data_Co-BDTriP-DMF _audit_creation_date 2016-02-03 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common 'Co-BDTriP-DMF' _chemical_name_systematic ? _chemical_formula_moiety '(C140 H140 Cl3 Co12 N76 O12) Co1.4 O1.4' _chemical_formula_sum 'C140 H140 Cl3 Co14.40 N76 O14.40' _chemical_formula_weight 4072.57 _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' 0.0040 0.0020 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 221 _space_group_name_H-M_alt 'P m -3 m' _space_group_name_Hall '-P 4 2 3' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 18.8345(7) _cell_length_b 18.8345(7) _cell_length_c 18.8345(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6681.3(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9810 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.174 _cell_measurement_theta_min 2.636 _shelx_estimated_absorpt_T_max 0.911 _shelx_estimated_absorpt_T_min 0.911 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1253 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.9275. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1683 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; An as-synthesized DMF-solvated single crystal of Co-BDTriP (Co3[(Co4Cl)3(BDTriP)8]2; H3BDTriP = 4,4'-(5-(1H-pyrazol-4-yl)-1,3-phenylene)bis(1H-1,2,3-triazole)) were mounted on a MiTeGen loop and frozen at a temperature of 100 K under a stream of flowing N2. Data was collected at Beamline 11.3.1 at the Advanced Light Source, Lawrence Berkeley National Laboratory using synchrotron radiation (lamda = 0.7749 angstroms) and a Bruker PHOTON100 CMOS diffractometer. ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_unetI/netI 0.0122 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 97274 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 27.706 _diffrn_reflns_theta_max 30.174 _diffrn_reflns_theta_min 2.358 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker PHOTON100 CMOS diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'channel-cut Si(111) crystal' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_source 'Advanced Light Source station 11.3.1' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1404 _reflns_number_total 1577 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX 2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.773 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.079 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0462 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+6.3029P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1537 _refine_ls_wR_factor_ref 0.1590 _refine_special_details ; Thermal parameters were refined anisotropically for all non-hydrogen atoms. Hydrogen atoms were placed in ideal positions and refined using a riding model. Co-BDTriP is an anionic framework ([(Co4Cl)3(BDTriP)8]3-) and, thus, contains charge-balancing cations. These cations are likely Co(II) (three Co(II) per two [(Co4Cl)3(BDTriP)8]3-). The location of these charge-balancing Co(II) cations (Co2) was assigned to electron density found between two triazolate groups that are adjacent to each other on the [Co4Cl]7+ cluster, corresponding to a model where nitrogen atoms on adjacent triazolate groups are coordinated to Co. Electron density near the charge-balancing Co centers was assigned to be an oxygen atom (O2) from a solvent molecule coordinated to Co. The site occupancy factors of Co2 and O2 were refined using an independent free variable then were fixed in the final refinement. This gave a chemical occupancy of 10% for both, corresponding to 4.8 extra-framework Co centers per formula unit. Each linker has two triazolate groups and one pyrazolate group that are disordered, due to the three-fold and mirror symmetery of the structure. Thus, C1 and N2 on the triazolate/pyrazolate rings were restrained to have the same coordinates and displacement parameters. The site occupancy factors of C1 and N2 were fixed to reflect a statistical distribution, corresponding to a chemical occupancy of 66.7% for C1 and 33.3% for N2. DMF coordinated to the framework Co centers was severely disordered. Only the coordinated oxygen of the DMF molecules could be located and modeled. The atoms that comprise the rest of the DMF fragment were omitted from the refinement, but not the formula. Disorder of residual solvent within the pores of the crystal was extensive and could not be modeled. Consequently, the unassigned electron density was accounted for using SQUEEZE as implemented in the PLATON interface. Refinement before SQUEEZE was applied gave an R1 of 12.68% (wR2 = 43.90%), while applying SQUEEZE resulted in an R1 of 4.62% (wR2 = 15.90%). ; _vrf_CHEMW03_djx031s_sq ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The given molecular weight is higher because it includes atoms that could not be located in the electron density difference map (from the disordered DMF coordinated to the framework Co sites), which were not included in the refinement. ; _vrf_PLAT308_djx031s_sq ; PROBLEM: Single Bonded Metal Atom (Unusual !) ........... RESPONSE: This metal atom is Co2 which is not single bonded in the structure but coordinated to two triazolate nitrogens and a solvent oxygen atom. Additional ligands coordinated to this Co center could not be located in the electron density difference map. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Shared sites {N2, C1} 3. Uiso/Uaniso restraints and constraints Co2 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(N2) = Uanis(C1) 4. Others Fixed Sof: C1(0.6667) H1(0.6667) Co2(0.05) O2(0.05) N2(0.3333) 5.a Aromatic/amide H refined with riding coordinates: C4(H4), C1(H1) ; _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36808(4) 0.0000 0.5000 0.0317(2) Uani 1 4 d S T P A . Cl1 Cl 0.5000 0.0000 0.5000 0.0315(5) Uani 1 16 d S T P . . O1 O 0.2488(2) 0.0000 0.5000 0.0596(11) Uani 1 4 d S T P . . N1 N 0.37154(10) 0.07406(9) 0.57762(11) 0.0353(5) Uani 1 1 d . . . . . C2 C 0.35155(13) 0.16474(16) 0.64845(13) 0.0348(7) Uani 1 2 d S T P . . C3 C 0.32005(12) 0.22839(17) 0.67995(12) 0.0335(7) Uani 1 2 d S T P A . C4 C 0.34951(18) 0.25930(12) 0.74070(12) 0.0340(7) Uani 1 2 d S T P . . H4 H 0.3905 0.2385 0.7615 0.041 Uiso 1 2 calc RS T P A . C1 C 0.32826(12) 0.12903(10) 0.58949(11) 0.0368(5) Uani 0.6667 1 d . . . A 1 H1 H 0.2880 0.1413 0.5617 0.044 Uiso 0.6667 1 calc R . . A 1 Co2 Co 0.2808(4) 0.1567(3) 0.5000 0.0558(14) Uani 0.1 2 d S TU P A 2 O2 O 0.1736(11) 0.1736(11) 0.5000 0.065(7) Uani 0.2 4 d S TU P A 2 N2 N 0.32826(12) 0.12903(10) 0.58949(11) 0.0368(5) Uani 0.3333 1 d . . . A 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 Co1 0.0455(4) 0.0150(3) 0.0345(4) 0.000 0.000 0.000 Cl1 0.0392(7) 0.0162(8) 0.0392(7) 0.000 0.000 0.000 O1 0.070(3) 0.055(2) 0.053(2) 0.000 0.000 0.000 N1 0.0450(12) 0.0207(8) 0.0403(10) 0.0029(7) -0.0019(8) -0.0003(7) C2 0.0380(10) 0.0283(15) 0.0380(10) -0.0006(9) -0.0020(13) 0.0006(9) C3 0.0351(10) 0.0303(15) 0.0351(10) -0.0025(8) -0.0018(12) 0.0025(8) C4 0.0346(16) 0.0338(10) 0.0338(10) -0.0001(12) -0.0065(9) 0.0065(9) C1 0.0465(12) 0.0262(10) 0.0376(11) 0.0000(8) -0.0030(9) 0.0052(9) Co2 0.088(4) 0.047(3) 0.032(2) 0.000 0.000 0.014(3) O2 0.088(11) 0.088(11) 0.020(8) 0.000 0.000 0.049(13) N2 0.0465(12) 0.0262(10) 0.0376(11) 0.0000(8) -0.0030(9) 0.0052(9) _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 Co1 Cl1 2.4846(7) . ? Co1 O1 2.248(5) . ? Co1 N1 2.022(2) 26_556 ? Co1 N1 2.022(2) 27 ? Co1 N1 2.022(2) 4_556 ? Co1 N1 2.022(2) . ? Cl1 Co1 2.4846(7) 45_655 ? Cl1 Co1 2.4846(7) 21_556 ? Cl1 Co1 2.4846(7) 25_656 ? N1 N1 1.355(4) 46_656 ? N1 C1 1.337(3) . ? N1 N2 1.337(3) . ? C2 C3 1.463(4) . ? C2 C1 1.370(3) . ? C2 C1 1.370(3) 46_656 ? C2 N2 1.370(3) 46_656 ? C2 N2 1.370(3) . ? C3 C4 1.399(2) . ? C3 C4 1.399(2) 11_566 ? C4 C3 1.399(2) 8_656 ? C4 H4 0.9500 . ? C1 H1 0.9500 . ? Co2 O2 2.044(18) . ? Co2 N2 1.978(4) . ? Co2 N2 1.978(4) 26_556 ? O2 Co2 2.044(18) 13_556 ? 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 Co1 Cl1 180.0 . . ? N1 Co1 Cl1 88.16(6) 4_556 . ? N1 Co1 Cl1 88.16(6) 27 . ? N1 Co1 Cl1 88.16(6) . . ? N1 Co1 Cl1 88.16(6) 26_556 . ? N1 Co1 O1 91.84(6) 4_556 . ? N1 Co1 O1 91.84(6) . . ? N1 Co1 O1 91.84(6) 27 . ? N1 Co1 O1 91.84(6) 26_556 . ? N1 Co1 N1 87.26(10) 27 . ? N1 Co1 N1 176.31(12) 4_556 . ? N1 Co1 N1 87.26(10) 4_556 26_556 ? N1 Co1 N1 92.62(10) 26_556 . ? N1 Co1 N1 92.62(10) 4_556 27 ? N1 Co1 N1 176.32(12) 27 26_556 ? Co1 Cl1 Co1 90.0 45_655 . ? Co1 Cl1 Co1 90.0 . 21_556 ? Co1 Cl1 Co1 180.0 . 25_656 ? Co1 Cl1 Co1 90.0 25_656 21_556 ? Co1 Cl1 Co1 180.0 45_655 21_556 ? Co1 Cl1 Co1 90.0 45_655 25_656 ? N1 N1 Co1 122.28(5) 46_656 . ? C1 N1 Co1 129.49(16) . . ? C1 N1 N1 108.23(13) . 46_656 ? N2 N1 Co1 129.49(16) . . ? N2 N1 N1 108.23(13) . 46_656 ? C1 C2 C3 126.93(14) 46_656 . ? C1 C2 C3 126.93(14) . . ? C1 C2 C1 106.1(3) 46_656 . ? N2 C2 C3 126.93(14) . . ? N2 C2 C3 126.93(14) 46_656 . ? N2 C2 N2 106.1(3) 46_656 . ? C4 C3 C2 120.79(16) 11_566 . ? C4 C3 C2 120.79(16) . . ? C4 C3 C4 118.4(3) . 11_566 ? C3 C4 C3 121.6(3) 8_656 . ? C3 C4 H4 119.2 . . ? C3 C4 H4 119.2 8_656 . ? N1 C1 C2 108.7(2) . . ? N1 C1 H1 125.7 . . ? C2 C1 H1 125.7 . . ? N2 Co2 O2 119.2(3) . . ? N2 Co2 O2 119.2(3) 26_556 . ? N2 Co2 N2 116.9(3) . 26_556 ? Co2 O2 Co2 108.0(13) . 13_556 ? N1 N2 C2 108.7(2) . . ? N1 N2 Co2 109.7(2) . . ? C2 N2 Co2 134.9(2) . . ? 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 Co1 N1 C1 C2 -179.98(19) . . . . ? Co1 N1 N2 C2 -179.98(19) . . . . ? Co1 N1 N2 Co2 -24.1(3) . . . . ? N1 N1 C1 C2 0.1(2) 46_656 . . . ? N1 N1 N2 C2 0.1(2) 46_656 . . . ? N1 N1 N2 Co2 156.0(2) 46_656 . . . ? C2 C3 C4 C3 -179.9(2) . . . 8_656 ? C3 C2 C1 N1 179.6(3) . . . . ? C3 C2 N2 N1 179.6(3) . . . . ? C3 C2 N2 Co2 32.5(6) . . . . ? C4 C3 C4 C3 -0.6(7) 11_566 . . 8_656 ? C1 C2 C3 C4 -179.8(3) 46_656 . . 11_566 ? C1 C2 C3 C4 0.5(5) . . . 11_566 ? C1 C2 C3 C4 179.8(3) . . . . ? C1 C2 C3 C4 -0.5(5) 46_656 . . . ? C1 C2 C1 N1 -0.1(4) 46_656 . . . ? N2 C2 C3 C4 -179.8(3) 46_656 . . 11_566 ? N2 C2 C3 C4 0.5(5) . . . 11_566 ? N2 C2 C3 C4 -0.5(5) 46_656 . . . ? N2 C2 C3 C4 179.8(3) . . . . ? N2 C2 N2 N1 -0.1(4) 46_656 . . . ? N2 C2 N2 Co2 -147.2(3) 46_656 . . . ? _shelx_res_file ; djx031s_sq.res created by SHELXL-2014/7 TITL DJX031S in Pm-3m CELL 0.7749 18.8345 18.8345 18.8345 90 90 90 ZERR 1 0.0007 0.0007 0.0007 0 0 0 LATT 1 SYMM -X,-Y,+Z SYMM -X,+Y,-Z SYMM +X,-Y,-Z SYMM +Z,+X,+Y SYMM +Z,-X,-Y SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,+Z,+X SYMM -Y,+Z,-X SYMM +Y,-Z,-X SYMM -Y,-Z,+X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM +Y,-X,+Z SYMM -Y,+X,+Z SYMM +X,+Z,-Y SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +X,-Z,+Y SYMM +Z,+Y,-X SYMM +Z,-Y,+X SYMM -Z,+Y,+X SYMM -Z,-Y,-X SFAC C H Cl Co N O DISP C 0.004 0.002 13.872 DISP H -0 0 0.627 DISP N 0.008 0.004 24.297 DISP O 0.014 0.007 40.889 UNIT 104 56 3 14.4 64 14.4 SIMU Co2 O2 EADP N2 C1 EXYZ N2 C1 L.S. 5 0 19 PLAN 20 SIZE 0.1 0.1 0.1 TEMP -273.15 BOND $H MORE -1 CONF ABIN fmap 2 53 acta REM REM REM WGHT 0.091600 6.302900 FVAR 0.09205 CO1 4 0.368081 0.000000 0.500000 10.25000 0.04545 0.01505 = 0.03447 0.00000 0.00000 0.00000 CL1 3 0.500000 0.000000 0.500000 10.06250 0.03917 0.01621 = 0.03917 0.00000 0.00000 0.00000 O1 6 0.248752 0.000000 0.500000 10.25000 0.07020 0.05536 = 0.05325 0.00000 0.00000 0.00000 N1 5 0.371535 0.074061 0.577615 11.00000 0.04498 0.02065 = 0.04027 0.00293 -0.00194 -0.00029 C2 1 0.351554 0.164736 0.648446 10.50000 0.03802 0.02831 = 0.03802 -0.00064 -0.00196 0.00064 C3 1 0.320048 0.228391 0.679952 10.50000 0.03514 0.03029 = 0.03514 -0.00254 -0.00177 0.00254 C4 1 0.349512 0.259302 0.740698 10.50000 0.03456 0.03379 = 0.03379 -0.00006 -0.00653 0.00653 AFIX 43 H4 2 0.390521 0.238537 0.761463 10.50000 -1.20000 AFIX 0 PART 1 C1 1 0.328258 0.129029 0.589492 10.66670 0.04653 0.02618 = 0.03757 0.00002 -0.00303 0.00516 AFIX 43 H1 2 0.288016 0.141310 0.561674 10.66670 -1.20000 AFIX 0 PART 0 PART 2 CO2 4 0.280823 0.156705 0.500000 10.05000 0.08759 0.04748 = 0.03239 0.00000 0.00000 0.01448 O2 6 0.173641 0.173641 0.500000 10.05000 0.08767 0.08767 = 0.01990 0.00000 0.00000 0.04902 N2 5 0.328258 0.129029 0.589492 10.33330 0.04653 0.02618 = 0.03757 0.00002 -0.00303 0.00516 HKLF 4 REM DJX031S in Pm-3m REM R1 = 0.0462 for 1404 Fo > 4sig(Fo) and 0.0503 for all 1577 data REM 57 parameters refined using 0 restraints END WGHT 0.0916 6.3032 REM Highest difference peak 0.773, deepest hole -0.441, 1-sigma level 0.079 Q1 1 0.1336 0.1336 0.5000 10.25000 0.05 0.77 Q2 1 0.2059 -0.0589 0.5000 10.50000 0.05 0.62 Q3 1 0.2207 0.0000 0.4496 10.50000 0.05 0.60 Q4 1 0.2145 0.0170 0.4542 11.00000 0.05 0.57 Q5 1 0.2804 0.0405 0.5000 10.50000 0.05 0.48 Q6 1 0.5000 0.0561 0.5000 10.12500 0.05 0.28 Q7 1 0.3398 0.1575 0.6211 11.00000 0.05 0.27 Q8 1 0.3418 0.1803 0.6582 10.50000 0.05 0.24 Q9 1 0.5000 -0.1833 0.5000 10.12500 0.05 0.24 Q10 1 0.1653 0.1983 0.5000 10.50000 0.05 0.22 Q11 1 0.3536 -0.0456 0.5000 10.50000 0.05 0.19 Q12 1 0.3600 0.1476 0.5000 10.50000 0.05 0.19 Q13 1 0.3428 0.1178 0.5778 11.00000 0.05 0.19 Q14 1 0.4011 0.0792 0.5989 10.50000 0.05 0.18 Q15 1 0.5000 0.1424 0.5000 10.12500 0.05 0.18 Q16 1 0.3650 0.0570 0.5335 11.00000 0.05 0.17 Q17 1 0.3627 0.1787 0.5462 11.00000 0.05 0.17 Q18 1 0.3256 0.1404 0.5552 11.00000 0.05 0.17 Q19 1 0.5000 0.2630 0.5000 10.12500 0.05 0.16 Q20 1 0.2432 0.2176 0.5000 10.50000 0.05 0.15 ; _shelx_res_checksum 50397 _shelx_hkl_file ; 0 2 0 527.97 24.92 0 2 0 586.46 25.01 2 0 0 518.56 24.89 0 0 2 513.93 24.96 0 0 -2 561.14 24.97 -2 0 0 551.91 24.89 0 -1 -2 59.49 2.69 1 -2 0 58.47 2.68 -2 -1 0 59.46 2.70 0 -2 1 58.60 2.68 1 0 -2 58.61 2.68 -1 -2 0 62.48 2.89 -1 2 0 61.86 2.86 0 -1 -2 55.29 2.83 0 -1 2 55.97 2.95 0 1 -2 61.08 2.96 0 1 2 56.34 2.84 1 -2 0 57.94 2.85 -2 0 -1 58.44 2.69 -1 -2 0 60.27 2.70 -2 -1 0 52.57 2.85 -2 1 0 57.14 2.76 -1 0 -2 56.27 2.91 -1 -2 0 56.51 2.67 0 -1 -2 57.89 2.68 0 1 -2 59.14 2.69 1 -2 0 58.81 2.69 2 0 -1 57.51 2.69 2 0 1 57.47 2.68 -1 0 -2 55.90 2.68 0 -2 -1 58.32 2.68 0 -2 1 58.41 2.69 1 0 -2 58.98 2.69 2 -1 0 59.33 2.70 2 1 0 57.59 2.67 1 0 -2 60.27 2.87 2 -1 0 58.64 2.67 -1 0 2 57.56 2.88 -2 0 1 55.41 2.67 -1 -2 0 58.84 2.69 0 -1 2 58.51 2.69 0 1 2 58.74 2.68 1 -2 0 55.97 2.68 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166.07 8.30 8 2 0 169.30 8.50 8 0 -2 169.08 7.96 8 0 2 171.76 7.93 0 -8 2 167.32 7.95 2 0 -8 191.77 7.99 8 -2 0 168.99 7.96 0 -2 -8 171.10 8.59 0 -8 -2 181.84 7.95 -2 0 -8 165.76 7.93 0 2 -8 177.00 7.96 2 0 8 174.42 7.96 8 2 0 173.47 7.92 2 0 -8 171.63 7.91 8 0 -2 165.32 8.30 8 0 2 172.85 8.54 -2 0 -8 169.76 8.68 -8 0 -2 167.64 8.49 0 -8 2 169.46 7.98 -2 0 8 181.26 7.96 2 -8 0 155.07 8.02 0 -8 2 175.65 7.93 8 2 0 169.04 7.92 2 1 8 2.37 0.94 -1 -2 -8 3.09 0.32 2 -1 -8 3.27 0.27 2 -8 1 2.99 0.32 2 -8 1 3.32 0.35 -2 8 1 3.27 0.88 8 -1 2 2.95 0.35 8 -2 -1 3.26 0.24 -8 -2 1 3.39 0.79 8 -1 2 3.10 0.32 -8 -1 -2 3.93 0.86 -2 -8 -1 3.61 0.38 1 8 2 2.85 0.80 -8 1 2 2.99 0.57 -2 -8 -1 3.37 0.81 2 -8 1 1.75 0.91 1 -8 -2 2.89 0.37 -8 2 -1 3.13 0.34 -2 1 -8 1.89 0.78 8 -1 2 3.60 0.81 8 1 -2 1.92 0.62 -1 2 8 2.91 0.34 1 -8 -2 2.94 0.34 -1 8 -2 2.55 0.85 8 2 1 2.63 0.31 2 -1 -8 2.66 0.38 -2 8 1 3.28 0.71 8 -2 -1 3.08 0.41 1 2 -8 3.34 0.35 -8 1 2 2.63 0.33 -8 -2 1 2.97 0.36 1 2 -8 3.08 0.22 -2 1 -8 2.99 0.30 -8 -2 1 2.94 0.34 -1 -8 2 2.79 0.28 1 -2 8 2.81 0.37 2 8 -1 4.46 1.17 8 -2 -1 2.74 0.59 -2 -1 8 3.00 0.36 1 -2 8 3.39 1.12 1 2 -8 3.99 1.05 2 -8 1 3.68 0.37 -1 -8 2 3.51 0.37 1 -8 -2 3.39 0.33 -1 -2 -8 3.22 0.37 -2 1 -8 3.10 0.37 2 1 8 2.85 0.32 -1 -8 2 2.68 0.32 -1 -2 -8 2.66 0.91 -8 2 -1 3.91 0.74 2 -1 -8 3.97 0.89 -2 -1 8 3.41 1.00 8 1 -2 3.26 0.37 -2 -8 -1 3.09 0.30 -8 -1 -2 3.35 0.38 8 2 1 3.39 0.29 -1 2 8 2.01 0.81 2 8 -1 3.67 0.94 8 2 1 2.78 0.80 -1 -8 -2 2.57 0.39 2 1 -8 3.15 1.00 -2 1 8 2.67 0.29 -8 -2 -1 3.65 