# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Arnaud Gautier' _publ_contact_author_address ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; _publ_contact_author_email arnaud.gautier@univ-bpclermont.fr _publ_contact_author_phone +33473407646 _publ_contact_author_fax +33473407717 loop_ _publ_author_name _publ_author_address A.Hospital ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; C.Gibard ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; C.Gaulier ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; L.Nauton ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; V.Thery ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; M.El-Ghozzi ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; ; D.Avignant ; ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; F.Cisnetti ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; A.Gautier ; Institut de Chimie de Clermont-Ferrand Universit\'e Blaise Pascal, CNRS BP 80026 63171 AUBIERE Cedex France ; _audit_creation_date 12-03-07 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 1 _chemical_name_systematic '[N,N?-bis(4-azido-2,6-diisopropylphenyl)imidazol-2-ylidene]chlorosilver(I)' _chemical_name_common AgCl(IPrN3) _chemical_formula_moiety 'C27 H34 Ag1 Cl1 N8, C H2 Cl2' _chemical_formula_sum 'C28 H36 Ag1 Cl3 N8' _exptl_crystal_recrystallization_method 'dichloromethane, n-pentane' _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints (Cooper et al, 2010). Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; _symmetry_cell_setting ? _symmetry_space_group_name_h-m ? _symmetry_int_tables_number ? _chemical_absolute_configuration ? _diffrn_radiation_probe ? # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # data_1a _database_code_depnum_ccdc_archive 'CCDC 864596' #TrackingRef '- 864596-21-reorder.cif.txt' _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 ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 10.0772(3) _cell_length_b 15.3419(5) _cell_length_c 21.5215(8) _cell_angle_alpha 90 _cell_angle_beta 92.1640(10) _cell_angle_gamma 90 _cell_volume 3324.92(19) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 = C28 H36 Ag1 Cl3 N8 # Dc = 1.40 Fooo = 1432.00 Mu = 8.78 M = 698.87 # Found Formula = C28 H36 Ag1 Cl3 N8 # Dc = 1.40 FOOO = 1432.00 Mu = 8.78 M = 698.87 _chemical_formula_sum 'C28 H36 Ag1 Cl3 N8' _chemical_formula_moiety 'C28 H36 Ag1 Cl3 N8' _chemical_compound_source ? _chemical_formula_weight 698.87 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.111 _exptl_crystal_size_mid 0.121 _exptl_crystal_size_max 0.811 _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.878 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _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 28174 _reflns_number_total 7223 _diffrn_reflns_av_R_equivalents 0.030 # Number of reflections without Friedels Law is 7223 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 7260 _diffrn_reflns_theta_min 1.630 _diffrn_reflns_theta_max 27.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.460 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _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 -0.60 _refine_diff_density_max 0.89 # 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 4562 _refine_ls_number_restraints 0 _refine_ls_number_parameters 361 _oxford_refine_ls_R_factor_ref 0.0400 _refine_ls_wR_factor_ref 0.0473 _refine_ls_goodness_of_fit_ref 0.8432 _refine_ls_shift/su_max 0.0005628 _refine_ls_shift/su_mean 0.0000212 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7200 _refine_ls_R_factor_all 0.0651 _refine_ls_wR_factor_all 0.0883 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5023 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_gt 0.0490 # 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 F _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, 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: 0.553 0.682 0.441 0.208 0.984E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. 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 C1 C 0.0249(3) 0.7113(2) 0.30330(15) 0.0417 1.0000 Uani . . . . . . C2 C -0.1825(3) 0.7494(3) 0.32874(18) 0.0517 1.0000 Uani . . . . . . C3 C -0.1949(3) 0.6936(2) 0.28146(18) 0.0520 1.0000 Uani . . . . . . C4 C 0.0105(3) 0.8133(2) 0.39055(16) 0.0461 1.0000 Uani . . . . . . C5 C 0.0326(4) 0.7763(3) 0.44907(18) 0.0560 1.0000 Uani . . . . . . C6 C 0.0922(4) 0.8280(3) 0.49487(19) 0.0633 1.0000 Uani . . . . . . C7 C 0.1288(4) 0.9117(3) 0.48256(19) 0.0598 1.0000 Uani . . . . . . C8 C 0.1036(4) 0.9485(3) 0.42450(19) 0.0581 1.0000 Uani . . . . . . C9 C 0.0432(4) 0.8994(2) 0.37694(17) 0.0493 1.0000 Uani . . . . . . C10 C -0.0083(6) 0.6832(3) 0.4636(2) 0.0768 1.0000 Uani . . . . . . C11 C -0.1058(10) 0.6802(5) 0.5150(4) 0.1676 1.0000 Uani . . . . . . C12 C 0.1123(8) 0.6281(4) 0.4803(4) 0.1406 1.0000 Uani . . . . . . C13 C 0.0168(4) 0.9404(3) 0.31375(19) 0.0588 1.0000 Uani . . . . . . C14 C -0.0751(6) 1.0187(4) 0.3163(3) 0.0905 1.0000 Uani . . . . . . C15 C 0.1455(6) 0.9639(4) 0.2828(3) 0.0981 1.0000 Uani . . . . . . C16 C -0.0361(3) 0.6107(2) 0.21703(16) 0.0447 1.0000 Uani . . . . . . C17 C -0.0080(4) 0.6452(3) 0.15915(17) 0.0522 1.0000 Uani . . . . . . C18 C -0.0103(5) 0.7426(3) 0.1455(2) 0.0661 1.0000 Uani . . . . . . C19 C 0.0247(4) 0.4988(3) 0.12304(18) 0.0536 1.0000 Uani . . . . . . C20 C -0.0029(4) 0.4656(3) 0.18052(18) 0.0524 1.0000 Uani . . . . . . C21 C -0.0337(3) 0.5215(2) 0.22923(17) 0.0503 1.0000 Uani . . . . . . C22 C 0.0208(4) 0.5871(3) 0.11216(18) 0.0570 1.0000 Uani . . . . . . C23 C 0.1255(7) 0.7736(4) 0.1248(4) 0.1167 1.0000 Uani . . . . . . C24 C -0.1220(7) 0.7651(4) 0.0991(3) 0.1032 1.0000 Uani . . . . . . C25 C -0.0567(4) 0.4858(3) 0.29395(19) 0.0600 1.0000 Uani . . . . . . C26 C 0.0755(6) 0.4620(4) 0.3257(2) 0.0975 1.0000 Uani . . . . . . C27 C -0.1489(6) 0.4068(4) 0.2931(3) 0.0887 1.0000 Uani . . . . . . N1 N -0.0475(3) 0.76007(19) 0.34147(13) 0.0435 1.0000 Uani . . . . . . N2 N -0.0673(3) 0.66985(19) 0.26646(13) 0.0443 1.0000 Uani . . . . . . N3 N 0.1946(4) 0.9560(3) 0.53294(19) 0.0795 1.0000 Uani . . . . . . N4 N 0.2245(4) 1.0323(4) 0.5247(2) 0.0814 1.0000 Uani . . . . . . N5 N 0.2590(5) 1.1021(4) 0.5243(3) 0.1070 1.0000 Uani . . . . . . N6 N 0.0598(4) 0.4477(3) 0.07079(17) 0.0693 1.0000 Uani . . . . . . N7 N 0.0672(5) 0.3693(3) 0.07700(18) 0.0803 1.0000 Uani . . . . . . N8 N 0.0808(8) 0.2973(4) 0.0742(3) 0.1363 1.0000 Uani . . . . . . Cl1 Cl 0.45433(10) 0.71754(8) 0.27885(7) 0.0809 1.0000 Uani . . . . . . Ag1 Ag 0.22895(2) 0.709670(19) 0.295092(14) 0.0517 1.0000 Uani . . . . . . C30 C 0.9678(9) 0.0874(5) 0.0817(5) 0.1515 1.0000 Uani . . . . . . Cl2 Cl 1.1033(3) 0.0241(2) 0.08862(19) 0.2108 1.0000 Uani . . . . . . Cl30 Cl 0.8303(4) 0.0277(2) 0.0968(2) 0.2512 1.0000 Uani . . . . . . H21 H -0.2500 0.7768 0.3490 0.0617 1.0000 Uiso R . . . . . H31 H -0.2722 0.6733 0.2626 0.0611 