#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006283.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2006283 loop_ _publ_author_name 'Kabak, Mehmet' 'Elmali, Ayhan' 'Elerman, Yal\?cin' _publ_contact_author ; Yalcin ELERMAN Dept. of Engineering Pyhsics, Faculty of Sciences University of Ankara, 06100 Besevler - Ankara, Turkey ; _publ_section_title ; [N-(2-Hydroxybenzyl)salicylaldiminato](piperidine)nickel(II) ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 868 _journal_page_last 870 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Ni (C5 H11 N) (C14 H11 N O2)]' _chemical_formula_sum 'C19 H22 N2 Ni O2' _chemical_formula_weight 369.11 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 103.340(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.838(2) _cell_length_b 18.347(4) _cell_length_c 8.9480(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12 _cell_measurement_theta_min 2 _cell_volume 1731.3(5) _computing_cell_refinement 'Enraf-Nonius SDP' _computing_data_collection 'Enraf-Nonius Structure Determination Package (SDP; Frenz, 1985)' _computing_data_reduction 'Enraf-Nonius SDP' _computing_molecular_graphics 'PLATON96 (Spek, 1996a), PLUTON96 (Spek, 1996a)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device CAD-4 _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3680 _diffrn_reflns_theta_max 27.29 _diffrn_reflns_theta_min 1.93 _diffrn_standards_decay_% 2.4 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_type '\y scans (Kopfman & Huber, 1968; North, Phillips & Mathews, 1968)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_meas none _exptl_crystal_description prismatic _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.42 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.736 _refine_ls_goodness_of_fit_obs 0.759 _refine_ls_hydrogen_treatment 'H-atom treatment: isotropic with fixed U~eq~ = 0.10\%A^2^' _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 2265 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 0.735 _refine_ls_restrained_S_obs 0.759 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_obs .0433 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.108P)^2^+3.7262P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1289 _refine_ls_wR_factor_obs .1233 _reflns_number_observed 1973 _reflns_number_total 2265 _reflns_observed_criterion >2\s(I) _[local]_cod_data_source_file bm1142.cif _[local]_cod_data_source_block new _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 1731.3(3) _cod_database_code 2006283 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Ni1 .41806(5) .12373(2) .05365(6) .0525(2) Uani d D 1 1 Ni O1 .5704(3) .1321(2) .1968(3) .0637(8) Uani d . 