#------------------------------------------------------------------------------ #$Date: 2023-11-23 01:39:40 +0200 (Thu, 23 Nov 2023) $ #$Revision: 287746 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247771.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_7247771 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_absolute_configuration ad _chemical_formula_moiety 'C8 H10 Co N4, 2.458(N4)' _chemical_formula_sum 'C8 H10 Co N13.83' _chemical_formula_weight 358.89 _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 16.7265(4) _cell_length_b 16.7265(4) _cell_length_c 16.7265(4) _cell_measurement_reflns_used 4140 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.7590 _cell_measurement_theta_min 3.4170 _cell_volume 4679.67(19) _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 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.989 _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 -73.00 -34.00 0.50 58.04 -- 24.20 -28.00 -95.00 78 2 \w 63.00 88.00 0.50 58.04 -- 24.20 28.00 65.00 50 3 \w -89.00 -64.00 0.50 58.04 -- -24.44 -28.00 -95.00 50 4 \w 74.00 104.00 0.50 58.04 -- 24.20 178.00 90.00 60 5 \w 33.00 63.00 0.50 58.04 -- 24.20 -99.00-150.00 60 6 \w 73.00 104.00 0.50 58.04 -- 24.20 178.00 -90.00 62 7 \w -29.00 -9.00 0.50 58.04 -- 24.20 77.00-180.00 40 8 \w -29.00 -9.00 0.50 58.04 -- 24.20 77.00 -30.00 40 9 \w -40.00 -5.00 0.50 58.04 -- 24.20 114.00 -45.00 70 10 \w -2.00 32.00 0.50 58.04 -- 24.20 26.00 -8.00 68 11 \w -128.00-104.00 0.50 58.04 -- -24.44 -77.00-180.00 48 12 \w 20.00 46.00 0.50 58.04 -- -24.44 -40.00-167.00 52 13 \w -36.00 -5.00 0.50 58.04 -- -24.44 97.00 -35.00 62 14 \w -76.00 -48.00 0.50 58.04 -- -24.44 97.00 -35.00 56 15 \w -26.00 0.00 0.50 58.04 -- -24.44 -26.00-171.00 52 16 \w 0.00 26.00 0.50 58.04 -- -24.44 -82.00-151.00 52 17 \w -56.00 12.00 0.50 58.04 -- -24.44 53.00 -17.00 136 18 \w -72.00 -46.00 0.50 58.04 -- -24.44 77.00-180.00 52 19 \w -57.00 -31.00 0.50 58.04 -- -24.44 57.00-180.00 52 20 \w -18.00 28.00 0.50 58.04 -- -24.44 -53.00-162.00 92 21 \w -39.00 -13.00 0.50 58.04 -- -24.44 13.00 -3.00 52 22 \w 21.00 48.00 0.50 58.04 -- -24.44-114.00-135.00 54 23 \w 9.00 35.00 0.50 58.04 -- -24.44-114.00 45.00 52 ; _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 0.0150193000 _diffrn_orient_matrix_UB_12 0.0071976000 _diffrn_orient_matrix_UB_13 0.0389868000 _diffrn_orient_matrix_UB_21 -0.0041016000 _diffrn_orient_matrix_UB_22 0.0417617000 _diffrn_orient_matrix_UB_23 -0.0061245000 _diffrn_orient_matrix_UB_31 -0.0394224000 _diffrn_orient_matrix_UB_32 -0.0016049000 _diffrn_orient_matrix_UB_33 0.0155629000 _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 0.0856 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 11050 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 20.825 _diffrn_reflns_theta_max 20.825 _diffrn_reflns_theta_min 3.445 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_T_max 0.7446 _exptl_absorpt_correction_T_min 0.6284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1012 before and 0.0855 after correction. The Ratio of minimum to maximum transmission is 0.8439. 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 1.528 _exptl_crystal_description block _exptl_crystal_F_000 2182 _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 0.895 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.140 _refine_ls_abs_structure_details ; Flack x determined using 192 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 491 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.210 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0744 _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^)+(0.1547P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1887 _refine_ls_wR_factor_ref 0.1935 _reflns_Friedel_coverage 0.773 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.991 _reflns_number_gt 458 _reflns_number_total 491 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL zif67_ln2_2300_a.res in I-43m zif67_ln2_2300.res created by SHELXL-2018/3 at 14:08:51 on 03-Oct-2023 REM Old TITL ZIF67_LN2_2300 in I-43m REM SHELXT solution in I-43m: R1 0.111, Rweak 0.039, Alpha 0.081 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.137 ( 0.023 ) from 193 Parsons' quotients REM Formula found by SHELXT: C21 N31 Co3 CELL 0.71073 16.7265 16.7265 16.7265 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 12 166 EQIV $1 1-Y,1-X,+Z DFIX 1.55 C3 C2 DFIX 1.337 0.01 N1 C2 DFIX 1.387 0.01 C1 