data_pbcn_Co_80k_H2O_ini _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA. M. KAWANO, M. TOMINAGA. M. FUJITA ; _journal_name_full 'Angew. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Co N6 O20' _chemical_formula_weight 971.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.681(2) _cell_length_b 20.6169(19) _cell_length_c 8.7336(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4263.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _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 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9297 _exptl_absorpt_correction_T_max 0.9524 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23007 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.48 _reflns_number_total 5064 _reflns_number_gt 3280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C23 to O5 and C24 to O4) converged to 51% and 49%, respectively. The occupancy of the disordered nitrate ions (N10 to O12, N11 to O17) converged to 60%, and 40%,respectively. The thermal temperature factors of all atoms were anisotropically refined. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered ethylene glycol groups and nitrate ions. ; _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^)+(0.1392P)^2^+16.0087P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5064 _refine_ls_number_parameters 379 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2716 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.003 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 1.0000 0.79523(4) 0.2500 0.0290(3) Uani 1 2 d S . . N1 N 0.93562(14) 0.72136(17) 0.2639(5) 0.0285(9) Uani 1 1 d . . . N2 N 0.93542(14) 0.86746(18) 0.2747(5) 0.0313(9) Uani 1 1 d . . . O1 O 0.99165(14) 0.79473(18) 0.0113(5) 0.0445(9) Uani 1 1 d . . . O2 O 0.86218(12) 0.48887(15) 0.3056(4) 0.0329(8) Uani 1 1 d . . . O3 O 0.76896(13) 0.40679(15) 0.3267(4) 0.0335(8) Uani 1 1 d . A . C1 C 0.88881(17) 0.7251(2) 0.1752(6) 0.0285(10) Uani 1 1 d . . . H1 H 0.8857 0.7599 0.1044 0.034 Uiso 1 1 calc R . . C2 C 0.84508(17) 0.6803(2) 0.1831(6) 0.0275(9) Uani 1 1 d . . . H2 H 0.8128 0.6853 0.1197 0.033 Uiso 1 1 calc R . . C3 C 0.93898(18) 0.6700(2) 0.3578(6) 0.0347(11) Uani 1 1 d . . . H3 H 0.9721 0.6654 0.4184 0.042 Uiso 1 1 calc R . . C4 C 0.89718(18) 0.6234(2) 0.3719(6) 0.0356(11) Uani 1 1 d . . . H4 H 0.9017 0.5884 0.4416 0.043 Uiso 1 1 calc R . . C5 C 0.84852(18) 0.6281(2) 0.2835(5) 0.0275(10) Uani 1 1 d . . . C6 C 0.80063(18) 0.5812(2) 0.2923(6) 0.0290(10) Uani 1 1 d . . . C7 C 0.74510(19) 0.6053(2) 0.2857(6) 0.0325(11) Uani 1 1 d . . . H7 H 0.7392 0.6507 0.2767 0.039 Uiso 1 1 calc R . . C8 C 0.69911(19) 0.5645(2) 0.2919(6) 0.0341(11) Uani 1 1 d . . . H8 H 0.6621 0.5822 0.2875 0.041 Uiso 1 1 calc R . . C9 C 0.80798(17) 0.5145(2) 0.3097(6) 0.0310(10) Uani 1 1 d . . . C10 C 0.76128(18) 0.4727(2) 0.3136(6) 0.0309(10) Uani 1 1 d . . . C11 C 0.70616(18) 0.4976(2) 0.3046(6) 0.0334(10) Uani 1 1 d . . . C12 C 0.65642(18) 0.4530(2) 0.2990(6) 0.0315(10) Uani 1 1 d . . . C13 C 0.61391(19) 0.4630(2) 0.1927(7) 0.0370(11) Uani 1 1 d . . . H13 H 0.6155 0.4994 0.1260 0.044 Uiso 1 1 calc R . . C14 C 0.65096(18) 0.4000(2) 0.3967(6) 0.0333(11) Uani 1 1 d . . . H14 H 0.6786 0.3920 0.4733 0.040 Uiso 1 1 calc R . . C15 C 0.93103(18) 0.9199(2) 0.1838(7) 0.0365(11) Uani 1 1 d . . . H15 H 0.9599 0.9277 0.1104 0.044 Uiso 1 1 calc R . . C16 C 0.89505(17) 0.8589(2) 0.3814(6) 0.0314(10) Uani 1 1 d . . . H16 H 0.8983 0.8231 0.4493 0.038 Uiso 1 1 calc R . . C20 C 0.87908(19) 0.4546(2) 0.4422(6) 0.0369(11) Uani 1 1 d . . . H20A H 0.8506 0.4212 0.4684 0.044 Uiso 1 1 calc R . . H20B H 0.8821 0.4852 0.5292 0.044 Uiso 1 1 calc R . . C21 C 0.9360(2) 0.4228(3) 0.4121(9) 0.0590(17) Uani 1 1 d . . . H21A H 0.9454 0.3948 0.5006 0.071 Uiso 1 1 calc R . . H21B H 0.9322 0.3943 0.3213 0.071 Uiso 1 1 calc R . . C22 C 0.7875(3) 0.3751(3) 0.1884(7) 0.0496(14) Uani 1 1 d D . . O4 O 0.98021(19) 0.4645(3) 0.3877(7) 0.0827(17) Uani 1 1 d . . . C23 C 0.7651(10) 0.3061(7) 0.207(2) 0.047(5) Uani 0.510(12) 1 d PD A 1 O6 O 0.7904(6) 0.2702(4) 0.3171(13) 0.091(5) Uani 0.510(12) 1 d P A 1 C24 C 0.7525(9) 0.3137(8) 0.159(3) 0.049(5) Uani 0.490(12) 1 d PD A 2 O5 O 0.7731(4) 0.2735(4) 0.0497(13) 0.068(4) Uani 0.490(12) 1 d P A 2 N10 N 0.8944(10) 0.2572(16) 0.260(2) 0.199(9) Uani 0.60 1 d PDU B 3 O10 O 0.8840(5) 0.2594(6) 0.1208(14) 0.105(4) Uani 0.60 1 d PDU B 3 O11 O 0.8646(11) 0.2236(15) 0.343(2) 0.238(11) Uani 0.60 1 d PDU B 3 O12 O 0.9426(9) 0.2708(10) 0.298(3) 0.239(9) Uani 0.60 1 d PDU B 3 N11 N 0.8815(11) 0.2121(11) 0.263(3) 0.142(8) Uani 0.40 1 d PDU C 4 O15 O 0.8428(17) 0.201(2) 0.176(5) 0.30(2) Uani 0.40 1 d PDU C 4 O16 O 0.9025(8) 0.1749(7) 0.353(2) 0.116(6) Uani 0.40 1 d PDU C 4 O17 O 0.9091(9) 0.2583(10) 0.214(3) 0.134(7) Uani 0.40 1 d PDU C 4 O1W O 0.9996(8) 0.0547(11) 0.1247(14) 0.120(6) Uani 0.50 1 d PU . 5 O2W O 0.9717(9) 0.1021(13) 0.163(3) 0.144(6) Uani 0.50 1 d PU . 5 O3W O 1.0000(15) 0.0742(9) 0.278(2) 0.133(7) Uani 0.50 1 d PU . 5 O4W O 0.9443(9) 0.1240(12) 0.276(3) 0.158(6) Uani 0.50 1 d PU . 5 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 0.0141(4) 0.0173(4) 0.0557(6) 0.000 0.0001(4) 0.000 N1 0.0182(16) 0.0183(16) 0.049(2) -0.0010(16) -0.0017(16) -0.0001(12) N2 0.0154(16) 0.0260(19) 0.052(3) 0.0046(17) 0.0007(16) 0.0023(13) O1 0.0273(17) 0.048(2) 0.058(2) 0.0052(19) -0.0036(16) -0.0047(14) O2 0.0213(14) 0.0284(16) 0.049(2) 0.0081(15) 0.0023(14) -0.0011(12) O3 0.0257(15) 0.0232(15) 0.051(2) 0.0052(15) 0.0023(14) -0.0033(12) C1 0.0213(19) 0.0194(19) 0.045(3) -0.0003(19) -0.0013(19) 0.0008(15) C2 0.0223(19) 0.021(2) 0.039(3) -0.0029(19) 0.0012(18) -0.0007(16) C3 0.0212(19) 0.023(2) 0.060(3) 0.005(2) -0.007(2) -0.0012(16) C4 0.025(2) 0.026(2) 0.056(3) 0.008(2) -0.006(2) -0.0025(17) C5 0.023(2) 0.023(2) 0.036(3) -0.0011(17) 0.0011(17) -0.0026(16) C6 0.024(2) 0.025(2) 0.038(3) 0.0030(18) -0.0021(18) -0.0057(16) C7 0.024(2) 0.027(2) 0.046(3) 0.004(2) -0.0038(19) -0.0028(17) C8 0.025(2) 0.027(2) 0.051(3) 0.004(2) -0.003(2) -0.0045(17) C9 0.0207(19) 0.029(2) 0.043(3) 0.004(2) -0.0023(19) -0.0021(16) C10 0.025(2) 0.026(2) 0.042(3) 0.004(2) 0.0007(19) -0.0047(16) C11 0.0214(19) 0.032(2) 0.047(3) 0.005(2) -0.004(2) -0.0038(18) C12 0.0223(19) 0.024(2) 0.049(3) 0.002(2) -0.0014(19) -0.0042(16) C13 0.025(2) 0.025(2) 0.062(3) 0.009(2) -0.006(2) -0.0024(17) C14 0.024(2) 0.030(2) 0.046(3) 0.004(2) -0.0025(19) -0.0022(17) C15 0.0197(19) 0.026(2) 0.063(3) 0.007(2) 0.007(2) 0.0019(16) C16 0.0220(19) 0.026(2) 0.046(3) 0.005(2) -0.0024(19) 0.0025(16) C20 0.026(2) 0.038(3) 0.046(3) 0.010(2) 0.000(2) -0.0026(19) C21 0.031(3) 0.060(4) 0.087(5) 0.012(4) -0.005(3) 0.004(2) C22 0.068(4) 0.031(3) 0.050(3) -0.002(2) 0.008(3) -0.009(3) O4 0.035(2) 0.121(5) 0.093(4) -0.007(3) 0.006(2) -0.013(3) C23 0.071(11) 0.027(6) 0.045(13) -0.005(5) -0.029(7) -0.006(6) O6 0.182(13) 0.025(4) 0.067(7) 0.007(4) -0.016(8) -0.004(6) C24 0.065(12) 0.040(8) 0.041(13) -0.007(7) -0.014(8) -0.015(8) O5 0.080(7) 0.041(5) 0.082(8) -0.019(5) 0.016(5) -0.011(4) N10 0.230(17) 0.181(17) 0.185(12) 0.076(13) -0.105(13) 0.002(15) O10 0.088(7) 0.114(9) 0.114(8) -0.018(7) -0.004(6) 0.029(7) O11 0.32(2) 0.24(2) 0.157(15) 0.093(15) -0.069(15) -0.004(17) O12 0.275(18) 0.155(14) 0.287(19) 0.047(14) -0.189(15) 0.000(14) N11 0.153(16) 0.063(10) 0.209(19) -0.001(11) -0.125(13) -0.011(10) O15 0.30(4) 0.31(4) 0.29(4) 0.08(3) -0.23(3) -0.10(3) O16 0.117(11) 0.048(7) 0.183(15) -0.001(8) -0.074(11) -0.004(7) O17 0.113(12) 0.077(9) 0.211(19) 0.031(11) -0.025(12) 0.066(8) O1W 0.140(12) 0.198(15) 0.024(6) -0.033(7) 0.032(7) -0.086(10) O2W 0.141(15) 0.205(16) 0.088(12) 0.017(11) -0.009(9) -0.046(12) O3W 0.158(11) 0.170(13) 0.070(11) -0.086(10) -0.045(11) 0.013(12) O4W 0.128(13) 0.192(16) 0.155(14) -0.020(12) -0.006(11) 0.007(11) _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 O1 2.094(4) 3_755 ? Co1 O1 2.094(4) . ? Co1 N2 2.145(4) . ? Co1 N2 2.145(4) 3_755 ? Co1 N1 2.158(4) . ? Co1 N1 2.158(4) 3_755 ? N1 C3 1.341(6) . ? N1 C1 1.355(6) . ? N2 C16 1.347(6) . ? N2 C15 1.345(6) . ? O2 C9 1.388(5) . ? O2 C20 1.443(6) . ? O3 C10 1.376(5) . ? O3 C22 1.441(7) . ? C1 C2 1.389(6) . ? C2 C5 1.391(6) . ? C3 C4 1.385(6) . ? C4 C5 1.390(6) . ? C5 C6 1.492(6) . ? C6 C9 1.396(6) . ? C6 C7 1.407(6) . ? C7 C8 1.376(6) . ? C8 C11 1.395(7) . ? C9 C10 1.401(6) . ? C10 C11 1.405(6) . ? C11 C12 1.495(6) . ? C12 C13 1.384(7) . ? C12 C14 1.393(7) . ? C13 C15 1.390(6) 8_755 ? C14 C16 1.386(6) 8_755 ? C15 C13 1.390(6) 8_765 ? C16 C14 1.386(6) 8_765 ? C20 C21 1.521(7) . ? C21 O4 1.373(8) . ? C22 C23 1.527(13) . ? C22 C24 1.535(13) . ? C23 O6 1.353(19) . ? C24 O5 1.35(3) . ? N10 O10 1.240(15) . ? N10 O11 1.229(14) . ? N10 O12 1.221(14) . ? O11 O12 2.13(2) . ? N11 O17 1.236(15) . ? N11 O15 1.213(15) . ? N11 O16 1.203(14) . ? O16 O17 2.114(19) . ? O1W O3W 0.94(2) 3_755 ? O1W O2W 1.22(3) . ? O1W O3W 1.40(2) . ? O2W O4W 1.26(3) . ? O2W O3W 1.02(3) 3_755 ? O2W O3W 1.34(3) . ? O3W O3W 0.50(4) 3_755 ? O3W O1W 0.94(2) 3_755 ? O3W O2W 1.02(3) 3_755 ? O3W O4W 1.67(4) . ? O3W O4W 1.74(4) 3_755 ? O4W O3W 1.74(4) 3_755 ? 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 Co1 O1 179.4(2) 3_755 . ? O1 Co1 N2 88.33(15) 3_755 . ? O1 Co1 N2 92.07(15) . . ? O1 Co1 N2 92.07(15) 3_755 3_755 ? O1 Co1 N2 88.33(15) . 3_755 ? N2 Co1 N2 92.1(2) . 3_755 ? O1 Co1 N1 90.41(15) 3_755 . ? O1 Co1 N1 89.19(15) . . ? N2 Co1 N1 88.89(14) . . ? N2 Co1 N1 177.36(16) 3_755 . ? O1 Co1 N1 89.19(15) 3_755 3_755 ? O1 Co1 N1 90.41(15) . 3_755 ? N2 Co1 N1 177.36(16) . 3_755 ? N2 Co1 N1 88.89(14) 3_755 3_755 ? N1 Co1 N1 90.23(19) . 3_755 ? C3 N1 C1 116.3(4) . . ? C3 N1 Co1 123.3(3) . . ? C1 N1 Co1 120.4(3) . . ? C16 N2 C15 117.3(4) . . ? C16 N2 Co1 119.0(3) . . ? C15 N2 Co1 123.6(3) . . ? C9 O2 C20 114.9(4) . . ? C10 O3 C22 114.7(4) . . ? N1 C1 C2 123.0(4) . . ? C1 C2 C5 120.1(4) . . ? N1 C3 C4 124.0(4) . . ? C3 C4 C5 119.6(4) . . ? C4 C5 C2 116.9(4) . . ? C4 C5 C6 123.8(4) . . ? C2 C5 C6 119.3(4) . . ? C9 C6 C7 118.0(4) . . ? C9 C6 C5 123.3(4) . . ? C7 C6 C5 118.7(4) . . ? C8 C7 C6 121.5(4) . . ? C7 C8 C11 120.8(4) . . ? O2 C9 C6 119.2(4) . . ? O2 C9 C10 119.8(4) . . ? C6 C9 C10 120.6(4) . . ? O3 C10 C9 120.3(4) . . ? O3 C10 C11 119.2(4) . . ? C9 C10 C11 120.5(4) . . ? C8 C11 C10 118.5(4) . . ? C8 C11 C12 120.8(4) . . ? C10 C11 C12 120.6(4) . . ? C13 C12 C14 117.4(4) . . ? C13 C12 C11 120.2(4) . . ? C14 C12 C11 122.4(4) . . ? C12 C13 C15 119.9(5) . 8_755 ? C16 C14 C12 119.5(4) 8_755 . ? N2 C15 C13 122.7(5) . 8_765 ? N2 C16 C14 123.0(4) . 8_765 ? O2 C20 C21 108.3(5) . . ? O4 C21 C20 115.6(5) . . ? O3 C22 C23 103.1(11) . . ? O3 C22 C24 110.5(11) . . ? C23 C22 C24 20.3(7) . . ? O6 C23 C22 115.5(12) . . ? O5 C24 C22 115.3(17) . . ? O10 N10 O11 119.0(15) . . ? O10 N10 O12 116.4(15) . . ? O11 N10 O12 120.4(15) . . ? N10 O11 O12 29.7(8) . . ? N10 O12 O11 29.9(8) . . ? O17 N11 O15 109(2) . . ? O17 N11 O16 120.2(17) . . ? O15 N11 O16 127(2) . . ? N11 O16 O17 30.3(9) . . ? N11 O17 O16 29.5(9) . . ? O3W O1W O2W 54.5(19) 3_755 . ? O3W O1W O3W 8.7(8) 3_755 . ? O2W O1W O3W 61.0(14) . . ? O4W O2W O3W 98(3) . 