C2 C1 1.388(5) . ? C2 H2 0.9300 . ? C1 C7 1.487(5) . ? O13 Ni1 2.025(2) 2_676 ? O13 H13 0.9800 . ? O1 C7 1.248(5) . ? O1 Ni1 2.050(3) 2_676 ? C8 O4 1.255(5) . ? C8 O3 1.267(5) . ? O3 Ni1 2.056(3) 1_455 ? O4 Ni2 2.071(3) 1_455 ? O1W H1WA 0.8514 . ? O1W H1WB 0.8514 . ? 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 O13 Ni1 O1 99.01(11) 2_676 2_676 ? O13 Ni1 O8 95.52(11) 2_676 2_676 ? O1 Ni1 O8 88.89(13) 2_676 2_676 ? O13 Ni1 O3 170.89(11) 2_676 1_655 ? O1 Ni1 O3 88.12(11) 2_676 1_655 ? O8 Ni1 O3 90.24(12) 2_676 1_655 ? O13 Ni1 O13 80.76(11) 2_676 . ? O1 Ni1 O13 178.33(11) 2_676 . ? O8 Ni1 O13 89.49(11) 2_676 . ? O3 Ni1 O13 92.27(11) 1_655 . ? O13 Ni1 O3W 87.18(11) 2_676 . ? O1 Ni1 O3W 86.81(13) 2_676 . ? O8 Ni1 O3W 175.23(12) 2_676 . ? O3 Ni1 O3W 87.57(12) 1_655 . ? O13 Ni1 O3W 94.83(11) . . ? O13 Ni2 O2 95.34(11) . . ? O13 Ni2 O7 94.30(12) . . ? O2 Ni2 O7 91.60(14) . . ? O13 Ni2 O4 93.08(10) . 1_655 ? O2 Ni2 O4 171.13(12) . 1_655 ? O7 Ni2 O4 90.54(13) . 1_655 ? O13 Ni2 O2W 177.06(14) . . ? O2 Ni2 O2W 84.84(13) . . ? O7 Ni2 O2W 88.62(15) . . ? O4 Ni2 O2W 86.60(13) 1_655 . ? O13 Ni2 O1W 91.23(15) . . ? O2 Ni2 O1W 87.17(17) . . ? O7 Ni2 O1W 174.42(15) . . ? O4 Ni2 O1W 89.88(17) 1_655 . ? O2W Ni2 O1W 85.85(18) . . ? C24 O8 Ni1 133.6(3) . 2_676 ? Ni1 O3W H3WA 110.6 . . ? Ni1 O3W H3WB 110.0 . . ? H3WA O3W H3WB 108.4 . . ? C1 C6 C5 121.6(4) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C9 C10 C15 123.5(4) . . ? C9 C10 C11 119.3(4) . . ? C15 C10 C11 117.3(4) . . ? C10 C9 C11 121.9(4) . 2_566 ? C10 C9 C5 119.5(4) . . ? C11 C9 C5 118.5(4) 2_566 . ? C9 C11 C12 123.7(4) 2_566 . ? C9 C11 C10 118.8(4) 2_566 . ? C12 C11 C10 117.5(4) . . ? Ni2 O2W H2WA 125.2 . . ? Ni2 O2W H2WB 125.4 . . ? H2WA O2W H2WB 109.5 . . ? O7 C24 O8 125.9(4) . . ? O7 C24 C18 117.0(4) . . ? O8 C24 C18 117.1(4) . . ? C19 C18 C23 118.8(4) . . ? C19 C18 C24 120.1(4) . . ? C23 C18 C24 121.0(4) . . ? C26 C27 C32 120.1(5) . . ? C26 C27 C28 122.7(5) . . ? C32 C27 C28 117.2(5) . . ? C22 C23 C18 122.1(5) . . ? C22 C23 H23 119.0 . . ? C18 C23 H23 119.0 . . ? C32 C26 C27 120.3(4) 2_667 . ? C32 C26 C22 120.6(5) 2_667 . ? C27 C26 C22 119.1(5) . . ? C29 O11 C33 115.4(5) . . ? C4 C5 C6 118.4(4) . . ? C4 C5 C9 121.1(4) . . ? C6 C5 C9 120.5(3) . . ? C13 C12 C11 123.3(5) . . ? C13 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C14 C15 C10 122.5(4) . . ? C14 C15 H15 118.7 . . ? C10 C15 H15 118.7 . . ? C14 O6 C16 115.9(5) . . ? C26 C32 C27 119.6(5) 2_667 . ? C26 C32 C31 120.9(5) 2_667 . ? C27 C32 C31 119.5(5) . . ? C30 O12 C34 115.8(5) . . ? C23 C22 C21 117.4(4) . . ? C23 C22 C26 123.6(5) . . ? C21 C22 C26 118.9(5) . . ? C20 C19 C18 121.4(5) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C7 O2 Ni2 138.1(3) . . ? C15 C14 O6 126.3(5) . . ? C15 C14 C13 120.2(5) . . ? O6 C14 C13 113.4(5) . . ? C13 O5 C17 117.3(6) . . ? C20 C21 C22 121.9(5) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C12 C13 O5 126.3(5) . . ? C12 C13 C14 119.1(5) . . ? O5 C13 C14 114.4(5) . . ? C30 C31 C32 120.9(5) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C29 C28 C27 122.0(5) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? O9 C25 O10 123.2(7) . . ? O9 C25 C20 121.2(7) . . ? O10 C25 C20 115.4(7) . . ? C28 C29 O11 125.9(5) . . ? C28 C29 C30 120.2(5) . . ? O11 C29 C30 113.9(5) . . ? O12 C30 C31 125.0(5) . . ? O12 C30 C29 115.1(5) . . ? C31 C30 C29 119.9(6) . . ? O11 C33 H33A 109.5 . . ? O11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C25 O10 H10 109.5 . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O12 C34 H34A 109.5 . . ? O12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C19 C20 C21 118.4(5) . . ? C19 C20 C25 123.4(6) . . ? C21 C20 C25 118.2(6) . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 C8 119.1(4) . . ? C2 C3 C8 122.1(3) . . ? C1 C2 C3 121.3(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C1 C6 118.6(4) . . ? C2 C1 C7 121.6(4) . . ? C6 C1 C7 119.7(3) . . ? C24 O7 Ni2 131.8(3) . . ? Ni2 O13 Ni1 115.15(12) . 2_676 ? Ni2 O13 Ni1 122.48(12) . . ? Ni1 O13 Ni1 99.24(11) 2_676 . ? Ni2 O13 H13 106.3 . . ? Ni1 O13 H13 106.3 2_676 . ? Ni1 O13 H13 106.3 . . ? C7 O1 Ni1 127.0(3) . 2_676 ? O4 C8 O3 126.3(4) . . ? O4 C8 C3 117.0(4) . . ? O3 C8 C3 116.6(3) . . ? C8 O3 Ni1 125.2(3) . 1_455 ? C8 O4 Ni2 134.0(3) . 1_455 ? O2 C7 O1 125.8(4) . . ? O2 C7 C1 116.1(4) . . ? O1 C7 C1 118.0(4) . . ? Ni2 O1W H1WA 125.5 . . ? Ni2 O1W H1WB 125.1 . . ? H1WA O1W H1WB 109.4 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.800 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.095 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.024 0.000 0.000 1393 486 ' ' _platon_squeeze_details ; ; _vrf_CHEMW03_p2 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This is caused by the given molecular weight being increased from the atom count to account for 6 disordered water molecules omitted by SQUEEZE. ; _vrf_PLAT222_p2 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: Structure contain disordered terminal methoxy group. ; _database_code_depnum_ccdc_archive 'CCDC 967537' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H66 Cd2 N4 O19' _chemical_formula_weight 1251.87 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4676(17) _cell_length_b 13.1962(15) _cell_length_c 26.497(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.729(2) _cell_angle_gamma 90.00 _cell_volume 5345.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5417 _exptl_absorpt_correction_T_max 0.9177 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25944 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9382 _reflns_number_gt 6846 _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^)+(0.0646P)^2^+0.0000P] 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 9382 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _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 Cd1 Cd 0.254073(17) 0.81505(2) 0.239368(10) 0.02781(10) Uani 1 1 d . . . Cd2 Cd 0.21126(2) 0.67755(2) 0.345514(11) 0.03666(11) Uani 1 1 d . . . C33 C 0.6089(3) 1.1902(3) 0.21695(15) 0.0319(9) Uani 1 1 d . . . O8 O 0.35152(18) 0.9614(2) 0.25114(10) 0.0429(7) Uani 1 1 d . . . O7 O 0.29562(18) 0.9035(2) 0.17431(10) 0.0417(7) Uani 1 1 d . . . C34 C 0.3484(3) 0.9583(3) 0.20325(16) 0.0341(9) Uani 1 1 d . . . C5 C 0.0039(3) 0.4993(3) 0.10985(14) 0.0341(9) Uani 1 1 d . . . O4 O -0.1811(2) 0.3430(2) 0.17884(13) 0.0524(8) Uani 1 1 d . . . C23 C 0.4192(2) 1.0038(3) 0.12805(14) 0.0306(9) Uani 1 1 d . . . H23 H 0.3776 0.9633 0.1086 0.037 Uiso 1 1 calc R . . C4 C 0.0646(3) 0.5592(3) 0.14011(15) 0.0360(10) Uani 1 1 d . . . H4 H 0.1051 0.5965 0.1252 0.043 Uiso 1 1 calc R . . O9 O 0.6013(2) 1.2140(2) 0.26130(11) 0.0462(8) Uani 1 1 d . . . C20 C 0.5409(2) 1.1260(3) 0.18551(13) 