N1 EADP C1 C2 N1 DFIX 2.175 0.01 C1 C2 FLAT C1 C2 N1 C3 RIGU C3 C2 EADP N15 N13 EADP N4 N5 DFIX 1.08 N9 N8 DFIX 1.08 N4 N5 EADP N3 N2 L.S. 10 PLAN 5 SIZE 0.09 0.1 0.14 CONF FREE C2 C1_$1 FREE C2 C1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.154700 0.298400 FVAR 0.13709 CO1 3 0.500000 0.250000 0.000000 10.25000 0.03238 0.03145 = 0.03238 0.00000 0.00000 0.00000 N1 4 0.586371 0.319939 0.038847 11.00000 0.03576 0.03813 = 0.03235 0.00073 -0.00048 -0.00827 C2 1 0.632420 0.367580 -0.005094 10.50000 0.03576 0.03813 = 0.03235 0.00073 -0.00048 -0.00827 C1 1 0.603652 0.337860 0.117602 11.00000 0.03576 0.03813 = 0.03235 0.00073 -0.00048 -0.00827 AFIX 43 1.0770 H1 2 0.576532 0.311162 0.169540 11.00000 -1.20000 AFIX 0 C3 1 0.628638 0.371362 -0.095526 10.50000 0.04419 0.04419 = 0.04111 0.01122 -0.01122 -0.01178 PART -1 AFIX 33 1.0830 H3A 2 0.585538 0.328154 -0.117151 10.50000 -1.50000 H3B 2 0.610702 0.430796 -0.113911 10.50000 -1.50000 H3C 2 0.686972 0.357838 -0.120152 10.50000 -1.50000 AFIX 0 PART 0 N5 4 0.500000 0.500000 -0.232784 10.25000 0.11607 N8 4 0.782400 0.217600 0.074397 10.50000 0.12233 N3 4 0.500000 0.500000 -0.038825 10.16667 0.06584 N9 4 0.763594 0.236406 0.023844 10.50000 0.11986 N4 4 0.543609 0.456391 -0.229342 10.25000 0.11607 N11 4 0.581699 0.418301 -0.418301 10.08333 0.09830 PART 2 N12 4 0.586188 0.413812 -0.455869 10.12500 0.12063 PART 0 N7 4 0.757179 0.242821 -0.242821 10.16667 0.08935 N13 4 0.875798 0.124202 -0.124202 10.12500 0.11000 PART 1 N10 4 0.539653 0.460347 -0.385830 10.08333 0.12611 PART 0 N15 4 0.827267 0.111220 -0.111220 10.12500 0.11000 N2 4 0.500000 0.500000 0.000000 10.08334 0.06584 HKLF 4 REM zif67_ln2_2300_a.res in I-43m REM wR2 = 0.1935, GooF = S = 1.162, Restrained GooF = 1.210 for all data REM R1 = 0.0744 for 458 Fo > 4sig(Fo) and 0.0788 for all 491 data REM 49 parameters refined using 10 restraints END WGHT 0.1551 0.7054 REM Highest difference peak 0.895, deepest hole -0.724, 1-sigma level 0.140 Q1 1 0.7637 0.2363 -0.2198 10.50000 0.05 0.89 Q2 1 0.7290 0.2710 -0.2710 10.16667 0.05 0.87 Q3 1 0.4762 0.4922 -0.2402 11.00000 0.05 0.67 Q4 1 0.5692 0.4308 -0.4308 10.16667 0.05 0.48 Q5 1 0.7708 0.2008 0.0412 11.00000 0.05 0.44 REM The information below was added by Olex2. REM REM R1 = 0.0744 for 458 Fo > 4sig(Fo) and 0.0788 for all 11050 data REM 49 parameters refined using n/a restraints REM Highest difference peak 0.89, deepest hole -0.72 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0788 REM R1_gt = 0.0744 REM wR_ref = 0.1935 REM GOOF = 1.162 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 11050 REM Reflections_gt = 458 REM Parameters = 49 REM Hole = -0.72 REM Peak = 0.89 REM Flack = 0.06(2) ; _cod_data_source_file d3ce00979c2.cif _cod_data_source_block zif67_ln2_2300 _cod_original_cell_volume 4679.7(3) _cod_database_code 7247771 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Co C8 H10 N4' _chemical_oxdiff_usercomment 'ZIF67 @ 2.3 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 0.906 _shelx_estimated_absorpt_t_min 0.859 _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 C3-C2 1.55 with sigma of 0.02 N1-C2 1.337 with sigma of 0.01 C1-N1 1.387 with sigma of 0.01 C1-C2 2.175 with sigma of 0.01 N9-N8 1.08 with sigma of 0.02 N4-N5 1.08 with sigma of 0.02 3. Restrained planarity C1, C2, N1, C3 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints Uanis(C1) = Uanis(C2) = Uanis(N1) Uiso(N15) = Uiso(N13) Uiso(N4) = Uiso(N5) Uiso(N3) = Uiso(N2) 5. Rigid body (RIGU) restrains C3, C2 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) N3(0.166667) N4(0.25) N11(0.083333) N12(0.125) N13(0.125) N10(0.083333) N15(0.125) N2(0.08334) 7.a Me refined with riding coordinates: C3(H3A,H3B,H3C) 7.b Aromatic/amide H refined with riding coordinates: C1(H1) ; _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 3.962 _oxdiff_exptl_absorpt_empirical_full_min 0.718 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 0.0321(14) Uani 1 4 d S T P . . N1 N 0.5864(6) 0.3199(6) 0.0388(5) 0.035(2) Uani 1 1 d D . . . . C2 C 0.6324(6) 0.3676(6) -0.0051(7) 0.035(2) Uani 1 2 d DS T P . . C1 C 0.6037(7) 0.3379(8) 0.1176(5) 0.035(2) Uani 1 1 d D . . . . H1 H 0.576532 0.311162 0.169540 0.042 Uiso 1 1 calc R U . . . C3 C 0.6286(8) 0.3714(8) -0.0955(11) 0.043(5) Uani 1 2 d DS T P . . H3A H 0.585538 0.328154 -0.117151 0.065 Uiso 0.5 1 calc R U P A -1 H3B H 0.610702 0.430796 -0.113911 0.065 Uiso 0.5 1 calc R U P A -1 H3C H 0.686972 0.357838 -0.120152 0.065 Uiso 0.5 1 calc R U P A -1 N5 N 0.500000 0.500000 -0.233(2) 0.116(11) Uiso 1 4 d DS . P . . N8 N 0.7824(12) 0.2176(12) 0.0744(17) 0.122(9) Uiso 1 2 d DS . P . . N3 N 0.500000 0.500000 -0.0388(19) 0.066(7) Uiso 0.6667 4 d S . P . . N9 N 0.7636(13) 0.2364(13) 0.0238(18) 0.120(9) Uiso 1 2 d DS . P . . N4 N 0.5436(11) 0.4564(11) -0.229(4) 0.116(11) Uiso 0.5 2 d DS . P . . N11 N 0.582(5) 0.418(5) -0.418(5) 0.10(4) Uiso 0.5 6 d S . P . . N12 N 0.586(7) 0.414(7) -0.456(9) 0.12(6) Uiso 0.25 2 d S . P . 