Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xin Liu' _publ_contact_author_email LIUXIN64@NANKAI.EDU.CN _publ_section_title ; Design of two 3D homochiral Co(?) metal-organic open frameworks by layered-pillar strategy: structure and properties ; loop_ _publ_author_name 'Ping Zhu.' 'Jun Chen.' 'Wen Gu.' 'Dai Liao.' 'Shi-Ping Yan.' # Attachment '1 CIF.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 643624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H12 Co N2 O5.50' _chemical_formula_sum 'C9 H12 Co N2 O5.50' _chemical_formula_weight 295.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, z' _cell_length_a 22.113(3) _cell_length_b 6.9149(12) _cell_length_c 7.7209(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1180.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2949 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.8 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7988 _exptl_absorpt_correction_T_max 0.8433 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8796 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2084 _reflns_number_gt 1956 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+7.4016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0.010(2) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(7) _refine_ls_number_reflns 2084 _refine_ls_number_parameters 170 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.71252(4) 0.45830(13) 0.24225(15) 0.0236(3) Uani 1 1 d . . . N1 N 0.6983(3) 1.0653(8) -0.2199(10) 0.0298(15) Uani 1 1 d D . . H1A H 0.6964 1.1629 -0.1392 0.036 Uiso 1 1 calc RD . . H1B H 0.6847 1.1115 -0.3246 0.036 Uiso 1 1 calc RD . . O1 O 0.6708(3) 0.6563(9) 0.0615(9) 0.0365(16) Uani 1 1 d . A . O2 O 0.7551(3) 0.7960(9) -0.0367(7) 0.0320(15) Uani 1 1 d . . . O3 O 0.7470(2) 0.7536(9) -0.4186(7) 0.0258(13) Uani 1 1 d . . . O4 O 0.6729(3) 0.6144(12) -0.5668(10) 0.0470(19) Uani 1 1 d . . . C1 C 0.6987(4) 0.7687(13) -0.0408(11) 0.030(2) Uani 1 1 d . . . C2 C 0.6624(3) 0.8958(11) -0.1636(11) 0.0284(18) Uani 1 1 d . A . H2 H 0.6254 0.9426 -0.1019 0.034 Uiso 1 1 calc R . . C3 C 0.6433(4) 0.7778(12) -0.3170(11) 0.0312(19) Uani 1 1 d . . . H3A H 0.6123 0.8521 -0.3814 0.037 Uiso 1 1 calc R A . H3B H 0.6235 0.6588 -0.2736 0.037 Uiso 1 1 calc R . . C4 C 0.6945(5) 0.7160(15) -0.4496(13) 0.040(3) Uani 1 1 d . A . N2 N 0.6318(4) 0.288(2) 0.2670(16) 0.026(2) Uani 0.521(11) 1 d PGU A 1 C5 C 0.5774(5) 0.3730(15) 0.3151(16) 0.027(4) Uani 0.521(11) 1 d PGU A 1 H5A H 0.5758 0.5080 0.3377 0.032 Uiso 0.521(11) 1 calc PR A 1 C6 C 0.5255(4) 0.2610(16) 0.3303(16) 0.035(4) Uani 0.521(11) 1 d PGU A 1 H6A H 0.4884 0.3194 0.3631 0.042 Uiso 0.521(11) 1 calc PR A 1 C7 C 0.5280(5) 0.0635(16) 0.2973(17) 0.027(4) Uani 0.521(11) 1 d PGU . 