# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Chih-Chieh Wang.' _publ_contact_author_name 'Chih-Chieh Wang' _publ_contact_author_email ccwang@scu.edu.tw _publ_section_title ; Synthesis, Structural Characterization and Magnetic Behavior of a 2D Bi-Layer MOF, {[Ni2(C5O5)2(bpe)2]H2O}n (bpe = 1,2-bis(4-pyridyl)ethylene) ; # Attachment '- nibpec5o5.cif' data_ic11068 _database_code_depnum_ccdc_archive 'CCDC 773841' #TrackingRef '- nibpec5o5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 N4 Ni2 O11' _chemical_formula_weight 779.98 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 7.9639(5) _cell_length_b 24.3259(16) _cell_length_c 16.0648(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.412(2) _cell_angle_gamma 90.00 _cell_volume 3112.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2462 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 24.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8019 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25212 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7147 _reflns_number_gt 5389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0488P)^2^+1.4746P] 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 7147 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 0.61868(6) 0.586006(19) 0.63055(3) 0.02008(14) Uani 1 1 d . . . Ni2 Ni 0.34567(6) 0.594606(18) 0.87263(3) 0.02019(14) Uani 1 1 d . . . O1 O 0.5526(3) 0.50415(10) 0.61602(15) 0.0258(6) Uani 1 1 d . . . O2 O 0.4736(3) 0.57520(10) 0.75032(15) 0.0257(6) Uani 1 1 d . . . O3 O 0.4110(3) 0.51378(11) 0.89793(15) 0.0270(6) Uani 1 1 d . . . O4 O 0.4205(5) 0.39385(12) 0.85091(19) 0.0491(9) Uani 1 1 d . . . O5 O 0.5421(4) 0.38794(12) 0.68107(19) 0.0480(9) Uani 1 1 d . . . O6 O 0.7297(3) 0.66233(11) 0.66516(17) 0.0297(6) Uani 1 1 d . . . O7 O 0.8228(3) 0.55579(10) 0.70046(16) 0.0266(6) Uani 1 1 d . . . O8 O 1.1302(3) 0.56005(10) 0.81728(16) 0.0268(6) Uani 1 1 d . . . O9 O 1.2265(3) 0.66815(10) 0.83219(17) 0.0282(6) Uani 1 1 d . . . O10 O 0.9746(4) 0.74163(11) 0.74402(19) 0.0394(8) Uani 1 1 d . . . N1 N 0.7458(4) 0.58142(13) 0.5192(2) 0.0272(7) Uani 1 1 d . . . N2 N 0.2458(4) 0.59788(13) 0.99109(19) 0.0260(7) Uani 1 1 d . . . N3 N 0.4183(4) 0.62593(13) 0.58035(19) 0.0239(7) Uani 1 1 d . . . N4 N 0.5577(4) 0.63567(13) 0.90591(19) 