#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/11/2011197.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_2011197 loop_ _publ_author_name 'Yilmaz, Veysel T.' 'Karada\(g, Ahmet' 'Th\"one, Carsten' 'Herbst-Irmer, Regine' _publ_section_title ; trans-Bis(diethanolamine)bis(isothiocyanato)nickel(II) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 948 _journal_page_last 949 _journal_paper_doi 10.1107/S0108270100007289 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Ni(SCN)2 (C4 H11 NO2 )2 ]' _chemical_formula_moiety 'C10 H22 N4 Ni O4 S2' _chemical_formula_sum 'C10 H22 N4 Ni O4 S2' _chemical_formula_weight 385.15 _chemical_melting_point 476 _chemical_name_common Bis(diethanolamine)bis(isothiocyanato)nickel(II) _chemical_name_systematic ; Bis(2,2\'-iminodiethanol)bis(isothiocyanato)nickel(II) ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.119(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.8157(8) _cell_length_b 8.3508(10) _cell_length_c 14.725(2) _cell_measurement_reflns_used 62 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 4 _cell_volume 825.06(18) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Fait, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics 'XP (Siemens, 1994b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full .831 _diffrn_measured_fraction_theta_max .831 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method Omega-scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0640 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 1568 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.11 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 247 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_T_max .7980 _exptl_absorpt_correction_T_min .7730 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(XEMP; Siemens 1994a)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'square prism' _exptl_crystal_F_000 404 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .14 _refine_diff_density_max .352 _refine_diff_density_min -.361 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .929 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1568 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .929 _refine_ls_R_factor_all .0628 _refine_ls_R_factor_gt .0335 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0316P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0711 _reflns_number_gt 1072 _reflns_number_total 1568 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bm1413.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Psi-scan' changed to 'psi-scan' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 825.08(18) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2011197 _cod_database_fobs_code 2011197 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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ni1 .0000 .5000 .5000 .01420(14) Uani d S 1 . . Ni S1 .22997(14) .15137(11) .27554(6) .0283(2) Uani d . 1 . . S O1 .2858(3) .5809(3) .55181(15) .0193(5) Uani d . 1 . . O H1 .294(6) .606(4) .599(3) .033(12) Uiso d . 1 . . H N2 -.0050(4) .6987(3) .41268(16) .0170(6) Uani d . 1 . . N H2 .036(5) .661(3) .364(2) .018(8) Uiso d . 1 . . H N1 .1135(4) .3647(3) .40347(16) .0201(6) Uani d . 1 . . N C1 .1627(5) .2782(4) .35009(19) .0170(7) Uani d . 1 . . C C21 -.2004(5) .7761(4) .3828(2) .0208(7) Uani d . 1 . . C H21A -.2393 .8307 .4366 .025 Uiso calc R 1 . . H H21B -.3007 .6917 .3626 .025 Uiso calc R 1 . . H C12 .1540(5) .8078(4) .4576(2) .0225(7) Uani d . 