# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 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 ; 'Eun-Young Choi' '' 'Chunhua Hu' '' 'Curtis A Wray' '' _publ_contact_author_name 'Wonyoung Choe' _publ_contact_author_email CHOE2@UNL.EDU _publ_section_title ; Highly Tunable Metal-Organic Frameworks with Open Metal Centers ; # Attachment 'c7ch30-i4mmmsq.cif' data_c7ch30-i4mmmsq _database_code_depnum_ccdc_archive 'CCDC 652596' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H30 N4 O11 Zn3' _chemical_formula_sum 'C48 H30 N4 O11 Zn3' _chemical_formula_weight 1034.87 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' 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 tetragonal _symmetry_space_group_name_H-M 'I 4/m m m' _symmetry_space_group_name_Hall '-I 4 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+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' '-x+1/2, y+1/2, -z+1/2' 'x+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' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+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' 'x+1/2, -y+1/2, z+1/2' '-x+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' _cell_length_a 16.6814(10) _cell_length_b 16.6814(10) _cell_length_c 17.4944(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4868.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6453 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.26 _exptl_crystal_description star-shape _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8439 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26855 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1393 _reflns_number_gt 1287 _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^)+(0.1370P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1393 _refine_ls_number_parameters 70 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.000 _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 -0.036 0.250 0.215 3155.9 739.3 _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 0.1151 _refine_ls_R_factor_gt 0.1081 _refine_ls_wR_factor_ref 0.3412 _refine_ls_wR_factor_gt 0.3324 ; 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 0.5000 0.5000 0.98061(6) 0.0314(5) Uani 0.50 8 d SP . . Zn2 Zn 0.0000 0.0000 1.08218(4) 0.0352(3) Uani 1 8 d S . . O1 O 0.08470(9) 0.08470(9) 1.06343(16) 0.0685(8) Uani 1 2 d S . . N1 N 0.37777(18) 0.5000 1.0000 0.0429(8) Uani 1 4 d S . . C1 C 0.32863(16) 0.43400(16) 1.0000 0.0467(8) Uani 1 2 d S . . C2 C 0.24608(16) 0.45999(19) 1.0000 0.0579(9) Uani 1 2 d S . . H2 H 0.2002 0.4263 1.0000 0.069 Uiso 1 2 calc SR . . C3 C 0.35445(16) 0.35445(16) 1.0000 0.0488(10) Uani 1 4 d S . . C4 C 0.29066(17) 0.29066(17) 1.0000 0.0479(11) Uani 1 4 d S . . C5 C 0.2487(3) 0.2730(3) 1.0663(3) 0.056(2) Uani 0.50 1 d P . . H5 H 0.2601 0.3013 1.1122 0.068 Uiso 0.50 1 calc PR . . C6 C 0.1902(3) 0.2139(4) 1.0658(3) 0.059(2) Uani 0.50 1 d P . . H6 H 0.1620 0.2020 1.1115 0.070 Uiso 0.50 1 calc PR . . C7 C 0.17236(15) 0.17236(15) 1.0000 0.0451(10) Uani 1 4 d S . . C8 C 0.10882(16) 0.10882(16) 1.0000 0.0458(10) Uani 1 4 d S . . O2 O 0.5000 0.5000 0.8572(5) 0.0448(19) Uani 0.50 8 d SPD . . H2O H 0.5361(8) 0.5361(8) 0.8370(7) 0.054 Uiso 0.25 2 d SPRD . . O3 O 0.0000 0.0000 1.1962(3) 0.0718(18) Uani 1 8 d SD . . H3O H 0.0000 0.0489 1.2210 0.086 Uiso 0.50 2 d SPRD . . 