0.39 -2 -1 -8 3.85 0.38 1 -2 -8 2.62 0.35 -1 -2 8 2.61 0.37 8 1 2 3.57 0.90 -1 -8 -2 2.80 0.31 -2 -1 -8 3.07 0.34 8 -2 1 2.48 0.27 8 2 -1 3.45 0.34 -8 1 -2 2.49 0.33 -1 2 -8 3.21 0.39 -1 2 -8 2.60 1.01 2 -8 -1 3.62 0.33 -1 -8 -2 3.77 0.78 -2 -1 -8 3.50 0.93 1 -8 2 3.08 0.39 1 -8 2 3.09 0.30 1 -2 -8 3.48 0.83 -8 -1 2 3.01 0.69 -8 1 -2 1.96 0.69 1 2 8 1.65 0.88 -1 2 -8 2.82 0.25 1 -2 -8 3.10 0.29 1 2 8 2.86 0.37 2 8 1 2.75 0.77 8 -1 -2 3.41 0.62 8 2 -1 2.80 0.74 2 -8 -1 3.15 0.34 8 1 2 2.43 0.31 8 1 2 3.04 0.33 2 -1 8 3.41 0.34 2 -8 -1 3.03 0.32 -8 -1 2 3.42 0.32 -8 2 1 2.52 0.33 -2 -8 1 2.85 0.31 -1 -8 -2 3.46 0.32 -2 1 8 4.00 0.94 -8 2 1 2.69 0.57 -2 -8 1 2.77 0.37 -1 8 2 2.23 0.71 -1 8 2 4.71 0.98 1 -8 2 2.57 1.00 1 8 -2 4.26 1.06 -2 -8 1 2.44 0.31 2 -1 8 2.22 0.82 -1 -2 8 2.12 1.02 -8 -1 2 3.06 0.39 -8 -2 -1 3.95 0.87 8 -1 -2 3.58 0.25 8 -2 1 2.23 0.66 2 1 -8 3.08 0.38 8 -1 -2 2.62 0.37 8 -2 1 2.21 0.34 -2 8 -1 4.68 1.01 8 -2 2 46.07 2.31 2 -2 -8 47.08 2.28 -2 2 8 46.56 2.96 -2 2 8 47.14 2.28 -8 2 -2 49.25 2.83 2 -2 8 42.80 3.19 -2 8 2 51.70 2.76 -2 -8 2 48.53 2.29 2 -8 -2 46.95 2.31 2 -2 -8 44.89 2.86 -2 -8 -2 49.09 2.35 -2 -8 -2 48.30 2.26 -2 -8 2 49.33 2.28 -2 -2 -8 47.86 2.29 -2 2 -8 39.92 2.33 2 -8 -2 49.80 2.33 2 -8 2 49.91 2.32 2 -2 -8 46.29 2.33 2 2 -8 49.98 2.34 8 -2 -2 46.32 2.33 -2 -2 -8 45.52 2.31 -2 -2 8 46.22 2.21 -2 2 -8 47.89 2.25 -2 -2 8 46.50 2.36 2 2 -8 45.09 3.12 2 2 8 47.36 3.13 2 8 -2 52.06 3.07 2 8 -2 50.66 3.32 -2 8 2 47.58 3.00 -8 2 2 45.53 2.31 -2 8 -2 46.31 3.09 -8 -2 2 49.20 2.28 -2 -8 2 46.30 2.33 2 -8 2 47.34 3.19 -2 -2 -8 49.76 2.98 8 2 -2 47.85 2.83 8 -2 -2 43.75 2.53 8 -2 2 46.90 2.87 -8 2 -2 44.37 2.32 -8 -2 -2 46.57 2.35 -8 -2 2 45.47 2.32 8 2 2 47.92 2.25 2 8 2 41.95 2.90 -8 -2 2 45.53 2.83 2 2 8 51.32 2.32 8 -2 -2 46.98 2.21 8 -2 2 48.40 2.26 -8 -2 -2 50.97 2.98 2 -8 -2 48.35 2.26 2 -8 2 50.25 2.33 8 2 2 43.46 2.86 -2 2 -8 46.64 3.13 -8 2 2 46.59 2.52 -2 -8 -2 48.94 2.93 -2 -2 8 48.86 3.28 8 2 -2 45.54 2.29 2 -8 2 48.36 2.26 -3 0 8 31.13 1.48 -3 -8 0 30.41 1.47 3 0 -8 30.33 1.58 0 -8 -3 30.82 1.50 0 -8 3 30.14 1.55 3 0 8 27.21 1.54 8 -3 0 31.94 1.46 -3 0 -8 31.91 1.52 8 0 3 32.08 1.51 0 -8 3 30.35 1.48 0 -8 -3 29.40 1.56 3 0 8 27.64 2.39 0 3 -8 28.89 1.55 8 -3 0 29.88 1.90 0 -3 8 30.24 1.58 -3 -8 0 29.59 1.56 3 -8 0 29.55 1.57 0 -8 -3 30.13 1.52 0 -8 3 30.11 1.52 -8 0 3 31.56 1.54 8 -3 0 29.63 1.55 8 3 0 31.79 1.49 8 0 3 30.10 2.12 -8 -3 0 32.76 1.58 -8 3 0 27.14 1.52 -3 0 -8 30.17 1.54 0 8 -3 33.48 2.63 0 8 3 31.34 2.10 3 0 -8 29.66 2.27 0 3 -8 30.41 1.41 3 -8 0 29.89 1.50 0 -3 8 31.72 2.57 3 -8 0 29.88 1.51 0 3 8 29.67 2.25 3 8 0 33.97 2.23 8 0 -3 30.85 1.91 -8 0 -3 30.62 2.19 -3 8 0 29.86 2.20 0 -3 -8 30.27 2.18 0 -3 -8 29.51 1.53 8 0 -3 28.04 2.11 8 0 -3 24.24 1.59 8 0 3 31.13 1.51 -3 0 8 29.17 1.52 8 3 0 28.08 2.12 -8 0 3 30.56 1.47 -8 3 0 33.14 1.88 -3 0 8 27.18 2.29 0 3 -8 30.94 2.33 0 3 8 28.77 1.51 -8 -3 0 31.84 2.12 -3 -8 0 30.66 1.56 -8 -3 0 25.51 1.54 -3 0 -8 35.14 2.30 0 -3 -8 30.90 1.56 0 -8 -3 34.39 2.15 0 -8 3 29.85 2.53 -8 0 -3 31.44 1.58 8 -3 -1 151.79 7.23 -8 -3 1 168.24 7.98 -3 -1 8 153.49 7.32 1 -8 -3 161.42 7.35 1 -3 8 166.62 8.27 -8 -1 -3 153.63 7.36 1 3 -8 159.30 7.34 -3 1 -8 164.12 7.30 -1 3 8 154.98 7.94 -1 8 -3 147.25 8.20 -8 -3 1 160.64 7.36 1 -8 -3 154.53 7.77 -3 1 -8 158.85 7.31 -8 3 -1 156.44 7.72 -3 -8 -1 159.89 7.26 -1 -8 3 135.25 7.34 1 3 -8 151.35 8.19 -1 -8 3 168.00 8.43 8 -3 -1 161.13 7.36 -8 -3 1 166.59 7.32 3 -1 -8 157.05 7.28 -1 -3 -8 157.79 7.95 3 -8 1 162.93 7.35 3 -8 1 152.06 8.03 3 8 -1 151.68 7.97 8 3 1 154.76 7.30 3 1 8 160.85 7.33 -1 -3 -8 159.26 7.30 -8 1 3 155.73 7.25 8 3 1 156.29 7.26 -3 -1 8 156.14 8.17 8 1 -3 163.77 7.33 3 -1 -8 152.85 7.34 -1 -3 -8 160.86 7.34 -3 1 -8 162.16 8.17 -3 -8 -1 149.64 7.32 -8 -1 -3 172.18 8.02 8 1 -3 146.18 7.93 8 -1 3 147.93 7.28 -3 8 1 170.82 7.75 -3 8 1 172.01 8.01 -3 -8 -1 142.20 7.41 3 1 8 158.92 8.13 8 -3 -1 152.64 7.55 8 -1 3 156.66 7.94 -8 3 -1 160.50 7.33 3 -8 1 156.41 7.29 -3 -1 8 162.82 7.26 8 -1 3 155.95 7.30 3 8 -1 131.19 8.25 1 -8 -3 156.51 7.32 -1 3 8 151.01 7.29 8 1 -3 164.19 7.78 1 -8 -3 163.78 7.29 -3 -8 -1 154.00 7.98 -1 -8 3 157.45 7.28 3 -8 1 161.66 7.31 -8 1 3 159.28 7.33 3 -1 -8 167.29 7.95 8 3 1 153.61 7.96 1 -3 8 149.43 7.33 8 -1 -3 164.78 7.61 3 -8 -1 156.96 7.28 -8 3 1 161.46 7.54 -3 -8 1 145.36 7.33 1 -8 3 156.21 8.32 8 -1 -3 158.35 7.35 -8 1 -3 158.56 7.89 -3 8 -1 162.32 8.07 -8 -1 3 154.21 7.33 8 3 -1 164.20 7.29 -1 -8 -3 161.32 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9.14 1.48 2 -3 8 9.41 1.42 2 8 3 8.39 1.30 -8 -2 -3 9.11 1.32 8 -2 3 7.31 1.19 -3 -8 -2 9.14 0.64 -3 -2 8 11.66 1.67 8 -2 3 9.28 0.56 3 8 -2 8.42 1.65 2 3 -8 9.40 0.62 8 -3 -2 9.49 0.48 -2 -8 3 9.38 0.59 3 2 8 9.08 0.60 -8 -2 -3 10.23 0.74 -3 2 -8 10.65 1.35 8 3 2 9.22 0.53 8 3 2 9.72 1.38 -2 -3 -8 9.19 0.64 8 3 2 9.88 0.61 -3 -8 -2 10.19 0.72 -3 -2 8 9.27 0.51 -3 2 -8 9.28 0.56 -2 -8 3 7.98 0.62 -2 -8 3 8.65 0.57 2 3 -8 8.08 1.44 8 -2 3 10.22 0.63 8 2 -3 10.37 1.54 -3 -8 -2 9.32 0.53 -2 -3 -8 10.51 0.62 3 -2 -8 8.34 1.12 -8 -3 2 9.32 0.63 -8 3 -2 8.57 0.60 3 2 8 8.91 1.46 8 2 -3 9.03 1.13 3 -2 -8 9.86 0.60 3 -8 2 10.20 0.57 3 -8 2 10.51 1.55 -3 -8 -2 7.63 1.13 -2 -3 -8 9.18 1.37 3 -2 -8 9.23 0.64 -8 -3 2 9.36 0.58 -3 8 2 11.76 1.07 3 -8 2 9.13 0.63 -8 -3 2 8.55 1.24 3 8 -2 8.54 1.19 2 -8 -3 9.79 0.66 8 -3 -2 8.53 0.68 3 -8 2 9.36 0.67 -8 2 3 8.65 0.60 8 2 -3 8.98 0.63 8 -3 2 8.34 0.55 3 -2 8 8.69 1.35 -8 -3 -2 9.07 0.67 -2 -3 8 8.84 0.48 -8 -2 3 9.70 0.60 8 -2 -3 10.79 0.85 -2 8 3 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2.88 -2 0 10 39.91 3.00 0 -2 -10 32.48 2.73 0 -2 10 43.93 3.04 0 2 -10 43.13 3.07 0 2 10 41.59 2.96 2 10 0 46.38 2.95 2 10 0 41.96 3.35 10 0 -2 42.83 2.60 10 0 2 44.37 2.80 2 0 10 41.65 3.08 10 -2 0 42.72 2.53 10 0 2 39.55 1.98 10 2 0 42.12 2.01 0 -2 -10 41.88 2.05 2 -10 0 39.49 2.05 -10 -2 0 40.18 2.68 10 0 2 42.00 2.01 -10 2 0 43.65 2.52 -2 -10 0 40.61 2.00 0 10 -2 41.36 2.75 0 10 2 38.07 2.69 0 -10 -2 40.12 2.02 10 2 0 39.93 2.76 -10 -2 0 37.68 2.06 -2 0 10 41.63 2.03 0 2 10 40.45 2.02 2 -10 0 36.15 2.21 0 -10 2 38.19 2.04 2 0 -10 45.93 2.91 -2 0 -10 42.27 2.04 -10 0 -2 42.12 2.08 -10 0 2 38.80 2.05 -1 2 10 53.50 2.69 -1 -10 2 56.21 2.69 10 -2 -1 56.29 2.74 10 -1 2 47.81 2.76 -2 1 -10 57.27 2.71 1 2 -10 51.65 2.72 2 -10 1 55.67 2.68 -2 1 -10 60.75 3.64 -1 10 -2 56.91 3.82 2 -1 -10 58.76 2.67 1 -10 -2 55.29 2.72 -2 -1 10 58.05 2.74 10 2 1 58.71 2.68 2 1 10 54.63 3.70 -1 -2 -10 45.80 2.74 -2 1 -10 58.21 2.67 -10 1 2 50.40 3.09 10 2 1 58.36 2.68 -2 10 1 56.14 3.33 -2 10 1 53.62 3.66 -2 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24.87 2.20 3 -1 -10 23.64 2.06 -1 -3 -10 23.90 1.30 10 -3 -1 24.52 1.72 1 -3 10 21.78 1.30 -10 3 -1 22.45 1.30 -1 -3 -10 24.82 1.30 -3 -1 10 24.35 1.21 -3 1 -10 22.83 1.25 -10 1 3 23.62 1.30 -3 10 1 22.59 2.28 1 -10 -3 25.45 1.33 10 -1 3 24.36 1.27 -10 -1 -3 24.68 2.06 10 -3 -1 23.85 1.35 10 1 -3 24.36 1.32 3 1 10 23.85 2.36 -1 -10 3 22.39 1.35 10 -1 3 22.02 2.04 -1 3 10 25.79 2.19 -1 -10 3 24.24 1.25 1 -3 10 26.91 2.51 1 3 -10 23.24 2.15 1 -10 -3 26.20 1.32 3 10 -1 31.08 2.76 10 -3 -1 22.44 1.18 -3 1 -10 25.64 2.41 -3 -10 -1 23.51 1.23 10 1 -3 21.61 1.88 -3 -1 10 25.10 2.41 10 3 1 24.51 1.27 -3 -1 10 24.41 1.30 -10 -3 1 24.73 1.35 3 -1 -10 23.02 1.34 -10 -3 1 22.84 1.99 -3 10 1 23.93 1.84 -1 3 10 22.88 1.27 1 3 -10 24.62 1.33 -1 -3 -10 25.09 2.02 10 3 1 24.77 1.25 -10 -1 -3 23.99 1.34 10 -1 3 25.07 1.30 -3 -10 -1 24.98 1.34 1 -10 -3 23.72 1.25 3 -10 1 25.69 1.26 -10 3 -1 23.62 1.83 -1 -10 3 23.20 1.28 -3 1 -10 24.15 1.29 -1 10 -3 25.87 2.42 1 -3 -10 24.64 1.33 1 10 -3 26.82 2.42 10 1 3 24.21 2.11 3 10 1 22.11 2.13 -1 -10 -3 25.09 1.28 10 1 3 22.96 1.25 10 1 3 23.87 1.25 1 -10 3 23.76 1.31 -10 -3 -1 24.85 1.36 1 -3 -10 22.98 2.03 10 3 -1 25.03 2.05 -10 3 1 23.87 1.30 10 -1 -3 24.74 1.76 -10 3 1 23.70 1.66 -1 -3 10 24.68 2.56 -1 3 -10 25.30 2.21 -10 1 -3 26.76 2.04 -1 -10 -3 24.98 1.35 -3 -1 -10 22.55 2.03 10 -3 1 24.65 1.95 -1 -3 10 24.87 1.16 -1 3 -10 23.46 1.17 10 -3 1 23.94 1.33 10 3 -1 24.42 1.28 -10 1 -3 25.70 1.38 3 -10 -1 24.16 1.26 -1 10 3 23.42 2.24 10 -1 -3 25.09 1.35 -3 -1 -10 25.28 1.32 -3 1 10 25.34 2.26 1 3 10 25.29 2.24 10 -3 1 24.95 1.22 -3 1 10 22.80 1.28 -1 -10 -3 26.09 1.28 1 3 10 24.07 1.30 -10 -1 3 26.03 1.36 1 -10 3 22.58 2.47 3 -1 10 22.42 1.32 3 -10 -1 25.03 1.34 3 1 -10 26.38 2.28 1 -10 3 24.58 1.24 -3 -10 1 25.03 1.25 1 -3 -10 23.61 1.27 3 -10 -1 25.82 1.29 -1 10 3 27.21 1.99 -10 -1 3 24.00 1.24 3 1 -10 22.58 1.34 3 -1 10 25.98 2.46 -3 -10 1 24.25 1.31 -1 3 -10 23.52 1.30 -3 -10 1 23.33 1.31 -1 -3 10 23.03 1.32 -1 -10 -3 21.80 1.85 -10 -3 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19.89 1.11 4 -10 -1 20.09 1.18 -1 -10 -4 20.70 1.09 -10 -4 -1 21.51 1.96 10 1 4 18.66 1.06 4 1 -10 19.69 2.02 10 1 4 20.33 1.08 -1 -10 -4 19.48 1.10 10 -4 1 21.30 1.04 -1 -4 10 18.21 2.39 4 -10 -1 19.67 1.09 10 -1 -4 18.85 1.14 4 -10 -1 20.05 1.07 -10 1 -4 19.05 1.83 -4 10 -1 23.01 2.20 -10 -1 4 19.26 1.06 -4 -1 -10 22.53 1.17 10 -1 -4 17.08 1.76 10 -1 -4 21.03 1.54 4 -1 10 20.78 1.13 4 10 1 22.06 2.06 1 -4 -10 19.76 1.10 10 -4 1 21.20 1.74 -10 4 1 20.09 1.12 -1 4 -10 19.85 1.14 10 1 4 21.81 1.89 -10 2 4 45.04 2.20 2 4 -10 40.34 3.13 -4 -10 -2 44.09 2.10 -4 10 2 46.69 2.99 10 4 2 43.87 2.16 4 -2 -10 43.93 2.15 2 4 -10 41.09 2.19 4 -10 2 42.92 3.31 -4 2 -10 42.60 2.15 -10 4 -2 41.85 2.78 -2 10 -4 50.02 3.47 10 -4 -2 39.82 2.38 -4 -2 10 44.53 3.21 -4 -10 -2 42.04 2.24 -2 4 10 47.80 3.11 2 -10 -4 46.68 2.22 10 4 2 43.41 2.09 -4 2 -10 46.18 3.29 -2 -10 4 45.90 2.27 10 -2 4 45.10 3.07 10 2 -4 42.11 3.07 -10 -2 -4 45.26 3.03 10 2 -4 42.42 2.21 2 -4 10 42.65 3.42 -4 -10 -2 45.01 2.19 10 4 2 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12 18 -0.80 0.00 3 12 18 -0.17 0.00 4 12 18 -0.29 0.00 5 12 18 0.19 0.00 6 12 18 0.17 0.00 7 12 18 0.10 0.00 8 12 18 0.57 0.00 9 12 18 -0.25 0.00 10 12 18 -1.15 0.00 11 12 18 1.00 0.00 0 13 18 -0.85 0.00 1 13 18 0.01 0.00 2 13 18 -0.15 0.00 3 13 18 -0.40 0.00 4 13 18 -1.12 0.00 5 13 18 0.08 0.00 6 13 18 -1.69 0.00 7 13 18 0.88 0.00 8 13 18 -1.20 0.00 9 13 18 -0.70 0.00 10 13 18 -1.93 0.00 0 14 18 0.21 0.00 1 14 18 1.43 0.00 2 14 18 -1.53 0.00 3 14 18 0.03 0.00 4 14 18 -1.29 0.00 5 14 18 2.20 0.00 6 14 18 -3.09 0.00 7 14 18 0.86 0.00 8 14 18 -0.40 0.00 0 15 18 2.69 0.00 1 15 18 -1.37 0.00 2 15 18 1.79 0.00 3 15 18 -1.34 0.00 4 15 18 1.69 0.00 5 15 18 -2.64 0.00 6 15 18 2.26 0.00 0 16 18 0.85 0.00 1 16 18 -0.69 0.00 2 16 18 -0.44 0.00 3 16 18 -1.02 0.00 4 16 18 -0.31 0.00 0 0 19 -2.63 0.00 0 1 19 3.51 0.00 1 1 19 -0.34 0.00 0 2 19 -1.08 0.00 1 2 19 -1.43 0.00 2 2 19 1.20 0.00 0 3 19 3.95 0.00 1 3 19 0.85 0.00 2 3 19 0.56 0.00 3 3 19 -2.37 0.00 0 4 19 -3.12 0.00 1 4 19 1.81 0.00 2 4 19 -1.02 0.00 3 4 19 1.77 0.00 4 4 19 -2.57 0.00 0 5 19 0.95 0.00 1 5 19 1.91 0.00 2 5 19 -0.91 0.00 3 5 19 -0.33 0.00 4 5 19 -0.76 0.00 5 5 19 3.30 0.00 0 6 19 -1.11 0.00 1 6 19 -0.33 0.00 2 6 19 2.69 0.00 3 6 19 0.95 0.00 4 6 19 0.89 0.00 5 6 19 -2.40 0.00 6 6 19 3.01 0.00 0 7 19 1.71 0.00 1 7 19 2.34 0.00 2 7 19 -1.17 0.00 3 7 19 -0.54 0.00 4 7 19 -0.41 0.00 5 7 19 1.29 0.00 6 7 19 -1.47 0.00 7 7 19 -0.62 0.00 0 8 19 0.50 0.00 1 8 19 0.39 0.00 2 8 19 -0.23 0.00 3 8 19 0.35 0.00 4 8 19 -0.92 0.00 5 8 19 -1.91 0.00 6 8 19 1.07 0.00 7 8 19 0.02 0.00 8 8 19 -0.92 0.00 0 9 19 1.59 0.00 1 9 19 0.69 0.00 2 9 19 -0.18 0.00 3 9 19 -0.51 0.00 4 9 19 0.40 0.00 5 9 19 0.59 0.00 6 9 19 1.15 0.00 7 9 19 -1.72 0.00 8 9 19 1.39 0.00 9 9 19 -0.25 0.00 0 10 19 -1.13 0.00 1 10 19 -0.14 0.00 2 10 19 -0.41 0.00 3 10 19 1.48 0.00 4 10 19 0.02 0.00 5 10 19 -1.01 0.00 6 10 19 2.29 0.00 7 10 19 -0.95 0.00 8 10 19 -0.24 0.00 9 10 19 2.41 0.00 10 10 19 0.04 0.00 0 11 19 -1.33 0.00 1 11 19 1.75 0.00 2 11 19 -2.23 0.00 3 11 19 -0.63 0.00 4 11 19 -0.88 0.00 5 11 19 1.35 0.00 6 11 19 -0.91 0.00 7 11 19 -0.11 0.00 8 11 19 -0.14 0.00 9 11 19 0.59 0.00 10 11 19 -1.22 0.00 0 12 19 -2.10 0.00 1 12 19 0.88 0.00 2 12 19 -0.41 0.00 3 12 19 2.11 0.00 4 12 19 -1.90 0.00 5 12 19 0.99 0.00 6 12 19 -1.36 0.00 7 12 19 1.51 0.00 8 12 19 -2.41 0.00 9 12 19 2.44 0.00 0 13 19 1.31 0.00 1 13 19 -2.34 0.00 2 13 19 1.57 0.00 3 13 19 -2.66 0.00 4 13 19 1.21 0.00 5 13 19 -0.83 0.00 6 13 19 1.22 0.00 7 13 19 -2.54 0.00 8 13 19 2.07 0.00 0 14 19 1.31 0.00 1 14 19 -0.43 0.00 2 14 19 0.43 0.00 3 14 19 -0.16 0.00 4 14 19 0.49 0.00 5 14 19 -0.90 0.00 6 14 19 -0.33 0.00 0 15 19 0.08 0.00 1 15 19 -0.02 0.00 2 15 19 -0.02 0.00 3 15 19 -0.64 0.00 0 0 20 8.20 0.00 0 1 20 -2.08 0.00 1 1 20 -1.01 0.00 0 2 20 -0.08 0.00 1 2 20 1.77 0.00 2 2 20 -2.81 0.00 0 3 20 -1.16 0.00 1 3 20 0.19 0.00 2 3 20 -0.51 0.00 3 3 20 2.10 0.00 0 4 20 2.95 0.00 1 4 20 0.26 0.00 2 4 20 -0.88 0.00 3 4 20 -1.14 0.00 4 4 20 -0.36 0.00 0 5 20 -2.65 0.00 1 5 20 -0.70 0.00 2 5 20 1.31 0.00 3 5 20 -0.73 0.00 4 5 20 0.19 0.00 5 5 20 -2.24 0.00 0 6 20 1.71 0.00 1 6 20 1.52 0.00 2 6 20 0.08 0.00 3 6 20 -0.51 0.00 4 6 20 -0.67 0.00 5 6 20 1.08 0.00 6 6 20 -0.66 0.00 0 7 20 0.44 0.00 1 7 20 0.17 0.00 2 7 20 2.06 0.00 3 7 20 0.51 0.00 4 7 20 1.09 0.00 5 7 20 -1.76 0.00 6 7 20 1.13 0.00 7 7 20 -0.77 0.00 0 8 20 1.46 0.00 1 8 20 1.09 0.00 2 8 20 -2.74 0.00 3 8 20 -0.51 0.00 4 8 20 -1.66 0.00 5 8 20 0.32 0.00 6 8 20 1.19 0.00 7 8 20 0.27 0.00 8 8 20 0.17 0.00 0 9 20 -1.29 0.00 1 9 20 -0.77 0.00 2 9 20 -0.59 0.00 3 9 20 0.86 0.00 4 9 20 0.36 0.00 5 9 20 -1.49 0.00 6 9 20 0.10 0.00 7 9 20 -0.41 0.00 8 9 20 -0.04 0.00 9 9 20 1.14 0.00 0 10 20 -0.35 0.00 1 10 20 2.89 0.00 2 10 20 -2.03 0.00 3 10 20 0.73 0.00 4 10 20 -0.80 0.00 5 10 20 1.59 0.00 6 10 20 -0.44 0.00 7 10 20 0.76 0.00 8 10 20 -0.18 0.00 9 10 20 0.98 0.00 0 11 20 0.88 0.00 1 11 20 0.09 0.00 2 11 20 1.57 0.00 3 11 20 -0.79 0.00 4 11 20 0.93 0.00 5 11 20 -1.03 0.00 6 11 20 0.83 0.00 7 11 20 -0.87 0.00 8 11 20 -0.18 0.00 0 12 20 -1.18 0.00 1 12 20 0.06 0.00 2 12 20 -0.06 0.00 3 12 20 -1.21 0.00 4 12 20 0.06 0.00 5 12 20 -0.73 0.00 6 12 20 0.31 0.00 7 12 20 -1.73 0.00 0 13 20 -1.81 0.00 1 13 20 0.22 0.00 2 13 20 0.10 0.00 3 13 20 1.04 0.00 4 13 20 -0.09 0.00 5 13 20 1.68 0.00 0 14 20 0.39 0.00 1 14 20 0.87 0.00 0 0 21 -2.97 0.00 0 1 21 1.00 0.00 1 1 21 0.06 0.00 0 2 21 -0.06 0.00 1 2 21 -0.79 0.00 2 2 21 2.33 0.00 0 3 21 0.59 0.00 1 3 21 -1.34 0.00 2 3 21 -0.05 0.00 3 3 21 -1.85 0.00 0 4 21 -2.21 0.00 1 4 21 0.68 0.00 2 4 21 -0.22 0.00 3 4 21 2.22 0.00 4 4 21 -1.36 0.00 0 5 21 0.37 0.00 1 5 21 -1.64 0.00 2 5 21 -0.19 0.00 3 5 21 -1.68 0.00 4 5 21 0.58 0.00 5 5 21 -0.32 0.00 0 6 21 -1.07 0.00 1 6 21 1.56 0.00 2 6 21 -0.07 0.00 3 6 21 0.57 0.00 4 6 21 -2.34 0.00 5 6 21 -0.20 0.00 6 6 21 -0.68 0.00 0 7 21 2.38 0.00 1 7 21 -0.55 0.00 2 7 21 1.32 0.00 3 7 21 -1.58 0.00 4 7 21 1.82 0.00 5 7 21 -0.21 0.00 6 7 21 0.95 0.00 7 7 21 -1.07 0.00 0 8 21 1.48 0.00 1 8 21 0.91 0.00 2 8 21 -0.77 0.00 3 8 21 0.33 0.00 4 8 21 -0.33 0.00 5 8 21 0.74 0.00 6 8 21 0.61 0.00 7 8 21 0.34 0.00 8 8 21 1.41 0.00 0 9 21 2.00 0.00 1 9 21 -0.36 0.00 2 9 21 -0.39 0.00 3 9 21 -1.07 0.00 4 9 21 0.54 0.00 5 9 21 -1.25 0.00 6 9 21 0.54 0.00 7 9 21 -0.05 0.00 8 9 21 -0.47 0.00 0 10 21 0.12 0.00 1 10 21 0.49 0.00 2 10 21 -0.44 0.00 3 10 21 -0.58 0.00 4 10 21 0.15 0.00 5 10 21 -0.83 0.00 6 10 21 -0.38 0.00 7 10 21 -0.38 0.00 0 11 21 -1.61 0.00 1 11 21 2.16 0.00 2 11 21 -2.55 0.00 3 11 21 0.27 0.00 4 11 21 -0.38 0.00 5 11 21 1.01 0.00 0 12 21 -0.94 0.00 1 12 21 -0.76 0.00 2 12 21 0.64 0.00 3 12 21 -0.99 0.00 0 0 22 2.44 0.00 0 1 22 -2.76 0.00 1 1 22 0.76 0.00 0 2 22 1.02 0.00 1 2 22 -0.24 0.00 2 2 22 1.49 0.00 0 3 22 -2.93 0.00 1 3 22 0.69 0.00 2 3 22 -2.92 0.00 3 3 22 2.80 0.00 0 4 22 3.37 0.00 1 4 22 -1.63 0.00 2 4 22 2.14 0.00 3 4 22 -2.01 0.00 4 4 22 1.68 0.00 0 5 22 -1.93 0.00 1 5 22 1.30 0.00 2 5 22 0.08 0.00 3 5 22 2.89 0.00 4 5 22 -0.96 0.00 5 5 22 1.17 0.00 0 6 22 3.15 0.00 1 6 22 -1.41 0.00 2 6 22 2.06 0.00 3 6 22 -3.80 0.00 