1 1 O O2 .2644(3) .1023(2) -.0712(4) .0692(8) Uani d . 1 1 O N1 .4553(3) .1995(2) -.0687(4) .0513(8) Uani d . 1 1 N N2 .3942(5) .0581(3) .2177(6) .0482(11) Uiso d PD .50 1 N C1 .6771(4) .1399(2) .1458(5) .0600(11) Uani d . 1 1 C C2 .7796(4) .0942(3) .1941(6) .0787(14) Uani d . 1 1 C H2 .7756 .0564 .2622 .100 Uiso calc . 1 1 H C3 .8882(5) .1047(3) .1411(8) .095(2) Uani d . 1 1 C H3 .9574 .0743 .1762 .100 Uiso calc . 1 1 H C4 .8971(5) .1583(4) .0392(7) .089(2) Uani d . 1 1 C H4 .9706 .1637 .0036 .100 Uiso calc . 1 1 H C5 .7947(4) .2047(3) -.0108(6) .0735(13) Uani d . 1 1 C H5 .7999 .2419 -.0797 .100 Uiso calc . 1 1 H C6 .6857(4) .1959(2) .0409(5) .0573(10) Uani d . 1 1 C C7 .5718(4) .2434(2) -.0082(5) .0622(11) Uani d . 1 1 C H71 .5604 .2722 .0786 .100 Uiso calc . 1 1 H H72 .5850 .2767 -.0872 .100 Uiso calc . 1 1 H C8 .3853(4) .2183(2) -.2002(5) .0543(10) Uani d . 1 1 C H8 .4141 .2569 -.2502 .100 Uiso calc . 1 1 H C9 .2682(4) .1857(2) -.2767(5) .0537(10) Uani d . 1 1 C C10 .2052(4) .2114(3) -.4209(6) .0669(12) Uani d . 1 1 C H10 .2412 .2493 -.4653 .100 Uiso calc . 1 1 H C11 .0932(4) .1828(3) -.4985(6) .0750(13) Uani d . 1 1 C H11 .0542 .1996 -.5961 .100 Uiso calc . 1 1 H C12 .0384(4) .1282(3) -.4291(7) .0801(14) Uani d . 1 1 C H12 -.0394 .1091 -.4801 .100 Uiso calc . 1 1 H C13 .0953(4) .1018(3) -.2884(7) .0773(14) Uani d . 1 1 C H13 .0561 .0649 -.2450 .100 Uiso calc . 1 1 H C14 .2129(4) .1295(2) -.2070(5) .0574(11) Uani d . 1 1 C C15 .2580(6) .0625(4) .2369(9) .0503(14) Uiso d PD .50 1 C H15A .2449 .1096 .2797 .100 Uiso calc P .50 1 H H15B .2004 .0588 .1366 .100 Uiso calc P .50 1 H C16 .2264(8) .0042(4) .3383(10) .062(2) Uiso d PD .50 1 C H16A .2523 .0222 .4427 .100 Uiso calc P .50 1 H H16B .1346 .0007 .3151 .100 Uiso calc P .50 1 H C17 .2711(8) -.0654(4) .3401(11) .065(2) Uiso d PD .50 1 C H17A .2157 -.0933 .2598 .100 Uiso calc P .50 1 H H17B .2697 -.0878 .4378 .100 Uiso calc P .50 1 H C18 .4113(7) -.0681(5) .3151(9) .0518(14) Uiso d PD .50 1 C H18A .4718 -.0481 .4026 .100 Uiso calc P .50 1 H H18B .4361 -.1175 .2964 .100 Uiso calc P .50 1 H C19 .3995(8) -.0188(3) .1686(8) .0503(14) Uiso d PD .50 1 C H19A .4719 -.0263 .1239 .100 Uiso calc P .50 1 H H19B .3231 -.0312 .0923 .100 Uiso calc P .50 1 H N2' .3582(5) .0428(3) .1614(7) .0482(11) Uiso d PD .50 2 N C15' .2873(7) .0698(4) .2798(8) .0503(14) Uiso d PD .50 2 C H15C .3362 .1094 .3364 .100 Uiso calc