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 0.0154(4) 0.0154(4) 0.0632(13) 0.000 0.000 0.000 Zn2 0.0177(3) 0.0177(3) 0.0703(5) 0.000 0.000 0.000 O1 0.0561(11) 0.0561(11) 0.0932(16) 0.0019(8) 0.0019(8) -0.0381(13) N1 0.0176(15) 0.0180(14) 0.093(2) 0.000 0.000 0.000 C1 0.0193(12) 0.0232(13) 0.097(2) 0.000 0.000 -0.0049(10) C2 0.0153(13) 0.0316(15) 0.127(3) 0.000 0.000 -0.0041(11) C3 0.0250(12) 0.0250(12) 0.096(3) 0.000 0.000 -0.0048(15) C4 0.0218(12) 0.0218(12) 0.100(3) 0.000 0.000 -0.0072(16) C5 0.040(4) 0.037(4) 0.093(2) -0.014(2) 0.007(2) -0.019(4) C6 0.039(4) 0.042(4) 0.095(3) -0.006(2) 0.011(2) -0.021(4) C7 0.0227(11) 0.0227(11) 0.090(3) 0.000 0.000 -0.0057(15) C8 0.0203(11) 0.0203(11) 0.097(3) 0.000 0.000 -0.0017(14) O2 0.035(3) 0.035(3) 0.065(5) 0.000 0.000 0.000 O3 0.066(3) 0.066(3) 0.083(4) 0.000 0.000 0.000 _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 N1 2.067(3) . ? Zn1 O2 2.158(9) . ? Zn2 O3 1.995(5) . ? Zn2 O1 2.025(2) . ? Zn2 Zn2 2.8755(13) 17_557 ? O1 C8 1.247(3) . ? N1 C1 1.373(3) . ? N1 Zn1 2.067(3) 17_667 ? C1 C3 1.395(3) . ? C1 C2 1.444(4) . ? C2 C2 1.335(6) 21_565 ? C2 H2 0.9500 . ? C3 C4 1.505(5) . ? C4 C5 1.387(5) . ? C4 C5 1.387(5) 24 ? C5 C6 1.388(6) . ? C5 H5 0.9500 . ? C6 C7 1.376(5) . ? C6 H6 0.9500 . ? C7 C6 1.376(5) 24 ? C7 C8 1.499(5) . ? O2 H2O 0.9224 . ? O3 H3O 0.9233 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 88.456(11) 19_567 17_667 ? N1 Zn1 N1 161.11(6) 19_567 3_655 ? N1 Zn1 N1 88.456(11) 17_667 3_655 ? N1 Zn1 N1 88.456(11) 19_567 . ? N1 Zn1 N1 161.11(6) 17_667 . ? N1 Zn1 N1 88.456(11) 3_655 . ? N1 Zn1 O2 99.45(3) 19_567 . ? N1 Zn1 O2 99.45(3) 17_667 . ? N1 Zn1 O2 99.45(3) 3_655 . ? N1 Zn1 O2 99.45(3) . . ? O3 Zn2 O1 99.32(8) . 2 ? O3 Zn2 O1 99.32(8) . 3 ? O1 Zn2 O1 88.50(3) 2 3 ? O3 Zn2 O1 99.32(8) . . ? O1 Zn2 O1 161.35(16) 2 . ? O1 Zn2 O1 88.50(3) 3 . ? O3 Zn2 O1 99.32(8) . 4 ? O1 Zn2 O1 88.50(3) 2 4 ? O1 Zn2 O1 161.35(16) 3 4 ? O1 Zn2 O1 88.50(3) . 4 ? O3 Zn2 Zn2 180.000(1) . 17_557 ? O1 Zn2 Zn2 80.68(8) 2 17_557 ? O1 Zn2 Zn2 80.68(8) 3 17_557 ? O1 Zn2 Zn2 80.68(8) . 17_557 ? O1 Zn2 Zn2 80.68(8) 4 17_557 ? C8 O1 Zn2 126.5(2) . . ? C1 N1 C1 106.7(3) . 21_565 ? C1 N1 Zn1 126.09(14) . 