#------------------------------------------------------------------------------ #$Date: 2016-03-25 13:44:41 +0200 (Fri, 25 Mar 2016) $ #$Revision: 179861 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/57/7015722.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_7015722 loop_ _publ_author_name 'Burrows, Andrew D.' 'Kelly, David J.' 'Mahon, Mary F.' 'Raithby, Paul R.' 'Richardson, Christopher' 'Stevenson, Anna J.' _publ_section_title ; Silver coordination networks and cages based on a semi-rigid bis(isoxazolyl) ligand. ; _journal_issue 20 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5483 _journal_page_last 5493 _journal_paper_doi 10.1039/c1dt10029g _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C18 H20 Ag2 N4 O8' _chemical_formula_weight 636.12 _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_space_group_name_H-M 'P c a b' _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 4 _cell_length_a 7.3890(1) _cell_length_b 15.9620(3) _cell_length_c 17.7590(4) _cell_measurement_reflns_used 19582 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 2.910 _cell_volume 2094.55(7) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _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 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 39756 _diffrn_reflns_theta_full 27.42 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_theta_min 3.76 _exptl_absorpt_coefficient_mu 1.925 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.866 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.179 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 147 _refine_ls_number_reflns 2380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0359 _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^)+(0.0566P)^2^+1.2963P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.1014 _reflns_number_gt 1687 _reflns_number_total 2380 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c1dt10029g.txt _cod_data_source_block Compound-1-k07adb23 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 1555 2011-01-17 13:19:09Z saulius ; _cod_original_sg_symbol_H-M Pcab _cod_database_code 7015722 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, 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 Ag1 Ag 0.72332(5) 0.430406(18) 0.349259(18) 0.04015(15) Uani 1 1 d . . . O1 O 0.7624(3) 0.32613(14) 0.49224(13) 0.0282(6) Uani 1 1 d . . . N1 N 0.7377(4) 0.31393(19) 0.41470(16) 0.0276(7) Uani 1 1 d . . . C1 C 0.8335(5) 0.2523(3) 0.60607(19) 0.0348(8) Uani 1 1 d . . . H1A H 0.9330 0.2911 0.6170 0.052 Uiso 1 1 calc R . . H1B H 0.8661 0.1959 0.6232 0.052 Uiso 1 1 calc R . . H1C H 0.7240 0.2709 0.6323 0.052 Uiso 1 1 calc R . . O2 O 0.5455(4) 0.54916(17) 0.34610(14) 0.0385(6) Uani 1 1 d . . . N2 N 0.4491(4) 0.54955(19) 0.28818(16) 0.0297(7) Uani 1 1 d . . . C2 C 0.7996(4) 0.2508(2) 0.52386(19) 0.0267(7) Uani 1 1 d . . . O3 O 0.3634(4) 0.61382(18) 0.27046(16) 0.0461(7) Uani 1 1 d . . . C3 C 0.7975(4) 0.1900(2) 0.46996(18) 0.0219(7) Uani 1 1 d . . . O4 O 0.4399(4) 0.48622(18) 0.24828(16) 0.0484(7) Uani 1 1 d . . . C4 C 0.7581(4) 0.2340(2) 0.40227(19) 0.0261(8) Uani 1 1 d . . . C5 C 0.7398(5) 0.1995(3) 0.3238(2) 0.0357(9) Uani 1 1 d . . . H5A H 0.6258 0.1684 0.3196 0.053 Uiso 1 1 calc R . . H5B H 0.8414 0.1618 0.3132 0.053 Uiso 1 1 calc R . . H5C H 0.7402 0.2457 0.2875 0.053 Uiso 1 1 calc R . . C6 C 0.8318(4) 0.0977(2) 0.4786(2) 0.0255(7) Uani 