Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Vance E. Williams' 'Farzad Haftbaradaran' 'Daniel Leznoff' _publ_contact_author_name 'Prof Vance E. Williams' _publ_contact_author_address ; Department of Chemistry Simon Fraser University 8888 University Dr. Burnaby British Columbia V5A 1S6 CANADA ; _publ_contact_author_email VANCEW@SFU.CA _publ_section_title ; A strained silver(I) coordination polymer of 1,4-diazatriphenylene ; data_CRYSTALS_cif_1 _database_code_CSD 197738 _audit_creation_date 03-17-04 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Isotropic thermal parameters were refined for all C atoms, since anisotropic refinement would result in an observation to parameters ratio of 5.4 as opposed to the present 8.5. H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 5.7422(5) _cell_angle_alpha 90 _cell_length_b 13.686(1) _cell_angle_beta 90 _cell_length_c 18.320(2) _cell_angle_gamma 90 _cell_volume 1439.7 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b n 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z x+1/2,-y+1/2,z+1/2 -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Ag ' -1.0850 1.1010 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8157 5.1790 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3499 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C16 H10 Ag1 B1 F4 N2 ' _chemical_formula_moiety ' C16 H10 Ag1 B1 F4 N2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 424.942 _cell_measurement_reflns_used 72 _cell_measurement_theta_min 16 _cell_measurement_theta_max 18 _cell_measurement_temperature 293 _cell_formula_units_Z 4 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow-orange ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_meas ? _exptl_crystal_F_000 827.941 _exptl_absorpt_coefficient_mu 14.30 # Sheldrick geometric definitions 1.00 1.00 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_radiation_monochromator graphite _computing_data_collection 'NRC DIFRAC' _computing_cell_refinement 'NRC DIFRAC' _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'SIR 92' #_computing_structure_refinement 'CRYSTALS' #_computing_molecular_graphics 'Ortep-3' #_computing_publication_material 'CRYSTALS' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6800 _exptl_absorpt_correction_T_max 0.8765 _diffrn_standards_interval_time 200 _diffrn_standards_interval_count 11 _diffrn_standards_number 2 _diffrn_standards_decay_% 0.37 _diffrn_ambient_temperature 293 _diffrn_reflns_number 1784 _reflns_number_total 1510 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 1511 # Number of reflections without Friedels Law is 1510 # Theoretical number of reflections is about 1423 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 1185 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min 0 _reflns_limit_h_max 7 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _refine_diff_density_min -0.75 _refine_diff_density_max 1.07 _reflns_threshold_expression >2.50\s(I) _refine_ls_number_reflns 1185 _refine_ls_number_parameters 139 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0495 _refine_ls_goodness_of_fit_ref 2.1636 _refine_ls_shift/su_max 0.000737 _refine_ls_abs_structure_Flack 0.00(12) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/(.150E-01*F +0.00 *\s^2^(F ) + 0.00 ) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # Data Acquisition # Gabe, E.J., White, P.S., Enright, G.D. DIFRAC A Fortran 77 Control Routine for 4-Circle Diffractometers, N.R.C., Ottawa, 1995. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #Ortep-3 Farrugia, L.J. (1997) J. Appl. Cryst., 30, 565. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type AG1 AG 0.07081(13) 0.19539(4) 0.70016(15) 0.0451 1.0000 Uani F1 F 0.7838(16) 0.1691(7) 0.5898(5) 0.0866 1.0000 Uani F2 F 0.3896(15) 0.1735(6) 0.5827(5) 0.0796 1.0000 Uani F3 F 0.5651(14) 0.1602(6) 0.6922(7) 0.0857 1.0000 Uani F4 F 0.5736(15) 0.0348(5) 0.6137(5) 0.0785 1.0000 Uani B1 B 0.582(3) 0.134(1) 0.6168(8) 0.0536 1.0000 Uani N1 N 0.1128(15) 0.0320(5) 0.7149(6) 0.0463 1.0000 Uani N2 N 0.3518(13) -0.1431(4) 0.7000(9) 0.0398 1.0000 Uani C1 C 0.088(2) -0.0248(8) 0.6575(6) 0.045(2) 1.0000 Uiso C2 C 0.1972(19) -0.1133(7) 0.6535(5) 0.041(2) 1.0000 Uiso C3 C 0.2496(17) -0.0015(7) 0.7700(5) 0.034(2) 1.0000 Uiso C4 C 0.3905(15) -0.0835(7) 0.7616(5) 0.031(2) 1.0000 Uiso C5 C 0.2492(19) 0.0493(7) 0.8400(5) 0.038(2) 1.0000 Uiso C6 C 0.077(2) 0.1179(7) 0.8570(5) 0.044(2) 1.0000 Uiso C7 C 0.068(2) 0.1634(9) 0.9236(6) 0.054(3) 1.0000 Uiso C8 C 0.234(2) 0.1428(9) 0.9733(6) 0.060(3) 1.0000 Uiso C9 C 0.403(2) 0.0730(8) 0.9611(6) 0.051(3) 1.0000 Uiso C10 C 0.4141(19) 0.0239(7) 0.8926(5) 0.041(2) 1.0000 Uiso C11 C 0.5883(19) -0.0511(7) 0.8779(5) 0.037(2) 1.0000 Uiso C12 C 0.765(2) -0.0744(8) 0.9264(6) 0.047(2) 1.0000 Uiso C13 C 0.928(2) -0.1440(8) 0.9117(6) 0.051(3) 1.0000 Uiso C14 C 0.924(2) -0.1926(8) 0.8442(6) 0.050(3) 1.0000 Uiso C15 C 0.7543(19) -0.1730(7) 0.7962(5) 0.042(2) 1.0000 Uiso C16 C 0.5760(17) -0.1053(7) 0.8116(5) 0.036(2) 1.0000 Uiso H1 H -0.007(2) -0.0039(8) 0.6180(6) 0.04(1) 1.0000 Uiso H2 H 0.1572(19) -0.1556(7) 0.6144(5) 0.04(1) 1.0000 Uiso H6 H -0.037(2) 0.1333(7) 0.8214(5) 0.04(1) 1.0000 Uiso H7 H -0.052(2) 0.2089(9) 0.9343(6) 0.06(1) 1.0000 Uiso H8 H 0.233(2) 0.1771(9) 1.0184(6) 0.06(1) 1.0000 Uiso H9 H 0.512(2) 0.0578(8) 0.9984(6) 0.05(1) 1.0000 Uiso H12 H 0.772(2) -0.0407(8) 0.9717(6) 0.05(1) 1.0000 Uiso H13 H 1.044(2) -0.1595(8) 0.9469(6) 0.05(1) 1.0000 Uiso H14 H 1.041(2) -0.2391(8) 0.8326(6) 0.05(1) 1.0000 Uiso H15 H 0.7542(19) -0.2057(7) 0.7505(5) 0.04(1) 1.0000 Uiso 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 0.0605(4) 0.0197(3) 0.0551(4) -0.0001(6) -0.003(1) 0.0002(3) F1 0.073(6) 0.106(6) 0.080(5) 0.038(5) 0.004(5) -0.020(5) F2 0.082(6) 0.073(5) 0.083(5) -0.011(4) -0.032(5) 0.021(4) F3 0.081(5) 0.093(5) 0.083(7) -0.046(6) 0.004(7) -0.023(4) F4 0.079(5) 0.049(4) 0.107(6) -0.014(4) 0.004(5) -0.003(4) B1 0.056(8) 0.054(7) 0.051(7) -0.008(6) -0.008(8) -0.003(8) N1 0.049(5) 0.023(3) 0.067(9) -0.003(4) 0.002(5) -0.002(3) N2 0.054(4) 0.023(3) 0.042(3) -0.009(7) 0.006(8) 0.005(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 . F1 1_455 2.633(9) yes Ag1 . F2 . 