# Electronic Supplementary Material (ESI) for Chemical Science # 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_n1703a _database_code_depnum_ccdc_archive 'CCDC 879693' #TrackingRef 'web_deposit_cif_file_0_OlgaKaragiaridi_1335821057.SALEM1.cif' _audit_creation_date 2012-03-29 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H10 Cd N4' _chemical_formula_sum 'C8 H10 Cd N4' _chemical_formula_weight 274.60 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 229 _space_group_name_H-M_alt 'I m -3 m' _space_group_name_Hall '-I 4 2 3' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z' 3 '-x, y, -z' 4 'x, -y, -z' 5 'z, x, y' 6 'z, -x, -y' 7 '-z, -x, y' 8 '-z, x, -y' 9 'y, z, x' 10 '-y, z, -x' 11 'y, -z, -x' 12 '-y, -z, x' 13 'y, x, -z' 14 '-y, -x, -z' 15 'y, -x, z' 16 '-y, x, z' 17 'x, z, -y' 18 '-x, z, y' 19 '-x, -z, -y' 20 'x, -z, y' 21 'z, y, -x' 22 'z, -y, x' 23 '-z, y, x' 24 '-z, -y, -x' 25 'x+1/2, y+1/2, z+1/2' 26 '-x+1/2, -y+1/2, z+1/2' 27 '-x+1/2, y+1/2, -z+1/2' 28 'x+1/2, -y+1/2, -z+1/2' 29 'z+1/2, x+1/2, y+1/2' 30 'z+1/2, -x+1/2, -y+1/2' 31 '-z+1/2, -x+1/2, y+1/2' 32 '-z+1/2, x+1/2, -y+1/2' 33 'y+1/2, z+1/2, x+1/2' 34 '-y+1/2, z+1/2, -x+1/2' 35 'y+1/2, -z+1/2, -x+1/2' 36 '-y+1/2, -z+1/2, x+1/2' 37 'y+1/2, x+1/2, -z+1/2' 38 '-y+1/2, -x+1/2, -z+1/2' 39 'y+1/2, -x+1/2, z+1/2' 40 '-y+1/2, x+1/2, z+1/2' 41 'x+1/2, z+1/2, -y+1/2' 42 '-x+1/2, z+1/2, y+1/2' 43 '-x+1/2, -z+1/2, -y+1/2' 44 'x+1/2, -z+1/2, y+1/2' 45 'z+1/2, y+1/2, -x+1/2' 46 'z+1/2, -y+1/2, x+1/2' 47 '-z+1/2, y+1/2, x+1/2' 48 '-z+1/2, -y+1/2, -x+1/2' 49 '-x, -y, -z' 50 'x, y, -z' 51 'x, -y, z' 52 '-x, y, z' 53 '-z, -x, -y' 54 '-z, x, y' 55 'z, x, -y' 56 'z, -x, y' 57 '-y, -z, -x' 58 'y, -z, x' 59 '-y, z, x' 60 'y, z, -x' 61 '-y, -x, z' 62 'y, x, z' 63 '-y, x, -z' 64 'y, -x, -z' 65 '-x, -z, y' 66 'x, -z, -y' 67 'x, z, y' 68 '-x, z, -y' 69 '-z, -y, x' 70 '-z, y, -x' 71 'z, -y, -x' 72 'z, y, x' 73 '-x+1/2, -y+1/2, -z+1/2' 74 'x+1/2, y+1/2, -z+1/2' 75 'x+1/2, -y+1/2, z+1/2' 76 '-x+1/2, y+1/2, z+1/2' 77 '-z+1/2, -x+1/2, -y+1/2' 78 '-z+1/2, x+1/2, y+1/2' 79 'z+1/2, x+1/2, -y+1/2' 80 'z+1/2, -x+1/2, y+1/2' 81 '-y+1/2, -z+1/2, -x+1/2' 82 'y+1/2, -z+1/2, x+1/2' 83 '-y+1/2, z+1/2, x+1/2' 84 'y+1/2, z+1/2, -x+1/2' 85 '-y+1/2, -x+1/2, z+1/2' 86 'y+1/2, x+1/2, z+1/2' 87 '-y+1/2, x+1/2, -z+1/2' 88 'y+1/2, -x+1/2, -z+1/2' 89 '-x+1/2, -z+1/2, y+1/2' 90 'x+1/2, -z+1/2, -y+1/2' 91 'x+1/2, z+1/2, y+1/2' 92 '-x+1/2, z+1/2, -y+1/2' 93 '-z+1/2, -y+1/2, x+1/2' 94 '-z+1/2, y+1/2, -x+1/2' 95 'z+1/2, -y+1/2, -x+1/2' 96 'z+1/2, y+1/2, x+1/2' _cell_length_a 30.5539(5) _cell_length_b 30.5539 _cell_length_c 30.5539 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28523.3(5) _cell_formula_units_Z 48 _cell_measurement_reflns_used 3846 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 46.26 _cell_measurement_theta_min 4.09 _exptl_absorpt_coefficient_mu 7.222 _exptl_absorpt_correction_T_max 0.7506 _exptl_absorpt_correction_T_min 0.5669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0680 before and 0.0543 after correction. The Ratio of minimum to maximum transmission is 0.7553. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 0.767 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 6432 _exptl_crystal_size_max 0.061 _exptl_crystal_size_mid 0.057 _exptl_crystal_size_min 0.041 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 16673 _diffrn_reflns_theta_full 53.99 _diffrn_reflns_theta_max 53.99 _diffrn_reflns_theta_min 2.04 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Quazar optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_source microsource _diffrn_source_current 0.65 _diffrn_source_power 0.02925 _diffrn_source_voltage 45.0 _reflns_number_gt 906 _reflns_number_total 1694 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.541 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 72 _refine_ls_number_reflns 1694 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0673 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2216 _refine_ls_wR_factor_ref 0.2352 _refine_special_details ; The disordered C5 and C6 carbon atoms were refined with group anisotropic displacement parameters. The disordered N2 to C5 and C4 to C6 bond distances were restrained to be similar. 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.7500 0.60413(2) 0.10413(2) 0.1156(7) Uani 1 2 d S . . N1 N 0.7287(3) 0.5375(3) 0.1168(3) 0.134(3) Uani 1 1 d . A . N2 N 0.8089(3) 0.6199(4) 0.1376(4) 0.157(4) Uani 1 1 d D . . C1 C 0.7480(4) 0.5000 0.1052(5) 0.121(5) Uani 1 2 d S . . C2 C 0.6935(5) 0.5231(4) 0.1397(7) 0.263(10) Uani 1 1 d . . . H2 H 0.6722 0.5412 0.1534 0.315 Uiso 1 1 calc R A . C3 C 0.7948(9) 0.5000 0.0873(12) 0.36(2) Uani 1 2 d P A 1 H3A H 0.8049 0.4698 0.0838 0.533 Uiso 0.5 1 calc PR A 1 H3B H 0.8140 0.5154 0.1078 0.533 Uiso 0.5 1 calc PR A 1 H3C H 0.7954 0.5148 0.0589 0.533 Uiso 0.5 1 calc PR A 1 C4 C 0.8216(4) 0.6087(6) 0.1784(4) 0.137(6) Uani 1 2 d PD B . C5 C 0.8518(6) 0.6112(6) 0.1138(7) 0.162(7) Uani 0.580(13) 1 d PD B 1 H5 H 0.8557 0.6066 0.0833 0.194 Uiso 0.580(13) 1 calc PR B 1 C5A C 0.8324(8) 0.6629(8) 0.1306(10) 0.162(7) Uani 0.420(13) 1 d PD B 2 H5A H 0.8265 0.6848 0.1093 0.194 Uiso 0.420(13) 1 calc PR B 2 C6 C 0.7817(8) 0.5917(16) 0.2183(8) 0.225(15) Uani 0.290(7) 1 d PD B 1 H6A H 0.7718 0.6172 0.2350 0.337 Uiso 0.290(7) 1 calc PR B 1 H6B H 0.7949 0.5704 0.2382 0.337 Uiso 0.290(7) 1 calc PR B 1 H6C H 0.7567 0.5783 0.2034 0.337 Uiso 0.290(7) 1 calc PR B 1 C6A C 0.8018(13) 