#------------------------------------------------------------------------------ #$Date: 2021-02-24 12:39:48 +0200 (Wed, 24 Feb 2021) $ #$Revision: 262195 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/06/1560620.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_1560620 loop_ _publ_author_name 'Amayuelas, Eder' 'Fidalgo-Marijuan, Arkaitz' 'Baz\'an, Bego\~na' 'Urtiaga, Miren Karmele' 'Barandika, Gotzone' 'Lezama, Luis' 'Arriortua, Mar\'ia Isabel' _publ_section_title ; Cationic Mn 2+ /H + exchange leading a slow solid-state transformation of a 2D porphyrinic network at ambient conditions ; _journal_name_full 'Journal of Solid State Chemistry' _journal_page_first 161 _journal_page_last 167 _journal_paper_doi 10.1016/j.jssc.2017.01.012 _journal_volume 247 _journal_year 2017 _chemical_formula_moiety '0.25(C192 H104 Mn4 N16 O40), C2 O2' _chemical_formula_sum 'C50 H26 Mn N4 O12' _chemical_formula_weight 931.7 _space_group_IT_number 125 _space_group_name_Hall '-P 4a 2b' _space_group_name_H-M_alt 'P 4/n b m :2' _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 125 _symmetry_space_group_name_Hall '-P 4a 2b' _symmetry_space_group_name_H-M 'P 4/n b m :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.3102(4) _cell_length_b 22.3102(4) _cell_length_c 12.0095(3) _cell_measurement_reflns_used 6187 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.0626 _cell_measurement_theta_min 2.7979 _cell_measurement_wavelength 1.54184 _cell_volume 5977.7(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 46592 _diffrn_reflns_theta_full 72.47 _diffrn_reflns_theta_max 72.47 _diffrn_reflns_theta_min 2.8 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.239 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_correction_T_min 0.874 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.035 _exptl_crystal_density_meas 1.346(5) _exptl_crystal_density_method Flotation _exptl_crystal_description prism _exptl_crystal_F_000 1908 _exptl_crystal_size_max 0.1948 _exptl_crystal_size_mid 0.1282 _exptl_crystal_size_min 0.0919 _refine_diff_density_max 0.611 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 158 _refine_ls_number_reflns 3089 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0864 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1852P)^2^+1.4750P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2748 _refine_ls_wR_factor_ref 0.3017 _reflns_number_gt 1919 _reflns_number_total 3089 