2 N7 N 0.7572(15) 0.2428(15) -0.2428(15) 0.089(11) Uiso 1 6 d S . P . . N13 N 0.876(3) 0.124(3) -0.124(3) 0.11(2) Uiso 0.75 6 d S . P . . N10 N 0.540(8) 0.460(8) -0.386(12) 0.13(6) Uiso 0.1667 2 d S . P . 1 N15 N 0.827(7) 0.111(5) -0.111(5) 0.11(2) Uiso 0.25 2 d S . P . . N2 N 0.500000 0.500000 0.000000 0.066(7) Uiso 0.6667 8 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 0.0324(15) 0.0314(19) 0.0324(15) 0.000 0.000 0.000 N1 0.036(5) 0.038(5) 0.032(4) 0.001(4) 0.000(3) -0.008(3) C2 0.036(5) 0.038(5) 0.032(4) 0.001(4) 0.000(3) -0.008(3) C1 0.036(5) 0.038(5) 0.032(4) 0.001(4) 0.000(3) -0.008(3) C3 0.044(8) 0.044(8) 0.041(8) 0.011(6) -0.011(6) -0.012(10) 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 -2 -2 0 157.88 11.1 -2 -2 0 138.19 11.5 2 0 -2 146.89 11.4 -2 2 0 134.29 10.9 -2 0 2 133.59 11.7 0 2 -2 164.18 14 -2 2 0 127.79 10.8 2 -2 0 138.39 10.9 0 2 -2 150.28 11 -2 -2 0 123.39 11 2 0 -2 144.49 12 0 -2 2 143.09 10.8 -2 0 2 119.59 10.8 2 -2 0 136.39 11.2 -2 2 0 120.89 11.1 2 2 0 147.19 10.9 2 -2 0 128.99 11.1 2 2 0 144.59 11 -2 2 0 131.89 11.3 2 2 0 149.09 11.3 2 2 -2 2594.94 231.48 2 2 -2 2415.76 199.98 2 2 -2 2694.63 215.88 2 2 -2 2567.84 197.58 -2 -2 2 2647.34 226.88 -2 -2 2 2592.94 222.78 0 -3 1 389.36 28.2 3 1 0 407.76 30.1 3 -1 0 385.36 31.5 0 -3 -1 387.66 31.5 0 3 -1 405.66 33.3 -3 1 0 377.26 31.7 0 3 -1 403.66 31.8 3 1 0 389.96 30.3 0 -3 1 404.96 30.3 -3 -1 0 363.26 31.8 0 -3 1 404.76 30.7 -3 -1 0 395.26 30.8 0 -3 1 388.56 33.6 0 3 -1 385.36 34 0 -3 1 413.66 31.7 1 3 0 422.06 29.9 1 3 0 421.36 31.2 1 -3 0 371.66 32.1 -1 -3 0 361.76 31.1 3 0 -1 411.86 30.2 -1 3 0 399.56 32.4 -3 0 1 399.06 29.9 1 -3 0 420.26 30.4 3 0 -1 370.36 30.2 -1 3 0 383.86 30.1 -3 0 1 394.96 30.6 -1 3 0 378.96 31.5 1 -3 0 346.57 29.9 3 0 -1 399.66 29.9 1 -3 0 336.87 30.3 -3 0 1 412.46 30.6 -1 3 0 353.26 30.2 1 3 0 401.96 30.5 3 0 -1 383.36 31.1 3 0 -1 421.46 31.2 3 2 -1 85.19 6.6 -3 2 1 83.59 6.7 -3 2 1 80.79 7.6 3 2 -1 86.69 6.7 1 3 -2 91.39 6.6 1 -3 2 95.49 6.8 1 -3 2 96.09 7 -3 2 1 87.29 7.4 1 3 -2 85.59 6.8 1 3 -2 92.59 8.2 3 -2 1 89.99 6.8 1 -3 2 84.19 6.4 3 2 -1 86.59 6.6 3 -2 -1 66.19 6.2 -1 -3 2 86.39 6.6 3 -2 -1 65.59 6.4 -3 -2 1 71.19 6.5 -1 -3 2 73.99 6.6 -2 -1 3 79.39 7.7 -3 -2 1 77.79 7.6 -1 3 -2 73.49 8.3 -3 -2 1 72.69 6.8 -3 -2 1 75.79 6.5 -1 -3 2 78.89 7.2 -3 -2 1 74.19 6.3 3 -2 -1 65.99 6.3 3 -2 -1 63.99 6.6 -1 -3 2 75.29 6.3 3 1 -2 83.99 7.2 -2 3 1 88.19 6.3 -2 3 1 78.29 7.1 3 1 -2 86.99 6.2 -3 1 2 81.09 7.1 2 3 -1 88.29 6.4 2 3 -1 81.69 6.4 -2 3 1 73.69 6.4 2 3 -1 80.59 6.5 3 1 -2 87.89 6.9 -3 1 2 82.09 7.4 2 -3 1 76.39 6.2 3 1 -2 82.39 6.5 -2 3 1 72.69 6.3 2 -3 1 86.99 6.5 -3 1 2 78.29 6.2 -2 3 1 79.69 7.2 -3 1 2 87.69 6.6 3 1 -2 83.49 6.7 -3 1 2 90.29 8 3 1 -2 91.39 6.9 -2 3 1 76.49 6.9 2 -3 -1 60.39 6.3 -3 -1 2 71.09 6.5 -2 -3 1 72.89 6.3 -3 -1 2 63.69 7.3 -2 3 -1 75.89 7.6 2 -3 -1 70.09 6.7 3 -1 -2 70.09 6.5 3 -1 -2 71.89 7 -3 -1 2 73.19 6.2 -2 -3 1 65.79 6.1 2 -3 -1 60.99 6.3 -2 -3 1 68.99 6.1 -1 -2 3 84.79 6.4 -2 -3 1 70.59 6.4 2 -3 -1 62.89 6.2 -3 -1 2 80.39 7.7 -2 3 -1 75.39 6.2 -2 -3 1 72.59 6.3 -2 -3 1 73.09 7.3 -3 -1 2 75.89 6.6 -3 3 0 143.09 12.2 -3 3 0 152.78 11.7 3 3 0 141.79 12.1 3 0 -3 157.68 12.6 -3 0 3 169.18 12.8 -3 3 0 145.39 12.4 -3 0 3 152.48 11.8 -3 -3 0 133.69 12.4 -3 3 0 141.49 12.8 0 3 -3 157.88 11.9 3 3 0 159.08 11.9 3 3 0 164.68 12.2 -3 3 0 143.59 13.1 -3 3 0 156.18 12.3 3 0 -3 150.38 13.2 0 -3 3 148.39 11.9 3 0 -3 139.49 15.3 3 -3 0 159.48 12.2 -3 -3 0 158.68 12.1 -3 3 2 491.35 41.6 3 2 -3 485.65 39.7 3 3 -2 542.15 40.5 2 3 -3 534.75 40.1 -3 3 2 503.05 43.6 3 2 -3 549.85 41.2 -3 3 2 464.95 44.8 3 3 -2 521.15 40.5 3 2 -3 532.35 45.9 3 3 -2 552.54 42.3 3 3 -2 512.35 40.5 -3 2 3 522.25 46.3 3 -3 2 490.45 40.9 2 3 -3 515.45 46.2 3 2 -3 511.95 43.1 2 3 -3 515.55 41.6 3 -3 2 557.94 41.3 3 3 -2 499.55 43.4 3 -3 -2 490.05 43.7 -3 -2 3 533.85 45.2 3 -2 -3 496.65 42.7 -2 -3 3 519.05 44.9 -3 -2 3 