17_667 ? C1 N1 Zn1 126.09(14) 21_565 17_667 ? C1 N1 Zn1 126.09(14) . . ? C1 N1 Zn1 126.09(14) 21_565 . ? N1 C1 C3 125.4(3) . . ? N1 C1 C2 109.2(2) . . ? C3 C1 C2 125.5(3) . . ? C2 C2 C1 107.48(17) 21_565 . ? C2 C2 H2 126.3 21_565 . ? C1 C2 H2 126.3 . . ? C1 C3 C1 126.0(4) 7_557 . ? C1 C3 C4 117.02(18) 7_557 . ? C1 C3 C4 117.02(18) . . ? C5 C4 C5 119.1(5) 7_557 . ? C5 C4 C5 113.6(5) 18_557 . ? C5 C4 C5 113.6(5) 7_557 24 ? C5 C4 C5 119.1(5) 18_557 24 ? C5 C4 C3 120.5(2) 7_557 . ? C5 C4 C3 120.5(2) 18_557 . ? C5 C4 C3 120.5(2) . . ? C5 C4 C3 120.5(2) 24 . ? C4 C5 C6 120.0(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C6 118.8(5) 24 18_557 ? C6 C7 C6 113.5(5) . 18_557 ? C6 C7 C6 113.5(5) 24 7_557 ? C6 C7 C6 118.8(5) . 7_557 ? C6 C7 C8 120.6(2) 24 . ? C6 C7 C8 120.6(2) . . ? C6 C7 C8 120.6(2) 18_557 . ? C6 C7 C8 120.6(2) 7_557 . ? O1 C8 O1 125.7(4) 18_557 . ? O1 C8 C7 117.15(19) 18_557 . ? O1 C8 C7 117.15(19) . . ? Zn1 O2 H2O 112.6 . . ? Zn2 O3 H3O 118.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.262 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.108 # start Validation Reply Form _vrf_PLAT049_c7ch30-i4mmmsq ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.71 RESPONSE: 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 disordered solvent molecules (DEF or MeOH) in the voids. ; _vrf_PLAT094_c7ch30-i4mmmsq ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.11 RESPONSE: We do suspect a kind of twinning based on the data and crystal morphology (star-shape). But the list of most disagreeable reflections did not indicate a clear twin law. ; _vrf_PLAT242_c7ch30-i4mmmsq ; PROBLEM: Check Low Ueq as Compared to Neighbors for Zn2 RESPONSE: Zn2 has more rigid bonding environment than its neighbors. ; _vrf_PLAT250_c7ch30-i4mmmsq ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.02 RESPONSE: Like graphite this layer structure has strong bonds along the layer i.e. ab plane and much weaker interactions along the c axis. Therefore, systematically atoms move more freely along the c axis than in the ab plane. ; _vrf_DIFMX01_c7ch30-i4mmmsq ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 2.262 Test value = 2.250 RESPONSE: This indicates a possible twinning. ; _vrf_DIFMX02_c7ch30-i4mmmsq ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. RESPONSE: Highest peak 2.26 is at 0.0000 0.0000 0.1361, which is 0.94 \%A from Zn2. ; _vrf_PLAT076_c7ch30-i4mmmsq ; PROBLEM: Occupancy 0.50 less than 1.0 for Sp.pos . H3O RESPONSE: H3O is disordered in two positions along a 4-fold axis, so its occupancy is refined as 0.25 for each position. ; _vrf_PLAT241_c7ch30-i4mmmsq ; PROBLEM: Check High Ueq as Compared to Neighbors for O1 RESPONSE: The Ueq of O1 should be higher than that of its bonded Zn2 atom, which has six coordinated neighbors. ; _vrf_PLAT301_c7ch30-i4mmmsq ; PROBLEM: Main Residue Disorder ......................... 21.00 Perc. RESPONSE: This MOF structure suffers a large fraction of disorder like many others. ; _vrf_PLAT602_c7ch30-i4mmmsq ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Yes, this MOF contains a lot of voids, which are ocuppied by disordered solvent molecules (DEF or MeOH). ; _vrf_PLAT860_c7ch30-i4mmmsq ; PROBLEM: Note: Number of Least-Squares Restraints ....... 