1.0000 Uiso R . . . . . H61 H 0.1101 0.8054 0.5342 0.0746 1.0000 Uiso R . . . . . H81 H 0.1265 1.0057 0.4173 0.0673 1.0000 Uiso R . . . . . H101 H -0.0501 0.6588 0.4263 0.0898 1.0000 Uiso R . . . . . H113 H -0.1106 0.6212 0.5306 0.2327 1.0000 Uiso R . . . . . H112 H -0.0785 0.7195 0.5481 0.2326 1.0000 Uiso R . . . . . H111 H -0.1920 0.6967 0.4992 0.2326 1.0000 Uiso R . . . . . H121 H 0.0857 0.5721 0.4944 0.1937 1.0000 Uiso R . . . . . H122 H 0.1651 0.6571 0.5121 0.1937 1.0000 Uiso R . . . . . H123 H 0.1639 0.6203 0.4447 0.1936 1.0000 Uiso R . . . . . H131 H -0.0279 0.8974 0.2877 0.0681 1.0000 Uiso R . . . . . H141 H -0.0991 1.0370 0.2743 0.1255 1.0000 Uiso R . . . . . H142 H -0.0274 1.0655 0.3378 0.1252 1.0000 Uiso R . . . . . H143 H -0.1549 1.0025 0.3386 0.1255 1.0000 Uiso R . . . . . H151 H 0.1280 0.9766 0.2401 0.1342 1.0000 Uiso R . . . . . H152 H 0.1821 1.0143 0.3034 0.1344 1.0000 Uiso R . . . . . H153 H 0.2068 0.9167 0.2873 0.1346 1.0000 Uiso R . . . . . H181 H -0.0266 0.7729 0.1842 0.0768 1.0000 Uiso R . . . . . H201 H -0.0005 0.4059 0.1871 0.0617 1.0000 Uiso R . . . . . H221 H 0.0382 0.6081 0.0725 0.0654 1.0000 Uiso R . . . . . H231 H 0.1241 0.8364 0.1195 0.1627 1.0000 Uiso R . . . . . H232 H 0.1928 0.7586 0.1558 0.1626 1.0000 Uiso R . . . . . H233 H 0.1450 0.7468 0.0861 0.1624 1.0000 Uiso R . . . . . H241 H -0.1220 0.8272 0.0921 0.1420 1.0000 Uiso R . . . . . H242 H -0.2062 0.7478 0.1151 0.1414 1.0000 Uiso R . . . . . H243 H -0.1071 0.7355 0.0605 0.1415 1.0000 Uiso R . . . . . H251 H -0.0969 0.5312 0.3184 0.0711 1.0000 Uiso R . . . . . H263 H 0.0611 0.4481 0.3687 0.1341 1.0000 Uiso R . . . . . H262 H 0.1354 0.5102 0.3236 0.1347 1.0000 Uiso R . . . . . H261 H 0.1127 0.4118 0.3053 0.1344 1.0000 Uiso R . . . . . H271 H -0.1645 0.3910 0.3359 0.1224 1.0000 Uiso R . . . . . H272 H -0.2322 0.4215 0.2724 0.1225 1.0000 Uiso R . . . . . H273 H -0.1073 0.3593 0.2723 0.1222 1.0000 Uiso R . . . . . H301 H 0.9766 0.1347 0.1108 0.1717 1.0000 Uiso R . . . . . H302 H 0.9556 0.1103 0.0384 0.1715 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 C1 0.0347(15) 0.0490(18) 0.0412(16) 0.0023(16) -0.0006(12) 0.0017(15) C2 0.0292(15) 0.064(2) 0.062(2) 0.0046(19) 0.0070(15) 0.0055(15) C3 0.0329(15) 0.060(2) 0.063(2) 0.0019(18) -0.0005(14) -0.0012(15) C4 0.0416(17) 0.052(2) 0.0453(19) -0.0020(15) 0.0048(14) 0.0053(14) C5 0.051(2) 0.067(3) 0.050(2) 0.0055(19) 0.0034(16) 0.0061(18) C6 0.065(2) 0.082(3) 0.043(2) 0.003(2) 0.0007(18) 0.013(2) C7 0.049(2) 0.078(3) 0.052(2) -0.015(2) -0.0045(17) 0.0144(19) C8 0.055(2) 0.055(2) 0.064(2) -0.0077(19) -0.0043(18) 0.0056(18) C9 0.0446(18) 0.056(2) 0.0473(19) -0.0023(16) -0.0004(15) 0.0063(16) C10 0.097(4) 0.069(3) 0.064(3) 0.020(2) -0.005(2) -0.001(3) C11 0.219(10) 0.112(6) 0.181(8) 0.048(5) 0.123(8) 0.000(6) C12 0.120(6) 0.071(4) 0.227(9) 0.012(5) -0.037(6) 0.016(4) C13 0.063(2) 0.059(2) 0.054(2) 0.0067(18) -0.0069(18) -0.0004(19) C14 0.101(4) 0.091(4) 0.079(3) 0.024(3) -0.005(3) 0.028(3) C15 0.079(3) 0.131(5) 0.085(4) 0.036(3) 0.012(3) 0.006(3) C16 0.0350(15) 0.0504(19) 0.0484(19) -0.0021(15) -0.0016(13) -0.0020(14) C17 0.051(2) 0.057(2) 0.048(2) 0.0026(17) -0.0053(16) 0.0007(17) C18 0.088(3) 0.056(2) 0.054(2) 0.0066(19) 0.004(2) -0.004(2) C19 0.0479(19) 0.063(2) 0.050(2) -0.0071(18) -0.0032(16) 0.0047(17) C20 0.0471(19) 0.051(2) 0.059(2) 0.0002(17) 0.0006(16) 0.0023(16) C21 0.0414(17) 0.056(2) 0.053(2) 0.0027(17) -0.0020(15) -0.0046(16) C22 0.059(2) 0.063(2) 0.049(2) 0.0033(18) 0.0029(17) 0.0002(18) C23 0.116(5) 0.081(4) 0.155(6) 0.029(4) 0.023(5) -0.029(4) C24 0.132(5) 0.074(3) 0.101(4) 0.006(3) -0.025(4) 0.030(3) C25 0.070(3) 0.055(2) 0.056(2) 0.0076(19) 0.0131(19) -0.0014(19) C26 0.098(4) 0.125(5) 0.068(3) 0.034(3) -0.017(3) -0.016(4) C27 0.092(4) 0.082(3) 0.093(4) 0.014(3) 0.021(3) -0.023(3) N1 0.0353(13) 0.0520(16) 0.0431(15) 0.0026(12) 0.0025(11) 0.0024(12) N2 0.0338(13) 0.0520(16) 0.0470(16) 0.0013(13) 0.0003(11) -0.0009(12) N3 0.080(3) 0.094(3) 0.064(2) -0.023(2) -0.0143(19) 0.007(2) N4 0.060(2) 0.098(3) 0.085(3) -0.038(3) -0.009(2) 0.016(2) N5 0.087(3) 0.102(4) 0.131(4) -0.047(3) -0.007(3) 0.005(3) N6 0.081(3) 0.070(2) 0.056(2) -0.0072(18) 0.0028(18) 0.010(2) N7 0.108(3) 0.069(3) 0.065(2) -0.014(2) 0.016(2) 0.004(2) N8 0.235(8) 0.074(3) 0.104(4) -0.010(3) 0.054(4) 0.013(4) Cl1 0.0369(4) 0.0801(8) 0.1267(10) -0.0101(7) 0.0162(5) -0.0011(5) Ag1 0.03219(13) 0.05716(17) 0.06594(18) -0.00620(15) 0.00299(10) 0.00007(13) C30 0.142(7) 0.090(5) 0.221(10) -0.011(5) -0.022(7) -0.016(5) Cl2 0.134(2) 0.214(3) 0.285(4) -0.001(3) 0.004(2) 0.024(2) Cl30 0.182(3) 0.187(3) 0.395(5) -0.095(3) 0.153(3) -0.062(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.10674(16) 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 C1 . Ag1 . 2.070(3) yes Cl1 . Ag1 . 2.3141(10) yes C1 . N1 . 1.346(4) yes C1 . N2 . 1.357(4) yes C2 . C3 . 1.332(6) yes C2 . N1 . 1.387(4) yes C2 . H21 . 0.923 no C3 . N2 . 1.387(4) yes C3 . H31 . 0.918 no C4 . C5 . 1.392(5) yes C4 . C9 . 1.395(5) yes C4 . N1 . 1.441(5) yes C5 . C6 . 1.385(6) yes C5 . C10 . 1.522(6) yes C6 . C7 . 1.364(6) yes C6 . H61 . 0.927 no C7 . C8 . 1.386(6) yes C7 . N3 . 1.423(5) yes C8 . C9 . 1.392(5) yes C8 . H81 . 0.921 no C9 . C13 . 1.513(5) yes C10 . C11 . 1.508(8) yes C10 . C12 . 1.512(8) yes C10 . H101 . 0.967 no C11 . H113 . 0.966 no C11 . H112 . 0.965 no C11 . H111 . 0.956 no C12 . H121 . 0.952 no C12 . H122 . 0.960 no C12 . H123 . 0.949 no C13 . C14 . 1.519(6) yes C13 . C15 . 1.523(7) yes C13 . H131 . 0.966 no C14 . H141 . 0.968 no C14 . H142 . 0.971 no C14 . H143 . 0.983 no C15 . H151 . 0.949 no C15 . H152 . 0.959 no C15 . H153 . 0.954 no C16 . C17 . 1.392(5) yes C16 . C21 . 1.394(5) yes C16 . N2 . 1.442(4) yes C17 . C18 . 1.523(6) yes C17 . C22 . 1.386(5) yes C18 . C23 . 1.531(8) yes C18 . C24 . 1.517(7) yes C18 . H181 . 0.973 no C19 . C20 . 1.376(5) yes C19 . C22 . 1.375(6) yes C19 . N6 . 1.427(5) yes C20 . C21 . 1.398(5) yes C20 . H201 . 0.926 no C21 . C25 . 1.522(5) yes C22 . H221 . 0.935 no C23 . H231 . 0.970 no C23 . H232 . 0.961 no C23 . H233 . 0.955 no C24 . H241 . 0.964 no C24 . H242 . 0.965 no C24 . H243 . 0.964 no C25 . C26 . 1.519(7) yes C25 . C27 . 1.527(6) yes C25 . H251 . 0.971 no C26 . H263 . 0.966 no C26 . H262 . 0.957 no C26 . H261 . 0.970 no C27 . H271 . 0.971 no C27 . H272 . 0.961 no C27 . H273 . 0.960 no N3 . N4 . 1.223(7) yes N4 . N5 . 1.126(7) yes N6 . N7 . 1.212(6) yes N7 . N8 . 1.115(6) yes C30 . Cl2 . 1.678(9) yes C30 . Cl30 . 1.703(9) yes C30 . H301 . 0.961 no C30 . H302 . 0.998 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 C1 . Ag1 . Cl1 . 174.71(10) yes N1 . C1 . N2 . 104.0(3) yes N1 . C1 . Ag1 . 128.5(2) yes N2 . C1 . Ag1 . 127.2(2) yes C3 . C2 . N1 . 106.9(3) yes C3 . C2 . H21 . 127.2 no N1 . C2 . H21 . 126.0 no C2 . C3 . N2 . 106.6(3) yes C2 . C3 . H31 . 127.5 no N2 . C3 . H31 . 125.9 no C5 . C4 . C9 . 123.0(3) yes C5 . C4 . N1 . 