Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_(Ni3(btc)2(4-AP)6.(BuOH)6(H2O)2) _database_code_CSD 154064 _publ_contact_author ; Matthew J. Rosseinsky Department of Chemistry University of Liverpool Liverpool L69 7ZD UK ; _publ_contact_author_phone '(44) 151 7943499' _publ_contact_author_fax '(44) 151 7943587' _publ_contact_author_email m.j.rosseinsky@liv.ac.uk _journal_coden_Cambridge 182 _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ; ? ; _publ_section_title ; Crystal engineering of a 3-D coordination polymer from 2-D building blocks. ; loop_ _publ_author_name _publ_author_address 'Prior, Timothy J.' ; Department of Chemistry University of Liverpool Liverpool L69 7ZD UK ; 'Rosseinsky, Matthew J.' ; Department of Chemistry University of Liverpool Liverpool L69 7ZD UK ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural 'Ni 1.5 (C 9 H 3 O 6) (C 5 N 2 H 6)3.3(C 4 H 10 O)(H 2 O)' _chemical_formula_sum 'C36 H53 N6 Ni1.5 O10' _chemical_formula_weight 818.015 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1698(9) _cell_length_b 19.1965(12) _cell_length_c 16.6969(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.9670(10) _cell_angle_gamma 90.00 _cell_volume 3992.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14214 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 29.25 _exptl_crystal_description 'rod' _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.99 _exptl_apsorpt_process_details ; Sheldrick, G. M., SADABS; Universitat Gottingen, 1997' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker AXS SMART CCD diffractometer' _diffrn_measurement_method 'omega rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13204 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.24 _reflns_number_total 9505 _reflns_number_gt 7586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'LSCELL (Clegg, 1997)' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg)' _computing_publication_material 'Stoe X-step' _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. The material is a 3-D coordination polymer. It is highly porous. Puckered sheets of (6,3) nets are linked together by 4-aminopyridine. Butan-1-ol is found hydrogen bonding to the framework. All non-hydrogen atoms in the framework and the pores are modelled using anisotropic temperature factors. Hydrogen atoms have isotropic temperature factors. Hydrogen atoms are placed using a riding model except those listed below. Constraints are given in SHELX format: SADI 0.02 N2 H2A N2 H2B N4 H41 N4 H42 SADI 0.02 O10 H101 O10 H102 DFIX 1.95 0.05 H102 O2 No significant disorder is present in this material. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_scheme_details 'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+20.8156P] 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 9505 _refine_ls_number_parameters 515 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2222 _refine_ls_wR_factor_gt 0.2068 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0073(3) 0.0722(2) 0.3381(3) 0.0141(8) Uani 1 d . . . C2 C 0.0746(3) 0.1209(2) 0.3059(2) 0.0134(8) Uani 1 d . . . C3 C 0.1787(3) 0.1359(3) 0.3585(3) 0.0159(8) Uani 1 d . . . H3 H 0.2059 0.1149 0.4129 0.019 Uiso 1 calc R . . C4 C 0.2429(3) 0.1817(2) 0.3312(2) 0.0145(8) Uani 1 d . . . C5 C 0.3553(3) 0.1950(3) 0.3856(3) 0.0157(8) Uani 1 d . . . C6 C 0.2026(3) 0.2138(3) 0.2529(3) 0.0172(9) Uani 1 d . . . H6 H 0.2454 0.2463 0.2352 0.021 Uiso 1 calc R . . C7 C 0.0993(3) 0.1983(2) 0.2002(2) 0.0148(8) Uani 1 d . . . C8 C 0.0631(3) 0.2311(3) 0.1147(3) 0.0181(9) Uani 1 d . . . C9 C 0.0368(3) 0.1506(2) 0.2255(3) 0.0159(8) Uani 1 d . . . H9 H -0.0320 0.1381 0.1879 0.019 Uiso 1 calc R . . C10 C -0.0753(4) 0.0944(3) 0.6172(3) 0.0191(9) Uani 1 d . . . H10 H -0.1115 0.0534 0.6249 0.023 Uiso 1 calc R . . C11 C -0.0792(4) 0.1515(3) 0.6650(3) 0.0230(10) Uani 1 d . . . H11 H -0.1174 0.1492 0.7044 0.028 Uiso 1 calc R . . C12 C -0.0276(4) 0.2132(3) 0.6565(3) 0.0205(9) Uani 1 d . . . C13 C 0.0230(4) 0.2133(3) 0.5943(3) 0.0211(9) Uani 1 d . . . H13 H 0.0569 0.2543 0.5835 0.025 Uiso 1 calc R . . C14 C 0.0227(3) 0.1533(3) 0.5492(3) 0.0184(9) Uani 1 d . . . H14 H 0.0575 0.1547 0.5074 0.022 Uiso 1 calc R . . C20 C 0.6114(4) 0.3527(3) 0.4008(3) 0.0239(10) Uani 1 d . . . H20 H 0.5406 0.3523 0.3615 0.029 Uiso 1 calc R . . C21 C 0.6779(4) 0.4052(3) 0.3952(3) 0.0285(11) Uani 1 d . . . H21 H 0.6535 0.4402 0.3532 0.034 Uiso 1 calc R . . C22 C 0.7832(4) 0.4071(3) 0.4524(3) 0.0277(11) Uani 1 d . . . C23 C 0.8133(4) 0.3538(3) 0.5116(3) 0.0282(11) Uani 1 d . . . H23 H 0.8837 0.3529 0.5514 0.034 Uiso 1 calc R . . C24 C 0.7413(3) 0.3028(3) 0.5124(3) 0.0232(10) Uani 1 d . . . H24 H 0.7641 0.2665 0.5531 0.028 Uiso 1 calc R . . C30 C 0.6819(3) 0.1575(3) 0.3901(3) 0.0184(9) Uani 1 d . . . H30 H 0.6784 0.2009 0.3621 0.022 Uiso 1 calc R . . C31 C 0.7526(3) 0.1082(3) 0.3802(3) 0.0188(9) Uani 1 d . . . H31 H 0.7974 0.1182 0.3471 0.023 Uiso 1 calc R . . C32 C 0.7579(3) 0.0441(3) 0.4186(3) 0.0165(8) Uani 