#------------------------------------------------------------------------------ #$Date: 2015-07-12 01:46:52 +0300 (Sun, 12 Jul 2015) $ #$Revision: 146542 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/37/4343701.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4343701 loop_ _publ_author_name 'Lewing, Dennis' 'Koppetz, Hannah' 'Hahn, F. Ekkehardt' _publ_section_title ; Reversible Formation and Transmetalation of Schiff-Base Complexes in Subcomponent Self-Assembly Reactions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 150710144333009 _journal_paper_doi 10.1021/acs.inorgchem.5b01334 _journal_year 2015 _chemical_formula_sum 'C46 H42 N6 Ni2 O2 S4' _chemical_formula_weight 956.52 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.3510(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.5835(5) _cell_length_b 11.9723(6) _cell_length_c 18.4742(9) _cell_measurement_reflns_used 900 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 1 _cell_volume 2070.61(18) _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ; 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. ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _diffrn_ambient_temperature 153(2) _diffrn_detector_area_resol_mean 80 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 24641 _diffrn_reflns_theta_full 30.50 _diffrn_reflns_theta_max 30.50 _diffrn_reflns_theta_min 2.04 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_correction_T_min 0.8929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.803617 ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'metallic hexagon' _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.500 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 6309 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0378 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.4869P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.0957 _reflns_number_gt 4893 _reflns_number_total 6309 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic5b01334_si_002.cif _cod_data_source_block '[6]' _cod_cif_authors_sg_H-M P2(1)/n _cod_database_code 4343701 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Ni1 Ni 0.33162(2) 0.866856(19) 0.109331(13) 0.01607(7) Uani 1 1 d . S1 S 0.56145(5) 0.89606(4) 0.12088(3) 0.02399(11) Uani 1 1 d . S2 S 0.41114(5) 0.71403(4) 0.16425(3) 0.02252(11) Uani 1 1 d . N1 N 0.29210(16) 0.99642(13) 0.04377(8) 0.0166(3) Uani 1 1 d . N2 N 0.13415(16) 0.84730(12) 0.11856(8) 0.0159(3) Uani 1 1 d . C1 C 0.35560(19) 1.09213(16) 0.05452(10) 0.0197(4) Uani 1 1 d . H1 H 0.3208 1.1502 0.0204 0.024 Uiso 1 1 calc R C2 C 0.4760(2) 1.11801(16) 0.11463(10) 0.0203(4) Uani 1 1 d . C3 C 0.5766(2) 1.03656(17) 0.14669(10) 0.0209(4) Uani 1 1 d . C4 C 0.6969(2) 1.07300(19) 0.19873(11) 0.0272(4) Uani 1 1 d . H4 H 0.7683 1.0203 0.2196 0.033 Uiso 1 1 calc R C5 C 0.7143(2) 1.1831(2) 0.22030(12) 0.0314(5) Uani 1 1 d . H5 H 0.7961 1.2050 0.2563 0.038 Uiso 1 1 calc R C6 C 0.6128(2) 1.26237(19) 0.18973(13) 0.0322(5) Uani 1 1 d . H6 H 0.6237 1.3380 0.2055 0.039 Uiso 1 1 calc R C7 C 0.4960(2) 1.23002(18) 0.13613(12) 