1 C8 C 0.5823(7) -0.0219(15) 0.2492(19) 0.039(16) Uani 0.521(11) 1 d PGU A 1 H8A H 0.5840 -0.1568 0.2266 0.047 Uiso 0.521(11) 1 calc PR A 1 C9 C 0.6342(5) 0.090(2) 0.2340(19) 0.022(3) Uani 0.521(11) 1 d PGU A 1 H9A H 0.6714 0.0318 0.2012 0.026 Uiso 0.521(11) 1 calc PR A 1 N3 N 0.6325(4) 0.288(2) 0.2083(18) 0.026(2) Uani 0.479(11) 1 d PGU A 2 C10 C 0.6353(5) 0.097(2) 0.2651(19) 0.018(3) Uani 0.479(11) 1 d PGU A 2 H10A H 0.6722 0.0462 0.3079 0.022 Uiso 0.479(11) 1 calc PR A 2 C11 C 0.5839(7) -0.0186(16) 0.2593(18) 0.017(11) Uani 0.479(11) 1 d PGU A 2 H11A H 0.5858 -0.1488 0.2981 0.021 Uiso 0.479(11) 1 calc PR A 2 C12 C 0.5298(5) 0.0562(15) 0.1967(17) 0.023(4) Uani 0.479(11) 1 d PGU . 2 C13 C 0.5270(4) 0.2467(17) 0.1399(17) 0.028(4) Uani 0.479(11) 1 d PGU A 2 H13A H 0.4900 0.2978 0.0972 0.033 Uiso 0.479(11) 1 calc PR A 2 C14 C 0.5784(5) 0.3625(15) 0.1457(18) 0.035(5) Uani 0.479(11) 1 d PGU A 2 H14A H 0.5765 0.4927 0.1069 0.042 Uiso 0.479(11) 1 calc PR 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 0.0206(5) 0.0237(5) 0.0265(5) -0.0037(5) -0.0025(6) -0.0006(3) N1 0.033(3) 0.021(3) 0.036(4) 0.003(3) -0.009(3) 0.001(2) O1 0.027(3) 0.032(3) 0.050(4) 0.023(3) 0.005(3) 0.000(3) O2 0.032(3) 0.039(3) 0.025(4) 0.018(3) -0.013(3) -0.010(3) O3 0.017(3) 0.037(3) 0.023(3) -0.004(3) 0.000(2) -0.002(3) O4 0.040(4) 0.057(4) 0.045(4) -0.011(3) -0.012(3) 0.013(4) C1 0.022(4) 0.040(5) 0.028(5) 0.007(4) 0.014(3) 0.019(4) C2 0.025(4) 0.030(4) 0.031(4) 0.010(3) 0.002(3) 0.011(3) C3 0.029(4) 0.031(4) 0.033(5) -0.005(3) -0.008(3) -0.006(4) C4 0.052(7) 0.039(5) 0.030(5) -0.015(4) 0.001(4) 0.010(5) N2 0.024(3) 0.020(3) 0.034(7) 0.006(5) 0.004(5) 0.003(2) C5 0.032(7) 0.026(6) 0.022(7) 0.001(5) -0.002(5) 0.005(6) C6 0.027(7) 0.037(7) 0.040(8) -0.002(6) 0.005(6) 0.003(6) C7 0.018(6) 0.024(7) 0.040(8) -0.001(7) 0.000(6) -0.002(6) C8 0.039(17) 0.035(17) 0.043(17) 0.000(9) -0.002(9) -0.001(8) C9 0.022(5) 0.025(5) 0.019(6) 0.008(5) -0.001(5) 0.000(5) N3 0.024(3) 0.020(3) 0.034(7) 0.006(5) 0.004(5) 0.003(2) C10 0.021(5) 0.019(5) 0.014(6) -0.005(5) -0.004(5) 0.000(5) C11 0.016(12) 0.011(13) 0.025(13) 0.005(7) 0.001(7) -0.001(6) C12 0.023(7) 0.021(7) 0.026(7) -0.003(7) -0.006(6) -0.008(6) C13 0.022(7) 0.024(7) 0.037(8) 0.001(6) -0.003(6) -0.001(6) C14 0.027(7) 0.038(8) 0.039(9) 0.000(7) 0.004(6) 0.000(7) _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 O4 2.025(7) 1_556 ? Co1 O2 2.072(6) 3_645 ? Co1 N1 2.113(6) 3_645 ? Co1 N3 2.143(10) . ? Co1 N2 2.148(10) . ? Co1 O3 2.158(6) 3_645 ? Co1 O1 2.162(6) . ? N1 C2 1.481(10) . ? N1 Co1 2.113(6) 3_655 ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? O1 C1 1.268(11) . ? O2 C1 1.261(11) . ? O2 Co1 2.072(6) 3_655 ? O3 C4 1.213(12) . ? O3 Co1 2.158(6) 3_655 ? O4 C4 1.241(12) . ? O4 Co1 2.026(7) 1_554 ? C1 C2 1.522(11) . ? C2 C3 1.499(11) . ? C2 H2 1.0000 . ? C3 C4 1.586(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N2 C5 1.3900 . ? N2 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 C8 1.3900 . ? C7 C7 1.517(19) 4_655 ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? N3 C10 1.3900 . ? N3 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10A 0.9500 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 C12 1.53(2) 4_655 ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 H14A 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 O4 Co1 O2 174.6(3) 1_556 3_645 ? O4 Co1 N1 106.0(3) 1_556 3_645 ? O2 Co1 N1 78.7(3) 3_645 3_645 ? O4 Co1 N3 91.5(5) 1_556 . ? O2 Co1 N3 83.9(4) 3_645 . ? N1 Co1 N3 162.4(4) 3_645 . ? O4 Co1 N2 82.5(4) 1_556 . ? O2 Co1 N2 93.3(4) 3_645 . ? N1 Co1 N2 167.1(4) 3_645 . ? N3 Co1 N2 12.1(5) . . ? O4 Co1 O3 94.0(3) 1_556 3_645 ? O2 Co1 O3 89.1(2) 3_645 3_645 ? N1 Co1 O3 83.9(2) 3_645 3_645 ? N3 Co1 O3 93.4(4) . 3_645 ? N2 Co1 O3 85.9(4) . 3_645 ? O4 Co1 O1 87.0(2) 1_556 . ? O2 Co1 O1 89.8(3) 3_645 . ? N1 Co1 O1 97.1(2) 3_645 . ? N3 Co1 O1 85.3(4) . . ? N2 Co1 O1 92.9(4) . . ? O3 Co1 O1 178.3(3) 3_645 . ? C2 N1 Co1 104.3(4) . 3_655 ? C2 N1 H1A 110.9 . . ? Co1 N1 H1A 110.9 3_655 . ? C2 N1 H1B 110.9 . . ? Co1 N1 H1B 110.9 3_655 . ? H1A N1 H1B 108.9 . . ? C1 O1 Co1 125.6(5) . . ? C1 O2 Co1 113.8(5) . 3_655 ? C4 O3 Co1 131.5(6) . 3_655 ? C4 O4 Co1 131.8(7) . 1_554 ? O2 C1 O1 123.8(8) . . ? O2 C1 C2 116.8(7) . . ? O1 C1 C2 119.0(7) . . ? N1 C2 C3 110.5(7) . . ? N1 C2 C1 110.9(6) . . ? C3 C2 C1 109.1(7) . . ? N1 C2 H2 108.8 . . ? C3 C2 H2 108.8 . . ? C1 C2 H2 108.8 . . ? C2 C3 C4 117.1(7) . . ? C2 C3 H3A 108.0 . . ? C4 C3 H3A 108.0 . . ? C2 C3 H3B 108.0 . . ? C4 C3 H3B 108.0 . . ? H3A C3 H3B 107.3 . . ? O3 C4 O4 129.3(9) . . ? O3 C4 C3 119.9(8) . . ? O4 C4 C3 110.4(9) . . ? C5 N2 C9 120.0 . . ? C5 N2 Co1 120.6(7) . . ? C9 N2 Co1 119.4(7) . . ? C6 C5 N2 120.0 . . ? C6 C5 H5A 120.0 . . ? N2 C5 H5A 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 C7 117.3(16) . 4_655 ? C6 C7 C7 122.5(16) . 4_655 ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 N2 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C9 H9A 120.0 . . ? C10 N3 C14 120.0 . . ? C10 N3 Co1 116.5(8) . . ? C14 N3 Co1 123.3(8) . . ? N3 C10 C11 120.0 . . ? N3 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 C12 116.3(15) . 