#------------------------------------------------------------------------------ #$Date: 2016-03-25 22:13:40 +0000 (Fri, 25 Mar 2016) $ #$Revision: 180066 $ #$URL: svn://www.crystallography.net/cod/cif/7/05/12/7051221.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_7051221 loop_ _publ_author_name 'Zheng, Shao-Liang' 'Tong, Ming-Liang' 'Zhu, Hai-Liang' 'Chen, Xiao-Ming' _publ_section_title ; Four two-dimensional highly undulating silver(I)\^a€“hexamethylenetetramine co-ordination networks containing micropores ; _journal_issue 11 _journal_name_full 'New Journal of Chemistry' _journal_page_first 1425 _journal_paper_doi 10.1039/b107193a _journal_volume 25 _journal_year 2001 _chemical_formula_sum 'C14 H27 Ag2 Cl2 N9 O8' _chemical_formula_weight 736.09 _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _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 18.112(10) _cell_length_b 10.860(5) _cell_length_c 23.781(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 7.5 _cell_volume 4678(4) _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL V. 5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.901 _diffrn_measured_fraction_theta_max 0.901 _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _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 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 5486 _diffrn_reflns_theta_full 27.01 _diffrn_reflns_theta_max 27.01 _diffrn_reflns_theta_min 2.05 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 200 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_T_max 0.5547 _exptl_absorpt_correction_T_min 0.4785 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2928 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _refine_diff_density_max 0.914 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.134 _refine_ls_extinction_coef 0.00003(7) _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 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 5103 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0492 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+9.8900P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.1289 _reflns_number_gt 3180 _reflns_number_total 5103 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b107193a.txt _cod_data_source_block complex_1 _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 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+9.8900P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+9.8900P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M Pbca _cod_database_code 7051221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.16536(2) 0.00076(4) 0.09029(2) 0.03320(15) Uani 1 d . . . Ag2 Ag 1.01753(3) 0.49348(4) 0.18441(2) 0.03866(16) Uani 1 d . . . N1 N 0.9345(3) 0.8722(5) 0.1335(3) 0.0376(13) Uani 1 d . . . N2 N 1.0126(3) 0.7114(4) 0.1744(2) 