#------------------------------------------------------------------------------ #$Date: 2023-11-23 01:39:40 +0200 (Thu, 23 Nov 2023) $ #$Revision: 287746 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247768.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247768 loop_ _publ_author_name 'Jones, Isabelle M.' 'Turner, Gemma F.' 'Pitts, Kari' 'Powell, Rees' 'Riboldi-Tunnicliffe, Alan' 'Williamson, Rachel' 'Boer, Stephanie' 'Allen, Lauren' 'Moggach, Stephen A.' _publ_section_title ; High-pressure induced guest-mediated gate opening behaviour of the Co-based framework ZIF-67 ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00979C _journal_year 2023 _chemical_formula_moiety 'C8 H10 Co N4, 1.521(N4)' _chemical_formula_sum 'C8 H10 Co N10.08' _chemical_formula_weight 306.36 _chemical_name_common ZIF-67 _space_group_crystal_system cubic _space_group_IT_number 217 _space_group_name_Hall 'I -4 2 3' _space_group_name_H-M_alt 'I -4 3 m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-10-03 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-10-04 deposited with the CCDC. 2023-11-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 17.0740(4) _cell_length_b 17.0740(4) _cell_length_c 17.0740(4) _cell_measurement_reflns_used 2043 _cell_measurement_temperature 293 _cell_measurement_theta_max 23.2390 _cell_measurement_theta_min 3.3520 _cell_volume 4977.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -37.00 29.00 0.50 75.00 -- -24.44 -53.00 39.00 132 2 \w 68.00 106.00 0.50 75.00 -- 24.20-178.00 90.00 76 3 \w -4.00 18.00 0.50 75.00 -- 24.20 -57.00 60.00 44 4 \w -18.00 4.00 0.50 75.00 -- 24.20 57.00 0.00 44 5 \w -4.00 18.00 0.50 75.00 -- -24.44 -57.00 30.00 44 6 \w -36.00 -16.00 0.50 75.00 -- -24.44 38.00 -30.00 40 7 \w -30.00 10.00 0.50 75.00 -- 24.20 82.00 -29.00 80 8 \w 30.00 55.00 0.50 75.00 -- 24.20 -99.00-150.00 50 9 \w -36.00 -16.00 0.50 75.00 -- -24.44 38.00 150.00 40 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0382768000 _diffrn_orient_matrix_UB_12 -0.0067060000 _diffrn_orient_matrix_UB_13 -0.0147251000 _diffrn_orient_matrix_UB_21 0.0056949000 _diffrn_orient_matrix_UB_22 -0.0409565000 _diffrn_orient_matrix_UB_23 0.0039480000 _diffrn_orient_matrix_UB_31 -0.0152184000 _diffrn_orient_matrix_UB_32 0.0015992000 _diffrn_orient_matrix_UB_33 0.0386108000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_unetI/netI 0.0487 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 4014 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 18.729 _diffrn_reflns_theta_max 18.729 _diffrn_reflns_theta_min 3.375 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_correction_T_min 0.4402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1171 before and 0.0857 after correction. The Ratio of minimum to maximum transmission is 0.5910. