Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1350 _publ_requested_journal CrystEngComm loop_ _publ_author_name _publ_author_address 'Wonyoung Choe.' ; University of Nebraska-Lincoln Nebraska Center for Materials and Nanoscience 33 Hamilton Hall Lincoln, NE 68588-0304 USA ; _publ_contact_author_name 'Wonyoung Choe' _publ_contact_author_address ; Chemistry University of Nebraska-Lincoln 647 Hamilton Hall P.O.BOX 880304 Lincoln 68588 UNITED STATES OF AMERICA ; _publ_contact_author_email CHOE2@UNLNOTES.UNL.EDU _publ_section_title ; A porphyrin framework with CdI2-type topology ; # Attachment 'c6ch14sq.cif' data_c6ch14sq _database_code_depnum_ccdc_archive 'CCDC 672314' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H34 Co N6 O4 Zn' _chemical_formula_sum 'C56 H34 Co N6 O4 Zn' _chemical_formula_weight 979.19 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' Co Co 0.3494 0.9721 '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' Zn Zn 0.2839 1.4301 '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/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 32.4649(15) _cell_length_b 16.5884(7) _cell_length_c 12.2905(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.198(2) _cell_angle_gamma 90.00 _cell_volume 6617.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9730 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.95 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7898 _exptl_absorpt_correction_T_max 0.9744 _exptl_absorpt_process_details SADABS loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.3640 0.00 0.00 -1.00 0.3990 1.00 0.00 -2.00 0.3340 -1.00 0.00 2.00 0.3230 -1.00 0.00 -1.00 0.2900 1.00 1.00 0.00 0.0460 -1.00 -1.00 0.00 0.0450 -2.00 1.00 0.00 0.0610 2.00 -1.00 0.00 0.0530 1.00 0.00 0.00 0.0480 -1.00 0.00 0.00 0.0680 1.00 -1.00 0.00 0.0660 _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 SMART Apex CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25035 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6029 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0910P)^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 6029 _refine_ls_number_parameters 400 _refine_ls_number_restraints 147 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.031 -0.009 1317.2 336.0 2 0.500 -0.013 0.562 1317.3 336.0 _platon_squeeze_details ; Disordered, independent solvent molecules were eliminated from the refinement using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13]. R factors before data are squeezed: # _refine_ls_R_factor_all 0.2292 # _refine_ls_R_factor_gt 0.2032 # _refine_ls_wR_factor_ref 0.5422 # _refine_ls_wR_factor_gt 0.5173 ; 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 Zn1 Zn 0.165014(15) 