#------------------------------------------------------------------------------ #$Date: 2017-03-16 05:01:06 +0200 (Thu, 16 Mar 2017) $ #$Revision: 194283 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/78/7227860.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_7227860 loop_ _publ_author_name 'Rodriguez-Dieguez, Antonio' 'Perez-Ya\~nez, Sonia' 'Ruiz-Rubio, Leire' 'Seco, Jos\'e M' 'Cepeda, Javier' _publ_section_title ; From isolated to 2D Coordination Polymers based on 6-aminonicotinate and 3d-Metal Ions: Towards Field-Induced Single-Ion-Magnets ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE00234C _journal_year 2017 _chemical_formula_moiety 'C12 H16 Co N4 O7, 2(H2 O)' _chemical_formula_sum 'C12 H20 Co N4 O9' _chemical_formula_weight 423.25 _chemical_name_systematic Poly{[triaqua(mu-6-aminopyridine-3-carboxylato-kN:kO)(6-aminopyridine-3-carboxylato-kO')cobalt(II)]dihydrate} _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014 _audit_update_record ; 2017-02-02 deposited with the CCDC. 2017-03-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8950(5) _cell_length_b 7.3902(2) _cell_length_c 18.7683(5) _cell_measurement_reflns_used 11388 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.052 _cell_measurement_theta_min 2.027 _cell_volume 1649.85(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'Sir92 (Altomare et al., 1993)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.2439 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_unetI/netI 0.0599 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 11388 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.052 _diffrn_reflns_theta_min 2.027 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) 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 'pale pink' _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method none _exptl_crystal_description plate _exptl_crystal_F_000 876 _exptl_crystal_preparation ', Magnetic properties' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.391 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.068 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 3244 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0227P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.0726 _reflns_Friedel_coverage 0.726 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 2948 _reflns_number_total 3244 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce00234c2.cif _cod_data_source_block Compound3 _cod_database_code 7227860 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL a20150346_Co6ampyc3_3 in P21 #4 CELL 0.71073 11.8950 7.3902 18.7683 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0002 0.0005 