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL CELL 1.54184 22.310194 22.310194 12.009543 90 90 90 ZERR 4 0.000438 0.000438 0.00029 0 0 0 LATT 1 SYMM 0.5-Y,+X,+Z SYMM 0.5-X,0.5-Y,+Z SYMM +Y,0.5-X,+Z SYMM +X,0.5-Y,-Z SYMM 0.5-X,+Y,-Z SYMM +Y,+X,-Z SYMM 0.5-Y,0.5-X,-Z SFAC C H Mn N O UNIT 200 112 4 16 48 EADP C8 C12 EADP C8 C10 EADP C8 C18 EADP C8 C0AA EADP C2AA C11 EADP C2AA C14 EADP C2AA C15 EADP C2AA C16 L.S. 50 PLAN 20 TEMP -173 MORE -1 BOND $H CONF fmap 2 acta OMIT -2 145 OMIT 1 1 2 OMIT 4 2 0 OMIT 0 0 2 OMIT 4 0 2 OMIT 4 3 2 OMIT 10 10 12 OMIT 4 2 1 REM REM REM WGHT 0.185200 1.475000 FVAR 3.24485 MN1 3 0.500000 0.500000 0.500000 10.25000 0.05630 0.05630 = 0.05641 -0.00330 0.00330 -0.00419 O2AA 5 0.541953 0.458047 0.652210 10.50000 0.08528 0.08528 = 0.07787 0.00779 -0.00779 0.01199 AFIX 7 H2AA 2 0.514303 0.445099 0.698828 10.50000 -1.50000 AFIX 0 N3 4 0.449769 0.550231 0.603549 10.50000 0.06338 0.06338 = 0.06133 -0.00398 0.00398 -0.00143 N4 4 0.563737 0.563737 0.500000 10.50000 0.06567 0.06567 = 0.07640 -0.00771 0.00771 -0.00837 C5 1 0.463865 0.605400 0.646590 11.00000 0.07018 0.06422 = 0.06604 -0.01144 0.00569 -0.00144 C7 1 0.517162 0.636462 0.628553 11.00000 0.07408 0.06714 = 0.07772 -0.00996 0.00110 -0.00960 C8 1 0.525633 0.694696 0.687019 11.00000 0.09381 0.07247 = 0.07904 -0.01315 0.00110 -0.01228 C9 1 0.416991 0.625056 0.717966 11.00000 0.08098 0.07840 = 0.10000 -0.02265 0.01364 -0.00606 AFIX 43 H9 2 0.415964 0.661658 0.758343 11.00000 -1.20000 AFIX 0 PART 1 C10 1 0.492712 0.744009 0.667563 10.50000 0.09381 0.07247 = 0.07904 -0.01315 0.00110 -0.01228 AFIX 43 H10 2 0.460961 0.741455 0.615068 10.50000 -1.20000 AFIX 0 PART 0 C2AA 1 0.543953 0.802356 0.794043 11.00000 0.14425 0.07710 = 0.06668 -0.00916 0.00505 -0.03110 C13 1 0.562264 0.616635 0.559026 11.00000 0.07078 0.06300 = 0.10130 -0.00963 0.01270 -0.01052 PART 2 C14 1 0.580832 0.751182 0.831806 10.50000 0.14425 0.07710 = 0.06668 -0.00916 0.00505 -0.03110 AFIX 43 H14 2 0.610002 0.754876 0.889024 10.50000 -1.20000 AFIX 0 C16 1 0.532963 0.803969 0.678773 10.50000 0.14425 0.07710 = 0.06668 -0.00916 0.00505 -0.03110 AFIX 43 H16 2 0.530454 0.841329 0.641107 10.50000 -1.20000 AFIX 0 PART 0 C17 1 0.617351 0.648814 0.535445 11.00000 0.08472 0.07671 = 0.14407 -0.03622 0.02820 -0.02132 AFIX 43 H17 2 0.628641 0.686367 0.566277 11.00000 -1.20000 AFIX 0 PART 2 C18 1 0.569914 0.698108 0.778381 10.50000 0.09381 0.07247 = 0.07904 -0.01315 