3_755 ? O4W O2W O1W 141(3) . . ? O3W O2W O1W 48.2(18) 3_755 . ? O4W O2W O3W 79.6(19) . . ? O3W O2W O3W 19(3) 3_755 . ? O1W O2W O3W 66.0(17) . . ? O3W O3W O1W 154.6(19) 3_755 3_755 ? O3W O3W O2W 120(8) 3_755 3_755 ? O1W O3W O2W 77(2) 3_755 3_755 ? O3W O3W O1W 16.7(15) 3_755 . ? O1W O3W O1W 138(3) 3_755 . ? O2W O3W O1W 130(4) 3_755 . ? O3W O3W O2W 41(5) 3_755 . ? O1W O3W O2W 150(4) 3_755 . ? O2W O3W O2W 118(3) 3_755 . ? O1W O3W O2W 53.0(13) . . ? O3W O3W O4W 89(6) 3_755 . ? O1W O3W O4W 107(3) 3_755 . ? O2W O3W O4W 100.3(19) 3_755 . ? O1W O3W O4W 99.1(17) . . ? O2W O3W O4W 48.1(14) . . ? O3W O3W O4W 74(6) 3_755 3_755 ? O1W O3W O4W 119(3) 3_755 3_755 ? O2W O3W O4W 46(2) 3_755 3_755 ? O1W O3W O4W 85(2) . 3_755 ? O2W O3W O4W 85.4(18) . 3_755 ? O4W O3W O4W 103.5(18) . 3_755 ? O2W O4W O3W 52.2(15) . . ? O2W O4W O3W 35.6(12) . 3_755 ? O3W O4W O3W 16.6(11) . 3_755 ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.893 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.114 #==END data_pbcn_Co_423k_NO3 _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA. M. KAWANO, M. TOMINAGA. M. FUJITA ; _journal_name_full 'Angew. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Co N6 O14' _chemical_formula_weight 875.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.092(5) _cell_length_b 20.572(5) _cell_length_c 8.496(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4036.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 696(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description black _exptl_crystal_colour red _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 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9286 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 'Bruker SMART CCD area detector system' _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 31805 _diffrn_reflns_av_R_equivalents 0.1113 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.58 _reflns_number_total 4835 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C42 to O42, C43 to O43, C41A to O44A, C41B to O44B, and C41C to O44C) converged to 66%, 34%, 40%, 35% and 35%,respectively. The occupancy of the disordered nitrate ions (N10 to O12, N10A to O12A) converged to 59%, and 41%,respectively. The thermal temperature factors of ethylene glycol groups and nitrate ions were isotropically refined because of severe disorder. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered nitrate ions and ethylene glycol groups. ; _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^)+(0.0380P)^2^+29.3559P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4835 _refine_ls_number_parameters 278 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.2127 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.3119 _refine_ls_wR_factor_gt 0.2384 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.003 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 0.5000 0.70849(6) 0.7500 0.0474(4) Uani 1 2 d S . . N1 N 0.4336(2) 0.7791(3) 0.7928(8) 0.0485(16) Uani 1 1 d . . . N2 N 0.4376(2) 0.6362(3) 0.8079(8) 0.0469(15) Uani 1 1 d . . . C10 C 0.3840(3) 0.7775(3) 0.7116(11) 0.055(2) Uani 1 1 d . . . H10 H 0.3789 0.7442 0.6390 0.066 Uiso 1 1 calc R . . C11 C 0.3405(3) 0.8216(3) 0.7284(10) 0.0508(19) Uani 1 1 d . . . H11 H 0.3069 0.8173 0.6692 0.061 Uiso 1 1 calc R . . C12 C 0.3462(3) 0.8725(3) 0.8331(9) 0.0450(17) Uani 1 1 d . . . C13 C 0.3974(3) 0.8745(4) 0.9196(10) 0.057(2) Uani 1 1 d . . . H13 H 0.4034 0.9074 0.9929 0.068 Uiso 1 1 calc R . . C14 C 0.4391(3) 0.8276(3) 0.8965(11) 0.057(2) Uani 1 1 d . . . H14 H 0.4728 0.8297 0.9561 0.068 Uiso 1 1 calc R . . C20 C 0.4019(3) 0.6427(4) 0.9289(10) 0.0523(19) Uani 1 1 d . . . H20 H 0.4089 0.6760 1.0006 0.063 Uiso 1 1 calc R . . C21 C 0.1450(3) 1.1026(3) 0.9538(10) 0.0507(19) Uani 1 1 d . . . H21 H 0.1702 1.1106 1.0369 0.061 Uiso 1 1 calc R . . C22 C 0.1543(3) 1.0504(3) 0.8543(10) 0.0493(19) Uani 1 1 d . . . C23 C 0.1152(3) 1.0424(4) 0.7330(11) 0.059(2) Uani 1 1 d . . . H23 H 0.1190 1.0073 0.6648 0.071 Uiso 1 1 calc R . . C24 C 0.4290(3) 0.5856(4) 0.7123(10) 0.058(2) Uani 1 1 d . . . H24 H 0.4542 0.5795 0.6282 0.069 Uiso 1 1 calc R . . C30 C 0.2418(3) 0.8977(4) 0.8481(10) 0.053(2) Uani 1 1 d . . . H30 H 0.2351 0.8532 0.8411 0.063 Uiso 1 1 calc R . . C31 C 0.1959(3) 0.9395(3) 0.8547(10) 0.054(2) Uani 1 1 d . . . H31 H 0.1583 0.9232 0.8514 0.065 Uiso 1 1 calc R . . C32 C 0.2048(3) 1.0066(3) 0.8663(10) 0.0492(19) Uani 1 1 d . . . C33 C 0.2608(3) 1.0294(3) 0.8748(10) 0.0480(18) Uani 1 1 d . B . C34 C 0.3080(3) 0.9869(3) 0.8655(9) 0.0447(17) Uani 1 1 d . . . C35 C 0.2981(3) 0.9205(3) 0.8517(10) 0.0468(18) Uani 1 1 d . . . C40 C 0.3846(3) 1.0437(4) 0.9927(12) 0.069(3) Uani 1 1 d D . . O40 O 0.36318(19) 1.0101(2) 0.8541(7) 0.0517(13) Uani 1 1 d . A . O41 O 0.2697(2) 1.0951(2) 0.8902(7) 0.0521(13) Uani 1 1 d D . . C42 C 0.4349(8) 1.0854(10) 0.938(3) 0.103(9) Uiso 0.661(19) 1 d PD A 1 O42 O 0.4813(5) 1.0459(6) 0.8976(15) 0.101(5) Uiso 0.661(19) 1 d PD A 1 C43 C 0.4437(10) 1.072(2) 0.962(4) 0.075(13) Uiso 0.339(19) 1 d PD A 2 O43 O 0.4453(13) 1.1078(13) 0.825(3) 0.130(13) Uiso 0.339(19) 1 d PD A 2 C41A C 0.2888(14) 1.1300(11) 0.752(2) 0.042(6) Uiso 0.40(2) 1 d PD B 3 C44A C 0.2856(17) 1.2010(13) 0.799(4) 0.098(7) Uiso 0.40(2) 1 d PD B 3 O44A O 0.3056(10) 1.2393(12) 0.678(3) 0.118(11) Uiso 0.40(2) 1 d PD B 3 C41B C 0.2644(16) 1.1287(12) 0.739(2) 0.065(9) Uiso 0.35(3) 1 d PD B 4 C44B C 0.2601(18) 1.2012(13) 0.768(5) 0.098(7) Uiso 0.35(3) 1 d PD B 4 O44B O 0.2974(12) 1.2323(13) 0.869(3) 0.103(11) Uiso 0.35(3) 1 d PD B 4 C41C C 0.293(3) 1.118(2) 0.739(4) 0.13(3) Uiso 0.35(3) 1 d PD B 5 C44C C 0.292(2) 1.1910(19) 0.734(5) 0.098(7) Uiso 0.35(3) 1 d PD B 5 O44C O 0.335(3) 1.210(3) 0.835(6) 0.24(3) Uiso 0.35(3) 1 d PD B 5 O10 O 0.4788(3) 0.7129(4) 0.5075(10) 0.092(2) Uiso 1 1 d D . . N10 N 0.4435(7) 0.7158(8) 0.4065(18) 0.075(4) Uiso 0.590(16) 1 d PD C 6 O11 O 0.4056(9) 0.6748(10) 0.396(3) 0.150(8) Uiso 0.590(16) 1 d PD C 6 O12 O 0.4378(9) 0.7625(11) 0.326(3) 0.167(9) Uiso 0.590(16) 1 d PD C 6 N10A N 0.4507(13) 0.679(2) 0.397(4) 0.146(13) Uiso 0.410(16) 1 d PD C 7 O11A O 0.4114(15) 0.6995(19) 0.317(4) 0.171(14) Uiso 0.410(16) 1 d PD C 7 O12A O 0.4702(13) 0.6264(18) 0.376(4) 0.176(14) Uiso 0.410(16) 1 d PD C 7 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 0.0259(6) 0.0320(6) 0.0842(11) 0.000 0.0072(7) 0.000 N1 0.037(3) 0.031(3) 0.077(5) -0.005(3) 0.004(3) 0.004(2) N2 0.034(3) 0.040(3) 0.067(4) -0.008(3) 0.010(3) -0.007(2) C10 0.046(4) 0.041(4) 0.079(6) -0.009(4) -0.004(4) 0.009(3) C11 0.033(3) 0.045(4) 0.074(6) -0.005(4) -0.002(4) 0.005(3) C12 0.032(3) 0.041(4) 0.062(5) -0.001(3) 0.000(3) 0.007(3) C13 0.042(4) 0.048(4) 0.080(6) -0.013(4) -0.013(4) 0.012(3) C14 0.032(4) 0.048(4) 0.090(7) -0.016(4) -0.014(4) 0.008(3) C20 0.047(4) 0.044(4) 0.067(5) -0.009(4) 0.010(4) -0.013(3) C21 0.038(4) 0.045(4) 0.069(5) -0.006(4) -0.011(4) 0.011(3) C22 0.033(4) 0.042(4) 0.073(6) -0.002(4) -0.006(4) 0.012(3) C23 0.046(4) 0.049(4) 0.082(6) -0.023(4) -0.018(4) 0.017(3) C24 0.045(4) 0.053(4) 0.075(6) -0.019(4) 0.018(4) -0.012(3) C30 0.036(4) 0.042(4) 0.080(6) -0.005(4) -0.002(4) 0.005(3) C31 0.035(4) 0.045(4) 0.083(6) -0.002(4) -0.008(4) 0.005(3) C32 0.035(3) 0.038(4) 0.075(6) -0.005(4) -0.006(4) 0.014(3) C33 0.041(4) 0.030(3) 0.073(5) -0.002(3) -0.006(4) 0.007(3) C34 0.033(3) 0.041(4) 0.061(5) -0.006(3) -0.003(3) 0.003(3) C35 0.035(4) 0.038(3) 0.068(5) -0.002(3) -0.005(3) 0.007(3) C40 0.050(5) 0.079(6) 0.077(6) -0.027(5) -0.007(5) -0.016(4) O40 0.039(3) 0.045(3) 0.071(4) -0.013(3) -0.002(2) 0.002(2) O41 0.051(3) 0.036(2) 0.069(4) -0.006(2) 0.003(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O10 2.120(8) 3_656 ? Co1 O10 2.120(8) . ? Co1 N2 2.129(5) . ? Co1 N2 2.129(5) 3_656 ? Co1 N1 2.144(5) 3_656 ? Co1 N1 2.144(5) . ? N1 C10 1.337(9) . ? N1 C14 1.336(9) . ? N2 C20 1.324(9) . ? N2 C24 1.335(9) . ? C10 C11 1.359(9) . ? C11 C12 1.380(10) . ? C12 C13 1.393(10) . ? C12 C35 1.495(9) . ? C13 C14 1.377(10) . ? C20 C21 1.378(9) 8_655 ? C21 C20 1.378(9) 8_665 ? C21 C22 1.384(10) . ? C22 C23 1.380(10) . ? C22 C32 1.478(9) . ? C23 C24 1.364(9) 8_665 ? C24 C23 1.364(9) 8_655 ? C30 C31 1.366(9) . ? C30 C35 1.382(9) . ? C31 C32 1.398(10) . ? C32 C33 1.377(9) . ? C33 O41 1.373(8) . ? C33 C34 1.401(9) . ? C34 O40 1.364(8) . ? C34 C35 1.390(9) . ? C40 O40 1.452(10) . ? C40 C43 1.502(17) . ? C40 C42 1.517(15) . ? O41 C41A 1.446(14) . ? O41 C41B 1.462(16) . ? O41 C41C 1.471(18) . ? C42 O42 1.39(2) . ? C43 O43 1.39(2) . ? C41A C44A 1.514(19) . ? C44A O44A 1.38(2) . ? C41B C44B 1.513(19) . ? C44B O44B 1.38(2) . ? C41C C44C 1.513(19) . ? C44C O44C 1.38(2) . ? O10 N10 1.184(17) . ? O10 N10A 1.34(4) . ? N10 O12 1.186(18) . ? N10 O11 1.220(19) . ? N10A O12A 1.18(3) . ? N10A O11A 1.21(3) . ? 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 O10 Co1 O10 175.1(4) 3_656 . ? O10 Co1 N2 87.8(3) 3_656 . ? O10 Co1 N2 95.6(3) . . ? O10 Co1 N2 95.6(3) 3_656 3_656 ? O10 Co1 N2 87.8(3) . 3_656 ? N2 Co1 N2 91.4(3) . 3_656 ? O10 Co1 N1 88.3(3) 3_656 3_656 ? O10 Co1 N1 88.4(3) . 3_656 ? N2 Co1 N1 175.7(3) . 3_656 ? N2 Co1 N1 87.1(2) 3_656 3_656 ? O10 Co1 N1 88.4(3) 3_656 . ? O10 Co1 N1 88.3(3) . . ? N2 Co1 N1 87.1(2) . . ? N2 Co1 N1 175.7(3) 3_656 . ? N1 Co1 N1 94.7(3) 3_656 . ? C10 N1 C14 116.1(6) . . ? C10 N1 Co1 120.6(5) . . ? C14 N1 Co1 123.3(5) . . ? C20 N2 C24 117.4(6) . . ? C20 N2 Co1 121.9(5) . . ? C24 N2 Co1 120.3(5) . . ? N1 C10 C11 124.1(7) . . ? C10 C11 C12 120.3(7) . . ? C11 C12 C13 116.2(6) . . ? C11 C12 C35 120.0(6) . . ? C13 C12 C35 123.8(7) . . ? C14 C13 C12 119.8(7) . . ? N1 C14 C13 123.4(7) . . ? N2 C20 C21 123.1(7) . 8_655 ? C20 C21 C22 119.6(7) 8_665 . ? C23 C22 C21 116.6(6) . . ? C23 C22 C32 119.6(7) . . ? C21 C22 C32 123.7(7) . . ? C24 C23 C22 120.5(7) 8_665 . ? N2 C24 C23 122.7(7) . 8_655 ? C31 C30 C35 121.0(7) . . ? C30 C31 C32 120.6(7) . . ? C33 C32 C31 118.6(6) . . ? C33 C32 C22 122.4(6) . . ? C31 C32 C22 118.7(6) . . ? O41 C33 C32 118.8(6) . . ? O41 C33 C34 120.2(6) . . ? C32 C33 C34 121.0(6) . . ? O40 C34 C35 119.5(6) . . ? O40 C34 C33 120.9(6) . . ? C35 C34 C33 119.3(6) . . ? C30 C35 C34 119.4(6) . . ? C30 C35 C12 118.2(6) . . ? C34 C35 C12 122.3(6) . . ? O40 C40 C43 110.6(15) . . ? O40 C40 C42 106.3(12) . . ? C43 C40 C42 15.4(18) . . ? C34 O40 C40 115.3(6) . . ? C33 O41 C41A 117.3(11) . . ? C33 O41 C41B 111.7(12) . . ? C41A O41 C41B 22.7(14) . . ? C33 O41 C41C 106.4(18) . . ? C41A O41 C41C 12(2) . . ? C41B O41 C41C 28(3) . . ? O42 C42 C40 109.7(15) . . ? O43 C43 C40 112(2) . . ? O41 C41A C44A 104.5(17) . . ? O44A C44A C41A 110(2) . . ? O41 C41B C44B 109(2) . . ? O44B C44B C41B 121(3) . . ? O41 C41C C44C 109(3) . . ? O44C C44C C41C 104(4) . . ? N10 O10 N10A 35.5(15) . . ? N10 O10 Co1 149.9(9) . . ? N10A O10 Co1 140.5(12) . . ? O12 N10 O10 122.4(18) . . ? O12 N10 O11 116(2) . . ? O10 N10 O11 120.8(19) . . ? O12A N10A O10 114(3) . . ? O12A N10A O11A 121(5) . . ? O10 N10A O11A 125(4) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.644 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.112 #==END data_pbcn_Co_80k_NO3 _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA, M. KAWANO, T. Hozumi, S. Ohkoshi, M. Fujita ; _journal_name_full 'Inorg. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Co N6 O14' _chemical_formula_weight 875.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.025(3) _cell_length_b 20.722(3) _cell_length_c 8.2790(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3950.