# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; ; _refine_special_details ; ? ; #end of refcif _cell_length_a 7.9645(10) _cell_length_b 10.138(6) _cell_length_c 6.1945(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 500.2(3) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.63 Fooo = 368.00 Mu = 38.91 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.63 FOOO = 368.00 Mu = 38.91 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source ? _chemical_formula_weight 197.93 _cell_measurement_reflns_used 290 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.09 _exptl_crystal_density_diffrn 2.628 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.891 # Sheldrick geometric approximatio 0.02 0.68 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Gaussian Integration (Busing and Levy, 1957) ; _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.68 _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _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 'Gemini, (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 83000 _diffrn_reflns_number 642 _reflns_number_total 250 _diffrn_reflns_av_R_equivalents 0.058 # Number of reflections without Friedels Law is 250 # Number of reflections with Friedels Law is 143 # Theoretical number of reflections is about 212 _diffrn_reflns_theta_min 3.253 _diffrn_reflns_theta_max 24.679 _diffrn_measured_fraction_theta_max 0.559 _diffrn_reflns_theta_full 19.250 _diffrn_measured_fraction_theta_full 0.596 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min -7 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 4.14 _oxford_diffrn_Wilson_scale 0.23 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.71 _refine_diff_density_max 0.82 # 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 246 _refine_ls_number_restraints 15 _refine_ls_number_parameters 24 _oxford_refine_ls_R_factor_ref 0.0537 _refine_ls_wR_factor_ref 0.1042 _refine_ls_goodness_of_fit_ref 0.9518 _refine_ls_shift/su_max 0.0000579 _refine_ls_shift/su_mean 0.0000135 # The values computed with all filters except I/sigma _oxford_reflns_number_all 246 _refine_ls_R_factor_all 0.0537 _refine_ls_wR_factor_all 0.1042 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 215 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_gt 0.0931 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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: 0.370E+04 -0.320E+04 0.472E+04 -0.140E+04 0.125E+04 ; # 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 0.2500 0.6515(3) 0.5594(7) 0.0632 1.0000 Uani S T . . . . N1 N 0.2500 0.514(4) 0.823(2) 0.050(3) 1.0000 Uiso DS U . . . . C1 C 0.2500 0.459(4) 0.981(3) 0.048(3) 1.0000 Uiso DS U . . . . N2 N 0.4678(15) 0.6830(17) 0.3405(19) 0.050(2) 1.0000 Uiso D U . . . . C2 C 0.5981(18) 0.652(3) 0.267(2) 0.048(2) 1.0000 Uiso D U . . . . C3 C 0.7500 0.615(3) 0.175(4) 0.048(2) 1.0000 Uiso DS U . . . . 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 0.0539(9) 0.085(3) 0.0511(10) 0.013(2) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.21(7) 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 . N2 3_555 2.225(12) yes Ag1 . N1 . 2.15(3) yes Ag1 . N2 . 2.225(12) yes N1 . C1 . 1.13(3) yes C1 . C3 5_466 1.413(18) yes N2 . C2 . 1.176(19) yes C2 . C3 . 1.391(18) yes 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 N2 3_555 Ag1 . N1 . 123.8(5) yes N2 3_555 Ag1 . N2 . 102.5(7) yes N1 . Ag1 . N2 . 123.8(5) yes Ag1 . N1 . C1 . 169(3) yes C3 5_466 C1 . N1 . 177(4) yes Ag1 . N2 . C2 . 152.3(18) yes N2 . C2 . C3 . 178.3(17) yes C1 5_564 C3 . C2 . 119.6(11) yes C1 5_564 C3 . C2 3_655 119.6(11) yes C2 . C3 . C2 3_655 121(2) yes _iucr_refine_instruction_details_constraints ; # # Punched on 11/09/13 at 13:42:31 # #LIST 12 BLOCK SCALE X'S CONT AG(1,U'S) CONT N(1,U[ISO]) UNTIL LAST END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/09/13 at 13:42:31 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.150000 , 0.050000 = N(1) TO C(1) DISTANCE 1.150000 , 0.050000 = N(2) TO C(2) DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) DISTANCE 1.400000 , 0.020000 = C(1) TO C(3,4,1,1,1,1) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00500 = N(1) TO N(2,2) VIBR .0, 0.00500 = N(2) TO N(2,2) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00200 = C(1) TO C(3,3,1,-1,1,1) VIBR .0, 0.00500 = N(1) TO C(3,3,1,-1,1,1) VIBR .0, 0.00200 = N(2) TO C(2) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO N(2) VIBR .0, 0.00500 = C(2) TO C(1,3,1,0,1,-1) VIBR .0, 0.00500 = C(2,2,1,1) TO C(1,3,1,0,1,-1) VIBR .0, 0.00500 = C(2,2,1,1) TO C(2) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = N(1) TO C(1) U(IJ) .0, 0.04000 = C(1) TO C(3,3,1,-1,1,1) U(IJ) .0, 0.04000 = N(2) TO C(2) U(IJ) .0, 0.04000 = C(2) TO C(3) REM THERMSIM 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 2 0 -4 x . 