0.00110 -0.01228 AFIX 43 H18 2 0.591031 0.663057 0.800256 10.50000 -1.20000 AFIX 0 PART 0 O1 5 0.543590 0.908475 0.809514 11.00000 0.17742 0.06860 = 0.11402 -0.01706 -0.00586 -0.01551 C3 1 0.554660 0.861299 0.854643 11.00000 0.21657 0.08137 = 0.07357 -0.00294 -0.00829 -0.04972 PART 1 O4 5 0.556964 0.863210 0.951841 10.50000 0.09122 0.13899 = 0.05394 -0.01926 -0.01551 -0.02797 PART 0 PART 2 C0AA 1 0.525793 0.750821 0.620200 10.50000 0.09381 0.07247 = 0.07904 -0.01315 0.00110 -0.01228 AFIX 43 H0AA 2 0.521228 0.750320 0.541558 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C11 1 0.543099 0.749443 0.844700 10.50000 0.14425 0.07710 = 0.06668 -0.00916 0.00505 -0.03110 AFIX 43 H11 2 0.548120 0.748794 0.923243 10.50000 -1.20000 AFIX 0 C12 1 0.535438 0.695580 0.791080 10.50000 0.09381 0.07247 = 0.07904 -0.01315 0.00110 -0.01228 AFIX 43 H12 2 0.537475 0.659124 0.831780 10.50000 -1.20000 AFIX 0 C15 1 0.502512 0.797607 0.719309 10.50000 0.14425 0.07710 = 0.06668 -0.00916 0.00505 -0.03110 AFIX 43 H15 2 0.478826 0.831491 0.700360 10.50000 -1.20000 AFIX 0 PART 0 PART 2 O0AA 5 0.603908 0.852559 0.939286 10.50000 0.16633 0.07123 = 0.06489 -0.00445 0.00783 -0.01876 PART 0 O1AA 5 0.463428 0.963428 1.040655 10.50000 0.12472 0.12472 = 0.34191 0.00214 0.00214 0.00690 C2 1 0.493965 0.993965 0.960910 10.50000 0.18272 0.18272 = 0.16470 -0.03207 -0.03207 -0.08169 HKLF 4 REM REM R1 = 0.0864 for 1919 Fo > 4sig(Fo) and 0.1129 for all 3089 data REM 158 parameters refined using 0 restraints END WGHT 0.1854 1.4682 REM Highest difference peak 0.611, deepest hole -0.412, 1-sigma level 0.062 Q1 1 0.4878 0.9160 0.8213 11.00000 0.05 0.61 Q2 1 0.5656 0.7857 0.8354 11.00000 0.05 0.45 Q3 1 0.4610 0.5390 0.5718 10.50000 0.05 0.29 Q4 1 0.5621 0.8983 0.8918 11.00000 0.05 0.29 Q5 1 0.4565 0.5040 0.5088 11.00000 0.05 0.29 Q6 1 0.5408 0.4225 0.6392 11.00000 0.05 0.27 Q7 1 0.5381 0.8032 0.7589 11.00000 0.05 0.27 Q8 1 0.5342 0.6871 0.7146 11.00000 0.05 0.26 Q9 1 0.5549 0.4451 0.6962 10.50000 0.05 0.24 Q10 1 0.5224 0.8117 0.8060 11.00000 0.05 0.23 Q11 1 0.5478 0.8672 0.9887 11.00000 0.05 0.23 Q12 1 0.3821 0.6179 0.7070 10.50000 0.05 0.23 Q13 1 0.5646 0.5782 0.5646 11.00000 0.05 0.23 Q14 1 0.6421 0.8381 0.9679 11.00000 0.05 0.22 Q15 1 0.5644 0.4356 0.6082 10.50000 0.05 0.21 Q16 1 0.5757 0.6328 0.5461 11.00000 0.05 0.21 Q17 1 0.4162 0.6439 0.7361 11.00000 0.05 0.21 Q18 1 0.5019 0.9432 1.1016 11.00000 0.05 0.21 Q19 1 0.5219 0.4781 0.5828 