# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Interconversion of Two New Nickel(II) Coordination Polymers with Different Topologies: Synthesis, Structure and Magnetic Properties ; loop_ _publ_author_name 'Xian-He Bu' 'Bo-Wen Hu' 'Fu-Chen Liu' 'Qian Yang' 'Jiong -Peng Zhao' # Attachment 'cif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 666576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl N3 Ni O4' _chemical_formula_weight 256.29 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 8.3567(17) _cell_length_b 9.0434(18) _cell_length_c 12.055(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 911.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8918 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.4 _exptl_crystal_description Block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.409 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 scx-mini _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9565 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2064 _reflns_number_gt 2018 _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^)+(0.0187P)^2^+0.1050P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(10) _refine_ls_number_reflns 2064 _refine_ls_number_parameters 134 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0181 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0418 _refine_ls_wR_factor_gt 0.0415 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 0.12879(2) 0.81024(2) 0.680742(17) 0.01539(6) Uani 1 1 d . . . O1 O 0.05948(14) 0.59132(13) 0.69370(12) 0.0224(3) Uani 1 1 d . . . O1W O 0.1902(2) 1.03129(17) 0.66274(15) 0.0339(4) Uani 1 1 d . . . O2W O 0.2171(2) 0.8144(2) 0.83980(12) 0.0401(4) Uani 1 1 d . . . N1 N 0.38051(19) 0.58384(15) 0.61242(12) 0.0181(3) Uani 1 1 d . . . N2 N 0.34219(18) 0.73128(15) 0.60980(13) 0.0196(3) Uani 1 1 d . . . C4 C 0.1421(2) 0.47855(19) 0.71404(14) 0.0172(3) Uani 1 1 d . . . C3 C 0.3241(2) 0.4818(2) 0.69830(16) 0.0205(4) Uani 1 1 d . . . H1A H 0.3733 0.5090 0.7683 0.025 Uiso 1 1 calc R . . H1B H 0.3601 0.3829 0.6798 0.025 Uiso 1 1 calc R . . C2 C 0.4820(2) 0.5548(2) 0.53035(15) 0.0222(4) Uani 1 1 d . . . H14A H 0.5250 0.4621 0.5152 0.027 Uiso 1 1 calc R . . N3A N 0.51345(18) 0.67692(16) 0.47305(12) 0.0199(3) Uani 1 1 d . . . O2A O 0.09179(14) 0.35828(13) 0.75230(11) 0.0217(3) Uani 1 1 d . . . Cl1 Cl 0.50189(6) 0.65832(5) 0.94695(4) 0.03063(12) Uani 1 1 d . . . C1 C 0.4248(2) 0.78168(19) 0.52402(15) 0.0211(4) Uani 1 1 d . . . H12B H 0.4220 0.8798 0.5011 0.025 Uiso 1 1 calc R . . H1WB H 0.157(5) 1.084(4) 0.707(3) 0.085(13) Uiso 1 1 d . . . H1WA H 0.276(4) 1.061(3) 0.642(2) 0.054(9) Uiso 1 1 d . . . H2WA H 0.151(4) 0.823(3) 0.889(3) 0.070(10) Uiso 1 1 d D . . H2WB H 0.283(5) 0.759(5) 0.866(4) 0.120(17) Uiso 1 1 d 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 Ni1 0.01567(10) 0.01317(10) 0.01734(10) -0.00038(9) 0.00051(9) 0.00063(9) O1 0.0199(6) 0.0149(6) 0.0325(7) 0.0055(6) 0.0047(6) 0.0011(5) O1W 0.0344(8) 0.0193(7) 0.0480(10) -0.0090(7) 0.0156(8) -0.0063(6) O2W 