#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316821.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4316821 loop_ _publ_author_name 'Shao-Ming Fang' 'Qiang Zhang' 'Min Hu' 'E. Carolina Sa\~nudo' 'Miao Du' 'Chun-Sen Liu' _publ_section_title ; From Infinite One-Dimensional Helix to Discrete CuII15 Cluster along with in Situ SN2 Ring-Cleavage of cis-Epoxysuccinic Acid: pH-Controlled Assemblies, Crystal Structures, and Properties ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9617 _journal_page_last 9626 _journal_paper_doi 10.1021/ic101278w _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C4 H7 Cu O7.5' _chemical_formula_weight 238.64 _chemical_name_systematic ; ? ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 7.783(7) _cell_length_b 10.951(10) _cell_length_c 18.722(18) _cell_measurement_reflns_used 3820 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 27.87 _cell_measurement_theta_min 3.21 _cell_volume 1596(3) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'SMART (Bruker, 2007)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _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 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 8247 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 3.21 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.744 _exptl_absorpt_correction_T_max 0.5965 _exptl_absorpt_correction_T_min 0.4141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.438 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.079 _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1405 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0297 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+3.3268P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.0847 _reflns_number_gt 1267 _reflns_number_total 1405 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ic101278w_si_002_1.cif _[local]_cod_data_source_block 1 _[local]_cod_chemical_formula_sum_orig 'C4 H7 Cu O7.50' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 4316821 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.23036(5) 0.76880(4) 0.409305(19) 0.02435(18) Uani 1 1 d . . . C1 C 0.4251(4) 0.6266(3) 0.53083(17) 0.0246(7) Uani 1 1 d . . . C2 C 0.4010(4) 0.5757(3) 0.60551(17) 0.0288(7) Uani 1 1 d . . . H2A H 0.3330 0.5006 0.6087 0.035 Uiso 1 1 calc R . . C3 C 0.4112(4) 0.7934(3) 0.66179(16) 0.0280(7) Uani 1 1 d . . . C4 C 0.3939(4) 0.6555(3) 0.66864(17) 0.0296(7) Uani 1 1 d . . . H4A H 0.3216 0.6266 0.7080 0.036 Uiso 1 1 calc R . . O1 O 0.2997(3) 0.6145(2) 0.49036(12) 0.0331(6) Uani 1 1 d . . . O1W O 0.0000 0.4446(3) 0.2500 0.0573(11) Uani 1 2 d S . . H1WA H 0.0645 0.4943 0.2277 0.069 Uiso 0.50 1 d PR . . H1WB H -0.0645 0.4943 0.2723 0.069 Uiso 0.50 1 d PR . . O2 O 0.5660(3) 0.6775(2) 0.51494(11) 0.0282(5) Uani 1 1 d . . . O3 O 0.5409(3) 0.8363(2) 0.62988(13) 0.0316(5) Uani 1 1 d . . . O4 O 0.2937(3) 0.8547(2) 0.68883(14) 0.0393(6) Uani 1 1 d . . . O5 O 0.5445(3) 0.5835(2) 0.65394(11) 0.0309(5) Uani 1 1 d . . . O6 O 0.3991(4) 0.8961(2) 0.44026(17) 0.0508(7) Uani 1 1 d . . . H6A H 0.4674 0.8817 0.4747 0.061 Uiso 1 1 d R . . H6B H 0.4025 0.9647 0.4190 0.061 Uiso 1 1 d R . . O7 O 0.3840(4) 0.7069(3) 0.33198(16) 0.0555(8) Uani 1 1 d . . . H7A H 0.4437 0.6429 0.3386 0.067 Uiso 1 1 d R . . H7B H 