#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/44/2204445.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204445 loop_ _publ_author_name 'N\"ather, Christian' 'Beck, Andreas' _publ_section_title ; Chlorotris(3-methylpyridine-\kN)silver(I) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1678 _journal_page_last m1680 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Ag Cl (C6 H7 N)3]' _chemical_formula_moiety 'C18 H21 Ag Cl N3' _chemical_formula_sum 'C18 H21 Ag Cl N3' _chemical_formula_weight 422.70 _chemical_name_systematic ; Chlorotris(3-methylpyridine-\kN)silver(I) ; _space_group_IT_number 160 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'R 3 -2"' _symmetry_space_group_name_H-M 'R 3 m :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 14.6795(10) _cell_length_b 14.6795(10) _cell_length_c 7.5114(4) _cell_measurement_reflns_used 4495 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 28 _cell_measurement_theta_min 3 _cell_volume 1401.76(15) _computing_cell_refinement 'IPDS Program Package' _computing_data_collection 'IPDS Program Package (Stoe & Cie, 1998)' _computing_data_reduction 'IPDS Program Package' _computing_molecular_graphics 'XP in SHELXTL (Bruker, 1998)' _computing_publication_material 'CIFTAB in SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997' _diffrn_ambient_temperature 170(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3908 _diffrn_reflns_theta_full 28.03 _diffrn_reflns_theta_max 28.03 _diffrn_reflns_theta_min 2.78 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1998)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 642 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.703 _refine_diff_density_min -0.556 _refine_ls_abs_structure_details 'Flack (1983), 397 Friedel reflections' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_extinction_coef 0.0105(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 51 _refine_ls_number_reflns 823 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0285 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.7193P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.0683 _reflns_number_gt 811 _reflns_number_total 823 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6543.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'R 3 m' _[local]_cod_cif_authors_sg_Hall 'R3 -2"' _cod_database_code 2204445 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Ag1 1.0000 0.0000 0.9994 0.0302(2) Uani d S 1 Ag Cl1 1.0000 0.0000 1.3464(2) 0.0274(4) Uani d S 1 Cl N1 0.91274(14) 0.08726(14) 0.9158(5) 0.0299(8) Uani d S 1 N C1 0.89529(19) 0.10471(19) 0.7493(7) 0.0316(9) Uani d S 1 C H1 0.9205 0.0795 0.6560 0.038 Uiso calc SR 1 H C2 0.8417(2) 0.1583(2) 0.7022(8) 0.0341(12) Uani d S 1 C C3 0.8058(2) 0.1942(2) 0.8388(8) 0.0414(12) Uani d S 1 C H3 0.7691 0.2309 0.8137 0.050 Uiso calc SR 1 H C4 0.8233(2) 0.1767(2) 1.0140(8) 0.0474(17) Uani d S 1 C H4 0.7990 0.2010 1.1101 0.057 Uiso calc SR 1 H C5 0.8774(2) 0.1226(2) 1.0457(7) 0.0386(11) Uani d S 1 C H5 0.8894 0.1106 1.1655 0.046 Uiso calc SR 1 H C6 0.8263(3) 0.1737(3) 0.5095(9) 0.0535(18) Uani d S 1 C H6A 0.7731 0.1950 0.4986 0.080 Uiso calc PR 0.50 H H6B 0.8029 0.1076 0.4450 0.080 Uiso calc PR 0.50 H H6C 0.8929 0.2285 0.4591 0.080 Uiso calc PR 0.50 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag1 0.0269(2) 0.0269(2) 0.0368(4) 0.01343(11) 0.000 0.000 Cl1 0.0282(6) 0.0282(6) 0.0259(10) 0.0141(3) 0.000 0.000 N1 0.0328(14) 0.0328(14) 0.029(2) 0.0203(16) -0.0007(7) 0.0007(7) C1 0.0367(18) 0.0367(18) 0.028(2) 0.023(2) 0.0011(9) -0.0011(9) C2 0.040(2) 0.040(2) 0.025(4) 0.022(2) -0.0018(12) 0.0018(12) C3 0.051(2) 0.051(2) 0.042(3) 0.040(3) -0.0017(10) 0.0017(10) C4 0.069(3) 0.069(3) 0.035(3) 0.056(4) 0.0043(10) -0.0043(10) C5 0.051(2) 0.051(2) 0.028(3) 0.037(3) -0.0005(9) 0.0005(9) C6 0.069(4) 0.069(4) 0.038(4) 0.045(4) -0.0048(14) 0.0048(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 N1 2_645 2.306(4) y Ag1 N1 3_765 2.306(4) n Ag1 N1 . 2.306(4) n Ag1 Cl1 . 2.6066(18) y N1 C5 . 1.327(6) y N1 C1 . 1.327(6) y C1 C2 . 1.409(7) y C1 H1 . 0.9500 n C2 C3 . 1.373(9) y C2 C6 . 1.499(9) y C3 C4 . 1.389(9) y C3 H3 . 0.9500 n C4 C5 . 1.395(7) n C4 H4 . 0.9500 n C5 H5 . 0.9500 n C6 H6A . 0.9800 n C6 H6B . 0.9800 n C6 H6C . 0.9800 n loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ag1 N1 2_645 3_765 112.88(8) y N1 Ag1 N1 2_645 . 112.88(8) n N1 Ag1 N1 3_765 . 112.88(8) n N1 Ag1 Cl1 2_645 . 105.80(10) y N1 Ag1 Cl1 3_765 . 105.80(10) n N1 Ag1 Cl1 . . 105.80(10) n C5 N1 C1 . . 117.8(4) y C5 N1 Ag1 . . 116.9(3) y C1 N1 Ag1 . . 125.3(3) y N1 C1 C2 . . 124.1(5) y N1 C1 H1 . . 118.0 n C2 C1 H1 . . 118.0 n C3 C2 C1 . . 117.1(5) y C3 C2 C6 . . 123.3(5) y C1 C2 C6 . . 119.6(6) y C2 C3 C4 . . 119.6(5) y C2 C3 H3 . . 120.2 n C4 C3 H3 . . 120.2 n C3 C4 C5 . . 118.5(5) y C3 C4 H4 . . 120.7 n C5 C4 H4 . . 120.7 n N1 C5 C4 . . 122.8(5) y N1 C5 H5 . . 118.6 n C4 C5 H5 . . 118.6 n C2 C6 H6A . . 109.5 y C2 C6 H6B . . 109.5 y H6A C6 H6B . . 109.5 y C2 C6 H6C . . 109.5 y H6A C6 H6C . . 109.5 y H6B C6 H6C . . 109.5 y _cod_database_fobs_code 2204445