0.0319(8) 0.0674(11) 0.0211(7) -0.0065(8) -0.0042(6) 0.0198(8) N1 0.0186(7) 0.0129(6) 0.0228(7) 0.0036(6) 0.0038(7) 0.0010(6) N2 0.0228(8) 0.0111(7) 0.0248(8) -0.0007(6) 0.0056(6) 0.0006(6) C4 0.0195(8) 0.0159(8) 0.0161(8) -0.0013(6) 0.0012(7) -0.0013(7) C3 0.0211(8) 0.0173(9) 0.0232(9) 0.0079(7) 0.0038(7) 0.0015(7) C2 0.0250(9) 0.0161(9) 0.0253(9) 0.0004(8) 0.0072(8) 0.0020(8) N3A 0.0221(7) 0.0165(7) 0.0212(7) -0.0006(6) 0.0043(6) 0.0010(7) O2A 0.0201(7) 0.0156(6) 0.0293(7) 0.0046(5) 0.0036(5) -0.0017(5) Cl1 0.0328(2) 0.0252(3) 0.0339(2) 0.0000(2) -0.0053(2) 0.0070(2) C1 0.0255(9) 0.0131(9) 0.0247(9) 0.0027(7) 0.0055(7) -0.0009(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 Ni1 O2W 2.0549(15) . ? Ni1 O2A 2.0587(13) 3_556 ? Ni1 O1 2.0687(13) . ? Ni1 O1W 2.0752(16) . ? Ni1 N3A 2.0928(14) 4_466 ? Ni1 N2 2.1027(15) . ? O1 C4 1.256(2) . ? O1W H1WB 0.76(4) . ? O1W H1WA 0.80(3) . ? O2W H2WA 0.81(3) . ? O2W H2WB 0.80(4) . ? N1 C2 1.330(2) . ? N1 N2 1.372(2) . ? N1 C3 1.465(2) . ? N2 C1 1.324(2) . ? C4 O2A 1.254(2) . ? C4 C3 1.533(3) . ? C3 H1A 0.9700 . ? C3 H1B 0.9700 . ? C2 N3A 1.329(2) . ? C2 H14A 0.9300 . ? N3A C1 1.351(2) . ? N3A Ni1 2.0928(14) 4_566 ? O2A Ni1 2.0587(12) 3_546 ? C1 H12B 0.9300 . ? 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 O2W Ni1 O2A 87.24(6) . 3_556 ? O2W Ni1 O1 92.72(7) . . ? O2A Ni1 O1 85.51(5) 3_556 . ? O2W Ni1 O1W 89.50(8) . . ? O2A Ni1 O1W 93.38(6) 3_556 . ? O1 Ni1 O1W 177.46(6) . . ? O2W Ni1 N3A 172.31(6) . 4_466 ? O2A Ni1 N3A 85.60(6) 3_556 4_466 ? O1 Ni1 N3A 89.49(6) . 4_466 ? O1W Ni1 N3A 88.15(6) . 4_466 ? O2W Ni1 N2 94.66(6) . . ? O2A Ni1 N2 172.10(5) 3_556 . ? O1 Ni1 N2 86.74(5) . . ? O1W Ni1 N2 94.30(6) . . ? N3A Ni1 N2 92.82(6) 4_466 . ? C4 O1 Ni1 129.66(11) . . ? Ni1 O1W H1WB 116(3) . . ? Ni1 O1W H1WA 125(2) . . ? H1WB O1W H1WA 110(3) . . ? Ni1 O2W H2WA 116(2) . . ? Ni1 O2W H2WB 127(3) . . ? H2WA O2W H2WB 104(3) . . ? C2 N1 N2 108.91(14) . . ? C2 N1 C3 127.37(15) . . ? N2 N1 C3 123.59(15) . . ? C1 N2 N1 103.35(14) . . ? C1 N2 Ni1 130.00(12) . . ? N1 N2 Ni1 121.25(11) . . ? O2A C4 O1 126.32(17) . . ? O2A C4 C3 113.25(15) . . ? O1 C4 C3 120.35(16) . . ? N1 C3 C4 114.79(15) . . ? N1 C3 H1A 108.6 . . ? C4 C3 H1A 108.6 . . ? N1 C3 H1B 108.6 . . ? C4 C3 H1B 108.6 . . ? H1A C3 H1B 107.5 . . ? N3A C2 N1 110.39(15) . . ? N3A C2 H14A 124.8 . . ? N1 C2 H14A 124.8 . . ? C2 N3A C1 103.78(15) . . ? C2 N3A Ni1 126.69(12) . 4_566 ? C1 N3A Ni1 128.09(12) . 4_566 ? C4 O2A Ni1 128.85(12) . 3_546 ? N2 C1 N3A 113.57(15) . . ? N2 C1 H12B 123.2 . . ? N3A C1 H12B 123.2 . . ? 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 O2W Ni1 O1 C4 -59.08(16) . . . . ? O2A Ni1 O1 C4 -146.09(16) 3_556 . . . ? O1W Ni1 O1 C4 149.8(14) . . . . ? N3A Ni1 O1 C4 128.29(16) 4_466 . . . ? N2 Ni1 O1 C4 35.44(16) . . . . ? C2 N1 N2 C1 0.25(19) . . . . ? C3 N1 N2 C1 176.43(17) . . . . ? C2 N1 N2 Ni1 156.70(12) . . . . ? C3 N1 N2 Ni1 -27.1(2) . . . . ? O2W Ni1 N2 C1 -129.26(17) . . . . ? O2A Ni1 N2 C1 127.1(4) 3_556 . . . ? O1 Ni1 N2 C1 