# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm #TrackingRef 'B920501B_ccdc_749380_749381_cif.txt' _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email JPLANG@SUDA.EDU.CN _publ_section_title ; Small Variations in Sodium Coordination Sphere Lead to the Remarkable Change from 2D to 3D of Two Nickel-Sodium Coordination Polymers ; loop_ _publ_author_name 'Jian-Ping Lang.' 'Xi Chen.' 'Dong Liu.' 'Shu-Lin Ma.' 'Shan-Bao Qiao.' ; Cheng Xu ; 'Yong Zhang.' # Attachment 'JPLangCIF.cif' data_[Ni(acac)2Na2(dca)2(m-DMF)2]n #TrackingRef 'B920501B_ccdc_749380_749381_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 749380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 N4 Na Ni0.50 O3' _chemical_formula_sum 'C10 H14 N4 Na Ni0.50 O3' _chemical_formula_weight 290.60 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' Na Na 0.0362 0.0249 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9185(19) _cell_length_b 9.3721(17) _cell_length_c 9.958(2) _cell_angle_alpha 66.366(11) _cell_angle_beta 89.136(18) _cell_angle_gamma 87.928(17) _cell_volume 676.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8254 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6631 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.34 _reflns_number_total 2455 _reflns_number_gt 2013 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0627P)^2^+0.0000P] 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 2455 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.004 _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 0.0000 0.5000 0.0267(2) Uani 1 2 d S . . Na1 Na 0.52418(15) 0.37317(13) 0.40785(12) 0.0337(3) Uani 1 1 d . . . O1 O 0.6921(3) 0.1480(2) 0.4404(2) 0.0314(5) Uani 1 1 d . . . O2 O 0.6313(2) -0.1584(2) 0.4452(2) 0.0314(5) Uani 1 1 d . . . O3 O 0.3516(3) 0.5951(2) 0.3904(2) 0.0392(6) Uani 1 1 d . . . N1 N 0.4044(3) 0.1136(3) 0.2865(3) 0.0362(6) Uani 1 1 d . . . N2 N 0.2732(4) 0.2680(4) 0.0491(3) 0.0538(9) Uani 1 1 d . . . N3 N 0.3926(4) 0.4812(3) -0.1620(3) 0.0478(8) Uani 1 1 d . . . N4 N 0.2551(3) 0.7376(3) 0.1601(3) 0.0368(7) Uani 1 1 d . . . C1 C 0.9423(4) 0.2646(4) 0.3213(4) 0.0391(8) Uani 1 1 d . . . H1A H 0.9130 0.3353 0.2207 0.059 Uiso 1 1 calc R . . H1B H 1.0586 0.2241 0.3239 0.059 Uiso 1 1 calc R . . H1C H 0.9326 0.3211 0.3854 0.059 Uiso 1 1 calc R . . C2 C 0.8240(4) 0.1317(3) 0.3734(3) 0.0304(7) Uani 1 1 d . . . C3 C 0.8660(4) 0.0002(4) 0.3442(3) 0.0339(7) Uani 1 1 d . . . H3 H 0.9698 0.0026 0.2944 0.041 Uiso 1 1 calc R . . C4 C 0.7735(4) -0.1327(4) 0.3798(3) 0.0306(7) Uani 1 1 d . . . C5 C 0.8423(4) -0.2612(4) 0.3376(4) 0.0468(9) Uani 1 1 d . . . H5A H 0.8413 -0.3607 0.4234 