# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_email YYG@FJIRSM.AC.CN _publ_section_title ; Distinct Ferromagnetic and Canted Antiferromagnetic Behaviors in Isostructural Co(II) and Ni(II) Frameworks with Helical lvt Topology ; loop_ _publ_author_name 'Yuan-Gen Yao' 'Xin-Yi Cao' 'Zhao-Ji Li' 'Qi-Pu Lin' 'Jian Zhang' ; Lei Zhang ; 'Zhangfeng Zhou' # Attachment '1Co1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 735476' #TrackingRef '1Co1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 Co N8 O2, H2 O' _chemical_formula_sum 'C12 H12 Co N8 O3' _chemical_formula_weight 375.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.6671(2) _cell_length_b 15.6671(2) _cell_length_c 12.6333(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3100.95(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5922 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.67 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max .22 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528.0 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8265 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.67 _reflns_number_total 1476 _reflns_number_gt 1372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+18.6529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1476 _refine_ls_number_parameters 112 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.2500 0.02144(18) Uani 1 2 d S . . N1 N 0.17598(15) 0.16923(15) 0.15300(19) 0.0236(5) Uani 1 1 d . . . N3 N 0.10511(15) 0.07762(16) 0.0466(2) 0.0271(6) Uani 1 1 d . . . N4 N 0.19669(16) 0.09510(18) -0.1079(2) 0.0319(6) Uani 1 1 d . . . N8 N 0.21278(15) 0.16648(15) 0.05509(19) 0.0225(5) Uani 1 1 d . . . C7 C 0.28731(18) 0.20998(18) 0.0309(2) 0.0253(6) Uani 1 1 d . . . C6 C 0.3126(2) 0.1950(2) -0.0737(3) 0.0324(7) Uani 1 1 d . . . H6A H 0.3604 0.2228 -0.1005 0.039 Uiso 1 1 calc R . . C5 C 0.2672(2) 0.1390(2) -0.1383(3) 0.0336(7) Uani 1 1 d . . . C3A C 0.17143(18) 0.11072(18) -0.0095(2) 0.0245(6) Uani 1 1 d . . . C2 C 0.11186(19) 0.11559(19) 0.1422(2) 0.0279(7) Uani 1 1 d . . . H2A H 0.0737 0.1046 0.1969 0.033 Uiso 1 1 calc R . . C51 C 0.2960(3) 0.1229(3) -0.2505(3) 0.0537(11) Uani 1 1 d . . . H51A H 0.3037 0.0627 -0.2612 0.081 Uiso 1 1 calc R . . H51B H 0.3490 0.1519 -0.2629 0.081 Uiso 1 1 calc R . . H51C H 0.2536 0.1439 -0.2988 0.081 Uiso 1 1 calc R . . O71 O 0.31975(13) 0.25584(13) 0.10263(17) 0.0286(5) Uani 1 1 d . . . O1W O 0.5000 0.2500 0.1805(7) 0.230(6) Uani 1 2 d SU . . H1W H 0.4571 0.2600 0.1412 0.346 Uiso 1 1 d 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 Co1 0.0215(3) 0.0179(3) 0.0249(3) -0.0017(2) -0.0069(2) 0.0009(2) N1 0.0226(12) 0.0250(12) 0.0233(12) -0.0040(10) -0.0022(10) -0.0019(10) N3 0.0233(13) 0.0300(13) 0.0280(13) -0.0067(11) 0.0019(11) -0.0048(10) N4 0.0273(14) 0.0384(15) 0.0299(14) -0.0084(12) 0.0003(11) -0.0050(11) N8 0.0214(12) 0.0241(12) 0.0219(12) -0.0013(10) -0.0024(10) -0.0008(10) C7 0.0226(14) 0.0229(14) 0.0305(16) 0.0041(12) -0.0023(12) -0.0021(12) C6 0.0258(16) 0.0395(18) 0.0318(17) 0.0040(14) 0.0016(13) -0.0068(14) C5 0.0304(17) 0.0414(19) 0.0291(17) -0.0016(14) 0.0011(14) -0.0005(14) C3A 0.0215(14) 0.0256(15) 0.0265(15) -0.0034(12) -0.0032(12) -0.0012(11) C2 0.0249(15) 0.0316(16) 0.0271(16) -0.0037(13) 0.0022(13) -0.0038(12) C51 0.046(2) 0.080(3) 0.035(2) -0.011(2) 0.0089(17) -0.012(2) O71 0.0257(11) 0.0272(11) 0.0331(12) -0.0011(9) -0.0041(9) -0.0074(9) O1W 0.054(4) 0.51(2) 0.124(7) 0.000 0.000 -0.026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.109(2) 13 ? Co1 N1 2.109(2) . ? Co1 N3 2.130(2) 8_444 ? Co1 N3 2.130(2) 12_666 ? Co1 O71 2.161(2) . ? Co1 O71 2.161(2) 13 ? N1 C2 1.317(4) . ? N1 N8 1.365(3) . ? N3 C2 1.351(4) . ? N3 C3A 1.360(4) . ? N3 Co1 2.130(2) 6_444 ? N4 C3A 1.328(4) . ? N4 C5 1.356(4) . ? N8 C3A 1.360(4) . ? N8 C7 1.386(4) . ? C7 O71 1.263(4) . ? C7 C6 1.400(4) . ? C6 C5 1.394(5) . ? C6 H6A 0.9300 . ? C5 C51 1.508(5) . ? C2 H2A 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O1W H1W 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(10) 13 . ? N1 Co1 N3 89.39(9) 13 8_444 ? N1 Co1 N3 90.61(9) . 8_444 ? N1 Co1 N3 90.61(9) 13 12_666 ? N1 Co1 N3 89.39(9) . 12_666 ? N3 Co1 N3 180.0 8_444 12_666 ? N1 Co1 O71 101.37(8) 13 . ? N1 Co1 O71 78.63(8) . . ? N3 Co1 O71 88.98(9) 8_444 . ? N3 Co1 O71 91.02(9) 12_666 . ? N1 Co1 O71 78.63(8) 13 13 ? N1 Co1 O71 101.37(8) . 13 ? N3 Co1 O71 91.02(9) 8_444 13 ? N3 Co1 O71 88.98(9) 12_666 13 ? O71 Co1 O71 180.0 . 13 ? C2 N1 N8 102.0(2) . . ? C2 N1 Co1 149.6(2) . . ? N8 N1 Co1 108.25(16) . . ? C2 N3 C3A 103.8(2) . . ? C2 N3 Co1 124.0(2) . 6_444 ? C3A N3 Co1 131.6(2) . 6_444 ? C3A N4 C5 114.5(3) . . ? C3A N8 N1 111.3(2) . . ? C3A N8 C7 125.8(3) . . ? N1 N8 C7 122.7(2) . . ? O71 C7 N8 117.4(3) . . ? O71 C7 C6 131.2(3) . . ? N8 C7 C6 111.3(3) . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? N4 C5 C6 124.7(3) . . ? N4 C5 C51 115.2(3) . . ? C6 C5 C51 120.1(3) . . ? N4 C3A N8 122.6(3) . . ? N4 C3A N3 130.2(3) . . ? N8 C3A N3 107.2(3) . . ? N1 C2 N3 115.7(3) . . ? N1 C2 H2A 122.2 . . ? N3 C2 H2A 122.2 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C7 O71 Co1 112.99(18) . . ? 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 H1W O71 0.85 2.21 2.992(3) 153.4 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.607 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.066 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; # Attachment '2Ni1.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 735477' #TrackingRef '2Ni1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 N8 Ni O2, H2 O' _chemical_formula_sum 'C12 H12 N8 Ni O3' _chemical_formula_weight 374.99 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.5470(10) _cell_length_b 15.5470(10) _cell_length_c 12.4988(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3021.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3975 _cell_measurement_theta_min 3.2597 _cell_measurement_theta_max 27.4424 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536.0 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.877 _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11479 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1735 _reflns_number_gt 1634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+8.5897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1735 _refine_ls_number_parameters 112 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.5000 0.0000 0.01855(15) Uani 1 2 d S . . O71 O -0.00686(11) 0.57059(10) 0.14472(13) 0.0252(4) Uani 1 1 d . . . N1 N 0.08059(12) 0.42630(12) 0.09410(15) 0.0209(4) Uani 1 1 d . . . N3 N 0.17252(13) 0.35463(12) 0.20140(16) 0.0239(4) Uani 1 1 d . . . N8 N 0.08274(12) 0.46297(12) 0.19345(15) 0.0204(4) Uani 1 1 d . . . N4 N 0.15399(14) 0.44649(13) 0.35873(17) 0.0288(5) Uani 1 1 d . . . C2 C 0.13469(15) 0.36156(15) 0.10457(18) 0.0243(5) Uani 1 1 d . . . H2A H 0.1460 0.3233 0.0491 0.029 Uiso 1 1 calc R . . C3A C 0.13903(15) 0.42117(14) 0.25842(18) 0.0221(5) Uani 