2 RESPONSE: DFIX 0.90 0.02 O2 H2O DFIX 0.90 0.02 O3 H3O ; # end Validation Reply Form # Attachment 'c7ch35-i4mmmsq.cif' data_c7ch35-i4mmmsq _database_code_depnum_ccdc_archive 'CCDC 652597' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H30 N4 O11 Zn3' _chemical_formula_sum 'C48 H30 N4 O11 Zn3' _chemical_formula_weight 1034.87 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' 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 tetragonal _symmetry_space_group_name_H-M 'I 4/m m m' _symmetry_space_group_name_Hall '-I 4 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+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' '-x+1/2, y+1/2, -z+1/2' 'x+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' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+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' 'x+1/2, -y+1/2, z+1/2' '-x+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' _cell_length_a 16.6940(10) _cell_length_b 16.6940(10) _cell_length_c 18.5799(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5178.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6692 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.92 _exptl_crystal_description plate _exptl_crystal_colour dark_purple _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7651 _exptl_absorpt_correction_T_max 0.9636 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29596 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.06 _reflns_number_total 1496 _reflns_number_gt 1195 _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^)+(0.0963P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1496 _refine_ls_number_parameters 98 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _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 -0.036 0.240 0.215 3418.8 805.3 _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 0.1223 _refine_ls_R_factor_gt 0.1022 _refine_ls_wR_factor_ref 0.3491 _refine_ls_wR_factor_gt 0.3232 ; 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 0.5000 0.5000 0.966217(2) 0.04575(1) Uani 0.50 8 d SP . . Zn2 Zn 0.0000 0.0000 0.921728(1) 0.04569(0) Uani 1 8 d SD . . N1 N 0.378427(5) 0.5000 0.981533(6) 0.05081(5) Uani 0.50 2 d SP . . C1 C 0.329095(4) 0.434279(4) 0.983357(7) 0.06293(4) Uani 0.50 1 d P . . C2 C 0.247180(4) 0.459305(4) 0.984109(7) 0.06814(4) Uani 0.50 1 d P . . H2 H 0.2024 0.4262 0.9845 0.082 Uiso 0.50 1 calc PR . . C3 C 0.354379(4) 0.354379(4) 0.983096(9) 0.06089(6) Uani 0.50 2 d SP A . C4 C 0.290756(4) 0.290756(4) 0.985299(6) 0.05073(4) Uani 0.50 2 d SPD . . O1A O 0.083030(7) 0.090339(7) 0.938574(6) 0.06948(2) Uani 0.25 1 d PD . -1 C5A C 0.261090(13) 0.257078(12) 0.922898(7) 0.08537(4) Uani 0.50 2 d SPD A -1 H5A H 0.2769 0.2775 0.8785 0.102 Uiso 0.50 2 calc SPR A -1 C6A C 0.207989(11) 0.193190(11) 0.925567(8) 