0.0286(11) Uani 1 d . . . N3 N 0.9930(3) 0.9064(4) 0.2255(2) 0.0275(11) Uani 1 d . . . N4 N 1.0683(3) 0.9041(4) 0.1395(2) 0.0268(11) Uani 1 d . . . N5 N 1.1489(2) 0.2178(4) 0.0769(2) 0.0236(10) Uani 1 d . . . N6 N 1.2181(2) 0.4133(4) 0.0740(2) 0.0249(11) Uani 1 d . . . N7 N 1.1102(3) 0.3816(4) 0.0126(2) 0.0312(12) Uani 1 d . . . N8 N 1.0928(2) 0.4063(4) 0.1145(2) 0.0235(10) Uani 1 d . . . C1 C 0.9456(3) 0.7394(6) 0.1398(3) 0.0329(15) Uani 1 d . . . H1A H 0.9513 0.7038 0.1031 0.080 Uiso 1 d R . . H1B H 0.9028 0.7033 0.1570 0.080 Uiso 1 d R . . C2 C 0.9996(3) 0.9241(5) 0.1053(3) 0.0313(14) Uani 1 d . . . H2A H 0.9922 1.0107 0.0997 0.080 Uiso 1 d R . . H2B H 1.0052 0.8861 0.0691 0.080 Uiso 1 d R . . C3 C 0.9257(3) 0.9262(6) 0.1890(3) 0.0372(16) Uani 1 d . . . H3A H 0.8836 0.8897 0.2070 0.080 Uiso 1 d R . . H3B H 0.9164 1.0128 0.1850 0.080 Uiso 1 d R . . C4 C 1.0040(3) 0.7716(5) 0.2300(3) 0.0301(14) Uani 1 d . . . H4A H 1.0472 0.7557 0.2523 0.080 Uiso 1 d R . . H4B H 0.9624 0.7361 0.2490 0.080 Uiso 1 d R . . C5 C 1.0766(3) 0.7678(5) 0.1458(3) 0.0243(12) Uani 1 d . . . H5A H 1.0823 0.7313 0.1093 0.080 Uiso 1 d R . . H5B H 1.1206 0.7510 0.1669 0.080 Uiso 1 d R . . C6 C 1.0585(3) 0.9584(6) 0.1957(3) 0.0294(14) Uani 1 d . . . H6A H 1.1021 0.9441 0.2178 0.080 Uiso 1 d R . . H6B H 1.0523 1.0458 0.1919 0.080 Uiso 1 d R . . C7 C 1.1003(3) 0.2704(5) 0.1205(3) 0.0269(13) Uani 1 d . . . H7A H 1.1204 0.2524 0.1569 0.080 Uiso 1 d R . . H7B H 1.0524 0.2328 0.1181 0.080 Uiso 1 d R . . C8 C 1.0626(3) 0.4314(5) 0.0573(3) 0.0295(13) Uani 1 d . . . H8A H 1.0145 0.3949 0.0542 0.080 Uiso 1 d R . . H8B H 1.0573 0.5187 0.0525 0.080 Uiso 1 d R . . C9 C 1.1834(3) 0.4386(6) 0.0184(3) 0.0323(14) Uani 1 d . . . H9A H 1.2149 0.4072 -0.0107 0.080 Uiso 1 d R . . H9B H 1.1789 0.5260 0.0132 0.080 Uiso 1 d R . . C10 C 1.1682(3) 0.4613(5) 0.1181(3) 0.0261(13) Uani 1 d . . . H10A H 1.1645 0.5492 0.1149 0.080 Uiso 1 d R . . H10B H 1.1890 0.4426 0.1543 0.080 Uiso 1 d R . . C11 C 1.1181(4) 0.2481(6) 0.0206(3) 0.0317(14) Uani 1 d . . . H11A H 1.0708 0.2093 0.0163 0.080 Uiso 1 d R . . H11B H 1.1504 0.2158 -0.0078 0.080 Uiso 1 d R . . C12 C 1.2227(3) 0.2777(5) 0.0808(3) 0.0277(13) Uani 1 d . . . H12A H 1.2546 0.2440 0.0524 0.080 Uiso 1 d R . . H12B H 1.2440 0.2598 0.1168 0.080 Uiso 1 d R . . C13 C 0.8371(4) 0.4365(7) 0.1432(4) 0.053(2) Uani 1 d . . . C14 C 0.7585(5) 0.4320(9) 0.1326(4) 0.067(2) Uani 1 d . . . N9 N 0.8976(4) 0.4411(7) 0.1539(4) 0.078(2) Uani 1 d . . . H14A H 0.7418 0.4430 0.1708 0.080 Uiso 1 d . . . H14B H 0.7368 0.3536 0.1242 0.080 Uiso 1 d . . . H14C H 0.7522 0.4612 0.0951 0.080 Uiso 1 d . . . Cl1 Cl 1.11930(8) -0.18291(15) -0.03499(7) 0.0363(4) Uani 1 d . . . O1 O 1.0727(3) -0.1911(5) -0.0824(3) 0.0715(18) Uani 1 d . . . O2 O 1.1908(3) -0.2265(7) -0.0488(3) 0.101(3) Uani 1 d . . . O3 O 1.0920(5) -0.2636(6) 0.0075(3) 0.101(3) Uani 1 d . . . O4 O 1.1222(4) -0.0610(5) -0.0131(2) 0.0667(17) Uani 1 d . . . Cl2 Cl 0.75090(9) 0.17642(16) 0.25773(7) 0.0404(4) Uani 1 d . . . O5 O 0.8208(3) 0.1204(6) 0.2499(3) 0.086(2) Uani 1 d . . . O6 O 0.7148(4) 0.1074(6) 0.3016(3) 0.091(2) Uani 1 d . . . O7 O 0.7098(5) 0.1711(8) 0.2092(3) 0.136(4) Uani 1 d . . . O8 O 0.7600(3) 0.3018(5) 0.2755(2) 0.0629(16) Uani 1 d . . . 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 0.0270(2) 0.0269(2) 0.0457(3) 0.0007(2) 0.0028(2) 0.0011(2) Ag2 0.0431(3) 0.0297(3) 0.0432(3) 0.0037(2) 0.0163(2) 0.0043(2) N1 0.021(3) 0.036(3) 0.055(4) 0.007(3) 0.002(3) 0.007(2) N2 0.025(3) 0.022(2) 0.038(3) -0.001(2) 0.001(2) -0.001(2) N3 0.027(3) 0.022(2) 0.034(3) -0.004(2) 0.008(2) 0.000(2) N4 0.023(2) 0.020(2) 0.037(3) -0.001(2) 0.003(2) 0.000(2) N5 0.022(2) 0.017(2) 0.032(3) -0.003(2) 0.001(2) -0.0006(18) N6 0.018(2) 0.021(2) 0.036(3) -0.002(2) 0.007(2) 0.0004(19) N7 0.036(3) 0.028(3) 0.030(3) 0.003(2) -0.001(2) 0.001(2) N8 0.019(2) 0.019(2) 0.032(3) 0.002(2) 0.001(2) -0.0006(19) C1 0.029(3) 0.030(3) 0.040(4) -0.003(3) -0.002(3) -0.003(3) C2 0.028(3) 0.028(3) 0.037(3) 0.005(3) 0.002(3) 0.004(3) C3 0.031(3) 0.030(3) 0.051(4) -0.002(3) 0.012(3) 0.004(3) C4 0.035(3) 0.022(3) 0.034(3) 0.001(2) 0.005(3) -0.002(3) C5 0.023(3) 0.019(3) 0.031(3) 0.003(2) 0.003(3) 0.006(2) C6 0.028(3) 0.026(3) 0.034(3) -0.001(3) 0.006(3) -0.004(2) C7 0.022(3) 0.022(3) 0.037(4) 0.003(3) 0.002(3) -0.002(2) C8 0.022(3) 0.026(3) 0.040(4) -0.002(3) -0.005(3) 0.006(2) C9 0.035(3) 0.028(3) 0.034(3) 0.008(3) 0.004(3) 0.001(3) C10 0.025(3) 0.023(3) 0.029(3) -0.001(2) 0.003(3) -0.002(2) C11 0.033(3) 0.034(3) 0.029(3) -0.011(3) -0.005(3) 0.000(3) C12 0.020(3) 0.021(3) 0.043(4) 0.002(3) 0.004(3) 0.003(2) C13 0.042(4) 0.051(5) 0.065(5) -0.017(4) 0.012(4) -0.014(4) C14 0.049(5) 0.092(7) 0.061(5) -0.016(5) -0.002(4) -0.010(5) N9 0.044(4) 0.064(5) 0.125(7) -0.025(5) -0.001(5) -0.009(4) Cl1 0.0319(8) 0.0410(9) 0.0360(8) -0.0023(7) -0.0065(7) 0.0029(7) O1 0.079(4) 0.050(3) 0.086(4) -0.014(3) -0.051(4) 0.012(3) O2 0.036(3) 0.135(6) 0.131(6) -0.070(5) 0.002(4) 0.006(4) O3 0.171(8) 0.061(4) 0.070(5) 0.015(3) 0.026(5) -0.002(5) O4 0.096(5) 0.045(3) 0.059(3) -0.015(3) -0.019(3) 0.003(3) Cl2 0.0345(8) 0.0447(9) 0.0419(9) -0.0121(8) -0.0048(8) 0.0042(8) O5 0.046(3) 0.085(5) 0.128(6) -0.035(4) 0.019(4) 0.010(3) O6 0.109(5) 0.059(4) 0.105(6) -0.001(4) 0.051(5) 0.003(4) O7 0.178(8) 0.108(6) 0.121(6) -0.035(5) -0.115(6) 0.040(6) O8 0.082(4) 0.036(3) 0.071(4) -0.009(3) 0.008(3) 0.001(3) 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' Cl Cl 0.1484 0.1585 '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 N6 Ag1 N4 124.90(17) 8_855 1_545 ? N6 Ag1 N5 119.19(16) 8_855 . ? N4 Ag1 N5 114.27(16) 1_545 . ? N3 Ag2 N8 122.02(16) 