0.0269(8) Uani 1 1 d . . . O10 O 0.67404(17) 1.2187(2) 0.19645(11) 0.0375(7) Uani 1 1 d . . . C17 C -0.1253(3) 0.3927(3) 0.20768(17) 0.0388(10) Uani 1 1 d . . . C22 C 0.4139(2) 1.0192(3) 0.17911(14) 0.0290(9) Uani 1 1 d . . . O11 O 0.5330(3) 0.6615(2) 0.09116(12) 0.0599(10) Uani 1 1 d . . . C19 C 0.5455(2) 1.1083(3) 0.13467(14) 0.0286(9) Uani 1 1 d . . . H19 H 0.5900 1.1379 0.1198 0.034 Uiso 1 1 calc R . . C18 C 0.4846(2) 1.0471(3) 0.10536(13) 0.0278(8) Uani 1 1 d . . . C1 C -0.0570(2) 0.4498(3) 0.18500(15) 0.0324(9) Uani 1 1 d . . . C21 C 0.4740(2) 1.0815(3) 0.20775(14) 0.0300(9) Uani 1 1 d . . . H21 H 0.4700 1.0938 0.2419 0.036 Uiso 1 1 calc R . . C7 C 0.0025(3) 0.4978(3) 0.05298(15) 0.0376(10) Uani 1 1 d . . . C24 C 0.4929(2) 1.0230(3) 0.05123(14) 0.0295(9) Uani 1 1 d . . . O12 O 0.5344(3) 0.6200(2) -0.00319(12) 0.0627(10) Uani 1 1 d . . . C10 C 0.0640(3) 0.4426(3) 0.03140(14) 0.0357(10) Uani 1 1 d . . . C2 C 0.0041(3) 0.5099(3) 0.21510(15) 0.0337(9) Uani 1 1 d . . . H2 H 0.0038 0.5136 0.2501 0.040 Uiso 1 1 calc R . . C8 C -0.0622(3) 0.5544(3) 0.02240(15) 0.0382(10) Uani 1 1 d . . . C11 C 0.1280(3) 0.3815(4) 0.06146(16) 0.0453(11) Uani 1 1 d . . . H11 H 0.1294 0.3792 0.0967 0.054 Uiso 1 1 calc R . . O3 O -0.1270(2) 0.4012(3) 0.25430(12) 0.0519(8) Uani 1 1 d . . . C6 C -0.0562(3) 0.4438(3) 0.13252(15) 0.0371(10) Uani 1 1 d . . . H6 H -0.0963 0.4023 0.1125 0.045 Uiso 1 1 calc R . . C28 C 0.5243(3) 0.7444(3) 0.05914(16) 0.0437(11) Uani 1 1 d . . . C29 C 0.5270(3) 0.7195(3) 0.00714(17) 0.0423(11) Uani 1 1 d . . . C3 C 0.0653(2) 0.5641(3) 0.19337(14) 0.0322(9) Uani 1 1 d . . . C12 C 0.1868(3) 0.3268(4) 0.03995(19) 0.0500(12) Uani 1 1 d . . . C26 C 0.5064(3) 0.9225(3) 0.03724(14) 0.0305(9) Uani 1 1 d . . . C9 C -0.1266(3) 0.6129(4) 0.04367(17) 0.0462(11) Uani 1 1 d . . . H9 H -0.1270 0.6115 0.0787 0.055 Uiso 1 1 calc R . . C30 C 0.5242(3) 0.7959(3) -0.02799(16) 0.0382(10) Uani 1 1 d . . . H30 H 0.5303 0.7800 -0.0615 0.046 Uiso 1 1 calc R . . C27 C 0.5148(3) 0.8419(3) 0.07378(15) 0.0372(10) Uani 1 1 d . . . H27 H 0.5138 0.8564 0.1080 0.045 Uiso 1 1 calc R . . C25 C 0.4878(2) 1.1012(3) 0.01479(14) 0.0310(9) Uani 1 1 d . . . C32 C 0.5383(5) 0.6828(4) 0.14501(19) 0.082(2) Uani 1 1 d . . . H32A H 0.4857 0.7160 0.1512 0.123 Uiso 1 1 calc R . . H32B H 0.5876 0.7259 0.1558 0.123 Uiso 1 1 calc R . . H32C H 0.5452 0.6204 0.1639 0.123 Uiso 1 1 calc R . . O6 O 0.2496(2) 0.2641(3) 0.06512(14) 0.0741(11) Uani 1 1 d . . . C13 C 0.1860(3) 0.3307(4) -0.01388(19) 0.0528(13) Uani 1 1 d . . . O5 O 0.2498(2) 0.2725(3) -0.03068(15) 0.0724(11) Uani 1 1 d . . . O1 O 0.1779(2) 0.6855(2) 0.20243(11) 0.0449(8) Uani 1 1 d . . . O2 O 0.1299(2) 0.6292(3) 0.27264(11) 0.0596(10) Uani 1 1 d . . . O2W O 0.0955(2) 0.6682(3) 0.38840(14) 0.0793(13) Uani 1 1 d . . . H2WA H 0.0846 0.6133 0.4030 0.095 Uiso 1 1 d R . . H2WB H 0.0630 0.7197 0.3899 0.095 Uiso 1 1 d R . . C16 C 0.1293(3) 0.6313(3) 0.22548(16) 0.0377(10) Uani 1 1 d . . . O13 O 0.2901(2) 0.7301(3) 0.41889(13) 0.0759(12) Uani 1 1 d . . . O1W O 0.2492(3) 0.5158(3) 0.36339(14) 0.0758(11) Uani 1 1 d . . . H1WA H 0.2194 0.4798 0.3810 0.091 Uiso 1 1 d R . . H1WB H 0.2936 0.4906 0.3526 0.091 Uiso 1 1 d R . . C31 C 0.5382(5) 0.5929(4) -0.0547(2) 0.091(2) Uani 1 1 d . . . H31A H 0.4868 0.6173 -0.0762 0.136 Uiso 1 1 calc R . . H31B H 0.5411 0.5205 -0.0575 0.136 Uiso 1 1 calc R . . H31C H 0.5892 0.6226 -0.0653 0.136 Uiso 1 1 calc R . . C14 C 0.2523(4) 0.2756(6) -0.0849(2) 0.095(2) Uani 1 1 d . . . H14A H 0.1942 0.2673 -0.1031 0.142 Uiso 1 1 calc R . . H14B H 0.2889 0.2219 -0.0939 0.142 Uiso 1 1 calc R . . H14C H 0.2755 0.3396 -0.0937 0.142 Uiso 1 1 calc R . . C15 C 0.2508(4) 0.2475(5) 0.1174(2) 0.0832(19) Uani 1 1 d . . . H15A H 0.1949 0.2224 0.1231 0.125 Uiso 1 1 calc R . . H15B H 0.2632 0.3100 0.1355 0.125 Uiso 1 1 calc R . . H15C H 0.2953 0.1986 0.1293 0.125 Uiso 1 1 calc R . . C38 C 0.2834(7) 0.8691(7) 0.5282(3) 0.235(6) Uiso 1 1 d G . . H38A H 0.3343 0.9027 0.5467 0.282 Uiso 1 1 calc R . . H38B H 0.2319 0.9081 0.5326 0.282 Uiso 1 1 calc R . . N1 N 0.2909(5) 0.8622(5) 0.4755(3) 0.178(3) Uiso 1 1 d G . . C35 C 0.2887(4) 0.7580(5) 0.4620(2) 0.094(2) Uiso 1 1 d G . . C36 C 0.2799(6) 0.7006(5) 0.5062(3) 0.202(5) Uiso 1 1 d G . . H36A H 0.3293 0.6550 0.5144 0.242 Uiso 1 1 calc R . . H36B H 0.2268 0.6604 0.5003 0.242 Uiso 1 1 calc R . . C37 C 0.2766(7) 0.7693(9) 0.5471(2) 0.222(6) Uiso 1 1 d G . . H37A H 0.2219 0.7614 0.5605 0.266 Uiso 1 1 calc R . . H37B H 0.3244 0.7559 0.5745 0.266 Uiso 1 1 calc R . . C39 C 0.3118(12) 0.9369(15) 0.4372(7) 0.298(9) Uiso 1 1 d . . . H39A H 0.3046 0.9057 0.4041 0.447 Uiso 1 1 calc R . . H39B H 0.3711 0.9593 0.4462 0.447 Uiso 1 1 calc R . . H39C H 0.2731 0.9939 0.4365 0.447 Uiso 1 1 calc 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 Cd1 0.02571(16) 0.03037(17) 0.02841(17) 0.00503(12) 0.00748(12) -0.00164(12) Cd2 0.03915(19) 0.0449(2) 0.02633(17) 0.00119(13) 0.00630(13) -0.00384(15) C33 0.034(2) 0.032(2) 0.030(2) -0.0026(17) 0.0049(18) -0.0003(19) O8 0.0486(18) 0.0481(18) 0.0360(17) 0.0028(14) 0.0198(14) -0.0119(15) O7 0.0388(16) 0.0500(18) 0.0365(16) 0.0075(14) 0.0063(13) -0.0219(15) C34 0.028(2) 0.032(2) 0.044(3) 0.0067(19) 0.0126(19) 0.0036(19) C5 0.035(2) 0.044(2) 0.0216(19) 0.0001(18) -0.0005(17) -0.004(2) O4 0.0411(18) 0.0490(19) 0.066(2) 0.0031(17) 0.0043(16) -0.0182(16) C23 0.029(2) 0.030(2) 0.033(2) -0.0025(17) 0.0035(17) -0.0076(18) C4 0.035(2) 0.042(2) 0.032(2) 0.0054(19) 0.0090(18) -0.009(2) O9 0.0518(19) 0.0570(19) 0.0313(16) -0.0140(14) 0.0112(14) -0.0174(16) C20 0.031(2) 0.026(2) 0.025(2) -0.0022(16) 0.0055(16) -0.0029(17) O10 0.0287(15) 0.0420(16) 0.0434(17) -0.0097(14) 0.0105(13) -0.0099(13) C17 0.031(2) 0.037(2) 0.048(3) 0.005(2) 0.005(2) -0.007(2) C22 0.030(2) 0.028(2) 0.029(2) 0.0064(16) 0.0046(17) -0.0022(17) O11 0.107(3) 0.0352(18) 0.0399(18) 0.0071(14) 0.0200(19) 0.0031(18) C19 0.030(2) 0.032(2) 0.026(2) 0.0053(17) 0.0104(16) -0.0065(18) C18 0.033(2) 0.028(2) 0.0244(19) -0.0006(16) 0.0099(16) -0.0038(18) C1 0.029(2) 0.034(2) 0.035(2) -0.0003(18) 0.0079(17) -0.0093(18) C21 0.034(2) 0.029(2) 0.028(2) -0.0005(17) 0.0089(17) -0.0018(18) C7 0.041(2) 0.042(2) 0.029(2) -0.0061(19) 0.0039(19) -0.011(2) C24 0.029(2) 0.035(2) 0.0246(19) -0.0029(17) 0.0040(16) -0.0104(18) O12 0.116(3) 0.0304(17) 0.0470(19) 0.0018(15) 0.028(2) 0.0042(19) C10 0.037(2) 0.042(2) 0.028(2) -0.0017(18) 0.0014(18) -0.006(2) C2 0.041(2) 0.036(2) 0.025(2) -0.0027(17) 0.0088(18) -0.007(2) C8 0.040(2) 0.043(2) 0.030(2) 0.0017(19) 0.0039(19) -0.005(2) C11 0.048(3) 0.055(3) 0.033(2) 0.011(2) 0.007(2) 0.005(2) O3 0.0484(19) 0.063(2) 0.049(2) 0.0006(16) 0.0221(15) -0.0113(17) C6 0.033(2) 0.041(2) 0.035(2) -0.0029(19) -0.0048(18) -0.007(2) C28 