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear bluish violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier bluish _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.226 _exptl_crystal_description block _exptl_crystal_F_000 1867 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.624 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.110 _refine_ls_abs_structure_details ; Flack x determined using 153 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 391 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.248 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0675 _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^)+(0.1473P)^2^+11.5625P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2079 _refine_ls_wR_factor_ref 0.2103 _reflns_Friedel_coverage 0.761 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.994 _reflns_number_gt 373 _reflns_number_total 391 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL zif67_ln2_700p_a.res in I-43m zif67_ln2_700p.res created by SHELXL-2018/3 at 16:11:47 on 03-Oct-2023 REM Old TITL ZIF67_LN2_700P in I-43m REM SHELXT solution in I-43m: R1 0.143, Rweak 0.068, Alpha 0.113 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.213 ( 0.031 ) from 190 Parsons' quotients REM Formula found by SHELXT: C48 N49 Co6 CELL 0.71073 17.074 17.074 17.074 90 90 90 ZERR 12 0.0004 0.0004 0.0004 0 0 0 LATT -2 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 Co N UNIT 96 120 12 121 EQIV $1 +Y,+X,+Z EQIV $2 1-Y,1-X,+Z EQIV $3 1-X,1-Y,+Z EQIV $4 1-Y,+Z,1-X EQIV $5 1-Z,+Y,1-X EQIV $6 1-Z,1-X,+Y EQIV $7 +X,+Z,+Y DFIX 1.55 C2 C3 DFIX 1.387 0.01 N1 C1 DFIX 1.337 0.01 N1 C2 DFIX 2.175 0.01 C1 C2 EADP N1 C1 C2 FLAT C1 N1 C2 C3 RIGU C2 C3 L.S. 20 0 0 PLAN 7 SIZE 0.09 0.1 0.14 TEMP 19.85 CONF FREE N4 N4_$1 FREE N4 N4_$2 FREE N4 N4_$3 FREE N11 N11_$4 FREE N11 N11_$5 FREE N11 N11_$6 FREE N11 N11_$7 FREE N11 N11_$2 list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.147300 11.562500 FVAR 0.05616 CO1 3 0.500000 0.250000 0.000000 10.25000 0.04244 0.04127 = 0.04244 0.00000 0.00000 0.00000 N1 4 0.587256 0.319532 0.033137 11.00000 