P .50 2 H H15D .2074 .0904 .2242 .100 Uiso calc P .50 2 H C16' .2586(8) .0171(4) .3943(10) .062(2) Uiso d PD .50 2 C H16C .2784 .0407 .4940 .100 Uiso calc P .50 2 H H16D .1680 .0080 .3682 .100 Uiso calc P .50 2 H C17' .3185(8) -.0488(5) .4096(10) .065(2) Uiso d PD .50 2 C H17C .2560 -.0852 .4200 .100 Uiso calc P .50 2 H H17D .3813 -.0479 .5063 .100 Uiso calc P .50 2 H C18' .3876(8) -.0779(4) .2831(9) .0518(14) Uiso d PD .50 2 C H18C .4492 -.1149 .3273 .100 Uiso calc P .50 2 H H18D .3260 -.0998 .1990 .100 Uiso calc P .50 2 H C19' .4562(6) -.0129(4) .2213(9) .0503(14) Uiso d PD .50 2 C H19C .5217 .0074 .3035 .100 Uiso calc P .50 2 H H19D .4953 -.0295 .1403 .100 Uiso calc P .50 2 H 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 Ni1 .0581(4) .0378(3) .0703(4) .0017(2) .0328(3) .0064(2) O1 .078(2) .063(2) .056(2) -.0126(14) .0262(15) -.0014(13) O2 .063(2) .059(2) .090(2) -.0083(14) .027(2) .021(2) N1 .058(2) .036(2) .068(2) -.0006(14) .032(2) -.0016(15) C1 .064(3) .057(2) .058(2) -.019(2) .012(2) -.010(2) C2 .067(3) .075(3) .085(3) -.013(2) .001(3) .011(3) C3 .054(3) .100(4) .125(5) -.006(3) .007(3) .014(4) C4 .053(3) .106(4) .109(4) -.018(3) .018(3) .008(3) C5 .066(3) .072(3) .081(3) -.026(2) .013(2) .004(2) C6 .059(2) .052(2) .062(2) -.016(2) .016(2) -.008(2) C7 .079(3) .040(2) .075(3) -.019(2) .031(2) -.005(2) C8 .066(2) .038(2) .069(3) .003(2) .035(2) .006(2) C9 .053(2) .047(2) .069(3) .003(2) .029(2) .003(2) C10 .064(3) .066(3) .078(3) .003(2) .031(2) .009(2) C11 .063(3) .082(3) .082(3) .008(2) .022(2) .008(3) C12 .054(3) .083(4) .105(4) -.006(2) .021(3) .002(3) C13 .060(3) .071(3) .106(4) -.006(2) .031(3) .013(3) C14 .053(2) .046(2) .080(3) .002(2) .031(2) .003(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 O2 . 1.822(3) ? Ni1 O1 . 1.848(3) ? Ni1 N1 . 1.871(3) ? Ni1 N2 . 1.961(4) ? O1 C1 . 1.345(5) ? O2 C14 . 1.313(5) ? N1 C8 . 1.291(5) ? N1 C7 . 1.489(5) ? N2 C19 . 1.484(6) ? N2 C15 . 1.528(6) ? C1 C2 . 1.379(7) ? C1 C6 . 1.409(6) ? C2 C3 . 1.380(8) ? C3 C4 . 1.358(8) ? C4 C5 . 1.388(7) ? C5 C6 . 1.375(6) ? C6 C7 . 1.493(6) ? C8 C9 . 1.427(6) ? C9 C10 . 1.396(6) ? C9 C14 . 1.408(6) ? C10 C11 . 1.357(7) ? C11 C12 . 1.383(7) ? C12 C13 . 1.357(8) ? C13 C14 . 1.409(7) ? C15 C16 . 1.493(7) ? C16 C17 . 1.364(8) ? C17 C18 . 1.587(7) ? C18 C19 . 1.573(7) ? N2' C19' . 1.483(6) ? N2' C15' . 1.528(6) ? C15' C16' . 1.493(7) ? C16' C17' . 1.364(8) ? C17' C18' . 1.587(7) ? C18' C19' . 