Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_address 'Kutasi, Anna M.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Batten, Stuart R.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Moubaraki, Boujemaa' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; 'Murray, Keith S.' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; _publ_contact_author_name 'Prof K S Murray' _publ_contact_author_address ; School of Chemistry Monash University PO Box 23 3800 Victoria AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email 'Keith.S.Murray@sci.monash.edu.au ' _publ_section_title ; New 2D coordination polymers containing both bidentate and tridentate dicyanamide bridges and intercalated phenazine. ; data_Co(dca)2(H2O).phz _database_code_CSD 175180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Co N8 O' _chemical_formula_weight 389.25 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 22.3876(4) _cell_length_b 7.41100(10) _cell_length_c 19.5978(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3251.56(9) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7740 _exptl_absorpt_correction_T_max 0.8997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32505 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4006 _reflns_number_gt 2870 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0301P)^2^+3.3751P] 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 4006 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.5000 -0.00761(5) 0.2500 0.01153(10) Uani 1 2 d S . . Co2 Co 0.5000 0.5000 0.5000 0.01030(10) Uani 1 2 d S . . O1 O 0.59023(7) 0.5425(2) 0.50696(8) 0.0221(3) Uani 1 1 d . . . H1 H 0.6182(14) 0.467(4) 0.5053(13) 0.040(8) Uiso 1 1 d . . . H2 H 0.6064(14) 0.633(4) 0.4977(14) 0.048(10) Uiso 1 1 d . . . N1 N 0.70107(7) 0.3675(2) 0.49948(8) 0.0163(3) Uani 1 1 d . . . C2 C 0.72442(9) 0.3000(3) 0.44182(10) 0.0173(4) Uani 1 1 d . . . C3 C 0.68561(10) 0.2421(3) 0.38811(11) 0.0221(5) Uani 1 1 d . . . H3A H 0.6435 0.2493 0.3936 0.027 Uiso 1 1 calc R . . C4 C 0.70919(10) 0.1769(3) 0.32926(11) 0.0253(5) Uani 1 1 d . . . H4A H 0.6833 0.1385 0.2937 0.030 Uiso 1 1 calc R . . C5 C 0.77198(10) 0.1653(3) 0.31996(11) 0.0260(5) Uani 1 1 d . . . H5A H 0.7874 0.1206 0.2781 0.031 Uiso 1 1 calc R . . C6 C 0.81028(10) 0.2167(3) 0.36972(11) 0.0245(5) Uani 1 1 d . . . H6A H 0.8522 0.2075 0.3627 0.029 Uiso 1 1 calc R . . C7 C 0.78779(9) 0.2846(3) 0.43268(10) 0.0182(4) Uani 1 