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CO UNIT 48 80 16 36 4 MERG 2 TWIN EQIV $1 X,Y-1,Z EQIV $2 X-1/2,-Y+1/2,-Z-2 EQIV $3 X-1/2,-Y+3/2,-Z-2 EQIV $4 -X+2,Y+1/2,-Z-3/2 EQIV $5 -X+3,Y+1/2,-Z-3/2 EQIV $6 X,Y+1,Z EQIV $7 X-1/2,-Y+3/2,-Z-2 EQIV $8 X+1,Y,Z HTAB O1W O5W_$1 HTAB O1W N1B_$2 HTAB O2W O72B HTAB O2W O72A HTAB O3W N1B_$3 HTAB O3W O4W HTAB O4W O72A_$6 HTAB O4W O72A_$4 HTAB O5W O72B_$5 HTAB O5W O71B HTAB O5W O3W HTAB N8A O71A HTAB N8A O5W_$7 HTAB N8B O4W_$8 FMAP 2 PLAN 20 ACTA BOND $H L.S. 10 WGHT 0.022700 BASF -0.00060 FVAR 2.26633 CO1 5 1.250915 0.370739 -0.908358 11.00000 0.01088 0.00743 = 0.00834 -0.00011 -0.00003 -0.00048 N1A 3 1.266048 0.366205 -1.022213 11.00000 0.00781 0.00905 = 0.00998 0.00081 -0.00032 -0.00107 C2A 1 1.369234 0.316781 -1.045726 11.00000 0.00674 0.00661 = 0.01469 0.00078 -0.00425 -0.00056 AFIX 43 H2A 2 1.418714 0.266984 -1.012749 11.00000 -1.20000 AFIX 0 C3A 1 1.406309 0.334897 -1.115007 11.00000 0.01508 0.00560 = 0.00868 -0.00115 0.00029 -0.00046 C5A 1 1.224714 0.454807 -1.142829 11.00000 0.01328 0.00912 = 0.01360 0.00199 -0.00197 -0.00090 AFIX 43 H5A 2 1.173569 0.501128 -1.175570 11.00000 -1.20000 AFIX 0 C6A 1 1.192395 0.431235 -1.070867 11.00000 0.01170 0.00423 = 0.01354 0.00062 -0.00019 -0.00083 C7A 1 1.022026 0.219919 -0.864291 11.00000 0.01574 0.00564 = 0.01292 -0.00221 0.00214 0.00373 O71A 4 1.080099 0.308115 -0.909537 11.00000 0.01211 0.01184 = 0.01107 0.00444 0.00097 -0.00141 N8A 3 1.088292 0.473745 -1.049371 11.00000 0.01110 0.01814 = 0.01111 0.00405 -0.00019 0.00334 AFIX 93 H8A1 2 1.069503 0.459518 -1.005479 11.00000 -1.20000 H8A2 2 1.040256 0.515260 -1.079463 11.00000 -1.20000 AFIX 0 N1B 3 1.724546 0.620025 -0.970813 11.00000 0.01148 0.00964 = 0.01369 0.00074 0.00029 0.00038 C2B 1 1.626799 0.550857 -0.947061 11.00000 0.01683 0.00742 = 0.01258 -0.00347 -0.00415 0.00371 AFIX 43 H2B 2 1.567942 0.541290 -0.979460 11.00000 -1.20000 AFIX 0 C3B 1 1.607297 0.492808 -0.877909 11.00000 0.01614 0.00422 = 0.01348 -0.00237 0.00017 -0.00060 C4B 1 1.698317 0.505797 -0.830364 11.00000 0.01679 0.00802 = 0.01043 -0.00243 0.00006 0.00264 AFIX 43 H4B 2 1.690291 0.466105 -0.783617 11.00000 -1.20000 AFIX 0 C5B 1 1.797762 0.575987 -0.852417 11.00000 0.01477 0.01292 = 0.01445 -0.00031 -0.00321 -0.00104 AFIX 43 H5B 2 1.858028 0.584235 -0.821017 11.00000 -1.20000 AFIX 0 C6B 1 1.809131 0.636790 -0.923843 11.00000 0.01557 0.00462 = 0.01745 -0.00219 0.00204 0.00289 C7B 1 1.494252 0.424467 -0.857085 11.00000 0.01758 0.00350 = 0.01713 -0.00285 -0.00101 0.00170 O71B 4 1.416617 0.451580 -0.902669 11.00000 0.01367 0.01718 = 0.01010 0.00257 -0.00271 -0.00214 O72B 4 1.479921 0.348021 -0.797932 11.00000 0.01446 0.01894 = 0.01493 0.00275 -0.00173 -0.00440 N8B 3 1.906994 0.707799 -0.947804 11.00000 0.01308 0.01961 = 0.01411 -0.00088 0.00025 -0.00342 AFIX 93 H8B1 2 1.913240 0.740211 -0.991634 11.00000 -1.20000 H8B2 2 1.962917 0.720495 -0.919195 11.00000 -1.20000 AFIX 0 O1W 4 1.290705 0.093023 -0.906566 11.00000 0.03156 0.01147 = 0.01229 -0.00281 -0.00898 0.00457 O2W 4 1.251454 0.367301 -0.796845 11.00000 0.01394 0.01281 = 0.01233 -0.00114 0.00040 -0.00315 O3W 4 1.214428 0.649204 -0.906341 11.00000 0.02363 0.01103 = 0.01174 0.00126 0.00449 0.00368 O4W 4 1.057757 0.798191 -0.818344 11.00000 0.02243 0.01036 = 0.01166 0.00117 0.00413 -0.00020 O5W 4 1.425437 0.853877 -0.837068 11.00000 0.02473 0.01060 = 0.01723 0.00056 -0.00615 -0.00067 C4A 1 1.329866 0.410148 -1.164192 11.00000 0.01315 0.00853 = 0.00899 -0.00052 -0.00057 0.00014 AFIX 43 H4A 2 1.351609 0.429072 -1.211202 11.00000 -1.20000 AFIX 0 O72A 4 1.057251 0.176549 -0.802733 11.00000 0.01338 0.01535 = 0.00795 0.00250 -0.00145 -0.00108 AFIX 1 H11W 2 1.327062 0.030520 -0.876266 11.00000 -1.50000 H12W 2 1.279811 0.021126 -0.941275 11.00000 -1.50000 H21W 2 1.317109 0.332929 -0.785135 11.00000 -1.50000 H22W 2 1.209041 0.279332 -0.784995 11.00000 -1.50000 H31W 2 1.203217 0.704719 -0.945287 11.00000 -1.50000 H32W 2 1.169596 0.699594 -0.876892 11.00000 -1.50000 H41W 2 1.068043 0.910747 -0.810932 11.00000 -1.50000 H42W 2 1.026853 0.760170 -0.780260 11.00000 -1.50000 H51W 2 1.447558 0.841691 -0.794286 11.00000 -1.50000 H52W 2 1.390372 0.755990 -0.846085 11.00000 -1.50000 AFIX 0 HKLF 4 REM a20150346_Co6ampyc3_3 in P21 #4 REM R1 = 0.0334 for 2948 Fo > 4sig(Fo) and 0.0393 for all 3244 data REM 236 parameters refined using 0 restraints END WGHT 0.0227 0.0000 REM Highest difference peak 0.391, deepest hole -0.389, 1-sigma level 0.068 Q1 1 1.2455 0.3794 -0.9735 11.00000 0.05 0.39 Q2 1 1.7427 0.6148 -1.0172 11.00000 0.05 0.30 Q3 1 1.6182 0.5497 -0.9041 11.00000 0.05 0.30 Q4 1 1.0304 0.3725 -0.7943 11.00000 0.05 0.24 Q5 1 1.2631 0.3775 -0.8503 11.00000 0.05 0.24 Q6 1 1.9163 0.5609 -0.8122 11.00000 0.05 0.23 Q7 1 1.4071 0.3839 -1.0888 11.00000 0.05 0.22 Q8 1 1.2993 0.4941 -0.9622 11.00000 0.05 0.22 Q9 1 1.2011 0.1128 -0.8236 11.00000 0.05 0.21 Q10 1 1.7860 0.3337 -0.7619 11.00000 0.05 0.21 Q11 1 1.0520 0.0456 -0.8186 11.00000 0.05 0.21 Q12 1 1.2560 0.4689 -1.2268 11.00000 0.05 0.21 Q13 1 1.2522 -0.1255 -0.8432 11.00000 0.05 0.21 Q14 1 1.3659 0.4383 -0.9187 11.00000 0.05 0.21 Q15 1 1.4978 0.4813 -0.7510 11.00000 0.05 0.20 Q16 1 1.2321 0.1836 -0.9715 11.00000 0.05 0.20 Q17 1 1.2201 0.6474 -1.0167 11.00000 0.05 0.20 Q18 1 1.2168 0.0630 -1.0001 11.00000 0.05 0.20 Q19 1 1.3814 0.0302 -0.9122 11.00000 0.05 0.20 Q20 1 1.4060 0.5032 -1.2869 11.00000 0.05 0.20 ; _shelx_res_checksum 12681 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+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 Co1 Co 1.25092(5) 0.37074(6) -0.90836(2) 0.00888(14) Uani 1 1 d . . N1A N 1.2660(3) 0.3662(4) -1.02221(13) 0.0089(7) Uani 1 1 d . . C2A C 1.3692(3) 0.3168(5) -1.04573(19) 0.0093(8) Uani 1 1 d . . H2A H 1.4187 0.2670 -1.0127 0.011 Uiso 1 1 calc R U C3A C 1.4063(3) 0.3349(5) -1.11501(17) 0.0098(8) Uani 1 1 d . . C5A C 1.2247(3) 0.4548(5) -1.14283(17) 0.0120(9) Uani 1 1 d . . H5A H 1.1736 0.5011 -1.1756 0.014 Uiso 1 1 calc R U C6A C 1.1924(3) 0.4312(5) -1.07087(18) 0.0098(8) Uani 1 1 d . . C7A C 1.0220(4) 0.2199(5) -0.86429(18) 0.0114(8) Uani 1 1 d . . O71A O 1.0801(2) 0.3081(3) -0.90954(12) 0.0117(6) Uani 1 1 d . . N8A N 1.0883(3) 0.4737(4) -1.04937(15) 0.0135(8) Uani 1 1 d . . H8A1 H 1.0695 0.4595 -1.0055 0.016 Uiso 1 1 calc R U H8A2 H 1.0403 0.5153 -1.0795 0.016 Uiso 1 1 calc R U N1B N 1.7245(3) 0.6200(4) -0.97081(15) 0.0116(8) Uani 1 1 d . . C2B C 1.6268(4) 0.5509(5) -0.94706(18) 0.0123(9) Uani 1 1 d . . H2B H 1.5679 0.5413 -0.9795 0.015 Uiso 1 1 calc R U C3B C 1.6073(4) 0.4928(5) -0.87791(18) 0.0113(9) Uani 1 1 d . . C4B C 1.6983(4) 0.5058(5) -0.83036(18) 0.0117(9) Uani 1 1 d . . H4B H 1.6903 0.4661 -0.7836 0.014 Uiso 1 1 calc R U C5B C 1.7978(4) 0.5760(5) -0.85242(18) 0.0140(9) Uani 1 1 d . . H5B H 1.8580 0.5842 -0.8210 0.017 Uiso 1 1 calc R U C6B C 1.8091(4) 0.6368(5) -0.92384(18) 0.0125(8) Uani 1 1 d . . C7B C 1.4943(4) 0.4245(5) -0.85708(18) 0.0127(9) Uani 1 1 d . . O71B O 1.4166(2) 0.4516(4) -0.90267(11) 0.0136(6) Uani 1 1 d . . O72B O 1.4799(2) 0.3480(4) -0.79793(12) 0.0161(6) Uani 1 1 d . . N8B N 1.9070(3) 0.7078(4) -0.94780(16) 0.0156(8) Uani 1 1 d . . H8B1 H 1.9132 0.7402 -0.9916 0.019 Uiso 1 1 calc R U H8B2 H 1.9629 0.7205 -0.9192 0.019 Uiso 1 1 calc R U O1W O 1.2907(3) 0.0930(3) -0.90657(12) 0.0184(7) Uani 1 1 d . . O2W O 1.2515(2) 0.3673(3) -0.79684(11) 0.0130(6) Uani 1 1 d . . O3W O 1.2144(2) 0.6492(3) -0.90634(12) 0.0155(6) Uani 1 1 d . . O4W O 1.0578(2) 0.7982(4) -0.81834(12) 0.0148(7) Uani 1 1 d . . O5W O 1.4254(2) 0.8539(4) -0.83707(12) 0.0175(7) Uani 1 1 d . . C4A C 1.3299(4) 0.4101(5) -1.16419(17) 0.0102(8) Uani 1 1 d . . H4A H 1.3516 0.4291 -1.2112 0.012 Uiso 1 1 calc R U O72A O 1.0573(2) 0.1765(3) -0.80273(11) 0.0122(6) Uani 1 1 d . . H11W H 1.3271 0.0305 -0.8763 0.018 Uiso 1 1 d . U H12W H 1.2798 0.0211 -0.9413 0.018 Uiso 1 1 d . U H21W H 1.3171 0.3329 -0.7851 0.018 Uiso 1 1 d . U H22W H 1.2090 0.2793 -0.7850 0.018 Uiso 1 1 d . U H31W H 1.2032 0.7047 -0.9453 0.018 Uiso 1 1 d . U H32W H 1.1696 0.6996 -0.8769 0.018 Uiso 1 1 d . U H41W H 1.0680 0.9107 -0.8109 0.018 Uiso 1 1 d . U H42W H 1.0269 