#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003477.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_2003477 loop_ _publ_author_name 'Haber, V.' 'F\'abry, J.' 'Pet\N-[3-(2-Aminoethylamino)propyl]salicylideneaminato-O,N,N',N''}bromozinc(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 884 _journal_page_last 887 _journal_paper_doi 10.1107/S010827019401245X _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C12 H18 Br1 N3 O1 Zn1' _chemical_formula_sum 'C12 H18 Br N3 O Zn' _chemical_formula_weight 365.58 _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2b' _symmetry_space_group_name_H-M 'P b n a' _atom_type_scat_source 'IntTabIV and Cromer & Waber (1974)' _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_formula_units_Z 8 _cell_length_a 19.951(6) _cell_length_b 7.170(2) _cell_length_c 19.761(8) _cell_measurement_reflns_used 46 _cell_measurement_temperature 291 _cell_measurement_theta_max 15.93 _cell_measurement_theta_min 8.01 _cell_volume 2826.8(16) _diffrn_measurement_device 'Hilger & Watts' _diffrn_measurement_method \q/2\q _diffrn_radiation_type 'Ag K\a (Pd filter)' _diffrn_radiation_wavelength 0.56087 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 6913 _diffrn_reflns_theta_max 22 _diffrn_standards_decay_% 5 _diffrn_standards_interval_count 30 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.441 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_type 'analytical (Ibers, 1978)' _exptl_crystal_colour 'yellow brown semi-transparent' _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_meas 1.71 _exptl_crystal_density_method ' flotation in bromoform/tetrachloromethane' _exptl_crystal_description 'hexagonal prism' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.88 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.65 _refine_ls_number_parameters 181 _refine_ls_number_reflns 3535 _refine_ls_R_factor_obs '[I>3\s(I)]=0.0486' _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F~o~) + (0.01F~o~)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0777 _reflns_number_observed 2564 _reflns_number_total 3535 _reflns_observed_criterion I>3\s(I) _cod_data_source_file mu1129.cif _cod_data_source_block mu1129a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F~o~) + (0.01F~o~)^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F~o~) + (0.01F~o~)^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2827(2) _cod_original_formula_sum 'C12 H18 Br1 N3 O1 Zn1' _cod_database_code 2003477 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z x,1/2-y,-z 1/2-x,-y,1/2+z -x,-y,-z 1/2+x,1/2-y,1/2+z -x,1/2+y,z 1/2+x,y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Zn .17337(3) .33766(8) .19157(3) .0406(2) Br .15464(3) .01938(7) .14605(3) .0554(2) O .1685(2) .3892(6) .2888(2) .051(1) N(1) .2788(2) .3148(7) .2022(2) .052(2) N(2) .2034(3) .5145(6) .1086(2) .058(2) N(3) .0761(2) .4386(7) .1805(3) .056(2) C(1) .3135(4) .4398(10) .1549(4) .070(3) C(2) .2739(4) .4563(11) .0920(4) .078(3) C(3) .1590(5) .5026(10) .0494(4) .084(3) C(4) .0884(4) .5644(9) .0642(4) .080(3) C(5) .0480(4) .4382(9) .1124(4) .079(3) C(6) .0395(3) .5010(8) .2302(4) .066(3) C(7) .0572(3) .5125(7) .2991(4) .057(2) C(8) .0084(4) .5853(9) .3441(5) .092(3) C(9) .0200(6) .6012(12) .4115(6) .106(4) C(10) .0795(6) .5463(11) .4361(5) .097(4) C(11) .1280(4) .4725(9) .3954(3) .069(2) C(12) .1191(3) .4530(7) .3256(3) .050(2) H(1N1) .2922(2) .1897(7) .1938(2) .07(2) H(2N1) .2912(2) .3457(7) .2472(2) .09(2) H(1C1) .3185(3) .5594(10) .1749(4) .09(2) H(2C1) .3564(3) .3904(10) .1445(4) .07(2) H(1C2) .2731(4) .3396(11) .0693(4) .08(2) H(2C2) .2937(4) .5469(11) .0633(4) .09(2) H(1C3) .1585(5) .3782(10) .0330(4) .07(2) H(2C3) .1768(5) .5761(10) .0137(4) .10(3) H(1C4) .0646(4) .5779(9) .0229(4) .08(2) H(2C4) .0891(4) .6878(9) .0818(4) .11(3) H(1C5) .0478(4) .3144(9) .0953(4) .09(2) H(2C5) .0028(4) .4794(9) .1141(4) .07(2) H(C6) -.0040(3) .5438(8) .2186(4) .09(2) H(N2) .2036(3) .6387(6) .1253(2) .04(1) H(C8) -.0337(4) .6250(9) .3270(5) .08(2) H(C9) -.0133(6) .6508(12) .4407(6) .13(3) H(C10) .0870(6) .5588(11) .4834(5) .10(3) H(C11) .1695(4) .4333(9) .4141(3) .10(3) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br Zn O . . 121.4(2) yes Br Zn N(1) . . 96.5(2) yes Br Zn N(2) . . 107.9(2) yes Br Zn N(3) . . 98.2(2) yes O Zn N(1) . . 88.1(2) yes O Zn N(2) . . 130.4(3) yes O Zn N(3) . . 89.5(2) yes N(1) Zn N(2) . . 81.1(2) yes N(1) Zn N(3) . . 164.1(3) yes N(2) Zn N(3) . . 88.6(2) yes Zn N(1) C(1) . . 110.9(3) yes N(1) C(1) C(2) . . 109.4(4) yes C(1) C(2) N(2) . . 109.9(4) yes C(2) N(2) Zn . . 105.2(3) yes C(3) N(2) Zn . . 113.8(4) yes C(2) N(2) C(3) . . 112.0(4) yes N(2) C(3) C(4) . . 113.1(6) yes C(3) C(4) C(5) . . 115.9(7) yes C(4) C(5) N(3) . . 111.6(6) yes C(5) N(3) Zn . . 117.0(5) yes C(5) N(3) C(6) . . 118.8(6) yes C(6) N(3) Zn . . 124.2(5) yes N(3) C(6) C(7) . . 127.5(8) yes C(6) C(7) C(12) . . 124.2(8) yes C(6) C(7) C(8) . . 117.2(7) yes C(8) C(7) C(12) . . 118.7(7) yes C(7) C(8) C(9) . . 122.1(6) yes C(8) C(9) C(10) . . 118.8(7) yes C(9) C(10) C(11) . . 121.7(10) yes C(10) C(11) C(12) . . 122.0(10) yes C(11) C(12) C(7) . . 116.6(9) yes C(7) C(12) O . . 124.1(8) yes C(11) C(12) O . . 119.2(9) yes C(12) O Zn . . 130.5(5) yes Br H(2N1) N(1) 2_545 2_545 162.1(5) yes O H(1N1) N(1) 2_555 2_555 161.1(6) yes 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 Zn Br . 2.4812(7) yes Zn O . 1.958(5) yes Zn N(1) . 2.122(5) yes Zn N(2) . 2.158(6) yes Zn N(3) . 2.082(6) yes N(1) C(1) . 1.469(5) yes C(1) C(2) . 1.476(7) yes C(2) N(2) . 1.502(6) yes N(2) C(3) . 1.469(8) yes C(3) C(4) . 1.506(11) yes C(4) C(5) . 1.541(11) yes C(5) N(3) . 1.458(9) yes N(3) C(6) . 1.302(9) yes C(6) C(7) . 1.409(11) yes C(7) C(8) . 1.419(11) yes C(8) C(9) . 1.355(11) yes C(9) C(10) . 1.342(10) yes C(10) C(11) . 1.367(14) yes C(11) C(12) . 1.398(14) yes C(7) C(12) . 1.407(13) yes C(12) O . 1.307(10) yes Br N(1) 2_545 3.593(5) yes Br H(2N1) 2_545 2.677(8) yes O N(1) 2_555 3.233(8) yes O H(1N1) 2_555 2.319(7) yes O N(1) . 2.839(9) yes O H(2N1) . 2.602(6) yes