0.05468 0.05865 = 0.04097 0.00926 -0.00283 -0.00668 C2 1 0.632163 0.367837 -0.009831 10.50000 0.05468 0.05865 = 0.04097 0.00926 -0.00283 -0.00668 C1 1 0.607094 0.336560 0.109967 11.00000 0.05468 0.05865 = 0.04097 0.00926 -0.00283 -0.00668 AFIX 43 1.0770 H1 2 0.582048 0.309636 0.161219 11.00000 -1.20000 AFIX 0 C3 1 0.628275 0.371725 -0.098360 10.50000 0.08924 0.08924 = 0.04682 0.01490 -0.01490 -0.05002 PART -1 AFIX 33 1.0830 H3A 2 0.669805 0.414767 -0.119477 10.50000 -1.50000 H3B 2 0.642523 0.314896 -0.122665 10.50000 -1.50000 H3C 2 0.569718 0.388291 -0.116244 10.50000 -1.50000 AFIX 0 PART 0 N2 4 0.500000 0.500000 0.000000 10.12500 0.16699 N5 4 0.500000 0.500000 -0.233016 10.18750 0.15492 N8 4 0.781382 0.218618 0.069705 10.25000 0.09887 N3 4 0.500000 0.500000 -0.046145 10.12500 0.10461 N9 4 0.778621 0.221379 0.027503 10.25000 0.08640 N6 4 0.817788 0.182212 -0.182212 10.05556 0.12375 N4 4 0.507826 0.454031 -0.233462 10.25000 0.13073 N7 4 0.765908 0.234092 -0.234092 10.11112 0.14801 N10 4 0.927493 0.072507 0.072507 10.08333 0.12842 N11 4 0.916267 0.083733 0.033130 10.08333 0.09815 HKLF 4 REM zif67_ln2_700p_a.res in I-43m REM wR2 = 0.2103, GooF = S = 1.249, Restrained GooF = 1.248 for all data REM R1 = 0.0675 for 373 Fo > 4sig(Fo) and 0.0707 for all 391 data REM 47 parameters refined using 8 restraints END WGHT 0.1471 11.5525 REM Highest difference peak 0.624, deepest hole -0.530, 1-sigma level 0.110 Q1 1 0.6994 0.3006 -0.3006 10.16667 0.05 0.62 Q2 1 0.8027 0.1973 -0.1973 10.16667 0.05 0.52 Q3 1 0.8610 0.1390 -0.1390 10.16667 0.05 0.52 Q4 1 0.7858 0.2142 0.0450 10.50000 0.05 0.43 Q5 1 0.7642 0.2358 0.0164 10.50000 0.05 0.43 Q6 1 0.7598 0.2219 0.0235 11.00000 0.05 0.41 Q7 1 0.7840 0.1894 0.0503 11.00000 0.05 0.39 REM The information below was added by Olex2. REM REM R1 = 0.0675 for 373 Fo > 4sig(Fo) and 0.0707 for all 4014 data REM 47 parameters refined using n/a restraints REM Highest difference peak 0.62, deepest hole -0.53 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0707 REM R1_gt = 0.0675 REM wR_ref = 0.2103 REM GOOF = 1.249 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 4014 REM Reflections_gt = 373 REM Parameters = 47 REM Hole = -0.53 REM Peak = 0.62 REM Flack = 0.07(3) ; _cod_data_source_file d3ce00979c2.cif _cod_data_source_block zif67_ln2_700p _cod_original_cell_volume 4977.4(3) _cod_database_code 7247768 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Co C8 H10 N4' _chemical_oxdiff_usercomment 