0.0240(7) Uani 1 1 d . . . C1 C 0.5171(4) 0.48704(15) 0.6885(2) 0.0229(8) Uani 1 1 d . . . C2 C 0.4773(4) 0.52270(15) 0.7551(2) 0.0211(8) Uani 1 1 d . . . C3 C 0.4445(5) 0.49213(15) 0.8288(2) 0.0226(8) Uani 1 1 d . . . C4 C 0.4532(5) 0.43303(17) 0.8074(2) 0.0290(9) Uani 1 1 d . . . C5 C 0.5102(5) 0.42993(17) 0.7188(2) 0.0277(9) Uani 1 1 d . . . C6 C 0.8545(5) 0.65248(15) 0.7102(2) 0.0249(9) Uani 1 1 d . . . C7 C 0.9015(4) 0.59624(15) 0.7298(2) 0.0217(8) Uani 1 1 d . . . C8 C 1.0483(5) 0.59814(15) 0.7837(2) 0.0223(8) Uani 1 1 d . . . C9 C 1.0968(5) 0.65506(15) 0.7927(2) 0.0242(8) Uani 1 1 d . . . C10 C 0.9748(5) 0.69146(16) 0.7489(2) 0.0260(9) Uani 1 1 d . . . C11 C 0.7975(5) 0.53316(17) 0.4894(3) 0.0340(10) Uani 1 1 d . . . H11A H 0.7850 0.5022 0.5227 0.041 Uiso 1 1 calc R . . C12 C 0.8685(5) 0.52659(17) 0.4116(3) 0.0338(10) Uani 1 1 d . . . H12A H 0.9013 0.4919 0.3938 0.041 Uiso 1 1 calc R . . C13 C 0.8907(5) 0.57154(16) 0.3605(2) 0.0287(9) Uani 1 1 d . . . C14 C 0.8331(5) 0.62177(17) 0.3907(3) 0.0346(10) Uani 1 1 d . . . H14A H 0.8409 0.6531 0.3579 0.041 Uiso 1 1 calc R . . C15 C 0.7651(5) 0.62504(17) 0.4685(3) 0.0328(10) Uani 1 1 d . . . H15A H 0.7302 0.6593 0.4874 0.039 Uiso 1 1 calc R . . C16 C 0.9691(5) 0.56546(17) 0.2786(3) 0.0325(10) Uani 1 1 d . . . H16A H 0.9718 0.5304 0.2556 0.039 Uiso 1 1 calc R . . C17 C 0.0360(5) 0.60559(18) 1.2352(2) 0.0335(10) Uani 1 1 d . . . H17A H 0.0344 0.6405 1.2586 0.040 Uiso 1 1 calc R . . C18 C 0.2577(5) 0.64211(16) 1.0393(3) 0.0307(9) Uani 1 1 d . . . H18A H 0.3110 0.6731 1.0181 0.037 Uiso 1 1 calc R . . C19 C 0.1956(6) 0.64464(16) 1.1189(3) 0.0327(10) Uani 1 1 d . . . H19A H 0.2092 0.6766 1.1501 0.039 Uiso 1 1 calc R . . C20 C 0.1131(5) 0.59998(16) 1.1527(2) 0.0279(9) Uani 1 1 d . . . C21 C 0.1033(6) 0.55321(17) 1.1031(3) 0.0347(10) Uani 1 1 d . . . H21A H 0.0516 0.5216 1.1231 0.042 Uiso 1 1 calc R . . C22 C 0.1699(5) 0.55381(16) 1.0246(3) 0.0326(10) Uani 1 1 d . . . H22A H 0.1622 0.5220 0.9928 0.039 Uiso 1 1 calc R . . C23 C 0.3549(5) 0.66938(15) 0.6215(2) 0.0299(9) Uani 1 1 d . . . H23A H 0.3952 0.6767 0.6748 0.036 Uiso 1 1 calc R . . C24 C 0.2340(5) 0.70336(17) 0.5887(3) 0.0320(10) Uani 1 1 d . . . H24A H 0.1930 0.7324 0.6201 0.038 Uiso 1 1 calc R . . C25 C 0.1726(5) 0.69453(16) 0.5089(2) 0.0273(9) Uani 