4 6 22 0.86 0.00 5 6 22 -1.45 0.00 6 6 22 0.98 0.00 0 7 22 -1.49 0.00 1 7 22 -0.65 0.00 2 7 22 -1.65 0.00 3 7 22 1.93 0.00 4 7 22 -1.65 0.00 5 7 22 1.16 0.00 6 7 22 -2.26 0.00 7 7 22 -2.86 0.00 0 8 22 3.28 0.00 1 8 22 -0.31 0.00 2 8 22 1.23 0.00 3 8 22 -2.98 0.00 4 8 22 2.20 0.00 5 8 22 -0.16 0.00 6 8 22 2.14 0.00 7 8 22 -2.05 0.00 0 9 22 0.74 0.00 1 9 22 1.86 0.00 2 9 22 -1.42 0.00 3 9 22 2.16 0.00 4 9 22 -1.66 0.00 5 9 22 1.73 0.00 0 10 22 2.32 0.00 1 10 22 -0.41 0.00 2 10 22 -0.54 0.00 3 10 22 -1.62 0.00 0 0 23 -5.03 0.00 0 1 23 0.38 0.00 1 1 23 -0.72 0.00 0 2 23 -0.70 0.00 1 2 23 1.31 0.00 2 2 23 2.37 0.00 0 3 23 0.81 0.00 1 3 23 -0.75 0.00 2 3 23 1.43 0.00 3 3 23 1.44 0.00 0 4 23 -1.17 0.00 1 4 23 -0.06 0.00 2 4 23 1.51 0.00 3 4 23 1.14 0.00 4 4 23 1.07 0.00 0 5 23 -0.57 0.00 1 5 23 -1.37 0.00 2 5 23 0.43 0.00 3 5 23 1.87 0.00 4 5 23 -0.55 0.00 5 5 23 1.80 0.00 0 6 23 -1.40 0.00 1 6 23 -0.84 0.00 2 6 23 -0.80 0.00 3 6 23 -0.52 0.00 4 6 23 -0.27 0.00 5 6 23 -0.20 0.00 0 7 23 -1.45 0.00 1 7 23 -0.60 0.00 2 7 23 -0.38 0.00 3 7 23 -0.49 0.00 4 7 23 0.30 0.00 0 8 23 2.25 0.00 1 8 23 -1.35 0.00 2 8 23 0.50 0.00 0 0 24 0.34 0.00 0 1 24 -2.86 0.00 1 1 24 0.27 0.00 0 2 24 0.16 0.00 1 2 24 0.69 0.00 2 2 24 0.74 0.00 0 3 24 0.47 0.00 1 3 24 -0.33 0.00 2 3 24 1.86 0.00 3 3 24 -0.22 0.00 0 4 24 1.12 0.00 1 4 24 1.51 0.00 2 4 24 0.18 0.00 0 0 1 -37.51 0.00 0 1 1 174.68 0.00 1 1 1 -114.06 0.00 11 15 16 -2.48 0.00 12 13 17 1.73 0.00 11 14 17 1.31 0.00 5 17 17 -2.32 0.00 9 14 18 -0.75 0.00 7 15 18 -1.41 0.00 5 16 18 -0.78 0.00 11 11 19 -1.98 0.00 10 12 19 -0.17 0.00 7 14 19 -0.80 0.00 4 15 19 -0.47 0.00 10 10 20 -0.17 0.00 9 11 20 0.90 0.00 6 13 20 -1.35 0.00 2 14 20 1.44 0.00 3 14 20 -0.17 0.00 9 9 21 0.96 0.00 8 10 21 1.29 0.00 6 11 21 -1.32 0.00 4 12 21 -0.17 0.00 6 9 22 -1.57 0.00 4 10 22 0.79 0.00 0 11 22 -0.91 0.00 1 11 22 -0.85 0.00 6 6 23 1.65 0.00 5 7 23 0.78 0.00 3 8 23 -0.07 0.00 3 4 24 2.72 0.00 0 5 24 -1.01 0.00 1 5 24 0.46 0.00 2 5 24 1.45 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 11015) # 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 -0.001 -0.001 3068 469 ' ' 2 0.500 0.500 0.500 1037 351 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 0 1 1.179 0 1 1 1.667 1 1 1 2.042 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL djx031s P m -3 m R = 0.13 CELL 18.8345 18.8345 18.8345 90.00 90.00 90.00 SPGR Pm-3m # Solvent Accessible Volume = 4105.7 # Electrons Found in S.A.V. = 804.3 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.500 0.266 0.500 ! 7.46 eA-3 C102 0.500 0.500 0.187 ! 6.92 eA-3 C103 0.500 0.500 0.500 ! 5.28 eA-3 C104 0.290 0.422 0.505 ! 2.09 eA-3 C105 1.000 1.000 0.000 ! 1.61 eA-3 Q106 0.233 0.500 0.000 ! 1.23 eA-3 C107 0.296 0.999 0.250 ! 1.19 eA-3 C108 0.537 0.541 0.457 ! 1.03 eA-3 C109 0.233 0.014 0.234 ! 0.93 eA-3 Q110 0.866 0.141 0.493 ! 0.81 eA-3 Q111 0.256 0.505 0.328 ! 0.79 eA-3 Q112 0.212 0.452 0.015 ! 0.73 eA-3 C113 0.581 0.419 0.419 ! 0.73 eA-3 Q114 0.132 0.500 0.500 ! 0.66 eA-3 C115 0.433 0.371 0.430 ! 0.65 eA-3 Q116 0.792 0.494 0.062 ! 0.64 eA-3 C117 0.917 0.109 0.392 ! 0.63 eA-3 C118 0.083 0.891 0.608 ! 0.63 eA-3 C119 0.391 0.104 0.923 ! 0.63 eA-3 C120 0.111 0.386 0.922 ! 0.63 eA-3 C121 0.889 0.386 0.922 ! 0.63 eA-3 C122 0.500 0.359 0.499 ! 0.58 eA-3 Q123 0.069 0.448 0.158 ! 0.57 eA-3 C124 0.683 0.313 0.504 ! 0.55 eA-3 C125 0.101 0.218 0.218 ! 0.54 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_Co-BDTriP-MeOH _audit_creation_date 2016-02-04 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common 'Co-BDTriP-MeOH' _chemical_name_systematic ? _chemical_formula_moiety '(C100 H76 Cl3 Co12 N80 O12) Co1.5' _chemical_formula_sum 'C100 H76 Cl3 Co13.5 N80 O12' _chemical_formula_weight 3492.20 _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' 0.0033 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 221 _space_group_name_H-M_alt 'P m -3 m' _space_group_name_Hall '-P 4 2 3' loop_ _space_group_symop_operation_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, -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' _cell_length_a 18.7059(4) _cell_length_b 18.7059(4) _cell_length_c 18.7059(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6545.4(4) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9578 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.07 _cell_measurement_theta_min 2.43 _shelx_estimated_absorpt_T_max 0.938 _shelx_estimated_absorpt_T_min 0.938 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1210 before and 0.0806 after correction. The Ratio of minimum to maximum transmission is 0.9369. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour pink _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 0.864 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1707 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_special_details ; An MeOH-solvated single crystal of Co-BDTriP (Co3[(Co4Cl)3(BDTriP)8]2; H3BDTriP = 4,4'-(5-(1H-pyrazol-4-yl)-1,3-phenylene)bis(1H-1,2,3-triazole)) were mounted on a Kaptan loop and frozen at a temperature of 100 K under a stream of flowing N2. Data was collected using a Bruker QUAZAR diffractometer equipped with a Bruker AXS APEX II detector, using MoKa radiation (lamda = 0.71073 angstroms). ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 55966 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.100 _diffrn_reflns_theta_max 24.100 _diffrn_reflns_theta_min 1.089 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w/\q scans' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 974 _reflns_number_total 1108 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX 2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.405 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.097 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 1108 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0593 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+18.7104P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1690 _refine_ls_wR_factor_ref 0.1761 _refine_special_details ; Thermal parameters were refined anisotropically for all non-hydrogen atoms. Hydrogen atoms were placed in ideal positions and refined using a riding model. Co-BTTri is an anionic framework ([(Co4Cl)3(BTTri)8]3-) and, thus, contains charge-balancing cations, which could not be located in the electron difference map. These cations are likely Co(II) (three Co(II) per two [(Co4Cl)3(BTTri)8]3-) and were included in the formula unit but not in the refinement. Each linker has two triazolate groups and one pyrazolate group that are disordered, due to the three-fold and mirror symmetery of the structure. Thus, C1 and N2 on the triazolate/pyrazolate rings were restrained to have the same coordinates and displacement parameters. The site occupancy factors of C1 and N2 were fixed to reflect a statistical distribution, corresponding to a chemical occupancy of 66.7% for C1 and 33.3% for N2. The methyl groups of methanol coordinated to the framework Co centers was disordered over four positions. The chemical occupancy of the disordered methanol fragments was fixed to be 25% in the refinement, because the disorder was caused by two perpendicular mirror planes in the structure. Disorder of the extra-framework Co cations and residual solvent within the pores of the crystal was extensive and could not be modeled. Consequently, the unassigned electron density was accounted for using SQUEEZE as implemented in the PLATON interface. Refinement before SQUEEZE was applied gave an R1 of 14.78% (wR2 = 45.05%), while applying SQUEEZE resulted in an R1 of 5.93% (wR2 = 17.61%). ; _vrf_THETM01_djx033_0m_sq ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Due weak scattering at high resolution, a sin(theta)/lambda > 0.575 could not be achieved. The data used for refinement was truncated to a resolution limit where I/sigma > 3 and Rint < 0.25. ; _vrf_PLAT232_djx033_0m_sq ; PROBLEM: Hirshfeld Test Diff (M-X) Co1 -- O1 .. 10.3 s.u. RESPONSE: This likely due to the larger atomic displacement parameters of a coordinated MeOH oxygen atom compared to the Co1, which is restrained by the rigid framework. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H,H,H,H) groups 2. Shared sites {N2, C1} 3. Uiso/Uaniso restraints and constraints O1 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C1) = Uanis(N2) 4. Rigid body (RIGU) restrains O1, C5 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: N2(0.667) C1(0.333) H1(0.333) C5(0.25) H5F(0.125) H5C(0.125) H5D(0.125) H5B(0.125) H5E(0.125) H5A(0.125) 6.a Aromatic/amide H refined with riding coordinates: C4(H4), C1(H1) 6.b Disordered Me refined with riding coordinates: C5(H5F,H5C,H5D,H5B,H5E,H5A) ; _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.36896(5) 0.5000 0.0272(4) Uani 1 4 d S T P . . Cl1 Cl 0.0000 0.5000 0.5000 0.0386(10) Uani 1 16 d S T P . . N1 N 0.07344(14) 0.37229(15) 0.57635(16) 0.0281(7) Uani 1 1 d . . . . . N2 N 0.12803(17) 0.32884(18) 0.58845(18) 0.0374(9) Uani 0.667 1 d . . . A 2 C3 C 0.2288(3) 0.32054(19) 0.67946(19) 0.0312(12) Uani 1 2 d S T P . . C2 C 0.1638(3) 0.3524(2) 0.6476(2) 0.0314(12) Uani 1 2 d S T P . . O1 O 0.0000 0.2525(4) 0.5000 0.0649(19) Uani 1 4 d S TU P . . C4 C 0.2597(2) 0.2597(2) 0.6503(3) 0.0342(12) Uani 1 2 d S T P . . H4 H 0.2386 0.2386 0.6092 0.041 Uiso 1 2 calc RS T P A . C1 C 0.12803(17) 0.32884(18) 0.58845(18) 0.0374(9) Uani 0.333 1 d . . . A 1 H1 H 0.1403 0.2881 0.5607 0.045 Uiso 0.333 1 calc R . . A 1 C5 C 0.022(2) 0.1940(15) 0.5562(14) 0.152(18) Uani 0.25 1 d . U . A . H5F H 0.0386 0.2173 0.5999 0.228 Uiso 0.125 1 calc R . . . . H5C H -0.0199 0.1642 0.5672 0.228 Uiso 0.125 1 calc R . . . . H5D H 0.0599 0.1642 0.5364 0.228 Uiso 0.125 1 calc R . . . . H5B H 0.0138 0.1464 0.5358 0.228 Uiso 0.125 1 calc R . . . . H5E H 0.0723 0.1996 0.5685 0.228 Uiso 0.125 1 calc R . . . . H5A H -0.0075 0.1996 0.5993 0.228 Uiso 0.125 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0162(5) 0.0379(7) 0.0275(6) 0.000 0.000 0.000 Cl1 0.0259(19) 0.0450(14) 0.0450(14) 0.000 0.000 0.000 N1 0.0182(14) 0.0334(17) 0.0326(16) -0.0012(12) 0.0010(13) 0.0009(12) N2 0.0312(19) 0.041(2) 0.040(2) -0.0026(16) 0.0002(15) 0.0057(15) C3 0.027(3) 0.0333(17) 0.0333(17) -0.001(2) -0.0030(15) 0.0030(15) C2 0.027(3) 0.0337(17) 0.0337(17) -0.003(2) -0.0023(16) 0.0023(16) O1 0.061(4) 0.079(5) 0.055(4) 0.000 0.000 0.000 C4 0.0334(18) 0.0334(18) 0.036(3) -0.0085(17) -0.0085(17) 0.002(2) C1 0.0312(19) 0.041(2) 0.040(2) -0.0026(16) 0.0002(15) 0.0057(15) C5 0.19(4) 0.111(15) 0.16(2) 0.032(15) -0.10(3) -0.058(17) _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 Co1 Cl1 2.4513(10) . ? Co1 N1 1.983(3) 9_556 ? Co1 N1 1.983(3) . ? Co1 N1 1.983(3) 27_556 ? Co1 N1 1.983(3) 30 ? Co1 O1 2.179(8) . ? Cl1 Co1 2.4513(10) 29_556 ? Cl1 Co1 2.4513(10) 5_565 ? Cl1 Co1 2.4513(10) 25_566 ? N1 N1 1.358(6) 45_566 ? N1 N2 1.325(4) . ? N1 C1 1.325(4) . ? N2 C2 1.366(5) . ? C3 C2 1.480(7) . ? C3 C4 1.388(4) 18_566 ? C3 C4 1.388(3) . ? C2 N2 1.366(5) 45_566 ? C2 C1 1.366(5) . ? C2 C1 1.366(5) 45_566 ? O1 C5 1.57(3) 30 ? O1 C5 1.57(3) 27_556 ? O1 C5 1.57(3) 9_556 ? O1 C5 1.57(3) . ? C4 C3 1.388(3) 17_656 ? C4 H4 0.9500 . ? C1 H1 0.9500 . ? C5 H5F 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5B 0.9800 . ? C5 H5E 0.9800 . ? C5 H5A 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 Co1 Cl1 88.19(9) 9_556 . ? N1 Co1 Cl1 88.19(9) 27_556 . ? N1 Co1 Cl1 88.20(9) . . ? N1 Co1 Cl1 88.19(9) 30 . ? N1 Co1 N1 92.17(16) 9_556 30 ? N1 Co1 N1 87.72(15) 9_556 27_556 ? N1 Co1 N1 92.17(16) 27_556 . ? N1 Co1 N1 176.39(18) 9_556 . ? N1 Co1 N1 87.72(15) 30 . ? N1 Co1 N1 176.39(18) 30 27_556 ? N1 Co1 O1 91.81(9) 9_556 . ? N1 Co1 O1 91.80(9) . . ? N1 Co1 O1 91.81(9) 30 . ? N1 Co1 O1 91.81(9) 27_556 . ? O1 Co1 Cl1 180.0 . . ? Co1 Cl1 Co1 90.0 . 5_565 ? Co1 Cl1 Co1 180.0 . 25_566 ? Co1 Cl1 Co1 90.0 25_566 5_565 ? Co1 Cl1 Co1 180.0 29_556 5_565 ? Co1 Cl1 Co1 90.0 29_556 25_566 ? Co1 Cl1 Co1 90.0 . 29_556 ? N1 N1 Co1 122.12(8) 45_566 . ? N2 N1 Co1 129.6(2) . . ? N2 N1 N1 108.2(2) . 45_566 ? C1 N1 Co1 129.6(2) . . ? C1 N1 N1 108.2(2) . 45_566 ? N1 N2 C2 108.5(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 C2 120.9(3) 18_566 . ? C4 C3 C4 118.1(5) . 18_566 ? N2 C2 N2 106.5(4) . 45_566 ? N2 C2 C3 126.8(2) . . ? N2 C2 C3 126.8(2) 45_566 . ? C1 C2 C3 126.8(2) . . ? C1 C2 C3 126.8(2) 45_566 . ? C1 C2 C1 106.5(4) . 45_566 ? C5 O1 Co1 134.1(11) 9_556 . ? C5 O1 Co1 134.1(11) 30 . ? C5 O1 Co1 134.1(11) 27_556 . ? C5 O1 Co1 134.1(11) . . ? C5 O1 C5 30(3) . 30 ? C5 O1 C5 30(3) 9_556 27_556 ? C5 O1 C5 92(2) 27_556 30 ? C5 O1 C5 92(2) 9_556 . ? C5 O1 C5 84(2) 9_556 30 ? C5 O1 C5 84(2) 27_556 . ? C3 C4 C3 121.9(5) . 17_656 ? C3 C4 H4 119.0 17_656 . ? C3 C4 H4 119.0 . . ? N1 C1 C2 108.5(3) . . ? N1 C1 H1 125.7 . . ? C2 C1 H1 125.7 . . ? O1 C5 H5F 109.5 . . ? O1 C5 H5C 109.5 . . ? O1 C5 H5D 109.5 . . ? O1 C5 H5B 109.5 . . ? O1 C5 H5E 109.5 . . ? O1 C5 H5A 109.5 . . ? H5F C5 H5C 109.5 . . ? H5F C5 H5D 109.5 . . ? H5F C5 H5B 141.1 . . ? H5F C5 H5E 56.3 . . ? H5F C5 H5A 56.3 . . ? H5C C5 H5D 109.5 . . ? H5C C5 H5B 56.3 . . ? H5C C5 H5E 141.1 . . ? H5C C5 H5A 56.3 . . ? H5D C5 H5B 56.3 . . ? H5D C5 H5E 56.3 . . ? H5D C5 H5A 141.1 . . ? H5B C5 H5E 109.5 . . ? H5B C5 H5A 109.5 . . ? H5E C5 H5A 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 Co1 N1 N2 C2 -179.7(3) . . . . ? Co1 N1 C1 C2 -179.7(3) . . . . ? N1 N1 N2 C2 -0.4(4) 45_566 . . . ? N1 N1 C1 C2 -0.4(4) 45_566 . . . ? N1 N2 C2 N2 0.6(6) . . . 45_566 ? N1 N2 C2 C3 -178.9(4) . . . . ? C3 C2 C1 N1 -178.9(4) . . . . ? C2 C3 C4 C3 -179.8(4) . . . 17_656 ? C4 C3 C2 N2 -179.5(5) 18_566 . . . ? C4 C3 C2 N2 1.0(8) 18_566 . . 45_566 ? C4 C3 C2 N2 -1.0(8) . . . . ? C4 C3 C2 N2 179.5(5) . . . 45_566 ? C4 C3 C2 C1 1.0(8) 18_566 . . 45_566 ? C4 C3 C2 C1 179.5(5) . . . 45_566 ? C4 C3 C2 C1 -1.0(8) . . . . ? C4 C3 C2 C1 -179.5(5) 18_566 . . . ? C4 C3 C4 C3 -1.2(11) 18_566 . . 