#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/07/2200771.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_2200771 loop_ _publ_author_name '\;Cakir, Semiha' 'Naumov, Pan\o-sulfobenzimidato-N)cadmium(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m431 _journal_page_last m432 _journal_paper_doi 10.1107/S1600536801014453 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cd (C7 H4 N O3 S)2, (C6 H6 N2 O)2 (H2 O)2]' _chemical_formula_moiety 'C26 H24 Cd N6 O10 S2' _chemical_formula_sum 'C26 H24 Cd N6 O10 S2' _chemical_formula_weight 757.03 _chemical_name_systematic ; Diaquabis(nicotinamide)bis(o-sulfobenzimidato-N)cadmium(II) ; _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 'Manual editing of SHELXL-97 cif' _cell_angle_alpha 90.00 _cell_angle_beta 106.0410(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.65470(10) _cell_length_b 19.1163(2) _cell_length_c 10.82850(10) _cell_measurement_reflns_used 8192 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.33 _cell_measurement_theta_min 2.13 _cell_volume 1522.83(3) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full .981 _diffrn_measured_fraction_theta_max .981 _diffrn_measurement_device_type 'Siemens CCD area-detector' _diffrn_measurement_method '\w scan' _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 .0646 _diffrn_reflns_av_sigmaI/netI .0644 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 10747 _diffrn_reflns_theta_full 28.33 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_min 2.13 _exptl_absorpt_coefficient_mu .919 _exptl_absorpt_correction_T_max .8668 _exptl_absorpt_correction_T_min .7451 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Parallelepiped _exptl_crystal_F_000 764 _exptl_crystal_size_max .34 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .16 _refine_diff_density_max .514 _refine_diff_density_min -1.482 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .985 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 3731 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .985 _refine_ls_R_factor_all .0455 _refine_ls_R_factor_gt .0372 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0431P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0958 _reflns_number_gt 3068 _reflns_number_total 3731 _reflns_threshold_expression I>2\s(I) _cod_data_source_file wn6051.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical' 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_sg_symbol_H-M 'P 21/c' _cod_database_code 2200771 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_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 Cd1 .5000 .5000 .5000 .02530(10) Uani d S 1 . . Cd S1 .55820(8) .34077(3) .66052(6) .0294(2) Uani d . 1 . . S O1 .4791(3) .37020(10) .7551(2) .0460(10) Uani d . 