1 1 d . . . C7 C 0.03924(14) 0.53787(14) 0.21794(19) 0.0231(5) Uani 1 1 d . . . C6 C 0.05385(17) 0.56340(16) 0.3240(2) 0.0298(5) Uani 1 1 d . . . H6A H 0.0257 0.6115 0.3510 0.036 Uiso 1 1 calc R . . C5 C 0.11005(17) 0.51737(17) 0.3893(2) 0.0304(5) Uani 1 1 d . . . C51 C 0.1255(3) 0.5462(2) 0.5030(2) 0.0484(8) Uani 1 1 d . . . H51A H 0.1068 0.5021 0.5515 0.073 Uiso 1 1 calc R . . H51B H 0.0938 0.5981 0.5165 0.073 Uiso 1 1 calc R . . H51C H 0.1857 0.5569 0.5134 0.073 Uiso 1 1 calc R . . O1W O 0.0000 0.7500 0.0670(6) 0.206(5) Uani 1 2 d SU . . H1W H 0.0123 0.7074 0.1068 0.309 Uiso 1 1 d 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 Ni1 0.0159(2) 0.0183(2) 0.0214(2) 0.00600(14) -0.00109(14) -0.00013(13) O71 0.0243(8) 0.0221(8) 0.0292(8) 0.0032(6) -0.0010(6) 0.0058(6) N1 0.0206(9) 0.0206(9) 0.0216(9) 0.0022(7) -0.0029(7) 0.0016(7) N3 0.0250(10) 0.0210(9) 0.0256(10) 0.0005(7) -0.0067(8) 0.0050(7) N8 0.0219(9) 0.0184(9) 0.0208(9) 0.0028(7) -0.0008(7) 0.0023(7) N4 0.0375(12) 0.0246(10) 0.0244(10) -0.0012(8) -0.0082(8) 0.0033(8) C2 0.0251(11) 0.0228(11) 0.0248(11) -0.0014(9) -0.0054(9) 0.0040(8) C3A 0.0234(11) 0.0170(10) 0.0259(11) 0.0045(8) -0.0035(8) 0.0007(8) C7 0.0215(10) 0.0197(10) 0.0281(11) 0.0031(9) 0.0027(9) 0.0006(8) C6 0.0344(13) 0.0256(12) 0.0294(12) -0.0022(9) 0.0026(10) 0.0063(10) C5 0.0374(14) 0.0284(12) 0.0255(12) -0.0016(10) -0.0019(10) 0.0018(10) C51 0.070(2) 0.0445(17) 0.0304(14) -0.0080(12) -0.0087(14) 0.0108(16) O1W 0.453(17) 0.050(3) 0.114(5) 0.000 0.000 0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1 N1 2.0654(18) 9_565 ? Ni1 N1 2.0654(18) . ? Ni1 N3 2.1132(18) 12_666 ? Ni1 N3 2.1132(18) 4_454 ? Ni1 O71 2.1184(17) 9_565 ? Ni1 O71 2.1184(17) . ? O71 C7 1.269(3) . ? N1 C2 1.318(3) . ? N1 N8 1.367(3) . ? N3 C2 1.350(3) . ? N3 C3A 1.360(3) . ? N3 Ni1 2.1132(18) 2 ? N8 C3A 1.359(3) . ? N8 C7 1.381(3) . ? N4 C3A 1.334(3) . ? N4 C5 1.352(3) . ? C2 H2A 0.9300 . ? C7 C6 1.402(3) . ? C6 C5 1.393(4) . ? C6 H6A 0.9300 . ? C5 C51 1.510(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O1W H1W 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.00(9) 9_565 . ? N1 Ni1 N3 90.74(7) 9_565 12_666 ? N1 Ni1 N3 89.26(7) . 12_666 ? N1 Ni1 N3 89.26(7) 9_565 4_454 ? N1 Ni1 N3 90.74(7) . 4_454 ? N3 Ni1 N3 180.00(9) 12_666 4_454 ? N1 Ni1 O71 80.31(7) 9_565 9_565 ? N1 Ni1 O71 99.69(7) . 9_565 ? N3 Ni1 O71 89.36(7) 12_666 9_565 ? N3 Ni1 O71 90.64(7) 4_454 9_565 ? N1 Ni1 O71 99.69(7) 9_565 . ? N1 Ni1 O71 80.31(7) . . ? N3 Ni1 O71 90.64(7) 12_666 . ? N3 Ni1 O71 89.36(7) 4_454 . ? O71 Ni1 O71 180.00(9) 9_565 . ? C7 O71 Ni1 112.31(15) . . ? C2 N1 N8 102.28(17) . . ? C2 N1 Ni1 150.13(16) . . ? N8 N1 Ni1 107.50(13) . . ? C2 N3 C3A 104.02(18) . . ? C2 N3 Ni1 124.57(16) . 2 ? C3A N3 Ni1 130.78(15) . 2 ? C3A N8 N1 111.04(18) . . ? C3A N8 C7 125.9(2) . . ? N1 N8 C7 122.76(18) . . ? C3A N4 C5 114.7(2) . . ? N1 C2 N3 115.3(2) . . ? N1 C2 H2A 122.3 . . ? N3 C2 H2A 122.3 . . ? N4 C3A N8 122.2(2) . . ? N4 C3A N3 130.5(2) . . ? N8 C3A N3 107.29(19) . . ? O71 C7 N8 117.1(2) . . ? O71 C7 C6 131.3(2) . . ? N8 C7 C6 111.6(2) . . ? C5 C6 C7 120.7(2) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? N4 C5 C6 124.8(2) . . ? N4 C5 C51 115.4(2) . . ? C6 C5 C51 119.9(2) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? 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 H1W O71 0.85 2.20 2.955(3) 148.1 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.705 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.073