'ZIF67 @ 0.7 GPa in LN2' _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. ; _shelx_estimated_absorpt_t_max 0.912 _shelx_estimated_absorpt_t_min 0.868 _diffrn_orient_matrix_axis[1] matrixX _diffrn_orient_matrix_axis[2] matrixY _diffrn_orient_matrix_axis[3] matrixZ _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) groups 2. Restrained distances C2-C3 1.55 with sigma of 0.02 N1-C1 1.387 with sigma of 0.01 N1-C2 1.337 with sigma of 0.01 C1-C2 2.175 with sigma of 0.01 3. Restrained planarity C1, N1, C2, C3 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints Uanis(N1) = Uanis(C1) = Uanis(C2) 5. Rigid body (RIGU) restrains C2, C3 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5) N5(0.1875) N8(0.25) N3(0.125) N9(0.25) N6(0.05556) N4(0.25) N7(0.11112) N10(0.083333) N11(0.083333) 7.a Me refined with riding coordinates: C3(H3A,H3B,H3C) 7.b Aromatic/amide H refined with riding coordinates: C1(H1) ; _platon_squeeze_void_probe_radius 1.20 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 3.026 _oxdiff_exptl_absorpt_empirical_full_min 0.617 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+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 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 0.500000 0.250000 0.000000 0.042(2) Uani 1 4 d S T P . . N1 N 0.5873(7) 0.3195(8) 0.0331(6) 0.051(4) Uani 1 1 d D . . . . C2 C 0.6322(8) 0.3678(8) -0.0098(9) 0.051(4) Uani 1 2 d DS T P . . C1 C 0.6071(11) 0.3366(12) 0.1100(7) 0.051(4) Uani 1 1 d D . . . . H1 H 0.582048 0.309636 0.161219 0.062 Uiso 1 1 calc R U . . . C3 C 0.6283(15) 0.3717(15) -0.0984(14) 0.075(11) Uani 1 2 d DS T P . . H3A H 0.669805 0.414767 -0.119477 0.113 Uiso 0.5 1 calc R U P A -1 H3B H 0.642523 0.314896 -0.122665 0.113 Uiso 0.5 1 calc R U P A -1 H3C H 0.569718 0.388291 -0.116244 0.113 Uiso 0.5 1 calc R U P A -1 N2 N 0.500000 0.500000 0.000000 0.17(4) Uiso 1 8 d S . P . . N5 N 0.500000 0.500000 -0.233(6) 0.15(4) Uiso 0.75 4 d S . P . . N8 N 0.781(3) 0.219(3) 0.070(4) 0.10(2) Uiso 0.5 2 d S . P . . N3 N 0.500000 0.500000 -0.046(5) 0.10(2) Uiso 0.5 4 d S . P . . N9 N 0.779(2) 0.221(2) 0.028(4) 0.09(2) Uiso 0.5 2 d S . P . . N6 N 0.818(6) 0.182(6) -0.182(6) 0.12(5) Uiso 0.3334 6 d S . P . . N4 N 0.508(8) 0.454(5) -0.233(6) 0.13(3) Uiso 0.25 1 d . . P . . N7 N 0.766(4) 0.234(4) -0.234(4) 0.15(4) Uiso 0.6667 6 d S . P . . N10 N 0.927(6) 0.073(6) 0.073(6) 0.13(6) Uiso 0.5 6 d S . P . . N11 N 0.916(9) 0.084(9) 0.033(12) 0.10(7) Uiso 0.1667 2 d S . P . . 