0.5570(13) 0.1982(13) 0.225(15) Uani 0.210(7) 1 d PD B 2 H6AA H 0.7751 0.5616 0.2153 0.337 Uiso 0.210(7) 1 calc PR B 2 H6AB H 0.8242 0.5434 0.2167 0.337 Uiso 0.210(7) 1 calc PR B 2 H6AC H 0.7954 0.5378 0.1733 0.337 Uiso 0.210(7) 1 calc PR B 2 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 Cd1 0.1200(10) 0.1134(8) 0.1134(8) -0.0025(6) -0.0099(4) 0.0099(4) N1 0.137(8) 0.138(9) 0.126(7) -0.004(6) 0.006(6) 0.033(7) N2 0.128(8) 0.205(10) 0.137(8) 0.033(8) -0.003(7) -0.010(7) C1 0.060(9) 0.195(19) 0.107(11) 0.000 -0.005(8) 0.000 C2 0.231(16) 0.179(15) 0.38(3) -0.012(13) 0.163(18) -0.027(11) C3 0.22(3) 0.121(16) 0.72(6) 0.000 0.18(3) 0.000 C4 0.129(8) 0.153(14) 0.129(8) -0.013(7) 0.020(13) 0.013(7) C5 0.118(13) 0.186(16) 0.181(15) -0.025(13) 0.001(11) -0.022(11) C5A 0.118(13) 0.186(16) 0.181(15) -0.025(13) 0.001(11) -0.022(11) C6 0.20(2) 0.27(5) 0.20(2) 0.00(2) 0.01(3) 0.00(2) C6A 0.20(2) 0.27(5) 0.20(2) 0.00(2) 0.01(3) 0.00(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 Cd1 N1 2.173(10) 42_654 ? Cd1 N1 2.173(10) . ? Cd1 N2 2.126(10) . ? Cd1 N2 2.126(10) 42_654 ? N1 C1 1.335(10) . ? N1 C2 1.356(14) . ? N2 C4 1.350(11) . ? N2 C5 1.520(18) . ? N2 C5A 1.51(2) . ? C1 N1 1.335(10) 51_565 ? C1 C3 1.53(3) . ? C2 C2 1.41(3) 51_565 ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N2 1.350(11) 70_656 ? C4 C6 1.80(3) . ? C4 C6A 1.80(3) . ? C5 C5 1.49(4) 70_656 ? C5 H5 0.9500 . ? C5A C5A 1.60(5) 70_656 ? C5A H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? 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 Cd1 N1 115.1(5) 42_654 . ? N2 Cd1 N1 112.4(4) 42_654 42_654 ? N2 Cd1 N1 99.0(4) . 42_654 ? N2 Cd1 N1 112.4(4) . . ? N2 Cd1 N1 99.0(4) 42_654 . ? N2 Cd1 N2 119.9(6) 42_654 . ? C1 N1 Cd1 128.6(8) . . ? C1 N1 C2 102.1(12) . . ? C2 N1 Cd1 129.2(8) . . ? C4 N2 Cd1 129.0(9) . . ? C4 N2 C5 98.6(12) . . ? C4 N2 C5A 102.4(17) . . ? C5 N2 Cd1 117.4(10) . . ? C5A N2 Cd1 122.1(12) . . ? C5A N2 C5 71.2(13) . . ? N1 C1 N1 118.0(14) 51_565 . ? N1 C1 C3 120.4(7) . . ? N1 C1 C3 120.4(7) 51_565 . ? N1 C2 C2 108.9(8) . 51_565 ? N1 C2 H2 125.6 . . ? C2 C2 H2 125.6 51_565 . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N2 117.8(17) . 70_656 ? N2 C4 C6 120.3(8) . . ? N2 C4 C6 120.3(8) 70_656 . ? N2 C4 C6A 115.9(11) 70_656 . ? N2 C4 C6A 115.9(11) . . ? C6A C4 C6 44.9(19) . . ? N2 C5 H5 127.1 . . ? C5 C5 N2 105.7(9) 70_656 . ? C5 C5 H5 127.1 70_656 . ? N2 C5A C5A 103.6(12) . 70_656 ? N2 C5A H5A 128.2 . . ? C5A C5A H5A 128.2 70_656 . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C6A H6AA 109.5 . . ? C4 C6A H6AB 109.5 . . ? C4 C6A H6AC 109.5 . . ? H6AA C6A H6AB 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd1 N1 C1 N1 179.8(5) . . . 