17_656 ? C1 C2 C1 N1 0.6(6) 45_566 . . . ? _shelx_res_file ; djx033_0m_sq.res created by SHELXL-2014/7 TITL djx033_0m in Pm-3m #221 REM reset to Pm-3m #221 CELL 0.71073 18.7059 18.7059 18.7059 90 90 90 ZERR 1 0.0004 0.0004 0.0004 0 0 0 LATT 1 SYMM -Y,+X,+Z SYMM -X,-Y,+Z SYMM +Y,-X,+Z SYMM +X,-Z,+Y SYMM +X,-Y,-Z SYMM +X,+Z,-Y SYMM +Z,+Y,-X SYMM -X,+Y,-Z SYMM -Z,+Y,+X SYMM +Z,+X,+Y SYMM +Y,+Z,+X SYMM -Y,-Z,+X SYMM +Z,-X,-Y SYMM -Y,+Z,-X SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,-Z,-X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +Z,-Y,+X SYMM -Z,-Y,-X SFAC C H Cl Co N O UNIT 99.98 75.98 3 12 80.02 12 EQIV $1 -X,+Y,+Z SIMU O1 C5 RIGU O1 C5 EADP C1 N2 EXYZ N2 C1 L.S. 100 0 18 PLAN 20 SIZE 0.08 0.08 0.08 TEMP -173(2) FREE C5 C5_$1 BOND MORE -1 BOND $H CONF ABIN fmap 2 acta 52 REM REM REM WGHT 0.097400 18.710407 FVAR 0.07689 CO1 4 0.000000 0.368957 0.500000 10.25000 0.01620 0.03787 = 0.02751 0.00000 0.00000 0.00000 CL1 3 0.000000 0.500000 0.500000 10.06250 0.02586 0.04497 = 0.04497 0.00000 0.00000 0.00000 N1 5 0.073438 0.372295 0.576355 11.00000 0.01821 0.03344 = 0.03256 -0.00119 0.00100 0.00085 PART 2 N2 5 0.128035 0.328841 0.588452 10.66700 0.03125 0.04064 = 0.04028 -0.00257 0.00016 0.00572 PART 0 C3 1 0.228772 0.320539 0.679461 10.50000 0.02695 0.03331 = 0.03331 -0.00137 -0.00304 0.00304 C2 1 0.163791 0.352428 0.647572 10.50000 0.02672 0.03370 = 0.03370 -0.00325 -0.00225 0.00225 O1 6 0.000000 0.252473 0.500000 10.25000 0.06071 0.07886 = 0.05527 0.00000 0.00000 0.00000 C4 1 0.259677 0.259677 0.650306 10.50000 0.03345 0.03345 = 0.03575 -0.00853 -0.00853 0.00222 AFIX 43 H4 2 0.238567 0.238569 0.609220 10.50000 -1.20000 AFIX 0 PART 1 C1 1 0.128035 0.328841 0.588452 10.33300 0.03125 0.04064 = 0.04028 -0.00257 0.00016 0.00572 AFIX 43 H1 2 0.140258 0.288120 0.560674 10.33300 -1.20000 AFIX 0 PART 0 C5 1 0.021701 0.194039 0.556169 10.25000 0.18878 0.11148 = 0.15575 0.03181 -0.09920 -0.05767 AFIX 123 H5F 2 0.038615 0.217325 0.599946 10.12500 -1.50000 H5C 2 -0.019882 0.164154 0.567232 10.12500 -1.50000 H5D 2 0.059921 0.164155 0.536399 10.12500 -1.50000 H5B 2 0.013822 0.146431 0.535772 10.12500 -1.50000 H5E 2 0.072318 0.199602 0.568486 10.12500 -1.50000 H5A 2 -0.007485 0.199601 0.599318 10.12500 -1.50000 AFIX 0 HKLF 4 REM djx033_0m in Pm-3m #221 REM R1 = 0.0593 for 974 Fo > 4sig(Fo) and 0.0650 for all 1108 data REM 56 parameters refined using 9 restraints END WGHT 0.0973 18.7245 REM Highest difference peak 1.405, deepest hole -0.682, 1-sigma level 0.097 Q1 1 0.1497 0.2706 0.5000 10.50000 0.05 1.41 Q2 1 0.0000 0.1364 0.5381 10.50000 0.05 0.61 Q3 1 0.0000 0.1988 0.6378 10.50000 0.05 0.50 Q4 1 0.0000 0.1822 0.6337 10.50000 0.05 0.47 Q5 1 -0.0435 0.1583 0.6033 11.00000 0.05 0.43 Q6 1 0.0000 0.2198 0.5509 10.50000 0.05 0.39 Q7 1 -0.0159 0.1636 0.6169 11.00000 0.05 0.39 Q8 1 0.0000 0.3004 0.5000 10.25000 0.05 0.32 Q9 1 0.1272 0.2765 0.5709 11.00000 0.05 0.31 Q10 1 0.0260 0.1499 0.5000 10.50000 0.05 0.29 Q11 1 0.0808 0.4123 0.5877 10.50000 0.05 0.27 Q12 1 0.1843 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0.00 3 15 15 3.83 0.00 0 0 16 19.58 0.00 0 1 16 -2.89 0.00 1 1 16 -4.43 0.00 0 2 16 4.17 0.00 1 2 16 4.74 0.00 2 2 16 -5.90 0.00 0 3 16 -5.74 0.00 1 3 16 -1.25 0.00 2 3 16 1.00 0.00 3 3 16 1.58 0.00 0 4 16 9.84 0.00 1 4 16 -0.22 0.00 2 4 16 1.90 0.00 3 4 16 -3.70 0.00 4 4 16 5.79 0.00 0 5 16 -6.05 0.00 1 5 16 0.28 0.00 2 5 16 0.99 0.00 3 5 16 1.79 0.00 4 5 16 -4.04 0.00 5 5 16 -0.34 0.00 0 6 16 6.58 0.00 1 6 16 -1.81 0.00 2 6 16 -0.43 0.00 3 6 16 -2.08 0.00 4 6 16 3.45 0.00 5 6 16 -1.52 0.00 6 6 16 2.36 0.00 0 7 16 -4.92 0.00 1 7 16 -2.14 0.00 2 7 16 0.89 0.00 3 7 16 0.54 0.00 4 7 16 -3.84 0.00 5 7 16 1.35 0.00 6 7 16 0.05 0.00 7 7 16 0.08 0.00 0 8 16 5.35 0.00 1 8 16 -0.62 0.00 2 8 16 -0.79 0.00 3 8 16 -2.58 0.00 4 8 16 1.55 0.00 5 8 16 0.06 0.00 6 8 16 2.69 0.00 7 8 16 0.45 0.00 8 8 16 3.44 0.00 0 9 16 -2.94 0.00 1 9 16 1.09 0.00 2 9 16 0.04 0.00 3 9 16 1.04 0.00 4 9 16 -3.56 0.00 5 9 16 2.07 0.00 6 9 16 -0.10 0.00 7 9 16 0.75 0.00 8 9 16 0.46 0.00 9 9 16 2.80 0.00 0 10 16 3.76 0.00 1 10 16 -1.05 0.00 2 10 16 -1.55 0.00 3 10 16 -3.16 0.00 4 10 16 1.07 0.00 5 10 16 -1.38 0.00 6 10 16 0.10 0.00 7 10 16 -0.24 0.00 8 10 16 3.80 0.00 9 10 16 0.76 0.00 10 10 16 1.56 0.00 0 11 16 -0.94 0.00 1 11 16 -1.52 0.00 2 11 16 1.87 0.00 3 11 16 -1.23 0.00 4 11 16 -0.35 0.00 5 11 16 -1.04 0.00 6 11 16 0.54 0.00 7 11 16 -0.53 0.00 8 11 16 1.60 0.00 9 11 16 0.98 0.00 0 12 16 0.63 0.00 1 12 16 1.66 0.00 2 12 16 -4.29 0.00 3 12 16 1.35 0.00 4 12 16 -1.38 0.00 5 12 16 -1.29 0.00 6 12 16 -0.53 0.00 7 12 16 -0.71 0.00 0 13 16 -2.63 0.00 1 13 16 2.46 0.00 2 13 16 0.35 0.00 3 13 16 2.32 0.00 4 13 16 -3.67 0.00 5 13 16 -1.68 0.00 6 13 16 -1.77 0.00 0 14 16 3.16 0.00 1 14 16 1.29 0.00 2 14 16 -0.24 0.00 3 14 16 -0.54 0.00 0 0 17 3.23 0.00 0 1 17 2.70 0.00 1 1 17 -1.31 0.00 0 2 17 4.78 0.00 1 2 17 -2.75 0.00 2 2 17 10.24 0.00 0 3 17 0.31 0.00 1 3 17 -1.46 0.00 2 3 17 -1.85 0.00 3 3 17 -1.89 0.00 0 4 17 -4.65 0.00 1 4 17 2.22 0.00 2 4 17 0.68 0.00 3 4 17 2.41 0.00 4 4 17 -3.91 0.00 0 5 17 1.85 0.00 1 5 17 -5.07 0.00 2 5 17 -3.30 0.00 3 5 17 -3.21 0.00 4 5 17 3.86 0.00 5 5 17 -0.24 0.00 0 6 17 -4.81 0.00 1 6 17 -0.05 0.00 2 6 17 0.84 0.00 3 6 17 2.58 0.00 4 6 17 -1.81 0.00 5 6 17 2.06 0.00 6 6 17 -1.04 0.00 0 7 17 5.66 0.00 1 7 17 -2.17 0.00 2 7 17 1.46 0.00 3 7 17 -2.44 0.00 4 7 17 3.52 0.00 5 7 17 -2.11 0.00 6 7 17 2.98 0.00 7 7 17 -1.50 0.00 0 8 17 -2.48 0.00 1 8 17 2.59 0.00 2 8 17 1.75 0.00 3 8 17 3.64 0.00 4 8 17 -2.80 0.00 5 8 17 1.68 0.00 6 8 17 0.85 0.00 7 8 17 2.77 0.00 8 8 17 1.19 0.00 0 9 17 5.02 0.00 1 9 17 -2.56 0.00 2 9 17 1.03 0.00 3 9 17 -2.59 0.00 4 9 17 2.38 0.00 5 9 17 -2.59 0.00 6 9 17 1.50 0.00 7 9 17 -1.70 0.00 8 9 17 2.00 0.00 9 9 17 -3.35 0.00 0 10 17 -3.44 0.00 1 10 17 0.06 0.00 2 10 17 1.01 0.00 3 10 17 -0.24 0.00 4 10 17 -2.60 0.00 5 10 17 -0.52 0.00 6 10 17 0.15 0.00 7 10 17 0.31 0.00 8 10 17 1.45 0.00 0 11 17 2.25 0.00 1 11 17 1.05 0.00 2 11 17 -1.74 0.00 3 11 17 0.32 0.00 4 11 17 -0.60 0.00 5 11 17 0.22 0.00 6 11 17 -0.41 0.00 7 11 17 -0.39 0.00 0 12 17 -0.56 0.00 1 12 17 0.51 0.00 2 12 17 2.99 0.00 3 12 17 1.61 0.00 4 12 17 1.17 0.00 5 12 17 -0.66 0.00 0 13 17 2.79 0.00 1 13 17 0.13 0.00 2 13 17 0.08 0.00 0 0 18 13.20 0.00 0 1 18 1.15 0.00 1 1 18 -5.13 0.00 0 2 18 1.56 0.00 1 2 18 4.06 0.00 2 2 18 -4.65 0.00 0 3 18 -3.22 0.00 1 3 18 -1.47 0.00 2 3 18 1.64 0.00 3 3 18 1.51 0.00 0 4 18 5.24 0.00 1 4 18 0.92 0.00 2 4 18 -1.24 0.00 3 4 18 -1.91 0.00 4 4 18 -0.08 0.00 0 5 18 -2.41 0.00 1 5 18 -4.00 0.00 2 5 18 2.25 0.00 3 5 18 -2.15 0.00 4 5 18 0.87 0.00 5 5 18 -3.46 0.00 0 6 18 1.81 0.00 1 6 18 -0.79 0.00 2 6 18 -1.94 0.00 3 6 18 -0.29 0.00 4 6 18 -0.14 0.00 5 6 18 -1.20 0.00 6 6 18 -3.61 0.00 0 7 18 -1.91 0.00 1 7 18 -0.76 0.00 2 7 18 2.35 0.00 3 7 18 0.43 0.00 4 7 18 -1.31 0.00 5 7 18 -2.49 0.00 6 7 18 -0.38 0.00 7 7 18 -0.13 0.00 0 8 18 -1.09 0.00 1 8 18 -1.18 0.00 2 8 18 -3.36 0.00 3 8 18 -0.68 0.00 4 8 18 -0.43 0.00 5 8 18 -0.17 0.00 6 8 18 0.39 0.00 7 8 18 1.76 0.00 8 8 18 0.88 0.00 0 9 18 -3.62 0.00 1 9 18 -2.11 0.00 2 9 18 0.68 0.00 3 9 18 0.61 0.00 4 9 18 -0.20 0.00 5 9 18 -2.11 0.00 6 9 18 0.82 0.00 7 9 18 -1.22 0.00 0 10 18 -0.83 0.00 1 10 18 -1.27 0.00 2 10 18 -0.05 0.00 3 10 18 -0.78 0.00 4 10 18 -0.92 0.00 5 10 18 0.66 0.00 6 10 18 0.64 0.00 0 11 18 -0.64 0.00 1 11 18 -2.32 0.00 2 11 18 3.47 0.00 3 11 18 -2.82 0.00 4 11 18 -0.90 0.00 0 0 19 0.31 0.00 0 1 19 2.22 0.00 1 1 19 -0.72 0.00 0 2 19 -0.38 0.00 1 2 19 -1.94 0.00 2 2 19 1.12 0.00 0 3 19 3.51 0.00 1 3 19 -2.50 0.00 2 3 19 0.97 0.00 3 3 19 -1.89 0.00 0 4 19 -0.91 0.00 1 4 19 1.22 0.00 2 4 19 0.20 0.00 3 4 19 1.24 0.00 4 4 19 -1.56 0.00 0 5 19 2.75 0.00 1 5 19 0.29 0.00 2 5 19 -2.73 0.00 3 5 19 -1.35 0.00 4 5 19 -0.61 0.00 5 5 19 2.31 0.00 0 6 19 -1.48 0.00 1 6 19 -1.52 0.00 2 6 19 1.17 0.00 3 6 19 -0.37 0.00 4 6 19 0.33 0.00 5 6 19 -0.80 0.00 6 6 19 -0.11 0.00 0 7 19 0.89 0.00 1 7 19 2.49 0.00 2 7 19 -0.87 0.00 3 7 19 0.22 0.00 4 7 19 -0.10 0.00 5 7 19 0.26 0.00 6 7 19 -0.02 0.00 7 7 19 0.72 0.00 0 8 19 -0.42 0.00 1 8 19 -1.29 0.00 2 8 19 0.91 0.00 3 8 19 -0.11 0.00 4 8 19 -0.69 0.00 5 8 19 -3.19 0.00 6 8 19 -0.95 0.00 0 9 19 1.72 0.00 1 9 19 2.29 0.00 2 9 19 1.54 0.00 3 9 19 1.37 0.00 4 9 19 0.00 0.00 0 10 19 -1.44 0.00 1 10 19 0.07 0.00 0 0 20 -9.17 0.00 0 1 20 -3.29 0.00 1 1 20 -1.85 0.00 0 2 20 -0.80 0.00 1 2 20 2.79 0.00 2 2 20 0.34 0.00 0 3 20 -0.78 0.00 1 3 20 -0.67 0.00 2 3 20 0.59 0.00 3 3 20 -1.61 0.00 0 4 20 1.38 0.00 1 4 20 0.25 0.00 2 4 20 -0.43 0.00 3 4 20 -1.71 0.00 4 4 20 -1.56 0.00 0 5 20 2.74 0.00 1 5 20 2.74 0.00 2 5 20 3.01 0.00 3 5 20 -1.03 0.00 4 5 20 -1.01 0.00 5 5 20 -1.15 0.00 0 6 20 0.65 0.00 1 6 20 3.02 0.00 2 6 20 -1.10 0.00 3 6 20 0.51 0.00 4 6 20 -0.96 0.00 5 6 20 -0.04 0.00 0 7 20 2.97 0.00 1 7 20 1.72 0.00 2 7 20 3.53 0.00 3 7 20 -0.36 0.00 0 0 21 -7.70 0.00 0 1 21 -2.47 0.00 1 1 21 3.83 0.00 0 2 21 1.72 0.00 1 2 21 -0.77 0.00 2 2 21 4.54 0.00 0 3 21 -0.42 0.00 1 3 21 0.52 0.00 2 3 21 -4.06 0.00 3 3 21 -3.56 0.00 0 4 21 -1.13 0.00 1 4 21 -1.40 0.00 2 4 21 0.48 0.00 10 13 14 -3.15 0.00 11 11 15 -3.92 0.00 10 12 15 -1.26 0.00 7 14 15 1.76 0.00 4 15 15 1.55 0.00 8 12 16 0.02 0.00 4 14 16 -1.12 0.00 9 10 17 1.34 0.00 6 12 17 -0.23 0.00 3 13 17 2.58 0.00 8 9 18 0.02 0.00 5 11 18 -2.47 0.00 0 12 18 1.16 0.00 1 12 18 0.18 0.00 5 9 19 -1.96 0.00 2 10 19 3.34 0.00 3 10 19 1.81 0.00 4 7 20 0.21 0.00 0 8 20 -0.10 0.00 1 8 20 2.29 0.00 2 8 20 -1.80 0.00 3 4 21 -3.22 0.00 0 5 21 2.30 0.00 1 5 21 4.00 0.00 2 5 21 -1.71 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 11015) # 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 -0.014 -0.012 -0.012 2685 584 ' ' 2 0.500 0.500 0.500 1006 200 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL djx033_0m P m -3 m R = 0.15 CELL 18.7059 18.7059 18.7059 90.00 90.00 90.00 SPGR Pm-3m # Solvent Accessible Volume = 3693.6 # Electrons Found in S.A.V. = 775.9 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.500 0.502 0.266 ! 6.92 eA-3 C102 0.190 0.500 0.500 ! 6.11 eA-3 C103 0.500 0.500 0.500 ! 4.31 eA-3 C104 0.432 0.297 0.493 ! 1.83 eA-3 C105 1.000 0.484-0.001 ! 1.76 eA-3 Q106 0.500 0.261 0.161 ! 1.67 eA-3 C107 0.500 0.167 0.167 ! 1.49 eA-3 C108 1.000 1.005 0.078 ! 0.92 eA-3 C109 0.235 0.281-0.003 ! 0.91 eA-3 Q110 0.239 0.500 0.000 ! 0.88 eA-3 C111 1.000 1.000 0.125 ! 0.88 eA-3 C112 1.000 1.000 0.000 ! 0.80 eA-3 C113 0.062 0.062 0.062 ! 0.74 eA-3 C114 0.354 1.000 0.000 ! 0.72 eA-3 Q115 0.500 0.994 0.125 ! 0.69 eA-3 Q116 0.870 0.453 0.007 ! 0.68 eA-3 C117 0.053 0.444 0.058 ! 0.65 eA-3 C118 0.844 0.219 0.151 ! 0.60 eA-3 C119 0.156 0.781 0.849 ! 0.60 eA-3 C120 0.787 0.843 0.843 ! 0.60 eA-3 Q121 0.331 0.768 0.333 ! 0.59 eA-3 Q122 0.694 0.172-0.002 ! 0.56 eA-3 C123 0.187 0.235 0.106 ! 0.56 eA-3 Q124 0.199 0.531 0.035 ! 0.55 eA-3 C125 0.446 0.497 0.234 ! 0.54 eA-3 Q126 0.818 0.375 0.000 ! 0.54 eA-3 C127 0.162 0.162 0.162 ! 0.53 eA-3 C128 0.687 0.870 0.130 ! 0.52 eA-3 Q129 0.596 0.409 0.076 ! 0.50 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_Co-BDTriP-Activated _audit_creation_date 2016-02-03 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common 'Co-BDTriP' _chemical_name_systematic ? _chemical_formula_moiety 'C109.02 H71.02 Cl3 Co13.44 N63.98 O5.04' _chemical_formula_sum 'C109.02 H71.02 Cl3 Co13.44 N63.98 O5.04' _chemical_formula_weight 3256.24 _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' 0.0033 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 221 _space_group_name_H-M_alt 'P m -3 m' _space_group_name_Hall '-P 4 2 3' loop_ _space_group_symop_operation_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, -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' _cell_length_a 18.6522(5) _cell_length_b 18.6522(5) _cell_length_c 18.6522(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6489.2(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9714 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.667 _cell_measurement_theta_min 2.442 _shelx_estimated_absorpt_T_max 0.915 _shelx_estimated_absorpt_T_min 0.915 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.6661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0697 before and 0.0427 after correction. The Ratio of minimum to maximum transmission is 0.8931. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'dark brown' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 0.814 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description cube _exptl_crystal_F_000 1582 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; A methanol-solvated single crystal of single crystal of Co-BDTriP (Co3[(Co4Cl)3(BDTriP)8]2, H3BDTriP = 4,4'-(5-(1H-pyrazol-4-yl)-1,3-phenylene)bis(1H-1,2,3-triazole)) was epoxied on a thin glass fiber and carefully inserted into a 1.0 mm borosilicate capillary. The capillary was then attached to a Micromeretics ASAP 2020 instrument via a custom-designed adapter, degassed at 453 K using a sand bath, and then dosed with 400 mbar He. After dosing He, the capillary was flame sealed. Data was collected using a Bruker QUAZAR diffractometer equipped with a Bruker AXS APEX II detector, using MoKa radiation (lamda = 0.71073 angstroms). ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_unetI/netI 0.0273 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7753 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 1.544 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 926 _reflns_number_total 1208 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX 2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.484 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.068 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 53 _refine_ls_number_reflns 1208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0463 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+13.2442P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1233 _refine_special_details ; Thermal parameters were refined anisotropically for all non-hydrogen atoms. Hydrogen atoms were placed in ideal positions and refined using a riding model. Co-BDTriP is an anionic framework ([(Co4Cl)3(BDTriP)8]3-) and, thus, contains charge-balancing cations. These cations are likely Co(II) (three Co(II) per two [(Co4Cl)3(BDTriP)8]3-). The location of these charge-balancing Co(II) cations (Co2) was assigned to electron density found between two triazolate groups that are adjacent to each other on the [Co4Cl]7+ cluster, corresponding to a model where nitrogen atoms on adjacent triazolate groups are coordinated to Co. The site occupancy factor of Co2 was refined then were fixed in the final refinement. This gave a chemical occupancy of 6% for both, corresponding to 2.88 extra-framework Co centers per formula unit. Each linker has two triazolate groups and one pyrazolate group that are disordered, due to the three-fold and mirror symmetery of the structure. Thus, C1 and N2 on the triazolate/pyrazolate rings were restrained to have the same coordinates and displacement parameters. The site occupancy factors of C1 and N2 were fixed to reflect a statistical distribution, corresponding to a chemical occupancy of 66.7% for C1 and 33.3% for N2. Despite multiple efforts to remove all of the solvent from the framework Co sites (Co1), electron density was still located above the Co site. This density likely corresponds to residual methanol and was assigned to be a coordinated oxygen atom. Refinement of the site occupancy factors of this oxygen atom resulted in a chemical occupancy of 42%, which was then fixed in the final refinement. The methyl groups on the residual methanol could not be modeled and were removed from the refinement but not the formula. Disorder of residual solvent within the pores of the crystal was extensive and could not be modeled. Consequently, the unassigned electron density was accounted for using SQUEEZE as implemented in the PLATON interface. Refinement before SQUEEZE was applied gave an R1 of 13.64% (wR2 = 44.76%), while applying SQUEEZE resulted in an R1 of 4.63% (wR2 = 12.33%). ; _vrf_PLAT307_djx044_0m_sq ; PROBLEM: Isolated Metal Atom (Unusual !) ................ RESPONSE: This metal atom is Co2 which is not single bonded in the structure but coordinated to two triazolate nitrogens. Additional ligands coordinated to this Co center could not be located in the electron density difference map, due to disorder and the low site occupancy of the extra-framework Co moieties. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Shared sites {C1, N2} 3. Uiso/Uaniso restraints and constraints Uanis(C1) = Uanis(N2) 4. Others Fixed Sof: O1(0.105) Co2(0.03) N2(0.333) C1(0.667) H1(0.667) 5.a Aromatic/amide H refined with riding coordinates: C4(H4), C1(H1) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.37226(4) 0.0243(3) Uani 1 4 d S T P . . Cl1 Cl 0.5000 0.0000 0.5000 0.0276(6) Uani 1 16 d S T P . . O1 O 0.5000 0.0000 0.2460(10) 0.108(6) Uani 0.42 4 d S T P . . N1 N 0.42456(12) 0.07238(11) 0.37319(12) 0.0236(5) Uani 1 1 d . . . . . C2 C 0.35194(16) 0.1632(2) 0.35194(16) 0.0299(10) Uani 1 2 d S T P . . C3 C 0.31974(15) 0.2279(2) 0.31974(15) 0.0277(9) Uani 1 2 d S T P . . C4 C 0.25857(16) 0.25857(16) 0.3493(2) 0.0290(10) Uani 1 2 d S T P . . H4 H 0.2373 0.2373 0.3904 0.035 Uiso 1 2 calc RS T P A . Co2 Co 0.5000 0.1461(9) 0.2707(7) 0.062(4) Uani 0.06 2 d S T P A 2 N2 N 0.41188(14) 0.12768(14) 0.32927(15) 0.0292(6) Uani 0.333 1 d . . . A 2 C1 C 0.41188(14) 0.12768(14) 0.32927(15) 0.0292(6) Uani 0.667 1 d . . . A 3 H1 H 0.4401 0.1403 0.2888 0.035 Uiso 0.667 1 calc R . . A 3 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 Co1 0.0234(4) 0.0164(4) 0.0332(5) 0.000 0.000 0.000 Cl1 0.0294(9) 0.0238(14) 0.0294(9) 0.000 0.000 0.000 O1 0.059(10) 0.159(18) 0.106(15) 0.000 0.000 0.000 N1 0.0254(12) 0.0166(11) 0.0288(13) 0.0048(10) 0.0004(10) 0.0003(9) C2 0.0328(14) 0.024(2) 0.0328(14) 0.0031(13) 0.0023(19) 0.0031(13) C3 0.0280(13) 0.027(2) 0.0280(13) 0.0046(13) 0.0033(18) 0.0046(13) C4 0.0301(14) 0.0301(14) 0.027(2) 0.0086(13) 0.0086(13) 0.0023(18) Co2 0.022(5) 0.112(12) 0.054(8) 0.032(8) 0.000 0.000 N2 0.0291(15) 0.0257(14) 0.0328(15) 0.0095(12) 0.0012(12) -0.0003(12) C1 0.0291(15) 0.0257(14) 0.0328(15) 0.0095(12) 0.0012(12) -0.0003(12) _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 Co1 Cl1 2.3826(8) . ? Co1 O1 2.354(19) . ? Co1 N1 1.950(2) . ? Co1 N1 1.950(2) 30_655 ? Co1 N1 1.950(2) 3_655 ? Co1 N1 1.950(2) 33 ? Cl1 Co1 2.3826(8) 32_655 ? Cl1 Co1 2.3826(8) 25_656 ? Cl1 Co1 2.3826(8) 8_556 ? N1 N1 1.355(4) 48 ? N1 N2 1.338(3) . ? N1 C1 1.338(3) . ? C2 C3 1.475(6) . ? C2 N2 1.367(4) . ? C2 N2 1.367(4) 48 ? C2 C1 1.367(4) . ? C2 C1 1.367(4) 48 ? C3 C4 1.390(3) 11 ? C3 C4 1.390(3) . ? C4 C3 1.390(3) 12 ? C4 H4 0.9500 . ? Co2 N2 2.003(8) 30_655 ? Co2 N2 2.003(8) . ? C1 H1 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 O1 Co1 Cl1 180.0 . . ? N1 Co1 Cl1 89.49(7) 33 . ? N1 Co1 Cl1 89.49(7) 30_655 . ? N1 Co1 Cl1 89.49(7) . . ? N1 Co1 Cl1 89.49(7) 3_655 . ? N1 Co1 O1 90.51(7) 33 . ? N1 Co1 O1 90.51(7) . . ? N1 Co1 O1 90.51(7) 30_655 . ? N1 Co1 O1 90.51(7) 3_655 . ? N1 Co1 N1 87.63(13) 33 . ? N1 Co1 N1 87.63(13) 30_655 3_655 ? N1 Co1 N1 92.36(13) 33 3_655 ? N1 Co1 N1 92.36(13) 30_655 . ? N1 Co1 N1 178.98(14) 33 30_655 ? N1 Co1 N1 178.98(14) 3_655 . ? Co1 Cl1 Co1 180.0 32_655 8_556 ? Co1 Cl1 Co1 90.0 32_655 . ? Co1 Cl1 Co1 90.0 8_556 25_656 ? Co1 Cl1 Co1 180.0 25_656 . ? Co1 Cl1 Co1 90.0 8_556 . ? Co1 Cl1 Co1 90.0 32_655 25_656 ? N1 N1 Co1 121.10(7) 48 . ? N2 N1 Co1 130.97(19) . . ? N2 N1 N1 107.93(15) . 48 ? C1 N1 Co1 130.97(19) . . ? C1 N1 N1 107.93(15) . 48 ? N2 C2 C3 127.13(17) 48 . ? N2 C2 C3 127.13(17) . . ? N2 C2 N2 105.7(3) . 48 ? C1 C2 C3 127.13(17) 48 . ? C1 C2 C3 127.13(17) . . ? C1 C2 C1 105.7(3) . 48 ? C4 C3 C2 120.6(2) . . ? C4 C3 C2 120.6(2) 11 . ? C4 C3 C4 118.8(4) . 11 ? C3 C4 C3 121.2(4) 12 . ? C3 C4 H4 119.4 12 . ? C3 C4 H4 119.4 . . ? N2 Co2 N2 110.3(6) 30_655 . ? N1 N2 C2 109.2(2) . . ? N1 N2 Co2 108.7(4) . . ? C2 N2 Co2 139.2(5) . . ? N1 C1 C2 109.2(2) . . ? N1 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? 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 Co1 N1 N2 C2 179.7(2) . . . . ? Co1 N1 N2 Co2 -15.6(6) . . . . ? Co1 N1 C1 C2 179.7(2) . . . . ? N1 N1 N2 C2 -0.4(3) 48 . . . ? N1 N1 N2 Co2 164.2(5) 48 . . . ? N1 N1 C1 C2 -0.4(3) 48 . . . ? C2 C3 C4 C3 179.6(3) . . . 12 ? C3 C2 N2 N1 178.9(4) . . . . ? C3 C2 N2 Co2 21.5(9) . . . . ? C3 C2 C1 N1 178.9(4) . . . . ? C4 C3 C4 C3 -1.5(9) 11 . . 12 ? N2 C2 C3 C4 179.5(4) 48 . . 11 ? N2 C2 C3 C4 1.7(7) . . . 11 ? N2 C2 C3 C4 -179.5(4) . . . . ? N2 C2 C3 C4 -1.7(7) 48 . . . ? N2 C2 N2 N1 0.7(5) 48 . . . ? N2 C2 N2 Co2 -156.7(6) 48 . . . ? C1 C2 C3 C4 -1.7(7) 48 . . . ? C1 C2 C3 C4 1.7(7) . . . 11 ? C1 C2 C3 C4 179.5(4) 48 . . 11 ? C1 C2 C3 C4 -179.5(4) . . . . ? C1 C2 C1 N1 0.7(5) 48 . . . ? _shelx_res_file ; djx044_0m_sq.res created by SHELXL-2014/7 TITL djx044_0m in Pm-3m #221 REM reset to Pm-3m #221 CELL 0.71073 18.6522 18.6522 18.6522 90 90 90 ZERR 1 0.0005 0.0005 0.0005 0 0 0 LATT 1 SYMM -Y,+X,+Z SYMM -X,-Y,+Z SYMM +Y,-X,+Z SYMM +X,-Z,+Y SYMM +X,-Y,-Z SYMM +X,+Z,-Y SYMM +Z,+Y,-X SYMM -X,+Y,-Z SYMM -Z,+Y,+X SYMM +Z,+X,+Y SYMM +Y,+Z,+X SYMM -Y,-Z,+X SYMM +Z,-X,-Y SYMM -Y,+Z,-X SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,-Z,-X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +Z,-Y,+X SYMM -Z,-Y,-X SFAC C H Cl Co N O UNIT 104.02 56.02 3 13.44 63.98 5.04 EADP C1 N2 EXYZ C1 N2 L.S. 5 0 6 PLAN 20 SIZE 0.1 0.1 0.1 TEMP -173(2) BOND MORE -1 CONF BOND $H ABIN fmap 2 acta 52 REM REM REM WGHT 0.044700 13.244200 FVAR 0.06428 CO1 4 0.500000 0.000000 0.372260 10.25000 0.02339 0.01641 = 0.03321 0.00000 0.00000 0.00000 CL1 3 0.500000 0.000000 0.500000 10.06250 0.02944 0.02383 = 0.02944 0.00000 0.00000 0.00000 O1 6 0.500000 0.000000 0.246038 10.10500 0.05866 0.15897 = 0.10614 0.00000 0.00000 0.00000 N1 5 0.424559 0.072384 0.373187 11.00000 0.02542 0.01659 = 0.02879 0.00479 0.00036 0.00026 C2 1 0.351936 0.163222 0.351936 10.50000 0.03281 0.02419 = 0.03281 0.00306 0.00230 0.00306 C3 1 0.319741 0.227908 0.319741 10.50000 0.02799 0.02724 = 0.02799 0.00456 0.00332 0.00456 C4 1 0.258571 0.258571 0.349265 10.50000 0.03010 0.03010 = 0.02694 0.00860 0.00860 0.00233 AFIX 43 H4 2 0.237323 0.237324 0.390388 10.50000 -1.20000 AFIX 0 PART 2 CO2 4 0.500000 0.146088 0.270695 10.03000 0.02169 0.11184 = 0.05369 0.03196 0.00000 0.00000 N2 5 0.411883 0.127685 0.329268 10.33300 0.02909 0.02573 = 0.03280 0.00954 0.00122 -0.00034 PART 0 PART 3 C1 1 0.411883 0.127685 0.329268 10.66700 0.02909 0.02573 = 0.03280 0.00954 0.00122 -0.00034 AFIX 43 H1 2 0.440080 0.140252 0.288758 10.66700 -1.20000 AFIX 0 HKLF 4 REM djx044_0m in Pm-3m #221 REM R1 = 0.0463 for 926 Fo > 4sig(Fo) and 0.0610 for all 1208 data REM 53 parameters refined using 0 restraints END WGHT 0.0449 13.1866 REM Highest difference peak 0.484, deepest hole -0.897, 1-sigma level 0.068 Q1 1 0.5000 0.0543 0.3837 10.50000 0.05 0.48 Q2 1 0.5485 0.0000 0.2081 10.50000 0.05 0.44 Q3 1 0.5000 0.1801 0.1801 10.25000 0.05 0.41 Q4 1 0.5000 0.0000 0.3236 10.25000 0.05 0.39 Q5 1 0.5000 0.0603 0.2030 10.50000 0.05 0.35 Q6 1 0.5000 -0.0635 0.5000 10.12500 0.05 0.34 Q7 1 0.5000 0.0000 0.4381 10.25000 0.05 0.34 Q8 1 0.5683 0.0000 0.4317 10.25000 0.05 0.29 Q9 1 0.5000 0.0000 0.1670 10.25000 0.05 0.29 Q10 1 0.5000 0.1989 0.3222 10.50000 0.05 0.28 Q11 1 0.5681 0.0000 0.3283 10.50000 0.05 0.28 Q12 1 0.4363 0.0000 0.3587 10.50000 0.05 0.27 Q13 1 0.4290 0.1027 0.2490 11.00000 0.05 0.25 Q14 1 0.3471 0.1683 0.3724 11.00000 0.05 0.25 Q15 1 0.5000 0.1424 0.3286 10.50000 0.05 0.25 Q16 1 0.4691 -0.0293 0.3356 11.00000 0.05 0.25 Q17 1 0.5000 0.4805 0.5000 10.12500 0.05 0.24 Q18 1 0.4405 0.1122 0.2255 11.00000 0.05 0.24 Q19 1 0.3846 0.1577 0.3487 11.00000 0.05 0.23 Q20 1 0.4595 0.0000 0.3973 10.50000 0.05 0.23 ; _shelx_res_checksum 7826 _shelx_hkl_file ; -1 -1 0 243.74 4.70 -1 0 -1 250.00 4.68 -1 0 1 201.04 4.70 1 0 -1 237.92 4.67 1 0 1 245.46 4.68 1 1 0 244.02 4.70 -1 -1 -1 1000.00 22.94 1 1 1 980.81 22.84 -2 0 0 207.07 4.08 2 0 0 203.34 4.05 2 -1 0 9.21 0.24 2 1 0 8.99 0.25 -2 1 0 9.82 0.24 1 0 2 8.99 0.23 -2 -1 0 9.01 0.26 2 0 1 9.39 0.26 0 -1 -2 9.58 0.20 2 0 -1 9.05 0.24 -2 0 -1 9.53 0.26 -2 0 1 8.87 0.23 -2 -1 -1 0.75 0.11 2 -1 1 0.97 0.11 -2 1 1 0.90 0.09 -1 -2 -1 1.03 0.11 -1 -1 -2 0.88 0.09 2 1 -1 1.04 0.12 2 -1 -1 0.94 0.09 -2 -1 1 0.88 0.11 1 1 2 0.93 0.09 2 1 1 0.86 0.11 -2 -2 0 298.13 5.85 -2 0 -2 298.32 5.89 -2 0 2 296.41 5.81 0 -2 -2 295.85 5.74 2 0 -2 294.84 5.82 2 0 2 299.04 5.90 -2 -2 -1 78.84 1.57 -2 -1 -2 76.53 1.56 -2 1 2 79.52 1.51 -1 -2 -2 78.01 1.54 1 2 2 79.08 1.54 2 -1 -2 76.14 1.54 2 1 2 80.19 1.56 2 2 1 78.13 1.57 -2 -2 -2 72.84 1.44 2 -2 -2 70.11 1.39 2 2 2 70.13 1.44 -3 0 0 244.37 4.86 3 0 0 235.23 4.81 -3 1 0 20.73 0.49 3 -1 0 20.32 0.49 3 1 0 19.57 0.50 3 2 0 0.10 0.05 3 -2 0 0.45 0.16 2 0 3 0.10 0.05 3 0 -1 19.45 0.47 0 1 3 19.80 0.41 -3 0 1 19.00 0.46 3 0 1 19.78 0.49 -1 -1 -3 16.19 0.38 -3 1 1 16.09 0.40 3 -1 1 16.47 0.43 3 1 -1 15.44 0.42 1 1 3 16.31 0.38 3 1 1 15.73 0.43 3 -1 -1 15.97 0.40 -1 -3 -2 0.66 0.18 3 -2 1 0.65 0.17 3 2 1 0.59 0.20 -3 0 2 0.47 0.15 3 0 -2 0.45 0.16 0 2 3 0.69 0.11 -1 -2 -3 0.06 0.03 -3 1 2 0.06 0.04 3 -1 2 0.04 0.05 3 1 2 0.03 0.05 1 2 3 0.45 0.15 3 -1 -2 0.11 0.04 -3 2 2 220.96 4.15 2 2 3 207.68 4.10 2 3 2 204.97 4.13 3 -2 -2 211.73 4.19 3 2 2 204.98 4.17 -3 0 3 152.54 2.98 0 -3 -3 148.17 2.90 3 0 3 153.58 2.98 -3 1 3 35.76 0.77 -1 -3 -3 36.19 0.80 3 -1 3 37.30 0.85 3 -1 -3 36.62 0.77 1 3 3 38.08 0.80 3 1 3 36.67 0.85 3 3 1 36.95 0.87 -3 2 3 25.28 0.55 2 3 3 24.56 0.63 3 -3 -2 25.76 0.56 3 -2 -3 24.25 0.55 3 2 3 24.52 0.64 3 3 2 24.80 0.67 3 -3 -3 428.06 8.29 3 3 3 426.99 8.45 4 0 0 16.39 0.48 4 1 0 14.14 0.45 4 -1 0 13.88 0.45 4 2 0 0.75 0.31 2 0 4 0.07 0.06 4 3 0 0.97 0.33 4 -3 0 0.65 0.25 4 0 1 13.76 0.45 4 0 -1 14.00 0.42 0 1 4 14.01 0.34 4 1 -1 141.24 2.85 -1 -1 -4 145.39 2.78 4 -1 1 145.35 2.86 1 1 4 150.90 2.80 4 1 1 143.98 2.87 4 -1 -1 140.86 2.89 4 2 -1 12.36 0.47 4 -2 1 12.29 0.44 4 2 1 12.63 0.46 2 1 4 11.48 0.40 4 -2 -1 11.91 0.41 3 -1 4 15.93 0.50 -3 1 4 16.43 0.40 4 -3 -1 16.07 0.47 3 1 4 16.20 0.52 4 3 1 16.50 0.55 4 0 -2 0.11 0.06 0 2 4 0.10 0.04 4 0 2 -0.09 0.07 -1 -2 -4 11.71 0.35 4 1 -2 12.54 0.44 1 2 4 11.56 0.35 4 1 2 11.48 0.45 4 -1 -2 11.80 0.39 4 -2 2 42.81 0.96 2 2 4 41.39 0.92 4 -2 -2 41.42 0.91 4 2 2 40.81 0.98 4 -3 -2 3.30 0.26 4 3 2 3.81 0.34 3 2 4 3.56 0.31 4 0 -3 1.22 0.27 4 -1 3 15.96 0.53 -1 -3 -4 15.79 0.42 -4 1 3 15.48 0.44 1 3 4 16.28 0.44 4 -1 -3 16.76 0.45 4 1 3 15.47 0.52 -4 2 3 3.61 0.24 4 -2 3 4.09 0.32 4 2 3 3.44 0.32 2 3 4 4.12 0.29 3 4 2 4.45 0.35 4 -2 -3 3.07 0.24 3 3 4 151.54 3.19 3 4 3 164.32 3.21 4 -3 -3 171.20 3.26 4 3 3 160.61 3.23 0 -4 -4 101.62 1.99 4 0 4 101.23 2.10 -4 1 4 56.20 1.17 4 -1 4 58.17 1.28 4 -1 -4 57.08 1.18 4 1 4 56.55 1.27 4 4 1 57.38 1.28 -4 2 4 29.75 0.65 4 -2 4 29.27 0.75 4 -2 -4 28.78 0.65 2 4 4 29.86 0.72 4 2 4 28.65 0.76 4 4 2 29.76 0.78 3 4 4 34.60 0.85 4 -4 -3 36.44 0.79 4 -3 -4 35.59 0.76 4 3 4 35.15 0.88 4 4 3 35.17 0.89 4 -4 -4 628.15 11.86 4 4 4 596.19 12.13 5 0 0 0.98 0.32 5 1 0 1.15 0.32 5 2 0 24.86 0.70 5 -2 0 25.57 0.68 2 0 5 24.91 0.63 5 3 0 12.11 0.49 5 -3 0 12.30 0.45 3 0 5 12.57 0.46 5 4 0 1.35 0.32 5 0 1 0.13 0.08 5 0 -1 0.19 0.07 0 1 5 0.92 0.18 5 1 -1 7.42 0.40 5 -1 1 6.55 0.40 1 1 5 6.93 0.30 5 -1 -1 7.31 0.36 5 1 1 7.12 0.40 5 2 -1 5.34 0.38 5 -2 1 4.85 0.35 5 2 1 4.97 0.38 5 -2 -1 4.29 0.32 2 1 5 4.58 0.29 5 3 -1 0.06 0.08 3 -1 5 0.02 0.06 5 -3 1 0.02 0.07 3 1 5 -0.05 0.07 5 -3 -1 -0.07 0.06 5 3 1 0.09 0.08 4 -1 5 2.47 0.32 -4 1 5 1.99 0.20 5 -4 -1 2.64 0.26 5 4 1 2.97 0.36 4 1 5 2.04 0.30 5 0 -2 25.39 0.66 5 0 2 24.86 0.71 5 1 -2 5.36 0.35 5 -1 2 4.71 0.36 -1 -2 -5 5.02 0.24 5 -1 -2 4.47 0.31 5 1 2 4.67 0.36 1 2 5 4.67 0.25 5 -2 2 13.72 0.50 5 2 -2 14.32 0.51 2 2 5 13.68 0.43 5 -2 -2 13.67 0.44 5 2 2 13.95 0.51 5 -3 2 2.37 0.30 3 2 5 2.06 0.27 5 3 2 2.10 0.32 5 -3 -2 1.98 0.26 -4 2 5 14.84 0.38 4 -2 5 14.97 0.49 5 4 2 14.83 0.54 4 -2 -5 14.72 0.38 5 -4 -2 15.09 0.46 4 2 5 14.68 0.50 5 0 -3 12.55 0.43 5 0 3 12.16 0.49 5 1 -3 0.14 0.07 5 -1 3 -0.08 0.07 -1 -3 -5 0.03 0.04 1 3 5 0.06 0.05 5 -1 -3 -0.01 0.06 5 1 3 -0.06 0.07 5 -2 3 2.27 0.31 2 3 5 2.05 0.24 5 -2 -3 1.84 0.24 5 2 3 2.20 0.31 5 -3 3 105.58 2.15 3 3 5 100.10 2.10 5 -3 -3 106.03 2.08 5 3 3 102.32 2.17 3 5 4 2.46 0.31 4 3 5 2.81 0.29 5 -4 -3 2.68 0.24 5 4 3 2.66 0.33 0 -4 -5 0.39 0.14 5 0 -4 0.59 0.24 5 -1 4 2.58 0.34 5 -1 -4 2.17 0.23 1 4 5 2.59 0.23 5 1 4 1.97 0.31 5 -2 4 14.87 0.53 5 -2 -4 14.48 0.42 5 2 4 14.63 0.53 2 4 5 14.45 0.45 5 -3 4 2.83 0.32 5 -3 -4 2.16 0.22 3 4 5 2.81 0.28 5 3 4 2.06 0.32 4 5 3 2.26 0.34 4 -5 -4 19.69 0.46 4 4 5 17.94 0.59 4 5 4 18.48 0.60 5 -4 -4 18.56 0.50 5 4 4 18.23 0.62 0 -5 -5 123.68 2.43 5 0 5 122.84 2.55 5 -1 5 9.83 0.46 5 1 5 9.50 0.45 5 -2 5 2.04 0.32 5 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0.40 6 -3 7 8.56 0.51 7 6 3 8.29 0.56 6 3 7 8.63 0.49 7 -6 -3 8.83 0.43 7 0 -4 28.54 0.77 7 0 4 28.80 0.85 7 1 -4 2.56 0.34 7 -1 4 2.69 0.37 7 1 4 3.18 0.38 7 -1 -4 3.07 0.30 1 4 7 3.15 0.23 7 -2 4 4.82 0.41 7 -2 -4 5.06 0.32 7 2 4 4.67 0.40 2 4 7 5.15 0.31 7 -3 4 2.30 0.37 7 3 4 1.84 0.38 7 -3 -4 1.76 0.27 3 4 7 2.06 0.29 7 -4 4 42.64 1.12 4 4 7 42.15 1.04 7 -4 -4 42.64 1.00 7 4 4 42.83 1.13 7 -5 4 61.95 1.46 7 -5 -4 63.58 1.38 7 5 4 60.07 1.49 5 4 7 61.91 1.44 6 -4 7 11.81 0.56 7 -6 -4 11.80 0.46 7 6 4 11.73 0.62 6 4 7 11.52 0.56 7 0 -5 92.21 1.97 7 0 5 95.51 2.09 7 -1 5 62.92 1.49 7 -1 -5 62.89 1.37 7 1 5 60.70 1.48 7 -2 5 1.85 0.40 7 2 5 1.38 0.38 2 5 7 2.52 0.29 7 -2 -5 2.50 0.28 7 3 5 1.16 0.38 7 -3 -5 1.06 0.25 3 5 7 1.20 0.31 7 -4 5 60.11 1.47 4 5 7 60.82 1.40 7 -4 -5 63.74 1.35 7 4 5 62.74 1.51 7 -5 5 10.66 0.54 7 5 5 10.52 0.56 7 -5 -5 10.09 0.41 5 5 7 10.03 0.51 5 7 6 0.16 0.11 5 -7 -6 0.03 0.05 7 6 5 0.03 0.11 7 -6 -5 0.04 0.07 6 5 7 -0.07 0.10 7 0 6 0.33 0.11 7 -1 6 0.21 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103.66 2.10 8 3 0 10.20 0.53 8 -3 0 9.26 0.50 3 0 8 10.00 0.45 8 4 0 117.39 2.56 4 0 8 116.63 2.47 8 -4 0 121.94 2.52 8 5 0 0.04 0.11 5 0 8 -0.05 0.09 8 -5 0 -0.01 0.09 8 -6 0 123.72 2.63 6 0 8 124.85 2.65 8 -7 0 4.21 0.43 7 0 8 3.91 0.48 8 0 -1 23.13 0.72 0 1 8 23.63 0.57 8 0 1 22.63 0.74 8 -1 1 48.23 1.18 8 1 -1 46.24 1.18 8 -1 -1 45.61 1.16 1 1 8 47.31 1.04 8 1 1 45.87 1.17 8 -2 1 0.31 0.10 8 2 -1 0.93 0.36 8 -2 -1 1.06 0.32 8 2 1 0.32 0.10 2 1 8 0.34 0.08 8 3 -1 70.48 1.66 8 -3 1 71.50 1.65 3 -1 8 72.84 1.57 3 1 8 73.98 1.58 8 3 1 70.01 1.67 8 -3 -1 74.71 1.64 8 -4 1 24.28 0.77 4 -1 8 23.79 0.73 8 4 -1 23.71 0.81 8 4 1 23.92 0.81 8 -4 -1 24.81 0.75 4 1 8 24.47 0.73 8 -5 1 9.90 0.52 5 -1 8 9.62 0.51 5 1 8 9.52 0.51 8 5 1 10.59 0.58 8 -5 -1 9.92 0.50 6 -1 8 24.89 0.82 8 -6 1 24.66 0.80 8 -6 -1 24.75 0.78 8 6 1 25.60 0.86 6 1 8 24.53 0.81 8 -7 1 8.03 0.50 7 -1 8 8.11 0.55 8 -7 -1 8.51 0.49 7 1 8 7.92 0.55 0 2 8 106.62 2.06 8 0 -2 102.57 2.22 8 0 2 102.81 2.26 8 -1 2 0.26 0.10 8 1 -2 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19.77 0.81 7 -8 -4 20.44 0.62 4 7 8 19.99 0.69 8 4 7 20.09 0.80 8 -4 -7 19.76 0.58 8 -5 7 57.72 1.51 8 -5 -7 57.79 1.29 8 5 7 59.65 1.53 7 -8 -5 58.82 1.32 5 7 8 58.57 1.42 8 -6 7 2.65 0.52 8 6 7 3.48 0.58 6 7 8 3.01 0.52 7 -8 -6 3.06 0.33 7 8 6 2.19 0.57 7 -8 -7 67.78 1.44 7 7 8 69.22 1.69 7 8 7 65.64 1.68 8 -7 -7 66.63 1.47 8 7 7 66.51 1.72 8 -8 0 137.22 2.86 8 0 8 136.43 2.97 8 -1 8 5.23 0.53 8 -8 -1 5.00 0.44 8 1 8 3.84 0.53 8 -2 8 27.31 0.93 8 -8 -2 27.72 0.82 8 2 8 26.61 0.92 8 -3 8 1.70 0.52 8 -8 -3 1.86 0.38 8 3 8 1.41 0.50 8 -4 8 49.02 1.35 8 -4 -8 47.36 1.09 8 -8 -4 48.70 1.19 8 4 8 49.83 1.34 8 -5 8 4.28 0.58 8 -8 -5 3.56 0.39 8 5 8 3.61 0.57 8 8 5 4.19 0.61 8 -6 8 146.44 3.19 8 -8 -6 149.20 3.00 6 8 8 148.14 3.13 8 6 8 149.32 3.19 8 8 6 145.17 3.19 8 -7 8 32.83 1.05 8 -8 -7 29.40 0.83 7 8 8 29.96 1.07 8 7 8 33.71 1.11 8 8 7 30.82 1.10 8 8 8 310.13 6.25 9 0 0 2.63 0.41 9 1 0 15.79 0.65 9 -1 0 15.60 0.65 9 -2 0 49.74 1.26 2 0 9 50.82 1.14 9 2 0 48.22 1.28 3 0 9 12.25 0.51 9 3 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3.75 0.00 2 2 16 -1.45 0.00 0 3 16 -5.19 0.00 1 3 16 -1.05 0.00 2 3 16 1.50 0.00 3 3 16 -0.57 0.00 0 4 16 5.78 0.00 1 4 16 -3.07 0.00 2 4 16 0.38 0.00 3 4 16 -2.95 0.00 4 4 16 0.84 0.00 0 5 16 -6.29 0.00 1 5 16 0.77 0.00 2 5 16 -0.99 0.00 3 5 16 3.03 0.00 4 5 16 -5.45 0.00 5 5 16 2.27 0.00 0 6 16 4.24 0.00 1 6 16 -1.30 0.00 2 6 16 0.19 0.00 3 6 16 -0.65 0.00 4 6 16 3.22 0.00 5 6 16 -0.75 0.00 6 6 16 1.03 0.00 0 7 16 -2.06 0.00 1 7 16 0.47 0.00 2 7 16 1.33 0.00 3 7 16 -0.71 0.00 4 7 16 -1.08 0.00 5 7 16 2.91 0.00 6 7 16 1.02 0.00 7 7 16 1.13 0.00 0 8 16 2.77 0.00 1 8 16 -2.55 0.00 2 8 16 -1.37 0.00 3 8 16 -4.37 0.00 4 8 16 2.59 0.00 5 8 16 -1.77 0.00 6 8 16 3.46 0.00 7 8 16 0.75 0.00 8 8 16 4.39 0.00 0 9 16 -5.29 0.00 1 9 16 0.18 0.00 2 9 16 0.27 0.00 3 9 16 -0.28 0.00 4 9 16 -0.85 0.00 5 9 16 3.07 0.00 6 9 16 0.91 0.00 7 9 16 0.59 0.00 8 9 16 4.83 0.00 9 9 16 1.60 0.00 0 10 16 3.90 0.00 1 10 16 -2.26 0.00 2 10 16 -0.48 0.00 3 10 16 -4.97 0.00 4 10 16 2.07 0.00 5 10 16 -2.68 0.00 6 10 16 2.27 0.00 7 10 16 1.29 0.00 8 10 16 4.13 0.00 9 10 16 3.11 0.00 10 10 16 -0.18 0.00 0 11 16 -1.06 0.00 1 11 16 -1.00 0.00 2 11 16 1.64 0.00 3 11 16 -1.43 0.00 4 11 16 -2.27 0.00 5 11 16 -1.15 0.00 6 11 16 -1.67 0.00 7 11 16 0.51 0.00 8 11 16 -1.80 0.00 9 11 16 -2.81 0.00 10 11 16 0.06 0.00 0 12 16 -0.77 0.00 1 12 16 0.13 0.00 2 12 16 -5.17 0.00 3 12 16 -1.94 0.00 4 12 16 -3.17 0.00 5 12 16 2.31 0.00 6 12 16 -2.04 0.00 7 12 16 -0.86 0.00 8 12 16 -2.31 