data_704f1m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _symmetry_space_group_name_Hall '-C 2yc' _chemical_formula_moiety 'C36 H36 Cu N12 O6, 2(F), 2(H2 O), 2(O)' _chemical_formula_sum 'C36 H44 Cu F2 N12 O10' _chemical_formula_weight 906.37 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.341(2) _cell_length_b 10.2257(9) _cell_length_c 19.3694(18) _cell_angle_alpha 90.00 _cell_angle_beta 118.396(2) _cell_angle_gamma 90.00 _cell_volume 4066.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8460 _exptl_absorpt_correction_T_max 0.9639 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Apex II' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9867 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3561 _reflns_number_gt 3125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.3, ORTEP3v2' _computing_publication_material 'SHELXTL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+9.7135P] 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 3561 _refine_ls_number_parameters 293 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 -0.34561(6) 0.2500 0.0306(2) Uani 1 2 d S . . F1 F 0.07972(13) 0.5456(3) 0.22601(16) 0.0591(7) Uani 1 1 d . . . N1 N 0.51280(15) -0.3445(3) 0.15398(18) 0.0348(7) Uani 1 1 d . . . C2 C 0.5543(2) -0.4273(4) 0.1479(2) 0.0427(10) Uani 1 1 d . . . H2 H 0.5753 -0.4897 0.1868 0.051 Uiso 1 1 calc R . . C3 C 0.5666(2) -0.4226(5) 0.0853(3) 0.0492(12) Uani 1 1 d . . . H3 H 0.5964 -0.4799 0.0826 0.059 Uiso 1 1 calc R . . C4 C 0.5346(2) -0.3323(4) 0.0268(2) 0.0429(10) Uani 1 1 d . . . H4 H 0.5426 -0.3284 -0.0158 0.051 Uiso 1 1 calc R . . C5 C 0.49068(18) -0.2478(4) 0.0315(2) 0.0327(9) Uani 1 1 d . . . C6 C 0.48111(18) -0.2562(4) 0.0971(2) 0.0348(9) Uani 1 1 d . . . H6 H 0.4520 -0.1992 0.1015 0.042 Uiso 1 1 calc R . . N7 N 0.45821(17) -0.1601(3) -0.03026(19) 0.0412(8) Uani 1 1 d . . . H7 H 0.4717 -0.1562 -0.0646 0.049 Uiso 1 1 calc R . . C8 C 0.40734(19) -0.0796(4) -0.0425(2) 0.0355(9) Uani 1 1 d . . . O9 O 0.38688(14) -0.0692(3) 0.00563(16) 0.0451(7) Uani 1 1 d . . . N10 N 0.38037(17) -0.0160(3) -0.11217(19) 0.0408(8) Uani 1 1 d . . . H10 H 0.3992 -0.0222 -0.1409 0.049 Uiso 1 1 calc R . . C11 C 0.32284(19) 0.0600(4) -0.1403(2) 0.0348(9) Uani 1 1 d . . . C12 C 0.2728(2) 0.0361(4) -0.2148(2) 0.0432(10) Uani 1 1 d . . . H12 H 0.2771 -0.0284 -0.2459 0.052 Uiso 1 1 calc R . . C13 C 0.2164(2) 0.1086(4) -0.2426(2) 0.0454(11) Uani 1 1 d . . . H13 H 0.1828 0.0924 -0.2929 0.054 Uiso 1 1 calc R . . C14 C 0.2086(2) 0.2047(4) -0.1978(2) 0.0411(10) Uani 1 1 d . . . H14 H 0.1700 0.2522 -0.2171 0.049 Uiso 1 1 calc R . . C15 C 0.25972(19) 0.2292(4) -0.1227(2) 0.0351(9) Uani 1 1 d . . . C16 C 0.3165(2) 0.1570(4) -0.0941(2) 0.0391(10) Uani 1 1 d . . . H16 H 0.3503 0.1731 -0.0440 0.047 Uiso 1 1 calc R . . N17 N 0.24925(16) 0.3273(3) -0.0787(2) 0.0447(9) Uani 1 1 d . . . H17 H 0.2093 0.3461 -0.0926 0.054 Uiso 1 1 calc R . . C18 C 0.2951(2) 0.3954(4) -0.0168(2) 0.0389(10) Uani 1 1 d . . . O19 O 0.35322(15) 0.3780(4) 0.0115(2) 0.0678(11) Uani 1 1 d . . . N20 N 0.26921(16) 0.4876(3) 0.0114(2) 0.0433(9) Uani 1 1 d . . . H20 H 0.2274 0.4920 -0.0114 0.052 Uiso 1 1 calc R . . C21 C 0.30242(18) 0.5754(4) 0.0729(2) 0.0334(9) Uani 1 1 d . . . C22 C 0.2669(2) 0.6716(4) 0.0858(3) 0.0425(10) Uani 1 1 d . . . H22 H 0.2221 0.6773 0.0539 0.051 Uiso 1 1 calc R . . C23 C 0.2984(2) 0.7581(4) 0.1459(3) 0.0481(11) Uani 1 1 d . . . H23 H 0.2749 0.8228 0.1553 0.058 Uiso 1 1 calc R . . C24 C 0.36483(19) 0.7496(4) 0.1928(2) 0.0393(10) Uani 1 1 d . . . H24 H 0.3857 0.8086 0.2338 0.047 Uiso 1 1 calc R . . N25 N 0.39978(15) 0.6587(3) 0.18039(18) 0.0328(7) Uani 1 1 d . . . C26 C 0.36981(18) 0.5724(4) 0.1223(2) 0.0324(9) Uani 1 1 d . . . H26 H 0.3945 0.5084 0.1145 0.039 Uiso 1 1 calc R . . O27 O 0.5000 -0.1109(5) 0.2500 0.0512(12) Uani 1 2 d S . . O28 O 0.5000 -0.5777(5) 0.2500 0.0553(13) Uani 1 2 d S . . O29 O 0.37914(18) 0.0803(4) 0.1231(2) 0.0659(10) Uani 1 1 d D . . O30 O 0.99571(17) 0.7235(3) 0.14790(19) 0.0603(9) Uani 1 1 d . . . H27 H 0.519(3) -0.068(5) 0.237(3) 0.064(17) Uiso 1 1 d . . . H28 H 0.499(2) -0.629(5) 0.283(3) 0.055(15) Uiso 1 1 d . . . H29A H 0.389(2) 0.012(3) 0.104(3) 0.054(14) Uiso 1 1 d D . . H29B H 0.393(3) 0.069(7) 0.1736(11) 0.11(3) Uiso 1 1 d 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 Cu1 0.0295(4) 0.0403(4) 0.0236(4) 0.000 0.0138(3) 0.000 F1 0.0661(18) 0.0616(17) 0.0649(17) 0.0047(14) 0.0435(15) 0.0015(14) N1 0.0362(18) 0.0415(18) 0.0294(16) 0.0045(15) 0.0179(14) 0.0061(15) C2 0.045(2) 0.049(3) 0.038(2) 0.0133(19) 0.022(2) 0.017(2) C3 0.051(3) 0.061(3) 0.046(3) 0.008(2) 0.033(2) 0.023(2) C4 0.046(2) 0.057(3) 0.033(2) 0.006(2) 0.0247(19) 0.011(2) C5 0.031(2) 0.038(2) 0.029(2) 0.0001(16) 0.0145(17) 0.0006(17) C6 0.035(2) 0.039(2) 0.031(2) 0.0032(17) 0.0152(17) 0.0094(18) N7 0.048(2) 0.052(2) 0.0315(18) 0.0124(16) 0.0259(16) 0.0151(17) C8 0.038(2) 0.037(2) 0.030(2) -0.0028(17) 0.0154(18) 0.0001(18) O9 0.0472(17) 0.0582(19) 0.0341(16) 0.0097(13) 0.0227(14) 0.0191(14) N10 0.049(2) 0.046(2) 0.0321(18) 0.0112(15) 0.0224(16) 0.0170(17) C11 0.038(2) 0.035(2) 0.032(2) 0.0065(17) 0.0167(18) 0.0029(17) C12 0.055(3) 0.042(2) 0.031(2) -0.0042(18) 0.018(2) 0.000(2) C13 0.042(2) 0.053(3) 0.029(2) -0.005(2) 0.0068(19) -0.002(2) C14 0.035(2) 0.043(2) 0.036(2) 0.0018(19) 0.0100(19) -0.0002(19) C15 