10.50000 0.05 0.21 Q20 1 0.6286 0.8340 0.9811 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0864 for 1919 Fo > 4sig(Fo) and 0.1129 for all 3089 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.61, deepest hole -0.41 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1129 REM R1_gt = 0.0864 REM wR_ref = 0.3017 REM GOOF = 1.099 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 3089 REM Reflections_gt = 1919 REM Parameters = n/a REM Hole = -0.41 REM Peak = 0.61 REM Flack = n/a ; _cod_data_source_file JSSC-2017-247-161.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 4/n b m' _cod_database_code 1560620 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' 'y, x, -z' '-y+1/2, -x+1/2, -z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' '-x, y-1/2, z' 'x-1/2, -y, z' '-y, -x, z' 'y-1/2, x-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 Mn1 Mn 0.5 0.5 0.5 0.0563(4) Uani 1 4 d S T P . . O2AA O 0.54195(14) 0.45805(14) 0.6522(4) 0.0828(12) Uani 1 2 d S T P . . H2AA H 0.5143 0.4451 0.6988 0.124 Uiso 0.5 1 d GR . . . . N3 N 0.44977(14) 0.55023(14) 0.6035(4) 0.0627(10) Uani 1 2 d S T P . . N4 N 0.56374(15) 0.56374(15) 0.5 0.0692(11) Uani 1 2 d S T P A . C5 C 0.46386(18) 0.60540(18) 0.6466(3) 0.0668(10) Uani 1 1 d . . . . . C7 C 0.5172(2) 0.63646(19) 0.6286(4) 0.0730(11) Uani 1 1 d . . . A . C8 C 0.5256(2) 0.6947(2) 0.6870(4) 0.0818(9) Uani 1 1 d . . . . . C9 C 0.4170(2) 0.6251(2) 0.7180(4) 0.0865(13) Uani 1 1 d . . . . . H9 H 0.416 0.6617 0.7583 0.104 Uiso 1 1 calc R . . . . C10 C 0.4927(5) 0.7440(4) 0.6676(9) 0.0818(9) Uani 0.5 1 d . . . A 1 H10 H 0.461 0.7415 0.6151 0.098 Uiso 0.5 1 calc R . . A 1 C2AA C 0.5440(3) 0.8024(2) 0.7940(4) 0.0960(13) Uani 1 1 d . . . . . C13 C 0.5623(2) 0.61663(19) 0.5590(4) 0.0784(12) Uani 1 1 d . . . . . C14 C 0.5808(7) 0.7512(5) 0.8318(8) 0.0960(13) Uani 0.5 1 d . . . A 2 H14 H 0.61 0.7549 0.889 0.115 Uiso 0.5 1 calc R . . A 2 C16 C 0.5330(6) 0.8040(5) 0.6788(8) 0.0960(13) Uani 0.5 1 d . . . A 2 H16 H 0.5305 0.8413 0.6411 0.115 Uiso 0.5 1 calc R . . A 2 C17 C 0.6174(2) 0.6488(2) 0.5354(5) 0.1018(17) Uani 1 1 d . . . A . H17 H 0.6286 0.6864 0.5663 0.122 Uiso 1 1 calc R . . . . C18 C 0.5699(5) 0.6981(4) 0.7784(8) 0.0818(9) Uani 0.5 1 d . . . A 2 H18 H 0.591 0.6631 0.8003 0.098 Uiso 0.5 1 calc R . . A 2 O1 O 0.5436(2) 0.90848(17) 0.8095(4) 0.1200(15) Uani 1 1 d . . . . . C3 C 0.5547(4) 0.8613(3) 0.8546(4) 0.124(3) Uani 1 1 d . . . A . O4 O 0.5570(4) 