1 . . O O2 .4365(3) .30130(10) .5619(2) .0570(10) Uani d . 1 . . O O3 .9463(3) .42630(10) .5881(2) .0450(10) Uani d . 1 . . O O4 .9333(4) .4898(2) .1474(3) .0930(10) Uani d . 1 . . O O1w .7820(3) .55300(10) .5312(2) .0410(10) Uani d . 1 . . O N1 .6595(3) .40160(10) .6010(2) .0280(10) Uani d . 1 . . N N2 .5082(3) .45190(10) .2998(2) .0320(10) Uani d . 1 . . N N3 .7929(4) .4435(2) -.0434(3) .0600(10) Uani d . 1 . . N C1 .7538(3) .29260(10) .7341(2) .0330(10) Uani d . 1 . . C C2 .7736(5) .2331(2) .8101(3) .0550(10) Uani d . 1 . . C C3 .9479(6) .2073(2) .8558(4) .0730(10) Uani d . 1 . . C C4 1.0943(5) .2391(2) .8277(4) .0700(10) Uani d . 1 . . C C5 1.0728(4) .2990(2) .7533(3) .0530(10) Uani d . 1 . . C C6 .8985(3) .32520(10) .7060(2) .0320(10) Uani d . 1 . . C C7 .8401(3) .38910(10) .6261(2) .0300(10) Uani d . 1 . . C C8 .3753(4) .4083(2) .2374(3) .0450(10) Uani d . 1 . . C C9 .3729(5) .3773(2) .1225(3) .0590(10) Uani d . 1 . . C C10 .5102(5) .3917(2) .0666(3) .0530(10) Uani d . 1 . . C C11 .6476(4) .4370(2) .1283(3) .0370(10) Uani d . 1 . . C C12 .6409(4) .4650(2) .2449(3) .0340(10) Uani d . 1 . . C C13 .8030(4) .4586(2) .0770(3) .0500(10) Uani d . 1 . . C H1w1 .828(6) .570(2) .482(4) .070(10) Uiso d . 1 . . H H1w2 .853(7) .524(3) .554(5) .08(2) Uiso d . 1 . . H H1n1 .877(4) .456(2) -.072(3) .040(10) Uiso d . 1 . . H H1n2 .697(5) .423(2) -.095(4) .060(10) Uiso d . 1 . . H H2 .675(5) .212(2) .826(4) .070(10) Uiso d . 1 . . H H3 .975(6) .165(2) .907(4) .090(10) Uiso d . 1 . . H H4 1.215(6) .224(3) .863(4) .11(2) Uiso d . 1 . . H H5 1.167(5) .326(2) .729(3) .050(10) Uiso d . 1 . . H H8 .279(4) .401(2) .271(3) .040(10) Uiso d . 1 . . H H9 .284(6) .345(2) .084(4) .080(10) Uiso d . 1 . . H H10 .515(4) .370(2) -.005(3) .060(10) Uiso d . 1 . . H H12 .728(6) .496(2) .284(4) .050(10) 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 Cd1 .02590(10) .0294(2) .0244(2) .00250(10) .01320(10) .00310(10) S1 .0222(3) .0331(3) .0303(3) -.0036(2) .0032(2) .0062(2) O1 .0360(10) .0580(10) .0540(10) -.0020(10) .0270(10) .0090(10) O2 .0460(10) .0530(10) .0560(10) -.0150(10) -.0160(10) .0020(10) O3 .0350(10) .0490(10) .0610(10) .0020(10) .0310(10) .0110(10) O4 .071(2) .168(3) .055(2) -.068(2) .042(2) -.052(2) O1w .0330(10) .0460(10) .0520(10) -.0020(10) .0250(10) .0070(10) N1 .0250(10) .0310(10) .0310(10) .0020(10) .0120(10) .0090(10) N2 .0370(10) .0360(10) .0270(10) .0030(10) .0170(10) .0020(10) N3 .057(2) .093(2) .041(2) -.028(2) .0340(10) -.024(2) C1 .0320(10) .0350(10) .0300(10) .0030(10) .0030(10) .0060(10) C2 .056(2) .050(2) .056(2) .002(2) .010(2) .023(2) C3 .074(3) .067(2) .070(3) .025(2) .007(2) .036(2) C4 .051(2) .082(3) .068(2) .032(2) -.001(2) .024(2) C5 .033(2) .068(2) .056(2) .013(2) .0090(10) .009(2) C6 .0290(10) .0370(10) .0310(10) .0060(10) .0070(10) .0040(10) C7 .0290(10) .0340(10) .0300(10) .0030(10) .0140(10) .0010(10) C8 .047(2) .057(2) .039(2) -.0120(10) .0270(10) -.0070(10) C9 .065(2) .074(2) .046(2) -.032(2) .028(2) -.022(2) C10 .063(2) .064(2) .040(2) -.021(2) .029(2) -.020(2) C11 .0400(10) .045(2) .0340(10) -.0030(10) .0210(10) -.0060(10) C12 .0370(10) .040(2) .0290(10) -.0020(10) .0160(10) -.0040(10) C13 .048(2) .073(2) .039(2) -.013(2) .0280(10) -.017(2) 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' Cd Cd -.8075 1.2024 '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 O1w Cd1 O1w . 3_666 180.000(10) yes O1w Cd1 N1 . . 86.51(8) yes O1w Cd1 N1 . 3_666 93.49(8) yes O1w Cd1 N2 . . 92.50(8) yes O1w Cd1 N2 . 3_666 87.50(8) yes O1w Cd1 N1 3_666 . 93.49(8) no O1w Cd1 N1 3_666 3_666 86.51(8) no O1w Cd1 N2 3_666 . 87.50(8) no O1w Cd1 N2 3_666 3_666 92.50(8) no N1 Cd1 N1 . 3_666 180.0 yes N1 Cd1 N2 . . 88.49(7) yes N1 Cd1 N2 . 3_666 91.51(7) yes N1 Cd1 N2 3_666 3_666 88.49(7) no N1 Cd1 N2 3_666 . 91.51(7) no N2 Cd1 N2 . 3_666 180.0 yes O2 S1 O1 . . 115.10(10) yes O2 S1 N1 . . 111.50(10) no O1 S1 N1 . . 110.00(10) no O2 S1 C1 . . 111.20(10) no O1 S1 C1 . . 110.90(10) no N1 S1 C1 . . 96.60(10) yes C7 N1 S1 . . 111.5(2) yes C7 N1 Cd1 . . 127.3(2) no S1 N1 Cd1 . . 121.00(10) no C12 N2 C8 . . 117.1(2) no C12 N2 Cd1 . . 123.4(2) no C8 N2 Cd1 . . 119.5(2) no C6 C1 C2 . . 122.7(3) no C6 C1 S1 . . 107.5(2) no C2 C1 S1 . . 129.8(2) no C3 C2 C1 . . 116.2(3) no C2 C3 C4 . . 121.8(3) no C5 C4 C3 . . 121.3(3) no C4 C5 C6 . . 117.6(3) no C1 C6 C5 . . 120.4(3) no C1 C6 C7 . . 111.7(2) no C5 C6 C7 . . 127.9(3) no O3 C7 N1 . . 124.2(2) no O3 C7 C6 . . 123.1(2) no N1 C7 C6 . . 112.7(2) yes N2 C8 C9 . . 122.9(3) no C8 C9 C10 . . 119.3(3) no C9 C10 C11 . . 118.9(3) no C12 C11 C10 . . 117.9(3) no C12 C11 C13 . . 117.6(3) no C10 C11 C13 . . 124.6(3) no N2 C12 C11 . . 123.9(3) no O4 C13 N3 . . 122.4(3) no O4 C13 C11 . . 119.6(3) no N3 C13 C11 . . 118.0(3) no Cd1 O1w H1w1 . . 131(3) no Cd1 O1w H1w2 . . 107(4) no H1w1 O1w H1w2 . . 95(4) no C13 N3 H1n1 . . 118(2) no C13 N3 H1n2 . . 122(2) no H1n1 N3 H1n2 . . 120(3) no C3 C2 H2 . . 122(2) no C1 C2 H2 . . 121(2) no C2 C3 H3 . . 122(3) no C4 C3 H3 . . 116(3) no C5 C4 H4 . . 116(3) no C3 C4 H4 . . 122(3) no C4 C5 H5 . . 128(2) no C6 C5 H5 . . 115(2) no N2 C8 H8 . . 118(2) no C9 C8 H8 . . 119(2) no C8 C9 H9 . . 121(3) no C10 C9 H9 . . 120(3) no C9 C10 H10 . . 120(2) no C11 C10 H10 . . 121(2) no N2 C12 H12 . . 118(3) no C11 C12 H12 . . 118(3) no 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 Cd1 O1w . 2.323(2) yes Cd1 O1w 3_666 2.323(2) no Cd1 N1 . 2.343(2) yes Cd1 N1 3_666 2.343(2) no Cd1 N2 . 2.371(2) yes Cd1 N2 3_666 2.371(2) no S1 O1 . 1.441(2) yes S1 O2 . 1.424(2) yes S1 N1 . 1.626(2) yes S1 C1 . 