data_UTSA-76 _audit_creation_date 2014-01-07 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.11(C180 H72 Cu18 N18 O90), O' _chemical_formula_sum 'C20 H8 Cu2 N2 O11' _chemical_formula_weight 579.36 _chemical_melting_point ? _chemical_oxdiff_formula 'C1 H1 N1 O1 Cu1' 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _space_group_crystal_system 'trigonal' _space_group_IT_number 166 _space_group_name_H-M_alt 'R -3 m' _space_group_name_Hall '-R 3 2"' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 'x-y, -y, -z' 5 '-x, -x+y, -z' 6 'y, x, -z' 7 'x+2/3, y+1/3, z+1/3' 8 '-y+2/3, x-y+1/3, z+1/3' 9 '-x+y+2/3, -x+1/3, z+1/3' 10 'x-y+2/3, -y+1/3, -z+1/3' 11 '-x+2/3, -x+y+1/3, -z+1/3' 12 'y+2/3, x+1/3, -z+1/3' 13 'x+1/3, y+2/3, z+2/3' 14 '-y+1/3, x-y+2/3, z+2/3' 15 '-x+y+1/3, -x+2/3, z+2/3' 16 'x-y+1/3, -y+2/3, -z+2/3' 17 '-x+1/3, -x+y+2/3, -z+2/3' 18 'y+1/3, x+2/3, -z+2/3' 19 '-x, -y, -z' 20 'y, -x+y, -z' 21 'x-y, x, -z' 22 '-x+y, y, z' 23 'x, x-y, z' 24 '-y, -x, z' 25 '-x+2/3, -y+1/3, -z+1/3' 26 'y+2/3, -x+y+1/3, -z+1/3' 27 'x-y+2/3, x+1/3, -z+1/3' 28 '-x+y+2/3, y+1/3, z+1/3' 29 'x+2/3, x-y+1/3, z+1/3' 30 '-y+2/3, -x+1/3, z+1/3' 31 '-x+1/3, -y+2/3, -z+2/3' 32 'y+1/3, -x+y+2/3, -z+2/3' 33 'x-y+1/3, x+2/3, -z+2/3' 34 '-x+y+1/3, y+2/3, z+2/3' 35 'x+1/3, x-y+2/3, z+2/3' 36 '-y+1/3, -x+2/3, z+2/3' _cell_length_a 18.6895(5) _cell_length_b 18.6895(5) _cell_length_c 37.6886(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11400.8(5) _cell_formula_units_Z 9 _cell_measurement_reflns_used 4447 _cell_measurement_temperature 100.00(19) _cell_measurement_theta_max 28.1360 _cell_measurement_theta_min 3.9000 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour '' _exptl_crystal_density_diffrn 0.759 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description '' _exptl_crystal_F_000 2592 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_number 9196 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.72 _diffrn_ambient_temperature 100.00(19) _diffrn_detector_area_resol_mean 10.5594 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0332838000 _diffrn_orient_matrix_UB_12 0.0364056000 _diffrn_orient_matrix_UB_13 -0.0073712000 _diffrn_orient_matrix_UB_21 0.0284265000 _diffrn_orient_matrix_UB_22 -0.0064289000 _diffrn_orient_matrix_UB_23 0.0100058000 _diffrn_orient_matrix_UB_31 0.0027614000 _diffrn_orient_matrix_UB_32 -0.0235627000 _diffrn_orient_matrix_UB_33 -0.0141258000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2110 _reflns_number_total 2452 _reflns_odcompleteness_completeness 99.68 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 1.122 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.152 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 98 _refine_ls_number_reflns 2452 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0808 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1551P)^2^+100.1149P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2558 _refine_ls_wR_factor_ref 0.2627 _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. ; _olex2_refinement_description ; 1. Others Fixed Sof: C7(0.5) H7(0.5) N1(0.5) O4(0.125) O5(0.125) Fixed Uiso: H3(0.071) H5(0.054) H7(0.078) Fixed X: H3(0.4229) H5(0.5666) H7(0.5743) O4(0.6667) O5(0.6667) Fixed Y: H3(0.3641) H5(0.4334) H7(0.6115) O4(0.3333) O5(0.3333) Fixed Z: H3(0.5769) H5(0.6636) H7(0.5381) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C1 C 0.5134(4) 0.4866(4) 0.5342(2) 0.072(3) Uani 1 2 d SD . . C2 C 0.5275(4) 0.4725(4) 0.5707(3) 0.064(3) Uani 1 2 d S . . C3 C 0.4714(4) 0.4019(4) 0.58834(17) 0.0590(18) Uani 1 1 d . . . H3 H 