1 d . . . C33 C 0.6891(3) 0.0319(3) 0.4658(3) 0.0202(9) Uani 1 d . . . H33 H 0.6891 -0.0118 0.4925 0.024 Uiso 1 calc R . . C34 C 0.6214(3) 0.0846(3) 0.4729(3) 0.0212(9) Uani 1 d . . . H34 H 0.5751 0.0757 0.5051 0.025 Uiso 1 calc R . . C71 C -0.2618(5) 0.1419(4) -0.0611(4) 0.0399(14) Uani 1 d . . . H71A H -0.2794 0.1870 -0.0913 0.048 Uiso 1 calc R . . H71B H -0.3298 0.1163 -0.0706 0.048 Uiso 1 calc R . . C72 C -0.1912(5) 0.1007(4) -0.0988(4) 0.0441(16) Uani 1 d . . . H72A H -0.2229 0.1010 -0.1613 0.053 Uiso 1 calc R . . H72B H -0.1196 0.1229 -0.0836 0.053 Uiso 1 calc R . . C73 C -0.1788(6) 0.0268(4) -0.0677(5) 0.0504(17) Uani 1 d . . . H73A H -0.2501 0.0040 -0.0854 0.060 Uiso 1 calc R . . H73B H -0.1506 0.0267 -0.0051 0.060 Uiso 1 calc R . . C74 C -0.1030(8) -0.0150(5) -0.1020(6) 0.074(3) Uani 1 d . . . H74A H -0.0972 -0.0628 -0.0803 0.089 Uiso 1 calc R . . H74B H -0.0318 0.0068 -0.0837 0.089 Uiso 1 calc R . . H74C H -0.1313 -0.0158 -0.1641 0.089 Uiso 1 calc R . . C80 C 0.3440(5) 0.1811(3) 0.6527(3) 0.0332(12) Uani 1 d . . . H80A H 0.3202 0.2288 0.6325 0.040 Uiso 1 calc R . . H80B H 0.4235 0.1805 0.6733 0.040 Uiso 1 calc R . . C81 C 0.3027(4) 0.1622(3) 0.7240(3) 0.0300(11) Uani 1 d . . . H81A H 0.3294 0.1153 0.7454 0.036 Uiso 1 calc R . . H81B H 0.2233 0.1602 0.7021 0.036 Uiso 1 calc R . . C82 C 0.3377(6) 0.2144(4) 0.7971(4) 0.0440(16) Uani 1 d . . . H82A H 0.3258 0.2622 0.7735 0.053 Uiso 1 calc R . . H82B H 0.2917 0.2083 0.8331 0.053 Uiso 1 calc R . . C83 C 0.4530(7) 0.2074(5) 0.8513(4) 0.058(2) Uani 1 d . . . H83A H 0.4698 0.2423 0.8966 0.070 Uiso 1 calc R . . H83B H 0.4994 0.2146 0.8165 0.070 Uiso 1 calc R . . H83C H 0.4653 0.1606 0.8762 0.070 Uiso 1 calc R . . C91 C -0.4674(4) 0.0322(3) 0.1963(4) 0.0325(12) Uani 1 d . . . H91A H -0.3979 0.0173 0.2371 0.039 Uiso 1 calc R . . H91B H -0.4928 -0.0050 0.1533 0.039 Uiso 1 calc R . . C92 C -0.5470(4) 0.0420(3) 0.2417(3) 0.0329(12) Uani 1 d . . . H92A H -0.6147 0.0602 0.2014 0.039 Uiso 1 calc R . . H92B H -0.5192 0.0771 0.2870 0.039 Uiso 1 calc R . . C93 C -0.5707(5) -0.0253(4) 0.2808(4) 0.0361(13) Uani 1 d . . . H93A H -0.5956 -0.0611 0.2360 0.043 Uiso 1 calc R . . H93B H -0.5035 -0.0425 0.3229 0.043 Uiso 1 calc R . . C94 C -0.6546(6) -0.0159(5) 0.3235(4) 0.0519(18) Uani 1 d . . . H94A H -0.6670 -0.0604 0.3475 0.062 Uiso 1 calc R . . H94B H -0.7217 0.0002 0.2819 0.062 Uiso 1 calc R . . H94C H -0.6297 0.0187 0.3688 0.062 Uiso 1 calc R . . N1 N -0.0228(3) 0.0926(2) 0.5594(2) 0.0177(7) Uani 1 d . . . N2 