0.036(2) 0.034(2) 0.033(2) -0.0051(17) 0.0143(18) -0.0047(18) C16 0.037(2) 0.043(2) 0.031(2) -0.0021(18) 0.0112(18) 0.0019(19) N17 0.0313(18) 0.048(2) 0.043(2) -0.0129(17) 0.0082(16) 0.0042(16) C18 0.036(2) 0.046(2) 0.035(2) -0.0043(19) 0.0168(19) -0.0022(19) O19 0.0355(18) 0.092(3) 0.071(2) -0.047(2) 0.0218(17) -0.0070(17) N20 0.0271(17) 0.049(2) 0.044(2) -0.0110(17) 0.0088(16) 0.0030(16) C21 0.034(2) 0.033(2) 0.036(2) -0.0003(16) 0.0186(18) -0.0004(17) C22 0.033(2) 0.047(2) 0.046(2) -0.002(2) 0.0172(19) 0.0045(19) C23 0.040(2) 0.050(3) 0.057(3) -0.012(2) 0.025(2) 0.006(2) C24 0.037(2) 0.044(2) 0.041(2) -0.0107(19) 0.0220(19) -0.0025(19) N25 0.0308(17) 0.0367(18) 0.0298(16) -0.0034(14) 0.0135(14) -0.0016(15) C26 0.030(2) 0.032(2) 0.034(2) -0.0006(16) 0.0137(17) 0.0040(16) O27 0.057(3) 0.043(3) 0.071(3) 0.000 0.044(3) 0.000 O28 0.081(4) 0.040(3) 0.048(3) 0.000 0.033(3) 0.000 O29 0.062(2) 0.078(3) 0.056(2) 0.000(2) 0.0265(19) 0.033(2) O30 0.082(2) 0.062(2) 0.0484(19) 0.0027(16) 0.0395(18) 0.0002(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.019(3) . ? Cu1 N1 2.019(3) 2_655 ? Cu1 N25 2.072(3) 1_545 ? Cu1 N25 2.072(3) 2_645 ? Cu1 O28 2.374(5) . ? Cu1 O27 2.401(5) . ? N1 C2 1.333(5) . ? N1 C6 1.342(5) . ? C2 C3 1.374(6) . ? C2 H2 0.9300 . ? C3 C4 1.374(6) . ? C3 H3 0.9300 . ? C4 C5 1.377(5) . ? C4 H4 0.9300 . ? C5 C6 1.394(5) . ? C5 N7 1.395(5) . ? C6 H6 0.9300 . ? N7 C8 1.370(5) . ? N7 H7 0.8600 . ? C8 O9 1.237(5) 1 ? C8 O9 1.237(5) . ? C8 N10 1.353(5) . ? O9 O9 0.000(6) 1 ? N10 C11 1.418(5) . ? N10 H10 0.8600 . ? C11 C12 1.379(5) . ? C11 C16 1.390(6) . ? C12 C13 1.378(6) . ? C12 H12 0.9300 . ? C13 C14 1.380(6) . ? C13 H13 0.9300 . ? C14 C15 1.396(5) . ? C14 H14 0.9300 . ? C15 C16 1.382(6) . ? C15 N17 1.411(5) . ? C16 H16 0.9300 . ? N17 C18 1.359(5) . ? N17 H17 0.8600 . ? C18 O19 1.211(5) . ? C18 N20 1.366(5) . ? N20 C21 1.395(5) . ? N20 H20 0.8600 . ? C21 C22 1.385(6) . ? C21 C26 1.400(5) . ? C22 C23 1.365(6) . ? C22 H22 0.9300 . ? C23 C24 1.378(6) . ? C23 H23 0.9300 . ? C24 N25 1.332(5) . ? C24 H24 0.9300 . ? N25 C26 1.336(5) . ? N25 Cu1 2.072(3) 1_565 ? C26 H26 0.9300 . ? O27 H27 0.75(5) . ? O28 H28 0.83(4) . ? O29 H29A 0.876(10) . ? O29 H29B 0.880(10) . ? 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 N1 Cu1 N1 179.37(19) . 2_655 ? N1 Cu1 N25 90.94(13) . 1_545 ? N1 Cu1 N25 89.05(13) 2_655 1_545 ? N1 Cu1 N25 89.05(13) . 