1 d . . . N8 N 0.82629(7) 0.3333(2) 0.48235(9) 0.0198(4) Uani 1 1 d . . . C9 C 0.80302(9) 0.4020(3) 0.53952(10) 0.0178(4) Uani 1 1 d . . . C10 C 0.84139(10) 0.4575(3) 0.59349(11) 0.0235(5) Uani 1 1 d . . . H10A H 0.8834 0.4426 0.5892 0.028 Uiso 1 1 calc R . . C11 C 0.81830(10) 0.5319(3) 0.65127(11) 0.0262(5) Uani 1 1 d . . . H11A H 0.8444 0.5694 0.6868 0.031 Uiso 1 1 calc R . . C12 C 0.75558(10) 0.5538(3) 0.65897(10) 0.0234(5) Uani 1 1 d . . . H12A H 0.7404 0.6081 0.6993 0.028 Uiso 1 1 calc R . . C13 C 0.71708(9) 0.4988(3) 0.60982(10) 0.0200(4) Uani 1 1 d . . . H13A H 0.6752 0.5118 0.6163 0.024 Uiso 1 1 calc R . . C14 C 0.73960(8) 0.4212(3) 0.54830(10) 0.0158(4) Uani 1 1 d . . . N23 N 0.50574(7) -0.0034(2) 0.36270(8) 0.0163(3) Uani 1 1 d . . . C21 C 0.50162(8) -0.1540(3) 0.39848(10) 0.0145(4) Uani 1 1 d . . . N21 N 0.49741(8) -0.2902(2) 0.42643(9) 0.0187(4) Uani 1 1 d . . . C22 C 0.50939(8) 0.1491(3) 0.39817(9) 0.0139(4) Uani 1 1 d . . . N22 N 0.51215(7) 0.2856(2) 0.42640(8) 0.0176(4) Uani 1 1 d . . . N33 N 0.61159(8) 0.4911(2) 0.22941(11) 0.0295(5) Uani 1 1 d . . . C31 C 0.58359(9) 0.3384(3) 0.23825(10) 0.0165(4) Uani 1 1 d . . . N31 N 0.56364(8) 0.1964(2) 0.24506(8) 0.0181(4) Uani 1 1 d . . . C32 C 0.58290(9) 0.6428(3) 0.23830(10) 0.0165(4) Uani 1 1 d . . . N32 N 0.56278(8) 0.7847(2) 0.24532(8) 0.0178(4) Uani 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 Co1 0.01536(18) 0.00865(18) 0.01059(17) 0.000 0.00050(14) 0.000 Co2 0.01122(17) 0.00853(17) 0.01115(17) 0.00009(13) -0.00004(13) -0.00058(14) O1 0.0109(7) 0.0145(8) 0.0408(10) 0.0008(7) 0.0003(6) -0.0010(6) N1 0.0151(8) 0.0153(8) 0.0185(9) 0.0021(7) -0.0013(7) 0.0013(7) C2 0.0203(10) 0.0149(9) 0.0167(10) 0.0015(8) -0.0008(8) 0.0035(9) C3 0.0213(11) 0.0208(11) 0.0242(11) -0.0006(9) -0.0060(8) 0.0023(9) C4 0.0371(13) 0.0199(11) 0.0190(11) -0.0011(9) -0.0069(9) 0.0032(10) C5 0.0395(13) 0.0208(11) 0.0178(11) -0.0007(8) 0.0011(9) 0.0080(10) C6 0.0256(11) 0.0224(11) 0.0255(12) 0.0013(9) 0.0045(9) 0.0057(9) C7 0.0207(10) 0.0152(9) 0.0186(10) 0.0027(8) 0.0003(8) 0.0042(9) N8 0.0173(8) 0.0199(9) 0.0222(9) 0.0024(7) 0.0005(7) 0.0021(7) C9 0.0188(10) 0.0149(9) 0.0196(10) 0.0043(8) -0.0011(8) 0.0000(8) C10 0.0187(10) 0.0243(11) 0.0275(12) 0.0021(9) -0.0065(9) -0.0016(9) C11 0.0315(12) 0.0234(11) 0.0237(11) 0.0031(9) -0.0108(9) -0.0057(10) C12 0.0356(12) 0.0183(10) 0.0163(10) -0.0001(8) 0.0001(9) -0.0004(9) C13 0.0236(10) 0.0160(10) 