1 1 d . . . C26 C 0.2406(5) 0.64992(18) 0.4660(3) 0.0356(11) Uani 1 1 d . . . H26A H 0.2059 0.6425 0.4118 0.043 Uiso 1 1 calc R . . C27 C 0.3588(5) 0.61703(17) 0.5040(2) 0.0309(9) Uani 1 1 d . . . H27A H 0.3993 0.5869 0.4747 0.037 Uiso 1 1 calc R . . C28 C 0.0469(5) 0.73021(17) 0.4691(3) 0.0335(10) Uani 1 1 d . . . H28A H 0.0369 0.7288 0.4114 0.040 Uiso 1 1 calc R . . C29 C 0.9470(5) 0.73578(17) 1.0093(3) 0.0321(10) Uani 1 1 d . . . H29A H 0.9602 0.7334 1.0668 0.039 Uiso 1 1 calc R . . C30 C 0.5924(5) 0.68507(17) 0.8733(2) 0.0297(9) Uani 1 1 d . . . H30A H 0.5276 0.6976 0.8288 0.036 Uiso 1 1 calc R . . C31 C 0.7204(5) 0.71812(17) 0.9032(3) 0.0329(10) Uani 1 1 d . . . H31A H 0.7422 0.7518 0.8780 0.039 Uiso 1 1 calc R . . C32 C 0.8159(5) 0.70120(17) 0.9704(2) 0.0286(9) Uani 1 1 d . . . C33 C 0.7814(5) 0.64930(18) 1.0029(3) 0.0372(11) Uani 1 1 d . . . H33A H 0.8446 0.6358 1.0473 0.045 Uiso 1 1 calc R . . C34 C 0.6538(5) 0.61812(17) 0.9692(3) 0.0324(10) Uani 1 1 d . . . H34A H 0.6336 0.5834 0.9914 0.039 Uiso 1 1 calc R . . O11 O 0.4565(11) 0.2787(2) 0.7761(5) 0.198(4) Uani 1 1 d . . . H11B H 0.5401 0.2829 0.7282 0.297 Uiso 1 1 d . . . H11C H 0.4645 0.2891 0.8357 0.297 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 0.0156(3) 0.0241(2) 0.0206(3) 0.0002(2) 0.00000(19) 0.00253(19) Ni2 0.0153(3) 0.0245(3) 0.0208(3) -0.0008(2) 0.00019(19) -0.00284(19) O1 0.0263(15) 0.0301(14) 0.0210(14) -0.0029(11) 0.0032(12) -0.0023(12) O2 0.0273(15) 0.0230(14) 0.0267(14) 0.0001(11) 0.0008(12) 0.0002(11) O3 0.0278(16) 0.0335(15) 0.0197(14) 0.0018(11) 0.0011(12) 0.0031(12) O4 0.075(3) 0.0319(16) 0.0411(19) 0.0089(14) 0.0152(18) -0.0013(16) O5 0.077(3) 0.0283(16) 0.0393(19) -0.0078(14) 0.0134(18) 0.0055(16) O6 0.0221(15) 0.0330(15) 0.0339(16) 0.0002(12) -0.0091(13) 0.0058(12) O7 0.0208(15) 0.0272(14) 0.0316(15) -0.0034(12) -0.0056(12) 0.0001(11) O8 0.0216(14) 0.0256(14) 0.0331(15) -0.0005(12) -0.0047(12) 0.0011(11) O9 0.0221(15) 0.0261(15) 0.0364(17) -0.0026(12) -0.0053(13) -0.0059(11) O10 0.0399(19) 0.0260(16) 0.052(2) 0.0000(14) -0.0050(16) -0.0024(13) N1 0.0235(18) 0.0318(18) 0.0262(18) -0.0011(14) 0.0052(15) -0.0008(14) N2 0.0217(18) 0.0321(18) 0.0243(17) -0.0020(14) 0.0035(14) -0.0038(14) N3 0.0215(17) 0.0295(17) 0.0209(17) -0.0018(13) -0.0006(14) 0.0036(14) N4 