#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/05/2010548.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_2010548 loop_ _publ_author_name 'Goto, Masato' 'Kani, Yoshiyuki' 'Tsuchimoto, Masanobu' 'Ohba, Shigeru' 'Matsushima, Hideaki' 'Tokii, Tadashi' _publ_section_title ; Dimeric copper(II) 3,3-dimethylbutyrate adducts with ethanol, 2-methylpyridine, 3-methylpyridine, 4-methylpyridine and 3,3-dimethylbutyric acid ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 7 _journal_page_last 11 _journal_paper_doi 10.1107/S0108270199012172 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Cu2 (C6 H11 O2 )4 (C2 H6 O)2 ], 2C2 H6 O' _chemical_formula_moiety 'C32 H68 Cu2 O12' _chemical_formula_structural '(Cu2 (C6 H11 O2)4 (C2 H6 O1)2) (C2 H6 O1)2' _chemical_formula_sum 'C32 H68 Cu2 O12' _chemical_formula_weight 771.98 _chemical_name_systematic ; tetrakis(\m-3,3-dimethylbutyrato-O:O')di(ethanol-O)dicopper(II) diethanol solvate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source 'International Tables Vol.IV (1974)' _cell_angle_alpha 105.430(10) _cell_angle_beta 106.500(10) _cell_angle_gamma 88.430(10) _cell_formula_units_Z 1 _cell_length_a 10.765(2) _cell_length_b 10.923(2) _cell_length_c 9.8200(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 299 _cell_measurement_theta_max 15 _cell_measurement_theta_min 10 _cell_volume 1065.8(3) _computing_cell_refinement 'MSC/AFC Diffractometer Control System' _computing_data_collection 'MSC/AFC Diffractometer Control System (Molecular Structure Corporation, 1993)' _computing_data_reduction 'local programs' _computing_molecular_graphics CRYSTAN-GM _computing_publication_material CRYSTAN-GM _computing_structure_refinement CRYSTAN-GM _computing_structure_solution 'CRYSTAN-GM (Edwards et al., 1996)' _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \q-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .012 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5151 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_T_max .822 _exptl_absorpt_correction_T_min .569 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 414 _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _refine_diff_density_max 1.23 _refine_diff_density_min -.91 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.44 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 182 _refine_ls_number_reflns 3646 _refine_ls_R_factor_gt .076 _refine_ls_shift/esd_mean .0066 _refine_ls_shift/su_max .03 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.000225F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .077 _reflns_number_gt 3646 _reflns_number_total 4888 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _cod_data_source_file oa1094.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 17 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 -1 ' _cod_database_code 2010548 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z 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 Cu1 .0601(3) .0467(2) .0412(2) -.0018(2) .0177(2) .0113(2) O2 .100(2) .054(2) .0480(10) -.0120(10) .0230(10) .0060(10) O3 .092(2) .062(2) .0470(10) -.0150(10) .0260(10) .0050(10) O4 .062(2) .074(2) .077(2) .0090(10) .0260(10) .030(2) O5 .060(2) .084(2) .070(2) .0120(10) .0210(10) .0290(10) C9 .063(2) .055(2) .053(2) .000(2) .018(2) .006(2) C10 .094(3) .063(3) .064(2) -.015(2) .028(2) -.010(2) C11 .088(3) .080(3) .062(2) -.025(3) .008(2) -.002(2) C12 .124(5) .231(8) .108(4) -.095(5) .028(4) .023(5) C13 .176(6) .115(5) .091(4) -.070(4) .025(4) -.035(3) C14 .115(5) .136(6) .240(8) .010(4) -.044(5) .036(6) C15 .060(2) .054(2) .061(2) -.003(2) .013(2) -.002(2) C16 .054(2) .074(3) .106(3) .007(2) .015(2) .013(2) C17 .070(3) .074(3) .101(3) .018(2) .028(2) .015(3) C18 .096(4) .120(5) .225(7) .052(3) .066(4) .056(5) C19 .192(7) .113(5) .368(12) .073(5) .173(8) .132(7) C20 .290(10) .250(10) .11000 .140(10) -.020(10) -.090(10) 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_occupancy Cu1 .02105(4) .06067(4) -.08944(4) .0488(2) Uani 1.000 O2 .0647(3) .2026(2) .0917(2) .0690(10) Uani 1.000 O3 .0303(3) .0997(2) .2458(2) .0680(10) Uani 1.000 O4 .1980(2) .0055(2) -.0346(3) .0680(10) Uani 1.000 O5 .1632(2) -.0944(3) .1221(3) .0690(10) Uani 1.000 O6 .0498(3) .1655(3) -.2376(3) .0756(8) Uiso 1.000 O7 .8388(9) -.0560(10) .4540(10) .092(3) Uiso .300 O8 .9068(4) .1333(4) .4773(5) .0940(10) Uiso .700 C9 .0642(3) .1982(3) .2174(4) .059(2) Uani 1.000 C10 .1042(4) .3205(4) .3434(4) .078(2) Uani 1.000 C11 .2511(4) .3557(4) .3911(4) .083(2) Uani 1.000 C12 .2858(6) .3980(7) .2717(6) .158(4) Uani 1.000 C13 .2804(6) .4691(5) .5302(6) .142(3) Uani 1.000 C14 .3327(6) .2444(7) .4243(9) .186(5) Uani 1.000 C15 .2332(3) -.0563(3) .0581(4) .063(2) Uani 1.000 C16 .3759(4) -.0935(4) .0957(5) .082(2) Uani 1.000 C17 .3975(4) -.2353(4) .0360(5) .083(2) Uani 1.000 C18 .5459(5) -.2505(5) .0677(8) .142(4) Uani 1.000 C19 .3464(7) -.3136(6) .1160(10) .193(6) Uani 1.000 C20 .3314(9) -.2814(8) -.1239(7) .267(6) Uani 1.000 C21 .0953(7) .3153(7) -.1819(8) .170(3) Uiso 1.000 C22 -.0060(10) .4050(10) -.1800(10) .410(8) Uiso 1.000 C23 .7810(7) .0587(7) .4208(8) .156(2) Uiso 1.000 C24 .6912(8) .1071(8) .4862(9) .194(3) Uiso 1.000 H6 -.03180 .15845 -.31197 .30 Uiso 1.000 H10A .07951 .30996 .42632 .30 Uiso 1.000 H10B .05871 .38926 .31132 .30 Uiso 1.000 H12A .37751 .41772 .30070 .30 Uiso 1.000 H12B .24021 .47162 .25400 .30 Uiso 1.000 H12C .26271 .33002 .18250 .30 Uiso 1.000 H13A .37209 .48879 .55921 .30 Uiso 1.000 H13B .25559 .44959 .60891 .30 Uiso 1.000 H13C .23339 .53989 .50551 .30 Uiso 1.000 H14A .42442 .26406 .45326 .30 Uiso 1.000 H14B .31102 .17326 .33816 .30 Uiso 1.000 H14C .31082 .22166 .50286 .30 Uiso 1.000 H16A .41088 -.07132 .20107 .30 Uiso 1.000 H16B .42248 -.04462 .05637 .30 Uiso 1.000 H18A .55850 -.33891 .02931 .30 Uiso 1.000 H18B .58830 -.22341 .17181 .30 Uiso 1.000 H18C .58090 -.20011 .01941 .30 Uiso 1.000 H19A .35895 -.40206 .07733 .30 Uiso 1.000 H19B .25525 -.30056 .09913 .30 Uiso 1.000 H19C .38875 -.28756 .21983 .30 Uiso 1.000 H20A .34393 -.36976 -.16223 .30 Uiso 1.000 H20B .36733 -.23186 -.17243 .30 Uiso 1.000 H20C .24033 -.26816 -.14193 .30 Uiso 1.000 H21A .14494 .33432 -.24168 .30 Uiso 1.000 H21B .14944 .33172 -.08198 .30 Uiso 1.000 H22A .03074 .49018 -.14843 .30 Uiso 1.000 H22B -.05370 .38900 -.11620 .30 Uiso 1.000 H22C -.06460 .38880 -.27840 .30 Uiso 1.000 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 O2 Cu1 O3 . 2_555 168.90(10) yes O2 Cu1 O4 . . 89.7(2) no O2 Cu1 O5 . 2_555 90.1(2) no O2 Cu1 O6 . . 97.30(10) no O3 Cu1 O4 2_555 . 89.8(2) no O3 Cu1 O5 2_555 2_555 88.2(2) no O3 Cu1 O6 2_555 . 93.70(10) no O4 Cu1 O5 . 2_555 168.8(2) yes O4 Cu1 O6 . . 96.6(2) no O5 Cu1 O6 2_555 . 94.5(2) no Cu1 O2 C9 . . 126.6(3) no Cu1 O3 C9 2_555 . 120.5(3) no Cu1 O4 C15 . . 121.6(3) no Cu1 O5 C15 2_555 . 123.3(3) no Cu1 O6 C21 . . 122.4(3) no O2 C9 O3 . . 