138.27(16) . . . . ? O1W Ni1 N2 C1 -39.41(17) . . . . ? N3A Ni1 N2 C1 48.95(17) 4_466 . . . ? O2W Ni1 N2 N1 81.24(14) . . . . ? O2A Ni1 N2 N1 -22.4(5) 3_556 . . . ? O1 Ni1 N2 N1 -11.23(13) . . . . ? O1W Ni1 N2 N1 171.09(13) . . . . ? N3A Ni1 N2 N1 -100.55(13) 4_466 . . . ? Ni1 O1 C4 O2A 157.66(14) . . . . ? Ni1 O1 C4 C3 -19.0(2) . . . . ? C2 N1 C3 C4 -130.32(19) . . . . ? N2 N1 C3 C4 54.2(2) . . . . ? O2A C4 C3 N1 153.85(15) . . . . ? O1 C4 C3 N1 -29.1(2) . . . . ? N2 N1 C2 N3A 0.1(2) . . . . ? C3 N1 C2 N3A -175.85(17) . . . . ? N1 C2 N3A C1 -0.5(2) . . . . ? N1 C2 N3A Ni1 -167.56(12) . . . 4_566 ? O1 C4 O2A Ni1 -11.1(3) . . . 3_546 ? C3 C4 O2A Ni1 165.69(11) . . . 3_546 ? N1 N2 C1 N3A -0.6(2) . . . . ? Ni1 N2 C1 N3A -154.08(13) . . . . ? C2 N3A C1 N2 0.7(2) . . . . ? Ni1 N3A C1 N2 167.50(12) 4_566 . . . ? 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 H1WB O1 0.76(4) 2.17(4) 2.764(2) 135(3) 3_556 O1W H1WB O2A 0.76(4) 2.60(3) 3.254(2) 145(3) 1_565 O1W H1WA Cl1 0.80(3) 2.32(3) 3.1131(18) 169(3) 3_656 O2W H2WA Cl1 0.81(3) 2.35(3) 3.1470(17) 169(3) 4_467 O2W H2WB Cl1 0.80(4) 2.27(4) 3.0537(17) 165(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.260 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.049 data_2 _database_code_depnum_ccdc_archive 'CCDC 706319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 N6 Ni O6' _chemical_formula_weight 346.95 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6673(15) _cell_length_b 12.559(3) _cell_length_c 7.9117(16) _cell_angle_alpha 90.00 _cell_angle_beta 118.58(3) _cell_angle_gamma 90.00 _cell_volume 669.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4392 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.7 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 6796 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1529 _reflns_number_gt 1407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker 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^)+(0.0338P)^2^+0.3132P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1529 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.002 _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 0.5000 0.5000 0.5000 0.01290(12) Uani 1 2 d S . . O1 O 0.7669(2) 0.44824(12) 0.7249(2) 0.0232(3) Uani 1 1 d . . . C1 C 0.9085(3) 0.39974(15) 0.7218(3) 0.0185(4) Uani 1 1 d . . . O1W O 0.3971(2) 0.52284(13) 0.6981(2) 0.0215(3) Uani 1 1 d . . . N3 N 1.3969(2) 0.15623(12) 0.9453(2) 0.0178(3) Uani 1 1 d . . . N1 N 1.2216(2) 0.29705(13) 0.9207(2) 0.0182(3) Uani 1 1 d . . . O2 O 0.9249(2) 0.37534(15) 0.5779(2) 0.0383(4) Uani 1 1 d . . . N2 N 1.3766(3) 0.33291(13) 0.8970(3) 0.0235(4) Uani 1 1 d . . . C4 C 1.4771(3) 0.24514(16) 0.9131(3) 0.0220(4) Uani 1 1 d . . . H4A H 1.5932 0.2442 0.9033 0.026 Uiso 1 1 calc R . . C3 C 1.2360(3) 0.19251(16) 0.9481(3) 0.0191(4) Uani 1 1 d . . . H3A H 1.1463 0.1508 0.9667 0.023 Uiso 1 1 calc R . . C2 C 1.0727(3) 0.36827(18) 0.9218(3) 0.0254(5) Uani 1 1 d . . . H2A H 1.1383 0.4324 0.9915 0.030 Uiso 1 1 calc R . . H2B H 1.0124 0.3342 0.9911 