0 0 -4 x . _database_code_depnum_ccdc_archive 'CCDC 961474' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0121(13) _cell_length_b 9.646(6) _cell_length_c 6.2169(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 480.5(3) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 Ag0.75 N2.25 # Dc = 2.05 Fooo = 368.00 Mu = 30.37 M = 74.22 # Found Formula = C4 Ag1 N3 # Dc = 2.74 FOOO = 368.00 Mu = 40.50 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source ? _chemical_formula_weight 197.93 _cell_measurement_reflns_used 507 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.09 _exptl_crystal_density_diffrn 2.736 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 4.050 # Sheldrick geometric approximatio 0.67 0.67 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Gaussian Integration (Busing and Levy, 1957) ; _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.67 _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _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 'Gemini, (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_ambient_pressure 830000 _diffrn_reflns_number 500 _reflns_number_total 221 _diffrn_reflns_av_R_equivalents 0.072 # Number of reflections without Friedels Law is 221 # Number of reflections with Friedels Law is 137 # Theoretical number of reflections is about 204 _diffrn_reflns_theta_min 3.305 _diffrn_reflns_theta_max 24.681 _diffrn_measured_fraction_theta_max 0.557 _diffrn_reflns_theta_full 20.238 _diffrn_measured_fraction_theta_full 0.587 _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 -6 _diffrn_reflns_limit_l_max 6 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min -6 _reflns_limit_l_max 6 _oxford_diffrn_Wilson_B_factor 3.01 _oxford_diffrn_Wilson_scale 0.26 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -1.29 _refine_diff_density_max 1.80 # 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 215 _refine_ls_number_restraints 14 _refine_ls_number_parameters 24 _oxford_refine_ls_R_factor_ref 0.0711 _refine_ls_wR_factor_ref 0.1092 _refine_ls_goodness_of_fit_ref 1.0434 _refine_ls_shift/su_max 0.0000882 _refine_ls_shift/su_mean 0.0000244 # The values computed with all filters except I/sigma _oxford_reflns_number_all 215 _refine_ls_R_factor_all 0.0711 _refine_ls_wR_factor_all 0.1092 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 186 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_gt 0.1050 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^) + ( 0.00P)^2^ +11.73P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.6517(4) 0.5559(10) 0.0557 1.0000 Uani S T . . . . N1 N 0.2500 0.506(5) 0.828(4) 0.050(4) 1.0000 Uiso DS U . . . . C1 C 0.2500 0.443(6) 0.987(4) 0.050(4) 1.0000 Uiso DS U . . . . N2 N 0.473(2) 0.684(2) 0.344(3) 0.050(4) 1.0000 Uiso D U . . . . C2 C 0.600(2) 0.656(3) 0.272(3) 0.050(4) 1.0000 Uiso D U . . . . C3 C 0.7500 0.629(7) 0.180(5) 0.050(4) 1.0000 Uiso DS U . . . . 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 0.0469(11) 0.073(4) 0.0473(17) 0.021(3) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 1.94(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 . N2 3_555 2.244(18) yes Ag1 . N1 . 2.20(4) yes Ag1 . N2 . 2.244(18) yes N1 . C1 . 1.16(4) yes C1 . C3 5_466 1.38(6) yes N2 . C2 . 1.14(2) yes C2 . C3 . 1.36(2) yes 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 N2 3_555 Ag1 . N1 . 122.8(6) yes N2 3_555 Ag1 . N2 . 105.7(9) yes N1 . Ag1 . N2 . 122.8(6) yes Ag1 . N1 . C1 . 172(4) yes C3 5_466 C1 . N1 . 179(6) yes Ag1 . N2 . C2 . 154(2) yes N2 . C2 . C3 . 176(4) yes C1 5_564 C3 . C2 . 