0.070 Uiso 1 1 calc R . . H5B H 0.9584 -0.2391 0.3018 0.070 Uiso 1 1 calc R . . H5C H 0.7718 -0.2675 0.2602 0.070 Uiso 1 1 calc R . . C6 C 0.3512(4) 0.1910(4) 0.1728(4) 0.0338(7) Uani 1 1 d . . . C7 C 0.3451(4) 0.3798(4) -0.0593(4) 0.0354(8) Uani 1 1 d . . . C8 C 0.1847(5) 0.6065(5) 0.1405(5) 0.0560(10) Uani 1 1 d . . . H8A H 0.1848 0.5160 0.2346 0.084 Uiso 1 1 calc R . . H8B H 0.2532 0.5816 0.0695 0.084 Uiso 1 1 calc R . . H8C H 0.0686 0.6334 0.1042 0.084 Uiso 1 1 calc R . . C9 C 0.2492(6) 0.8871(5) 0.0350(4) 0.0666(12) Uani 1 1 d . . . H9A H 0.2956 0.9667 0.0631 0.100 Uiso 1 1 calc R . . H9B H 0.1317 0.9160 0.0032 0.100 Uiso 1 1 calc R . . H9C H 0.3161 0.8793 -0.0455 0.100 Uiso 1 1 calc R . . C10 C 0.3330(4) 0.7193(4) 0.2817(4) 0.0365(8) Uani 1 1 d . . . H10 H 0.3790 0.8093 0.2866 0.044 Uiso 1 1 calc 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 0.0314(3) 0.0211(3) 0.0254(3) -0.0069(2) 0.0048(2) -0.0036(2) Na1 0.0492(7) 0.0233(6) 0.0259(7) -0.0071(5) 0.0030(5) -0.0015(5) O1 0.0340(11) 0.0242(11) 0.0337(12) -0.0092(10) 0.0068(9) -0.0052(9) O2 0.0352(11) 0.0251(11) 0.0340(12) -0.0119(10) 0.0074(10) -0.0027(9) O3 0.0540(14) 0.0300(12) 0.0327(13) -0.0120(11) -0.0012(11) 0.0018(11) N1 0.0409(15) 0.0306(15) 0.0301(16) -0.0049(13) 0.0015(13) -0.0028(12) N2 0.0573(19) 0.0526(19) 0.0346(17) 0.0017(16) -0.0086(15) -0.0161(16) N3 0.063(2) 0.0438(18) 0.0271(16) -0.0046(15) 0.0010(14) 0.0041(15) N4 0.0426(15) 0.0360(15) 0.0338(15) -0.0164(13) -0.0024(13) 0.0028(12) C1 0.0364(17) 0.0337(18) 0.0410(19) -0.0081(16) 0.0045(15) -0.0070(14) C2 0.0330(16) 0.0275(16) 0.0251(16) -0.0043(13) -0.0001(13) -0.0061(13) C3 0.0296(16) 0.0393(18) 0.0343(18) -0.0162(16) 0.0076(13) -0.0053(14) C4 0.0306(16) 0.0358(17) 0.0260(16) -0.0134(14) 0.0020(13) 0.0027(13) C5 0.044(2) 0.050(2) 0.059(2) -0.036(2) 0.0110(17) -0.0043(17) C6 0.0371(17) 0.0312(17) 0.0317(19) -0.0108(16) 0.0041(15) -0.0060(14) C7 0.0434(19) 0.0350(18) 0.0271(18) -0.0121(16) -0.0046(15) 0.0041(15) C8 0.055(2) 0.061(3) 0.064(3) -0.038(2) -0.008(2) -0.009(2) C9 0.089(3) 0.054(3) 0.044(2) -0.006(2) -0.013(2) 0.010(2) C10 0.0454(19) 0.0320(18) 0.0348(19) -0.0164(16) 0.0001(15) 0.0006(15) _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 2.014(2) . ? Ni1 O1 2.014(2) 2_656 ? Ni1 O2 2.0262(19) 2_656 ? Ni1 O2 2.0262(19) . ? Ni1 N1 2.098(3) . ? Ni1 N1 2.098(3) 2_656 ? Ni1 Na1 3.2528(13) . ? Ni1 Na1 3.2528(13) 2_656 ? Na1 O2 2.339(2) 2_656 ? Na1 O1 2.364(2) . ? Na1 N3 2.372(3) 2_665 ? Na1 O3 2.377(3) 2_666 ? Na1 O3 2.395(2) . ? Na1 C10 3.078(4) 2_666 ? Na1 Na1 3.546(2) 2_666 ? O1 C2 1.268(4) . ? O2 C4 1.273(4) . ? O2 Na1 2.339(2) 2_656 ? O3 C10 1.237(4) . ? O3 