0.062(3) 0.036(2) 0.035(2) 0.010(2) 0.014(2) -0.004(2) C29 0.061(3) 0.028(2) 0.040(3) 0.0008(19) 0.013(2) -0.005(2) C3 0.032(2) 0.038(2) 0.026(2) -0.0068(17) 0.0030(17) -0.0049(19) C12 0.039(3) 0.059(3) 0.051(3) 0.010(2) 0.005(2) 0.003(2) C26 0.036(2) 0.033(2) 0.0237(19) 0.0003(16) 0.0083(17) -0.0068(18) C9 0.047(3) 0.060(3) 0.033(2) -0.004(2) 0.006(2) 0.009(2) C30 0.049(3) 0.037(2) 0.030(2) -0.0026(18) 0.010(2) -0.005(2) C27 0.053(3) 0.034(2) 0.026(2) 0.0038(18) 0.0103(19) -0.004(2) C25 0.033(2) 0.034(2) 0.027(2) -0.0010(17) 0.0067(17) -0.0092(19) C32 0.149(6) 0.066(4) 0.036(3) 0.025(3) 0.028(3) 0.008(4) O6 0.060(2) 0.102(3) 0.062(2) 0.030(2) 0.0156(19) 0.033(2) C13 0.051(3) 0.057(3) 0.051(3) 0.002(2) 0.012(2) 0.008(3) O5 0.063(2) 0.090(3) 0.067(2) 0.005(2) 0.0200(19) 0.032(2) O1 0.0448(18) 0.0476(18) 0.0429(18) -0.0075(14) 0.0087(14) -0.0207(15) O2 0.061(2) 0.089(3) 0.0278(17) -0.0119(17) 0.0028(15) -0.033(2) O2W 0.057(2) 0.116(4) 0.070(3) 0.027(2) 0.026(2) 0.003(2) C16 0.031(2) 0.041(3) 0.041(3) -0.004(2) 0.0034(19) -0.002(2) O13 0.064(2) 0.116(3) 0.044(2) -0.028(2) -0.0031(18) 0.009(2) O1W 0.104(3) 0.046(2) 0.084(3) 0.0095(19) 0.038(2) 0.004(2) C31 0.182(7) 0.032(3) 0.068(4) -0.013(3) 0.051(4) -0.006(4) C14 0.088(5) 0.128(6) 0.073(4) -0.008(4) 0.029(4) 0.046(5) C15 0.083(4) 0.096(5) 0.065(4) 0.022(4) -0.007(3) 0.023(4) _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 Cd1 O1 2.218(3) . ? Cd1 O7 2.255(3) . ? Cd1 O10 2.274(3) 2_645 ? Cd1 O3 2.299(3) 2 ? Cd1 O8 2.440(3) . ? Cd1 O9 2.607(3) 2_645 ? Cd1 O4 2.617(3) 2 ? Cd1 C34 2.654(4) . ? Cd2 O2 2.232(3) . ? Cd2 O13 2.242(3) . ? Cd2 O1W 2.245(3) . ? Cd2 O2W 2.265(3) . ? Cd2 O10 2.297(3) 2_645 ? Cd2 O4 2.304(3) 2 ? C33 O9 1.239(5) . ? C33 O10 1.272(4) . ? C33 C20 1.501(5) . ? O8 C34 1.263(5) . ? O7 C34 1.260(5) . ? C34 C22 1.509(5) . ? C5 C4 1.386(5) . ? C5 C6 1.390(5) . ? C5 C7 1.504(5) . ? O4 C17 1.249(5) . ? O4 Cd2 2.304(3) 2_545 ? O4 Cd1 2.617(3) 2_545 ? C23 C18 1.377(5) . ? C23 C22 1.383(5) . ? C23 H23 0.9300 . ? C4 C3 1.411(5) . ? C4 H4 0.9300 . ? O9 Cd1 2.607(3) 2_655 ? C20 C19 1.379(5) . ? C20 C21 1.396(5) . ? O10 Cd1 2.274(3) 2_655 ? O10 Cd2 2.297(3) 2_655 ? C17 O3 1.245(5) . ? C17 C1 1.496(5) . ? C22 C21 1.380(5) . ? O11 C28 1.378(5) . ? O11 C32 1.444(6) . ? C19 C18 1.386(5) . ? C19 H19 0.9300 . ? C18 C24 1.493(5) . ? C1 C6 1.395(5) . ? C1 C2 1.390(5) . ? C21 H21 0.9300 . ? C7 C10 1.390(6) . ? C7 C8 1.403(6) . ? C24 C26 1.401(5) . ? C24 C25 1.407(5) . ? O12 C29 1.350(5) . ? O12 C31 1.421(6) . ? C10 C11 1.422(6) . ? C10 C8 1.422(5) 3_565 ? C2 C3 1.380(5) . ? C2 H2 0.9300 . ? C8 C10 1.422(5) 3_565 ? C8 C9 1.441(6) . ? C11 C12 1.354(6) . ? C11 H11 0.9300 . ? O3 Cd1 2.299(3) 2_545 ? C6 H6 0.9300 . ? C28 C27 1.358(6) . ? C28 C29 1.423(6) . ? C29 C30 1.368(6) . ? C3 C16 1.494(6) . ? C12 O6 1.369(6) . ? C12 C13 1.425(7) . ? C26 C27 1.431(5) . ? C26 C25 1.429(5) 3_675 ? C9 C13 1.342(6) 3_565 ? C9 H9 0.9300 . ? C30 C25 1.422(6) 3_675 ? C30 H30 0.9300 . ? C27 H27 0.9300 . ? C25 C30 1.422(6) 3_675 ? C25 C26 1.429(5) 3_675 ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O6 C15 1.399(6) . ? C13 C9 1.342(6) 3_565 ? C13 O5 1.377(6) . ? O5 C14 1.442(6) . ? O1 C16 1.261(5) . ? O2 C16 1.249(5) . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8501 . ? O13 C35 1.203(6) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C38 C37 1.4200 . ? C38 N1 1.4200 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? N1 C35 1.4200 . ? N1 C39 1.486(18) . ? C35 C36 1.4200 . ? C36 C37 1.4200 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 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 O1 Cd1 O7 104.82(11) . . ? O1 Cd1 O10 93.78(11) . 2_645 ? O7 Cd1 O10 134.23(10) . 2_645 ? O1 Cd1 O3 90.60(12) . 2 ? O7 Cd1 O3 98.37(11) . 2 ? O10 Cd1 O3 123.26(10) 2_645 2 ? O1 Cd1 O8 160.53(10) . . ? O7 Cd1 O8 56.35(10) . . ? O10 Cd1 O8 97.14(10) 2_645 . ? O3 Cd1 O8 96.75(11) 2 . ? O1 Cd1 O9 90.13(11) . 2_645 ? O7 Cd1 O9 85.13(10) . 2_645 ? O10 Cd1 O9 52.87(9) 2_645 2_645 ? O3 Cd1 O9 176.11(10) 2 2_645 ? O8 Cd1 O9 83.76(10) . 2_645 ? O1 Cd1 O4 101.95(11) . 2 ? O7 Cd1 O4 140.25(10) . 2 ? O10 Cd1 O4 71.51(10) 2_645 2 ? O3 Cd1 O4 52.33(10) 2 2 ? O8 Cd1 O4 96.78(10) . 2 ? O9 Cd1 O4 123.79(9) 2_645 2 ? O1 Cd1 C34 132.40(12) . . ? O7 Cd1 C34 28.27(11) . . ? O10 Cd1 C34 115.77(11) 2_645 . ? O3 Cd1 C34 101.36(12) 2 . ? O8 Cd1 C34 28.32(11) . . ? O9 Cd1 C34 80.92(11) 2_645 . ? O4 Cd1 C34 121.87(12) 2 . ? O2 Cd2 O13 178.20(14) . . ? O2 Cd2 O1W 90.35(15) . . ? O13 Cd2 O1W 91.18(15) . . ? O2 Cd2 O2W 91.92(13) . . ? O13 Cd2 O2W 87.08(14) . . ? O1W Cd2 O2W 92.49(14) . . ? O2 Cd2 O10 91.40(11) . 2_645 ? O13 Cd2 O10 89.33(12) . 2_645 ? O1W Cd2 O10 97.49(12) . 2_645 ? O2W Cd2 O10 169.46(13) . 2_645 ? O2 Cd2 O4 87.98(13) . 2 ? O13 Cd2 O4 90.58(15) . 2 ? O1W Cd2 O4 174.40(12) . 2 ? O2W Cd2 O4 92.91(13) . 2 ? O10 Cd2 O4 77.22(11) 2_645 2 ? O9 C33 O10 121.7(4) . . ? O9 C33 C20 120.6(3) . . ? O10 C33 C20 117.6(3) . . ? C34 O8 Cd1 85.3(2) . . ? C34 O7 Cd1 93.7(2) . . ? O8 C34 O7 123.5(4) . . ? O8 C34 C22 118.9(4) . . ? O7 C34 C22 117.5(3) . . ? O8 C34 Cd1 66.4(2) . . ? O7 C34 Cd1 57.98(19) . . ? C22 C34 Cd1 166.7(3) . . ? C4 C5 C6 119.3(3) . . ? C4 C5 C7 119.5(3) . . ? C6 C5 C7 121.1(4) . . ? C17 O4 Cd2 139.6(3) . 2_545 ? C17 O4 Cd1 85.0(3) . 2_545 ? Cd2 O4 Cd1 90.23(10) 2_545 2_545 ? C18 C23 C22 121.5(4) . . ? C18 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C33 O9 Cd1 85.3(2) . 2_655 ? C19 C20 C21 119.5(3) . . ? C19 C20 C33 120.2(3) . . ? C21 C20 C33 120.4(3) . . ? C33 O10 Cd1 100.1(2) . 2_655 ? C33 O10 Cd2 149.0(3) . 2_655 ? Cd1 O10 Cd2 99.69(10) 2_655 2_655 ? O3 C17 O4 122.6(4) . . ? O3 C17 C1 118.4(4) . . ? O4 C17 C1 118.9(4) . . ? C21 C22 C23 119.4(3) . . ? C21 C22 C34 121.6(3) . . ? C23 C22 C34 118.7(3) . . ? C28 O11 C32 116.1(4) . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C23 C18 C19 118.6(3) . . ? C23 C18 C24 120.5(3) . . ? C19 C18 C24 120.8(3) . . ? C6 C1 C2 119.8(3) . . ? C6 C1 C17 119.0(4) . . ? C2 C1 C17 121.2(4) . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C10 C7 C8 121.0(4) . . ? C10 C7 C5 120.8(4) . . ? C8 C7 C5 118.2(4) . . ? C26 C24 C25 120.5(3) . . ? C26 C24 C18 119.6(3) . . ? C25 C24 C18 119.9(3) . . ? C29 O12 C31 117.2(4) . . ? C7 C10 C11 121.9(4) . . ? C7 C10 C8 119.2(4) . 3_565 ? C11 C10 C8 118.9(4) . 3_565 ? C3 C2 C1 120.4(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C7 C8 C10 119.8(4) . 3_565 ? C7 C8 C9 122.2(4) . . ? C10 C8 C9 117.9(4) 3_565 . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C17 O3 Cd1 100.1(3) . 