117.4(19) yes C1 5_564 C3 . C2 3_655 117.4(19) yes C2 . C3 . C2 3_655 125(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 11/09/13 at 11:57:07 # #LIST 12 BLOCK SCALE X'S CONT AG(1,U'S) CONT N(1,U[ISO]) UNTIL LAST END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/09/13 at 11:57:07 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.150000 , 0.050000 = N(1) TO C(1) DISTANCE 1.150000 , 0.050000 = N(2) TO C(2) DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00500 = N(1) TO N(2,2) VIBR .0, 0.00500 = N(2) TO N(2,2) VIBR .0, 0.00500 = N(2) TO N(1) VIBR .0, 0.00200 = N(1) TO C(1) VIBR .0, 0.00200 = C(1) TO C(3,3,1,-1,1,1) VIBR .0, 0.00500 = N(1) TO C(3,3,1,-1,1,1) VIBR .0, 0.00200 = N(2) TO C(2) VIBR .0, 0.00200 = C(2) TO C(3) VIBR .0, 0.00500 = C(3) TO N(2) VIBR .0, 0.00500 = C(2) TO C(1,3,1,0,1,-1) VIBR .0, 0.00500 = C(2,2,1,1) TO C(1,3,1,0,1,-1) VIBR .0, 0.00500 = C(2,2,1,1) TO C(2) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = N(1) TO C(1) U(IJ) .0, 0.04000 = C(1) TO C(3,3,1,-1,1,1) U(IJ) .0, 0.04000 = N(2) TO C(2) U(IJ) .0, 0.04000 = C(2) TO C(3) REM THERMSIM 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 3 1 4 x . 7 4 -3 x . 6 6 -4 x . 5 7 4 x . 6 5 -3 x . 6 5 3 x . _database_code_depnum_ccdc_archive 'CCDC 961475' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0667(5) _cell_length_b 9.7791(6) _cell_length_c 6.2784(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 495.27(5) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.65 Fooo = 368.00 Mu = 39.29 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.65 FOOO = 368.00 Mu = 39.29 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 611 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.654 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.929 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 838 _reflns_number_total 530 _diffrn_reflns_av_R_equivalents 0.017 # Number of reflections without Friedels Law is 530 # Number of reflections with Friedels Law is 346 # Theoretical number of reflections is about 340 _diffrn_reflns_theta_min 3.274 _diffrn_reflns_theta_max 29.333 _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 26.941 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 1.42 _oxford_diffrn_Wilson_scale 0.23 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.82 _refine_diff_density_max 0.67 # 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 530 _refine_ls_number_restraints 1 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0241 _refine_ls_wR_factor_ref 0.0501 _refine_ls_goodness_of_fit_ref 0.9946 _refine_ls_shift/su_max 0.0001880 _refine_ls_shift/su_mean 0.0000450 # The values computed with all filters except I/sigma _oxford_reflns_number_all 530 _refine_ls_R_factor_all 0.0241 _refine_ls_wR_factor_all 0.0501 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 502 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_gt 0.0488 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^) + ( 0.03P)^2^ + 0.57P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64735(4) 0.5547(2) 0.0172 1.0000 Uani S T . . . . N1 N 0.2500 0.5144(7) 0.8319(10) 0.0249 1.0000 Uani S T . . . . C1 C 0.2500 0.4534(8) 0.9888(10) 0.0155 1.0000 Uani S T . . . . N2 N 0.4715(5) 0.6830(4) 0.3459(6) 0.0190 1.0000 Uani . . . . . . C2 C 0.5977(6) 0.6562(5) 0.2736(7) 0.0153 1.0000 Uani . . . . . . C3 C 0.7500 0.6208(7) 0.1795(10) 0.0138 1.0000 Uani S T . . . . 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 0.0152(2) 0.0204(2) 0.0159(2) 0.0028(4) 0.0000 0.0000 N1 0.017(3) 0.027(3) 0.031(3) 0.009(3) 0.0000 0.0000 C1 0.011(3) 0.009(3) 0.027(4) -0.003(3) 0.0000 0.0000 N2 0.021(2) 0.016(2) 0.020(2) -0.0059(17) 0.0021(19) -0.0023(17) C2 0.020(2) 0.009(2) 0.017(2) 0.0003(18) -0.001(2) -0.0043(18) C3 0.017(3) 0.009(4) 0.015(3) 0.000(3) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.15(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 . N2 3_555 2.243(4) yes Ag1 . N1 . 2.173(7) yes Ag1 . N2 . 2.243(4) yes N1 . C1 . 1.151(9) yes C1 . C3 5_466 1.400(10) yes N2 . C2 . 1.145(7) yes C2 . C3 . 1.407(6) yes 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 N2 3_555 Ag1 . N1 . 124.14(12) yes N2 3_555 Ag1 . N2 . 105.6(2) yes N1 . Ag1 . N2 . 124.14(12) yes Ag1 . N1 . C1 . 174.4(6) yes C3 5_466 C1 . N1 . 179.9(8) yes Ag1 . N2 . C2 . 154.7(4) yes N2 . C2 . C3 . 178.0(5) yes C2 3_655 C3 . C2 . 