Na1 2.377(3) 2_666 ? N1 C6 1.149(4) . ? N2 C6 1.302(4) . ? N2 C7 1.306(4) . ? N3 C7 1.152(4) . ? N3 Na1 2.372(3) 2_665 ? N4 C10 1.314(4) . ? N4 C8 1.450(4) . ? N4 C9 1.454(5) . ? C1 C2 1.500(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.403(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.509(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Na1 3.078(4) 2_666 ? C10 H10 0.9500 . ? 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 180.00(10) . 2_656 ? O1 Ni1 O2 87.81(8) . 2_656 ? O1 Ni1 O2 92.19(8) 2_656 2_656 ? O1 Ni1 O2 92.19(8) . . ? O1 Ni1 O2 87.81(8) 2_656 . ? O2 Ni1 O2 180.0 2_656 . ? O1 Ni1 N1 88.25(9) . . ? O1 Ni1 N1 91.75(9) 2_656 . ? O2 Ni1 N1 88.37(9) 2_656 . ? O2 Ni1 N1 91.63(9) . . ? O1 Ni1 N1 91.75(9) . 2_656 ? O1 Ni1 N1 88.25(9) 2_656 2_656 ? O2 Ni1 N1 91.63(9) 2_656 2_656 ? O2 Ni1 N1 88.37(9) . 2_656 ? N1 Ni1 N1 180.00(9) . 2_656 ? O1 Ni1 Na1 46.32(6) . . ? O1 Ni1 Na1 133.68(6) 2_656 . ? O2 Ni1 Na1 45.65(6) 2_656 . ? O2 Ni1 Na1 134.35(6) . . ? N1 Ni1 Na1 72.32(8) . . ? N1 Ni1 Na1 107.68(8) 2_656 . ? O1 Ni1 Na1 133.68(6) . 2_656 ? O1 Ni1 Na1 46.32(6) 2_656 2_656 ? O2 Ni1 Na1 134.35(6) 2_656 2_656 ? O2 Ni1 Na1 45.65(6) . 2_656 ? N1 Ni1 Na1 107.68(8) . 2_656 ? N1 Ni1 Na1 72.32(8) 2_656 2_656 ? Na1 Ni1 Na1 180.0 . 2_656 ? O2 Na1 O1 73.12(8) 2_656 . ? O2 Na1 N3 142.69(11) 2_656 2_665 ? O1 Na1 N3 95.95(10) . 2_665 ? O2 Na1 O3 94.30(9) 2_656 2_666 ? O1 Na1 O3 93.51(8) . 2_666 ? N3 Na1 O3 122.35(11) 2_665 2_666 ? O2 Na1 O3 104.65(9) 2_656 . ? O1 Na1 O3 176.56(9) . . ? N3 Na1 O3 87.39(10) 2_665 . ? O3 Na1 O3 83.99(9) 2_666 . ? O2 Na1 C10 75.55(9) 2_656 2_666 ? O1 Na1 C10 77.71(8) . 2_666 ? N3 Na1 C10 138.16(11) 2_665 2_666 ? O3 Na1 C10 21.73(8) 2_666 2_666 ? O3 Na1 C10 99.25(9) . 2_666 ? O2 Na1 Ni1 38.27(5) 2_656 . ? O1 Na1 Ni1 38.03(5) . . ? N3 Na1 Ni1 115.23(9) 2_665 . ? O3 Na1 Ni1 106.61(6) 2_666 . ? O3 Na1 Ni1 140.65(8) . . ? C10 Na1 Ni1 85.02(7) 2_666 . ? O2 Na1 Na1 102.77(7) 2_656 2_666 ? O1 Na1 Na1 135.65(8) . 2_666 ? N3 Na1 Na1 109.14(9) 2_665 2_666 ? O3 Na1 Na1 42.19(6) 2_666 2_666 ? O3 Na1 Na1 41.80(6) . 2_666 ? C10 Na1 Na1 59.07(7) 2_666 2_666 ? Ni1 Na1 Na1 135.54(5) . 2_666 ? C2 O1 Ni1 124.8(2) . . ? C2 O1 Na1 130.43(19) . . ? Ni1 O1 Na1 95.65(8) . . ? C4 O2 Ni1 123.71(19) . . ? C4 O2 Na1 138.02(19) . 2_656 ? Ni1 O2 Na1 96.08(8) . 2_656 ? C10 O3 Na1 112.9(2) . 2_666 ? C10 O3 Na1 126.9(2) . . ? Na1 O3 Na1 96.01(9) 2_666 . ? C6 N1 Ni1 172.1(3) . . ? C6 N2 C7 121.8(3) . . ? C7 N3 Na1 160.4(3) . 