0.0203(10) 0.0024(8) 0.0035(8) 0.0012(9) C14 0.0175(10) 0.0139(10) 0.0160(9) 0.0038(8) -0.0007(8) 0.0015(8) N23 0.0279(9) 0.0090(7) 0.0119(8) 0.0013(6) 0.0010(7) -0.0003(7) C21 0.0166(9) 0.0151(9) 0.0119(9) -0.0032(7) -0.0002(8) 0.0002(8) N21 0.0264(9) 0.0130(8) 0.0166(9) 0.0004(7) -0.0018(7) -0.0010(8) C22 0.0160(10) 0.0148(9) 0.0109(9) 0.0025(7) 0.0020(7) -0.0001(8) N22 0.0250(9) 0.0131(8) 0.0147(8) -0.0005(7) 0.0016(7) 0.0003(7) N33 0.0192(9) 0.0117(9) 0.0576(14) -0.0004(8) 0.0120(9) -0.0005(8) C31 0.0138(9) 0.0154(10) 0.0202(11) -0.0008(8) 0.0012(8) 0.0046(8) N31 0.0191(9) 0.0158(9) 0.0196(9) -0.0005(7) 0.0011(7) -0.0009(7) C32 0.0139(9) 0.0158(10) 0.0197(11) 0.0021(8) 0.0017(8) -0.0039(8) N32 0.0181(8) 0.0136(8) 0.0216(9) 0.0016(7) 0.0009(7) -0.0001(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 N31 2.0798(17) . ? Co1 N31 2.0798(17) 4_655 ? Co1 N32 2.0861(17) 4_645 ? Co1 N32 2.0861(17) 1_545 ? Co1 N23 2.2126(16) . ? Co1 N23 2.2126(16) 4_655 ? Co2 O1 2.0490(15) 5_666 ? Co2 O1 2.0490(15) . ? Co2 N21 2.1213(16) 5_656 ? Co2 N21 2.1213(16) 1_565 ? Co2 N22 2.1630(16) 5_666 ? Co2 N22 2.1630(16) . ? O1 H1 0.84(3) . ? O1 H2 0.78(3) . ? N1 C2 1.342(2) . ? N1 C14 1.348(2) . ? C2 C3 1.431(3) . ? C2 C7 1.434(3) . ? C3 C4 1.357(3) . ? C3 H3A 0.9500 . ? C4 C5 1.420(3) . ? C4 H4A 0.9500 . ? C5 C6 1.353(3) . ? C5 H5A 0.9500 . ? C6 C7 1.425(3) . ? C6 H6A 0.9500 . ? C7 N8 1.349(3) . ? N8 C9 1.337(3) . ? C9 C10 1.423(3) . ? C9 C14 1.437(3) . ? C10 C11 1.361(3) . ? C10 H10A 0.9500 . ? C11 C12 1.422(3) . ? C11 H11A 0.9500 . ? C12 C13 1.356(3) . ? C12 H12A 0.9500 . ? C13 C14 1.428(3) . ? C13 H13A 0.9500 . ? N23 C21 1.321(2) . ? N23 C22 1.329(2) . ? C21 N21 1.153(2) . ? N21 Co2 2.1213(16) 1_545 ? C22 N22 1.154(2) . ? N33 C31 1.306(3) . ? N33 C32 1.306(3) . ? C31 N31 1.151(3) . ? C32 N32 1.153(3) . ? N32 Co1 2.0861(17) 1_565 ? 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 N31 Co1 N31 86.73(9) . 4_655 ? N31 Co1 N32 179.09(7) . 4_645 ? N31 Co1 N32 94.17(7) 4_655 4_645 ? N31 Co1 N32 94.17(7) . 1_545 ? N31 Co1 N32 179.09(7) 4_655 1_545 ? N32 Co1 N32 84.93(9) 4_645 1_545 ? N31 Co1 N23 89.79(6) . . ? N31 Co1 N23 89.02(6) 4_655 . ? N32 Co1 N23 90.33(6) 4_645 . ? N32 Co1 N23 90.87(6) 1_545 . ? N31 Co1 N23 89.02(6) . 4_655 ? N31 Co1 N23 89.79(6) 4_655 4_655 ? N32 Co1 N23 90.87(6) 4_645 4_655 ? N32 Co1 N23 90.33(6) 1_545 4_655 ? N23 Co1 N23 178.37(8) . 