N -0.0269(4) 0.2701(3) 0.7043(3) 0.0291(10) Uani 1 d D . . H2A H -0.051(5) 0.269(3) 0.747(3) 0.022(15) Uiso 1 d D . . H2B H 0.002(5) 0.306(3) 0.690(4) 0.035(18) Uiso 1 d D . . N3 N 0.6396(3) 0.3012(2) 0.4586(2) 0.0196(8) Uani 1 d . . . N4 N 0.8536(4) 0.4577(3) 0.4503(4) 0.0441(13) Uani 1 d D . . H41 H 0.822(7) 0.492(4) 0.419(5) 0.08(3) Uiso 1 d D . . H42 H 0.915(5) 0.456(5) 0.490(5) 0.08(3) Uiso 1 d D . . N5 N 0.6169(3) 0.1475(2) 0.4374(2) 0.0170(7) Uani 1 d . . . N6 N 0.8316(3) -0.0066(2) 0.4132(2) 0.0146(7) Uani 1 d . . . H61 H 0.843(5) -0.004(3) 0.362(4) 0.022(14) Uiso 1 d . . . H62 H 0.802(5) -0.049(4) 0.415(4) 0.037(18) Uiso 1 d . . . O1 O 0.0458(2) 0.05709(17) 0.41593(18) 0.0161(6) Uani 1 d . . . O2 O -0.0802(2) 0.0492(2) 0.2885(2) 0.0213(7) Uani 1 d D . . O3 O 0.3944(2) 0.16533(18) 0.45664(18) 0.0171(6) Uani 1 d . . . O4 O 0.4120(2) 0.23778(17) 0.36005(19) 0.0167(6) Uiso 1 d . . . O5 O 0.1135(2) 0.28293(19) 0.10061(19) 0.0205(7) Uani 1 d . . . O6 O -0.0140(2) 0.20454(19) 0.05522(19) 0.0214(7) Uani 1 d . . . O7 O -0.2144(3) 0.1551(3) 0.0273(3) 0.0392(10) Uani 1 d . . . H70 H -0.146(7) 0.167(5) 0.039(5) 0.059 Uiso 1 d . . . O8 O 0.3049(3) 0.1330(2) 0.5852(2) 0.0337(9) Uani 1 d . . . H81 H 0.3194 0.1475 0.5426 0.051 Uiso 1 calc R . . O9 O -0.4524(3) 0.0949(2) 0.1558(3) 0.0398(10) Uani 1 d . . . H90 H -0.3908 0.0950 0.1511 0.060 Uiso 1 calc R . . O10 O -0.2524(3) 0.0809(3) 0.1498(3) 0.0357(10) Uani 1 d D . . H101 H -0.239(6) 0.102(4) 0.113(4) 0.04(2) Uiso 1 d D . . H102 H -0.206(5) 0.072(5) 0.193(4) 0.08(3) Uiso 1 d D . . Ni1 Ni 0.53753(4) 0.22617(3) 0.47213(3) 0.01418(15) Uani 1 d . . . Ni2 Ni 0.0000 0.0000 0.5000 0.01233(18) Uani 1 d S . . 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 C1 0.0110(17) 0.016(2) 0.0146(17) 0.0004(15) 0.0032(14) 0.0002(14) C2 0.0115(17) 0.015(2) 0.0117(16) 0.0014(14) 0.0011(13) -0.0023(14) C3 0.0097(16) 0.024(3) 0.0123(17) -0.0021(15) 0.0008(13) -0.0010(15) C4 0.0073(16) 0.021(3) 0.0123(17) 0.0000(15) -0.0001(13) 0.0004(14) C5 0.0097(16) 0.021(3) 0.0138(17) -0.0022(16) 0.0003(13) -0.0019(15) C6 0.0103(17) 0.024(3) 0.0158(18) 0.0039(16) 0.0018(14) -0.0021(15) C7 0.0094(16) 0.022(2) 0.0106(16) 0.0040(15) -0.0009(13) -0.0016(15) C8 0.0110(17) 0.029(3) 0.0111(17) 0.0036(16) -0.0003(14) 0.0013(16) C9 0.0083(16) 0.021(3) 0.0145(18) -0.0010(16) -0.0014(13) -0.0041(15) C10 0.0195(19) 0.020(3) 0.0172(18) 0.0017(16) 0.0048(15) 0.0021(16) C11 0.018(2) 0.030(3) 0.020(2) 0.0024(18) 0.0066(16) 0.0009(18) C12 0.020(2) 