0.0000 0.47448(4) 0.02861(17) Uani 1 2 d S . . Co1 Co -0.031078(17) 0.5000 0.92949(5) 0.02736(18) Uani 1 2 d S . . O1 O 0.00012(8) 0.41507(15) 0.84583(19) 0.0441(6) Uani 1 1 d . . . O2 O 0.05163(7) 0.41253(14) 0.96966(18) 0.0377(6) Uani 1 1 d . . . N1 N 0.12387(11) 0.0000 0.6006(3) 0.0316(9) Uani 1 2 d S . . N2 N 0.15751(8) 0.12308(16) 0.4621(2) 0.0331(6) Uani 1 1 d . . . N3 N 0.18996(12) 0.0000 0.3212(3) 0.0328(9) Uani 1 2 d S . . C1 C 0.10740(10) 0.0665(2) 0.6502(3) 0.0349(8) Uani 1 1 d . . . C2 C 0.07956(11) 0.0403(2) 0.7334(3) 0.0426(9) Uani 1 1 d . . . H2 H 0.0641 0.0741 0.7797 0.051 Uiso 1 1 calc R . . C3 C 0.11575(10) 0.1471(2) 0.6245(3) 0.0341(8) Uani 1 1 d . . . C4 C 0.14035(10) 0.1724(2) 0.5377(3) 0.0366(8) Uani 1 1 d . . . C5 C 0.15114(12) 0.2555(2) 0.5158(3) 0.0506(10) Uani 1 1 d . . . H5 H 0.1432 0.3016 0.5560 0.061 Uiso 1 1 calc R . . C6 C 0.17485(12) 0.2542(2) 0.4264(3) 0.0537(11) Uani 1 1 d . . . H6 H 0.1869 0.2997 0.3925 0.064 Uiso 1 1 calc R . . C7 C 0.17855(11) 0.1721(2) 0.3923(3) 0.0398(8) Uani 1 1 d . . . C8 C 0.20002(11) 0.1472(2) 0.3003(3) 0.0399(8) Uani 1 1 d . A . C9 C 0.20431(11) 0.0658(2) 0.2670(3) 0.0376(8) Uani 1 1 d . . . C10 C 0.22705(11) 0.0406(2) 0.1724(3) 0.0441(9) Uani 1 1 d . . . H10 H 0.2395 0.0748 0.1206 0.053 Uiso 1 1 calc R . . C11 C 0.09552(10) 0.21077(19) 0.6912(3) 0.0356(8) Uani 1 1 d . . . C12 C 0.10545(11) 0.2201(2) 0.8013(3) 0.0443(9) Uani 1 1 d U . . H12 H 0.1253 0.1856 0.8349 0.053 Uiso 1 1 calc R . . C13 C 0.08641(10) 0.2795(2) 0.8624(3) 0.0375(8) Uani 1 1 d U . . H13 H 0.0944 0.2871 0.9365 0.045 Uiso 1 1 calc R . . C14 C 0.05624(11) 0.3272(2) 0.8163(3) 0.0382(8) Uani 1 1 d . . . C15 C 0.04611(14) 0.3180(3) 0.7069(3) 0.0598(12) Uani 1 1 d U . . H15 H 0.0253 0.3508 0.6742 0.072 Uiso 1 1 calc R . . C16 C 0.06637(14) 0.2607(3) 0.6448(3) 0.0580(11) Uani 1 1 d U . . H16 H 0.0599 0.2561 0.5693 0.070 Uiso 1 1 calc R . . C17 C 0.03473(10) 0.3905(2) 0.8826(3) 0.0354(8) Uani 1 1 d . . . C18 C 0.22080(12) 0.2119(2) 0.2360(3) 0.0547(11) Uani 1 1 d D . . C19 C 0.2560(3) 0.2505(7) 0.2781(12) 0.056(4) Uani 0.50 1 d PDU A -1 H19 H 0.2674 0.2282 0.3433 0.067 Uiso 0.50 1 calc PR A -1 C20 C 0.2766(3) 0.3177(5) 0.2367(7) 0.048(2) Uani 0.50 1 d PDU A -1 H20 H 0.3023 0.3362 0.2655 0.057 Uiso 0.50 1 calc PR A -1 C21 C 0.2564(2) 0.3548(5) 0.1506(6) 0.051(2) Uani 0.50 1 d PDU A -1 H21 H 0.2677 0.4016 0.1183 0.061 Uiso 0.50 1 calc PR A -1 C22 C 0.2200(3) 0.3239(5) 0.1122(8) 0.056(3) Uani 0.50 1 d PDU A -1 H22 H 0.2070 0.3504 0.0522 0.067 Uiso 0.50 1 calc PR A -1 C23 C 0.2003(5) 0.2559(9) 0.1547(12) 0.056(5) Uani 0.50 1 d PDU A -1 H23 H 0.1737 0.2402 0.1287 0.068 Uiso 0.50 1 calc PR A -1 C19' C 0.2620(3) 0.2298(8) 0.2596(13) 