2_665 ? C10 N4 C8 121.3(3) . . ? C10 N4 C9 121.3(3) . . ? C8 N4 C9 117.2(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.0(3) . . ? O1 C2 C1 116.8(3) . . ? C3 C2 C1 118.2(3) . . ? C4 C3 C2 127.4(3) . . ? C4 C3 H3 116.3 . . ? C2 C3 H3 116.3 . . ? O2 C4 C3 126.2(3) . . ? O2 C4 C5 115.0(3) . . ? C3 C4 C5 118.8(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 N2 172.5(3) . . ? N3 C7 N2 172.9(4) . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 N4 125.7(3) . . ? O3 C10 Na1 45.34(16) . 2_666 ? N4 C10 Na1 169.9(3) . 2_666 ? O3 C10 H10 117.2 . . ? N4 C10 H10 117.2 . . ? Na1 C10 H10 72.0 2_666 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.460 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.068 #===END data_[Ni(acac)2Na(dca)(MeCN)]n #TrackingRef 'B920501B_ccdc_749380_749381_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 749381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N4 Na Ni O4' _chemical_formula_sum 'C14 H17 N4 Na Ni O4' _chemical_formula_weight 387.02 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.330(4) _cell_length_b 10.9143(15) _cell_length_c 17.122(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.890(4) _cell_angle_gamma 90.00 _cell_volume 3721.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6153 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour light-blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7502 _exptl_absorpt_correction_T_max 0.8625 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18103 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3395 _reflns_number_gt 2895 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0344P)^2^+7.5888P] 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 3395 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.0000 0.0000 0.02920(16) Uani 1 2 d S . . Ni2 Ni 0.7500 -0.2500 0.5000 0.02674(16) Uani 1 2 d S . . Na1 Na 0.64389(6) 0.11487(12) 0.05295(8) 0.0385(3) Uani 1 1 d . . . O1 O 0.54435(11) 0.1586(2) 0.05914(13) 0.0360(5) Uani 1 1 d . . . O2 O 0.43940(11) 0.0016(2) 0.05884(14) 0.0388(5) Uani 1 1 d . . . O3 O 0.75875(11) -0.42519(19) 0.46596(13) 0.0328(5) Uani 1 1 d . . . O4 O 0.65344(11) -0.2797(2) 0.47329(14) 0.0377(5) Uani 1 1 d . . . N1 N 0.57260(15) -0.0968(3) 0.10236(18) 0.0461(7) Uani 1 1 d . . . N2 N 0.6503(2) -0.2353(3) 0.2122(2) 0.0780(13) Uani 1 1 d . . . N3 N 0.71776(14) -0.2056(2) 0.36920(17) 0.0381(7) Uani 1 1 d . . . N4 N 0.70790(17) 0.0929(4) 0.2138(2) 0.0613(10) Uani 1 1 d . . . C1 C 0.5674(2) 0.3375(4) 0.1440(3) 0.0647(12) Uani 1 1 d . . . H1A H 0.6153 0.3173 0.1746 0.097 Uiso 1 1 calc R . . H1B H 0.5537 0.3761 0.1850 0.097 Uiso 1 1 calc R . . H1C H 0.5593 0.3942 0.0958 0.097 Uiso 1 1 calc R . . C2 C 0.52721(17) 0.2218(3) 0.1078(2) 0.0389(8) Uani 1 1 d . . . C3 C 0.47677(18) 0.1912(3) 0.1311(2) 0.0455(9) Uani 