# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_General _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 2003-10-21 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _journal_volume ? _journal_year ? _journal_page_first ? #=========================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) #=========================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Masaaki Kojima' _publ_contact_author_email kojima@cc.okayama-u.ac.jp _publ_contact_author_fax +81-86-251-7842 _publ_contact_author_phone +81-86-251-7842 _publ_contact_letter ; ENTER TEXT OF LETTER ; #=========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Ferromagnetic Ni(II)-Gd(III) interactions in complexes with NiGd, NiGdNi, and NiGdGdNi cores supported by tripodal ligands ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; #=========================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. Larson, A. C. (1970), Crystallographic Computing, 291-294. ed F. R. Ahmed, Munksgaard, Copenhagen. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #--------------------------------------------------------------------------= #--- loop_ _publ_manuscript_incl_extra_item '_geom_extra_table_head_3' '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _publ_author_name 'Masaaki Kojima' 'Haruo Akashi' 'Naohide Matsumoto' 'Shutaro Osa' 'Nazzareno Re' 'Yukinari Sunatsuki' ; M.Tsuchimoto ; 'Tomoka Yamaguchi' # #--------------------------------------------------------------------------= #=========================================================================== data_030131 _database_code_depnum_ccdc_archive 'CCDC 229921' #=========================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H40 F12 Gd N3 O10 Ni ' _chemical_formula_moiety 'C40 H40 F12 Gd N3 O10 Ni ' _chemical_formula_weight 1166.70 _chemical_melting_point ? #=========================================================================== # CRYSTAL DATA _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 13.027(1) _cell_length_b 13.346(1) _cell_length_c 15.242(1) _cell_angle_alpha 95.100(5) _cell_angle_beta 115.364(2) _cell_angle_gamma 91.537(6) _cell_volume 2378.8(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6668 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.1 #--------------------------------------------------------------------------= _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1162.00 _exptl_absorpt_coefficient_mu 1.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.828 #=========================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 18741 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9181 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.9231 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #=========================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10009 _reflns_number_gt 15221 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1190 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 16979 _refine_ls_number_parameters 632 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w == 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.51 _refine_diff_density_min -1.83 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 313(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Gd Gd -0.165 3.904 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Gd(1) Gd 0.96289(1) 0.76425(1) 0.23430(1) 0.03398(5) Uani 1.00 1 d . . . Ni(1) Ni 1.14036(4) 0.77473(3) 0.45680(3) 0.0368(1) Uani 1.00 1 d . . . F(1) F 0.7653(3) 0.4064(2) 0.1457(3) 0.102(1) Uani 1.00 1 d . . . F(2) F 0.6745(4) 0.4991(3) 0.1969(4) 0.136(2) Uani 1.00 1 d . . . F(3) F 0.6088(4) 0.4492(4) 0.0469(4) 0.205(2) Uani 1.00 1 d . . . F(4) F 0.8071(4) 0.7194(7) -0.1351(3) 0.241(3) Uani 1.00 1 d . . . F(5) F 0.6405(4) 0.6612(3) -0.1675(2) 0.137(2) Uani 1.00 1 d . . . F(6) F 0.6931(4) 0.8046(3) -0.1114(3) 0.138(2) Uani 1.00 1 d . . . F(7) F 0.5509(4) 0.8549(7) 0.1767(4) 0.229(3) Uani 1.00 1 d . . . F(8) F 0.5111(3) 0.9044(5) 0.0514(5) 0.217(3) Uani 1.00 1 d . . . F(9) F 0.5372(4) 0.7632(4) 0.0668(6) 0.221(3) Uani 1.00 1 d . . . F(10) F 0.9401(6) 1.1390(3) 0.1794(4) 0.185(2) Uani 1.00 1 d . . . F(11) F 0.9488(5) 1.0607(3) 0.0627(5) 0.168(3) Uani 1.00 1 d . . . F(12) F 0.7993(4) 1.1200(3) 0.0460(4) 0.146(2) Uani 1.00 1 d . . . O(1) O 0.9635(2) 0.7888(2) 0.3862(2) 0.0397(6) Uani 1.00 1 d . . . O(2) O 1.0909(2) 0.6580(2) 0.3441(2) 0.0397(6) Uani 1.00 1 d . . . O(3) O 1.1363(2) 0.8541(2) 0.3443(2) 0.0366(6) Uani 1.00 1 d . . . O(4) O 0.8462(2) 0.6113(2) 0.1873(2) 0.0500(7) Uani 1.00 1 d . . . O(5) O 0.8616(2) 0.7430(2) 0.0591(2) 0.0484(7) Uani 1.00 1 d . . . O(6) O 0.7639(2) 0.8047(2) 0.1864(2) 0.0473(7) Uani 1.00 1 d . . . O(7) O 0.9351(2) 0.9313(2) 0.1867(2) 0.0483(7) Uani 1.00 1 d . . . O(8) O 1.0922(2) 0.7134(2) 0.1664(2) 0.0476(7) Uani 1.00 1 d . . . O(9) O 0.2924(3) 0.6354(3) 0.2711(3) 0.103(2) Uani 1.00 1 d . . . O(10) O 0.364(1) 0.483(1) 0.4245(9) 0.322(6) Uiso 1.00 1 d . . . N(1) N 1.1477(3) 0.8827(2) 0.5644(2) 0.0425(8) Uani 1.00 1 d . . . N(2) N 1.1570(3) 0.6735(2) 0.5540(2) 0.0479(9) Uani 1.00 1 d . . . N(3) N 1.3168(3) 0.7889(3) 0.5175(2) 0.0465(8) Uani 1.00 1 d . . . C(1) C 1.3890(4) 0.8061(5) 0.7870(3) 0.078(2) Uani 1.00 1 d . . . C(2) C 1.3086(4) 0.7943(3) 0.6764(3) 0.054(1) Uani 1.00 1 d . . . C(3) C 1.2612(3) 0.8995(3) 0.6492(3) 0.054(1) Uani 1.00 1 d . . . C(4) C 1.0626(3) 0.9098(3) 0.5794(3) 0.0409(9) Uani 1.00 1 d . . . C(5) C 0.9427(3) 0.8822(3) 0.5191(2) 0.0389(9) Uani 1.00 1 d . . . C(6) C 0.8984(3) 0.8192(2) 0.4293(2) 0.0354(8) Uani 1.00 1 d . . . C(7) C 0.7832(3) 0.7876(3) 0.3882(3) 0.046(1) Uani 1.00 1 d . . . C(8) C 0.7130(3) 0.8192(3) 0.4299(3) 0.055(1) Uani 1.00 1 d . . . C(9) C 0.7544(4) 0.8841(3) 0.5148(3) 0.058(1) Uani 1.00 1 d . . . C(10) C 0.8689(3) 0.9143(3) 0.5594(3) 0.047(1) Uani 1.00 1 d . . . C(11) C 1.2123(4) 0.7150(3) 0.6579(3) 0.058(1) Uani 1.00 1 d . . . C(12) C 1.1444(4) 0.5782(3) 0.5348(3) 0.055(1) Uani 1.00 1 d . . . C(13) C 1.1069(4) 0.5191(3) 0.4406(3) 0.053(1) Uani 1.00 1 d . . . C(14) C 1.0848(3) 0.5596(3) 0.3513(3) 0.043(1) Uani 1.00 1 d . . . C(15) C 1.0601(3) 0.4910(3) 0.2681(3) 0.050(1) Uani 1.00 1 d . . . C(16) C 1.0554(4) 0.3868(3) 0.2719(4) 0.063(1) Uani 1.00 1 d . . . C(17) C 1.0757(5) 0.3495(3) 0.3604(4) 0.075(2) Uani 1.00 1 d . . . C(18) C 1.1019(4) 0.4137(3) 0.4415(4) 0.068(1) Uani 1.00 1 d . . . C(19) C 1.3746(4) 0.7623(4) 0.6185(3) 0.059(1) Uani 1.00 1 d . . . C(20) C 1.3768(3) 0.8386(3) 0.4863(3) 0.049(1) Uani 1.00 1 d . . . C(21) C 1.3391(3) 0.8855(3) 0.3966(3) 0.043(1) Uani 1.00 1 d . . . C(22) C 1.2232(3) 0.8914(2) 0.3308(3) 0.0388(9) Uani 1.00 1 d . . . C(23) C 1.2027(3) 0.9440(3) 0.2492(3) 0.048(1) Uani 1.00 1 d . . . C(24) C 1.2882(4) 0.9854(3) 0.2320(3) 0.059(1) Uani 1.00 1 d . . . C(25) C 1.4016(4) 0.9777(4) 0.2957(4) 0.063(1) Uani 1.00 1 d . . . C(26) C 1.4248(3) 0.9299(3) 0.3769(3) 0.054(1) Uani 1.00 1 d . . . C(27) C 0.7637(4) 0.5748(3) 0.1104(3) 0.054(1) Uani 1.00 1 d . . . C(28) C 0.7007(4) 0.4821(4) 0.1226(4) 0.073(2) Uani 1.00 1 d . . . C(29) C 0.7240(4) 0.6063(3) 0.0167(3) 0.062(1) Uani 1.00 1 d . . . C(30) C 0.7786(3) 0.6878(3) -0.0004(3) 0.050(1) Uani 1.00 1 d . . . C(31) C 0.7344(5) 0.7147(5) -0.1056(3) 0.079(2) Uani 1.00 1 d . . . C(32) C 0.7016(3) 0.8675(3) 0.1366(3) 0.048(1) Uani 1.00 1 d . . . C(33) C 0.5754(4) 0.8488(4) 0.1073(4) 0.062(1) Uani 1.00 1 d . . . C(34) C 0.7371(4) 0.9530(3) 0.1067(3) 0.053(1) Uani 1.00 1 d . . . C(35) C 0.8507(4) 0.9776(3) 0.1353(3) 0.049(1) Uani 1.00 1 d . . . C(36) C 0.8846(5) 1.0753(4) 0.1054(4) 0.072(2) Uani 1.00 1 d . . . C(37) C 1.1031(4) 0.7274(4) 0.0780(3) 0.065(1) Uani 1.00 1 d . . . C(38) C 1.0871(6) 0.6310(6) 0.0171(4) 0.111(3) Uani 1.00 1 d . . . C(39) C 0.3970(6) 0.6728(6) 0.2685(8) 0.133(3) Uani 1.00 1 d . . . C(40) C 0.454(1) 0.6021(7) 0.2332(8) 0.163(4) Uani 1.00 1 d . . . H(1) H 1.4198 0.7435 0.8059 0.086 Uiso 1.00 1 c . . . H(2) H 1.4492 0.8553 0.7997 0.086 Uiso 1.00 1 c . . . H(3) H 1.3480 0.8272 0.8231 0.086 Uiso 1.00 1 c . . . H(4) H 1.3115 0.9376 0.6324 0.060 Uiso 1.00 1 c . . . H(5) H 1.2545 0.9351 0.7032 0.060 Uiso 1.00 1 c . . . H(6) H 1.0802 0.9538 0.6373 0.049 Uiso 1.00 1 c . . . H(7) H 0.8985 0.9577 0.6189 0.057 Uiso 1.00 1 c . . . H(8) H 0.7051 0.9074 0.5423 0.072 Uiso 1.00 1 c . . . H(9) H 0.6347 0.7963 0.3994 0.066 Uiso 1.00 1 c . . . H(10) H 0.7524 0.7430 0.3294 0.056 Uiso 1.00 1 c . . . H(11) H 1.1571 0.7454 0.6748 0.068 Uiso 1.00 1 c . . . H(12) H 1.2426 0.6619 0.6971 0.068 Uiso 1.00 1 c . . . H(13) H 1.1610 0.5411 0.5891 0.067 Uiso 1.00 1 c . . . H(14) H 1.1175 0.3869 0.5013 0.081 Uiso 1.00 1 c . . . H(15) H 1.0716 0.2788 0.3633 0.089 Uiso 1.00 1 c . . . H(16) H 1.0386 0.3416 0.2150 0.074 Uiso 1.00 1 c . . . H(17) H 1.0460 0.5160 0.2079 0.061 Uiso 1.00 1 c . . . H(18) H 1.3797 0.6914 0.6165 0.066 Uiso 1.00 1 c . . . H(19) H 1.4490 0.7951 0.6496 0.066 Uiso 1.00 1 c . . . H(20) H 1.4564 0.8458 0.5271 0.057 Uiso 1.00 1 c . . . H(21) H 1.5021 0.9268 0.4222 0.065 Uiso 1.00 1 c . . . H(22) H 1.4613 1.0047 0.2828 0.079 Uiso 1.00 1 c . . . H(23) H 1.2702 1.0201 0.1761 0.073 Uiso 1.00 1 c . . . H(24) H 1.1261 0.9509 0.2044 0.057 Uiso 1.00 1 c . . . H(25) H 0.6594 0.5712 -0.0357 0.065 Uiso 1.00 1 c . . . H(26) H 0.6820 0.9942 0.0660 0.062 Uiso 1.00 1 c . . . H(27) H 1.0130 0.6011 -0.0005 0.134 Uiso 1.00 1 c . . . H(28) H 1.0956 0.6418 -0.0403 0.134 Uiso 1.00 1 c . . . H(29) H 1.1424 0.5875 0.0537 0.134 Uiso 1.00 1 c . . . H(30) H 1.0475 0.7706 0.0413 0.084 Uiso 1.00 1 c . . . H(31) H 1.1770 0.7574 0.0949 0.084 Uiso 1.00 1 c . . . H(32) H 1.1749 0.6940 0.2184 0.060 Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Gd(1) 0.0350(1) 0.0345(1) 0.0305(1) 0.00236(6) 0.01153(7) 0.00815(6) Ni(1) 0.0366(2) 0.0400(2) 0.0314(2) 0.0044(2) 0.0113(2) 