# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_PCN-82 _database_code_depnum_ccdc_archive 'CCDC 846791' #TrackingRef '7438_web_deposit_cif_file_0_WeigangLu_1317458825.1-sr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Cu2 N2 O12' _chemical_formula_sum 'C36 H24 Cu2 N2 O12' _chemical_formula_weight 803.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3240 0.8257 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -z, y' 'x, -y, -z' 'x, z, -y' 'z, y, -x' '-x, y, -z' '-z, y, x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' 'y, x, -z' '-y, -x, -z' '-x, z, y' '-x, -z, -y' 'z, -y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-y, x+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'y, -x+1/2, z+1/2' 'x, -z+1/2, y+1/2' 'x, -y+1/2, -z+1/2' 'x, z+1/2, -y+1/2' 'z, y+1/2, -x+1/2' '-x, y+1/2, -z+1/2' '-z, y+1/2, x+1/2' 'z, x+1/2, y+1/2' 'y, z+1/2, x+1/2' '-y, -z+1/2, x+1/2' 'z, -x+1/2, -y+1/2' '-y, z+1/2, -x+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, -z+1/2, -x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'z, -y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-y+1/2, x, z+1/2' '-x+1/2, -y, z+1/2' 'y+1/2, -x, z+1/2' 'x+1/2, -z, y+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, z, -y+1/2' 'z+1/2, y, -x+1/2' '-x+1/2, y, -z+1/2' '-z+1/2, y, x+1/2' 'z+1/2, x, y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, -z, x+1/2' 'z+1/2, -x, -y+1/2' '-y+1/2, z, -x+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, x, -z+1/2' '-y+1/2, -x, -z+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-y+1/2, x+1/2, z' '-x+1/2, -y+1/2, z' 'y+1/2, -x+1/2, z' 'x+1/2, -z+1/2, y' 'x+1/2, -y+1/2, -z' 'x+1/2, z+1/2, -y' 'z+1/2, y+1/2, -x' '-x+1/2, y+1/2, -z' '-z+1/2, y+1/2, x' 'z+1/2, x+1/2, y' 'y+1/2, z+1/2, x' '-y+1/2, -z+1/2, x' 'z+1/2, -x+1/2, -y' '-y+1/2, z+1/2, -x' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, -z+1/2, -x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'z+1/2, -y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, z, -y' '-x, y, z' '-x, -z, y' '-z, -y, x' 'x, -y, z' 'z, -y, -x' '-z, -x, -y' '-y, -z, -x' 'y, z, -x' '-z, x, y' 'y, -z, x' 'z, x, -y' 'z, -x, y' '-y, z, x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' 'x, y+1/2, -z+1/2' '-y, x+1/2, -z+1/2' '-x, z+1/2, -y+1/2' '-x, y+1/2, z+1/2' '-x, -z+1/2, y+1/2' '-z, -y+1/2, x+1/2' 'x, -y+1/2, z+1/2' 'z, -y+1/2, -x+1/2' '-z, -x+1/2, -y+1/2' '-y, -z+1/2, -x+1/2' 'y, z+1/2, -x+1/2' '-z, x+1/2, y+1/2' 'y, -z+1/2, x+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, z+1/2, x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-z, y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'y+1/2, -x, -z+1/2' 'x+1/2, y, -z+1/2' '-y+1/2, x, -z+1/2' '-x+1/2, z, -y+1/2' '-x+1/2, y, z+1/2' '-x+1/2, -z, y+1/2' '-z+1/2, -y, x+1/2' 'x+1/2, -y, z+1/2' 'z+1/2, -y, -x+1/2' '-z+1/2, -x, -y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, z, -x+1/2' '-z+1/2, x, y+1/2' 'y+1/2, -z, x+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, -x, z+1/2' 'y+1/2, x, z+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'y+1/2, -x+1/2, -z' 'x+1/2, y+1/2, -z' '-y+1/2, x+1/2, -z' '-x+1/2, z+1/2, -y' '-x+1/2, y+1/2, z' '-x+1/2, -z+1/2, y' '-z+1/2, -y+1/2, x' 'x+1/2, -y+1/2, z' 'z+1/2, -y+1/2, -x' '-z+1/2, -x+1/2, -y' '-y+1/2, -z+1/2, -x' 'y+1/2, z+1/2, -x' '-z+1/2, x+1/2, y' 'y+1/2, -z+1/2, x' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, z+1/2, x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-z+1/2, y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 40.026(6) _cell_length_b 40.026(6) _cell_length_c 40.026(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 64123(16) _cell_formula_units_Z 24 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9915 _cell_measurement_theta_min 2.1785 _cell_measurement_theta_max 11.7235 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9792 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9824 