118.6(3) yes C9 . C4 . N1 . 118.4(3) yes C4 . C5 . C6 . 117.4(4) yes C4 . C5 . C10 . 122.2(4) yes C6 . C5 . C10 . 120.3(4) yes C5 . C6 . C7 . 120.9(4) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 119.0 no C6 . C7 . C8 . 121.2(4) yes C6 . C7 . N3 . 115.1(4) yes C8 . C7 . N3 . 123.8(4) yes C7 . C8 . C9 . 120.1(4) yes C7 . C8 . H81 . 120.1 no C9 . C8 . H81 . 119.8 no C4 . C9 . C8 . 117.3(3) yes C4 . C9 . C13 . 123.2(3) yes C8 . C9 . C13 . 119.5(4) yes C5 . C10 . C11 . 111.6(5) yes C5 . C10 . C12 . 110.6(5) yes C11 . C10 . C12 . 110.4(6) yes C5 . C10 . H101 . 107.7 no C11 . C10 . H101 . 108.7 no C12 . C10 . H101 . 107.6 no C10 . C11 . H113 . 109.0 no C10 . C11 . H112 . 110.2 no H113 . C11 . H112 . 110.2 no C10 . C11 . H111 . 109.9 no H113 . C11 . H111 . 108.4 no H112 . C11 . H111 . 109.1 no C10 . C12 . H121 . 110.2 no C10 . C12 . H122 . 109.2 no H121 . C12 . H122 . 110.2 no C10 . C12 . H123 . 109.8 no H121 . C12 . H123 . 108.2 no H122 . C12 . H123 . 109.2 no C9 . C13 . C14 . 112.5(4) yes C9 . C13 . C15 . 111.6(4) yes C14 . C13 . C15 . 111.1(4) yes C9 . C13 . H131 . 107.4 no C14 . C13 . H131 . 106.9 no C15 . C13 . H131 . 107.1 no C13 . C14 . H141 . 109.0 no C13 . C14 . H142 . 108.1 no H141 . C14 . H142 . 109.3 no C13 . C14 . H143 . 109.2 no H141 . C14 . H143 . 110.4 no H142 . C14 . H143 . 110.8 no C13 . C15 . H151 . 110.0 no C13 . C15 . H152 . 107.9 no H151 . C15 . H152 . 109.6 no C13 . C15 . H153 . 109.6 no H151 . C15 . H153 . 110.5 no H152 . C15 . H153 . 109.1 no C17 . C16 . C21 . 122.6(3) yes C17 . C16 . N2 . 118.6(3) yes C21 . C16 . N2 . 118.8(3) yes C16 . C17 . C18 . 122.9(4) yes C16 . C17 . C22 . 117.6(4) yes C18 . C17 . C22 . 119.5(3) yes C17 . C18 . C23 . 110.7(4) yes C17 . C18 . C24 . 110.8(4) yes C23 . C18 . C24 . 112.8(5) yes C17 . C18 . H181 . 107.8 no C23 . C18 . H181 . 106.4 no C24 . C18 . H181 . 108.0 no C20 . C19 . C22 . 120.9(4) yes C20 . C19 . N6 . 124.7(4) yes C22 . C19 . N6 . 114.5(4) yes C19 . C20 . C21 . 120.3(4) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.8 no C20 . C21 . C16 . 117.6(3) yes C20 . C21 . C25 . 120.7(3) yes C16 . C21 . C25 . 121.5(3) yes C17 . C22 . C19 . 120.9(4) yes C17 . C22 . H221 . 119.7 no C19 . C22 . H221 . 119.4 no C18 . C23 . H231 . 109.5 no C18 . C23 . H232 . 109.8 no H231 . C23 . H232 . 109.0 no C18 . C23 . H233 . 109.6 no H231 . C23 . H233 . 109.1 no H232 . C23 . H233 . 109.9 no C18 . C24 . H241 . 108.8 no C18 . C24 . H242 . 110.1 no H241 . C24 . H242 . 109.5 no C18 . C24 . H243 . 109.0 no H241 . C24 . H243 . 109.2 no H242 . C24 . H243 . 110.2 no C21 . C25 . C26 . 109.7(4) yes C21 . C25 . C27 . 112.8(4) yes C26 . C25 . C27 . 109.8(4) yes C21 . C25 . H251 . 108.5 no C26 . C25 . H251 . 107.8 no C27 . C25 . H251 . 108.1 no C25 . C26 . H263 . 108.9 no C25 . C26 . H262 . 109.7 no H263 . C26 . H262 . 109.5 no C25 . C26 . H261 . 109.5 no H263 . C26 . H261 . 109.5 no H262 . C26 . H261 . 109.7 no C25 . C27 . H271 . 107.9 no C25 . C27 . H272 . 109.9 no H271 . C27 . H272 . 109.2 no C25 . C27 . H273 . 109.3 no H271 . C27 . H273 . 110.0 no H272 . C27 . H273 . 110.6 no C4 . N1 . C2 . 125.4(3) yes C4 . N1 . C1 . 123.2(3) yes C2 . N1 . C1 . 111.4(3) yes C16 . N2 . C3 . 124.5(3) yes C16 . N2 . C1 . 124.2(3) yes C3 . N2 . C1 . 111.2(3) yes C7 . N3 . N4 . 117.3(4) yes N3 . N4 . N5 . 171.5(6) yes C19 . N6 . N7 . 118.4(4) yes N6 . N7 . N8 . 169.8(5) yes Cl2 . C30 . Cl30 . 109.7(5) yes Cl2 . C30 . H301 . 108.9 no Cl30 . C30 . H301 . 109.7 no Cl2 . C30 . H302 . 110.9 no Cl30 . C30 . H302 . 107.2 no H301 . C30 . H302 . 110.4 no _iucr_refine_instruction_details_constraints ; # # Punched on 07/03/12 at 15:42:45 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 113,X'S) H ( 112,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 263,X'S) H ( 262,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) H ( 273,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 07/03/12 at 15:42:45 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _chemical_name_common ;(N,N?-bis(4-azido-2,6-diisopropylphenyl)imidazol-2- ylidene)chlorosilver(i) ; data_1b _database_code_depnum_ccdc_archive 'CCDC 864597' #TrackingRef '- 864597-16-reorder.cif.txt' _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 ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 11.5948(9) _cell_length_b 14.2010(12) _cell_length_c 14.4224(12) _cell_angle_alpha 74.320(5) _cell_angle_beta 66.567(4) _cell_angle_gamma 88.958(4) _cell_volume 2087.1(3) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 2 # Given Formula = C43 H46 Ag1 Cl1 N8 # Dc = 1.30 Fooo = 848.00 Mu = 5.86 M = 818.21 # Found Formula = C43 H46 Ag1 Cl1 N8 # Dc = 1.30 FOOO = 848.00 Mu = 5.86 M = 818.21 _chemical_formula_sum 'C43 H46 Ag1 Cl1 N8' _chemical_formula_moiety 'C43 H46 Ag1 Cl1 N8' _chemical_compound_source ? _chemical_formula_weight 818.21 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.124 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_max 0.918 _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.586 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _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 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _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 31783 _reflns_number_total 16178 _diffrn_reflns_av_R_equivalents 0.140 # Number of reflections without Friedels Law is 16178 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 8480 _diffrn_reflns_theta_min 1.497 _diffrn_reflns_theta_max 27.323 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.137 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 18 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _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 -0.74 _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 3747 _refine_ls_number_restraints 0 _refine_ls_number_parameters 478 _oxford_refine_ls_R_factor_ref 0.0499 _refine_ls_wR_factor_ref 0.0431 _refine_ls_goodness_of_fit_ref 1.1601 _refine_ls_shift/su_max 0.0002475 _refine_ls_shift/su_mean 0.0000094 # The values computed with all filters except I/sigma _oxford_reflns_number_all 16121 _refine_ls_R_factor_all 0.2721 _refine_ls_wR_factor_all 0.1374 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4658 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_gt 0.0523 # 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 F _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, 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: 1.30 0.104 1.56 0.965E-01 0.553 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. 