0.0275(4) Uani 1 1 d . H7 H 0.4284 1.2845 0.1136 0.033 Uiso 1 1 calc R C8 C 0.0728(2) 0.75933(15) 0.13980(10) 0.0186(4) Uani 1 1 d . H8 H -0.0243 0.7690 0.1425 0.022 Uiso 1 1 calc R C9 C 0.1309(2) 0.64981(15) 0.15969(10) 0.0190(4) Uani 1 1 d . C10 C 0.2750(2) 0.62029(15) 0.16797(10) 0.0191(4) Uani 1 1 d . C11 C 0.3140(2) 0.50792(16) 0.18463(11) 0.0231(4) Uani 1 1 d . H11 H 0.4102 0.4855 0.1876 0.028 Uiso 1 1 calc R C12 C 0.2154(2) 0.43002(16) 0.19662(11) 0.0253(4) Uani 1 1 d . H12 H 0.2445 0.3551 0.2080 0.030 Uiso 1 1 calc R C13 C 0.0736(2) 0.46034(17) 0.19216(11) 0.0270(4) Uani 1 1 d . H13 H 0.0064 0.4072 0.2020 0.032 Uiso 1 1 calc R C14 C 0.0322(2) 0.56870(17) 0.17324(11) 0.0243(4) Uani 1 1 d . H14 H -0.0649 0.5893 0.1692 0.029 Uiso 1 1 calc R C15 C 0.03534(19) 0.94024(15) 0.09940(10) 0.0163(3) Uani 1 1 d . C16 C 0.0661(2) 1.04401(15) 0.13248(10) 0.0180(3) Uani 1 1 d . H16 H 0.1512 1.0553 0.1690 0.022 Uiso 1 1 calc R C17 C -0.0300(2) 1.13130(16) 0.11112(10) 0.0202(4) Uani 1 1 d . H17 H -0.0128 1.2017 0.1351 0.024 Uiso 1 1 calc R C18 C -0.1505(2) 1.11624(15) 0.05515(10) 0.0188(4) Uani 1 1 d . H18 H -0.2147 1.1766 0.0404 0.023 Uiso 1 1 calc R C19 C -0.17742(18) 1.01317(15) 0.02082(10) 0.0158(3) Uani 1 1 d . C20 C -0.08660(19) 0.92347(15) 0.04444(10) 0.0163(3) Uani 1 1 d . H20 H -0.1078 0.8516 0.0232 0.020 Uiso 1 1 calc R O31 O 0.1843(2) 0.32348(14) 1.01384(10) 0.0452(5) Uani 1 1 d . N31 N 0.2580(2) 0.48540(15) 0.96977(10) 0.0294(4) Uani 1 1 d . C31 C 0.1825(2) 0.42538(18) 1.00837(12) 0.0312(5) Uani 1 1 d . H31 H 0.1218 0.4650 1.0339 0.037 Uiso 1 1 calc R C32 C 0.3501(3) 0.4322(2) 0.92697(15) 0.0452(6) Uani 1 1 d . H32A H 0.3549 0.3519 0.9373 0.068 Uiso 1 1 calc R H32B H 0.4461 0.4645 0.9407 0.068 Uiso 1 1 calc R H32C H 0.3113 0.4445 0.8740 0.068 Uiso 1 1 calc R C33 C 0.2414(3) 0.60560(18) 0.96448(13) 0.0359(5) Uani 1 1 d . H33A H 0.1713 0.6296 0.9929 0.054 Uiso 1 1 calc R H33B H 0.2083 0.6270 0.9124 0.054 Uiso 1 1 calc R H33C H 0.3334 0.6415 0.9846 0.054 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01336(11) 0.01579(12) 0.01794(12) 0.00233(9) 0.00089(8) 0.00073(8) S1 0.0152(2) 0.0237(2) 0.0324(3) 0.0047(2) 0.00369(19) 0.00202(17) S2 0.0169(2) 0.0190(2) 0.0295(3) 0.00486(18) 0.00017(18) 0.00198(17) N1 0.0125(7) 0.0179(7) 0.0183(7) 0.0014(6) 0.0009(5) 0.0010(6) N2 0.0164(7) 0.0144(7) 0.0154(7) 0.0009(5) -0.0003(6) 0.0011(5) C1 0.0169(9) 0.0195(9) 0.0215(9) 0.0031(7) 0.0013(7) -0.0005(7) C2 0.0155(8) 0.0246(10) 0.0198(9) 0.0012(7) 0.0015(7) -0.0039(7) C3 0.0161(8) 0.0265(10) 0.0199(9) 0.0032(7) 0.0034(7) -0.0027(7) C4 0.0167(9) 0.0389(12) 0.0243(10) 0.0068(9) 0.0006(7) -0.0022(8) C5 0.0224(10) 0.0457(13) 0.0232(10) -0.0005(9) -0.0015(8) -0.0125(9) C6 0.0304(11) 0.0311(11) 0.0327(12) -0.0053(9) 0.0015(9) -0.0100(9) C7 0.0232(10) 0.0270(10) 0.0302(11) -0.0002(8) 0.0007(8) -0.0041(8) C8 0.0182(9) 0.0193(9) 0.0182(9) 0.0022(7) 0.0034(7) 0.0011(7) C9 0.0234(9) 0.0167(9) 0.0162(8) 0.0025(7) 0.0031(7) 0.0001(7) C10 0.0218(9) 0.0193(9) 0.0144(8) 0.0006(7) 0.0002(7) 0.0005(7) C11 0.0277(10) 0.0197(9) 0.0196(9) 0.0003(7) 