# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' #TrackingRef '- CrystallographicData.cif' #============================================================================== _journal_coden_Cambridge 1475 _journal_year 2012 _publ_contact_author 'Andrew L. Goodwin' _publ_contact_author_email andrew.goodwin@chem.ox.ac.uk _publ_contact_author_phone '+44 1865 272137' _contact_author_fax '+44 1865 272690' loop_ _publ_author_name _publ_author_address J.M.Ogborn ; Department of Chemistry, University of Oxford, Inorganic Chemistry Laboratory, South Parks Road, Oxford OX1 3QR. UK. ; I.E.Collings ; Department of Chemistry, University of Oxford, Inorganic Chemistry Laboratory, South Parks Road, Oxford OX1 3QR. UK. ; A.L.Thompson ; Chemical Crystallography, Chemistry Research Laboratory, Department of Chemistry, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; S.A.Moggach ; The University of Edinburgh Joseph Black Building West Mains Road Edinburgh EH9 3JJ ; A.L.Goodwin ; Department of Chemistry, University of Oxford, Inorganic Chemistry Laboratory, South Parks Road, Oxford OX1 3QR. UK. ; _journal_volume ? _journal_page_first ? _journal_page_last ? _ccdc_journal_depnumber ? _publ_section_title ; Supramolecular Mechanics in a Metal-Organic Framework ; _publ_section_abstract ; A combination of variable-temperature and variable-pressure single-crystal and powder X-ray diffraction is used to study the thermo- and piezo-mechanical properties of the metal-organic framework (MOF) silver(I) 2-methylimidazolate, Ag(mim). We find the material to exhibit a number of anomalous mechanical properties: negative thermal expansion, colossal positive thermal expansion and the most extreme negative linear compressibility yet observed for a MOF. By considering the mechanical response of individual supramolecular motifs we are able to rationalise the varied and unconventional behaviour of the bulk material. A general inverse correspondence between strength of supramolecular interaction and magnitude of mechanical response is identified. We propose that the consideration of MOF structures in terms of their underlying mechanical building units provides a straightforward qualitative method of directing framework design in order to maximise anomalous mechanical response. ; _publ_contact_author_name 'Andrew L. Goodwin' #============================================================================== data_300K _database_code_depnum_ccdc_archive 'CCDC 881740' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 019jmo11 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 7.8946(6) _cell_length_b 5.9692(4) _cell_length_c 10.8812(10) _cell_angle_alpha 90 _cell_angle_beta 92.454(3) _cell_angle_gamma 90 _cell_volume 512.30(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H6 Ag0.25 N0.25 O3 # Dc = 1.56 Fooo = 360.00 Mu = 10.39 M = 120.55 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.45 FOOO = 360.00 Mu = 37.86 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source . _chemical_formula_weight 188.97 _cell_measurement_reflns_used 1106 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 300 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 2.450 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.786 # Sheldrick geometric approximatio 0.68 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 300 _diffrn_reflns_number 4050 _reflns_number_total 1174 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections without Friedels Law is 2023 # Number of reflections with Friedels Law is 1174 # Theoretical number of reflections is about 1179 _diffrn_reflns_theta_min 3.125 _diffrn_reflns_theta_max 27.514 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.963 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.44 _refine_diff_density_max 1.13 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1169 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0728 _refine_ls_wR_factor_ref 0.0735 _refine_ls_goodness_of_fit_ref 1.0241 _refine_ls_shift/su_max 0.0000499 _refine_ls_shift/su_mean 0.0000072 # The values computed from all data _oxford_reflns_number_all 1169 _refine_ls_R_factor_all 0.0728 _refine_ls_wR_factor_all 0.0735 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 631 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_gt 0.0466 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 5.84 7.15 2.02 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0364 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0391 1.0000 Uani S . . . . . C1 C 0.3806(11) 0.9500(15) 0.6846(8) 0.0468 1.0000 Uani . . . . . . C2 C 0.4797(8) 0.7634(12) 0.7444(6) 0.0237 1.0000 Uani . . . . . . C3 C 0.6194(9) 0.4535(13) 0.7728(6) 0.0320 1.0000 Uani . . . . . . C4 C 0.6155(10) 0.5588(13) 0.8805(6) 0.0371 1.0000 Uani . . . . . . N1 N 0.5320(7) 0.5817(10) 0.6841(4) 0.0281 1.0000 Uani . . . . . . N2 N 0.5286(8) 0.7588(10) 0.8653(5) 0.0296 1.0000 Uani . . . . . . H13 H 0.3919 1.0817 0.7334 0.0699 1.0000 Uiso R . . . . . H12 H 0.4197 0.9807 0.6051 0.0699 1.0000 Uiso R . . . . . H11 H 0.2647 0.9090 0.6778 0.0701 1.0000 Uiso R . . . . . H31 H 0.6722 0.3164 0.7587 0.0381 1.0000 Uiso R . . . . . H41 H 0.6645 0.5086 0.9540 0.0439 1.0000 Uiso 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 0.0562(5) 0.0358(5) 0.0172(4) -0.0100(3) 0.0027(3) -0.0037(4) Ag2 0.0576(6) 0.0390(5) 0.0210(4) -0.0143(3) 0.0059(3) -0.0042(4) C1 0.050(5) 0.043(5) 0.047(4) 0.001(4) -0.004(4) 0.004(4) C2 0.031(3) 0.022(3) 0.018(3) -0.005(2) 0.003(2) -0.003(3) C3 0.031(4) 0.034(4) 0.030(3) -0.002(3) 0.000(3) 0.000(3) C4 0.049(4) 0.038(4) 0.024(3) 0.004(3) 0.000(3) -0.002(4) N1 0.035(3) 0.032(3) 0.017(2) -0.010(2) 0.002(2) -0.001(3) N2 0.040(3) 0.033(3) 0.016(2) -0.005(2) 0.005(2) -0.002(3) _refine_ls_extinction_coef 7.9(6) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2522(4) 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 . N1 2_666 2.067(5) yes Ag1 . N1 . 2.067(5) yes Ag2 . N2 2_677 2.074(5) yes Ag2 . N2 . 2.074(5) yes C1 . C2 . 1.494(10) yes C1 . H13 . 0.951 no C1 . H12 . 0.949 no C1 . H11 . 0.947 no C2 . N1 . 1.342(8) yes C2 . N2 . 1.356(8) yes C3 . C4 . 1.332(9) yes C3 . N1 . 1.391(8) yes C3 . H31 . 0.934 no C4 . N2 . 1.383(10) yes C4 . H41 . 0.924 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 109.8 no C2 . C1 . H12 . 110.9 no H13 . C1 . H12 . 108.8 no C2 . C1 . H11 . 109.1 no H13 . C1 . H11 . 109.0 no H12 . C1 . H11 . 109.2 no C1 . C2 . N1 . 123.8(6) yes C1 . C2 . N2 . 124.0(7) yes N1 . C2 . N2 . 112.2(6) yes C4 . C3 . N1 . 108.7(6) yes C4 . C3 . H31 . 125.8 no N1 . C3 . H31 . 125.4 no C3 . C4 . N2 . 109.4(6) yes C3 . C4 . H41 . 125.8 no N2 . C4 . H41 . 124.8 no C3 . N1 . C2 . 105.0(5) yes C3 . N1 . Ag1 . 125.4(4) yes C2 . N1 . Ag1 . 129.6(5) yes C4 . N2 . C2 . 104.6(6) yes C4 . N2 . Ag2 . 125.7(4) yes C2 . N2 . Ag2 . 129.6(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/01/12 at 15:46:05 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/01/12 at 15:46:05 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 1 1 0 x . _chemical_name_common . #============================================================================== data_250K _database_code_depnum_ccdc_archive 'CCDC 881741' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 016jmo11 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 7.8401(6) _cell_length_b 5.9549(4) _cell_length_c 10.8935(10) _cell_angle_alpha 90 _cell_angle_beta 92.556(3) _cell_angle_gamma 90 _cell_volume 508.08(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C4 H5 Ag1 N2 # Dc = 2.47 Fooo = 360.00 Mu = 38.17 M = 188.97 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.47 FOOO = 360.00 Mu = 38.17 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source . _chemical_formula_weight 188.97 _cell_measurement_reflns_used 1090 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 250 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.817 # Sheldrick geometric approximatio 0.68 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 250 _diffrn_reflns_number 3941 _reflns_number_total 1162 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 1996 # Number of reflections with Friedels Law is 1162 # Theoretical number of reflections is about 1170 _diffrn_reflns_theta_min 3.136 _diffrn_reflns_theta_max 27.522 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.320 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 2.15 _oxford_diffrn_Wilson_scale 17.85 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.17 _refine_diff_density_max 1.20 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1157 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0673 _refine_ls_wR_factor_ref 0.0699 _refine_ls_goodness_of_fit_ref 1.0417 _refine_ls_shift/su_max 0.0000526 _refine_ls_shift/su_mean 0.0000045 # The values computed from all data _oxford_reflns_number_all 1157 _refine_ls_R_factor_all 0.0673 _refine_ls_wR_factor_all 0.0699 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 641 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_gt 0.0463 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 5.94 7.22 2.09 