0.0202(17) 0.0337(18) 0.0182(16) -0.0003(14) 0.0033(14) -0.0047(14) C1 0.0146(19) 0.031(2) 0.023(2) -0.0020(16) 0.0012(16) 0.0007(15) C2 0.0134(18) 0.031(2) 0.0192(19) 0.0001(16) 0.0033(15) 0.0016(15) C3 0.0181(19) 0.027(2) 0.022(2) 0.0009(16) 0.0000(16) 0.0002(15) C4 0.028(2) 0.034(2) 0.025(2) 0.0018(18) 0.0007(18) 0.0043(18) C5 0.029(2) 0.031(2) 0.023(2) -0.0002(17) 0.0024(18) -0.0006(17) C6 0.019(2) 0.030(2) 0.026(2) -0.0022(16) 0.0030(17) 0.0008(16) C7 0.0147(18) 0.028(2) 0.0225(19) 0.0003(16) 0.0007(15) -0.0005(15) C8 0.0174(19) 0.027(2) 0.0223(19) 0.0005(16) -0.0005(16) -0.0028(15) C9 0.016(2) 0.031(2) 0.026(2) -0.0001(17) -0.0008(16) -0.0009(16) C10 0.021(2) 0.029(2) 0.028(2) 0.0013(17) 0.0011(17) -0.0013(16) C11 0.030(2) 0.036(2) 0.036(2) 0.0092(19) 0.014(2) 0.0105(19) C12 0.033(2) 0.033(2) 0.036(2) 0.0005(19) 0.014(2) 0.0071(19) C13 0.024(2) 0.034(2) 0.029(2) 0.0004(17) 0.0061(18) 0.0004(17) C14 0.041(3) 0.031(2) 0.032(2) 0.0084(18) 0.014(2) 0.0017(19) C15 0.039(3) 0.027(2) 0.033(2) -0.0010(18) 0.007(2) -0.0007(18) C16 0.035(3) 0.031(2) 0.032(2) -0.0014(18) 0.007(2) 0.0048(18) C17 0.036(3) 0.034(2) 0.030(2) -0.0038(18) 0.007(2) -0.0012(19) C18 0.033(2) 0.026(2) 0.033(2) 0.0029(17) 0.0066(19) -0.0041(17) C19 0.040(3) 0.030(2) 0.028(2) -0.0037(17) 0.001(2) -0.0002(18) C20 0.030(2) 0.031(2) 0.023(2) 0.0000(16) 0.0025(17) 0.0004(17) C21 0.037(3) 0.034(2) 0.033(2) -0.0012(19) 0.011(2) -0.0098(19) C22 0.040(3) 0.026(2) 0.032(2) -0.0036(17) 0.007(2) -0.0103(18) C23 0.034(2) 0.033(2) 0.023(2) -0.0052(17) -0.0021(18) 0.0061(18) C24 0.033(2) 0.031(2) 0.033(2) -0.0032(18) 0.001(2) 0.0095(18) C25 0.018(2) 0.035(2) 0.029(2) 0.0032(17) -0.0007(17) 0.0064(17) C26 0.028(2) 0.052(3) 0.026(2) -0.0056(19) -0.0056(19) 0.013(2) C27 0.024(2) 0.039(2) 0.030(2) -0.0053(18) -0.0005(18) 0.0086(18) C28 0.026(2) 0.038(2) 0.036(3) 0.0025(19) -0.007(2) 0.0087(18) C29 0.028(2) 0.037(2) 0.031(2) -0.0012(18) -0.0051(19) -0.0048(18) C30 0.027(2) 0.038(2) 0.024(2) 0.0059(18) -0.0027(18) -0.0042(18) C31 0.025(2) 0.035(2) 0.039(3) 0.0049(19) 0.0006(19) -0.0093(18) C32 0.020(2) 0.038(2) 0.028(2) -0.0007(18) 0.0000(17) -0.0085(17) C33 0.027(2) 0.046(3) 0.038(3) 0.008(2) -0.014(2) -0.0079(19) C34 0.029(2) 0.034(2) 0.034(2) 0.0087(18) -0.003(2) -0.0093(18) O11 0.284(10) 0.063(4) 