0.0093(2) F(1) 0.128(3) 0.054(2) 0.140(3) 0.005(2) 0.071(3) 0.028(2) F(2) 0.153(4) 0.087(3) 0.229(5) -0.014(2) 0.143(4) 0.014(3) F(3) 0.136(4) 0.175(4) 0.174(5) -0.109(3) -0.063(3) 0.098(4) F(4) 0.121(4) 0.58(1) 0.066(2) 0.130(6) 0.060(3) 0.126(5) F(5) 0.153(4) 0.141(3) 0.051(2) -0.023(3) -0.016(2) 0.016(2) F(6) 0.180(4) 0.121(3) 0.082(3) 0.021(3) 0.021(3) 0.052(2) F(7) 0.056(2) 0.53(1) 0.105(3) 0.002(4) 0.040(2) 0.016(5) F(8) 0.046(2) 0.269(7) 0.318(8) 0.029(3) 0.026(3) 0.211(6) F(9) 0.061(2) 0.150(5) 0.40(1) -0.029(3) 0.067(4) -0.078(5) F(10) 0.297(7) 0.074(2) 0.119(3) -0.081(4) 0.035(4) 0.009(2) F(11) 0.216(5) 0.121(3) 0.290(7) 0.067(3) 0.203(6) 0.124(4) F(12) 0.111(3) 0.120(3) 0.209(5) 0.033(2) 0.050(3) 0.125(3) O(1) 0.035(1) 0.053(1) 0.031(1) 0.003(1) 0.014(1) 0.006(1) O(2) 0.048(1) 0.031(1) 0.038(1) 0.0087(9) 0.015(1) 0.0117(9) O(3) 0.033(1) 0.040(1) 0.034(1) -0.0013(9) 0.012(1) 0.0079(9) O(4) 0.048(2) 0.042(1) 0.048(1) -0.004(1) 0.009(1) 0.012(1) O(5) 0.054(2) 0.055(2) 0.033(1) 0.000(1) 0.015(1) 0.009(1) O(6) 0.044(1) 0.052(2) 0.045(1) 0.010(1) 0.016(1) 0.015(1) O(7) 0.048(1) 0.039(1) 0.052(2) 0.005(1) 0.014(1) 0.013(1) O(8) 0.049(2) 0.056(2) 0.043(1) 0.006(1) 0.025(1) 0.007(1) O(9) 0.056(2) 0.124(3) 0.125(4) 0.013(2) 0.028(2) 0.053(3) N(1) 0.041(2) 0.048(2) 0.031(1) -0.003(1) 0.009(1) 0.004(1) N(2) 0.053(2) 0.053(2) 0.034(2) 0.007(1) 0.013(1) 0.018(1) N(3) 0.036(2) 0.058(2) 0.037(2) 0.010(1) 0.008(1) 0.008(1) C(1) 0.062(3) 0.112(4) 0.040(2) 0.015(3) 0.001(2) 0.017(2) C(2) 0.048(2) 0.073(3) 0.030(2) 0.009(2) 0.004(2) 0.012(2) C(3) 0.044(2) 0.071(3) 0.035(2) -0.002(2) 0.008(2) 0.003(2) C(4) 0.051(2) 0.034(2) 0.038(2) 0.004(1) 0.018(2) 0.008(1) C(5) 0.047(2) 0.035(2) 0.036(2) 0.008(1) 0.017(2) 0.010(1) C(6) 0.038(2) 0.029(2) 0.041(2) 0.008(1) 0.018(1) 0.013(1) C(7) 0.039(2) 0.058(2) 0.042(2) 0.005(2) 0.017(2) 0.008(2) C(8) 0.036(2) 0.067(3) 0.061(3) 0.003(2) 0.020(2) 0.007(2) C(9) 0.053(2) 0.063(3) 0.063(3) 0.019(2) 0.030(2) 0.005(2) C(10) 0.055(2) 0.041(2) 0.048(2) 0.016(2) 0.022(2) 0.007(2) C(11) 0.061(3) 0.071(3) 0.038(2) 0.011(2) 0.015(2) 0.020(2) C(12) 0.067(3) 0.053(2) 0.048(2) 0.013(2) 0.023(2) 0.025(2) C(13) 0.058(2) 0.044(2) 0.055(2) 0.006(2) 0.020(2) 0.018(2) C(14) 0.043(2) 0.039(2) 0.045(2) 0.004(1) 0.016(2) 0.009(1) C(15) 0.057(2) 0.039(2) 0.055(2) 0.008(2) 0.023(2) 0.012(2) C(16) 0.074(3) 0.037(2) 0.074(3) 0.006(2) 0.029(2) 0.003(2) C(17) 0.092(4) 0.039(2) 0.091(4) 0.009(2) 0.033(3) 0.023(2) C(18) 0.085(3) 0.048(2) 0.071(3) 0.010(2) 0.028(3) 0.025(2) C(19) 0.045(2) 0.076(3) 0.045(2) 0.013(2) 0.006(2) 0.019(2) C(20) 0.035(2) 0.054(2) 0.054(2) 0.006(2) 0.015(2) 0.002(2) C(21) 0.037(2) 0.045(2) 0.046(2) 0.001(1) 0.018(2) 0.001(1) C(22) 0.045(2) 0.033(2) 0.044(2) -0.001(1) 0.024(2) 0.001(1) C(23) 0.046(2) 0.049(2) 0.047(2) -0.006(2) 0.019(2) 0.009(2) C(24) 0.069(3) 0.058(2) 0.056(3) -0.009(2) 0.033(2) 0.010(2) C(25) 0.053(3) 0.071(3) 0.073(3) -0.013(2) 0.038(2) 0.000(2) C(26) 0.041(2) 0.057(2) 0.064(3) -0.003(2) 0.025(2) -0.003(2) C(27) 0.048(2) 0.044(2) 0.060(2) 0.002(2) 0.014(2) 0.008(2) C(28) 0.057(3) 0.061(3) 0.082(3) -0.014(2) 0.012(3) 0.015(2) C(29) 0.058(3) 0.059(2) 0.045(2) -0.006(2) 0.003(2) -0.000(2) C(30) 0.050(2) 0.057(2) 0.039(2) 0.010(2) 0.013(2) 0.009(2) C(31) 0.084(4) 0.100(4) 0.032(2) 0.010(3) 0.005(2) 0.004(2) C(32) 0.050(2) 0.053(2) 0.037(2) 0.012(2) 0.014(2) 0.007(2) C(33) 0.041(2) 0.078(3) 0.063(3) 0.011(2) 0.016(2) 0.014(2) C(34) 0.050(2) 0.055(2) 0.050(2) 0.019(2) 0.015(2) 0.022(2) C(35) 0.061(2) 0.043(2) 0.042(2) 0.007(2) 0.018(2) 0.013(2) C(36) 0.082(4) 0.052(3) 0.081(3) 0.013(2) 0.030(3) 0.030(2) C(37) 0.069(3) 0.082(3) 0.059(3) 0.011(2) 0.039(2) 0.017(2) C(38) 0.119(5) 0.154(6) 0.061(3) 0.039(5) 0.043(4) -0.010(4) C(39) 0.066(4) 0.111(6) 0.206(9) 0.003(4) 0.045(5) 0.007(6) C(40) 0.20(1) 0.109(6) 0.22(1) -0.028(6) 0.147(9) -0.051(6) #=========================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Gd(1) Ni(1) 3.1697(4) yes . . Gd(1) O(1) 2.306(3) yes . . Gd(1) O(2) 2.398(2) yes . . Gd(1) O(3) 2.367(2) yes . . Gd(1) O(4) 2.373(2) yes . . Gd(1) O(5) 2.404(2) yes . . Gd(1) O(6) 2.463(3) yes . . Gd(1) O(7) 2.395(2) yes . . Gd(1) O(8) 2.409(3) yes . . Ni(1) O(1) 2.106(2) yes . . Ni(1) O(2) 2.078(2) yes . . Ni(1) O(3) 2.077(3) yes . . Ni(1) N(1) 2.052(3) yes . . Ni(1) N(2) 2.041(3) yes . . Ni(1) N(3) 2.073(3) yes . . F(1) C(28) 1.308(6) yes . . F(2) C(28) 1.32(1) yes . . F(3) C(28) 1.287(6) yes . . F(4) C(31) 1.212(9) yes . . F(5) C(31) 1.319(6) yes . . F(6) C(31) 1.323(8) yes . . F(7) C(33) 1.226(9) yes . . F(8) C(33) 1.230(8) yes . . F(9) C(33) 1.230(7) yes . . F(10) C(36) 1.271(6) yes . . F(11) C(36) 1.27(1) yes . . F(12) C(36) 1.295(6) yes . . O(1) C(6) 1.328(5) yes . . O(2) C(14) 1.330(4) yes . . O(3) C(22) 1.326(5) yes . . O(4) C(27) 1.249(4) yes . . O(5) C(30) 1.238(4) yes . . O(6) C(32) 1.249(4) yes . . O(7) C(35) 1.260(4) yes . . O(8) C(37) 1.442(7) yes . . O(8) H(32) 1.084 no . . O(9) C(39) 1.46(1) yes . . N(1) C(3) 1.484(4) yes . . N(1) C(4) 1.280(6) yes . . N(2) C(11) 1.476(5) yes . . N(2) C(12) 1.269(5) yes . . N(3) C(19) 1.476(5) yes . . N(3) C(20) 1.275(6) yes . . C(1) C(2) 1.548(5) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) C(3) 1.567(6) yes . . C(2) C(11) 1.531(7) yes . . C(2) C(19) 1.517(7) yes . . C(3) H(4) 0.950(7) no . . C(3) H(5) 0.950 no . . C(4) C(5) 1.449(5) yes . . C(4) H(6) 0.950 no . . C(5) C(6) 1.416(4) yes . . C(5) C(10) 1.401(7) yes . . C(6) C(7) 1.392(5) yes . . C(7) C(8) 1.375(7) yes . . C(7) H(10) 0.950 no . . C(8) C(9) 1.376(6) yes . . C(8) H(9) 0.950 no . . C(9) C(10) 1.378(6) yes . . C(9) H(8) 0.950 no . . C(10) H(7) 0.950 no . . C(11) H(11) 0.950 no . . C(11) H(12) 0.950 no . . C(12) C(13) 1.449(6) yes . . C(12) H(13) 0.950 no . . C(13) C(14) 1.427(6) yes . . C(13) C(18) 1.408(6) yes . . C(14) C(15) 1.406(5) yes . . C(15) C(16) 1.397(5) yes . . C(15) H(17) 0.950 no . . C(16) C(17) 1.399(8) yes . . C(16) H(16) 0.950 no . . C(17) C(18) 1.346(7) yes . . C(17) H(15) 0.950 no . . C(18) H(14) 0.950 no . . C(19) H(18) 0.950 no . . C(19) H(19) 0.950 no . . C(20) C(21) 1.447(6) yes . . C(20) H(20) 0.950(5) no . . C(21) C(22) 1.419(5) yes . . C(21) C(26) 1.404(7) yes . . C(22) C(23) 1.411(6) yes . . C(23) C(24) 1.363(7) yes . . C(23) H(24) 0.950 no . . C(24) C(25) 1.390(6) yes . . C(24) H(23) 0.950 no . . C(25) C(26) 1.365(7) yes . . C(25) H(22) 0.950 no . . C(26) H(21) 0.950 no . . C(27) C(28) 1.535(7) yes . . C(27) C(29) 1.403(6) yes . . C(29) C(30) 1.386(7) yes . . C(29) H(25) 0.950 no . . C(30) C(31) 1.535(6) yes . . C(32) C(33) 1.514(6) yes . . C(32) C(34) 1.403(6) yes . . C(34) C(35) 1.372(6) yes . . C(34) H(26) 0.950 no . . C(35) C(36) 1.534(7) yes . . C(37) C(38) 1.472(9) yes . . C(37) H(30) 0.950 no . . C(37) H(31) 0.950 no . . C(38) H(27) 0.95 no . . C(38) H(28) 0.95 no . . C(38) H(29) 0.95 no . . C(39) C(40) 1.42(2) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ni(1) Gd(1) O(1) 41.62(6) yes . . . Ni(1) Gd(1) O(2) 40.95(5) yes . . . Ni(1) Gd(1) O(3) 40.95(6) yes . . . Ni(1) Gd(1) O(4) 109.86(6) yes . . . Ni(1) Gd(1) O(5) 167.68(8) yes . . . Ni(1) Gd(1) O(6) 121.51(7) yes . . . Ni(1) Gd(1) O(7) 109.56(5) yes . . . Ni(1) Gd(1) O(8) 96.61(5) yes . . . O(1) Gd(1) O(2) 68.89(9) yes . . . O(1) Gd(1) O(3) 71.54(9) yes . . . O(1) Gd(1) O(4) 93.9(1) yes . . . O(1) Gd(1) O(5) 150.4(1) yes . . . O(1) Gd(1) O(6) 80.14(9) yes . . . O(1) Gd(1) O(7) 100.7(1) yes . . . O(1) Gd(1) O(8) 137.84(8) yes . . . O(2) Gd(1) O(3) 68.06(7) yes . . . O(2) Gd(1) O(4) 79.79(8) yes . . . O(2) Gd(1) O(5) 130.53(9) yes . . . O(2) Gd(1) O(6) 135.7(1) yes . . . O(2) Gd(1) O(7) 145.61(7) yes . . . O(2) Gd(1) O(8) 73.53(9) yes . . . O(3) Gd(1) O(4) 147.63(8) yes . . . O(3) Gd(1) O(5) 133.0(1) yes . . . O(3) Gd(1) O(6) 130.89(8) yes . . . O(3) Gd(1) O(7) 77.55(8) yes . . . O(3) Gd(1) O(8) 77.34(8) yes . . . O(4) Gd(1) O(5) 72.0(1) yes . . . O(4) Gd(1) O(6) 71.31(9) yes . . . O(4) Gd(1) O(7) 134.49(8) yes . . . O(4) Gd(1) O(8) 97.6(1) yes . . . O(5) Gd(1) O(6) 70.8(1) yes . . . O(5) Gd(1) O(7) 74.41(9) yes . . . O(5) Gd(1) O(8) 71.11(9) yes . . . O(6) Gd(1) O(7) 69.22(9) yes . . . O(6) Gd(1) O(8) 141.88(8) yes . . . O(7) Gd(1) O(8) 99.5(1) yes . . . O(1) Ni(1) O(2) 79.01(9) yes . . . O(1) Ni(1) O(3) 81.5(1) yes . . . O(1) Ni(1) N(1) 88.1(1) yes . . . O(1) Ni(1) N(2) 103.8(1) yes . . . O(1) Ni(1) N(3) 168.6(1) yes . . . O(1) Ni(1) Gd(1) 46.64(7) yes . . . O(2) Ni(1) O(3) 79.87(9) yes . . . O(2) Ni(1) N(1) 165.3(1) yes . . . O(2) Ni(1) N(2) 90.4(1) yes . . . O(2) Ni(1) N(3) 105.7(1) yes . . . O(2) Ni(1) Gd(1) 49.17(6) yes . . . O(3) Ni(1) N(1) 105.2(1) yes . . . O(3) Ni(1) N(2) 167.9(1) yes . . . O(3) Ni(1) N(3) 89.0(1) yes . . . O(3) Ni(1) Gd(1) 48.32(5) yes . . . N(1) Ni(1) N(2) 86.0(1) yes . . . N(1) Ni(1) N(3) 88.3(1) yes . . . N(1) Ni(1) Gd(1) 124.42(8) yes . . . N(2) Ni(1) N(3) 86.8(1) yes . . . N(2) Ni(1) Gd(1) 128.51(8) yes . . . N(3) Ni(1) Gd(1) 129.0(1) yes . . . C(6) O(1) Gd(1) 141.3(2) yes . . . C(6) O(1) Ni(1) 125.8(2) yes . . . Ni(1) O(1) Gd(1) 91.7(1) yes . . . C(14) O(2) Gd(1) 132.5(2) yes . . . C(14) O(2) Ni(1) 127.2(2) yes . . . Ni(1) O(2) Gd(1) 89.88(8) yes . . . C(22) O(3) Gd(1) 131.5(2) yes . . . C(22) O(3) Ni(1) 128.4(2) yes . . . Ni(1) O(3) Gd(1) 90.74(9) yes . . . C(27) O(4) Gd(1) 133.9(3) yes . . . C(30) O(5) Gd(1) 134.2(3) yes . . . C(32) O(6) Gd(1) 135.0(3) yes . . . C(35) O(7) Gd(1) 135.3(2) yes . . . C(37) O(8) H(32) 106.3 no . . . C(37) O(8) Gd(1) 135.4(3) yes . . . H(32) O(8) Gd(1) 115.7 no . . . C(3) N(1) C(4) 116.4(3) yes . . . C(3) N(1) Ni(1) 114.0(3) yes . . . C(4) N(1) Ni(1) 125.4(2) yes . . . C(11) N(2) C(12) 117.5(3) yes . . . C(11) N(2) Ni(1) 115.4(3) yes . . . C(12) N(2) Ni(1) 125.8(3) yes . . . C(19) N(3) C(20) 117.0(3) yes . . . C(19) N(3) Ni(1) 115.1(3) yes . . . C(20) N(3) Ni(1) 125.8(2) yes . . . C(2) C(1) H(1) 109.8 no . . . C(2) C(1) H(2) 108.9 no . . . C(2) C(1) H(3) 109.7 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . C(3) C(2) C(11) 111.2(3) yes . . . C(3) C(2) C(19) 109.4(4) yes . . . C(3) C(2) C(1) 107.6(4) yes . . . C(11) C(2) C(19) 111.0(4) yes . . . C(11) C(2) C(1) 107.9(4) yes . . . C(19) C(2) C(1) 109.7(4) yes . . . H(4) C(3) H(5) 109.5 no . . . H(4) C(3) N(1) 109.6 no . . . H(4) C(3) C(2) 109.5 no . . . H(5) C(3) N(1) 109.9 no . . . H(5) C(3) C(2) 110.0 no . . . N(1) C(3) C(2) 108.4(3) yes . . . C(5) C(4) H(6) 115.9 no . . . C(5) C(4) N(1) 128.2(3) yes . . . H(6) C(4) N(1) 115.9 no . . . C(6) C(5) C(10) 119.4(3) yes . . . C(6) C(5) C(4) 124.8(4) yes . . . C(10) C(5) C(4) 115.5(3) yes . . . C(7) C(6) O(1) 120.5(3) yes . . . C(7) C(6) C(5) 117.3(4) yes . . . O(1) C(6) C(5) 122.2(3) yes . . . C(8) C(7) H(10) 119.3 no . . . C(8) C(7) C(6) 122.0(3) yes . . . H(10) C(7) C(6) 118.8 no . . . C(9) C(8) H(9) 119.6 no . . . C(9) C(8) C(7) 120.9(4) yes . . . H(9) C(8) C(7) 119.5 no . . . C(10) C(9) H(8) 120.7 no . . . C(10) C(9) C(8) 118.7(5) yes . . . H(8) C(9) C(8) 120.6 no . . . H(7) C(10) C(5) 119.3 no . . . H(7) C(10) C(9) 119.2 no . . . C(5) C(10) C(9) 121.6(4) yes . . . H(11) C(11) H(12) 109.5 no . . . H(11) C(11) N(2) 109.0 no . . . H(11) C(11) C(2) 109.2 no . . . H(12) C(11) N(2) 109.3 no . . . H(12) C(11) C(2) 109.3 no . . . N(2) C(11) C(2) 110.6(4) yes . . . C(13) C(12) H(13) 116.0 no . . . C(13) C(12) N(2) 128.3(4) yes . . . H(13) C(12) N(2) 115.7 no . . . C(14) C(13) C(18) 119.1(4) yes . . . C(14) C(13) C(12) 124.9(4) yes . . . C(18) C(13) C(12) 115.8(4) yes . . . C(15) C(14) O(2) 119.1(4) yes . . . C(15) C(14) C(13) 117.5(3) yes . . . O(2) C(14) C(13) 123.3(3) yes . . . C(16) C(15) H(17) 119.2 no . . . C(16) C(15) C(14) 121.6(4) yes . . . H(17) C(15) C(14) 119.2 no . . . C(17) C(16) H(16) 120.1 no . . . C(17) C(16) C(15) 119.4(4) yes . . . H(16) C(16) C(15) 120.4 no . . . C(18) C(17) H(15) 120.0 no . . . C(18) C(17) C(16) 120.1(4) yes . . . H(15) C(17) C(16) 119.9 no . . . H(14) C(18) C(13) 119.0 no . . . H(14) C(18) C(17) 118.9 no . . . C(13) C(18) C(17) 122.1(5) yes . . . H(18) C(19) H(19) 109.5 no . . . H(18) C(19) N(3) 108.8 no . . . H(18) C(19) C(2) 109.1 no . . . H(19) C(19) N(3) 109.5 no . . . H(19) C(19) C(2) 109.2 no . . . N(3) C(19) C(2) 110.8(3) yes . . . C(21) C(20) H(20) 115.9 no . . . C(21) C(20) N(3) 128.3(3) yes . . . H(20) C(20) N(3) 115.8 no . . . C(22) C(21) C(26) 119.4(4) yes . . . C(22) C(21) C(20) 124.3(4) yes . . . C(26) C(21) C(20) 116.3(3) yes . . . C(23) C(22) O(3) 119.9(3) yes . . . C(23) C(22) C(21) 116.3(4) yes . . . O(3) C(22) C(21) 123.8(3) yes . . . C(24) C(23) H(24) 118.6 no . . . C(24) C(23) C(22) 122.7(3) yes . . . H(24) C(23) C(22) 118.7 no . . . C(25) C(24) H(23) 119.6 no . . . C(25) C(24) C(23) 120.8(5) yes . . . H(23) C(24) C(23) 119.7 no . . . C(26) C(25) H(22) 120.9 no . . . C(26) C(25) C(24) 118.2(5) yes . . . H(22) C(25) C(24) 120.9 no . . . H(21) C(26) C(21) 118.7 no . . . H(21) C(26) C(25) 118.8 no . . . C(21) C(26) C(25) 122.6(4) yes . . . C(28) C(27) C(29) 117.5(3) yes . . . C(28) C(27) O(4) 113.8(4) yes . . . C(29) C(27) O(4) 128.7(4) yes . . . F(1) C(28) F(2) 103.2(5) yes . . . F(1) C(28) F(3) 106.8(4) yes . . . F(1) C(28) C(27) 111.7(5) yes . . . F(2) C(28) F(3) 107.7(6) yes . . . F(2) C(28) C(27) 111.7(4) yes . . . F(3) C(28) C(27) 114.9(5) yes . . . C(30) C(29) H(25) 119.6 no . . . C(30) C(29) C(27) 120.7(3) yes . . . H(25) C(29) C(27) 119.7 no . . . C(31) C(30) O(5) 113.8(4) yes . . . C(31) C(30) C(29) 117.9(4) yes . . . O(5) C(30) C(29) 128.3(4) yes . . . F(4) C(31) F(5) 113.5(5) yes . . . F(4) C(31) F(6) 106.1(7) yes . . . F(4) C(31) C(30) 113.9(5) yes . . . F(5) C(31) F(6) 98.4(5) yes . . . F(5) C(31) C(30) 113.8(5) yes . . . F(6) C(31) C(30) 109.8(5) yes . . . C(33) C(32) C(34) 117.7(4) yes . . . C(33) C(32) O(6) 115.8(4) yes . . . C(34) C(32) O(6) 126.6(4) yes . . . F(7) C(33) F(8) 104.0(6) yes . . . F(7) C(33) F(9) 103.1(7) yes . . . F(7) C(33) C(32) 113.6(4) yes . . . F(8) C(33) F(9) 104.1(5) yes . . . F(8) C(33) C(32) 117.2(5) yes . . . F(9) C(33) C(32) 113.4(5) yes . . . C(35) C(34) H(26) 119.6 no . . . C(35) C(34) C(32) 120.7(4) yes . . . H(26) C(34) C(32) 119.7 no . . . C(36) C(35) O(7) 113.1(4) yes . . . C(36) C(35) C(34) 118.3(4) yes . . . O(7) C(35) C(34) 128.6(4) yes . . . F(10) C(36) F(11) 106.0(6) yes . . . F(10) C(36) F(12) 106.9(5) yes . . . F(10) C(36) C(35) 111.3(5) yes . . . F(11) C(36) F(12) 105.6(6) yes . . . F(11) C(36) C(35) 112.3(5) yes . . . F(12) C(36) C(35) 114.2(5) yes . . . C(38) C(37) H(30) 108.7 no . . . C(38) C(37) H(31) 108.8 no . . . C(38) C(37) O(8) 111.7(5) yes . . . H(30) C(37) H(31) 109.5 no . . . H(30) C(37) O(8) 109.3 no . . . H(31) C(37) O(8) 108.8 no . . . H(27) C(38) H(28) 109.5 no . . . H(27) C(38) H(29) 109 no . . . H(27) C(38) C(37) 109.1 no . . . H(28) C(38) H(29) 109 no . . . H(28) C(38) C(37) 110.3 no . . . H(29) C(38) C(37) 109.0 no . . . C(40) C(39) O(9) 116.8(7) yes . . . #======END #=========================================================================== data_030226 _database_code_depnum_ccdc_archive 'CCDC 229922' #=========================================================================== # CHEMICAL DATA _chemical_formula_sum 'C54 H60 Gd N7 O13 Ni2 ' _chemical_formula_moiety 'C54 H60 Gd N7 O13 Ni2 ' _chemical_formula_weight 1289.76 _chemical_melting_point ? #=========================================================================== # CRYSTAL DATA _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 13.2245(5) _cell_length_b 13.8535(4) _cell_length_c 16.4979(5) _cell_angle_alpha 90.290(2) _cell_angle_beta 104.022(2) _cell_angle_gamma 111.761(1) _cell_volume 2708.3(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8524 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.0 _cell_measurement_temperature 296.1 #--------------------------------------------------------------------------= _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1314.00 _exptl_absorpt_coefficient_mu 1.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.821 #=========================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 40228 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.8565 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.8565 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 #=========================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10631 _reflns_number_gt 8846 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1280 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 10630 _refine_ls_number_parameters 733 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w == 1/[0.0016Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.89 _refine_diff_density_min -1.41 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 281(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Gd Gd -0.165 3.904 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Gd(1) Gd 0.32655(2) 0.11971(2) 0.74909(2) 0.01572(7) Uani 1.00 1 d . . . Ni(1) Ni 0.27478(5) 0.13334(5) 0.55270(4) 0.0178(2) Uani 1.00 1 d . . . Ni(2) Ni 0.48892(5) 0.25598(5) 0.91892(4) 0.0174(2) Uani 1.00 1 d . . . O(1) O 0.2710(3) 0.0029(3) 0.6196(2) 0.0231(9) Uani 1.00 1 d . . . O(2) O 0.2106(3) 0.1687(3) 0.6478(2) 0.0187(9) Uani 1.00 1 d . . . O(3) O 0.4247(3) 0.1905(3) 0.6469(2) 0.0190(9) Uani 1.00 1 d . . . O(4) O 0.4152(3) 0.2971(3) 0.8052(2) 0.0187(9) Uani 1.00 1 d . . . O(5) O 0.3136(3) 0.1556(3) 0.8904(2) 0.0196(9) Uani 1.00 1 d . . . O(6) O 0.4986(3) 0.1466(3) 0.8386(2) 0.0219(9) Uani 1.00 1 d . . . O(7) O 0.2883(3) -0.0465(3) 0.8149(2) 0.024(1) Uani 1.00 1 d . . . O(8) O 0.1403(3) -0.0219(3) 0.7437(2) 0.027(1) Uani 1.00 1 d . . . O(9) O 0.1213(4) -0.1606(3) 0.8121(3) 0.048(1) Uani 1.00 1 d . . . O(10) O 0.0659(4) 0.4369(4) 1.0799(4) 0.056(2) Uani 1.00 1 d . . . O(11) O -0.0594(4) 0.3661(4) 0.9132(4) 0.057(2) Uani 1.00 1 d . . . O(12) O 1.011(3) 0.625(3) 0.633(2) 0.48(2) Uiso 1.00 1 d . . . O(13) O 0.887(2) 0.544(2) 0.426(2) 0.44(2) Uiso 1.00 1 d . . . N(1) N 0.3188(4) 0.0705(3) 0.4615(3) 0.021(1) Uani 1.00 1 d . . . N(2) N 0.1184(4) 0.1028(3) 0.4723(3) 0.019(1) Uani 1.00 1 d . . . N(3) N 0.3299(4) 0.2707(3) 0.4968(3) 0.020(1) Uani 1.00 1 d . . . N(4) N 0.6358(4) 0.3816(3) 0.9241(3) 0.020(1) Uani 1.00 1 d . . . N(5) N 0.4654(4) 0.3416(3) 1.0078(3) 0.019(1) Uani 1.00 1 d . . . N(6) N 0.5814(4) 0.2046(4) 1.0158(3) 0.020(1) Uani 1.00 1 d . . . N(7) N 0.1814(4) -0.0795(4) 0.7914(3) 0.028(1) Uani 1.00 1 d . . . C(1) C 0.1878(5) 0.1721(5) 0.2683(3) 0.030(1) Uani 1.00 1 d . . . C(2) C 0.2187(5) 0.1615(4) 0.3623(3) 0.023(1) Uani 1.00 1 d . . . C(3) C 0.3131(5) 0.1189(4) 0.3817(3) 0.023(1) Uani 1.00 1 d . . . C(4) C 0.3449(4) -0.0101(4) 0.4641(3) 0.022(1) Uani 1.00 1 d . . . C(5) C 0.3443(4) -0.0791(4) 0.5305(3) 0.022(1) Uani 1.00 1 d . . . C(6) C 0.3029(5) -0.0734(4) 0.6012(3) 0.023(1) Uani 1.00 1 d . . . C(7) C 0.2934(6) -0.1566(5) 0.6522(4) 0.032(2) Uani 1.00 1 d . . . C(8) C 0.3273(6) -0.2349(5) 0.6353(4) 0.033(2) Uani 1.00 1 d . . . C(9) C 0.3681(5) -0.2400(5) 0.5677(4) 0.033(2) Uani 1.00 1 d . . . C(10) C 0.3764(5) -0.1622(4) 0.5149(4) 0.025(1) Uani 1.00 1 d . . . C(11) C 0.1115(5) 0.0808(5) 0.3840(3) 0.026(1) Uani 1.00 1 d . . . C(12) C 0.0394(4) 0.1297(4) 0.4858(4) 0.025(1) Uani 1.00 1 d . . . C(13) C 0.0328(4) 0.1670(4) 0.5668(3) 0.023(1) Uani 1.00 1 d . . . C(14) C 0.1163(4) 0.1855(4) 0.6431(3) 0.021(1) Uani 1.00 1 d . . . C(15) C 0.1007(5) 0.2240(4) 0.7149(4) 0.026(1) Uani 1.00 1 d . . . C(16) C 0.0040(5) 0.2440(5) 0.7122(4) 0.033(2) Uani 1.00 1 d . . . C(17) C -0.0768(5) 0.2294(6) 0.6364(4) 0.039(2) Uani 1.00 1 d . . . C(18) C -0.0621(5) 0.1915(5) 0.5665(4) 0.030(2) Uani 1.00 1 d . . . C(19) C 0.2574(4) 