#------------------------------------------------------------------------------ #$Date: 2026-06-04 18:02:04 +0100 (Thu, 04 Jun 2026) $ #$Revision: 306217 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721093.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_7721093 loop_ _publ_author_name 'Panja, Anangamohan' 'Jana, Narayan Ch' 'Aravena, Daniel' 'Jagličić, Zvonko' _publ_section_title ; Tuning magnetic exchange and relaxation dynamics in dinuclear Dy(III) single-molecule magnets via co-ligand modulation on a hydrazone-based Schiff base platform. ; _journal_issue 18 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7329 _journal_page_last 7341 _journal_paper_doi 10.1039/d6dt00433d _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C15 H15 N3 O3, H2 O' _chemical_formula_sum 'C15 H17 N3 O4' _chemical_formula_weight 303.32 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_date 2026-03-22 _audit_creation_method ; Olex2 1.5 (compiled 2026.03.20 svn.r2bc28608 for OlexSys, GUI svn.r7524) ; _audit_update_record ; 2026-03-23 deposited with the CCDC. 2026-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.8688(3) _cell_length_b 22.4405(12) _cell_length_c 13.4798(8) _cell_measurement_reflns_used 4383 _cell_measurement_temperature 297.13(10) _cell_measurement_theta_max 77.9180 _cell_measurement_theta_min 3.7670 _cell_volume 1472.78(15) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (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 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 297.28 _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.975 _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 -44.00 29.72 0.38 1.13 -- -38.50 19.00 31.00 194 2 \w -108.00 -34.28 0.38 1.13 -- -38.50 -19.00-135.00 194 3 \w -20.00 53.72 0.38 1.13 -- 49.56 -19.00-135.00 194 4 \w 59.00 117.14 0.38 1.13 -- 49.56 19.00 31.00 153 5 \w 115.00 171.24 0.38 3.03 -- 107.46 19.00 31.00 148 6 \w 39.00 111.20 0.38 3.03 -- 107.46 -19.00-135.00 190 7 \w -48.00 22.30 0.38 1.13 -- -38.50 57.00 90.00 185 8 \w 3.00 36.06 0.38 1.13 -- 49.56 -37.00 120.00 87 9 \w 40.00 80.28 0.38 3.03 -- 107.46 -94.00 -90.00 106 10 \w 45.00 96.30 0.38 3.03 -- 107.46-125.00 120.00 135 11 \w 46.00 88.18 0.38 3.03 -- 107.46-125.00-120.00 111 12 \w 50.00 97.88 0.38 3.03 -- 107.46 -94.00 -60.00 126 13 \w 48.00 74.22 0.38 3.03 -- 107.46 -94.00-180.00 69 14 \w 63.00 105.94 0.38 3.03 -- 107.46 -94.00 120.00 113 15 \w 45.00 71.22 0.38 3.03 -- 107.46-125.00 -90.00 69 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7009 _diffrn_reflns_point_group_measured_fraction_full 0.956 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.989 _diffrn_reflns_theta_min 3.825 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66201 