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 C1 C 0.6613(8) 0.2272(7) 0.1385(7) 0.0515 1.0000 Uani . . . . . . C2 C 0.7360(8) 0.1861(6) 0.2679(7) 0.0520 1.0000 Uani . . . . . . C3 C 0.7830(7) 0.2772(7) 0.2093(7) 0.0548 1.0000 Uani . . . . . . C4 C 0.5871(8) 0.0601(6) 0.2683(6) 0.0434 1.0000 Uani . . . . . . C5 C 0.4687(8) 0.0494(6) 0.3517(7) 0.0495 1.0000 Uani . . . . . . C6 C 0.4000(7) -0.0404(7) 0.3939(6) 0.0528 1.0000 Uani . . . . . . C7 C 0.4493(8) -0.1181(7) 0.3576(7) 0.0495 1.0000 Uani . . . . . . C8 C 0.5653(9) -0.1083(6) 0.2751(7) 0.0530 1.0000 Uani . . . . . . C9 C 0.6376(8) -0.0172(7) 0.2290(6) 0.0512 1.0000 Uani . . . . . . C10 C 0.4139(7) 0.1371(6) 0.3907(7) 0.0576 1.0000 Uani . . . . . . C11 C 0.3383(8) 0.1113(7) 0.5085(7) 0.0840 1.0000 Uani . . . . . . C12 C 0.3310(9) 0.1871(7) 0.3349(7) 0.0946 1.0000 Uani . . . . . . C13 C 0.7689(8) -0.0058(6) 0.1426(7) 0.0626 1.0000 Uani . . . . . . C14 C 0.8573(9) -0.0651(9) 0.1845(9) 0.1469 1.0000 Uani . . . . . . C15 C 0.7692(10) -0.0309(11) 0.0507(9) 0.1761 1.0000 Uani . . . . . . C16 C 0.3606(7) -0.2834(7) 0.3702(7) 0.0496 1.0000 Uani . . . . . . C17 C 0.2916(8) -0.3586(6) 0.4538(8) 0.0522 1.0000 Uani . . . . . . C18 C 0.2339(8) -0.4535(7) 0.4602(8) 0.0599 1.0000 Uani . . . . . . C19 C 0.2186(10) -0.5346(9) 0.5395(9) 0.1034 1.0000 Uani . . . . . . C20 C 0.1614(14) -0.6257(11) 0.5470(14) 0.1343 1.0000 Uani . . . . . . C21 C 0.1197(12) -0.6265(11) 0.4728(15) 0.1195 1.0000 Uani . . . . . . C22 C 0.1345(10) -0.5477(11) 0.3916(12) 0.1067 1.0000 Uani . . . . . . C23 C 0.1909(9) -0.4601(7) 0.3864(9) 0.0764 1.0000 Uani . . . . . . C24 C 0.7650(8) 0.3968(6) 0.0518(7) 0.0477 1.0000 Uani . . . . . . C25 C 0.6842(8) 0.4691(7) 0.0780(7) 0.0508 1.0000 Uani . . . . . . C26 C 0.7182(8) 0.5621(6) 0.0068(7) 0.0518 1.0000 Uani . . . . . . C27 C 0.8215(8) 0.5780(6) -0.0854(7) 0.0491 1.0000 Uani . . . . . . C28 C 0.8979(8) 0.5056(7) -0.1124(7) 0.0610 1.0000 Uani . . . . . . C29 C 0.8668(8) 0.4117(7) -0.0415(7) 0.0536 1.0000 Uani . . . . . . C30 C 0.5686(8) 0.4487(6) 0.1814(8) 0.0685 1.0000 Uani . . . . . . C31 C 0.5774(9) 0.5082(8) 0.2508(7) 0.1098 1.0000 Uani . . . . . . C32 C 0.4520(8) 0.4649(7) 0.1581(8) 0.1051 1.0000 Uani . . . . . . C33 C 0.9472(9) 0.3282(6) -0.0750(7) 0.0691 1.0000 Uani . . . . . . C34 C 1.0874(9) 0.3600(7) -0.1202(10) 0.1176 1.0000 Uani . . . . . . C35 C 0.9172(9) 0.2945(8) -0.1530(9) 0.1174 1.0000 Uani . . . . . . C36 C 0.8166(8) 0.7641(7) -0.1434(7) 0.0531 1.0000 Uani . . . . . . C37 C 0.8856(9) 0.8331(7) -0.2349(8) 0.0523 1.0000 Uani . . . . . . C38 C 0.8788(10) 0.9408(6) -0.2662(8) 0.0548 1.0000 Uani . . . . . . C39 C 0.7865(9) 0.9833(8) -0.2039(8) 0.0696 1.0000 Uani . . . . . . C40 C 0.7826(11) 1.0841(9) -0.2353(10) 0.0905 1.0000 Uani . . . . . . C41 C 0.8698(13) 1.1399(8) -0.3287(11) 0.0866 1.0000 Uani . . . . . . C42 C 0.9607(10) 1.0974(8) -0.3928(10) 0.0974 1.0000 Uani . . . . . . C43 C 0.9666(9) 0.9972(8) -0.3607(9) 0.0805 1.0000 Uani . . . . . . N1 N 0.6616(5) 0.1551(5) 0.2248(5) 0.0443 1.0000 Uani . . . . . . N2 N 0.7389(6) 0.3017(5) 0.1297(5) 0.0492 1.0000 Uani . . . . . . N3 N 0.3802(6) -0.2140(5) 0.4096(7) 0.0565 1.0000 Uani . . . . . . N4 N 0.3264(8) -0.2447(7) 0.5155(7) 0.0869 1.0000 Uani . . . . . . N5 N 0.2698(7) -0.3333(6) 0.5442(6) 0.0842 1.0000 Uani . . . . . . N6 N 0.8587(6) 0.6767(5) -0.1562(6) 0.0490 1.0000 Uani . . . . . . N7 N 0.9472(7) 0.6909(5) -0.2543(7) 0.0685 1.0000 Uani . . . . . . N8 N 0.9662(6) 0.7858(6) -0.3025(6) 0.0686 1.0000 Uani . . . . . . Cl1 Cl 0.4804(2) 0.22231(17) -0.07465(18) 0.0704 1.0000 Uani . . . . . . Ag1 Ag 0.57310(7) 0.22168(5) 0.04094(6) 0.0521 1.0000 Uani . . . . . . H21 H 0.7502 0.1487 0.3267 0.0630 1.0000 Uiso R . . . . . H31 H 0.8362 0.3193 0.2182 0.0662 1.0000 Uiso R . . . . . H61 H 0.3201 -0.0496 0.4478 0.0637 1.0000 Uiso R . . . . . H81 H 0.5948 -0.1620 0.2506 0.0638 1.0000 Uiso R . . . . . H101 H 0.4842 0.1855 0.3722 0.0691 1.0000 Uiso R . . . . . H111 H 0.3145 0.1706 0.5278 0.1259 1.0000 Uiso R . . . . . H112 H 0.3860 0.0783 0.5461 0.1259 1.0000 Uiso R . . . . . H113 H 0.2638 0.0690 0.5279 0.1259 1.0000 Uiso R . . . . . H123 H 0.3039 0.2458 0.3555 0.1421 1.0000 Uiso R . . . . . H122 H 0.3780 0.2041 0.2587 0.1420 1.0000 Uiso R . . . . . H121 H 0.2579 0.1423 0.3554 0.1420 1.0000 Uiso R . . . . . H131 H 0.8006 0.0640 0.1195 0.0750 1.0000 Uiso R . . . . . H143 H 0.9339 -0.0683 0.1264 0.2189 1.0000 Uiso R . . . . . H142 H 0.8756 -0.0333 0.2287 0.2190 1.0000 Uiso R . . . . . H141 H 0.8174 -0.1300 0.2246 0.2189 1.0000 Uiso R . . . . . H151 H 0.8414 0.0036 -0.0114 0.2640 1.0000 Uiso R . . . . . H152 H 0.7724 -0.1002 0.0611 0.2640 1.0000 Uiso R . . . . . H153 H 0.6940 -0.0125 0.0411 0.2640 1.0000 Uiso R . . . . . H161 H 0.3885 -0.2802 0.2993 0.0589 1.0000 Uiso R . . . . . H191 H 0.2466 -0.5312 0.5908 0.1239 1.0000 Uiso R . . . . . H201 H 0.1532 -0.6821 0.6013 0.1611 1.0000 Uiso R . . . . . H211 H 0.0788 -0.6847 0.4776 0.1430 1.0000 Uiso R . . . . . H221 H 0.1080 -0.5515 0.3394 0.1281 1.0000 Uiso R . . . . . H231 H 0.1999 -0.4049 0.3312 0.0922 1.0000 Uiso R . . . . . H261 H 0.6709 0.6129 0.0228 0.0620 1.0000 Uiso R . . . . . H281 H 0.9683 0.5191 -0.1764 0.0727 1.0000 Uiso R . . . . . H301 H 0.5597 0.3789 0.2199 0.0829 1.0000 Uiso R . . . . . H311 H 0.4996 0.4976 0.3126 0.1649 1.0000 Uiso R . . . . . H312 H 0.6444 0.4884 0.2730 0.1649 1.0000 Uiso R . . . . . H313 H 0.5958 0.5776 0.2123 0.1649 1.0000 Uiso R . . . . . H323 H 0.3770 0.4385 0.2213 0.1580 1.0000 Uiso R . . . . . H322 H 0.4491 0.5345 0.1301 0.1580 1.0000 Uiso R . . . . . H321 H 0.4562 0.4324 0.1058 0.1580 1.0000 Uiso R . . . . . H331 H 0.9265 0.2732 -0.0119 0.0833 1.0000 Uiso R . . . . . H341 H 1.1338 0.3068 -0.1380 0.1769 1.0000 Uiso R . . . . . H342 H 1.1070 0.3787 -0.0686 0.1770 1.0000 Uiso R . . . . . H343 H 1.1102 0.4147 -0.1827 0.1770 1.0000 Uiso R . . . . . H353 H 0.9645 0.2410 -0.1702 0.1760 1.0000 Uiso R . . . . . H352 H 0.9390 0.3478 -0.2162 0.1760 1.0000 Uiso R . . . . . H351 H 0.8285 0.2742 -0.1246 0.1760 1.0000 Uiso R . . . . . H361 H 0.7521 0.7734 -0.0832 0.0640 1.0000 Uiso R . . . . . H391 H 0.7265 0.9446 -0.1406 0.0829 1.0000 Uiso R . . . . . H401 H 0.7187 1.1121 -0.1912 0.1079 1.0000 Uiso R . . . . . H411 H 0.8675 1.2082 -0.3490 0.1038 1.0000 Uiso R . . . . . H421 H 1.0190 1.1355 -0.4583 0.1168 1.0000 Uiso R . . . . . H431 H 1.0300 0.9677 -0.4036 0.0959 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 C1 0.060(6) 0.047(6) 0.041(6) -0.013(5) -0.013(5) 0.000(5) C2 0.061(6) 0.048(6) 0.061(6) -0.002(5) -0.047(5) 0.004(5) C3 0.056(6) 0.054(6) 0.067(6) -0.013(6) -0.039(5) 0.002(5) C4 0.040(6) 0.049(6) 0.035(5) -0.003(5) -0.014(5) 0.000(5) C5 0.042(6) 0.045(6) 0.061(6) -0.016(5) -0.019(6) 0.000(5) C6 0.029(5) 0.060(6) 0.064(6) -0.025(6) -0.007(5) 0.007(5) C7 0.044(6) 0.045(6) 0.055(6) -0.009(6) -0.019(6) 0.000(6) C8 0.052(7) 0.046(6) 0.061(6) -0.020(5) -0.021(6) 0.007(5) C9 0.052(6) 0.052(6) 0.047(6) -0.018(6) -0.015(5) 0.010(6) C10 0.047(6) 0.062(6) 0.069(7) -0.018(6) -0.029(5) 0.011(5) C11 0.098(8) 0.091(8) 0.085(8) -0.039(7) -0.052(7) 0.046(6) C12 0.104(8) 0.094(8) 0.094(7) -0.027(7) -0.051(7) 0.059(6) C13 0.062(7) 0.057(6) 0.052(6) -0.018(5) -0.003(6) 0.003(5) C14 0.053(7) 0.198(13) 