0.00 9 12 16 1.94 0.00 0 13 16 -2.77 0.00 1 13 16 0.20 0.00 2 13 16 -0.82 0.00 3 13 16 1.76 0.00 4 13 16 -0.50 0.00 5 13 16 0.84 0.00 6 13 16 -1.23 0.00 7 13 16 2.02 0.00 8 13 16 -0.25 0.00 0 14 16 0.89 0.00 1 14 16 -1.29 0.00 2 14 16 1.19 0.00 3 14 16 2.22 0.00 4 14 16 3.12 0.00 5 14 16 3.48 0.00 6 14 16 3.37 0.00 0 15 16 -1.11 0.00 1 15 16 -3.39 0.00 2 15 16 -1.33 0.00 3 15 16 -3.17 0.00 0 0 17 -3.53 0.00 0 1 17 1.55 0.00 1 1 17 3.31 0.00 0 2 17 2.84 0.00 1 2 17 0.12 0.00 2 2 17 10.22 0.00 0 3 17 1.65 0.00 1 3 17 1.53 0.00 2 3 17 -2.14 0.00 3 3 17 -4.62 0.00 0 4 17 -3.11 0.00 1 4 17 1.29 0.00 2 4 17 1.35 0.00 3 4 17 1.26 0.00 4 4 17 -9.81 0.00 0 5 17 2.38 0.00 1 5 17 -3.19 0.00 2 5 17 -0.13 0.00 3 5 17 -1.64 0.00 4 5 17 2.93 0.00 5 5 17 -2.92 0.00 0 6 17 -6.14 0.00 1 6 17 2.10 0.00 2 6 17 0.09 0.00 3 6 17 4.86 0.00 4 6 17 -3.38 0.00 5 6 17 3.98 0.00 6 6 17 -3.18 0.00 0 7 17 1.59 0.00 1 7 17 0.08 0.00 2 7 17 1.55 0.00 3 7 17 -1.83 0.00 4 7 17 2.18 0.00 5 7 17 -4.22 0.00 6 7 17 2.88 0.00 7 7 17 -2.05 0.00 0 8 17 -0.65 0.00 1 8 17 1.36 0.00 2 8 17 1.72 0.00 3 8 17 1.70 0.00 4 8 17 -2.32 0.00 5 8 17 2.60 0.00 6 8 17 -0.57 0.00 7 8 17 2.17 0.00 8 8 17 1.66 0.00 0 9 17 1.22 0.00 1 9 17 -2.00 0.00 2 9 17 1.36 0.00 3 9 17 -3.40 0.00 4 9 17 1.17 0.00 5 9 17 -3.44 0.00 6 9 17 0.26 0.00 7 9 17 -0.07 0.00 8 9 17 1.94 0.00 9 9 17 1.21 0.00 0 10 17 -2.70 0.00 1 10 17 1.39 0.00 2 10 17 1.11 0.00 3 10 17 -0.59 0.00 4 10 17 0.16 0.00 5 10 17 0.43 0.00 6 10 17 0.48 0.00 7 10 17 2.96 0.00 8 10 17 1.60 0.00 9 10 17 -1.36 0.00 10 10 17 -0.74 0.00 0 11 17 0.64 0.00 1 11 17 -0.27 0.00 2 11 17 0.68 0.00 3 11 17 -0.19 0.00 4 11 17 2.44 0.00 5 11 17 2.21 0.00 6 11 17 2.46 0.00 7 11 17 -1.40 0.00 8 11 17 0.49 0.00 9 11 17 -2.37 0.00 0 12 17 2.92 0.00 1 12 17 -2.47 0.00 2 12 17 2.21 0.00 3 12 17 -0.63 0.00 4 12 17 1.33 0.00 5 12 17 2.76 0.00 6 12 17 2.24 0.00 7 12 17 -1.51 0.00 0 13 17 0.37 0.00 1 13 17 -1.03 0.00 2 13 17 -0.25 0.00 3 13 17 -1.37 0.00 4 13 17 0.29 0.00 5 13 17 -0.21 0.00 0 14 17 -3.19 0.00 1 14 17 1.11 0.00 2 14 17 -0.63 0.00 0 0 18 7.06 0.00 0 1 18 -2.22 0.00 1 1 18 -1.66 0.00 0 2 18 -0.06 0.00 1 2 18 4.22 0.00 2 2 18 -1.14 0.00 0 3 18 -2.88 0.00 1 3 18 2.45 0.00 2 3 18 0.05 0.00 3 3 18 2.01 0.00 0 4 18 2.31 0.00 1 4 18 0.10 0.00 2 4 18 -0.12 0.00 3 4 18 -3.84 0.00 4 4 18 -2.43 0.00 0 5 18 -5.17 0.00 1 5 18 -1.07 0.00 2 5 18 -2.54 0.00 3 5 18 3.31 0.00 4 5 18 -4.66 0.00 5 5 18 1.54 0.00 0 6 18 -0.55 0.00 1 6 18 -0.87 0.00 2 6 18 0.06 0.00 3 6 18 0.27 0.00 4 6 18 1.24 0.00 5 6 18 -2.93 0.00 6 6 18 -0.12 0.00 0 7 18 -2.02 0.00 1 7 18 -2.78 0.00 2 7 18 0.91 0.00 3 7 18 2.35 0.00 4 7 18 -1.35 0.00 5 7 18 -0.48 0.00 6 7 18 -0.38 0.00 7 7 18 2.67 0.00 0 8 18 0.31 0.00 1 8 18 -0.98 0.00 2 8 18 -0.45 0.00 3 8 18 -0.78 0.00 4 8 18 2.56 0.00 5 8 18 -1.33 0.00 6 8 18 2.88 0.00 7 8 18 1.03 0.00 8 8 18 1.01 0.00 0 9 18 -3.41 0.00 1 9 18 -1.91 0.00 2 9 18 0.74 0.00 3 9 18 -2.60 0.00 4 9 18 0.24 0.00 5 9 18 -4.11 0.00 6 9 18 3.06 0.00 7 9 18 1.89 0.00 8 9 18 1.92 0.00 9 9 18 -0.18 0.00 0 10 18 2.12 0.00 1 10 18 0.34 0.00 2 10 18 1.05 0.00 3 10 18 -2.69 0.00 4 10 18 -0.80 0.00 5 10 18 -0.89 0.00 6 10 18 1.12 0.00 7 10 18 3.12 0.00 8 10 18 3.68 0.00 0 11 18 -2.02 0.00 1 11 18 -1.64 0.00 2 11 18 0.71 0.00 3 11 18 -0.44 0.00 4 11 18 -0.98 0.00 5 11 18 -0.88 0.00 6 11 18 3.14 0.00 0 12 18 1.87 0.00 1 12 18 2.61 0.00 2 12 18 0.06 0.00 3 12 18 0.28 0.00 4 12 18 -2.97 0.00 5 12 18 2.32 0.00 0 13 18 -1.03 0.00 0 0 19 1.94 0.00 0 1 19 5.52 0.00 1 1 19 -0.86 0.00 0 2 19 -0.85 0.00 1 2 19 1.61 0.00 2 2 19 -0.59 0.00 0 3 19 6.50 0.00 1 3 19 0.41 0.00 2 3 19 1.55 0.00 3 3 19 -2.35 0.00 0 4 19 -4.33 0.00 1 4 19 0.34 0.00 2 4 19 -3.05 0.00 3 4 19 3.52 0.00 4 4 19 -2.80 0.00 0 5 19 0.68 0.00 1 5 19 -2.87 0.00 2 5 19 -3.09 0.00 3 5 19 -0.54 0.00 4 5 19 1.52 0.00 5 5 19 2.77 0.00 0 6 19 -0.94 0.00 1 6 19 -1.21 0.00 2 6 19 0.18 0.00 3 6 19 1.01 0.00 4 6 19 1.31 0.00 5 6 19 -0.57 0.00 6 6 19 1.74 0.00 0 7 19 -1.37 0.00 1 7 19 0.46 0.00 2 7 19 -1.35 0.00 3 7 19 -0.29 0.00 4 7 19 1.41 0.00 5 7 19 -0.48 0.00 6 7 19 2.62 0.00 7 7 19 2.58 0.00 0 8 19 0.27 0.00 1 8 19 -1.80 0.00 2 8 19 -2.23 0.00 3 8 19 0.04 0.00 4 8 19 1.45 0.00 5 8 19 -0.66 0.00 6 8 19 1.61 0.00 7 8 19 0.58 0.00 8 8 19 -1.96 0.00 0 9 19 1.47 0.00 1 9 19 0.25 0.00 2 9 19 1.12 0.00 3 9 19 0.08 0.00 4 9 19 3.07 0.00 5 9 19 1.88 0.00 6 9 19 0.99 0.00 7 9 19 2.91 0.00 0 10 19 -1.00 0.00 1 10 19 1.27 0.00 2 10 19 0.99 0.00 3 10 19 0.50 0.00 4 10 19 2.67 0.00 5 10 19 -1.29 0.00 0 11 19 -3.11 0.00 1 11 19 -5.20 0.00 2 11 19 -0.72 0.00 3 11 19 -2.52 0.00 0 0 20 8.04 0.00 0 1 20 -4.00 0.00 1 1 20 0.02 0.00 0 2 20 5.28 0.00 1 2 20 4.71 0.00 2 2 20 1.27 0.00 0 3 20 0.01 0.00 1 3 20 3.52 0.00 2 3 20 0.09 0.00 3 3 20 1.24 0.00 0 4 20 1.70 0.00 1 4 20 -1.71 0.00 2 4 20 -0.97 0.00 3 4 20 -1.40 0.00 4 4 20 -3.15 0.00 0 5 20 -1.76 0.00 1 5 20 -0.62 0.00 2 5 20 -0.37 0.00 3 5 20 -1.88 0.00 4 5 20 1.24 0.00 5 5 20 -1.43 0.00 0 6 20 -0.14 0.00 1 6 20 0.94 0.00 2 6 20 -0.47 0.00 3 6 20 -1.19 0.00 4 6 20 -2.62 0.00 5 6 20 0.25 0.00 6 6 20 -2.03 0.00 0 7 20 0.99 0.00 1 7 20 -0.76 0.00 2 7 20 3.53 0.00 3 7 20 -0.17 0.00 4 7 20 1.83 0.00 5 7 20 -2.47 0.00 6 7 20 1.27 0.00 0 8 20 0.65 0.00 1 8 20 -2.12 0.00 2 8 20 -1.31 0.00 3 8 20 -2.78 0.00 4 8 20 0.03 0.00 5 8 20 -2.29 0.00 0 9 20 -2.38 0.00 1 9 20 0.42 0.00 2 9 20 0.30 0.00 3 9 20 0.09 0.00 0 0 21 -5.76 0.00 0 1 21 3.52 0.00 1 1 21 -2.39 0.00 0 2 21 -0.56 0.00 1 2 21 1.82 0.00 2 2 21 2.23 0.00 0 3 21 -0.76 0.00 1 3 21 -4.08 0.00 2 3 21 -1.13 0.00 3 3 21 -1.45 0.00 0 4 21 -6.35 0.00 1 4 21 -0.85 0.00 2 4 21 0.60 0.00 3 4 21 2.00 0.00 4 4 21 -0.96 0.00 0 5 21 3.62 0.00 1 5 21 -2.66 0.00 2 5 21 1.19 0.00 3 5 21 -2.48 0.00 4 5 21 0.03 0.00 5 5 21 0.98 0.00 0 6 21 0.51 0.00 1 6 21 1.16 0.00 2 6 21 0.08 0.00 3 6 21 -4.46 0.00 4 6 21 -1.85 0.00 0 7 21 3.09 0.00 1 7 21 2.83 0.00 0 0 22 12.11 0.00 0 1 22 0.73 0.00 1 1 22 3.38 0.00 0 2 22 4.48 0.00 1 2 22 3.19 0.00 2 2 22 -1.57 0.00 0 3 22 -3.23 0.00 0 0 1 -42.31 0.00 10 13 15 -3.36 0.00 7 15 15 -2.36 0.00 11 11 16 -0.75 0.00 10 12 16 -0.60 0.00 7 14 16 0.24 0.00 4 15 16 5.71 0.00 8 12 17 -0.21 0.00 6 13 17 0.17 0.00 3 14 17 3.10 0.00 4 14 17 -0.56 0.00 7 11 18 2.33 0.00 1 13 18 -2.07 0.00 2 13 18 -0.56 0.00 6 10 19 1.72 0.00 4 11 19 -0.13 0.00 7 7 20 0.62 0.00 6 8 20 -1.86 0.00 4 9 20 2.27 0.00 0 10 20 0.75 0.00 1 10 20 0.83 0.00 2 7 21 1.87 0.00 3 7 21 -0.62 0.00 1 3 22 -1.67 0.00 2 3 22 -2.46 0.00 0 4 22 1.73 0.00 1 4 22 -2.44 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 11015) # 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 -0.001 -0.001 3019 126 ' ' 2 0.500 0.500 0.500 921 144 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 0 1 1.092 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL djx044_0m P m -3 m R = 0.14 CELL 18.6522 18.6522 18.6522 90.00 90.00 90.00 SPGR Pm-3m # Solvent Accessible Volume = 3941.2 # Electrons Found in S.A.V. = 261.8 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.500 0.500 0.500 ! 6.55 eA-3 C102 0.500 0.504 0.266 ! 5.51 eA-3 C103 0.500 0.188 0.505 ! 3.93 eA-3 Q104 0.129 0.500 0.500 ! 2.10 eA-3 C105 0.423 0.297 0.495 ! 1.68 eA-3 C106 0.500 1.000 0.000 ! 1.33 eA-3 C107 0.059 0.059 0.059 ! 1.24 eA-3 Q108 0.370 0.500 0.000 ! 1.23 eA-3 C109 1.000 0.125 0.000 ! 1.19 eA-3 Q110 1.000 0.496 0.125 ! 1.07 eA-3 Q111 0.500 0.234-0.001 ! 0.84 eA-3 Q112 0.793 1.004 0.437 ! 0.77 eA-3 Q113 0.500 0.283 0.168 ! 0.73 eA-3 Q114 0.127 0.507 0.250 ! 0.71 eA-3 Q115 0.437 1.000 0.500 ! 0.67 eA-3 Q116 0.356 0.182 0.343 ! 0.60 eA-3 C117 1.000 1.000 0.438 ! 0.60 eA-3 C118 0.048 0.050 0.439 ! 0.54 eA-3 C119 0.500 0.356 0.426 ! 0.51 eA-3 Q120 0.765 0.998 0.375 ! 0.50 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_Co-BDTriP-O2 _audit_creation_date 2016-02-04 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common 'Co-BDTriP-O2' _chemical_name_systematic ? _chemical_formula_moiety '(C87.98 H39.98 Cl3 Co12 N80.02 O23.62) Co1.5' _chemical_formula_sum 'C87.98 H39.98 Cl3 Co13.5 N80.02 O23.62' _chemical_formula_weight 3497.71 _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' 0.0033 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 221 _space_group_name_H-M_alt 'P m -3 m' _space_group_name_Hall '-P 4 2 3' loop_ _space_group_symop_operation_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, -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' _cell_length_a 18.6011(7) _cell_length_b 18.6011(7) _cell_length_c 18.6011(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6436.0(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9928 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.774 _cell_measurement_theta_min 2.449 _shelx_estimated_absorpt_T_max 0.932 _shelx_estimated_absorpt_T_min 0.932 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0585 before and 0.0439 after correction. The Ratio of minimum to maximum transmission is 0.6850. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'dark green' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 0.894 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1717 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_special_details ; A methanol-solvated single crystal of single crystal of Co-BDTriP (Co3[(Co4Cl)3(BDTriP)8]2, H3BDTriP = 4,4'-(5-(1H-pyrazol-4-yl)-1,3-phenylene)bis(1H-1,2,3-triazole)) was epoxied on a thin glass fiber and carefully inserted into a 1.0 mm borosilicate capillary. The capillary was then attached to a Micromeretics ASAP 2020 instrument via a custom-designed adapter, degassed at 453 K using a sand bath, and then dosed with 400 mbar O2. After dosing O2, the capillary was flame sealed. Data was collected using a Bruker QUAZAR diffractometer equipped with a Bruker AXS APEX II detector, using MoKa radiation (lamda = 0.71073 angstroms). ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0166 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_number 1367 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.330 _diffrn_reflns_theta_min 1.548 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w/\q scans' _diffrn_radiation_monochromator 'channel-cut Si(111) crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1158 _reflns_number_total 1367 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX 2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.399 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.102 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1367 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0619 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+16.2555P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1830 _refine_ls_wR_factor_ref 0.1918 _refine_special_details ; Thermal parameters were refined anisotropically for all non-hydrogen atoms. Hydrogen atoms were placed in ideal positions and refined using a riding model. Co-BDTriP is an anionic framework ([(Co4Cl)3(BDTriP)8]3-) and, thus, contains charge-balancing cations. These cations are likely Co(II) (three Co(II) per two [(Co4Cl)3(BDTriP)8]3-). The location of these charge-balancing Co(II) cations (Co2) was assigned to electron density found between two triazolate groups that are adjacent to each other on the [Co4Cl]7+ cluster, corresponding to a model where nitrogen atoms on adjacent triazolate groups are coordinated to Co. The site occupancy factor of Co2 was refined then were fixed in the final refinement. This gave a chemical occupancy of 3.8% for both, corresponding to 0.9 extra-framework Co centers per formula unit. The remaining extra-framework Co cations could not be located and were omitted from the refinement but not the formula. Each linker has two triazolate groups and one pyrazolate group that are disordered, due to the three-fold and mirror symmetery of the structure. Thus, C1 and N2 on the triazolate/pyrazolate rings were restrained to have the same coordinates and displacement parameters. The site occupancy factors of C1 and N2 were fixed to reflect a statistical distribution, corresponding to a chemical occupancy of 66.7% for C1 and 33.3% for N2. O2 coordinated to the framework Co centers was disordered over two positions and required displacement parameter and distance restraints. The site occupancy factors of the coordinated O2 were refined using a free variable then fixed in the final refinement. This resulted in a chemical occupancy of 98.4% for O2. Disorder of the remaining extra-framework Co cations and residual solvent within the pores of the crystal was extensive and could not be modeled. Consequently, the unassigned electron density was accounted for using SQUEEZE as implemented in the PLATON interface. Refinement before SQUEEZE was applied gave an R1 of 13.64% (wR2 = 44.76%), while applying SQUEEZE resulted in an R1 of 4.63% (wR2 = 12.33%). ; _vrf_PLAT307_djx045_0m_sq ; PROBLEM: Isolated Metal Atom (Unusual !) ................ RESPONSE: This metal atom is Co2 which is not single bonded in the structure but coordinated to two triazolate nitrogens. Additional ligands coordinated to this Co center could not be located in the electron density difference map, due to disorder and the low site occupancy of the extra-framework Co moieties. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Shared sites {C1, N2} 3. Restrained distances O2-O1 1.21 with sigma of 0.02 4. Rigid bond restraints O1, O2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints O1 \\sim O2 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C1) = Uanis(N2) Uanis(C1) = Uanis(N2) 6. Others Fixed Sof: O1(0.246) O2(0.246) Co2(0.019) N2(0.667) C1(0.333) H1(0.333) 7.a Aromatic/amide H refined with riding coordinates: C4(H4), C1(H1) ; _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.13023(5) 0.0000 0.5000 0.0227(3) Uani 1 4 d S T P . . Cl1 Cl 0.0000 0.0000 0.5000 0.0259(7) Uani 1 16 d S T P . . O1 O 0.2360(4) 0.0000 0.5000 0.070(2) Uani 0.984 4 d DS TU P . . O2 O 0.2749(9) 0.0495(10) 0.5000 0.146(7) Uani 0.492 2 d DS TU P . . N1 N 0.12684(14) 0.07567(14) 0.42716(13) 0.0222(6) Uani 1 1 d . . . . . C2 C 0.14629(18) 0.14629(18) 0.3356(2) 0.0258(10) Uani 1 2 d S T P . . C3 C 0.17803(18) 0.17803(18) 0.2706(2) 0.0257(10) Uani 1 2 d S T P . . C4 C 0.1486(3) 0.23948(18) 0.23948(18) 0.0281(10) Uani 1 2 d S T P . . H4 H 0.1073 0.2607 0.2607 0.034 Uiso 1 2 calc RS T P A . Co2 Co 0.2294(9) 0.0000 0.3544(10) 0.028(4) Uani 0.038 2 d S T P A 1 N2 N 0.16982(16) 0.08762(16) 0.37155(15) 0.0291(7) Uani 0.667 1 d . . . A 1 C1 C 0.16982(16) 0.08762(16) 0.37155(15) 0.0291(7) Uani 0.333 1 d . . . A 2 H1 H 0.2106 0.0595 0.3590 0.035 Uiso 0.333 1 calc R . . A 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 Co1 0.0298(6) 0.0229(5) 0.0155(5) 0.000 0.000 0.000 Cl1 0.0306(10) 0.0306(10) 0.0167(14) 0.000 0.000 0.000 O1 0.065(5) 0.059(4) 0.087(5) 0.000 0.000 0.000 O2 0.107(13) 0.174(16) 0.157(16) 0.000 0.000 -0.061(10) N1 0.0241(14) 0.0258(13) 0.0166(12) -0.0023(11) 0.0023(10) -0.0003(10) C2 0.0267(14) 0.0267(14) 0.024(2) -0.0004(13) -0.0004(13) 0.0033(18) C3 0.0270(14) 0.0270(14) 0.023(2) 0.0061(13) 0.0061(13) 0.0029(19) C4 0.028(2) 0.0284(15) 0.0284(15) 0.0021(19) 0.0114(14) 0.0114(14) Co2 0.016(7) 0.022(8) 0.044(10) 0.000 0.022(7) 0.000 N2 0.0306(16) 0.0323(16) 0.0245(15) 0.0004(12) 0.0082(12) 0.0003(13) C1 0.0306(16) 0.0323(16) 0.0245(15) 0.0004(12) 0.0082(12) 0.0003(13) _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 Co1 Cl1 2.4224(9) . ? Co1 O1 1.967(8) . ? Co1 N1 1.955(3) . ? Co1 N1 1.955(3) 27_556 ? Co1 N1 1.955(3) 6_556 ? Co1 N1 1.955(3) 33 ? Cl1 Co1 2.4225(9) 25_556 ? Cl1 Co1 2.4225(9) 2 ? Cl1 Co1 2.4225(9) 26_556 ? O1 O2 1.172(12) . ? O1 O2 1.172(12) 6_556 ? N1 N1 1.346(5) 44 ? N1 N2 1.326(4) . ? N1 C1 1.326(4) . ? C2 C3 1.469(6) . ? C2 N2 1.353(4) 44 ? C2 N2 1.353(4) . ? C2 C1 1.353(4) . ? C2 C1 1.353(4) 44 ? C3 C4 1.393(3) 11 ? C3 C4 1.393(3) . ? C4 C3 1.393(3) 12 ? C4 H4 0.9500 . ? Co2 N2 1.996(9) 33 ? Co2 N2 1.996(9) . ? C1 H1 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 O1 Co1 Cl1 180.0 . . ? N1 Co1 Cl1 88.15(8) 27_556 . ? N1 Co1 Cl1 88.15(8) 33 . ? N1 Co1 Cl1 88.15(8) . . ? N1 Co1 Cl1 88.15(8) 6_556 . ? N1 Co1 O1 91.85(8) 33 . ? N1 Co1 O1 91.85(8) . . ? N1 Co1 O1 91.85(8) 27_556 . ? N1 Co1 O1 91.85(8) 6_556 . ? N1 Co1 N1 92.12(14) 33 . ? N1 Co1 N1 92.12(14) 27_556 6_556 ? N1 Co1 N1 87.76(14) 33 6_556 ? N1 Co1 N1 176.30(16) 6_556 . ? N1 Co1 N1 176.30(16) 33 27_556 ? N1 Co1 N1 87.76(14) 27_556 . ? Co1 Cl1 Co1 90.0 . 