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light white' _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description plate _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.193 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Flack x determined using 898 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.11(19) _refine_ls_extinction_coef 0.0018(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 2814 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0462 _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^)+(0.0836P)^2^+0.2095P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1385 _refine_ls_wR_factor_ref 0.1430 _reflns_Friedel_coverage 0.612 _reflns_Friedel_fraction_full 0.910 _reflns_Friedel_fraction_max 0.869 _reflns_number_gt 2574 _reflns_number_total 2814 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00433d2.cif _cod_data_source_block ligand-h2l _cod_database_code 7721093 _shelx_shelxl_version_number 2018/3 _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 0.921 _shelx_estimated_absorpt_t_min 0.850 _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, All O(H) groups, All O(H,H) groups 2.a Free rotating group: O4(H4A,H4B) 2.b Aromatic/amide H refined with riding coordinates: C8(H8), C3(H3), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14) 2.c Idealised Me refined as rotating group: C00I(H00A,H00B,H00C), C5(H5A,H5B,H5C) 2.d Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL meval-iso-nicotinic_a.res in P2(1)2(1)2(1) ligand-h2l.res created by SHELXL-2018/3 at 21:21:28 on 22-Mar-2026 REM Old TITL MeVal-Iso-Nicotinic in P21212 #18 REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.129, Rweak 0.028, Alpha 0.011, Orientation as input REM Flack x = 0.359 ( 0.288 ) from Parsons' quotients REM Formula found by SHELXT: C16 N2 O4 CELL 1.54184 4.8688 22.4405 13.4798 90 90 90 ZERR 4 0.0003 0.0012 0.0008 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 60 68 12 16 L.S. 20 0 0 PLAN 5 SIZE 0.1 0.2 0.2 TEMP 24.13 CONF BOND $H list 4 MORE -1 fmap 2 53 acta OMIT 0 150 OMIT -4 1 7 OMIT -4 13 1 OMIT -1 2 7 OMIT 1 0 7 OMIT 1 1 6 OMIT 1 2 7 OMIT 2 0 0 OMIT 2 0 1 OMIT 2 0 8 OMIT 2 1 6 OMIT 3 0 6 OMIT 4 0 8 OMIT 5 0 9 REM REM REM WGHT 0.083600 0.209500 EXTI 0.001801 FVAR 0.29071 O2 4 1.095117 0.667044 0.639947 11.00000 0.05801 0.05802 = 0.04708 -0.00694 0.00058 -0.02331 O1 4 0.729011 0.584782 0.615976 11.00000 0.05276 0.05042 = 0.05472 0.00327 0.00180 -0.01579 AFIX 147 H1 2 0.629552 0.556425 0.602506 11.00000 -1.50000 AFIX 6 O4 4 0.211529 0.544477 0.746052 11.00000 0.09082 0.05589 = 0.04836 -0.00243 -0.01208 -0.01314 H4A 2 0.195851 0.513849 0.709419 11.00000 -1.50000 H4B 2 0.099890 0.569519 0.721332 11.00000 -1.50000 AFIX 0 N2 3 0.271964 0.469738 0.461114 11.00000 0.04744 0.03653 = 0.05163 -0.00561 -0.01032 -0.00612 O3 4 0.136649 0.451235 0.618592 11.00000 0.10322 0.06254 = 0.04503 -0.00953 -0.01323 -0.01774 N1 3 0.457512 0.512777 0.490637 11.00000 0.04685 0.03091 = 0.06184 -0.00240 -0.01325 -0.00231 C9 1 0.118786 0.441197 0.530095 11.00000 0.05201 0.03500 = 0.04548 -0.00390 -0.00920 0.00164 C1 1 0.856192 0.604036 0.532484 11.00000 0.03800 0.03513 = 0.04965 0.00207 -0.00247 -0.00036 C8 1 0.596975 0.536354 0.420164 11.00000 0.04626 0.04012 = 0.05999 -0.00480 -0.01196 0.00096 AFIX 43 H8 2 0.566991 0.523493 0.355478 11.00000 -1.20000 AFIX 0 C7 1 0.800694 0.582586 0.438058 11.00000 0.03693 0.03288 = 0.05618 -0.00112 -0.00869 0.00190 C2 1 1.055533 0.648835 0.544165 11.00000 0.03626 0.03648 = 0.04712 -0.00192 -0.00321 -0.00202 C3 1 1.191593 0.671209 0.462679 11.00000 0.04060 0.03877 = 0.04965 -0.00099 -0.00196 -0.00201 AFIX 43 H3 2 1.321427 0.701144 0.471473 11.00000 -1.20000 AFIX 0 C10 1 -0.077636 0.395309 0.491731 11.00000 0.04284 0.03194 = 0.04307 -0.00180 -0.00455 0.00233 C4 1 1.138885 0.649907 0.366872 11.00000 0.03925 0.04376 = 0.04752 0.00007 -0.00376 0.00632 N 3 -0.404658 0.320327 0.538602 11.00000 0.07096 0.06984 = 0.06226 0.01200 0.00011 -0.02484 C6 1 0.943781 0.605594 0.357096 11.00000 0.04694 0.04455 = 0.04908 -0.00589 -0.00962 0.00649 AFIX 43 H6 2 0.906559 0.590569 0.294219 11.00000 -1.20000 AFIX 0 C11 1 -0.125006 0.382750 0.393224 11.00000 0.05994 0.05195 = 0.04393 -0.00426 -0.00033 -0.01546 AFIX 43 H11 2 -0.032370 0.403574 0.343843 11.00000 -1.20000 AFIX 0 C00I 1 1.314321 0.706659 0.658986 11.00000 0.05097 0.05479 = 0.06239 -0.01375 0.00014 -0.01210 AFIX 137 H00A 2 1.283518 0.743377 0.624175 11.00000 -1.50000 H00B 2 1.483370 0.689131 0.636800 11.00000 -1.50000 H00C 2 1.325053 0.714394 0.728923 11.00000 -1.50000 AFIX 0 C12 1 -0.311673 0.338872 0.368673 11.00000 0.06475 0.06047 = 0.04823 -0.00803 -0.00611 -0.01659 AFIX 43 H12 2 -0.347014 0.329765 0.302589 11.00000 -1.20000 AFIX 0 C5 1 1.287064 0.675368 0.279313 11.00000 0.05505 0.06779 = 0.05110 0.00147 0.00171 0.00024 AFIX 137 H5A 2 1.277972 0.718080 0.281624 11.00000 -1.50000 H5B 2 1.202572 0.661411 0.219308 11.00000 -1.50000 H5C 2 1.475694 0.662946 0.280845 11.00000 -1.50000 AFIX 0 C13 1 -0.443771 0.309017 0.443116 11.00000 0.06024 0.04760 = 0.06937 0.00105 -0.00400 -0.01332 AFIX 43 H13 2 -0.567571 0.279209 0.425857 11.00000 -1.20000 AFIX 0 C14 1 -0.227237 0.363410 0.560614 11.00000 0.06196 0.06117 = 0.04240 0.00412 -0.00239 -0.00767 AFIX 43 H14 2 -0.202163 0.372714 0.627233 11.00000 -1.20000 AFIX 0 H2 2 0.257684 0.460656 0.397304 11.00000 0.04220 HKLF 4 REM meval-iso-nicotinic_a.res in P2(1)2(1)2(1) REM wR2 = 0.1430, GooF = S = 1.111, Restrained GooF = 1.111 for all data REM R1 = 0.0462 for 2574 Fo > 4sig(Fo) and 0.0502 for all 2814 data REM 210 parameters refined using 0 restraints END WGHT 0.0836 0.2094 REM Highest difference peak 0.193, deepest hole -0.173, 1-sigma level 0.044 Q1 1 0.1558 0.5014 0.6210 11.00000 0.05 0.19 Q2 1 0.2783 0.4210 0.4637 11.00000 0.05 0.17 Q3 1 0.4620 0.4616 0.4846 11.00000 0.05 0.17 Q4 1 1.1403 0.7007 0.2333 11.00000 0.05 0.16 Q5 1 0.7110 0.6332 0.6042 11.00000 0.05 0.16 ; _shelx_res_checksum 16469 _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 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 O2 O 1.0951(5) 0.66704(10) 0.63995(17) 0.0544(6) Uani 1 1 d . . . . . O1 O 0.7290(5) 0.58478(10) 0.61598(18) 0.0526(6) Uani 1 1 d . . . . . H1 H 0.629552 0.556425 0.602506 0.079 Uiso 1 1 calc R U . . . O4 O 0.2115(7) 0.54448(11) 0.74605(19) 0.0650(8) Uani 1 1 d G . . . . H4A H 0.195851 0.513849 0.709419 0.098 Uiso 1 1 d G U . . . H4B H 0.099890 0.569519 0.721332 0.098 Uiso 1 1 d G U . . . N2 N 0.2720(6) 0.46974(11) 0.4611(2) 0.0452(6) Uani 1 1 d . . . . . O3 O 0.1366(8) 0.45123(11) 0.61859(18) 0.0703(8) Uani 1 1 d . . . . . N1 N 0.4575(6) 0.51278(10) 0.4906(2) 0.0465(6) Uani 1 1 d . . . . . C9 C 0.1188(7) 0.44120(12) 0.5301(2) 0.0442(7) Uani 1 1 d . . . . . C1 C 0.8562(6) 0.60404(12) 0.5325(2) 0.0409(6) Uani 1 1 d . . . . . C8 C 0.5970(7) 0.53635(14) 0.4202(3) 0.0488(7) Uani 1 1 d . . . . . H8 H 0.566991 0.523493 0.355478 0.059 Uiso 1 1 calc R U . . . C7 C 0.8007(6) 0.58259(12) 0.4381(2) 0.0420(7) Uani 1 1 d . . . . . C2 C 1.0555(6) 0.64884(12) 0.5442(2) 0.0400(6) Uani 1 1 d . . . . . C3 C 1.1916(6) 0.67121(13) 0.4627(2) 0.0430(7) Uani 1 1 d . . . . . H3 H 1.321427 0.701144 0.471473 0.052 Uiso 1 1 calc R U . . . C10 C -0.0776(6) 0.39531(12) 0.4917(2) 0.0393(6) Uani 1 1 d . . . . . C4 C 1.1389(6) 0.64991(13) 0.3669(2) 0.0435(7) Uani 1 1 d . . . . . N N -0.4047(8) 0.32033(15) 0.5386(3) 0.0677(9) Uani 1 1 d . . . . . C6 C 0.9438(7) 0.60559(13) 0.3571(2) 0.0469(7) Uani 1 1 d . . . . . H6 H 0.906559 0.590569 0.294219 0.056 Uiso 1 1 calc R U . . . C11 C -0.1250(8) 0.38275(14) 0.3932(2) 0.0519(8) Uani 1 1 d . . . . . H11 H -0.032370 0.403574 0.343843 0.062 Uiso 1 1 calc R U . . . C00I C 1.3143(8) 0.70666(15) 0.6590(3) 0.0561(9) Uani 1 1 d . . . . . H00A H 1.283518 0.743377 0.624175 0.084 Uiso 1 1 calc R U . . . H00B H 1.483370 0.689131 0.636800 0.084 Uiso 1 1 calc R U . . . H00C H 1.325053 0.714394 0.728923 0.084 Uiso 1 1 calc R U . . . C12 C -0.3117(8) 0.33887(15) 0.3687(3) 0.0578(9) Uani 1 1 d . . . . . H12 H -0.347014 0.329765 0.302589 0.069 Uiso 1 1 calc R U . . . C5 C 1.2871(8) 0.67537(17) 0.2793(3) 0.0580(9) Uani 1 1 d . . . . . H5A H 1.277972 0.718080 0.281624 