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0301 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0319 1.0000 Uani S . . . . . C1 C 0.3801(9) 0.9487(14) 0.6848(7) 0.0352 1.0000 Uani . . . . . . C2 C 0.4813(9) 0.7643(13) 0.7447(6) 0.0234 1.0000 Uani . . . . . . C3 C 0.6190(9) 0.4520(12) 0.7720(6) 0.0273 1.0000 Uani . . . . . . C4 C 0.6144(9) 0.5577(13) 0.8808(6) 0.0285 1.0000 Uani . . . . . . N1 N 0.5320(7) 0.5806(9) 0.6842(5) 0.0241 1.0000 Uani . . . . . . N2 N 0.5284(7) 0.7580(10) 0.8640(5) 0.0269 1.0000 Uani . . . . . . H13 H 0.3831 1.0782 0.7363 0.0528 1.0000 Uiso R . . . . . H12 H 0.4273 0.9857 0.6080 0.0531 1.0000 Uiso R . . . . . H11 H 0.2652 0.9000 0.6712 0.0532 1.0000 Uiso R . . . . . H31 H 0.6716 0.3149 0.7580 0.0331 1.0000 Uiso R . . . . . H41 H 0.6619 0.5059 0.9546 0.0340 1.0000 Uiso 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 0.0455(5) 0.0302(5) 0.0148(3) -0.0083(3) 0.0026(3) -0.0025(4) Ag2 0.0473(5) 0.0312(5) 0.0176(4) -0.0112(3) 0.0053(3) -0.0034(4) C1 0.034(4) 0.031(4) 0.041(4) -0.003(4) 0.002(3) 0.004(3) C2 0.027(3) 0.027(3) 0.016(3) -0.008(2) 0.002(2) 0.002(3) C3 0.033(4) 0.023(3) 0.027(3) -0.002(3) 0.006(3) 0.003(3) C4 0.033(4) 0.034(4) 0.019(3) 0.001(3) 0.001(2) 0.006(3) N1 0.031(3) 0.025(3) 0.016(2) -0.007(2) 0.002(2) 0.001(3) N2 0.032(3) 0.029(3) 0.020(3) -0.005(2) 0.002(2) -0.002(3) _refine_ls_extinction_coef 7.5(6) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2531(4) 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 . N1 2_666 2.068(5) yes Ag1 . N1 . 2.068(5) yes Ag2 . N2 2_677 2.086(6) yes Ag2 . N2 . 2.086(6) yes C1 . C2 . 1.488(10) yes C1 . H13 . 0.953 no C1 . H12 . 0.955 no C1 . H11 . 0.952 no C2 . N1 . 1.346(9) yes C2 . N2 . 1.336(8) yes C3 . C4 . 1.343(9) yes C3 . N1 . 1.381(8) yes C3 . H31 . 0.930 no C4 . N2 . 1.378(9) yes C4 . H41 . 0.924 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 109.9 no C2 . C1 . H12 . 109.6 no H13 . C1 . H12 . 109.2 no C2 . C1 . H11 . 109.0 no H13 . C1 . H11 . 109.7 no H12 . C1 . H11 . 109.5 no C1 . C2 . N1 . 123.3(6) yes C1 . C2 . N2 . 124.5(7) yes N1 . C2 . N2 . 112.2(6) yes C4 . C3 . N1 . 108.6(6) yes C4 . C3 . H31 . 125.8 no N1 . C3 . H31 . 125.6 no C3 . C4 . N2 . 108.7(6) yes C3 . C4 . H41 . 125.8 no N2 . C4 . H41 . 125.4 no C3 . N1 . C2 . 105.0(5) yes C3 . N1 . Ag1 . 125.3(4) yes C2 . N1 . Ag1 . 129.6(5) yes C4 . N2 . C2 . 105.4(6) yes C4 . N2 . Ag2 . 124.8(4) yes C2 . N2 . Ag2 . 129.6(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/01/12 at 16:11:11 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/01/12 at 16:11:11 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 1 1 0 x . _chemical_name_common . #============================================================================== data_200K _database_code_depnum_ccdc_archive 'CCDC 881742' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 017jmo11 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 7.7899(6) _cell_length_b 5.9402(4) _cell_length_c 10.9075(10) _cell_angle_alpha 90 _cell_angle_beta 92.670(3) _cell_angle_gamma 90 _cell_volume 504.18(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C4 H5 Ag1 N2 # Dc = 2.49 Fooo = 360.00 Mu = 38.46 M = 188.97 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.49 FOOO = 360.00 Mu = 38.46 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source . _chemical_formula_weight 188.97 _cell_measurement_reflns_used 1084 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 2.489 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.846 # Sheldrick geometric approximatio 0.68 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 3980 _reflns_number_total 1147 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections without Friedels Law is 1989 # Number of reflections with Friedels Law is 1147 # Theoretical number of reflections is about 1158 _diffrn_reflns_theta_min 3.145 _diffrn_reflns_theta_max 27.502 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.302 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 1.84 _oxford_diffrn_Wilson_scale 17.21 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.20 _refine_diff_density_max 1.13 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1143 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0615 _refine_ls_wR_factor_ref 0.0843 _refine_ls_goodness_of_fit_ref 1.0074 _refine_ls_shift/su_max 0.0000438 _refine_ls_shift/su_mean 0.0000077 # The values computed from all data _oxford_reflns_number_all 1143 _refine_ls_R_factor_all 0.0615 _refine_ls_wR_factor_all 0.0843 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 626 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_gt 0.0538 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 9.30 13.4 6.58 1.73 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0248 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0262 1.0000 Uani S . . . . . C1 C 0.3775(9) 0.9503(12) 0.6848(6) 0.0308 1.0000 Uani . . . . . . C2 C 0.4794(7) 0.7644(11) 0.7440(5) 0.0211 1.0000 Uani . . . . . . C3 C 0.6171(7) 0.4491(12) 0.7719(5) 0.0252 1.0000 Uani . . . . . . C4 C 0.6141(8) 0.5569(12) 0.8806(5) 0.0274 1.0000 Uani . . . . . . N1 N 0.5313(6) 0.5800(9) 0.6848(4) 0.0198 1.0000 Uani . . . . . . N2 N 0.5288(7) 0.7573(10) 0.8647(4) 0.0230 1.0000 Uani . . . . . . H13 H 0.3760 1.0765 0.7379 0.0447 1.0000 Uiso R . . . . . H12 H 0.4273 0.9939 0.6107 0.0448 1.0000 Uiso R . . . . . H11 H 0.2632 0.8997 0.6667 0.0454 1.0000 Uiso R . . . . . H31 H 0.6685 0.3118 0.7575 0.0290 1.0000 Uiso R . . . . . H41 H 0.6621 0.5038 0.9540 0.0319 1.0000 Uiso 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 0.0368(4) 0.0247(4) 0.0129(3) -0.0066(2) 0.0018(2) -0.0013(3) Ag2 0.0386(4) 0.0257(4) 0.0147(3) -0.0088(2) 0.0039(2) -0.0021(3) C1 0.038(4) 0.023(3) 0.032(3) 0.000(3) 0.002(3) 0.003(3) C2 0.025(3) 0.025(3) 0.014(2) -0.004(2) 0.003(2) -0.010(3) C3 0.022(3) 0.027(3) 0.027(3) 0.004(3) 0.005(2) 0.003(3) C4 0.031(3) 0.033(4) 0.017(3) 0.004(3) -0.003(2) 0.001(3) N1 0.024(2) 0.023(2) 0.013(2) -0.006(2) 0.0027(17) 0.005(2) N2 0.030(3) 0.026(3) 0.012(2) -0.0046(19) 0.0022(18) -0.003(2) _refine_ls_extinction_coef 9.9(10) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2555(5) 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 . N1 2_666 2.074(4) yes Ag1 . N1 . 2.074(4) yes Ag2 . N2 2_677 2.083(5) yes Ag2 . N2 . 2.083(5) yes C1 . C2 . 1.490(9) yes C1 . H13 . 0.947 no C1 . H12 . 0.948 no C1 . H11 . 0.952 no C2 . N1 . 1.344(8) yes C2 . N2 . 1.355(6) yes C3 . C4 . 1.348(8) yes C3 . N1 . 1.377(7) yes C3 . H31 . 0.925 no C4 . N2 . 1.371(9) yes C4 . H41 . 0.924 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 110.0 no C2 . C1 . H12 . 109.9 no H13 . C1 . H12 . 108.8 no C2 . C1 . H11 . 109.3 no H13 . C1 . H11 . 109.8 no H12 . C1 . H11 . 109.0 no C1 . C2 . N1 . 124.2(5) yes C1 . C2 . N2 . 124.5(6) yes N1 . C2 . N2 . 111.3(6) yes C4 . C3 . N1 . 108.1(6) yes C4 . C3 . H31 . 126.4 no N1 . C3 . H31 . 125.5 no C3 . C4 . N2 . 109.2(5) yes C3 . C4 . H41 . 125.3 no N2 . C4 . H41 . 125.5 no C3 . N1 . C2 . 106.0(5) yes C3 . N1 . Ag1 . 124.9(4) yes C2 . N1 . Ag1 . 129.0(4) yes C4 . N2 . C2 . 105.3(5) yes C4 . N2 . Ag2 . 125.4(4) yes C2 . N2 . Ag2 . 129.2(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/01/12 at 16:26:53 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/01/12 at 16:26:53 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _chemical_name_common . #============================================================================== data_150K _database_code_depnum_ccdc_archive 'CCDC 881743' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 018jmo11 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 7.7378(6) _cell_length_b 5.9245(4) _cell_length_c 10.9232(9) _cell_angle_alpha 90 _cell_angle_beta 92.821(3) _cell_angle_gamma 90 _cell_volume 500.14(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C4 H5 Ag1 N2 # Dc = 2.51 Fooo = 360.00 Mu = 38.78 M = 188.97 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.51 FOOO = 360.00 Mu = 38.78 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source . _chemical_formula_weight 188.97 _cell_measurement_reflns_used 1094 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 2.509 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.878 # Sheldrick geometric approximatio 0.68 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 3972 _reflns_number_total 1126 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 1980 # Number of reflections with Friedels Law is 1126 # Theoretical number of reflections is about 1136 _diffrn_reflns_theta_min 3.154 _diffrn_reflns_theta_max 27.387 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.839 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 1.51 _oxford_diffrn_Wilson_scale 16.97 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.39 _refine_diff_density_max 1.18 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1122 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0562 _refine_ls_wR_factor_ref 0.0642 _refine_ls_goodness_of_fit_ref 1.0290 _refine_ls_shift/su_max 0.0000627 _refine_ls_shift/su_mean 0.0000115 # The values computed from