26_556 ? Co1 Cl1 Co1 90.0 . 2 ? Co1 Cl1 Co1 90.0 26_556 25_556 ? Co1 Cl1 Co1 90.0 25_556 2 ? Co1 Cl1 Co1 180.0 26_556 2 ? Co1 Cl1 Co1 180.0 . 25_556 ? O2 O1 Co1 128.2(11) . . ? O2 O1 Co1 128.2(11) 6_556 . ? O2 O1 O2 104(2) . 6_556 ? N1 N1 Co1 122.14(8) 44 . ? N2 N1 Co1 129.9(2) . . ? N2 N1 N1 107.93(18) . 44 ? C1 N1 Co1 129.9(2) . . ? C1 N1 N1 107.93(18) . 44 ? N2 C2 C3 127.0(2) . . ? N2 C2 C3 126.9(2) 44 . ? N2 C2 N2 106.1(4) . 44 ? C1 C2 C3 126.9(2) 44 . ? C1 C2 C3 127.0(2) . . ? C1 C2 C1 106.1(4) . 44 ? C4 C3 C2 120.9(2) 11 . ? C4 C3 C2 120.9(2) . . ? C4 C3 C4 118.1(4) 11 . ? C3 C4 C3 121.8(4) 12 . ? C3 C4 H4 119.1 12 . ? C3 C4 H4 119.1 . . ? N2 Co2 N2 109.4(7) 33 . ? N1 N2 C2 109.0(3) . . ? N1 N2 Co2 108.8(4) . . ? C2 N2 Co2 139.4(5) . . ? N1 C1 C2 109.0(3) . . ? N1 C1 H1 125.5 . . ? C2 C1 H1 125.5 . . ? 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 Co1 N1 N2 C2 179.7(3) . . . . ? Co1 N1 N2 Co2 14.7(6) . . . . ? Co1 N1 C1 C2 179.7(3) . . . . ? N1 N1 N2 C2 -0.2(3) 44 . . . ? N1 N1 N2 Co2 -165.1(6) 44 . . . ? N1 N1 C1 C2 -0.2(3) 44 . . . ? C2 C3 C4 C3 179.8(3) . . . 12 ? C3 C2 N2 N1 -179.7(4) . . . . ? C3 C2 N2 Co2 -21.9(10) . . . . ? C3 C2 C1 N1 -179.7(4) . . . . ? C4 C3 C4 C3 1.4(10) 11 . . 12 ? N2 C2 C3 C4 0.8(7) 44 . . . ? N2 C2 C3 C4 -179.2(5) . . . . ? N2 C2 C3 C4 -0.8(7) . . . 11 ? N2 C2 C3 C4 179.2(5) 44 . . 11 ? N2 C2 N2 N1 0.3(5) 44 . . . ? N2 C2 N2 Co2 158.1(7) 44 . . . ? C1 C2 C3 C4 179.2(5) 44 . . 11 ? C1 C2 C3 C4 -179.2(5) . . . . ? C1 C2 C3 C4 0.8(7) 44 . . . ? C1 C2 C3 C4 -0.8(7) . . . 11 ? C1 C2 C1 N1 0.3(5) 44 . . . ? _shelx_res_file ; djx045_0m_sq.res created by SHELXL-2014/7 TITL djx045_0m in Pm-3m #221 REM reset to Pm-3m #221 CELL 0.71073 18.6011 18.6011 18.6011 90 90 90 ZERR 1 0.0007 0.0007 0.0007 0 0 0 LATT 1 SYMM -Y,+X,+Z SYMM -X,-Y,+Z SYMM +Y,-X,+Z SYMM +X,-Z,+Y SYMM +X,-Y,-Z SYMM +X,+Z,-Y SYMM +Z,+Y,-X SYMM -X,+Y,-Z SYMM -Z,+Y,+X SYMM +Z,+X,+Y SYMM +Y,+Z,+X SYMM -Y,-Z,+X SYMM +Z,-X,-Y SYMM -Y,+Z,-X SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,-Z,-X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +Z,-Y,+X SYMM -Z,-Y,-X SFAC C H Cl Co N O UNIT 87.98 39.98 3 12.91 80.02 23.62 DFIX 1.21 O2 O1 DELU O1 O2 SIMU O1 O2 O2 EADP C1 N2 EADP C1 N2 EXYZ C1 N2 L.S. 5 0 10 PLAN 20 SIZE 0.08 0.08 0.08 TEMP -173(2) BOND MORE -1 CONF BOND $H ABIN fmap 2 acta 52 REM REM REM WGHT 0.097300 16.255499 FVAR 0.07875 CO1 4 0.130229 0.000000 0.500000 10.25000 0.02978 0.02291 = 0.01548 0.00000 0.00000 0.00000 CL1 3 0.000000 0.000000 0.500000 10.06250 0.03056 0.03056 = 0.01671 0.00000 0.00000 0.00000 O1 6 0.235989 0.000000 0.500000 10.24600 0.06498 0.05884 = 0.08727 0.00000 0.00000 0.00000 O2 6 0.274931 0.049534 0.500000 10.24600 0.10663 0.17413 = 0.15713 0.00000 0.00000 -0.06077 N1 5 0.126839 0.075669 0.427156 11.00000 0.02408 0.02583 = 0.01660 -0.00233 0.00227 -0.00027 C2 1 0.146285 0.146285 0.335575 10.50000 0.02674 0.02674 = 0.02378 -0.00040 -0.00040 0.00333 C3 1 0.178034 0.178034 0.270612 10.50000 0.02703 0.02703 = 0.02315 0.00609 0.00609 0.00285 C4 1 0.148618 0.239480 0.239480 10.50000 0.02758 0.02839 = 0.02839 0.00208 0.01144 0.01144 AFIX 43 H4 2 0.107341 0.260749 0.260747 10.50000 -1.20000 AFIX 0 PART 1 CO2 4 0.229393 0.000000 0.354443 10.01900 0.01610 0.02240 = 0.04436 0.00000 0.02209 0.00000 N2 5 0.169818 0.087617 0.371551 10.66700 0.03056 0.03227 = 0.02445 0.00036 0.00815 0.00026 PART 0 PART 2 C1 1 0.169818 0.087617 0.371551 10.33300 0.03056 0.03227 = 0.02445 0.00036 0.00815 0.00026 AFIX 43 H1 2 0.210570 0.059509 0.358998 10.33300 -1.20000 AFIX 0 HKLF 4 REM djx045_0m in Pm-3m #221 REM R1 = 0.0619 for 1158 Fo > 4sig(Fo) and 0.0701 for all 1367 data REM 59 parameters refined using 8 restraints END WGHT 0.0972 16.2462 REM Highest difference peak 1.399, deepest hole -0.508, 1-sigma level 0.102 Q1 1 0.3373 0.0000 0.3373 10.25000 0.05 1.40 Q2 1 0.0000 0.0000 0.5489 10.12500 0.05 0.97 Q3 1 0.2760 0.0000 0.4593 10.50000 0.05 0.84 Q4 1 0.0445 0.0000 0.5000 10.25000 0.05 0.59 Q5 1 0.0263 0.0485 0.5000 10.50000 0.05 0.41 Q6 1 0.0358 0.2823 0.2823 10.50000 0.05 0.39 Q7 1 0.2495 0.0000 0.2495 10.25000 0.05 0.36 Q8 1 0.1439 0.0000 0.4681 10.50000 0.05 0.35 Q9 1 0.0000 0.0500 0.4767 10.50000 0.05 0.34 Q10 1 0.1718 0.0561 0.4627 11.00000 0.05 0.33 Q11 1 0.1627 0.0973 0.4223 11.00000 0.05 0.32 Q12 1 0.1308 0.1308 0.3048 10.50000 0.05 0.32 Q13 1 0.1712 0.1328 0.2177 11.00000 0.05 0.31 Q14 1 0.0957 0.0957 0.3061 10.50000 0.05 0.31 Q15 1 0.1327 0.2864 0.2864 10.50000 0.05 0.30 Q16 1 0.1503 0.2956 0.2956 10.50000 0.05 0.29 Q17 1 0.2181 0.0588 0.3821 11.00000 0.05 0.29 Q18 1 0.2410 0.0000 0.2790 10.50000 0.05 0.29 Q19 1 0.2498 0.0442 0.5000 10.50000 0.05 0.29 Q20 1 0.2373 0.0692 0.3879 11.00000 0.05 0.29 ; _shelx_res_checksum 33143 _shelx_hkl_file ; 0 1 1 333.03 5.28 0 2 0 292.77 3.63 0 2 1 6.99 0.25 0 2 2 192.93 1.73 0 3 0 330.65 3.00 0 3 1 77.51 0.26 0 3 2 2.49 0.06 0 3 3 218.40 0.71 0 4 0 1.12 0.11 0 4 1 26.86 0.13 0 4 2 10.47 0.08 0 4 3 1.40 0.23 0 4 4 356.36 5.07 0 5 0 12.27 0.25 0 5 1 4.17 0.06 0 5 2 26.51 0.07 0 5 3 75.34 0.31 0 5 4 0.99 0.05 0 5 5 207.69 1.67 0 6 0 355.85 7.08 0 6 1 35.39 0.12 0 6 2 28.43 0.08 0 6 3 26.71 0.24 0 6 4 158.58 0.82 0 6 5 14.42 0.11 0 6 6 130.79 1.13 0 7 0 82.69 0.19 0 7 1 53.65 0.28 0 7 2 31.96 0.23 0 7 3 24.27 0.11 0 7 4 34.73 0.17 0 7 5 190.35 0.99 0 7 6 4.00 0.09 0 7 7 144.74 0.78 0 8 0 742.99 9.48 0 8 1 33.57 0.24 0 8 2 148.54 0.83 0 8 3 21.78 0.17 0 8 4 237.27 1.12 0 8 5 0.04 0.10 0 8 6 202.10 1.13 0 8 7 5.95 0.11 0 8 8 205.51 2.23 0 9 0 0.51 0.20 0 9 1 33.68 0.20 0 9 2 58.57 0.36 0 9 3 27.15 0.19 0 9 4 20.34 0.24 0 9 5 43.23 0.33 0 9 6 9.76 0.14 0 9 7 12.38 0.16 0 9 8 23.39 0.22 0 9 9 2.55 0.19 0 10 0 27.23 0.53 0 10 1 4.20 0.11 0 10 2 55.21 0.28 0 10 3 0.02 0.06 0 10 4 10.20 0.17 0 10 5 0.05 0.04 0 10 6 29.86 0.29 0 10 7 13.54 0.18 0 10 8 54.26 0.41 0 10 9 1.84 0.16 0 10 10 43.01 0.80 0 11 0 0.95 0.19 0 11 1 37.88 0.22 0 11 2 54.04 0.26 0 11 3 73.77 0.35 0 11 4 37.22 0.32 0 11 5 7.02 0.14 0 11 6 1.81 0.19 0 11 7 41.11 0.35 0 11 8 21.94 0.24 0 11 9 82.53 0.81 0 11 10 0.00 0.06 0 11 11 7.94 0.36 0 12 0 377.27 3.33 0 12 1 29.52 0.23 0 12 2 3.92 0.13 0 12 3 24.30 0.24 0 12 4 25.12 0.23 0 12 5 0.30 0.08 0 12 6 27.51 0.28 0 12 7 30.96 0.34 0 12 8 156.57 1.04 0 12 9 6.02 0.22 0 12 10 3.21 0.22 0 12 11 8.56 0.23 0 12 12 7.52 0.34 0 13 0 12.87 0.32 0 13 1 52.87 0.37 0 13 2 9.99 0.16 0 13 3 17.23 0.20 0 13 4 0.76 0.10 0 13 5 3.90 0.20 0 13 6 2.14 0.20 0 13 7 14.19 0.24 0 13 8 11.16 0.25 0 13 9 0.43 0.10 0 13 10 5.53 0.22 0 13 11 25.85 0.31 0 13 12 0.21 0.10 0 13 13 1.95 0.33 0 14 0 360.91 4.31 0 14 1 35.55 0.28 0 14 2 79.06 0.58 0 14 3 9.82 0.20 0 14 4 1.27 0.28 0 14 5 6.32 0.20 0 14 6 45.79 0.48 0 14 7 14.25 0.27 0 14 8 89.28 0.77 0 14 9 41.77 0.43 0 14 10 13.66 0.27 0 14 11 29.82 0.39 0 14 12 11.45 0.28 0 14 13 0.12 0.11 0 14 14 52.77 0.95 0 15 0 3.52 0.27 0 15 1 51.21 0.40 0 15 2 18.72 0.23 0 15 3 18.93 0.29 0 15 4 19.74 0.31 0 15 5 6.08 0.24 0 15 6 13.74 0.25 0 15 7 2.54 0.62 0 15 8 0.26 0.11 0 15 9 2.85 0.26 0 15 10 4.72 0.26 0 15 11 37.79 0.50 0 15 12 3.22 0.31 0 15 13 27.81 0.45 0 15 14 11.60 0.40 0 15 15 4.40 0.63 0 16 0 237.10 2.82 0 16 1 25.29 0.27 0 16 2 70.10 0.58 0 16 3 9.52 0.24 0 16 4 18.74 0.32 0 16 5 7.28 0.27 0 16 6 12.97 0.32 0 16 7 11.49 0.27 0 16 8 54.09 0.51 0 16 9 4.55 0.28 0 16 10 38.61 0.52 0 16 11 0.79 0.12 0 16 12 22.66 0.44 0 16 13 0.08 0.12 0 16 14 52.75 0.70 0 16 15 4.72 0.52 0 16 16 42.94 2.26 0 17 0 0.40 0.24 0 17 1 18.27 0.29 0 17 2 2.28 0.22 0 17 3 5.74 0.23 0 17 4 11.44 0.29 0 17 5 12.21 0.31 0 17 6 1.50 0.30 0 17 7 9.92 0.29 0 17 8 2.16 0.49 0 17 9 7.94 0.33 0 17 10 4.88 0.34 0 17 11 1.98 0.51 0 17 12 0.25 0.12 0 17 13 3.73 0.41 0 17 14 5.60 0.59 0 17 15 2.99 0.58 0 18 0 21.04 0.82 0 18 1 5.22 0.29 0 18 2 6.66 0.30 0 18 3 0.42 0.10 0 18 4 1.66 0.25 0 18 5 0.84 0.08 0 18 6 13.66 0.33 0 18 7 2.90 0.27 0 18 8 27.75 0.45 0 18 9 0.80 0.12 0 18 10 6.29 0.32 0 18 11 0.01 0.11 0 18 12 0.02 0.13 0 18 13 0.00 0.13 0 18 14 5.14 0.54 0 19 0 12.43 0.72 0 19 1 3.56 0.30 0 19 2 3.48 0.31 0 19 3 4.81 0.30 0 19 4 2.95 0.48 0 19 5 16.82 0.42 0 19 6 2.20 0.45 0 19 7 32.18 0.57 0 19 8 5.21 0.38 0 19 9 6.48 0.33 0 19 10 0.03 0.12 0 19 11 0.32 0.26 0 19 12 0.10 0.12 0 19 13 0.46 0.13 0 20 0 0.32 0.28 0 20 1 0.07 0.13 0 20 2 0.01 0.12 0 20 3 0.45 0.13 0 20 4 7.77 0.37 0 20 5 0.00 0.13 0 20 6 18.58 0.50 0 20 7 2.87 0.53 0 20 8 34.07 0.83 0 20 9 8.16 0.77 0 20 10 0.43 0.14 0 20 11 16.61 0.72 0 21 0 9.55 1.61 0 21 1 0.82 0.60 0 21 2 3.96 0.33 0 21 3 17.47 0.44 0 21 4 0.07 0.13 0 21 5 9.04 0.46 0 21 6 2.89 0.54 0 21 7 7.33 0.84 0 21 8 1.07 1.22 0 21 9 4.71 1.03 0 22 0 81.41 3.19 0 22 1 3.72 0.64 0 22 2 9.98 0.62 0 22 3 1.83 0.78 0 22 4 11.64 0.85 0 22 5 1.95 0.65 0 22 6 38.49 0.91 0 22 7 3.13 0.74 0 23 0 5.44 0.94 0 23 1 9.69 0.71 0 23 2 6.43 0.76 0 23 3 4.61 0.72 1 1 1 1641.92 8.84 1 2 1 0.45 0.04 1 2 2 78.35 0.24 1 3 1 7.91 0.04 1 3 2 2.12 0.04 1 3 3 38.87 0.09 1 4 1 154.72 1.44 1 4 2 20.44 0.16 1 4 3 0.91 0.04 1 4 4 104.94 0.51 1 5 1 8.18 0.06 1 5 2 1.16 0.02 1 5 3 13.44 0.07 1 5 4 0.94 0.06 1 5 5 35.27 0.12 1 6 1 1.51 0.03 1 6 2 0.14 0.06 1 6 3 0.31 0.02 1 6 4 26.44 0.14 1 6 5 0.00 0.08 1 6 6 117.70 0.60 1 7 1 267.01 1.00 1 7 2 0.15 0.02 1 7 3 54.93 0.27 1 7 4 0.92 0.07 1 7 5 117.59 0.41 1 7 6 0.87 0.06 1 7 7 146.08 0.62 1 8 1 88.66 0.64 1 8 2 0.19 0.03 1 8 3 134.25 0.40 1 8 4 38.27 0.19 1 8 5 23.69 0.12 1 8 6 39.06 0.19 1 8 7 15.73 0.11 1 8 8 11.44 0.16 1 9 1 97.15 0.41 1 9 2 3.72 0.08 1 9 3 44.91 0.17 1 9 4 2.39 0.07 1 9 5 65.31 0.30 1 9 6 6.27 0.08 1 9 7 76.71 0.31 1 9 8 12.00 0.13 1 9 9 40.25 0.36 1 10 1 4.76 0.11 1 10 2 39.31 0.21 1 10 3 8.55 0.09 1 10 4 21.48 0.16 1 10 5 0.21 0.07 1 10 6 6.15 0.10 1 10 7 4.18 0.10 1 10 8 17.15 0.15 1 10 9 0.21 0.06 1 10 10 21.33 0.27 1 11 1 23.77 0.21 1 11 2 0.27 0.03 1 11 3 14.25 0.12 1 11 4 12.32 0.11 1 11 5 5.80 0.11 1 11 6 2.01 0.14 1 11 7 31.11 0.23 1 11 8 25.34 0.18 1 11 9 36.30 0.23 1 11 10 1.54 0.19 1 11 11 25.10 0.35 1 12 1 4.81 0.13 1 12 2 11.29 0.11 1 12 3 39.81 0.20 1 12 4 10.41 0.13 1 12 5 4.16 0.12 1 12 6 2.41 0.12 1 12 7 0.44 0.23 1 12 8 30.91 0.24 1 12 9 3.94 0.15 1 12 10 2.01 0.15 1 12 11 2.91 0.15 1 12 12 0.03 0.10 1 13 1 91.40 0.54 1 13 2 0.03 0.04 1 13 3 17.66 0.14 1 13 4 31.15 0.21 1 13 5 0.55 0.12 1 13 6 1.86 0.19 1 13 7 79.03 0.44 1 13 8 30.40 0.25 1 13 9 17.34 0.20 1 13 10 0.91 0.09 1 13 11 2.62 0.17 1 13 12 9.23 0.19 1 13 13 0.78 0.11 1 14 1 1.43 0.15 1 14 2 22.78 0.17 1 14 3 2.97 0.11 1 14 4 5.00 0.13 1 14 5 7.00 0.14 1 14 6 4.60 0.15 1 14 7 6.74 0.18 1 14 8 0.00 0.08 1 14 9 0.00 0.07 1 14 10 11.25 0.19 1 14 11 1.12 0.08 1 14 12 17.17 0.22 1 14 13 3.01 0.24 1 14 14 6.53 0.31 1 15 1 151.91 0.86 1 15 2 0.15 0.05 1 15 3 14.87 0.17 1 15 4 16.21 0.20 1 15 5 7.53 0.17 1 15 6 0.11 0.06 1 15 7 48.74 0.34 1 15 8 41.74 0.31 1 15 9 41.81 0.32 1 15 10 0.91 0.35 1 15 11 9.13 0.22 1 15 12 7.94 0.22 1 15 13 30.77 0.35 1 15 14 1.19 0.09 1 15 15 51.75 0.70 1 16 1 4.86 0.17 1 16 2 7.45 0.14 1 16 3 20.08 0.20 1 16 4 6.85 0.18 1 16 5 3.35 0.16 1 16 6 4.27 0.16 1 16 7 0.07 0.07 1 16 8 2.67 0.21 1 16 9 5.30 0.19 1 16 10 6.06 0.21 1 16 11 3.57 0.21 1 16 12 8.65 0.24 1 16 13 5.42 0.24 1 16 14 3.81 0.33 1 16 15 10.39 0.38 1 16 16 2.30 0.19 1 17 1 52.99 0.54 1 17 2 1.00 0.07 1 17 3 5.21 0.16 1 17 4 7.02 0.19 1 17 5 1.42 0.09 1 17 6 0.39 0.06 1 17 7 19.21 0.24 1 17 8 4.09 0.20 1 17 9 23.85 0.39 1 17 10 0.03 0.08 1 17 11 2.80 0.27 1 17 12 0.04 0.08 1 17 13 5.84 0.28 1 17 14 0.40 0.09 1 17 15 21.49 0.55 1 18 1 1.08 0.33 1 18 2 1.68 0.22 1 18 3 0.01 0.06 1 18 4 0.89 0.24 1 18 5 1.20 0.18 1 18 6 16.84 0.24 1 18 7 2.60 0.21 1 18 8 8.99 0.24 1 18 9 0.01 0.08 1 18 10 0.97 0.18 1 18 11 0.06 0.08 1 18 12 0.00 0.08 1 18 13 0.07 0.09 1 18 14 1.27 0.12 1 19 1 0.17 0.12 1 19 2 0.02 0.09 1 19 3 0.24 0.11 1 19 4 0.00 0.08 1 19 5 0.62 0.11 1 19 6 0.02 0.07 1 19 7 14.40 0.27 1 19 8 9.06 0.27 1 19 9 4.51 0.27 1 19 10 0.75 0.08 1 19 11 4.18 0.27 1 19 12 1.62 0.28 1 19 13 0.53 0.09 1 20 1 5.93 0.33 1 20 2 4.00 0.22 1 20 3 7.19 0.23 1 20 4 7.29 0.26 1 20 5 0.02 0.09 1 20 6 4.80 0.28 1 20 7 0.00 0.10 1 20 8 5.38 0.32 1 20 9 4.74 0.40 1 20 10 2.98 0.38 1 20 11 0.03 0.09 1 21 1 3.34 0.35 1 21 2 0.18 0.10 1 21 3 1.97 0.47 1 21 4 0.08 0.10 1 21 5 12.92 0.33 1 21 6 2.02 0.54 1 21 7 26.87 0.43 1 21 8 4.84 0.56 1 21 9 5.84 0.59 1 22 1 3.77 0.58 1 22 2 2.90 0.34 1 22 3 1.04 0.19 1 22 4 4.94 0.34 1 22 5 0.65 0.51 1 22 6 5.84 0.42 1 22 7 0.75 0.77 1 23 1 39.96 1.17 1 23 2 0.17 0.23 1 23 3 3.24 0.49 2 2 2 398.28 1.67 2 3 2 334.97 1.19 2 3 3 14.56 0.39 2 4 2 101.78 0.61 2 4 3 0.70 0.07 2 4 4 12.27 0.11 2 5 2 24.75 0.41 2 5 3 8.37 0.13 2 5 4 17.53 0.10 2 5 5 16.58 0.17 2 6 2 21.24 0.10 2 6 3 5.15 0.05 2 6 4 28.49 0.16 2 6 5 1.10 0.06 2 6 6 1.90 0.09 2 7 2 124.49 0.80 2 7 3 12.70 0.07 2 7 4 9.74 0.11 2 7 5 0.99 0.07 2 7 6 3.27 0.08 2 7 7 0.09 0.03 2 8 2 28.44 0.24 2 8 3 8.62 0.07 2 8 4 31.49 0.14 2 8 5 0.13 0.03 2 8 6 24.79 0.19 2 8 7 12.35 0.10 2 8 8 35.59 0.28 2 9 2 5.54 0.10 2 9 3 0.20 0.06 2 9 4 17.90 0.14 2 9 5 0.00 0.08 2 9 6 1.19 0.10 2 9 7 0.81 0.12 2 9 8 0.00 0.03 2 9 9 0.03 0.06 2 10 2 21.98 0.16 2 10 3 32.70 0.15 2 10 4 24.97 0.14 2 10 5 6.65 0.10 2 10 6 0.61 0.11 2 10 7 24.76 0.22 2 10 8 23.53 0.18 2 10 9 11.10 0.15 2 10 10 14.38 0.24 2 11 2 34.23 0.24 2 11 3 1.78 0.12 2 11 4 13.31 0.13 2 11 5 0.31 0.04 2 11 6 10.24 0.13 2 11 7 0.03 0.04 2 11 8 1.54 0.23 2 11 9 0.48 0.06 2 11 10 31.73 0.25 2 11 11 24.08 0.33 2 12 2 11.10 0.14 2 12 3 5.56 0.10 2 12 4 53.26 0.28 2 12 5 16.59 0.17 2 12 6 7.10 0.13 2 12 7 6.02 0.14 2 12 8 11.09 0.16 2 12 9 20.67 0.19 2 12 10 3.85 0.15 2 12 11 16.98 0.20 2 12 12 49.82 0.49 2 13 2 2.03 0.17 2 13 3 0.01 0.04 2 13 4 0.01 0.04 2 13 5 0.49 0.20 2 13 6 2.35 0.13 2 13 7 0.10 0.08 2 13 8 3.51 0.16 2 13 9 0.67 0.20 2 13 10 1.39 0.16 2 13 11 3.10 0.16 2 13 12 0.85 0.08 2 13 13 1.40 0.49 2 14 2 0.00 0.11 2 14 3 29.65 0.19 2 14 4 5.55 0.13 2 14 5 7.57 0.15 2 14 6 8.52 0.16 2 14 7 25.32 0.24 2 14 8 26.80 0.25 2 14 9 2.43 0.31 2 14 10 0.48 0.07 2 14 11 4.77 0.18 2 14 12 0.46 0.08 2 14 13 2.07 0.15 2 14 14 7.03 0.33 2 15 2 10.88 0.21 2 15 3 0.01 0.05 2 15 4 10.64 0.16 2 15 5 1.41 0.21 2 15 6 0.02 0.06 2 15 7 0.24 0.11 2 15 8 3.09 0.32 2 15 9 0.06 0.07 2 15 10 4.32 0.17 2 15 11 0.13 0.08 2 15 12 8.91 0.22 2 15 13 0.00 0.08 2 15 14 8.25 0.26 2 15 15 0.08 0.13 2 16 2 5.12 0.20 2 16 3 7.61 0.14 2 16 4 0.09 0.05 2 16 5 0.41 0.06 2 16 6 6.47 0.17 2 16 7 10.29 0.19 2 16 8 35.22 0.31 2 16 9 3.87 0.19 2 16 10 0.97 0.09 2 16 11 8.75 0.22 2 16 12 0.15 0.08 2 16 13 0.06 0.08 2 16 14 10.35 0.30 2 16 15 2.07 0.30 2 16 16 21.35 0.73 2 17 2 0.66 0.09 2 17 3 0.38 0.05 2 17 4 0.13 0.06 2 17 5 0.03 0.06 2 17 6 0.12 0.08 2 17 7 2.88 0.19 2 17 8 0.51 0.14 2 17 9 0.08 0.08 2 17 10 0.23 0.08 2 17 11 0.08 0.08 2 17 12 0.54 0.08 2 17 13 0.07 0.08 2 17 14 0.37 0.09 2 17 15 1.24 0.55 2 18 2 1.53 0.14 2 18 3 0.28 0.07 2 18 4 10.59 0.21 2 18 5 0.62 0.07 2 18 6 0.00 0.07 2 18 7 3.16 0.20 2 18 8 6.83 0.24 2 18 9 2.96 0.33 2 18 10 2.55 0.32 2 18 11 2.89 0.32 2 18 12 4.84 0.28 2 18 13 0.08 0.09 2 18 14 0.11 0.09 2 19 2 10.92 0.35 2 19 3 0.15 0.09 2 19 4 3.97 0.22 2 19 5 0.57 0.13 2 19 6 0.05 0.23 2 19 7 0.71 0.27 2 19 8 2.92 0.47 2 19 9 1.37 0.42 2 19 10 3.56 0.29 2 19 11 0.01 0.08 2 19 12 3.60 0.32 2 19 13 0.01 0.09 2 20 2 3.24 