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 0.042(2) 0.041(3) 0.042(2) 0.000 0.000 0.000 N1 0.055(8) 0.059(8) 0.041(7) 0.009(6) -0.003(6) -0.007(6) C2 0.055(8) 0.059(8) 0.041(7) 0.009(6) -0.003(6) -0.007(6) C1 0.055(8) 0.059(8) 0.041(7) 0.009(6) -0.003(6) -0.007(6) C3 0.089(17) 0.089(17) 0.047(11) 0.015(11) -0.015(11) -0.05(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _axis.id _axis.type _axis.equipment _axis.parity _axis.depends_on _axis.zero _axis.vector[1] _axis.vector[2] _axis.vector[3] source . source . . . 1.00000000 0.00000000 0.00003403 omega rotation goniometer -1 . 0.12240000 0.00000000 0.00000000 1.00000000 kappa rotation goniometer -1 omega 0.28425000 -0.76560404 0.00000000 0.64331210 phi rotation goniometer -1 kappa . -0.00006266 0.00000000 1.00000000 theta rotation goniometer -1 . 0.19892000 0.00000000 0.00000000 1.00000000 matrixX general general . phi . 1.00000000 0.00000000 0.00000000 matrixY general general . phi . 0.00000000 1.00000000 0.00000000 matrixZ general general . phi . 0.00000000 0.00000000 1.00000000 dacX translation general . phi . 0.00000000 1.00000000 0.00000000 dacY translation general . phi . -1.00000000 0.00000000 0.00000000 dacZ translation general . phi . 0.00000000 0.00000000 1.00000000 loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 -2 2 32.4 2.87 2 0 2 35.75 3.04 -2 -2 0 34.02 2.92 -2 -2 0 41.71 3.18 -2 0 -2 37.21 2.98 2 2 0 38.07 3.03 -2 -2 2 328.18 27.12 -2 -2 -2 335.31 25.47 1 3 0 72.9 5.75 -1 -3 0 61.56 5.04 -1 -3 0 61.73 4.97 -1 -3 0 56.49 4.71 0 -1 -3 65.94 6.24 -1 -3 0 56.49 4.91 1 3 0 60.4 4.84 1 0 3 58.66 4.83 -1 0 3 57.18 5.64 -1 0 -3 62.06 4.95 0 -3 1 61.16 4.99 1 0 3 64.82 5.08 1 0 -3 64.28 6.14 -1 2 -3 7.86 0.74 1 2 3 10.17 0.9 -1 2 -3 9.33 0.85 -1 -2 3 9.1 0.82 1 2 3 10.01 0.8 -2 -3 1 8.97 0.8 2 3 1 8.88 0.79 2 3 1 9.01 0.77 -2 -3 1 8.7 0.81 2 3 1 9.08 0.8 2 3 1 9.51 0.93 -2 -3 -1 11.65 0.83 -2 -3 -1 11.19 0.87 -2 -3 -1 11.07 0.88 1 2 -3 10.1 0.81 -2 -3 -1 11.38 0.86 2 3 -1 10.49 0.84 2 3 -1 9.5 1.42 -1 -3 2 9.22 0.82 -2 1 -3 9.27 0.74 2 1 3 9.63 0.8 -1 -3 2 7.28 0.77 2 1 3 10.11 0.76 -1 -3 2 8.04 0.79 1 3 2 9.72 0.88 -2 1 -3 9.41 0.84 1 -3 2 10.58 0.85 1 3 -2 9.91 1 -2 -1 -3 9.92 0.84 2 -1 3 9.71 0.88 -2 -1 -3 10.84 0.84 1 3 -2 9.9 0.82 2 1 -3 8.49 1.42 -3 -2 -1 10.83 0.86 0 -3 3 30.97 2.63 -3 -3 0 32.85 2.6 3 3 0 33.73 2.59 -3 0 -3 37.96 2.5 -3 -3 0 40.11 3.41 0 -3 3 29.63 2.69 -3 0 -3 29.95 2.85 0 3 -3 31.41 