2.841(9) yes Ag1 . F3 1_455 2.947(8) yes Ag1 . F3 . 2.882(8) yes Ag1 . N1 . 2.265(8) yes Ag1 . N2 2_555 2.255(6) yes F1 . B1 . 1.347(17) yes F2 . B1 . 1.380(17) yes F3 . B1 . 1.430(19) yes F4 . B1 . 1.361(16) yes N1 . C1 . 1.316(15) yes N1 . C3 . 1.359(13) yes N2 . C2 . 1.295(16) yes N2 . C4 . 1.410(16) yes C1 . C2 . 1.365(15) yes C1 . H1 . 0.950 no C2 . H2 . 0.950 no C3 . C4 . 1.393(13) yes C3 . C5 . 1.459(12) yes C4 . C16 . 1.436(13) yes C5 . C6 . 1.398(14) yes C5 . C10 . 1.396(14) yes C6 . C7 . 1.370(16) yes C6 . H6 . 0.950 no C7 . C8 . 1.346(17) yes C7 . H7 . 0.950 no C8 . C9 . 1.379(17) yes C8 . H8 . 0.950 no C9 . C10 . 1.426(14) yes C9 . H9 . 0.950 no C10 . C11 . 1.458(14) yes C11 . C12 . 1.387(15) yes C11 . C16 . 1.425(13) yes C12 . C13 . 1.362(16) yes C12 . H12 . 0.950 no C13 . C14 . 1.405(16) yes C13 . H13 . 0.950 no C14 . C15 . 1.340(15) yes C14 . H14 . 0.950 no C15 . C16 . 1.409(14) yes C15 . H15 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F1 1_455 Ag1 . F2 . 78.9(3) yes F1 1_455 Ag1 . F3 1_455 47.4(3) yes F2 . Ag1 . F3 1_455 125.5(3) yes F1 1_455 Ag1 . F3 . 123.7(3) yes F2 . Ag1 . F3 . 46.3(3) yes F3 1_455 Ag1 . F3 . 160.1(3) yes F1 1_455 Ag1 . N1 . 91.3(3) yes F2 . Ag1 . N1 . 85.3(3) yes F3 1_455 Ag1 . N1 . 87.1(3) yes F3 . Ag1 . N1 . 74.7(3) yes F1 1_455 Ag1 . N2 2_555 104.8(4) yes F2 . Ag1 . N2 2_555 88.6(4) yes F3 1_455 Ag1 . N2 2_555 110.8(2) yes F3 . Ag1 . N2 2_555 88.3(2) yes N1 . Ag1 . N2 2_555 161.3(3) yes Ag1 1_655 F1 . B1 . 107.7(7) yes Ag1 . F2 . B1 . 102.4(8) yes Ag1 . F3 . Ag1 1_655 160.1(3) yes Ag1 . F3 . B1 . 99.1(8) yes Ag1 1_655 F3 . B1 . 91.2(8) yes F1 . B1 . F2 . 112.6(12) yes F1 . B1 . F3 . 109.0(11) yes F2 . B1 . F3 . 106.6(12) yes F1 . B1 . F4 . 111.7(13) yes F2 . B1 . F4 . 110.0(11) yes F3 . B1 . F4 . 106.7(12) yes Ag1 . N1 . C1 . 118.5(8) yes Ag1 . N1 . C3 . 118.9(6) yes C1 . N1 . C3 . 117.2(8) yes Ag1 2_545 N2 . C2 . 116.4(7) yes Ag1 2_545 N2 . C4 . 122.3(9) yes C2 . N2 . C4 . 116.8(7) yes N1 . C1 . C2 . 121.1(10) yes N1 . C1 . H1 . 119.5(6) no C2 . C1 . H1 . 119.5(6) no N2 . C2 . C1 . 124.0(10) yes N2 . C2 . H2 . 118.0(6) no C1 . C2 . H2 . 118.0(6) no N1 . C3 . C4 . 121.8(8) yes N1 . C3 . C5 . 119.4(8) yes C4 . C3 . C5 . 118.8(8) yes N2 . C4 . C3 . 117.6(8) yes N2 . C4 . C16 . 120.5(8) yes C3 . C4 . C16 . 121.9(8) yes C3 . C5 . C6 . 121.2(9) yes C3 . C5 . C10 . 119.1(9) yes C6 . C5 . C10 . 119.6(9) yes C5 . C6 . C7 . 122.0(11) yes C5 . C6 . H6 . 119.0(6) no C7 . C6 . H6 . 119.0(8) no C6 . C7 . C8 . 118.8(12) yes C6 . C7 . H7 . 120.6(8) no C8 . C7 . H7 . 120.6(8) no C7 . C8 . C9 . 122.1(12) yes C7 . C8 . H8 . 118.8(8) no C9 . C8 . H8 . 119.0(7) no C8 . C9 . C10 . 120.1(11) yes C8 . C9 . H9 . 