# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Leroy Cronin' 'Georg Seeber' 'Geoff Cooper' 'Graham Newton' 'De-Liang Long.' 'Benson Kariuki' 'Paul Koegerler' _publ_contact_author_name 'Leroy Cronin' _publ_contact_author_email L.Cronin@chem.gla.ac.uk _publ_section_title ; Following the Self Assembly of Supramolecular MOFs using X-ray Crystallography and Cryospray Mass Spectrometry ; # Attachment '- compound1.cif' data_gs182 _database_code_depnum_ccdc_archive 'CCDC 772923' #TrackingRef '- compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H64 Cu4 F4 N12 8+), 8(F -), 8.17(C H4 O),' _chemical_formula_sum 'C32 H138 Cu4 F4 N12 O33' _chemical_formula_weight 1549.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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 Cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 37.295(4) _cell_length_b 37.295(4) _cell_length_c 37.295(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 51872(10) _cell_formula_units_Z 24 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3027 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 58.9 _exptl_crystal_description Cube _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 19920 _exptl_absorpt_coefficient_mu 1.802 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7145 _exptl_absorpt_correction_T_max 0.7145 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART AXS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32868 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 58.90 _reflns_number_total 3022 _reflns_number_gt 2787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond3 _computing_publication_material Wingx _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^)+(0.1192P)^2^+87.0636P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(6) _refine_ls_number_reflns 3022 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.467920(19) 0.28975(2) 0.25581(2) 0.0341(3) Uani 1 1 d . . . F1 F 0.30460(8) 0.35205(8) 0.24753(9) 0.0471(7) Uani 1 1 d . . . O1 O 0.47024(9) 0.25458(9) 0.21603(9) 0.0338(8) Uani 1 1 d . . . O2 O 0.47807(17) 0.32168(16) 0.14437(14) 0.0781(15) Uani 1 1 d . . . H2 H 0.4815 0.3063 0.1283 0.117 Uiso 1 1 calc R . . O3 O 0.5688(2) 0.3960(2) 0.1620(2) 0.112(2) Uani 1 1 d . . . H3 H 0.5588 0.3929 0.1820 0.168 Uiso 1 1 calc R . . O4 O 0.37225(17) 0.37225(17) 0.37225(17) 0.083(3) Uiso 1 3 d S . . O5 O 0.4639(3) 0.4435(3) 0.2066(4) 0.168(5) Uani 1 1 d . . . O6 O 0.51986(19) 0.3891(2) 0.2185(2) 0.108(2) Uani 1 1 d . . . O7 O 0.33411(12) 0.41653(12) 0.24996(17) 0.0715(14) Uani 1 1 d . . . O8 O 0.3686(6) 0.3686(6) 0.1314(6) 0.142(11) Uiso 0.50 3 d SP . . O8' O 0.3660(10) 