0.060(5) Uani 0.50 1 d PDU A -2 H19' H 0.2774 0.2066 0.3180 0.072 Uiso 0.50 1 calc PR A -2 C20' C 0.2779(3) 0.2868(5) 0.1862(7) 0.058(3) Uani 0.50 1 d PDU A -2 H20' H 0.3044 0.3079 0.2037 0.069 Uiso 0.50 1 calc PR A -2 C21' C 0.2594(3) 0.3149(5) 0.0927(7) 0.053(2) Uani 0.50 1 d PDU A -2 H21' H 0.2736 0.3515 0.0474 0.064 Uiso 0.50 1 calc PR A -2 C22' C 0.2207(3) 0.2902(6) 0.0647(7) 0.054(2) Uani 0.50 1 d PDU A -2 H22' H 0.2065 0.3099 0.0017 0.065 Uiso 0.50 1 calc PR A -2 C23' C 0.2031(5) 0.2338(9) 0.1348(10) 0.052(4) Uani 0.50 1 d PDU A -2 H23' H 0.1778 0.2091 0.1129 0.063 Uiso 0.50 1 calc PR A -2 N4 N 0.22273(11) 0.0000 0.5603(3) 0.0301(8) Uani 1 2 d S . . N5 N 0.41526(11) 0.0000 0.8384(3) 0.0291(8) Uani 1 2 d S . . C26 C 0.29881(14) 0.0000 0.6691(4) 0.0298(10) Uani 1 2 d S . . C29 C 0.33910(14) 0.0000 0.7276(4) 0.0317(10) Uani 1 2 d S . . C24 C 0.2274(2) -0.0294(4) 0.6604(5) 0.0384(17) Uani 0.50 1 d P . . H24 H 0.2036 -0.0495 0.6951 0.046 Uiso 0.50 1 calc PR . . C25 C 0.2643(2) -0.0326(4) 0.7170(5) 0.0414(17) Uani 0.50 1 d P . . H25 H 0.2661 -0.0565 0.7872 0.050 Uiso 0.50 1 calc PR . . C27 C 0.29469(19) 0.0303(4) 0.5652(5) 0.0347(15) Uani 0.50 1 d P . . H27 H 0.3181 0.0509 0.5292 0.042 Uiso 0.50 1 calc PR . . C28 C 0.2570(2) 0.0308(4) 0.5140(5) 0.0354(16) Uani 0.50 1 d P . . H28 H 0.2546 0.0536 0.4433 0.042 Uiso 0.50 1 calc PR . . C30 C 0.3654(2) -0.0638(4) 0.7267(8) 0.0411(18) Uani 0.50 1 d PU . . H30 H 0.3581 -0.1110 0.6870 0.049 Uiso 0.50 1 calc PR . . C31 C 0.4027(2) -0.0604(5) 0.7835(7) 0.0398(18) Uani 0.50 1 d PU . . H31 H 0.4201 -0.1063 0.7811 0.048 Uiso 0.50 1 calc PR . . C32 C 0.3518(3) 0.0696(4) 0.7888(6) 0.0390(18) Uani 0.50 1 d PU . . H32 H 0.3343 0.1153 0.7938 0.047 Uiso 0.50 1 calc PR . . C33 C 0.3905(2) 0.0687(4) 0.8409(7) 0.0375(17) Uani 0.50 1 d PU . . H33 H 0.4001 0.1154 0.8785 0.045 Uiso 0.50 1 calc PR . . 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 Zn1 0.0320(3) 0.0267(3) 0.0276(3) 0.000 0.0110(2) 0.000 Co1 0.0279(3) 0.0278(3) 0.0268(3) 0.000 0.0105(3) 0.000 O1 0.0473(15) 0.0498(15) 0.0356(13) -0.0047(11) 0.0093(11) 0.0168(12) O2 0.0406(13) 0.0378(13) 0.0351(13) -0.0040(10) 0.0096(11) 0.0077(10) N1 0.033(2) 0.029(2) 0.033(2) 0.000 0.0068(17) 0.000 N2 0.0378(16) 0.0284(14) 0.0336(15) 0.0030(11) 0.0126(12) 0.0043(12) N3 0.044(2) 0.031(2) 0.024(2) 0.000 0.0049(17) 0.000 C1 0.0363(18) 0.0357(18) 0.0334(18) -0.0009(14) 0.0143(15) 0.0048(15) C2 0.044(2) 0.0428(18) 0.042(2) -0.0013(16) 0.0244(17) 0.0074(16) C3 0.0361(18) 0.0332(18) 0.0335(18) -0.0039(14) 0.0116(15) 0.0080(14) C4 0.0356(19) 0.0308(18) 0.044(2) -0.0006(15) 0.0108(15) 0.0044(14) C5 0.061(2) 0.0266(19) 0.065(3) 0.0013(17) 0.029(2) 0.0068(17) C6 0.059(2) 0.032(2) 0.071(3) 