4_655 ? C11 C12 C12 123.6(14) . 4_655 ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 N3 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C14 H14A 120.0 . . ? 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 O4 Co1 O1 C1 116.9(8) 1_556 . . . ? O2 Co1 O1 C1 -67.5(8) 3_645 . . . ? N1 Co1 O1 C1 11.1(8) 3_645 . . . ? N3 Co1 O1 C1 -151.4(9) . . . . ? N2 Co1 O1 C1 -160.8(8) . . . . ? O3 Co1 O1 C1 -115(8) 3_645 . . . ? Co1 O2 C1 O1 172.0(7) 3_655 . . . ? Co1 O2 C1 C2 -14.8(10) 3_655 . . . ? Co1 O1 C1 O2 -8.5(13) . . . . ? Co1 O1 C1 C2 178.4(6) . . . . ? Co1 N1 C2 C3 -85.1(6) 3_655 . . . ? Co1 N1 C2 C1 36.0(7) 3_655 . . . ? O2 C1 C2 N1 -15.9(11) . . . . ? O1 C1 C2 N1 157.6(8) . . . . ? O2 C1 C2 C3 106.1(9) . . . . ? O1 C1 C2 C3 -80.4(10) . . . . ? N1 C2 C3 C4 51.5(9) . . . . ? C1 C2 C3 C4 -70.6(9) . . . . ? Co1 O3 C4 O4 170.1(8) 3_655 . . . ? Co1 O3 C4 C3 -18.2(14) 3_655 . . . ? Co1 O4 C4 O3 1.6(18) 1_554 . . . ? Co1 O4 C4 C3 -170.7(6) 1_554 . . . ? C2 C3 C4 O3 4.8(13) . . . . ? C2 C3 C4 O4 177.9(8) . . . . ? O4 Co1 N2 C5 31.5(7) 1_556 . . . ? O2 Co1 N2 C5 -145.1(7) 3_645 . . . ? N1 Co1 N2 C5 163.7(15) 3_645 . . . ? N3 Co1 N2 C5 -106(4) . . . . ? O3 Co1 N2 C5 126.1(7) 3_645 . . . ? O1 Co1 N2 C5 -55.1(7) . . . . ? O4 Co1 N2 C9 -148.7(6) 1_556 . . . ? O2 Co1 N2 C9 34.8(6) 3_645 . . . ? N1 Co1 N2 C9 -16(2) 3_645 . . . ? N3 Co1 N2 C9 74(4) . . . . ? O3 Co1 N2 C9 -54.1(6) 3_645 . . . ? O1 Co1 N2 C9 124.7(6) . . . . ? C9 N2 C5 C6 0.0 . . . . ? Co1 N2 C5 C6 179.8(8) . . . . ? N2 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C7 -174.9(4) . . . 4_655 ? C6 C7 C8 C9 0.0 . . . . ? C7 C7 C8 C9 175.2(5) 4_655 . . . ? C7 C8 C9 N2 0.0 . . . . ? C5 N2 C9 C8 0.0 . . . . ? Co1 N2 C9 C8 -179.8(8) . . . . ? O4 Co1 N3 C10 -108.5(6) 1_556 . . . ? O2 Co1 N3 C10 74.4(6) 3_645 . . . ? N1 Co1 N3 C10 66.1(16) 3_645 . . . ? N2 Co1 N3 C10 -66(3) . . . . ? O3 Co1 N3 C10 -14.4(6) 3_645 . . . ? O1 Co1 N3 C10 164.6(6) . . . . ? O4 Co1 N3 C14 66.7(8) 1_556 . . . ? O2 Co1 N3 C14 -110.5(8) 3_645 . . . ? N1 Co1 N3 C14 -118.8(14) 3_645 . . . ? N2 Co1 N3 C14 109(4) . . . . ? O3 Co1 N3 C14 160.8(7) 3_645 . . . ? O1 Co1 N3 C14 -20.2(7) . . . . ? C14 N3 C10 C11 0.0 . . . . ? Co1 N3 C10 C11 175.3(9) . . . . ? N3 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C12 -175.8(8) . . . 