4_655 ? O1 Co2 O1 180.0 5_666 . ? O1 Co2 N21 87.68(7) 5_666 5_656 ? O1 Co2 N21 92.32(7) . 5_656 ? O1 Co2 N21 92.32(7) 5_666 1_565 ? O1 Co2 N21 87.68(7) . 1_565 ? N21 Co2 N21 180.00(7) 5_656 1_565 ? O1 Co2 N22 91.91(6) 5_666 5_666 ? O1 Co2 N22 88.09(6) . 5_666 ? N21 Co2 N22 95.09(6) 5_656 5_666 ? N21 Co2 N22 84.91(6) 1_565 5_666 ? O1 Co2 N22 88.09(6) 5_666 . ? O1 Co2 N22 91.91(6) . . ? N21 Co2 N22 84.91(6) 5_656 . ? N21 Co2 N22 95.09(6) 1_565 . ? N22 Co2 N22 180.0 5_666 . ? Co2 O1 H1 129(2) . . ? Co2 O1 H2 125(2) . . ? H1 O1 H2 102(3) . . ? C2 N1 C14 117.28(17) . . ? N1 C2 C3 119.65(18) . . ? N1 C2 C7 121.34(18) . . ? C3 C2 C7 119.01(18) . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 121.2(2) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? N8 C7 C6 119.58(19) . . ? N8 C7 C2 121.36(18) . . ? C6 C7 C2 119.06(19) . . ? C9 N8 C7 117.24(17) . . ? N8 C9 C10 119.85(18) . . ? N8 C9 C14 121.54(18) . . ? C10 C9 C14 118.61(19) . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 121.21(19) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 119.78(19) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? N1 C14 C13 119.48(17) . . ? N1 C14 C9 121.19(18) . . ? C13 C14 C9 119.32(18) . . ? C21 N23 C22 116.42(16) . . ? C21 N23 Co1 120.91(12) . . ? C22 N23 Co1 122.52(12) . . ? N21 C21 N23 176.3(2) . . ? C21 N21 Co2 164.35(16) . 1_545 ? N22 C22 N23 177.1(2) . . ? C22 N22 Co2 163.01(16) . . ? C31 N33 C32 119.50(18) . . ? N31 C31 N33 174.0(2) . . ? C31 N31 Co1 159.39(16) . . ? N32 C32 N33 173.4(2) . . ? C32 N32 Co1 160.36(16) . 1_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.291 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.064 #=END data_Ni(dca)2(H2O).phz _database_code_CSD 175181 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 N8 Ni O' _chemical_formula_weight 389.03 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 22.4149(7) _cell_length_b 7.3152(1) _cell_length_c 19.5234(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3201.24(13) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7474 _exptl_absorpt_correction_T_max 0.8863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35930 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3894 _reflns_number_gt 2066 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0683P)^2^+1.9811P] 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 3894 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.5000 -0.00881(7) 0.2500 0.01751(18) Uani 1 2 d S . . Ni2 Ni 0.5000 0.5000 0.5000 0.01682(18) Uani 1 2 d S . . O1 O 0.58927(13) 0.5419(4) 0.51215(14) 0.0321(7) Uani 1 1 d . . . H1 H 0.613(2) 0.458(6) 0.5065(18) 0.038(13) Uiso 1 1 d . . . H2 H 0.607(2) 0.626(6) 0.500(2) 0.054(16) Uiso 1 1 d . . . N1 N 0.70144(13) 0.3684(3) 0.50006(14) 0.0216(6) Uani 1 1 d . . . C2 C 0.72499(15) 0.3004(4) 0.44195(17) 0.0236(8) Uani 1 1 d . . . C3 C 0.68655(17) 0.2419(4) 0.38832(18) 0.0288(9) Uani 1 1 d . . . H3A H 0.6445 0.2481 0.3938 0.035 Uiso 1 1 calc R . . C4 C 0.71032(18) 0.1775(5) 0.32956(19) 0.0319(9) Uani 1 1 d . . . H4A H 0.6846 0.1380 0.2938 0.038 Uiso 1 1 calc R . . C5 C 0.77265(18) 0.1678(5) 0.32014(19) 0.0332(10) Uani 1 1 d . . . H5A H 0.7881 0.1244 0.2778 0.040 Uiso 1 1 calc R . . C6 C 0.81087(18) 0.2189(4) 0.37026(19) 0.0312(9) Uani 1 1 d . . . H6A H 0.8527 0.2092 0.3632 0.037 Uiso 1 1 calc R . . C7 C 0.78856(15) 0.2869(4) 0.43326(18) 0.0237(8) Uani 1 1 d . . . N8 N 0.82663(13) 0.3363(4) 0.48350(15) 0.0255(7) Uani 1 1 d . . . C9 C 0.80298(15) 0.4037(4) 0.54072(17) 0.0227(8) Uani 1 1 d . . . C10 C 0.84113(17) 0.4604(4) 0.59508(19) 0.0292(9) Uani 1 1 d . . . H10A H 0.8831 0.4465 0.5909 0.035 Uiso 1 1 calc R . . C11 C 0.81762(18) 0.5343(4) 0.65294(19) 0.0322(9) Uani 1 1 d . . . H11A H 0.8434 0.5729 0.6888 0.039 Uiso 1 1 calc R . . C12 C 0.75501(16) 0.5545(4) 0.66038(17) 0.0270(8) Uani 1 1 d . . . H12A H 0.7395 0.6082 0.7009 0.032 Uiso 1 1 calc R . . C13 C 0.71730(16) 0.4992(4) 0.61122(17) 0.0232(8) Uani 1 1 d . . . H13A H 0.6755 0.5117 0.6177 0.028 Uiso 1 1 calc R . . C14 C 0.73966(15) 0.4220(4) 0.54940(17) 0.0219(8) Uani 1 1 d . . . N23 N 0.50657(12) -0.0041(3) 0.36232(15) 0.0248(7) Uani 1 1 d . . . C21 C 0.50342(14) -0.1555(4) 0.39876(17) 0.0222(8) Uani 1 1 d . . . N21 N 0.50013(12) -0.2938(4) 0.42720(15) 0.0249(7) Uani 1 1 d . . . C22 C 0.51055(15) 0.1517(4) 0.39859(17) 0.0210(8) Uani 1 1 d . . . N22 N 0.51364(13) 0.2891(4) 0.42682(15) 0.0258(7) Uani 1 1 d . . . N33 N 0.61104(14) 0.4893(3) 0.23081(18) 0.0362(8) Uani 1 1 d . . . C31 C 0.58286(15) 0.3358(4) 0.23897(17) 0.0231(8) Uani 1 1 d . . . N31 N 0.56300(13) 0.1920(4) 0.24516(13) 0.0244(7) Uani 1 1 d . . . C32 C 0.58194(15) 0.6446(5) 0.23895(17) 0.0244(8) Uani 1 1 d . . . N32 N 0.56181(13) 0.7883(4) 0.24550(14) 0.0244(7) Uani 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 0.0203(3) 0.0138(3) 0.0184(3) 0.000 0.0017(3) 0.000 Ni2 0.0170(3) 0.0131(3) 0.0204(3) -0.0002(2) 