0.0110(19) 0.034(2) 0.0067(17) C7 0.043(2) 0.0300(18) 0.047(2) 0.0040(15) 0.0159(17) 0.0062(15) C8 0.045(2) 0.038(2) 0.0376(19) 0.0090(15) 0.0149(16) 0.0093(16) C9 0.041(2) 0.0383(19) 0.0336(18) 0.0058(15) 0.0082(16) 0.0032(15) C10 0.052(2) 0.0473(19) 0.0339(19) 0.0100(16) 0.0185(17) 0.0044(17) C11 0.0403(19) 0.0275(17) 0.0393(19) -0.0003(14) 0.0107(15) 0.0004(15) C12 0.043(2) 0.043(2) 0.047(2) -0.0044(17) 0.0060(17) 0.0125(17) C13 0.0407(19) 0.0365(19) 0.0355(19) -0.0061(15) 0.0066(15) 0.0019(15) C14 0.041(2) 0.0384(19) 0.0351(19) -0.0017(15) 0.0117(16) 0.0064(16) C15 0.079(3) 0.065(3) 0.035(2) -0.0028(19) 0.003(2) 0.043(2) C16 0.075(3) 0.064(3) 0.035(2) -0.0034(19) 0.0107(19) 0.030(2) C17 0.039(2) 0.0354(19) 0.0320(18) 0.0013(15) 0.0133(16) 0.0039(15) C18 0.050(2) 0.054(2) 0.061(3) 0.026(2) 0.033(2) 0.017(2) C19 0.027(5) 0.043(7) 0.099(9) 0.028(6) 0.037(5) 0.025(5) C20 0.046(5) 0.046(5) 0.052(6) -0.004(4) 0.017(4) -0.004(4) C21 0.060(5) 0.039(5) 0.054(5) -0.004(4) 0.034(4) -0.018(4) C22 0.095(7) 0.035(5) 0.037(5) 0.002(4) 0.021(5) -0.004(5) C23 0.051(7) 0.045(9) 0.074(8) 0.015(6) 0.027(6) 0.024(6) C19' 0.030(6) 0.056(8) 0.094(8) 0.020(6) 0.028(6) 0.023(5) C20' 0.083(6) 0.046(5) 0.044(5) -0.010(4) 0.013(5) -0.028(5) C21' 0.075(6) 0.036(4) 0.050(5) -0.003(4) 0.038(5) -0.007(4) C22' 0.080(6) 0.047(6) 0.036(5) 0.015(4) 0.024(5) 0.008(5) C23' 0.053(6) 0.043(8) 0.062(7) 0.026(7) 0.044(5) 0.024(5) N4 0.029(2) 0.028(2) 0.034(2) 0.000 0.0118(16) 0.000 N5 0.031(2) 0.039(2) 0.0180(18) 0.000 0.0062(15) 0.000 C26 0.033(2) 0.026(2) 0.030(2) 0.000 0.008(2) 0.000 C29 0.032(2) 0.037(3) 0.027(2) 0.000 0.0092(19) 0.000 C24 0.030(3) 0.047(4) 0.038(4) 0.002(3) 0.014(3) -0.005(3) C25 0.047(4) 0.050(4) 0.027(3) 0.009(3) 0.003(3) -0.001(3) C27 0.029(3) 0.036(4) 0.039(4) 0.003(3) 0.009(3) -0.005(2) C28 0.040(4) 0.034(3) 0.033(3) 0.003(3) 0.010(3) -0.002(3) C30 0.037(4) 0.023(3) 0.063(5) -0.018(4) 0.004(4) 0.001(3) C31 0.034(4) 0.046(4) 0.039(5) -0.011(4) 0.004(4) 0.006(3) C32 0.045(5) 0.036(4) 0.036(4) -0.005(3) 0.012(4) 0.006(3) C33 0.044(5) 0.032(4) 0.036(4) -0.008(3) 0.007(4) 0.001(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 Zn1 N2 2.062(3) 6 ? Zn1 N2 2.062(3) . ? Zn1 N3 2.066(4) . ? Zn1 N1 2.067(4) . ? Zn1 N4 2.131(4) . ? Co1 O1 2.028(2) 6_565 ? Co1 O1 2.028(2) . ? Co1 O2 2.030(2) 2_557 ? Co1 O2 2.030(2) 5_567 ? Co1 N5 2.051(4) 3_455 ? Co1 Co1 2.6323(12) 5_567 ? O1 C17 1.269(4) . ? O2 C17 1.248(4) . ? O2 Co1 2.030(2) 5_567 ? N1 C1 1.373(4) 6 ? N1 C1 1.373(4) . ? N2 C4 1.366(4) . ? N2 C7 1.374(4) . ? N3 C9 1.365(4) 6 ? N3 C9 1.365(4) . ? C1 C3 1.403(5) . ? C1 C2 1.446(4) . ? C2 C2 1.336(7) 6 ? C2 H2 0.9500 . ? C3 C4 1.409(5) . ? C3 C11 1.497(4) . ? C4 C5 1.448(5) . ? C5 C6 1.354(5) . ? C5 H5 0.9500 . ? C6 C7 1.431(5) . ? C6 H6 0.9500 . ? C7 C8 1.403(5) . ? C8 C9 1.419(5) . ? C8 C18 1.501(5) . ? C9 C10 1.452(5) . ? C10 C10 1.346(7) 6 ? C10 H10 0.9500 . ? C11 C16 1.373(5) . ? C11 C12 1.394(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.373(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(5) . ? C14 C17 1.509(5) . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 C19' 1.393(11) . ? C18 C23 1.395(11) . ? C18 C19 1.399(8) . ? C18 C23' 1.407(12) . ? C19 C20 1.402(7) . ? C19 H19 0.9500 . ? C20 C21 1.377(7) . ? C20 H20 0.9500 . ? C21 C22 1.363(10) . ? C21 H21 0.9500 . ? C22 C23 1.403(12) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C19' C20' 1.411(12) . ? C19' H19' 0.9500 . ? C20' C21' 1.367(10) . ? C20' H20' 0.9500 . ? C21' C22' 1.360(10) . ? C21' H21' 0.9500 . ? C22' C23' 1.402(11) . ? C22' H22' 0.9500 . ? C23' H23' 0.9500 . ? N4 C24 1.328(7) 6 ? N4 C24 1.328(7) . ? N4 C28 1.361(7) . ? N4 C28 1.361(7) 6 ? N5 C31 1.269(8) . ? N5 C31 1.269(8) 6 ? N5 C33 1.395(8) 6 ? N5 C33 1.395(8) . ? N5 Co1 2.051(4) 3_545 ? C26 C27 1.376(7) 6 ? C26 C27 1.376(7) . ? C26 C25 1.387(8) . ? C26 C25 1.387(8) 6 ? C26 C29 1.479(6) . ? C29 C30 1.359(7) 6 ? C29 C30 1.359(7) . ? C29 C32 1.434(8) . ? C29 C32 1.434(8) 6 ? C24 C25 1.373(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C27 C28 1.363(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 C31 1.388(10) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.400(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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 Zn1 N2 164.12(15) 6 . ? N2 Zn1 N3 88.89(7) 6 . ? N2 Zn1 N3 88.89(7) . . ? N2 Zn1 N1 88.75(7) 6 . ? N2 Zn1 N1 88.75(7) . . ? N3 Zn1 N1 162.84(15) . . ? N2 Zn1 N4 97.93(8) 6 . ? N2 Zn1 N4 97.93(8) . . ? N3 Zn1 N4 95.40(14) . . ? N1 Zn1 N4 101.77(14) . . ? O1 Co1 O1 88.02(15) 6_565 . ? O1 Co1 O2 168.59(10) 6_565 2_557 ? O1 Co1 O2 89.26(10) . 2_557 ? O1 Co1 O2 89.26(10) 6_565 5_567 ? O1 Co1 O2 168.59(10) . 5_567 ? O2 Co1 O2 91.24(13) 2_557 5_567 ? O1 Co1 N5 98.67(10) 6_565 3_455 ? O1 Co1 N5 98.67(10) . 3_455 ? O2 Co1 N5 92.69(10) 2_557 3_455 ? O2 Co1 N5 92.69(10) 5_567 3_455 ? O1 Co1 Co1 87.12(7) 6_565 5_567 ? O1 Co1 Co1 87.12(7) . 5_567 ? O2 Co1 Co1 81.68(7) 2_557 5_567 ? O2 Co1 Co1 81.68(7) 5_567 5_567 ? N5 Co1 Co1 171.91(10) 3_455 5_567 ? C17 O1 Co1 119.4(2) . . ? C17 O2 Co1 126.1(2) . 