# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gotzone.barandika@ehu.es _publ_contact_author_name 'Gotzone Barandika' loop_ _publ_author_name A.Calderon-Casado G.Barandika B.Bazan M.Urtiaga O.Vallcorba.J.Rius C.Miravittles M.Arriortua #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-07-26 at 12:56:32 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : h-nipb-p21c ac16iv_100kabs data_[ni2(4,4-bipy)1.5(2,5-PDC)2(H2O)2]3.5H2O _database_code_depnum_ccdc_archive 'CCDC 825600' #TrackingRef '- NiPB55.cif' _audit_creation_date 2010-07-26T12:56:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C29 H18 N5 Ni2 O10),6(O0.50), 2(O0.50),2(O0.50)' _chemical_formula_sum 'C58 H36 N10 Ni4 O27' _chemical_formula_weight 1539.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.6280(16) _cell_length_b 11.6031(11) _cell_length_c 22.004(3) _cell_angle_alpha 90 _cell_angle_beta 116.141(9) _cell_angle_gamma 90 _cell_volume 3352.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1482 _cell_measurement_theta_min 2.6225 _cell_measurement_theta_max 28.9699 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.1337 _exptl_crystal_size_mid 0.0615 _exptl_crystal_size_min 0.0321 _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 -0.0416381487 _diffrn_orient_matrix_ub_12 0.0259668046 _diffrn_orient_matrix_ub_13 0.0049848225 _diffrn_orient_matrix_ub_21 -0.0114686578 _diffrn_orient_matrix_ub_22 -0.051726881 _diffrn_orient_matrix_ub_23 0.0146535631 _diffrn_orient_matrix_ub_31 0.02503812 _diffrn_orient_matrix_ub_32 0.0195365085 _diffrn_orient_matrix_ub_33 0.0324202271 _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire2 (l' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.1321 _diffrn_reflns_av_unetI/netI 0.2954 _diffrn_reflns_number 11305 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4624 _reflns_number_gt 1934 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution DIRDIF2008 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0200P)^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_number_reflns 4624 _refine_ls_number_parameters 201 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1572 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.744 _refine_ls_restrained_S_all 0.743 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.656 _refine_diff_density_min -0.75 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C -0.1899(6) -0.3588(6) -0.0706(4) 0.0160(6) Uani 1 1 d . . . H1 H -0.1273 -0.3708 -0.073 0.019 Uiso 1 1 calc R . . C2 C -0.1894(6) -0.3514(6) -0.0079(4) 0.0160(6) Uani 1 1 d . . . H2 H -0.1275 -0.3611 0.0319 0.019 Uiso 1 1 calc R . . C3 C -0.2794(5) -0.3297(6) -0.0028(4) 0.0160(6) Uani 1 1 d . . . C4 C -0.3695(5) -0.3261(6) -0.0624(3) 0.0160(6) Uani 1 1 d . . . H4 H -0.4327 -0.3162 -0.0605 0.019 Uiso 1 1 calc R . . C5 C -0.3674(6) -0.3369(6) -0.1240(4) 0.0160(6) Uani 1 1 d . . . H5 H -0.4299 -0.3356 -0.164 0.019 Uiso 1 1 calc R . . C6 C -0.1962(6) -0.2460(6) 0.1796(4) 0.0160(6) Uani 1 1 d . . . H6 H -0.1348 -0.2236 0.2171 0.019 Uiso 1 1 calc R . . C7 C -0.1924(6) -0.2767(6) 0.1193(3) 0.0160(6) Uani 1 1 d . . . H7 H -0.1293 -0.276 0.1167 0.019 Uiso 1 1 calc R . . C8 C -0.2810(5) -0.3084(6) 0.0633(3) 0.0160(6) Uani 1 1 d . . . C9 C -0.3702(5) -0.3107(6) 0.0711(4) 0.0160(6) Uani 1 1 d . . . H9 H -0.4329 -0.3323 0.0344 0.019 Uiso 1 1 calc R . . C10 C -0.3663(5) -0.2810(6) 0.1334(3) 0.0160(6) Uani 1 1 d . . . H10 H -0.4276 -0.2854 0.1382 0.019 Uiso 1 1 calc R . . C11 C -0.2556(5) -0.0722(6) -0.1762(3) 0.0147(5) Uani 1 1 d . . . C12 C -0.2746(5) 0.0373(6) -0.1598(3) 0.0147(5) Uani 1 1 d . . . H12 H -0.2203 0.089 -0.1355 0.018 Uiso 1 1 calc R . . C13 C -0.3749(5) 0.0696(6) -0.1798(3) 0.0147(5) Uani 1 1 d . . . H13 H -0.3905 0.1452 -0.1706 0.018 Uiso 1 1 calc R . . C14 C -0.4512(5) -0.0077(6) -0.2127(3) 0.0147(5) Uani 1 1 d . . . C15 C -0.4263(6) -0.1149(6) -0.2292(4) 0.0147(5) Uani 1 1 d . . . H15 H -0.4794 -0.1669 -0.255 0.018 Uiso 1 1 calc R . . C16 C -0.5625(5) 0.0208(7) -0.2323(3) 0.0147(5) Uani 1 1 d . . . C17 C -0.1494(6) -0.1174(6) -0.1540(4) 0.0147(5) Uani 1 1 d . . . C18 C 0.2752(5) -0.0183(6) -0.1029(4) 0.0203(9) Uani 1 1 d . . . H18 H 0.2339 -0.0279 -0.1501 0.024 Uiso 1 1 calc R . . C19 C 0.3795(5) -0.0158(6) -0.0801(4) 0.0203(9) Uani 1 1 d . . . H19 H 0.4074 -0.0237 -0.1116 0.024 Uiso 1 1 calc R . . C20 C 0.4428(5) -0.0023(6) -0.0135(4) 0.0203(9) Uani 1 1 d . . . C21 C 0.3957(5) 0.0112(6) 0.0280(4) 0.0203(9) Uani 1 1 d . . . H21 H 0.4358 0.0221 0.0752 0.024 Uiso 1 1 calc R . . C22 C 0.2913(5) 0.0091(6) 0.0020(3) 0.0203(9) Uani 1 1 d . . . H22 H 0.2622 0.0205 0.0326 0.024 Uiso 1 1 calc R . . C23 C 0.0262(6) -0.3715(7) -0.2883(4) 0.0196(5) Uani 1 1 d . . . C24 C 0.0678(5) -0.2285(7) -0.1943(4) 0.0196(5) Uani 1 1 d . . . H24 H 0.0646 -0.1702 -0.2255 0.024 Uiso 1 1 calc R . . C25 C 0.0567(5) -0.3449(7) -0.2156(4) 0.0196(5) Uani 1 1 d . . . C26 C 0.0942(5) -0.2814(7) -0.0868(4) 0.0196(5) Uani 1 1 d . . . C27 C 0.0657(5) -0.4274(7) -0.1689(3) 0.0196(5) Uani 1 1 d . . . H27 H 0.0562 -0.5062 -0.1819 0.024 Uiso 1 1 calc R . . C28 C 0.0883(5) -0.3979(7) -0.1034(4) 0.0196(5) Uani 1 1 d . . . H28 H 0.0995 -0.4555 -0.0702 0.024 Uiso 1 1 calc R . . C29 C 0.1129(6) -0.2404(7) -0.0177(4) 0.0196(5) Uani 1 1 d . . . N1 N -0.2779(4) -0.3495(5) -0.1296(3) 0.0160(6) Uani 1 1 d . . . N2 N -0.2821(5) -0.2467(5) 0.1870(3) 0.0160(6) Uani 1 1 d . . . N3 N -0.3307(4) -0.1465(5) -0.2100(3) 0.0147(5) Uani 1 1 d . . . N4 N 0.2286(4) -0.0079(5) -0.0626(3) 0.0203(9) Uani 1 1 d . . . N5 N 0.0826(4) -0.1970(5) -0.1327(3) 0.0196(5) Uani 1 1 d . . . O1 O -0.1408(3) -0.2207(4) -0.1704(2) 0.0147(5) Uani 1 1 d . . . O2 O -0.0779(3) -0.0513(4) -0.1197(2) 0.0147(5) Uani 1 1 d . . . O1W O 0.3416(4) -0.1562(5) -0.3807(3) 0.0431(17) Uiso 