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8615 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41924 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.53 _reflns_number_total 4814 _reflns_number_gt 3832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C23 to O6 and C24 to O5) converged to 51% and 49%,respectively. The occupancy of the disordered nitrate ions (N10 to O12, N11 to O17) converged to 60% and 40%,respectively. The thermal temperature factors of ethylene glycol groups were isotropically refined because of severe disorder. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered nitrate ions and ethylene glycol groups. ; _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^)+(0.0760P)^2^+17.3529P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4814 _refine_ls_number_parameters 317 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1904 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.003 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 0.5000 0.71025(3) 0.7500 0.0140(2) Uani 1 2 d S . . N1 N 0.43335(13) 0.78012(13) 0.7981(4) 0.0150(6) Uani 1 1 d . . . N2 N 0.43787(12) 0.63823(14) 0.8085(4) 0.0148(6) Uani 1 1 d . . . C10 C 0.38312(16) 0.77677(17) 0.7161(5) 0.0191(8) Uani 1 1 d . . . H10 H 0.3777 0.7422 0.6424 0.023 Uiso 1 1 calc R . . C11 C 0.33875(16) 0.82145(17) 0.7340(5) 0.0199(8) Uani 1 1 d . . . H11 H 0.3039 0.8171 0.6736 0.024 Uiso 1 1 calc R . . C12 C 0.34568(15) 0.87309(17) 0.8420(5) 0.0166(7) Uani 1 1 d . . . C13 C 0.39707(15) 0.87542(17) 0.9300(5) 0.0187(8) Uani 1 1 d . . . H13 H 0.4034 0.9089 1.0063 0.022 Uiso 1 1 calc R . . C14 C 0.43913(15) 0.82841(17) 0.9054(5) 0.0170(7) Uani 1 1 d . . . H14 H 0.4738 0.8305 0.9675 0.020 Uiso 1 1 calc R . . C20 C 0.40179(15) 0.64553(17) 0.9353(5) 0.0160(7) Uani 1 1 d . . . H20 H 0.4087 0.6799 1.0089 0.019 Uiso 1 1 calc R . . C21 C 0.14493(15) 1.10506(16) 0.9626(5) 0.0154(7) Uani 1 1 d . . . H21 H 0.1706 1.1129 1.0504 0.019 Uiso 1 1 calc R . . C22 C 0.15408(14) 1.05280(16) 0.8604(5) 0.0145(7) Uani 1 1 d . . . C23 C 0.11422(14) 1.04311(17) 0.7351(5) 0.0176(7) Uani 1 1 d . . . H23 H 0.1175 1.0065 0.6665 0.021 Uiso 1 1 calc R . . C24 C 0.42997(15) 0.58737(18) 0.7123(5) 0.0173(7) Uani 1 1 d . . . H24 H 0.4558 0.5813 0.6243 0.021 Uiso 1 1 calc R . . C30 C 0.24046(15) 0.89867(17) 0.8537(5) 0.0180(7) Uani 1 1 d . . . H30 H 0.2332 0.8537 0.8452 0.022 Uiso 1 1 calc R . . C31 C 0.19393(15) 0.94109(17) 0.8616(5) 0.0170(7) Uani 1 1 d . . . H31 H 0.1553 0.9251 0.8581 0.020 Uiso 1 1 calc R . . C32 C 0.20394(14) 1.00751(17) 0.8749(5) 0.0169(7) Uani 1 1 d . . . C33 C 0.26079(15) 1.03019(16) 0.8848(5) 0.0176(7) Uani 1 1 d . C . C34 C 0.30778(15) 0.98735(17) 0.8747(5) 0.0170(7) Uani 1 1 d . . . C35 C 0.29794(15) 0.92085(17) 0.8580(5) 0.0176(7) Uani 1 1 d . . . C40 C 0.38522(16) 1.0439(2) 1.0010(6) 0.0243(9) Uani 1 1 d . . . H40A H 0.3975 1.0126 1.0846 0.029 Uiso 1 1 calc R A 1 H40B H 0.3543 1.0715 1.0471 0.029 Uiso 1 1 calc R A 1 O40 O 0.36360(10) 1.01021(12) 0.8618(3) 0.0183(6) Uani 1 1 d . B . O41 O 0.27038(11) 1.09545(12) 0.9026(4) 0.0192(6) Uani 1 1 d D . . C42 C 0.43626(19) 1.0849(2) 0.9506(7) 0.0405(12) Uani 1 1 d . B 1 H42A H 0.4244 1.1127 0.8591 0.049 Uiso 1 1 calc R B 1 H42B H 0.4472 1.1134 1.0415 0.049 Uiso 1 1 calc R B 1 O42 O 0.48523(13) 1.04823(19) 0.9041(4) 0.0418(9) Uani 1 1 d . B 1 C41A C 0.2837(8) 1.1314(5) 0.7630(14) 0.010(3) Uiso 0.366(11) 1 d PDU C 3 C44A C 0.2891(5) 1.1996(6) 0.8214(18) 0.024(3) Uiso 0.366(11) 1 d PD C 3 O44A O 0.3049(4) 1.2404(4) 0.6904(10) 0.030(3) Uiso 0.366(11) 1 d PD C 3 C41B C 0.2747(8) 1.1252(7) 0.7409(16) 0.046(6) Uiso 0.443(13) 1 d PDU C 4 C44B C 0.2704(7) 1.1969(6) 0.7502(17) 0.044(3) Uiso 0.443(13) 1 d PD C 4 O44B O 0.2972(4) 1.2342(5) 0.8734(11) 0.053(3) Uiso 0.443(13) 1 d PD C 4 C41C C 0.2991(11) 1.1245(9) 0.762(2) 0.043(7) Uiso 0.278(12) 1 d PDU C 5 C44C C 0.2959(8) 1.1957(7) 0.761(2) 0.024(4) Uiso 0.278(12) 1 d PD C 5 O44C O 0.3532(5) 1.1949(6) 0.8295(15) 0.034(4) Uiso 0.278(12) 1 d PD C 5 O10 O 0.47787(13) 0.71843(16) 0.4985(4) 0.0315(7) Uani 1 1 d D . . N10 N 0.4376(3) 0.7171(3) 0.4019(7) 0.0234(14) Uani 0.599(7) 1 d PD D 6 O11 O 0.4004(3) 0.6745(4) 0.4165(13) 0.053(2) Uani 0.599(7) 1 d PD D 6 O12 O 0.4294(3) 0.7567(4) 0.2960(9) 0.057(2) Uani 0.599(7) 1 d PD D 6 N10A N 0.4535(3) 0.6775(5) 0.3992(11) 0.027(2) Uani 0.401(7) 1 d PD D 7 O11A O 0.4050(5) 0.6883(6) 0.3294(12) 0.039(3) Uani 0.401(7) 1 d PD D 7 O12A O 0.4813(4) 0.6292(4) 0.3638(10) 0.038(2) Uani 0.401(7) 1 d PD D 7 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 0.0084(3) 0.0072(3) 0.0265(4) 0.000 0.0021(3) 0.000 N1 0.0118(13) 0.0086(13) 0.0246(16) -0.0012(11) -0.0005(12) -0.0006(10) N2 0.0094(13) 0.0098(13) 0.0252(16) 0.0009(12) 0.0009(12) -0.0004(10) C10 0.0190(17) 0.0090(15) 0.029(2) -0.0020(14) -0.0025(15) 0.0019(13) C11 0.0151(16) 0.0148(16) 0.030(2) -0.0020(16) -0.0056(15) 0.0036(13) C12 0.0121(15) 0.0115(15) 0.026(2) 0.0007(14) 0.0002(14) 0.0024(12) C13 0.0139(16) 0.0131(16) 0.029(2) -0.0053(15) -0.0020(15) -0.0001(13) C14 0.0100(15) 0.0143(16) 0.027(2) -0.0003(14) -0.0023(14) -0.0008(12) C20 0.0135(16) 0.0113(15) 0.0233(19) -0.0017(14) 0.0012(14) -0.0015(12) C21 0.0136(16) 0.0131(15) 0.0197(18) 0.0023(14) -0.0027(13) 0.0004(12) C22 0.0091(14) 0.0113(15) 0.0231(19) 0.0016(14) 0.0003(13) 0.0020(12) C23 0.0119(15) 0.0125(15) 0.028(2) -0.0042(15) -0.0008(14) 0.0013(12) C24 0.0141(16) 0.0178(17) 0.0199(19) -0.0033(14) 0.0042(14) 0.0000(13) C30 0.0147(16) 0.0107(15) 0.028(2) -0.0014(14) -0.0042(15) 0.0004(13) C31 0.0110(15) 0.0149(16) 0.025(2) -0.0003(14) -0.0003(14) 0.0004(12) C32 0.0119(15) 0.0122(16) 0.027(2) -0.0008(14) -0.0014(14) 0.0041(13) C33 0.0143(16) 0.0097(15) 0.029(2) -0.0032(14) -0.0013(14) 0.0029(13) C34 0.0115(15) 0.0143(17) 0.025(2) -0.0023(15) -0.0028(14) 0.0009(12) C35 0.0149(16) 0.0118(16) 0.026(2) -0.0017(14) -0.0044(14) 0.0025(13) C40 0.0118(16) 0.0240(19) 0.037(2) -0.0147(18) -0.0012(15) -0.0008(14) O40 0.0092(11) 0.0122(12) 0.0334(15) -0.0074(11) -0.0007(10) 0.0000(9) O41 0.0140(12) 0.0097(11) 0.0338(16) -0.0021(11) 0.0011(11) 0.0004(9) C42 0.023(2) 0.037(3) 0.062(3) -0.015(2) -0.002(2) -0.0138(19) O42 0.0162(14) 0.068(2) 0.041(2) -0.0058(18) 0.0046(14) -0.0056(15) O10 0.0274(15) 0.0390(18) 0.0280(16) -0.0012(14) -0.0044(13) -0.0052(13) N10 0.018(3) 0.026(3) 0.027(3) 0.003(3) -0.004(2) -0.002(2) O11 0.034(4) 0.045(4) 0.081(7) -0.017(5) -0.010(4) -0.020(3) O12 0.053(4) 0.061(5) 0.057(4) 0.028(4) 0.000(3) 0.015(3) N10A 0.020(4) 0.031(6) 0.030(5) 0.000(4) 0.001(4) 0.010(4) O11A 0.031(5) 0.063(7) 0.023(5) -0.013(5) -0.009(4) -0.001(5) O12A 0.045(5) 0.036(5) 0.033(5) -0.012(4) -0.002(4) 0.006(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 Co1 N2 2.123(3) 3_656 ? Co1 N2 2.123(3) . ? Co1 N1 2.147(3) 3_656 ? Co1 N1 2.147(3) . ? Co1 O10 2.151(3) 3_656 ? Co1 O10 2.151(3) . ? N1 C10 1.343(5) . ? N1 C14 1.344(5) . ? N2 C24 1.334(5) . ? N2 C20 1.347(5) . ? C10 C11 1.387(5) . ? C11 C12 1.404(5) . ? C12 C13 1.390(5) . ? C12 C35 1.485(5) . ? C13 C14 1.389(5) . ? C20 C21 1.382(5) 8_655 ? C21 C20 1.382(5) 8_665 ? C21 C22 1.390(5) . ? C22 C23 1.400(5) . ? C22 C32 1.488(4) . ? C23 C24 1.383(5) 8_665 ? C24 C23 1.383(5) 8_655 ? C30 C31 1.387(5) . ? C30 C35 1.402(5) . ? C31 C32 1.400(5) . ? C32 C33 1.393(5) . ? C33 O41 1.378(4) . ? C33 C34 1.402(5) . ? C34 O40 1.374(4) . ? C34 C35 1.403(5) . ? C40 O40 1.437(5) . ? C40 C42 1.509(6) . ? O41 C41A 1.409(9) . ? O41 C41C 1.470(14) . ? O41 C41B 1.477(12) . ? C42 O42 1.413(6) . ? C41A C44A 1.498(13) . ? C44A O44A 1.423(13) . ? C41B C44B 1.492(14) . ? C44B O44B 1.421(14) . ? C41C C44C 1.478(15) . ? C44C O44C 1.438(16) . ? O10 N10 1.225(6) . ? O10 N10A 1.308(10) . ? N10 O12 1.216(8) . ? N10 O11 1.235(8) . ? N10A O12A 1.224(11) . ? N10A O11A 1.277(11) . ? 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 N2 Co1 N2 90.68(16) 3_656 . ? N2 Co1 N1 87.14(11) 3_656 3_656 ? N2 Co1 N1 176.23(12) . 3_656 ? N2 Co1 N1 176.23(12) 3_656 . ? N2 Co1 N1 87.14(11) . . ? N1 Co1 N1 95.20(15) 3_656 . ? N2 Co1 O10 96.71(12) 3_656 3_656 ? N2 Co1 O10 89.65(13) . 3_656 ? N1 Co1 O10 87.55(12) 3_656 3_656 ? N1 Co1 O10 86.36(12) . 3_656 ? N2 Co1 O10 89.65(13) 3_656 . ? N2 Co1 O10 96.71(12) . . ? N1 Co1 O10 86.36(12) 3_656 . ? N1 Co1 O10 87.55(12) . . ? O10 Co1 O10 170.96(18) 3_656 . ? C10 N1 C14 117.2(3) . . ? C10 N1 Co1 119.1(2) . . ? C14 N1 Co1 123.6(2) . . ? C24 N2 C20 118.0(3) . . ? C24 N2 Co1 120.7(2) . . ? C20 N2 Co1 121.0(2) . . ? N1 C10 C11 123.1(3) . . ? C10 C11 C12 119.6(3) . . ? C13 C12 C11 117.2(3) . . ? C13 C12 C35 124.1(3) . . ? C11 C12 C35 118.7(3) . . ? C14 C13 C12 119.5(3) . . ? N1 C14 C13 123.4(3) . . ? N2 C20 C21 122.6(3) . 8_655 ? C20 C21 C22 119.4(3) 8_665 . ? C21 C22 C23 117.6(3) . . ? C21 C22 C32 124.0(3) . . ? C23 C22 C32 118.4(3) . . ? C24 C23 C22 119.2(3) 8_665 . ? N2 C24 C23 122.9(3) . 8_655 ? C31 C30 C35 121.4(3) . . ? C30 C31 C32 120.0(3) . . ? C33 C32 C31 119.4(3) . . ? C33 C32 C22 121.1(3) . . ? C31 C32 C22 119.1(3) . . ? O41 C33 C32 119.2(3) . . ? O41 C33 C34 120.3(3) . . ? C32 C33 C34 120.5(3) . . ? O40 C34 C33 120.6(3) . . ? O40 C34 C35 118.8(3) . . ? C33 C34 C35 120.2(3) . . ? C30 C35 C34 118.5(3) . . ? C30 C35 C12 118.6(3) . . ? C34 C35 C12 122.9(3) . . ? O40 C40 C42 108.8(4) . . ? C34 O40 C40 115.4(3) . . ? C33 O41 C41A 117.8(6) . . ? C33 O41 C41C 112.9(8) . . ? C41A O41 C41C 15.1(11) . . ? C33 O41 C41B 108.9(7) . . ? C41A O41 C41B 11.8(10) . . ? C41C O41 C41B 23.0(12) . . ? O42 C42 C40 113.2(4) . . ? O41 C41A C44A 104.6(9) . . ? O44A C44A C41A 109.6(11) . . ? O41 C41B C44B 111.4(12) . . ? O44B C44B C41B 123.3(13) . . ? C44C C41C O41 113.0(16) . . ? O44C C44C C41C 86.6(14) . . ? N10 O10 N10A 41.5(4) . . ? N10 O10 Co1 144.0(3) . . ? N10A O10 Co1 131.2(4) . . ? O12 N10 O10 125.0(6) . . ? O12 N10 O11 116.5(8) . . ? O10 N10 O11 118.4(7) . . ? O12A N10A O11A 119.6(10) . . ? O12A N10A O10 117.1(8) . . ? O11A N10A O10 123.1(9) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.650 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.111 #==END data_pbcn_Co_80k_H2O_again _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA. M. KAWANO, M. TOMINAGA. M. FUJITA ; _journal_name_full 'Angew. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Co N6 O20' _chemical_formula_weight 971.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.677(3) _cell_length_b 20.576(2) _cell_length_c 8.7155(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4246.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _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 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9294 _exptl_absorpt_correction_T_max 0.9522 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45347 _diffrn_reflns_av_R_equivalents 0.1026 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.76 _reflns_number_total 5235 _reflns_number_gt 2866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C23 to O5 and C24 to O4) converged to 52% and 48%, respectively. The occupancy of the disordered nitrate ions (N10 to O12, N11 to O17) converged to 60%, and 40%,respectively. The thermal temperature factors of all atoms were anisotropically refined. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered ethylene glycol groups and nitrate ions. ; _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^)+(0.1392P)^2^+16.0087P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5235 _refine_ls_number_parameters 379 _refine_ls_number_restraints 173 _refine_ls_R_factor_all 0.1770 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.3340 _refine_ls_wR_factor_gt 0.2592 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.006 _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 1.0000 0.79610(5) 0.2500 0.0309(4) Uani 1 2 d S . . N1 N 0.93569(18) 0.7219(2) 0.2632(6) 0.0300(11) Uani 1 1 d . . . N2 N 0.93521(18) 0.8683(2) 0.2750(6) 0.0340(12) Uani 1 1 d . . . O1 O 0.99148(17) 0.7957(2) 0.0117(6) 0.0472(12) Uani 1 1 d . . . O2 O 0.86207(15) 0.48935(19) 0.3066(5) 0.0350(10) Uani 1 1 d . . . O3 O 0.76892(16) 0.40738(18) 0.3285(5) 0.0355(10) Uani 1 1 d . A . C1 C 0.8888(2) 0.7257(3) 0.1759(8) 0.0324(13) Uani 1 1 d . . . H1 H 0.8856 0.7610 0.1060 0.039 Uiso 1 1 calc R . . C2 C 0.8450(2) 0.6811(3) 0.1824(7) 0.0305(12) Uani 1 1 d . . . H2 H 0.8128 0.6862 0.1185 0.037 Uiso 1 1 calc R . . C3 C 0.9387(2) 0.6705(3) 0.3596(8) 0.0367(14) Uani 1 1 d . . . H3 H 0.9715 0.6663 0.4219 0.044 Uiso 1 1 calc R . . C4 C 0.8975(2) 0.6239(3) 0.3730(8) 0.0388(14) Uani 1 1 d . . . H4 H 0.9022 0.5888 0.4425 0.047 Uiso 1 1 calc R . . C5 C 0.8486(2) 0.6285(3) 0.2841(7) 0.0333(14) Uani 1 1 d . . . C6 C 0.8008(2) 0.5824(3) 0.2943(7) 0.0336(13) Uani 1 1 d . . . C7 C 0.7449(2) 0.6066(3) 0.2884(8) 0.0386(15) Uani 1 1 d . . . H7 H 0.7390 0.6521 0.2796 0.046 Uiso 1 1 calc R . . C8 C 0.6993(2) 0.5659(3) 0.2951(8) 0.0384(15) Uani 1 1 d . . . H8 H 0.6623 0.5837 0.2919 0.046 Uiso 1 1 calc R . . C9 C 0.8083(2) 0.5152(3) 0.3108(8) 0.0333(13) Uani 1 1 d . . . C10 C 0.7611(2) 0.4737(3) 0.3170(8) 0.0333(13) Uani 1 1 d . . . C11 C 0.7061(2) 0.4985(3) 0.3064(8) 0.0371(14) Uani 1 1 d . . . C12 C 0.6564(2) 0.4540(3) 0.3009(8) 0.0350(13) Uani 1 1 d . . . C13 C 0.6137(2) 0.4646(3) 0.1952(9) 0.0396(15) Uani 1 1 d . . . H13 H 0.6150 0.5014 0.1294 0.047 Uiso 1 1 calc R . . C14 C 0.6510(2) 0.4006(3) 0.3977(8) 0.0341(13) Uani 1 1 d . . . H14 H 0.6788 0.3924 0.4739 0.041 Uiso 1 1 calc R . . C15 C 0.9308(2) 0.9211(3) 0.1861(8) 0.0366(14) Uani 1 1 d . . . H15 H 0.9598 0.9292 0.1130 0.044 Uiso 1 1 calc R . . C16 C 0.8951(2) 0.8593(3) 0.3830(8) 0.0347(13) Uani 1 1 d . . . H16 H 0.8985 0.8235 0.4512 0.042 Uiso 1 1 calc R . . C20 C 0.8789(2) 0.4547(3) 0.4424(9) 0.0409(15) Uani 1 1 d . . . H20A H 0.8506 0.4210 0.4677 0.049 Uiso 1 1 calc R . . H20B H 0.8818 0.4851 0.5303 0.049 Uiso 1 1 calc R . . C21 C 0.9358(3) 0.4235(4) 0.4117(12) 0.067(2) Uani 1 1 d . . . H21A H 0.9453 0.3955 0.5004 0.080 Uiso 1 1 calc R . . H21B H 0.9319 0.3949 0.3211 0.080 Uiso 1 1 calc R . . C22 C 0.7875(3) 0.3754(3) 0.1895(9) 0.0525(18) Uani 1 1 d D . . O4 O 0.9799(2) 0.4640(4) 0.3865(8) 0.089(2) Uani 1 1 d . . . C23 C 0.7600(13) 0.3087(9) 0.205(6) 0.053(9) Uani 0.524(14) 1 d PD A 1 O6 O 0.7888(7) 0.2708(5) 0.3208(15) 0.088(5) Uani 0.524(14) 1 d P A 1 C24 C 0.756(2) 0.3116(15) 0.163(7) 0.086(19) Uani 0.476(14) 1 d PD A 2 O5 O 0.7735(6) 0.2738(5) 0.0516(15) 0.068(4) Uani 0.476(14) 1 d P A 2 N10 N 0.9126(9) 0.2605(13) 0.237(2) 0.169(10) Uani 0.60 1 d PDU B 3 O10 O 0.8886(6) 0.2585(7) 0.1378(19) 0.110(5) Uani 0.60 1 d PDU B 3 O11 O 0.8933(15) 0.260(2) 0.345(2) 0.276(13) Uani 0.60 1 d PDU B 3 O12 O 0.9573(10) 0.2661(15) 0.235(4) 0.259(12) Uani 0.60 1 d PDU . 3 N11 N 0.8826(11) 0.2096(15) 0.269(3) 0.137(9) Uani 0.40 1 d PDU C 4 O15 O 0.8511(12) 0.2205(13) 0.355(3) 0.155(8) Uani 0.40 1 d PDU C 4 O16 O 0.9119(10) 0.1743(9) 0.312(3) 0.152(8) Uani 0.40 1 d PDU C 4 O17 O 0.8641(17) 0.210(2) 0.156(3) 0.221(12) Uani 0.40 1 d PDU C 4 O1W O 0.9962(7) 0.0630(10) 0.1241(13) 0.102(5) Uani 0.50 1 d PU . 5 O2W O 0.9643(13) 0.1221(17) 0.183(3) 0.172(8) Uani 0.50 1 d PU . 5 O3W O 0.9982(14) 0.0758(11) 0.2845(19) 0.129(7) Uani 0.50 1 d PU . 5 O4W O 0.9457(11) 0.1215(15) 0.291(3) 0.161(8) Uani 0.50 1 d PU . 5 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 0.0141(5) 0.0199(5) 0.0588(8) 0.000 -0.0009(5) 0.000 N1 0.020(2) 0.0163(19) 0.054(3) 0.0001(19) -0.002(2) 0.0000(16) N2 0.015(2) 0.027(2) 0.060(3) 0.000(2) 0.001(2) 0.0008(17) O1 0.030(2) 0.045(3) 0.066(3) 0.010(2) -0.004(2) -0.0059(18) O2 0.0188(18) 0.028(2) 0.058(3) 0.0081(19) 0.0034(17) -0.0013(15) O3 0.0242(19) 0.0239(19) 0.058(3) 0.0044(18) 0.0019(18) -0.0027(15) C1 0.020(2) 0.023(3) 0.054(4) -0.002(2) -0.002(2) -0.001(2) C2 0.019(2) 0.023(3) 0.049(3) -0.001(2) -0.001(2) 0.005(2) C3 0.023(3) 0.023(3) 0.064(4) 0.003(3) -0.003(3) 0.001(2) C4 0.023(3) 0.030(3) 0.064(4) 0.004(3) -0.002(3) -0.003(2) C5 0.021(3) 0.025(3) 0.054(4) 0.001(2) 0.004(2) -0.004(2) C6 0.025(3) 0.027(3) 0.049(4) 0.002(2) -0.003(2) -0.004(2) C7 0.027(3) 0.027(3) 0.062(4) 0.002(3) -0.003(3) -0.002(2) C8 0.023(3) 0.028(3) 0.064(4) 0.001(3) -0.005(3) -0.002(2) C9 0.025(3) 0.026(3) 0.049(3) 0.000(3) -0.003(2) -0.001(2) C10 0.026(3) 0.023(3) 0.052(4) 0.004(2) -0.001(2) -0.003(2) C11 0.027(3) 0.029(3) 0.056(4) 0.004(3) -0.005(3) -0.005(2) C12 0.023(3) 0.026(3) 0.056(4) 0.006(3) 0.000(2) -0.005(2) C13 0.024(3) 0.029(3) 0.065(4) 0.008(3) -0.003(3) -0.002(2) C14 0.021(2) 0.029(3) 0.052(4) 0.007(3) -0.004(2) -0.003(2) C15 0.021(3) 0.026(3) 0.062(4) 0.005(3) 0.003(3) 0.002(2) C16 0.022(3) 0.027(3) 0.056(4) 0.003(3) 0.001(2) 0.004(2) C20 0.026(3) 0.038(3) 0.059(4) 0.012(3) -0.003(3) 0.000(2) C21 0.030(3) 0.065(5) 0.104(7) 0.017(5) -0.006(4) 0.005(3) C22 0.072(5) 0.028(3) 0.058(4) -0.003(3) 0.009(4) -0.006(3) O4 0.037(3) 0.136(6) 0.095(5) -0.007(5) 0.008(3) -0.017(4) C23 0.072(14) 0.018(9) 0.07(3) -0.015(8) 0.000(12) 0.000(9) O6 0.160(14) 0.032(6) 0.071(8) 0.011(5) -0.018(8) -0.003(7) C24 0.14(3) 0.050(17) 0.07(3) -0.020(13) 0.05(2) -0.049(19) O5 0.093(10) 0.035(6) 0.076(9) -0.020(6) 0.008(7) -0.008(6) N10 0.157(16) 0.150(16) 0.201(17) 0.038(15) -0.028(13) 0.121(14) O10 0.083(8) 0.079(9) 0.169(13) -0.032(10) 0.050(8) -0.005(8) O11 0.38(3) 0.26(3) 0.186(15) 0.02(3) 0.02(2) 0.08(3) O12 0.170(16) 0.24(2) 0.37(3) 0.04(2) -0.099(17) 0.08(2) N11 0.120(17) 0.100(15) 0.190(17) -0.044(16) -0.114(12) 0.009(13) O15 0.156(19) 0.107(16) 0.201(18) -0.026(17) -0.068(15) -0.046(13) O16 0.151(16) 0.060(11) 0.247(19) 0.000(13) -0.125(14) -0.029(10) O17 0.24(3) 0.24(3) 0.179(17) -0.02(2) -0.113(16) 0.05(2) O1W 0.113(11) 0.178(13) 0.015(6) -0.015(7) 0.015(6) -0.083(9) O2W 0.180(19) 0.232(18) 0.106(14) 0.001(14) 0.003(12) 0.000(14) O3W 0.158(14) 0.167(14) 0.063(11) -0.080(10) -0.011(15) 0.005(13) O4W 0.152(16) 0.199(18) 0.134(15) -0.019(14) 0.029(13) 0.015(13) _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 O1 2.086(6) 3_755 ? Co1 O1 2.086(6) . ? Co1 N2 2.147(5) 3_755 ? Co1 N2 2.147(5) . ? Co1 N1 2.159(4) . ? Co1 N1 2.159(4) 3_755 ? N1 C1 1.348(7) . ? N1 C3 1.354(7) . ? N2 C15 1.338(8) . ? N2 C16 1.349(8) . ? O2 C9 1.380(6) . ? O2 C20 1.438(8) . ? O3 C10 1.381(6) . ? O3 C22 1.447(9) . ? C1 C2 1.386(8) . ? C2 C5 1.402(8) . ? C3 C4 1.372(8) . ? C4 C5 1.397(8) . ? C5 C6 1.479(8) . ? C6 C9 1.402(8) . ? C6 C7 1.415(8) . ? C7 C8 1.369(8) . ? C8 C11 1.399(8) . ? C9 C10 1.407(8) . ? C10 C11 1.401(8) . ? C11 C12 1.492(8) . ? C12 C13 1.386(9) . ? C12 C14 1.391(8) . ? C13 C15 1.386(8) 8_755 ? C14 C16 1.389(7) 8_755 ? C15 C13 1.386(8) 8_765 ? C16 C14 1.389(7) 8_765 ? C20 C21 1.516(9) . ? C21 O4 1.353(10) . ? C22 C23 1.524(16) . ? C22 C24 1.524(17) . ? C23 O6 1.45(5) . ? C24 O5 1.31(6) . ? N10 O11 1.047(16) . ? N10 O10 1.033(15) . ? N10 O12 1.066(16) . ? O12 O12 2.04(4) 3_755 ? N11 O15 1.075(18) . ? N11 O16 1.071(17) . ? N11 O17 1.082(16) . ? O15 O16 1.76(2) . ? O15 O17 1.77(2) . ? O1W O3W 0.85(2) 3_755 ? O1W O3W 1.42(2) . ? O1W O2W 1.52(4) . ? O2W O4W 1.04(3) . ? O2W O3W 1.33(4) 3_755 ? O2W O3W 1.53(4) . ? O3W O3W 0.61(4) 3_755 ? O3W O1W 0.85(2) 3_755 ? O3W O2W 1.33(4) 3_755 ? O3W O4W 1.56(4) . ? O3W O4W 1.76(4) 3_755 ? O4W O3W 1.76(4) 3_755 ? 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 Co1 O1 179.5(3) 3_755 . ? O1 Co1 N2 92.01(19) 3_755 3_755 ? O1 Co1 N2 88.34(19) . 3_755 ? O1 Co1 N2 88.34(19) 3_755 . ? O1 Co1 N2 92.01(19) . . ? N2 Co1 N2 92.4(2) 3_755 . ? O1 Co1 N1 90.69(19) 3_755 . ? O1 Co1 N1 88.95(18) . . ? N2 Co1 N1 177.1(2) 3_755 . ? N2 Co1 N1 88.86(17) . . ? O1 Co1 N1 88.95(18) 3_755 3_755 ? O1 Co1 N1 90.69(19) . 3_755 ? N2 Co1 N1 88.86(17) 3_755 3_755 ? N2 Co1 N1 177.1(2) . 3_755 ? N1 Co1 N1 90.0(2) . 3_755 ? C1 N1 C3 116.1(5) . . ? C1 N1 Co1 120.6(4) . . ? C3 N1 Co1 123.3(4) . . ? C15 N2 C16 117.5(5) . . ? C15 N2 Co1 123.9(4) . . ? C16 N2 Co1 118.6(4) . . ? C9 O2 C20 115.1(5) . . ? C10 O3 C22 115.4(5) . . ? N1 C1 C2 123.7(6) . . ? C1 C2 C5 119.5(5) . . ? N1 C3 C4 124.1(6) . . ? C3 C4 C5 119.7(6) . . ? C4 C5 C2 116.9(5) . . ? C4 C5 C6 123.9(5) . . ? C2 C5 C6 119.1(5) . . ? C9 C6 C7 117.9(5) . . ? C9 C6 C5 122.9(5) . . ? C7 C6 C5 119.2(5) . . ? C8 C7 C6 121.4(6) . . ? C7 C8 C11 121.3(6) . . ? O2 C9 C6 119.5(5) . . ? O2 C9 C10 120.0(5) . . ? C6 C9 C10 120.2(5) . . ? O3 C10 C11 119.3(5) . . ? O3 C10 C9 119.7(5) . . ? C11 C10 C9 120.9(5) . . ? C8 C11 C10 118.2(5) . . ? C8 C11 C12 121.0(5) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C14 117.4(5) . . ? C13 C12 C11 120.0(5) . . ? C14 C12 C11 122.6(5) . . ? C12 C13 C15 119.4(6) . 8_755 ? C16 C14 C12 120.0(5) 8_755 . ? N2 C15 C13 123.4(6) . 8_765 ? N2 C16 C14 122.2(5) . 8_765 ? O2 C20 C21 108.1(6) . . ? O4 C21 C20 117.0(7) . . ? O3 C22 C23 102.0(18) . . ? O3 C22 C24 112(2) . . ? C23 C22 C24 14(4) . . ? O6 C23 C22 110(2) . . ? O5 C24 C22 118(3) . . ? O11 N10 O10 120.7(17) . . ? O11 N10 O12 116.8(16) . . ? O10 N10 O12 122.4(17) . . ? N10 O12 O12 169(3) . 3_755 ? O15 N11 O16 110(2) . . ? O15 N11 O17 111(2) . . ? O16 N11 O17 126(3) . . ? N11 O15 O16 34.7(11) . . ? N11 O15 O17 34.9(10) . . ? O16 O15 O17 65.6(12) . . ? N11 O16 O15 34.9(11) . . ? N11 O17 O15 34.6(11) . . ? O3W O1W O3W 10(3) 3_755 . ? O3W O1W O2W 61(2) 3_755 . ? O3W O1W O2W 62.4(15) . . ? O4W O2W O3W 95(3) . 3_755 ? O4W O2W O3W 72(3) . . ? O3W O2W O3W 23.2(17) 3_755 . ? O4W O2W O1W 120(4) . . ? O3W O2W O1W 33.8(12) 3_755 . ? O3W O2W O1W 55.6(15) . . ? O3W O3W O1W 155(6) 3_755 3_755 ? O3W O3W O2W 97(5) 3_755 3_755 ? O1W O3W O2W 85(3) 3_755 3_755 ? O3W O3W O1W 15(4) 3_755 . ? O1W O3W O1W 150(4) 3_755 . ? O2W O3W O1W 111(3) 3_755 . ? O3W O3W O2W 60(4) 3_755 . ? O1W O3W O2W 145(3) 3_755 . ? O2W O3W O2W 92(3) 3_755 . ? O1W O3W O2W 62.0(16) . . ? O3W O3W O4W 99(5) 3_755 . ? O1W O3W O4W 106(2) 3_755 . ? O2W O3W O4W 95(2) 3_755 . ? O1W O3W O4W 97(2) . . ? O2W O3W O4W 39.4(13) . . ? O3W O3W O4W 61(5) 3_755 3_755 ? O1W O3W O4W 114(3) 3_755 3_755 ? O2W O3W O4W 36.2(16) 3_755 3_755 ? O1W O3W O4W 75.8(17) . 3_755 ? O2W O3W O4W 81.1(18) . 3_755 ? O4W O3W O4W 107(2) . 3_755 ? O2W O4W O3W 69(3) . . ? O2W O4W O3W 49(2) . 3_755 ? O3W O4W O3W 19.9(11) . 3_755 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.012 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.135 #==END data_pbcn_Ni_80K_H2O_ini _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA, M. KAWANO, T. Hozumi, S. Ohkoshi, M. Fujita ; _journal_name_full 'Inorg. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 N6 Ni O18.88' _chemical_formula_weight 953.39 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.481(2) _cell_length_b 20.5272(18) _cell_length_c 8.8844(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4282.