0.06533(4) Uani 0.25 1 d PD A -1 H6A H 0.1965 0.1644 0.8840 0.078 Uiso 0.25 1 calc PR A -1 O1B O 0.091657(6) 0.073314(7) 0.942747(6) 0.06948(2) Uani 0.25 1 d PD . -2 C5B C 0.254595(12) 0.270057(12) 0.950423(7) 0.08537(4) Uani 0.25 1 d PD . -2 H5B H 0.2719 0.2936 0.9078 0.102 Uiso 0.25 1 calc PR . -2 C6B C 0.192853(11) 0.214663(10) 0.948872(8) 0.06533(4) Uani 0.25 1 d PD . -2 H6B H 0.1650 0.2059 0.9062 0.078 Uiso 0.25 1 calc PR . -2 C7 C 0.172207(3) 0.172207(3) 0.989973(7) 0.05493(4) Uani 0.50 2 d SPD . . C8 C 0.109065(3) 0.109065(3) 0.993906(9) 0.05963(3) Uani 0.50 2 d SPD . . O2 O 0.5000 0.5000 0.845067(13) 0.07175(7) Uani 0.50 8 d SPD . . H2O H 0.535528(18) 0.535528(18) 0.825127(16) 0.086 Uiso 0.25 2 d SPRD . . O3 O 0.0000 0.0000 0.816528(7) 0.09489(5) Uani 1 8 d SD . . H3O H 0.0000 0.0489 0.7918 0.114 Uiso 0.50 2 d SPRD . . 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 0.02508(1) 0.02508(1) 0.08709(2) 0.000 0.000 0.000 Zn2 0.02987(0) 0.02987(0) 0.07732(1) 0.000 0.000 0.000 N1 0.02514(4) 0.02440(3) 0.10290(13) 0.000 -0.00407(5) 0.000 C1 0.02834(3) 0.03308(3) 0.12738(12) 0.00292(5) 0.00111(5) -0.00371(3) C2 0.02716(3) 0.04307(4) 0.13418(12) -0.00080(6) 0.00127(5) -0.00338(3) C3 0.03122(3) 0.03122(3) 0.12022(17) -0.00200(5) -0.00200(5) -0.00600(4) C4 0.03323(3) 0.03323(3) 0.08573(12) -0.00042(4) -0.00042(4) -0.00596(4) O1A 0.04011(3) 0.03937(3) 0.12897(4) -0.01128(4) 0.00731(4) -0.01282(2) C5A 0.10530(7) 0.08009(7) 0.07071(9) 0.00833(7) -0.00757(7) -0.05831(4) C6A 0.05487(6) 0.05626(7) 0.08486(9) -0.01305(6) -0.00129(6) -0.02144(4) O1B 0.04011(3) 0.03937(3) 0.12897(4) -0.01128(4) 0.00731(4) -0.01282(2) C5B 0.10530(7) 0.08009(7) 0.07071(9) 0.00833(7) -0.00757(7) -0.05831(4) C6B 0.05487(6) 0.05626(7) 0.08486(9) -0.01305(6) -0.00129(6) -0.02144(4) C7 0.03614(3) 0.03614(3) 0.09252(9) 0.00183(6) 0.00183(6) -0.01029(4) C8 0.02886(2) 0.02886(2) 0.12117(9) -0.00366(10) -0.00366(10) -0.00142(3) O2 0.06594(8) 0.06594(8) 0.08337(13) 0.000 0.000 0.000 O3 0.08826(5) 0.08826(5) 0.10816(10) 0.000 0.000 0.000 _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 N1 2.04939(14) 2_665 ? Zn1 N1 2.04939(14) 4_565 ? Zn1 N1 2.04939(14) . ? Zn1 N1 2.04939(14) 3_655 ? Zn1 O2 2.2510(3) . ? Zn2 O3 1.9546(2) . ? Zn2 O1B 1.99793(16) 24 ? Zn2 O1B 1.99793(16) 2 ? Zn2 O1B 1.99793(16) . ? Zn2 O1B 1.99793(16) 23 ? Zn2 O1B 1.99793(16) 22 ? Zn2 O1B 1.99793(16) 3 ? Zn2 O1B 1.99793(16) 4 ? Zn2 O1B 1.99793(16) 21 ? Zn2 O1A 2.07212(17) 24 ? Zn2 O1A 2.07212(17) . ? Zn2 O1A 2.07212(17) 23 ? N1 C1 1.37227(12) . ? N1 C1 1.37227(11) 21_565 ? N1 Zn1 2.24977(14) 17_667 ? C1 C3 1.39905(11) . ? C1 C2 1.42995(14) . ? C2 C2 1.35872(17) 21_565 ? C2 H2 0.9300 . ? C3 C1 1.39905(12) 24 ? C3 C4 1.50263(16) . ? C4 C5A 1.3804(2) . ? C4 C5B 1.3821(2) 18_557 ? C4 C5B 1.3821(2) 7_557 ? O1A C8 1.1591(2) . ? C5A C6A 1.3877(3) . ? C5A H5A 0.9300 . ? C6A C7 1.3826(2) . ? C6A H6A 0.9300 . ? O1B