0.2680(4) 0.4137(3) 0.022(1) Uani 1.00 1 d . . . C(20) C 0.4320(4) 0.3367(4) 0.5155(3) 0.021(1) Uani 1.00 1 d . . . C(21) C 0.5248(4) 0.3421(4) 0.5858(3) 0.019(1) Uani 1.00 1 d . . . C(22) C 0.5192(4) 0.2678(4) 0.6457(3) 0.019(1) Uani 1.00 1 d . . . C(23) C 0.6208(4) 0.2784(4) 0.7032(3) 0.021(1) Uani 1.00 1 d . . . C(24) C 0.7234(4) 0.3584(4) 0.7038(3) 0.024(1) Uani 1.00 1 d . . . C(25) C 0.7280(5) 0.4314(4) 0.6469(4) 0.027(1) Uani 1.00 1 d . . . C(26) C 0.6290(5) 0.4221(4) 0.5885(3) 0.023(1) Uani 1.00 1 d . . . C(27) C 0.7572(5) 0.4551(5) 1.1583(3) 0.029(1) Uani 1.00 1 d . . . C(28) C 0.6683(5) 0.3877(4) 1.0791(3) 0.023(1) Uani 1.00 1 d . . . C(29) C 0.7239(5) 0.4060(4) 1.0038(3) 0.024(1) Uani 1.00 1 d . . . C(30) C 0.6491(4) 0.4538(4) 0.8735(3) 0.019(1) Uani 1.00 1 d . . . C(31) C 0.5638(4) 0.4607(4) 0.8018(3) 0.019(1) Uani 1.00 1 d . . . C(32) C 0.4523(4) 0.3887(4) 0.7734(3) 0.018(1) Uani 1.00 1 d . . . C(33) C 0.3753(4) 0.4138(4) 0.7116(3) 0.019(1) Uani 1.00 1 d . . . C(34) C 0.4085(5) 0.5090(4) 0.6781(3) 0.023(1) Uani 1.00 1 d . . . C(35) C 0.5201(5) 0.5803(4) 0.7050(3) 0.023(1) Uani 1.00 1 d . . . C(36) C 0.5972(5) 0.5557(4) 0.7647(3) 0.022(1) Uani 1.00 1 d . . . C(37) C 0.5685(4) 0.4232(4) 1.0616(3) 0.024(1) Uani 1.00 1 d . . . C(38) C 0.3741(5) 0.3208(4) 1.0309(3) 0.024(1) Uani 1.00 1 d . . . C(39) C 0.2640(4) 0.2437(4) 0.9923(3) 0.022(1) Uani 1.00 1 d . . . C(40) C 0.2378(4) 0.1659(4) 0.9254(3) 0.020(1) Uani 1.00 1 d . . . C(41) C 0.1226(4) 0.0927(4) 0.8991(3) 0.023(1) Uani 1.00 1 d . . . C(42) C 0.0416(5) 0.0976(5) 0.9359(4) 0.028(1) Uani 1.00 1 d . . . C(43) C 0.0682(5) 0.1717(5) 1.0032(4) 0.031(2) Uani 1.00 1 d . . . C(44) C 0.1778(5) 0.2423(4) 1.0307(4) 0.025(1) Uani 1.00 1 d . . . C(45) C 0.6271(5) 0.2719(4) 1.0958(3) 0.024(1) Uani 1.00 1 d . . . C(46) C 0.6228(5) 0.1353(4) 1.0102(3) 0.024(1) Uani 1.00 1 d . . . C(47) C 0.6044(4) 0.0675(4) 0.9359(3) 0.021(1) Uani 1.00 1 d . . . C(48) C 0.5452(4) 0.0762(4) 0.8545(3) 0.020(1) Uani 1.00 1 d . . . C(49) C 0.5404(5) 0.0101(4) 0.7877(4) 0.027(1) Uani 1.00 1 d . . . C(50) C 0.5886(5) -0.0631(5) 0.8002(4) 0.028(2) Uani 1.00 1 d . . . C(51) C 0.6467(5) -0.0726(5) 0.8801(4) 0.030(2) Uani 1.00 1 d . . . C(52) C 0.6551(5) -0.0067(5) 0.9465(4) 0.029(2) Uani 1.00 1 d . . . C(53) C 0.0395(7) 0.3865(7) 1.1466(6) 0.061(3) Uani 1.00 1 d . . . C(54) C -0.1493(6) 0.2631(5) 0.8997(5) 0.040(2) Uani 1.00 1 d . . . H(1) H 0.1538 0.2220 0.2585 0.032 Uiso 1.00 1 c . . . H(2) H 0.2541 0.1945 0.2490 0.032 Uiso 1.00 1 c . . . H(3) H 0.1363 0.1065 0.2389 0.032 Uiso 1.00 1 c . . . H(4) H 0.3833 0.1748 0.3857 0.027 Uiso 1.00 1 c . . . H(5) H 0.2991 0.0679 0.3373 0.027 Uiso 1.00 1 c . . . H(6) H 0.3673 -0.0268 0.4171 0.025 Uiso 1.00 1 c . . . H(7) H 0.4042 -0.1647 0.4673 0.030 Uiso 1.00 1 c . . . H(8) H 0.3902 -0.2957 0.5572 0.040 Uiso 1.00 1 c . . . H(9) H 0.3224 -0.2878 0.6724 0.040 Uiso 1.00 1 c . . . H(10) H 0.2628 -0.1582 0.6989 0.042 Uiso 1.00 1 c . . . H(11) H 0.1083 0.0120 0.3743 0.029 Uiso 1.00 1 c . . . H(12) H 0.0456 0.0868 0.3496 0.029 Uiso 1.00 1 c . . . H(13) H -0.0204 0.1245 0.4383 0.026 Uiso 1.00 1 c . . . H(14) H -0.1179 0.1807 0.5149 0.035 Uiso 1.00 1 c . . . H(15) H -0.1409 0.2460 0.6339 0.048 Uiso 1.00 1 c . . . H(16) H -0.0067 0.2676 0.7624 0.041 Uiso 1.00 1 c . . . H(17) H 0.1566 0.2369 0.7667 0.031 Uiso 1.00 1 c . . . H(18) H 0.1931 0.2794 0.4200 0.025 Uiso 1.00 1 c . . . H(19) H 0.2982 0.3216 0.3848 0.024 Uiso 1.00 1 c . . . H(20) H 0.4492 0.3892 0.4785 0.025 Uiso 1.00 1 c . . . H(21) H 0.6319 0.4719 0.5489 0.028 Uiso 1.00 1 c . . . H(22) H 0.7974 0.4867 0.6476 0.030 Uiso 1.00 1 c . . . H(23) H 0.7905 0.3627 0.7437 0.027 Uiso 1.00 1 c . . . H(24) H 0.6199 0.2292 0.7432 0.026 Uiso 1.00 1 c . . . H(25) H 0.8151 0.4285 1.1749 0.032 Uiso 1.00 1 c . . . H(26) H 0.7891 0.5252 1.1460 0.032 Uiso 1.00 1 c . . . H(27) H 0.7222 0.4529 1.2025 0.032 Uiso 1.00 1 c . . . H(28) H 0.7647 0.3620 1.0046 0.028 Uiso 1.00 1 c . . . H(29) H 0.7741 0.4770 1.0088 0.028 Uiso 1.00 1 c . . . H(30) H 0.7220 0.5079 0.8844 0.023 Uiso 1.00 1 c . . . H(31) H 0.6738 0.6031 0.7814 0.027 Uiso 1.00 1 c . . . H(32) H 0.5429 0.6454 0.6821 0.028 Uiso 1.00 1 c . . . H(33) H 0.3551 0.5256 0.6369 0.028 Uiso 1.00 1 c . . . H(34) H 0.2995 0.3652 0.6924 0.024 Uiso 1.00 1 c . . . H(35) H 0.5869 0.4851 1.0341 0.028 Uiso 1.00 1 c . . . H(36) H 0.5546 0.4371 1.1135 0.028 Uiso 1.00 1 c . . . H(37) H 0.3803 0.3616 1.0797 0.029 Uiso 1.00 1 c . . . H(38) H 0.1971 0.2921 1.0774 0.032 Uiso 1.00 1 c . . . H(39) H 0.0121 0.1736 1.0291 0.040 Uiso 1.00 1 c . . . H(40) H -0.0341 0.0494 0.9150 0.035 Uiso 1.00 1 c . . . H(41) H 0.1018 0.0393 0.8548 0.025 Uiso 1.00 1 c . . . H(42) H 0.5699 0.2578 1.1246 0.029 Uiso 1.00 1 c . . . H(43) H 0.6886 0.2580 1.1293 0.029 Uiso 1.00 1 c . . . H(44) H 0.6711 0.1273 1.0603 0.030 Uiso 1.00 1 c . . . H(45) H 0.6964 -0.0114 1.0011 0.037 Uiso 1.00 1 c . . . H(46) H 0.6797 -0.1233 0.8887 0.041 Uiso 1.00 1 c . . . H(47) H 0.5820 -0.1077 0.7537 0.036 Uiso 1.00 1 c . . . H(48) H 0.5028 0.0160 0.7322 0.032 Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Gd(1) 0.0164(1) 0.0158(1) 0.0138(1) 0.0070(1) 0.00039(9) 0.00179(9) Ni(1) 0.0184(3) 0.0180(3) 0.0141(3) 0.0058(3) 0.0010(3) 0.0021(3) Ni(2) 0.0176(3) 0.0191(3) 0.0151(3) 0.0088(3) 0.0010(3) 0.0014(3) O(1) 0.028(2) 0.020(2) 0.021(2) 0.011(2) 0.003(2) 0.001(2) O(2) 0.015(2) 0.024(2) 0.018(2) 0.011(1) 0.001(1) 0.005(2) O(3) 0.015(2) 0.023(2) 0.018(2) 0.006(1) 0.003(1) 0.002(2) O(4) 0.018(2) 0.015(2) 0.019(2) 0.006(1) -0.001(1) 0.001(1) O(5) 0.016(2) 0.021(2) 0.020(2) 0.006(1) 0.003(1) 0.002(2) O(6) 0.022(2) 0.029(2) 0.017(2) 0.019(2) -0.005(1) -0.001(2) O(7) 0.022(2) 0.025(2) 0.025(2) 0.012(2) -0.001(2) -0.001(2) O(8) 0.028(2) 0.033(2) 0.019(2) 0.012(2) 0.002(2) 0.006(2) O(9) 0.040(3) 0.029(2) 0.068(3) 0.001(2) 0.023(2) 0.027(2) O(10) 0.044(3) 0.060(3) 0.056(3) 0.013(3) 0.008(3) 0.007(3) O(11) 0.044(3) 0.050(3) 0.071(4) 0.011(2) 0.013(3) 0.034(3) N(1) 0.023(2) 0.022(2) 0.015(2) 0.006(2) 0.001(2) -0.001(2) N(2) 0.016(2) 0.018(2) 0.014(2) -0.000(2) -0.000(2) 0.007(2) N(3) 0.021(2) 0.022(2) 0.016(2) 0.009(2) 0.001(2) -0.000(2) N(4) 0.017(2) 0.021(2) 0.020(2) 0.009(2) 0.004(2) 0.003(2) N(5) 0.016(2) 0.021(2) 0.020(2) 0.008(2) 0.002(2) 0.000(2) N(6) 0.020(2) 0.029(2) 0.012(2) 0.013(2) -0.002(2) 0.002(2) N(7) 0.032(3) 0.023(2) 0.024(2) 0.005(2) 0.007(2) 0.005(2) C(1) 0.031(3) 0.033(3) 0.015(3) 0.007(3) -0.005(2) -0.003(2) C(2) 0.026(3) 0.025(3) 0.008(2) 0.004(2) -0.001(2) 0.004(2) C(3) 0.029(3) 0.022(3) 0.016(2) 0.008(2) 0.004(2) 0.001(2) C(4) 0.018(3) 0.023(3) 0.022(3) 0.005(2) 0.005(2) 0.003(2) C(5) 0.020(3) 0.021(3) 0.023(3) 0.006(2) 0.004(2) 0.000(2) C(6) 0.025(3) 0.015(2) 0.022(3) 0.007(2) -0.001(2) -0.004(2) C(7) 0.056(4) 0.024(3) 0.024(3) 0.019(3) 0.018(3) 0.011(3) C(8) 0.054(4) 0.024(3) 0.023(3) 0.017(3) 0.009(3) 0.010(3) C(9) 0.035(3) 0.031(3) 0.033(3) 0.021(3) -0.004(3) -0.007(3) C(10) 0.021(3) 0.028(3) 0.025(3) 0.012(2) 0.004(2) 0.003(2) C(11) 0.020(3) 0.035(3) 0.018(3) 0.010(2) -0.003(2) -0.002(2) C(12) 0.016(3) 0.023(3) 0.027(3) 0.003(2) -0.000(2) 0.001(2) C(13) 0.014(3) 0.020(3) 0.026(3) 0.003(2) -0.001(2) 0.004(2) C(14) 0.024(3) 0.013(2) 0.023(3) 0.003(2) 0.011(2) 0.009(2) C(15) 0.021(3) 0.030(3) 0.027(3) 0.012(2) 0.004(2) -0.001(2) C(16) 0.023(3) 0.042(4) 0.038(3) 0.016(3) 0.008(3) -0.004(3) C(17) 0.022(3) 0.057(4) 0.041(4) 0.020(3) 0.006(3) -0.002(3) C(18) 0.020(3) 0.036(3) 0.031(3) 0.009(2) 0.003(2) 0.008(3) C(19) 0.021(3) 0.019(2) 0.021(3) 0.003(2) 0.005(2) 0.010(2) C(20) 0.021(3) 0.018(2) 0.023(3) 0.006(2) 0.003(2) -0.005(2) C(21) 0.023(3) 0.016(2) 0.018(2) 0.009(2) 0.003(2) -0.001(2) C(22) 0.020(3) 0.020(2) 0.017(2) 0.008(2) 0.003(2) -0.004(2) C(23) 0.022(3) 0.024(3) 0.018(2) 0.010(2) 0.006(2) 0.006(2) C(24) 0.016(3) 0.031(3) 0.021(3) 0.006(2) 0.003(2) 0.002(2) C(25) 0.018(3) 0.027(3) 0.030(3) 0.004(2) 0.005(2) -0.003(3) C(26) 0.026(3) 0.024(3) 0.020(3) 0.012(2) 0.004(2) -0.003(2) C(27) 0.024(3) 0.035(3) 0.022(3) 0.012(3) -0.007(2) -0.010(3) C(28) 0.026(3) 0.027(3) 0.017(2) 0.016(2) -0.001(2) -0.006(2) C(29) 0.019(3) 0.027(3) 0.025(3) 0.009(2) 0.001(2) 0.000(2) C(30) 0.020(3) 0.021(2) 0.017(2) 0.007(2) 0.010(2) 0.009(2) C(31) 0.023(3) 0.019(2) 0.018(2) 0.009(2) 0.008(2) 0.005(2) C(32) 0.018(3) 0.023(3) 0.017(2) 0.011(2) 0.003(2) -0.001(2) C(33) 0.022(3) 0.018(2) 0.020(2) 0.008(2) 0.009(2) 0.006(2) C(34) 0.026(3) 0.023(3) 0.021(3) 0.012(2) 0.005(2) 0.010(2) C(35) 0.030(3) 0.018(2) 0.021(3) 0.008(2) 0.010(2) 0.008(2) C(36) 0.022(3) 0.023(3) 0.021(3) 0.009(2) 0.006(2) 0.001(2) C(37) 0.019(3) 0.026(3) 0.025(3) 0.010(2) -0.003(2) -0.009(2) C(38) 0.028(3) 0.023(3) 0.022(3) 0.014(2) 0.006(2) -0.002(2) C(39) 0.022(3) 0.022(3) 0.023(3) 0.011(2) 0.006(2) 0.009(2) C(40) 0.018(3) 0.024(3) 0.020(2) 0.010(2) 0.005(2) 0.009(2) C(41) 0.024(3) 0.016(2) 0.024(3) 0.002(2) 0.008(2) 0.006(2) C(42) 0.020(3) 0.033(3) 0.034(3) 0.010(2) 0.010(2) 0.007(3) C(43) 0.024(3) 0.037(3) 0.038(3) 0.017(3) 0.011(3) 0.002(3) C(44) 0.025(3) 0.027(3) 0.028(3) 0.011(2) 0.013(2) 0.007(2) C(45) 0.028(3) 0.032(3) 0.013(2) 0.018(2) -0.005(2) 0.001(2) C(46) 0.030(3) 0.026(3) 0.019(2) 0.016(2) 0.002(2) 0.010(2) C(47) 0.021(3) 0.024(3) 0.020(2) 0.013(2) 0.003(2) 0.006(2) C(48) 0.022(3) 0.016(2) 0.026(3) 0.010(2) 0.009(2) 0.008(2) C(49) 0.027(3) 0.029(3) 0.024(3) 0.013(2) 0.006(2) 0.005(2) C(50) 0.034(3) 0.028(3) 0.028(3) 0.016(3) 0.012(3) 0.003(3) C(51) 0.040(3) 0.027(3) 0.035(3) 0.021(3) 0.017(3) 0.015(3) C(52) 0.037(3) 0.030(3) 0.027(3) 0.020(3) 0.007(3) 0.012(3) C(53) 0.065(6) 0.060(5) 0.069(6) 0.022(4) 0.037(5) 0.020(5) C(54) 0.036(4) 0.027(3) 0.055(4) 0.007(3) 0.014(3) 0.006(3) #=========================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Gd(1) Ni(1) 3.1669(7) yes . . Gd(1) Ni(2) 3.1702(6) yes . . Gd(1) O(1) 