all data _oxford_reflns_number_all 1122 _refine_ls_R_factor_all 0.0562 _refine_ls_wR_factor_all 0.0642 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 640 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_gt 0.0418 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.30 7.76 2.17 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0183 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0193 1.0000 Uani S . . . . . C1 C 0.3782(8) 0.9537(11) 0.6869(6) 0.0224 1.0000 Uani . . . . . . C2 C 0.4790(7) 0.7625(11) 0.7447(5) 0.0156 1.0000 Uani . . . . . . C3 C 0.6161(7) 0.4467(11) 0.7714(5) 0.0198 1.0000 Uani . . . . . . C4 C 0.6147(7) 0.5569(11) 0.8806(5) 0.0204 1.0000 Uani . . . . . . N1 N 0.5316(6) 0.5793(8) 0.6841(4) 0.0166 1.0000 Uani . . . . . . N2 N 0.5270(6) 0.7585(9) 0.8645(4) 0.0178 1.0000 Uani . . . . . . H13 H 0.3805 1.0823 0.7396 0.0341 1.0000 Uiso R . . . . . H12 H 0.4265 0.9962 0.6122 0.0338 1.0000 Uiso R . . . . . H11 H 0.2606 0.9096 0.6693 0.0342 1.0000 Uiso R . . . . . H31 H 0.6668 0.3072 0.7577 0.0238 1.0000 Uiso R . . . . . H41 H 0.6649 0.5056 0.9541 0.0247 1.0000 Uiso 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 0.0270(4) 0.0179(3) 0.0100(3) -0.0045(2) 0.0016(2) -0.0013(3) Ag2 0.0291(4) 0.0186(4) 0.0104(3) -0.0062(2) 0.0034(2) -0.0017(3) C1 0.025(3) 0.017(3) 0.026(3) 0.002(3) -0.002(2) 0.000(3) C2 0.016(3) 0.016(3) 0.015(2) -0.003(2) 0.006(2) -0.005(2) C3 0.021(3) 0.018(3) 0.022(3) -0.002(2) 0.002(2) 0.005(2) C4 0.019(3) 0.025(3) 0.017(3) 0.003(3) -0.003(2) 0.000(3) N1 0.019(2) 0.018(2) 0.013(2) -0.0039(19) 0.0021(18) 0.002(2) N2 0.021(2) 0.024(3) 0.009(2) -0.005(2) 0.0018(17) 0.001(2) _refine_ls_extinction_coef 7.2(6) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2502(4) 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 . N1 2_666 2.068(4) yes Ag1 . N1 . 2.068(4) yes Ag2 . N2 2_677 2.077(5) yes Ag2 . N2 . 2.077(5) yes C1 . C2 . 1.497(8) yes C1 . H13 . 0.955 no C1 . H12 . 0.949 no C1 . H11 . 0.957 no C2 . N1 . 1.345(8) yes C2 . N2 . 1.343(7) yes C3 . C4 . 1.360(8) yes C3 . N1 . 1.376(7) yes C3 . H31 . 0.930 no C4 . N2 . 1.381(8) yes C4 . H41 . 0.926 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 110.8 no C2 . C1 . H12 . 110.1 no H13 . C1 . H12 . 108.1 no C2 . C1 . H11 . 110.4 no H13 . C1 . H11 . 109.2 no H12 . C1 . H11 . 108.1 no C1 . C2 . N1 . 124.6(5) yes C1 . C2 . N2 . 122.5(5) yes N1 . C2 . N2 . 112.9(5) yes C4 . C3 . N1 . 108.0(5) yes C4 . C3 . H31 . 126.1 no N1 . C3 . H31 . 125.8 no C3 . C4 . N2 . 109.2(5) yes C3 . C4 . H41 . 125.6 no N2 . C4 . H41 . 125.3 no C3 . N1 . C2 . 105.4(5) yes C3 . N1 . Ag1 . 125.0(4) yes C2 . N1 . Ag1 . 129.6(4) yes C4 . N2 . C2 . 104.5(5) yes C4 . N2 . Ag2 . 124.8(4) yes C2 . N2 . Ag2 . 130.5(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/01/12 at 16:57:01 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/01/12 at 16:57:01 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _chemical_name_common . #============================================================================== data_100K _database_code_depnum_ccdc_archive 'CCDC 881744' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 019jmo11 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 7.6885(6) _cell_length_b 5.9097(4) _cell_length_c 10.9351(9) _cell_angle_alpha 90 _cell_angle_beta 92.984(3) _cell_angle_gamma 90 _cell_volume 496.18(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C4 H5 Ag1 N2 # Dc = 2.53 Fooo = 360.00 Mu = 39.09 M = 188.97 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.53 FOOO = 360.00 Mu = 39.09 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source . _chemical_formula_weight 188.97 _cell_measurement_reflns_used 1092 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 100 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 2.529 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.909 # Sheldrick geometric approximatio 0.68 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 100 _diffrn_reflns_number 3937 _reflns_number_total 1135 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections without Friedels Law is 1990 # Number of reflections with Friedels Law is 1135 # Theoretical number of reflections is about 1149 _diffrn_reflns_theta_min 3.163 _diffrn_reflns_theta_max 27.579 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.752 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 1.13 _oxford_diffrn_Wilson_scale 16.86 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.08 _refine_diff_density_max 1.35 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1131 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0547 _refine_ls_wR_factor_ref 0.0636 _refine_ls_goodness_of_fit_ref 1.0166 _refine_ls_shift/su_max 0.0000526 _refine_ls_shift/su_mean 0.0000082 # The values computed from all data _oxford_reflns_number_all 1131 _refine_ls_R_factor_all 0.0547 _refine_ls_wR_factor_all 0.0636 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 654 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_gt 0.0438 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.83 8.48 2.45 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0126 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0134 1.0000 Uani S . . . . . C1 C 0.3769(7) 0.9516(11) 0.6857(5) 0.0168 1.0000 Uani . . . . . . C2 C 0.4804(7) 0.7623(11) 0.7446(5) 0.0125 1.0000 Uani . . . . . . C3 C 0.6180(7) 0.4447(10) 0.7715(5) 0.0129 1.0000 Uani . . . . . . C4 C 0.6159(7) 0.5552(11) 0.8812(5) 0.0161 1.0000 Uani . . . . . . N1 N 0.5304(6) 0.5788(8) 0.6840(4) 0.0132 1.0000 Uani . . . . . . N2 N 0.5272(6) 0.7563(9) 0.8649(4) 0.0142 1.0000 Uani . . . . . . H13 H 0.3818 1.0811 0.7385 0.0251 1.0000 Uiso R . . . . . H12 H 0.4239 0.9917 0.6104 0.0245 1.0000 Uiso R . . . . . H11 H 0.2579 0.9062 0.6709 0.0250 1.0000 Uiso R . . . . . H31 H 0.6690 0.3048 0.7566 0.0160 1.0000 Uiso R . . . . . H41 H 0.6650 0.5026 0.9544 0.0189 1.0000 Uiso 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 0.0187(3) 0.0123(3) 0.0070(3) -0.0031(2) 0.0013(2) -0.0004(2) Ag2 0.0193(3) 0.0130(3) 0.0080(3) -0.0041(2) 0.0020(2) -0.0011(2) C1 0.015(3) 0.018(3) 0.017(3) 0.002(3) -0.001(2) 0.002(2) C2 0.015(3) 0.013(3) 0.009(2) 0.000(2) 0.0033(19) -0.002(2) C3 0.013(3) 0.011(3) 0.014(3) 0.000(2) -0.001(2) 0.003(2) C4 0.015(3) 0.023(3) 0.010(2) 0.005(2) 0.0007(19) -0.002(2) N1 0.016(2) 0.013(2) 0.011(2) -0.0034(18) -0.0018(17) 0.001(2) N2 0.017(2) 0.016(2) 0.009(2) -0.0041(19) 0.0001(17) 0.003(2) _refine_ls_extinction_coef 6.2(5) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2484(4) 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 . N1 2_666 2.067(4) yes Ag1 . N1 . 2.067(4) yes Ag2 . N2 2_677 2.082(5) yes Ag2 . N2 . 2.082(5) yes C1 . C2 . 1.499(8) yes C1 . H13 . 0.959 no C1 . H12 . 0.947 no C1 . H11 . 0.959 no C2 . N1 . 1.338(8) yes C2 . N2 . 1.345(7) yes C3 . C4 . 1.367(8) yes C3 . N1 . 1.389(7) yes C3 . H31 . 0.933 no C4 . N2 . 1.377(8) yes C4 . H41 . 0.921 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 109.5 no C2 . C1 . H12 . 110.0 no H13 . C1 . H12 . 108.6 no C2 . C1 . H11 . 110.1 no H13 . C1 . H11 . 109.4 no H12 . C1 . H11 . 109.1 no C1 . C2 . N1 . 123.5(5) yes C1 . C2 . N2 . 123.2(5) yes N1 . C2 . N2 . 113.2(5) yes C4 . C3 . N1 . 107.7(5) yes C4 . C3 . H31 . 126.9 no N1 . C3 . H31 . 125.4 no C3 . C4 . N2 . 109.0(5) yes C3 . C4 . H41 . 125.3 no N2 . C4 . H41 . 125.6 no C3 . N1 . C2 . 105.2(4) yes C3 . N1 . Ag1 . 124.6(4) yes C2 . N1 . Ag1 . 130.1(4) yes C4 . N2 . C2 . 104.8(5) yes C4 . N2 . Ag2 . 124.9(4) yes C2 . N2 . Ag2 . 130.1(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/01/12 at 17:04:58 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/01/12 at 17:04:58 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _chemical_name_common . #============================================================================== data_0.0GPa _database_code_depnum_ccdc_archive 'CCDC 881745' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-05-11 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'ST1020 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C5 H5 Ag0.25 N1 # Dc = 1.37 Fooo = 360.00 Mu = 9.91 M = 106.07 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.45 FOOO = 360.00 Mu = 37.84 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure '101.325 ' _publ_section_exptl_refinement ; 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.02 This is caused by the methyl group on the imidazole ligand, which shows slightly larger thermal motion due to its greater flexibility than those atoms within the ring. The principal axes of the thermal elipsoids however are all very reasonable for room temperature data; Principal axes of the thermal ellipsoids, A**2 Min Med Max Uarith Ugeom Uprime AG 1. 0.0123 0.0408 0.0542 0.0358 0.0301 0.1795 AG 2. 0.0124 0.0442 0.0589 0.0385 0.0318 0.2103 C 1. 0.0358 0.0388 0.0540 0.0429 0.0422 0.0585 C 2. 0.0164 0.0288 0.0355 0.0269 0.0256 0.0626 C 3. 0.0263 0.0329 0.0357 0.0316 0.0314 0.0448 C 4. 0.0237 0.0379 0.0393 0.0337 0.0328 0.0630 N 1. 0.0148 0.0312 0.0384 0.0281 0.0261 0.0810 N 2. 