2_545 ? C5 C6 C1 120.6(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C27 C28 O11 125.5(4) . . ? C27 C28 C29 121.0(4) . . ? O11 C28 C29 113.5(4) . . ? O12 C29 C30 125.0(4) . . ? O12 C29 C28 115.9(4) . . ? C30 C29 C28 119.1(4) . . ? C2 C3 C4 119.5(4) . . ? C2 C3 C16 120.4(3) . . ? C4 C3 C16 120.0(4) . . ? C11 C12 O6 126.1(4) . . ? C11 C12 C13 119.8(4) . . ? O6 C12 C13 114.0(4) . . ? C24 C26 C27 121.8(3) . . ? C24 C26 C25 119.7(3) . 3_675 ? C27 C26 C25 118.6(4) . 3_675 ? C13 C9 C8 121.3(4) 3_565 . ? C13 C9 H9 119.4 3_565 . ? C8 C9 H9 119.4 . . ? C29 C30 C25 121.9(4) . 3_675 ? C29 C30 H30 119.1 . . ? C25 C30 H30 119.1 3_675 . ? C28 C27 C26 120.9(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C24 C25 C30 121.8(3) . 3_675 ? C24 C25 C26 119.8(4) . 3_675 ? C30 C25 C26 118.4(3) 3_675 3_675 ? O11 C32 H32A 109.5 . . ? O11 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O11 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C12 O6 C15 118.6(4) . . ? C9 C13 O5 125.4(5) 3_565 . ? C9 C13 C12 120.6(4) 3_565 . ? O5 C13 C12 113.9(4) . . ? C13 O5 C14 115.8(4) . . ? C16 O1 Cd1 122.7(3) . . ? C16 O2 Cd2 141.0(3) . . ? Cd2 O2W H2WA 120.1 . . ? Cd2 O2W H2WB 119.9 . . ? H2WA O2W H2WB 120.0 . . ? O2 C16 O1 125.6(4) . . ? O2 C16 C3 117.4(4) . . ? O1 C16 C3 116.9(4) . . ? C35 O13 Cd2 146.3(4) . . ? Cd2 O1W H1WA 120.0 . . ? Cd2 O1W H1WB 120.0 . . ? H1WA O1W H1WB 120.0 . . ? O12 C31 H31A 109.5 . . ? O12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C37 C38 N1 108.0 . . ? C37 C38 H38A 110.1 . . ? N1 C38 H38A 110.1 . . ? C37 C38 H38B 110.1 . . ? N1 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? C35 N1 C38 108.0 . . ? C35 N1 C39 117.9(10) . . ? C38 N1 C39 133.4(10) . . ? O13 C35 C36 129.6(7) . . ? O13 C35 N1 122.3(7) . . ? C36 C35 N1 108.0 . . ? C35 C36 C37 108.0 . . ? C35 C36 H36A 110.1 . . ? C37 C36 H36A 110.1 . . ? C35 C36 H36B 110.1 . . ? C37 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C38 C37 C36 108.0 . . ? C38 C37 H37A 110.1 . . ? C36 C37 H37A 110.1 . . ? C38 C37 H37B 110.1 . . ? C36 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.853 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.007 0.002 1846 565 ' ' _platon_squeeze_details ; ; _vrf_CHEMW03_p3 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This is caused by the given molecular weight being increased from the atom count to account for 2 disordered DMF molecules, 1 disordered NMP molecule, and 1 disordered water molecule omitted by SQUEEZE. ; _vrf_PLAT222_p3 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: Structure contain disordered NMP molecule. ; _database_code_depnum_ccdc_archive 'CCDC 967538' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 Co2 N3 O19' _chemical_formula_weight 1097.83 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' O O 0.0106 0.0060 '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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.168(3) _cell_length_b 18.035(5) _cell_length_c 27.054(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.321(5) _cell_angle_gamma 90.00 _cell_volume 4896(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9280 _exptl_absorpt_correction_T_max 0.9992 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24112 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8614 _reflns_number_gt 6424 _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^)+(0.0938P)^2^+0.0000P] 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 8614 _refine_ls_number_parameters 452 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _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 0.46930(4) 0.69084(2) 0.309507(15) 0.02717(14) Uani 1 1 d . . . Co2 Co 0.64085(5) 0.76571(3) 0.216911(17) 0.03816(16) Uani 1 1 d . . . O4 O 1.3550(2) 0.64781(15) 0.35658(9) 0.0455(6) Uani 1 1 d . . . O3 O 1.2418(2) 0.70493(16) 0.29330(10) 0.0502(7) Uani 1 1 d . . . O1 O 0.6549(2) 0.66851(17) 0.33874(10) 0.0544(7) Uani 1 1 d . . . O5 O 0.5626(3) 0.84480(15) 0.25399(10) 0.0610(8) Uani 1 1 d . . . C16 C 0.7520(3) 0.6833(2) 0.31815(12) 0.0363(8) Uani 1 1 d . . . C17 C 1.2454(3) 0.6676(2) 0.33175(13) 0.0362(8) Uani 1 1 d . . . O2 O 0.7483(2) 0.71696(19) 0.27867(10) 0.0628(8) Uani 1 1 d . . . C5 C 1.1200(3) 0.6474(2) 0.35020(12) 0.0345(7) Uani 1 1 d . . . C4 C 1.1237(3) 0.6027(2) 0.39145(13) 0.0396(8) Uani 1 1 d . . . H4 H 1.2049 0.5835 0.4069 0.047 Uiso 1 1 calc R . . C24 C 0.5041(4) 0.9971(2) 0.44849(13) 0.0447(9) Uani 1 1 d . . . O6 O 0.4817(3) 0.79715(15) 0.31803(12) 0.0607(8) Uani 1 1 d . . . C1 C 0.8839(3) 0.6571(2) 0.34405(12) 0.0341(7) Uani 1 1 d . . . O8 O 0.5451(3) 1.11749(17) 0.24296(11) 0.0663(9) Uani 1 1 d . . . C18 C 0.5233(3) 0.92265(19) 0.31980(12) 0.0352(7) Uani 1 1 d . . . C2 C 0.8902(3) 0.6143(2) 0.38656(12) 0.0380(8) Uani 1 1 d . . . H2 H 0.8126 0.6045 0.3994 0.046 Uiso 1 1 calc R . . C20 C 0.5194(3) 1.05416(19) 0.31537(12) 0.0384(8) Uani 1 1 d . . . C8 C 1.0808(3) 0.5632(2) 0.50189(12) 0.0399(8) Uani 1 1 d . . . C7 C 1.0097(3) 0.5400(2) 0.45619(12) 0.0384(8) Uani 1 1 d . . . C6 C 0.9991(3) 0.6739(2) 0.32605(12) 0.0369(8) Uani 1 1 d . . . H6 H 0.9956 0.7033 0.2976 0.044 Uiso 1 1 calc R . . C3 C 1.0096(3) 0.5857(2) 0.41031(12) 0.0369(8) Uani 1 1 d . . . C22 C 0.5093(4) 0.9939(2) 0.39397(12) 0.0421(8) Uani 1 1 d . . . C19 C 0.5278(3) 0.98710(19) 0.29275(13) 0.0384(8) Uani 1 1 d . . . H19 H 0.5366 0.9849 0.2591 0.046 Uiso 1 1 calc R . . C23 C 0.5158(4) 0.92679(19) 0.36990(13) 0.0417(8) Uani 1 1 d . . . H23 H 0.5150 0.8832 0.3882 0.050 Uiso 1 1 calc R . . C33 C 0.5243(3) 0.8489(2) 0.29543(13) 0.0377(8) Uani 1 1 d . . . C13 C 1.0691(3) 0.5229(2) 0.54650(13) 0.0407(9) Uani 1 1 d . . . C21 C 0.5100(4) 1.0583(2) 0.36574(13) 0.0438(9) Uani 1 1 d . . . H21 H 0.5040 1.1043 0.3808 0.053 Uiso 1 1 calc R . . O10 O 0.0614(4) 0.8890(2) 0.42421(12) 0.0901(11) Uani 1 1 d . . . O11 O 1.3088(3) 0.7111(2) 0.55812(13) 0.0863(11) Uani 1 1 d . . . C28 C 0.6139(4) 1.0242(2) 0.48113(13) 0.0475(9) Uani 1 1 d . . . O12 O 1.2858(4) 0.6408(3) 0.63694(13) 0.1093(15) Uani 1 1 d U . . C9 C 1.1605(4) 0.6288(2) 0.50628(14) 0.0492(10) Uani 1 1 d . . . H9 H 1.1654 0.6571 0.4779 0.059 Uiso 1 1 calc R . . C25 C 0.3917(4) 0.97220(19) 0.46628(13) 0.0440(9) Uani 1 1 d . . . C12 C 1.1376(4) 0.5508(3) 0.59238(14) 0.0546(11) Uani 1 1 d . . . H12 H 1.1289 0.5266 0.6220 0.066 Uiso 1 1 calc R . . C26 C 0.2810(5) 0.9431(2) 0.43445(15) 0.0573(11) Uani 1 1 d . . . H26 H 0.2841 0.9393 0.4004 0.069 Uiso 1 1 calc R . . C10 C 1.2281(4) 0.6502(3) 0.55033(16) 0.0591(11) Uani 1 1 d . . . O9 O 0.9545(3) 1.0935(2) 0.48449(12) 0.0857(11) Uani 1 1 d . . . C29 C 0.7327(5) 1.0458(2) 0.46473(15) 0.0555(11) Uani 1 1 d . . . H29 H 0.7380 1.0418 0.4308 0.067 Uiso 1 1 calc R . . O7 O 0.4837(4) 1.18283(16) 0.30331(12) 0.0826(11) Uani 1 1 d . . . C27 C 0.1690(5) 0.9201(3) 0.45175(16) 0.0637(12) Uani 1 1 d . . . C11 C 1.2150(4) 0.6112(3) 0.59418(15) 0.0661(13) Uani 1 1 d . . . C30 C 0.8391(5) 