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.40663 _diffrn_radiation_type synchrotron _diffrn_radiation_source 15ID-B _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75012 _diffrn_reflns_av_R_equivalents 0.2448 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 0.50 _diffrn_reflns_theta_max 13.06 _reflns_number_total 2305 _reflns_number_gt 1547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2305 _refine_ls_number_parameters 90 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1479 _refine_ls_R_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.3269 _refine_ls_wR_factor_gt 0.3149 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.002 -0.004 -0.002 45868 14233 ' ' _platon_squeeze_details ; ; 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 0.0000 0.0000 0.17280(3) 0.0692(8) Uani 1 8 d S . . Cu2 Cu 0.0000 0.0000 0.23844(4) 0.0820(8) Uani 1 8 d S . . O1 O -0.04871(11) 0.0000 0.17679(10) 0.0846(14) Uani 1 2 d S . . O2 O -0.04844(13) 0.0000 0.23417(11) 0.1063(17) Uani 1 2 d S . . O3 O 0.0000 0.0000 0.11905(18) 0.085(2) Uani 1 8 d S . . O4 O 0.0000 0.0000 0.2927(2) 0.112(3) Uani 1 8 d S . . O5 O -0.2065(6) 0.0557(6) 0.2472(7) 0.313(17) Uiso 0.25 1 d PD . . C10 C -0.1838(6) 0.0549(6) 0.2717(7) 0.376 Uiso 0.25 1 d PRD . . H10A H -0.1923 0.0669 0.2912 0.470 Uiso 0.25 1 calc PR . . H10B H -0.1631 0.0655 0.2639 0.470 Uiso 0.25 1 calc PR . . H10C H -0.1792 0.0316 0.2778 0.470 Uiso 0.25 1 calc PR . . N1 N -0.2008(3) 0.0000 0.2008(3) 0.181(5) Uani 1 4 d SDU . . C1 C -0.06146(18) 0.0000 0.2045(2) 0.103(2) Uani 1 2 d S . . C2 C -0.1001(2) 0.0000 0.2048(2) 0.120(3) Uani 1 2 d SU . . C3 C -0.1155(2) 0.0000 0.1750(2) 0.121(3) Uani 1 2 d SU . . H3 H -0.1030 0.0000 0.1548 0.145 Uiso 1 2 calc SR . . C4 C -0.1514(2) 0.0000 0.1744(2) 0.117(3) Uani 1 2 d SU . . C5 C -0.1654(3) 0.0000 0.2052(3) 0.141(3) Uani 1 2 d SU . . C6 C -0.1490(3) 0.0000 0.2355(3) 0.176(5) Uani 1 2 d SU . . H6 H -0.1608 0.0000 0.2561 0.211 Uiso 1 2 calc SR . . C7 C -0.1167(3) 0.0000 0.2344(3) 0.144(4) Uani 1 2 d SU . . H7 H -0.1044 0.0000 0.2546 0.172 Uiso 1 2 calc SR . . C8 C -0.2278(3) 0.0000 0.2278(3) 0.176(5) Uani 1 4 d SDU . . C9 C -0.2270(3) 0.0288(4) 0.2480(3) 0.189(8) Uani 0.50 1 d PDU . . 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 0.0772(9) 0.0772(9) 0.0532(10) 0.000 0.000 0.000 Cu2 0.0980(10) 0.0980(10) 0.0501(10) 0.000 0.000 0.000 O1 0.077(3) 0.124(4) 0.053(2) 0.000 0.025(2) 0.000 O2 0.103(4) 0.163(5) 0.053(3) 0.000 -0.005(2) 0.000 O3 0.102(4) 0.102(4) 0.050(4) 0.000 0.000 0.000 O4 0.130(5) 0.130(5) 0.075(6) 0.000 0.000 0.000 N1 0.177(5) 0.190(6) 0.177(5) 0.000 0.004(5) 0.000 C1 0.086(5) 0.136(7) 0.088(6) 0.000 -0.002(4) 0.000 C2 0.118(4) 0.132(5) 0.111(4) 0.000 0.009(4) 0.000 C3 0.114(4) 0.128(5) 0.122(4) 0.000 -0.001(4) 0.000 C4 0.111(4) 0.126(4) 0.116(4) 0.000 0.007(3) 0.000 C5 0.134(5) 0.158(5) 0.133(5) 0.000 0.005(4) 0.000 C6 0.168(6) 0.186(6) 0.174(6) 0.000 0.001(4) 0.000 C7 0.138(5) 0.156(5) 0.137(5) 0.000 0.011(4) 0.000 C8 0.173(5) 0.182(7) 0.173(5) 0.000 0.006(5) 0.000 C9 0.183(9) 0.191(9) 0.192(9) 0.001(4) 0.002(5) 0.001(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 Cu1 O1 1.956(4) 4 ? Cu1 O1 1.956(4) 2 ? Cu1 O1 1.956(4) 3 ? Cu1 O1 1.956(4) . ? Cu1 O3 2.151(7) . ? Cu1 Cu2 2.627(2) . ? Cu2 O2 1.946(5) 2 ? Cu2 O2 1.946(5) 4 ? Cu2 O2 1.946(5) . ? Cu2 O2 1.946(5) 3 ? Cu2 O4 2.173(9) . ? O1 C1 1.222(8) . ? O2 C1 1.296(8) . ? O5 C10 1.3355 . ? O5 C9 1.354(18) . ? N1 C5 1.429(12) 119 ? N1 C5 1.430(12) . ? N1 C8 1.528(15) . ? C1 C2 1.545(11) . ? C2 C3 1.343(11) . ? C2 C7 1.359(11) . ? C3 C4 1.439(11) . ? C4 C4 1.301(17) 119 ? C4 C5 1.353(11) . ? C5 C6 1.378(14) . ? C6 C7 1.294(14) . ? C8 C9 1.410(14) . ? C8 C9 1.410(14) 105 ? C8 C9 1.410(14) 24 ? C8 C9 1.410(14) 119 ? C9 C9 1.19(3) 119 ? C9 C9 1.415(17) 168_455 ? C9 C9 1.85(2) 57_455 ? 