123.9(4) yes O2 C9 C10 . . 117.6(4) no O3 C9 C10 . . 118.4(3) no C9 C10 C11 . . 113.1(4) no C10 C11 C12 . . 109.6(4) no C10 C11 C13 . . 107.7(4) no C10 C11 C14 . . 112.0(4) no C12 C11 C13 . . 107.9(5) no C12 C11 C14 . . 109.7(5) no C13 C11 C14 . . 109.9(5) no O4 C15 O5 . . 126.2(4) yes O4 C15 C16 . . 117.6(4) no O5 C15 C16 . . 116.2(4) no C15 C16 C17 . . 115.5(4) no C16 C17 C18 . . 107.7(4) no C16 C17 C19 . . 110.2(5) no C16 C17 C20 . . 111.1(5) no C18 C17 C19 . . 108.1(5) no C18 C17 C20 . . 110.7(6) no C19 C17 C20 . . 108.9(6) no O6 C21 C22 . . 116.6(7) no O7 C23 O8 . . 93.8(6) no O7 C23 C24 . . 116.5(8) no O8 C23 C24 . . 115.1(7) no Cu1 O6 H6 . . 105.9 no C21 O6 H6 . . 106.0 no C9 C10 H10A . . 108.7 no C9 C10 H10B . . 108.6 no C11 C10 H10A . . 109.3 no C11 C10 H10B . . 108.1 no H10A C10 H10B . . 109.0 no C11 C12 H12A . . 109.3 no C11 C12 H12B . . 111.1 no C11 C12 H12C . . 108.8 no H12A C12 H12B . . 109.3 no H12A C12 H12C . . 109.3 no H12B C12 H12C . . 109.0 no C11 C13 H13A . . 106.6 no C11 C13 H13B . . 112.0 no C11 C13 H13C . . 108.7 no H13A C13 H13B . . 110.3 no H13A C13 H13C . . 110.3 no H13B C13 H13C . . 109.0 no C11 C14 H14A . . 113.3 no C11 C14 H14B . . 109.0 no C11 C14 H14C . . 107.7 no H14A C14 H14B . . 108.9 no H14A C14 H14C . . 108.8 no H14B C14 H14C . . 109.0 no C15 C16 H16A . . 108.3 no C15 C16 H16B . . 107.7 no C17 C16 H16A . . 107.7 no C17 C16 H16B . . 108.5 no H16A C16 H16B . . 109.0 no C17 C18 H18A . . 107.2 no C17 C18 H18B . . 110.7 no C17 C18 H18C . . 109.6 no H18A C18 H18B . . 110.2 no H18A C18 H18C . . 110.2 no H18B C18 H18C . . 109.0 no C17 C19 H19A . . 110.0 no C17 C19 H19B . . 107.6 no C17 C19 H19C . . 111.2 no H19A C19 H19B . . 109.5 no H19A C19 H19C . . 109.5 no H19B C19 H19C . . 109.0 no C17 C20 H20A . . 111.9 no C17 C20 H20B . . 107.3 no C17 C20 H20C . . 109.6 no H20A C20 H20B . . 109.5 no H20A C20 H20C . . 109.5 no H20B C20 H20C . . 109.0 no O6 C21 H21A . . 109.9 no O6 C21 H21B . . 107.3 no C22 C21 H21A . . 107.4 no C22 C21 H21B . . 106.3 no H21A C21 H21B . . 109.0 no C21 C22 H22A . . 109.9 no C21 C22 H22B . . 107.8 no C21 C22 H22C . . 108.5 no H22A C22 H22B . . 112.3 no H22A C22 H22C . . 109.8 no H22B C22 H22C . . 108.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 Cu1 . 2_555 2.602(3) yes Cu1 O2 . . 1.971(3) yes Cu1 O3 . 2_555 1.968(3) yes Cu1 O4 . . 1.952(3) yes Cu1 O5 . 2_555 1.958(3) yes Cu1 O6 . . 2.164(3) yes O2 C9 . . 1.250(4) yes O3 C9 . . 1.268(5) yes O4 C15 . . 1.243(5) yes O5 C15 . . 1.250(5) yes O6 C21 . . 1.623(8) no O7 C23 . . 1.461(13) no O8 C23 . . 1.483(9) no C9 C10 . . 1.533(6) no C10 C11 . . 1.544(7) no C11 C12 . . 1.509(8) no C11 C13 . . 1.541(7) no C11 C14 . . 1.531(9) no C15 C16 . . 1.544(6) no C16 C17 . . 1.539(7) no C17 C18 . . 1.552(7) no C17 C19 . . 1.508(9) no C17 C20 . . 1.480(9) no C21 C22 . . 1.448(14) no C23 C24 . . 1.331(12) no O6 H6 . . .960 no C10 H10A . . .960 no C10 H10B . . .960 no C12 H12A . . .960 no C12 H12B . . .960 no C12 H12C . . .960 no C13 H13A . . .960 no C13 H13B . . .960 no C13 H13C . . .960 no C14 H14A . . .960 no C14 H14B . . .960 no C14 H14C . . .960 no C16 H16A . . .960 no C16 H16B . . .959 no C18 H18A . . .960 no C18 H18B . . .960 no C18 H18C . . .960 no C19 H19A . . .961 no C19 H19B . . .960 no C19 H19C . . .960 no C20 H20A . . .959 no C20 H20B . . .960 no C20 H20C . . .960 no C21 H21A . . .960 no C21 H21B . . .960 no C22 H22A . . .960 no C22 H22B . . .964 no C22 H22C . . .962 no