0.8632(4) 0.9518(5) 0.095(2) Uani 0.5 1 d . . . A 1 C0AA C 0.5258(5) 0.7508(4) 0.6202(9) 0.0818(9) Uani 0.5 1 d . . . A 2 H0AA H 0.5212 0.7503 0.5416 0.098 Uiso 0.5 1 calc R . . A 2 C11 C 0.5431(6) 0.7494(5) 0.8447(9) 0.0960(13) Uani 0.5 1 d . . . A 1 H11 H 0.5481 0.7488 0.9232 0.115 Uiso 0.5 1 calc R . . A 1 C12 C 0.5354(5) 0.6956(4) 0.7911(8) 0.0818(9) Uani 0.5 1 d . . . A 1 H12 H 0.5375 0.6591 0.8318 0.098 Uiso 0.5 1 calc R . . A 1 C15 C 0.5025(6) 0.7976(5) 0.7193(8) 0.0960(13) Uani 0.5 1 d . . . A 1 H15 H 0.4788 0.8315 0.7004 0.115 Uiso 0.5 1 calc R . . A 1 O0AA O 0.6039(5) 0.8526(3) 0.9393(5) 0.101(2) Uani 0.5 1 d . . . A 2 O1AA O 0.4634(3) 0.9634(3) 1.0407(12) 0.197(4) Uani 1 2 d S T P . . C2 C 0.4940(5) 0.9940(5) 0.9609(16) 0.177(7) Uani 1 2 d S T 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 Mn1 0.0563(5) 0.0563(5) 0.0564(6) -0.0033(4) 0.0033(4) -0.0042(5) O2AA 0.0853(18) 0.0853(18) 0.078(3) 0.0078(15) -0.0078(15) 0.012(2) N3 0.0634(15) 0.0634(15) 0.061(2) -0.0040(14) 0.0040(14) -0.0014(19) N4 0.0657(16) 0.0657(16) 0.076(3) -0.0077(16) 0.0077(16) -0.008(2) C5 0.070(2) 0.064(2) 0.066(2) -0.0114(18) 0.0057(18) -0.0014(17) C7 0.074(2) 0.067(2) 0.078(2) -0.010(2) 0.001(2) -0.0096(19) C8 0.094(3) 0.0725(19) 0.0790(18) -0.0132(16) 0.0011(18) -0.0123(17) C9 0.081(3) 0.078(3) 0.100(3) -0.023(2) 0.014(2) -0.006(2) C10 0.094(3) 0.0725(19) 0.0790(18) -0.0132(16) 0.0011(18) -0.0123(17) C2AA 0.144(4) 0.077(2) 0.0667(19) -0.0092(15) 0.005(2) -0.031(2) C13 0.071(2) 0.063(2) 0.101(3) -0.010(2) 0.013(2) -0.0105(19) C14 0.144(4) 0.077(2) 0.0667(19) -0.0092(15) 0.005(2) -0.031(2) C16 0.144(4) 0.077(2) 0.0667(19) -0.0092(15) 0.005(2) -0.031(2) C17 0.085(3) 0.077(3) 0.144(5) -0.036(3) 0.028(3) -0.021(2) C18 0.094(3) 0.0725(19) 0.0790(18) -0.0132(16) 0.0011(18) -0.0123(17) O1 0.177(5) 0.069(2) 0.114(3) -0.017(2) -0.006(3) -0.016(2) C3 0.217(8) 0.081(4) 0.074(3) -0.003(3) -0.008(4) -0.050(4) O4 0.091(5) 0.139(6) 0.054(3) -0.019(4) -0.016(3) -0.028(5) C0AA 0.094(3) 0.0725(19) 0.0790(18) -0.0132(16) 0.0011(18) -0.0123(17) C11 0.144(4) 0.077(2) 0.0667(19) -0.0092(15) 0.005(2) -0.031(2) C12 0.094(3) 0.0725(19) 0.0790(18) -0.0132(16) 0.0011(18) -0.0123(17) C15 0.144(4) 0.077(2) 0.0667(19) -0.0092(15) 0.005(2) -0.031(2) O0AA 0.166(8) 0.071(4) 0.065(4) -0.004(3) 0.008(5) -0.019(5) O1AA 0.125(4) 0.125(4) 0.342(15) 0.002(6) 0.002(6) 0.007(5) C2 0.183(10) 0.183(10) 