#------------------------------------------------------------------------------ #$Date: 2016-01-28 16:16:35 +0200 (Thu, 28 Jan 2016) $ #$Revision: 175236 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100908.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_1100908 loop_ _publ_author_name 'Baggio, Ricardo' 'Foxman, Bruce' 'Garland, Maria Teresa' 'Perec, Mireille' 'Shang, Wen' _publ_section_title ; Aquabis(crotonato)bis(pyridine)copper(II) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e505 _journal_page_last e506 _journal_paper_doi 10.1107/S0108270100013937 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Cu (C4 H5 O2)2 (C5 H5 N)2 (H2 O)]' _chemical_formula_moiety 'C18 H22 Cu N2 O5' _chemical_formula_sum 'C18 H22 Cu N2 O5' _chemical_formula_weight 409.92 _chemical_name_systematic ; Aqua-bis(trans-2-butenoate)- bis(pyridine)copper(II) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 91.097(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.922(2) _cell_length_b 5.7331(8) _cell_length_c 21.341(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 7.5 _cell_volume 1947.6(5) _computing_cell_refinement P3/P4-PC _computing_data_collection 'P3/P4-PC (Siemens, 1991)' _computing_data_reduction 'XDISK in SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'CIFTAB (Sheldrick, 1993) and PARST (Nardelli, 1983)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .496 _diffrn_measured_fraction_theta_max .496 _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method \w/2\q _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 .026 _diffrn_reflns_av_sigmaI/netI .029 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 1866 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.91 _diffrn_standards_decay_% <2 _diffrn_standards_interval_count 98 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.15 _exptl_absorpt_correction_T_max .73 _exptl_absorpt_correction_T_min .50 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(XEMP in SHELXTL/PC; Sheldrick, 1994)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 852 _exptl_crystal_size_max .36 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .08 _refine_diff_density_max .287 _refine_diff_density_min -.280 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 1699 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all .041 _refine_ls_R_factor_gt .031 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ' w = 1/[\s^2^(Fo^2^)+(0.04P)^2^+2P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .082 _reflns_number_gt 1476 _reflns_number_total 1699 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0401sup1.cif _cod_data_source_block I _cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 1100908 _cod_database_fobs_code 1100908 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -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 Cu .0000 .38067(8) .2500 .02892(16) Uani d S 1 . . Cu N1 .10999(12) .4139(4) .20392(9) .0329(5) Uani d . 1 . . N C2 .16242(17) .5918(5) .21513(13) .0420(6) Uani d . 1 . . C H2A .1464 .7078 .2429 .050 Uiso calc R 1 . . H C3 .23942(18) .6096(6) .18688(15) .0503(7) Uani d . 