0.030 Uiso 1 1 calc R . . H1WB H 0.282(5) 0.553(3) 0.638(5) 0.060(10) Uiso 1 1 d . . . H1WA H 0.390(5) 0.474(2) 0.759(4) 0.042(8) 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 Ni1 0.00926(19) 0.01120(19) 0.01890(19) -0.00082(12) 0.00727(14) 0.00021(12) O1 0.0140(7) 0.0295(8) 0.0231(7) -0.0014(6) 0.0067(6) 0.0088(6) C1 0.0136(9) 0.0170(9) 0.0250(10) 0.0023(7) 0.0093(8) 0.0040(7) O1W 0.0219(8) 0.0212(7) 0.0262(8) 0.0040(6) 0.0154(7) 0.0035(6) N3 0.0144(8) 0.0157(8) 0.0247(8) 0.0024(6) 0.0105(7) 0.0023(6) N1 0.0136(8) 0.0212(8) 0.0195(8) 0.0034(6) 0.0078(6) 0.0060(6) O2 0.0284(9) 0.0647(12) 0.0256(8) 0.0086(8) 0.0159(7) 0.0249(8) N2 0.0193(8) 0.0188(8) 0.0334(9) 0.0047(7) 0.0135(7) 0.0020(7) C4 0.0156(9) 0.0219(10) 0.0311(11) 0.0057(8) 0.0131(8) 0.0035(8) C3 0.0138(9) 0.0214(10) 0.0233(10) 0.0043(8) 0.0097(8) 0.0030(7) C2 0.0218(11) 0.0296(11) 0.0237(10) 0.0025(8) 0.0100(9) 0.0159(9) _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 O1 2.0715(16) . ? Ni1 O1 2.0715(16) 3_666 ? Ni1 N3 2.0821(16) 4_465 ? Ni1 N3 2.0821(16) 2_756 ? Ni1 O1W 2.0841(15) 3_666 ? Ni1 O1W 2.0841(15) . ? O1 C1 1.255(2) . ? C1 O2 1.243(2) . ? C1 C2 1.529(3) . ? N3 C3 1.325(2) . ? N3 C4 1.356(2) . ? N3 Ni1 2.0821(16) 2_746 ? N1 C3 1.327(3) . ? N1 N2 1.365(2) . ? N1 C2 1.454(2) . ? N2 C4 1.316(3) . ? 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 O1 Ni1 O1 180.0 . 3_666 ? O1 Ni1 N3 90.21(6) . 4_465 ? O1 Ni1 N3 89.79(6) 3_666 4_465 ? O1 Ni1 N3 89.79(6) . 2_756 ? O1 Ni1 N3 90.21(6) 3_666 2_756 ? N3 Ni1 N3 180.0 4_465 2_756 ? O1 Ni1 O1W 91.67(6) . 3_666 ? O1 Ni1 O1W 88.33(6) 3_666 3_666 ? N3 Ni1 O1W 87.51(6) 4_465 3_666 ? N3 Ni1 O1W 92.49(6) 2_756 3_666 ? O1 Ni1 O1W 88.33(6) . . ? O1 Ni1 O1W 91.67(6) 3_666 . ? N3 Ni1 O1W 92.49(6) 4_465 . ? N3 Ni1 O1W 87.51(6) 2_756 . ? O1W Ni1 O1W 180.0 3_666 . ? C1 O1 Ni1 130.05(13) . . ? O2 C1 O1 127.26(18) . . ? O2 C1 C2 119.34(17) . . ? O1 C1 C2 113.40(16) . . ? C3 N3 C4 103.27(16) . . ? C3 N3 Ni1 125.76(13) . 2_746 ? C4 N3 Ni1 130.82(13) . 2_746 ? C3 N1 N2 109.85(15) . . ? C3 N1 C2 127.73(17) . . ? N2 N1 C2 122.38(16) . . ? C4 N2 N1 102.61(15) . . ? N2 C4 N3 114.25(17) . . ? N3 C3 N1 110.02(17) . . ? N1 C2 C1 114.42(16) . . ? 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 O1 Ni1 O1 C1 -125(100) 3_666 . . . ? N3 Ni1 O1 C1 73.48(17) 4_465 . . . ? N3 Ni1 O1 C1 -106.52(17) 2_756 . . . ? O1W Ni1 O1 C1 -14.04(18) 3_666 . . . ? O1W Ni1 O1 C1 165.96(18) . . . . ? Ni1 O1 C1 O2 3.8(3) . . . . ? Ni1 O1 C1 C2 -175.43(13) . . . . ? C3 N1 N2 C4 -0.3(2) . . . . ? C2 N1 N2 C4 177.46(17) . . . . ? N1 N2 C4 N3 0.0(2) . . . . ? C3 N3 C4 N2 0.2(2) . . . . ? Ni1 N3 C4 N2 -175.35(13) 2_746 . . . ? C4 N3 C3 N1 -0.4(2) . . . . ? Ni1 N3 C3 N1 175.48(12) 2_746 . . . ? N2 N1 C3 N3 0.5(2) . . . . ? C2 N1 C3 N3 -177.13(17) . . . . ? C3 N1 C2 C1 -100.8(2) . . . . ? N2 N1 C2 C1 81.9(2) . . . . ? O2 C1 C2 N1 -9.0(3) . . . . ? O1 C1 C2 N1 170.24(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.380 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.076