0.246(8) -0.029(5) -0.045(8) -0.025(5) _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 N3 2.030(3) . ? Ni1 N1 2.065(3) . ? Ni1 O1 2.072(3) . ? Ni1 O7 2.102(2) . ? Ni1 O6 2.129(3) . ? Ni1 O2 2.267(3) . ? Ni2 N4 2.030(3) . ? Ni2 N2 2.070(3) . ? Ni2 O3 2.073(3) . ? Ni2 O8 2.102(3) 1_455 ? Ni2 O9 2.125(3) 1_455 ? Ni2 O2 2.269(3) . ? O1 C1 1.270(4) . ? O2 C2 1.280(4) . ? O3 C3 1.260(4) . ? O4 C4 1.211(5) . ? O5 C5 1.215(5) . ? O6 C6 1.248(4) . ? O7 C7 1.257(4) . ? O8 C8 1.253(4) . ? O8 Ni2 2.102(3) 1_655 ? O9 C9 1.250(4) . ? O9 Ni2 2.125(3) 1_655 ? O10 C10 1.223(5) . ? N1 C11 1.334(5) . ? N1 C15 1.347(5) . ? N2 C18 1.329(5) . ? N2 C22 1.345(5) . ? N3 C27 1.329(5) . ? N3 C23 1.346(5) . ? N4 C34 1.339(5) . ? N4 C30 1.340(5) . ? C1 C2 1.416(5) . ? C1 C5 1.473(5) . ? C2 C3 1.424(5) . ? C3 C4 1.480(5) . ? C4 C5 1.500(6) . ? C6 C7 1.452(5) . ? C6 C10 1.481(5) . ? C7 C8 1.451(5) . ? C8 C9 1.444(5) . ? C9 C10 1.488(5) . ? C11 C12 1.385(6) . ? C12 C13 1.379(5) . ? C13 C14 1.394(6) . ? C13 C16 1.468(6) . ? C14 C15 1.367(6) . ? C16 C17 1.315(6) 1_654 ? C17 C16 1.315(6) 1_456 ? C17 C20 1.470(6) . ? C18 C19 1.375(6) . ? C19 C20 1.383(6) . ? C20 C21 1.391(5) . ? C21 C22 1.371(6) . ? C23 C24 1.372(5) . ? C24 C25 1.385(5) . ? C25 C26 1.396(6) . ? C25 C28 1.468(5) . ? C26 C27 1.375(5) . ? C28 C29 1.320(6) 4_475 ? C29 C28 1.320(6) 4_676 ? C29 C32 1.476(5) . ? C30 C31 1.382(5) . ? C31 C32 1.379(5) . ? C32 C33 1.394(6) . ? C33 C34 1.376(5) . ? 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 N3 Ni1 N1 94.04(13) . . ? N3 Ni1 O1 102.52(12) . . ? N1 Ni1 O1 88.63(11) . . ? N3 Ni1 O7 169.19(11) . . ? N1 Ni1 O7 93.55(12) . . ? O1 Ni1 O7 85.35(10) . . ? N3 Ni1 O6 90.60(11) . . ? N1 Ni1 O6 93.90(12) . . ? O1 Ni1 O6 166.44(10) . . ? O7 Ni1 O6 81.21(10) . . ? N3 Ni1 O2 89.35(11) . . ? N1 Ni1 O2 170.13(11) . . ? O1 Ni1 O2 81.58(10) . . ? O7 Ni1 O2 84.43(10) . . ? O6 Ni1 O2 95.33(10) . . ? N4 Ni2 N2 93.64(12) . . ? N4 Ni2 O3 102.00(12) . . ? N2 Ni2 O3 87.36(11) . . ? N4 Ni2 O8 169.38(12) . 1_455 ? N2 Ni2 O8 94.95(12) . 1_455 ? O3 Ni2 O8 84.65(10) . 1_455 ? N4 Ni2 O9 92.01(11) . 1_455 ? N2 Ni2 O9 94.29(12) . 1_455 ? O3 Ni2 O9 165.77(10) . 