#------------------------------------------------------------------------------ #$Date: 2021-10-01 01:16:56 +0300 (Fri, 01 Oct 2021) $ #$Revision: 269405 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564779.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_1564779 loop_ _publ_author_name 'Turner, Gemma F.' 'McKellar, Scott C.' 'Allan, David R.' 'Cheetham, Anthony K.' 'Henke, Sebastian' 'Moggach, Stephen A.' _publ_section_title ; Guest-mediated phase transitions in a flexible pillared-layered metal--organic framework under high-pressure ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03108B _journal_year 2021 _chemical_formula_moiety '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)' _chemical_formula_sum 'C34 H48 N6 O12 Zn2' _chemical_formula_weight 863.55 _space_group_IT_number 140 _space_group_name_Hall '-I 4 2c' _space_group_name_H-M_alt 'I 4/m c m' _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4 2c' _symmetry_space_group_name_H-M 'I 4/m c m' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary other _audit_creation_date 2021-05-26 _audit_creation_method CRYSTALS_ver_14.61_build_6999 _audit_update_record ; 2021-06-03 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.1100(10) _cell_length_b 15.1100(10) _cell_length_c 19.2672(12) _cell_measurement_reflns_used 4952 _cell_measurement_temperature 298 _cell_measurement_theta_max 18 _cell_measurement_theta_min 3 _cell_volume 4398.9(5) _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_pressure 100000 _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full 0.759 _diffrn_measured_fraction_theta_max 0.759 _diffrn_measurement_device Area _diffrn_measurement_device_type Synchrotron _diffrn_measurement_method \w _diffrn_radiation_monochromator 'focussing mirrors' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48590 _diffrn_reflns_av_R_equivalents 0.112 _diffrn_reflns_av_unetI/netI 0.145 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 10160 _diffrn_reflns_theta_full 17.667 _diffrn_reflns_theta_max 17.667 _diffrn_reflns_theta_min 2.184 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1800 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.79 _refine_diff_density_min -1.28 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9768 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 904 _refine_ls_number_restraints 165 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.1009 _refine_ls_shift/su_max 0.0015416 _refine_ls_shift/su_mean 0.0000748 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +59.13P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.3887 _refine_ls_wR_factor_gt 0.3645 _refine_ls_wR_factor_ref 0.1969 _reflns_limit_h_max 13 _reflns_limit_h_min 0 _reflns_limit_k_max 18 _reflns_limit_k_min 0 _reflns_limit_l_max 24 _reflns_limit_l_min 0 _reflns_number_gt 575 _reflns_number_total 935 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 1.77 _oxford_diffrn_Wilson_scale 855.88 _oxford_refine_ls_r_factor_ref 0.1087 _oxford_refine_ls_scale 0.424(2) _oxford_reflns_number_all 935 _iucr_refine_instructions_details ; # # Punched on 26/05/21 at 12:56:14 # #LIST 12 BLOCK CONT SCALE CONT ZN ( 1 ,X'S,U'S) UNTIL C ( 5 ) CONT C ( 10 ,X'S,U[ISO]) UNTIL C ( 11 ) CONT N ( 1 ,X'S,U'S) CONT N ( 10 ,X'S,U[ISO]) CONT O ( 1 ,X'S,U'S) CONT O ( 10 ,X'S,U[ISO]) RIDE C ( 3,X'S) H ( 32,X'S) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) END # # Punched on 26/05/21 at 12:56:14 # #LIST 16 PLANAR 0.01 C(4,-5,1,0,1,1) C(4) N(1) C(4,3,1,1,1) PLANAR 0.01 C(5,-8,1,0,0,1) C(5) N(1) C(5,3,1,1,1) DIST 1.499,.01= C(1) TO C(2) DIST 1.252,.01= C(1) TO O(1) DIST 1.252,.01= C(1) TO O(1,-3,1,0,0,1) DIST 1.375,.01= C(2) TO C(3) DIST 1.375,.01= C(2) TO C(3,-3,1,0,0,1) DIST 1.397,.01= C(3) TO C(3,8,2,1,1,-1) DIST 1.54,.01= C(4) TO C(4,-5,1,0,1,1) DIST 1.54,.01= C(5) TO C(5,-8,1,0,0,1) DIST 1.472,.01= C(4) TO N(1) DIST 1.459,.01= C(5) TO N(1) DIST 1.523,.01= C(10) TO N(10) DIST 1.248,.01= C(10) TO O(10) DIST 1.248,.01= C(10) TO O(10,8,2,1,1,-1) DIST 1.443,.01= C(11) TO N(10) ANGL 117,1= O(1) TO C(1) TO C(2) ANGL 117,1= O(1,-3,1,0,0,1) TO C(1) TO C(2) ANGL 125,1= O(1,-3,1,0,0,1) TO C(1) TO O(1) ANGL 120,1= C(3) TO C(2) TO C(1) ANGL 120,1= C(3,-3,1,0,0,1) TO C(2) TO C(1) ANGL 119,1= C(3,-3,1,0,0,1) TO C(2) TO C(3) ANGL 120,1= C(3,8,2,1,1,-1) TO C(3) TO C(2) ANGL 110,1= O(10) TO C(10) TO N(10) ANGL 110,1= O(10,8,2,1,1,-1) TO C(10) TO N(10) ANGL 140,1= O(10,8,2,1,1,-1) TO C(10) TO O(10) ANGL 122,1= C(11) TO N(10) TO C(10) ANGL 122,1= C(11,8,2,1,1,-1) TO N(10) TO C(10) ANGL 113,1= C(11,8,2,1,1,-1) TO N(10) TO C(11) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 2.060000 , 0.050000 = ZN(1) TO N(1) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO O(1,-3,1,0,0,1) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(1) TO O(1) VIBR .0, 0.00500 = C(2) TO O(1,-3,1,0,0,1) VIBR .0, 0.00500 = O(1) TO O(1,-3,1,0,0,1) VIBR .0, 0.00500 = O(1) TO C(2) VIBR .0, 0.00200 = C(2) TO C(3,-3,1,0,0,1) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3,-3,1,0,0,1) TO C(1) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00500 = C(3) TO C(3,-3,1,0,0,1) VIBR .0, 0.00200 = C(3) TO C(3,8,2,1,1,-1) VIBR .0, 0.00500 = C(2) TO C(3,8,2,1,1,-1) VIBR .0, 0.00200 = C(4) TO C(4,-5,1,0,1,1) VIBR .0, 0.00200 = C(4) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4,-5,1,0,1,1) VIBR .0, 0.00200 = C(5) TO C(5,-8,1,0,0,1) VIBR .0, 0.00200 = C(5) TO C(5,-5,1,0,1,1) VIBR .0, 0.00200 = C(5) TO C(5,4,1,0,1) VIBR .0, 0.00200 = C(5) TO C(5,2,1,1) VIBR .0, 0.00200 = C(5) TO N(1) VIBR .0, 0.00500 = C(5,-5,1,0,1,1) TO C(5,-8,1,0,0,1) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(5,-8,1,0,0,1) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(5,-5,1,0,1,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(5,-8,1,0,0,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(5,-5,1,0,1,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(5,4,1,0,1) VIBR .0, 0.00500 = N(1) TO C(5,-8,1,0,0,1) VIBR .0, 0.00500 = N(1) TO C(5,-5,1,0,1,1) VIBR .0, 0.00500 = N(1) TO C(5,4,1,0,1) VIBR .0, 0.00500 = N(1) TO C(5,2,1,1) VIBR .0, 0.00200 = C(10) TO O(10,8,2,1,1,-1) VIBR .0, 0.00200 = C(10) TO N(10) VIBR .0, 0.00200 = C(10) TO O(10) VIBR .0, 0.00500 = N(10) TO O(10,8,2,1,1,-1) VIBR .0, 0.00500 = O(10) TO O(10,8,2,1,1,-1) VIBR .0, 0.00500 = O(10) TO N(10) VIBR .0, 0.00200 = C(11) TO N(10) VIBR .0, 0.00500 = C(4,2,1,1) TO C(4) VIBR .0, 0.00500 = C(4,3,1,1,1) TO C(4) VIBR .0, 0.00500 = C(4,3,1,1,1) TO C(4,2,1,1) VIBR .0, 0.00500 = C(4,4,1,0,1) TO C(4) VIBR .0, 0.00500 = C(4,4,1,0,1) TO C(4,2,1,1) VIBR .0, 0.00500 = C(4,4,1,0,1) TO C(4,3,1,1,1) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(4) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(4,2,1,1) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(4,3,1,1,1) VIBR .0, 0.00500 = C(5,4,1,0,1) TO C(4,4,1,0,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(4) VIBR .0, 0.00500 = C(5,2,1,1) TO C(4,2,1,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(4,3,1,1,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(4,4,1,0,1) VIBR .0, 0.00500 = C(5,2,1,1) TO C(5,4,1,0,1) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(4) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(4,2,1,1) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(4,3,1,1,1) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(4,4,1,0,1) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(5,4,1,0,1) VIBR .0, 0.00500 = C(5,3,1,1,1) TO C(5,2,1,1) VIBR .0, 0.00500 = C(5) TO C(4) VIBR .0, 0.00500 = C(5) TO C(4,2,1,1) VIBR .0, 0.00500 = C(5) TO C(4,3,1,1,1) VIBR .0, 0.00500 = C(5) TO C(4,4,1,0,1) VIBR .0, 0.00500 = C(5) TO C(5,4,1,0,1) VIBR .0, 0.00500 = C(5) TO C(5,2,1,1) VIBR .0, 0.00500 = C(5) TO C(5,3,1,1,1) VIBR .0, 0.00500 = C(11,8,2,1,1,-1) TO C(10) VIBR .0, 0.00500 = C(11) TO C(10) VIBR .0, 0.00500 = C(11) TO C(11,8,2,1,1,-1) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = C(1) TO O(1,-3,1,0,0,1) U(IJ) .0, 0.04000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(1) TO O(1) U(IJ) .0, 0.04000 = C(2) TO C(3,-3,1,0,0,1) U(IJ) .0, 0.04000 = C(2) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(3,8,2,1,1,-1) U(IJ) .0, 0.04000 = C(4) TO C(4,-5,1,0,1,1) U(IJ) .0, 0.04000 = C(4) TO N(1) U(IJ) .0, 0.04000 = C(5) TO C(5,-8,1,0,0,1) U(IJ) .0, 0.04000 = C(5) TO C(5,-5,1,0,1,1) U(IJ) .0, 0.04000 = C(5) TO C(5,4,1,0,1) U(IJ) .0, 0.04000 = C(5) TO C(5,2,1,1) U(IJ) .0, 0.04000 = C(5) TO N(1) U(IJ) .0, 0.04000 = C(10) TO O(10,8,2,1,1,-1) U(IJ) .0, 0.04000 = C(10) TO N(10) U(IJ) .0, 0.04000 = C(10) TO O(10) U(IJ) .0, 0.04000 = C(11) TO N(10) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; _cod_data_source_file d1sc03108b2.cif _cod_data_source_block 2_DMF_010GPa _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 4398.9(6) _cod_original_sg_symbol_Hall '-I 4 2c ' _cod_original_sg_symbol_H-M 'I 4/m c m ' _cod_database_code 1564779 _oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I) _iucr_refine_reflections_details ; # Data was input as F-squared # punching LIST 6 as LIST 6 with all keys set # NBGNXT= 36 #LIST 6 READ NCOEF= 8 TYPE=FIX, F'S = FSQ UNIT=DATA, CHECK=NO L30=NO ARCH=NO STORE NCOEF= 6 OUTPUT INDICES /FO/ SIGMA(/FO/) RATIO/JCODE CORRECTIONS SERIAL CONT INPUT H K L /FO/ SIGMA(/FO/) JCODE CONT CORRECTIONS SERIAL FOR (I4,I4,I4,F10.2,F8.2,F4.0,F7.4,F7.0) END 3 -3 0 2385.43 126.60 0. 1.0000 0. -3 3 0 2564.35 129.06 0. 1.0000 0. 3 -3 0 2293.04 129.06 0. 1.0000 0. -3 3 0 1901.87 125.75 0. 1.0000 0. 3 -3 0 2205.21 127.69 0. 