0.0144 0.0329 0.0397 0.0290 0.0266 0.0907 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 7 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 76 The data are complete. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.998 531 530 1 23.01 0.550 0.999 715 714 1 25.24 0.600 0.999 929 928 1 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.998 1178 1176 2 29.43 0.691 0.946 1417 1340 77 128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n This was chosen as to get a beta angle closer to 90 degrees. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 7.8926(5) _cell_length_b 5.9767(3) _cell_length_c 10.8739(6) _cell_angle_alpha 90 _cell_angle_beta 92.470(5) _cell_angle_gamma 90 _cell_volume 512.46(5) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 3476 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.449 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.784 # Sheldrick geometric approximatio 0.47 0.68 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.68 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 9493 _reflns_number_total 1341 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1341 # Theoretical number of reflections is about 2837 _diffrn_reflns_theta_min 3.126 _diffrn_reflns_theta_max 29.431 _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.605 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 8 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 2.56 _oxford_diffrn_Wilson_scale 0.01 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.64 _refine_diff_density_max 0.64 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 1340 _refine_ls_number_restraints 0 _refine_ls_number_parameters 68 _oxford_refine_ls_R_factor_ref 0.0379 _refine_ls_wR_factor_ref 0.0681 _refine_ls_goodness_of_fit_ref 1.0721 _refine_ls_shift/su_max 0.0004978 _refine_ls_shift/su_mean 0.0000832 # The values computed from all data _oxford_reflns_number_all 1340 _refine_ls_R_factor_all 0.0379 _refine_ls_wR_factor_all 0.0681 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1026 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_gt 0.0602 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.52P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Oxford Diffraction, (2010). CrysAlisPro. Oxford Diffraction, (2002). Xcalibur User Manual. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0358 1.0000 Uani S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0385 1.0000 Uani S . . . . . C1 C 0.3799(5) 0.9478(6) 0.6858(3) 0.0429 1.0000 Uani . . . . . . C2 C 0.4799(3) 0.7640(4) 0.7447(2) 0.0269 1.0000 Uani . . . . . . C3 C 0.6173(4) 0.4523(5) 0.7713(3) 0.0316 1.0000 Uani . . . . . . C4 C 0.6149(4) 0.5600(5) 0.8805(3) 0.0337 1.0000 Uani . . . . . . N1 N 0.5320(3) 0.5813(4) 0.68473(19) 0.0281 1.0000 Uani . . . . . . N2 N 0.5279(3) 0.7582(4) 0.86418(19) 0.0290 1.0000 Uani . . . . . . H13 H 0.2676 0.9033 0.6662 0.0685 1.0000 Uiso R . . . . . H12 H 0.4294 0.9947 0.6106 0.0682 1.0000 Uiso R . . . . . H11 H 0.3773 1.0759 0.7393 0.0673 1.0000 Uiso R . . . . . H31 H 0.6693 0.3118 0.7571 0.0401 1.0000 Uiso R . . . . . H41 H 0.6646 0.5070 0.9561 0.0433 1.0000 Uiso 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 0.0533(3) 0.0364(2) 0.01769(19) -0.01138(11) 0.00231(14) -0.00360(13) Ag2 0.0560(3) 0.0386(2) 0.0213(2) -0.01510(12) 0.00630(15) -0.00454(14) C1 0.048(2) 0.0396(17) 0.0402(19) -0.0041(15) -0.0037(15) 0.0046(16) C2 0.0324(14) 0.0290(14) 0.0194(13) -0.0062(11) 0.0022(11) -0.0033(12) C3 0.0334(16) 0.0307(14) 0.0311(16) -0.0034(12) 0.0044(12) 0.0009(12) C4 0.0375(17) 0.0382(16) 0.0249(14) 0.0004(13) -0.0030(12) -0.0004(14) N1 0.0312(12) 0.0327(13) 0.0204(11) -0.0100(10) 0.0012(9) 0.0006(11) N2 0.0371(13) 0.0322(13) 0.0178(10) -0.0077(9) 0.0031(9) -0.0029(10) _refine_ls_extinction_coef 14.8(13) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 5.37(17) 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 . N1 2_666 2.072(2) yes Ag1 . N1 . 2.072(2) yes Ag2 . N2 2_677 2.085(2) yes Ag2 . N2 . 2.085(2) yes C1 . C2 . 1.482(4) yes C1 . H13 . 0.941 no C1 . H12 . 0.963 no C1 . H11 . 0.961 no C2 . N1 . 1.345(3) yes C2 . N2 . 1.338(3) yes C3 . C4 . 1.351(4) yes C3 . N1 . 1.371(4) yes C3 . H31 . 0.950 no C4 . N2 . 1.377(4) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H13 . 111.5 no C2 . C1 . H12 . 110.8 no H13 . C1 . H12 . 107.5 no C2 . C1 . H11 . 110.7 no H13 . C1 . H11 . 108.6 no H12 . C1 . H11 . 107.6 no C1 . C2 . N1 . 124.1(2) yes C1 . C2 . N2 . 124.2(2) yes N1 . C2 . N2 . 111.7(2) yes C4 . C3 . N1 . 108.1(3) yes C4 . C3 . H31 . 125.9 no N1 . C3 . H31 . 126.0 no C3 . C4 . N2 . 108.8(3) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.7 no C3 . N1 . C2 . 105.9(2) yes C3 . N1 . Ag1 . 124.74(19) yes C2 . N1 . Ag1 . 129.30(19) yes C4 . N2 . C2 . 105.4(2) yes C4 . N2 . Ag2 . 124.92(18) yes C2 . N2 . Ag2 . 129.49(19) yes _iucr_refine_instruction_details_constraints ; # # Punched on 11/05/11 at 09:21:19 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/05/11 at 09:21:19 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -6 2 12 x . #============================================================================== data_1.1GPa _database_code_depnum_ccdc_archive 'CCDC 881746' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-05-19 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'st1025 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag1 N2 # Dc = 2.50 Fooo = 360.00 Mu = 41.16 M = 176.95 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.67 FOOO = 360.00 Mu = 41.25 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure '1 100 000 ' _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.36 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 17.38 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.38 023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.17 Deg. 342_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 25 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.554 57 088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.57 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6 These are all caused by shading of the pressure cell. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). 380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 This has been placed geometrically. 731_ALERT_1_C Bond Calc 1.48(3), Rep 1.481(9) ...... 3.33 su-Ra C1 -C2 1.555 1.555 731_ALERT_1_C Bond Calc 1.35(2), Rep 1.355(9) ...... 2.22 su-Ra C3 -C4 1.555 1.555 731_ALERT_1_C Bond Calc 1.368(19), Rep 1.369(9) ...... 2.11 su-Ra C3 -N1 1.555 1.555 731_ALERT_1_C Bond Calc 1.38(2), Rep 1.378(9) ...... 2.22 su-Ra C4 -N2 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 7.433(2) _cell_length_b 5.8092(3) _cell_length_c 10.9101(5) _cell_angle_alpha 90 _cell_angle_beta 93.736(10) _cell_angle_gamma 90 _cell_volume 470.09(13) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 518 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.670 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.125 # Sheldrick geometric approximatio 0.44 0.66 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.66 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 1222 _reflns_number_total 241 _diffrn_reflns_av_R_equivalents 0.033 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 241 # Theoretical number of reflections is about 1337 _diffrn_reflns_theta_min 3.743 _diffrn_reflns_theta_max 23.175 _diffrn_measured_fraction_theta_max 0.357 _diffrn_reflns_theta_full 17.381 _diffrn_measured_fraction_theta_full 0.378 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -2 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.54 _refine_diff_density_max 1.34 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 240 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.1072 _refine_ls_wR_factor_ref 0.2123 _refine_ls_goodness_of_fit_ref 1.1132 _refine_ls_shift/su_max 0.0019476 _refine_ls_shift/su_mean 0.0003112 # The values computed from all data _oxford_reflns_number_all 240 _refine_ls_R_factor_all 0.1072 _refine_ls_wR_factor_all 0.2123 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 151 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_gt 0.2029 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +41.61P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0202(13) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0234(14) 1.0000 Uiso S . . . . . C1 C 0.376(7) 0.951(4) 0.682(2) 0.013(3) 1.0000 Uiso D U . . . . C2 C 0.4804(15) 0.762(2) 0.7434(12) 0.013(3) 1.0000 Uiso D U . . . . C3 C 0.6173(15) 0.435(2) 0.7731(16) 0.012(3) 1.0000 Uiso D U . . . . C4 C 0.6157(15) 0.547(3) 0.8818(13) 0.012(3) 1.0000 Uiso D U . . . . N1 N 0.5312(16) 0.571(2) 0.6853(12) 0.013(3) 1.0000 Uiso D U . . . . N2 N 0.5290(16) 0.755(2) 0.8635(12) 0.012(3) 1.0000 Uiso D U . . . . H11 H 0.3552 1.0683 0.7404 0.0153 1.0000 Uiso R . . . . . H12 H 0.4422 1.0136 0.6183 0.0153 1.0000 Uiso R . . . . . H13 H 0.2639 0.8938 0.6485 0.0153 1.0000 Uiso R . . . . . H31 H 0.6689 0.2878 0.7602 0.0150 1.0000 Uiso R . . . . . H41 H 0.6663 0.4917 0.9584 0.0150 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1742(9) loop_ _oxford_twin_element_scale_factors 0.67(2) 0.33(2) 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 . N1 2_666 2.061(13) yes Ag1 . N1 . 