1 1 d . . . O3 O -0.6241(3) -0.0624(4) -0.2499(2) 0.0147(5) Uani 1 1 d . . . O2W O 0.0707(4) -0.4017(4) 0.1213(2) 0.0234(14) Uiso 1 1 d . . . O4 O -0.5823(3) 0.1239(4) -0.2270(2) 0.0147(5) Uani 1 1 d . . . O4W O 0.4232(9) -0.0761(12) -0.4640(6) 0.070(4) Uiso 0.5 1 d P . . O5 O 0.0544(3) 0.1139(4) -0.0489(2) 0.0152(9) Uani 1 1 d U . . O3W O -0.2857(9) -0.7652(11) -0.2890(6) 0.072(4) Uiso 0.5 1 d P . . O6 O -0.2038(3) -0.4593(4) -0.2253(2) 0.0152(9) Uani 1 1 d U . . O5W O 0.4075(10) -0.0909(12) -0.5938(7) 0.085(5) Uiso 0.5 1 d P . . O7 O 0.1035(4) -0.1336(4) -0.0098(2) 0.0196(5) Uani 1 1 d . . . O8 O 0.1305(3) -0.3148(4) 0.0275(2) 0.0196(5) Uani 1 1 d . . . O9 O -0.0284(3) -0.4620(4) -0.3119(2) 0.0196(5) Uani 1 1 d . . . O10 O 0.0484(3) -0.3046(4) -0.3240(2) 0.0196(5) Uani 1 1 d . . . Ni1 Ni -0.27580(7) -0.30598(8) -0.22185(5) 0.0131(3) Uani 1 1 d . . . Ni2 Ni 0.07255(7) -0.03851(8) -0.09494(5) 0.0136(3) 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 C1 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C2 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C3 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C4 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C5 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C6 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C7 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C8 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C9 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C10 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) C11 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C12 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C13 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C14 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C15 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C16 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C17 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) C18 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) C19 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) C20 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) C21 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) C22 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) C23 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C24 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C25 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C26 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C27 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C28 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) C29 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) N1 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) N2 0.0185(13) 0.0137(13) 0.0167(16) -0.0044(12) 0.0085(12) -0.0011(11) N3 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) N4 0.0136(19) 0.034(2) 0.0111(17) -0.0028(17) 