4_655 ? C11 C12 C13 C14 0.0 . . . . ? C12 C12 C13 C14 176.1(6) 4_655 . . . ? C12 C13 C14 N3 0.0 . . . . ? C10 N3 C14 C13 0.0 . . . . ? Co1 N3 C14 C13 -175.0(9) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.021 0.255 84.7 26.6 2 0.500 -0.033 0.745 84.7 27.3 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.742 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.129 # Attachment '2 CIF.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 650893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H13 Co N3 O5' _chemical_formula_sum 'C9 H9 Co N2 O4' _chemical_formula_weight 268.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, z' _cell_length_a 21.956(4) _cell_length_b 6.8823(14) _cell_length_c 7.7410(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1169.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2974 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7992 _exptl_absorpt_correction_T_max 0.8437 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8112 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2030 _reflns_number_gt 1929 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+33.0420P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.30(12) _refine_ls_number_reflns 2030 _refine_ls_number_parameters 177 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.2517 _refine_ls_wR_factor_gt 0.2504 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.28808(6) 0.5244(2) 0.7551(3) 0.0288(6) Uani 1 1 d . . . N1 N 0.3014(5) -0.0877(15) 1.227(2) 0.052(4) Uani 1 1 d D . . H1A H 0.3155 -0.1259 1.3331 0.062 Uiso 1 1 calc RD . . H1B H 0.3028 -0.1921 1.1524 0.062 Uiso 1 1 calc RD . . O1 O 0.3303(4) 0.3305(18) 0.9344(15) 0.040(3) Uani 1 1 d . A . O2 O 0.2447(5) 0.1891(15) 1.0360(12) 0.031(2) Uani 1 1 d U . . O3 O 0.2535(5) 0.2308(16) 1.4187(12) 0.035(2) Uani 1 1 d . . . O4 O 0.3292(6) 0.3705(19) 1.5569(16) 0.046(3) Uani 1 1 d U . . C1 C 0.3003(8) 0.219(3) 1.049(2) 0.053(5) Uani 1 1 d U . . C2 C 0.3374(7) 0.077(2) 1.158(2) 0.044(4) Uani 1 1 d U A . H2 H 0.3729 0.0273 1.0904 0.052 Uiso 1 1 calc R . . C3 C 0.3598(6) 0.200(2) 1.3092(18) 0.034(3) Uani 1 1 d U . . H3A H 0.3769 0.3218 1.2623 0.041 Uiso 1 1 calc R A . H3B H 0.3935 0.1290 1.3663 0.041 Uiso 1 1 calc R . . C4 C 0.3092(8) 0.256(3) 1.456(2) 0.046(4) Uani 1 1 d U A . N2 N 0.3688(6) 0.693(2) 0.732(2) 0.027(4) Uani 0.513(15) 1 d PGU A 1 C5 C 0.4251(7) 0.6150(19) 0.687(2) 0.028(4) Uani 0.513(15) 1 d PGU A 1 H5A H 0.4289 0.4798 0.6648 0.033 Uiso 0.513(15) 1 calc PR A 1 C6 C 0.4758(6) 0.735(2) 0.675(2) 0.028(3) Uani 0.513(15) 1 d PGU A 1 H6A H 0.5142 0.6823 0.6446 0.034 Uiso 0.513(15) 1 calc PR A 1 C7 C 0.4702(7) 0.933(2) 0.708(2) 0.028(3) Uani 0.513(15) 1 d PGU . 