2.459(4) yes . . Gd(1) O(2) 2.268(4) yes . . Gd(1) O(3) 2.372(4) yes . . Gd(1) O(4) 2.364(3) yes . . Gd(1) O(5) 2.441(4) yes . . Gd(1) O(6) 2.288(4) yes . . Gd(1) O(7) 2.483(4) yes . . Gd(1) O(8) 2.497(4) yes . . Ni(1) O(1) 2.114(4) yes . . Ni(1) O(2) 2.090(4) yes . . Ni(1) O(3) 2.074(3) yes . . Ni(1) N(1) 2.037(5) yes . . Ni(1) N(2) 2.057(4) yes . . Ni(1) N(3) 2.078(4) yes . . Ni(2) O(4) 2.081(4) yes . . Ni(2) O(5) 2.146(3) yes . . Ni(2) O(6) 2.068(4) yes . . Ni(2) N(4) 2.054(4) yes . . Ni(2) N(5) 2.033(5) yes . . Ni(2) N(6) 2.065(5) yes . . O(1) C(6) 1.332(8) yes . . O(2) C(14) 1.336(8) yes . . O(3) C(22) 1.315(6) yes . . O(4) C(32) 1.341(6) yes . . O(5) C(40) 1.320(8) yes . . O(6) C(48) 1.329(8) yes . . O(7) N(7) 1.270(6) yes . . O(8) N(7) 1.294(7) yes . . O(9) N(7) 1.218(6) yes . . O(10) C(53) 1.35(1) yes . . O(11) C(54) 1.453(7) yes . . N(1) C(3) 1.479(7) yes . . N(1) C(4) 1.283(8) yes . . N(2) C(11) 1.461(7) yes . . N(2) C(12) 1.296(9) yes . . N(3) C(19) 1.461(6) yes . . N(3) C(20) 1.279(6) yes . . N(4) C(29) 1.471(6) yes . . N(4) C(30) 1.294(7) yes . . N(5) C(37) 1.478(6) yes . . N(5) C(38) 1.285(8) yes . . N(6) C(45) 1.470(6) yes . . N(6) C(46) 1.282(9) yes . . C(1) C(2) 1.529(7) yes . . C(1) H(1) 0.95 no . . C(1) H(2) 0.950 no . . C(1) H(3) 0.950 no . . C(2) C(3) 1.54(1) yes . . C(2) C(11) 1.569(7) yes . . C(2) C(19) 1.541(8) yes . . C(3) H(4) 0.950 no . . C(3) H(5) 0.950 no . . C(4) C(5) 1.458(8) yes . . C(4) H(6) 0.950 no . . C(5) C(6) 1.417(9) yes . . C(5) C(10) 1.41(1) yes . . C(6) C(7) 1.417(8) yes . . C(7) C(8) 1.37(1) yes . . C(7) H(10) 0.95 no . . C(8) C(9) 1.36(1) yes . . C(8) H(9) 0.950 no . . C(9) C(10) 1.378(9) yes . . C(9) H(8) 0.95 no . . C(10) H(7) 0.950 no . . C(11) H(11) 0.950 no . . C(11) H(12) 0.950 no . . C(12) C(13) 1.463(9) yes . . C(12) H(13) 0.950 no . . C(13) C(14) 1.408(7) yes . . C(13) C(18) 1.42(1) yes . . C(14) C(15) 1.387(9) yes . . C(15) C(16) 1.40(1) yes . . C(15) H(17) 0.950 no . . C(16) C(17) 1.391(8) yes . . C(16) H(16) 0.95 no . . C(17) C(18) 1.35(1) yes . . C(17) H(15) 0.95 no . . C(18) H(14) 0.950 no . . C(19) H(18) 0.950 no . . C(19) H(19) 0.950 no . . C(20) C(21) 1.448(7) yes . . C(20) H(20) 0.950 no . . C(21) C(22) 1.425(8) yes . . C(21) C(26) 1.402(7) yes . . C(22) C(23) 1.400(7) yes . . C(23) C(24) 1.395(7) yes . . C(23) H(24) 0.950 no . . C(24) C(25) 1.378(8) yes . . C(24) H(23) 0.950 no . . C(25) C(26) 1.386(8) yes . . C(25) H(22) 0.950 no . . C(26) H(21) 0.950 no . . C(27) C(28) 1.545(6) yes . . C(27) H(25) 0.95 no . . C(27) H(26) 0.950 no . . C(27) H(27) 0.950 no . . C(28) C(29) 1.568(9) yes . . C(28) C(37) 1.54(1) yes . . C(28) C(45) 1.541(8) yes . . C(29) H(28) 0.95 no . . C(29) H(29) 0.950 no . . C(30) C(31) 1.454(7) yes . . C(30) H(30) 0.950 no . . C(31) C(32) 1.399(6) yes . . C(31) C(36) 1.417(8) yes . . C(32) C(33) 1.400(8) yes . . C(33) C(34) 1.391(7) yes . . C(33) H(34) 0.950 no . . C(34) C(35) 1.395(7) yes . . C(34) H(33) 0.950 no . . C(35) C(36) 1.380(8) yes . . C(35) H(32) 0.950 no . . C(36) H(31) 0.950 no . . C(37) H(35) 0.950 no . . C(37) H(36) 0.950 no . . C(38) C(39) 1.435(6) yes . . C(38) H(37) 0.950 no . . C(39) C(40) 1.424(8) yes . . C(39) C(44) 1.426(9) yes . . C(40) C(41) 1.439(6) yes . . C(41) C(42) 1.37(1) yes . . C(41) H(41) 0.950 no . . C(42) C(43) 1.393(9) yes . . C(42) H(40) 0.950 no . . C(43) C(44) 1.374(7) yes . . C(43) H(39) 0.95 no . . C(44) H(38) 0.950 no . . C(45) H(42) 0.950 no . . C(45) H(43) 0.950 no . . C(46) C(47) 1.455(8) yes . . C(46) H(44) 0.950 no . . C(47) C(48) 1.413(7) yes . . C(47) C(52) 1.41(1) yes . . C(48) C(49) 1.404(9) yes . . C(49) C(50) 1.38(1) yes . . C(49) H(48) 0.950 no . . C(50) C(51) 1.389(8) yes . . C(50) H(47) 0.950 no . . C(51) C(52) 1.379(9) yes . . C(51) H(46) 0.95 no . . C(52) H(45) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Ni(1) O(2) 82.3(2) yes . . . O(1) Ni(1) O(3) 76.5(1) yes . . . O(1) Ni(1) N(1) 89.0(2) yes . . . O(1) Ni(1) N(2) 109.6(1) yes . . . O(1) Ni(1) N(3) 162.8(2) yes . . . O(1) Ni(1) Gd(1) 50.9(1) yes . . . O(2) Ni(1) O(3) 82.2(1) yes . . . O(2) Ni(1) N(1) 169.2(2) yes . . . O(2) Ni(1) N(2) 86.9(2) yes . . . O(2) Ni(1) N(3) 105.3(2) yes . . . O(2) Ni(1) Gd(1) 45.6(1) yes . . . O(3) Ni(1) N(1) 102.1(2) yes . . . O(3) Ni(1) N(2) 166.7(2) yes . . . O(3) Ni(1) N(3) 89.2(1) yes . . . O(3) Ni(1) Gd(1) 48.5(1) yes . . . N(1) Ni(1) N(2) 89.9(2) yes . . . N(1) Ni(1) N(3) 84.7(2) yes . . . N(1) Ni(1) Gd(1) 131.2(1) yes . . . N(2) Ni(1) N(3) 86.4(2) yes . . . N(2) Ni(1) Gd(1) 125.9(1) yes . . . N(3) Ni(1) Gd(1) 124.6(1) yes . . . O(4) Ni(2) O(5) 74.9(1) yes . . . O(4) Ni(2) O(6) 81.2(2) yes . . . O(4) Ni(2) N(4) 89.0(2) yes . . . O(4) Ni(2) N(5) 104.6(2) yes . . . O(4) Ni(2) N(6) 167.1(2) yes . . . O(4) Ni(2) Gd(1) 48.20(9) yes . . . O(5) Ni(2) O(6) 84.1(1) yes . . . O(5) Ni(2) N(4) 161.9(2) yes . . . O(5) Ni(2) N(5) 89.4(2) yes . . . O(5) Ni(2) N(6) 110.2(2) yes . . . O(5) Ni(2) Gd(1) 50.3(1) yes . . . O(6) Ni(2) N(4) 101.7(2) yes . . . O(6) Ni(2) N(5) 169.9(2) yes . . . O(6) Ni(2) N(6) 87.5(2) yes . . . O(6) Ni(2) Gd(1) 46.1(1) yes . . . N(4) Ni(2) N(5) 86.8(2) yes . . . N(4) Ni(2) N(6) 87.2(2) yes . . . N(4) Ni(2) Gd(1) 123.1(1) yes . . . N(5) Ni(2) N(6) 87.5(2) yes . . . N(5) Ni(2) Gd(1) 132.7(1) yes . . . N(6) Ni(2) Gd(1) 125.5(1) yes . . . C(6) O(1) Gd(1) 131.4(3) yes . . . C(6) O(1) Ni(1) 127.2(4) yes . . . Ni(1) O(1) Gd(1) 87.3(1) yes . . . C(14) O(2) Gd(1) 134.3(3) yes . . . C(14) O(2) Ni(1) 130.3(3) yes . . . Ni(1) O(2) Gd(1) 93.1(2) yes . . . C(22) O(3) Gd(1) 136.5(3) yes . . . C(22) O(3) Ni(1) 127.9(3) yes . . . Ni(1) O(3) Gd(1) 90.6(1) yes . . . C(32) O(4) Gd(1) 135.2(3) yes . . . C(32) O(4) Ni(2) 127.5(3) yes . . . Ni(2) O(4) Gd(1) 90.8(1) yes . . . C(40) O(5) Gd(1) 137.4(3) yes . . . C(40) O(5) Ni(2) 126.2(3) yes . . . Ni(2) O(5) Gd(1) 87.2(1) yes . . . C(48) O(6) Gd(1) 126.4(3) yes . . . C(48) O(6) Ni(2) 130.6(3) yes . . . Ni(2) O(6) Gd(1) 93.3(2) yes . . . N(7) O(7) Gd(1) 96.9(3) yes . . . N(7) O(8) Gd(1) 95.5(3) yes . . . C(3) N(1) C(4) 116.4(5) yes . . . C(3) N(1) Ni(1) 116.5(4) yes . . . C(4) N(1) Ni(1) 127.0(4) yes . . . C(11) N(2) C(12) 115.3(5) yes . . . C(11) N(2) Ni(1) 114.3(4) yes . . . C(12) N(2) Ni(1) 127.1(3) yes . . . C(19) N(3) C(20) 118.2(4) yes . . . C(19) N(3) Ni(1) 113.8(3) yes . . . C(20) N(3) Ni(1) 124.0(4) yes . . . C(29) N(4) C(30) 116.0(4) yes . . . C(29) N(4) Ni(2) 115.8(3) yes . . . C(30) N(4) Ni(2) 126.3(3) yes . . . C(37) N(5) C(38) 116.6(5) yes . . . C(37) N(5) Ni(2) 116.0(4) yes . . . C(38) N(5) Ni(2) 126.3(3) yes . . . C(45) N(6) C(46) 115.6(5) yes . . . C(45) N(6) Ni(2) 115.3(4) yes . . . C(46) N(6) Ni(2) 127.4(4) yes . . . O(7) N(7) O(8) 115.8(4) yes . . . O(7) N(7) O(9) 122.2(5) yes . . . O(8) N(7) O(9) 122.1(5) yes . . . C(2) C(1) H(1) 109.6 no . . . C(2) C(1) H(2) 109.3 no . . . C(2) C(1) H(3) 109.5 no . . . H(1) C(1) H(2) 109.5 no . . . H(1) C(1) H(3) 109.5 no . . . H(2) C(1) H(3) 109.5 no . . . C(3) C(2) C(11) 109.0(5) yes . . . C(3) C(2) C(19) 110.5(4) yes . . . C(3) C(2) C(1) 108.7(5) yes . . . C(11) C(2) C(19) 110.2(5) yes . . . C(11) C(2) C(1) 107.9(4) yes . . . C(19) C(2) C(1) 110.5(5) yes . . . H(4) C(3) H(5) 109.5 no . . . H(4) C(3) N(1) 108.9 no . . . H(4) C(3) C(2) 108.9 no . . . H(5) C(3) N(1) 109.0 no . . . H(5) C(3) C(2) 108.9 no . . . N(1) C(3) C(2) 111.6(5) yes . . . C(5) C(4) H(6) 116.1 no . . . C(5) C(4) N(1) 127.8(6) yes . . . H(6) C(4) N(1) 116.1 no . . . C(6) C(5) C(10) 120.6(5) yes . . . C(6) C(5) C(4) 124.4(6) yes . . . C(10) C(5) C(4) 114.6(5) yes . . . C(7) C(6) O(1) 120.1(6) yes . . . C(7) C(6) C(5) 116.1(6) yes . . . O(1) C(6) C(5) 123.8(5) yes . . . C(8) C(7) H(10) 119.4 no . . . C(8) C(7) C(6) 121.2(6) yes . . . H(10) C(7) C(6) 119.4 no . . . C(9) C(8) H(9) 118.7 no . . . C(9) C(8) C(7) 122.6(6) yes . . . H(9) C(8) C(7) 118.7 no . . . C(10) C(9) H(8) 120.8 no . . . C(10) C(9) C(8) 118.3(7) yes . . . H(8) C(9) C(8) 120.8 no . . . H(7) C(10) C(5) 119.5 no . . . H(7) C(10) C(9) 119.5 no . . . C(5) C(10) C(9) 121.1(6) yes . . . H(11) C(11) H(12) 109.5 no . . . H(11) C(11) N(2) 109.6 no . . . H(11) C(11) C(2) 109.5 no . . . H(12) C(11) N(2) 109.6 no . . . H(12) C(11) C(2) 109.6 no . . . N(2) C(11) C(2) 109.1(4) yes . . . C(13) C(12) H(13) 116.7 no . . . C(13) C(12) N(2) 126.7(5) yes . . . H(13) C(12) N(2) 116.6 no . . . C(14) C(13) C(18) 118.2(6) yes . . . C(14) C(13) C(12) 124.9(6) yes . . . C(18) C(13) C(12) 116.8(5) yes . . . C(15) C(14) O(2) 119.3(4) yes . . . C(15) C(14) C(13) 118.9(6) yes . . . O(2) C(14) C(13) 121.8(5) yes . . . C(16) C(15) H(17) 119.5 no . . . C(16) C(15) C(14) 121.0(5) yes . . . H(17) C(15) C(14) 119.6 no . . . C(17) C(16) H(16) 119.8 no . . . C(17) C(16) C(15) 120.4(7) yes . . . H(16) C(16) C(15) 119.8 no . . . C(18) C(17) H(15) 120.6 no . . . C(18) C(17) C(16) 118.8(7) yes . . . H(15) C(17) C(16) 120.6 no . . . H(14) C(18) C(13) 118.6 no . . . H(14) C(18) C(17) 118.7 no . . . C(13) C(18) C(17) 122.7(5) yes . . . H(18) C(19) H(19) 109.5 no . . . H(18) C(19) N(3) 109.1 no . . . H(18) C(19) C(2) 109.2 no . . . H(19) C(19) N(3) 109.1 no . . . H(19) C(19) C(2) 109.1 no . . . N(3) C(19) C(2) 110.7(5) yes . . . C(21) C(20) H(20) 115.8 no . . . C(21) C(20) N(3) 128.6(5) yes . . . H(20) C(20) N(3) 115.7 no . . . C(22) C(21) C(26) 119.3(5) yes . . . C(22) C(21) C(20) 124.9(4) yes . . . C(26) C(21) C(20) 115.6(5) yes . . . C(23) C(22) O(3) 120.4(5) yes . . . C(23) C(22) C(21) 116.9(4) yes . . . O(3) C(22) C(21) 122.7(4) yes . . . C(24) C(23) H(24) 118.7 no . . . C(24) C(23) C(22) 122.5(5) yes . . . H(24) C(23) C(22) 118.8 no . . . C(25) C(24) H(23) 119.7 no . . . C(25) C(24) C(23) 120.4(5) yes . . . H(23) C(24) C(23) 119.9 no . . . C(26) C(25) H(22) 120.8 no . . . C(26) C(25) C(24) 118.4(5) yes . . . H(22) C(25) C(24) 120.8 no . . . H(21) C(26) C(21) 