0.022(3) 0.0154(18) 0.0011(16) 0.0001(15) 0.0016(17) C13 0.023(2) 0.019(3) 0.019(2) -0.0010(17) 0.0049(16) -0.0040(17) C14 0.0178(19) 0.020(3) 0.0167(18) 0.0018(16) 0.0050(15) 0.0012(16) C20 0.0149(19) 0.030(3) 0.023(2) 0.0007(19) 0.0014(16) 0.0009(18) C21 0.024(2) 0.029(3) 0.032(2) 0.001(2) 0.0076(19) 0.000(2) C22 0.020(2) 0.031(3) 0.034(3) -0.008(2) 0.0120(19) -0.0038(19) C23 0.0131(19) 0.040(3) 0.027(2) -0.006(2) 0.0008(17) -0.0053(19) C24 0.0125(19) 0.033(3) 0.020(2) 0.0011(19) 0.0001(16) 0.0009(17) C30 0.0184(19) 0.018(3) 0.0177(19) 0.0027(16) 0.0049(15) 0.0017(16) C31 0.0159(18) 0.021(3) 0.0192(19) 0.0016(17) 0.0061(15) 0.0009(16) C32 0.0094(16) 0.023(3) 0.0142(17) -0.0006(16) 0.0000(13) 0.0027(15) C33 0.0180(19) 0.022(3) 0.021(2) 0.0036(17) 0.0073(16) 0.0011(17) C34 0.0137(18) 0.030(3) 0.020(2) 0.0012(18) 0.0057(15) -0.0016(17) C71 0.031(3) 0.047(4) 0.032(3) 0.001(3) -0.005(2) -0.006(2) C72 0.039(3) 0.052(4) 0.035(3) -0.006(3) 0.003(2) -0.014(3) C73 0.043(4) 0.047(5) 0.053(4) -0.008(3) 0.005(3) -0.009(3) C74 0.076(6) 0.074(7) 0.058(5) -0.019(5) 0.003(4) 0.024(5) C80 0.044(3) 0.031(3) 0.026(2) -0.006(2) 0.014(2) -0.010(2) C81 0.028(2) 0.035(3) 0.026(2) 0.002(2) 0.0076(19) -0.001(2) C82 0.070(5) 0.036(4) 0.029(3) 0.000(2) 0.021(3) 0.007(3) C83 0.067(5) 0.073(6) 0.028(3) -0.007(3) 0.006(3) -0.026(4) C91 0.023(2) 0.035(3) 0.038(3) 0.001(2) 0.008(2) 0.000(2) C92 0.031(3) 0.038(4) 0.025(2) -0.002(2) 0.003(2) 0.000(2) C93 0.034(3) 0.039(4) 0.030(3) 0.000(2) 0.003(2) -0.008(2) C94 0.048(4) 0.073(6) 0.035(3) 0.005(3) 0.014(3) -0.010(4) N1 0.0157(16) 0.022(2) 0.0145(15) 0.0031(14) 0.0031(13) 0.0012(14) N2 0.042(3) 0.020(3) 0.027(2) -0.0054(18) 0.0140(19) -0.0026(19) N3 0.0096(15) 0.025(2) 0.0208(17) -0.0039(15) 0.0006(13) -0.0028(14) N4 0.028(2) 0.039(4) 0.063(4) -0.001(3) 0.011(2) -0.014(2) N5 0.0112(15) 0.024(2) 0.0144(15) -0.0015(14) 0.0018(12) -0.0002(13) N6 0.0096(15) 0.017(2) 0.0173(16) 0.0000(14) 0.0044(12) -0.0003(13) O1 0.0172(14) 0.0160(18) 0.0133(13) -0.0003(11) 0.0024(11) -0.0018(11) O2 0.0108(13) 0.032(2) 0.0175(14) 0.0017(13) -0.0006(11) -0.0072(12) O3 0.0113(13) 0.0248(19) 0.0112(12) 0.0028(12) -0.0018(10) -0.0028(11) O5 0.0159(14) 0.027(2) 0.0138(13) 0.0036(12) -0.0020(11) -0.0041(12) O6 0.0134(14) 0.030(2) 0.0129(13) 0.0021(13) -0.0066(11) -0.0054(12) O7 0.0262(19) 0.054(3) 0.035(2) -0.0053(19) 0.0066(16) -0.0168(18) O8 0.041(2) 0.039(3) 0.0223(17) -0.0056(16) 0.0116(15) -0.0167(18) O9 0.0224(18) 0.041(3) 0.056(3) 0.017(2) 