3_745 . ? N3 Ag2 N9 96.3(3) 3_745 . ? N8 Ag2 N9 102.7(2) . . ? N3 Ag2 N2 119.21(17) 3_745 . ? N8 Ag2 N2 110.58(16) . . ? N9 Ag2 N2 100.1(2) . . ? C3 N1 C1 108.7(5) . . ? C3 N1 C2 110.4(5) . . ? C1 N1 C2 108.3(5) . . ? C5 N2 C4 108.1(4) . . ? C5 N2 C1 107.3(5) . . ? C4 N2 C1 108.4(5) . . ? C5 N2 Ag2 115.4(3) . . ? C4 N2 Ag2 110.7(3) . . ? C1 N2 Ag2 106.7(3) . . ? C4 N3 C6 107.4(5) . . ? C4 N3 C3 106.9(5) . . ? C6 N3 C3 108.3(5) . . ? C4 N3 Ag2 110.1(4) . 3_755 ? C6 N3 Ag2 110.2(3) . 3_755 ? C3 N3 Ag2 113.7(3) . 3_755 ? C6 N4 C5 108.6(5) . . ? C6 N4 C2 109.5(5) . . ? C5 N4 C2 106.3(4) . . ? C6 N4 Ag1 111.3(3) . 1_565 ? C5 N4 Ag1 114.5(3) . 1_565 ? C2 N4 Ag1 106.5(3) . 1_565 ? C7 N5 C11 108.9(4) . . ? C7 N5 C12 108.9(4) . . ? C11 N5 C12 107.2(5) . . ? C7 N5 Ag1 111.2(3) . . ? C11 N5 Ag1 112.5(3) . . ? C12 N5 Ag1 108.0(3) . . ? C10 N6 C12 107.8(5) . . ? C10 N6 C9 107.9(4) . . ? C12 N6 C9 107.7(5) . . ? C10 N6 Ag1 106.8(3) . 8_865 ? C12 N6 Ag1 109.4(3) . 8_865 ? C9 N6 Ag1 116.9(3) . 8_865 ? C11 N7 C9 108.4(5) . . ? C11 N7 C8 109.1(5) . . ? C9 N7 C8 107.7(5) . . ? C7 N8 C8 107.6(5) . . ? C7 N8 C10 107.9(4) . . ? C8 N8 C10 108.4(4) . . ? C7 N8 Ag2 112.6(4) . . ? C8 N8 Ag2 111.1(3) . . ? C10 N8 Ag2 109.2(3) . . ? N1 C1 N2 111.6(5) . . ? N1 C2 N4 111.2(5) . . ? N1 C3 N3 112.1(5) . . ? N3 C4 N2 112.7(5) . . ? N2 C5 N4 112.1(4) . . ? N4 C6 N3 112.1(5) . . ? N5 C7 N8 111.8(5) . . ? N7 C8 N8 112.2(4) . . ? N7 C9 N6 112.8(5) . . ? N6 C10 N8 112.1(5) . . ? N7 C11 N5 111.8(5) . . ? N6 C12 N5 112.1(4) . . ? N9 C13 C14 176.9(10) . . ? C13 N9 Ag2 167.5(7) . . ? O1 Cl1 O2 109.8(4) . . ? O1 Cl1 O4 111.8(3) . . ? O2 Cl1 O4 111.2(4) . . ? O1 Cl1 O3 108.7(4) . . ? O2 Cl1 O3 106.1(5) . . ? O4 Cl1 O3 109.0(4) . . ? O7 Cl2 O5 110.8(5) . . ? O7 Cl2 O8 110.4(4) . . ? O5 Cl2 O8 110.1(4) . . ? O7 Cl2 O6 109.9(6) . . ? O5 Cl2 O6 106.1(4) . . ? O8 Cl2 O6 109.4(4) . . ? 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 N6 2.347(5) 8_855 ? Ag1 N4 2.359(5) 1_545 ? Ag1 N5 2.397(4) . ? Ag2 N3 2.349(5) 3_745 ? Ag2 N8 2.350(5) . ? Ag2 N9 2.360(7) . ? Ag2 N2 2.380(5) . ? N1 C3 1.452(8) . ? N1 C1 1.463(8) . ? N1 C2 1.470(8) . ? N2 C5 1.478(7) . ? N2 C4 1.483(7) . ? N2 C1 1.499(8) . ? N3 C4 1.482(7) . ? N3 C6 1.493(7) . ? N3 C3 1.512(8) . ? N3 Ag2 2.349(5) 3_755 ? N4 C6 1.472(7) . ? N4 C5 1.495(7) . ? N4 C2 1.503(7) . ? N4 Ag1 2.359(5) 1_565 ? N5 C7 1.474(7) . ? N5 C11 1.488(8) . ? N5 C12 1.489(7) . ? N6 C10 1.480(7) . ? N6 C12 1.485(7) . ? N6 C9 1.488(8) . ? N6 Ag1 2.347(5) 8_865 ? N7 C11 1.470(8) . ? N7 C9 1.471(8) . ? N7 C8 1.471(7) . ? N8 C7 1.490(7) . ? N8 C8 1.492(7) . ? N8 C10 1.493(7) . ? C13 N9 1.125(10) . ? C13 C14 1.448(11) . ? Cl1 O1 1.411(5) . ? Cl1 O2 1.418(6) . ? Cl1 O4 1.424(5) . ? Cl1 O3 1.426(7) . ? Cl2 O7 1.374(6) . ? Cl2 O5 1.418(6) . ? Cl2 O8 1.436(5) . ? Cl2 O6 1.442(6) . ?