51_565 ? Cd1 N1 C1 C3 12(2) . . . . ? Cd1 N1 C2 C2 -179.0(7) . . . 51_565 ? Cd1 N2 C4 N2 174.8(6) . . . 70_656 ? Cd1 N2 C4 C6 -20(3) . . . . ? Cd1 N2 C4 C6A 31(3) . . . . ? Cd1 N2 C5 C5 -162.3(5) . . . 70_656 ? Cd1 N2 C5A C5A 171.2(7) . . . 70_656 ? N1 Cd1 N1 C1 45.8(10) 42_654 . . . ? N1 Cd1 N1 C2 -136.6(15) 42_654 . . . ? N1 Cd1 N2 C4 -161.2(13) 42_654 . . . ? N1 Cd1 N2 C4 -39.2(15) . . . . ? N1 Cd1 N2 C5 90.2(10) . . . . ? N1 Cd1 N2 C5 -31.8(10) 42_654 . . . ? N1 Cd1 N2 C5A 174.3(14) . . . . ? N1 Cd1 N2 C5A 52.3(15) 42_654 . . . ? N2 Cd1 N1 C1 165.8(10) 42_654 . . . ? N2 Cd1 N1 C1 -66.5(11) . . . . ? N2 Cd1 N1 C2 111.1(14) . . . . ? N2 Cd1 N1 C2 -16.6(14) 42_654 . . . ? N2 Cd1 N2 C4 76.4(13) 42_654 . . . ? N2 Cd1 N2 C5 -154.2(11) 42_654 . . . ? N2 Cd1 N2 C5A -70.1(15) 42_654 . . . ? C1 N1 C2 C2 -0.9(10) . . . 51_565 ? C2 N1 C1 N1 1.7(19) . . . 51_565 ? C2 N1 C1 C3 -166(2) . . . . ? C4 N2 C5 C5 -19.6(11) . . . 70_656 ? C4 N2 C5A C5A 17.2(11) . . . 70_656 ? C5 N2 C4 N2 39(2) . . . 70_656 ? C5 N2 C4 C6 -156(2) . . . . ? C5 N2 C4 C6A -105(2) . . . . ? C5 N2 C5A C5A -77.7(9) . . . 70_656 ? C5A N2 C4 N2 -34(2) . . . 70_656 ? C5A N2 C4 C6 131(2) . . . . ? C5A N2 C4 C6A -178(2) . . . . ? C5A N2 C5 C5 80.7(12) . . . 70_656 ? _smtbx_masks_special_details ; The solvent masking procedure as implemented in Olex2 was used to remove the electronic contribution of solvent molecules from the refinement. Only the atoms used in the refinement model are reported in the formula here. Total solvent accessible volume / cell = 16997.2 Ang^3^ [59.6%] Total electron count / cell = 6934.0 ; loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.168 -0.564 -0.026 16912.4 6934.0 ? 2 0.000 0.250 0.500 7.1 0.0 ? 3 0.000 0.500 0.250 7.1 0.0 ? 4 0.000 0.500 0.750 7.1 0.0 ? 5 0.000 0.750 0.500 7.1 0.0 ? 6 0.250 0.000 0.500 7.1 0.0 ? 7 0.250 0.500 0.000 7.1 0.0 ? 8 0.500 0.000 0.250 7.1 0.0 ? 9 0.500 0.000 0.750 7.1 0.0 ? 10 0.500 0.250 0.000 7.1 0.0 ? 11 0.500 0.750 0.000 7.1 0.0 ? 12 0.750 0.000 0.500 7.1 0.0 ? 13 0.750 0.500 0.000 7.1 0.0 ? # end Validation Reply Form _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 53.99 Deg. RESPONSE: There was no observable intensity beyone 1.1Ang. resolution despite long exposure times. ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 16621 A**3 RESPONSE: The solvent masking procedure in Olex2 was used to remove electronic contributions from disorderd solvent molecules. ; _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: There was no observable intensity beyone 1.1Ang. resolution despite long exposure times. ; _vrf_ABSMU01_I ; PROBLEM: The ratio of given/expected absorption coefficient lies RESPONSE: In the table above both the calculated and reported Mu values are the same. ;