0.3888(13) 0.1107(13) 0.101(13) Uiso 0.17 1 d P . . O9 O 0.4579(16) 0.3753(15) 0.0318(15) 0.122(16) Uiso 0.15 1 d P . . O10 O 0.4238(10) 0.4238(10) 0.0762(10) 0.134(19) Uiso 0.25 3 d SP . . O11 O 0.55888(17) 0.39501(17) 0.27691(18) 0.0918(19) Uani 1 1 d . . . O12 O 0.2276(2) 0.2724(2) 0.2276(2) 0.073(5) Uani 0.50 3 d SP . . C10 C 0.2500 0.2500 0.2500 0.018(5) Uani 0.50 12 d SP . . N1 N 0.45547(12) 0.31945(12) 0.29898(12) 0.0413(11) Uani 1 1 d . . . H1C H 0.4485 0.3039 0.3168 0.050 Uiso 1 1 calc R . . H1D H 0.4762 0.3304 0.3066 0.050 Uiso 1 1 calc R . . N2 N 0.46263(13) 0.33130(13) 0.22268(13) 0.0427(11) Uani 1 1 d . . . H2C H 0.4834 0.3445 0.2237 0.051 Uiso 1 1 calc R . . H2D H 0.4607 0.3225 0.1997 0.051 Uiso 1 1 calc R . . N3 N 0.35037(11) 0.29770(12) 0.25124(13) 0.0401(10) Uani 1 1 d . . . H3C H 0.3454 0.2829 0.2700 0.060 Uiso 1 1 calc R . . H3D H 0.3488 0.2852 0.2303 0.060 Uiso 1 1 calc R . . H3E H 0.3344 0.3161 0.2509 0.060 Uiso 1 1 calc R . . C1 C 0.43179(15) 0.35631(15) 0.22891(16) 0.0443(13) Uani 1 1 d . . . H1A H 0.4331 0.3760 0.2107 0.053 Uiso 1 1 calc R . . C2 C 0.39616(15) 0.33726(16) 0.22444(16) 0.0429(12) Uani 1 1 d . . . H2A H 0.3967 0.3233 0.2019 0.051 Uiso 1 1 calc R . . H2B H 0.3769 0.3554 0.2222 0.051 Uiso 1 1 calc R . . C3 C 0.38698(14) 0.31208(14) 0.25523(14) 0.0367(11) Uani 1 1 d . . . H3A H 0.4042 0.2915 0.2546 0.044 Uiso 1 1 calc R . . C4 C 0.39045(15) 0.33047(16) 0.29137(15) 0.0408(12) Uani 1 1 d . . . H4A H 0.3865 0.3127 0.3107 0.049 Uiso 1 1 calc R . . H4B H 0.3717 0.3492 0.2935 0.049 Uiso 1 1 calc R . . C5 C 0.42745(15) 0.34772(15) 0.29621(16) 0.0428(13) Uani 1 1 d . . . H5A H 0.4273 0.3617 0.3191 0.051 Uiso 1 1 calc R . . C6 C 0.43529(17) 0.37295(15) 0.26598(18) 0.0494(14) Uani 1 1 d . . . H6A H 0.4600 0.3822 0.2688 0.059 Uiso 1 1 calc R . . H6B H 0.4187 0.3936 0.2676 0.059 Uiso 1 1 calc R . . C8 C 0.4810(4) 0.3564(4) 0.1295(3) 0.107(4) Uani 0.80 1 d P . . H8A H 0.4685 0.3736 0.1449 0.160 Uiso 1 1 calc R . . H8B H 0.4701 0.3565 0.1056 0.160 Uiso 1 1 calc R . . H8C H 0.5063 0.3630 0.1276 0.160 Uiso 1 1 calc R . . C9 C 0.5616(5) 0.4319(5) 0.1494(5) 0.114(7) Uani 0.60 1 d P . . H9A H 0.5516 0.4463 0.1690 0.171 Uiso 1 1 calc R . . H9B H 0.5443 0.4310 0.1296 0.171 Uiso 1 1 calc R . . H9C H 0.5839 0.4429 0.1410 0.171 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0283(4) 0.0362(4) 0.0380(5) 0.0008(3) 0.0024(3) 0.0044(3) F1 0.0355(15) 0.0523(18) 0.0535(18) 0.0001(15) -0.0026(14) 0.0088(13) O1 0.0304(17) 0.0364(18) 0.0345(17) -0.0020(14) -0.0051(15) -0.0003(16) O2 0.083(4) 0.086(4) 0.065(3) 0.005(3) -0.011(3) 0.011(3) O3 0.092(5) 0.128(6) 0.117(6) -0.020(5) 