0.7602 -0.7803 0.018 Uiso 1 1 d . U H51W H 1.4476 0.8417 -0.7943 0.018 Uiso 1 1 d . U H52W H 1.3904 0.7560 -0.8461 0.018 Uiso 1 1 d . U 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 0.0109(3) 0.0074(2) 0.0083(2) -0.00011(17) 0.0000(2) -0.0005(3) N1A 0.008(2) 0.0091(15) 0.0100(14) 0.0008(11) -0.0003(13) -0.0011(18) C2A 0.007(2) 0.0066(19) 0.0147(17) 0.0008(14) -0.0043(16) -0.0006(17) C3A 0.015(2) 0.0056(19) 0.0087(16) -0.0012(14) 0.0003(15) -0.0005(17) C5A 0.013(3) 0.0091(19) 0.0136(17) 0.0020(14) -0.0020(16) -0.0009(18) C6A 0.012(2) 0.0042(18) 0.0135(17) 0.0006(14) -0.0002(16) -0.0008(17) C7A 0.016(2) 0.0056(18) 0.0129(18) -0.0022(14) 0.0021(17) 0.0037(18) O71A 0.0121(15) 0.0118(14) 0.0111(12) 0.0044(10) 0.0010(12) -0.0014(12) N8A 0.011(2) 0.0181(18) 0.0111(15) 0.0040(13) -0.0002(14) 0.0033(16) N1B 0.011(2) 0.0096(16) 0.0137(15) 0.0007(12) 0.0003(13) 0.0004(15) C2B 0.017(2) 0.0074(19) 0.0126(18) -0.0035(15) -0.0041(17) 0.0037(19) C3B 0.016(2) 0.0042(18) 0.0135(17) -0.0024(14) 0.0002(17) -0.0006(18) C4B 0.017(2) 0.008(2) 0.0104(17) -0.0024(14) 0.0001(16) 0.0026(19) C5B 0.015(2) 0.013(2) 0.0145(18) -0.0003(16) -0.0032(17) -0.0010(19) C6B 0.016(2) 0.0046(18) 0.0175(18) -0.0022(16) 0.0020(17) 0.0029(18) C7B 0.018(2) 0.0035(18) 0.0171(18) -0.0028(15) -0.0010(17) 0.0017(19) O71B 0.0137(16) 0.0172(15) 0.0101(12) 0.0026(11) -0.0027(12) -0.0021(13) O72B 0.0145(16) 0.0189(16) 0.0149(12) 0.0027(11) -0.0017(12) -0.0044(14) N8B 0.013(2) 0.0196(19) 0.0141(16) -0.0009(14) 0.0003(15) -0.0034(17) O1W 0.0316(19) 0.0115(14) 0.0123(12) -0.0028(10) -0.0090(12) 0.0046(13) O2W 0.0139(15) 0.0128(13) 0.0123(11) -0.0011(9) 0.0004(12) -0.0031(19) O3W 0.0236(18) 0.0110(13) 0.0117(12) 0.0013(10) 0.0045(12) 0.0037(13) O4W 0.0224(18) 0.0104(14) 0.0117(13) 0.0012(11) 0.0041(12) -0.0002(14) O5W 0.0247(18) 0.0106(15) 0.0172(13) 0.0006(11) -0.0061(12) -0.0007(15) C4A 0.013(2) 0.009(2) 0.0090(16) -0.0005(14) -0.0006(15) 0.0001(17) O72A 0.0134(15) 0.0153(15) 0.0080(11) 0.0025(10) -0.0015(11) -0.0011(13) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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_3 O71B Co1 O71A 175.33(10) . O71B Co1 O2W 87.07(10) . O71A Co1 O2W 90.62(10) . O71B Co1 O3W 85.00(11) . O71A Co1 O3W 90.93(11) . O2W Co1 O3W 89.69(9) . O71B Co1 O1W 93.82(11) . O71A Co1 O1W 90.16(11) . O2W Co1 O1W 88.37(9) . O3W Co1 O1W 177.78(10) . O71B Co1 N1A 88.62(11) . O71A Co1 N1A 93.89(11) . O2W Co1 N1A 174.76(12) . O3W Co1 N1A 92.90(10) . O1W Co1 N1A 88.96(10) . C6A N1A C2A 117.5(3) . C6A N1A Co1 127.8(3) . C2A N1A Co1 113.9(2) . N1A C2A C3A 124.8(4) . N1A C2A H2A 117.6 . C3A C2A H2A 117.6 . C2A C3A C4A 116.7(4) . C2A C3A C7A 121.1(3) 3_553 C4A C3A C7A 122.2(3) 