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 170.6(3) 4 2 ? O1 Cu1 O1 89.61(2) 4 3 ? O1 Cu1 O1 89.61(2) 2 3 ? O1 Cu1 O1 89.62(2) 4 . ? O1 Cu1 O1 89.62(2) 2 . ? O1 Cu1 O1 170.6(3) 3 . ? O1 Cu1 O3 94.68(13) 4 . ? O1 Cu1 O3 94.68(13) 2 . ? O1 Cu1 O3 94.68(13) 3 . ? O1 Cu1 O3 94.68(13) . . ? O1 Cu1 Cu2 85.32(13) 4 . ? O1 Cu1 Cu2 85.32(13) 2 . ? O1 Cu1 Cu2 85.32(13) 3 . ? O1 Cu1 Cu2 85.32(13) . . ? O3 Cu1 Cu2 180.0 . . ? O2 Cu2 O2 169.9(3) 2 4 ? O2 Cu2 O2 89.56(2) 2 . ? O2 Cu2 O2 89.56(2) 4 . ? O2 Cu2 O2 89.55(2) 2 3 ? O2 Cu2 O2 89.55(2) 4 3 ? O2 Cu2 O2 169.9(3) . 3 ? O2 Cu2 O4 95.04(13) 2 . ? O2 Cu2 O4 95.04(13) 4 . ? O2 Cu2 O4 95.04(13) . . ? O2 Cu2 O4 95.04(13) 3 . ? O2 Cu2 Cu1 84.96(13) 2 . ? O2 Cu2 Cu1 84.96(13) 4 . ? O2 Cu2 Cu1 84.96(13) . . ? O2 Cu2 Cu1 84.96(13) 3 . ? O4 Cu2 Cu1 180.0 . . ? C1 O1 Cu1 119.4(5) . . ? C1 O2 Cu2 118.8(5) . . ? C10 O5 C9 112.0(6) . . ? C5 N1 C5 104.0(14) 119 . ? C5 N1 C8 128.0(7) 119 . ? C5 N1 C8 128.0(7) . . ? O1 C1 O2 131.6(7) . . ? O1 C1 C2 115.0(7) . . ? O2 C1 C2 113.4(7) . . ? C3 C2 C7 123.3(10) . . ? C3 C2 C1 117.0(8) . . ? C7 C2 C1 119.8(9) . . ? C2 C3 C4 118.3(8) . . ? C4 C4 C5 110.6(6) 119 . ? C4 C4 C3 135.9(5) 119 . ? C5 C4 C3 113.4(8) . . ? C4 C5 C6 127.3(11) . . ? C4 C5 N1 107.3(11) . . ? C6 C5 N1 125.4(11) . . ? C7 C6 C5 116.3(13) . . ? C6 C7 C2 121.4(12) . . ? C9 C8 C9 109.8(13) . 105 ? C9 C8 C9 134.2(17) . 24 ? C9 C8 C9 50.1(10) 105 24 ? C9 C8 C9 50.1(10) . 119 ? C9 C8 C9 134.2(17) 105 119 ? C9 C8 C9 109.8(13) 24 119 ? C9 C8 N1 112.9(9) . . ? C9 C8 N1 112.9(9) 105 . ? C9 C8 N1 112.9(9) 24 . ? C9 C8 N1 112.9(9) 119 . ? C9 C9 O5 114.3(6) 119 . ? C9 C9 C8 65.0(5) 119 . ? O5 C9 C8 130.6(17) . . ? C9 C9 C9 89.996(6) 119 168_455 ? O5 C9 C9 116.5(14) . 168_455 ? C8 C9 C9 112.9(9) . 168_455 ? C9 C9 C9 49.9(7) 119 57_455 ? O5 C9 C9 127.3(10) . 57_455 ? C8 C9 C9 91.4(10) . 57_455 ? C9 C9 C9 40.1(7) 168_455 57_455 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 13.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.631 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.143 _vrf_RINTA01_PCN-82 ; PROBLEM: The value of Rint is greater than 0.18 Rint given 0.245 RESPONSE: We think the very high Rint value is due to the fact that there are many severely disordered solvent molecules in the pores of PCN-82. We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality and very weak diffraction, the Rint value is high. We are confident the structural framework characterization is valid. ; _vrf_THETM01_PCN-82 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5557 RESPONSE: A full set of data was collected, however the very high angle data was dominated by noise [I/sigma(I) < 1.0] and was omitted. So the diffraction of the crystal was rather weak and there was just no significant intensity at angles > 11.72 deg. We have tried to our best to get big crystal with stronger diffraction, however we fail. This arbitrary theta limit is inappropriate for highly porous structures. It would rule out some MOF structures. ; _vrf_PLAT020_PCN-82 ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.245 RESPONSE: We think the very high Rint value is due to the fact that there are many severely disordered solvent molecules in the pores of PCN-82. We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality and very weak diffraction, the Rint value is high. We are confident the structural framework characterization is valid. ; _vrf_PLAT049_PCN-82 ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.4957 RESPONSE: We have used SQEEZE procedure to remove solvent electron density from pores of the MOF, hence the calculated density does not include this data. ; _vrf_PLAT230_PCN-82 ; PROBLEM: Hirshfeld Test Diff for O1 -- C1 .. 7.3 su RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; _vrf_PLAT241_PCN-82 ; PROBLEM: Check High Ueq as Compared to Neighbors for C6 RESPONSE: Due to very weak diffraction from crystal and the bad quality of the data, the light atoms in framework have very bad thermal parameters. ; _vrf_PLAT412_PCN-82 ; PROBLEM: Short Intra XH3 .. XHn H6 .. H10C .. 