0.087 Uiso 1 1 calc R U . . . H5B H 1.202572 0.661411 0.219308 0.087 Uiso 1 1 calc R U . . . H5C H 1.475694 0.662946 0.280845 0.087 Uiso 1 1 calc R U . . . C13 C -0.4438(9) 0.30902(15) 0.4431(3) 0.0591(9) Uani 1 1 d . . . . . H13 H -0.567571 0.279209 0.425857 0.071 Uiso 1 1 calc R U . . . C14 C -0.2272(8) 0.36341(16) 0.5606(3) 0.0552(8) Uani 1 1 d . . . . . H14 H -0.202163 0.372714 0.627233 0.066 Uiso 1 1 calc R U . . . H2 H 0.258(8) 0.4607(14) 0.397(3) 0.042(9) Uiso 1 1 d . . . . . 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 O2 0.0580(14) 0.0580(13) 0.0471(12) -0.0069(10) 0.0006(11) -0.0233(11) O1 0.0528(13) 0.0504(12) 0.0547(14) 0.0033(9) 0.0018(11) -0.0158(10) O4 0.091(2) 0.0559(14) 0.0484(13) -0.0024(11) -0.0121(13) -0.0131(14) N2 0.0474(14) 0.0365(11) 0.0516(15) -0.0056(11) -0.0103(12) -0.0061(11) O3 0.103(2) 0.0625(14) 0.0450(13) -0.0095(11) -0.0132(14) -0.0177(15) N1 0.0468(14) 0.0309(11) 0.0618(17) -0.0024(10) -0.0133(13) -0.0023(10) C9 0.0520(17) 0.0350(13) 0.0455(15) -0.0039(12) -0.0092(14) 0.0016(12) C1 0.0380(14) 0.0351(13) 0.0496(16) 0.0021(12) -0.0025(13) -0.0004(11) C8 0.0463(16) 0.0401(14) 0.0600(18) -0.0048(13) -0.0120(16) 0.0010(13) C7 0.0369(14) 0.0329(13) 0.0562(18) -0.0011(12) -0.0087(13) 0.0019(11) C2 0.0363(14) 0.0365(13) 0.0471(16) -0.0019(12) -0.0032(12) -0.0020(11) C3 0.0406(15) 0.0388(13) 0.0496(16) -0.0010(12) -0.0020(13) -0.0020(12) C10 0.0428(15) 0.0319(12) 0.0431(15) -0.0018(11) -0.0045(13) 0.0023(11) C4 0.0392(15) 0.0438(15) 0.0475(16) 0.0001(12) -0.0038(13) 0.0063(12) N 0.071(2) 0.0698(19) 0.0623(19) 0.0120(16) 0.0001(17) -0.0248(17) C6 0.0469(16) 0.0446(15) 0.0491(16) -0.0059(13) -0.0096(14) 0.0065(13) C11 0.060(2) 0.0519(17) 0.0439(17) -0.0043(13) -0.0003(16) -0.0155(16) C00I 0.0510(18) 0.0548(18) 0.062(2) -0.0137(16) 0.0001(17) -0.0121(15) C12 0.065(2) 0.060(2) 0.0482(18) -0.0080(15) -0.0061(17) -0.0166(17) C5 0.055(2) 0.068(2) 0.0511(19) 0.0015(16) 0.0017(16) 0.0002(17) C13 0.060(2) 0.0476(18) 0.069(2) 0.0010(15) -0.0040(19) -0.0133(16) C14 0.062(2) 0.0612(19) 0.0424(17) 0.0041(14) -0.0024(16) -0.0077(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 O2 C00I 117.8(3) . . ? C1 O1 H1 109.5 . . ? H4A O4 H4B 104.4 . . ? N1 N2 H2 119(2) . . ? C9 N2 N1 119.6(3) . . ? C9 N2 H2 121(2) . . ? C8 N1 N2 114.9(3) . . ? N2 C9 C10 116.1(3) . . ? O3 C9 N2 123.1(3) . . ? O3 C9 C10 120.8(3) . . ? O1 C1 C7 124.2(3) . . ? O1 C1 C2 116.8(3) . . ? C7 C1 C2 119.0(3) . . ? N1 C8 H8 118.9 . . ? N1 C8 C7 122.2(3) . . ? C7 C8 H8 118.9 . . ? C1 C7 C8 122.1(3) . . ? C1 C7 C6 119.5(3) . . ? C6 C7 C8 118.4(3) . . ? O2 C2 C1 114.6(3) . . ? O2 C2 C3 125.2(3) . . ? C3 C2 C1 120.2(3) . . ? C2 C3 H3 119.2 . . ? C2 C3 C4 121.5(3) . . ? C4 C3 H3 119.2 . . ? C11 C10 C9 125.5(3) . . ? C11 C10 C14 117.0(3) . . ? C14 C10 C9 117.5(3) . . ? C3 C4 C5 120.6(3) . . ? C6 C4 C3 117.4(3) . . ? C6 C4 C5 122.1(3) . . ? C13 N C14 116.7(3) . . ? C7 C6 H6 118.8 . . ? C4 C6 C7 122.4(3) . . ? C4 C6 H6 118.8 . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.2(3) . . ? C12 C11 H11 120.4 . . ? O2 C00I H00A 109.5 . . ? O2 C00I H00B 109.5 . . ? O2 C00I H00C 109.5 . . ? H00A C00I H00B 109.5 . . ? H00A C00I H00C 109.5 . . ? H00B C00I H00C 109.5 . . ? C11 C12 H12 120.5 . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12 120.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N C13 C12 123.4(3) . . ? N C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C10 C14 H14 117.6 . . ? N C14 C10 124.7(3) . . ? N C14 H14 117.6 . . ? 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 O2 C2 1.368(4) . ? O2 C00I 1.413(4) . ? O1 H1 0.8200 . ? O1 C1 1.355(4) . ? O4 H4A 0.8497 . ? O4 H4B 0.8499 . ? N2 N1 1.381(3) . ? N2 C9 1.353(4) . ? N2 H2 0.89(4) . ? O3 C9 1.217(4) . ? N1 C8 1.282(4) . ? C9 C10 1.497(4) . ? C1 C7 1.387(4) . ? C1 C2 1.406(4) . ? C8 H8 0.9300 . ? C8 C7 1.455(4) . ? C7 C6 1.394(5) . ? C2 C3 1.377(4) . ? C3 H3 0.9300 . ? C3 C4 1.401(5) . ? C10 C11 1.377(4) . ? C10 C14 1.380(5) . ? C4 C6 1.382(4) . ? C4 C5 1.497(5) . ? N C13 1.326(5) . ? N C14 1.330(5) . ? C6 H6 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.380(5) . ? C00I H00A 0.9600 . ? C00I H00B 0.9600 . ? C00I H00C 0.9600 . ? C12 H12 0.9300 . ? C12 C13 1.367(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? 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 O2 C2 C3 C4 179.9(3) . . . . ? O1 C1 C7 C8 -0.2(5) . . . . ? O1 C1 C7 C6 180.0(3) . . . . ? O1 C1 C2 O2 0.2(4) . . . . ? O1 C1 C2 C3 -179.3(3) . . . . ? N2 N1 C8 C7 179.7(3) . . . . ? N2 C9 C10 C11 -4.1(5) . . . . ? N2 C9 C10 C14 177.0(3) . . . . ? O3 C9 C10 C11 176.3(4) . . . . ? O3 C9 C10 C14 -2.7(5) . . . . ? N1 N2 C9 O3 -0.5(5) . . . . ? N1 N2 C9 C10 179.9(2) . . . . ? N1 C8 C7 C1 -0.1(5) . . . . ? N1 C8 C7 C6 179.8(3) . . . . ? C9 N2 N1 C8 178.6(3) . . . . ? C9 C10 C11 C12 179.7(3) . . . . ? C9 C10 C14 N -178.4(4) . . . . ? C1 C7 C6 C4 -0.8(5) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C8 C7 C6 C4 179.4(3) . . . . ? C7 C1 C2 O2 179.9(3) . . . . ? C7 C1 C2 C3 0.5(4) . . . . ? C2 C1 C7 C8 -179.9(3) . . . . ? C2 C1 C7 C6 0.3(4) . . . . ? C2 C3 C4 C6 0.2(4) . . . . ? C2 C3 C4 C5 179.3(3) . . . . ? C3 C4 C6 C7 0.5(4) . . . . ? C10 C11 C12 C13 -0.2(6) . . . . ? C11 C10 C14 N 2.6(5) . . . . ? C11 C12 C13 N 0.7(6) . . . . ? C00I O2 C2 C1 172.6(3) . . . . ? C00I O2 C2 C3 -8.0(4) . . . . ? C5 C4 C6 C7 -178.6(3) . . . . ? C13 N C14 C10 -2.0(6) . . . . ? C14 C10 C11 C12 -1.4(5) . . . . ? C14 N C13 C12 0.3(6) . . . . ?