1 . . C H12A .1085 .8666 .5085 .027 Uiso calc R 1 . . H H12B .1862 .8870 .4124 .027 Uiso calc R 1 . . H C22 -.2075(5) .8970(4) .3053(2) .0246(8) Uani d . 1 . . C H22A -.3434 .9423 .2894 .030 Uiso calc R 1 . . H H22B -.1138 .9858 .3257 .030 Uiso calc R 1 . . H C11 .3379(5) .7089(4) .4952(2) .0239(7) Uani d . 1 . . C H11A .3951 .6640 .4434 .029 Uiso calc R 1 . . H H11B .4398 .7781 .5322 .029 Uiso calc R 1 . . H O2 -.1544(4) .8212(3) .22578(15) .0344(7) Uani d . 1 . . O H3 -.033(6) .805(5) .233(3) .044(12) Uiso d . 1 . . 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 .0146(3) .0177(3) .0105(2) -.0007(3) .00266(19) -.0007(3) S1 .0324(5) .0274(5) .0295(4) -.0063(4) .0179(4) -.0111(4) O1 .0195(12) .0240(13) .0140(10) -.0031(11) .0019(10) .0011(9) N2 .0171(14) .0220(15) .0126(11) .0002(13) .0046(11) .0013(10) N1 .0219(15) .0232(15) .0163(12) -.0016(13) .0065(11) .0013(11) C1 .0151(15) .0206(17) .0155(13) -.0012(14) .0027(12) .0022(13) C21 .0199(16) .0221(18) .0201(14) .0027(15) .0026(13) .0015(13) C12 .0240(18) .0218(18) .0205(14) -.0059(16) .0005(14) .0050(13) C22 .0208(18) .0294(19) .0231(15) .0010(16) .0022(14) .0070(14) C11 .0177(16) .0298(19) .0231(15) -.0081(16) .0008(13) .0058(14) O2 .0238(14) .0579(19) .0205(11) .0124(14) .0015(11) .0128(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ni1 N1 . 3_566 180.00(9) ? N1 Ni1 N2 . . 88.78(10) y N1 Ni1 O1 . 3_566 90.56(10) ? N1 Ni1 O1 3_566 3_566 89.44(10) ? N1 Ni1 O1 . . 89.44(10) y N1 Ni1 O1 3_566 . 90.56(10) ? O1 Ni1 O1 3_566 . 180.0 ? N1 Ni1 N2 3_566 . 91.22(10) ? O1 Ni1 N2 3_566 . 96.84(9) ? N2 Ni1 O1 . . 83.16(9) y N1 Ni1 N2 . 3_566 91.22(10) ? N1 Ni1 N2 3_566 3_566 88.78(10) ? O1 Ni1 N2 3_566 3_566 83.16(9) ? O1 Ni1 N2 . 3_566 96.84(9) ? N2 Ni1 N2 . 3_566 180.0000(10) ? Ni1 O1 C11 . . 109.89(18) y C21 N2 C12 . . 114.5(3) y Ni1 N2 C21 . . 116.5(2) y Ni1 N2 C12 . . 106.34(18) y Ni1 N1 C1 . . 173.4(3) y N1 C1 S1 . . 178.5(3) y N2 C21 C22 . . 115.0(3) ? N2 C12 C11 . . 108.7(3) ? O2 C22 C21 . . 110.0(3) y O1 C11 C12 . . 110.0(3) y 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 N1 . 2.069(3) y Ni1 N1 3_566 2.069(3) ? Ni1 N2 . 2.096(2) y Ni1 O1 3_566 2.076(2) ? Ni1 O1 . 2.076(2) y Ni1 N2 3_566 2.096(2) ? S1 C1 . 1.647(3) y O1 C11 . 1.438(4) y N2 C21 . 1.476(4) y N2 C12 . 1.480(4) y N1 C1 . 1.159(4) y C21 C22 . 1.518(4) y C12 C11 . 1.522(4) y C22 O2 . 1.432(4) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1 H1 O2 4_676 .72(4) 1.93(4) 2.651(3) 174(5) N2 H2 S1 2 .88(3) 2.81(3) 3.630(3) 156(3) O2 H3 S1 2 .83(4) 2.45(4) 3.225(3) 156(4) 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_site_symmetry_1 _geom_torsion N1 Ni1 O1 C11 . 80.9(2) N1 Ni1 O1 C11 3_566 -99.1(2) O1 Ni1 O1 C11 3_566 10E1(10) N2 Ni1 O1 C11 . -8.0(2) N2 Ni1 O1 C11 3_566 172.0(2) N1 Ni1 N2 C21 . 121.7(2) N1 Ni1 N2 C21 3_566 -58.3(2) O1 Ni1 N2 C21 3_566 31.3(2) O1 Ni1 N2 C21 . -148.7(2) N2 Ni1 N2 C21 3_566 -12E1(10) N1 Ni1 N2 C12 . -109.3(2) N1 Ni1 N2 C12 3_566 70.7(2) O1 Ni1 N2 C12 3_566 160.3(2) O1 Ni1 N2 C12 . -19.7(2) N2 Ni1 N2 C12 3_566 1E1(10) N1 Ni1 N1 C1 3_566 12E1(10) O1 Ni1 N1 C1 3_566 -33(2) O1 Ni1 N1 C1 . 147(2) N2 Ni1 N1 C1 . -130(2) N2 Ni1 N1 C1 3_566 50(2) Ni1 N1 C1 S1 . -26(13) C12 N2 C21 C22 . 66.8(3) Ni1 N2 C21 C22 . -168.2(2) C21 N2 C12 C11 . 173.0(2) Ni1 N2 C12 C11 . 42.9(3) N2 C21 C22 O2 . 59.0(4) Ni1 O1 C11 C12 . 33.9(3) N2 C12 C11 O1 . -52.3(3)