C8 1.1594(2) . ? C5B C4 1.3821(2) 18_557 ? C5B C6B 1.3851(3) . ? C5B H5B 0.9300 . ? C6B C7 1.3828(2) 18_557 ? C6B H6B 0.9300 . ? C7 C6A 1.3826(2) 24 ? C7 C6B 1.3828(2) 18_557 ? C7 C6B 1.3828(2) 7_557 ? C7 C8 1.49250(14) . ? C8 O1A 1.1591(2) 24 ? C8 O1B 1.1594(2) 24 ? C8 O1B 1.3513(2) 18_557 ? C8 O1B 1.3513(2) 7_557 ? O2 H2O 0.9170 . ? O3 H3O 0.9367 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 88.895(1) 2_665 4_565 ? N1 Zn1 N1 164.037(7) 2_665 . ? N1 Zn1 N1 88.895(1) 4_565 . ? N1 Zn1 N1 88.895(1) 2_665 3_655 ? N1 Zn1 N1 164.037(7) 4_565 3_655 ? N1 Zn1 N1 88.895(1) . 3_655 ? N1 Zn1 O2 97.982(3) 2_665 . ? N1 Zn1 O2 97.982(3) 4_565 . ? N1 Zn1 O2 97.982(3) . . ? N1 Zn1 O2 97.982(3) 3_655 . ? O3 Zn2 O1B 101.272(3) . 24 ? O3 Zn2 O1B 101.272(3) . 2 ? O1B Zn2 O1B 154.170(7) 24 2 ? O3 Zn2 O1B 101.272(3) . . ? O1B Zn2 O1B 157.456(7) 2 . ? O3 Zn2 O1B 101.272(3) . 23 ? O1B Zn2 O1B 157.456(7) 24 23 ? O1B Zn2 O1B 154.170(7) . 23 ? O3 Zn2 O1B 101.272(3) . 22 ? O1B Zn2 O1B 87.810(1) 24 22 ? O1B Zn2 O1B 75.553(6) 2 22 ? O1B Zn2 O1B 99.966(6) . 22 ? O1B Zn2 O1B 87.810(1) 23 22 ? O3 Zn2 O1B 101.272(3) . 3 ? O1B Zn2 O1B 75.553(6) 24 3 ? O1B Zn2 O1B 87.810(1) 2 3 ? O1B Zn2 O1B 87.810(1) . 3 ? O1B Zn2 O1B 99.966(6) 23 3 ? O3 Zn2 O1B 101.272(3) . 4 ? O1B Zn2 O1B 99.966(6) 24 4 ? O1B Zn2 O1B 87.810(1) 2 4 ? O1B Zn2 O1B 87.810(1) . 4 ? O1B Zn2 O1B 75.553(6) 23 4 ? O1B Zn2 O1B 154.170(7) 22 4 ? O1B Zn2 O1B 157.456(7) 3 4 ? O3 Zn2 O1B 101.272(3) . 21 ? O1B Zn2 O1B 87.810(1) 24 21 ? O1B Zn2 O1B 99.966(6) 2 21 ? O1B Zn2 O1B 75.553(6) . 21 ? O1B Zn2 O1B 87.810(1) 23 21 ? O1B Zn2 O1B 157.456(7) 22 21 ? O1B Zn2 O1B 154.170(7) 3 21 ? O3 Zn2 O1A 98.688(3) . 24 ? O1B Zn2 O1A 159.661(5) 2 24 ? O1B Zn2 O1A 158.221(5) 23 24 ? O1B Zn2 O1A 96.782(5) 22 24 ? O1B Zn2 O1A 84.492(5) 3 24 ? O1B Zn2 O1A 92.116(5) 4 24 ? O1B Zn2 O1A 79.796(5) 21 24 ? O3 Zn2 O1A 98.688(3) . . ? O1B Zn2 O1A 158.222(5) 2 . ? O1B Zn2 O1A 159.661(5) 23 . ? O1B Zn2 O1A 92.116(5) 22 . ? O1B Zn2 O1A 79.796(5) 3 . ? O1B Zn2 O1A 96.782(5) 4 . ? O1B Zn2 O1A 84.492(5) 21 . ? O3 Zn2 O1A 98.688(3) . 23 ? O1B Zn2 O1A 158.221(5) 24 23 ? O1B Zn2 O1A 4.654(5) 2 23 ? O1B Zn2 O1A 159.661(5) . 23 ? O1B Zn2 O1A 9.004(5) 23 23 ? O1B Zn2 O1A 79.796(5) 22 23 ? O1B Zn2 O1A 92.116(5) 3 23 ? O1B Zn2 O1A 84.492(5) 4 23 ? O1B Zn2 O1A 96.782(5) 21 23 ? O1A Zn2 O1A 162.624(6) 24 23 ? O1A Zn2 O1A 161.971(6) . 23 ? C1 N1 C1 106.168(8) . 21_565 ? C1 N1 Zn1 126.709(4) . . ? C1 N1 Zn1 126.709(4) 21_565 . ? C1 N1 Zn1 122.055(5) . 17_667 ? C1 N1 Zn1 122.055(5) 21_565 17_667 ? N1 C1 C3 125.529(7) . . ? N1 C1 C2 109.912(6) . . ? C3 C1 C2 124.549(7) . . ? C2 C2 C1 106.988(4) 21_565 . ? C2 C2 H2 126.5 21_565 . ? C1 C2 H2 126.5 . . ? C1 C3 C1 125.118(9) 24 . ? C1 C3 C4 117.423(4) 24 . ? C1 C3 C4 117.423(5) . . ? C5A C4 C5B 117.855(14) . 18_557 ? C5A C4 C5B 117.269(14) . 