2.061(13) yes Ag2 . N2 2_677 2.080(13) yes Ag2 . N2 . 2.080(13) yes C1 . C2 . 1.481(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.344(9) yes C2 . N2 . 1.337(9) yes C3 . C4 . 1.355(9) yes C3 . N1 . 1.369(9) yes C3 . H31 . 0.950 no C4 . N2 . 1.378(9) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.5 no C2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.8(7) yes C1 . C2 . N2 . 124.3(7) yes N1 . C2 . N2 . 111.9(6) yes C4 . C3 . N1 . 107.7(6) yes C4 . C3 . H31 . 126.2 no N1 . C3 . H31 . 126.2 no C3 . C4 . N2 . 109.1(6) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.5 no C3 . N1 . C2 . 106.2(6) yes C3 . N1 . Ag1 . 126.1(9) yes C2 . N1 . Ag1 . 127.6(9) yes C4 . N2 . C2 . 105.1(6) yes C4 . N2 . Ag2 . 124.4(9) yes C2 . N2 . Ag2 . 130.4(9) yes _iucr_refine_instruction_details_constraints ; # # Punched on 19/05/11 at 11:17:59 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 19/05/11 at 11:17:59 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -2 1 5 x . #============================================================================== data_2.2GPa _database_code_depnum_ccdc_archive 'CCDC 881747' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-05-19 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'st1026 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag1 N2 # Dc = 2.64 Fooo = 360.00 Mu = 43.40 M = 176.95 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.82 FOOO = 360.00 Mu = 43.50 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure '2 200 000 ' _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.32 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.33 342_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 23 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 63 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 10 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6 These are all caused by shading of the pressure cell. 084_ALERT_2_C High R2 Value .................................. 0.26 The sample is weakly diffracting, causing the high value of R2. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). 731_ALERT_1_C Bond Calc 1.48(3), Rep 1.482(9) ...... 3.33 su-Ra C1 -C2 1.555 1.55 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 7.2027(16) _cell_length_b 5.6926(3) _cell_length_c 10.9057(4) _cell_angle_alpha 90 _cell_angle_beta 94.504(8) _cell_angle_gamma 90 _cell_volume 445.78(10) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 699 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.815 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.350 # Sheldrick geometric approximatio 0.42 0.65 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.65 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 1631 _reflns_number_total 295 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 295 # Theoretical number of reflections is about 1821 _diffrn_reflns_theta_min 3.748 _diffrn_reflns_theta_max 26.362 _diffrn_measured_fraction_theta_max 0.323 _diffrn_reflns_theta_full 25.044 _diffrn_measured_fraction_theta_full 0.329 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -2 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.30 _refine_diff_density_max 1.32 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 295 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.1055 _refine_ls_wR_factor_ref 0.2574 _refine_ls_goodness_of_fit_ref 1.0632 _refine_ls_shift/su_max 0.0012710 _refine_ls_shift/su_mean 0.0002000 # The values computed from all data _oxford_reflns_number_all 295 _refine_ls_R_factor_all 0.1055 _refine_ls_wR_factor_all 0.2574 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 198 _refine_ls_R_factor_gt 0.0891 _refine_ls_wR_factor_gt 0.2447 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.10P)^2^ +32.31P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0193(11) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0215(11) 1.0000 Uiso S . . . . . C1 C 0.372(5) 0.946(3) 0.6820(15) 0.015(3) 1.0000 Uiso D U . . . . C2 C 0.4779(15) 0.751(2) 0.7443(9) 0.015(2) 1.0000 Uiso D U . . . . C3 C 0.6264(15) 0.423(2) 0.7740(12) 0.015(2) 1.0000 Uiso D U . . . . C4 C 0.6224(15) 0.535(2) 0.8833(11) 0.015(2) 1.0000 Uiso D U . . . . N1 N 0.5344(16) 0.560(2) 0.6857(10) 0.015(2) 1.0000 Uiso D U . . . . N2 N 0.5282(16) 0.744(2) 0.8652(10) 0.015(2) 1.0000 Uiso D U . . . . H11 H 0.3488 1.0652 0.7400 0.0156 1.0000 Uiso R . . . . . H12 H 0.4472 1.0081 0.6220 0.0156 1.0000 Uiso R . . . . . H13 H 0.2569 0.8932 0.6430 0.0156 1.0000 Uiso R . . . . . H31 H 0.6786 0.2723 0.7614 0.0150 1.0000 Uiso R . . . . . H41 H 0.6756 0.4777 0.9601 0.0149 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1766(10) loop_ _oxford_twin_element_scale_factors 0.73(2) 0.27(2) 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 . N1 2_666 2.049(10) yes Ag1 . N1 . 2.049(10) yes Ag2 . N2 2_677 2.091(11) yes Ag2 . N2 . 2.091(11) yes C1 . C2 . 1.482(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.343(9) yes C2 . N2 . 1.340(9) yes C3 . C4 . 1.354(9) yes C3 . N1 . 1.369(9) yes C3 . H31 . 0.950 no C4 . N2 . 1.378(9) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.995 yes C2 . C1 . H11 . 109.9 no C2 . C1 . H12 . 106.9 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 111.6 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.6(7) yes C1 . C2 . N2 . 124.3(7) yes N1 . C2 . N2 . 112.1(6) yes C4 . C3 . N1 . 108.0(6) yes C4 . C3 . H31 . 126.0 no N1 . C3 . H31 . 126.0 no C3 . C4 . N2 . 109.0(6) yes C3 . C4 . H41 . 125.4 no N2 . C4 . H41 . 125.6 no C3 . N1 . C2 . 106.0(6) yes C3 . N1 . Ag1 . 128.0(8) yes C2 . N1 . Ag1 . 126.0(8) yes C4 . N2 . C2 . 105.0(6) yes C4 . N2 . Ag2 . 125.1(8) yes C2 . N2 . Ag2 . 129.6(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 19/05/11 at 11:21:04 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 19/05/11 at 11:21:04 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; #============================================================================== data_3.3GPa _database_code_depnum_ccdc_archive 'CCDC 881748' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-05-19 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'st1027 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag2 N2 # Dc = 4.41 Fooo = 360.00 Mu = 89.56 M = 284.82 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.93 FOOO = 360.00 Mu = 45.25 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure '3 300 000 ' _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.31 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 72 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 19 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 16 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6 These are all caused by shading of the pressure cell. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). 060_ALERT_4_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.25 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. Here, residual absorption errors from the pressure cell are an obvious source of further systematic error. 380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 The methyl group was placed geometrically and could not be refined. 731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2.22 su-Ra C1 -C2 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 7.0544(17) _cell_length_b 5.6024(3) _cell_length_c 10.8873(4) _cell_angle_alpha 90 _cell_angle_beta 95.062(9) _cell_angle_gamma 90 _cell_volume 428.61(11) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 569 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.928 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.525 # Sheldrick geometric approximatio 0.40 0.64 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.64 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 283 _reflns_number_total 283 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 283 # Theoretical number of reflections is about 1835 _diffrn_reflns_theta_min 3.758 _diffrn_reflns_theta_max 26.809 _diffrn_measured_fraction_theta_max 0.308 _diffrn_reflns_theta_full 25.201 _diffrn_measured_fraction_theta_full 0.318 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -2 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.58 _refine_diff_density_max 1.34 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 283 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.0996 _refine_ls_wR_factor_ref 0.1910 _refine_ls_goodness_of_fit_ref 1.0400 _refine_ls_shift/su_max 0.0017690 _refine_ls_shift/su_mean 0.0002787 # The values computed from all data _oxford_reflns_number_all 283 _refine_ls_R_factor_all 0.0996 _refine_ls_wR_factor_all 0.1910 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 174 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_gt 0.1758 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +28.97P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0162(8) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0178(8) 1.0000 Uiso S . . . . . C1 C 0.380(5) 0.948(3) 0.6799(14) 0.011(2) 1.0000 Uiso D U . . . . C2 C 0.4868(14) 0.750(2) 0.7439(9) 0.011(2) 1.0000 Uiso D U . . . . C3 C 0.6249(15) 0.408(2) 0.7771(12) 0.011(2) 1.0000 Uiso D U . . . . C4 C 0.6265(15) 0.527(2) 0.8852(10) 0.011(2) 1.0000 Uiso D U . . . . N1 N 0.5364(15) 0.550(2) 0.6870(9) 0.011(2) 1.0000 Uiso D U . . . . N2 N 0.5387(15) 0.745(2) 0.8649(9) 0.011(2) 1.0000 Uiso D U . . . . H11 H 0.3606 1.0714 0.7374 0.0146 1.0000 Uiso R . . . . . H12 H 0.4501 1.0085 0.6163 0.0146 1.0000 Uiso R . . . . . H13 H 0.2598 0.8911 0.6452 0.0146 1.0000 Uiso R . . . . . H31 H 0.6757 0.2531 0.7656 0.0137 1.0000 Uiso R . . . . . H41 H 0.6799 0.4692 0.9627 0.0136 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1789(7) loop_ _oxford_twin_element_scale_factors 0.788(19) 0.212(19) 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 . N1 2_666 2.048(10) yes Ag1 . N1 . 