1.0721(3) 0.49601(16) 0.0586(11) Uani 1 1 d . . . C15 C 1.3257(6) 0.7527(3) 0.5152(2) 0.0950(19) Uani 1 1 d . . . H15A H 1.3764 0.7243 0.4949 0.142 Uiso 1 1 calc R . . H15B H 1.3722 0.7979 0.5255 0.142 Uiso 1 1 calc R . . H15C H 1.2400 0.7642 0.4962 0.142 Uiso 1 1 calc R . . C31 C 0.9695(6) 1.0865(4) 0.4328(2) 0.112(2) Uani 1 1 d . . . H31A H 0.9084 1.1197 0.4130 0.167 Uiso 1 1 d R . . H31B H 1.0592 1.0998 0.4297 0.167 Uiso 1 1 d R . . H31C H 0.9521 1.0366 0.4213 0.167 Uiso 1 1 d R . . C32 C 0.0692(8) 0.8712(5) 0.3729(2) 0.132(3) Uani 1 1 d . . . H32A H 0.1165 0.9098 0.3588 0.197 Uiso 1 1 calc R . . H32B H -0.0191 0.8670 0.3542 0.197 Uiso 1 1 calc R . . H32C H 0.1155 0.8250 0.3716 0.197 Uiso 1 1 calc R . . C14 C 1.2748(8) 0.6026(5) 0.6828(2) 0.151(3) Uani 1 1 d U . . H14A H 1.3164 0.5548 0.6828 0.226 Uiso 1 1 calc R . . H14B H 1.1824 0.5964 0.6854 0.226 Uiso 1 1 calc R . . H14C H 1.3181 0.6310 0.7107 0.226 Uiso 1 1 calc R . . C34 C 0.5142(4) 1.1243(2) 0.28512(15) 0.0473(9) Uani 1 1 d . . . O2W O 0.5570(3) 0.81652(19) 0.14882(11) 0.0750(10) Uani 1 1 d . . . H2WA H 0.5288 0.7830 0.1277 0.090 Uiso 1 1 d R . . H2WB H 0.4888 0.8470 0.1527 0.113 Uiso 1 1 d R . . O1W O 0.8053(7) 0.8062(4) 0.2023(3) 0.089(2) Uiso 0.50 1 d P . . H1WA H 0.8060 0.8317 0.1759 0.107 Uiso 1 1 d R . . H1WB H 0.8770 0.7997 0.2228 0.107 Uiso 1 1 d R . . O1W' O 0.7778(12) 0.7255(7) 0.1774(5) 0.156(4) Uiso 0.50 1 d P . . H1WC H 0.8335 0.6849 0.1920 0.187 Uiso 0.50 1 calc PR . . H1WD H 0.7532 0.7232 0.1412 0.187 Uiso 0.50 1 calc PR . . 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 0.0219(2) 0.0321(3) 0.0287(3) 0.00041(17) 0.00773(17) -0.00122(17) Co2 0.0448(3) 0.0399(3) 0.0301(3) 0.00914(19) 0.0068(2) 0.0035(2) O4 0.0233(12) 0.0705(18) 0.0430(14) 0.0199(13) 0.0062(10) 0.0025(11) O3 0.0287(12) 0.0755(19) 0.0484(16) 0.0296(14) 0.0123(11) 0.0014(12) O1 0.0208(12) 0.085(2) 0.0574(17) 0.0240(15) 0.0067(11) 0.0056(12) O5 0.096(2) 0.0502(17) 0.0360(15) -0.0067(12) 0.0095(14) 0.0233(16) C16 0.0265(17) 0.051(2) 0.0303(18) 0.0052(15) 0.0022(14) 0.0036(15) C17 0.0229(16) 0.052(2) 0.0355(19) 0.0047(16) 0.0096(14) -0.0016(15) O2 0.0360(14) 0.106(2) 0.0452(16) 0.0395(16) 0.0044(12) 0.0167(15) C5 0.0243(16) 0.045(2) 0.0353(18) 0.0088(15) 0.0078(13) -0.0007(15) C4 0.0222(16) 0.061(2) 0.0353(18) 0.0161(17) 0.0038(13) 0.0017(16) C24 0.071(3) 0.0338(19) 0.0289(18) 0.0001(15) 0.0076(18) 0.0065(18) O6 0.0720(19) 0.0376(16) 0.080(2) -0.0185(15) 0.0337(16) -0.0084(14) C1 0.0228(15) 0.049(2) 0.0292(17) 0.0086(15) 0.0018(13) 0.0034(15) O8 0.0696(19) 0.073(2) 0.0618(19) 0.0354(16) 0.0280(15) 0.0128(16) C18 0.0405(18) 0.0348(18) 0.0304(18) -0.0015(14) 0.0065(14) 0.0038(15) C2 0.0212(15) 0.061(2) 0.0328(18) 0.0146(16) 0.0067(13) 0.0014(15) C20 0.047(2) 0.0336(19) 0.0340(19) 0.0059(15) 0.0056(15) 0.0011(16) C8 0.0253(16) 0.057(2) 0.0368(19) 0.0193(17) 0.0036(14) 0.0006(16) C7 0.0231(16) 0.058(2) 0.0336(19) 0.0189(16) 0.0033(14) 0.0019(16) C6 0.0301(17) 0.052(2) 0.0296(17) 0.0117(15) 0.0075(14) 0.0010(15) C3 0.0261(16) 0.053(2) 0.0309(18) 0.0166(16) 0.0036(13) 0.0007(15) C22 0.062(2) 0.038(2) 0.0269(17) 0.0035(15) 0.0095(16) 0.0023(18) C19 0.0423(19) 0.043(2) 0.0299(18) 0.0006(15) 0.0060(14) 0.0046(16) C23 0.062(2) 0.0307(18) 0.0325(19) 0.0039(14) 0.0078(16) 0.0030(17) C33 0.0408(19) 0.036(2) 0.0335(19) -0.0046(15) -0.0016(15) 0.0082(16) C13 0.0260(17) 0.057(2) 0.038(2) 0.0186(17) 0.0015(14) 0.0005(16) C21 0.064(2) 0.0325(19) 0.0344(19) -0.0018(15) 0.0073(17) 0.0042(17) O10 0.093(2) 0.120(3) 0.056(2) -0.0182(19) 0.0085(18) -0.040(2) O11 0.086(2) 0.091(2) 0.073(2) 0.0194(19) -0.0150(18) -0.049(2) C28 0.074(3) 0.035(2) 0.034(2) -0.0007(16) 0.0111(19) 0.0088(19) O12 0.119(3) 0.143(4) 0.053(2) 0.018(2) -0.0240(19) -0.075(3) C9 0.0386(19) 0.062(3) 0.045(2) 0.0212(19) 0.0006(17) -0.0085(18) C25 0.070(2) 0.0329(19) 0.0294(18) -0.0020(15) 0.0086(17) 0.0020(18) C12 0.043(2) 0.079(3) 0.038(2) 0.019(2) -0.0032(17) -0.011(2) C26 0.084(3) 0.053(3) 0.035(2) -0.0034(18) 0.009(2) -0.006(2) C10 0.051(2) 0.064(3) 0.059(3) 0.016(2) 0.001(2) -0.017(2) O9 0.082(2) 0.119(3) 0.061(2) -0.011(2) 0.0245(18) -0.021(2) C29 0.083(3) 0.051(2) 0.035(2) -0.0019(18) 0.016(2) -0.001(2) O7 0.144(3) 0.0346(17) 0.058(2) 0.0039(14) -0.015(2) 0.0160(18) C27 0.081(3) 0.059(3) 0.048(3) -0.007(2) 0.003(2) -0.012(2) C11 0.054(2) 0.093(4) 0.044(2) 0.017(2) -0.0156(19) -0.023(2) C30 0.066(3) 0.062(3) 0.048(2) 0.001(2) 0.011(2) -0.005(2) C15 0.109(4) 0.066(3) 0.108(5) 0.029(3) 0.010(4) -0.036(3) C31 0.089(4) 0.178(7) 0.075(4) -0.018(4) 0.036(3) -0.033(4) C32 0.153(6) 0.175(8) 0.061(4) -0.028(4) -0.001(4) -0.073(6) C14 0.161(6) 0.213(7) 0.063(4) 0.025(4) -0.028(4) -0.091(5) C34 0.047(2) 0.046(2) 0.046(2) 0.0118(18) -0.0016(18) 0.0027(18) O2W 0.094(2) 0.086(2) 0.0441(17) 0.0259(15) 0.0096(16) 0.0253(19) _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 O8 1.928(3) 2_645 ? Co1 O6 1.933(3) . ? Co1 O1 1.966(2) . ? Co1 O4 2.014(2) 1_455 ? Co1 O3 2.298(2) 1_455 ? Co1 C17 2.483(3) 1_455 ? Co2 O1W 1.923(7) . ? Co2 O7 1.978(3) 2_645 ? Co2 O5 1.983(3) . ? Co2 O1W' 2.023(12) . ? Co2 O2 2.041(2) . ? Co2 O2W 2.110(3) . ? O4 C17 1.257(4) . ? O4 Co1 2.014(2) 1_655 ? O3 C17 1.234(4) . ? O3 Co1 2.298(2) 1_655 ? O1 C16 1.238(4) . ? O5 C33 1.247(4) . ? C16 O2 1.223(4) . ? C16 C1 1.486(4) . ? C17 C5 1.488(4) . ? C17 Co1 2.483(3) 1_655 ? C5 C4 1.372(4) . ? C5 C6 1.381(4) . ? C4 C3 1.375(4) . ? C4 H4 0.9300 . ? C24 C25 1.385(5) . ? C24 C28 1.394(5) . ? C24 C22 1.485(5) . ? O6 C33 1.232(4) . ? C1 C6 1.373(4) . ? C1 C2 1.378(4) . ? O8 C34 1.237(5) . ? O8 Co1 1.928(3) 2_655 ? C18 C23 1.372(5) . ? C18 C19 1.378(5) . ? C18 C33 1.486(5) . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C20 C19 1.364(5) . ? C20 C21 1.383(5) . ? C20 C34 1.503(5) . ? C8 C7 1.391(5) . ? C8 C9 1.429(5) . ? C8 C13 1.430(4) . ? C7 C13 1.385(5) 3_766 ? C7 C3 1.490(4) . ? C6 H6 0.9300 . ? C22 C23 1.381(5) . ? C22 C21 1.391(5) . ? C19 H19 0.9300 . ? C23 H23 0.9300 . ? C13 C7 1.385(5) 3_766 ? C13 C12 1.414(5) . ? C21 H21 0.9300 . ? O10 C27 1.343(5) . ? O10 C32 1.438(6) . ? O11 C10 1.366(5) . ? O11 C15 1.416(6) . ? C28 C29 1.408(6) . ? C28 C25 1.435(5) 3_676 ? O12 C11 1.368(5) . ? O12 C14 1.439(7) . ? C9 C10 1.333(6) . ? C9 H9 0.9300 . ? C25 C26 1.404(6) . ? C25 C28 1.435(5) 3_676 ? C12 C11 1.340(6) . ? C12 H12 0.9300 . ? C26 C27 1.364(6) . ? C26 H26 0.9300 . ? C10 C11 1.404(6) . ? O9 C30 1.319(5) . ? O9 C31 1.436(6) . ? C29 C30 1.347(6) . ? C29 H29 0.9300 . ? O7 C34 1.226(5) . ? O7 Co2 1.978(3) 2_655 ? C27 C30 1.436(6) 3_676 ? C30 C27 1.436(6) 3_676 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C31 H31A 0.9602 . ? C31 H31B 0.9602 . ? C31 H31C 0.9598 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.9046 . ? O1W O1W' 1.608(13) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O1W' H1WC 0.9700 . ? O1W' H1WD 0.9700 . ? 