0.0002(2) -0.0008(2) O1 0.0204(15) 0.0211(16) 0.055(2) -0.0001(13) 0.0006(13) -0.0028(13) N1 0.0201(15) 0.0171(15) 0.0274(17) 0.0020(12) -0.0014(13) 0.0011(11) C2 0.025(2) 0.0226(18) 0.023(2) 0.0036(15) 0.0016(16) 0.0017(15) C3 0.030(2) 0.0245(19) 0.032(2) -0.0026(16) -0.0074(17) 0.0013(15) C4 0.043(3) 0.027(2) 0.025(2) -0.0003(15) -0.0075(18) 0.0021(16) C5 0.049(3) 0.026(2) 0.025(2) -0.0001(15) -0.0010(19) 0.0101(17) C6 0.035(2) 0.0275(19) 0.031(2) 0.0047(17) 0.0064(19) 0.0092(16) C7 0.027(2) 0.0182(17) 0.026(2) 0.0020(15) 0.0016(16) 0.0056(14) N8 0.0224(16) 0.0226(16) 0.0315(18) 0.0027(12) 0.0000(14) 0.0015(12) C9 0.0231(19) 0.0204(18) 0.025(2) 0.0060(14) -0.0035(16) 0.0007(14) C10 0.026(2) 0.0285(19) 0.033(2) 0.0046(16) -0.0054(17) 0.0002(15) C11 0.043(3) 0.0251(19) 0.029(2) 0.0072(16) -0.0124(18) -0.0076(17) C12 0.040(2) 0.0198(17) 0.022(2) 0.0018(14) 0.0024(18) 0.0001(15) C13 0.029(2) 0.0162(18) 0.0245(19) 0.0006(14) 0.0024(16) 0.0030(14) C14 0.026(2) 0.0178(18) 0.0215(19) 0.0040(13) -0.0009(16) 0.0017(14) N23 0.0349(19) 0.0160(15) 0.0235(16) 0.0032(12) 0.0015(13) 0.0032(12) C21 0.0205(18) 0.0208(19) 0.0253(19) -0.0057(15) 0.0010(15) 0.0004(14) N21 0.0330(18) 0.0177(15) 0.0238(16) 0.0002(12) -0.0011(14) -0.0024(13) C22 0.026(2) 0.0185(19) 0.0185(18) 0.0009(14) 0.0029(15) 0.0002(14) N22 0.0318(18) 0.0188(16) 0.0266(17) 0.0008(13) 0.0032(13) -0.0011(12) N33 0.0248(18) 0.0216(17) 0.062(2) -0.0024(14) 0.0132(16) -0.0011(13) C31 0.0205(18) 0.020(2) 0.029(2) -0.0026(14) 0.0033(15) 0.0040(15) N31 0.0244(16) 0.0236(17) 0.0252(17) -0.0008(13) 0.0012(13) 0.0017(13) C32 0.0171(18) 0.026(2) 0.030(2) 0.0006(15) 0.0021(15) -0.0086(15) N32 0.0223(15) 0.0160(15) 0.0350(18) -0.0015(13) 0.0024(13) 0.0014(12) _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 N32 2.032(3) 4_645 ? Ni1 N32 2.032(3) 1_545 ? Ni1 N31 2.040(3) . ? Ni1 N31 2.040(3) 4_655 ? Ni1 N23 2.198(3) . ? Ni1 N23 2.198(3) 4_655 ? Ni2 O1 2.038(3) 5_666 ? Ni2 O1 2.038(3) . ? Ni2 N21 2.072(3) 5_656 ? Ni2 N21 2.072(3) 1_565 ? Ni2 N22 2.125(3) . ? Ni2 N22 2.125(3) 5_666 ? O1 H1 0.81(4) . ? O1 H2 0.77(5) . ? N1 C2 1.347(4) . ? N1 C14 1.347(4) . ? C2 C3 1.422(5) . ? C2 C7 1.438(5) . ? C3 C4 1.350(5) . ? C3 H3A 0.9500 . ? C4 C5 1.411(5) . ? C4 H4A 0.9500 . ? C5 C6 1.353(5) . ? C5 H5A 0.9500 . ? C6 C7 1.418(5) . ? C6 H6A 0.9500 . ? C7 N8 1.349(4) . ? N8 C9 1.331(4) . ? C9 C10 1.425(5) . ? C9 C14 1.436(5) . ? C10 C11 1.359(5) . ? C10 H10A 0.9500 . ? C11 C12 1.419(5) . ? C11 H11A 0.9500 . ? C12 C13 1.341(5) . ? C12 H12A 0.9500 . ? C13 C14 1.424(5) . ? C13 H13A 0.9500 . ? N23 C21 1.318(4) . ? N23 C22 1.345(4) . ? C21 N21 1.157(4) . ? N21 Ni2 2.072(3) 1_545 ? C22 N22 1.148(4) . ? N33 C31 1.299(4) . ? N33 C32 1.320(4) . ? C31 N31 1.149(4) . ? C32 N32 1.151(4) . ? N32 Ni1 2.032(3) 1_565 ? 