121.7(6) yes C2 3_655 C3 . C1 7_664 119.1(3) yes C2 . C3 . C1 7_664 119.1(3) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 13:46:55 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 13:46:55 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 961476' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0636(8) _cell_length_b 9.7766(9) _cell_length_c 6.2791(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 495.01(8) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.66 Fooo = 368.00 Mu = 39.31 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.66 FOOO = 368.00 Mu = 39.31 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 595 _cell_measurement_theta_min 4 _cell_measurement_theta_max 29 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.656 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.931 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 844 _reflns_number_total 539 _diffrn_reflns_av_R_equivalents 0.017 # Number of reflections without Friedels Law is 539 # Number of reflections with Friedels Law is 352 # Theoretical number of reflections is about 339 _diffrn_reflns_theta_min 3.857 _diffrn_reflns_theta_max 29.331 _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 26.939 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 1.43 _oxford_diffrn_Wilson_scale 0.23 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.90 _refine_diff_density_max 0.79 # 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 539 _refine_ls_number_restraints 1 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0273 _refine_ls_wR_factor_ref 0.0532 _refine_ls_goodness_of_fit_ref 1.0113 _refine_ls_shift/su_max 0.0003150 _refine_ls_shift/su_mean 0.0000139 # The values computed with all filters except I/sigma _oxford_reflns_number_all 539 _refine_ls_R_factor_all 0.0273 _refine_ls_wR_factor_all 0.0532 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 517 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_gt 0.0517 # 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 ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^ + 4.15P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64736(5) 0.5546(2) 0.0176 1.0000 Uani S T . . . . N1 N 0.2500 0.5139(8) 0.8313(11) 0.0257 1.0000 Uani S T . . . . C1 C 0.2500 0.4525(9) 0.9889(12) 0.0162 1.0000 Uani S T . . . . N2 N 0.4718(6) 0.6835(5) 0.3469(7) 0.0191 1.0000 Uani . . . . . . C2 C 0.5973(7) 0.6570(6) 0.2734(8) 0.0145 1.0000 Uani . . . . . . C3 C 0.7500 0.6219(9) 0.1798(12) 0.0156 1.0000 Uani S T . . . . 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 0.0161(2) 0.0206(3) 0.0162(2) 0.0038(5) 0.0000 0.0000 N1 0.019(3) 0.027(4) 0.030(4) 0.010(4) 0.0000 0.0000 C1 0.006(3) 0.017(4) 0.025(5) -0.003(4) 0.0000 0.0000 N2 0.021(3) 0.020(2) 0.017(2) -0.006(2) 0.005(2) -0.004(2) C2 0.022(3) 0.010(2) 0.012(2) 0.001(2) -0.002(2) -0.005(2) C3 0.021(4) 0.012(4) 0.013(4) -0.006(3) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.17(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 . N2 3_555 2.241(5) yes Ag1 . N1 . 2.173(8) yes Ag1 . N2 . 2.241(5) yes N1 . C1 . 1.157(11) yes C1 . C3 5_466 1.402(11) yes N2 . C2 . 1.142(7) yes C2 . C3 . 1.407(7) yes 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 N2 3_555 Ag1 . N1 . 124.06(14) yes N2 3_555 Ag1 . N2 . 105.9(2) yes N1 . Ag1 . N2 . 124.06(14) yes Ag1 . N1 . C1 . 174.3(7) yes C3 5_466 C1 . N1 . 180.0(4) yes Ag1 . N2 . C2 . 155.0(5) yes N2 . C2 . C3 . 178.6(6) yes C2 . C3 . C2 3_655 122.1(7) yes C2 . C3 . C1 7_664 118.9(4) yes C2 3_655 C3 . C1 7_664 118.9(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 12:43:38 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 12:43:38 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 961477' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.047(5) _cell_length_b 9.871(5) _cell_length_c 6.261(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 497.3(6) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.64 Fooo = 368.00 Mu = 39.13 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.64 FOOO = 368.00 Mu = 39.13 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 549 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.913 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 844 _reflns_number_total 535 _diffrn_reflns_av_R_equivalents 0.019 # Number of reflections without Friedels Law is 535 # Number of reflections with Friedels Law is 350 # Theoretical number of reflections is about 342 _diffrn_reflns_theta_min 3.266 _diffrn_reflns_theta_max 29.369 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 26.974 