1 C8 C 0.4139(9) 1.0106(19) 0.752(2) 0.028(3) Uani 0.513(15) 1 d PGU A 1 H8A H 0.4100 1.1458 0.7746 0.033 Uiso 0.513(15) 1 calc PR A 1 C9 C 0.3632(7) 0.890(3) 0.764(2) 0.027(3) Uani 0.513(15) 1 d PGU A 1 H9A H 0.3247 0.9434 0.7949 0.032 Uiso 0.513(15) 1 calc PR A 1 N3 N 0.3685(6) 0.712(3) 0.796(2) 0.022(4) Uani 0.487(15) 1 d PGU A 2 C10 C 0.3674(8) 0.900(3) 0.730(2) 0.026(3) Uani 0.487(15) 1 d PGU A 2 H10A H 0.3311 0.9491 0.6794 0.031 Uiso 0.487(15) 1 calc PR A 2 C11 C 0.4194(10) 1.015(2) 0.737(2) 0.027(3) Uani 0.487(15) 1 d PGU A 2 H11A H 0.4186 1.1428 0.6909 0.033 Uiso 0.487(15) 1 calc PR A 2 C12 C 0.4725(8) 0.942(2) 0.810(2) 0.026(3) Uani 0.487(15) 1 d PGU . 2 C13 C 0.4736(6) 0.755(3) 0.877(2) 0.027(3) Uani 0.487(15) 1 d PGU A 2 H13A H 0.5099 0.7053 0.9271 0.033 Uiso 0.487(15) 1 calc PR A 2 C14 C 0.4216(7) 0.640(2) 0.870(2) 0.029(4) Uani 0.487(15) 1 d PGU A 2 H14A H 0.4224 0.5116 0.9156 0.034 Uiso 0.487(15) 1 calc PR 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 0.0242(8) 0.0228(8) 0.0396(10) -0.0073(10) -0.0209(9) -0.0004(6) N1 0.039(6) 0.027(5) 0.089(12) -0.004(8) -0.032(8) 0.003(5) O1 0.018(4) 0.048(7) 0.054(7) 0.015(5) 0.013(4) 0.007(5) O2 0.031(3) 0.032(3) 0.031(3) 0.0008(10) -0.0003(10) -0.0002(10) O3 0.038(5) 0.042(6) 0.025(5) 0.008(5) -0.013(4) -0.002(5) O4 0.046(3) 0.047(3) 0.046(3) -0.0001(10) -0.0005(10) 0.0001(10) C1 0.048(8) 0.064(9) 0.047(7) 0.024(7) 0.018(6) 0.022(7) C2 0.041(6) 0.047(7) 0.043(7) 0.009(6) -0.004(6) 0.011(6) C3 0.030(6) 0.037(6) 0.036(7) 0.000(5) -0.002(5) 0.001(5) C4 0.046(5) 0.047(5) 0.046(5) -0.0004(10) -0.0003(10) 0.0002(10) N2 0.020(6) 0.028(6) 0.034(7) 0.006(6) -0.002(6) -0.004(5) C5 0.027(6) 0.031(6) 0.025(6) 0.003(5) -0.001(5) 0.001(5) C6 0.027(5) 0.029(5) 0.028(6) 0.000(5) 0.000(5) 0.003(5) C7 0.027(5) 0.027(5) 0.029(5) 0.002(5) -0.001(4) 0.001(4) C8 0.025(4) 0.028(4) 0.030(4) 0.001(4) -0.004(4) 0.000(4) C9 0.025(5) 0.029(5) 0.026(5) 0.001(5) -0.004(5) 0.000(4) N3 0.022(4) 0.022(4) 0.022(4) -0.0002(10) 0.0000(10) 0.0000(10) C10 0.026(3) 0.026(3) 0.026(3) 0.0000(10) -0.0002(10) 0.0001(10) C11 0.027(3) 0.027(3) 0.027(3) 0.0002(10) -0.0003(10) 0.0000(10) C12 0.024(5) 0.026(5) 0.028(5) -0.001(5) -0.002(5) 0.001(4) C13 0.025(5) 0.029(5) 0.028(6) -0.001(5) 0.000(5) 0.001(5) C14 0.027(6) 0.029(6) 0.030(7) -0.003(6) -0.002(6) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.071(13) 1_554 ? Co1 O2 2.102(10) 3_557 ? Co1 N1 2.115(11) 3_557 ? Co1 N2 2.124(12) . ? Co1 O1 2.136(11) . ? Co1 O3 2.160(10) 3_557 ? Co1 N3 2.212(14) . ? N1 C2 1.480(19) . ? N1 Co1 2.115(11) 3_547 ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? O1 C1 