118.8 no . . . H(21) C(26) C(25) 118.7 no . . . C(21) C(26) C(25) 122.5(5) yes . . . C(28) C(27) H(25) 109.5 no . . . C(28) C(27) H(26) 109.5 no . . . C(28) C(27) H(27) 109.4 no . . . H(25) C(27) H(26) 109.5 no . . . H(25) C(27) H(27) 109.5 no . . . H(26) C(27) H(27) 109.5 no . . . C(29) C(28) C(37) 110.3(5) yes . . . C(29) C(28) C(45) 111.5(5) yes . . . C(29) C(28) C(27) 108.3(4) yes . . . C(37) C(28) C(45) 109.4(4) yes . . . C(37) C(28) C(27) 107.9(5) yes . . . C(45) C(28) C(27) 109.3(4) yes . . . H(28) C(29) H(29) 109.4 no . . . H(28) C(29) N(4) 109.4 no . . . H(28) C(29) C(28) 109.4 no . . . H(29) C(29) N(4) 109.4 no . . . H(29) C(29) C(28) 109.4 no . . . N(4) C(29) C(28) 109.7(4) yes . . . C(31) C(30) H(30) 116.6 no . . . C(31) C(30) N(4) 126.7(4) yes . . . H(30) C(30) N(4) 116.7 no . . . C(32) C(31) C(36) 119.0(5) yes . . . C(32) C(31) C(30) 126.2(5) yes . . . C(36) C(31) C(30) 114.5(4) yes . . . C(33) C(32) O(4) 118.4(4) yes . . . C(33) C(32) C(31) 119.4(5) yes . . . O(4) C(32) C(31) 122.1(5) yes . . . C(34) C(33) H(34) 119.6 no . . . C(34) C(33) C(32) 120.8(4) yes . . . H(34) C(33) C(32) 119.6 no . . . C(35) C(34) H(33) 120.0 no . . . C(35) C(34) C(33) 120.1(5) yes . . . H(33) C(34) C(33) 119.9 no . . . C(36) C(35) H(32) 120.2 no . . . C(36) C(35) C(34) 119.6(5) yes . . . H(32) C(35) C(34) 120.2 no . . . H(31) C(36) C(31) 119.5 no . . . H(31) C(36) C(35) 119.6 no . . . C(31) C(36) C(35) 121.0(4) yes . . . H(35) C(37) H(36) 109.5 no . . . H(35) C(37) N(5) 109.1 no . . . H(35) C(37) C(28) 109.2 no . . . H(36) C(37) N(5) 109.1 no . . . H(36) C(37) C(28) 109.0 no . . . N(5) C(37) C(28) 111.0(5) yes . . . C(39) C(38) H(37) 115.9 no . . . C(39) C(38) N(5) 128.2(6) yes . . . H(37) C(38) N(5) 115.9 no . . . C(40) C(39) C(44) 119.2(4) yes . . . C(40) C(39) C(38) 125.5(6) yes . . . C(44) C(39) C(38) 115.1(5) yes . . . C(41) C(40) O(5) 119.9(5) yes . . . C(41) C(40) C(39) 116.3(5) yes . . . O(5) C(40) C(39) 123.7(4) yes . . . C(42) C(41) H(41) 119.0 no . . . C(42) C(41) C(40) 122.1(5) yes . . . H(41) C(41) C(40) 118.9 no . . . C(43) C(42) H(40) 119.3 no . . . C(43) C(42) C(41) 121.5(5) yes . . . H(40) C(42) C(41) 119.3 no . . . C(44) C(43) H(39) 121.0 no . . . C(44) C(43) C(42) 118.1(7) yes . . . H(39) C(43) C(42) 121.0 no . . . H(38) C(44) C(39) 118.6 no . . . H(38) C(44) C(43) 118.7 no . . . C(39) C(44) C(43) 122.8(6) yes . . . H(42) C(45) H(43) 109.5 no . . . H(42) C(45) N(6) 109.4 no . . . H(42) C(45) C(28) 109.3 no . . . H(43) C(45) N(6) 109.3 no . . . H(43) C(45) C(28) 109.4 no . . . N(6) C(45) C(28) 109.9(4) yes . . . C(47) C(46) H(44) 116.2 no . . . C(47) C(46) N(6) 127.6(5) yes . . . H(44) C(46) N(6) 116.2 no . . . C(48) C(47) C(52) 119.0(5) yes . . . C(48) C(47) C(46) 123.8(6) yes . . . C(52) C(47) C(46) 117.0(5) yes . . . C(49) C(48) O(6) 119.4(5) yes . . . C(49) C(48) C(47) 117.7(6) yes . . . O(6) C(48) C(47) 122.8(5) yes . . . C(50) C(49) H(48) 119.0 no . . . C(50) C(49) C(48) 121.9(5) yes . . . H(48) C(49) C(48) 119.1 no . . . C(51) C(50) H(47) 119.5 no . . . C(51) C(50) C(49) 120.8(6) yes . . . H(47) C(50) C(49) 119.6 no . . . C(52) C(51) H(46) 120.9 no . . . C(52) C(51) C(50) 118.4(7) yes . . . H(46) C(51) C(50) 120.8 no . . . H(45) C(52) C(47) 118.9 no . . . H(45) C(52) C(51) 119.0 no . . . C(47) C(52) C(51) 122.1(5) yes . . . Ni(1) Gd(1) Ni(2) 139.94(2) yes . . . #======END #=========================================================================== data_030227 _database_code_depnum_ccdc_archive 'CCDC 229923' #=========================================================================== _audit_creation_date 2004-02-25 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? # CHEMICAL DATA _chemical_formula_sum 'C66 H84 Gd2 N6 O20 Ni2 ' _chemical_formula_moiety 'C66 H84 Gd2 N6 O20 Ni2 ' _chemical_formula_weight 1713.32 _chemical_melting_point ? #=========================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #--------------------------------------------------------------------------= _cell_length_a 10.971(3) _cell_length_b 12.584(2) _cell_length_c 14.195(3) _cell_angle_alpha 63.82(2) _cell_angle_beta 70.819(4) _cell_angle_gamma 81.437(7) _cell_volume 1661.1(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4656 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 25.0 _cell_measurement_temperature 93.1 #--------------------------------------------------------------------------= _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 866.00 _exptl_absorpt_coefficient_mu 2.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 1.000 #=========================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 10051 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.8055 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.8655 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #=========================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6137 _reflns_number_gt 4100 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1550 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5627 _refine_ls_number_parameters 475 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w == 1/[0.0016Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.85 _refine_diff_density_min -2.51 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Gd Gd -0.165 3.904 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Gd(1) Gd 0.45359(4) 0.17799(4) 0.39560(4) 0.0215(1) Uani 1.00 1 d . . . Ni(1) Ni 0.3241(1) 0.4368(1) 0.3238(1) 0.0239(3) Uani 1.00 1 d . . . O(1) O 0.5089(5) 0.3772(5) 0.2683(5) 0.021(2) Uani 1.00 1 d . . . O(2) O 0.2843(5) 0.2821(5) 0.3216(5) 0.022(2) Uani 1.00 1 d . . . O(3) O 0.3500(6) 0.3152(6) 0.4713(5) 0.026(2) Uani 1.00 1 d . . . O(4) O 0.5503(6) 0.0424(5) 0.5506(5) 0.022(2) Uani 1.00 1 d . . . O(5) O 0.6179(6) 0.2271(6) 0.4506(5) 0.028(2) Uani 1.00 1 d . . . O(6) O 0.6634(6) 0.1114(6) 0.3065(5) 0.026(2) Uani 1.00 1 d . . . O(7) O 0.5176(6) 0.1539(6) 0.2187(5) 0.029(2) Uani 1.00 1 d . . . O(8) O 0.2605(6) 0.0779(6) 0.5441(5) 0.027(2) Uani 1.00 1 d . . . O(9) O 0.071(1) 0.066(1) 0.025(1) 0.127(6) Uani 1.00 1 d . . . O(10) O 0.335(2) 0.035(2) 0.011(2) 0.075(7) Uani 0.50 1 d P . . O(11) O 0.449(2) 0.054(2) 0.108(2) 0.10(1) Uani 0.50 1 d P . . N(1) N 0.3422(7) 0.5624(7) 0.1681(7) 0.027(2) Uani 1.00 1 d . . . N(2) N 0.1272(7) 0.4756(7) 0.3568(6) 0.026(2) Uani 1.00 1 d . . . N(3) N 0.3386(7) 0.5684(7) 0.3660(6) 0.027(2) Uani 1.00 1 d . . . C(1) C 0.134(1) 0.8059(9) 0.2197(9) 0.038(3) Uani 1.00 1 d . . . C(2) C 0.1959(9) 0.686(1) 0.2533(8) 0.033(3) Uani 1.00 1 d . . . C(3) C 0.2371(9) 0.6512(9) 0.1557(8) 0.031(3) Uani 1.00 1 d . . . C(4) C 0.4448(9) 0.5858(9) 0.0866(8) 0.029(3) Uani 1.00 1 d . . . C(5) C 0.5682(8) 0.5287(9) 0.0834(8) 0.026(3) Uani 1.00 1 d . . . C(6) C 0.5966(8) 0.4294(9) 0.1734(8) 0.025(3) Uani 1.00 1 d . . . C(7) C 0.7237(9) 0.3880(8) 0.1599(8) 0.023(2) Uani 1.00 1 d . . . C(8) C 0.8214(9) 0.4392(9) 0.0631(8) 0.031(3) Uani 1.00 1 d . . . C(9) C 0.7945(9) 0.5367(9) -0.0260(8) 0.031(3) Uani 1.00 1 d . . . C(10) C 0.6703(9) 0.5768(8) -0.0152(8) 0.026(3) Uani 1.00 1 d . . . C(11) C 0.0925(9) 0.5954(8) 0.3514(8) 0.030(3) Uani 1.00 1 d . . . C(12) C 0.0438(9) 0.4204(9) 0.3493(8) 0.029(3) Uani 1.00 1 d . . . C(13) C 0.0600(8) 0.3174(8) 0.3284(7) 0.023(2) Uani 1.00 1 d . . . C(14) C 0.1797(8) 0.2571(8) 0.3075(7) 0.019(2) Uani 1.00 1 d . . . C(15) C 0.1873(9) 0.1730(8) 0.2698(8) 0.028(3) Uani 1.00 1 d . . . C(16) C 0.0825(9) 0.1390(9) 0.2571(9) 0.034(3) Uani 1.00 1 d . . . C(17) C -0.0358(9) 0.1920(9) 0.2824(9) 0.032(3) Uani 1.00 1 d . . . C(18) C -0.0473(9) 0.2785(9) 0.3158(8) 0.034(3) Uani 1.00 1 d . . . C(19) C 0.312(1) 0.6878(8) 0.2895(8) 0.031(3) Uani 1.00 1 d . . . C(20) C 0.3378(8) 0.556(1) 0.4611(8) 0.031(3) Uani 1.00 1 d . . . C(21) C 0.3442(9) 0.4466(9) 0.5546(8) 0.029(3) Uani 1.00 1 d . . . C(22) C 0.3512(8) 0.3332(9) 0.5545(8) 0.025(3) Uani 1.00 1 d . . . C(23) C 0.3598(9) 0.2362(9) 0.6519(8) 0.029(3) Uani 1.00 1 d . . . C(24) C 0.3554(9) 0.2499(9) 0.7449(8) 0.030(3) Uani 1.00 1 d . . . C(25) C 0.3444(9) 0.3628(9) 0.7430(8) 0.031(3) Uani 1.00 1 d . . . C(26) C 0.341(1) 0.4598(9) 0.6495(8) 0.031(3) Uani 1.00 1 d . . . C(27) C 0.6278(8) 0.1245(9) 0.5223(8) 0.026(3) Uani 1.00 1 d . . . C(28) C 0.7346(9) 0.0973(8) 0.5756(9) 0.028(3) Uani 1.00 1 d . . . C(29) C 0.6293(9) 0.1169(9) 0.2268(8) 0.030(3) Uani 1.00 1 d . . . C(30) C 0.726(1) 0.0820(9) 0.1407(9) 0.040(3) Uani 1.00 1 d . . . C(31) C 0.1407(9) 0.1274(9) 0.5847(9) 0.032(3) Uani 1.00 1 d . . . C(32) C 0.060(2) 0.199(2) -0.029(2) 0.105(7) Uani 1.00 1 d . . . C(33) C 0.390(1) 0.112(1) 0.034(1) 0.058(4) Uani 1.00 1 d . . . H(1) H 0.1980 0.8647 0.1894 0.045 Uiso 1.00 1 c R . . H(2) H 0.0715 0.8116 0.2822 0.045 Uiso 1.00 1 c R . . H(3) H 0.0931 0.8176 0.1663 0.045 Uiso 1.00 1 c R . . H(4) H 0.2663 0.7195 0.0889 0.034 Uiso 1.00 1 c R . . H(5) H 0.1654 0.6184 0.1543 0.034 Uiso 1.00 1 c R . . H(6) H 0.4386 0.6494 0.0198 0.032 Uiso 1.00 1 c R . . H(7) H 0.7439 0.3228 0.2200 0.027 Uiso 1.00 1 c R . . H(8) H 0.9065 0.4078 0.0568 0.037 Uiso 1.00 1 c R . . H(9) H 0.8613 0.5743 -0.0922 0.032 Uiso 1.00 1 c R . . H(10) H 0.6513 0.6398 -0.0772 0.032 Uiso 1.00 1 c R . . H(11) H 0.0099 0.6166 0.3402 0.038 Uiso 1.00 1 c R . . H(12) H 0.0906 0.5968 0.4182 0.038 Uiso 1.00 1 c R . . H(13) H -0.0410 0.4527 0.3593 0.032 Uiso 1.00 1 c R . . H(14) H 0.2686 0.1369 0.2510 0.029 Uiso 1.00 1 c R . . H(15) H 0.0914 0.0791 0.2316 0.038 Uiso 1.00 1 c R . . H(16) H -0.1092 0.1673 0.2759 0.042 Uiso 1.00 1 c R . . H(17) H -0.1292 0.3150 0.3316 0.036 Uiso 1.00 1 c R . . H(18) H 0.2945 0.7397 0.3248 0.036 Uiso 1.00 1 c R . . H(19) H 0.3857 0.7152 0.2267 0.036 Uiso 1.00 1 c R . . H(20) H 0.3323 0.6266 0.4708 0.039 Uiso 1.00 1 c R . . H(21) H 0.3690 0.1588 0.6544 0.034 Uiso 1.00 1 c R . . H(22) H 