119.9(7) no C10 . C9 . H9 . 120.0(6) no C5 . C10 . C9 . 117.3(9) yes C5 . C10 . C11 . 120.9(9) yes C9 . C10 . C11 . 121.8(9) yes C10 . C11 . C12 . 123.1(9) yes C10 . C11 . C16 . 119.4(9) yes C12 . C11 . C16 . 117.6(9) yes C11 . C12 . C13 . 122.5(10) yes C11 . C12 . H12 . 118.7(6) no C13 . C12 . H12 . 118.8(7) no C12 . C13 . C14 . 119.6(12) yes C12 . C13 . H13 . 120.2(7) no C14 . C13 . H13 . 120.2(8) no C13 . C14 . C15 . 119.6(11) yes C13 . C14 . H14 . 120.2(8) no C15 . C14 . H14 . 120.1(6) no C14 . C15 . C16 . 122.0(10) yes C14 . C15 . H15 . 119.0(6) no C16 . C15 . H15 . 119.0(6) no C4 . C16 . C11 . 118.2(8) yes C4 . C16 . C15 . 123.2(9) yes C11 . C16 . C15 . 118.5(9) yes data_CRYSTALS_cif _database_code_CSD 209272 _audit_creation_date 03-17-04 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Isotropic thermal parameters were refined for all C atoms, since anisotropic refinement would result in an observation to parameters ratio of 4.8 as opposed to the present 7.6. H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.668(2) _cell_angle_alpha 90 _cell_length_b 5.5754(9) _cell_angle_beta 111.963(15) _cell_length_c 13.323(2) _cell_angle_gamma 90 _cell_volume 734.9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Ag ' -1.0850 1.1010 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8157 5.1790 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C16 H10 Ag1 Cl1 N2 O4 ' _chemical_formula_moiety ' C16 H10 Ag1 Cl1 N2 O4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 437.583 _cell_measurement_reflns_used 42 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow-orange ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 1.97 _exptl_crystal_density_meas ? _exptl_crystal_F_000 430.192 _exptl_absorpt_coefficient_mu 15.64 # Sheldrick geometric definitions 1.00 1.00 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_radiation_monochromator graphite _computing_data_collection 'NRC DIFRAC' _computing_cell_refinement 'NRC DIFRAC' _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'SIR 92' #_computing_structure_refinement 'CRYSTALS' #_computing_molecular_graphics 'Ortep-3' #_computing_publication_material 'CRYSTALS' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6834 _exptl_absorpt_correction_T_max 0.8663 _diffrn_standards_interval_time 150 _diffrn_standards_interval_count 27 _diffrn_standards_number 2 _diffrn_standards_decay_% 2.04 _diffrn_ambient_temperature 293 _diffrn_reflns_number 1682 _reflns_number_total 1504 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 1505 # Number of reflections without Friedels Law is 1504 # Theoretical number of reflections is about 1302 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 1052 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -15 _reflns_limit_l_max 15 _refine_diff_density_min -1.66 _refine_diff_density_max 0.98 _reflns_threshold_expression >2.50\s(I) _refine_ls_number_reflns 1052 _refine_ls_number_parameters 139 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0413 _refine_ls_goodness_of_fit_ref 1.1992 _refine_ls_shift/su_max 0.000131 _refine_ls_abs_structure_Flack 0.15(13) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/(.170E-01*F +0.00 *\s^2^(F ) + 0.00 ) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # Data Acquisition # Gabe, E.J., White, P.S., Enright, G.D. DIFRAC A Fortran 77 Control Routine for 4-Circle Diffractometers, N.R.C., Ottawa, 1995. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #Ortep-3 Farrugia, L.J. (1997) J. Appl. Cryst., 30, 565. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type AG1 AG 0.4639(2) 0.19474(17) 1.2857(2) 0.0447 1.0000 Uani CL1 CL -0.1251(4) 0.3351(7) 0.8894(3) 0.0577 1.0000 Uani O1 O -0.2197(15) 0.491(3) 0.8151(13) 0.1303 1.0000 Uani O2 O -0.0149(12) 0.314(3) 0.8510(12) 0.1237 1.0000 Uani O3 O -0.1796(12) 0.103(2) 0.8837(8) 0.0795 1.0000 Uani O4 O -0.082(2) 0.411(3) 0.993(1) 0.1621 1.0000 Uani N1 N 0.3068(12) 0.123(3) 1.121(1) 0.0358 1.0000 Uani N2 N 0.1536(13) -0.135(3) 0.9376(11) 0.0415 1.0000 Uani C1 C 0.2105(13) -0.029(3) 1.119(1) 0.040(3) 1.0000 Uiso C2 C 0.1296(14) -0.146(3) 1.0267(11) 0.046(4) 1.0000 Uiso C3 C 0.3218(11) 0.154(2) 1.0244(8) 0.027(3) 1.0000 Uiso C4 C 0.2538(11) 0.005(2) 0.9353(8) 0.028(3) 1.0000 Uiso C5 C 0.294(1) 0.005(2) 0.8437(7) 0.029(2) 1.0000 Uiso C6 C 0.249(1) -0.183(2) 0.7655(7) 0.032(2) 1.0000 Uiso C7 C 0.2903(11) -0.190(2) 0.6801(9) 0.041(3) 1.0000 Uiso C8 C 0.3810(13) -0.023(3) 0.672(1) 0.050(3) 1.0000 Uiso C9 C 0.4288(11) 0.154(2) 0.7482(8) 0.043(3) 1.0000 Uiso C10 C 0.389(1) 0.171(2) 0.8362(8) 0.036(2) 1.0000 Uiso C11 C 0.4459(11) 0.346(2) 0.9221(9) 0.040(3) 1.0000 Uiso C12 C 0.5364(12) 0.525(2) 0.9150(9) 0.043(3) 1.0000 Uiso C13 C 0.5847(12) 0.698(3) 0.9943(9) 0.047(3) 1.0000 Uiso C14 C 0.5489(12) 0.695(3) 1.081(1) 0.044(3) 1.0000 Uiso C15 C 0.4627(12) 0.515(2) 1.0925(9) 0.039(3) 1.0000 Uiso C16 C 0.413(1) 0.341(2) 1.0134(8) 0.031(2) 1.0000 Uiso H1 H 0.1980(13) -0.058(3) 1.185(1) 0.04(1) 1.0000 Uiso H2 H 0.0566(14) -0.240(3) 1.0289(11) 0.04(1) 1.0000 Uiso H6 H 0.190(1) -0.304(2) 0.7728(7) 0.02(1) 1.0000 Uiso H7 H 0.2569(11) -0.309(2) 0.6259(9) 0.04(1) 1.0000 Uiso H8 H 0.4098(13) -0.029(3) 0.613(1) 0.05(1) 1.0000 Uiso H9 H 0.4911(11) 0.267(2) 0.7408(8) 0.04(1) 1.0000 Uiso H12 H 0.5619(12) 0.526(2) 0.8538(9) 0.04(1) 1.0000 Uiso H13 H 0.6444(12) 0.815(3) 0.9854(9) 0.04(1) 1.0000 Uiso H14 H 0.5867(12) 0.813(3) 1.135(1) 0.04(1) 1.0000 Uiso H15 H 0.4306(12) 0.521(2) 1.1500(9) 0.03(1) 1.0000 Uiso 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 0.0403(4) 0.0569(5) 0.0255(3) -0.0041(11) -0.0009(3) 0.0082(12) Cl1 0.083(2) 0.053(2) 0.0437(16) 0.0031(18) 0.0314(16) -0.015(2) O1 0.138(12) 0.133(13) 0.168(13) 0.092(12) 0.112(11) 0.060(11) O2 0.082(8) 0.126(11) 0.176(13) 0.11(1) 0.06(1) 0.017(9) O3 0.12(1) 0.062(7) 0.056(6) -0.007(5) 0.037(6) -0.048(7) O4 0.31(3) 0.113(13) 0.071(9) -0.025(9) 0.077(12) -0.131(16) N1 0.024(6) 0.053(9) 0.025(5) -0.007(5) 0.002(4) 0.001(5) N2 0.032(7) 0.044(9) 0.046(7) 0.003(6) 0.012(5) 0.005(6) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 . O1 2_565 2.765(14) yes Ag1 . O2 2_555 2.951(16) yes Ag1 . O2 2_565 2.857(13) yes Ag1 . O3 2_555 2.882(12) yes Ag1 . N1 . 