0.128(10) -0.012(10) 0.001(7) 0.041(8) C15 0.097(10) 0.31(2) 0.100(10) -0.124(12) 0.030(8) -0.045(11) C16 0.053(6) 0.047(6) 0.046(6) -0.012(6) -0.017(5) 0.003(5) C17 0.052(6) 0.044(7) 0.050(6) -0.004(6) -0.015(5) -0.002(5) C18 0.049(6) 0.041(7) 0.058(7) 0.008(6) -0.005(5) 0.001(5) C19 0.126(10) 0.068(8) 0.085(9) -0.026(8) -0.009(7) -0.010(8) C20 0.141(14) 0.079(12) 0.125(14) -0.010(11) -0.007(11) -0.015(9) C21 0.093(10) 0.057(10) 0.155(16) -0.051(11) 0.018(11) -0.022(8) C22 0.085(9) 0.082(9) 0.155(13) -0.066(10) -0.029(9) -0.010(8) C23 0.069(7) 0.065(8) 0.100(9) -0.035(7) -0.033(7) 0.018(6) C24 0.042(6) 0.038(6) 0.060(7) -0.007(6) -0.023(6) -0.004(5) C25 0.037(6) 0.053(6) 0.056(7) -0.013(6) -0.014(5) -0.001(5) C26 0.043(6) 0.040(6) 0.050(6) 0.007(5) -0.010(5) 0.002(4) C27 0.045(6) 0.045(6) 0.044(6) 0.004(6) -0.016(5) -0.010(5) C28 0.053(6) 0.057(6) 0.064(7) -0.023(7) -0.012(5) 0.009(6) C29 0.047(6) 0.054(7) 0.049(6) -0.006(6) -0.013(5) 0.000(5) C30 0.065(7) 0.055(6) 0.071(7) -0.024(6) -0.009(6) 0.014(5) C31 0.103(9) 0.128(10) 0.066(7) -0.033(8) 0.000(6) 0.016(7) C32 0.039(7) 0.131(9) 0.127(10) -0.033(8) -0.017(6) 0.003(6) C33 0.077(8) 0.045(6) 0.067(7) -0.012(6) -0.014(6) 0.015(6) C34 0.082(9) 0.117(9) 0.199(12) -0.083(9) -0.079(9) 0.048(7) C35 0.085(8) 0.137(10) 0.179(11) -0.120(10) -0.057(8) 0.043(7) C36 0.060(6) 0.051(6) 0.058(7) -0.029(7) -0.026(5) 0.022(6) C37 0.048(6) 0.062(7) 0.036(6) -0.003(6) -0.013(5) -0.006(6) C38 0.065(7) 0.028(6) 0.068(7) -0.003(6) -0.030(6) 0.005(6) C39 0.082(8) 0.054(8) 0.068(7) -0.022(7) -0.022(6) 0.005(6) C40 0.099(9) 0.074(9) 0.105(10) -0.027(8) -0.049(9) 0.029(7) C41 0.083(9) 0.057(7) 0.113(10) -0.009(9) -0.043(8) 0.006(8) C42 0.065(8) 0.061(9) 0.123(10) 0.000(8) -0.012(7) -0.006(6) C43 0.063(7) 0.048(7) 0.107(10) -0.013(7) -0.017(7) 0.004(6) N1 0.037(4) 0.046(5) 0.040(4) -0.001(4) -0.012(4) 0.000(4) N2 0.042(4) 0.037(5) 0.065(5) -0.008(4) -0.022(4) -0.003(4) N3 0.058(5) 0.049(6) 0.054(6) -0.009(5) -0.017(5) -0.005(4) N4 0.104(7) 0.075(7) 0.052(6) -0.011(5) -0.005(5) -0.029(5) N5 0.106(7) 0.067(6) 0.050(6) -0.005(5) -0.009(5) -0.031(5) N6 0.042(5) 0.058(6) 0.039(5) -0.011(5) -0.011(4) 0.002(4) N7 0.077(6) 0.044(6) 0.066(6) -0.004(5) -0.019(5) 0.007(4) N8 0.053(5) 0.058(6) 0.071(6) -0.007(5) -0.009(4) 0.005(4) Cl1 0.0699(17) 0.0915(18) 0.0685(16) -0.0322(15) -0.0415(14) 0.0184(14) Ag1 0.0496(5) 0.0522(5) 0.0593(5) -0.0157(4) -0.0275(4) 0.0068(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1446(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 C1 . Ag1 . 2.058(8) yes Cl1 . Ag1 . 2.314(2) yes C1 . N1 . 1.383(8) yes C1 . N2 . 1.348(9) yes C2 . C3 . 1.325(9) yes C2 . N1 . 1.383(8) yes C2 . H21 . 0.945 no C3 . N2 . 1.395(8) yes C3 . H31 . 0.934 no C4 . C5 . 1.397(10) yes C4 . C9 . 1.385(10) yes C4 . N1 . 1.454(9) yes C5 . C6 . 1.366(10) yes C5 . C10 . 1.528(11) yes C6 . C7 . 1.367(10) yes C6 . H61 . 0.926 no C7 . C8 . 1.374(11) yes C7 . N3 . 1.439(10) yes C8 . C9 . 1.397(10) yes C8 . H81 . 0.929 no C9 . C13 . 1.512(11) yes C10 . C11 . 1.510(10) yes C10 . C12 . 1.536(10) yes C10 . H101 . 0.979 no C11 . H111 . 0.959 no C11 . H112 . 0.953 no C11 . H113 . 0.960 no C12 . H123 . 0.965 no C12 . H122 . 0.974 no C12 . H121 . 0.964 no C13 . C14 . 1.520(11) yes C13 . C15 . 1.460(12) yes C13 . H131 . 0.983 no C14 . H143 . 0.959 no C14 . H142 . 0.960 no C14 . H141 . 0.956 no C15 . H151 . 0.962 no C15 . H152 . 0.957 no C15 . H153 . 0.957 no C16 . C17 . 1.342(10) yes C16 . N3 . 1.326(9) yes C16 . H161 . 0.931 no C17 . C18 . 1.480(12) yes C17 . N5 . 1.371(10) yes C18 . C19 . 1.342(11) yes C18 . C23 . 1.368(11) yes C19 . C20 . 1.422(16) yes C19 . H191 . 0.930 no C20 . C21 . 1.341(16) yes C20 . H201 . 0.931 no C21 . C22 . 1.338(15) yes C21 . H211 . 0.933 no C22 . C23 . 1.386(13) yes C22 . H221 . 0.933 no C23 . H231 . 0.927 no C24 . C25 . 1.402(10) yes C24 . C29 . 1.357(10) yes C24 . N2 . 1.451(9) yes C25 . C26 . 1.386(9) yes C25 . C30 . 1.515(11) yes C26 . C27 . 1.355(10) yes C26 . H261 . 0.921 no C27 . C28 . 1.379(10) yes C27 . N6 . 1.447(9) yes C28 . C29 . 1.394(10) yes C28 . H281 . 0.930 no C29 . C33 . 1.555(12) yes C30 . C31 . 1.506(12) yes C30 . C32 . 1.518(11) yes C30 . H301 . 0.981 no C31 . H311 . 0.961 no C31 . H312 . 0.963 no C31 . H313 . 0.971 no C32 . H323 . 0.961 no C32 . H322 . 0.967 no C32 . H321 . 0.970 no C33 . C34 . 1.516(11) yes C33 . C35 . 1.492(12) yes C33 . H331 . 0.972 no C34 . H341 . 0.952 no C34 . H342 . 0.959 no C34 . H343 . 0.961 no C35 . H353 . 0.958 no C35 . H352 . 0.958 no C35 . H351 . 0.959 no C36 . C37 . 1.353(9) yes C36 . N6 . 1.357(9) yes C36 . H361 . 0.935 no C37 . C38 . 1.483(11) yes C37 . N8 . 1.371(10) yes C38 . C39 . 1.350(11) yes C38 . C43 . 1.368(11) yes C39 . C40 . 1.386(11) yes C39 . H391 . 0.925 no C40 . C41 . 1.355(12) yes C40 . H401 . 0.929 no C41 . C42 . 1.354(13) yes C41 . H411 . 0.937 no C42 . C43 . 1.383(11) yes C42 . H421 . 0.933 no C43 . H431 . 0.930 no N3 . N4 . 1.344(9) yes N4 . N5 . 1.311(9) yes N6 . N7 . 1.340(8) yes N7 . N8 . 1.316(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 C1 . Ag1 . Cl1 . 177.2(3) yes N1 . C1 . N2 . 103.0(6) yes N1 . C1 . Ag1 . 129.2(6) yes N2 . C1 . Ag1 . 127.7(6) yes C3 . C2 . N1 . 105.9(7) yes C3 . C2 . H21 . 127.8 no N1 . C2 . H21 . 126.3 no C2 . C3 . N2 . 108.1(7) yes C2 . C3 . H31 . 127.4 no N2 . C3 . H31 . 124.6 no C5 . C4 . C9 . 122.5(8) yes C5 . C4 . N1 . 118.2(8) yes C9 . C4 . N1 . 119.2(8) yes C4 . C5 . C6 . 118.1(9) yes C4 . C5 . C10 . 121.1(8) yes C6 . C5 . C10 . 120.7(8) yes C5 . C6 . C7 . 120.2(8) yes C5 . C6 . H61 . 120.4 no C7 . C6 . H61 . 119.3 no C6 . C7 . C8 . 122.1(8) yes C6 . C7 . N3 . 119.2(8) yes C8 . C7 . N3 . 118.7(9) yes C7 . C8 . C9 . 119.3(8) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.7 no C8 . C9 . C4 . 117.7(8) yes C8 . C9 . C13 . 120.5(9) yes C4 . C9 . C13 . 121.8(8) yes C5 . C10 . C11 . 113.8(7) yes C5 . C10 . C12 . 110.9(7) yes C11 . C10 . C12 . 109.0(7) yes C5 . C10 . H101 . 108.0 no C11 . C10 . H101 . 107.8 no C12 . C10 . H101 . 107.0 no C10 . C11 . H111 . 108.9 no C10 . C11 . H112 . 111.4 no H111 . C11 . H112 . 108.9 no C10 . C11 . H113 . 109.4 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 108.6 no C10 . C12 . H123 . 109.7 no C10 . C12 . H122 . 110.3 no H123 . C12 . H122 . 109.8 no C10 . C12 . H121 . 108.8 no H123 . C12 . H121 . 109.3 no H122 . C12 . H121 . 109.1 no C9 . C13 . C14 . 110.9(7) yes C9 . C13 . C15 . 112.6(8) yes C14 . C13 . C15 . 111.1(10) yes C9 . C13 . H131 . 106.9 no C14 . C13 . H131 . 107.7 no C15 . C13 . H131 . 107.4 no C13 . C14 . H143 . 109.4 no C13 . C14 . H142 . 108.7 no H143 . C14 . H142 . 110.1 no C13 . C14 . H141 . 109.4 no H143 . C14 . H141 . 109.6 no H142 . C14 . H141 . 109.7 no C13 . C15 . H151 . 109.9 no C13 . C15 . H152 . 109.7 no H151 . C15 . H152 . 109.4 no C13 . C15 . H153 . 109.8 no H151 . C15 . H153 . 108.9 no H152 . C15 . H153 . 