7_557 ? C5A C4 C3 121.238(13) . . ? C5B C4 C3 120.598(13) 18_557 . ? C5B C4 C3 120.598(13) 7_557 . ? C8 O1A Zn2 125.527(10) . . ? C4 C5A C6A 120.809(13) . . ? C4 C5A H5A 119.6 . . ? C6A C5A H5A 119.6 . . ? C7 C6A C5A 120.109(13) . . ? C7 C6A H6A 119.9 . . ? C5A C6A H6A 119.9 . . ? C8 O1B Zn2 131.880(10) . . ? C4 C5B C6B 120.661(14) 18_557 . ? C4 C5B H5B 119.7 18_557 . ? C6B C5B H5B 119.7 . . ? C7 C6B C5B 120.703(14) 18_557 . ? C7 C6B H6B 119.6 18_557 . ? C5B C6B H6B 119.6 . . ? C6A C7 C6B 115.252(13) 24 18_557 ? C6A C7 C6B 118.271(13) . 18_557 ? C6A C7 C6B 118.271(13) 24 7_557 ? C6A C7 C6B 115.252(12) . 7_557 ? C6A C7 C8 121.766(13) 24 . ? C6A C7 C8 121.766(13) . . ? C6B C7 C8 119.854(13) 18_557 . ? C6B C7 C8 119.854(14) 7_557 . ? O1A C8 O1B 123.293(11) 24 18_557 ? O1A C8 O1B 124.944(11) . 18_557 ? O1B C8 O1B 119.518(13) 24 18_557 ? O1B C8 O1B 115.648(13) . 18_557 ? O1A C8 O1B 124.944(11) 24 7_557 ? O1A C8 O1B 123.293(11) . 7_557 ? O1B C8 O1B 115.648(13) 24 7_557 ? O1B C8 O1B 119.518(13) . 7_557 ? O1A C8 C7 114.323(14) 24 . ? O1A C8 C7 114.323(14) . . ? O1B C8 C7 120.030(14) 24 . ? O1B C8 C7 120.030(14) . . ? O1B C8 C7 120.429(12) 18_557 . ? O1B C8 C7 120.429(12) 7_557 . ? Zn1 O2 H2O 113.8 . . ? Zn2 O3 H3O 119.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.641 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.061 # start Validation Reply Form _vrf_PLAT230_c7ch35-i4mmmsq ; PROBLEM: Hirshfeld Test Diff for C7 - C6B .. 167.46 su Hirshfeld Test Diff for C6B - C5A_u .. 101.74 su Hirshfeld Test Diff for N1 - C1 .. 28.87 su Hirshfeld Test Diff for C1 - C2_m .. 18.71 su Hirshfeld Test Diff for C2 - C1_m .. 18.71 su Hirshfeld Test Diff for C3 - C4 .. 19.01 su Hirshfeld Test Diff for C4 - C5A .. 71.67 su Hirshfeld Test Diff for C4 - C5B .. 22.54 su Hirshfeld Test Diff for C5A - C6A .. 24.54 su Hirshfeld Test Diff for C5A - C6B .. 33.99 su Hirshfeld Test Diff for C7 - C6A .. 54.68 su Hirshfeld Test Diff for C5B - C6A .. 56.61 su Hirshfeld Test Diff for C5B - C6B .. 23.06 su Hirshfeld Test Diff for C5B - C4_h .. 85.84 su Hirshfeld Test Diff for C5B - C5A_u .. 90.56 su Hirshfeld Test Diff for C5B - C6A_u .. 49.89 su Hirshfeld Test Diff for C6A - C7_h .. 10.38 su Hirshfeld Test Diff for C6A - C5A_u .. 51.13 su Hirshfeld Test Diff for C6A - C5B_u .. 49.89 su Hirshfeld Test Diff for C6A - C6B_u .. 58.76 su Hirshfeld Test Diff for C6B - C7_h .. 76.58 su Hirshfeld Test Diff for C6B - C6A_u .. 58.76 su RESPONSE: These atoms are disordered. ; _vrf_PLAT049_c7ch35-i4mmmsq ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.66 RESPONSE: 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 disordered solvent molecules (DEF or MeOH) in the voids. ; _vrf_PLAT242_c7ch35-i4mmmsq ; PROBLEM: Check Low Ueq as Compared to Neighbors for Zn2 Check Low Ueq as Compared to Neighbors for Zn1 RESPONSE: Zn2 and Zn1 have more rigid bonding environments than its neighbors. ; _vrf_PLAT301_c7ch35-i4mmmsq ; PROBLEM: Main Residue Disorder ......................... 