1.34(2) . ? O2 C1 1.24(2) . ? O2 Co1 2.102(10) 3_547 ? O3 C4 1.27(2) . ? O3 Co1 2.160(10) 3_547 ? O4 C4 1.19(2) . ? O4 Co1 2.071(13) 1_556 ? C1 C2 1.53(2) . ? C2 C3 1.52(2) . ? C2 H2 1.0000 . ? C3 C4 1.64(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N2 C5 1.3900 . ? N2 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 C8 1.3900 . ? C7 C7 1.60(3) 4_675 ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? N3 C10 1.3900 . ? N3 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10A 0.9500 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 C12 1.45(3) 4_675 ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 H14A 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 O4 Co1 O2 174.2(5) 1_554 3_557 ? O4 Co1 N1 105.5(6) 1_554 3_557 ? O2 Co1 N1 80.0(5) 3_557 3_557 ? O4 Co1 N2 81.5(6) 1_554 . ? O2 Co1 N2 93.3(6) 3_557 . ? N1 Co1 N2 168.3(5) 3_557 . ? O4 Co1 O1 88.5(4) 1_554 . ? O2 Co1 O1 89.2(4) 3_557 . ? N1 Co1 O1 97.6(5) 3_557 . ? N2 Co1 O1 91.9(5) . . ? O4 Co1 O3 93.4(5) 1_554 3_557 ? O2 Co1 O3 88.8(4) 3_557 3_557 ? N1 Co1 O3 83.6(5) 3_557 3_557 ? N2 Co1 O3 86.6(5) . 3_557 ? O1 Co1 O3 177.5(5) . 3_557 ? O4 Co1 N3 93.3(6) 1_554 . ? O2 Co1 N3 81.2(6) 3_557 . ? N1 Co1 N3 160.9(6) 3_557 . ? N2 Co1 N3 13.5(6) . . ? O1 Co1 N3 85.7(6) . . ? O3 Co1 N3 92.5(6) 3_557 . ? C2 N1 Co1 104.0(8) . 3_547 ? C2 N1 H1A 111.0 . . ? Co1 N1 H1A 111.0 3_547 . ? C2 N1 H1B 111.0 . . ? Co1 N1 H1B 111.0 3_547 . ? H1A N1 H1B 109.0 . . ? C1 O1 Co1 125.0(10) . . ? C1 O2 Co1 111.3(10) . 3_547 ? C4 O3 Co1 129.7(12) . 3_547 ? C4 O4 Co1 131.4(13) . 1_556 ? O2 C1 O1 121.5(16) . . ? O2 C1 C2 117.6(16) . . ? O1 C1 C2 118.0(14) . . ? N1 C2 C3 108.9(14) . . ? N1 C2 C1 113.7(13) . . ? C3 C2 C1 104.1(13) . . ? N1 C2 H2 110.0 . . ? C3 C2 H2 110.0 . . ? C1 C2 H2 110.0 . . ? C2 C3 C4 116.5(12) . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? C4 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? O4 C4 O3 126.4(19) . . ? O4 C4 C3 111.2(15) . . ? O3 C4 C3 117.5(15) . . ? C5 N2 C9 120.0 . . ? C5 N2 Co1 123.6(9) . . ? C9 N2 Co1 116.4(9) . . ? N2 C5 C6 120.0 . . ? N2 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 C7 120(2) . 4_675 ? C6 C7 C7 119(2) . 4_675 ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 N2 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C9 H9A 120.0 . . ? C10 N3 C14 120.0 . . ? C10 N3 Co1 118.3(10) . . ? C14 N3 Co1 121.3(10) . . ? N3 C10 C11 120.0 . . ? N3 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 C12 120(2) . 4_675 ? C11 C12 C12 120(2) . 4_675 ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 N3 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C14 H14A 120.0 . . ? 