0.0031(15) -0.0037(17) N5 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) O1 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) O2 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) O3 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) O4 0.0179(13) 0.0099(13) 0.0175(12) -0.0007(10) 0.0089(11) -0.0013(9) O5 0.026(2) 0.004(2) 0.018(2) -0.0026(18) 0.0118(19) 0.0031(17) O6 0.026(2) 0.004(2) 0.018(2) -0.0026(18) 0.0118(19) 0.0031(17) O7 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) O8 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) O9 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) O10 0.0272(12) 0.0184(13) 0.0165(13) 0.0019(10) 0.0127(11) 0.0001(10) Ni1 0.0147(6) 0.0102(6) 0.0145(6) 0.0011(5) 0.0066(5) 0.0017(5) Ni2 0.0159(6) 0.0105(6) 0.0153(7) -0.0001(5) 0.0078(5) -0.0014(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 1.373(8) . ? C1 C2 1.378(9) . ? C2 C3 1.393(9) . ? C3 C4 1.392(9) . ? C3 C8 1.485(9) . ? C4 C5 1.375(8) . ? C5 N1 1.376(8) . ? C6 N2 1.336(8) . ? C6 C7 1.398(8) . ? C7 C8 1.388(9) . ? C8 C9 1.390(8) . ? C9 C10 1.390(8) . ? C10 N2 1.337(8) . ? C11 N3 1.336(8) . ? C11 C12 1.381(9) . ? C11 C17 1.503(9) . ? C12 C13 1.385(8) . ? C13 C14 1.364(9) . ? C14 C15 1.389(9) . ? C14 C16 1.524(9) . ? C15 N3 1.321(8) . ? C16 O4 1.248(8) . ? C16 O3 1.260(8) . ? C17 O2 1.248(7) . ? C17 O1 1.274(7) . ? C18 N4 1.342(8) . ? C18 C19 1.381(9) . ? C19 C20 1.354(9) . ? C20 C21 1.372(9) . ? C20 C20 1.511(13) 3_655 ? C21 C22 1.375(8) . ? C22 N4 1.325(8) . ? C23 O10 1.246(8) . ? C23 O9 1.282(8) . ? C23 C25 1.490(9) . ? C24 N5 1.326(8) . ? C24 C25 1.416(9) . ? C25 C27 1.368(9) . ? C26 N5 1.363(8) . ? C26 C28 1.393(10) . ? C26 C29 1.498(9) . ? C27 C28 1.372(9) . ? C29 O8 1.255(8) . ? C29 O7 1.267(8) . ? N1 Ni1 2.104(6) . ? N2 Ni1 2.060(6) 4_556 ? N3 Ni1 2.079(6) . ? N4 Ni2 2.100(6) . ? N5 Ni2 2.050(6) . ? O1 Ni1 2.046(4) . ? O2 Ni2 2.026(5) . ? O4 Ni1 2.045(5) 2_454 ? O5 Ni2 2.112(4) . ? O6 Ni1 2.085(4) . ? O7 Ni2 2.046(5) . ? O9 Ni2 2.060(5) 2_544 ? Ni1 O4 2.045(5) 2_444 ? Ni1 N2 2.060(6) 4 ? Ni2 O9 2.060(5) 2_554 ? 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 N1 C1 C2 122.1(7) . . ? C1 C2 C3 120.3(7) . . ? C4 C3 C2 117.8(7) . . ? C4 C3 C8 120.1(7) . . ? C2 C3 C8 122.2(6) . . ? C5 C4 C3 120.2(7) . . ? C4 C5 N1 122.3(7) . . ? N2 C6 C7 123.1(7) . . ? C8 C7 C6 119.9(7) . . ? C7 C8 C9 117.1(7) . . ? C7 C8 C3 120.2(7) . . ? C9 C8 C3 122.5(6) . . ? C10 C9 C8 118.9(7) . . ? N2 C10 C9 124.5(7) . . ? N3 C11 C12 121.9(7) . . ? N3 C11 C17 115.7(7) . . ? C12 C11 C17 122.3(7) . . ? C11 C12 C13 118.2(7) . . ? C14 C13 C12 119.7(7) . . ? C13 C14 C15 118.6(7) . . ? C13 C14 C16 122.0(7) . . ? C15 C14 C16 119.4(6) . . ? N3 C15 C14 121.9(7) . . ? O4 C16 O3 126.8(7) . . ? O4 C16 C14 116.4(6) . . ? O3 C16 C14 116.8(7) . . ? O2 C17 O1 126.0(7) . . ? O2 C17 C11 117.0(7) . . ? O1 C17 C11 117.0(7) . . ? N4 C18 C19 124.0(7) . . ? C20 C19 C18 121.0(7) . . ? C19 C20 C21 115.4(6) . . ? C19 C20 C20 122.6(8) . 