5_567 ? C1 N1 C1 106.8(4) 6 . ? C1 N1 Zn1 126.60(19) 6 . ? C1 N1 Zn1 126.60(19) . . ? C4 N2 C7 106.6(3) . . ? C4 N2 Zn1 126.3(2) . . ? C7 N2 Zn1 124.9(2) . . ? C9 N3 C9 106.1(4) 6 . ? C9 N3 Zn1 126.09(19) 6 . ? C9 N3 Zn1 126.09(19) . . ? N1 C1 C3 125.9(3) . . ? N1 C1 C2 109.1(3) . . ? C3 C1 C2 124.9(3) . . ? C2 C2 C1 107.49(19) 6 . ? C2 C2 H2 126.3 6 . ? C1 C2 H2 126.3 . . ? C1 C3 C4 124.7(3) . . ? C1 C3 C11 117.4(3) . . ? C4 C3 C11 117.8(3) . . ? N2 C4 C3 125.6(3) . . ? N2 C4 C5 109.9(3) . . ? C3 C4 C5 124.6(3) . . ? C6 C5 C4 106.3(3) . . ? C6 C5 H5 126.9 . . ? C4 C5 H5 126.9 . . ? C5 C6 C7 107.8(3) . . ? C5 C6 H6 126.1 . . ? C7 C6 H6 126.1 . . ? N2 C7 C8 126.2(3) . . ? N2 C7 C6 109.5(3) . . ? C8 C7 C6 124.3(3) . . ? C7 C8 C9 124.5(3) . . ? C7 C8 C18 116.7(3) . . ? C9 C8 C18 118.8(3) . . ? N3 C9 C8 125.7(3) . . ? N3 C9 C10 110.2(3) . . ? C8 C9 C10 124.0(3) . . ? C10 C10 C9 106.7(2) 6 . ? C10 C10 H10 126.6 6 . ? C9 C10 H10 126.6 . . ? C16 C11 C12 118.7(3) . . ? C16 C11 C3 120.3(3) . . ? C12 C11 C3 121.0(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.3(3) . . ? C13 C14 C17 120.8(3) . . ? C15 C14 C17 119.8(3) . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.9(4) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O2 C17 O1 125.6(3) . . ? O2 C17 C14 117.8(3) . . ? O1 C17 C14 116.6(3) . . ? C19' C18 C23 118.6(9) . . ? C23 C18 C19 113.5(9) . . ? C19' C18 C23' 120.1(9) . . ? C19 C18 C23' 121.6(8) . . ? C19' C18 C8 118.9(6) . . ? C23 C18 C8 122.5(7) . . ? C19 C18 C8 120.3(6) . . ? C23' C18 C8 118.0(7) . . ? C18 C19 C20 128.4(11) . . ? C18 C19 H19 115.8 . . ? C20 C19 H19 115.8 . . ? C21 C20 C19 114.3(9) . . ? C21 C20 H20 122.9 . . ? C19 C20 H20 122.9 . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 124.9(10) . . ? C21 C22 H22 117.6 . . ? C23 C22 H22 117.6 . . ? C18 C23 C22 118.2(12) . . ? C18 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C18 C19' C20' 111.8(10) . . ? C18 C19' H19' 124.1 . . ? C20' C19' H19' 124.1 . . ? C21' C20' C19' 127.3(9) . . ? C21' C20' H20' 116.3 . . ? C19' C20' H20' 116.3 . . ? C22' C21' C20' 119.8(8) . . ? C22' C21' H21' 120.1 . . ? C20' C21' H21' 120.1 . . ? C21' C22' C23' 115.6(10) . . ? C21' C22' H22' 122.2 . . ? C23' C22' H22' 122.2 . . ? C22' C23' C18 123.5(12) . . ? C22' C23' H23' 118.3 . . ? C18 C23' H23' 118.3 . . ? C24 N4 C28 116.5(5) . . ? C24 N4 C28 116.5(5) 6 6 ? C24 N4 Zn1 122.7(3) 6 . ? C24 N4 Zn1 122.7(3) . . ? C28 N4 Zn1 120.8(4) . . ? C28 N4 Zn1 120.8(4) 6 . ? C31 N5 C33 118.6(5) 6 6 ? C31 N5 C33 118.6(5) . . ? C31 N5 Co1 123.3(4) . 3_545 ? C31 N5 Co1 123.3(4) 6 3_545 ? C33 N5 Co1 118.1(4) 6 3_545 ? C33 N5 Co1 118.1(4) . 