2.048(10) yes Ag2 . N2 2_677 2.086(10) yes Ag2 . N2 . 2.086(10) yes C1 . C2 . 1.480(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.345(8) yes C2 . N2 . 1.336(8) yes C3 . C4 . 1.352(9) yes C3 . N1 . 1.370(9) yes C3 . H31 . 0.950 no C4 . N2 . 1.379(9) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.4 no C2 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.6 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.5(6) yes C1 . C2 . N2 . 124.3(6) yes N1 . C2 . N2 . 112.1(6) yes C4 . C3 . N1 . 107.8(6) yes C4 . C3 . H31 . 126.2 no N1 . C3 . H31 . 126.0 no C3 . C4 . N2 . 109.2(6) yes C3 . C4 . H41 . 125.3 no N2 . C4 . H41 . 125.5 no C3 . N1 . C2 . 106.0(6) yes C3 . N1 . Ag1 . 130.0(8) yes C2 . N1 . Ag1 . 123.8(7) yes C4 . N2 . C2 . 104.9(6) yes C4 . N2 . Ag2 . 125.4(7) yes C2 . N2 . Ag2 . 129.7(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 19/05/11 at 11:23:04 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 19/05/11 at 11:23:04 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; #============================================================================== data_3.8GPa _database_code_depnum_ccdc_archive 'CCDC 881749' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-05-19 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'st1028 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag2 N2 # Dc = 4.49 Fooo = 360.00 Mu = 91.21 M = 284.82 # Found Formula = C4 H5 Ag1 N2 # Dc = 2.98 FOOO = 360.00 Mu = 46.08 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure '3 800 000 ' _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.31 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 71 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 18 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 3 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 16 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6 These are all caused by shading of the pressure cell. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 413_ALERT_2_B Short Inter XH3 .. XHn H13 .. H41 .. 2.08 Ang. Short contacts are expected at high pressure. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). 060_ALERT_4_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.14 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. Here, residual absorption errors from the pressure cell are an obvious source of further systematic error. 380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 The methyl group was placed geometrically and could not be refined. 731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2.22 su-Ra C1 -C2 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 3 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 6.9920(13) _cell_length_b 5.5590(2) _cell_length_c 10.8750(4) _cell_angle_alpha 90 _cell_angle_beta 95.344(7) _cell_angle_gamma 90 _cell_volume 420.86(8) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 704 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.982 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.608 # Sheldrick geometric approximatio 0.40 0.63 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.63 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 281 _reflns_number_total 281 _diffrn_reflns_av_R_equivalents 0.019 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 281 # Theoretical number of reflections is about 1817 _diffrn_reflns_theta_min 3.764 _diffrn_reflns_theta_max 26.889 _diffrn_measured_fraction_theta_max 0.309 _diffrn_reflns_theta_full 25.007 _diffrn_measured_fraction_theta_full 0.321 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -2 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 1.04 _oxford_diffrn_Wilson_scale 84.51 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.62 _refine_diff_density_max 1.23 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 280 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.0954 _refine_ls_wR_factor_ref 0.2066 _refine_ls_goodness_of_fit_ref 0.9796 _refine_ls_shift/su_max 0.0016779 _refine_ls_shift/su_mean 0.0002653 # The values computed from all data _oxford_reflns_number_all 280 _refine_ls_R_factor_all 0.0954 _refine_ls_wR_factor_all 0.2066 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 188 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_gt 0.1932 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +36.79P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0153(9) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0166(9) 1.0000 Uiso S . . . . . C1 C 0.381(6) 0.951(3) 0.6789(15) 0.013(2) 1.0000 Uiso D U . . . . C2 C 0.4794(14) 0.7454(18) 0.7443(9) 0.012(2) 1.0000 Uiso D U . . . . C3 C 0.6219(15) 0.4024(19) 0.7776(11) 0.012(2) 1.0000 Uiso D U . . . . C4 C 0.6276(15) 0.524(2) 0.8854(10) 0.012(2) 1.0000 Uiso D U . . . . N1 N 0.5283(15) 0.543(2) 0.6875(9) 0.012(2) 1.0000 Uiso D U . . . . N2 N 0.5371(15) 0.7431(19) 0.8650(9) 0.012(2) 1.0000 Uiso D U . . . . H11 H 0.3601 1.0743 0.7365 0.0147 1.0000 Uiso R . . . . . H12 H 0.4580 1.0105 0.6185 0.0147 1.0000 Uiso R . . . . . H13 H 0.2605 0.8987 0.6398 0.0147 1.0000 Uiso R . . . . . H31 H 0.6733 0.2466 0.7663 0.0139 1.0000 Uiso R . . . . . H41 H 0.6846 0.4684 0.9629 0.0140 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1734(8) loop_ _oxford_twin_element_scale_factors 0.80(2) 0.20(2) 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 . N1 2_666 2.044(10) yes Ag1 . N1 . 2.044(10) yes Ag2 . N2 2_677 2.081(10) yes Ag2 . N2 . 2.081(10) yes C1 . C2 . 1.480(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.344(8) yes C2 . N2 . 1.337(8) yes C3 . C4 . 1.352(9) yes C3 . N1 . 1.371(9) yes C3 . H31 . 0.950 no C4 . N2 . 1.379(9) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.5 no C2 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.5(6) yes C1 . C2 . N2 . 124.3(6) yes N1 . C2 . N2 . 112.2(6) yes C4 . C3 . N1 . 107.9(6) yes C4 . C3 . H31 . 126.0 no N1 . C3 . H31 . 126.1 no C3 . C4 . N2 . 109.1(6) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.4 no C3 . N1 . C2 . 105.9(6) yes C3 . N1 . Ag1 . 129.9(8) yes C2 . N1 . Ag1 . 123.5(7) yes C4 . N2 . C2 . 105.0(6) yes C4 . N2 . Ag2 . 125.2(7) yes C2 . N2 . Ag2 . 129.8(7) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C1 . H11 . C2 3_556 121.1(6) 0.950 2.583 3.18(2) yes C3 . H31 . C3 3_646 165.2(4) 0.950 2.463 3.39(2) yes C3 . H31 . C4 3_646 139.0(4) 0.950 2.572 3.35(2) yes C3 . H31 . N1 3_646 137.7(4) 0.950 2.386 3.15(2) yes _iucr_refine_instruction_details_constraints ; # # Punched on 19/05/11 at 11:24:28 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 19/05/11 at 11:24:28 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 2 4 4 x . #============================================================================== data_4.9GPa _database_code_depnum_ccdc_archive 'CCDC 881750' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-08-08 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'st1031 in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.335 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 73 088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.89 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 18 950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 6 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1 These are all caused by shading of the pressure cell. 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 413_ALERT_2_C Short Inter XH3 .. XHn H13 .. H41 .. 2.11 Ang. Short contacts are expected at high pressure. 731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2 su-Ra C1 -C2 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1 These are correct. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked ! No action taken. 808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found ! A shelx weighting scheme was not used. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 6.9259(16) _cell_length_b 5.5072(2) _cell_length_c 10.8549(4) _cell_angle_alpha 90 _cell_angle_beta 95.667(8) _cell_angle_gamma 90 _cell_volume 412.01(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C3 H5 Ag2 N2 # Dc = 4.59 Fooo = 360.00 Mu = 93.17 M = 284.82 # Found Formula = C4 H5 Ag1 N2 # Dc = 3.05 FOOO = 360.00 Mu = 47.07 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_formula_moiety 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_formula_weight 188.97 _cell_measurement_reflns_used 545 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 3.046 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.707 # Sheldrick geometric approximatio 0.39 0.62 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.62 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 277 _reflns_number_total 277 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 277 # Theoretical number of reflections is about 1825 _diffrn_reflns_theta_min 3.773 _diffrn_reflns_theta_max 27.141 _diffrn_measured_fraction_theta_max 0.304 _diffrn_reflns_theta_full 25.241 _diffrn_measured_fraction_theta_full 0.335 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -2 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.47 _refine_diff_density_max 1.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 277 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.1020 _refine_ls_wR_factor_ref 0.2048 _refine_ls_goodness_of_fit_ref 1.0542 _refine_ls_shift/su_max 0.0054769 _refine_ls_shift/su_mean 0.0007388 # The values computed from all data _oxford_reflns_number_all 277 _refine_ls_R_factor_all 0.1020 _refine_ls_wR_factor_all 0.2048 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 175 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_gt 0.1891 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +21.17P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0161(8) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0169(9) 1.0000 Uiso S . . . . . C1 C 0.374(5) 0.946(3) 0.6786(13) 0.014(2) 1.0000 Uiso D U . . . . C2 C 0.4812(14) 0.7442(18) 0.7443(8) 0.013(2) 1.0000 Uiso D U . . . . C3 C 0.6238(15) 0.3972(19) 0.7792(11) 0.012(2) 1.0000 Uiso D U . . . . C4 C 0.6296(15) 0.522(2) 0.8867(10) 0.013(2) 1.0000 Uiso D U . . . . N1 N 0.5296(15) 0.5388(19) 0.6886(9) 0.013(2) 1.0000 Uiso D U . . . . N2 N 0.5392(15) 0.7430(19) 0.8652(9) 0.013(2) 1.0000 Uiso D U . . . . H11 H 0.3561 1.0734 0.7355 0.0184 1.0000 Uiso R . . . . . H12 H 0.4453 1.0058 0.6145 0.0184 1.0000 Uiso R . . . . . H13 H 0.2515 0.8885 0.6439 0.0184 1.0000 Uiso R . . . . . H31 H 0.6752 0.2395 0.7686 0.0172 1.0000 Uiso R . . . . . H41 H 0.6858 0.4654 0.9649 0.0177 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1716(8) loop_ _oxford_twin_element_scale_factors 0.87(2) 0.13(2) 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 . N1 2_666 2.049(9) yes Ag1 . N1 . 2.049(9) yes Ag2 . N2 2_677 2.073(10) yes Ag2 . N2 . 2.073(10) yes C1 . C2 . 1.480(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.341(8) yes C2 . N2 . 1.334(8) yes C3 . C4 . 1.351(8) yes C3 . N1 . 1.369(9) yes C3 . H31 . 0.950 no C4 . N2 . 1.379(9) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.4 no C2 . C1 . H12 . 110.0 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.0 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.5(6) yes C1 . C2 . N2 . 124.5(6) yes N1 . C2 . N2 . 112.0(6) yes C4 . C3 . N1 . 107.7(6) yes C4 . C3 . H31 . 126.1 no N1 . C3 . H31 . 126.3 no C3 . C4 . N2 . 109.1(6) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.4 no C3 . N1 . C2 . 106.2(6) yes C3 . N1 . Ag1 . 130.7(7) yes C2 . N1 . Ag1 . 122.3(6) yes C4 . N2 . C2 . 105.0(6) yes C4 . N2 . Ag2 . 124.9(7) yes C2 . N2 . Ag2 . 130.0(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 08/08/11 at 15:28:52 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/08/11 at 15:28:52 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; #============================================================================== data_5.6GPa _database_code_depnum_ccdc_archive 'CCDC 881751' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 11-08-08 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'st1033 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag2 N2 # Dc = 4.67 Fooo = 360.00 Mu = 94.78 M = 284.82 # Found Formula = C4 H5 Ag1 N2 # Dc = 3.10 FOOO = 360.00 Mu = 47.88 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure ' 5 600 000 ' _publ_section_exptl_refinement ; 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.337 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 186 088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.64 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 16 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 43 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3 950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 5 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 2 These are all caused by shading and absorption from the pressure cell. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 413_ALERT_2_B Short Inter XH3 .. XHn H13 .. H41 .. 2.05 Ang. Short contacts are expected at high pressure. 731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2 su-Ra C1 -C2 1.555 1.555 # 5 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1 This has been alerted because the Ag-atoms have been pushed closer together at high pressure (see text). 128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K This is correct. 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 The methyl group was placed geometrically and could not be refined. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found ! A shelx weighting scheme was not used. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 6.8710(13) _cell_length_b 5.4670(2) _cell_length_c 10.8393(3) _cell_angle_alpha 90 _cell_angle_beta 95.878(7) _cell_angle_gamma 90 _cell_volume 405.02(8) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 648 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 3.099 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.788 # Sheldrick geometric approximatio 0.38 0.62 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.62 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 1488 _reflns_number_total 270 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 270 # Theoretical number of reflections is about 1795 _diffrn_reflns_theta_min 3.779 _diffrn_reflns_theta_max 27.142 _diffrn_measured_fraction_theta_max 0.302 _diffrn_reflns_theta_full 25.243 _diffrn_measured_fraction_theta_full 0.337 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -3 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.23 _refine_diff_density_max 1.29 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 270 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.0753 _refine_ls_wR_factor_ref 0.1595 _refine_ls_goodness_of_fit_ref 1.0147 _refine_ls_shift/su_max 0.0018230 _refine_ls_shift/su_mean 0.0002636 # The values computed from all data _oxford_reflns_number_all 270 _refine_ls_R_factor_all 0.0753 _refine_ls_wR_factor_all 0.1595 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 192 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_gt 0.1492 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +23.28P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0138(7) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0143(7) 1.0000 Uiso S . . . . . C1 C 0.373(5) 0.946(3) 0.6777(12) 0.013(2) 1.0000 Uiso D U . . . . C2 C 0.4753(14) 0.7395(15) 0.7445(8) 0.0120(17) 1.0000 Uiso D U . . . . C3 C 0.6215(15) 0.3919(17) 0.7795(9) 0.0117(18) 1.0000 Uiso D U . . . . C4 C 0.6288(15) 0.5176(19) 0.8874(8) 0.0116(18) 1.0000 Uiso D U . . . . N1 N 0.5239(15) 0.5328(16) 0.6887(7) 0.0119(17) 1.0000 Uiso D U . . . . N2 N 0.5362(15) 0.7398(16) 0.8658(8) 0.0112(17) 1.0000 Uiso D U . . . . H11 H 0.3529 1.0732 0.7347 0.0151 1.0000 Uiso R . . . . . H12 H 0.4503 1.0055 0.6164 0.0151 1.0000 Uiso R . . . . . H13 H 0.2501 0.8920 0.6390 0.0151 1.0000 Uiso R . . . . . H31 H 0.6746 0.2339 0.7686 0.0141 1.0000 Uiso R . . . . . H41 H 0.6881 0.4619 0.9654 0.0140 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1879(7) loop_ _oxford_twin_element_scale_factors 0.892(18) 0.108(18) 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 . N1 2_666 2.043(8) yes Ag1 . N1 . 2.043(8) yes Ag2 . N2 2_677 2.068(8) yes Ag2 . N2 . 2.068(8) yes C1 . C2 . 1.480(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.340(8) yes C2 . N2 . 1.338(8) yes C3 . C4 . 1.353(8) yes C3 . N1 . 1.370(8) yes C3 . H31 . 0.950 no C4 . N2 . 1.380(8) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.5 no C2 . C1 . H12 . 109.4 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.6 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.4(6) yes C1 . C2 . N2 . 124.4(6) yes N1 . C2 . N2 . 112.2(5) yes C4 . C3 . N1 . 107.9(6) yes C4 . C3 . H31 . 126.0 no N1 . C3 . H31 . 126.0 no C3 . C4 . N2 . 109.0(6) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.5 no C3 . N1 . C2 . 106.1(5) yes C3 . N1 . Ag1 . 130.8(6) yes C2 . N1 . Ag1 . 121.8(6) yes C4 . N2 . C2 . 104.9(5) yes C4 . N2 . Ag2 . 124.9(6) yes C2 . N2 . Ag2 . 