0.023(4) -0.010(5) O5 0.112(6) 0.119(7) 0.274(14) 0.016(8) 0.064(8) -0.003(5) O6 0.099(5) 0.116(5) 0.109(5) -0.007(4) 0.022(4) -0.035(4) O7 0.054(3) 0.048(2) 0.112(4) 0.011(3) 0.013(3) 0.011(2) O11 0.096(4) 0.077(4) 0.102(4) -0.022(3) 0.028(3) -0.026(3) O12 0.073(5) 0.073(5) 0.073(5) 0.022(4) -0.022(4) 0.022(4) C10 0.018(5) 0.018(5) 0.018(5) 0.000 0.000 0.000 N1 0.035(2) 0.043(2) 0.046(3) -0.001(2) -0.001(2) 0.0022(19) N2 0.038(2) 0.039(3) 0.052(3) 0.008(2) 0.008(2) 0.0071(19) N3 0.037(2) 0.043(2) 0.040(2) -0.002(2) 0.0027(19) 0.0070(19) C1 0.037(3) 0.040(3) 0.056(3) 0.013(3) 0.009(3) 0.012(2) C2 0.041(3) 0.045(3) 0.043(3) 0.003(2) 0.001(2) 0.008(2) C3 0.032(3) 0.039(3) 0.038(3) 0.000(2) 0.004(2) 0.007(2) C4 0.039(3) 0.047(3) 0.037(3) -0.002(2) 0.002(2) 0.010(2) C5 0.038(3) 0.041(3) 0.049(3) -0.011(3) -0.001(3) 0.008(2) C6 0.047(3) 0.035(3) 0.067(4) -0.006(3) -0.001(3) 0.006(2) C8 0.131(11) 0.101(9) 0.088(8) 0.042(7) -0.025(7) 0.004(8) C9 0.080(11) 0.124(15) 0.138(16) 0.061(13) 0.028(10) 0.036(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.960(3) 28 ? Cu1 O1 1.982(3) . ? Cu1 N2 1.992(5) . ? Cu1 N1 2.009(5) . ? Cu1 O1 2.317(3) 67_554 ? Cu1 Cu1 2.9962(15) 28 ? O1 Cu1 1.960(3) 28 ? O1 Cu1 2.317(3) 90_545 ? O2 C8 1.412(14) . ? O3 C9 1.446(17) . ? O8 O8' 1.08(4) 35 ? O8 O8' 1.08(4) 56 ? O8 O8' 1.08(4) . ? O8' O8' 1.21(7) 56 ? O8' O8' 1.21(7) 35 ? O12 C10 1.448(14) . ? C10 O12 1.448(14) 51 ? C10 O12 1.448(14) 74 ? C10 O12 1.448(14) 28 ? N1 C5 1.488(7) . ? N2 C1 1.499(7) . ? N3 C3 1.475(7) . ? C1 C2 1.516(8) . ? C1 C6 1.521(9) . ? C2 C3 1.522(7) . ? C3 C4 1.518(8) . ? C4 C5 1.533(8) . ? C5 C6 1.498(9) . ? 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 Cu1 O1 80.85(15) 28 . ? O1 Cu1 N2 173.11(18) 28 . ? O1 Cu1 N2 93.14(18) . . ? O1 Cu1 N1 92.63(16) 28 . ? O1 Cu1 N1 167.15(17) . . ? N2 Cu1 N1 92.6(2) . . ? O1 Cu1 O1 83.58(14) 28 67_554 ? O1 Cu1 O1 83.12(14) . 67_554 ? N2 Cu1 O1 99.14(16) . 67_554 ? N1 Cu1 O1 107.29(16) . 67_554 ? O1 Cu1 Cu1 40.81(9) 28 28 ? O1 Cu1 Cu1 40.27(10) . 28 ? N2 Cu1 Cu1 132.85(16) . 28 ? N1 Cu1 Cu1 131.43(14) . 28 ? O1 Cu1 Cu1 84.55(9) 67_554 28 ? Cu1 O1 Cu1 98.92(15) 28 . ? Cu1 O1 Cu1 96.34(14) 28 90_545 ? Cu1 O1 Cu1 95.74(14) . 90_545 ? O8' O8 O8' 68(4) 35 56 ? O8' O8 O8' 68(4) 35 . ? O8' O8 O8' 68(4) 56 . ? O8 O8' O8' 56(2) . 56 ? O8 O8' O8' 56(2) . 35 ? O8' O8' O8' 60.000(15) 56 35 ? O12 C10 O12 109.472(5) 51 74 ? O12 C10 O12 109.471(2) 51 . ? O12 C10 O12 109.471(1) 74 . ? O12 C10 O12 109.5 51 28 ? O12 C10 O12 109.471(2) 74 28 ? O12 C10 O12 109.471(3) . 