0.0131(17) 0.0107(17) O10 0.0164(16) 0.052(3) 0.033(2) 0.0143(19) -0.0001(15) -0.0008(16) Ni1 0.0078(2) 0.0201(3) 0.0110(2) -0.0027(2) -0.00189(17) 0.00045(19) Ni2 0.0101(3) 0.0148(4) 0.0109(3) 0.0011(3) 0.0017(2) 0.0000(3) _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 C1 O2 1.260(5) . ? C1 O1 1.266(5) . ? C1 C2 1.503(6) . ? C2 C9 1.394(6) . ? C2 C3 1.397(5) . ? C3 C4 1.395(6) . ? C4 C6 1.385(6) . ? C4 C5 1.486(5) . ? C5 O3 1.264(5) . ? C5 O4 1.274(5) . ? C5 Ni1 2.439(4) . ? C6 C7 1.392(5) . ? C7 C9 1.385(6) . ? C7 C8 1.490(6) . ? C8 O5 1.260(6) . ? C8 O6 1.273(5) . ? C8 Ni1 2.435(4) 4_565 ? C10 N1 1.359(6) . ? C10 C11 1.367(7) . ? C11 C12 1.396(7) . ? C12 N2 1.352(7) . ? C12 C13 1.403(6) . ? C13 C14 1.377(7) . ? C14 N1 1.346(6) . ? C20 N3 1.347(6) . ? C20 C21 1.357(7) . ? C21 C22 1.405(7) . ? C22 N4 1.352(7) . ? C22 C23 1.387(8) . ? C23 C24 1.367(7) . ? C24 N3 1.349(5) . ? C30 N5 1.354(6) . ? C30 C31 1.375(6) . ? C31 C32 1.378(7) . ? C32 N6 1.398(6) . ? C32 C33 1.401(6) . ? C33 C34 1.379(7) . ? C34 N5 1.338(7) . ? C71 O7 1.426(7) . ? C71 C72 1.506(10) . ? C72 C73 1.501(11) . ? C73 C74 1.530(11) . ? C80 O8 1.420(6) . ? C80 C81 1.505(7) . ? C81 C82 1.531(8) . ? C82 C83 1.501(11) . ? C91 O9 1.425(7) . ? C91 C92 1.492(8) . ? C92 C93 1.525(9) . ? C93 C94 1.508(9) . ? N1 Ni2 2.104(4) . ? N3 Ni1 2.032(4) . ? N5 Ni1 2.026(4) . ? N6 Ni2 2.223(3) 1_655 ? O1 Ni2 2.021(3) . ? O3 Ni1 2.161(3) . ? O4 Ni1 2.067(3) . ? O5 Ni1 2.059(3) 4_565 ? O6 Ni1 2.183(3) 4_565 ? Ni1 O5 2.059(3) 4_666 ? Ni1 O6 2.183(3) 4_666 ? Ni1 C8 2.435(4) 4_666 ? Ni2 O1 2.021(3) 3_556 ? Ni2 N1 2.104(4) 3_556 ? Ni2 N6 2.223(3) 3_656 ? Ni2 N6 2.223(3) 1_455 ? 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 O2 C1 O1 124.8(4) . . ? O2 C1 C2 120.2(4) . . ? O1 C1 C2 115.0(3) . . ? C9 C2 C3 119.5(4) . . ? C9 C2 C1 122.1(3) . . ? C3 C2 C1 118.4(4) . . ? C4 C3 C2 119.9(4) . . ? C6 C4 C3 120.2(4) . . ? C6 C4 C5 120.1(4) . . ? C3 C4 C5 119.7(4) . . ? O3 C5 O4 120.1(4) . . ? O3 C5 C4 121.2(4) . . ? O4 C5 C4 118.8(4) . . ? O3 C5 Ni1 62.2(2) . . ? O4 C5 Ni1 57.9(2) . . ? C4 C5 Ni1 175.6(3) . . ? C4 C6 C7 119.8(4) . . ? C9 C7 C6 120.3(4) . . ? C9 C7 C8 122.3(4) . . ? C6 C7 C8 117.2(4) . . ? O5 C8 O6 120.4(4) . . ? O5 C8 C7 119.3(4) . . ? O6 C8 C7 120.2(4) . . ? O5 C8 Ni1 57.7(2) . 4_565 ? O6 C8 Ni1 63.3(2) . 4_565 ? C7 C8 Ni1 168.1(3) . 