3_655 ? C21 C20 C20 121.9(9) . 3_655 ? C20 C21 C22 120.9(7) . . ? N4 C22 C21 124.4(7) . . ? O10 C23 O9 122.9(7) . . ? O10 C23 C25 120.7(7) . . ? O9 C23 C25 116.3(7) . . ? N5 C24 C25 122.9(7) . . ? C27 C25 C24 117.4(7) . . ? C27 C25 C23 123.1(7) . . ? C24 C25 C23 119.2(7) . . ? N5 C26 C28 121.9(7) . . ? N5 C26 C29 115.6(7) . . ? C28 C26 C29 122.5(7) . . ? C25 C27 C28 120.9(8) . . ? C27 C28 C26 118.5(7) . . ? O8 C29 O7 124.1(7) . . ? O8 C29 C26 117.8(7) . . ? O7 C29 C26 117.9(7) . . ? C1 N1 C5 117.1(6) . . ? C1 N1 Ni1 121.7(5) . . ? C5 N1 Ni1 118.7(4) . . ? C6 N2 C10 116.4(6) . . ? C6 N2 Ni1 118.4(5) . 4_556 ? C10 N2 Ni1 125.2(5) . 4_556 ? C15 N3 C11 119.5(7) . . ? C15 N3 Ni1 128.3(5) . . ? C11 N3 Ni1 112.1(5) . . ? C22 N4 C18 114.2(6) . . ? C22 N4 Ni2 121.6(5) . . ? C18 N4 Ni2 123.7(5) . . ? C24 N5 C26 118.1(7) . . ? C24 N5 Ni2 130.7(5) . . ? C26 N5 Ni2 110.6(5) . . ? C17 O1 Ni1 114.8(5) . . ? C17 O2 Ni2 136.9(5) . . ? C16 O4 Ni1 123.4(5) . 2_454 ? C29 O7 Ni2 113.3(5) . . ? C23 O9 Ni2 128.5(5) . 2_544 ? O4 Ni1 O1 174.27(19) 2_444 . ? O4 Ni1 N2 89.0(2) 2_444 4 ? O1 Ni1 N2 90.8(2) . 4 ? O4 Ni1 N3 93.9(2) 2_444 . ? O1 Ni1 N3 80.4(2) . . ? N2 Ni1 N3 90.3(2) 4 . ? O4 Ni1 O6 92.70(18) 2_444 . ? O1 Ni1 O6 93.03(18) . . ? N2 Ni1 O6 91.4(2) 4 . ? N3 Ni1 O6 173.2(2) . . ? O4 Ni1 N1 89.6(2) 2_444 . ? O1 Ni1 N1 90.2(2) . . ? N2 Ni1 N1 175.4(2) 4 . ? N3 Ni1 N1 85.5(2) . . ? O6 Ni1 N1 93.0(2) . . ? O2 Ni2 O7 89.00(19) . . ? O2 Ni2 N5 95.1(2) . . ? O7 Ni2 N5 82.0(2) . . ? O2 Ni2 O9 86.37(18) . 2_554 ? O7 Ni2 O9 171.9(2) . 2_554 ? N5 Ni2 O9 91.7(2) . 2_554 ? O2 Ni2 N4 173.2(2) . . ? O7 Ni2 N4 90.7(2) . . ? N5 Ni2 N4 91.6(2) . . ? O9 Ni2 N4 94.7(2) 2_554 . ? O2 Ni2 O5 80.75(19) . . ? O7 Ni2 O5 92.09(19) . . ? N5 Ni2 O5 172.9(2) . . ? O9 Ni2 O5 93.78(18) 2_554 . ? N4 Ni2 O5 92.5(2) . . ? data_[ni2(4,4-bipy)2(2,5-PDC(H))2(OH)] _database_code_depnum_ccdc_archive 'CCDC 826700' #TrackingRef '- NiPB1 revised.CIF' # CHEMICAL INFORMATION _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H17 N5 Ni2 O9' _chemical_formula_sum 'C29 H17 N5 Ni2 O9' _chemical_formula_weight 697.87 # UNIT CELL INFORMATION _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z +X+1/2,-Y+1/2,+Z+1/2 -X+1/2,+Y+1/2,-Z+1/2 _cell_length_a 13.6038(7) _cell_length_b 10.8508(7) _cell_length_c 19.3004(12) _cell_angle_alpha 90.0000 _cell_angle_beta 95.047(4) _cell_angle_gamma 90.0000 _cell_volume 2837.9(4) _cell_formula_units_Z 4 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv C18 C 0.2943(10) -0.1165(13) -0.0117(16) 1.00000 0.119 H18 H 0.2380 -0.1273 -0.0420 1.00000 0.119 C19 C 0.3737(8) -0.0519(11) -0.0319(11) 1.00000 0.119 H19 H 0.3700 -0.0191 -0.0765 1.00000 0.119 C20 C 0.4564(6) -0.0353(6) 0.0115(7) 1.00000 0.119 C21 C 0.4588(16) -0.0856(9) 0.0770(8) 1.00000 0.119 H21 