3_553 C4A C5A C6A 120.2(4) . C4A C5A H5A 119.9 . C6A C5A H5A 119.9 . N8A C6A N1A 118.6(3) . N8A C6A C5A 120.6(3) . N1A C6A C5A 120.8(4) . O72A C7A O71A 123.8(4) . O72A C7A C3A 118.3(3) 3_453 O71A C7A C3A 117.9(3) 3_453 C7A O71A Co1 129.4(2) . C6A N8A H8A1 120.0 . C6A N8A H8A2 120.0 . H8A1 N8A H8A2 120.0 . C6B N1B C2B 117.7(3) . N1B C2B C3B 124.9(4) . N1B C2B H2B 117.6 . C3B C2B H2B 117.6 . C2B C3B C4B 116.4(4) . C2B C3B C7B 120.1(4) . C4B C3B C7B 123.5(3) . C5B C4B C3B 120.3(3) . C5B C4B H4B 119.9 . C3B C4B H4B 119.9 . C4B C5B C6B 119.5(4) . C4B C5B H5B 120.3 . C6B C5B H5B 120.3 . N1B C6B N8B 117.5(3) . N1B C6B C5B 121.3(4) . N8B C6B C5B 121.2(4) . O72B C7B O71B 124.4(4) . O72B C7B C3B 120.4(4) . O71B C7B C3B 115.1(3) . C7B O71B Co1 133.0(2) . C6B N8B H8B1 120.0 . C6B N8B H8B2 120.0 . H8B1 N8B H8B2 120.0 . Co1 O1W H11W 130.8 . Co1 O1W H12W 124.2 . H11W O1W H12W 104.5 . Co1 O2W H21W 105.4 . Co1 O2W H22W 105.6 . H21W O2W H22W 104.4 . Co1 O3W H31W 119.3 . Co1 O3W H32W 124.6 . H31W O3W H32W 104.4 . H41W O4W H42W 104.3 . H51W O5W H52W 104.4 . C5A C4A C3A 119.9(3) . C5A C4A H4A 120.1 . C3A C4A H4A 120.1 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 O71B 2.062(3) . Co1 O71A 2.084(3) . Co1 O2W 2.093(2) . Co1 O3W 2.104(3) . Co1 O1W 2.107(3) . Co1 N1A 2.145(3) . N1A C6A 1.354(5) . N1A C2A 1.354(5) . C2A C3A 1.380(5) . C2A H2A 0.9300 . C3A C4A 1.410(5) . C3A C7A 1.487(6) 3_553 C5A C4A 1.354(6) . C5A C6A 1.415(5) . C5A H5A 0.9300 . C6A N8A 1.340(5) . C7A O72A 1.270(4) . C7A O71A 1.274(4) . C7A C3A 1.486(6) 3_453 N8A H8A1 0.8600 . N8A H8A2 0.8600 . N1B C6B 1.343(5) . N1B C2B 1.346(5) . C2B C3B 1.386(5) . C2B H2B 0.9300 . C3B C4B 1.406(5) . C3B C7B 1.489(6) . C4B C5B 1.356(6) . C4B H4B 0.9300 . C5B C6B 1.420(5) . C5B H5B 0.9300 . C6B N8B 1.354(5) . C7B O72B 1.257(4) . C7B O71B 1.275(4) . N8B H8B1 0.8600 . N8B H8B2 0.8600 . O1W H11W 0.8508 . O1W H12W 0.8506 . O2W H21W 0.8501 . O2W H22W 0.8524 . O3W H31W 0.8488 . O3W H32W 0.8536 . O4W H41W 0.8522 . O4W H42W 0.8515 . O5W H51W 0.8497 . O5W H52W 0.8520 . C4A H4A 0.9300 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W O5W 0.85 1.90 2.719(4) 160.8 1_545 O1W H12W N1B 0.85 2.06 2.897(4) 168.1 3_453 O2W H21W O72B 0.85 1.95 2.721(4) 149.5 . O2W H22W O72A 0.85 1.99 2.708(4) 141.8 . O3W H31W N1B 0.85 2.05 2.870(4) 161.0 3_463 O3W H32W O4W 0.85 1.87 2.723(4) 173.4 . O4W H41W O72A 0.85 1.97 2.811(4) 167.0 1_565 O4W H42W O72A 0.85 1.95 2.801(3) 174.7 4_753 O5W H51W O72B 0.85 1.93 2.773(4) 168.8 4_853 O5W H52W O71B 0.85 2.51 3.220(4) 141.7 . O5W H52W O3W 0.85 2.51 3.206(4) 140.0 . N8A H8A1 O71A 0.86 2.12 2.897(4) 149.4 . N8A H8A2 O5W 0.86 2.29 3.149(4) 174.4 3_463 N8B H8B2 O4W 0.86 2.28 3.093(4) 158.4 1_655