1.0000 0. -4 4 0 1889.16 109.64 0. 1.0000 0. 4 -4 0 1983.26 110.80 0. 1.0000 0. 4 -4 0 1869.77 112.20 0. 1.0000 0. 4 -4 0 1873.26 118.00 0. 1.0000 0. 5 -1 0 523.81 42.61 0. 1.0000 0. 5 -1 0 567.58 47.78 0. 1.0000 0. 5 -1 0 529.66 41.64 0. 1.0000 0. 5 -3 0 4617.86 263.63 0. 1.0000 0. 3 -5 0 4661.55 261.40 0. 1.0000 0. 3 -5 0 4885.35 258.50 0. 1.0000 0. 5 -3 0 4675.32 260.22 0. 1.0000 0. 6 -2 0 4762.94 280.62 0. 1.0000 0. 6 -2 0 5422.93 278.86 0. 1.0000 0. -6 2 0 5069.19 279.07 0. 1.0000 0. 6 -6 0 1256.45 105.54 0. 1.0000 0. -6 6 0 1287.12 88.69 0. 1.0000 0. -6 6 0 1291.07 99.80 0. 1.0000 0. 6 -6 0 1142.85 103.50 0. 1.0000 0. 7 -1 0 5293.52 286.93 0. 1.0000 0. 7 -1 0 5093.90 289.87 0. 1.0000 0. 5 -7 0 7004.80 384.26 0. 1.0000 0. -7 5 0 7124.06 385.09 0. 1.0000 0. 7 -5 0 6900.10 391.91 0. 1.0000 0. -7 7 0 716.24 93.55 0. 1.0000 0. -7 7 0 726.22 77.18 0. 1.0000 0. 7 -7 0 774.40 94.93 0. 1.0000 0. 7 -7 0 697.49 70.79 0. 1.0000 0. 4 -8 0 6044.30 330.36 0. 1.0000 0. -8 4 0 5821.34 332.05 0. 1.0000 0. 8 -4 0 6072.69 339.02 0. 1.0000 0. -8 4 0 6025.85 331.07 0. 1.0000 0. 8 -4 0 5812.71 327.82 0. 1.0000 0. -8 6 0 4671.36 255.90 0. 1.0000 0. 8 -6 0 4469.12 263.17 0. 1.0000 0. 6 -8 0 4037.33 263.56 0. 1.0000 0. -8 6 0 4340.25 256.37 0. 1.0000 0. 8 -6 0 4439.10 260.50 0. 1.0000 0. 6 -8 0 4723.02 260.48 0. 1.0000 0. -8 8 0 1016.73 111.42 0. 1.0000 0. 8 -8 0 1048.60 109.31 0. 1.0000 0. 8 -8 0 952.25 113.63 0. 1.0000 0. -8 8 0 703.54 85.24 0. 1.0000 0. 9 -1 0 4477.65 258.16 0. 1.0000 0. 9 -3 0 5234.99 307.51 0. 1.0000 0. -9 3 0 5399.00 300.66 0. 1.0000 0. 9 -3 0 5255.18 295.44 0. 1.0000 0. 5 -9 0 5090.47 300.05 0. 1.0000 0. 9 -5 0 5155.51 297.10 0. 1.0000 0. 9 -5 0 5228.77 303.38 0. 1.0000 0. -9 5 0 5649.62 301.82 0. 1.0000 0. -9 5 0 5225.43 299.58 0. 1.0000 0. 7 -9 0 1634.44 139.45 0. 1.0000 0. -9 7 0 1294.56 121.65 0. 1.0000 0. 7 -9 0 1563.19 132.86 0. 1.0000 0. -9 7 0 1340.65 137.95 0. 1.0000 0. 9 -7 0 1510.39 138.04 0. 1.0000 0. 9 -7 0 1712.77 135.95 0. 1.0000 0. -9 9 0 988.13 138.11 0. 1.0000 0. -9 9 0 1058.26 102.34 0. 1.0000 0. 9 -9 0 1204.35 121.75 0. 1.0000 0. 9 -9 0 1220.45 143.76 0. 1.0000 0. 10 -2 0 5553.97 313.89 0. 1.0000 0. 10 -4 0 4836.61 282.28 0. 1.0000 0. 10 -4 0 4635.33 273.18 0. 1.0000 0. -10 4 0 4663.08 274.96 0. 1.0000 0. -10 4 0 5079.16 278.26 0. 1.0000 0. -10 6 0 2481.08 186.97 0. 1.0000 0. 10 -6 0 2890.85 171.49 0. 1.0000 0. -10 6 0 2183.02 171.27 0. 1.0000 0. 6 -10 0 2415.96 173.25 0. 1.0000 0. 10 -6 0 2065.75 170.75 0. 1.0000 0. 10 -8 0 1200.02 139.03 0. 1.0000 0. 8 -10 0 1257.71 147.72 0. 1.0000 0. -8 10 0 1298.82 128.10 0. 1.0000 0. -10 8 0 1377.36 133.47 0. 1.0000 0. 8 -10 0 1184.07 138.95 0. 1.0000 0. 10 -8 0 1473.32 149.27 0. 1.0000 0. -10 8 0 1325.83 124.23 0. 1.0000 0. -10 10 0 1137.37 123.66 0. 1.0000 0. -10 10 0 1109.07 135.74 0. 1.0000 0. 10 -10 0 1266.26 159.95 0. 1.0000 0. 10 -10 0 1370.82 153.33 0. 1.0000 0. 11 -3 0 2368.33 184.34 0. 1.0000 0. 11 -3 0 2627.48 162.89 0. 1.0000 0. -11 5 0 2652.75 188.85 0. 1.0000 0. 11 -5 0 2830.75 202.26 0. 1.0000 0. 11 -5 0 3187.57 186.59 0. 1.0000 0. -11 5 0 3019.78 195.52 0. 1.0000 0. -11 7 0 2924.62 194.43 0. 1.0000 0. -11 7 0 2953.12 210.76 0. 