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 O8 Co1 O6 139.82(14) 2_645 . ? O8 Co1 O1 96.25(13) 2_645 . ? O6 Co1 O1 96.62(13) . . ? O8 Co1 O4 102.62(12) 2_645 1_455 ? O6 Co1 O4 109.88(12) . 1_455 ? O1 Co1 O4 106.35(10) . 1_455 ? O8 Co1 O3 88.94(12) 2_645 1_455 ? O6 Co1 O3 87.56(12) . 1_455 ? O1 Co1 O3 166.05(10) . 1_455 ? O4 Co1 O3 59.79(9) 1_455 1_455 ? O8 Co1 C17 95.72(12) 2_645 1_455 ? O6 Co1 C17 100.55(12) . 1_455 ? O1 Co1 C17 136.57(11) . 1_455 ? O4 Co1 C17 30.21(10) 1_455 1_455 ? O3 Co1 C17 29.60(10) 1_455 1_455 ? O1W Co2 O7 140.3(2) . 2_645 ? O1W Co2 O5 105.3(2) . . ? O7 Co2 O5 113.09(15) 2_645 . ? O1W Co2 O1W' 48.0(4) . . ? O7 Co2 O1W' 92.7(4) 2_645 . ? O5 Co2 O1W' 153.1(4) . . ? O1W Co2 O2 87.9(3) . . ? O7 Co2 O2 97.73(13) 2_645 . ? O5 Co2 O2 95.80(12) . . ? O1W' Co2 O2 87.5(4) . . ? O1W Co2 O2W 84.1(3) . . ? O7 Co2 O2W 86.37(14) 2_645 . ? O5 Co2 O2W 89.47(12) . . ? O1W' Co2 O2W 84.8(4) . . ? O2 Co2 O2W 171.41(12) . . ? C17 O4 Co1 96.03(19) . 1_655 ? C17 O3 Co1 83.55(18) . 1_655 ? C16 O1 Co1 123.9(2) . . ? C33 O5 Co2 134.9(3) . . ? O2 C16 O1 125.9(3) . . ? O2 C16 C1 117.8(3) . . ? O1 C16 C1 116.3(3) . . ? O3 C17 O4 120.5(3) . . ? O3 C17 C5 120.4(3) . . ? O4 C17 C5 119.0(3) . . ? O3 C17 Co1 66.85(16) . 1_655 ? O4 C17 Co1 53.76(15) . 1_655 ? C5 C17 Co1 172.7(2) . 1_655 ? C16 O2 Co2 149.9(2) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 C17 120.3(3) . . ? C6 C5 C17 120.1(3) . . ? C5 C4 C3 121.2(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C25 C24 C28 121.0(3) . . ? C25 C24 C22 119.8(3) . . ? C28 C24 C22 119.2(3) . . ? C33 O6 Co1 135.5(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 C16 121.2(3) . . ? C2 C1 C16 119.2(3) . . ? C34 O8 Co1 127.6(3) . 2_655 ? C23 C18 C19 119.4(3) . . ? C23 C18 C33 119.5(3) . . ? C19 C18 C33 121.1(3) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C19 C20 C21 120.6(3) . . ? C19 C20 C34 120.1(3) . . ? C21 C20 C34 119.2(3) . . ? C7 C8 C9 121.9(3) . . ? C7 C8 C13 119.7(3) . . ? C9 C8 C13 118.3(3) . . ? C13 C7 C8 120.4(3) 3_766 . ? C13 C7 C3 119.2(3) 3_766 . ? C8 C7 C3 120.3(3) . . ? C1 C6 C5 120.0(3) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C4 C3 C2 118.4(3) . . ? C4 C3 C7 123.0(3) . . ? C2 C3 C7 118.5(3) . . ? C23 C22 C21 117.9(3) . . ? C23 C22 C24 121.0(3) . . ? C21 C22 C24 121.1(3) . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C18 C23 C22 121.9(3) . . ? C18 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? O6 C33 O5 126.0(3) . . ? O6 C33 C18 115.5(3) . . ? O5 C33 C18 118.5(3) . . ? C7 C13 C12 122.5(3) 3_766 . ? C7 C13 C8 119.9(3) 3_766 . ? C12 C13 C8 117.6(3) . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C27 O10 C32 117.4(4) . . ? C10 O11 C15 116.7(4) . . ? C24 C28 C29 122.5(3) . . ? C24 C28 C25 119.2(4) . 3_676 ? C29 C28 C25 118.3(4) . 3_676 ? C11 O12 C14 115.9(4) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C24 C25 C26 122.2(3) . . ? C24 C25 C28 119.8(3) . 3_676 ? C26 C25 C28 117.9(4) . 3_676 ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C27 C26 C25 122.3(4) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C9 C10 O11 125.5(4) . . ? C9 C10 C11 120.3(4) . . ? O11 C10 C11 114.1(4) . . ? C30 O9 C31 116.3(4) . . ? C30 C29 C28 122.9(4) . . ? C30 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C34 O7 Co2 137.1(3) . 2_655 ? O10 C27 C26 125.9(4) . . ? O10 C27 C30 114.5(4) . 3_676 ? C26 C27 C30 119.5(4) . 3_676 ? C12 C11 O12 125.0(4) . . ? C12 C11 C10 120.8(4) . . ? O12 C11 C10 114.2(4) . . ? O9 C30 C29 127.5(4) . . ? O9 C30 C27 113.5(4) . 3_676 ? C29 C30 C27 118.9(4) . 3_676 ? O11 C15 H15A 109.5 . . ? O11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O9 C31 H31A 109.1 . . ? O9 C31 H31B 108.5 . . ? H31A C31 H31B 109.5 . . ? O9 C31 H31C 110.8 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.4 . . ? O10 C32 H32A 109.5 . . ? O10 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O10 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C14 H14A 109.5 . . ? O12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O7 C34 O8 125.0(4) . . ? O7 C34 C20 119.7(4) . . ? O8 C34 C20 115.3(4) . . ? Co2 O2W H2WA 108.8 . . ? Co2 O2W H2WB 111.9 . . ? H2WA O2W H2WB 109.3 . . ? O1W' O1W Co2 69.2(5) . . ? O1W' O1W H1WA 99.3 . . ? Co2 O1W H1WA 120.3 . . ? O1W' O1W H1WB 102.8 . . ? Co2 O1W H1WB 119.7 . . ? H1WA O1W H1WB 120.0 . . ? O1W O1W' Co2 62.7(5) . . ? O1W O1W' H1WC 117.5 . . ? Co2 O1W' H1WC 117.5 . . ? O1W O1W' H1WD 117.5 . . ? Co2 O1W' H1WD 117.5 . . ? H1WC O1W' H1WD 114.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.633 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.070 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.280 0.108 -0.110 2118 562 ' ' _platon_squeeze_details ; ; _vrf_CHEMW03_p4 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This is caused by the given molecular weight being increased from the atom count to account for 2 disordered NMP molecules, 1 disordered DMA molecule, and 2 disordered water molecule omitted by SQUEEZE. ; _database_code_depnum_ccdc_archive 'CCDC 967539' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H56 N2 O20 Zn2' _chemical_formula_weight 1111.69 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.107(4) _cell_length_b 18.338(7) _cell_length_c 27.084(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.285(8) _cell_angle_gamma 90.00 _cell_volume 4954(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9023 _exptl_absorpt_correction_T_max 0.9896 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28358 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11147 _reflns_number_gt 6207 _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^)+(0.0683P)^2^+0.0000P] 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 11147 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 Zn1 Zn 0.46427(4) 0.80393(2) 0.307576(14) 0.02792(11) Uani 1 1 d . . . Zn2 Zn 0.63667(4) 0.73013(2) 0.219178(15) 0.03267(12) Uani 1 1 d . . . O4 O -0.3532(2) 0.82958(15) 0.33933(10) 0.0519(7) Uani 1 1 d . . . O7 O 0.4835(3) 0.69871(14) 0.31377(11) 0.0545(7) Uani 1 1 d . . . C6 C -0.1132(3) 0.88177(19) 0.38873(13) 0.0351(8) Uani 1 1 d . . . H6 H -0.1912 0.8933 0.4011 0.042 Uiso 1 1 calc R . . C1 C -0.1214(3) 0.83738(18) 0.34702(12) 0.0300(7) Uani 1 1 d . . . O8 O 0.5664(3) 0.64691(13) 0.25119(9) 0.0522(7) Uani 1 1 d . . . O3 O -0.2540(3) 0.77277(16) 0.28356(10) 0.0564(8) Uani 1 1 d . . . C2 C -0.0054(3) 0.81919(18) 0.32940(13) 0.0343(8) Uani 1 1 d . . . H2 H -0.0093 0.7890 0.3016 0.041 Uiso 1 1 calc R . . C22 C 0.5099(4) 0.44396(18) 0.31553(13) 0.0347(8) Uani 1 1 d . . . C7 C -0.2525(3) 0.8104(2) 0.32107(13) 