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 O4 Co1 O1 C1 -121.2(15) 1_554 . . . ? O2 Co1 O1 C1 64.1(15) 3_557 . . . ? N1 Co1 O1 C1 -15.7(15) 3_557 . . . ? N2 Co1 O1 C1 157.3(15) . . . . ? O3 Co1 O1 C1 102(9) 3_557 . . . ? N3 Co1 O1 C1 145.3(15) . . . . ? Co1 O2 C1 O1 -176.2(14) 3_547 . . . ? Co1 O2 C1 C2 24(2) 3_547 . . . ? Co1 O1 C1 O2 15(3) . . . . ? Co1 O1 C1 C2 175.4(12) . . . . ? Co1 N1 C2 C3 88.0(12) 3_547 . . . ? Co1 N1 C2 C1 -27.5(17) 3_547 . . . ? O2 C1 C2 N1 4(2) . . . . ? O1 C1 C2 N1 -157.2(16) . . . . ? O2 C1 C2 C3 -114.6(18) . . . . ? O1 C1 C2 C3 84.4(19) . . . . ? N1 C2 C3 C4 -47.3(17) . . . . ? C1 C2 C3 C4 74.3(16) . . . . ? Co1 O4 C4 O3 18(3) 1_556 . . . ? Co1 O4 C4 C3 172.3(10) 1_556 . . . ? Co1 O3 C4 O4 -178.3(13) 3_547 . . . ? Co1 O3 C4 C3 29(2) 3_547 . . . ? C2 C3 C4 O4 -171.5(15) . . . . ? C2 C3 C4 O3 -15(2) . . . . ? O4 Co1 N2 C5 -33.6(10) 1_554 . . . ? O2 Co1 N2 C5 143.8(10) 3_557 . . . ? N1 Co1 N2 C5 -161(3) 3_557 . . . ? O1 Co1 N2 C5 54.6(10) . . . . ? O3 Co1 N2 C5 -127.5(10) 3_557 . . . ? N3 Co1 N2 C5 117(4) . . . . ? O4 Co1 N2 C9 146.6(9) 1_554 . . . ? O2 Co1 N2 C9 -36.0(9) 3_557 . . . ? N1 Co1 N2 C9 19(4) 3_557 . . . ? O1 Co1 N2 C9 -125.3(8) . . . . ? O3 Co1 N2 C9 52.7(8) 3_557 . . . ? N3 Co1 N2 C9 -63(3) . . . . ? C9 N2 C5 C6 0.0 . . . . ? Co1 N2 C5 C6 -179.8(12) . . . . ? N2 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C7 175.3(5) . . . 4_675 ? C6 C7 C8 C9 0.0 . . . . ? C7 C7 C8 C9 -175.2(7) 4_675 . . . ? C7 C8 C9 N2 0.0 . . . . ? C5 N2 C9 C8 0.0 . . . . ? Co1 N2 C9 C8 179.8(12) . . . . ? O4 Co1 N3 C10 101.8(9) 1_554 . . . ? O2 Co1 N3 C10 -80.2(9) 3_557 . . . ? N1 Co1 N3 C10 -69(2) 3_557 . . . ? N2 Co1 N3 C10 73(3) . . . . ? O1 Co1 N3 C10 -170.0(9) . . . . ? O3 Co1 N3 C10 8.3(9) 3_557 . . . ? O4 Co1 N3 C14 -71.2(10) 1_554 . . . ? O2 Co1 N3 C14 106.8(10) 3_557 . . . ? N1 Co1 N3 C14 118(2) 3_557 . . . ? N2 Co1 N3 C14 -100(4) . . . . ? O1 Co1 N3 C14 17.0(10) . . . . ? O3 Co1 N3 C14 -164.7(10) 3_557 . . . ? C14 N3 C10 C11 0.0 . . . . ? Co1 N3 C10 C11 -173.1(12) . . . . ? N3 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C12 177.0(14) . . . 4_675 ? C11 C12 C13 C14 0.0 . . . . ? C12 C12 C13 C14 -177.0(13) 4_675 . . . ? C12 C13 C14 N3 0.0 . . . . ? C10 N3 C14 C13 0.0 . . . . ? Co1 N3 C14 C13 172.8(12) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 -0.041 0.271 79.2 13.4 2 0.000 -0.025 0.729 79.2 14.0 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.834 _refine_diff_density_min -2.291 _refine_diff_density_rms 0.201