H 0.5146 -0.0759 0.1081 1.00000 0.119 C22 C 0.3771(19) -0.1488(9) 0.0936(13) 1.00000 0.119 H22 H 0.3796 -0.1824 0.1381 1.00000 0.119 N4 N 0.2958(16) -0.1655(11) 0.0520(18) 1.00000 0.119 C3 C -0.3422(16) -0.2470(15) -0.0434(15) 1.00000 0.119 C2 C -0.3634(19) -0.3122(13) 0.0149(17) 1.00000 0.119 H2 H -0.4199 -0.3609 0.0131 1.00000 0.119 C1 C -0.3024(23) -0.3053(17) 0.0752(16) 1.00000 0.119 H1 H -0.3183 -0.3496 0.1139 1.00000 0.119 C4 C -0.2579(18) -0.1760(12) -0.0389(16) 1.00000 0.119 H4 H -0.2413 -0.1317 -0.0775 1.00000 0.119 C5 C -0.1991(17) -0.1718(15) 0.0222(18) 1.00000 0.119 H5 H -0.1424 -0.1235 0.0243 1.00000 0.119 C6 C -0.5390(16) -0.3461(20) -0.1802(20) 1.00000 0.119 H6 H -0.5879 -0.4062 -0.1850 1.00000 0.119 C7 C -0.4791(17) -0.3402(14) -0.1181(18) 1.00000 0.119 H7 H -0.4881 -0.3954 -0.0823 1.00000 0.119 C8 C -0.4059(16) -0.2526(14) -0.1091(15) 1.00000 0.119 C9 C -0.3959(17) -0.1737(14) -0.1637(16) 1.00000 0.119 H9 H -0.3477 -0.1127 -0.1603 1.00000 0.119 C10 C -0.4589(20) -0.1866(20) -0.2233(16) 1.00000 0.119 H10 H -0.4514 -0.1323 -0.2597 1.00000 0.119 N1 N -0.2191(22) -0.2355(20) 0.0806(16) 1.00000 0.119 N2 N -0.5298(18) -0.2701(25) -0.2332(17) 1.00000 0.119 Ni1 NI -0.1199(11) -0.2202(11) 0.1750(10) 1.00000 0.119 O6 O -0.0940(34) -0.3972(29) 0.1716(27) 1.00000 0.119 Ni2 NI 0.1623(8) -0.2201(12) 0.0912(8) 1.00000 0.119 N3 N -0.1088(11) -0.0286(12) 0.1770(6) 1.00000 0.119 C11 C -0.1618(10) 0.0602(18) 0.2042(6) 1.00000 0.119 H11 H -0.2101 0.0358 0.2325 1.00000 0.119 C12 C -0.1484(10) 0.1850(17) 0.1922(6) 1.00000 0.119 C13 C -0.0778(11) 0.2222(18) 0.1509(6) 1.00000 0.119 H13 H -0.0690 0.3059 0.1431 1.00000 0.119 C14 C -0.0213(10) 0.1335(18) 0.1218(6) 1.00000 0.119 H14 H 0.0274 0.1565 0.0934 1.00000 0.119 C15 C -0.0397(10) 0.0112(17) 0.1366(6) 1.00000 0.119 C16 C 0.0211(10) -0.0869(18) 0.1056(6) 1.00000 0.119 O1 O 0.0014(8) -0.1972(19) 0.1207(5) 1.00000 0.119 O2 O 0.0847(11) -0.0495(19) 0.0680(6) 1.00000 0.119 C17 C -0.2121(11) 0.2803(20) 0.2256(6) 1.00000 0.119 O3 O -0.1978(17) 0.3934(21) 0.2170(9) 1.00000 0.119 O4 O -0.2756(10) 0.2336(28) 0.2600(6) 1.00000 0.119 N5 N 0.2112(9) -0.3986(15) 0.1190(10) 1.00000 0.119 C26 C 0.1386(10) -0.5966(14) 0.1083(12) 1.00000 0.119 H26 H 0.0998 -0.6531 0.0820 1.00000 0.119 C23 C 0.2507(10) -0.4247(20) 0.1819(11) 1.00000 0.119 H23 H 0.2891 -0.3666 0.2073 1.00000 0.119 C24 C 0.2363(10) -0.5394(21) 0.2114(11) 1.00000 0.119 C25 C 0.1804(11) -0.6251(18) 0.1746(12) 1.00000 0.119 H25 H 0.1700 -0.7022 0.1937 1.00000 0.119 C27 C 0.1560(7) -0.4813(14) 0.0821(10) 1.00000 0.119 C28 C 0.1170(7) -0.4379(20) 0.0109(10) 1.00000 0.119 O7 O 0.1068(8) -0.3216(21) 0.0018(12) 1.00000 0.119 O8 O 0.0983(9) -0.5179(28) -0.0349(13) 1.00000 0.119 C29 C 0.2848(11) -0.5628(23) 0.2840(11) 1.00000 0.119 O9 O 0.2740(16) -0.6697(23) 0.3066(18) 1.00000 0.119 O10 O 0.3284(12) -0.4716(26) 0.3110(15) 1.00000 0.119