1_455 ? O8 Ni2 O9 81.13(10) 1_455 1_455 ? N4 Ni2 O2 87.29(11) . . ? N2 Ni2 O2 169.15(11) . . ? O3 Ni2 O2 81.88(10) . . ? O8 Ni2 O2 85.45(10) 1_455 . ? O9 Ni2 O2 96.48(10) 1_455 . ? C1 O1 Ni1 105.7(2) . . ? C2 O2 Ni1 98.9(2) . . ? C2 O2 Ni2 99.6(2) . . ? Ni1 O2 Ni2 161.00(13) . . ? C3 O3 Ni2 106.1(2) . . ? C6 O6 Ni1 108.2(2) . . ? C7 O7 Ni1 108.0(2) . . ? C8 O8 Ni2 107.9(2) . 1_655 ? C9 O9 Ni2 107.8(2) . 1_655 ? C11 N1 C15 116.1(3) . . ? C11 N1 Ni1 120.9(3) . . ? C15 N1 Ni1 122.7(3) . . ? C18 N2 C22 116.2(3) . . ? C18 N2 Ni2 122.8(3) . . ? C22 N2 Ni2 121.0(3) . . ? C27 N3 C23 116.6(3) . . ? C27 N3 Ni1 124.2(3) . . ? C23 N3 Ni1 118.5(3) . . ? C34 N4 C30 117.7(3) . . ? C34 N4 Ni2 120.9(3) . . ? C30 N4 Ni2 120.8(3) . . ? O1 C1 C2 123.0(3) . . ? O1 C1 C5 128.4(3) . . ? C2 C1 C5 108.6(3) . . ? O2 C2 C1 124.9(3) . . ? O2 C2 C3 124.5(3) . . ? C1 C2 C3 110.6(3) . . ? O3 C3 C2 123.8(3) . . ? O3 C3 C4 128.4(3) . . ? C2 C3 C4 107.8(3) . . ? O4 C4 C3 128.3(4) . . ? O4 C4 C5 125.2(4) . . ? C3 C4 C5 106.5(3) . . ? O5 C5 C1 128.3(4) . . ? O5 C5 C4 125.5(4) . . ? C1 C5 C4 106.2(3) . . ? O6 C6 C7 120.6(3) . . ? O6 C6 C10 129.1(3) . . ? C7 C6 C10 110.3(3) . . ? O7 C7 C8 130.3(3) . . ? O7 C7 C6 122.0(3) . . ? C8 C7 C6 107.7(3) . . ? O8 C8 C9 121.9(3) . . ? O8 C8 C7 130.4(3) . . ? C9 C8 C7 107.7(3) . . ? O9 C9 C8 121.0(3) . . ? O9 C9 C10 128.5(3) . . ? C8 C9 C10 110.5(3) . . ? O10 C10 C6 127.7(4) . . ? O10 C10 C9 128.7(4) . . ? C6 C10 C9 103.6(3) . . ? N1 C11 C12 123.7(4) . . ? C13 C12 C11 120.0(4) . . ? C12 C13 C14 116.4(4) . . ? C12 C13 C16 120.7(4) . . ? C14 C13 C16 122.9(4) . . ? C15 C14 C13 120.2(4) . . ? N1 C15 C14 123.6(4) . . ? C17 C16 C13 125.3(4) 1_654 . ? C16 C17 C20 125.6(4) 1_456 . ? N2 C18 C19 123.6(4) . . ? C18 C19 C20 120.4(4) . . ? C19 C20 C21 116.2(4) . . ? C19 C20 C17 118.9(4) . . ? C21 C20 C17 124.8(4) . . ? C22 C21 C20 119.9(4) . . ? N2 C22 C21 123.7(4) . . ? N3 C23 C24 123.3(4) . . ? C23 C24 C25 120.3(4) . . ? C24 C25 C26 116.2(4) . . ? C24 C25 C28 123.1(4) . . ? C26 C25 C28 120.7(4) . . ? C27 C26 C25 120.0(4) . . ? N3 C27 C26 123.6(4) . . ? C29 C28 C25 124.6(4) 4_475 . ? C28 C29 C32 125.2(4) 4_676 . ? N4 C30 C31 122.6(4) . . ? C32 C31 C30 120.0(4) . . ? C31 C32 C33 117.0(4) . . ? C31 C32 C29 123.1(4) . . ? C33 C32 C29 119.8(4) . . ? C34 C33 C32 119.9(4) . . ? N4 C34 C33 122.7(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.753 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.099