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 N32 Ni1 N32 86.17(15) 4_645 1_545 ? N32 Ni1 N31 179.14(11) 4_645 . ? N32 Ni1 N31 92.98(12) 1_545 . ? N32 Ni1 N31 92.98(12) 4_645 4_655 ? N32 Ni1 N31 179.14(11) 1_545 4_655 ? N31 Ni1 N31 87.88(15) . 4_655 ? N32 Ni1 N23 90.80(10) 4_645 . ? N32 Ni1 N23 90.51(10) 1_545 . ? N31 Ni1 N23 89.35(10) . . ? N31 Ni1 N23 89.36(10) 4_655 . ? N32 Ni1 N23 90.51(10) 4_645 4_655 ? N32 Ni1 N23 90.80(10) 1_545 4_655 ? N31 Ni1 N23 89.36(10) . 4_655 ? N31 Ni1 N23 89.35(10) 4_655 4_655 ? N23 Ni1 N23 178.21(12) . 4_655 ? O1 Ni2 O1 180.0 5_666 . ? O1 Ni2 N21 88.22(12) 5_666 5_656 ? O1 Ni2 N21 91.78(12) . 5_656 ? O1 Ni2 N21 91.78(12) 5_666 1_565 ? O1 Ni2 N21 88.22(12) . 1_565 ? N21 Ni2 N21 180.0 5_656 1_565 ? O1 Ni2 N22 87.35(11) 5_666 . ? O1 Ni2 N22 92.65(11) . . ? N21 Ni2 N22 86.15(11) 5_656 . ? N21 Ni2 N22 93.85(11) 1_565 . ? O1 Ni2 N22 92.65(11) 5_666 5_666 ? O1 Ni2 N22 87.35(11) . 5_666 ? N21 Ni2 N22 93.85(11) 5_656 5_666 ? N21 Ni2 N22 86.15(11) 1_565 5_666 ? N22 Ni2 N22 180.00(12) . 5_666 ? Ni2 O1 H1 120(3) . . ? Ni2 O1 H2 126(3) . . ? H1 O1 H2 103(5) . . ? C2 N1 C14 117.4(3) . . ? N1 C2 C3 119.6(3) . . ? N1 C2 C7 120.9(3) . . ? C3 C2 C7 119.5(3) . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C6 C5 C4 121.2(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? N8 C7 C6 120.1(3) . . ? N8 C7 C2 121.5(3) . . ? C6 C7 C2 118.4(3) . . ? C9 N8 C7 117.2(3) . . ? N8 C9 C10 119.6(3) . . ? N8 C9 C14 121.8(3) . . ? C10 C9 C14 118.6(3) . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? N1 C14 C13 119.8(3) . . ? N1 C14 C9 121.2(3) . . ? C13 C14 C9 119.0(3) . . ? C21 N23 C22 115.6(3) . . ? C21 N23 Ni1 121.5(2) . . ? C22 N23 Ni1 122.9(2) . . ? N21 C21 N23 176.0(4) . . ? C21 N21 Ni2 165.0(3) . 1_545 ? N22 C22 N23 176.9(4) . . ? C22 N22 Ni2 161.7(3) . . ? C31 N33 C32 119.3(3) . . ? N31 C31 N33 173.6(4) . . ? C31 N31 Ni1 158.9(3) . . ? N32 C32 N33 173.4(3) . . ? C32 N32 Ni1 159.9(3) . 1_565 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.551 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.097 #=END OF CIF