3_545 ? C27 C26 C25 118.2(5) . . ? C27 C26 C25 118.2(5) 6 6 ? C27 C26 C29 121.3(4) 6 . ? C27 C26 C29 121.3(4) . . ? C25 C26 C29 120.5(4) . . ? C25 C26 C29 120.5(4) 6 . ? C30 C29 C32 117.2(5) . . ? C30 C29 C32 117.2(5) 6 6 ? C30 C29 C26 123.0(4) 6 . ? C30 C29 C26 123.0(4) . . ? C32 C29 C26 119.8(4) . . ? C32 C29 C26 119.8(4) 6 . ? N4 C24 C25 124.4(6) . . ? N4 C24 H24 117.8 . . ? C25 C24 H24 117.8 . . ? C24 C25 C26 118.3(6) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? N4 C28 C27 122.6(6) . . ? N4 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C29 C30 C31 120.4(6) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? N5 C31 C30 124.5(7) . . ? N5 C31 H31 117.8 . . ? C30 C31 H31 117.8 . . ? C33 C32 C29 118.5(6) . . ? C33 C32 H32 120.7 . . ? C29 C32 H32 120.7 . . ? N5 C33 C32 120.7(6) . . ? N5 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.897 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.096 # start Validation Reply Form _vrf_PLAT049_c6ch14sq ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.98 RESPONSE: Three dimensional metal-organic framework structure may have density less than 1.0 gcm-3 becasue of empty voids. In this case the calculated density is based on the model without disorder solvent molecules (DMF or MeOH) in the voids. ; _vrf_PLAT094_c6ch14sq ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 5.40 RESPONSE: The highest residual peak is 1.90 at 0.1416 0.0000 0.4278 which is 0.94 A from Zn1. We suppose that the crystal may suffer from some minor twinning. ; _vrf_PLAT215_c6ch14sq ; PROBLEM: Disordered C19 has ADP max/min Ratio ....... 4.70 RESPONSE: C19 is disordered. ; _vrf_PLAT230_c6ch14sq ; PROBLEM: Hirshfeld Test Diff for C30 - C32_c .. 5.08 su Hirshfeld Test Diff for C32 - C30_c .. 5.08 su RESPONSE: C30 and C32 are disordered. ; _vrf_PLAT250_c6ch14sq ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.07 RESPONSE: The structure has stronger bonding along the porphyrin plane than along its perpendicular direction. Therefore, systematically atoms move more freely along one direction than other two. ; _vrf_PLAT301_c6ch14sq ; PROBLEM: Main Residue Disorder ......................... 20.00 Perc. RESPONSE: This MOF structure suffers from a large fraction of disorder. ; _vrf_PLAT602_c6ch14sq ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: This is a three dimensional metal-organic framework structure, in which there are many voids occupied by disorder solvent molecules (DMF or MeOH in this case). Disordered solvent molecules were squeezed out from the refinement by PLATON. ; _vrf_PLAT860_c6ch14sq ; PROBLEM: Number of Least-Squares Restraints ....... 147 RESPONSE: The following restrains were applied to the disordered parts: SIMU 0.04 0.08 3.0 C30 C31 C32 C33 SIMU 0.04 0.08 3.0 C12 C13 C15 C16 SIMU 0.04 0.08 3.0 C19 C19' SIMU 0.04 0.08 3.0 C23 C23' SIMU 0.04 0.08 3.0 C20 C20' C22 C22' SIMU 0.04 0.08 3.0 C21 C21' DFIX 1.39 0.01 C18 C19 C19 C20 C20 C21 SADI C18 C19 C18 C19' C18 C23 C18 C23' SADI C19 C20 C19' C20' C22 C23 C22' C23' SADI C20 C21 C20' C21' C21 C22 C21' C22' ; # end Validation Reply Form