109.2 no C17 . C16 . N3 . 105.7(7) yes C17 . C16 . H161 . 127.3 no N3 . C16 . H161 . 127.0 no C16 . C17 . C18 . 131.0(10) yes C16 . C17 . N5 . 108.9(8) yes C18 . C17 . N5 . 120.0(9) yes C17 . C18 . C19 . 121.6(10) yes C17 . C18 . C23 . 120.4(9) yes C19 . C18 . C23 . 118.0(10) yes C18 . C19 . C20 . 121.8(12) yes C18 . C19 . H191 . 119.0 no C20 . C19 . H191 . 119.2 no C19 . C20 . C21 . 117.1(14) yes C19 . C20 . H201 . 121.2 no C21 . C20 . H201 . 121.7 no C20 . C21 . C22 . 123.1(15) yes C20 . C21 . H211 . 118.6 no C22 . C21 . H211 . 118.3 no C21 . C22 . C23 . 118.5(13) yes C21 . C22 . H221 . 121.0 no C23 . C22 . H221 . 120.5 no C22 . C23 . C18 . 121.6(10) yes C22 . C23 . H231 . 119.0 no C18 . C23 . H231 . 119.5 no C25 . C24 . C29 . 123.6(8) yes C25 . C24 . N2 . 117.9(8) yes C29 . C24 . N2 . 118.5(8) yes C24 . C25 . C26 . 116.8(8) yes C24 . C25 . C30 . 122.1(8) yes C26 . C25 . C30 . 121.0(8) yes C25 . C26 . C27 . 119.7(8) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 120.5 no C26 . C27 . C28 . 123.1(8) yes C26 . C27 . N6 . 118.7(9) yes C28 . C27 . N6 . 118.0(8) yes C27 . C28 . C29 . 118.3(8) yes C27 . C28 . H281 . 120.9 no C29 . C28 . H281 . 120.8 no C28 . C29 . C24 . 118.3(9) yes C28 . C29 . C33 . 118.4(8) yes C24 . C29 . C33 . 123.2(8) yes C25 . C30 . C31 . 112.7(8) yes C25 . C30 . C32 . 108.9(8) yes C31 . C30 . C32 . 112.3(8) yes C25 . C30 . H301 . 108.7 no C31 . C30 . H301 . 107.9 no C32 . C30 . H301 . 106.1 no C30 . C31 . H311 . 110.3 no C30 . C31 . H312 . 109.9 no H311 . C31 . H312 . 108.3 no C30 . C31 . H313 . 110.2 no H311 . C31 . H313 . 109.9 no H312 . C31 . H313 . 108.2 no C30 . C32 . H323 . 110.3 no C30 . C32 . H322 . 109.5 no H323 . C32 . H322 . 109.7 no C30 . C32 . H321 . 109.3 no H323 . C32 . H321 . 109.3 no H322 . C32 . H321 . 108.8 no C29 . C33 . C34 . 111.5(7) yes C29 . C33 . C35 . 111.8(8) yes C34 . C33 . C35 . 109.5(8) yes C29 . C33 . H331 . 107.3 no C34 . C33 . H331 . 108.3 no C35 . C33 . H331 . 108.5 no C33 . C34 . H341 . 109.4 no C33 . C34 . H342 . 109.2 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 109.9 no H341 . C34 . H343 . 109.1 no H342 . C34 . H343 . 109.8 no C33 . C35 . H353 . 110.7 no C33 . C35 . H352 . 109.1 no H353 . C35 . H352 . 108.6 no C33 . C35 . H351 . 109.7 no H353 . C35 . H351 . 109.7 no H352 . C35 . H351 . 108.9 no C37 . C36 . N6 . 106.2(8) yes C37 . C36 . H361 . 127.9 no N6 . C36 . H361 . 126.0 no C36 . C37 . C38 . 129.8(10) yes C36 . C37 . N8 . 107.7(8) yes C38 . C37 . N8 . 122.5(9) yes C37 . C38 . C39 . 121.1(10) yes C37 . C38 . C43 . 119.1(10) yes C39 . C38 . C43 . 119.8(8) yes C38 . C39 . C40 . 119.7(9) yes C38 . C39 . H391 . 119.5 no C40 . C39 . H391 . 120.8 no C39 . C40 . C41 . 120.4(11) yes C39 . C40 . H401 . 118.5 no C41 . C40 . H401 . 121.1 no C40 . C41 . C42 . 120.2(10) yes C40 . C41 . H411 . 120.0 no C42 . C41 . H411 . 119.8 no C41 . C42 . C43 . 119.6(10) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 120.2 no C42 . C43 . C38 . 120.2(10) yes C42 . C43 . H431 . 120.1 no C38 . C43 . H431 . 119.7 no C4 . N1 . C1 . 123.9(6) yes C4 . N1 . C2 . 124.1(6) yes C1 . N1 . C2 . 111.9(6) yes C24 . N2 . C3 . 125.0(7) yes C24 . N2 . C1 . 123.8(7) yes C3 . N2 . C1 . 111.1(7) yes C7 . N3 . C16 . 130.6(9) yes C7 . N3 . N4 . 118.9(9) yes C16 . N3 . N4 . 110.4(7) yes N3 . N4 . N5 . 107.8(8) yes C17 . N5 . N4 . 107.1(7) yes C27 . N6 . C36 . 131.3(8) yes C27 . N6 . N7 . 119.2(8) yes C36 . N6 . N7 . 109.5(7) yes N6 . N7 . N8 . 108.0(8) yes C37 . N8 . N7 . 108.6(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 07/03/12 at 14:09:21 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 123,X'S) H ( 122,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 143,X'S) H ( 142,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S) RIDE C ( 32,X'S) H ( 323,X'S) H ( 322,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) H ( 343,X'S) RIDE C ( 35,X'S) H ( 353,X'S) H ( 352,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 07/03/12 at 14:09:21 # #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 2 15 10 x . 1 1 3 x . -1 1 2 x . _chemical_name_common ;(N,N?-bis(4-azido-2,6-diisopropylphenyl)imidazol-2- ylidene)chlorosilver(i) ; data_1c _database_code_depnum_ccdc_archive 'CCDC 864598' #TrackingRef '- 864598-22-reorder.cif.txt' # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; _chemical_formula_moiety 'C27 H34 Au1 Cl1 N8' # Given Formula = C27 H34 Au1 Cl1 N7 # Dc = 1.40 Fooo = 1392.00 Mu = 45.21 M = 703.04 # Found Formula = C27 H34 Au1 Cl1 N7 # Dc = 1.40 FOOO = 1392.00 Mu = 45.21 M = 703.04 _chemical_formula_sum 'C27 H34 Au1 Cl1 N8' _chemical_formula_weight 703.04 # 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 . _chemical_compound_source ? 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z 3 -x+1/2,y+1/2,-z+1/2 4 x+1/2,-y+1/2,z+1/2 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 9.9292(3) _cell_length_b 15.3418(5) _cell_length_c 21.8821(7) _cell_angle_alpha 90 _cell_angle_beta 90.9950(10) _cell_angle_gamma 90 _cell_volume 3332.84(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 0 _cell_measurement_temperature 293 _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _exptl_absorpt_coefficient_mu 4.521 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 1.0000 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle # Non-dispersive F(000): _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.433 _exptl_crystal_size_mid 0.087 _exptl_crystal_size_min 0.044 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 29646 _diffrn_reflns_theta_full 26.733 _diffrn_reflns_theta_max 28.140 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 7943 # Theoretical number of reflections is about 16209 _diffrn_reflns_theta_min 1.621 _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device Serial _diffrn_measurement_device_type Unknown _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_decay_% ? _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_number 0 _reflns_limit_h_max 13 _reflns_limit_h_min -13 _reflns_limit_k_max 19 _reflns_limit_k_min 0 _reflns_limit_l_max 28 _reflns_limit_l_min 0 _reflns_number_gt 5136 _reflns_number_total 7943 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _refine_diff_density_max 3.06 _refine_diff_density_min -0.70 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9989 _refine_ls_hydrogen_treatment none # none, undef, noref, refall, _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 4341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0598 _refine_ls_shift/su_max 0.0013079 _refine_ls_shift/su_mean 0.0000172 _refine_ls_structure_factor_coef F _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: 0.872 1.08 0.834 0.343 0.195 ; # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0832 _refine_ls_wR_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.0539 _refine_special_details ; ? ; # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct #heavy,direct,difmap,geom # 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 H2 H 0.2490 0.7755 0.6467 0.0620 1.0000 Uiso R . . . . . H3 H 0.2735 0.6737 0.7338 0.0630 1.0000 Uiso R . . . . . H6 H -0.1235 0.8064 0.4699 0.0790 1.0000 Uiso R . . . . . H8 H -0.1242 1.0082 0.5839 0.0710 1.0000 Uiso R . . . . . H10 H 0.0410 0.6594 0.5748 0.0960 1.0000 Uiso R . . . . . H11A H 0.0911 0.6157 0.4687 0.2420 1.0000 Uiso R . . . . . H11B H 0.1670 0.7006 0.4897 0.2420 1.0000 Uiso R . . . . . H11C H 0.0364 0.7073 0.4487 0.2420 1.0000 Uiso R . . . . . H12A H -0.1161 0.5691 0.5257 0.1970 1.0000 Uiso R . . . . . H12B H -0.1902 0.6339 0.5694 0.1970 1.0000 Uiso R . . . . . H12C H -0.1899 0.6516 0.4988 0.1970 1.0000 Uiso R . . . . . H13 H 0.0310 0.8981 0.7101 0.0720 1.0000 Uiso R . . . . . H14A H 0.1131 1.0385 0.7192 0.1390 1.0000 Uiso R . . . . . H14B H 0.0427 1.0655 0.6576 0.1390 1.0000 Uiso R . . . . . H14C H 0.1639 0.9997 0.6577 0.1390 1.0000 Uiso R . . . . . H15A H -0.1204 0.9828 0.7587 0.1409 1.0000 Uiso R . . . . . H15B H -0.1727 1.0223 0.6971 0.1410 1.0000 Uiso R . . . . . H15C H -0.2062 0.9257 0.7137 0.1410 1.0000 Uiso R . . . . . H18 H 0.0010 0.4052 0.8105 0.0691 1.0000 Uiso R . . . . . H20 H -0.0394 0.6076 0.9241 0.0711 1.0000 Uiso R . . . . . H22 H 0.0931 0.5337 0.6810 0.0791 1.0000 Uiso R . . . . . H23A H 0.1593 0.3863 0.6630 0.1480 1.0000 Uiso R . . . . . H23B H 0.2339 0.4227 0.7213 0.1480 1.0000 Uiso R . . . . . H23C H 0.1093 0.3610 0.7283 0.1481 1.0000 Uiso R . . . . . H24A H -0.1100 0.4088 0.6934 0.1470 1.0000 Uiso R . . . . . H24B H -0.1436 0.5078 0.6837 0.1470 1.0000 Uiso R . . . . . H24C H -0.0710 0.4551 0.6322 0.1470 1.0000 Uiso R . . . . . H25 H 0.0260 0.7743 0.8150 0.0890 1.0000 Uiso R . . . . . H26A H 0.1466 0.8238 0.8972 0.1329 1.0000 Uiso R . . . . . H26B H 0.0950 0.7494 0.9396 0.1329 1.0000 Uiso R . . . . . H26C H 0.2003 0.7292 0.8894 0.1330 1.0000 Uiso R . . . . . H27A H -0.1199 0.8305 0.8887 0.1639 1.0000 Uiso R . . . . . H27B H -0.1461 0.7345 0.9099 0.1640 1.0000 Uiso R . . . . . H27C H -0.1943 0.7654 0.8447 0.1640 1.0000 Uiso R . . . . . C1 C -0.0279(7) 0.7126(5) 0.6976(3) 0.0426 1.0000 Uani . . . . . . C2 C 0.1803(7) 0.7493(6) 0.6681(4) 0.0513 1.0000 Uani . . . . . . C3 C 0.1941(7) 0.6929(6) 0.7154(4) 0.0543 1.0000 Uani . . . . . . C4 C -0.0147(7) 0.8148(5) 0.6103(3) 0.0444 1.0000 Uani . . . . . . C5 C -0.0426(9) 0.7753(6) 0.5534(4) 0.0567 1.0000 Uani . . . . . . C6 C -0.1036(10) 0.8291(7) 0.5085(4) 0.0656 1.0000 Uani . . . . . . C7 C -0.1334(9) 0.9130(7) 0.5208(4) 0.0615 1.0000 Uani . . . . . . C8 C -0.1043(9) 0.9499(6) 0.5770(4) 0.0581 1.0000 Uani . . . . . . C9 C -0.0443(7) 0.9009(5) 0.6228(4) 0.0458 1.0000 Uani . . . . . . C10 C -0.0106(13) 0.6829(8) 0.5401(5) 0.0786 1.0000 Uani . . . . . . C11 C 0.080(3) 0.6753(14) 0.4812(10) 0.1892 1.0000 Uani . . . . . . C12 C -0.139(2) 0.6291(11) 0.5329(10) 0.1398 1.0000 Uani . . . . . . C13 C -0.0119(9) 0.9426(6) 0.6846(4) 0.0567 1.0000 Uani . . . . . . C14 C 0.0859(14) 1.0187(10) 0.6795(6) 0.0955 1.0000 Uani . . . . . . C15 C -0.1393(13) 0.9706(11) 0.7166(6) 0.1025 1.0000 Uani . . . . . . C16 C 0.0338(7) 0.6115(5) 0.7814(4) 0.0430 1.0000 Uani . . . . . . C17 C 0.0301(7) 0.5209(5) 0.7687(4) 0.0483 1.0000 Uani . . . . . . C18 C 0.0024(8) 0.4653(6) 0.8173(4) 0.0556 1.0000 Uani . . . . . . C19 C -0.0217(8) 0.4980(6) 0.8745(4) 0.0512 1.0000 Uani . . . . . . C20 C -0.0194(9) 0.5865(6) 0.8853(4) 0.0574 1.0000 Uani . . . . . . C21 C 0.0084(8) 0.6458(6) 0.8390(4) 0.0507 1.0000 Uani . . . . . . C22 C 0.0532(10) 0.4867(6) 0.7048(5) 0.0604 1.0000 Uani . . . . . . C23 C 0.1481(15) 0.4065(9) 0.7041(6) 0.0983 1.0000 Uani . . . . . . C24 C -0.0799(14) 0.4623(11) 0.6756(6) 0.0979 1.0000 Uani . . . . . . C25 C 0.0103(11) 0.7420(7) 0.8529(5) 0.0691 1.0000 Uani . . . . . . C26 C 0.1232(14) 0.7635(8) 0.8990(6) 0.0902 1.0000 Uani . . . . . . C27 C -0.1251(16) 0.7710(9) 0.8754(8) 0.1109 1.0000 Uani . . . . . . N1 N 0.0432(6) 0.7611(4) 0.6576(3) 0.0442 1.0000 Uani . . . . . . N2 N 0.0644(6) 0.6707(4) 0.7323(3) 0.0439 1.0000 Uani . . . . . . N3 N -0.1999(10) 0.9585(8) 0.4722(4) 0.0810 1.0000 Uani . . . . . . N4 N -0.2251(9) 1.0350(10) 0.4799(5) 0.0860 1.0000 Uani . . . . . . N5 N -0.2550(12) 1.1061(10) 0.4802(6) 0.1099 1.0000 Uani . . . . . . N6 N -0.0531(10) 0.4467(6) 0.9274(4) 0.0722 1.0000 Uani . . . . . . N7 N -0.0555(11) 0.3685(7) 0.9213(4) 0.0809 1.0000 Uani . . . . . . N8 N -0.064(2) 0.2970(9) 0.9251(6) 0.1330 1.0000 Uani . . . . . . Cl1 Cl -0.4528(2) 0.71549(19) 0.72127(16) 0.0821 1.0000 Uani . . . . . . Au1 Au -0.22636(3) 0.71205(2) 0.707014(15) 0.0489 1.0000 Uani . . . . . . 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 C1 0.035(3) 0.045(4) 0.048(4) -0.007(4) -0.002(3) 0.003(3) C2 0.030(3) 0.063(5) 0.061(5) -0.008(4) 0.008(3) -0.007(3) C3 0.029(3) 0.062(5) 0.072(6) 0.001(4) -0.001(3) 0.001(3) C4 0.039(3) 0.054(4) 0.040(4) 0.001(3) 0.003(3) -0.004(3) C5 0.061(5) 0.062(6) 0.047(5) -0.008(4) -0.003(4) -0.005(4) C6 0.071(6) 0.077(7) 0.048(5) -0.002(5) -0.005(4) -0.020(5) C7 0.052(4) 0.080(7) 0.052(5) 0.018(5) -0.007(4) -0.017(4) C8 0.057(5) 0.056(5) 0.061(5) 0.009(4) -0.004(4) -0.002(4) C9 0.042(4) 0.053(4) 0.043(4) 0.001(3) -0.002(3) -0.005(3) C10 0.094(8) 0.076(7) 0.065(6) -0.028(5) -0.008(5) 0.004(6) C11 0.30(3) 0.109(13) 0.167(19) -0.042(13) 0.13(2) 0.011(16) C12 0.151(15) 0.085(10) 0.182(17) -0.001(11) -0.048(13) -0.030(11) C13 0.057(5) 0.058(5) 0.056(5) -0.003(4) -0.005(4) 0.001(4) C14 0.095(8) 0.113(10) 0.078(8) -0.028(7) -0.008(6) -0.039(8) C15 0.082(8) 0.137(12) 0.089(9) -0.045(8) 0.010(6) -0.013(8) C16 0.032(3) 0.041(4) 0.055(5) 0.007(3) -0.009(3) 0.006(3) C17 0.039(3) 0.049(4) 0.056(5) -0.002(4) -0.003(3) -0.002(3) C18 0.047(4) 0.050(5) 0.069(6) -0.003(4) -0.010(4) -0.003(4) C19 0.049(4) 0.054(5) 0.050(5) 0.003(4) -0.004(3) -0.002(4) C20 0.065(5) 0.066(6) 0.041(4) -0.003(4) -0.006(4) -0.008(4) C21 0.051(4) 0.052(5) 0.049(4) -0.008(4) -0.010(3) 0.002(4) C22 0.066(5) 0.043(4) 0.073(6) -0.006(4) 0.009(4) 0.004(4) C23 0.107(9) 0.090(9) 0.098(9) -0.031(7) 0.015(7) 0.027(7) C24 0.099(9) 0.125(11) 0.069(7) -0.036(7) -0.022(6) 0.017(8) C25 0.085(7) 0.060(6) 0.062(6) -0.009(5) -0.014(5) 0.004(5) C26 0.105(9) 0.067(7) 0.097(8) -0.007(6) -0.028(7) -0.022(6) C27 0.111(10) 0.080(9) 0.142(13) -0.037(9) 0.019(9) 0.022(7) N1 0.033(3) 0.047(3) 0.052(4) -0.003(3) 0.000(2) -0.005(2) N2 0.032(3) 0.050(4) 0.049(4) -0.003(3) -0.002(2) 0.002(2) N3 0.087(6) 0.094(7) 0.061(5) 0.025(5) -0.023(4) -0.013(6) N4 0.058(5) 0.111(9) 0.088(7) 0.047(7) -0.016(4) -0.014(6) N5 0.088(7) 0.110(10) 0.131(10) 0.049(8) -0.003(7) 0.004(7) N6 0.088(6) 0.073(6) 0.056(5) 0.007(4) -0.004(4) -0.006(5) N7 0.107(7) 0.070(7) 0.066(5) 0.007(5) -0.002(5) -0.019(5) N8 0.233(18) 0.074(8) 0.093(8) 0.013(7) 0.023(9) -0.007(9) Cl1 0.0347(9) 0.0771(15) 0.135(2) 0.0207(17) 0.0089(11) 0.0000(11) Au1 0.03227(14) 0.04983(17) 0.0644(2) 0.00425(19) -0.00174(10) -0.00028(14) 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 Au1 . C1 . 