0.0353(8) Uani 1 1 d . . . C26 C 0.5016(4) 0.50493(18) 0.44826(13) 0.0395(9) Uani 1 1 d . . . C24 C 0.5257(4) 0.64519(19) 0.29228(14) 0.0367(8) Uani 1 1 d . . . C10 C 0.0740(3) 0.9347(2) 0.50403(13) 0.0382(9) Uani 1 1 d . . . C9 C 0.0086(3) 0.9572(2) 0.45756(13) 0.0357(8) Uani 1 1 d . . . O5 O 0.2928(3) 0.78713(16) 0.56520(11) 0.0685(9) Uani 1 1 d . . . C3 C 0.1163(3) 0.8455(2) 0.35284(13) 0.0373(8) Uani 1 1 d . . . C15 C 0.0646(3) 0.9773(2) 0.54769(13) 0.0394(9) Uani 1 1 d . . . C21 C 0.5007(4) 0.44277(19) 0.36595(13) 0.0401(9) Uani 1 1 d . . . H21 H 0.4905 0.3985 0.3816 0.048 Uiso 1 1 calc R . . C5 C 0.0076(3) 0.9095(2) 0.41251(13) 0.0357(8) Uani 1 1 d . . . C20 C 0.5065(4) 0.50727(19) 0.39349(13) 0.0407(9) Uani 1 1 d . . . C18 C 0.5223(3) 0.57361(18) 0.31818(12) 0.0326(8) Uani 1 1 d . . . C19 C 0.5130(4) 0.57191(18) 0.36805(13) 0.0373(8) Uani 1 1 d . . . H19 H 0.5111 0.6157 0.3853 0.045 Uiso 1 1 calc R . . C4 C 0.1234(3) 0.8909(2) 0.39433(13) 0.0384(9) Uani 1 1 d . . . H4 H 0.2059 0.9088 0.4098 0.046 Uiso 1 1 calc R . . C30 C 0.6131(4) 0.47673(18) 0.48071(13) 0.0413(9) Uani 1 1 d . . . C23 C 0.5247(3) 0.50925(18) 0.29211(12) 0.0335(8) Uani 1 1 d . . . H23 H 0.5362 0.5100 0.2587 0.040 Uiso 1 1 calc R . . C27 C 0.3899(4) 0.52919(19) 0.46752(13) 0.0399(9) Uani 1 1 d . . . C11 C 0.1505(4) 0.8685(2) 0.51082(14) 0.0470(10) Uani 1 1 d . . . H11 H 0.1556 0.8392 0.4832 0.056 Uiso 1 1 calc R . . C31 C 0.7336(4) 0.4562(2) 0.46289(15) 0.0517(10) Uani 1 1 d . . . H31 H 0.7388 0.4623 0.4292 0.062 Uiso 1 1 calc R . . O12 O 0.0599(3) 0.6157(2) 0.42883(12) 0.0827(10) Uani 1 1 d . . . C13 C 0.2012(4) 0.8887(2) 0.59945(15) 0.0517(11) Uani 1 1 d . . . C28 C 0.2756(4) 0.5603(2) 0.43582(15) 0.0500(10) Uani 1 1 d . . . H28 H 0.2770 0.5656 0.4018 0.060 Uiso 1 1 calc R . . C14 C 0.1292(4) 0.9507(2) 0.59530(14) 0.0486(10) Uani 1 1 d . . . H14 H 0.1210 0.9769 0.6240 0.058 Uiso 1 1 calc R . . C12 C 0.2150(4) 0.8476(2) 0.55590(16) 0.0520(11) Uani 1 1 d . . . O11 O 0.9568(3) 0.4083(2) 0.48040(12) 0.0851(11) Uani 1 1 d . . . C33 C 0.9688(6) 0.4221(4) 0.4287(2) 0.117(2) Uani 1 1 d . . . H33A H 0.9078 0.3912 0.4073 0.175 Uiso 1 1 calc R . . H33B H 1.0589 0.4122 0.4237 0.175 Uiso 1 1 calc R . . H33C H 0.9476 0.4722 0.4208 0.175 Uiso 1 1 calc R . . C32 C 0.8387(5) 0.4288(2) 0.49328(16) 0.0575(11) Uani 1 1 d . . . C17 C 0.3079(6) 0.7435(3) 0.5228(2) 0.0899(18) Uani 1 1 d . . . H17A H 0.3380 0.7735 0.4978 0.135 Uiso 1 1 calc R . . H17B H 0.2232 0.7218 0.5093 0.135 Uiso 1 1 calc R . . H17C H 0.3725 0.7057 0.5328 0.135 Uiso 1 1 calc R . . C29 C 0.1679(5) 0.5817(2) 0.45464(16) 0.0577(11) Uani 1 1 d . . . O2 O 0.3533(2) 0.84565(16) 0.35613(10) 0.0528(7) Uani 1 1 d . . . O1 O 0.2355(2) 0.78669(16) 0.29485(10) 0.0529(7) Uani 1 1 d . . . O2W O 0.5468(3) 0.69222(16) 0.14686(10) 0.0593(8) Uani 1 1 d . . . H2WA H 0.4593 0.6884 0.1450 0.089 Uiso 1 1 d R . . H2WB H 0.5776 0.6489 0.1401 0.089 Uiso 1 1 d R . . O9 O 0.5518(3) 0.37242(14) 0.24843(11) 0.0550(7) Uani 1 1 d . . . C8 C 0.2417(3) 0.8241(2) 0.33300(14) 0.0389(9) Uani 1 1 d . . . O10 O 0.4423(4) 0.32323(15) 0.30357(11) 0.0835(12) Uani 1 1 d . . . O1W O 0.8059(3) 0.7007(2) 0.19800(13) 0.0961(13) Uani 1 1 d . . . H1WA H 0.8200 0.6483 0.1813 0.144 Uiso 1 1 d R . . H1WB H 0.8920 0.6974 0.2251 0.144 Uiso 1 1 d R . . C34 C 0.0654(7) 0.6394(4) 0.3790(2) 0.125(3) Uani 1 1 d . . . H34A H 0.0747 0.5978 0.3583 0.187 Uiso 1 1 calc R . . H34B H 0.1408 0.6713 0.3792 0.187 Uiso 1 1 calc R . . H34C H -0.0156 0.6650 0.3661 0.187 Uiso 1 1 calc R . . C25 C 0.5005(4) 0.3738(2) 0.28674(13) 0.0398(9) Uani 1 1 d . . . O6 O 0.2663(3) 0.86003(18) 0.64279(11) 0.0730(9) Uani 1 1 d . . . C16 C 0.2452(6) 0.8953(4) 0.68812(18) 0.119(3) Uani 1 1 d . . . H16A H 0.1508 0.9005 0.6882 0.179 Uiso 1 1 calc R . . H16B H 0.2865 0.9426 0.6901 0.179 Uiso 1 1 calc R . . H16C H 0.2843 0.8665 0.7163 0.179 Uiso 1 1 calc 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 Zn1 0.0237(2) 0.0319(2) 0.0289(2) 0.00003(17) 0.00668(15) 0.00203(17) Zn2 0.0379(2) 0.0328(2) 0.0281(2) -0.00209(17) 0.00759(17) -0.00305(18) O4 0.0267(14) 0.0753(19) 0.0538(18) -0.0264(15) 0.0073(12) -0.0055(13) O7 0.0614(18) 0.0319(15) 0.078(2) 0.0120(14) 0.0355(16) 0.0094(13) C6 0.0183(17) 0.056(2) 0.032(2) -0.0104(17) 0.0070(14) 0.0038(15) C1 0.0250(17) 0.0391(19) 0.0249(18) -0.0063(15) 0.0003(14) 0.0021(15) O8 0.090(2) 0.0404(15) 0.0278(15) -0.0010(11) 0.0130(14) -0.0139(15) O3 0.0373(15) 0.088(2) 0.0444(17) -0.0316(16) 0.0071(12) -0.0118(14) C2 0.0267(18) 0.044(2) 0.032(2) -0.0114(15) 0.0028(14) 0.0023(15) C22 0.042(2) 0.0312(19) 0.030(2) -0.0020(15) 0.0024(15) 0.0005(16) C7 0.0314(19) 0.047(2) 0.0271(19) -0.0053(16) 0.0045(15) -0.0046(17) C26 0.064(3) 0.0297(19) 0.0233(19) -0.0003(15) 0.0031(17) -0.0010(18) C24 0.038(2) 0.034(2) 0.036(2) 0.0031(16) -0.0022(16) -0.0073(16) C10 0.0257(18) 0.052(2) 0.036(2) -0.0181(17) 0.0018(15) 0.0016(17) C9 0.0192(17) 0.055(2) 0.032(2) -0.0147(17) 0.0005(14) 0.0012(16) O5 0.073(2) 0.066(2) 0.060(2) -0.0113(16) -0.0104(16) 0.0333(17) C3 0.0234(18) 0.055(2) 0.034(2) -0.0099(17) 0.0079(15) 0.0010(16) C15 0.0245(18) 0.059(3) 0.032(2) -0.0169(18) -0.0019(15) 0.0018(17) C21 0.060(2) 0.0288(19) 0.031(2) 0.0056(15) 0.0035(17) -0.0001(17) C5 0.0297(19) 0.048(2) 0.030(2) -0.0117(16) 0.0062(15) -0.0009(16) C20 0.059(2) 0.035(2) 0.028(2) 0.0001(16) 0.0067(17) -0.0008(18) C18 0.041(2) 0.0315(19) 0.0261(19) 0.0022(14) 0.0063(15) 0.0021(16) C19 0.055(2) 0.0263(19) 0.032(2) -0.0022(15) 0.0088(17) -0.0026(16) C4 0.0265(19) 0.054(2) 0.034(2) -0.0097(17) 0.0028(15) 0.0023(17) C30 0.061(2) 0.031(2) 0.033(2) -0.0035(16) 0.0080(18) -0.0004(18) C23 0.044(2) 0.0350(19) 0.0211(18) -0.0017(14) 0.0027(15) -0.0024(16) C27 0.061(2) 0.035(2) 0.0216(19) 0.0006(15) 0.0013(17) -0.0020(18) C11 0.035(2) 0.064(3) 0.040(2) -0.0202(19) -0.0002(17) 0.0080(19) C31 0.068(3) 0.056(3) 0.032(2) 0.0047(19) 0.011(2) 0.003(2) O12 0.076(2) 0.114(3) 0.056(2) 0.019(2) 0.0043(17) 0.029(2) C13 0.044(2) 0.069(3) 0.037(2) -0.009(2) -0.0096(18) 0.010(2) C28 0.067(3) 0.050(2) 0.032(2) 0.0024(18) 0.004(2) 0.001(2) C14 0.036(2) 0.070(3) 0.036(2) -0.019(2) -0.0052(17) 0.013(2) C12 0.038(2) 0.061(3) 0.053(3) -0.011(2) -0.0051(19) 0.008(2) O11 0.076(2) 0.124(3) 0.060(2) 0.016(2) 0.0244(18) 0.024(2) C33 0.100(5) 0.185(7) 0.077(4) 0.030(4) 0.049(4) 0.045(5) C32 0.060(3) 0.070(3) 0.046(3) 0.009(2) 0.016(2) 0.006(2) C17 0.106(4) 0.068(3) 0.091(4) -0.024(3) 0.002(3) 0.040(3) C29 0.063(3) 0.064(3) 0.043(3) 0.006(2) -0.002(2) 0.010(2) O2 0.0230(14) 0.083(2) 0.0531(18) -0.0166(15) 0.0082(12) 0.0059(13) O1 0.0357(15) 0.075(2) 0.0521(18) -0.0226(15) 0.0185(13) 0.0011(13) O2W 0.0584(18) 0.074(2) 0.0436(17) -0.0111(15) 0.0020(14) -0.0067(16) O9 0.0566(18) 0.0558(17) 