1.70 Ang. RESPONSE: Due to freely rotation of the methoxy group and the high symmetry, the methoxy group in framework is highly disordered and occupy eight different positions, which will result in some short intra XH3 .. XHn. ; _vrf_PLAT430_PCN-82 ; PROBLEM: Short Inter D...A Contact O5 .. O5 .. 2.62 Ang. RESPONSE: Due to freely rotation of the methoxy group and the high symmetry, the methoxy group in framework is highly disordered and occupy eight different positions, which will result in some short inter D...A Contact. ; _vrf_RFACG01_PCN-82 ; PROBLEM: The value of the R factor is > 0.10 R factor given 0.125 RESPONSE: We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality the R2 value is high. We are confidant the structural characterization is valid. ; _vrf_RFACR01_PCN-82 ; PROBLEM: The value of the weighted R factor is > 0.25 Weighted R factor given 0.327 RESPONSE: We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality the R2 value is high. We are confidant the structural characterization is valid. ; _vrf_PLAT220_PCN-82 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.7 Ratio RESPONSE: Due to very weak diffraction from crystal and the bad quality of the data, the light atoms in framework have very bad thermal parameters. ; _vrf_PLAT234_PCN-82 ; PROBLEM: Large Hirshfeld Difference Cu2 -- O4 .. 0.16 Ang. RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; _vrf_PLAT242_PCN-82 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Cu1 RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; _vrf_PLAT334_PCN-82 ; PROBLEM: Small Average Benzene C-C Dist. C2 -C7 1.37 Ang. RESPONSE: Quality of the data is not enough to get good bond length parameters. ; _vrf_PLAT341_PCN-82 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0133 Ang RESPONSE: Quality of the data is not enough to get good bond length parameters. ; _vrf_PLAT369_PCN-82 ; PROBLEM: Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.55 Ang. RESPONSE: Quality of the data is not enough to get good bond length parameters. ; data_PCN-81 _database_code_depnum_ccdc_archive 'CCDC 846792' #TrackingRef '7439_web_deposit_cif_file_1_WeigangLu_1317458825.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H20 Cu2 N2 O10' _chemical_formula_sum 'C34 H20 Cu2 N2 O10' _chemical_formula_weight 743.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.3240 0.8257 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/2, -z, x+1/2' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-z-1/2, x-1/2, y' 'y, -z-1/2, x-1/2' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 39.4840(16) _cell_length_b 39.4840(16) _cell_length_c 39.4840(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 61555(4) _cell_formula_units_Z 24 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9273 _cell_measurement_theta_min 2.2035 _cell_measurement_theta_max 14.172 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9024 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9819 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type synchrotron _diffrn_radiation_source 15ID-B _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 543624 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 0.60 _diffrn_reflns_theta_max 14.99 _reflns_number_total 21027 _reflns_number_gt 16504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21027 _refine_ls_number_parameters 433 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3161 _refine_ls_wR_factor_gt 0.2983 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.003 -0.002 48573 28397 ' ' _platon_squeeze_details ; ; 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 0.035426(12) 0.540868(12) 0.263812(12) 0.02733(17) Uani 1 1 d . . . Cu2 Cu 0.025540(11) 0.529290(11) 0.328529(11) 0.02498(16) Uani 1 1 d . . . O1 O 0.03368(7) 0.48148(7) 0.31775(7) 0.0343(6) Uani 1 1 d . . . O2 O 0.03498(7) 0.49361(8) 0.25905(7) 0.0356(7) Uani 1 1 d . . . O3 O 0.03757(7) 0.33318(7) 0.42595(6) 0.0268(6) Uani 1 1 d . . . O4 O 0.03980(7) 0.27697(7) 0.41716(7) 0.0312(6) Uani 1 1 d . . . O5 O 0.03806(7) 0.23948(7) 0.01362(7) 0.0314(6) Uani 1 1 d . . . O6 O 0.02368(7) 0.18560(7) 0.02104(7) 0.0349(7) Uani 1 1 d . . . O7 O -0.01582(8) 0.07866(8) 0.16869(8) 0.0416(7) Uani 1 1 d . . . O8 O -0.03374(8) 0.08733(9) 0.22217(9) 0.0456(8) Uani 1 1 d . . . O9 O 0.04623(9) 0.55063(9) 0.21026(9) 0.0496(8) Uani 1 1 d . . . O10 O 0.01798(9) 0.51909(9) 0.38141(9) 0.0494(8) Uani 1 1 d . . . N1 N 0.03599(12) 0.33305(14) 0.26581(13) 0.0835(18) Uani 1 1 d D . . N2 N 0.01403(12) 0.23230(14) 0.16940(14) 0.0774(16) Uani 1 1 d D . . C1 C 0.03351(9) 0.47190(12) 0.28511(14) 0.0476(12) Uani 1 1 d D . . C2 C 0.03578(6) 0.41161(10) 0.30746(9) 0.0281(8) Uani 1 1 d D . . H2 H 0.0367 0.4192 0.3303 0.034 Uiso 1 1 calc R . . C3 C 0.03405(7) 0.43666(15) 0.28085(14) 0.0579(14) Uani 1 1 d D . . C4 C 0.03270(13) 0.42581(17) 0.24561(15) 0.0687(17) Uani 1 1 d D . . H4 H 0.0318 0.4418 0.2277 0.082 Uiso 1 1 calc R . . C5 C 0.03285(14) 0.3870(2) 0.2384(2) 0.088(2) Uani 1 1 d D . . H5 H 0.0318 0.3776 0.2162 0.106 Uiso 1 1 calc R . . C6 C 0.03479(15) 0.3663(2) 0.2698(2) 0.108(3) Uani 1 1 d D . . C7 C 0.03616(11) 0.37971(15) 0.30174(15) 0.0618(15) Uani 1 1 d D . . C8 C 0.03789(11) 0.35183(14) 0.32261(14) 0.0528(13) Uani 1 1 d D . . C9 C 0.03763(12) 0.32013(14) 0.30081(14) 0.0553(13) Uani 1 1 d D . . C10 C 0.03828(14) 0.2892(2) 0.3137(2) 0.089(2) Uani 1 1 d D . . H10 H 0.0374 0.2705 0.2985 0.106 Uiso 1 1 calc R . . C11 C 0.04015(14) 0.2825(2) 0.3482(2) 0.090(2) Uani 1 1 d D . . H11 H 0.0409 0.2601 0.3570 0.108 Uiso 1 1 calc R . . C12 C 0.04083(11) 0.31170(12) 0.36964(13) 0.0471(11) Uani 1 1 d D . . C13 C 0.03965(9) 0.34512(10) 0.35678(10) 0.0321(9) Uani 1 1 d D . . H13 H 0.0401 0.3635 0.3722 0.038 Uiso 1 1 calc R . . C14 C 0.04232(11) 0.30735(13) 0.40728(13) 0.0469(11) Uani 1 1 d D . . C15 C 0.03132(13) 0.30949(16) 0.24360(16) 0.085(2) Uani 1 1 d D . . C16 C 0.0055(2) 0.3098(2) 0.22100(19) 0.133(4) Uani 1 1 d D . . H16 H -0.0112 0.3271 0.2223 0.160 Uiso 1 1 calc R . . C17 C 0.0033(3) 0.2856(2) 0.1964(2) 0.139(4) Uani 1 1 d D . . H17 H -0.0153 0.2875 0.1812 0.166 Uiso 1 1 calc R . . C18 C 0.02271(14) 0.26142(15) 0.19141(13) 0.0557(13) Uani 1 1 d D . . C19 C 0.05031(18) 0.25899(18) 0.21330(18) 0.091(2) Uani 1 1 d D . . H19 H 0.0659 0.2408 0.2105 0.109 Uiso 1 1 calc R . . C20 C 0.0558(2) 0.2828(2) 0.2396(2) 0.147(5) Uani 1 1 d D . . H20 H 0.0750 0.2813 0.2540 0.176 Uiso 1 1 calc R . . C21 C 0.01186(6) 0.19913(13) 0.12500(13) 0.0519(12) Uani 1 1 d D . . C22 C 0.01795(9) 0.2310(2) 0.1374(2) 0.098(2) Uani 1 1 d D . . C23 C 0.02820(9) 0.26016(14) 0.11403(15) 0.0564(13) Uani 1 1 d D . . H23 H 0.0325 0.2822 0.1228 0.068 Uiso 1 1 calc R . . C24 C 0.03077(11) 0.25416(13) 0.08320(13) 0.0483(12) Uani 1 1 d D . . H24 H 0.0370 0.2718 0.0681 0.058 Uiso 1 1 calc R . . C25 C 0.02433(10) 0.22051(12) 0.07009(12) 0.0442(11) Uani 1 1 d D . . C26 C 0.01505(9) 0.19351(11) 0.09076(11) 0.0383(10) Uani 1 1 d D . . H26 H 0.0110 0.1717 0.0814 0.046 Uiso 1 1 calc R . . C27 C 0.02848(9) 0.21431(10) 0.03194(9) 0.0283(8) Uani 1 1 d D . . C28 C -0.00555(11) 0.14671(13) 0.15848(14) 0.0520(12) Uani 1 1 d D . . H28 H -0.0066 0.1321 0.1394 0.062 Uiso 1 1 calc R . . C29 C 0.00359(12) 0.18012(17) 0.15188(16) 0.0704(17) Uani 1 1 d D . . C30 C 0.00483(14) 0.2025(2) 0.1825(2) 0.092(2) Uani 1 1 d D . . C31 C -0.00298(14) 0.18691(18) 0.21381(19) 0.086(2) Uani 1 1 d D . . H31 H -0.0021 0.2004 0.2337 0.104 Uiso 1 1 calc R . . C32 C -0.01096(11) 0.15622(13) 0.21676(13) 0.0491(12) Uani 1 1 d D . . H32 H -0.0159 0.1480 0.2388 0.059 Uiso 1 1 calc R . . C33 C -0.01312(10) 0.13237(11) 0.18860(11) 0.0372(9) Uani 1 1 d D . . C34 C -0.02162(11) 0.09916(13) 0.19289(12) 0.0451(11) Uani 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 