1.985(7) yes Au1 . Cl1 . 2.276(2) yes C1 . N1 . 1.356(10) yes C1 . N2 . 1.343(9) yes C2 . H2 . 0.927 no C2 . N1 . 1.389(9) yes C3 . H3 . 0.927 no C3 . C2 . 1.354(13) yes C4 . C5 . 1.407(12) yes C4 . C9 . 1.382(11) yes C5 . C6 . 1.411(14) yes C5 . C10 . 1.482(15) yes C6 . H6 . 0.932 no C6 . C7 . 1.349(15) yes C7 . C8 . 1.380(14) yes C7 . N3 . 1.426(13) yes C8 . H8 . 0.929 no C8 . C9 . 1.379(12) yes C9 . C13 . 1.526(12) yes C10 . H10 . 0.976 no C10 . C11 . 1.59(2) yes C10 . C12 . 1.53(2) yes C11 . H11A . 0.960 no C11 . H11B . 0.960 no C11 . H11C . 0.962 no C12 . H12A . 0.961 no C12 . H12B . 0.957 no C12 . H12C . 0.958 no C13 . H13 . 0.976 no C13 . C14 . 1.523(15) yes C13 . C15 . 1.518(15) yes C14 . H14A . 0.956 no C14 . H14B . 0.960 no C14 . H14C . 0.960 no C15 . H15A . 0.956 no C15 . H15B . 0.958 no C15 . H15C . 0.959 no C16 . C17 . 1.417(11) yes C16 . C21 . 1.393(11) yes C17 . C18 . 1.395(12) yes C17 . C22 . 1.514(13) yes C18 . H18 . 0.933 no C18 . C19 . 1.374(13) yes C19 . C20 . 1.378(13) yes C19 . N6 . 1.438(12) yes C20 . H20 . 0.933 no C20 . C21 . 1.394(13) yes C21 . C25 . 1.507(14) yes C22 . H22 . 0.978 no C22 . C23 . 1.551(15) yes C22 . C24 . 1.506(16) yes C23 . H23A . 0.960 no C23 . H23B . 0.958 no C23 . H23C . 0.962 no C24 . H24A . 0.958 no C24 . H24B . 0.960 no C24 . H24C . 0.961 no C25 . H25 . 0.980 no C25 . C26 . 1.532(15) yes C25 . C27 . 1.508(18) yes C26 . H26A . 0.955 no C26 . H26B . 0.959 no C26 . H26C . 0.957 no C27 . H27A . 0.958 no C27 . H27B . 0.965 no C27 . H27C . 0.957 no N1 . C4 . 1.436(10) yes N2 . C3 . 1.388(9) yes N2 . C16 . 1.444(10) yes N3 . N4 . 1.213(16) yes N4 . N5 . 1.131(17) yes N6 . N7 . 1.207(13) yes N7 . N8 . 1.103(15) 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 Cl1 . Au1 . C1 . 177.5(2) yes N2 . C1 . N1 . 105.7(6) yes Au1 . C1 . N1 . 126.7(5) yes Au1 . C1 . N2 . 127.4(6) yes C3 . C2 . H2 . 126.8 no C3 . C2 . N1 . 107.2(7) yes N1 . C2 . H2 . 126.0 no C2 . C3 . H3 . 127.5 no N2 . C3 . H3 . 126.4 no N2 . C3 . C2 . 106.1(7) yes C5 . C4 . C9 . 123.2(8) yes N1 . C4 . C5 . 117.4(7) yes N1 . C4 . C9 . 119.3(7) yes C4 . C5 . C6 . 116.0(9) yes C4 . C5 . C10 . 123.0(9) yes C6 . C5 . C10 . 120.9(9) yes C5 . C6 . H6 . 119.6 no C5 . C6 . C7 . 120.8(9) yes C7 . C6 . H6 . 119.6 no C6 . C7 . C8 . 121.8(9) yes C6 . C7 . N3 . 114.7(10) yes N3 . C7 . C8 . 123.5(10) yes C7 . C8 . H8 . 119.9 no C7 . C8 . C9 . 120.3(9) yes C9 . C8 . H8 . 119.8 no C4 . C9 . C8 . 117.9(8) yes C4 . C9 . C13 . 122.3(7) yes C8 . C9 . C13 . 119.8(8) yes C5 . C10 . H10 . 108.2 no C5 . C10 . C11 . 110.8(12) yes C5 . C10 . C12 . 110.9(12) yes C11 . C10 . H10 . 107.8 no C12 . C10 . H10 . 107.9 no C12 . C10 . C11 . 111.1(15) yes H11A . C11 . H11B . 109.5 no H11A . C11 . H11C . 109.1 no H11B . C11 . H11C . 109.2 no C10 . C11 . H11A . 111.7 no C10 . C11 . H11B . 109.4 no C10 . C11 . H11C . 107.8 no H12A . C12 . H12B . 109.9 no H12A . C12 . H12C . 110.0 no H12B . C12 . H12C . 109.9 no C10 . C12 . H12A . 109.6 no C10 . C12 . H12B . 109.0 no C10 . C12 . H12C . 108.3 no C9 . C13 . H13 . 107.2 no C9 . C13 . C14 . 112.3(8) yes C9 . C13 . C15 . 111.2(8) yes C14 . C13 . H13 . 107.9 no C14 . C13 . C15 . 110.8(10) yes C15 . C13 . H13 . 107.1 no H14A . C14 . H14B . 109.4 no H14A . C14 . H14C . 109.3 no H14B . C14 . H14C . 109.7 no C13 . C14 . H14A . 110.2 no C13 . C14 . H14B . 109.3 no C13 . C14 . H14C . 109.0 no H15A . C15 . H15B . 109.0 no H15A . C15 . H15C . 109.2 no H15B . C15 . H15C . 109.4 no C13 . C15 . H15A . 110.4 no C13 . C15 . H15B . 108.3 no C13 . C15 . H15C . 110.5 no C17 . C16 . C21 . 122.9(8) yes N2 . C16 . C17 . 118.4(7) yes N2 . C16 . C21 . 118.7(7) yes C16 . C17 . C18 . 117.1(8) yes C16 . C17 . C22 . 121.2(8) yes C18 . C17 . C22 . 121.8(8) yes C17 . C18 . H18 . 119.1 no C17 . C18 . C19 . 120.7(8) yes C19 . C18 . H18 . 120.2 no C18 . C19 . C20 . 121.0(8) yes C18 . C19 . N6 . 125.2(8) yes N6 . C19 . C20 . 113.8(8) yes C19 . C20 . H20 . 119.7 no C19 . C20 . C21 . 121.4(8) yes C21 . C20 . H20 . 118.8 no C16 . C21 . C25 . 123.4(8) yes C20 . C21 . C16 . 116.9(8) yes C20 . C21 . C25 . 119.7(8) yes C17 . C22 . H22 . 107.8 no C17 . C22 . C23 . 112.7(9) yes C17 . C22 . C24 . 109.5(8) yes C23 . C22 . H22 . 109.1 no C23 . C22 . C24 . 109.1(10) yes C24 . C22 . H22 . 108.5 no H23A . C23 . H23B . 109.6 no H23A . C23 . H23C . 109.7 no H23B . C23 . H23C . 109.5 no C22 . C23 . H23A . 110.2 no C22 . C23 . H23B . 109.1 no C22 . C23 . H23C . 108.8 no H24B . C24 . H24A . 109.6 no H24C . C24 . H24A . 109.7 no H24C . C24 . H24B . 109.8 no C22 . C24 . H24A . 108.5 no C22 . C24 . H24B . 108.4 no C22 . C24 . H24C . 110.7 no C21 . C25 . H25 . 109.1 no C21 . C25 . C26 . 110.6(9) yes C21 . C25 . C27 . 110.3(10) yes C26 . C25 . H25 . 108.9 no C26 . C25 . C27 . 111.5(11) yes C27 . C25 . H25 . 106.4 no H26A . C26 . H26B . 109.4 no H26A . C26 . H26C . 109.2 no H26B . C26 . H26C . 109.0 no C25 . C26 . H26A . 111.0 no C25 . C26 . H26B . 109.8 no C25 . C26 . H26C . 108.4 no H27A . C27 . H27B . 109.0 no H27A . C27 . H27C . 109.4 no H27B . C27 . H27C . 109.6 no C25 . C27 . H27A . 109.6 no C25 . C27 . H27B . 106.9 no C25 . C27 . H27C . 112.2 no C1 . N1 . C4 . 125.1(6) yes C2 . N1 . C1 . 109.9(7) yes C2 . N1 . C4 . 125.0(7) yes C1 . N2 . C3 . 111.1(7) yes C1 . N2 . C16 . 124.9(6) yes C16 . N2 . C3 . 124.1(6) yes C7 . N3 . N4 . 117.6(10) yes N3 . N4 . N5 . 171.6(13) yes C19 . N6 . N7 . 117.4(9) yes N6 . N7 . N8 . 168.9(13) yes _iucr_refine_instruction_details_constraints ; # # Punched on 17/03/11 at 23:21:08 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 2,X'S) RIDE C ( 3,X'S) H ( 3,X'S) RIDE C ( 6,X'S) H ( 6,X'S) RIDE C ( 8,X'S) H ( 8,X'S) RIDE C ( 18,X'S) H ( 18,X'S) RIDE C ( 20,X'S) H ( 20,X'S) RIDE C ( 10,X'S) H ( 10,X'S) RIDE C ( 13,X'S) H ( 13,X'S) RIDE C ( 22,X'S) H ( 22,X'S) RIDE C ( 25,X'S) H ( 25,X'S) RIDE C ( 11,X'S) H ( 11A,X'S) H ( 11B,X'S) H ( 11C,X'S) RIDE C ( 12,X'S) H ( 12A,X'S) H ( 12B,X'S) H ( 12C,X'S) RIDE C ( 14,X'S) H ( 14A,X'S) H ( 14B,X'S) H ( 14C,X'S) RIDE C ( 15,X'S) H ( 15A,X'S) H ( 15B,X'S) H ( 15C,X'S) RIDE C ( 23,X'S) H ( 23A,X'S) H ( 23B,X'S) H ( 23C,X'S) RIDE C ( 24,X'S) H ( 24A,X'S) H ( 24B,X'S) H ( 24C,X'S) RIDE C ( 26,X'S) H ( 26A,X'S) H ( 26B,X'S) H ( 26C,X'S) RIDE C ( 27,X'S) H ( 27A,X'S) H ( 27B,X'S) H ( 27C,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 17/03/11 at 23:21:08 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _oxford_diffrn_Wilson_B_factor 3.47 _oxford_diffrn_Wilson_scale 202.82 _oxford_refine_ls_R_factor_ref 0.0531 _oxford_refine_ls_scale 0.07651(15) # The values computed from all data _oxford_reflns_number_all 7921 # 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>4.0\s(I) _chemical_name_common ;(N,N?-bis(4-azido-2,6-diisopropylphenyl)imidazol-2- ylidene)chlorosilver(i) ;