1.751(3) no O3 C7 . 1.233(3) yes O4 C13 . 1.229(4) no N1 C7 . 1.355(3) yes N2 C12 . 1.335(3) no N2 C8 . 1.344(4) no N3 C13 . 1.317(4) no C1 C6 . 1.376(4) no C1 C2 . 1.387(4) no C2 C3 . 1.380(5) no C3 C4 . 1.381(6) no C4 C5 . 1.383(5) no C5 C6 . 1.384(4) no C6 C7 . 1.492(4) no C8 C9 . 1.374(4) no C9 C10 . 1.378(5) no C10 C11 . 1.383(4) no C11 C12 . 1.385(4) no C11 C13 . 1.503(4) no O1w H1w1 . .78(4) no O1w H1w2 . .77(5) no N3 H1n1 . .82(3) no N3 H1n2 . .88(4) no C2 H2 . .92(4) no C3 H3 . .97(5) no C4 H4 . .94(5) no C5 H5 . .98(3) no C8 H8 . .91(3) no C9 H9 . .93(4) no C10 H10 . .89(4) no C12 H12 . .90(4) no 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 _geom_hbond_publ_flag O1w H1w2 O3 . .77(5) 2.00(5) 2.720(3) 156(5) yes O1w H1w1 O3 3_766 .78(4) 2.07(5) 2.763(3) 147(4) yes N3 H1n2 O1 1_554 .88(4) 2.23(4) 3.098(4) 171(3) yes N3 H1n1 O4 3_765 .82(3) 2.12(3) 2.931(4) 167(3) yes 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 _geom_torsion_publ_flag O2 S1 N1 C7 . -113.3(2) no O1 S1 N1 C7 . 117.8(2) no C1 S1 N1 C7 . 2.6(2) no O2 S1 N1 Cd1 . 70.8(2) no O1 S1 N1 Cd1 . -58.1(2) no C1 S1 N1 Cd1 . -173.20(10) no O1w Cd1 N1 C7 3_666 166.4(2) no O1w Cd1 N1 C7 . -13.6(2) no N1 Cd1 N1 C7 3_666 4E1(10) no N2 Cd1 N1 C7 3_666 -101.0(2) no N2 Cd1 N1 C7 . 79.0(2) no O1w Cd1 N1 S1 3_666 -18.48(14) no O1w Cd1 N1 S1 . 161.50(10) no N1 Cd1 N1 S1 3_666 -15E1(10) no N2 Cd1 N1 S1 3_666 74.10(10) no N2 Cd1 N1 S1 . -105.88(13) no O1w Cd1 N2 C12 3_666 175.7(2) no O1w Cd1 N2 C12 . -4.3(2) no N1 Cd1 N2 C12 . -90.7(2) no N1 Cd1 N2 C12 3_666 89.3(2) no N2 Cd1 N2 C12 3_666 7E1(10) no O1w Cd1 N2 C8 3_666 -5.3(2) no O1w Cd1 N2 C8 . 174.7(2) no N1 Cd1 N2 C8 . 88.3(2) no N1 Cd1 N2 C8 3_666 -91.7(2) no N2 Cd1 N2 C8 3_666 -11E1(10) no O2 S1 C1 C6 . 114.3(2) no O1 S1 C1 C6 . -116.3(2) no N1 S1 C1 C6 . -1.9(2) no O2 S1 C1 C2 . -67.0(3) no O1 S1 C1 C2 . 62.5(3) no N1 S1 C1 C2 . 176.9(3) no C6 C1 C2 C3 . -.7(5) no S1 C1 C2 C3 . -179.3(3) no C1 C2 C3 C4 . .2(7) no C2 C3 C4 C5 . .7(8) no C3 C4 C5 C6 . -1.1(7) no C2 C1 C6 C5 . .3(5) no S1 C1 C6 C5 . 179.2(2) no C2 C1 C6 C7 . -178.2(3) no S1 C1 C6 C7 . .6(3) no C4 C5 C6 C1 . .6(5) no C4 C5 C6 C7 . 178.9(3) no S1 N1 C7 O3 . 177.7(2) no Cd1 N1 C7 O3 . -6.8(4) no S1 N1 C7 C6 . -2.6(3) no Cd1 N1 C7 C6 . 172.9(2) no C1 C6 C7 O3 . -179.1(3) no C5 C6 C7 O3 . 2.5(5) no C1 C6 C7 N1 . 1.2(3) no C5 C6 C7 N1 . -177.2(3) no C12 N2 C8 C9 . .6(5) no Cd1 N2 C8 C9 . -178.5(3) no N2 C8 C9 C10 . -1.0(6) no C8 C9 C10 C11 . .4(6) no C9 C10 C11 C12 . .7(5) no C9 C10 C11 C13 . -178.6(4) no C8 N2 C12 C11 . .6(4) no Cd1 N2 C12 C11 . 179.7(2) no C10 C11 C12 N2 . -1.3(5) no C13 C11 C12 N2 . 178.1(3) no C12 C11 C13 O4 . 12.4(5) no C10 C11 C13 O4 . -168.3(4) no C12 C11 C13 N3 . -167.1(3) no C10 C11 C13 N3 . 12.2(5) no