1 . . C H3A .2744 .7361 .1953 .060 Uiso calc R 1 . . H C4 .26358(19) .4389(6) .14639(15) .0541(9) Uani d . 1 . . C H4A .3153 .4469 .1270 .065 Uiso calc R 1 . . H C5 .2103(2) .2561(6) .13483(16) .0564(9) Uani d . 1 . . C H5A .2258 .1366 .1079 .068 Uiso calc R 1 . . H C6 .13350(18) .2505(5) .16343(14) .0451(7) Uani d . 1 . . C H6A .0968 .1285 .1542 .054 Uiso calc R 1 . . H O7 -.03881(15) .7474(4) .14482(10) .0583(6) Uani d . 1 . . O O8 -.05988(11) .3752(4) .17009(8) .0407(4) Uani d . 1 . . O C9 -.05941(16) .5459(5) .13186(12) .0370(6) Uani d . 1 . . C C10 -.0859(2) .4903(6) .06611(13) .0489(7) Uani d . 1 . . C H10A -.0988 .6138 .0394 .059 Uiso calc R 1 . . H C11 -.0920(2) .2790(6) .04387(14) .0518(8) Uani d . 1 . . C H11A -.0801 .1568 .0713 .062 Uiso calc R 1 . . H C12 -.1166(3) .2168(9) -.02215(17) .0879(14) Uani d . 1 . . C H12A -.1159 .0503 -.0269 .132 Uiso calc R 1 . . H H12B -.0776 .2857 -.0505 .132 Uiso calc R 1 . . H H12C -.1721 .2745 -.0313 .132 Uiso calc R 1 . . H O1W .0000 -.0050(6) .2500 .0499(8) Uani d S 1 . . O H1W -.011(2) -.089(6) .2228(14) .052(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 Cu .0280(2) .0293(3) .0294(2) .000 .00047(15) .000 N1 .0295(11) .0351(12) .0341(11) -.0002(9) .0000(8) .0006(9) C2 .0392(14) .0396(16) .0473(15) -.0020(13) .0011(12) -.0036(13) C3 .0362(14) .0516(18) .0632(19) -.0115(15) -.0023(13) .0060(17) C4 .0342(15) .066(2) .0623(19) .0035(15) .0128(14) .0119(17) C5 .059(2) .053(2) .0578(19) .0032(16) .0235(16) -.0103(16) C6 .0454(16) .0422(17) .0480(16) -.0051(13) .0084(13) -.0092(14) O7 .0891(17) .0386(13) .0470(12) .0084(12) -.0068(11) -.0065(10) O8 .0386(10) .0495(11) .0338(9) -.0076(9) -.0041(7) .0067(9) C9 .0343(14) .0415(17) .0352(14) .0084(12) .0024(11) -.0020(12) C10 .0568(19) .0529(19) .0367(15) .0057(16) -.0045(13) .0069(15) C11 .0584(19) .059(2) .0385(16) -.0125(16) .0033(13) -.0027(15) C12 .102(3) .108(4) .053(2) -.028(3) -.005(2) -.026(2) O1W .082(2) .0271(16) .0405(17) .000 -.0059(16) .000 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' Cu Cu .3201 1.2651 '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 O8 Cu O8 6_556 . 178.13(12) y O8 Cu N1 6_556 . 90.77(8) y O8 Cu N1 . . 89.41(8) y O8 Cu N1 6_556 6_556 89.41(8) n O8 Cu N1 . 6_556 90.77(8) n N1 Cu N1 . 6_556 169.26(12) y O8 Cu O1W 6_556 . 89.07(6) n O8 Cu O1W . . 89.07(6) y N1 Cu O1W . . 95.37(6) y N1 Cu O1W 6_556 . 95.37(6) n C6 N1 C2 . . 118.0(2) ? C6 N1 Cu . . 120.19(18) ? C2 N1 Cu . . 121.69(18) ? N1 C2 C3 . . 122.3(3) ? C4 C3 C2 . . 119.1(3) ? C3 C4 C5 . . 118.8(3) ? C4 C5 C6 . . 119.4(3) ? N1 C6 C5 . . 122.3(3) ? C9 O8 Cu . . 122.82(18) ? O7 C9 O8 . . 125.6(3) ? O7 C9 C10 . . 118.8(3) ? O8 C9 C10 . . 115.7(3) ? C11 C10 C9 . . 124.0(3) ? C10 C11 C12 . . 125.4(3) ? 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 Cu O8 6_556 1.9381(17) ? Cu O8 . 1.9381(17) y Cu N1 . 2.034(2) y Cu N1 6_556 2.034(2) ? Cu O1W . 2.211(3) y N1 C6 . 1.333(3) ? N1 C2 . 1.337(3) ? C2 C3 . 1.380(4) ? C3 C4 . 1.365(5) ? C4 C5 . 1.368(5) ? C5 C6 . 1.378(4) ? O7 C9 . 1.231(4) ? O8 C9 . 1.274(3) ? C9 C10 . 1.492(4) ? C10 C11 . 1.304(5) ? C11 C12 . 1.498(4) ?