521.55 46.8 -3 -3 2 533.75 40.9 -3 -2 3 513.75 42.2 -3 -3 2 515.65 45.2 -2 -3 3 541.05 40.2 -2 -3 3 549.15 37.2 -3 -3 2 487.75 41.3 3 -3 -2 471.15 41.8 -4 0 0 726.83 54.69 0 -4 0 647.84 53.99 0 -4 0 710.43 54.29 0 4 0 711.43 56.09 0 4 0 651.73 53.69 0 -4 0 688.53 60.69 0 -4 0 718.03 55.29 0 4 0 729.03 53.99 0 4 0 686.73 56.29 -4 2 0 10.3 1.8 4 -2 0 11.4 1.5 -4 -2 0 11.7 1.5 4 -2 0 10.1 1.2 0 -4 2 3 3.1 0 -4 2 14.3 2.2 0 4 -2 12.2 2 4 2 0 11.9 2 -4 -2 0 10.7 1.9 -4 -2 0 11.1 2.2 4 -2 0 13.4 2.6 -4 2 0 10.7 1.5 0 -4 2 10.9 1.9 0 -4 2 14.6 2.4 4 1 -1 160.88 12.9 1 4 -1 170.88 12.7 -4 1 1 161.58 12.5 1 -4 1 187.28 13.3 -1 -4 -1 177.88 13.8 1 4 -1 166.68 13.4 4 1 -1 164.98 13.1 4 1 -1 183.38 12.6 1 4 -1 181.98 13.5 -1 4 1 155.58 12.8 1 -4 1 173.28 12.9 -4 1 1 186.78 15.2 -4 1 1 158.08 12.7 -4 1 1 177.88 13.2 4 1 -1 167.08 12.6 1 4 -1 183.18 13.7 -1 -4 -1 156.58 14.2 4 1 -1 165.28 12.8 1 4 -1 172.88 12.7 4 1 -1 161.48 12.7 -1 -4 1 152.98 12.5 4 -1 -1 155.88 12.6 4 -1 -1 153.88 13.2 -1 4 -1 140.49 12.5 -1 4 -1 149.99 12.5 -1 4 -1 148.99 12.6 4 -1 -1 142.59 13 -4 1 -1 146.19 12.6 -1 4 -1 140.19 13.3 1 -4 -1 131.99 12.7 4 -1 -1 141.49 12.3 -4 -1 1 148.89 12.8 1 -4 -1 142.89 12.4 -4 -1 1 142.79 12.4 -1 -4 1 161.98 14.4 4 -1 -1 149.09 12.3 -1 4 -1 152.58 13.3 -1 -4 1 153.98 12.5 -3 1 4 399.26 28.9 4 3 -1 428.76 31.5 1 4 -3 445.86 34.9 -4 3 1 400.26 33.1 1 4 -3 432.96 31.3 4 3 -1 438.66 31.4 -4 3 1 389.66 31.6 1 -4 3 396.86 31 4 3 -1 415.06 31.3 1 -4 3 467.15 31.9 4 -3 1 439.26 31.8 4 3 -1 414.46 31.3 -4 3 1 381.26 31 -4 3 1 373.76 31.9 4 3 -1 392.16 32 -4 3 1 401.46 31.3 -4 3 1 389.36 33.9 4 -3 -1 374.56 32.1 4 -3 -1 399.66 32.5 -4 -3 1 427.46 36.9 4 -3 -1 380.26 33.8 -4 -3 1 425.76 32.4 -1 -4 3 454.95 29.8 -3 -1 4 464.95 29.4 4 -3 -1 370.76 33.2 4 -3 -1 365.96 32.8 -4 -3 1 415.76 32.6 -4 -3 1 447.66 33.1 -3 -1 4 445.46 36.2 -1 -4 3 427.26 32.3 -4 3 -1 402.66 33.3 -3 -1 4 481.75 32.4 -1 4 -3 445.26 39.1 -4 -3 1 411.66 33.9 4 -3 -1 426.86 29.8 -1 -4 3 428.26 36.2 -4 0 2 13.3 2.2 -2 -4 0 10.8 1.9 2 4 0 12.5 2.1 -2 4 0 14.8 2.2 2 -4 0 10.6 1.3 4 0 -2 12.4 2.1 2 4 0 12.4 1.9 -2 -4 0 9.7 1.8 -2 4 0 12.2 1.7 -4 0 2 10.4 2 -2 4 0 10.2 2.6 -2 4 0 10.6 1.5 -2 4 0 13.8 2.3 4 0 -2 10.8 2.2 2 -4 0 11.5 2.1 4 0 -2 9 1.2 -2 4 0 10.4 1.6 2 4 0 14 2.2 4 0 -2 11.5 1.7 4 0 -2 10.4 2.2 -4 0 2 10.9 2.2 -2 -4 0 13.9 2.2 -4 0 2 14.7 1.6 2 -4 0 11.2 1.7 4 0 -2 13.6 2.2 4 0 -2 13 2 -4 2 2 65.79 5.8 2 -4 2 90.79 6.9 -4 2 2 71.49 5.8 4 2 -2 79.79 6.4 4 2 -2 82.39 6.2 2 4 -2 82.39 6.2 4 2 -2 83.69 6.8 2 -4 2 77.89 6.5 4 2 -2 72.99 6.4 2 4 -2 84.39 6.4 -4 2 2 76.59 7.2 -4 2 2 72.59 6.9 2 4 -2 80.79 6.7 2 -4 2 73.89 6.1 2 4 -2 77.89 6.4 -4 2 2 72.59 7.4 -4 2 2 70.79 6.4 2 4 -2 86.59 6.4 -2 -4 2 72.29 6.2 -2 -2 4 61.49 9.3 -4 -2 2 71.59 6.1 4 -2 -2 65.99 6.6 -2 -4 2 72.39 6.4 -2 -4 2 74.39 7.9 -4 -2 2 72.99 8 -2 -4 2 69.19 6.4 -4 -2 2 69.69 6.3 -2 4 -2 65.09 8.2 -2 -4 2 76.99 6.7 -2 4 -2 71.79 6.4 -4 -2 2 62.49 6.4 -4 1 3 405.56 33.8 4 1 -3 423.26 30.8 -3 4 1 394.76 31.6 3 -4 1 372.96 30.4 4 1 -3 358.56 29.5 -4 1 3 393.16 30.1 -3 4 1 338.67 29.6 4 1 -3 408.96 33.2 3 4 -1 405.06 30.3 -3 4 1 344.67 32.3 -4 1 3 427.26 31.4 4 1 -3 419.86 30.1 3 -4 1 384.66 29.7 3 4 -1 411.16 31 -3 4 1 389.66 32.2 -3 4 1 354.86 30.3 -4 1 3 414.76 32.7 3 4 -1 453.65 30.2 3 4 -1 398.76 30.3 -3 4 1 365.66 33.1 -4 1 3 408.36 31.5 4 1 -3 400.66 30.7 4 1 -3 409.66 31.6 -4 1 3 394.16 30.3 -3 4 1 367.36 30 -4 -1 3 441.86 31.4 -3 4 -1 371.86 32.2 3 -4 -1 361.46 31.6 -3 4 -1 394.26 35.8 -4 -1 3 426.06 33 -3 4 -1 383.46 31.8 4 -1 -3 415.86 33.8 4 -1 -3 417.06 32.7 -3 -4 1 400.56 31.1 3 -4 -1 398.46 33.6 -3 -4 1 410.86 31.3 3 -4 -1 402.36 29.6 -3 -4 1 418.06 32.7 -3 -4 1 401.06 31.7 -4 -1 3 415.26 32.9 -3 -4 1 422.16 35.2 3 -4 -1 392.16 31.3 -3 4 -1 410.96 31 3 -4 -1 395.26 32.2 3 -4 -1 358.76 31.3 4 -1 -3 416.66 37.6 -3 -4 1 441.86 31.8 -4 -1 3 429.26 32.2 4 3 -3 1392.26 112.69 4 3 -3 1411.56 106.59 3 3 -4 1431.46 108.39 4 3 -3 1345.77 108.69 -4 3 3 1290.07 109.29 4 3 -3 1511.95 107.69 -3 3 4 1245.08 99.69 3 3 -4 1335.37 105.09 4 3 -3 1323.67 105.09 3 4 -3 1353.66 106.89 3 4 -3 1464.75 113.69 -4 3 3 1321.17 114.79 3 4 -3 1334.27 109.09 4 3 -3 1351.16 108.49 3 4 -3 1430.76 105.49 -4 3 3 1260.47 117.49 3 3 -4 1344.47 120.29 -4 -3 3 1397.46 106.49 -4 -3 3 1327.17 106.89 -3 -4 3 1414.26 109.29 4 -3 -3 1365.86 110.09 -3 -4 3 1368.36 106.59 -3 -4 3 1444.96 119.69 4 -3 -3 1165.28 112.19 -3 -3 4 1422.86 111.29 -4 -3 3 1438.16 