1 1 d . . . H6A H 0.9124 0.0888 0.5225 0.031 Uiso 1 1 calc R . . H6B H 0.8959 0.0771 0.4333 0.031 Uiso 1 1 calc R . . C7 C 0.5742(4) 0.0444(2) 0.55895(18) 0.0235(7) Uani 1 1 d . . . H7 H 0.6244 0.0747 0.6000 0.028 Uiso 1 1 calc R . . C8 C 0.6599(4) 0.0463(2) 0.48956(19) 0.0225(7) Uani 1 1 d . . . C9 C 0.5850(4) 0.00137(19) 0.43052(19) 0.0251(7) Uani 1 1 d . . . H9 H 0.6421 0.0017 0.3826 0.030 Uiso 1 1 calc 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 Ag1 0.0493(2) 0.0295(2) 0.0416(2) 0.01054(12) 0.01152(13) 0.00586(13) O1 0.0317(13) 0.0213(13) 0.0315(14) -0.0018(11) 0.0000(10) 0.0001(10) N1 0.0296(16) 0.0234(16) 0.0299(16) 0.0019(12) 0.0005(12) -0.0024(11) C1 0.035(2) 0.035(2) 0.034(2) -0.0004(16) -0.0045(16) -0.0040(17) O2 0.0423(16) 0.0404(16) 0.0328(14) -0.0016(12) -0.0118(12) 0.0062(12) N2 0.0309(16) 0.0329(17) 0.0252(16) 0.0012(14) 0.0001(12) -0.0042(13) C2 0.0188(17) 0.0286(19) 0.0325(18) 0.0024(16) -0.0007(13) -0.0008(13) O3 0.0461(16) 0.0428(17) 0.0495(17) 0.0112(13) -0.0092(13) 0.0059(14) C3 0.0183(15) 0.0206(17) 0.0267(18) -0.0002(13) 0.0020(12) -0.0044(13) O4 0.0605(19) 0.0461(18) 0.0386(16) -0.0080(14) -0.0066(14) -0.0017(14) C4 0.0234(17) 0.0267(19) 0.0283(18) -0.0010(14) 0.0028(13) -0.0013(13) C5 0.045(2) 0.034(2) 0.0274(18) 0.0041(17) -0.0010(15) 0.0001(17) C6 0.0221(16) 0.0228(18) 0.0314(19) 0.0019(14) 0.0003(14) -0.0003(14) C7 0.0234(17) 0.0195(16) 0.0277(18) -0.0017(14) -0.0016(13) 0.0030(13) C8 0.0210(15) 0.0171(16) 0.0293(18) 0.0025(14) 0.0018(13) 0.0019(13) C9 0.0266(17) 0.0211(17) 0.0275(18) 0.0034(14) 0.0033(14) 0.0007(13) 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' N N 0.0061 0.0033 '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' Ag Ag -0.8971 1.1015 '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 N1 Ag1 O2 137.42(10) . . ? N1 Ag1 O3 101.16(10) . 3_565 ? O2 Ag1 O3 116.93(9) . 3_565 ? C2 O1 N1 108.1(2) . . ? C4 N1 O1 106.7(3) . . ? C4 N1 Ag1 138.2(2) . . ? O1 N1 Ag1 114.1(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 O2 Ag1 110.4(2) . . ? O4 N2 O3 120.0(3) . . ? O4 N2 O2 119.9(3) . . ? O3 N2 O2 120.1(3) . . ? O1 C2 C3 109.8(3) . . ? O1 C2 C1 115.4(3) . . ? C3 C2 C1 134.9(3) . . ? N2 O3 Ag1 101.3(2) . 3_465 ? C2 C3 C4 104.2(3) . . ? C2 C3 C6 128.6(3) . . ? C4 C3 C6 127.2(3) . . ? N1 C4 C3 111.3(3) . . ? N1 C4 C5 120.3(3) . . ? C3 C4 C5 128.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 C8 113.6(3) . . ? C3 C6 H6A 108.8 . . ? C8 C6 H6A 108.8 . . ? C3 C6 H6B 108.8 . . ? C8 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C9 121.0(3) . 5_656 ? C8 C7 H7 119.5 . . ? C9 C7 H7 119.5 5_656 . ? C9 C8 C7 118.6(3) . . ? C9 C8 C6 121.0(3) . . ? C7 C8 C6 120.4(3) . . ? C8 C9 C7 120.4(3) . 5_656 ? C8 C9 H9 119.8 . . ? C7 C9 H9 119.8 5_656 . ? 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 Ag1 N1 2.195(3) . ? Ag1 O2 2.307(3) . ? Ag1 O3 2.468(3) 3_565 ? O1 C2 1.355(4) . ? O1 N1 1.403(4) . ? N1 C4 1.303(5) . ? C1 C2 1.482(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 N2 1.251(4) . ? N2 O4 1.236(4) . ? N2 O3 1.246(4) . ? C2 C3 1.363(5) . ? O3 Ag1 2.468(3) 3_465 ? C3 C4 1.422(5) . ? C3 C6 1.504(4) . ? C4 C5 1.505(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C8 1.525(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.386(5) . ? C7 C9 1.397(4) 5_656 ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C9 C7 1.397(4) 5_656 ? C9 H9 0.9500 . ?