0.0269(3) 0.0289(3) 0.0262(3) 0.00007(18) 0.00009(18) 0.00052(18) Cu2 0.0247(3) 0.0254(3) 0.0248(3) 0.00003(17) -0.00004(17) -0.00031(17) O1 0.0316(15) 0.0375(16) 0.0338(16) -0.0077(12) -0.0062(12) 0.0042(12) O2 0.0401(17) 0.0356(16) 0.0312(15) -0.0003(12) 0.0004(12) 0.0006(12) O3 0.0291(14) 0.0276(14) 0.0237(13) 0.0033(10) 0.0016(10) -0.0019(10) O4 0.0364(16) 0.0273(14) 0.0297(15) 0.0008(11) -0.0003(12) -0.0016(11) O5 0.0370(16) 0.0250(14) 0.0321(15) -0.0032(11) -0.0062(12) -0.0001(11) O6 0.0357(16) 0.0332(16) 0.0356(16) -0.0037(12) -0.0033(12) 0.0040(12) O7 0.0419(18) 0.0415(18) 0.0414(18) -0.0030(14) 0.0042(14) -0.0037(14) O8 0.0461(19) 0.0475(19) 0.0433(19) 0.0003(15) 0.0026(14) 0.0020(15) O9 0.052(2) 0.050(2) 0.047(2) 0.0016(16) 0.0024(16) -0.0039(16) O10 0.049(2) 0.052(2) 0.047(2) 0.0001(16) 0.0021(15) 0.0057(16) N1 0.119(5) 0.064(4) 0.067(4) -0.006(3) -0.011(3) 0.001(3) N2 0.104(5) 0.070(4) 0.058(3) -0.007(3) 0.006(3) -0.011(3) C1 0.050(3) 0.038(3) 0.055(3) 0.002(2) 0.008(2) 0.004(2) C2 0.034(2) 0.032(2) 0.0182(17) -0.0018(14) -0.0017(14) 0.0011(16) C3 0.071(4) 0.053(3) 0.050(3) -0.015(2) 0.000(3) -0.001(3) C4 0.091(5) 0.069(4) 0.046(3) 0.004(3) -0.002(3) -0.014(3) C5 0.109(6) 0.080(5) 0.075(5) -0.009(4) -0.014(4) 0.010(4) C6 0.165(9) 0.071(5) 0.088(6) -0.009(4) -0.011(6) -0.009(5) C7 0.076(4) 0.054(3) 0.056(3) -0.004(3) 0.002(3) 0.001(3) C8 0.062(3) 0.047(3) 0.049(3) -0.003(2) -0.004(2) -0.004(2) C9 0.072(4) 0.046(3) 0.047(3) -0.002(2) 0.011(3) -0.008(3) C10 0.103(6) 0.090(6) 0.072(5) -0.017(4) -0.003(4) -0.010(4) C11 0.115(6) 0.079(5) 0.076(5) 0.001(4) 0.001(4) -0.007(4) C12 0.054(3) 0.039(3) 0.048(3) -0.004(2) -0.001(2) -0.001(2) C13 0.036(2) 0.027(2) 0.033(2) -0.0026(16) -0.0019(17) 0.0016(16) C14 0.047(3) 0.049(3) 0.045(3) 0.002(2) 0.002(2) 0.001(2) C15 0.113(6) 0.053(4) 0.091(6) 0.005(4) -0.021(5) 0.008(4) C16 0.173(11) 0.126(9) 0.101(7) -0.026(6) -0.012(7) 0.036(8) C17 0.176(11) 0.139(10) 0.101(8) 0.003(7) -0.015(7) 0.031(9) C18 0.059(3) 0.062(4) 0.046(3) -0.001(3) -0.003(2) -0.013(3) C19 0.092(6) 0.078(5) 0.101(6) -0.016(4) 0.009(5) 0.007(4) C20 0.118(9) 0.218(14) 0.104(8) -0.027(8) -0.008(6) -0.047(9) C21 0.057(3) 0.054(3) 0.045(3) 0.003(2) 0.001(2) -0.005(2) C22 0.119(7) 0.075(5) 0.101(7) 0.002(4) -0.005(5) 0.003(4) C23 0.066(4) 0.047(3) 0.057(3) -0.004(2) 0.000(3) -0.005(2) C24 0.060(3) 0.041(3) 0.044(3) 0.011(2) 0.002(2) 0.003(2) C25 0.049(3) 0.043(3) 0.041(3) -0.005(2) 0.001(2) -0.007(2) C26 0.039(2) 0.037(2) 0.039(2) -0.0084(18) -0.0048(18) -0.0023(18) C27 0.0256(19) 0.035(2) 0.0244(19) -0.0008(15) 0.0023(14) -0.0053(15) C28 0.054(3) 0.044(3) 0.058(3) -0.011(2) -0.004(2) 0.006(2) C29 0.085(5) 0.071(4) 0.055(4) -0.002(3) 0.003(3) -0.010(3) C30 0.107(6) 0.096(6) 0.072(5) -0.002(4) 0.007(4) -0.028(5) C31 0.116(6) 0.075(5) 0.068(4) -0.002(4) 0.008(4) -0.004(4) C32 0.060(3) 0.043(3) 0.044(3) -0.001(2) 0.001(2) -0.001(2) C33 0.042(2) 0.036(2) 0.033(2) -0.0035(17) 0.0023(18) -0.0042(18) C34 0.042(3) 0.049(3) 0.044(3) 0.001(2) -0.002(2) 0.011(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 Cu1 O2 1.876(3) . ? Cu1 O8 1.917(3) 12 ? Cu1 O4 1.943(3) 17_665 ? Cu1 O5 1.944(3) 8 ? Cu1 O9 2.191(3) . ? Cu1 Cu2 2.6250(7) . ? Cu2 O6 1.935(3) 8 ? Cu2 O3 1.952(3) 17_665 ? Cu2 O1 1.962(3) . ? Cu2 O7 1.990(3) 12 ? Cu2 O10 2.147(3) . ? O1 C1 1.343(6) . ? O2 C1 1.340(6) . ? O3 C14 1.272(6) . ? O3 Cu2 1.952(3) 16_556 ? O4 C14 1.265(6) . ? O4 Cu1 1.943(3) 16_556 ? O5 C27 1.286(5) . ? O5 Cu1 1.944(3) 9_455 ? O6 C27 1.227(5) . ? O6 Cu2 1.935(3) 9_455 ? O7 C34 1.273(6) . ? O7 Cu2 1.990(3) 12_545 ? O8 C34 1.336(6) . ? O8 Cu1 1.917(3) 12_545 ? N1 C15 1.292(9) . ? N1 C6 1.321(10) . ? N1 C9 1.475(7) . ? N2 C22 1.274(10) . ? N2 C30 1.337(9) . ? N2 C18 1.481(8) . ? C1 C3 1.402(7) . ? C2 C7 1.280(7) . ? C2 C3 1.444(7) . ? C2 H2 0.9500 . ? C3 C4 1.457(8) . ? C4 C5 1.560(10) . ? C4 H4 0.9500 . ? C5 C6 1.489(11) . ? C5 H5 0.9500 . ? C6 C7 