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -7 _reflns_limit_l_max 8 _oxford_diffrn_Wilson_B_factor 2.08 _oxford_diffrn_Wilson_scale 0.25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.90 _refine_diff_density_max 0.74 # 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 535 _refine_ls_number_restraints 1 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0314 _refine_ls_wR_factor_ref 0.0610 _refine_ls_goodness_of_fit_ref 1.0265 _refine_ls_shift/su_max 0.0002712 _refine_ls_shift/su_mean 0.0000520 # The values computed with all filters except I/sigma _oxford_reflns_number_all 535 _refine_ls_R_factor_all 0.0314 _refine_ls_wR_factor_all 0.0610 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 502 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_gt 0.0584 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^) + ( 0.03P)^2^ + 1.26P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64836(6) 0.5560(3) 0.0259 1.0000 Uani S T . . . . N1 N 0.2500 0.5145(9) 0.8304(12) 0.0343 1.0000 Uani S T . . . . C1 C 0.2500 0.4524(10) 0.9881(13) 0.0205 1.0000 Uani S T . . . . N2 N 0.4712(7) 0.6837(5) 0.3444(8) 0.0280 1.0000 Uani . . . . . . C2 C 0.5974(7) 0.6564(6) 0.2697(9) 0.0203 1.0000 Uani . . . . . . C3 C 0.7500 0.6207(9) 0.1780(12) 0.0167 1.0000 Uani S T . . . . 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 0.0227(3) 0.0314(3) 0.0235(3) 0.0046(5) 0.0000 0.0000 N1 0.024(4) 0.043(5) 0.037(4) 0.020(4) 0.0000 0.0000 C1 0.011(3) 0.020(4) 0.031(5) 0.000(4) 0.0000 0.0000 N2 0.026(3) 0.031(3) 0.027(3) -0.004(2) 0.003(2) -0.006(2) C2 0.020(3) 0.019(3) 0.022(3) 0.002(2) -0.001(2) -0.003(2) C3 0.022(4) 0.015(4) 0.013(4) -0.002(4) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.07(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 . N2 3_555 2.246(5) yes Ag1 . N1 . 2.168(8) yes Ag1 . N2 . 2.246(5) yes N1 . C1 . 1.162(11) yes C1 . C3 5_466 1.391(11) yes N2 . C2 . 1.150(8) yes C2 . C3 . 1.401(7) yes 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 N2 3_555 Ag1 . N1 . 124.22(16) yes N2 3_555 Ag1 . N2 . 104.8(3) yes N1 . Ag1 . N2 . 124.22(16) yes Ag1 . N1 . C1 . 174.3(8) yes C3 5_466 C1 . N1 . 179.5(10) yes Ag1 . N2 . C2 . 154.6(5) yes N2 . C2 . C3 . 178.9(7) yes C2 . C3 . C2 3_655 122.5(8) yes C2 . C3 . C1 7_664 118.7(4) yes C2 3_655 C3 . C1 7_664 118.7(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 13:15:59 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 13:15:59 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 961478' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0584(6) _cell_length_b 9.8752(8) _cell_length_c 6.2692(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 498.90(7) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.64 Fooo = 368.00 Mu = 39.00 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.64 FOOO = 368.00 Mu = 39.00 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 556 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.635 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.900 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 843 _reflns_number_total 534 _diffrn_reflns_av_R_equivalents 0.019 # Number of reflections without Friedels Law is 534 # Number of reflections with Friedels Law is 350 # Theoretical number of reflections is about 342 _diffrn_reflns_theta_min 3.263 _diffrn_reflns_theta_max 29.331 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 26.939 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 2.12 _oxford_diffrn_Wilson_scale 0.23 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.71 _refine_diff_density_max 0.93 # 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 533 _refine_ls_number_restraints 5 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0261 _refine_ls_wR_factor_ref 0.0454 _refine_ls_goodness_of_fit_ref 1.0363 _refine_ls_shift/su_max 0.0004185 _refine_ls_shift/su_mean 0.0000174 # The values computed with all filters except I/sigma _oxford_reflns_number_all 534 _refine_ls_R_factor_all 0.0265 _refine_ls_wR_factor_all 0.0459 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 505 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_gt 0.0412 # 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 ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^) + ( 0.01P)^2^ + 1.24P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64833(5) 0.5555(2) 0.0259 1.0000 Uani S T . . . . N1 N 0.2500 0.5135(7) 0.8310(10) 0.0356 1.0000 Uani S TU . . . . C1 C 0.2500 0.4534(8) 0.9878(11) 0.0234 1.0000 Uani S TU . . . . N2 N 0.4711(5) 0.6833(4) 0.3439(7) 0.0279 1.0000 Uani . . . . . . C2 C 0.5967(6) 0.6559(5) 0.2720(7) 0.0205 1.0000 Uani . . . . . . C3 C 0.7500 0.6216(8) 0.1795(10) 0.0195 1.0000 Uani S T . . . . 