2_645 ? N1 Cu1 N25 90.93(13) 2_655 2_645 ? N25 Cu1 N25 177.58(18) 1_545 2_645 ? N1 Cu1 O28 90.32(9) . . ? N1 Cu1 O28 90.32(9) 2_655 . ? N25 Cu1 O28 91.21(9) 1_545 . ? N25 Cu1 O28 91.21(9) 2_645 . ? N1 Cu1 O27 89.68(9) . . ? N1 Cu1 O27 89.68(9) 2_655 . ? N25 Cu1 O27 88.79(9) 1_545 . ? N25 Cu1 O27 88.79(9) 2_645 . ? O28 Cu1 O27 180.0 . . ? C2 N1 C6 119.6(3) . . ? C2 N1 Cu1 120.7(3) . . ? C6 N1 Cu1 119.7(3) . . ? N1 C2 C3 121.4(4) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 117.9(4) . . ? C4 C5 N7 117.7(3) . . ? C6 C5 N7 124.3(3) . . ? N1 C6 C5 121.7(3) . . ? N1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C8 N7 C5 127.4(3) . . ? C8 N7 H7 116.3 . . ? C5 N7 H7 116.3 . . ? O9 C8 O9 0.0(3) 1 . ? O9 C8 N10 123.1(4) 1 . ? O9 C8 N10 123.1(4) . . ? O9 C8 N7 122.3(4) 1 . ? O9 C8 N7 122.3(4) . . ? N10 C8 N7 114.5(3) . . ? O9 O9 C8 0(10) 1 . ? C8 N10 C11 123.6(3) . . ? C8 N10 H10 118.2 . . ? C11 N10 H10 118.2 . . ? C12 C11 C16 120.2(4) . . ? C12 C11 N10 118.7(4) . . ? C16 C11 N10 121.0(3) . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.7(4) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C15 118.6(4) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 N17 123.1(3) . . ? C14 C15 N17 116.6(4) . . ? C15 C16 C11 119.9(4) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C18 N17 C15 127.4(3) . . ? C18 N17 H17 116.3 . . ? C15 N17 H17 116.3 . . ? O19 C18 N17 124.5(4) . . ? O19 C18 N20 122.3(4) . . ? N17 C18 N20 113.2(4) . . ? C18 N20 C21 127.8(3) . . ? C18 N20 H20 116.1 . . ? C21 N20 H20 116.1 . . ? C22 C21 N20 118.3(3) . . ? C22 C21 C26 117.8(4) . . ? N20 C21 C26 123.9(3) . . ? C23 C22 C21 119.3(4) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? N25 C24 C23 121.3(4) . . ? N25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 N25 C26 119.5(3) . . ? C24 N25 Cu1 119.7(3) . 1_565 ? C26 N25 Cu1 120.7(3) . 1_565 ? N25 C26 C21 122.0(3) . . ? N25 C26 H26 119.0 . . ? C21 C26 H26 119.0 . . ? Cu1 O27 H27 126(4) . . ? Cu1 O28 H28 129(3) . . ? H29A O29 H29B 110(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O30 0.86 2.20 3.017(5) 159.1 7_655 N10 H10 F1 0.86 1.95 2.788(4) 166.0 7 N17 H17 O29 0.86 2.00 2.857(5) 170.9 7 N20 H20 O29 0.86 2.51 3.268(5) 147.7 7 O27 H27 F1 0.75(5) 1.92(5) 2.657(4) 168(6) 3_545 O28 H28 O30 0.83(4) 1.99(5) 2.804(5) 169(5) 4_635 O29 H29A O9 0.876(10) 2.05(3) 2.818(5) 146(4) 1 O29 H29B F1 0.880(10) 1.751(11) 2.631(5) 179(8) 4_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.827 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.080 # _vrf_PLAT306_704f1m ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O30 RESPONSE: We are unable to locate hydrogen atom associated with solvent water molecule containing O30. ; _vrf_PLAT431_704f1m ; PROBLM:Short Inter HL..A Contact F1 .. O30 . 2.57 Ang. RESPONSE: We are unable to locate hydrogen atom associated with solvent water molecule containing O30. ; # end Validation Reply Form