1 1 d . . . H3 H 0.4678 0.2493 0.1657 0.055 Uiso 1 1 calc R . . C4 C 0.43796(17) 0.0845(4) 0.1090(2) 0.0420(8) Uani 1 1 d . . . C5 C 0.3915(2) 0.0630(4) 0.1499(3) 0.0667(13) Uani 1 1 d . . . H5A H 0.3489 0.0291 0.1060 0.100 Uiso 1 1 calc R . . H5B H 0.3830 0.1409 0.1717 0.100 Uiso 1 1 calc R . . H5C H 0.4124 0.0052 0.1987 0.100 Uiso 1 1 calc R . . C6 C 0.7250(2) -0.6145(3) 0.3922(3) 0.0588(11) Uani 1 1 d . . . H6A H 0.7355 -0.6010 0.3432 0.088 Uiso 1 1 calc R . . H6B H 0.6862 -0.6694 0.3736 0.088 Uiso 1 1 calc R . . H6C H 0.7638 -0.6517 0.4412 0.088 Uiso 1 1 calc R . . C7 C 0.70863(18) -0.4931(3) 0.4209(2) 0.0371(8) Uani 1 1 d . . . C8 C 0.64181(18) -0.4661(3) 0.3976(2) 0.0426(8) Uani 1 1 d . . . H8 H 0.6094 -0.5233 0.3605 0.051 Uiso 1 1 calc R . . C9 C 0.61727(17) -0.3636(3) 0.4230(2) 0.0407(8) Uani 1 1 d . . . C10 C 0.54274(19) -0.3472(5) 0.3896(3) 0.0670(13) Uani 1 1 d . . . H10A H 0.5325 -0.3390 0.4393 0.101 Uiso 1 1 calc R . . H10B H 0.5192 -0.4187 0.3545 0.101 Uiso 1 1 calc R . . H10C H 0.5281 -0.2733 0.3533 0.101 Uiso 1 1 calc R . . C11 C 0.60941(18) -0.1564(3) 0.1576(2) 0.0411(8) Uani 1 1 d . . . C12 C 0.68449(18) -0.2132(3) 0.2952(2) 0.0387(8) Uani 1 1 d . . . C13 C 0.7931(2) 0.0629(4) 0.3763(2) 0.0546(10) Uani 1 1 d . . . H13A H 0.7829 0.1203 0.4127 0.082 Uiso 1 1 calc R . . H13B H 0.8386 0.0784 0.3838 0.082 Uiso 1 1 calc R . . H13C H 0.7901 -0.0213 0.3941 0.082 Uiso 1 1 calc R . . C14 C 0.74506(19) 0.0800(3) 0.2847(2) 0.0457(9) 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 0.0243(3) 0.0382(3) 0.0217(3) 0.0011(2) 0.0074(2) -0.0013(2) Ni2 0.0263(3) 0.0321(3) 0.0198(3) 0.0006(2) 0.0086(2) 0.0025(2) Na1 0.0314(7) 0.0515(8) 0.0314(7) 0.0013(6) 0.0132(6) -0.0069(6) O1 0.0321(12) 0.0434(13) 0.0310(12) -0.0016(10) 0.0130(10) -0.0046(10) O2 0.0346(13) 0.0516(14) 0.0348(12) -0.0078(11) 0.0200(11) -0.0077(11) O3 0.0334(12) 0.0350(12) 0.0280(11) 0.0010(9) 0.0120(10) 0.0043(10) O4 0.0294(12) 0.0485(14) 0.0330(12) -0.0091(10) 0.0122(10) -0.0022(10) N1 0.0433(18) 0.0528(18) 0.0294(16) 0.0029(14) 0.0051(14) 0.0030(15) N2 0.106(3) 0.063(2) 0.0249(17) -0.0028(15) -0.0050(18) 0.047(2) N3 0.0476(18) 0.0404(16) 0.0241(15) 0.0042(12) 0.0143(13) 0.0049(13) N4 0.050(2) 0.091(3) 0.0377(19) 0.0057(18) 0.0158(17) -0.0211(19) C1 0.081(3) 0.053(2) 0.066(3) -0.019(2) 0.038(2) -0.020(2) C2 0.039(2) 0.0429(19) 0.0295(18) -0.0002(15) 0.0110(16) -0.0002(15) C3 0.049(2) 0.051(2) 0.044(2) -0.0156(17) 0.0273(18) -0.0049(18) C4 0.0344(19) 0.063(2) 0.0297(17) -0.0075(17) 0.0156(15) -0.0040(17) C5 0.057(3) 0.097(3) 0.062(3) -0.030(3) 0.040(2) -0.027(2) C6 0.073(3) 0.039(2) 0.059(3) -0.0130(18) 0.025(2) 0.0020(19) C7 