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 0.0225(2) 0.0319(3) 0.0232(2) 0.0052(5) 0.0000 0.0000 N1 0.027(3) 0.039(4) 0.041(3) 0.014(3) 0.0000 0.0000 C1 0.011(3) 0.022(3) 0.037(5) -0.003(3) 0.0000 0.0000 N2 0.028(2) 0.028(2) 0.029(2) -0.007(2) 0.004(2) -0.0072(19) C2 0.025(3) 0.016(2) 0.020(2) 0.001(2) -0.003(2) -0.005(2) C3 0.019(3) 0.027(4) 0.013(3) -0.001(3) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.126(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 . N2 3_555 2.248(4) yes Ag1 . N1 . 2.181(7) yes Ag1 . N2 . 2.248(4) yes N1 . C1 . 1.148(10) yes C1 . C3 5_466 1.412(10) yes N2 . C2 . 1.140(6) yes C2 . C3 . 1.406(6) yes 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 N2 3_555 Ag1 . N1 . 124.13(13) yes N2 3_555 Ag1 . N2 . 104.9(2) yes N1 . Ag1 . N2 . 124.13(13) yes Ag1 . N1 . C1 . 173.5(7) yes C3 5_466 C1 . N1 . 179.5(8) yes Ag1 . N2 . C2 . 154.2(4) yes N2 . C2 . C3 . 178.9(5) yes C1 5_564 C3 . C2 . 118.5(3) yes C1 5_564 C3 . C2 3_655 118.5(3) yes C2 . C3 . C2 3_655 123.0(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 12:47:53 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 12:47:53 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = N(1) TO C(1) END ; _database_code_depnum_ccdc_archive 'CCDC 961479' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0260(6) _cell_length_b 9.9680(10) _cell_length_c 6.2459(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 499.69(7) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.63 Fooo = 368.00 Mu = 38.94 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.63 FOOO = 368.00 Mu = 38.94 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 490 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 200 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.631 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.894 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 855 _reflns_number_total 534 _diffrn_reflns_av_R_equivalents 0.017 # Number of reflections without Friedels Law is 534 # Number of reflections with Friedels Law is 351 # Theoretical number of reflections is about 345 _diffrn_reflns_theta_min 3.259 _diffrn_reflns_theta_max 29.395 _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 26.873 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 2.84 _oxford_diffrn_Wilson_scale 0.26 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.78 _refine_diff_density_max 0.60 # 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 534 _refine_ls_number_restraints 1 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0341 _refine_ls_wR_factor_ref 0.0626 _refine_ls_goodness_of_fit_ref 1.0248 _refine_ls_shift/su_max 0.0004195 _refine_ls_shift/su_mean 0.0000180 # The values computed with all filters except I/sigma _oxford_reflns_number_all 534 _refine_ls_R_factor_all 0.0341 _refine_ls_wR_factor_all 0.0626 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 491 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_gt 0.0602 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^) + ( 0.03P)^2^ + 1.79P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64951(6) 0.5567(3) 0.0355 1.0000 Uani S T . . . . N1 N 0.2500 0.5137(9) 0.8294(14) 0.0469 1.0000 Uani S T . . . . C1 C 0.2500 0.4521(11) 0.9863(14) 0.0299 1.0000 Uani S T . . . . N2 N 0.4697(7) 0.6829(5) 0.3418(9) 0.0371 1.0000 Uani . . . . . . C2 C 0.5982(8) 0.6549(6) 0.2696(9) 0.0263 1.0000 Uani . . . . . . C3 C 0.7500 0.6211(10) 0.1787(13) 0.0277 1.0000 Uani S T . . . . 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 0.0316(3) 0.0437(4) 0.0314(3) 0.0080(6) 0.0000 0.0000 N1 0.038(4) 0.055(5) 0.048(4) 0.026(4) 0.0000 0.0000 C1 0.018(4) 0.032(5) 0.040(5) 0.006(4) 0.0000 0.0000 N2 0.036(3) 0.037(3) 0.038(3) -0.008(3) 0.005(3) -0.002(2) C2 0.031(3) 0.023(3) 0.025(3) 0.003(2) -0.001(2) -0.005(2) C3 0.030(4) 0.030(6) 0.022(4) -0.009(4) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.03(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 . N2 3_555 2.241(6) yes Ag1 . N1 . 