0.31 2 20 3 1.36 0.33 2 20 4 5.32 0.25 2 20 5 0.59 0.09 2 20 6 0.01 0.10 2 20 7 3.65 0.47 2 20 8 0.10 0.10 2 20 9 0.04 0.10 2 20 10 0.01 0.10 2 20 11 0.00 0.09 2 21 2 0.13 0.14 2 21 3 0.06 0.09 2 21 4 0.51 0.10 2 21 5 0.09 0.09 2 21 6 0.12 0.11 2 21 7 0.07 0.20 2 21 8 1.06 0.56 2 21 9 0.05 0.12 2 22 2 6.83 0.34 2 22 3 0.43 0.10 2 22 4 0.27 0.24 2 22 5 0.72 0.41 2 22 6 4.11 0.63 2 22 7 5.02 0.50 2 23 2 4.50 0.50 3 3 3 657.87 6.93 3 4 3 220.46 1.86 3 4 4 41.53 0.82 3 5 3 196.04 0.53 3 5 4 0.23 0.07 3 5 5 166.62 1.06 3 6 3 0.03 0.03 3 6 4 35.14 0.14 3 6 5 4.84 0.07 3 6 6 73.83 0.37 3 7 3 0.16 0.06 3 7 4 0.01 0.07 3 7 5 0.49 0.08 3 7 6 17.26 0.12 3 7 7 0.36 0.13 3 8 3 27.86 0.19 3 8 4 12.02 0.10 3 8 5 38.32 0.19 3 8 6 22.02 0.15 3 8 7 1.33 0.11 3 8 8 3.25 0.18 3 9 3 55.02 0.42 3 9 4 44.71 0.23 3 9 5 17.12 0.14 3 9 6 0.01 0.03 3 9 7 8.57 0.12 3 9 8 39.00 0.24 3 9 9 2.38 0.18 3 10 3 2.53 0.12 3 10 4 2.91 0.09 3 10 5 1.55 0.13 3 10 6 7.83 0.11 3 10 7 0.01 0.08 3 10 8 18.99 0.19 3 10 9 4.26 0.12 3 10 10 16.24 0.24 3 11 3 85.07 0.71 3 11 4 24.54 0.19 3 11 5 62.58 0.35 3 11 6 0.20 0.04 3 11 7 0.36 0.05 3 11 8 35.30 0.25 3 11 9 25.85 0.23 3 11 10 0.00 0.07 3 11 11 26.73 0.35 3 12 3 4.15 0.15 3 12 4 8.73 0.13 3 12 5 2.05 0.13 3 12 6 3.97 0.12 3 12 7 0.63 0.13 3 12 8 24.57 0.22 3 12 9 9.86 0.17 3 12 10 0.00 0.06 3 12 11 12.02 0.21 3 12 12 0.85 0.11 3 13 3 17.14 0.23 3 13 4 10.99 0.16 3 13 5 19.86 0.20 3 13 6 1.77 0.20 3 13 7 0.52 0.14 3 13 8 27.00 0.24 3 13 9 5.38 0.16 3 13 10 0.70 0.07 3 13 11 38.05 0.33 3 13 12 7.28 0.20 3 13 13 19.14 0.39 3 14 3 11.10 0.19 3 14 4 0.52 0.07 3 14 5 2.64 0.14 3 14 6 3.46 0.15 3 14 7 0.13 0.07 3 14 8 0.31 0.22 3 14 9 7.18 0.18 3 14 10 12.37 0.20 3 14 11 8.51 0.19 3 14 12 12.23 0.24 3 14 13 0.26 0.08 3 14 14 0.34 0.29 3 15 3 9.66 0.21 3 15 4 16.69 0.18 3 15 5 0.08 0.05 3 15 6 14.21 0.19 3 15 7 33.23 0.28 3 15 8 5.07 0.18 3 15 9 5.66 0.19 3 15 10 0.42 0.07 3 15 11 1.10 0.16 3 15 12 1.14 0.14 3 15 13 0.33 0.08 3 15 14 0.21 0.09 3 15 15 5.74 0.44 3 16 3 6.10 0.20 3 16 4 6.79 0.15 3 16 5 0.62 0.13 3 16 6 0.00 0.06 3 16 7 6.63 0.18 3 16 8 1.24 0.16 3 16 9 3.61 0.20 3 16 10 2.11 0.22 3 16 11 9.55 0.24 3 16 12 8.74 0.23 3 16 13 6.41 0.25 3 16 14 2.25 0.40 3 16 15 2.11 0.50 3 16 16 0.01 0.13 3 17 3 12.27 0.30 3 17 4 0.42 0.18 3 17 5 6.37 0.19 3 17 6 0.02 0.06 3 17 7 15.72 0.24 3 17 8 16.64 0.25 3 17 9 0.00 0.08 3 17 10 3.94 0.22 3 17 11 12.49 0.26 3 17 12 3.67 0.29 3 17 13 0.16 0.08 3 17 14 1.32 0.20 3 17 15 1.89 0.50 3 18 3 10.58 0.30 3 18 4 3.70 0.20 3 18 5 0.00 0.06 3 18 6 14.53 0.24 3 18 7 2.00 0.48 3 18 8 2.23 0.36 3 18 9 5.99 0.24 3 18 10 0.26 0.08 3 18 11 1.11 0.08 3 18 12 1.00 0.23 3 18 13 0.94 0.09 3 18 14 0.10 0.09 3 19 3 33.10 0.48 3 19 4 7.11 0.24 3 19 5 24.44 0.37 3 19 6 1.89 0.38 3 19 7 7.44 0.28 3 19 8 0.25 0.08 3 19 9 5.71 0.32 3 19 10 0.02 0.08 3 19 11 7.60 0.33 3 19 12 0.05 0.09 3 19 13 8.32 0.47 3 20 3 0.10 0.13 3 20 4 5.59 0.26 3 20 5 0.39 0.09 3 20 6 7.22 0.29 3 20 7 4.85 0.61 3 20 8 3.59 0.65 3 20 9 0.02 0.10 3 20 10 0.92 0.57 3 20 11 2.02 0.57 3 21 3 4.43 0.45 3 21 4 4.32 0.32 3 21 5 9.47 0.35 3 21 6 0.18 0.10 3 21 7 0.90 0.60 3 21 8 6.42 0.52 3 21 9 0.24 0.59 3 22 3 6.42 0.66 3 22 4 3.50 0.51 3 22 5 2.58 0.50 3 22 6 0.54 0.19 4 4 4 646.30 4.57 4 5 4 35.17 0.12 4 5 5 82.99 0.37 4 6 4 4.13 0.11 4 6 5 8.19 0.10 4 6 6 43.15 0.26 4 7 4 70.92 0.35 4 7 5 90.28 0.42 4 7 6 15.76 0.13 4 7 7 59.08 0.53 4 8 4 18.76 0.15 4 8 5 19.37 0.12 4 8 6 0.03 0.04 4 8 7 29.84 0.21 4 8 8 78.07 0.57 4 9 4 1.23 0.12 4 9 5 7.78 0.11 4 9 6 14.10 0.16 4 9 7 12.21 0.15 4 9 8 10.66 0.14 4 9 9 20.89 0.27 4 10 4 93.20 0.57 4 10 5 12.93 0.14 4 10 6 10.12 0.15 4 10 7 10.86 0.15 4 10 8 0.02 0.05 4 10 9 13.71 0.16 4 10 10 27.47 0.30 4 11 4 2.66 0.16 4 11 5 7.75 0.13 4 11 6 7.96 0.15 4 11 7 7.68 0.16 4 11 8 16.84 0.18 4 11 9 23.55 0.22 4 11 10 9.24 0.17 4 11 11 0.42 0.11 4 12 4 52.11 0.47 4 12 5 0.62 0.05 4 12 6 7.80 0.15 4 12 7 13.39 0.19 4 12 8 6.07 0.17 4 12 9 5.49 0.16 4 12 10 28.22 0.24 4 12 11 8.91 0.18 4 12 12 47.67 0.55 4 13 4 0.29 0.07 4 13 5 2.41 0.15 4 13 6 1.68 0.27 4 13 7 5.81 0.17 4 13 8 0.82 0.10 4 13 9 4.36 0.15 4 13 10 0.10 0.06 4 13 11 4.91 0.18 4 13 12 0.86 0.08 4 13 13 16.06 0.39 4 14 4 0.11 0.08 4 14 5 0.77 0.10 4 14 6 3.22 0.20 4 14 7 1.08 0.25 4 14 8 31.44 0.27 4 14 9 7.49 0.18 4 14 10 0.30 0.06 4 14 11 3.50 0.18 4 14 12 15.69 0.26 4 14 13 0.50 0.08 4 14 14 0.22 0.12 4 15 4 11.93 0.26 4 15 5 1.90 0.23 4 15 6 0.39 0.06 4 15 7 2.85 0.19 4 15 8 8.05 0.20 4 15 9 2.73 0.18 4 15 10 14.12 0.22 4 15 11 16.25 0.27 4 15 12 7.35 0.22 4 15 13 9.95 0.25 4 15 14 0.55 0.09 4 15 15 0.23 0.13 4 16 4 15.28 0.26 4 16 5 0.47 0.06 4 16 6 23.15 0.26 4 16 7 11.39 0.22 4 16 8 11.98 0.22 4 16 9 0.05 0.07 4 16 10 0.16 0.07 4 16 11 2.57 0.23 4 16 12 2.32 0.25 4 16 13 0.01 0.08 4 16 14 0.66 0.10 4 16 15 3.29 0.47 4 16 16 0.92 0.37 4 17 4 0.88 0.08 4 17 5 11.34 0.20 4 17 6 34.78 0.31 4 17 7 16.64 0.25 4 17 8 0.02 0.07 4 17 9 0.02 0.08 4 17 10 0.08 0.07 4 17 11 4.87 0.23 4 17 12 2.10 0.39 4 17 13 0.23 0.09 4 17 14 0.15 0.16 4 17 15 3.45 0.43 4 18 4 28.87 0.50 4 18 5 0.85 0.08 4 18 6 3.39 0.20 4 18 7 6.58 0.23 4 18 8 0.97 0.30 4 18 9 1.10 0.30 4 18 10 11.69 0.26 4 18 11 2.46 0.27 4 18 12 7.99 0.38 4 18 13 1.45 0.22 4 18 14 1.21 0.59 4 19 4 0.10 0.10 4 19 5 9.70 0.25 4 19 6 10.04 0.28 4 19 7 9.46 0.31 4 19 8 0.16 0.09 4 19 9 6.43 0.31 4 19 10 4.25 0.31 4 19 11 0.57 0.12 4 19 12 1.06 0.16 4 20 4 37.71 0.66 4 20 5 3.13 0.29 4 20 6 27.61 0.40 4 20 7 3.97 0.43 4 20 8 0.40 0.09 4 20 9 0.64 0.11 4 20 10 8.98 0.35 4 20 11 0.79 0.10 4 21 4 0.59 0.14 4 21 5 5.87 0.41 4 21 6 0.40 0.25 4 21 7 3.35 0.56 4 21 8 0.00 0.11 4 21 9 2.89 0.74 4 22 4 4.84 0.63 4 22 5 1.78 0.57 4 22 6 0.04 0.11 5 5 5 11.55 0.18 5 6 5 64.74 0.25 5 6 6 143.51 0.87 5 7 5 5.22 0.17 5 7 6 0.86 0.09 5 7 7 52.88 0.33 5 8 5 51.96 0.40 5 8 6 14.08 0.15 5 8 7 89.97 0.47 5 8 8 5.22 0.17 5 9 5 13.64 0.21 5 9 6 5.42 0.13 5 9 7 45.49 0.25 5 9 8 20.93 0.17 5 9 9 28.40 0.35 5 10 5 1.56 0.17 5 10 6 0.20 0.05 5 10 7 3.27 0.14 5 10 8 0.49 0.05 5 10 9 0.00 0.04 5 10 10 3.74 0.21 5 11 5 22.54 0.28 5 11 6 6.54 0.14 5 11 7 5.13 0.15 5 11 8 16.69 0.19 5 11 9 6.03 0.16 5 11 10 1.57 0.19 5 11 11 47.88 0.52 5 12 5 19.01 0.30 5 12 6 0.72 0.06 5 12 7 30.53 0.24 5 12 8 0.29 0.06 5 12 9 4.21 0.16 5 12 10 3.39 0.17 5 12 11 5.18 0.17 5 12 12 0.53 0.11 5 13 5 3.23 0.21 5 13 6 2.47 0.18 5 13 7 1.08 0.14 5 13 8 1.20 0.11 5 13 9 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17 0.44 0.00 2 5 17 -1.02 0.00 3 5 17 1.10 0.00 4 5 17 3.24 0.00 5 5 17 3.89 0.00 0 6 17 6.85 0.00 1 6 17 3.56 0.00 2 6 17 0.24 0.00 3 6 17 3.57 0.00 4 6 17 2.42 0.00 5 6 17 2.62 0.00 6 6 17 3.04 0.00 0 7 17 4.14 0.00 1 7 17 0.82 0.00 2 7 17 0.21 0.00 3 7 17 0.91 0.00 4 7 17 1.28 0.00 5 7 17 1.85 0.00 6 7 17 1.34 0.00 7 7 17 1.44 0.00 0 8 17 2.87 0.00 1 8 17 0.24 0.00 2 8 17 -2.23 0.00 3 8 17 0.77 0.00 4 8 17 0.54 0.00 5 8 17 2.17 0.00 6 8 17 2.44 0.00 7 8 17 1.29 0.00 8 8 17 0.56 0.00 0 9 17 4.86 0.00 1 9 17 0.93 0.00 2 9 17 -1.78 0.00 3 9 17 0.87 0.00 4 9 17 1.96 0.00 5 9 17 1.12 0.00 6 9 17 1.17 0.00 7 9 17 0.55 0.00 8 9 17 0.59 0.00 9 9 17 -0.13 0.00 0 10 17 5.12 0.00 1 10 17 1.17 0.00 2 10 17 -1.05 0.00 3 10 17 0.94 0.00 4 10 17 0.74 0.00 5 10 17 0.23 0.00 6 10 17 0.00 0.00 7 10 17 -0.62 0.00 8 10 17 0.63 0.00 9 10 17 -0.76 0.00 10 10 17 -0.89 0.00 0 11 17 4.97 0.00 1 11 17 -0.43 0.00 2 11 17 -3.09 0.00 3 11 17 1.62 0.00 4 11 17 0.25 0.00 5 11 17 -0.90 0.00 6 11 17 -0.03 0.00 7 11 17 -0.68 0.00 8 11 17 -0.92 0.00 9 11 17 1.02 0.00 10 11 17 -1.13 0.00 11 11 17 -0.48 0.00 0 12 17 2.48 0.00 1 12 17 -1.58 0.00 2 12 17 -3.97 0.00 3 12 17 -0.12 0.00 4 12 17 -0.19 0.00 5 12 17 -1.06 0.00 6 12 17 -0.41 0.00 7 12 17 -0.63 0.00 8 12 17 -0.09 0.00 9 12 17 -1.04 0.00 10 12 17 -0.78 0.00 0 13 17 3.97 0.00 1 13 17 -0.37 0.00 2 13 17 -2.46 0.00 3 13 17 0.06 0.00 4 13 17 0.25 0.00 5 13 17 -0.51 0.00 6 13 17 1.68 0.00 7 13 17 0.04 0.00 8 13 17 1.57 0.00 9 13 17 1.76 0.00 0 14 17 3.97 0.00 1 14 17 0.65 0.00 2 14 17 -0.93 0.00 3 14 17 2.05 0.00 4 14 17 0.35 0.00 5 14 17 1.18 0.00 6 14 17 2.79 0.00 7 14 17 0.77 0.00 0 15 17 3.79 0.00 1 15 17 -0.61 0.00 2 15 17 -1.44 0.00 3 15 17 2.39 0.00 4 15 17 -0.50 0.00 5 15 17 -1.40 0.00 0 0 18 2.60 0.00 0 1 18 -0.39 0.00 1 1 18 -2.07 0.00 0 2 18 -0.15 0.00 1 2 18 -3.44 0.00 2 2 18 -3.70 0.00 0 3 18 1.69 0.00 1 3 18 -0.10 0.00 2 3 18 -1.35 0.00 3 3 18 1.94 0.00 0 4 18 -0.08 0.00 1 4 18 -1.86 0.00 2 4 18 -2.31 0.00 3 4 18 0.17 0.00 4 4 18 0.50 0.00 0 5 18 1.31 0.00 1 5 18 -0.84 0.00 2 5 18 -1.96 0.00 3 5 18 1.03 0.00 4 5 18 1.18 0.00 5 5 18 -0.29 0.00 0 6 18 2.87 0.00 1 6 18 0.24 0.00 2 6 18 0.40 0.00 3 6 18 0.91 0.00 4 6 18 1.28 0.00 5 6 18 -0.82 0.00 6 6 18 0.76 0.00 0 7 18 2.06 0.00 1 7 18 -0.77 0.00 2 7 18 -0.79 0.00 3 7 18 1.58 0.00 4 7 18 0.62 0.00 5 7 18 0.61 0.00 6 7 18 1.61 0.00 7 7 18 1.39 0.00 0 8 18 0.33 0.00 1 8 18 -1.54 0.00 2 8 18 -2.24 0.00 3 8 18 0.79 0.00 4 8 18 0.62 0.00 5 8 18 0.22 0.00 6 8 18 1.21 0.00 7 8 18 0.35 0.00 8 8 18 -0.03 0.00 0 9 18 2.04 0.00 1 9 18 -0.52 0.00 2 9 18 -1.21 0.00 3 9 18 0.27 0.00 4 9 18 -0.28 0.00 5 9 18 -0.99 0.00 6 9 18 0.75 0.00 7 9 18 0.11 0.00 8 9 18 -0.68 0.00 9 9 18 0.05 0.00 0 10 18 3.35 0.00 1 10 18 -0.72 0.00 2 10 18 -1.16 0.00 3 10 18 0.30 0.00 4 10 18 1.00 0.00 5 10 18 -0.59 0.00 6 10 18 0.36 0.00 7 10 18 -0.75 0.00 8 10 18 -0.84 0.00 9 10 18 -0.41 0.00 10 10 18 0.39 0.00 0 11 18 0.77 0.00 1 11 18 -1.66 0.00 2 11 18 -3.24 0.00 3 11 18 -0.09 0.00 4 11 18 -0.12 0.00 5 11 18 -2.00 0.00 6 11 18 -1.12 0.00 7 11 18 -1.39 0.00 8 11 18 -1.50 0.00 9 11 18 -0.39 0.00 0 12 18 0.38 0.00 1 12 18 -2.61 0.00 2 12 18 -3.88 0.00 3 12 18 -1.40 0.00 4 12 18 -0.96 0.00 5 12 18 -1.51 0.00 6 12 18 -0.61 0.00 7 12 18 -1.03 0.00 8 12 18 -0.86 0.00 0 13 18 1.67 0.00 1 13 18 -2.13 0.00 2 13 18 -2.86 0.00 3 13 18 0.28 0.00 4 13 18 0.69 0.00 5 13 18 0.30 0.00 6 13 18 3.01 0.00 0 14 18 3.58 0.00 1 14 18 -0.97 0.00 2 14 18 -2.97 0.00 3 14 18 1.18 0.00 4 14 18 0.61 0.00 0 0 19 2.78 0.00 0 1 19 3.06 0.00 1 1 19 0.04 0.00 0 2 19 0.09 0.00 1 2 19 1.36 0.00 2 2 19 0.62 0.00 0 3 19 4.19 0.00 1 3 19 1.50 0.00 2 3 19 2.70 0.00 3 3 19 5.35 0.00 0 4 19 1.50 0.00 1 4 19 0.22 0.00 2 4 19 0.75 0.00 3 4 19 2.27 0.00 4 4 19 1.54 0.00 0 5 19 0.59 0.00 1 5 19 -1.16 0.00 2 5 19 -1.68 0.00 3 5 19 0.77 0.00 4 5 19 -0.62 0.00 5 5 19 -2.91 0.00 0 6 19 1.12 0.00 1 6 19 0.02 0.00 2 6 19 0.92 0.00 3 6 19 1.79 0.00 4 6 19 0.42 0.00 5 6 19 -1.58 0.00 6 6 19 -1.09 0.00 0 7 19 -0.64 0.00 1 7 19 -0.35 0.00 2 7 19 0.20 0.00 3 7 19 2.24 0.00 4 7 19 -0.20 0.00 5 7 19 -1.11 0.00 6 7 19 0.43 0.00 7 7 19 1.71 0.00 0 8 19 0.10 0.00 1 8 19 -0.28 0.00 2 8 19 -0.65 0.00 3 8 19 2.11 0.00 4 8 19 1.15 0.00 5 8 19 -0.21 0.00 6 8 19 1.02 0.00 7 8 19 1.43 0.00 8 8 19 0.88 0.00 0 9 19 2.64 0.00 1 9 19 1.75 0.00 2 9 19 1.84 0.00 3 9 19 3.69 0.00 4 9 19 1.39 0.00 5 9 19 1.14 0.00 6 9 19 2.01 0.00 7 9 19 1.66 0.00 8 9 19 0.85 0.00 9 9 19 1.66 0.00 0 10 19 3.43 0.00 1 10 19 1.47 0.00 2 10 19 0.40 0.00 3 10 19 3.37 0.00 4 10 19 0.45 0.00 5 10 19 -0.43 0.00 6 10 19 1.55 0.00 7 10 19 0.60 0.00 8 10 19 0.15 0.00 0 11 19 1.90 0.00 1 11 19 -0.25 0.00 2 11 19 -0.90 0.00 3 11 19 2.12 0.00 4 11 19 0.59 0.00 5 11 19 -0.32 0.00 6 11 19 0.67 0.00 7 11 19 1.08 0.00 0 12 19 1.73 0.00 1 12 19 -1.18 0.00 2 12 19 -0.59 0.00 3 12 19 1.71 0.00 4 12 19 1.38 0.00 5 12 19 0.41 0.00 0 13 19 4.39 0.00 1 13 19 0.09 0.00 2 13 19 -2.10 0.00 3 13 19 3.62 0.00 0 0 20 5.15 0.00 0 1 20 -0.14 0.00 1 1 20 -0.48 0.00 0 2 20 0.62 0.00 1 2 20 -1.90 0.00 2 2 20 0.07 0.00 0 3 20 0.36 0.00 1 3 20 -1.26 0.00 2 3 20 1.06 0.00 3 3 20 -0.40 0.00 0 4 20 -1.37 0.00 1 4 20 -1.76 0.00 2 4 20 -2.18 0.00 3 4 20 1.62 0.00 4 4 20 -1.10 0.00 0 5 20 -1.22 0.00 1 5 20 -2.38 0.00 2 5 20 -2.39 0.00 3 5 20 -0.90 0.00 4 5 20 -2.32 0.00 5 5 20 -2.94 0.00 0 6 20 -0.19 0.00 1 6 20 -0.94 0.00 2 6 20 -0.96 0.00 3 6 20 0.46 0.00 4 6 20 -1.56 0.00 5 6 20 -2.40 0.00 6 6 20 -2.10 0.00 0 7 20 -1.77 0.00 1 7 20 -3.19 0.00 2 7 20 -2.59 0.00 3 7 20 1.06 0.00 4 7 20 -1.06 0.00 5 7 20 -2.27 0.00 6 7 20 -1.36 0.00 7 7 20 -0.81 0.00 0 8 20 -1.76 0.00 1 8 20 -3.07 0.00 2 8 20 1.62 0.00 3 8 20 -0.16 0.00 4 8 20 -0.97 0.00 5 8 20 -1.98 0.00 6 8 20 0.44 0.00 7 8 20 -0.00 0.00 8 8 20 0.76 0.00 0 9 20 1.94 0.00 1 9 20 0.07 0.00 2 9 20 -1.17 0.00 3 9 20 1.92 0.00 4 9 20 -0.79 0.00 5 9 20 -1.16 0.00 6 9 20 0.97 0.00 7 9 20 0.04 0.00 0 10 20 1.27 0.00 1 10 20 -0.64 0.00 2 10 20 0.13 0.00 3 10 20 2.87 0.00 4 10 20 -1.11 0.00 5 10 20 -0.53 0.00 6 10 20 0.91 0.00 0 11 20 0.23 0.00 1 11 20 -1.70 0.00 2 11 20 -0.78 0.00 3 11 20 0.35 0.00 4 11 20 -0.43 0.00 0 0 21 4.63 0.00 0 1 21 3.06 0.00 1 1 21 1.70 0.00 0 2 21 0.57 0.00 1 2 21 -0.18 0.00 2 2 21 -2.31 0.00 0 3 21 -0.74 0.00 1 3 21 -0.63 0.00 2 3 21 -0.28 0.00 3 3 21 1.49 0.00 0 4 21 -1.57 0.00 1 4 21 -2.23 0.00 2 4 21 -2.70 0.00 3 4 21 -1.29 0.00 4 4 21 -1.78 0.00 0 5 21 2.28 0.00 1 5 21 0.37 0.00 2 5 21 -0.55 0.00 3 5 21 0.09 0.00 4 5 21 -0.23 0.00 5 5 21 -0.31 0.00 0 6 21 1.47 0.00 1 6 21 0.22 0.00 2 6 21 -0.14 0.00 3 6 21 0.63 0.00 4 6 21 -0.07 0.00 5 6 21 -0.39 0.00 6 6 21 -0.04 0.00 0 7 21 -0.93 0.00 1 7 21 -1.24 0.00 2 7 21 -0.95 0.00 3 7 21 0.89 0.00 4 7 21 -0.61 0.00 5 7 21 -1.79 0.00 6 7 21 -0.04 0.00 7 7 21 -0.66 0.00 0 8 21 -1.65 0.00 1 8 21 -2.83 0.00 2 8 21 -2.17 0.00 3 8 21 -0.88 0.00 4 8 21 -1.97 0.00 5 8 21 -2.20 0.00 0 9 21 -0.82 0.00 1 9 21 -1.86 0.00 2 9 21 0.37 0.00 3 9 21 -0.62 0.00 4 9 21 -1.13 0.00 0 0 22 6.96 0.00 0 1 22 4.14 0.00 1 1 22 3.76 0.00 0 2 22 1.68 0.00 1 2 22 2.05 0.00 2 2 22 2.52 0.00 0 3 22 -0.50 0.00 1 3 22 -0.24 0.00 2 3 22 0.98 0.00 3 3 22 -0.44 0.00 0 4 22 2.11 0.00 1 4 22 0.85 0.00 2 4 22 0.35 0.00 3 4 22 -0.81 0.00 4 4 22 1.14 0.00 0 5 22 3.18 0.00 1 5 22 1.84 0.00 2 5 22 0.92 0.00 3 5 22 0.11 0.00 4 5 22 1.34 0.00 5 5 22 -0.01 0.00 0 6 22 5.85 0.00 1 6 22 4.22 0.00 2 6 22 2.91 0.00 3 6 22 2.66 0.00 4 6 22 2.17 0.00 0 7 22 1.82 0.00 1 7 22 0.92 0.00 2 7 22 2.16 0.00 0 0 23 1.11 0.00 0 1 23 -0.79 0.00 1 1 23 -0.63 0.00 0 2 23 -0.45 0.00 1 2 23 0.11 0.00 2 2 23 -0.39 0.00 0 3 23 -1.81 0.00 1 3 23 -1.42 0.00 0 0 1 82.65 0.00 11 14 15 -1.41 0.00 12 12 16 3.66 0.00 11 13 16 -1.07 0.00 8 15 16 -0.60 0.00 0 16 17 0.73 0.00 1 16 17 1.45 0.00 10 11 18 -1.79 0.00 7 13 18 0.73 0.00 5 14 18 -1.09 0.00 9 10 19 2.15 0.00 8 11 19 0.02 0.00 6 12 19 1.94 0.00 4 13 19 -0.07 0.00 8 9 20 0.00 0.00 5 11 20 -0.64 0.00 0 12 20 2.22 0.00 1 12 20 0.00 0.00 6 8 21 -0.73 0.00 5 9 21 -1.48 0.00 0 10 21 -1.23 0.00 1 10 21 -1.34 0.00 2 10 21 -1.66 0.00 5 6 22 2.24 0.00 3 7 22 0.62 0.00 2 3 23 -0.40 0.00 3 3 23 1.07 0.00 0 4 23 -2.00 0.00 1 4 23 -2.18 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 11015) # 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 -0.000 -0.000 892 247 ' ' 2 -0.021 0.482 0.486 2797 172 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 0 1 1.095 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL djx045_0m P m -3 m R = 0.13 CELL 18.6011 18.6011 18.6011 90.00 90.00 90.00 SPGR Pm-3m # Solvent Accessible Volume = 3696.9 # Electrons Found in S.A.V. = 411.7 # Note: Atoms in Void as Cxxx and Qxxx all others C101 1.000 0.312-0.003 ! 6.23 eA-3 C102 0.228 1.000 0.000 ! 6.04 eA-3 Q103 0.362 1.000-0.000 ! 2.04 eA-3 C104 1.000 0.793 0.075 ! 1.81 eA-3 Q105 1.000 0.453-0.000 ! 1.46 eA-3 Q106 1.000 0.336 0.336 ! 1.36 eA-3 Q107 0.532 0.281-0.006 ! 1.27 eA-3 C108 0.500 0.500 0.500 ! 0.95 eA-3 C109 0.500 1.000 0.500 ! 0.85 eA-3 Q110 0.131 0.500 0.000 ! 0.79 eA-3 C111 0.907 0.141 0.007 ! 0.78 eA-3 C112 1.000 0.833 0.167 ! 0.70 eA-3 C113 0.153 1.000 0.000 ! 0.69 eA-3 C114 0.717 0.938 0.024 ! 0.67 eA-3 C115 0.252 0.491 0.266 ! 0.62 eA-3 Q116 0.500 0.047-0.006 ! 0.62 eA-3 Q117 0.320 0.065 0.065 ! 0.61 eA-3 Q118 0.151 0.323 0.157 ! 0.57 eA-3 Q119 0.031 0.953 0.476 ! 0.53 eA-3 Q120 0.410 0.076 0.119 ! 0.52 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'