1.572(7) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 Ni1 O1 170.86(12) y O2 Ni1 N1 95.28(14) y O1 Ni1 N1 93.73(14) y O2 Ni1 N2 93.8(2) y O1 Ni1 N2 77.5(2) y N1 Ni1 N2 167.9(2) y C1 O1 Ni1 118.4(2) y C14 O2 Ni1 128.2(3) y C8 N1 C7 117.2(3) ? C8 N1 Ni1 124.8(3) ? C7 N1 Ni1 117.9(3) ? C19 N2 C15 100.8(5) y C19 N2 Ni1 110.0(4) ? C15 N2 Ni1 110.5(4) ? O1 C1 C2 121.5(4) ? O1 C1 C6 119.8(4) ? C2 C1 C6 118.7(4) ? C1 C2 C3 119.7(5) ? C4 C3 C2 122.0(5) ? C3 C4 C5 119.0(5) ? C6 C5 C4 120.3(5) ? C5 C6 C1 120.2(4) ? C5 C6 C7 123.3(4) ? C1 C6 C7 116.5(4) ? N1 C7 C6 111.4(3) ? N1 C8 C9 126.6(4) ? C10 C9 C14 119.3(4) ? C10 C9 C8 119.5(4) ? C14 C9 C8 121.1(4) ? C11 C10 C9 122.1(4) ? C10 C11 C12 118.4(5) ? C11 C12 C13 121.7(5) ? C12 C13 C14 120.9(4) ? O2 C14 C9 123.7(4) ? O2 C14 C13 118.8(4) ? C9 C14 C13 117.5(4) ? C16 C15 N2 113.2(6) ? C17 C16 C15 123.1(8) ? C16 C17 C18 112.1(8) ? C19 C18 C17 101.7(6) ? N2 C19 C18 107.5(5) ? C19' N2' C15' 113.9(5) y C16' C15' N2' 118.9(6) ? C17' C16' C15' 118.3(8) ? C16' C17' C18' 121.2(8) ? C19' C18' C17' 109.6(6) ? N2' C19' C18' 107.0(6) ? 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 O2 Ni1 O1 C1 126.1(8) N1 Ni1 O1 C1 -44.4(3) N2 Ni1 O1 C1 143.9(3) O1 Ni1 O2 C14 -164.5(7) N1 Ni1 O2 C14 6.0(4) N2 Ni1 O2 C14 178.1(4) O2 Ni1 N1 C8 -3.9(3) O1 Ni1 N1 C8 174.6(3) N2 Ni1 N1 C8 -142.8(8) O2 Ni1 N1 C7 173.8(3) O1 Ni1 N1 C7 -7.7(3) N2 Ni1 N1 C7 35.0(10) O2 Ni1 N2 C19 70.2(5) O1 Ni1 N2 C19 -107.1(5) N1 Ni1 N2 C19 -150.9(7) O2 Ni1 N2 C15 -40.2(5) O1 Ni1 N2 C15 142.6(5) N1 Ni1 N2 C15 98.7(10) Ni1 O1 C1 C2 -126.4(4) Ni1 O1 C1 C6 53.6(4) O1 C1 C2 C3 -179.0(5) C6 C1 C2 C3 1.0(7) C1 C2 C3 C4 -1.4(9) C2 C3 C4 C5 1.3(10) C3 C4 C5 C6 -0.7(9) C4 C5 C6 C1 0.3(7) C4 C5 C6 C7 -179.8(5) O1 C1 C6 C5 179.5(4) C2 C1 C6 C5 -0.5(6) O1 C1 C6 C7 -0.4(5) C2 C1 C6 C7 179.6(4) C8 N1 C7 C6 -129.8(4) Ni1 N1 C7 C6 52.4(4) C5 C6 C7 N1 126.5(4) C1 C6 C7 N1 -53.6(5) C7 N1 C8 C9 -177.7(4) Ni1 N1 C8 C9 0.0(5) N1 C8 C9 C10 -178.5(4) N1 C8 C9 C14 3.6(6) C14 C9 C10 C11 -1.5(6) C8 C9 C10 C11 -179.5(4) C9 C10 C11 C12 2.2(7) C10 C11 C12 C13 -1.6(8) C11 C12 C13 C14 0.2(8) Ni1 O2 C14 C9 -4.2(6) Ni1 O2 C14 C13 176.3(3) C10 C9 C14 O2 -179.4(4) C8 C9 C14 O2 -1.4(6) C10 C9 C14 C13 0.1(6) C8 C9 C14 C13 178.1(4) C12 C13 C14 O2 -180.0(5) C12 C13 C14 C9 0.5(7) C19 N2 C15 C16 52.8(8) Ni1 N2 C15 C16 169.1(6) N2 C15 C16 C17 -37.1(12) C15 C16 C17 C18 35.6(13) C16 C17 C18 C19 -49.9(10) C15 N2 C19 C18 -76.1(6) Ni1 N2 C19 C18 167.3(5) C17 C18 C19 N2 75.4(8) C19' N2' C15' C16' -36.1(9) N2' C15' C16' C17' 13.2(12) C15' C16' C17' C18' -15.8(13) C16' C17' C18' C19' 38.7(12) C15' N2' C19' C18' 57.4(8) C17' C18' C19' N2' -57.1(8)