1.0000 0. 7 -11 0 2874.95 196.08 0. 1.0000 0. 11 -7 0 3027.55 188.91 0. 1.0000 0. 11 -9 0 881.56 92.85 0. 1.0000 0. 11 -9 0 654.13 82.41 0. 1.0000 0. 9 -11 0 1118.46 147.73 0. 1.0000 0. 9 -11 0 727.24 83.71 0. 1.0000 0. -11 9 0 665.66 76.07 0. 1.0000 0. -9 11 0 1078.73 104.56 0. 1.0000 0. -11 11 0 1514.03 152.02 0. 1.0000 0. -11 11 0 1633.09 153.75 0. 1.0000 0. 11 -11 0 1403.97 164.63 0. 1.0000 0. 11 -11 0 1446.67 179.09 0. 1.0000 0. 12 -2 0 1044.70 107.37 0. 1.0000 0. 12 -4 0 2468.99 186.65 0. 1.0000 0. 12 -4 0 2191.86 157.82 0. 1.0000 0. 12 -6 0 2577.07 169.57 0. 1.0000 0. -12 6 0 2254.34 172.03 0. 1.0000 0. 12 -6 0 1993.13 175.03 0. 1.0000 0. -12 6 0 1985.78 182.58 0. 1.0000 0. -12 8 0 1391.96 163.74 0. 1.0000 0. -12 8 0 1513.71 146.60 0. 1.0000 0. 8 -12 0 1447.71 159.11 0. 1.0000 0. 12 -8 0 1468.85 129.44 0. 1.0000 0. 12 -8 0 1263.72 156.69 0. 1.0000 0. -12 10 0 1110.75 111.78 0. 1.0000 0. 12 -10 0 1065.87 115.45 0. 1.0000 0. 12 -10 0 1391.05 119.00 0. 1.0000 0. 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1.0000 0. 0 -3 23 42.25 114.97 0. 1.0000 0. -3 -2 23 -155.84 83.50 0. 1.0000 0. 2 -3 23 13.36 78.35 0. 1.0000 0. -2 -3 -23 -11.29 68.95 0. 1.0000 0. -3 2 -23 -52.11 76.68 0. 1.0000 0. -3 -2 23 129.56 141.50 0. 1.0000 0. 2 3 -23 -83.65 81.65 0. 1.0000 0. 2 -3 23 -28.54 112.01 0. 1.0000 0. 3 2 23 13.63 137.51 0. 1.0000 0. 3 2 23 -135.43 85.22 0. 1.0000 0. -2 -3 -23 -41.23 82.33 0. 1.0000 0. -2 3 23 -27.17 116.07 0. 1.0000 0. -2 3 23 -88.04 88.54 0. 1.0000 0. -3 2 -23 -57.82 80.03 0. 1.0000 0. 3 -2 -23 56.55 89.35 0. 1.0000 0. 3 -2 -23 -57.49 81.26 0. 1.0000 0. -3 -2 -23 -69.28 69.62 0. 1.0000 0. 3 -2 23 1.87 85.28 0. 1.0000 0. -3 2 23 -9.52 86.67 0. 1.0000 0. 2 -3 -23 75.93 88.26 0. 1.0000 0. -2 -3 23 204.96 96.21 0. 1.0000 0. 2 3 23 -16.06 78.26 0. 1.0000 0. 3 -2 23 8.27 103.81 0. 1.0000 0. -3 -2 -23 1.69 76.63 0. 1.0000 0. 2 3 23 -97.19 118.03 0. 1.0000 0. -2 -3 23 358.82 150.11 0. 1.0000 0. 3 2 -23 2.56 76.56 0. 1.0000 0. -2 3 -23 67.18 73.15 0. 1.0000 0. -2 3 -23 -56.60 78.73 0. 1.0000 0. -3 2 23 -21.59 99.72 0. 1.0000 0. 2 -3 -23 -9.62 86.23 0. 1.0000 0. -1 -4 -23 2.67 69.87 0. 1.0000 0. 1 -4 23 40.33 124.12 0. 1.0000 0. 1 -4 23 24.06 81.14 0. 1.0000 0. 4 1 23 58.06 84.40 0. 1.0000 0. 4 -1 -23 104.01 95.78 0. 1.0000 0. -1 4 23 -40.69 133.98 0. 1.0000 0. 4 1 23 99.73 141.61 0. 1.0000 0. -4 -1 23 219.48 138.28 0. 1.0000 0. 4 -1 -23 99.67 79.00 0. 1.0000 0. -1 4 23 96.25 83.78 0. 1.0000 0. -4 1 -23 58.30 80.00 0. 1.0000 0. -4 1 -23 141.71 90.72 0. 1.0000 0. -4 -1 23 87.33 82.54 0. 1.0000 0. 1 -4 -23 30.71 87.18 0. 1.0000 0. -4 1 23 -17.23 71.60 0. 1.0000 0. 4 -1 23 -6.28 103.05 0. 1.0000 0. -4 -1 -23 23.13 74.94 0. 1.0000 0. -1 4 -23 -88.48 66.18 0. 1.0000 0. 4 1 -23 161.35 84.93 0. 1.0000 0. -4 -1 -23 -92.37 63.86 0. 1.0000 0. 1 4 23 -10.43 81.38 0. 1.0000 0. 1 4 23 -33.28 138.04 0. 1.0000 0. 4 -1 23 21.49 69.27 0. 1.0000 0. 1 -4 -23 -27.07 74.87 0. 1.0000 0. -4 1 23 56.06 98.13 0. 1.0000 0. 3 -4 23 -15.94 85.96 0. 1.0000 0. 4 3 23 138.55 109.09 0. 1.0000 0. -3 4 23 14.02 113.56 0. 1.0000 0. 4 -3 -23 -95.82 90.72 0. 1.0000 0. -4 3 -23 -90.68 78.52 0. 1.0000 0. 