36.00 Perc. RESPONSE: This MOF structure suffers a large fraction of disorder. ; _vrf_PLAT420_c7ch35-i4mmmsq ; PROBLEM: D-H Without Acceptor O3 - *H3O ... ? RESPONSE: The possible acceptors are solvent molecules (DEF or MEOH). They are disordered and squeezed by PLATON without refinment. ; _vrf_CHEMW03_c7ch35-i4mmmsq ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1034.87 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 52.00 624.57 H 1.01 34.00 34.27 N 14.01 4.00 56.03 O 16.00 11.00 175.99 Zn 65.39 3.00 196.17 Calculated formula weight 1087.03 RESPONSE: Shelx and Platon have different algorithms to count the number of disordered atoms at special positions. ; _vrf_PLAT076_c7ch35-i4mmmsq ; PROBLEM: Occupancy 0.50 less than 1.0 for Sp.pos . N1 Occupancy 0.50 less than 1.0 for Sp.pos . C3 Occupancy 0.50 less than 1.0 for Sp.pos . C4 Occupancy 0.50 less than 1.0 for Sp.pos . C5A Occupancy 0.50 less than 1.0 for Sp.pos . H5A Occupancy 0.50 less than 1.0 for Sp.pos . C7 Occupancy 0.50 less than 1.0 for Sp.pos . C8 Occupancy 0.50 less than 1.0 for Sp.pos . H3O RESPONSE: These atoms are disordered and refined with half occupancy. ; _vrf_PLAT241_c7ch35-i4mmmsq ; PROBLEM: Check High Ueq as Compared to Neighbors for C5A Check High Ueq as Compared to Neighbors for C5B RESPONSE: C5A and C5B are strongly disordered. ; _vrf_PLAT250_c7ch35-i4mmmsq ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.91 RESPONSE: Like graphite this layer structure has strong bonds along the layer i.e. ab plane and much weaker interactions along the c axis. Therefore, systematically atoms move more freely along the c axis than in the ab plane. ; _vrf_PLAT602_c7ch35-i4mmmsq ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Yes, this MOF contains a lot of voids, which are ocuppied by disordered solvent molecules (DEF or MeOH). ; _vrf_FORMU01_c7ch35-i4mmmsq ; PROBLEM: There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C48 H30 N4 O11 Zn3 Atom count from the _atom_site data: C52 H34 N4 O11 Zn3 RESPONSE: Shelx and Platon have different algorithms to count the number of disordered atoms at special positions. ; _vrf_CELLZ01_c7ch35-i4mmmsq ; PROBLEM: Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C48 H30 N4 O11 Zn3 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 96.00 104.00 -8.00 H 60.00 68.00 -8.00 N 8.00 8.00 0.00 O 22.00 22.00 0.00 Zn 6.00 6.00 0.00 RESPONSE: Shelx and Platon have different algorithms to count the number of disordered atoms at special positions. ; _vrf_PLAT860_c7ch35-i4mmmsq ; PROBLEM: Note: Number of Least-Squares Restraints ....... 10 RESPONSE: DFIX 1.39 0.01 C4 C5A C7 C6A DFIX 1.39 0.01 C4_$4 C5B C7_$4 C6B DFIX 1.46 0.01 C7 C8 DFIX 2.00 0.01 Zn2 O1B DFIX 0.90 0.02 O2 H2O DFIX 0.90 0.02 O3 H3O DFIX 1.16 0.01 C8 O1A C8 O1B EADP C5A C5B EADP C6A C6B EADP O1A O1B ; # end Validation Reply Form