0.049(2) 0.0348(18) 0.0278(17) -0.0021(14) 0.0171(16) -0.0013(16) C8 0.041(2) 0.045(2) 0.0374(19) -0.0111(16) 0.0145(16) -0.0110(16) C9 0.0331(19) 0.055(2) 0.0307(18) -0.0040(16) 0.0117(15) -0.0046(16) C10 0.035(2) 0.095(3) 0.064(3) -0.032(3) 0.017(2) -0.010(2) C11 0.044(2) 0.049(2) 0.0243(17) -0.0064(16) 0.0102(16) 0.0047(17) C12 0.049(2) 0.0361(18) 0.029(2) 0.0037(14) 0.0162(17) 0.0120(15) C13 0.061(3) 0.057(2) 0.038(2) 0.0071(18) 0.0157(19) -0.002(2) C14 0.045(2) 0.056(2) 0.042(2) 0.0010(18) 0.0255(19) -0.0097(18) _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 O2 2.020(2) . ? Ni1 O2 2.020(2) 5_655 ? Ni1 O1 2.024(2) . ? Ni1 O1 2.024(2) 5_655 ? Ni1 N1 2.061(3) 5_655 ? Ni1 N1 2.061(3) . ? Ni1 Na1 3.1753(13) 5_655 ? Ni1 Na1 3.1753(13) . ? Ni2 O4 2.018(2) . ? Ni2 O4 2.018(2) 7_646 ? Ni2 O3 2.034(2) 7_646 ? Ni2 O3 2.034(2) . ? Ni2 N3 2.076(3) 7_646 ? Ni2 N3 2.076(3) . ? Ni2 Na1 3.2487(13) 6_556 ? Ni2 Na1 3.2487(13) 4_645 ? Na1 O1 2.322(3) . ? Na1 O4 2.325(3) 6 ? Na1 O2 2.349(3) 5_655 ? Na1 O3 2.379(3) 4_655 ? Na1 N4 2.475(3) . ? Na1 Ni2 3.2487(12) 4_655 ? O1 C2 1.266(4) . ? O2 C4 1.257(4) . ? O2 Na1 2.349(3) 5_655 ? O3 C7 1.271(4) . ? O3 Na1 2.379(3) 4_645 ? O4 C9 1.266(4) . ? O4 Na1 2.325(3) 6_556 ? N1 C11 1.135(4) . ? N2 C12 1.296(4) . ? N2 C11 1.295(5) . ? N3 C12 1.146(4) . ? N4 C14 1.127(4) . ? C1 C2 1.510(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.395(5) . ? C3 C4 1.398(5) . ? C3 H3 0.9500 . ? C4 C5 1.511(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.515(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.391(5) . ? C8 C9 1.399(5) . ? C8 H8 0.9500 . ? C9 C10 1.506(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C13 C14 1.457(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 Ni1 O2 180.00(15) . 5_655 ? O2 Ni1 O1 91.69(9) . . ? O2 Ni1 O1 88.31(9) 5_655 . ? O2 Ni1 O1 88.31(9) . 5_655 ? O2 Ni1 O1 91.69(9) 5_655 5_655 ? O1 Ni1 O1 180.0(2) . 5_655 ? O2 Ni1 N1 88.44(11) . 5_655 ? O2 Ni1 N1 91.56(11) 5_655 5_655 ? O1 Ni1 N1 90.31(10) . 5_655 ? O1 Ni1 N1 89.69(10) 5_655 5_655 ? O2 Ni1 N1 91.56(11) . . ? O2 Ni1 N1 88.44(11) 5_655 . ? O1 Ni1 N1 89.69(10) . . ? O1 Ni1 N1 90.31(10) 5_655 . ? N1 Ni1 N1 180.0(3) 5_655 . ? O2 Ni1 Na1 47.64(7) . 5_655 ? O2 Ni1 Na1 132.36(7) 5_655 5_655 ? O1 Ni1 Na1 133.12(7) . 5_655 ? O1 Ni1 Na1 46.88(7) 5_655 5_655 ? N1 Ni1 Na1 69.78(9) 5_655 5_655 ? N1 Ni1 Na1 110.22(9) . 5_655 ? O2 Ni1 Na1 132.36(7) . . ? O2 Ni1 Na1 47.64(7) 5_655 . ? O1 Ni1 Na1 46.88(7) . . ? O1 Ni1 Na1 133.12(7) 5_655 . ? N1 Ni1 Na1 110.22(9) 5_655 . ? N1 Ni1 Na1 69.78(9) . . ? Na1 Ni1 Na1 180.00(6) 5_655 . ? O4 Ni2 O4 180.0 . 7_646 ? O4 Ni2 O3 89.13(9) . 