0.4229 0.3641 0.5769 0.071 Uiso 1 1 calc R . . C4 C 0.4859(3) 0.3862(4) 0.62307(15) 0.0467(14) Uani 1 1 d . . . C5 C 0.5570(3) 0.4430(3) 0.6403(2) 0.0451(18) Uani 1 2 d S . . H5 H 0.5666 0.4334 0.6636 0.054 Uiso 1 2 calc SR . . C6 C 0.4273(3) 0.3057(4) 0.64028(14) 0.0423(13) Uani 1 1 d . . . C7 C 0.5460(10) 0.5673(5) 0.5226(3) 0.065(4) Uani 0.50 1 d PDU . . H7 H 0.5743 0.6115 0.5381 0.078 Uiso 0.50 1 calc PR . . Cu1 Cu 0.37974(5) 0.18987(2) 0.695864(19) 0.0312(4) Uani 1 2 d S . . N1 N 0.5799(6) 0.5352(9) 0.5126(3) 0.078(4) Uani 0.50 1 d PDU . . O1 O 0.4445(2) 0.2948(3) 0.67133(10) 0.0481(10) Uani 1 1 d . . . O2 O 0.3654(2) 0.2558(3) 0.62238(10) 0.0515(11) Uani 1 1 d . . . O3 O 0.4403(5) 0.2201(2) 0.74616(18) 0.079(2) Uani 1 2 d S . . O4 O 0.6667 0.3333 0.727(2) 0.33(4) Uiso 0.75 6 d SP . . O5 O 0.6667 0.3333 0.596(3) 0.52(7) Uiso 0.75 6 d SP . . 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 C1 0.053(3) 0.053(3) 0.059(6) 0.017(3) -0.017(3) -0.012(5) C2 0.051(4) 0.051(4) 0.057(6) 0.012(3) -0.012(3) 0.002(4) C3 0.043(3) 0.052(4) 0.052(3) 0.008(3) -0.009(3) 0.001(3) C4 0.037(3) 0.045(3) 0.042(3) 0.007(3) -0.001(2) 0.009(3) C5 0.042(3) 0.042(3) 0.042(4) 0.0013(18) -0.0013(18) 0.014(4) C6 0.030(3) 0.046(3) 0.040(3) 0.005(2) 0.003(2) 0.011(2) C7 0.072(7) 0.046(6) 0.050(6) 0.014(5) -0.011(6) 0.008(5) Cu1 0.0206(5) 0.0424(5) 0.0233(5) -0.00124(14) -0.0025(3) 0.0103(3) N1 0.058(6) 0.079(7) 0.056(6) 0.020(6) -0.011(5) 0.003(5) O1 0.039(2) 0.045(2) 0.041(2) 0.0049(17) -0.0049(16) 0.0069(18) O2 0.039(2) 0.048(2) 0.041(2) 0.0100(18) -0.0051(17) 0.0018(19) O3 0.078(5) 0.097(4) 0.055(4) -0.0181(18) -0.036(4) 0.039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.450(13) . ? C1 C7 1.383(7) 24_665 ? C1 C7 1.383(7) . ? C1 N1 1.381(6) 24_665 ? C1 N1 1.381(6) . ? C2 C3 1.378(8) . ? C2 C3 1.378(8) 24_665 ? C3 H3 0.9300 . ? C3 C4 1.397(8) . ? C4 C5 1.380(7) . ? C4 C6 1.496(8) . ? C5 C4 1.380(7) 24_665 ? C5 H5 0.9300 . ? C6 O1 1.257(7) . ? C6 O2 1.257(7) . ? C7 H7 0.9300 . ? C7 N1 1.379(6) 6_556 ? Cu1 Cu1 2.6645(15) 25_556 ? Cu1 O1 1.947(4) 23 ? Cu1 O1 1.947(4) . ? Cu1 O2 1.951(4) 11_556 ? Cu1 O2 1.951(4) 25_556 ? Cu1 O3 2.134(6) . ? N1 C7 1.379(6) 6_556 ? O2 Cu1 1.951(4) 25_556 ? 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 C7 C1 C2 118.5(8) . . ? C7 C1 C2 118.5(8) 24_665 . ? C7 C1 C7 99.8(14) . 24_665 ? N1 C1 C2 119.6(7) . . ? N1 C1 C2 119.6(7) 24_665 . ? N1 C1 C7 121.9(8) 24_665 . ? N1 C1 C7 48.5(9) 24_665 24_665 ? N1 C1 C7 48.5(9) . . ? N1 C1 C7 121.9(8) . 24_665 ? N1 C1 N1 102.3(12) 24_665 . ? C3 C2 C1 120.8(4) . . ? C3 C2 C1 120.8(4) 24_665 . ? C3 C2 C3 118.5(9) 24_665 . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.2(6) . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 119.7(5) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 C6 120.6(5) . . ? C4 C5 C4 119.9(7) . 24_665 ? C4 C5 H5 120.0 24_665 . ? C4 C5 H5 120.0 . . ? O1 C6 C4 116.6(5) . . ? O1 C6 O2 126.5(5) . . ? O2 C6 C4 116.9(5) . . ? C1 C7 H7 121.1 . . ? N1 C7 C1 117.9(10) 6_556 . ? N1 C7 H7 121.1 6_556 . ? O1 Cu1 Cu1 84.92(12) 23 25_556 ? O1 Cu1 Cu1 84.92(12) . 25_556 ? O1 Cu1 O1 88.3(3) . 23 ? O1 Cu1 O2 167.65(16) . 25_556 ? O1 Cu1 O2 167.65(16) 23 11_556 ? O1 Cu1 O2 90.1(2) . 11_556 ? O1 Cu1 O2 90.1(2) 23 25_556 ? O1 Cu1 O3 100.1(2) 23 . ? O1 Cu1 O3 100.1(2) . . ? O2 Cu1 Cu1 82.74(11) 25_556 25_556 ? O2 Cu1 Cu1 82.74(11) 11_556 25_556 ? O2 Cu1 O2 88.9(3) 25_556 11_556 ? O2 Cu1 O3 92.3(2) 25_556 . ? O2 Cu1 O3 92.3(2) 11_556 . ? O3 Cu1 Cu1 173.0(2) . 25_556 ? C7 N1 C1 120.0(8) 6_556 . ? C6 O1 Cu1 121.6(4) . . ? C6 O2 Cu1 124.0(4) . 25_556 ?