0.3898 0.7446 0.2924 0.067 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0197(3) 0.0261(3) 0.0273(3) -0.00043(15) 0.00072(15) -0.00132(15) C1 0.0275(18) 0.0160(15) 0.0304(16) -0.0006(12) -0.0040(14) 0.0041(12) C2 0.0278(18) 0.0259(17) 0.0328(17) 0.0080(13) -0.0035(14) -0.0025(14) C3 0.0276(18) 0.0349(18) 0.0217(16) 0.0002(13) -0.0018(13) 0.0057(15) C4 0.0247(17) 0.0372(18) 0.0270(16) 0.0088(14) 0.0029(13) 0.0007(14) O1 0.0335(13) 0.0288(12) 0.0370(13) 0.0035(10) -0.0144(11) -0.0045(10) O1W 0.068(3) 0.0292(19) 0.075(3) 0.000 -0.002(2) 0.000 O2 0.0257(12) 0.0331(12) 0.0258(12) 0.0029(9) -0.0022(9) -0.0004(10) O3 0.0267(12) 0.0275(12) 0.0406(13) -0.0008(10) 0.0066(11) 0.0006(10) O4 0.0335(14) 0.0440(15) 0.0404(14) 0.0020(12) 0.0113(11) 0.0118(12) O5 0.0326(14) 0.0301(12) 0.0300(12) 0.0061(9) -0.0062(10) 0.0050(10) O6 0.0432(17) 0.0405(15) 0.0688(19) 0.0030(14) -0.0078(14) -0.0046(13) O7 0.0486(18) 0.071(2) 0.0473(17) 0.0003(15) 0.0058(14) 0.0135(16) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cu1 O2 176.38(12) . 4_466 ? O7 Cu1 O6 93.07(14) . . ? O2 Cu1 O6 90.55(12) 4_466 . ? O7 Cu1 O3 88.87(13) . 4_466 ? O2 Cu1 O3 87.59(11) 4_466 4_466 ? O6 Cu1 O3 170.57(11) . 4_466 ? O7 Cu1 O1 94.99(13) . . ? O2 Cu1 O1 84.25(11) 4_466 . ? O6 Cu1 O1 99.45(12) . . ? O3 Cu1 O1 89.57(10) 4_466 . ? O1 C1 O2 125.7(3) . . ? O1 C1 C2 115.2(3) . . ? O2 C1 C2 119.1(3) . . ? O5 C2 C4 59.2(2) . . ? O5 C2 C1 117.5(3) . . ? C4 C2 C1 121.8(3) . . ? O5 C2 H2A 115.5 . . ? C4 C2 H2A 115.5 . . ? C1 C2 H2A 115.5 . . ? O4 C3 O3 125.4(3) . . ? O4 C3 C4 115.9(3) . . ? O3 C3 C4 118.7(3) . . ? O5 C4 C2 59.4(2) . . ? O5 C4 C3 117.1(3) . . ? C2 C4 C3 121.2(3) . . ? O5 C4 H4A 115.8 . . ? C2 C4 H4A 115.8 . . ? C3 C4 H4A 115.8 . . ? C1 O1 Cu1 120.1(2) . . ? H1WA O1W H1WB 100.5 . . ? C1 O2 Cu1 121.2(2) . 4_566 ? C3 O3 Cu1 123.1(2) . 4_566 ? C4 O5 C2 61.4(2) . . ? Cu1 O6 H6A 120.0 . . ? Cu1 O6 H6B 120.0 . . ? H6A O6 H6B 120.0 . . ? Cu1 O7 H7A 120.0 . . ? Cu1 O7 H7B 119.9 . . ? H7A O7 H7B 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.997(3) . ? Cu1 O2 1.999(3) 4_466 ? Cu1 O6 2.001(3) . ? Cu1 O3 2.009(3) 4_466 ? Cu1 O1 2.334(3) . ? C1 O1 1.242(4) . ? C1 O2 1.265(4) . ? C1 C2 1.517(4) . ? C2 O5 1.441(4) . ? C2 C4 1.471(5) . ? C2 H2A 0.9800 . ? C3 O4 1.243(4) . ? C3 O3 1.264(4) . ? C3 C4 1.521(5) . ? C4 O5 1.439(4) . ? C4 H4A 0.9800 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8499 . ? O2 Cu1 1.999(3) 4_566 ? O3 Cu1 2.009(3) 4_566 ? O6 H6A 0.8499 . ? O6 H6B 0.8500 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O5 177.9(3) . . . . ? O2 C1 C2 O5 -2.7(4) . . . . ? O1 C1 C2 C4 -112.9(3) . . . . ? O2 C1 C2 C4 66.5(4) . . . . ? C1 C2 C4 O5 -105.3(3) . . . . ? O5 C2 C4 C3 105.1(3) . . . . ? C1 C2 C4 C3 -0.2(5) . . . . ? O4 C3 C4 O5 -165.3(3) . . . . ? O3 C3 C4 O5 14.6(4) . . . . ? O4 C3 C4 C2 125.8(3) . . . . ? O3 C3 C4 C2 -54.3(4) . . . . ? O2 C1 O1 Cu1 -36.6(4) . . . . ? C2 C1 O1 Cu1 142.7(2) . . . . ? O7 Cu1 O1 C1 87.6(3) . . . . ? O2 Cu1 O1 C1 -95.9(3) 4_466 . . . ? O6 Cu1 O1 C1 -6.3(3) . . . . ? O3 Cu1 O1 C1 176.4(2) 4_466 . . . ? O1 C1 O2 Cu1 163.1(2) . . . 4_566 ? C2 C1 O2 Cu1 -16.2(4) . . . 4_566 ? O4 C3 O3 Cu1 177.6(2) . . . 4_566 ? C4 C3 O3 Cu1 -2.3(4) . . . 4_566 ? C3 C4 O5 C2 -112.0(3) . . . . ? C1 C2 O5 C4 112.4(3) . . . . ?