3 4 -23 36.87 80.05 0. 1.0000 0. 4 -3 -23 6.04 79.77 0. 1.0000 0. -3 4 23 88.18 78.28 0. 1.0000 0. -4 -3 23 65.61 107.85 0. 1.0000 0. 3 -4 23 -120.74 125.88 0. 1.0000 0. -4 3 -23 -107.30 82.54 0. 1.0000 0. 3 -4 -23 0.43 88.56 0. 1.0000 0. 4 3 -23 43.90 74.16 0. 1.0000 0. -4 3 23 -122.41 102.13 0. 1.0000 0. -4 3 23 -108.92 78.97 0. 1.0000 0. -3 4 -23 -56.05 72.50 0. 1.0000 0. 3 -4 -23 90.37 88.33 0. 1.0000 0. 3 4 23 157.79 123.85 0. 1.0000 0. 4 -3 23 -33.49 103.09 0. 1.0000 0. -3 -4 23 -95.95 85.90 0. 1.0000 0. -4 -3 -23 -60.84 90.83 0. 1.0000 0. 4 -3 23 61.28 86.09 0. 1.0000 0. -3 4 -23 120.73 81.16 0. 1.0000 0. -5 0 -23 -36.85 70.63 0. 1.0000 0. -5 0 23 136.39 120.62 0. 1.0000 0. 0 -5 -23 4.02 64.28 0. 1.0000 0. -5 0 23 -15.34 74.71 0. 1.0000 0. -5 0 -23 72.90 75.10 0. 1.0000 0. 5 0 -23 -7.02 76.08 0. 1.0000 0. 0 -5 23 370.52 137.85 0. 1.0000 0. 0 -5 23 -90.69 78.46 0. 1.0000 0. 5 0 23 -6.47 68.62 0. 1.0000 0. 0 5 23 -12.49 95.64 0. 1.0000 0. 5 0 23 30.65 138.86 0. 1.0000 0. 0 5 23 -14.58 140.01 0. 1.0000 0. 0 5 -23 4.28 78.36 0. 1.0000 0. -5 2 -23 -82.34 85.09 0. 1.0000 0. -5 2 -23 -103.20 79.61 0. 1.0000 0. 5 -2 -23 33.23 78.56 0. 1.0000 0. 5 -2 -23 -5.60 84.50 0. 1.0000 0. 2 5 -23 -67.63 77.34 0. 1.0000 0. 2 -5 23 426.24 156.12 0. 1.0000 0. 5 2 23 176.44 117.49 0. 1.0000 0. -5 -2 23 -26.60 106.42 0. 1.0000 0. 5 2 23 32.30 93.21 0. 1.0000 0. -2 -5 -23 79.20 80.78 0. 1.0000 0. -2 5 23 -67.92 75.50 0. 1.0000 0. -2 5 23 170.76 137.98 0. 1.0000 0. 2 -5 23 35.85 74.84 0. 1.0000 0. -5 2 23 -40.00 93.89 0. 1.0000 0. 5 2 -23 -20.41 77.99 0. 1.0000 0. -5 2 23 91.82 76.68 0. 1.0000 0. 5 -2 23 -242.37 121.42 0. 1.0000 0. -5 -2 -23 -41.74 79.20 0. 1.0000 0. 5 -2 23 -68.82 76.72 0. 1.0000 0. 2 5 23 92.31 88.21 0. 1.0000 0. 2 -5 -23 75.52 86.58 0. 1.0000 0. -2 -5 23 116.28 84.39 0. 1.0000 0. -2 5 -23 95.86 73.81 0. 1.0000 0. 2 5 23 179.44 122.69 0. 1.0000 0. 2 -5 -23 -36.75 76.76 0. 1.0000 0. 0 0 -24 133.56 100.27 0. 1.0000 0. 0 0 -24 60.08 88.99 0. 1.0000 0. 0 0 24 94.55 104.98 0. 1.0000 0. 0 0 24 218.22 98.90 0. 1.0000 0. 1 1 24 140.39 90.53 0. 1.0000 0. -1 1 24 235.92 85.54 0. 1.0000 0. 1 -1 24 261.01 91.63 0. 1.0000 0. -1 1 -24 208.43 92.91 0. 1.0000 0. 1 -1 -24 114.51 95.33 0. 1.0000 0. 1 1 -24 30.51 90.58 0. 1.0000 0. -1 -1 24 170.91 85.53 0. 1.0000 0. -1 -1 -24 252.05 92.87 0. 1.0000 0. -1 1 -24 110.99 95.91 0. 1.0000 0. 1 -1 -24 126.54 92.21 0. 1.0000 0. 1 1 -24 95.92 75.38 0. 1.0000 0. -1 -1 -24 233.56 89.45 0. 1.0000 0. -512 # 10453 reflections output ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 -y,x,z y,-x,-z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,-z+1/2 -x,-y,z x,y,-z -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,z -y,x,-z y+1/2,-x+1/2,z+1/2 -y+1/2,x+1/2,-z+1/2 -x,y,z+1/2 x,-y,-z+1/2 -x+1/2,y+1/2,z+1 x+1/2,-y+1/2,-z+1 y,x,z+1/2 -y,-x,-z+1/2 y+1/2,x+1/2,z+1 -y+1/2,-x+1/2,-z+1 x,-y,z+1/2 -x,y,-z+1/2 x+1/2,-y+1/2,z+1 -x+1/2,y+1/2,-z+1 -y,-x,z+1/2 y,x,-z+1/2 -y+1/2,-x+1/2,z+1 y+1/2,x+1/2,-z+1 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.5000 0.5000 0.57665(6) 0.0270 1.0000 Uani DS T . . . . C1 C 0.6505(6) 0.5804(6) 0.5000 0.0388 1.0000 Uani DS TU . . . . C2 C 0.7275(6) 