28 ? C5 N1 Cu1 119.8(4) . . ? C1 N2 Cu1 117.7(3) . . ? N2 C1 C2 111.3(5) . . ? N2 C1 C6 109.2(5) . . ? C2 C1 C6 111.5(5) . . ? C1 C2 C3 113.8(5) . . ? N3 C3 C4 109.4(4) . . ? N3 C3 C2 110.9(4) . . ? C4 C3 C2 111.8(5) . . ? C3 C4 C5 111.8(5) . . ? N1 C5 C6 111.1(5) . . ? N1 C5 C4 110.1(5) . . ? C6 C5 C4 110.5(5) . . ? C5 C6 C1 114.3(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 58.90 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.621 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.095 # Attachment '- compound2.cif' data_nk12m7 _database_code_depnum_ccdc_archive 'CCDC 772924' #TrackingRef '- compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12 H32 Cu N6 4+), 2(S O4 2-), (C H4 O), 4(H2 O)' _chemical_formula_sum 'C13 H44 Cu N6 O13 S2' _chemical_formula_weight 620.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 28.3688(3) _cell_length_b 28.3688(3) _cell_length_c 12.3891(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8634.80(19) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3948 _exptl_absorpt_coefficient_mu 3.001 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Axs' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29031 _diffrn_reflns_av_R_equivalents 0.1188 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 58.96 _reflns_number_total 4151 _reflns_number_gt 2279 _reflns_threshold_expression >2sigma(I) _computing_data_collection Texray _computing_cell_refinement Texray _computing_data_reduction Texray _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; At the final state of refinement, solvent accessable voids have been calculated and then PLATON SQUEEZE was used. Around 380 electons were addiationally found. From these electrons, two more water and a half methanol molecules per formula were added to the sum of atom list. ; _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^)+(0.1841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 4151 _refine_ls_number_parameters 303 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2694 _refine_ls_wR_factor_gt 0.2439 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.32966(4) 0.41176(4) 0.42533(11) 0.0609(5) Uani 1 1 d . . . S1 S 0.38746(15) 0.33605(14) 0.4663(4) 0.1240(16) Uani 1 1 d D . . S2 S 0.25003(9) 0.52521(9) 0.2459(3) 0.0834(8) Uani 1 1 d . . . O1 O 0.3744(3) 0.3640(3) 0.3860(6) 0.108(3) Uani 1 1 d D . . O2 O 0.3376(4) 0.2921(3) 0.5098(8) 0.151(4) Uani 1 1 d D . . O3 O 0.4141(5) 0.3725(4) 0.5575(11) 0.195(6) Uani 1 1 d D . . O4A O 0.4011(5) 0.2999(5) 0.3951(9) 0.093(3) Uiso 0.60 1 d PD . . O4B O 0.4405(6) 0.3368(8) 0.4593(15) 0.099(5) Uiso 0.40 1 d PD . . O5 O 0.2308(3) 0.5235(3) 0.1368(7) 0.108(2) Uani 1 1 d . . . O6 O 0.2047(2) 0.5104(3) 0.3223(6) 0.090(2) Uani 1 1 d . . . O7 O 0.2932(3) 