2.242(13) yes Ag1 . N2 2_555 2.288(15) yes Cl1 . O1 . 1.415(14) yes Cl1 . O2 . 1.452(13) yes Cl1 . O3 . 1.41(1) yes Cl1 . O4 . 1.356(13) yes N1 . C1 . 1.321(19) yes N1 . C3 . 1.370(17) yes N2 . C2 . 1.306(18) yes N2 . C4 . 1.331(18) yes C1 . C2 . 1.372(19) yes C1 . H1 . 0.950 no C2 . H2 . 0.950 no C3 . C4 . 1.411(16) yes C3 . C16 . 1.467(16) yes C4 . C5 . 1.438(14) yes C5 . C6 . 1.427(15) yes C5 . C10 . 1.408(15) yes C6 . C7 . 1.367(14) yes C6 . H6 . 0.950 no C7 . C8 . 1.375(17) yes C7 . H7 . 0.950 no C8 . C9 . 1.368(16) yes C8 . H8 . 0.950 no C9 . C10 . 1.390(15) yes C9 . H9 . 0.950 no C10 . C11 . 1.450(15) yes C11 . C12 . 1.417(17) yes C11 . C16 . 1.388(14) yes C12 . C13 . 1.381(17) yes C12 . H12 . 0.950 no C13 . C14 . 1.347(16) yes C13 . H13 . 0.950 no C14 . C15 . 1.406(19) yes C14 . H14 . 0.950 no C15 . C16 . 1.385(16) yes C15 . H15 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ag1 . N2 2_555 158.2(4) yes O1 . Cl1 . O2 . 105.3(7) yes O1 . Cl1 . O3 . 110.7(9) yes O2 . Cl1 . O3 . 106.2(9) yes O1 . Cl1 . O4 . 113.8(12) yes O2 . Cl1 . O4 . 112.0(12) yes O3 . Cl1 . O4 . 108.6(7) yes Ag1 . N1 . C1 . 115.4(10) yes Ag1 . N1 . C3 . 126.1(9) yes C1 . N1 . C3 . 115.0(12) yes Ag1 2_454 N2 . C2 . 112.8(10) yes Ag1 2_454 N2 . C4 . 121.1(10) yes C2 . N2 . C4 . 118.6(15) yes N1 . C1 . C2 . 123.2(14) yes N1 . C1 . H1 . 117.5(8) no C2 . C1 . H1 . 119.3(10) no N2 . C2 . C1 . 121.4(16) yes N2 . C2 . H2 . 119.6(10) no C1 . C2 . H2 . 119.0(10) no N1 . C3 . C4 . 120.8(11) yes N1 . C3 . C16 . 120.1(11) yes C4 . C3 . C16 . 119.1(10) yes N2 . C4 . C3 . 119.4(11) yes N2 . C4 . C5 . 121.1(11) yes C3 . C4 . C5 . 119.4(10) yes C4 . C5 . C6 . 119.5(10) yes C4 . C5 . C10 . 120.8(10) yes C6 . C5 . C10 . 119.3(9) yes C5 . C6 . C7 . 120.0(11) yes C5 . C6 . H6 . 120.2(6) no C7 . C6 . H6 . 119.9(8) no C6 . C7 . C8 . 120.3(12) yes C6 . C7 . H7 . 120.3(7) no C8 . C7 . H7 . 119.4(7) no C7 . C8 . C9 . 120.3(12) yes C7 . C8 . H8 . 119.9(7) no C9 . C8 . H8 . 119.7(7) no C8 . C9 . C10 . 122.1(12) yes C8 . C9 . H9 . 118.9(7) no C10 . C9 . H9 . 119.0(7) no C5 . C10 . C9 . 117.8(10) yes C5 . C10 . C11 . 119.1(9) yes C9 . C10 . C11 . 123.0(10) yes C10 . C11 . C12 . 120.9(10) yes C10 . C11 . C16 . 120.6(10) yes C12 . C11 . C16 . 118.4(11) yes C11 . C12 . C13 . 120.6(11) yes C11 . C12 . H12 . 118.7(7) no C13 . C12 . H12 . 120.6(8) no C12 . C13 . C14 . 120.2(13) yes C12 . C13 . H13 . 117.3(8) no C14 . C13 . H13 . 122.5(9) no C13 . C14 . C15 . 120.6(14) yes C13 . C14 . H14 . 117.7(9) no C15 . C14 . H14 . 121.6(8) no C14 . C15 . C16 . 119.9(12) yes C14 . C15 . H15 . 120.5(8) no C16 . C15 . H15 . 119.3(7) no C3 . C16 . C11 . 119.9(10) yes C3 . C16 . C15 . 120.0(10) yes C11 . C16 . C15 . 120.1(11) yes