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9234 _exptl_absorpt_correction_T_max 0.9480 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34419 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.79 _reflns_number_total 5191 _reflns_number_gt 2966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C43 to O43 and C43A to O43A) converged to 65% and 35%, respectively. The occupancy of the disordered nitrate ions (N20 to O23, N25 to O28) converged to 50%, and 50%,respectively. The thermal temperature factors of all atoms were anisotropically refined. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered ethylene glycol groups, nitrate ions and water molecules. ; _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^)+(0.1065P)^2^+12.9297P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5191 _refine_ls_number_parameters 382 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2385 _refine_ls_wR_factor_gt 0.1966 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.5000 0.20725(3) 0.2500 0.0294(3) Uani 1 2 d S . . O1 O 0.49345(13) 0.20694(16) 0.0166(5) 0.0440(9) Uani 1 1 d . . . N1 N 0.43616(14) 0.13594(17) 0.2675(5) 0.0309(9) Uani 1 1 d . . . N2 N 0.43657(14) 0.27971(17) 0.2608(5) 0.0293(9) Uani 1 1 d . . . C10 C 0.43180(19) 0.0855(2) 0.1738(7) 0.0385(13) Uani 1 1 d . . . H10 H 0.4608 0.0793 0.1007 0.046 Uiso 1 1 calc R . . C11 C 0.38666(18) 0.0413(2) 0.1782(7) 0.0374(12) Uani 1 1 d . . . H11 H 0.3854 0.0058 0.1098 0.045 Uiso 1 1 calc R . . C12 C 0.34387(17) 0.0498(2) 0.2831(6) 0.0313(11) Uani 1 1 d . . . C13 C 0.34895(18) 0.1018(2) 0.3834(6) 0.0337(11) Uani 1 1 d . . . H13 H 0.3207 0.1090 0.4580 0.040 Uiso 1 1 calc R . . C14 C 0.39561(18) 0.1426(2) 0.3729(6) 0.0327(11) Uani 1 1 d . . . H14 H 0.3992 0.1770 0.4438 0.039 Uiso 1 1 calc R . . C20 C 0.38945(17) 0.2749(2) 0.1742(6) 0.0293(10) Uani 1 1 d . . . H20 H 0.3861 0.2387 0.1081 0.035 Uiso 1 1 calc R . . C21 C 0.34593(17) 0.3201(2) 0.1774(6) 0.0267(10) Uani 1 1 d . . . H21 H 0.3137 0.3148 0.1139 0.032 Uiso 1 1 calc R . . C22 C 0.34923(16) 0.3739(2) 0.2742(5) 0.0254(10) Uani 1 1 d . . . C23 C 0.39815(17) 0.3788(2) 0.3623(6) 0.0316(11) Uani 1 1 d . . . H23 H 0.4029 0.4145 0.4290 0.038 Uiso 1 1 calc R . . C24 C 0.43978(17) 0.3313(2) 0.3522(6) 0.0329(11) Uani 1 1 d . . . H24 H 0.4726 0.3357 0.4139 0.040 Uiso 1 1 calc R . . C30 C 0.19098(17) -0.0121(2) 0.2961(5) 0.0267(10) Uani 1 1 d . . . C31 C 0.23825(18) 0.0299(2) 0.2982(6) 0.0279(10) Uani 1 1 d . . . C32 C 0.29386(18) 0.0051(2) 0.2873(6) 0.0308(11) Uani 1 1 d . . . C33 C 0.30118(18) -0.0623(2) 0.2751(6) 0.0331(11) Uani 1 1 d . . . H33 H 0.3385 -0.0799 0.2697 0.040 Uiso 1 1 calc R . . C34 C 0.25457(18) -0.1036(2) 0.2708(6) 0.0302(10) Uani 1 1 d . . . H34 H 0.2605 -0.1492 0.2607 0.036 Uiso 1 1 calc R . . C35 C 0.19895(17) -0.0795(2) 0.2808(5) 0.0263(10) Uani 1 1 d . . . O40 O 0.13658(11) 0.01367(14) 0.2947(4) 0.0266(7) Uani 1 1 d . . . C40 C 0.12092(18) 0.0469(2) 0.4314(6) 0.0326(11) Uani 1 1 d . . . H40A H 0.1501 0.0799 0.4571 0.039 Uiso 1 1 calc R . . H40B H 0.1184 0.0154 0.5155 0.039 Uiso 1 1 calc R . . C41 C 0.06396(18) 0.0794(2) 0.4075(7) 0.0381(12) Uani 1 1 d . . . H41A H 0.0554 0.1073 0.4956 0.046 Uiso 1 1 calc R . . H41B H 0.0664 0.1080 0.3179 0.046 Uiso 1 1 calc R . . O41 O 0.23058(12) 0.09610(14) 0.3093(4) 0.0293(7) Uani 1 1 d . A . O42 O 0.01891(14) 0.0347(2) 0.3872(5) 0.0529(11) Uani 1 1 d . . . C42 C 0.2110(2) 0.1277(2) 0.1742(6) 0.0385(12) Uani 1 1 d D . . C43 C 0.2455(7) 0.1891(6) 0.1438(17) 0.050(4) Uani 0.648(11) 1 d PD A 1 O43 O 0.2249(3) 0.2286(3) 0.0363(8) 0.067(3) Uani 0.648(11) 1 d PD A 1 C43A C 0.2386(13) 0.1935(9) 0.199(3) 0.059(9) Uani 0.352(11) 1 d PD A 2 O43A O 0.2165(7) 0.2340(5) 0.3007(16) 0.072(5) Uani 0.352(11) 1 d PD A 2 N20 N 0.1271(7) 0.2848(5) 0.2973(19) 0.089(5) Uani 0.50 1 d PDU B 3 O21 O 0.1432(6) 0.2965(6) 0.1619(14) 0.110(4) Uani 0.50 1 d PDU B 3 O22 O 0.0964(4) 0.3281(4) 0.3593(11) 0.063(2) Uani 0.50 1 d PDU B 3 O23 O 0.1050(14) 0.2257(6) 0.312(3) 0.198(12) Uani 0.50 1 d PDU B 3 N25 N 0.0881(7) 0.2459(8) 0.2333(15) 0.104(5) Uani 0.50 1 d PDU C 4 O26 O 0.1106(5) 0.2419(5) 0.1064(11) 0.075(3) Uani 0.50 1 d PDU C 4 O27 O 0.0353(7) 0.2302(8) 0.244(2) 0.180(8) Uani 0.50 1 d PDU . 4 O28 O 0.1237(12) 0.2543(17) 0.346(2) 0.205(10) Uani 0.50 1 d PDU C 4 O1W O 0.0000 0.4220(5) 0.2500 0.082(3) Uani 0.764(12) 2 d SPU . . O2W O -0.0045(7) 0.4497(7) 0.1434(17) 0.081(4) Uani 0.382(6) 1 d PU . . O3W O 0.0311(4) 0.3959(5) 0.1540(13) 0.046(3) Uani 0.382(6) 1 d PU . . O4W O 0.0525(9) 0.3888(12) 0.253(2) 0.130(7) Uani 0.382(6) 1 d PU . . 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 0.0083(3) 0.0152(4) 0.0645(6) 0.000 0.0017(3) 0.000 O1 0.0202(16) 0.0388(19) 0.073(3) -0.0088(18) -0.0005(16) 0.0016(14) N1 0.0114(16) 0.0189(17) 0.062(3) -0.0027(18) 0.0033(17) -0.0001(12) N2 0.0124(16) 0.0190(17) 0.056(3) 0.0001(17) -0.0006(16) 0.0014(12) C10 0.017(2) 0.024(2) 0.074(4) -0.006(2) 0.010(2) -0.0029(17) C11 0.018(2) 0.022(2) 0.072(4) -0.008(2) 0.005(2) -0.0016(17) C12 0.0149(18) 0.023(2) 0.056(3) 0.003(2) 0.0007(19) -0.0054(16) C13 0.020(2) 0.031(2) 0.050(3) -0.001(2) 0.002(2) -0.0037(18) C14 0.019(2) 0.027(2) 0.053(3) 0.000(2) -0.001(2) -0.0059(17) C20 0.0158(19) 0.020(2) 0.052(3) -0.003(2) 0.0044(19) -0.0018(15) C21 0.0147(18) 0.0202(19) 0.045(3) 0.0039(19) -0.0001(18) 0.0001(15) C22 0.0149(18) 0.0188(18) 0.042(3) 0.0047(18) 0.0035(17) 0.0013(14) C23 0.0174(19) 0.025(2) 0.053(3) -0.003(2) -0.0003(19) 0.0020(17) C24 0.0135(18) 0.023(2) 0.062(3) -0.003(2) -0.0026(19) -0.0005(16) C30 0.0170(18) 0.022(2) 0.041(3) -0.0013(18) -0.0013(17) -0.0023(16) C31 0.020(2) 0.022(2) 0.042(3) -0.0004(18) -0.0017(18) -0.0048(16) C32 0.0191(19) 0.025(2) 0.048(3) 0.002(2) -0.0003(19) -0.0066(17) C33 0.0149(19) 0.027(2) 0.058(3) 0.000(2) 0.0022(19) -0.0025(16) C34 0.0185(19) 0.0214(19) 0.051(3) 0.001(2) -0.0010(19) -0.0042(16) C35 0.0177(19) 0.0201(19) 0.041(3) 0.0007(18) -0.0032(17) -0.0055(15) O40 0.0149(13) 0.0248(15) 0.0402(19) -0.0052(13) -0.0023(12) -0.0001(11) C40 0.019(2) 0.035(2) 0.043(3) -0.013(2) 0.0009(19) -0.0026(18) C41 0.019(2) 0.039(3) 0.056(3) -0.003(2) 0.006(2) 0.0011(19) O41 0.0218(14) 0.0193(14) 0.047(2) -0.0004(14) -0.0035(14) -0.0022(12) O42 0.0198(16) 0.078(3) 0.061(3) 0.002(2) -0.0047(16) -0.0152(18) C42 0.040(3) 0.027(2) 0.048(3) 0.004(2) -0.010(2) -0.006(2) C43 0.075(8) 0.040(6) 0.033(9) 0.016(5) -0.014(6) -0.034(5) O43 0.094(6) 0.048(4) 0.059(5) 0.012(3) -0.014(4) -0.028(4) C43A 0.10(2) 0.044(13) 0.031(17) 0.023(10) 0.008(13) -0.019(11) O43A 0.125(13) 0.023(6) 0.067(10) 0.000(6) -0.027(9) -0.012(7) N20 0.098(10) 0.057(7) 0.112(12) 0.018(8) 0.068(10) 0.001(6) O21 0.124(11) 0.117(11) 0.089(8) 0.001(7) 0.023(8) 0.001(8) O22 0.061(5) 0.043(4) 0.085(7) 0.006(4) 0.027(5) -0.006(4) O23 0.29(3) 0.041(6) 0.26(3) 0.009(11) 0.08(2) -0.018(11) N25 0.132(10) 0.091(11) 0.087(8) 0.055(8) 0.036(8) 0.085(9) O26 0.102(8) 0.060(6) 0.062(6) 0.004(5) -0.008(5) 0.018(6) O27 0.135(10) 0.140(13) 0.264(19) 0.093(12) 0.093(11) 0.091(10) O28 0.32(2) 0.21(2) 0.078(10) -0.029(16) -0.014(13) 0.04(2) O1W 0.108(8) 0.076(7) 0.062(6) 0.000 0.014(5) 0.000 O2W 0.102(10) 0.066(8) 0.077(9) 0.016(6) -0.018(8) -0.019(6) O3W 0.029(5) 0.057(6) 0.052(7) -0.022(5) -0.006(4) -0.013(4) O4W 0.119(13) 0.167(17) 0.102(12) 0.025(12) -0.014(9) 0.035(11) _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 O1 2.080(4) . ? Ni1 O1 2.080(4) 3_655 ? Ni1 N1 2.101(3) 3_655 ? Ni1 N1 2.101(3) . ? Ni1 N2 2.107(3) 3_655 ? Ni1 N2 2.107(3) . ? N1 C10 1.333(6) . ? N1 C14 1.343(6) . ? N2 C24 1.337(6) . ? N2 C20 1.351(6) . ? C10 C11 1.395(6) . ? C11 C12 1.381(7) . ? C12 C13 1.396(7) . ? C12 C32 1.491(6) . ? C13 C14 1.382(6) . ? C20 C21 1.382(6) . ? C21 C22 1.401(6) . ? C22 C23 1.394(6) . ? C22 C35 1.483(5) 8_665 ? C23 C24 1.383(6) . ? C30 O40 1.382(5) . ? C30 C35 1.403(6) . ? C30 C31 1.405(6) . ? C31 O41 1.375(5) . ? C31 C32 1.405(6) . ? C32 C33 1.397(6) . ? C33 C34 1.385(6) . ? C34 C35 1.399(6) . ? C35 C22 1.483(5) 8_655 ? O40 C40 1.440(6) . ? C40 C41 1.510(6) . ? C41 O42 1.412(6) . ? O41 C42 1.440(6) . ? C42 C43A 1.513(16) . ? C42 C43 1.522(10) . ? C43 O43 1.342(14) . ? C43A O43A 1.333(18) . ? N20 O22 1.270(12) . ? N20 O21 1.284(13) . ? N20 O23 1.325(14) . ? N25 O26 1.248(12) . ? N25 O27 1.283(14) . ? N25 O28 1.317(14) . ? O27 O27 1.66(3) 3 ? O1W O2W 1.111(14) 3 ? O1W O2W 1.111(14) . ? O1W O3W 1.244(11) . ? O1W O3W 1.244(11) 3 ? O1W O4W 1.41(2) 3 ? O1W O4W 1.41(2) . ? O2W O3W 1.389(18) . ? O3W O4W 1.022(19) . ? 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 Ni1 O1 179.65(19) . 3_655 ? O1 Ni1 N1 88.67(15) . 3_655 ? O1 Ni1 N1 91.09(15) 3_655 3_655 ? O1 Ni1 N1 91.09(15) . . ? O1 Ni1 N1 88.67(15) 3_655 . ? N1 Ni1 N1 91.67(18) 3_655 . ? O1 Ni1 N2 90.51(15) . 3_655 ? O1 Ni1 N2 89.73(15) 3_655 3_655 ? N1 Ni1 N2 89.09(13) 3_655 3_655 ? N1 Ni1 N2 178.24(17) . 3_655 ? O1 Ni1 N2 89.73(15) . . ? O1 Ni1 N2 90.51(15) 3_655 . ? N1 Ni1 N2 178.24(17) 3_655 . ? N1 Ni1 N2 89.09(13) . . ? N2 Ni1 N2 90.19(19) 3_655 . ? C10 N1 C14 117.4(4) . . ? C10 N1 Ni1 123.4(3) . . ? C14 N1 Ni1 119.2(3) . . ? C24 N2 C20 116.8(4) . . ? C24 N2 Ni1 123.2(3) . . ? C20 N2 Ni1 120.1(3) . . ? N1 C10 C11 123.1(5) . . ? C12 C11 C10 119.4(5) . . ? C11 C12 C13 117.7(4) . . ? C11 C12 C32 120.9(4) . . ? C13 C12 C32 121.5(4) . . ? C14 C13 C12 119.2(4) . . ? N1 C14 C13 123.2(5) . . ? N2 C20 C21 123.0(4) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C21 116.6(4) . . ? C23 C22 C35 124.0(4) . 8_665 ? C21 C22 C35 119.4(4) . 8_665 ? C24 C23 C22 119.7(4) . . ? N2 C24 C23 123.9(4) . . ? O40 C30 C35 120.0(3) . . ? O40 C30 C31 119.7(4) . . ? C35 C30 C31 120.1(4) . . ? O41 C31 C30 120.2(4) . . ? O41 C31 C32 119.0(4) . . ? C30 C31 C32 120.7(4) . . ? C33 C32 C31 118.6(4) . . ? C33 C32 C12 120.7(4) . . ? C31 C32 C12 120.7(4) . . ? C34 C33 C32 120.7(4) . . ? C33 C34 C35 121.3(4) . . ? C34 C35 C30 118.6(4) . . ? C34 C35 C22 118.8(4) . 8_655 ? C30 C35 C22 122.6(4) . 8_655 ? C30 O40 C40 114.2(3) . . ? O40 C40 C41 108.5(4) . . ? O42 C41 C40 113.2(4) . . ? C31 O41 C42 115.3(4) . . ? O41 C42 C43A 98.3(13) . . ? O41 C42 C43 110.5(6) . . ? C43A C42 C43 19.9(10) . . ? O43 C43 C42 115.8(9) . . ? O43A C43A C42 119.2(16) . . ? O22 N20 O21 116.3(13) . . ? O22 N20 O23 112.0(13) . . ? O21 N20 O23 112.4(15) . . ? O26 N25 O27 117.4(16) . . ? O26 N25 O28 115.3(15) . . ? O27 N25 O28 126.0(18) . . ? N25 O27 O27 165.4(9) . 3 ? O2W O1W O2W 118.3(19) 3 . ? O2W O1W O3W 138.6(9) 3 . ? O2W O1W O3W 72.0(10) . . ? O2W O1W O3W 72.0(10) 3 3 ? O2W O1W O3W 138.6(9) . 3 ? O3W O1W O3W 129.0(14) . 3 ? O2W O1W O4W 110.3(12) 3 3 ? O2W O1W O4W 98.6(12) . 3 ? O3W O1W O4W 107.1(11) . 3 ? O3W O1W O4W 44.8(9) 3 3 ? O2W O1W O4W 98.6(12) 3 . ? O2W O1W O4W 110.3(12) . . ? O3W O1W O4W 44.8(9) . . ? O3W O1W O4W 107.1(11) 3 . ? O4W O1W O4W 122(2) 3 . ? O1W O2W O3W 58.4(8) . . ? O4W O3W O1W 76.2(14) . . ? O4W O3W O2W 118.0(17) . . ? O1W O3W O2W 49.5(7) . . ? O3W O4W O1W 59.0(12) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.79 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.788 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.100 #==END data_pbcn_Ni_373K_NO3 _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA, M. KAWANO, T. Hozumi, S. Ohkoshi, M. Fujita ; _journal_name_full 'Inorg. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H20 N6 Ni O14' _chemical_formula_weight 867.33 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.000(5) _cell_length_b 20.625(4) _cell_length_c 8.5022(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4033.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale blue _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 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9211 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 'Bruker SMART CCD area detector system' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19895 _diffrn_reflns_av_R_equivalents 0.1135 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.54 _reflns_number_total 4637 _reflns_number_gt 1757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C42 to O42, C43 to O43, C41A to O44A, C41B to O44B, and C41C to O44C) converged to 75%, 25%, 32%, 39% and 29%,respectively. The occupancy of the disordered nitrate ions (N10 to O12, N10A to O12A) converged to 57%, and 43%,respectively. The thermal temperature factors of ethylene glycol groups and nitrate ions were isotropically refined because of severe disorder. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered nitrate ions and ethylene glycol groups. ; _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^)+(0.0380P)^2^+29.3559P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4637 _refine_ls_number_parameters 280 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.2268 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.035 _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 Ni1 Ni 0.5000 0.70775(6) 0.7500 0.0442(4) Uani 1 2 d S . . N1 N 0.4346(2) 0.7782(3) 0.7908(8) 0.0441(16) Uani 1 1 d . . . N2 N 0.4380(2) 0.6373(3) 0.8039(8) 0.0462(17) Uani 1 1 d . . . C10 C 0.3853(3) 0.7759(4) 0.7099(11) 0.055(2) Uani 1 1 d . . . H10 H 0.3803 0.7425 0.6378 0.066 Uiso 1 1 calc R . . C11 C 0.3413(3) 0.8204(3) 0.7274(11) 0.052(2) Uani 1 1 d . . . H11 H 0.3076 0.8161 0.6682 0.062 Uiso 1 1 calc R . . C12 C 0.3465(3) 0.8712(4) 0.8310(10) 0.047(2) Uani 1 1 d . . . C13 C 0.3982(3) 0.8732(4) 0.9177(11) 0.055(2) Uani 1 1 d . . . H13 H 0.4046 0.9064 0.9898 0.066 Uiso 1 1 calc R . . C14 C 0.4404(3) 0.8249(4) 0.8949(11) 0.057(2) Uani 1 1 d . . . H14 H 0.4739 0.8259 0.9561 0.069 Uiso 1 1 calc R . . C20 C 0.4025(3) 0.6440(4) 0.9249(10) 0.050(2) Uani 1 1 d . . . H20 H 0.4091 0.6776 0.9957 0.060 Uiso 1 1 calc R . . C21 C 0.1451(3) 1.1021(4) 0.9511(10) 0.051(2) Uani 1 1 d . . . H21 H 0.1702 1.1090 1.0352 0.061 Uiso 1 1 calc R . . C22 C 0.1537(3) 1.0508(3) 0.8495(10) 0.046(2) Uani 1 1 d . . . C23 C 0.1143(3) 1.0426(4) 0.7280(11) 0.057(2) Uani 1 1 d . . . H23 H 0.1179 1.0076 0.6597 0.068 Uiso 1 1 calc R . . C24 C 0.4301(3) 0.5863(4) 0.7086(11) 0.056(2) Uani 1 1 d . . . H24 H 0.4559 0.5803 0.6256 0.067 Uiso 1 1 calc R . . C30 C 0.2416(3) 0.8974(4) 0.8446(10) 0.052(2) Uani 1 1 d . . . H30 H 0.2346 0.8531 0.8374 0.063 Uiso 1 1 calc R . . C31 C 0.1956(3) 0.9388(4) 0.8504(10) 0.051(2) Uani 1 1 d . . . H31 H 0.1579 0.9226 0.8467 0.061 Uiso 1 1 calc R . . C32 C 0.2047(3) 1.0053(4) 0.8617(11) 0.049(2) Uani 1 1 d . . . C33 C 0.2616(3) 1.0290(3) 0.8716(10) 0.048(2) Uani 1 1 d . B . C34 C 0.3086(3) 0.9855(4) 0.8637(10) 0.047(2) Uani 1 1 d . . . C35 C 0.2988(3) 0.9190(3) 0.8492(10) 0.046(2) Uani 1 1 d . . . C40 C 0.3850(3) 1.0428(5) 0.9962(12) 0.071(3) Uani 1 1 d D . . O40 O 0.36479(19) 1.0097(3) 0.8531(7) 0.0532(15) Uani 1 1 d . A . O41 O 0.2706(2) 1.0946(2) 0.8869(7) 0.0508(14) Uani 1 1 d D . . C42 C 0.4386(7) 1.0811(9) 0.945(2) 0.081(7) Uiso 0.756(14) 1 d PD A 1 O42 O 0.4841(4) 1.0466(5) 0.8999(11) 0.089(4) Uiso 0.756(14) 1 d PD A 1 C43 C 0.437(3) 1.089(4) 0.979(5) 0.16(5) Uiso 0.244(14) 1 d PD A 2 O43 O 0.4426(14) 1.1079(16) 0.831(4) 0.097(13) Uiso 0.244(14) 1 d PD A 2 C41A C 0.290(2) 1.1297(16) 0.750(3) 0.042(9) Uiso 0.321(18) 1 d PD B 3 C44A C 0.2861(18) 1.2012(16) 0.793(5) 0.073(11) Uiso 0.321(18) 1 d PDU B 3 O44A O 0.3053(10) 1.2382(12) 0.679(3) 0.085(10) Uiso 0.321(18) 1 d PD B 3 C41B C 0.2696(15) 1.1274(13) 0.735(2) 0.063(9) Uiso 0.39(3) 1 d PD B 4 C44B C 0.2625(18) 1.1989(15) 0.776(5) 0.125(16) Uiso 0.39(3) 1 d PDU B 4 O44B O 0.2995(10) 1.2305(11) 0.866(2) 0.088(9) Uiso 0.39(3) 1 d PD B 4 C41C C 0.293(3) 1.1182(19) 0.737(5) 0.09(2) Uiso 0.29(3) 1 d PD B 5 C44C C 0.292(2) 1.1921(17) 0.727(5) 0.068(11) Uiso 0.29(3) 1 d PDU B 5 O44C O 0.335(2) 1.203(2) 0.826(5) 0.17(2) Uiso 0.29(3) 1 d PD B 5 O10 O 0.4799(3) 0.7124(4) 0.5097(8) 0.078(2) Uiso 1 1 d D . . N10 N 0.4449(8) 0.7165(9) 0.407(2) 0.083(5) Uiso 0.568(15) 1 d PD C 6 O11 O 0.4071(11) 0.6745(12) 0.398(3) 0.170(11) Uiso 0.568(15) 1 d PD C 6 O12 O 0.4393(9) 0.7631(11) 0.322(2) 0.161(9) Uiso 0.568(15) 1 d PD C 6 N10A N 0.4560(12) 0.683(2) 0.413(5) 0.167(15) Uiso 0.432(15) 1 d PD C 7 O11A O 0.4109(12) 0.6937(14) 0.324(3) 0.126(10) Uiso 0.432(15) 1 d PD C 7 O12A O 0.4732(11) 0.6272(14) 0.372(3) 0.152(11) Uiso 0.432(15) 1 d PD C 7 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 0.0182(5) 0.0285(6) 0.0858(11) 0.000 0.0057(7) 0.000 N1 0.024(3) 0.029(3) 0.079(5) -0.004(3) 0.000(3) 0.010(2) N2 0.021(3) 0.033(3) 0.084(5) -0.006(3) 0.013(3) -0.006(2) C10 0.042(4) 0.040(4) 0.082(6) -0.011(4) -0.006(4) 0.011(4) C11 0.025(3) 0.035(4) 0.096(7) -0.004(4) 0.003(4) 0.013(3) C12 0.029(4) 0.038(4) 0.074(6) -0.001(4) -0.003(4) 0.007(3) C13 0.027(3) 0.047(5) 0.092(7) -0.012(5) -0.012(4) 0.018(3) C14 0.021(3) 0.053(5) 0.098(7) -0.011(5) -0.013(4) 0.000(3) C20 0.029(4) 0.037(4) 0.084(6) -0.006(4) 0.010(4) -0.009(3) C21 0.029(4) 0.046(5) 0.078(6) -0.007(4) -0.015(4) 0.007(3) C22 0.028(3) 0.034(4) 0.076(6) 0.000(4) -0.008(4) 0.006(3) C23 0.035(4) 0.044(4) 0.092(7) -0.018(5) -0.014(5) 0.014(3) C24 0.032(4) 0.038(4) 0.097(7) -0.017(4) 0.013(4) -0.003(3) C30 0.023(3) 0.035(4) 0.099(7) -0.006(4) -0.006(4) 0.002(3) C31 0.025(3) 0.038(4) 0.089(7) -0.005(4) -0.007(4) 0.006(3) C32 0.026(3) 0.036(4) 0.085(6) -0.005(4) -0.005(4) 0.012(3) C33 0.034(4) 0.029(4) 0.080(6) -0.003(4) -0.007(4) 0.001(3) C34 0.026(3) 0.036(4) 0.078(6) -0.001(4) 0.000(4) 0.006(3) C35 0.026(3) 0.032(4) 0.081(6) -0.005(4) -0.009(4) 0.006(3) C40 0.041(5) 0.085(7) 0.087(7) -0.036(6) -0.008(5) -0.016(5) O40 0.027(2) 0.045(3) 0.088(4) -0.012(3) -0.003(3) -0.002(2) O41 0.038(3) 0.039(3) 0.076(4) -0.006(3) -0.002(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.087(5) . ? Ni1 N2 2.087(5) 3_656 ? Ni1 O10 2.097(7) . ? Ni1 O10 2.097(7) 3_656 ? Ni1 N1 2.121(5) 3_656 ? Ni1 N1 2.121(5) . ? N1 C14 1.314(10) . ? N1 C10 1.326(9) . ? N2 C20 1.321(9) . ? N2 C24 1.340(9) . ? C10 C11 1.374(9) . ? C11 C12 1.374(11) . ? C12 C13 1.400(10) . ? C12 C35 1.482(9) . ? C13 C14 1.405(10) . ? C20 C21 1.411(9) 8_655 ? C21 C22 1.381(10) . ? C21 C20 1.411(9) 8_665 ? C22 C23 1.384(11) . ? C22 C32 1.505(9) . ? C23 C24 1.372(9) 8_665 ? C24 C23 1.372(9) 8_655 ? C30 C31 1.362(9) . ? C30 C35 1.389(9) . ? C31 C32 1.390(10) . ? C32 C33 1.400(9) . ? C33 O41 1.376(8) . ? C33 C34 1.407(9) . ? C34 O40 1.389(8) . ? C34 C35 1.396(10) . ? C40 O40 1.470(10) . ? C40 C43 1.53(2) . ? C40 C42 1.528(13) . ? O41 C41A 1.447(15) . ? O41 C41B 1.459(16) . ? O41 C41C 1.465(18) . ? C42 O42 1.323(19) . ? C43 O43 1.32(2) . ? C41A C44A 1.526(19) . ? C44A O44A 1.31(2) . ? C41B C44B 1.525(18) . ? C44B O44B 1.32(2) . ? C41C C44C 1.527(19) . ? C44C O44C 1.32(2) . ? O10 N10A 1.16(5) . ? O10 N10 1.19(2) . ? N10 O12 1.212(19) . ? N10 O11 1.23(2) . ? N10A O12A 1.27(3) . ? N10A O11A 1.30(3) . ? 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 N2 Ni1 N2 91.8(3) . 3_656 ? N2 Ni1 O10 95.5(3) . . ? N2 Ni1 O10 88.2(3) 3_656 . ? N2 Ni1 O10 88.2(3) . 3_656 ? N2 Ni1 O10 95.5(3) 3_656 3_656 ? O10 Ni1 O10 174.7(4) . 3_656 ? N2 Ni1 N1 176.4(3) . 3_656 ? N2 Ni1 N1 87.5(2) 3_656 3_656 ? O10 Ni1 N1 88.0(3) . 3_656 ? O10 Ni1 N1 88.4(3) 3_656 3_656 ? N2 Ni1 N1 87.5(2) . . ? N2 Ni1 N1 176.4(3) 3_656 . ? O10 Ni1 N1 88.4(3) . . ? O10 Ni1 N1 88.0(3) 3_656 . ? N1 Ni1 N1 93.5(3) 3_656 . ? C14 N1 C10 117.6(6) . . ? C14 N1 Ni1 122.6(5) . . ? C10 N1 Ni1 119.8(5) . . ? C20 N2 C24 118.0(6) . . ? C20 N2 Ni1 121.4(5) . . ? C24 N2 Ni1 120.4(5) . . ? N1 C10 C11 123.3(8) . . ? C12 C11 C10 121.0(7) . . ? C11 C12 C13 115.7(7) . . ? C11 C12 C35 120.6(7) . . ? C13 C12 C35 123.7(7) . . ? C12 C13 C14 119.6(8) . . ? N1 C14 C13 122.8(7) . . ? N2 C20 C21 122.6(7) . 8_655 ? C22 C21 C20 118.8(7) . 8_665 ? C21 C22 C23 117.8(7) . . ? C21 C22 C32 123.1(7) . . ? C23 C22 C32 119.0(7) . . ? C24 C23 C22 119.8(8) 8_665 . ? N2 C24 C23 122.9(8) . 8_655 ? C31 C30 C35 122.3(7) . . ? C30 C31 C32 120.3(7) . . ? C31 C32 C33 119.3(6) . . ? C31 C32 C22 119.5(6) . . ? C33 C32 C22 121.0(7) . . ? O41 C33 C32 119.4(6) . . ? O41 C33 C34 121.0(6) . . ? C32 C33 C34 119.6(7) . . ? O40 C34 C35 119.8(6) . . ? O40 C34 C33 119.3(6) . . ? C35 C34 C33 120.5(6) . . ? C30 C35 C34 118.0(6) . . ? C30 C35 C12 119.0(7) . . ? C34 C35 C12 122.9(6) . . ? O40 C40 C43 117(2) . . ? O40 C40 C42 105.1(10) . . ? C43 C40 C42 13(3) . . ? C34 O40 C40 114.0(6) . . ? C33 O41 C41A 117.6(15) . . ? C33 O41 C41B 111.7(13) . . ? C41A O41 C41B 20(2) . . ? C33 O41 C41C 107.4(19) . . ? C41A O41 C41C 11(2) . . ? C41B O41 C41C 23(3) . . ? O42 C42 C40 116.3(14) . . ? O43 C43 C40 111(3) . . ? O41 C41A C44A 105(2) . . ? O44A C44A C41A 111(3) . . ? O41 C41B C44B 104(2) . . ? O44B C44B C41B 123(3) . . ? O41 C41C C44C 112(3) . . ? O44C C44C C41C 97(4) . . ? N10A O10 N10 36.5(17) . . ? N10A O10 Ni1 140.6(13) . . ? N10 O10 Ni1 149.9(9) . . ? O10 N10 O12 125(2) . . ? O10 N10 O11 118(2) . . ? O12 N10 O11 116(3) . . ? O10 N10A O12A 121(3) . . ? O10 N10A O11A 135(4) . . ? O12A N10A O11A 104(4) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.736 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.119 #==END data_pbcn_Ni_80K_H2O_again _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA, M. KAWANO, T. Hozumi, S. Ohkoshi, M. Fujita ; _journal_name_full 'Inorg. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 N6 Ni O19' _chemical_formula_weight 955.39 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.401(9) _cell_length_b 20.501(8) _cell_length_c 8.723(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4185(3) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9217 _exptl_absorpt_correction_T_max 0.9468 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21851 _diffrn_reflns_av_R_equivalents 0.1774 _diffrn_reflns_av_sigmaI/netI 0.1773 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.70 _reflns_number_total 4947 _reflns_number_gt 2003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The occupancy of the disordered ethylene glycol groups (C43 to O43 and C43A to O43A) converged to 43% and 57%, respectively. The occupancy of the disordered nitrate ions (N20 to O23, N25 to O28) converged to 40%, and 60%,respectively. The thermal temperature factors of ethylene glycol groups, nitrate ions and guest molecules were isotropically refined because of severe disorder. Hydrogen atoms were treated as a riding model. Several restraints were applied to disordered ethylene glycol groups, nitrate ions and water molecules. ; _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^)+(0.1065P)^2^+12.9297P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4947 _refine_ls_number_parameters 304 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.2517 _refine_ls_R_factor_gt 0.1165 _refine_ls_wR_factor_ref 0.3165 _refine_ls_wR_factor_gt 0.2613 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.003 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 0.5000 0.20357(7) 0.2500 0.0305(5) Uani 1 2 d S . . O1 O 0.4897(2) 0.2030(3) 0.0138(8) 0.0438(16) Uani 1 1 d . . . N1 N 0.4359(2) 0.1320(3) 0.2779(9) 0.0302(17) Uani 1 1 d . . . N2 N 0.4371(2) 0.2760(3) 0.2644(8) 0.0267(16) Uani 1 1 d . . . C10 C 0.4321(3) 0.0803(4) 0.1874(11) 0.037(2) Uani 1 1 d . . . H10 H 0.4613 0.0730 0.1139 0.045 Uiso 1 1 calc R . . C11 C 0.3866(3) 0.0359(4) 0.1954(11) 0.037(2) Uani 1 1 d . . . H11 H 0.3851 -0.0006 0.1287 0.045 Uiso 1 1 calc R . . C12 C 0.3446(3) 0.0461(4) 0.3005(10) 0.031(2) Uani 1 1 d . . . C13 C 0.3493(3) 0.0998(4) 0.3997(10) 0.030(2) Uani 1 1 d . . . H13 H 0.3214 0.1079 0.4764 0.037 Uiso 1 1 calc R . . C14 C 0.3959(3) 0.1406(4) 0.3821(11) 0.035(2) Uani 1 1 d . . . H14 H 0.3993 0.1769 0.4492 0.042 Uiso 1 1 calc R . . C20 C 0.3900(3) 0.2732(4) 0.1782(10) 0.0292(19) Uani 1 1 d . . . H20 H 0.3864 0.2377 0.1087 0.035 Uiso 1 1 calc R . . C21 C 0.3462(3) 0.3182(3) 0.1831(10) 0.0246(18) Uani 1 1 d . . . H21 H 0.3138 0.3136 0.1180 0.030 Uiso 1 1 calc R . . C22 C 0.3500(3) 0.3706(4) 0.2850(10) 0.030(2) Uani 1 1 d . . . C23 C 0.3980(3) 0.3734(4) 0.3743(11) 0.034(2) Uani 1 1 d . . . H23 H 0.4023 0.4081 0.4457 0.041 Uiso 1 1 calc R . . C24 C 0.4402(3) 0.3268(4) 0.3621(10) 0.030(2) Uani 1 1 d . . . H24 H 0.4730 0.3307 0.4256 0.036 Uiso 1 1 calc R . . C30 C 0.1911(3) -0.0157(4) 0.3161(11) 0.038(2) Uani 1 1 d . . . C31 C 0.2383(3) 0.0251(4) 0.3167(11) 0.034(2) Uani 1 1 d . . . C32 C 0.2941(3) 0.0016(4) 0.3045(11) 0.038(2) Uani 1 1 d . . . C33 C 0.3008(3) -0.0662(4) 0.2951(11) 0.036(2) Uani 1 1 d . . . H33 H 0.3382 -0.0842 0.2938 0.043 Uiso 1 1 calc R . . C34 C 0.2549(3) -0.1065(4) 0.2880(10) 0.034(2) Uani 1 1 d . . . H34 H 0.2611 -0.1521 0.2770 0.041 Uiso 1 1 calc R . . C35 C 0.1989(3) -0.0830(4) 0.2963(10) 0.031(2) Uani 1 1 d . . . O40 O 0.1365(2) 0.0095(3) 0.3122(7) 0.0329(14) Uani 1 1 d . . . C40 C 0.1200(3) 0.0439(4) 0.4483(11) 0.039(2) Uani 1 1 d . . . H40A H 0.1496 0.0765 0.4754 0.046 Uiso 1 1 calc R . . H40B H 0.1161 0.0130 0.5349 0.046 Uiso 1 1 calc R . . C41 C 0.0634(4) 0.0777(6) 0.4182(17) 0.081(5) Uani 1 1 d . . . H41A H 0.0539 0.1045 0.5092 0.097 Uiso 1 1 calc R . . H41B H 0.0686 0.1079 0.3309 0.097 Uiso 1 1 calc R . . O41 O 0.2306(2) 0.0925(2) 0.3312(7) 0.0343(15) Uani 1 1 d . A . O42 O 0.0179(3) 0.0389(5) 0.3870(11) 0.092(3) Uani 1 1 d . . . C42 C 0.2110(5) 0.1245(4) 0.1903(12) 0.050(3) Uani 1 1 d D . . C43 C 0.2481(13) 0.1845(13) 0.162(4) 0.085(13) Uiso 0.435(16) 1 d PD A 1 O43 O 0.2234(8) 0.2262(9) 0.055(2) 0.075(7) Uiso 0.435(16) 1 d PD A 1 C43A C 0.2349(8) 0.1931(7) 0.201(2) 0.037(5) Uiso 0.565(16) 1 d PD A 2 O43A O 0.2140(6) 0.2273(7) 0.3244(17) 0.078(6) Uiso 0.565(16) 1 d PD A 2 N20 N 0.1223(14) 0.2840(17) 0.285(4) 0.123(11) Uiso 0.40 1 d PDU B 3 O21 O 0.138(3) 0.282(3) 0.156(4) 0.34(3) Uiso 0.40 1 d PDU B 3 O22 O 0.0929(18) 0.331(2) 0.310(5) 0.232(17) Uiso 0.40 1 d PDU B 3 O23 O 0.160(2) 0.279(3) 0.376(5) 0.31(3) Uiso 0.40 1 d PDU B 3 N25 N 0.0888(9) 0.2435(10) 0.244(3) 0.099(6) Uiso 0.60 1 d PDU C 4 O26 O 0.1126(7) 0.2428(9) 0.132(2) 0.101(5) Uiso 0.60 1 d PDU C 4 O27 O 0.0405(12) 0.221(2) 0.246(5) 0.34(2) Uiso 0.60 1 d PDU C 4 O28 O 0.1140(18) 0.227(3) 0.355(4) 0.36(2) Uiso 0.60 1 d PDU C 4 O1W O 0.0000 0.4131(10) 0.2500 0.098(6) Uiso 0.754(14) 2 d SPU . . O2W O -0.0074(9) 0.4461(11) 0.135(3) 0.068(6) Uiso 0.377(7) 1 d PU . . O3W O 0.0162(11) 0.4195(13) 0.124(3) 0.082(8) Uiso 0.377(7) 1 d PU B . O4W O 0.0490(14) 0.3786(16) 0.252(4) 0.127(10) Uiso 0.377(7) 1 d PU . . 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 0.0084(6) 0.0166(7) 0.0665(11) 0.000 -0.0008(7) 0.000 O1 0.019(3) 0.034(3) 0.079(5) -0.010(3) -0.001(3) 0.004(3) N1 0.010(3) 0.018(3) 0.062(5) -0.006(3) -0.002(3) 0.008(2) N2 0.014(3) 0.013(3) 0.053(5) -0.002(3) -0.003(3) 0.003(2) C10 0.022(4) 0.023(4) 0.067(7) -0.018(4) 0.006(4) -0.006(3) C11 0.015(4) 0.030(5) 0.067(7) -0.010(4) 0.004(4) -0.001(3) C12 0.019(4) 0.025(4) 0.050(6) -0.006(4) 0.004(4) -0.010(3) C13 0.015(3) 0.032(5) 0.045(6) -0.006(4) 0.001(4) -0.002(3) C14 0.023(4) 0.029(5) 0.053(6) -0.001(4) 0.001(4) -0.001(4) C20 0.016(4) 0.032(5) 0.040(5) 0.000(4) 0.001(4) -0.001(3) C21 0.011(3) 0.016(4) 0.047(5) -0.005(3) -0.003(3) -0.002(3) C22 0.016(3) 0.023(4) 0.051(6) -0.007(4) 0.001(4) 0.003(3) C23 0.015(4) 0.025(4) 0.062(6) -0.006(4) 0.000(4) 0.003(3) C24 0.016(4) 0.026(4) 0.047(6) -0.004(4) -0.002(4) -0.001(3) C30 0.018(4) 0.023(5) 0.074(7) -0.006(4) -0.002(4) 0.002(3) C31 0.020(4) 0.014(4) 0.067(6) -0.003(4) 0.003(4) 0.000(3) C32 0.020(4) 0.024(4) 0.071(7) -0.005(4) 0.005(4) -0.006(3) C33 0.013(3) 0.019(4) 0.076(8) -0.008(4) 0.004(4) -0.001(3) C34 0.028(4) 0.022(4) 0.052(6) -0.006(4) 0.005(4) -0.003(3) C35 0.012(3) 0.027(4) 0.055(6) -0.009(4) -0.001(4) -0.004(3) O40 0.015(2) 0.023(3) 0.061(4) -0.010(3) -0.001(3) -0.001(2) C40 0.023(4) 0.039(5) 0.054(6) -0.015(5) 0.007(4) 0.003(4) C41 0.019(5) 0.065(8) 0.158(13) -0.054(8) 0.010(6) 0.000(5) O41 0.017(3) 0.015(3) 0.070(4) -0.008(3) -0.002(3) -0.004(2) O42 0.031(4) 0.125(8) 0.119(8) -0.008(6) -0.004(4) -0.015(4) C42 0.072(7) 0.019(5) 0.060(7) 0.000(4) -0.005(6) -0.003(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 Ni1 O1 2.074(7) . ? Ni1 O1 2.074(7) 3_655 ? Ni1 N2 2.095(6) . ? Ni1 N2 2.095(6) 3_655 ? Ni1 N1 2.111(6) . ? Ni1 N1 2.111(6) 3_655 ? N1 C14 1.317(10) . ? N1 C10 1.326(10) . ? N2 C20 1.336(9) . ? N2 C24 1.348(10) . ? C10 C11 1.402(11) . ? C11 C12 1.360(11) . ? C12 C13 1.405(11) . ? C12 C32 1.493(10) . ? C13 C14 1.383(10) . ? C20 C21 1.380(10) . ? C21 C22 1.398(10) . ? C22 C23 1.369(10) . ? C22 C35 1.490(10) 8_665 ? C23 C24 1.379(10) . ? C30 O40 1.377(9) . ? C30 C31 1.385(11) . ? C30 C35 1.403(11) . ? C31 C32 1.396(10) . ? C31 O41 1.400(9) . ? C32 C33 1.400(11) . ? C33 C34 1.357(10) . ? C34 C35 1.400(10) . ? C35 C22 1.490(10) 8_655 ? O40 C40 1.434(10) . ? C40 C41 1.520(12) . ? C41 O42 1.357(12) . ? O41 C42 1.467(11) . ? C42 C43A 1.516(15) . ? C42 C43 1.53(2) . ? C43 O43 1.39(3) . ? C43A O43A 1.37(2) . ? N20 O21 1.185(10) . ? N20 O23 1.191(10) . ? N20 O22 1.208(10) . ? O22 O4W 1.50(4) . ? N25 O26 1.124(16) . ? N25 O28 1.18(2) . ? N25 O27 1.22(2) . ? O1W O3W 1.17(3) . ? O1W O3W 1.17(3) 3 ? O1W O2W 1.22(2) . ? O1W O2W 1.22(2) 3 ? O1W O4W 1.35(3) 3 ? O1W O4W 1.35(3) . ? O2W O3W 0.78(3) . ? O3W O4W 1.59(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 179.3(3) . 3_655 ? O1 Ni1 N2 89.0(2) . . ? O1 Ni1 N2 91.5(3) 3_655 . ? O1 Ni1 N2 91.5(3) . 3_655 ? O1 Ni1 N2 89.0(2) 3_655 3_655 ? N2 Ni1 N2 89.7(3) . 3_655 ? O1 Ni1 N1 91.6(3) . . ? O1 Ni1 N1 88.0(2) 3_655 . ? N2 Ni1 N1 89.2(2) . . ? N2 Ni1 N1 176.7(3) 3_655 . ? O1 Ni1 N1 88.0(2) . 3_655 ? O1 Ni1 N1 91.6(3) 3_655 3_655 ? N2 Ni1 N1 176.7(3) . 3_655 ? N2 Ni1 N1 89.2(2) 3_655 3_655 ? N1 Ni1 N1 92.0(3) . 3_655 ? C14 N1 C10 118.0(7) . . ? C14 N1 Ni1 119.5(5) . . ? C10 N1 Ni1 122.4(6) . . ? C20 N2 C24 115.7(6) . . ? C20 N2 Ni1 121.0(5) . . ? C24 N2 Ni1 123.2(5) . . ? N1 C10 C11 122.8(8) . . ? C12 C11 C10 118.9(8) . . ? C11 C12 C13 118.6(7) . . ? C11 C12 C32 119.5(7) . . ? C13 C12 C32 121.9(7) . . ? C14 C13 C12 117.9(8) . . ? N1 C14 C13 123.8(8) . . ? N2 C20 C21 124.5(8) . . ? C20 C21 C22 119.1(7) . . ? C23 C22 C21 116.5(7) . . ? C23 C22 C35 124.5(7) . 8_665 ? C21 C22 C35 118.9(7) . 8_665 ? C22 C23 C24 121.0(8) . . ? N2 C24 C23 123.1(7) . . ? O40 C30 C31 120.9(7) . . ? O40 C30 C35 119.1(7) . . ? C31 C30 C35 119.3(7) . . ? C30 C31 C32 122.6(7) . . ? C30 C31 O41 119.6(7) . . ? C32 C31 O41 117.9(7) . . ? C31 C32 C33 116.8(7) . . ? C31 C32 C12 122.1(7) . . ? C33 C32 C12 121.1(7) . . ? C34 C33 C32 121.3(7) . . ? C33 C34 C35 121.9(7) . . ? C34 C35 C30 117.9(7) . . ? C34 C35 C22 119.7(7) . 8_655 ? C30 C35 C22 122.4(7) . 8_655 ? C30 O40 C40 114.4(6) . . ? O40 C40 C41 108.4(8) . . ? O42 C41 C40 116.9(10) . . ? C31 O41 C42 113.9(7) . . ? O41 C42 C43A 104.3(10) . . ? O41 C42 C43 108.7(14) . . ? C43A C42 C43 18.8(16) . . ? O43 C43 C42 112(2) . . ? O43A C43A C42 113.1(15) . . ? O21 N20 O23 113(2) . . ? O21 N20 O22 113(2) . . ? O23 N20 O22 112(2) . . ? N20 O22 O4W 148(4) . . ? O26 N25 O28 117(3) . . ? O26 N25 O27 118(3) . . ? O28 N25 O27 110(3) . . ? O3W O1W O3W 167(3) . 3 ? O3W O1W O2W 38.1(14) . . ? O3W O1W O2W 132(2) 3 . ? O3W O1W O2W 132(2) . 3 ? O3W O1W O2W 38.1(14) 3 3 ? O2W O1W O2W 113(3) . 3 ? O3W O1W O4W 108.9(18) . 3 ? O3W O1W O4W 78.0(17) 3 3 ? O2W O1W O4W 99.3(16) . 3 ? O2W O1W O4W 114.8(17) 3 3 ? O3W O1W O4W 78.0(17) . . ? O3W O1W O4W 108.9(18) 3 . ? O2W O1W O4W 114.8(17) . . ? O2W O1W O4W 99.3(16) 3 . ? O4W O1W O4W 117(3) 3 . ? O3W O2W O1W 67(3) . . ? O2W O3W O1W 75(3) . . ? O2W O3W O4W 128(4) . . ? O1W O3W O4W 55.9(16) . . ? O1W O4W O22 157(3) . . ? O1W O4W O3W 46.1(14) . . ? O22 O4W O3W 155(3) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 0.849 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.142 #==END data_cc _publ_contact_author 'Masaki Kawano' _publ_contact_author_email 'mkawano@appchem.t.u-tokyo.ac.jp' loop_ _publ_author_name ; K. TAKAOKA. M. KAWANO, M. TOMINAGA. M. FUJITA ; _journal_name_full 'Angew. Chem.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H24 Co N6 O13' _chemical_formula_weight 795.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.8603(19) _cell_length_b 15.6965(18) _cell_length_c 15.2546(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.062(2) _cell_angle_gamma 90.00 _cell_volume 3741.