2.81 3 2 3 84.57 6.58 2 3 3 84.26 6.68 2 3 3 84.76 7.46 -2 -3 3 78.23 6.75 -3 -3 2 80.39 7.55 2 3 -3 79.51 6.61 -3 -3 -2 86.62 6.42 -3 -2 -3 84.65 6.57 -3 -3 -2 83.46 6.6 0 0 4 103.31 9.53 0 0 4 112.81 9.79 -2 -4 0 6.59 0.65 2 4 0 4.19 1.13 -2 -4 0 7.53 0.59 -2 -4 0 7.37 0.65 0 -2 -4 8.15 0.87 -2 -4 0 6.9 0.61 2 4 0 7.24 0.66 0 2 4 6.77 0.68 -1 1 -4 32.49 2.83 1 4 1 44.85 3.42 -1 -4 1 36.25 2.86 1 1 4 35.53 2.83 1 4 1 33.1 2.82 -1 -4 1 32.76 2.88 1 1 4 43.04 3.88 1 -1 -4 35.1 3.81 -1 -4 1 30.98 2.67 -1 -1 4 31.57 2.7 -1 -4 1 33.68 2.9 1 1 4 37.47 3.1 1 -1 4 38.61 2.9 1 4 -1 37.03 2.86 1 -1 4 37.93 3.06 1 1 -4 38.88 3.81 1 4 -1 34.5 3.34 -1 -1 -4 37.37 2.94 -1 1 4 39.84 3.51 1 4 -1 34.58 3.31 -3 -4 1 80.83 6.65 1 3 4 87 6.96 3 4 1 86.57 6.58 -1 -3 4 80.89 6.43 -1 3 -4 87.83 6.95 -1 3 -4 73.5 6.41 -1 -3 4 82.81 6.82 -3 -4 1 81.13 6.51 3 4 -1 86.65 7.24 -1 -3 -4 82.9 8.49 -3 -4 -1 86.34 6.56 -3 -4 -1 79.6 6.72 -3 -4 -1 81.82 6.24 1 3 -4 75.83 6.56 3 4 -1 78.64 6.6 0 -4 2 6.89 0.71 -2 0 -4 8.28 0.64 2 0 4 8.01 0.68 -2 0 -4 8.03 0.68 -2 2 -4 14.41 1.23 -2 -4 2 13.43 1.11 2 4 2 14.29 1.35 -2 -4 2 13.21 1.17 2 2 4 13.67 1.14 -2 2 -4 13.46 1.07 -2 -4 2 12.9 1.15 -2 -2 4 15.22 1.43 2 4 -2 13.36 1.12 2 4 -2 13.64 1.18 2 4 -2 11.92 1.3 -2 -2 -4 13.09 1.06 -2 -2 -4 13.23 1.1 -2 -4 -2 12.81 1.04 -2 -4 -2 12.99 1.08 -2 -4 -2 12.37 1.13 2 4 -2 13.93 1.51 2 -2 4 14.16 1.13 2 2 -4 13.74 1.55 -3 1 -4 90.99 6.24 1 4 3 85.77 6.51 1 4 3 90.8 7.38 -1 -4 3 82.63 6.99 -1 4 -3 82.56 7.06 -3 1 -4 91.25 7.05 -1 -4 3 83.32 6.68 3 1 4 87.99 6.89 -1 -4 3 71.82 6.92 3 -1 4 88.8 6.9 -4 -3 -1 83.56 6.7 1 4 -3 74.27 7.74 1 4 -3 76.26 6.53 1 -4 3 84.88 7 -3 -1 -4 86.43 6.71 -3 -3 4 104.91 11.41 3 3 4 122.54 9.45 -3 -4 3 113.73 9.63 3 4 3 118.8 9.53 4 3 3 124.3 9.44 -4 -3 -3 128.07 9.17 3 4 -3 117.11 9.68 -3 -3 -4 128.46 9.32 -3 -4 -3 117.38 9.83 3 4 -3 116.21 12.8 -3 -4 -3 124.64 9.37 0 4 -4 975.41 70.02 -4 -4 0 979.86 66.79 -4 -4 0 823.93 84.6 4 4 0 991.33 70.24 0 -4 4 977.13 67.17 4 4 0 987.98 66.86 0 -4 4 1000 68.11 -4 -4 2 109.73 10.4 4 4 2 94.4 8.51 -2 4 -4 88.53 9.13 4 2 4 105.59 8.42 4 2 4 106.07 8.1 2 4 4 111.28 8.91 -2 -4 4 106.63 8.37 2 4 4 106.23 8.28 -4 -4 -2 112.46 8.84 -4 -4 -2 104.18 7.93 -4 -2 -4 111.71 8.55 -4 -2 -4 107.89 8.97 2 4 -4 98.82 8.32 4 4 4 245.64 18.29 -4 -4 4 220.31 22.48 -4 -4 -4 242.9 18.43 0 -1 5 0.72 0.27 0 1 -5 0.81 0.15 -1 -5 0 0.45 0.24 1 5 0 0.94 0.44 0 1 5 1.03 0.32 1 5 0 0.75 0.33 3 5 0 4.09 0.67 -3 -5 