7_646 ? O4 Ni2 O3 90.87(9) 7_646 7_646 ? O4 Ni2 O3 90.87(9) . . ? O4 Ni2 O3 89.13(9) 7_646 . ? O3 Ni2 O3 180.000(1) 7_646 . ? O4 Ni2 N3 91.18(10) . 7_646 ? O4 Ni2 N3 88.82(10) 7_646 7_646 ? O3 Ni2 N3 86.66(9) 7_646 7_646 ? O3 Ni2 N3 93.34(9) . 7_646 ? O4 Ni2 N3 88.82(10) . . ? O4 Ni2 N3 91.18(10) 7_646 . ? O3 Ni2 N3 93.34(9) 7_646 . ? O3 Ni2 N3 86.66(9) . . ? N3 Ni2 N3 180.00(6) 7_646 . ? O4 Ni2 Na1 45.32(7) . 6_556 ? O4 Ni2 Na1 134.68(7) 7_646 6_556 ? O3 Ni2 Na1 46.89(6) 7_646 6_556 ? O3 Ni2 Na1 133.11(6) . 6_556 ? N3 Ni2 Na1 75.27(8) 7_646 6_556 ? N3 Ni2 Na1 104.73(8) . 6_556 ? O4 Ni2 Na1 134.68(7) . 4_645 ? O4 Ni2 Na1 45.32(7) 7_646 4_645 ? O3 Ni2 Na1 133.11(6) 7_646 4_645 ? O3 Ni2 Na1 46.89(6) . 4_645 ? N3 Ni2 Na1 104.73(8) 7_646 4_645 ? N3 Ni2 Na1 75.27(8) . 4_645 ? Na1 Ni2 Na1 180.00(4) 6_556 4_645 ? O1 Na1 O4 102.19(9) . 6 ? O1 Na1 O2 74.16(8) . 5_655 ? O4 Na1 O2 100.94(9) 6 5_655 ? O1 Na1 O3 175.21(9) . 4_655 ? O4 Na1 O3 74.36(8) 6 4_655 ? O2 Na1 O3 103.01(9) 5_655 4_655 ? O1 Na1 N4 92.98(10) . . ? O4 Na1 N4 124.59(11) 6 . ? O2 Na1 N4 134.44(11) 5_655 . ? O3 Na1 N4 91.74(10) 4_655 . ? O1 Na1 Ni1 39.51(6) . . ? O4 Na1 Ni1 119.18(7) 6 . ? O2 Na1 Ni1 39.44(5) 5_655 . ? O3 Na1 Ni1 139.25(7) 4_655 . ? N4 Na1 Ni1 106.26(8) . . ? O1 Na1 Ni2 138.87(8) . 4_655 ? O4 Na1 Ni2 38.10(6) 6 4_655 ? O2 Na1 Ni2 115.27(7) 5_655 4_655 ? O3 Na1 Ni2 38.62(5) 4_655 4_655 ? N4 Na1 Ni2 103.16(8) . 4_655 ? Ni1 Na1 Ni2 150.59(4) . 4_655 ? C2 O1 Ni1 124.7(2) . . ? C2 O1 Na1 136.2(2) . . ? Ni1 O1 Na1 93.61(9) . . ? C4 O2 Ni1 125.2(2) . . ? C4 O2 Na1 133.6(2) . 5_655 ? Ni1 O2 Na1 92.92(9) . 5_655 ? C7 O3 Ni2 123.3(2) . . ? C7 O3 Na1 129.3(2) . 4_645 ? Ni2 O3 Na1 94.49(9) . 4_645 ? C9 O4 Ni2 123.9(2) . . ? C9 O4 Na1 139.4(2) . 6_556 ? Ni2 O4 Na1 96.59(9) . 6_556 ? C11 N1 Ni1 175.3(3) . . ? C12 N2 C11 122.8(3) . . ? C12 N3 Ni2 155.7(3) . . ? C14 N4 Na1 169.6(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.5(3) . . ? O1 C2 C1 115.1(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 127.1(3) . . ? C2 C3 H3 116.4 . . ? C4 C3 H3 116.4 . . ? O2 C4 C3 125.4(3) . . ? O2 C4 C5 116.1(3) . . ? C3 C4 C5 118.4(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 125.9(3) . . ? O3 C7 C6 115.6(3) . . ? C8 C7 C6 118.5(3) . . ? C7 C8 C9 126.9(3) . . ? C7 C8 H8 116.5 . . ? C9 C8 H8 116.5 . . ? O4 C9 C8 124.8(3) . . ? O4 C9 C10 115.3(3) . . ? C8 C9 C10 119.9(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 N2 172.0(4) . . ? N3 C12 N2 172.8(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C13 179.9(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.008 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.065 #===END