0.6423(6) 0.5000 0.0369 1.0000 Uani DS TU . . . . C3 C 0.7626(5) 0.6722(5) 0.5619(2) 0.0468 1.0000 Uani D U . . . . C4 C 0.5898(6) 0.5010(4) 0.7102(2) 0.0553 0.3750 Uani D U . . . . C5 C 0.5640(5) 0.5634(5) 0.7101(2) 0.0544 0.3750 Uani D U . . . . C10 C 0.6706(16) 0.8294(16) 0.7189(13) 0.250(9) 1.0000 Uiso DS U . . . . C11 C 0.5718(13) 0.8154(13) 0.6105(11) 0.249(9) 1.0000 Uiso D U . . . . N1 N 0.5000 0.5000 0.6831(4) 0.0286 1.0000 Uani DS TU . . . . N10 N 0.6354(12) 0.8646(12) 0.6509(11) 0.249(9) 1.0000 Uiso DS U . . . . O1 O 0.6197(4) 0.5583(4) 0.5577(2) 0.0506 1.0000 Uani D U . . . . O10 O 0.7387(14) 0.8714(15) 0.7357(16) 0.250(9) 0.5000 Uiso D U . . . . H32 H 0.7374 0.6537 0.6046 0.0722 1.0000 Uiso R . . . . . H111 H 0.5571 0.8496 0.5690 0.3980 1.0000 Uiso R . . . . . H112 H 0.5185 0.8072 0.6385 0.3980 1.0000 Uiso R . . . . . H113 H 0.5954 0.7577 0.5969 0.3980 1.0000 Uiso R . . . . . H41 H 0.6195 0.5541 0.6942 0.0665 0.3750 Uiso R . . . . . H42 H 0.6208 0.4493 0.6931 0.0665 0.3750 Uiso R . . . . . H51 H 0.6226 0.5474 0.6938 0.0662 0.3750 Uiso R . . . . . H52 H 0.5489 0.6220 0.6933 0.0662 0.3750 Uiso R . . . . . H101 H 0.6467 0.7806 0.7437 0.3003 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0305(5) 0.0305(5) 0.0201(6) 0.0000 0.0000 0.0000 C1 0.031(5) 0.048(6) 0.038(2) 0.0000 0.0000 -0.008(3) C2 0.036(5) 0.041(6) 0.034(3) 0.0000 0.0000 -0.009(3) C3 0.048(4) 0.064(5) 0.028(2) 0.008(3) -0.003(3) -0.019(3) C4 0.031(3) 0.107(10) 0.027(5) 0.009(17) -0.000(3) -0.0009(10) C5 0.069(5) 0.070(6) 0.024(5) 0.000(9) -0.002(9) -0.038(5) N1 0.031(3) 0.031(3) 0.024(4) 0.0000 0.0000 0.0000 O1 0.042(3) 0.066(4) 0.043(2) 0.008(2) 0.001(2) -0.021(2) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0016 0.0014 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0036 0.0026 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.3043 0.7253 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zn1 2_666 Zn1 . O1 5_655 79.73(12) yes Zn1 2_666 Zn1 . O1 13_565 79.73(12) yes O1 5_655 Zn1 . O1 13_565 159.5(2) yes Zn1 2_666 Zn1 . O1 9_665 79.73(12) yes O1 5_655 Zn1 . O1 9_665 88.18(4) yes O1 13_565 Zn1 . O1 9_665 88.18(4) yes Zn1 2_666 Zn1 . N1 . 179.99 yes O1 5_655 Zn1 . N1 . 100.27(12) yes O1 13_565 Zn1 . N1 . 100.27(12) yes O1 9_665 Zn1 . N1 . 100.27(12) yes Zn1 2_666 Zn1 . O1 . 79.73(12) yes O1 5_655 Zn1 . O1 . 88.18(4) yes O1 13_565 Zn1 . O1 . 88.18(4) yes O1 9_665 Zn1 . O1 . 159.5(2) yes N1 . Zn1 . O1 . 100.27(12) yes O1 10_556 C1 . C2 . 117.2(3) yes O1 10_556 C1 . O1 . 125.6(5) yes C2 . C1 . O1 . 117.2(3) yes C1 . C2 . C3 10_556 120.3(2) yes C1 . C2 . C3 . 120.3(2) yes C3 10_556 C2 . C3 . 119.4(5) yes C3 31_664 C3 . C2 . 120.2(2) yes C3 31_664 C3 . H32 . 119.5 no C2 . C3 . H32 . 119.9 no C4 18_566 C4 . N1 . 111.1(4) yes C4 18_566 C4 . H41 . 109.6 no N1 . C4 . H41 . 109.1 no C4 18_566 C4 . H42 . 108.9 no N1 . C4 . H42 . 108.7 no H41 . C4 . H42 . 109.5 no C5 30_556 C5 . N1 . 110.9(4) yes C5 30_556 C5 . H51 . 109.3 no N1 . C5 . H51 . 109.0 no C5 30_556 C5 . H52 . 109.2 no N1 . C5 . H52 . 109.0 no H51 . C5 . H52 . 109.5 no H101 31_664 C10 . O10 31_664 125.2 no H101 31_664 C10 . N10 . 125.1 no O10 31_664 C10 . N10 . 