0.3597 0.1824 0.8100 0.035 Uiso 1.00 1 c R . . H(23) H 0.3397 0.3717 0.8073 0.040 Uiso 1.00 1 c R . . H(24) H 0.3359 0.5366 0.6479 0.038 Uiso 1.00 1 c R . . H(25) H 0.7490 0.0142 0.6067 0.039 Uiso 1.00 1 c R . . H(26) H 0.7102 0.1249 0.6317 0.039 Uiso 1.00 1 c R . . H(27) H 0.8115 0.1358 0.5217 0.039 Uiso 1.00 1 c R . . H(28) H 0.7734 0.1497 0.0834 0.043 Uiso 1.00 1 c R . . H(29) H 0.6812 0.0507 0.1114 0.043 Uiso 1.00 1 c R . . H(30) H 0.7832 0.0237 0.1732 0.043 Uiso 1.00 1 c R . . H(31) H 0.1446 0.1447 0.6424 0.038 Uiso 1.00 1 c R . . H(32) H 0.0735 0.0724 0.6119 0.038 Uiso 1.00 1 c R . . H(33) H 0.1241 0.1983 0.5271 0.038 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Gd(1) 0.0155(2) 0.0241(3) 0.0226(3) -0.0028(2) -0.0028(2) -0.0089(2) Ni(1) 0.0203(6) 0.0253(7) 0.0237(7) -0.0002(5) -0.0043(5) -0.0097(5) O(1) 0.019(3) 0.011(3) 0.019(3) -0.004(2) -0.001(3) 0.002(2) O(2) 0.013(3) 0.029(4) 0.023(3) 0.006(2) -0.011(3) -0.007(3) O(3) 0.021(3) 0.036(4) 0.024(4) 0.000(3) -0.005(3) -0.017(3) O(4) 0.022(3) 0.007(3) 0.030(4) -0.003(2) -0.002(3) -0.005(3) O(5) 0.025(3) 0.030(4) 0.030(4) -0.008(3) -0.010(3) -0.008(3) O(6) 0.019(3) 0.028(4) 0.024(4) -0.004(3) -0.004(3) -0.007(3) O(7) 0.026(4) 0.030(4) 0.028(4) -0.002(3) -0.006(3) -0.010(3) O(8) 0.017(3) 0.028(4) 0.029(4) -0.003(3) 0.002(3) -0.011(3) O(9) 0.11(1) 0.13(1) 0.15(1) 0.017(9) -0.05(1) -0.06(1) O(10) 0.06(1) 0.08(1) 0.07(1) -0.00(1) -0.02(1) -0.01(1) O(11) 0.14(2) 0.13(2) 0.15(2) 0.10(2) -0.13(2) -0.12(2) N(1) 0.028(4) 0.028(5) 0.025(4) 0.008(3) -0.012(4) -0.011(4) N(2) 0.031(4) 0.018(4) 0.028(5) 0.002(3) -0.007(4) -0.012(3) N(3) 0.025(4) 0.025(4) 0.022(4) 0.001(3) -0.002(3) -0.006(3) C(1) 0.042(6) 0.030(6) 0.040(7) 0.002(5) -0.012(5) -0.014(5) C(2) 0.023(5) 0.047(7) 0.027(6) 0.005(4) -0.006(4) -0.017(5) C(3) 0.019(5) 0.031(6) 0.034(6) 0.005(4) -0.005(4) -0.008(5) C(4) 0.024(5) 0.026(5) 0.031(6) -0.000(4) -0.004(4) -0.009(4) C(5) 0.019(5) 0.035(6) 0.025(5) -0.001(4) -0.003(4) -0.016(4) C(6) 0.020(5) 0.035(6) 0.025(5) -0.004(4) -0.004(4) -0.017(4) C(7) 0.030(5) 0.011(4) 0.026(5) 0.005(4) -0.009(4) -0.006(4) C(8) 0.022(5) 0.042(6) 0.030(6) -0.011(4) 0.003(4) -0.021(5) C(9) 0.025(5) 0.034(6) 0.021(5) -0.008(4) 0.003(4) -0.006(4) C(10) 0.031(5) 0.022(5) 0.026(5) -0.003(4) -0.013(4) -0.007(4) C(11) 0.031(5) 0.026(5) 0.037(6) 0.004(4) -0.009(4) -0.018(5) C(12) 0.023(5) 0.032(6) 0.024(5) -0.001(4) -0.003(4) -0.007(4) C(13) 0.021(4) 0.024(5) 0.021(5) -0.005(4) -0.006(4) -0.006(4) C(14) 0.017(4) 0.021(5) 0.022(5) -0.000(3) -0.011(4) -0.008(4) C(15) 0.021(5) 0.024(5) 0.028(5) -0.005(4) -0.006(4) -0.001(4) C(16) 0.025(5) 0.028(6) 0.043(6) -0.007(4) -0.007(5) -0.009(5) C(17) 0.027(5) 0.027(5) 0.050(7) -0.010(4) -0.011(5) -0.023(5) C(18) 0.016(5) 0.049(7) 0.026(5) -0.004(4) -0.006(4) -0.004(5) C(19) 0.036(6) 0.021(5) 0.033(6) -0.004(4) -0.008(5) -0.010(4) C(20) 0.017(5) 0.045(7) 0.036(6) -0.004(4) -0.002(4) -0.023(5) C(21) 0.021(5) 0.027(6) 0.033(6) -0.009(4) -0.005(4) -0.008(4) C(22) 0.019(5) 0.030(6) 0.026(5) 0.002(4) -0.003(4) -0.014(4) C(23) 0.026(5) 0.028(6) 0.032(6) 0.000(4) -0.008(4) -0.010(4) C(24) 0.031(5) 0.027(6) 0.028(6) -0.006(4) -0.011(4) -0.007(4) C(25) 0.031(5) 0.036(6) 0.031(6) -0.000(4) -0.008(4) -0.021(5) C(26) 0.039(6) 0.035(6) 0.022(5) -0.011(5) -0.009(4) -0.011(4) C(27) 0.015(4) 0.038(6) 0.022(5) -0.007(4) -0.001(4) -0.010(4) C(28) 0.031(5) 0.020(5) 0.045(6) -0.001(4) -0.024(5) -0.014(4) C(29) 0.027(5) 0.027(6) 0.029(6) -0.010(4) -0.002(4) -0.008(4) C(30) 0.047(7) 0.026(6) 0.034(6) -0.004(5) -0.007(5) -0.004(5) C(31) 0.022(5) 0.032(6) 0.041(6) -0.001(4) -0.000(4) -0.020(5) C(32) 0.12(2) 0.08(1) 0.09(1) -0.01(1) -0.03(1) -0.01(1) C(33) 0.066(9) 0.060(9) 0.054(8) -0.021(7) -0.007(7) -0.033(7) #=========================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution ? _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Gd(1) Ni(1) 3.211(1) ? . . Gd(1) O(1) 2.377(5) ? . . Gd(1) O(2) 2.369(6) ? . . Gd(1) O(3) 2.383(8) ? . . Gd(1) O(4) 2.561(6) ? . . Gd(1) O(5) 2.434(8) ? . . Gd(1) O(6) 2.459(6) ? . . Gd(1) O(7) 2.518(8) ? . . Gd(1) O(8) 2.457(5) ? . . Gd(1) C(27) 2.85(1) ? . . Ni(1) O(1) 2.077(6) ? . . Ni(1) O(2) 2.073(8) ? . . Ni(1) O(3) 2.059(6) ? . . Ni(1) N(1) 2.036(7) ? . . Ni(1) N(2) 2.085(8) ? . . Ni(1) N(3) 2.03(1) ? . . O(1) C(6) 1.315(9) ? . . O(2) C(14) 1.33(1) ? . . O(3) C(22) 1.30(2) ? . . O(4) C(27) 1.27(1) ? . . O(5) C(27) 1.26(1) ? . . O(6) C(29) 1.27(2) ? . . O(7) C(29) 1.27(1) ? . . O(8) C(31) 1.42(1) ? . . O(9) C(32) 1.51(2) ? . . O(10) C(33) 1.41(3) ? . . O(11) C(33) 1.30(3) ? . . N(1) C(3) 1.48(1) ? . . N(1) C(4) 1.28(1) ? . . N(2) C(11) 1.47(1) ? . . N(2) C(12) 1.28(2) ? . . N(3) C(19) 1.47(1) ? . . N(3) C(20) 1.28(2) ? . . C(1) C(2) 1.50(1) ? . . C(2) C(3) 1.54(2) ? . . C(2) C(11) 1.57(1) ? . . C(2) C(19) 1.53(2) ? . . C(4) C(5) 1.43(1) ? . . C(5) C(6) 1.42(1) ? . . C(5) C(10) 1.42(1) ? . . C(6) C(7) 1.40(1) ? . . C(7) C(8) 1.38(1) ? . . C(8) C(9) 1.40(1) ? . . C(9) C(10) 1.36(1) ? . . C(12) C(13) 1.43(2) ? . . C(13) C(14) 1.43(1) ? . . C(13) C(18) 1.43(2) ? . . C(14) C(15) 1.36(2) ? . . C(15) C(16) 1.37(2) ? . . C(16) C(17) 1.38(1) ? . . C(17) C(18) 1.34(2) ? . . C(20) C(21) 1.44(1) ? . . C(21) C(22) 1.42(2) ? . . C(21) C(26) 1.42(2) ? . . C(22) C(23) 1.40(1) ? . . C(23) C(24) 1.39(2) ? . . C(24) C(25) 1.40(2) ? . . C(25) C(26) 1.36(1) ? . . C(27) C(28) 1.52(2) ? . . C(29) C(30) 1.51(2) ? . . C(33) O(10) 1.41(3) ? . . C(33) O(11) 1.30(3) ? . . C(1) H(1) 0.9501 ? . . C(1) H(2) 0.9500 ? . . C(1) H(3) 0.9500 ? . . C(3) H(4) 0.9500 ? . . C(3) H(5) 0.9500 ? . . C(4) H(6) 0.9500 ? . . C(7) H(7) 0.9500 ? . . C(8) H(8) 0.9500 ? . . C(9) H(9) 0.9500 ? . . C(10) H(10) 0.9501 ? . . C(11) H(11) 0.9500 ? . . C(11) H(12) 0.9500 ? . . C(12) H(13) 0.9500 ? . . C(15) H(14) 0.9500 ? . . C(16) H(15) 0.9499 ? . . C(17) H(16) 0.9500 ? . . C(18) H(17) 0.9500 ? . . C(19) H(18) 0.9499 ? . . C(19) H(19) 0.9500 ? . . C(20) H(20) 0.9501 ? . . C(23) H(21) 0.9500 ? . . C(24) H(22) 0.9500 ? . . C(25) H(23) 0.9500 ? . . C(26) H(24) 0.9500 ? . . C(28) H(25) 0.9500 ? . . C(28) H(26) 0.9500 ? . . C(28) H(27) 0.9500 ? . . C(30) H(28) 0.9500 ? . . C(30) H(29) 0.9500 ? . . C(30) H(30) 0.9501 ? . . C(31) H(31) 0.9500 ? . . C(31) H(32) 0.9500 ? . . C(31) H(33) 0.9501 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Gd(1) Ni(1) O(1) 47.7(1) ? . . . O(1) Gd(1) Ni(1) 40.3(1) ? . . . Gd(1) Ni(1) O(2) 47.5(2) ? . . . O(2) Gd(1) Ni(1) 40.2(2) ? . . . Gd(1) Ni(1) O(3) 47.9(2) ? . . . O(3) Gd(1) Ni(1) 39.8(2) ? . . . O(4) Gd(1) Ni(1) 135.7(2) ? . . . O(5) Gd(1) Ni(1) 95.3(2) ? . . . O(6) Gd(1) Ni(1) 129.7(1) ? . . . O(7) Gd(1) Ni(1) 101.1(1) ? . . . O(8) Gd(1) Ni(1) 95.0(1) ? . . . C(27) Gd(1) Ni(1) 117.7(2) ? . . . Gd(1) Ni(1) N(1) 127.3(3) ? . . . Gd(1) Ni(1) N(2) 126.6(2) ? . . . Gd(1) Ni(1) N(3) 128.5(2) ? . . . Gd(1) O(1) Ni(1) 92.0(2) ? . . . O(2) Gd(1) O(1) 67.4(2) ? . . . O(3) Gd(1) O(1) 67.9(2) ? . . . O(4) Gd(1) O(1) 128.2(2) ? . . . O(5) Gd(1) O(1) 75.8(2) ? . . . O(6) Gd(1) O(1) 89.9(2) ? . . . O(7) Gd(1) O(1) 80.5(2) ? . . . O(8) Gd(1) O(1) 135.2(2) ? . . . Gd(1) O(1) C(6) 135.5(6) ? . . . C(27) Gd(1) O(1) 101.7(3) ? . . . Gd(1) O(2) Ni(1) 92.3(3) ? . . . O(3) Gd(1) O(2) 68.1(3) ? . . . O(4) Gd(1) O(2) 154.7(2) ? . . . O(5) Gd(1) O(2) 135.5(2) ? . . . O(6) Gd(1) O(2) 129.8(2) ? . . . O(7) Gd(1) O(2) 79.0(2) ? . . . O(8) Gd(1) O(2) 77.6(2) ? . . . Gd(1) O(2) C(14) 137.9(5) ? . . . C(27) Gd(1) O(2) 155.8(3) ? . . . Gd(1) O(3) Ni(1) 92.3(3) ? . . . O(4) Gd(1) O(3) 97.6(2) ? . . . O(5) Gd(1) O(3) 75.5(2) ? . . . O(6) Gd(1) O(3) 144.4(3) ? . . . O(7) Gd(1) O(3) 140.9(2) ? . . . O(8) Gd(1) O(3) 73.7(2) ? . . . Gd(1) O(3) C(22) 134.7(6) ? . . . C(27) Gd(1) O(3) 87.8(3) ? . . . O(5) Gd(1) O(4) 52.4(2) ? . . . O(6) Gd(1) O(4) 74.0(2) ? . . . O(7) Gd(1) O(4) 120.4(2) ? . . . O(8) Gd(1) O(4) 78.3(2) ? . . . Gd(1) O(4) C(27) 89.7(5) ? . . . C(27) Gd(1) O(4) 26.5(2) ? . . . O(6) Gd(1) O(5) 72.1(3) ? . . . O(7) Gd(1) O(5) 119.3(2) ? . . . O(8) Gd(1) O(5) 116.2(2) ? . . . Gd(1) O(5) C(27) 95.9(7) ? . . . C(27) Gd(1) O(5) 26.0(2) ? . . . O(7) Gd(1) O(6) 52.6(2) ? . . . O(8) Gd(1) O(6) 134.8(2) ? . . . C(27) Gd(1) O(6) 69.2(3) ? . . . Gd(1) O(6) C(29) 94.8(5) ? . . . O(8) Gd(1) O(7) 119.9(3) ? . . . C(27) Gd(1) O(7) 121.8(3) ? . . . Gd(1) O(7) C(29) 92.2(7) ? . . . C(27) Gd(1) O(8) 99.1(2) ? . . . Gd(1) O(8) C(31) 129.3(5) ? . . . Gd(1) C(27) O(4) 63.8(5) ? . . . Gd(1) C(27) O(5) 58.0(6) ? . . . Gd(1) C(27) C(28) 172.2(6) ? . . . O(2) Ni(1) O(1) 78.7(3) ? . . . O(3) Ni(1) O(1) 80.0(2) ? . . . Ni(1) O(1) C(6) 128.0(5) ? . . . N(1) Ni(1) O(1) 89.0(3) ? . . . N(2) Ni(1) O(1) 164.8(4) ? . . . N(3) Ni(1) O(1) 108.3(3) ? . . . O(3) Ni(1) O(2) 80.2(3) ? . . . Ni(1) O(2) C(14) 127.8(5) ? . . . N(1) Ni(1) O(2) 104.6(4) ? . . . N(2) Ni(1) O(2) 88.4(3) ? . . . N(3) Ni(1) O(2) 165.8(2) ? . . . Ni(1) O(3) C(22) 128.5(6) ? . . . N(1) Ni(1) O(3) 167.1(3) ? . . . N(2) Ni(1) O(3) 105.9(3) ? . . . N(3) Ni(1) O(3) 88.8(3) ? . . . N(2) Ni(1) N(1) 86.4(3) ? . . . N(3) Ni(1) N(1) 88.1(4) ? . . . Ni(1) N(1) C(3) 115.6(6) ? . . . Ni(1) N(1) C(4) 126.0(7) ? . . . N(3) Ni(1) N(2) 86.0(4) ? . . . Ni(1) N(2) C(11) 115.0(6) ? . . . Ni(1) N(2) C(12) 124.4(7) ? . . . Ni(1) N(3) C(19) 114.6(8) ? . . . Ni(1) N(3) C(20) 126.4(7) ? . . . O(1) C(6) C(5) 122.7(8) ? . . . O(1) C(6) C(7) 119.2(8) ? . . . O(2) C(14) C(13) 122(1) ? . . . O(2) C(14) C(15) 119.3(8) ? . . . O(3) C(22) C(23) 119(1) ? . . . O(3) C(22) C(21) 124.2(8) ? . . . O(4) C(27) O(5) 121(1) ? . . . O(4) C(27) C(28) 119.1(8) ? . . . O(5) C(27) C(28) 119.6(9) ? . . . O(6) C(29) O(7) 120(1) ? . . . O(6) C(29) C(30) 118.9(9) ? . . . O(7) C(29) C(30) 120(1) ? . . . O(10) C(33) O(11) 111(1) ? . . . N(1) C(3) C(2) 109.6(9) ? . . . C(4) N(1) C(3) 116.7(7) ? . . . N(1) C(4) C(5) 128.3(8) ? . . . N(2) C(11) C(2) 