121.89 -3 -4 3 1427.66 120.09 -3 -4 3 1273.67 108.59 -3 -3 4 1355.46 116.59 -3 -3 4 1442.46 108.49 -4 4 0 8957.8 727.93 4 -4 0 9835.42 734.03 -4 -4 0 9232.78 736.73 -4 0 4 9999 764.22 4 4 0 9649.63 716.13 -4 4 0 9266.37 755.02 4 0 -4 7447.15 847.82 4 4 0 9742.23 705.03 -4 4 0 9464.85 728.63 -4 4 0 9228.08 754.12 4 0 -4 9701.83 732.73 4 0 -4 9336.87 775.72 4 4 0 9834.72 734.33 -4 4 0 9288.67 717.23 -4 -4 0 9639.84 720.93 -4 0 4 9564.64 712.73 -4 4 2 370.56 36.3 -4 2 4 465.15 37.7 4 4 -2 461.55 35.6 4 2 -4 460.65 36.5 2 4 -4 473.35 40.7 -4 4 2 439.96 38.6 4 2 -4 492.95 38.8 -4 4 2 437.86 39.6 -4 4 2 395.06 36.1 4 -4 2 442.26 36.6 4 2 -4 462.75 34.6 4 -4 2 478.15 37.1 4 4 -2 470.35 35.7 4 4 -2 468.75 36 -4 2 4 459.45 38.9 4 4 -2 458.25 36.9 4 2 -4 419.36 39.9 2 4 -4 480.25 35.3 -4 -4 2 484.45 36 4 -4 -2 432.66 37.7 -4 -2 4 474.75 37.8 -4 -4 2 457.05 40.8 4 -2 -4 447.36 38 -2 -4 4 474.15 40.5 4 -4 -2 415.26 38.9 -4 -4 2 469.15 36.7 4 -4 -2 453.65 37.6 -2 -4 4 490.65 34.1 -4 -4 2 473.25 37.1 -2 -4 4 484.95 35.9 -4 -2 4 456.95 36.1 -4 -2 4 470.55 40.6 -4 -4 2 470.85 36.5 4 4 -4 1847.52 149.59 4 4 -4 1879.01 143.29 4 4 -4 1968 159.38 4 4 -4 1867.01 145.59 -4 -4 4 1876.51 158.38 -4 -4 4 1738.33 147.49 0 -5 1 21.3 2.4 -5 -1 0 24 3.1 0 5 -1 20.6 2.4 0 -5 1 19.3 2.6 0 -5 -1 18.8 3 0 5 -1 22.4 2.2 0 5 -1 20.9 2.9 0 -5 1 24.2 2.6 5 -1 0 19.8 3.5 -5 1 0 18.8 3 0 -5 1 20.5 3.2 0 5 -1 23.8 3.5 0 -5 -1 24.2 3 0 5 1 27.6 2.9 0 -5 -1 16.4 5.1 0 5 -1 20.4 3.1 0 5 -1 22.5 2 0 5 -1 19.2 2.8 0 -5 3 0.7 2.6 -5 3 0 2.2 2.4 -5 3 0 2.8 2.3 -5 -3 0 0.5 3.2 0 -5 3 -0.5 3.8 0 -5 3 3.1 3.1 5 -3 0 0.6 2.1 5 3 0 0.1 2.9 -5 -3 0 -0.5 2.1 0 5 -3 1.8 2.5 -5 3 0 0.4 3.1 -5 -3 0 -0.5 2.7 1 -5 0 20.4 3.2 1 -5 0 18.7 2.3 5 0 -1 19.4 2.6 -5 0 1 22.7 3.2 -1 -5 0 25.9 2.8 1 -5 0 19.9 2 5 0 -1 22.8 2.9 -5 0 1 20.1 2 -5 0 1 22.2 2.3 -1 -5 0 18.2 2.7 -1 -5 0 19.6 3 1 5 0 18.9 2.4 -1 -5 0 19.1 2.6 -1 5 0 22.7 2.5 -5 0 1 24.7 3.2 -1 5 0 17.4 3.5 -1 5 0 22.5 2.3 -1 5 0 20.1 3 1 -5 0 19.8 2.4 1 5 0 22.1 2.9 1 5 0 22 3.4 5 0 -1 22.2 2.4 5 0 -1 17.6 3.3 1 -5 0 21.1 2.7 -5 2 1 219.48 19.7 1 -5 2 235.58 20.7 5 2 -1 249.78 19.3 5 2 -1 253.87 18.7 1 -5 2 235.98 18.9 5 2 -1 216.78 19.3 -5 2 1 223.68 21.3 5 2 -1 232.48 19.1 1 5 -2 254.37 19.3 1 5 -2 254.77 19.5 1 -5 2 243.78 20 -5 2 1 204.28 18.6 1 5 -2 239.88 19.3 1 5 -2 238.08 19 5 -2 -1 236.18 17.5 5 -2 -1 228.18 18.9 -1 5 -2 260.27 23.1 -5 -2 1 248.78 20.5 -1 -5 2 245.38 18.1 -1 5 -2 252.67 20.4 -1 -5 2 231.68 19.4 -5 -2 1 249.18 19.1 5 -2 -1 240.58 18.8 -5 2 -1 249.18 19.6 5 -2 -1 251.67 19.4 -1 -5 2 257.87 19.4 5 -2 -1 254.97 20.4 -1 5 -2 265.27 19.5 5 -2 -1 255.17 20.7 -1 5 -2 252.17 19.3 -1 5 -2 266.57 20.8 -5 -2 1 245.48 19.7 5 4 -1 118.29 9.9 -5 4 1 109.59 9.8 1 5 -4 131.09 10 -5 4 1 120.49 9.3 4 1 -5 120.59 10.9 -5 4 1 120.39 10.3 5 4 -1 124.59 10.1 -5 4 1 117.89 11 5 -4 1 113.19 10.8 -5 4 1 118.19 9.3 -5 4 1 128.69 11.1 5 4 -1 118.49 9.9 5 -4 1 128.09 10.1 -5 -4 1 115.59 10.6 -5 -4 1 116.79 9.8 -1 -5 4 115.79 11.4 -4 -1 5 117.99 10.3 5 -4 -1 100.09 9.5 -5 -4 1 113.89 10.6 -1 5 -4 108.59 13.5 5 -4 -1 104.69 9.5 -5 -4 1 123.29 10.1 -4 -1 5 121.79 9.6 -5 4 -1 132.49 12.7 -5 -4 1 133.99 12.4 -5 4 -1 103.79 10.1 -5 4 -1 97.09 10.2 -1 -5 4 123.69 9.9 5 -4 -1 110.89 10.2 5 -4 -1 115.89 9.5 -2 5 1 234.38 20.3 -2 5 1 211.48 18.6 -5 1 2 222.08 21.1 2 5 -1 219.38 19.1 -5 1 2 222.28 18.1 5 1 -2 273.77 19.3 -2 5 1 196.58 18.7 2 5 -1 217.18 18.4 2 5 -1 238.08 18.8 2 -5 1 236.08 18.9 -2 5 1 216.08 18.8 5 1 -2 237.18 18.3 5 1 -2 243.88 18.4 -2 -5 -1 229.88 19.6 -5 1 2 230.38 19.8 5 1 -2 229.78 18.7 2 5 -1 217.88 18.4 5 1 -2 220.78 18.5 5 1 -2 227.58 18.6 2 5 -1 218.48 19.3 -5 1 2 231.78 19.1 -5 1 2 243.38 22.7 -5 1 2 206.08 19 5 1 -2 234.38 19.5 5 1 -2 241.78 19.3 2 -5 1 234.48 18.5 -2 -5 1 257.37 21.4 -5 -1 2 269.07 18.7 -2 -5 1 237.28 18.7 -2 -5 1 277.27 19.8 -2 5 -1 225.08 18.8 -5 -1 2 237.58 19.7 2 -5 -1 249.97 17.9 -2 5 -1 243.78 20.3 -5 -1 2 257.27 19.5 5 -1 -2 241.38 18.5 -2 5 -1 236.08 18.8 -2 -5 1 254.77 19.3 5 -1 -2 247.88 19.1 2 -5 -1 201.98 17.4 -2 5 -1 250.47 18.8 5 -1 -2 230.78 19.6 -5 -1 2 237.78 18.8 5 -1 -2 236.88 20.1 2 -5 -1 224.88 18.8 -2 5 -1 240.38 20.8 -2 -5 1 241.38 18.8 -2 5 -1 240.88 19.8 5 -1 -2 248.98 18.8 5 -1 -2 234.48 19.9 2 -5 -1 221.88 21.6 2 -5 3 40.7 4.7 2 5 -3 41 4.8 2 5 -3 44.1 4.5 -5 3 2 34.2 5.7 2 -5 3 46.8 4.4 -5 3 2 35.8 4.7 2 -5 3 44.2 5.7 5 3 -2 37 4.7 5 3 -2 43.5 5.4 5 3 -2 40 4.9 5 3 -2 45.3 4.4 -5 -3 2 41.3 4.6 -5 -3 2 45.5 5.6 -5 -3 2 47.5 7.1 -2 -5 3 41.3 4.9 -2 5 -3 52.89 7.5 -5 -3 2 43.9 4.1 -5 -3 2 39.7 4.9 -2 -5 3 45.1 5.5 -2 5 -3 43.5 4.8 -2 -5 3 49 6.1 -3 -2 5 55.49 8.2 5 -3 -2 42.9 4.6 -2 -5 3 44.9 4.6 5 -3 -2 42 5.5 -5 -3 2 44.3 4.7 5 -3 -2 43.5 4 5 -3 -2 38.8 4.6 -3 5 0 0.9 2.3 5 0 -3 1.4 3.1 5 0 -3 3.6 3 -3 5 0 1.6 1.7 3 -5 0 0.3 2.9 -5 0 3 1.1 2 -3 -5 0 1.1 3 3 -5 0 -0.7 1.3 -5 0 3 3.9 3.6 -3 -5 0 1.2 2.7 -5 0 3 0.4 4.7 3 -5 0 1.6 1.4 -3 -5 0 0.1 2.4 3 5 0 -0.1 2.9 -3 5 0 -0.7 2.3 -5 0 3 0.7 4.1 -3 -5 0 -0.5 2.7 5 0 -3 -0.6 3 -3 5 0 2.6 3.5 3 5 0 -0.9 2.8 -5 0 3 1.6 3 -3 5 0 1 2.8 3 -5 0 0.5 1.2 -5 0 3 2.8 2.6 -3 5 0 1.2 4 5 0 -3 2.5 2.4 3 5 -2 39.3 4.2 3 5 -2 34.3 4.7 5 2 -3 38.1 4.5 -5 2 3 39.1 4.8 3 -5 2 39.2 5.2 5 2 -3 43.8 4.1 3 5 -2 42.3 4.6 5 2 -3 36.4 5.2 3 -5 2 41.4 4 3 5 -2 34.8 4.6 -5 2 3 30.4 5.5 3 5 -2 42.9 5.1 3 5 -2 35.4 4.3 3 -5 2 36.5 4.7 -5 2 3 46.4 3.6 -5 2 3 32.1 5.1 -3 5 2 40.3 4.1 3 5 -2 47.6 4.4 -5 2 3 37.9 5.7 5 2 -3 37.1 5.2 -5 2 3 36 3.6 -3 5 2 40 4.7 -5 2 3 35.6 6.3 3 -5 -2 41.7 4.9 3 -5 -2 36.8 4.3 -5 -2 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34.4 5.7 -6 8 4 46 7.7 8 -4 -6 29.6 8.5 -6 -8 4 36.9 10.2 8 -4 -6 34.5 9.3 -8 -4 6 35.1 7.6 -6 8 -4 -2.5 12.9 -6 -8 4 33.5 5.7 -8 -4 6 28.5 6 -6 -8 4 31.9 7.4 -8 -4 6 39.2 5.6 8 6 -6 48.7 7.2 8 6 -6 39.3 8.1 8 6 -6 63.69 9 6 8 -6 66.59 7.9 6 8 -6 53.79 8 8 6 -6 40.1 8 6 8 -6 57.19 9.1 -6 8 6 35.9 7.5 6 8 -6 51.89 8.2 8 6 -6 35.6 7.8 6 8 -6 52.19 7.9 -8 6 6 51.99 11.8 6 6 -8 44 8.7 8 6 -6 42.2 7.9 -8 6 6 55.39 10.2 -8 -6 6 33.2 7.6 -8 -6 6 42.8 8.1 -6 -6 8 50.49 7.9 -6 -6 8 48.8 12 -8 -6 6 49 6 -6 -8 6 39.5 8.2 -6 -6 8 50.39 8.8 -8 -6 6 42 6.2 -7 8 1 87.19 13.2 -7 8 1 96.69 8.7 8 1 -7 89.99 11.8 -8 1 7 104.09 11 8 1 -7 107.49 10 7 -8 1 87.49 7.8 -8 1 7 89.79 9.2 7 -8 1 98.59 11.1 8 1 -7 113.29 13.3 -7 8 1 93.69 8.8 -7 8 1 93.39 12.1 -8 1 7 96.19 13.7 7 8 -1 106.09 9.7 7 -8 1 107.09 10.1 7 8 -1 100.89 10 7 8 -1 125.69 12.2 7 8 -1 92.89 10.4 -8 1 7 111.59 10.8 8 1 -7 117.89 11.2 -7 8 1 87.39 10 -7 8 -1 96.49 10 -7 -8 1 99.89 11.1 -7 -8 1 99.69 14.1 -7 8 -1 90.09 8.1 -7 8 -1 117.69 12.3 7 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8.6 -3 15 -4 6.9 12.4 -15 -4 3 19 16.2 15 -4 -3 0.4 11.6 -3 15 -4 25.4 10.6 3 -15 6 33.1 8.6 15 6 -3 21.9 13.2 -15 6 3 1.3 13 3 15 -6 46.5 11.5 -15 6 3 -2.5 13.5 3 15 -6 21 10.2 -15 6 3 2.1 14.7 3 15 -6 47.5 9.4 15 6 -3 34.1 12.6 -15 6 3 22.4 15.4 3 15 -6 13.2 13.2 3 15 -6 38.1 12 -15 -6 3 2.7 17.6 15 -6 -3 12.7 12.7 -3 -15 6 29.8 9.6 -15 -6 3 13.7 10.6 -3 15 -6 21.9 10.7 15 -6 -3 5.6 12.9 -3 -15 6 6.8 8.9 15 -6 -3 1.6 10.9 -3 15 -6 12 9.5 4 -15 1 13.9 12.9 15 1 -4 2.5 10.9 15 1 -4 -1.1 10.7 -4 15 1 12 7.5 4 15 -1 5.3 9.5 15 1 -4 11.6 10.5 -15 1 4 -1.4 10.3 4 15 -1 -10.1 14 -15 1 4 1.5 13 -15 1 4 10.3 14.6 -4 15 1 -15.7 10.2 -15 1 4 -4.6 10.4 4 -15 1 9.9 8.9 -15 -1 4 9.3 9.7 -4 -15 1 -1.2 9.7 15 -1 -4 1.7 10.6 -4 15 -1 -2 6.8 4 -15 -1 2.3 15.7 -4 -15 1 -15.5 17.2 -4 15 -1 15.8 9.4 -4 -15 1 6.8 11.3 -15 -1 4 26.2 14.7 -15 -1 4 -14.3 11 4 -15 -1 0.7 10.9 -4 15 -1 18 9.9 15 -1 -4 5 11.5 4 15 1 23.6 13.2 4 15 -3 12 10.2 15 3 -4 25 11 4 15 -3 3.2 9.6 -15 3 4 14 13.4 4 -15 3 16.7 9 -15 3 4 22.1 15.4 15 3 -4 11.8 11 -15 3 4 19.6 12.1 4 15 -3 10.4 11.7 4 15 -3 28.5 10.6 4 -15 3 9 12.1 15 3 -4 19.9 10.7 -15 3 4 21.1 10.2 15 -3 -4 25.3 10.7 -4 -15 3 17.6 13 -4 15 -3 19.8 9.7 -15 -3 4 31 9.1 15 -3 -4 1.7 10.4 -4 15 -3 24.1 13 -15 -3 4 14.8 10.5 -4 15 -3 11.5 9.1 -4 -15 3 5.3 8.5 -15 -3 4 4.1 10.5 -15 -3 4 -2.4 16 4 -15 -3 -33.8 21.6 -4 15 -3 18.6 8.2 -4 -15 3 9.5 9.3 -15 5 4 -1.3 10 4 15 -5 29.3 12.1 4 -15 5 14.4 12.5 4 15 -5 4.3 10.8 -15 5 4 11.2 14 15 5 -4 3.9 11.1 4 15 -5 5.9 10.5 15 5 -4 1.8 11.1 4 15 -5 -2.3 9.6 4 15 -5 12.7 8.6 4 -15 5 8.8 9.3 -15 5 4 4.1 14.7 -15 5 4 20.9 14.5 -4 -15 5 15.9 9.4 -4 15 -5 1.8 8.9 -4 15 -5 5.5 11.7 -4 -15 5 28.3 12.8 15 -5 -4 22.5 10.4 15 -5 -4 -0.4 11.5 -4 -15 5 4.2 9 -15 -5 4 6.8 10.1 -4 15 -5 14.8 9.5 -4 15 -5 19.1 11.4 15 -5 -4 15.4 12.2 -5 15 0 33.8 9.6 -15 0 5 35.6 9.7 15 0 -5 43.3 12 -15 0 5 29.2 13.7 5 15 0 50.49 13.7 5 -15 0 35 14.8 -15 0 5 42.8 11.9 15 0 -5 19.2 11.4 -15 0 5 32.6 16.7 15 0 -5 33 10.1 15 0 -5 52.19 10.5 5 -15 0 38.6 10 -5 15 0 38.5 8.6 15 2 -5 28.2 10.3 5 15 -2 29.4 9.9 5 -15 2 35.1 13.6 -15 2 5 19.6 15.4 15 2 -5 32 11.6 15 2 -5 38.8 12.4 -15 2 5 59.59 12 5 15 -2 42.4 11.3 5 -15 2 38.8 9.1 -15 2 5 33.1 11.7 5 15 -2 45.4 10.8 -5 15 2 34.3 10 5 15 -2 48.9 14.6 -15 2 5 40.2 13.9 -15 -2 