0 5.19 0.46 0 3 5 3.98 0.7 -3 -5 0 4.93 0.53 0 -3 -5 3.5 0.92 3 5 0 6.1 0.61 -1 0 -5 0.85 0.21 0 -5 1 0.8 0.29 -1 0 5 0.98 0.42 1 0 -5 0.87 0.59 1 0 5 0.67 0.22 2 5 1 20.49 1.57 -2 -5 1 19.67 1.55 -2 -5 1 19.72 1.65 -2 -5 1 19.18 1.6 2 5 1 19.57 1.59 1 2 5 19.63 1.76 -1 -2 -5 18.66 1.53 -1 2 5 16.37 2.08 2 5 -1 18.14 1.51 -2 -5 -1 18.03 1.52 -2 -5 -1 18.24 1.46 -2 -5 -1 18.05 1.46 2 5 -1 16.67 1.58 1 -2 5 15.76 1.5 2 5 -1 19.65 2.1 2 5 -1 16.36 1.74 -2 -5 -1 17.02 1.55 1 -2 5 16.7 1.49 1 -2 5 18.79 1.59 4 5 1 15.3 1.32 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-1 -14 5 0.85 1.12 -5 1 -14 2.16 0.99 -5 1 -14 1.73 0.88 1 14 5 1.26 2.32 -5 -1 -14 -0.3 1.01 5 -1 14 1.65 1.03 -5 -1 -14 1.71 0.91 1 -14 5 0.35 1.09 1 14 -5 1.59 1.47 -3 -14 5 2.14 1 -5 3 -14 2.98 0.84 -3 -14 5 1.24 0.92 -5 3 -14 1.4 1.13 5 -3 14 1.55 0.92 -5 -3 -14 2.07 1.02 -5 -3 -14 1.09 0.96 3 14 -5 3.15 1.61 5 -3 14 1.77 0.76 3 14 -5 1.22 2.04 -3 -14 -5 1.77 1.16 -3 -14 -5 1.16 0.82 -6 0 -14 2.5 0.97 0 -14 6 0.42 1.02 0 -14 6 0.9 1.13 0 14 -6 3.2 1.57 -6 2 -14 28.17 2.18 -2 -14 6 26.83 2.48 -2 -14 6 24.89 2.65 -6 2 -14 25.2 2.58 2 14 6 23.25 3.83 6 -2 14 29.49 2.25 -6 -2 -14 20.67 2.59 2 14 -6 25.56 3.13 -2 -14 -6 27.47 2.59 -6 -2 -14 27.7 2.31 0 -1 -15 0.06 0.81 0 1 -15 0.31 2.05 0 -1 -15 -1.22 1.57 1 15 0 -0.17 1.76 -1 -15 0 -0.26 0.96 0 1 15 0.84 2.17 -1 -15 0 0.39 0.91 0 -1 15 0.49 1.7 -1 -15 0 -0.75 0.97 -3 -15 0 7.44 1.17 -3 -15 0 7.61 1.1 0 3 15 3.41 2.86 0 -3 -15 6.67 1.17 0 -3 15 5.77 1.52 0 -3 -15 5.79 1.82 0 -3 15 0.45 3.44 0 3 -15 0.56 2.68 3 15 0 6.2 1.93 -3 -15 0 7.26 1.03 -1 0 -15 -0.04 2.01 1 0 -15 -0.07 1.82 0 15 -1 -0.04 1.73 1 0 15 1.37 1.35 -1 0 15 -0.11 2.81 -1 2 -15 0.41 2.57 1 -2 -15 3.37 0.97 2 15 1 6.75 2.04 1 -2 -15 2.82 1.8 -2 -15 1 3.24 1 -1 -2 15 5.88 2.2 -2 -15 1 3.85 0.9 1 2 15 3.58 1.88 -2 -15 1 2.98 1.02 2 15 -1 3 1.88 -2 -15 -1 3.06 0.97 2 15 -1 -1.1 1.93 -2 -15 -1 3.39 0.89 -2 -15 -1 2.54 1.08 1 2 -15 0.28 2.2 -1 -2 -15 4.3 0.97 1 -2 15 1.71 3.13 -1 -2 -15 3.85 1.79 -1 2 15 8.47 3.6 1 -2 15 3.68 1.28 -2 -1 15 -0.42 3.21 1 15 2 1.29 2.02 2 -1 -15 4.24 0.98 -1 -15 2 2.36 0.9 2 1 15 3.43 1.36 2 -1 -15 3.28 1.52 -1 -15 2 3.78 1.03 -1 -15 2 2.34 1.09 2 1 -15 0.27 1.94 -2 -1 -15 4.23 2.1 -2 -1 -15 3.64 0.91 -1 -15 -2 5.2 1.18 1 15 -2 3.73 1.75 2 3 15 3.15 1.56 -3 -15 2 2.15 0.87 -2 -3 15 5.24 2.97 -3 -15 2 3.05 0.99 3 15 2 2.02 1.96 -3 -15 2 2.13 0.94 2 3 -15 0.08 2.03 -2 -3 -15 2.7 1.02 2 -3 15 2.83 2.06 3 15 -2 3.18 1.76 -3 -15 -2 1.71 1.11 3 15 -2 -0.38 2.11 -2 -3 -15 3.48 1.76 0 -15 3 8.96 1.25 0 15 -3 3.13 1.84 0 -15 3 6.03 1.07 -3 0 -15 8.19 1.09 -3 2 -15 3.45 0.91 -2 -15 3 2.27 1.06 -2 -15 3 2.3 0.98 2 15 3 2.94 2.08 -2 -15 3 3.51 0.9 2 15 -3 2.07 2.02 -3 -2 -15 1.13 0.99 2 15 -3 2.88 1.8 3 -2 15 2.86 2.09 -2 -15 -3 3.47 1.17 3 2 -15 0.17 1.95 -3 -2 -15 2.99 1.95 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 N1 110.9(4) 46 3_655 ? N1 Co1 N1 106.6(8) 3_655 . ? N1 Co1 N1 110.9(4) 46 . ? N1 Co1 N1 106.6(8) 46 48_554 ? N1 Co1 N1 110.9(4) 3_655 48_554 ? N1 Co1 N1 110.9(4) 48_554 . ? C2 N1 Co1 129.7(8) . . ? C2 N1 C1 104.4(11) . . ? C1 N1 Co1 125.3(10) . . ? N1 C2 N1 113.7(14) . 14_665 ? N1 C2 C3 123.1(7) 14_665 . ? N1 C2 C3 123.1(7) . . ? N1 C1 H1 125.6 . . ? C1 C1 N1 108.7(9) 14_665 . ? C1 C1 H1 125.6 14_665 . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 N2 N3 180.000(12) . 3_655 ? N4 N5 N4 109(10) 13 . ? N4 N5 N4 71(10) . 14_665 ? N4 N5 N4 179(10) 13 14_665 ? N4 N5 N4 71(10) 13 2_665 ? N4 N5 N4 109(10) 2_665 14_665 ? N4 N5 N4 179(10) . 2_665 ? N2 N3 N3 0.000(5) . 3_655 ? N11 N10 N11 115(10) 23_656 . ? N11 N10 N11 115(10) 23_656 10_656 ? N11 N10 N11 115(10) 7_665 . ? N11 N10 N11 115(10) 10_656 . ? N11 N10 N11 115(10) 14_665 10_656 ? N11 N10 N11 115(10) 23_656 17 ? N11 N10 N11 0(10) 10_656 17 ? N11 N10 N11 0(10) 14_665 . ? N11 N10 N11 0(10) 7_665 23_656 ? N11 N10 N11 115(10) 7_665 17 ? N11 N10 N11 115(10) 7_665 14_665 ? N11 N10 N11 115(10) 14_665 17 ? N11 N10 N11 115(10) 23_656 14_665 ? N11 N10 N11 115(10) . 17 ? N11 N10 N11 115(10) 7_665 10_656 ? 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 N1 1.987(11) 46 ? Co1 N1 1.987(11) . ? Co1 N1 1.987(11) 3_655 ? Co1 N1 1.987(11) 48_554 ? N1 C2 1.344(11) . ? N1 C1 1.386(13) . ? C2 C3 1.51(2) . ? C1 C1 1.36(4) 14_665 ? C1 H1 1.0770 . ? C3 H3A 1.0830 . ? C3 H3B 1.0830 . ? C3 H3C 1.0830 . ? N2 N3 0.79(8) . ? N2 N3 0.79(8) 3_655 ? N5 N4 0.80(10) 13 ? N5 N4 0.80(10) 14_665 ? N5 N4 0.80(10) . ? N5 N4 0.80(10) 2_665 ? N8 N9 0.72(7) . ? N3 N3 1.58(17) 3_655 ? N6 N7 1.53(18) . ? N10 N11 0.7(2) 7_665 ? N10 N11 0.7(2) . ? N10 N11 0.7(2) 10_656 ? N10 N11 0.7(2) 23_656 ? N10 N11 0.7(2) 17 ? N10 N11 0.7(2) 14_665 ? 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 C2 N1 173.2(6) . . . 14_665 ? Co1 N1 C2 C3 -6(3) . . . . ? Co1 N1 C1 C1 -172.9(8) . . . 14_665 ? C2 N1 C1 C1 -1.0(14) . . . 14_665 ? C1 N1 C2 N1 2(2) . . . 14_665 ? C1 N1 C2 C3 -177.9(18) . . . . ?