0.5819(2) 0.2682(6) 0.097(2) Uani 1 1 d . . . O8 O 0.2701(2) 0.4874(2) 0.2592(6) 0.091(2) Uani 1 1 d . . . O9 O 0.3704(5) 0.6292(5) 0.1018(10) 0.075(3) Uani 0.50 1 d P . . O10 O 0.2783(4) 0.2365(5) 0.6782(8) 0.088(3) Uani 0.60 1 d P . . O11 O 0.2760(7) 0.2413(7) 0.3378(14) 0.098(5) Uiso 0.40 1 d P . . O12 O 0.3473(3) 0.4449(3) 0.7453(6) 0.095(2) Uani 1 1 d . . . N1 N 0.3932(3) 0.4638(3) 0.5196(6) 0.078(2) Uani 1 1 d . . . H1A H 0.3785 0.4726 0.5770 0.093 Uiso 1 1 calc R . . H1B H 0.4081 0.4441 0.5473 0.093 Uiso 1 1 calc R . . N2 N 0.3634(3) 0.4536(2) 0.2899(6) 0.0632(17) Uani 1 1 d . . . H2A H 0.3667 0.4299 0.2442 0.076 Uiso 1 1 calc R . . H2B H 0.3378 0.4604 0.2594 0.076 Uiso 1 1 calc R . . N3 N 0.3787(3) 0.6059(3) 0.4032(6) 0.074(2) Uani 1 1 d . . . H3A H 0.3504 0.6000 0.3598 0.112 Uiso 1 1 calc R . . H3B H 0.4097 0.6357 0.3794 0.112 Uiso 1 1 calc R . . H3C H 0.3717 0.6117 0.4721 0.112 Uiso 1 1 calc R . . N4 N 0.2649(3) 0.3617(4) 0.3340(8) 0.115(4) Uani 1 1 d . . . H4C H 0.2656 0.3813 0.2743 0.138 Uiso 1 1 calc R . . H4D H 0.2709 0.3345 0.3096 0.138 Uiso 1 1 calc R . . N5 N 0.2926(2) 0.3686(3) 0.5619(6) 0.0653(18) Uani 1 1 d . . . H5A H 0.3031 0.3428 0.5699 0.078 Uiso 1 1 calc R . . H5B H 0.3073 0.3922 0.6192 0.078 Uiso 1 1 calc R . . N6 N 0.2023(3) 0.4540(3) 0.5073(7) 0.084(2) Uani 1 1 d . . . H6C H 0.2034 0.4703 0.4434 0.126 Uiso 1 1 calc R . . H6D H 0.2248 0.4796 0.5555 0.126 Uiso 1 1 calc R . . H6E H 0.1677 0.4368 0.5333 0.126 Uiso 1 1 calc R . . C1 C 0.4159(3) 0.5056(3) 0.2839(8) 0.067(2) Uani 1 1 d . . . H1 H 0.4323 0.5069 0.2117 0.081 Uiso 1 1 calc R . . C2 C 0.4050(3) 0.5532(3) 0.2888(7) 0.062(2) Uani 1 1 d . . . H2C H 0.4387 0.5875 0.2706 0.075 Uiso 1 1 calc R . . H2D H 0.3768 0.5476 0.2350 0.075 Uiso 1 1 calc R . . C3 C 0.3860(3) 0.5577(3) 0.4004(6) 0.0536(19) Uani 1 1 d . . . H3 H 0.3499 0.5245 0.4140 0.064 Uiso 1 1 calc R . . C4 C 0.4258(4) 0.5609(3) 0.4876(8) 0.074(2) Uani 1 1 d . . . H4A H 0.4597 0.5966 0.4823 0.089 Uiso 1 1 calc R . . H4B H 0.4097 0.5589 0.5595 0.089 Uiso 1 1 calc R . . C5 C 0.4398(3) 0.5164(3) 0.4787(9) 0.075(3) Uani 1 1 d . . . H5 H 0.4716 0.5262 0.5270 0.090 Uiso 1 1 calc R . . C6 C 0.4555(3) 0.5091(4) 0.3675(9) 0.081(3) Uani 1 1 d . . . H6A H 0.4578 0.4754 0.3653 0.097 Uiso 1 1 calc R . . H6B H 0.4920 0.5401 0.3504 0.097 Uiso 1 1 calc R . . C7 C 0.2073(4) 0.3341(4) 0.3775(10) 0.095(4) Uani 1 1 d . . . H7 H 0.1827 0.3071 0.3227 0.114 Uiso 1 1 calc R . . C8 C 0.1880(4) 0.3765(4) 0.3963(9) 0.086(3) Uani 1 1 d . . . H8A H 0.1941 0.3984 0.3302 0.104 Uiso 1 1 calc R . . H8B H 0.1486 0.3573 0.4132 0.104 Uiso 1 1 calc R . . C9 C 0.2203(3) 0.4139(3) 0.4906(8) 