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(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 'Bruker SMART CCD area detector system' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10741 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.82 _reflns_number_total 6797 _reflns_number_gt 6341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XSHELL' _computing_publication_material 'Bruker SHELXTL' _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. The thermal temperature factors of all atoms were anisotropically refined. Hydrogen atoms were treated as a riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+48.0830P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(3) _refine_ls_number_reflns 6797 _refine_ls_number_parameters 506 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2056 _refine_ls_wR_factor_gt 0.2029 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.005 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 0.79826(6) 0.47923(4) 0.46936(7) 0.00869(18) Uani 1 1 d . . . O1 O 0.8160(4) 0.4882(3) 0.3398(4) 0.0138(11) Uani 1 1 d . . . O2 O 0.7815(4) 0.4784(3) 0.5992(4) 0.0173(12) Uani 1 1 d . . . N1 N 0.8050(5) 0.3420(3) 0.4674(5) 0.0130(10) Uani 1 1 d . . . N2 N 0.7960(5) 0.6163(3) 0.4724(5) 0.0120(9) Uani 1 1 d . . . N3 N 0.6616(4) 0.4742(3) 0.3949(5) 0.0102(13) Uani 1 1 d . . . N4 N 0.9350(5) 0.4832(4) 0.5464(5) 0.0147(14) Uani 1 1 d . . . C10 C 0.7571(4) 0.2972(4) 0.3903(5) 0.0110(13) Uani 1 1 d . . . H10 H 0.7229 0.3279 0.3354 0.013 Uiso 1 1 calc R . . C11 C 0.8559(5) 0.2978(4) 0.5430(5) 0.0143(14) Uani 1 1 d . . . H11 H 0.8927 0.3280 0.5969 0.017 Uiso 1 1 calc R . . C12 C 0.7548(5) 1.2090(5) 0.3864(6) 0.0172(15) Uani 1 1 d . . . H12 H 0.7189 1.1804 0.3307 0.021 Uiso 1 1 calc R . . C13 C 0.8055(5) 1.1632(3) 0.4647(6) 0.0120(12) Uani 1 1 d . . . C14 C 0.8564(5) 1.2097(4) 0.5448(5) 0.0130(14) Uani 1 1 d . . . H14 H 0.8912 1.1804 0.6004 0.016 Uiso 1 1 calc R . . C15 C 0.8046(6) 1.0680(3) 0.4654(7) 0.0139(13) Uani 1 1 d . . . C20 C 0.8591(5) 0.6607(5) 0.4606(5) 0.0154(14) Uani 1 1 d . . . H20 H 0.9038 0.6297 0.4515 0.019 Uiso 1 1 calc R . . C21 C 0.7322(5) 0.6622(4) 0.4823(6) 0.0172(15) Uani 1 1 d . . . H21 H 0.6856 0.6325 0.4887 0.021 Uiso 1 1 calc R . . C22 C 0.7312(5) 0.7511(4) 0.4835(6) 0.0186(16) Uani 1 1 d . . . H22 H 0.6853 0.7809 0.4915 0.022 Uiso 1 1 calc R . . C23 C 0.7988(6) 0.7956(3) 0.4727(7) 0.0136(10) Uani 1 1 d . . . C24 C 0.8636(5) 0.7480(5) 0.4609(5) 0.0162(15) Uani 1 1 d . . . H24 H 0.9106 0.7757 0.4531 0.019 Uiso 1 1 calc R . . C25 C 0.8012(7) 0.8902(3) 0.4729(7) 0.0152(11) Uani 1 1 d . . . C26 C 0.7269(6) 0.9368(4) 0.4264(6) 0.0174(16) Uani 1 1 d . . . H26 H 0.6742 0.9075 0.3969 0.021 Uiso 1 1 calc R . . C27 C 0.7284(6) 1.0244(4) 0.4224(7) 0.0179(17) Uani 1 1 d . . . H27 H 0.6770 1.0550 0.3901 0.022 Uiso 1 1 calc R . . C28 C 0.8797(6) 1.0225(4) 0.5122(6) 0.0149(16) Uani 1 1 d . . . H28 H 0.9320 1.0519 0.5431 0.018 Uiso 1 1 calc R . . C29 C 0.8777(5) 0.9325(4) 0.5135(5) 0.0132(14) Uani 1 1 d . . . H29 H 0.9293 0.9013 0.5425 0.016 Uiso 1 1 calc R . . C30 C 0.6233(6) 0.5243(4) 0.3183(6) 0.0170(16) Uani 1 1 d . . . H30 H 0.6582 0.5578 0.2951 0.020 Uiso 1 1 calc R . . C31 C 1.5349(5) 0.4713(4) 0.7721(6) 0.0154(15) Uani 1 1 d . . . H31 H 1.5100 0.4341 0.7198 0.018 Uiso 1 1 calc R . . C32 C 1.4822(5) 0.5232(4) 0.8044(6) 0.0134(15) Uani 1 1 d . . . C33 C 1.5235(5) 0.5758(5) 0.8811(6) 0.0173(15) Uani 1 1 d . . . H33 H 1.4907 0.6129 0.9036 0.021 Uiso 1 1 calc R . . C34 C 1.6115(5) 0.5752(5) 0.9252(6) 0.0157(15) Uani 1 1 d . . . H34 H 1.6377 0.6107 0.9788 0.019 Uiso 1 1 calc R . . C40 C 0.9723(5) 0.5319(5) 0.6220(6) 0.0173(16) Uani 1 1 d . . . H40 H 0.9371 0.5613 0.6482 0.021 Uiso 1 1 calc R . . C41 C 1.0597(5) 0.5416(5) 0.6640(6) 0.0200(17) Uani 1 1 d . . . H41 H 1.0828 0.5782 0.7172 0.024 Uiso 1 1 calc R . . C42 C 1.1142(5) 0.4995(4) 0.6309(5) 0.0119(13) Uani 1 1 d . . . C43 C 1.0758(4) 0.4473(4) 0.5523(5) 0.0110(13) Uani 1 1 d . . . H43 H 1.1100 0.4160 0.5263 0.013 Uiso 1 1 calc R . . C44 C 0.9876(5) 0.4416(4) 0.5127(5) 0.0141(14) Uani 1 1 d . . . H44 H 0.9626 0.4063 0.4587 0.017 Uiso 1 1 calc R . . C45 C 1.2098(4) 0.5055(5) 0.6747(5) 0.0133(13) Uani 1 1 d . . . C46 C 1.2481(5) 0.5838(4) 0.7109(6) 0.0159(14) Uani 1 1 d . . . H46 H 1.2137 0.6327 0.7064 0.019 Uiso 1 1 calc R . . C47 C 1.3378(4) 0.5894(4) 0.7539(5) 0.0129(14) Uani 1 1 d . . . H47 H 1.3639 0.6421 0.7796 0.016 Uiso 1 1 calc R . . C48 C 1.3891(5) 0.5175(5) 0.7592(6) 0.0162(15) Uani 1 1 d . . . C49 C 1.3475(5) 0.4406(5) 0.7212(5) 0.0164(14) Uani 1 1 d . . . H49 H 1.3810 0.3913 0.7236 0.020 Uiso 1 1 calc R . . C50 C 1.2607(5) 0.4349(4) 0.6812(5) 0.0157(15) Uani 1 1 d . . . H50 H 1.2347 0.3817 0.6575 0.019 Uiso 1 1 calc R . . N10 N 0.5975(4) 0.6995(4) 0.1785(5) 0.0254(14) Uani 1 1 d . . . O10 O 0.6641(4) 0.7263(4) 0.2383(4) 0.0329(13) Uani 1 1 d . . . O11 O 0.5957(5) 0.6457(4) 0.1167(4) 0.0371(15) Uani 1 1 d . . . O12 O 0.5255(4) 0.7228(4) 0.1795(6) 0.0471(19) Uani 1 1 d . . . N11 N 0.5888(4) 0.2668(4) 0.1758(4) 0.0223(13) Uani 1 1 d . . . O13 O 0.6469(5) 0.2580(4) 0.1441(6) 0.0437(19) Uani 1 1 d . . . O14 O 0.5570(4) 0.2026(3) 0.2002(4) 0.0289(12) Uani 1 1 d . . . O15 O 0.5642(4) 0.3410(3) 0.1860(4) 0.0298(12) Uani 1 1 d . . . O1W O 0.3099(3) 0.1354(3) 0.2384(3) 0.0153(10) Uani 1 1 d . . . O2W O 0.6305(4) 0.4616(4) 0.1003(5) 0.0366(14) Uani 1 1 d . . . C3M C 0.5386(7) 0.1828(8) 0.4006(9) 0.054(3) Uani 1 1 d . . . O3M O 0.4700(4) 0.2150(4) 0.3166(5) 0.0315(14) Uani 1 1 d . . . C4M C 0.3317(10) 0.8274(13) 0.2133(9) 0.110(8) Uani 1 1 d . . . O4M O 0.3913(8) 0.8718(5) 0.2746(7) 0.076(3) Uani 1 1 d . . . C5M C 0.5052(7) 0.7192(7) 0.4065(9) 0.051(3) Uani 1 1 d . . . O5M O 0.5227(10) 0.7858(5) 0.3521(10) 0.109(5) Uani 1 1 d . . . 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 0.0067(3) 0.0074(3) 0.0112(3) 0.0016(4) 0.0024(3) 0.0002(4) O1 0.022(3) 0.010(2) 0.013(3) -0.0011(17) 0.011(2) 0.0029(18) O2 0.010(3) 0.011(2) 0.030(3) -0.0027(19) 0.006(2) 0.0022(17) N1 0.011(3) 0.011(2) 0.014(2) 0.004(3) 0.0016(19) -0.001(2) N2 0.016(2) 0.0116(19) 0.010(2) -0.002(3) 0.0065(17) 0.006(3) N3 0.009(3) 0.005(2) 0.012(3) 0.0008(19) -0.001(3) 0.0026(18) N4 0.013(4) 0.015(3) 0.015(3) 0.001(2) 0.005(3) 0.004(2) C10 0.008(3) 0.010(3) 0.011(3) 0.000(2) -0.001(3) -0.002(2) C11 0.008(3) 0.017(3) 0.017(3) 0.002(3) 0.004(3) -0.003(2) C12 0.019(4) 0.014(3) 0.017(4) -0.007(3) 0.005(3) -0.001(3) C13 0.014(3) 0.009(2) 0.018(3) -0.004(3) 0.011(2) -0.003(3) C14 0.016(3) 0.010(3) 0.012(3) 0.001(2) 0.005(3) 0.001(2) C15 0.020(3) 0.009(2) 0.015(3) 0.003(3) 0.009(2) 0.000(3) C20 0.016(4) 0.018(3) 0.013(4) -0.005(3) 0.006(3) 0.003(3) C21 0.017(4) 0.012(3) 0.024(4) -0.003(3) 0.011(3) 0.001(3) C22 0.023(4) 0.010(3) 0.027(4) 0.000(3) 0.015(4) -0.001(3) C23 0.018(3) 0.011(2) 0.011(3) 0.000(3) 0.005(2) 0.004(3) C24 0.012(4) 0.023(4) 0.017(4) 0.002(3) 0.010(3) -0.005(3) C25 0.022(3) 0.010(2) 0.016(3) 0.003(3) 0.010(2) 0.012(3) C26 0.021(4) 0.012(3) 0.022(4) -0.003(3) 0.011(3) -0.001(3) C27 0.019(4) 0.010(3) 0.027(5) -0.002(3) 0.011(4) 0.002(3) C28 0.017(4) 0.015(3) 0.012(4) 0.001(2) 0.005(3) 0.000(3) C29 0.011(3) 0.011(3) 0.014(4) 0.002(3) 0.001(3) 0.004(3) C30 0.022(4) 0.009(3) 0.019(4) 0.000(3) 0.006(4) 0.000(3) C31 0.019(4) 0.013(3) 0.015(4) 0.002(2) 0.009(3) 0.003(3) C32 0.012(3) 0.007(3) 0.022(4) 0.003(2) 0.007(3) 0.001(2) C33 0.012(3) 0.018(3) 0.023(4) 0.000(3) 0.008(3) 0.001(3) C34 0.011(3) 0.017(3) 0.018(4) -0.006(3) 0.004(3) -0.004(2) C40 0.012(4) 0.023(3) 0.017(4) -0.008(3) 0.005(3) 0.004(3) C41 0.008(4) 0.017(3) 0.023(4) -0.011(3) -0.008(3) 0.000(3) C42 0.011(3) 0.011(3) 0.010(3) -0.001(2) 0.000(3) -0.004(3) C43 0.010(3) 0.014(3) 0.010(3) 0.001(2) 0.003(3) 0.001(2) C44 0.015(4) 0.011(3) 0.012(3) -0.006(2) 0.002(3) -0.001(2) C45 0.007(3) 0.018(3) 0.012(3) 0.000(3) 0.001(3) -0.004(3) C46 0.011(3) 0.014(3) 0.019(4) 0.003(3) 0.002(3) 0.002(3) C47 0.004(3) 0.011(3) 0.017(3) -0.004(2) -0.003(3) -0.003(2) C48 0.014(4) 0.021(4) 0.014(3) 0.000(3) 0.005(3) -0.001(3) C49 0.014(3) 0.020(3) 0.015(3) 0.000(3) 0.005(3) 0.005(3) C50 0.025(4) 0.013(3) 0.013(3) -0.002(2) 0.012(3) 0.001(3) N10 0.028(4) 0.021(3) 0.026(3) 0.007(2) 0.008(3) 0.007(3) O10 0.032(3) 0.027(3) 0.037(3) -0.007(2) 0.010(3) -0.012(2) O11 0.058(4) 0.027(3) 0.031(3) -0.010(2) 0.023(3) -0.008(3) O12 0.033(4) 0.018(3) 0.092(6) -0.003(3) 0.026(4) 0.006(2) N11 0.017(3) 0.028(3) 0.018(3) -0.005(2) 0.003(3) 0.001(2) O13 0.058(5) 0.030(3) 0.067(5) 0.013(3) 0.051(4) 0.016(3) O14 0.029(3) 0.023(3) 0.032(3) -0.001(2) 0.009(3) -0.006(2) O15 0.037(3) 0.023(3) 0.034(3) 0.002(2) 0.017(3) 0.007(2) O1W 0.026(3) 0.011(2) 0.010(2) 0.0009(17) 0.008(2) 0.0034(18) O2W 0.037(3) 0.028(3) 0.052(4) -0.001(3) 0.025(3) 0.000(2) C3M 0.030(5) 0.066(7) 0.074(8) 0.011(6) 0.030(6) 0.008(5) O3M 0.027(3) 0.024(3) 0.052(4) -0.002(3) 0.025(3) 0.000(2) C4M 0.074(10) 0.180(17) 0.036(6) 0.063(9) -0.026(6) -0.094(11) O4M 0.128(9) 0.043(4) 0.083(7) 0.003(4) 0.071(7) 0.012(5) C5M 0.045(6) 0.042(5) 0.073(8) -0.016(5) 0.029(6) -0.006(4) O5M 0.205(15) 0.035(4) 0.165(12) -0.013(5) 0.158(12) -0.007(6) _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 O2 2.102(6) . ? Co1 O1 2.112(5) . ? Co1 N2 2.153(4) . ? Co1 N4 2.160(7) . ? Co1 N3 2.154(7) . ? Co1 N1 2.158(5) . ? N1 C11 1.343(10) . ? N1 C10 1.348(10) . ? N2 C20 1.339(11) . ? N2 C21 1.349(10) . ? N3 C30 1.355(10) . ? N3 C34 1.350(10) 2_464 ? N4 C40 1.329(11) . ? N4 C44 1.348(10) . ? C10 C12 1.386(10) 1_545 ? C11 C14 1.384(10) 1_545 ? C12 C13 1.381(12) . ? C12 C10 1.386(10) 1_565 ? C13 C14 1.404(11) . ? C13 C15 1.495(7) . ? C14 C11 1.384(10) 1_565 ? C15 C27 1.384(13) . ? C15 C28 1.394(12) . ? C20 C24 1.373(10) . ? C21 C22 1.396(10) . ? C22 C23 1.397(11) . ? C23 C24 1.390(11) . ? C23 C25 1.485(7) . ? C25 C29 1.375(12) . ? C25 C26 1.393(12) . ? C26 C27 1.378(10) . ? C28 C29 1.413(10) . ? C30 C31 1.391(13) 2_464 ? C31 C30 1.391(13) 2_665 ? C31 C32 1.422(10) . ? C32 C33 1.388(11) . ? C32 C48 1.461(11) . ? C33 C34 1.380(11) . ? C34 N3 1.350(10) 2_665 ? C40 C41 1.377(11) . ? C41 C42 1.372(11) . ? C42 C43 1.394(9) . ? C42 C45 1.498(10) . ? C43 C44 1.382(10) . ? C45 C50 1.382(10) . ? C45 C46 1.401(10) . ? C46 C47 1.408(10) . ? C47 C48 1.406(10) . ? C48 C49 1.406(11) . ? C49 C50 1.362(11) . ? N10 O10 1.226(9) . ? N10 O11 1.257(9) . ? N10 O12 1.272(9) . ? N11 O13 1.252(9) . ? N11 O14 1.262(8) . ? N11 O15 1.266(8) . ? C3M O3M 1.457(14) . ? C4M O4M 1.289(16) . ? C5M O5M 1.432(15) . ? 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 O2 Co1 O1 176.52(16) . . ? O2 Co1 N2 88.7(2) . . ? O1 Co1 N2 87.9(2) . . ? O2 Co1 N4 88.9(3) . . ? O1 Co1 N4 90.5(3) . . ? N2 Co1 N4 89.1(3) . . ? O2 Co1 N3 90.1(2) . . ? O1 Co1 N3 90.5(2) . . ? N2 Co1 N3 91.4(3) . . ? N4 Co1 N3 178.9(3) . . ? O2 Co1 N1 91.9(2) . . ? O1 Co1 N1 91.5(2) . . ? N2 Co1 N1 178.1(3) . . ? N4 Co1 N1 89.1(3) . . ? N3 Co1 N1 90.4(2) . . ? C11 N1 C10 117.5(5) . . ? C11 N1 Co1 121.5(5) . . ? C10 N1 Co1 121.0(5) . . ? C20 N2 C21 116.4(5) . . ? C20 N2 Co1 119.7(5) . . ? C21 N2 Co1 123.8(5) . . ? C30 N3 C34 118.2(7) . 2_464 ? C30 N3 Co1 120.2(6) . . ? C34 N3 Co1 121.6(5) 2_464 . ? C40 N4 C44 116.4(7) . . ? C40 N4 Co1 123.3(5) . . ? C44 N4 Co1 120.0(6) . . ? N1 C10 C12 123.8(7) . 1_545 ? N1 C11 C14 121.9(7) . 1_545 ? C13 C12 C10 119.0(7) . 1_565 ? C12 C13 C14 117.4(5) . . ? C12 C13 C15 121.4(8) . . ? C14 C13 C15 121.1(8) . . ? C11 C14 C13 120.3(7) 1_565 . ? C27 C15 C28 119.5(5) . . ? C27 C15 C13 120.1(8) . . ? C28 C15 C13 120.4(8) . . ? N2 C20 C24 124.3(7) . . ? N2 C21 C22 123.3(7) . . ? C23 C22 C21 118.9(7) . . ? C22 C23 C24 117.5(5) . . ? C22 C23 C25 121.5(8) . . ? C24 C23 C25 121.0(8) . . ? C20 C24 C23 119.5(7) . . ? C29 C25 C26 119.2(5) . . ? C29 C25 C23 120.3(8) . . ? C26 C25 C23 120.3(9) . . ? C27 C26 C25 121.3(8) . . ? C26 C27 C15 120.1(8) . . ? C15 C28 C29 119.9(7) . . ? C25 C29 C28 120.0(7) . . ? N3 C30 C31 122.6(7) . 2_464 ? C30 C31 C32 119.1(7) 2_665 . ? C33 C32 C31 116.9(7) . . ? C33 C32 C48 123.0(7) . . ? C31 C32 C48 120.1(7) . . ? C34 C33 C32 120.9(7) . . ? N3 C34 C33 122.2(7) 2_665 . ? N4 C40 C41 122.8(7) . . ? C42 C41 C40 121.5(7) . . ? C41 C42 C43 116.1(7) . . ? C41 C42 C45 124.2(6) . . ? C43 C42 C45 119.6(7) . . ? C42 C43 C44 119.3(7) . . ? N4 C44 C43 123.7(7) . . ? C50 C45 C46 119.5(7) . . ? C50 C45 C42 121.1(7) . . ? C46 C45 C42 119.3(7) . . ? C47 C46 C45 119.6(6) . . ? C46 C47 C48 120.4(6) . . ? C49 C48 C47 117.7(7) . . ? C49 C48 C32 121.9(7) . . ? C47 C48 C32 120.4(6) . . ? C50 C49 C48 121.8(7) . . ? C49 C50 C45 120.9(7) . . ? O10 N10 O11 123.0(7) . . ? O10 N10 O12 120.3(7) . . ? O11 N10 O12 116.6(7) . . ? O13 N11 O14 120.4(6) . . ? O13 N11 O15 119.3(7) . . ? O14 N11 O15 120.3(6) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 28.82 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 2.485 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.154