2.176(8) yes Ag1 . N2 . 2.241(6) yes N1 . C1 . 1.156(12) yes C1 . C3 5_466 1.406(12) yes N2 . C2 . 1.160(8) yes C2 . C3 . 1.386(7) yes 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 N2 3_555 Ag1 . N1 . 124.14(17) yes N2 3_555 Ag1 . N2 . 103.8(3) yes N1 . Ag1 . N2 . 124.14(17) yes Ag1 . N1 . C1 . 173.6(9) yes C3 5_466 C1 . N1 . 179.2(10) yes Ag1 . N2 . C2 . 153.8(5) yes N2 . C2 . C3 . 178.7(7) yes C1 5_564 C3 . C2 . 118.5(4) yes C1 5_564 C3 . C2 3_655 118.5(4) yes C2 . C3 . C2 3_655 123.1(8) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 13:06:55 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 13:06:55 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 961480' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0280(6) _cell_length_b 9.9637(10) _cell_length_c 6.2461(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 499.62(7) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.63 Fooo = 368.00 Mu = 38.95 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.63 FOOO = 368.00 Mu = 38.95 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 493 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 200 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.631 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.895 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 853 _reflns_number_total 535 _diffrn_reflns_av_R_equivalents 0.019 # Number of reflections without Friedels Law is 535 # Number of reflections with Friedels Law is 351 # Theoretical number of reflections is about 345 _diffrn_reflns_theta_min 3.259 _diffrn_reflns_theta_max 29.396 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 26.998 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -8 _reflns_limit_l_max 7 _oxford_diffrn_Wilson_B_factor 2.82 _oxford_diffrn_Wilson_scale 0.25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.87 _refine_diff_density_max 0.91 # 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 535 _refine_ls_number_restraints 5 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0326 _refine_ls_wR_factor_ref 0.0568 _refine_ls_goodness_of_fit_ref 1.0252 _refine_ls_shift/su_max 0.0001011 _refine_ls_shift/su_mean 0.0000122 # The values computed with all filters except I/sigma _oxford_reflns_number_all 535 _refine_ls_R_factor_all 0.0326 _refine_ls_wR_factor_all 0.0540 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 482 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_gt 0.0540 # 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 ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^ + 1.48P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.64942(6) 0.5569(3) 0.0355 1.0000 Uani S T . . . . N1 N 0.2500 0.5137(9) 0.8300(12) 0.0450 1.0000 Uani S TU . . . . C1 C 0.2500 0.4531(10) 0.9855(13) 0.0297 1.0000 Uani S TU . . . . N2 N 0.4709(7) 0.6832(5) 0.3420(9) 0.0374 1.0000 Uani . . . . . . C2 C 0.5970(8) 0.6562(6) 0.2695(9) 0.0277 1.0000 Uani . . . . . . C3 C 0.7500 0.6199(9) 0.1766(12) 0.0266 1.0000 Uani S T . . . . 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 0.0309(3) 0.0443(4) 0.0312(3) 0.0074(6) 0.0000 0.0000 N1 0.038(4) 0.052(5) 0.045(4) 0.027(4) 0.0000 0.0000 C1 0.021(3) 0.030(5) 0.039(5) 0.003(4) 0.0000 0.0000 N2 0.034(3) 0.041(3) 0.038(3) -0.007(3) 0.010(3) -0.007(2) C2 0.035(3) 0.022(3) 0.026(3) 0.002(2) -0.001(2) -0.006(3) C3 0.026(4) 0.029(6) 0.025(4) -0.003(4) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 2.05(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 . N2 3_555 2.250(5) yes Ag1 . N1 . 2.177(8) yes Ag1 . N2 . 2.250(5) yes N1 . C1 . 1.144(12) yes C1 . C3 5_466 1.397(11) yes N2 . C2 . 1.141(8) yes C2 . C3 . 1.406(7) yes 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 N2 3_555 Ag1 . N1 . 124.09(16) yes N2 3_555 Ag1 . N2 . 104.1(3) yes N1 . Ag1 . N2 . 124.09(16) yes Ag1 . N1 . C1 . 173.5(9) yes C3 5_466 C1 . N1 . 179.4(10) yes Ag1 . N2 . C2 . 154.3(5) yes N2 . C2 . C3 . 