0.0577(19) -0.0257(14) 0.0244(14) -0.0122(14) C8 0.027(2) 0.051(2) 0.040(2) 0.0023(18) 0.0087(16) 0.0089(16) O10 0.171(4) 0.0383(17) 0.046(2) -0.0073(14) 0.033(2) -0.035(2) O1W 0.052(2) 0.158(4) 0.080(3) -0.069(2) 0.0142(17) -0.002(2) C34 0.123(5) 0.173(7) 0.078(5) 0.068(4) 0.015(4) 0.061(5) C25 0.051(2) 0.040(2) 0.027(2) -0.0022(16) 0.0022(17) -0.0048(18) O6 0.075(2) 0.096(2) 0.0391(18) -0.0088(16) -0.0172(15) 0.0307(19) C16 0.131(5) 0.180(7) 0.037(3) -0.004(4) -0.014(3) 0.068(5) _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 O7 1.944(3) . ? Zn1 O9 1.956(3) 2_655 ? Zn1 O4 1.963(2) 1_655 ? Zn1 O2 2.012(2) . ? Zn1 O1 2.304(3) . ? Zn1 C8 2.484(4) . ? Zn2 O10 1.943(3) 2_655 ? Zn2 O8 1.945(3) . ? Zn2 O1W 1.965(3) . ? Zn2 O3 2.062(3) 1_655 ? Zn2 O2W 2.138(3) . ? O4 C7 1.251(4) . ? O4 Zn1 1.962(2) 1_455 ? O7 C24 1.251(4) . ? C6 C5 1.382(4) . ? C6 C1 1.384(4) . ? C6 H6 0.9300 . ? C1 C2 1.375(4) . ? C1 C7 1.481(4) . ? O8 C24 1.248(4) . ? O3 C7 1.227(4) . ? O3 Zn2 2.062(3) 1_455 ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C22 C23 1.374(5) . ? C22 C21 1.384(5) . ? C22 C25 1.499(5) . ? C26 C27 1.391(5) . ? C26 C30 1.411(5) . ? C26 C20 1.493(5) . ? C24 C18 1.491(5) . ? C10 C9 1.386(5) . ? C10 C15 1.433(4) . ? C10 C11 1.436(5) . ? C9 C15 1.407(5) 3_576 ? C9 C5 1.500(4) . ? O5 C12 1.359(5) . ? O5 C17 1.428(5) . ? C3 C4 1.391(5) . ? C3 C8 1.506(5) . ? C15 C9 1.407(5) 3_576 ? C15 C14 1.433(5) . ? C21 C20 1.395(5) . ? C21 H21 0.9300 . ? C5 C4 1.384(5) . ? C20 C19 1.378(5) . ? C18 C19 1.369(5) . ? C18 C23 1.378(4) . ? C19 H19 0.9300 . ? C4 H4 0.9300 . ? C30 C27 1.412(5) 3_666 ? C30 C31 1.431(5) . ? C23 H23 0.9300 . ? C27 C30 1.412(5) 3_666 ? C27 C28 1.442(5) . ? C11 C12 1.344(5) . ? C11 H11 0.9300 . ? C31 C32 1.333(6) . ? C31 H31 0.9300 . ? O12 C29 1.351(5) . ? O12 C34 1.426(6) . ? C13 C14 1.344(5) . ? C13 O6 1.356(5) . ? C13 C12 1.426(5) . ? C28 C29 1.333(6) . ? C28 H28 0.9300 . ? C14 H14 0.9300 . ? O11 C32 1.350(5) . ? O11 C33 1.448(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C32 C29 1.436(6) 3_666 ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C29 C32 1.436(6) 3_666 ? O2 C8 1.262(4) . ? O1 C8 1.234(4) . ? O2W H2WA 0.8813 . ? O2W H2WB 0.8837 . ? O9 C25 1.233(4) . ? O9 Zn1 1.956(3) 2_645 ? O10 C25 1.225(4) . ? O10 Zn2 1.943(3) 2_645 ? O1W H1WA 1.0824 . ? O1W H1WB 1.0457 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? O6 C16 1.434(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 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 O7 Zn1 O9 134.35(12) . 2_655 ? O7 Zn1 O4 97.25(12) . 1_655 ? O9 Zn1 O4 98.08(12) 2_655 1_655 ? O7 Zn1 O2 112.30(12) . . ? O9 Zn1 O2 106.10(12) 2_655 . ? O4 Zn1 O2 101.90(11) 1_655 . ? O7 Zn1 O1 87.74(11) . . ? O9 Zn1 O1 90.93(11) 2_655 . ? O4 Zn1 O1 161.46(10) 1_655 . ? O2 Zn1 O1 59.88(10) . . ? O7 Zn1 C8 101.92(12) . . ? O9 Zn1 C8 98.83(12) 2_655 . ? O4 Zn1 C8 132.22(12) 1_655 . ? O2 Zn1 C8 30.34(11) . . ? O1 Zn1 C8 29.56(10) . . ? O10 Zn2 O8 132.06(15) 2_655 . ? O10 Zn2 O1W 118.78(17) 2_655 . ? O8 Zn2 O1W 108.19(16) . . ? O10 Zn2 O3 94.11(14) 2_655 1_655 ? O8 Zn2 O3 96.02(12) . 1_655 ? O1W Zn2 O3 88.74(12) . 1_655 ? O10 Zn2 O2W 84.44(13) 2_655 . ? O8 Zn2 O2W 91.24(11) . . ? O1W Zn2 O2W 84.51(13) . . ? O3 Zn2 O2W 171.34(11) 1_655 . ? C7 O4 Zn1 121.8(2) . 1_455 ? C24 O7 Zn1 140.9(3) . . ? C5 C6 C1 121.9(3) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C2 C1 C6 118.9(3) . . ? C2 C1 C7 120.1(3) . . ? C6 C1 C7 121.0(3) . . ? C24 O8 Zn2 127.9(2) . . ? C7 O3 Zn2 147.9(2) . 1_455 ? C1 C2 C3 120.2(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 C25 120.7(3) . . ? C21 C22 C25 119.4(3) . . ? O3 C7 O4 125.7(3) . . ? O3 C7 C1 118.1(3) . . ? O4 C7 C1 116.2(3) . . ? C27 C26 C30 119.9(3) . . ? C27 C26 C20 121.5(3) . . ? C30 C26 C20 118.6(3) . . ? O8 C24 O7 125.6(3) . . ? O8 C24 C18 118.5(3) . . ? O7 C24 C18 115.9(3) . . ? C9 C10 C15 120.1(3) . . ? C9 C10 C11 122.4(3) . . ? C15 C10 C11 117.5(3) . . ? C10 C9 C15 120.8(3) . 3_576 ? C10 C9 C5 120.3(3) . . ? C15 C9 C5 118.8(3) 3_576 . ? C12 O5 C17 116.2(3) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 C8 119.0(3) . . ? C4 C3 C8 120.5(3) . . ? C9 C15 C10 119.1(3) 3_576 . ? C9 C15 C14 122.5(3) 3_576 . ? C10 C15 C14 118.4(3) . . ? C22 C21 C20 120.7(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C6 C5 C4 118.5(3) . . ? C6 C5 C9 118.9(3) . . ? C4 C5 C9 122.5(3) . . ? C19 C20 C21 117.6(3) . . ? C19 C20 C26 122.2(3) . . ? C21 C20 C26 120.1(3) . . ? C19 C18 C23 119.7(3) . . ? C19 C18 C24 119.6(3) . . ? C23 C18 C24 120.6(3) . . ? C18 C19 C20 122.0(3) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C26 C30 C27 120.3(3) . 3_666 ? C26 C30 C31 121.6(4) . . ? C27 C30 C31 118.1(3) 3_666 . ? C22 C23 C18 119.8(3) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C26 C27 C30 119.8(3) . 3_666 ? C26 C27 C28 121.6(3) . . ? C30 C27 C28 118.6(4) 3_666 . ? C12 C11 C10 122.0(3) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C32 C31 C30 121.9(4) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C29 O12 C34 118.6(4) . . ? C14 C13 O6 125.5(4) . . ? C14 C13 C12 120.1(4) . . ? O6 C13 C12 114.4(4) . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C11 C12 O5 125.6(4) . . ? C11 C12 C13 120.2(4) . . ? O5 C12 C13 114.1(4) . . ? C32 O11 C33 114.6(4) . . ? O11 C33 H33A 109.5 . . ? O11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C32 O11 126.5(4) . . ? C31 C32 C29 119.9(4) . 3_666 ? O11 C32 C29 113.6(4) . 3_666 ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C28 C29 O12 125.4(4) . . ? C28 C29 C32 120.5(4) . 3_666 ? O12 C29 C32 114.1(4) . 3_666 ? C8 O2 Zn1 96.0(2) . . ? C8 O1 Zn1 83.3(2) . . ? Zn2 O2W H2WA 110.7 . . ? Zn2 O2W H2WB 111.8 . . ? H2WA O2W H2WB 107.4 . . ? C25 O9 Zn1 132.3(3) . 2_645 ? O1 C8 O2 120.7(3) . . ? O1 C8 C3 120.8(3) . . ? O2 C8 C3 118.5(3) . . ? O1 C8 Zn1 67.12(19) . . ? O2 C8 Zn1 53.66(17) . . ? C3 C8 Zn1 171.7(3) . . ? C25 O10 Zn2 138.2(3) . 2_645 ? Zn2 O1W H1WA 123.1 . . ? Zn2 O1W H1WB 118.4 . . ? H1WA O1W H1WB 95.3 . . ? O12 C34 H34A 109.5 . . ? O12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O10 C25 O9 126.1(4) . . ? O10 C25 C22 116.8(3) . . ? O9 C25 C22 117.1(3) . . ? C13 O6 C16 116.6(4) . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.785 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.087 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.241 0.609 0.129 2138 741 ' ' _platon_squeeze_details ; ; _vrf_CHEMW03_p5 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This is caused by the given molecular weight being increased from the atom count to account for 2 disordered NMP molecules, 1 disordered DOE molecule, and 2 disordered water molecule omitted by SQUEEZE. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 967540'