1.370(10) . ? C7 C8 1.377(8) . ? C8 C13 1.377(7) . ? C8 C9 1.519(7) . ? C9 C10 1.323(9) . ? C10 C11 1.391(10) . ? C10 H10 0.9500 . ? C11 C12 1.430(9) . ? C11 H11 0.9500 . ? C12 C13 1.415(6) . ? C12 C14 1.497(7) . ? C13 H13 0.9500 . ? C15 C16 1.354(8) . ? C15 C20 1.438(8) . ? C16 C17 1.367(8) . ? C16 H16 0.9500 . ? C17 C18 1.239(8) . ? C17 H17 0.9500 . ? C18 C19 1.394(7) . ? C19 C20 1.418(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C29 1.340(8) . ? C21 C22 1.373(10) . ? C21 C26 1.376(7) . ? C22 C23 1.529(10) . ? C23 C24 1.244(7) . ? C23 H23 0.9500 . ? C24 C25 1.448(7) . ? C24 H24 0.9500 . ? C25 C26 1.392(7) . ? C25 C27 1.535(6) . ? C26 H26 0.9500 . ? C28 C33 1.351(7) . ? C28 C29 1.392(8) . ? C28 H28 0.9500 . ? C29 C30 1.496(10) . ? C30 C31 1.415(10) . ? C31 C32 1.258(8) . ? C31 H31 0.9500 . ? C32 C33 1.459(6) . ? C32 H32 0.9500 . ? C33 C34 1.364(7) . ? 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 Cu1 O8 168.68(14) . 12 ? O2 Cu1 O4 90.83(12) . 17_665 ? O8 Cu1 O4 88.68(13) 12 17_665 ? O2 Cu1 O5 85.83(12) . 8 ? O8 Cu1 O5 92.24(13) 12 8 ? O4 Cu1 O5 167.49(12) 17_665 8 ? O2 Cu1 O9 94.59(13) . . ? O8 Cu1 O9 96.73(14) 12 . ? O4 Cu1 O9 94.27(12) 17_665 . ? O5 Cu1 O9 98.01(12) 8 . ? O2 Cu1 Cu2 85.58(9) . . ? O8 Cu1 Cu2 83.13(10) 12 . ? O4 Cu1 Cu2 83.06(8) 17_665 . ? O5 Cu1 Cu2 84.66(8) 8 . ? O9 Cu1 Cu2 177.32(10) . . ? O6 Cu2 O3 168.32(12) 8 17_665 ? O6 Cu2 O1 89.03(12) 8 . ? O3 Cu2 O1 91.19(11) 17_665 . ? O6 Cu2 O7 86.83(13) 8 12 ? O3 Cu2 O7 91.15(12) 17_665 12 ? O1 Cu2 O7 170.51(13) . 12 ? O6 Cu2 O10 97.27(13) 8 . ? O3 Cu2 O10 94.38(12) 17_665 . ? O1 Cu2 O10 93.05(13) . . ? O7 Cu2 O10 95.93(13) 12 . ? O6 Cu2 Cu1 83.15(9) 8 . ? O3 Cu2 Cu1 85.21(8) 17_665 . ? O1 Cu2 Cu1 86.10(9) . . ? O7 Cu2 Cu1 84.93(9) 12 . ? O10 Cu2 Cu1 179.05(10) . . ? C1 O1 Cu2 118.6(3) . . ? C1 O2 Cu1 124.0(3) . . ? C14 O3 Cu2 121.2(3) . 16_556 ? C14 O4 Cu1 123.3(3) . 16_556 ? C27 O5 Cu1 121.7(2) . 9_455 ? C27 O6 Cu2 125.6(3) . 9_455 ? C34 O7 Cu2 123.1(3) . 12_545 ? C34 O8 Cu1 126.6(3) . 12_545 ? C15 N1 C6 142.2(5) . . ? C15 N1 C9 113.2(4) . . ? C6 N1 C9 103.5(6) . . ? C22 N2 C30 112.4(7) . . ? C22 N2 C18 125.7(6) . . ? C30 N2 C18 121.4(6) . . ? O2 C1 O1 123.8(4) . . ? O2 C1 C3 122.8(5) . . ? O1 C1 C3 113.2(5) . . ? C7 C2 C3 123.1(4) . . ? C7 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? C1 C3 C2 126.4(5) . . ? C1 C3 C4 113.9(5) . . ? C2 C3 C4 119.7(5) . . ? C3 C4 C5 117.7(6) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C6 C5 C4 112.8(6) . . ? C6 C5 H5 123.6 . . ? C4 C5 H5 123.6 . . ? N1 C6 C7 119.5(8) . . ? N1 C6 C5 116.6(7) . . ? C7 C6 C5 123.8(7) . . ? C2 C7 C6 122.9(6) . . ? C2 C7 C8 133.0(6) . . ? C6 C7 C8 104.1(6) . . ? C13 C8 C7 138.0(5) . . ? C13 C8 C9 113.4(5) . . ? C7 C8 C9 108.6(5) . . ? C10 C9 N1 132.9(6) . . ? C10 C9 C8 122.8(6) . . ? N1 C9 C8 104.2(5) . . ? C9 C10 C11 123.6(7) . . ? C9 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 115.3(7) . . ? C10 C11 H11 122.4 . . ? C12 C11 H11 122.4 . . ? C13 C12 C11 122.6(5) . . ? C13 C12 C14 117.7(4) . . ? C11 C12 C14 119.7(5) . . ? C8 C13 C12 122.2(4) . . ? C8 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? O4 C14 O3 124.7(4) . . ? O4 C14 C12 114.3(4) . . ? O3 C14 C12 118.5(4) . . ? N1 C15 C16 123.2(6) . . ? N1 C15 C20 120.4(6) . . ? C16 C15 C20 116.1(8) . . ? C15 C16 C17 120.7(10) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 127.8(10) . . ? C18 C17 H17 116.1 . . ? C16 C17 H17 116.1 . . ? C17 C18 C19 116.0(7) . . ? C17 C18 N2 123.2(7) . . ? C19 C18 N2 119.4(6) . . ? C18 C19 C20 121.8(7) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 117.6(8) . . ? C19 C20 H20 121.2 . . ? C15 C20 H20 121.2 . . ? C29 C21 C22 105.9(6) . . ? C29 C21 C26 135.2(6) . . ? C22 C21 C26 118.8(6) . . ? N2 C22 C21 111.6(7) . . ? N2 C22 C23 127.0(7) . . ? C21 C22 C23 121.4(7) . . ? C24 C23 C22 118.0(6) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 122.6(4) . . ? C26 C25 C27 