130.1(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 08/08/11 at 15:41:10 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/08/11 at 15:41:10 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; #============================================================================== data_6.4GPa _database_code_depnum_ccdc_archive 'CCDC 881752' #TrackingRef '- CrystallographicData.cif' #============================================================================== _audit_creation_date 12-01-19 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 'st1034 in P2(1)/n' _chemical_name_systematic ? _chemical_formula_moiety 'C4 H5 Ag1 N2' # Given Formula = C3 H5 Ag2 N2 # Dc = 4.74 Fooo = 360.00 Mu = 96.23 M = 284.82 # Found Formula = C4 H5 Ag1 N2 # Dc = 3.15 FOOO = 360.00 Mu = 48.61 M = 188.97 _chemical_formula_sum 'C4 H5 Ag1 N2' _chemical_compound_source ? _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 293 _diffrn_ambient_pressure ' 6 400 000 ' _publ_section_exptl_refinement ; 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 186 088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.50 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 16 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 36 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 2 950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 5 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1 These are all caused by shading and absorption from the pressure cell. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8 210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ? This refinement strategy was based on the low completeness of the data, which meant that non-H atoms could only be refined with isotropic thermal parameters. 413_ALERT_2_C Short Inter XH3 .. XHn H13 .. H41 .. 2.12 Ang. Short contacts are expected at high pressure. 731_ALERT_1_C Bond Calc 1.48(2), Rep 1.479(9) ...... 2 su-Ra C1 -C2 1.555 1.555 # 5 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif is badly in error. 004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1 This has been alerted because the Ag-atoms have been pushed closer together at high pressure (see text). 128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n This has been chosen to have a beta angle closer to 90 degrees, and therefore reduce correlation between positional parameters. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K This is correct. 380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 The methyl group was placed geometrically and could not be refined. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. 808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found ! A shelx weighting scheme was not used. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31 All 1,2 and 1,3 distances were restrained to ambient pressure values (see text). ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 6.828(2) _cell_length_b 5.4298(3) _cell_length_c 10.8209(5) _cell_angle_alpha 90 _cell_angle_beta 96.076(11) _cell_angle_gamma 90 _cell_volume 398.92(12) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_weight 188.97 _cell_measurement_reflns_used 569 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_measurement_temperature 293 _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 3.146 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.861 # Sheldrick geometric approximatio 0.38 0.61 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 0.61 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 1463 _reflns_number_total 266 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 266 # Theoretical number of reflections is about 1702 _diffrn_reflns_theta_min 3.787 _diffrn_reflns_theta_max 26.773 _diffrn_measured_fraction_theta_max 0.312 _diffrn_reflns_theta_full 25.167 _diffrn_measured_fraction_theta_full 0.324 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -3 _reflns_limit_h_max 2 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.47 _refine_diff_density_max 1.69 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 266 _refine_ls_number_restraints 31 _refine_ls_number_parameters 28 _oxford_refine_ls_R_factor_ref 0.0820 _refine_ls_wR_factor_ref 0.1545 _refine_ls_goodness_of_fit_ref 1.0033 _refine_ls_shift/su_max 0.0040945 _refine_ls_shift/su_mean 0.0006928 # The values computed with all filters except I/sigma _oxford_reflns_number_all 266 _refine_ls_R_factor_all 0.0820 _refine_ls_wR_factor_all 0.1545 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 177 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_gt 0.1410 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +30.29P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.5000 0.5000 0.5000 0.0114(7) 1.0000 Uiso S . . . . . Ag2 Ag 0.5000 1.0000 1.0000 0.0125(7) 1.0000 Uiso S . . . . . C1 C 0.371(5) 0.941(3) 0.6776(12) 0.010(2) 1.0000 Uiso D U . . . . C2 C 0.4826(14) 0.7390(16) 0.7441(8) 0.0100(17) 1.0000 Uiso D U . . . . C3 C 0.6200(15) 0.3835(17) 0.7802(9) 0.0099(18) 1.0000 Uiso D U . . . . C4 C 0.6282(15) 0.510(2) 0.8882(8) 0.0099(18) 1.0000 Uiso D U . . . . N1 N 0.5275(15) 0.5290(17) 0.6887(8) 0.0102(18) 1.0000 Uiso D U . . . . N2 N 0.5412(15) 0.7377(17) 0.8661(8) 0.0097(18) 1.0000 Uiso D U . . . . H11 H 0.3556 1.0726 0.7338 0.0118 1.0000 Uiso R . . . . . H12 H 0.4416 0.9987 0.6120 0.0118 1.0000 Uiso R . . . . . H13 H 0.2456 0.8831 0.6444 0.0118 1.0000 Uiso R . . . . . H31 H 0.6697 0.2222 0.7697 0.0119 1.0000 Uiso R . . . . . H41 H 0.6847 0.4518 0.9668 0.0119 1.0000 Uiso R . . . . . _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1676(6) loop_ _oxford_twin_element_scale_factors 1.07(2) 0.08(2) 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 . N1 2_666 2.037(8) yes Ag1 . N1 . 2.037(8) yes Ag2 . N2 2_677 2.072(8) yes Ag2 . N2 . 2.072(8) yes C1 . C2 . 1.479(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . N1 . 1.339(8) yes C2 . N2 . 1.338(8) yes C3 . C4 . 1.352(8) yes C3 . N1 . 1.368(8) yes C3 . H31 . 0.950 no C4 . N2 . 1.381(8) yes C4 . H41 . 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 2_666 Ag1 . N1 . 179.994 yes N2 2_677 Ag2 . N2 . 179.994 yes C2 . C1 . H11 . 109.5 no C2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . N1 . 123.1(6) yes C1 . C2 . N2 . 124.6(6) yes N1 . C2 . N2 . 112.2(5) yes C4 . C3 . N1 . 107.8(6) yes C4 . C3 . H31 . 126.1 no N1 . C3 . H31 . 126.1 no C3 . C4 . N2 . 109.1(6) yes C3 . C4 . H41 . 125.5 no N2 . C4 . H41 . 125.5 no C3 . N1 . C2 . 106.1(6) yes C3 . N1 . Ag1 . 131.9(6) yes C2 . N1 . Ag1 . 120.9(6) yes C4 . N2 . C2 . 104.7(6) yes C4 . N2 . Ag2 . 125.5(6) yes C2 . N2 . Ag2 . 129.6(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 19/01/12 at 16:21:14 # #LIST 12 BLOCK SCALE X'S, U[ISO] SUMFIX ELEMENT SCALES RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 19/01/12 at 16:21:14 # #LIST 16 DIST 1.482,.01= C(1) TO C(2) DIST 1.345,.01= C(2) TO N(1) DIST 1.338,.01= C(2) TO N(2) DIST 1.351,.01= C(3) TO C(4) DIST 1.371,.01= C(3) TO N(1) DIST 1.377,.01= C(4) TO N(2) ANGL 124,1= N(1) TO C(2) TO C(1) ANGL 124,1= N(2) TO C(2) TO C(1) ANGL 112,1= N(2) TO C(2) TO N(1) ANGL 108,1= N(1) TO C(3) TO C(4) ANGL 109,1= N(2) TO C(4) TO C(3) ANGL 106,1= C(3) TO N(1) TO C(2) ANGL 105,1= C(4) TO N(2) TO C(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(2) VIBR .0, 0.00200 = C(2) TO N(1) VIBR .0, 0.00200 = C(2) TO N(2) VIBR .0, 0.00500 = N(1) TO C(1) VIBR .0, 0.00500 = N(2) TO C(1) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(3) TO N(1) VIBR .0, 0.00500 = N(1) TO C(4) VIBR .0, 0.00200 = C(4) TO N(2) VIBR .0, 0.00500 = N(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(2) TO C(4) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(2) U(IJ) .0, 0.04000 = C(2) TO N(1) U(IJ) .0, 0.04000 = C(2) TO N(2) U(IJ) .0, 0.04000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(3) TO N(1) U(IJ) .0, 0.04000 = C(4) TO N(2) REM THERMSIM END (DO NOT REMOVE THIS LINE) PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2) END ; #============================================================================== # start Validation Reply Form #============================================================================== _vrf_PLAT022_1.1GPa ; PROBLEM: Ratio Unique / Expected Reflections (too) Low .. 0.358 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT027_1.1GPa ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 17.38 Deg. RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_1.1GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.378 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_2.2GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.329 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_3.3GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.318 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_3.8GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.321 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_4.9GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.335 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_5.6GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.337 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; _vrf_PLAT029_6.4GPa ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.324 RESPONSE: This is caused by shading of the pressure cell. For more information please see the experimental special details. ; #============================================================================== # end Validation Reply Form #==============================================================================