178.2(7) yes C2 . C3 . C2 3_655 121.7(8) yes C2 . C3 . C1 7_664 119.1(4) yes C2 3_655 C3 . C1 7_664 119.1(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 12:51:55 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 12:51:55 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = N(1) TO C(1) END ; _database_code_depnum_ccdc_archive 'CCDC 961481' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #end of refcif _cell_length_a 8.0174(6) _cell_length_b 10.0853(11) _cell_length_c 6.2353(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 504.17(8) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m a 2 ' _symmetry_space_group_name_Hall 'I 2 -2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x+1/2,y,z -x+1,y+1/2,z+1/2 x+1/2,-y,z x+1,-y+1/2,z+1/2 -x,-y,z -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' 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 = C4 Ag1 N3 # Dc = 2.61 Fooo = 368.00 Mu = 38.60 M = 98.97 # Found Formula = C4 Ag1 N3 # Dc = 2.61 FOOO = 368.00 Mu = 38.60 M = 98.97 _chemical_formula_sum 'C4 Ag1 N3' _chemical_formula_moiety 'C4 Ag1 N3' _chemical_compound_source 'Sigma Aldrich and Alfa Aeser' _chemical_formula_weight 197.93 _cell_measurement_reflns_used 435 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_measurement_temperature 250 _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_min 0.044 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_max 0.094 _exptl_crystal_density_diffrn 2.607 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.860 # Sheldrick geometric approximatio 0.82 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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 857 _reflns_number_total 533 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections without Friedels Law is 533 # Number of reflections with Friedels Law is 349 # Theoretical number of reflections is about 339 _diffrn_reflns_theta_min 3.246 _diffrn_reflns_theta_max 29.114 _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 26.743 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -7 _reflns_limit_l_max 8 _oxford_diffrn_Wilson_B_factor 3.48 _oxford_diffrn_Wilson_scale 0.28 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_diff_density_min -0.78 _refine_diff_density_max 0.94 # 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 533 _refine_ls_number_restraints 5 _refine_ls_number_parameters 43 _oxford_refine_ls_R_factor_ref 0.0411 _refine_ls_wR_factor_ref 0.0585 _refine_ls_goodness_of_fit_ref 1.0498 _refine_ls_shift/su_max 0.0001688 _refine_ls_shift/su_mean 0.0000089 # The values computed with all filters except I/sigma _oxford_reflns_number_all 533 _refine_ls_R_factor_all 0.0411 _refine_ls_wR_factor_all 0.0585 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 468 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_gt 0.0552 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref #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^ + 0.29P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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 0.2500 0.65069(7) 0.5582(3) 0.0447 1.0000 Uani S T . . . . N1 N 0.2500 0.5126(9) 0.8289(13) 0.0542 1.0000 Uani S TU . . . . C1 C 0.2500 0.4529(12) 0.9841(16) 0.0423 1.0000 Uani S TU . . . . N2 N 0.4704(7) 0.6823(5) 0.3387(9) 0.0452 1.0000 Uani . . . . . . C2 C 0.5970(8) 0.6554(6) 0.2674(9) 0.0334 1.0000 Uani . . . . . . C3 C 0.7500 0.6194(11) 0.1752(14) 0.0358 1.0000 Uani S T . . . . 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 0.0390(3) 0.0565(4) 0.0387(3) 0.0105(7) 0.0000 0.0000 N1 0.043(4) 0.065(6) 0.055(4) 0.028(4) 0.0000 0.0000 C1 0.023(4) 0.054(6) 0.051(6) 0.005(5) 0.0000 0.0000 N2 0.038(3) 0.055(4) 0.043(3) -0.011(3) 0.010(3) -0.009(3) C2 0.040(4) 0.025(3) 0.035(3) -0.003(3) 0.000(3) -0.010(3) C3 0.033(5) 0.047(7) 0.027(5) -0.006(5) 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 1.956(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 . N2 3_555 2.258(6) yes Ag1 . N1 . 2.188(9) yes Ag1 . N2 . 2.258(6) yes N1 . C1 . 1.139(13) yes C1 . C3 5_466 1.397(13) yes N2 . C2 . 1.141(8) yes C2 . C3 . 1.403(8) yes 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 N2 3_555 Ag1 . N1 . 123.89(17) yes N2 3_555 Ag1 . N2 . 103.0(3) yes N1 . Ag1 . N2 . 123.89(17) yes Ag1 . N1 . C1 . 172.4(9) yes C3 5_466 C1 . N1 . 179.6(11) yes Ag1 . N2 . C2 . 154.0(5) yes N2 . C2 . C3 . 178.1(7) yes C2 3_655 C3 . C2 . 122.0(8) yes C2 3_655 C3 . C1 7_664 119.0(4) yes C2 . C3 . C1 7_664 119.0(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/09/13 at 12:55:52 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/09/13 at 12:55:52 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = N(1) TO C(1) END ; _database_code_depnum_ccdc_archive 'CCDC 961482'