118.8(4) . . ? C24 C25 C27 118.6(4) . . ? C21 C26 C25 118.5(4) . . ? C21 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? O6 C27 O5 124.2(4) . . ? O6 C27 C25 118.4(4) . . ? O5 C27 C25 117.4(4) . . ? C33 C28 C29 128.3(5) . . ? C33 C28 H28 115.9 . . ? C29 C28 H28 115.9 . . ? C21 C29 C28 137.9(6) . . ? C21 C29 C30 107.5(6) . . ? C28 C29 C30 114.6(6) . . ? N2 C30 C31 141.1(7) . . ? N2 C30 C29 102.6(6) . . ? C31 C30 C29 116.3(7) . . ? C32 C31 C30 123.6(7) . . ? C32 C31 H31 118.2 . . ? C30 C31 H31 118.2 . . ? C31 C32 C33 124.5(6) . . ? C31 C32 H32 117.8 . . ? C33 C32 H32 117.8 . . ? C28 C33 C34 124.5(4) . . ? C28 C33 C32 112.8(4) . . ? C34 C33 C32 122.7(4) . . ? O7 C34 O8 119.5(4) . . ? O7 C34 C33 118.3(4) . . ? O8 C34 C33 122.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 14.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.134 _refine_diff_density_min -1.849 _refine_diff_density_rms 0.120 _vrf_PLAT220_PCN-81 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.23 Ratio RESPONSE: Due to very weak diffraction from crystal, the carbon atoms in bridge benzene ring have very high thermal parameters. ; _vrf_PLAT241_PCN-81 ; PROBLEM: Check High Ueq as Compared to Neighbors for C20 RESPONSE: Due to very weak diffraction from crystal, the carbon atoms in bridge benzene ring have very high thermal parameters. ; _vrf_PLAT230_PCN-81 ; PROBLEM: Hirshfeld Test Diff for O1 -- C1 .. 7.34 su RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; _vrf_PLAT232_PCN-81 ; PROBLEM: Hirshfeld Test Diff (M-X) Cu2 -- O10 .. 11.06 su RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; _vrf_PLAT242_PCN-81 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C2 RESPONSE: Crystal had very week diffraction, therefore not many high angle reflections have been detected. Some atoms have no good anisotropic displacement parameters. ; _vrf_PLAT049_PCN-81 ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.48 RESPONSE: We have used SQEEZE procedure to remove solvent electron density from pores of the MOF, hence the calculated density does not include this data. ; _vrf_RFACG01_PCN-81 ; PROBLEM: The value of the R factor is > 0.10 R factor given 0.112 RESPONSE: We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality the R2 value is high. We are confidant the structural characterization is valid. ; _vrf_RFACR01_PCN-81 ; PROBLEM: The value of the weighted R factor is > 0.25 Weighted R factor given 0.316 RESPONSE: We made several attempts to obtain better quality data for this structure, however, due to poor crystal quality the R2 value is high. We are confidant the structural characterization is valid. ; _vrf_PLAT222_PCN-81 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uso(min) ... 5.18 Ratio RESPONSE: The H atoms have very hing thermal parameters due to the high Ueq values for relative C-atoms. ; _vrf_PLAT334_PCN-81 ; PROBLEM: Small Average Benzene C-C Dist. C15 -C20 1.37 Ang. RESPONSE: Quality of the data is not enough to get good bond length parameters. ; _vrf_PLAT041_PCN-81 ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: This is because the atoms from anions and solvents are not included in the structure but are in the formula. ; _vrf_PLAT042_PCN-81 ; PROBLEM: Calc. and Reported MoietyFormula Strings Differ ? RESPONSE: This is because the atoms from anions and solvents are not included in the structure but are in the formula. ; _vrf_PLAT341_PCN-81 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang .. 9 RESPONSE: Quality of the data is not enough to get good bond length parameters. ; _vrf_PLAT369_PCN-81 ; PROBLEM: Long C(sp2)-C(sp2) Bond C4 - C5 ... 1.56 Ang. RESPONSE: Quality of the data is not enough to get good bond length parameters. ; _vrf_PLAT234_PCN-81 ; PROBLEM: Large Hirshfeld Difference C6 -- C7 .. 0.16 Ang. RESPONSE: Quality of the data is not enough to get good anisotropic displacement parameters. ; # end Validation Reply Form