#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/35/2203505.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_2203505 loop_ _publ_author_name 'Ernest Me\O)bis(1-phenylbutane-1,3-dionato-\k^2^O,O')nickel(II) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m367 _journal_page_last m369 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Ni (C10 H9 O2)2 (C2 H6 O S)2]' _chemical_formula_moiety 'C24 H30 Ni O6 S2' _chemical_formula_sum 'C24 H30 Ni O6 S2' _chemical_formula_weight 537.31 _chemical_name_systematic ;Bis(dimethyl sulfoxide-\kO)bis(1-phenylbutane-1,3-dionate-\k^2^O,O')nickel(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 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 92.026(18) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.3772(17) _cell_length_b 13.453(2) _cell_length_c 12.085(2) _cell_measurement_reflns_used 5096 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 21.3 _cell_measurement_theta_min 2.1 _cell_volume 1198.6(4) _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2003) ; _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2003) ; _computing_data_reduction ; CrysAlis RED ; _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; WinGX (Farrugia, 1999) and PARST97 (Nardelli, 1995) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100.00(10) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur CCD ; _diffrn_measurement_method \w _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 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 32533 _diffrn_reflns_theta_full 30.07 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_min 4.10 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number '3 frames' _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(Alcock, 1970)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 564 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.574 _refine_diff_density_min -0.319 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 3516 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.950 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0351 _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^)+(0.0219P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.0637 _reflns_number_gt 2561 _reflns_number_total 3516 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wk6011.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_original_cell_volume 1198.7(4) _cod_database_code 2203505 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' 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' Ni Ni 0.3393 1.1124 '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' 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_type_symbol Ni -0.5000 0.0000 0.5000 0.01175(9) Uani d S 1 Ni O12 -0.57523(16) -0.12538(9) 0.57711(10) 0.0143(3) Uani d . 1 O O11 -0.42381(16) 0.05995(9) 0.64556(10) 0.0142(3) Uani d . 1 O O2 -0.23567(17) -0.05838(9) 0.49094(10) 0.0156(3) Uani d . 1 O S2 -0.16864(6) -0.11127(4) 0.38974(4) 0.01535(11) Uani d . 1 S C21 -0.0646(3) -0.01827(14) 0.30905(16) 0.0213(5) Uani d . 1 C H21B 0.0288 0.0143 0.3529 0.032 Uiso calc R 1 H H21A -0.1540 0.0296 0.2850 0.032 Uiso calc R 1 H H21C -0.0123 -0.0485 0.2457 0.032 Uiso calc R 1 H C22 0.0312(2) -0.17378(14) 0.43539(16) 0.0183(4) Uani d . 1 C H22C -0.0001 -0.2295 0.4804 0.028 Uiso calc R 1 H H22B 0.1071 -0.1290 0.4781 0.028 Uiso calc R 1 H H22A 0.0952 -0.1967 0.3725 0.028 Uiso calc R 1 H C11 -0.6024(3) -0.24838(14) 0.71412(16) 0.0199(4) Uani d . 1 C H11A -0.6916 -0.2751 0.6626 0.030 Uiso calc R 1 H H11C -0.6515 -0.2457 0.7866 0.030 Uiso calc R 1 H H11B -0.4967 -0.2901 0.7159 0.030 Uiso calc R 1 H C12 -0.5510(2) -0.14487(14) 0.67841(16) 0.0150(4) Uani d . 1 C C13 -0.4801(2) -0.07943(14) 0.75847(15) 0.0159(4) Uani d . 1 C H13 -0.4732 -0.1019 0.8313 0.019 Uiso calc R 1 H C14 -0.4186(2) 0.01675(14) 0.73870(14) 0.0132(4) Uani d . 1 C C15 -0.3386(2) 0.07743(15) 0.83229(15) 0.0150(4) Uani d . 