0.071(2) Uani 1 1 d . . . H9 H 0.2597 0.4340 0.4699 0.085 Uiso 1 1 calc R . . C10 C 0.2146(3) 0.3824(3) 0.5917(8) 0.070(2) Uani 1 1 d . . . H10A H 0.1762 0.3638 0.6156 0.084 Uiso 1 1 calc R . . H10B H 0.2371 0.4079 0.6494 0.084 Uiso 1 1 calc R . . C11 C 0.2323(3) 0.3399(3) 0.5751(8) 0.073(3) Uani 1 1 d . . . H11 H 0.2226 0.3168 0.6414 0.088 Uiso 1 1 calc R . . C12 C 0.2042(4) 0.3035(4) 0.4804(10) 0.090(3) Uani 1 1 d . . . H12A H 0.1654 0.2791 0.4990 0.108 Uiso 1 1 calc R . . H12B H 0.2207 0.2805 0.4668 0.108 Uiso 1 1 calc R . . C13 C 0.3190(11) 0.6279(8) 0.0617(14) 0.099(7) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0402(7) 0.0415(7) 0.1019(9) -0.0003(6) 0.0134(6) 0.0213(5) S1 0.117(2) 0.090(2) 0.212(4) 0.084(2) 0.108(3) 0.087(2) S2 0.0578(13) 0.0596(14) 0.144(2) -0.0130(14) -0.0070(14) 0.0381(11) O1 0.123(6) 0.090(5) 0.159(7) 0.052(5) 0.073(5) 0.088(5) O2 0.196(10) 0.096(6) 0.171(8) 0.058(6) 0.099(8) 0.080(7) O3 0.160(10) 0.112(8) 0.340(18) 0.068(10) -0.032(11) 0.087(8) O5 0.128(6) 0.100(5) 0.135(6) -0.025(5) -0.029(5) 0.085(5) O6 0.059(4) 0.081(4) 0.145(6) -0.022(4) -0.005(4) 0.045(3) O7 0.070(4) 0.063(4) 0.160(7) 0.002(4) -0.010(4) 0.035(3) O8 0.058(3) 0.057(4) 0.169(7) 0.005(4) 0.008(4) 0.037(3) O9 0.068(7) 0.070(8) 0.080(8) -0.018(6) -0.016(6) 0.029(6) O10 0.094(8) 0.110(8) 0.081(7) 0.025(6) 0.039(6) 0.067(7) O12 0.076(4) 0.089(5) 0.134(6) -0.045(4) -0.023(4) 0.052(4) N1 0.053(4) 0.058(4) 0.118(6) 0.025(4) -0.008(4) 0.025(3) N2 0.056(4) 0.048(4) 0.090(5) -0.003(3) -0.001(3) 0.029(3) N3 0.089(5) 0.058(4) 0.086(5) -0.002(4) -0.015(4) 0.044(4) N4 0.067(5) 0.093(6) 0.129(7) -0.050(6) 0.017(5) -0.001(5) N5 0.053(4) 0.057(4) 0.095(5) 0.010(4) 0.021(3) 0.035(3) N6 0.049(4) 0.067(5) 0.141(7) -0.008(5) -0.017(4) 0.032(4) C1 0.049(5) 0.055(5) 0.104(7) 0.017(5) 0.022(5) 0.031(4) C2 0.042(4) 0.047(4) 0.097(6) 0.017(4) 0.006(4) 0.020(4) C3 0.048(4) 0.038(4) 0.076(5) 0.002(4) 0.001(4) 0.023(3) C4 0.060(5) 0.056(5) 0.101(7) 0.008(5) -0.005(5) 0.024(4) C5 0.049(5) 0.043(4) 0.130(8) 0.018(5) -0.004(5) 0.021(4) C6 0.036(4) 0.059(5) 0.147(9) 0.017(6) 0.010(5) 0.024(4) C7 0.052(5) 0.061(6) 0.132(9) -0.029(6) 0.013(6) 0.000(5) C8 0.060(6) 0.055(5) 0.113(8) -0.007(5) -0.006(5) 0.005(5) C9 0.045(4) 0.060(5) 0.114(7) -0.018(5) -0.005(5) 0.031(4) C10 0.056(5) 0.062(5) 0.102(7) 0.011(5) 0.022(5) 0.037(4) C11 0.053(5) 0.055(5) 0.114(7) 0.009(5) 0.036(5) 0.029(4) C12 0.053(5) 0.050(5) 0.149(10) -0.001(6) 0.031(6) 0.013(4) C13 0.119(18) 0.092(14) 0.055(10) 0.001(10) -0.017(12) 0.029(15) _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 N2 2.001(7) . ? Cu1 N4 2.016(8) . ? Cu1 N1 2.032(7) . ? Cu1 N5 