0.165(15) -0.032(6) -0.032(6) -0.082(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -3 3 -7 0.0938 -3.0027 2.9850 -6.9995 0.0025 -0.0887 0.9398 3 -3 7 0.1052 3.0027 -2.9850 6.9995 -0.0025 0.0887 -0.9398 -11 9 0 0.0441 -11.0179 8.9763 -0.0075 0.9336 -0.0356 0.2978 11 -9 0 0.0477 11.0179 -8.9763 0.0075 -0.9336 0.0356 -0.2978 -2 -1 8 0.0925 -2.0037 -0.9938 7.9959 0.3744 -0.0199 -0.9670 8 12 0 0.0561 7.9940 12.0102 0.0035 0.0897 0.9807 0.1510 5 -2 -7 0.0709 5.0087 -1.9983 -6.9942 -0.6124 0.0168 0.7538 -10 -10 -1 0.0508 -9.9973 -10.0158 -1.0046 0.0559 -0.9837 0.0315 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 O2AA Mn1 O2AA 180.00(13) 9_666 . N3 Mn1 O2AA 87.79(17) . . N3 Mn1 O2AA 87.79(17) 9_666 9_666 N3 Mn1 O2AA 92.21(17) . 9_666 N3 Mn1 O2AA 92.21(17) 9_666 . N3 Mn1 N3 179.9990(10) 9_666 . N4 Mn1 O2AA 90 . 9_666 N4 Mn1 O2AA 90.0000(10) . . N4 Mn1 O2AA 90.0010(10) 9_666 9_666 N4 Mn1 O2AA 90 9_666 . N4 Mn1 N3 90.0010(10) 9_666 . N4 Mn1 N3 89.9990(10) . 9_666 N4 Mn1 N3 90 . . N4 Mn1 N3 90 9_666 9_666 N4 Mn1 N4 179.9990(10) 9_666 . Mn1 O2AA H2AA 111.1 . . C5 N3 Mn1 127.2(2) 15_665 . C5 N3 Mn1 127.2(2) . . C5 N3 C5 105.6(4) . 15_665 C13 N4 Mn1 126.1(2) 7_556 . C13 N4 Mn1 126.1(2) . . C13 N4 C13 107.8(5) . 7_556 N3 C5 C7 125.7(4) . . N3 C5 C9 109.6(4) . . C7 C5 C9 124.6(4) . . C5 C7 C8 118.0(4) . . C13 C7 C5 123.8(4) . . C13 C7 C8 118.2(4) . . C10 C8 C7 124.3(6) . . C10 C8 C18 116.9(7) . . C18 C8 C7 118.7(6) . . C18 C8 C0AA 110.8(6) . . C0AA C8 C7 118.7(5) . . C12 C8 C7 120.0(6) . . C12 C8 C10 104.6(7) . . C12 C8 C0AA 121.2(7) . . C5 C9 H9 126.2 . . C9 C9 C5 107.6(2) 15_665 . C9 C9 H9 126.2 15_665 . C8 C10 H10 118.3 . . C8 C10 C15 123.4(10) . . C15 C10 H10 118.3 . . C14 C2AA C3 115.7(6) . . C16 C2AA C14 114.8(8) . . C16 C2AA C3 118.4(6) . . C11 C2AA C16 118.1(7) . . C11 C2AA C3 123.5(6) . . C15 C2AA C14 123.2(8) . . C15 C2AA C3 121.0(8) . . C15 C2AA C11 103.6(8) . . N4 C13 C7 127.1(4) . . N4 C13 C17 107.7(4) . . C7 C13 C17 125.2(4) . . C2AA C14 H14 122.4 . . C18 C14 C2AA 115.2(10) . . C18 C14 H14 122.4 . . C2AA C16 H16 120.1 . . C0AA C16 C2AA 119.8(9) . . C0AA C16 H16 120.1 . . C13 C17 H17 125.8 . . C17 C17 C13 108.4(3) 7_556 . C17 C17 H17 125.8 7_556 . C8 C18 H18 119.6 . . C14 C18 C8 120.8(10) . . C14 C18 H18 119.6 . . O1 C3 C2AA 120.4(5) . . O1 C3 O0AA 124.3(6) . . O4 C3 C2AA 121.1(6) . . O4 C3 O1 115.1(7) . . O4 C3 O0AA 45.6(5) . . O0AA C3 C2AA 108.9(6) . . C8 C0AA H0AA 121.8 . . C16 C0AA C8 116.5(9) . . C16 C0AA H0AA 121.8 . . C2AA C11 H11 117.8 . . C2AA C11 C12 124.4(9) . . C12 C11 H11 117.8 . . C8 C12 C11 119.8(9) . . C8 C12 H12 120.1 . . C11 C12 H12 120.1 . . C10 C15 H15 119.9 . . C2AA C15 C10 120.2(11) . . C2AA C15 H15 119.9 . . O1AA C2 O1AA 136.0(13) 9_677 . C2 C2 O1AA 67(2) 9_677 . C2 C2 O1AA 68.7(15) 9_677 9_677 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 O2AA 2.257(4) . Mn1 O2AA 2.257(4) 9_666 Mn1 N3 2.015(4) . Mn1 N3 2.014(4) 9_666 Mn1 N4 2.011(5) 9_666 Mn1 N4 2.011(5) . O2AA H2AA 0.8817 . N3 C5 1.372(5) . N3 C5 1.372(5) 15_665 N4 C13 1.377(5) . N4 C13 1.377(5) 7_556 C5 C7 1.393(6) . C5 C9 1.422(6) . C7 C8 1.489(6) . C7 C13 1.380(6) . C8 C10 1.343(11) . C8 C18 1.478(12) . C8 C0AA 1.487(11) . C8 C12 1.269(10) . C9 C9 1.327(10) 15_665 C9 H9 0.95 . C10 H10 0.95 . C10 C15 1.365(13) . C2AA C14 1.479(14) . C2AA C16 1.406(11) . C2AA C3 1.522(7) . C2AA C11 1.328(12) . C2AA C15 1.293(12) . C13 C17 1.451(6) . C14 H14 0.95 . C14 C18 1.369(13) . C16 H16 0.95 . C16 C0AA 1.388(13) . C17 C17 1.308(10) 7_556 C17 H17 0.95 . C18 H18 0.95 . O1 C3 1.209(7) . C3 O4 1.169(8) . C3 O0AA 1.509(12) . C0AA H0AA 0.95 . C11 H11 0.95 . C11 C12 1.374(13) . C12 H12 0.95 . C15 H15 0.95 . O1AA C2 1.344(19) 9_677 O1AA C2 1.36(2) . C2 O1AA 1.344(19) 9_677 C2 C2 1.01(3) 9_677 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 Mn1 N3 C5 C7 -1.9(7) . . . . Mn1 N3 C5 C9 -178.8(3) . . . . Mn1 N4 C13 C7 -0.5(6) . . . . Mn1 N4 C13 C17 179.5(3) . . . . O2AA Mn1 N3 C5 -90.3(4) 9_666 . . . O2AA Mn1 N3 C5 -89.6(4) . . . 15_665 O2AA Mn1 N3 C5 89.7(4) . . . . O2AA Mn1 N3 C5 90.4(4) 9_666 . . 15_665 O2AA Mn1 N4 C13 93.7(3) . . . 7_556 O2AA Mn1 N4 C13 -86.3(3) 9_666 . . 7_556 O2AA Mn1 N4 C13 -86.3(3) . . . . O2AA Mn1 N4 C13 93.7(3) 9_666 . . . N3 Mn1 N4 C13 -178.5(3) 9_666 . . . N3 Mn1 N4 C13 1.5(3) . . . . N3 Mn1 N4 C13 1.4(3) 9_666 . . 7_556 N3 Mn1 N4 C13 -178.6(3) . . . 7_556 N3 C5 C7 C8 -177.0(4) . . . . N3 C5 C7 C13 3.5(8) . . . . N3 C5 C9 C9 -0.4(4) . . . 15_665 N4 Mn1 N3 C5 179.7(4) 9_666 . . . N4 Mn1 N3 C5 -0.3(4) . . . . N4 Mn1 N3 C5 -179.6(4) . . . 15_665 N4 Mn1 N3 C5 0.3(4) 9_666 . . 15_665 N4 C13 C17 C17 1.4(9) . . . 7_556 C5 N3 C5 C7 177.5(3) 15_665 . . . C5 N3 C5 C9 0.7(6) 15_665 . . . C5 C7 C8 C10 -66.0(8) . . . . C5 C7 C8 C18 109.3(7) . . . . C5 C7 C8 C0AA -111.1(7) . . . . C5 C7 C8 C12 72.3(8) . . . . C5 C7 C13 N4 -2.3(8) . . . . C5 C7 C13 C17 177.8(5) . . . . C7 C5 C9 C9 -177.3(4) . . . 