5 22.9 17 -15 -2 5 30.6 12 15 -2 -5 29.1 11.8 -5 15 -2 45.1 10.4 -5 15 -2 22.5 9.7 15 -2 -5 40.7 10.8 -15 -2 5 43.1 10.9 15 -2 -5 40.8 11.8 5 -15 -2 16.7 20.1 -5 -15 2 -1.7 15.3 -5 -15 2 35 11.6 -5 -15 2 30 10.3 -15 -2 5 21.9 9.3 15 -2 -5 25.7 9.8 -15 4 5 5.2 10.6 -15 4 5 2 13.6 15 4 -5 32 11 15 4 -5 13 9.5 -15 4 5 14.1 11.7 5 15 -4 7.4 8.3 5 15 -4 22.9 12.2 5 -15 4 -5.9 12.5 5 15 -4 9.9 10.3 15 4 -5 23.8 11.6 15 4 -5 0.4 11.6 -15 4 5 13.6 16.1 15 4 -5 11.3 11.8 5 -15 4 22 8.8 5 -15 4 -0.3 8.4 5 15 -4 12.9 11.3 5 15 -4 8.7 10.5 -5 -15 4 23.6 9.8 -5 15 -4 7.3 8.3 -15 -4 5 4.9 9.8 -5 15 -4 15.6 9 -5 15 -4 3.7 12.5 -15 -4 5 9 11.5 -5 -15 4 17.2 13.6 15 -4 -5 12.5 11.3 15 -4 -5 0.4 11.4 15 -4 -5 11.8 13.6 -15 -4 5 -3.9 16.6 -5 -15 4 16.4 10.4 -5 15 -4 12.3 10.5 15 -4 -5 -0.4 10.3 -5 15 -4 -17.1 13.8 -15 1 6 22.4 10.6 -6 15 1 13 9.5 -15 1 6 20.2 16.9 6 -15 1 19.2 8 6 -15 1 27.8 13.6 15 1 -6 -2.3 9.6 -15 1 6 24.9 12.1 6 15 -1 17.7 9.9 6 15 -1 34.8 13.8 -6 15 1 20.7 8 -15 1 6 7.9 12.4 15 1 -6 30.8 11.5 15 1 -6 9.4 10 15 1 -6 26.4 11.9 15 -1 -6 15.8 12 -15 -1 6 3.9 11.1 15 -1 -6 8.6 10.4 -6 -15 1 18.9 11.8 -15 -1 6 16.6 11.3 15 -1 -6 27 11.4 -15 -1 6 28.8 8.4 6 -15 -1 21.7 16.5 -15 -1 6 23 17 -6 15 -1 19.7 9.5 15 -1 -6 41.5 11.2 -6 15 -1 29.8 9.8 -15 -1 6 13 8.9 6 -15 -1 19 10.5 -15 3 6 16.4 13.8 6 15 -3 20.3 9.5 15 3 -6 23.1 11.1 6 -15 3 21.4 10.2 -6 15 3 31.9 9 6 -15 3 42.8 12.1 6 15 -3 11.5 11.6 15 3 -6 18.2 10.1 6 15 -3 14.3 10.7 15 3 -6 38.5 12.4 6 15 -3 27.8 11.2 -15 3 6 37.9 12 -15 3 6 14.7 11.5 6 -15 3 10.8 9.4 -15 3 6 19.3 16.2 15 3 -6 30.7 11 15 -3 -6 -16 21.5 -15 -3 6 18.4 18 -6 15 -3 13.4 10.2 15 -3 -6 32.3 12.5 -6 15 -3 1 13.4 6 -15 -3 5.1 28.4 -15 -3 6 28.6 11.5 -15 -3 6 33.3 9.1 -6 15 -3 2.2 12.1 -15 -3 6 17.4 12.2 15 -3 -6 29.8 11.8 -6 -15 3 24.3 9.9 -6 -15 3 -3.8 14.8 -6 -15 3 31.3 11.5 -6 15 -3 8.1 9.1 15 0 -7 19.2 11 15 0 -7 13.1 11.3 15 0 -7 7.1 12.2 -15 0 7 13.4 12.6 -15 0 7 -5.7 12.9 7 -15 0 17 9.1 7 -15 0 2.3 13.4 15 0 -7 23.1 11.6 7 15 0 0.8 12.8 -15 0 7 -1.6 10.4 -7 15 0 2.9 8.3 -7 15 0 7.8 10.4 -15 2 7 53.19 16.5 15 2 -7 31.6 11.6 7 15 -2 52.19 10.6 7 15 -2 50.29 12.9 7 -15 2 43.4 13.9 15 2 -7 60.79 13.9 -7 15 2 63.19 11.7 15 2 -7 34.4 11.5 7 -15 2 50.79 9.7 15 2 -7 42.7 12.7 7 15 -2 60.99 15.7 7 -15 2 37 12 -15 2 7 41.2 14.2 7 15 -2 63.39 12.4 -15 -2 7 27.5 13.6 -7 -15 2 32.3 12.1 15 -2 -7 53.29 13.6 7 -15 -2 41.1 24.1 15 -2 -7 53.49 13.1 -7 15 -2 29.2 10.8 -7 15 -2 45.6 11.1 -15 -2 7 71.69 19.4 -7 15 -2 53.49 15 -15 -2 7 51.29 10.6 15 -2 -7 69.29 13.5 15 -2 -7 41.6 13.5 -15 -2 7 55.69 12.8 0 16 0 212.28 20.8 0 -16 0 118.99 25.2 0 16 0 134.59 16.3 0 -16 0 168.48 20.1 0 16 -2 27.1 11.3 0 -16 2 27.8 15.4 0 16 -2 19.1 11.3 0 16 -2 22.9 9.9 0 -16 2 34.7 9.2 0 -16 2 29.2 10.1 -16 4 0 96.29 19.1 0 -16 4 113.29 13.2 0 16 -4 94.39 14.3 0 16 -4 124.49 16.2 0 16 -4 105.09 14.6 0 -16 4 115.39 18.5 0 -16 4 131.29 14.4 0 16 -4 125.99 18 1 -16 1 38.1 11 -1 16 1 59.59 14.7 1 -16 1 29.2 10.4 -16 1 1 51.49 15.7 16 1 -1 45 16.5 1 16 -1 42.7 10.3 -16 1 1 58.89 20.3 1 -16 1 31.9 16.4 1 16 -1 45 11 1 16 -1 30.1 12.7 -16 -1 1 3.2 21.1 1 -16 -1 30 21.4 -1 -16 1 31.3 11.1 -1 16 -1 29.1 9.4 -1 16 -1 52.69 10.8 -1 -16 1 50.99 12.2 1 -16 -1 42.5 15.4 -1 16 -1 32.7 11.7 -16 -1 1 20.1 16.1 16 -1 -1 53.09 13.3 1 -16 3 33.2 9 1 -16 3 33.8 10.1 1 16 -3 53.99 11.5 1 16 -3 9.3 10.4 1 16 -3 35.4 13.5 -16 3 1 17.6 16.3 16 3 -1 46.2 17.2 -16 3 1 43.3 19.7 1 -16 3 39.5 15.1 1 16 -3 33.7 11.1 -1 16 -3 25.4 10.4 -1 16 -3 43.9 12.2 -1 -16 3 31.9 9.5 -16 -3 1 12.9 15.8 -1 -16 3 38.4 9.4 16 -3 -1 25.8 12.7 -16 -3 1 0.6 20.9 -1 16 -3 24.6 10.4 -16 0 2 24.2 12.6 -2 -16 0 -16.3 30.6 -16 0 2 50.79 18.5 2 16 0 30.3 12 -16 0 2 42 12.3 2 -16 0 16.5 12.1 -2 16 0 39.4 10.3 16 0 -2 26.3 13.3 2 16 0 49.99 13.4 -2 -16 0 62.09 14.9 2 -16 0 30.1 17.2 -2 16 0 35.9 12.4 16 0 -2 38.3 11.3 2 16 0 23.9 10.5 16 2 -2 38.9 13.7 2 -16 2 23 14.6 2 16 -2 14.5 10.7 -16 2 2 31.2 17 -16 2 2 46 14.4 2 16 -2 22 10.9 16 2 -2 31.5 12.6 2 16 -2 22.9 10.9 -16 2 2 14.5 9.6 2 -16 2 23.9 9.1 -16 2 2 60.99 13.4 -2 -16 2 43.1 10.8 -16 -2 2 54.89 20.1 -16 -2 2 38.2 11.9 16 -2 -2 30.5 13.1 -2 16 -2 35.1 10.8 -2 16 -2 26.8 9.5 -2 -16 2 26.1 9.5 -2 16 -2 24.3 11.4 -2 -16 2 39.5 16.1 -16 -2 2 38.9 13 2 16 2 1.2 8.9 2 -16 -2 6.7 22.4 2 16 -4 11.6 11.1 2 -16 4 0.9 9.2 -16 4 2 19.2 12.9 2 16 -4 10.8 14 2 16 -4 2.5 10.9 16 4 -2 12.4 13.1 -16 4 2 30.9 16.4 -16 4 2 9.6 15.5 2 -16 4 24 15 -16 4 2 19.6 17.1 2 -16 4 9.3 7.5 -2 16 -4 22.9 12.1 -2 16 -4 20.2 10 -2 16 -4 23.4 14.9 -2 -16 4 20.9 14.6 16 -4 -2 14.4 11.2 16 -4 -2 0.4 12.4 -2 16 -4 11.7 10.7 -2 -16 4 8.6 8.9 -16 -4 2 17.1 12.2 -16 -4 2 7.9 19.6 -16 -4 2 13 13.1 3 -16 1 31.6 10.8 -16 1 3 42 16.5 16 1 -3 29.1 11 16 1 -3 27.6 12.9 3 16 -1 35.9 10.7 -16 1 3 47 12.3 3 16 -1 35.6 12.8 -3 16 1 41.4 12.7 -16 1 3 51.69 11.4 3 -16 1 57.49 15.1 -16 1 3 41.2 13.3 -3 16 -1 32.4 10.8 -3 16 -1 25.3 10.8 -3 -16 1 16.2 19.7 3 -16 -1 6.4 18.4 -16 -1 3 51.39 12.3 -3 -16 1 20 12.6 3 16 1 52.59 14.4 -16 -1 3 21.6 16.8 -3 16 -1 34.4 8.5 16 -1 -3 55.59 13.3 -16 -1 3 38.7 11.4 16 -1 -3 33.8 12.3 -16 -1 3 27.3 12.2 3 -16 -1 49.99 14.5 16 -1 -3 37.3 10.5 -16 3 3 21.1 15.5 -16 3 3 20.2 13.2 16 3 -3 22.5 12.7 -16 3 3 11.1 16.5 3 -16 3 19 9.1 -16 3 3 11.6 11.1 16 3 -3 17.4 13.2 3 -16 3 5.8 13.5 3 16 -3 16.7 13.9 3 16 -3 17.7 11.5 -3 16 -3 0.9 13.9 -3 -16 3 36.9 14.7 -16 -3 3 25.6 11.4 -3 16 -3 -5.3 10.2 -3 16 -3 1.8 11.4 -16 -3 3 13.2 17.2 -16 -3 3 16.4 11.3 -3 16 -3 4.4 9.5 16 -3 -3 15.7 11.1 -3 -16 3 18.9 9.3 4 -16 0 85.29 19.7 -16 0 4 96.79 15 -16 0 4 89.99 19.6 4 -16 0 114.49 15.7 -4 16 0 139.49 14.3 16 0 -4 121.49 14.4 -16 0 4 109.89 15.5 16 0 -4 95.29 16 16 0 -4 111.19 17.1 -4 16 0 88.09 14.7 4 16 0 163.68 19.8 4 -16 2 11.3 14.6 -16 2 4 19.7 11.2 -16 2 4 34.8 15.3 16 2 -4 18.5 12.3 4 -16 2 0.5 9.4 -16 2 4 16.2 16.7 16 2 -4 12.6 11.8 -16 2 4 27.2 12.9 4 16 -2 22.4 11.4 -4 16 2 19 10.5 16 2 -4 1.3 11.1 4 -16 -2 29.2 22.4 -16 -2 4 12.3 10.3 -4 16 -2 1.8 11.2 -4 -16 2 18.4 11.6 -4 -16 2 7.6 10.7 -16 -2 4 12.5 11.3 -4 -16 2 12.8 17.3 16 -2 -4 7.4 10.8 -16 -2 4 11.2 17.4 16 -2 -4 1.7 11.4 -4 16 -2 7.1 10.2 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 110.7(3) . 46 ? N1 Co1 N1 110.7(3) 46 3_655 ? N1 Co1 N1 107.1(6) . 3_655 ? N1 Co1 N1 110.7(3) . 48_554 ? N1 Co1 N1 107.1(6) 46 48_554 ? N1 Co1 N1 110.7(3) 48_554 3_655 ? C2 N1 Co1 126.8(6) . . ? C2 N1 C1 106.0(9) . . ? C1 N1 Co1 126.7(7) . . ? N1 C2 N1 112.9(11) 14_665 . ? N1 C2 C3 123.5(5) 14_665 . ? N1 C2 C3 123.5(5) . . ? N1 C1 C1 107.5(7) . 14_665 ? N1 C1 H1 126.2 . . ? C1 C1 H1 126.2 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 . . ? N4 N5 N4 174(9) 2_665 . ? N2 N3 N3 0.000(3) . 3_655 ? N12 N11 N12 103(10) . 6_665 ? N12 N11 N12 103(10) 12_654 6_665 ? N12 N11 N10 53(7) . 12_654 ? N12 N11 N10 128(10) 6_665 6_665 ? N12 N11 N10 53(7) 12_654 6_665 ? N12 N11 N10 128(10) 12_654 12_654 ? N12 N11 N10 53(7) 6_665 12_654 ? N12 N11 N10 53(7) . 6_665 ? N10 N11 N10 102(10) 12_654 . ? N10 N11 N10 102(10) 6_665 . ? N10 N11 N10 102(10) 12_654 6_665 ? N11 N12 N12 39(10) . 12_654 ? N11 N12 N12 39(10) . 6_665 ? N12 N12 N12 60.00(4) 12_654 6_665 ? N15 N13 N15 114(9) 6_665 . ? N15 N13 N15 114(9) 12_654 . ? N15 N13 N15 114(9) 6_665 12_654 ? N11 N10 N10 39(7) . 12_654 ? N11 N10 N10 151(10) . 2_665 ? N11 N10 N10 39(7) . 6_665 ? N10 N10 N10 119.998(16) 6_665 2_665 ? N10 N10 N10 59.998(15) 12_654 6_665 ? N10 N10 N10 119.998(13) 12_654 2_665 ? N13 N15 N15 33(5) . 6_665 ? N13 N15 N15 33(5) . 12_654 ? N15 N15 N15 59.999(12) 6_665 12_654 ? N3 N2 N3 180.0 3_655 . ? 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 1.969(9) . ? Co1 N1 1.969(9) 48_554 ? Co1 N1 1.969(9) 46 ? Co1 N1 1.969(9) 3_655 ? N1 C2 1.330(9) . ? N1 C1 1.382(10) . ? C2 C3 1.52(2) . ? C1 C1 1.38(3) 14_665 ? C1 H1 1.0770 . ? C3 H3A 1.0830 . ? C3 H3B 1.0830 . ? C3 H3C 1.0830 . ? N5 N4 1.03(3) 2_665 ? N5 N4 1.03(3) . ? N8 N9 0.96(2) . ? N3 N3 1.30(6) 3_655 ? N3 N2 0.65(3) . ? N11 N12 0.64(16) . ? N11 N12 0.64(16) 12_654 ? N11 N12 0.64(16) 6_665 ? N11 N10 1.1(2) 6_665 ? N11 N10 1.1(2) . ? N11 N10 1.1(2) 12_654 ? N12 N12 1.0(3) 12_654 ? N12 N12 1.0(3) 6_665 ? N13 N15 0.87(11) 6_665 ? N13 N15 0.87(11) 12_654 ? N13 N15 0.87(11) . ? N10 N10 1.8(3) 6_665 ? N10 N10 1.9(4) 2_665 ? N10 N10 1.8(3) 12_654 ? N15 N15 1.46(19) 6_665 ? N15 N15 1.46(19) 12_654 ? 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 173.5(5) . . . 14_665 ? Co1 N1 C2 C3 -4.2(18) . . . . ? Co1 N1 C1 C1 -172.8(6) . . . 14_665 ? C2 N1 C1 C1 -1.0(9) . . . 14_665 ? C1 N1 C2 N1 1.8(16) . . . 14_665 ? C1 N1 C2 C3 -175.9(12) . . . . ? N12 N11 N12 N12 -106(51) 12_654 . . 6_665 ? N12 N11 N12 N12 106(51) 6_665 . . 12_654 ? N10 N11 N10 N10 105(23) 6_665 . . 12_654 ? N10 N11 N10 N10 53(11) 6_665 . . 2_665 ? N10 N11 N10 N10 -105(23) 12_654 . . 6_665 ? N10 N11 N10 N10 -53(11) 12_654 . . 2_665 ? N15 N13 N15 N15 -133(32) 12_654 . . 6_665 ? N15 N13 N15 N15 133(32) 6_665 . . 12_654 ?