2.045(6) . ? Cu1 O1 2.325(5) . ? S1 O1 1.432(7) . ? S1 O2 1.443(8) . ? S1 O3 1.461(12) . ? S1 O4B 1.497(13) . ? S1 O4A 1.542(10) . ? S2 O5 1.449(8) . ? S2 O8 1.453(6) . ? S2 O6 1.478(7) . ? S2 O7 1.481(7) . ? O4A O4B 1.344(19) . ? O9 C13 1.53(3) . ? O9 C13 1.80(3) 2_665 ? N1 C5 1.502(10) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C1 1.484(10) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C3 1.482(9) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 C7 1.515(12) . ? N4 H4C 0.9200 . ? N4 H4D 0.9200 . ? N5 C11 1.491(9) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? N6 C9 1.477(10) . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? C1 C6 1.493(12) . ? C1 C2 1.532(10) . ? C1 H1 1.0000 . ? C2 C3 1.512(11) . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.534(11) . ? C3 H3 1.0000 . ? C4 C5 1.506(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.493(13) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.520(16) . ? C7 C8 1.568(14) . ? C7 H7 1.0000 . ? C8 C9 1.535(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.500(12) . ? C9 H9 1.0000 . ? C10 C11 1.533(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.502(13) . ? C11 H11 1.0000 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C13 1.67(4) 3_565 ? C13 C13 1.67(4) 2_665 ? C13 O9 1.80(3) 3_565 ? 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 Cu1 N4 86.8(3) . . ? N2 Cu1 N1 93.6(3) . . ? N4 Cu1 N1 177.6(3) . . ? N2 Cu1 N5 178.0(3) . . ? N4 Cu1 N5 91.6(3) . . ? N1 Cu1 N5 87.9(3) . . ? N2 Cu1 O1 86.1(2) . . ? N4 Cu1 O1 92.4(4) . . ? N1 Cu1 O1 90.0(3) . . ? N5 Cu1 O1 95.2(2) . . ? O1 S1 O2 108.9(6) . . ? O1 S1 O3 109.4(5) . . ? O2 S1 O3 105.0(7) . . ? O1 S1 O4B 119.3(8) . . ? O2 S1 O4B 125.3(8) . . ? O3 S1 O4B 82.8(9) . . ? O1 S1 O4A 101.0(6) . . ? O2 S1 O4A 95.9(6) . . ? O3 S1 O4A 134.4(7) . . ? O4B S1 O4A 52.5(8) . . ? O5 S2 O8 111.2(4) . . ? O5 S2 O6 109.2(4) . . ? O8 S2 O6 108.9(4) . . ? O5 S2 O7 107.6(5) . . ? O8 S2 O7 111.3(4) . . ? O6 S2 O7 108.6(4) . . ? S1 O1 Cu1 123.0(4) . . ? O4B O4A S1 62.1(7) . . ? O4A O4B S1 65.5(7) . . ? C13 O9 C13 59.4(15) . 2_665 ? C5 N1 Cu1 123.3(6) . . ? C5 N1 H1A 106.5 . . ? Cu1 N1 H1A 106.5 . . ? C5 N1 H1B 106.5 . . ? Cu1 N1 H1B 106.5 . . ? H1A N1 H1B 106.5 . . ? C1 N2 Cu1 125.2(6) . . ? C1 N2 H2A 106.0 . . ? Cu1 N2 H2A 106.0 . . ? C1 N2 H2B 106.0 . . ? Cu1 N2 H2B 106.0 . . ? H2A N2 H2B 106.3 . . ? C3 N3 H3A 109.5 . . ? C3 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C3 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C7 N4 Cu1 122.2(7) . . ? C7 N4 H4C 106.8 . . ? Cu1 N4 H4C 106.8 . . ? C7 N4 H4D 106.8 . . ? Cu1 N4 H4D 106.8 . . ? H4C N4 H4D 106.6 . . ? C11 