109.6(5) yes H101 31_664 C10 . O10 . 16.0 no O10 31_664 C10 . O10 . 140.1(9) yes N10 . C10 . O10 . 109.6(5) yes H101 31_664 C10 . H101 . 109.8 no O10 31_664 C10 . H101 . 16.0 no N10 . C10 . H101 . 125.1 no O10 . C10 . H101 . 125.2 no N10 . C11 . H111 . 108.7 no N10 . C11 . H112 . 108.4 no H111 . C11 . H112 . 109.4 no N10 . C11 . H113 . 111.2 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C5 5_655 N1 . C5 9_665 82.7(3) yes C5 5_655 N1 . C5 . 82.7(3) yes C5 9_665 N1 . C5 . 138.2(8) yes C5 5_655 N1 . C5 13_565 138.2(8) yes C5 9_665 N1 . C5 13_565 82.7(3) yes C5 . N1 . C5 13_565 82.7(3) yes C5 5_655 N1 . C4 9_665 42.7(3) yes C5 9_665 N1 . C4 9_665 41.0(3) yes C5 . N1 . C4 9_665 119.8(5) yes C5 13_565 N1 . C4 9_665 118.6(5) yes C5 5_655 N1 . C4 . 118.6(5) yes C5 9_665 N1 . C4 . 119.8(5) yes C5 . N1 . C4 . 41.0(3) yes C5 13_565 N1 . C4 . 42.7(3) yes C4 9_665 N1 . C4 . 137.8(8) yes C5 5_655 N1 . C4 13_565 119.8(5) yes C5 9_665 N1 . C4 13_565 42.7(3) yes C5 . N1 . C4 13_565 118.6(5) yes C5 13_565 N1 . C4 13_565 41.0(3) yes C4 9_665 N1 . C4 13_565 82.6(3) yes C5 5_655 N1 . C4 5_655 41.0(3) yes C5 9_665 N1 . C4 5_655 118.6(5) yes C5 . N1 . C4 5_655 42.7(3) yes C5 13_565 N1 . C4 5_655 119.8(5) yes C4 9_665 N1 . C4 5_655 82.6(3) yes C5 5_655 N1 . Zn1 . 110.9(4) yes C5 9_665 N1 . Zn1 . 110.9(4) yes C5 . N1 . Zn1 . 110.9(4) yes C5 13_565 N1 . Zn1 . 110.9(4) yes C4 9_665 N1 . Zn1 . 111.1(4) yes C4 . N1 . C4 13_565 82.6(3) yes C4 . N1 . C4 5_655 82.6(3) yes C4 13_565 N1 . C4 5_655 137.8(8) yes C4 . N1 . Zn1 . 111.1(4) yes C4 13_565 N1 . Zn1 . 111.1(4) yes C4 5_655 N1 . Zn1 . 111.1(4) yes C10 . N10 . C11 . 121.4(6) yes C10 . N10 . C11 31_664 121.4(6) yes C11 . N10 . C11 31_664 113.3(9) yes Zn1 . O1 . C1 . 127.0(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . Zn1 2_666 2.954(2) yes Zn1 . O1 5_655 2.045(5) yes Zn1 . O1 13_565 2.045(5) yes Zn1 . O1 9_665 2.045(5) yes Zn1 . N1 . 2.051(8) yes Zn1 . O1 . 2.045(5) yes C1 . O1 10_556 1.251(4) yes C1 . C2 . 1.493(7) yes C1 . O1 . 1.251(4) yes C2 . C3 10_556 1.382(5) yes C2 . C3 . 1.382(5) yes C3 . C3 31_664 1.393(7) yes C3 . H32 . 0.948 no C4 . C4 18_566 1.533(9) yes C4 . N1 . 1.454(8) yes C4 . H41 . 0.970 no C4 . H42 . 0.970 no C5 . C5 30_556 1.538(9) yes C5 . N1 . 1.458(8) yes C5 . H51 . 0.970 no C5 . H52 . 0.970 no C10 . H101 31_664 0.950 no C10 . O10 31_664 1.251(6) yes C10 . N10 . 1.511(9) yes C10 . O10 . 1.251(6) yes C10 . H101 . 0.950 no C11 . N10 . 1.442(9) yes C11 . H111 . 0.978 no C11 . H112 . 0.978 no C11 . H113 . 0.979 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C4 . H42 . O10 19_644 131 0.97 2.56 3.286(15) yes C5 13_565 H42 . O10 19_644 123 0.95 2.56 3.184(15) yes C4 5_655 H52 . O10 31_664 133 0.96 2.56 3.286(15) yes C5 . H52 . O10 31_664 122 0.97 2.56 3.184(15) yes loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 1 2 3 x . 0 12 12 x . 1 1 4 x . 3 5 4 x . 2 5 5 x . 6 7 3 x . 4 5 7 x . 1 1 12 x . 1 2 19 x . 2 9 9 x . 9 12 1 x . 0 8 4 x . 3 17 8 x . 2 14 2 x . 2 16 12 x . 1 13 8 x . 1 13 10 x . 1 9 2 x . 1 5 0 x . 2 14 4 x . 7 11 14 x . 2 2 2 x . 4 5 3 x . 5 14 3 x . 1 2 15 x . 5 8 1 x . 4 8 4 x . 2 5 1 x . 1 1 16 x . 1 4 3 x . 10 11 3 x .