109.3(8) ? . . . C(12) N(2) C(11) 117.3(8) ? . . . N(2) C(12) C(13) 129.3(9) ? . . . N(3) C(19) C(2) 110.4(9) ? . . . C(20) N(3) C(19) 116(1) ? . . . N(3) C(20) C(21) 127(1) ? . . . C(1) C(2) C(3) 109.0(9) ? . . . C(1) C(2) C(11) 107.8(8) ? . . . C(1) C(2) C(19) 109(1) ? . . . C(11) C(2) C(3) 109(1) ? . . . C(19) C(2) C(3) 111.0(8) ? . . . C(19) C(2) C(11) 110.2(8) ? . . . C(4) C(5) C(6) 124.7(7) ? . . . C(4) C(5) C(10) 117.6(8) ? . . . C(5) C(6) C(7) 118.1(7) ? . . . C(10) C(5) C(6) 117.6(8) ? . . . C(5) C(10) C(9) 123.4(8) ? . . . C(6) C(7) C(8) 122.5(8) ? . . . C(7) C(8) C(9) 119.9(9) ? . . . C(8) C(9) C(10) 118.4(8) ? . . . C(12) C(13) C(14) 124(1) ? . . . C(12) C(13) C(18) 118.2(9) ? . . . C(13) C(14) C(15) 118(1) ? . . . C(18) C(13) C(14) 116(1) ? . . . C(13) C(18) C(17) 121.9(9) ? . . . C(14) C(15) C(16) 122.7(9) ? . . . C(15) C(16) C(17) 119(1) ? . . . C(16) C(17) C(18) 120(1) ? . . . C(20) C(21) C(22) 123(1) ? . . . C(20) C(21) C(26) 114(1) ? . . . C(21) C(22) C(23) 116(1) ? . . . C(26) C(21) C(22) 121.3(8) ? . . . C(21) C(26) C(25) 120(1) ? . . . C(22) C(23) C(24) 122(1) ? . . . C(23) C(24) C(25) 120.2(9) ? . . . C(24) C(25) C(26) 120(1) ? . . . O(8) C(31) H(33) 109.5748 ? . . . O(8) C(31) H(31) 109.3686 ? . . . O(8) C(31) H(32) 109.4624 ? . . . N(1) C(3) H(4) 109.5285 ? . . . N(1) C(3) H(5) 109.2758 ? . . . N(1) C(4) H(6) 115.9032 ? . . . N(2) C(11) H(11) 109.5558 ? . . . N(2) C(11) H(12) 109.5259 ? . . . N(2) C(12) H(13) 115.2655 ? . . . N(3) C(19) H(18) 109.3482 ? . . . N(3) C(19) H(19) 109.1771 ? . . . N(3) C(20) H(20) 116.2737 ? . . . H(1) C(1) C(2) 109.3862 ? . . . H(2) C(1) C(2) 109.4778 ? . . . H(3) C(1) C(2) 109.5424 ? . . . H(2) C(1) H(1) 109.4677 ? . . . H(3) C(1) H(1) 109.4788 ? . . . H(3) C(1) H(2) 109.4744 ? . . . C(2) C(3) H(4) 109.5237 ? . . . C(2) C(3) H(5) 109.4221 ? . . . C(2) C(11) H(11) 109.5683 ? . . . C(2) C(11) H(12) 109.4427 ? . . . C(2) C(19) H(18) 109.2374 ? . . . C(2) C(19) H(19) 109.2413 ? . . . H(5) C(3) H(4) 109.4560 ? . . . H(6) C(4) C(5) 115.8152 ? . . . C(5) C(10) H(10) 118.3421 ? . . . C(6) C(7) H(7) 118.6433 ? . . . H(7) C(7) C(8) 118.8125 ? . . . C(7) C(8) H(8) 120.0039 ? . . . H(8) C(8) C(9) 120.1274 ? . . . C(8) C(9) H(9) 120.7288 ? . . . C(9) C(10) H(10) 118.2783 ? . . . H(9) C(9) C(10) 120.8429 ? . . . H(12) C(11) H(11) 109.4638 ? . . . H(13) C(12) C(13) 115.3952 ? . . . C(13) C(18) H(17) 119.0052 ? . . . C(14) C(15) H(14) 118.5574 ? . . . H(14) C(15) C(16) 118.7597 ? . . . C(15) C(16) H(15) 120.1587 ? . . . H(15) C(16) C(17) 120.4094 ? . . . C(16) C(17) H(16) 119.8780 ? . . . C(17) C(18) H(17) 119.0604 ? . . . H(16) C(17) C(18) 119.9177 ? . . . H(19) C(19) H(18) 109.4634 ? . . . H(20) C(20) C(21) 116.3523 ? . . . C(21) C(26) H(24) 120.0468 ? . . . C(22) C(23) H(21) 119.0802 ? . . . H(21) C(23) C(24) 118.8826 ? . . . C(23) C(24) H(22) 120.1161 ? . . . H(22) C(24) C(25) 119.6933 ? . . . C(24) C(25) H(23) 119.9314 ? . . . C(25) C(26) H(24) 119.8230 ? . . . H(23) C(25) C(26) 120.0390 ? . . . C(27) C(28) H(25) 109.4982 ? . . . C(27) C(28) H(26) 109.4463 ? . . . C(27) C(28) H(27) 109.4692 ? . . . H(26) C(28) H(25) 109.4716 ? . . . H(27) C(28) H(25) 109.4729 ? . . . H(27) C(28) H(26) 109.4691 ? . . . C(29) C(30) H(28) 109.3959 ? . . . C(29) C(30) H(29) 109.4819 ? . . . C(29) C(30) H(30) 109.5240 ? . . . H(29) C(30) H(28) 109.4773 ? . . . H(30) C(30) H(28) 109.4749 ? . . . H(30) C(30) H(29) 109.4731 ? . . . H(33) C(31) H(31) 109.4772 ? . . . H(32) C(31) H(31) 109.4739 ? . . . H(33) C(31) H(32) 109.4703 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Gd(1) Ni(1) O(1) C(6) 159(1) ? . . . . O(2) Ni(1) O(1) Gd(1) -41.4(2) ? . . . . O(2) Ni(1) O(1) C(6) 117(1) ? . . . . O(3) Ni(1) O(1) Gd(1) 40.5(2) ? . . . . O(3) Ni(1) O(1) C(6) -160(1) ? . . . . N(1) Ni(1) O(1) Gd(1) -146.5(2) ? . . . . N(1) Ni(1) O(1) C(6) 12(1) ? . . . . N(2) Ni(1) O(1) Gd(1) -73.9(6) ? . . . . N(2) Ni(1) O(1) C(6) 85(1) ? . . . . N(3) Ni(1) O(1) Gd(1) 125.8(2) ? . . . . N(3) Ni(1) O(1) C(6) -75(1) ? . . . . Gd(1) Ni(1) O(2) C(14) 166.4(7) ? . . . . O(1) Ni(1) O(2) Gd(1) 41.6(1) ? . . . . O(1) Ni(1) O(2) C(14) -152.0(7) ? . . . . O(3) Ni(1) O(2) Gd(1) -40.1(1) ? . . . . O(3) Ni(1) O(2) C(14) 126.4(6) ? . . . . N(1) Ni(1) O(2) Gd(1) 127.6(1) ? . . . . N(1) Ni(1) O(2) C(14) -66.0(6) ? . . . . N(2) Ni(1) O(2) Gd(1) -146.5(2) ? . . . . N(2) Ni(1) O(2) C(14) 19.9(6) ? . . . . N(3) Ni(1) O(2) Gd(1) -79.6(7) ? . . . . N(3) Ni(1) O(2) C(14) 86(1) ? . . . . Gd(1) Ni(1) O(3) C(22) 158.5(8) ? . . . . O(1) Ni(1) O(3) Gd(1) -40.4(1) ? . . . . O(1) Ni(1) O(3) C(22) 118.2(7) ? . . . . O(2) Ni(1) O(3) Gd(1) 39.8(2) ? . . . . O(2) Ni(1) O(3) C(22) -161.7(7) ? . . . . N(1) Ni(1) O(3) Gd(1) -72(1) ? . . . . N(1) Ni(1) O(3) C(22) 85(1) ? . . . . N(2) Ni(1) O(3) Gd(1) 125.3(1) ? . . . . N(2) Ni(1) O(3) C(22) -76.2(7) ? . . . . N(3) Ni(1) O(3) Gd(1) -149.2(2) ? . . . . N(3) Ni(1) O(3) C(22) 9.4(7) ? . . . . Gd(1) Ni(1) N(1) C(3) 156.8(7) ? . . . . Gd(1) Ni(1) N(1) C(4) -38(1) ? . . . . O(1) Ni(1) N(1) C(3) -172.3(8) ? . . . . O(1) Ni(1) N(1) C(4) -7(1) ? . . . . O(2) Ni(1) N(1) C(3) 109.6(8) ? . . . . O(2) Ni(1) N(1) C(4) -85(1) ? . . . . O(3) Ni(1) N(1) C(3) -140(1) ? . . . . O(3) Ni(1) N(1) C(4) 24(2) ? . . . . N(2) Ni(1) N(1) C(3) 22.2(8) ? . . . . N(2) Ni(1) N(1) C(4) -173(1) ? . . . . N(3) Ni(1) N(1) C(3) -63.9(8) ? . . . . N(3) Ni(1) N(1) C(4) 100(1) ? . . . . Gd(1) Ni(1) N(2) C(11) 158.8(6) ? . . . . Gd(1) Ni(1) N(2) C(12) -42.2(8) ? . . . . O(1) Ni(1) N(2) C(11) -138.9(8) ? . . . . O(1) Ni(1) N(2) C(12) 20(1) ? . . . . O(2) Ni(1) N(2) C(11) -170.8(7) ? . . . . O(2) Ni(1) N(2) C(12) -11.8(7) ? . . . . O(3) Ni(1) N(2) C(11) 109.9(7) ? . . . . O(3) Ni(1) N(2) C(12) -91.1(7) ? . . . . N(1) Ni(1) N(2) C(11) -66.1(7) ? . . . . N(1) Ni(1) N(2) C(12) 92.9(7) ? . . . . N(3) Ni(1) N(2) C(11) 22.3(7) ? . . . . N(3) Ni(1) N(2) C(12) -178.7(7) ? . . . . Gd(1) Ni(1) N(3) C(19) 157.4(5) ? . . . . Gd(1) Ni(1) N(3) C(20) -40.0(8) ? . . . . O(1) Ni(1) N(3) C(19) 107.4(6) ? . . . . O(1) Ni(1) N(3) C(20) -90.1(7) ? . . . . O(2) Ni(1) N(3) C(19) -134.8(8) ? . . . . O(2) Ni(1) N(3) C(20) 27(1) ? . . . . O(3) Ni(1) N(3) C(19) -173.6(6) ? . . . . O(3) Ni(1) N(3) C(20) -11.0(7) ? . . . . N(1) Ni(1) N(3) C(19) 19.0(5) ? . . . . N(1) Ni(1) N(3) C(20) -178.4(7) ? . . . . N(2) Ni(1) N(3) C(19) -67.6(6) ? . . . . N(2) Ni(1) N(3) C(20) 95.0(7) ? . . . . Gd(1) O(1) C(6) C(5) 137(1) ? . . . . Gd(1) O(1) C(6) C(7) -44(1) ? . . . . Ni(1) O(1) C(6) C(5) -12(1) ? . . . . Ni(1) O(1) C(6) C(7) 166.7(9) ? . . . . Gd(1) O(2) C(14) C(13) 137.6(7) ? . . . . Gd(1) O(2) C(14) C(15) -43(1) ? . . . . Ni(1) O(2) C(14) C(13) -21(1) ? . . . . Ni(1) O(2) C(14) C(15) 156.7(6) ? . . . . Gd(1) O(3) C(22) C(21) 143.9(7) ? . . . . Gd(1) O(3) C(22) C(23) -36(1) ? . . . . Ni(1) O(3) C(22) C(21) -5(1) ? . . . . Ni(1) O(3) C(22) C(23) 174.7(6) ? . . . . Gd(1) O(4) C(27) O(5) 7(1) ? . . . . Gd(1) O(4) C(27) C(28) -171.8(9) ? . . . . Gd(1) O(5) C(27) O(4) -7(1) ? . . . . Gd(1) O(5) C(27) C(28) 171.4(9) ? . . . . Gd(1) O(6) C(29) O(7) 2.5(9) ? . . . . Gd(1) O(6) C(29) C(30) -179.2(8) ? . . . . Gd(1) O(7) C(29) O(6) -2.4(9) ? . . . . Gd(1) O(7) C(29) C(30) 179.3(8) ? . . . . Ni(1) N(1) C(3) C(2) 39(1) ? . . . . C(4) N(1) C(3) C(2) -126(1) ? . . . . Ni(1) N(1) C(4) C(5) 2(2) ? . . . . C(3) N(1) C(4) C(5) 166(1) ? . . . . Ni(1) N(2) C(11) C(2) 38(1) ? . . . . C(12) N(2) C(11) C(2) -121.9(9) ? . . . . Ni(1) N(2) C(12) C(13) 6(1) ? . . . . C(11) N(2) C(12) C(13) 165.1(8) ? . . . . Ni(1) N(3) C(19) C(2) 41(1) ? . . . . C(20) N(3) C(19) C(2) -122(1) ? . . . . Ni(1) N(3) C(20) C(21) 9(1) ? . . . . C(19) N(3) C(20) C(21) 171.4(8) ? . . . . C(1) C(2) C(3) N(1) 156.5(8) ? . . . . C(11) C(2) C(3) N(1) -85.9(9) ? . . . . C(19) C(2) C(3) N(1) 35(1) ? . . . . C(1) C(2) C(11) N(2) 156(1) ? . . . . C(3) C(2) C(11) N(2) 38(1) ? . . . . C(19) C(2) C(11) N(2) -83(1) ? . . . . C(1) C(2) C(19) N(3) 154.8(8) ? . . . . C(3) C(2) C(19) N(3) -84(1) ? . . . . C(11) C(2) C(19) N(3) 36(1) ? . . . . N(1) C(4) C(5) C(6) 2(2) ? . . . . N(1) C(4) C(5) C(10) -175(1) ? . . . . C(4) C(5) C(6) O(1) 2(2) ? . . . . C(4) C(5) C(6) C(7) -175(1) ? . . . . C(10) C(5) C(6) O(1) -179(1) ? . . . . C(10) C(5) C(6) C(7) 1(1) ? . . . . C(4) C(5) C(10) C(9) 174(1) ? . . . . C(6) C(5) C(10) C(9) -3(2) ? . . . . O(1) C(6) C(7) C(8) -179(1) ? . . . . C(5) C(6) C(7) C(8) 0(1) ? . . . . C(6) C(7) C(8) C(9) 0(1) ? . . . . C(7) C(8) C(9) C(10) -1(2) ? . . . . C(8) C(9) C(10) C(5) 3(2) ? . . . . N(2) C(12) C(13) C(14) -2(1) ? . . . . N(2) C(12) C(13) C(18) -175.3(9) ? . . . . C(12) C(13) C(14) O(2) 10(1) ? . . . . C(12) C(13) C(14) C(15) -168.5(8) ? . . . . C(18) C(13) C(14) O(2) -176.9(7) ? . . . . C(18) C(13) C(14) C(15) 4(1) ? . . . . C(12) C(13) C(18) C(17) 171.4(8) ? . . . . C(14) C(13) C(18) C(17) -2(1) ? . . . . O(2) C(14) C(15) C(16) 177.5(8) ? . . . . C(13) C(14) C(15) C(16) -3(1) ? . . . . C(14) C(15) C(16) C(17) 0(1) ? . . . . C(15) C(16) C(17) C(18) 2(1) ? . . . . C(16) C(17) C(18) C(13) -1(1) ? . . . . N(3) C(20) C(21) C(22) 0(1) ? . . . . N(3) C(20) C(21) C(26) -179.7(7) ? . . . . C(20) C(21) C(22) O(3) -1(1) ? . . . . C(20) C(21) C(22) C(23) 178.6(8) ? . . . . C(26) C(21) C(22) O(3) 177.5(8) ? . . . . C(26) C(21) C(22) C(23) -2(1) ? . . . . C(20) C(21) C(26) C(25) 179.0(9) ? . . . . C(22) C(21) C(26) C(25) 0(1) ? . . . . O(3) C(22) C(23) C(24) -176.9(9) ? . . . . C(21) C(22) C(23) C(24) 3(1) ? . . . . C(22) C(23) C(24) C(25) -1(1) ? . . . . C(23) C(24) C(25) C(26) -1(1) ? . . . . C(24) C(25) C(26) C(21) 2(1) ? . . . . #=========================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #=========================================================================== # End of CIF #===========================================================================