N5 Cu1 121.5(6) . . ? C11 N5 H5A 106.9 . . ? Cu1 N5 H5A 106.9 . . ? C11 N5 H5B 106.9 . . ? Cu1 N5 H5B 106.9 . . ? H5A N5 H5B 106.7 . . ? C9 N6 H6C 109.5 . . ? C9 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C9 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? N2 C1 C6 112.3(7) . . ? N2 C1 C2 109.2(6) . . ? C6 C1 C2 113.0(8) . . ? N2 C1 H1 107.4 . . ? C6 C1 H1 107.4 . . ? C2 C1 H1 107.4 . . ? C3 C2 C1 110.4(7) . . ? C3 C2 H2C 109.6 . . ? C1 C2 H2C 109.6 . . ? C3 C2 H2D 109.6 . . ? C1 C2 H2D 109.6 . . ? H2C C2 H2D 108.1 . . ? N3 C3 C2 108.6(6) . . ? N3 C3 C4 111.5(6) . . ? C2 C3 C4 111.5(7) . . ? N3 C3 H3 108.4 . . ? C2 C3 H3 108.4 . . ? C4 C3 H3 108.4 . . ? C5 C4 C3 113.2(8) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 N1 110.4(8) . . ? C6 C5 C4 113.9(8) . . ? N1 C5 C4 109.8(7) . . ? C6 C5 H5 107.5 . . ? N1 C5 H5 107.5 . . ? C4 C5 H5 107.5 . . ? C5 C6 C1 112.5(7) . . ? C5 C6 H6A 109.1 . . ? C1 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N4 C7 C12 109.4(10) . . ? N4 C7 C8 110.9(8) . . ? C12 C7 C8 111.7(9) . . ? N4 C7 H7 108.2 . . ? C12 C7 H7 108.2 . . ? C8 C7 H7 108.2 . . ? C9 C8 C7 109.0(8) . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N6 C9 C10 111.5(7) . . ? N6 C9 C8 108.8(7) . . ? C10 C9 C8 112.0(8) . . ? N6 C9 H9 108.2 . . ? C10 C9 H9 108.2 . . ? C8 C9 H9 108.2 . . ? C9 C10 C11 112.1(7) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N5 C11 C12 111.1(7) . . ? N5 C11 C10 108.9(6) . . ? C12 C11 C10 112.0(8) . . ? N5 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C10 C11 H11 108.3 . . ? C11 C12 C7 113.8(8) . . ? C11 C12 H12A 108.8 . . ? C7 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? C7 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O9 C13 C13 124.9(17) . 3_565 ? O9 C13 C13 68.6(19) . 2_665 ? C13 C13 C13 60.000(6) 3_565 2_665 ? O9 C13 O9 144.9(14) . 3_565 ? C13 C13 O9 52.0(17) 3_565 3_565 ? C13 C13 O9 109.4(17) 2_665 3_565 ? 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 N2 H2A O4A 0.92 2.39 2.835(13) 109.9 4 N6 H6E O4A 0.91 1.86 2.763(14) 171.9 9_556 N6 H6E O4B 0.91 1.87 2.659(18) 143.6 9_556 N6 H6D O5 0.91 1.97 2.825(10) 156.1 11_556 N6 H6C O6 0.91 1.87 2.777(11) 172.7 . N3 H3A O7 0.91 1.83 2.737(10) 174.3 . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.009 1621.6 383.4 2 0.000 0.347 0.250 6.9 -0.3 3 0.000 0.653 0.750 6.9 -0.8 4 0.347 0.000 0.250 6.9 -0.3 5 0.347 0.347 0.750 7.0 -0.8 6 0.653 0.000 0.750 6.9 -0.8 7 0.653 0.653 0.250 7.0 -0.3 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 58.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.039 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.122