1 C C16 -0.2716(3) 0.03618(17) 0.93050(16) 0.0263(5) Uani d . 1 C H16 -0.2812 -0.0319 0.9423 0.032 Uiso calc R 1 H C17 -0.1906(3) 0.09593(19) 1.01094(17) 0.0333(6) Uani d . 1 C H17 -0.1454 0.0677 1.0765 0.040 Uiso calc R 1 H C18 -0.1761(3) 0.19714(18) 0.99491(17) 0.0293(5) Uani d . 1 C H18 -0.1213 0.2368 1.0495 0.035 Uiso calc R 1 H C19 -0.2425(3) 0.23897(16) 0.89860(17) 0.0252(5) Uani d . 1 C H19 -0.2337 0.3072 0.8875 0.030 Uiso calc R 1 H C110 -0.3227(2) 0.17923(15) 0.81806(16) 0.0186(4) Uani d . 1 C H110 -0.3671 0.2080 0.7526 0.022 Uiso calc R 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 Ni 0.01212(16) 0.01274(19) 0.01040(17) -0.00004(15) 0.00074(12) -0.00066(15) O12 0.0155(6) 0.0140(7) 0.0136(7) -0.0005(5) 0.0011(5) 0.0002(5) O11 0.0173(7) 0.0133(7) 0.0120(7) 0.0001(6) -0.0001(5) 0.0010(6) O2 0.0134(6) 0.0196(8) 0.0140(7) 0.0023(6) 0.0009(5) -0.0039(6) S2 0.0122(2) 0.0167(3) 0.0172(2) 0.0000(2) 0.00126(18) -0.0035(2) C21 0.0193(10) 0.0251(13) 0.0197(10) 0.0073(9) 0.0041(8) 0.0068(9) C22 0.0176(10) 0.0152(11) 0.0225(11) 0.0041(8) 0.0039(8) 0.0031(9) C11 0.0205(10) 0.0186(11) 0.0206(11) -0.0015(9) 0.0003(8) 0.0033(9) C12 0.0099(8) 0.0157(11) 0.0196(10) 0.0033(8) 0.0032(7) 0.0027(8) C13 0.0171(9) 0.0174(11) 0.0131(10) 0.0013(8) 0.0005(7) 0.0032(8) C14 0.0084(8) 0.0190(12) 0.0124(9) 0.0042(8) 0.0013(7) -0.0014(8) C15 0.0118(9) 0.0205(11) 0.0129(9) -0.0002(8) 0.0023(7) -0.0029(8) C16 0.0306(12) 0.0291(13) 0.0189(11) -0.0059(10) -0.0035(9) 0.0031(9) C17 0.0363(13) 0.0505(17) 0.0125(11) -0.0073(12) -0.0068(9) 0.0033(10) C18 0.0249(11) 0.0438(16) 0.0193(11) -0.0100(11) 0.0016(9) -0.0132(10) C19 0.0231(11) 0.0255(13) 0.0272(12) -0.0041(9) 0.0031(9) -0.0093(10) C110 0.0163(9) 0.0229(12) 0.0165(10) 0.0010(9) -0.0003(8) -0.0032(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni O11 1.9978(12) yes Ni O12 2.0145(13) yes Ni O2 2.1087(13) yes O12 C12 1.259(2) yes O11 C14 1.266(2) yes O2 S2 1.5131(13) yes S2 C22 1.7688(18) yes S2 C21 1.7772(19) yes C21 H21B 0.9600 ? C21 H21A 0.9600 ? C21 H21C 0.9600 ? C22 H22C 0.9600 ? C22 H22B 0.9600 ? C22 H22A 0.9600 ? C11 C12 1.510(3) yes C11 H11A 0.9600 ? C11 H11C 0.9600 ? C11 H11B 0.9600 ? C12 C13 1.396(3) yes C13 C14 1.394(2) yes C13 H13 0.9300 ? C14 C15 1.499(2) yes C15 C16 1.385(3) yes C15 C110 1.386(3) yes C16 C17 1.381(3) yes C16 H16 0.9300 ? C17 C18 1.380(3) yes C17 H17 0.9300 ? C18 C19 1.368(3) yes C18 H18 0.9300 ? C19 C110 1.379(3) yes C19 H19 0.9300 ? C110 H110 0.9300 ? 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 O11 Ni O12 90.24(5) yes O11 Ni O2 87.95(5) yes O12 Ni O2 89.00(5) yes C12 O12 Ni 126.33(12) yes C14 O11 Ni 126.60(12) yes S2 O2 Ni 123.12(7) yes O2 S2 C22 105.31(8) yes O2 S2 C21 105.80(9) yes C22 S2 C21 97.72(9) yes S2 C21 H21B 109.5 ? S2 C21 H21A 109.5 ? H21B C21 H21A 109.5 ? S2 C21 H21C 109.5 ? H21B C21 H21C 109.5 ? H21A C21 H21C 109.5 ? S2 C22 H22C 109.5 ? S2 C22 H22B 109.5 ? H22C C22 H22B 109.5 ? S2 C22 H22A 109.5 ? H22C C22 H22A 109.5 ? H22B C22 H22A 109.5 ? C12 C11 H11A 109.5 ? C12 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? C12 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? H11C C11 H11B 109.5 ? O12 C12 C13 125.43(18) yes O12 C12 C11 116.20(17) yes C13 C12 C11 118.37(17) yes C14 C13 C12 125.63(17) yes C14 C13 H13 117.2 ? C12 C13 H13 117.2 ? O11 C14 C13 125.34(16) yes O11 C14 C15 114.80(16) yes C13 C14 C15 119.86(16) yes C16 C15 C110 118.23(18) yes C16 C15 C14 123.18(18) yes C110 C15 C14 118.52(16) yes C17 C16 C15 120.1(2) yes C17 C16 H16 119.9 ? C15 C16 H16 119.9 ? C18 C17 C16 120.6(2) yes C18 C17 H17 119.7 ? C16 C17 H17 119.7 ? C19 C18 C17 119.9(2) yes C19 C18 H18 120.1 ? C17 C18 H18 120.1 ? C18 C19 C110 119.5(2) yes C18 C19 H19 120.2 ? C110 C19 H19 120.2 ? C19 C110 C15 121.63(19) yes C19 C110 H110 119.2 ? C15 C110 H110 119.2 ? _cod_database_fobs_code 2203505 _journal_paper_doi 10.1107/S1600536804004854