0.0000(7) 0.0046(8) C12 0.0377(12) 0.0163(9) 0.0198(9) 0.0019(7) 0.0017(8) 0.0015(8) C13 0.0348(11) 0.0219(10) 0.0247(10) 0.0039(8) 0.0072(8) -0.0058(8) C14 0.0247(10) 0.0231(10) 0.0253(10) 0.0033(8) 0.0056(8) -0.0011(8) C15 0.0163(8) 0.0160(8) 0.0166(8) 0.0030(6) 0.0037(6) 0.0016(6) C16 0.0186(8) 0.0190(9) 0.0157(8) -0.0008(7) 0.0021(7) -0.0002(7) C17 0.0236(9) 0.0161(8) 0.0199(9) -0.0036(7) 0.0025(7) -0.0007(7) C18 0.0179(9) 0.0167(9) 0.0213(9) 0.0004(7) 0.0032(7) 0.0026(7) C19 0.0141(8) 0.0188(8) 0.0144(8) 0.0016(6) 0.0026(6) -0.0011(6) C20 0.0172(8) 0.0143(8) 0.0171(8) 0.0017(6) 0.0030(6) -0.0009(6) O31 0.0576(12) 0.0191(8) 0.0517(11) 0.0002(7) -0.0041(9) -0.0026(8) N31 0.0360(10) 0.0219(9) 0.0291(9) -0.0035(7) 0.0047(8) 0.0049(7) C31 0.0358(12) 0.0237(10) 0.0288(11) -0.0025(8) -0.0046(9) 0.0016(9) C32 0.0402(14) 0.0505(16) 0.0444(15) -0.0132(12) 0.0081(12) 0.0087(12) C33 0.0470(14) 0.0224(11) 0.0355(12) 0.0024(9) 0.0026(11) 0.0016(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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_ _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 N2 Ni1 N1 94.96(6) . . N2 Ni1 S2 96.27(5) . . N1 Ni1 S2 165.81(5) . . N2 Ni1 S1 169.40(5) . . N1 Ni1 S1 89.50(5) . . S2 Ni1 S1 80.95(2) . . C3 S1 Ni1 101.73(7) . . C10 S2 Ni1 112.08(7) . . C1 N1 C19 116.59(15) . 3_575 C1 N1 Ni1 125.86(13) . . C19 N1 Ni1 117.48(11) 3_575 . C8 N2 C15 112.23(15) . . C8 N2 Ni1 129.07(13) . . C15 N2 Ni1 118.69(11) . . N1 C1 C2 125.24(17) . . C7 C2 C3 120.26(18) . . C7 C2 C1 117.31(18) . . C3 C2 C1 122.23(18) . . C4 C3 C2 117.42(19) . . C4 C3 S1 119.66(16) . . C2 C3 S1 122.84(15) . . C5 C4 C3 121.8(2) . . C4 C5 C6 120.37(19) . . C7 C6 C5 119.3(2) . . C6 C7 C2 120.8(2) . . N2 C8 C9 129.49(17) . . C10 C9 C14 119.21(17) . . C10 C9 C8 125.10(17) . . C14 C9 C8 115.68(17) . . C9 C10 C11 118.18(18) . . C9 C10 S2 124.38(14) . . C11 C10 S2 117.35(15) . . C12 C11 C10 121.41(19) . . C11 C12 C13 120.52(18) . . C14 C13 C12 118.98(19) . . C13 C14 C9 121.55(19) . . C16 C15 C20 121.16(16) . . C16 C15 N2 120.76(16) . . C20 C15 N2 118.00(15) . . C15 C16 C17 118.78(17) . . C18 C17 C16 120.55(17) . . C19 C18 C17 120.02(17) . . C18 C19 C20 120.04(16) . . C18 C19 N1 118.89(16) . 3_575 C20 C19 N1 120.80(16) . 3_575 C15 C20 C19 119.31(16) . . C31 N31 C33 120.54(19) . . C31 N31 C32 121.3(2) . . C33 N31 C32 118.0(2) . . O31 C31 N31 125.6(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 N2 1.9503(16) . Ni1 N1 1.9545(15) . Ni1 S2 2.1511(5) . Ni1 S1 2.1949(6) . S1 C3 1.746(2) . S2 C10 1.733(2) . N1 C1 1.293(2) . N1 C19 1.444(2) 3_575 N2 C8 1.307(2) . N2 C15 1.455(2) . C1 C2 1.454(3) . C2 C7 1.400(3) . C2 C3 1.409(3) . C3 C4 1.403(3) . C4 C5 1.377(3) . C5 C6 1.389(3) . C6 C7 1.382(3) . C8 C9 1.441(3) . C9 C10 1.402(3) . C9 C14 1.415(3) . C10 C11 1.412(3) . C11 C12 1.379(3) . C12 C13 1.392(3) . C13 C14 1.380(3) . C15 C16 1.388(2) . C15 C20 1.389(2) . C16 C17 1.393(3) . C17 C18 1.388(3) . C18 C19 1.386(2) . C19 C20 1.392(2) . C19 N1 1.444(2) 3_575 O31 C31 1.224(3) . N31 C31 1.330(3) . N31 C33 1.449(3) . N31 C32 1.452(3) .