15_665 C7 C8 C10 C15 -177.7(8) . . . . C7 C8 C18 C14 177.6(8) . . . . C7 C8 C0AA C16 179.1(9) . . . . C7 C8 C12 C11 -179.9(9) . . . . C7 C13 C17 C17 -178.6(7) . . . 7_556 C8 C7 C13 N4 178.3(4) . . . . C8 C7 C13 C17 -1.7(8) . . . . C8 C10 C15 C2AA -2.4(17) . . . . C9 C5 C7 C8 -0.7(7) . . . . C9 C5 C7 C13 179.9(5) . . . . C10 C8 C18 C14 -6.8(14) . . . . C10 C8 C0AA C16 69.0(12) . . . . C10 C8 C12 C11 -34.5(13) . . . . C2AA C14 C18 C8 2.2(15) . . . . C2AA C16 C0AA C8 4.6(17) . . . . C2AA C11 C12 C8 -3(2) . . . . C13 N4 C13 C7 179.5(6) 7_556 . . . C13 N4 C13 C17 -0.5(3) 7_556 . . . C13 C7 C8 C10 113.4(8) . . . . C13 C7 C8 C18 -71.3(8) . . . . C13 C7 C8 C0AA 68.3(8) . . . . C13 C7 C8 C12 -108.2(8) . . . . C14 C2AA C16 C0AA 34.6(15) . . . . C14 C2AA C3 O1 154.9(8) . . . . C14 C2AA C3 O4 -47.1(12) . . . . C14 C2AA C3 O0AA 1.9(9) . . . . C14 C2AA C11 C12 -90.0(17) . . . . C14 C2AA C15 C10 -2.9(15) . . . . C16 C2AA C14 C18 -37.9(13) . . . . C16 C2AA C3 O1 12.9(12) . . . . C16 C2AA C3 O4 170.9(10) . . . . C16 C2AA C3 O0AA -140.1(9) . . . . C16 C2AA C11 C12 3.7(19) . . . . C16 C2AA C15 C10 84.5(16) . . . . C18 C8 C10 C15 7.0(14) . . . . C18 C8 C0AA C16 -38.4(13) . . . . C18 C8 C12 C11 83.1(15) . . . . C3 C2AA C14 C18 178.6(8) . . . . C3 C2AA C16 C0AA 177.0(10) . . . . C3 C2AA C11 C12 -177.8(11) . . . . C3 C2AA C15 C10 -178.6(8) . . . . C0AA C8 C10 C15 -83.2(12) . . . . C0AA C8 C18 C14 35.0(12) . . . . C0AA C8 C12 C11 3.6(15) . . . . C11 C2AA C14 C18 66.3(13) . . . . C11 C2AA C16 C0AA -4.5(17) . . . . C11 C2AA C3 O1 -165.6(10) . . . . C11 C2AA C3 O4 -7.5(14) . . . . C11 C2AA C3 O0AA 41.4(11) . . . . C11 C2AA C15 C10 -34.8(13) . . . . C12 C8 C10 C15 38.9(13) . . . . C12 C8 C18 C14 -80.8(15) . . . . C12 C8 C0AA C16 -4.4(15) . . . . C15 C2AA C14 C18 2.7(14) . . . . C15 C2AA C16 C0AA -78.4(15) . . . . C15 C2AA C3 O1 -29.1(11) . . . . C15 C2AA C3 O4 129.0(10) . . . . C15 C2AA C3 O0AA 177.9(8) . . . . C15 C2AA C11 C12 39.6(16) . . . . C2 O1AA C2 O1AA 0.000(2) 9_677 . . 9_677 loop_ _solvent_mask_void_nr _solvent_mask_void_average_x _solvent_mask_void_average_y _solvent_mask_void_average_z _solvent_mask_void_volume _solvent_mask_void_count_electrons _solvent_mask_void_content 1 -0.250 0.250 -0.544 833.3 236.9 ' DMF and water of crystallisation' 2 0.250 0.750 -0.718 833.3 236.9 ' DMF and water of crystallisation' 3 0.250 0.250 -0.661 227.2 62.9 ' DMF and water of crystallisation' 4 0.750 0.750 -0.948 227.2 62.6 ' DMF and water of crystallisation'