4_565 ? C7 C9 C2 120.1(4) . . ? N1 C10 C11 124.0(5) . . ? C10 C11 C12 120.6(4) . . ? N2 C12 C11 122.3(4) . . ? N2 C12 C13 121.5(5) . . ? C11 C12 C13 116.2(4) . . ? C14 C13 C12 119.1(4) . . ? N1 C14 C13 125.2(4) . . ? N3 C20 C21 124.1(4) . . ? C20 C21 C22 119.3(5) . . ? N4 C22 C23 120.6(5) . . ? N4 C22 C21 122.4(6) . . ? C23 C22 C21 117.0(5) . . ? C24 C23 C22 119.9(4) . . ? N3 C24 C23 123.4(5) . . ? N5 C30 C31 123.7(4) . . ? C30 C31 C32 119.5(4) . . ? C31 C32 N6 121.5(4) . . ? C31 C32 C33 117.8(4) . . ? N6 C32 C33 120.6(4) . . ? C34 C33 C32 118.7(4) . . ? N5 C34 C33 124.1(4) . . ? O7 C71 C72 113.8(5) . . ? C73 C72 C71 111.4(6) . . ? C72 C73 C74 112.1(7) . . ? O8 C80 C81 109.9(5) . . ? C80 C81 C82 112.3(5) . . ? C83 C82 C81 113.9(6) . . ? O9 C91 C92 111.3(5) . . ? C91 C92 C93 112.7(5) . . ? C94 C93 C92 112.6(6) . . ? C14 N1 C10 114.8(4) . . ? C14 N1 Ni2 122.2(3) . . ? C10 N1 Ni2 122.7(3) . . ? C20 N3 C24 116.3(4) . . ? C20 N3 Ni1 124.2(3) . . ? C24 N3 Ni1 119.4(3) . . ? C34 N5 C30 116.2(4) . . ? C34 N5 Ni1 119.9(3) . . ? C30 N5 Ni1 123.0(3) . . ? C32 N6 Ni2 119.0(3) . 1_655 ? C1 O1 Ni2 136.6(3) . . ? C5 O3 Ni1 86.7(2) . . ? C5 O4 Ni1 90.6(2) . . ? C8 O5 Ni1 91.2(2) . 4_565 ? C8 O6 Ni1 85.3(3) . 4_565 ? N5 Ni1 N3 94.29(16) . . ? N5 Ni1 O5 96.52(14) . 4_666 ? N3 Ni1 O5 93.50(15) . 4_666 ? N5 Ni1 O4 99.00(13) . . ? N3 Ni1 O4 100.72(14) . . ? O5 Ni1 O4 158.03(13) 4_666 . ? N5 Ni1 O3 94.24(14) . . ? N3 Ni1 O3 162.32(14) . . ? O5 Ni1 O3 100.87(13) 4_666 . ? O4 Ni1 O3 62.61(12) . . ? N5 Ni1 O6 158.73(13) . 4_666 ? N3 Ni1 O6 89.57(15) . 4_666 ? O5 Ni1 O6 62.34(12) 4_666 4_666 ? O4 Ni1 O6 100.81(12) . 4_666 ? O3 Ni1 O6 88.06(13) . 4_666 ? N5 Ni1 C8 127.62(15) . 4_666 ? N3 Ni1 C8 89.09(16) . 4_666 ? O5 Ni1 C8 31.15(14) 4_666 4_666 ? O4 Ni1 C8 131.64(14) . 4_666 ? O3 Ni1 C8 97.87(13) . 4_666 ? O6 Ni1 C8 31.40(13) 4_666 4_666 ? N5 Ni1 C5 98.49(15) . . ? N3 Ni1 C5 131.84(15) . . ? O5 Ni1 C5 130.36(14) 4_666 . ? O4 Ni1 C5 31.47(14) . . ? O3 Ni1 C5 31.15(13) . . ? O6 Ni1 C5 94.39(13) 4_666 . ? C8 Ni1 C5 117.25(14) 4_666 . ? O1 Ni2 N1 90.58(14) 3_556 . ? O1 Ni2 N1 89.42(14) . . ? O1 Ni2 N1 89.42(14) 3_556 3_556 ? O1 Ni2 N1 90.58(14) . 3_556 ? O1 Ni2 N6 92.17(13) 3_556 3_656 ? O1 Ni2 N6 87.83(13) . 3_656 ? N1 Ni2 N6 84.81(14) . 3_656 ? N1 Ni2 N6 95.19(14) 3_556 3_656 ? O1 Ni2 N6 87.83(13) 3_556 1_455 ? O1 Ni2 N6 92.17(13) . 1_455 ? N1 Ni2 N6 95.19(14) . 1_455 ? N1 Ni2 N6 84.81(14) 3_556 1_455 ? _diffrn_measured_theta_max 30.24 _diffrn_measured_fraction_theta_max 0.778 _diffrn_reflns_theta_full 24.60 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.694 _refine_diff_density_min -1.961 _refine_diff_density_rms 0.143