#------------------------------------------------------------------------------ #$Date: 2014-10-25 20:23:10 +0300 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/51/2105142.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_2105142 loop_ _publ_author_name 'Liu, Jianguo' 'Zeng, Xiaoyan' 'Li, Hua' _publ_section_title ; Synthesis, structure and spectroscopic properties of a novel compound bis(benzylamino)silver(I) benzylcarbamate ; _journal_coeditor_code BP5042 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 401 _journal_page_last 406 _journal_volume 68 _journal_year 2012 _chemical_formula_sum 'C22 H26 Ag N3 O2' _chemical_formula_weight 472.33 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 68.729(2) _cell_angle_beta 83.507(2) _cell_angle_gamma 85.412(2) _cell_formula_units_Z 2 _cell_length_a 5.2006(5) _cell_length_b 14.6298(15) _cell_length_c 14.7246(15) _cell_measurement_reflns_used 328 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.0301 _cell_measurement_theta_min 2.4595 _cell_volume 1036.37(18) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type Bruker _diffrn_measurement_method Semisphere _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 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 6094 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.46 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_T_max 0.7820 _exptl_absorpt_correction_T_min 0.7414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 484 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.327 _refine_diff_density_min -0.511 _refine_ls_extinction_coef 0.0129(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 4009 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0267 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.2277P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0675 _reflns_number_gt 3622 _reflns_number_total 4009 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bp5042.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius ; _cod_database_code 2105142 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _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_symmetry_multiplicity Ag Ag1 0.53362(3) 0.873586(12) 0.034393(13) 0.04639(9) Uani d . 1 1 C C1 0.1886(4) 0.80409(18) -0.09264(18) 0.0475(5) Uani d . 1 1 H H1A 0.0677 0.8262 -0.1426 0.057 Uiso calc R 1 1 H H1B 0.1020 0.7581 -0.0339 0.057 Uiso calc R 1 1 C C2 0.4212(5) 0.75304(17) -0.12702(17) 0.0462(5) Uani d . 1 1 C C3 0.5345(6) 0.7933(2) -0.2216(2) 0.0594(7) Uani d . 1 1 H H3 0.4632 0.8511 -0.2644 0.071 Uiso calc R 1 1 C C4 0.7522(6) 0.7489(3) -0.2537(3) 0.0741(9) Uani d . 1 1 H H4 0.8270 0.7770 -0.3175 0.089 Uiso calc R 1 1 C C5 0.8568(6) 0.6642(3) -0.1918(3) 0.0804(10) Uani d . 1 1 H H5 1.0030 0.6342 -0.2133 0.096 Uiso calc R 1 1 C C6 0.7476(7) 0.6233(2) -0.0984(3) 0.0844(11) Uani d . 1 1 H H6 0.8197 0.5653 -0.0564 0.101 Uiso calc R 1 1 C C7 0.5290(6) 0.6676(2) -0.0653(2) 0.0652(7) Uani d . 1 1 H H7 0.4559 0.6393 -0.0013 0.078 Uiso calc R 1 1 C C8 0.9235(5) 0.75033(17) 0.19255(18) 0.0478(5) Uani d . 1 1 H H8A 1.0005 0.7503 0.2496 0.057 Uiso calc R 1 1 H H8B 1.0617 0.7389 0.1473 0.057 Uiso calc R 1 1 C C9 0.7383(4) 0.66834(16) 0.22339(16) 0.0429(5) Uani d . 1 1 C C10 0.7522(5) 0.60312(19) 0.17517(19) 0.0550(6) Uani d . 1 1 H H10 0.8791 0.6092 0.1237 0.066 Uiso calc R 1 1 C C11 0.5795(6) 0.5284(2) 0.2022(2) 0.0629(7) Uani d . 1 1 H H11 0.5909 0.4849 0.1687 0.075 Uiso calc R 1 1 C C12 0.3928(5) 0.51837(19) 0.2778(2) 0.0613(7) Uani d . 1 1 H H12 0.2765 0.4684 0.2959 0.074 Uiso calc R 1 1 C C13 0.3778(5) 0.5821(2) 0.3268(2) 0.0646(7) Uani d . 1 1 H H13 0.2518 0.5752 0.3787 0.078 Uiso calc R 1 1 C C14 0.5484(5) 0.6568(2) 0.2999(2) 0.0561(6) Uani d . 1 1 H H14 0.5356 0.7000 0.3337 0.067 Uiso calc R 1 1 C C15 1.0662(5) 0.2159(2) 0.56050(19) 0.0591(7) Uani d . 1 1 H H15 1.1947 0.1949 0.6036 0.071 Uiso calc R 1 1 C C16 1.0397(6) 0.3139(2) 0.5046(2) 0.0688(8) Uani d . 1 1 H H16 1.1494 0.3583 0.5104 0.083 Uiso calc R 1 1 C C17 0.8519(6) 0.3464(2) 0.4403(2) 0.0678(8) Uani d . 1 1 H H17 0.8315 0.4128 0.4031 0.081 Uiso calc R 1 1 C C18 0.6956(6) 0.2800(3) 0.4316(2) 0.0736(9) Uani d . 1 1 H H18 0.5701 0.3012 0.3873 0.088 Uiso calc R 1 1 C C19 0.7216(5) 0.1818(2) 0.4878(2) 0.0634(7) Uani d . 1 1 H H19 0.6131 0.1376 0.4811 0.076 Uiso calc R 1 1 C C20 0.9076(4) 0.1481(2) 0.55430(16) 0.0482(6) Uani d . 1 1 C C21 0.9360(5) 0.04127(19) 0.61706(17) 0.0522(6) Uani d . 1 1 H H21A 0.7875 0.0078 0.6120 0.063 Uiso calc R 1 1 H H21B 1.0891 0.0127 0.5917 0.063 Uiso calc R 1 1 C C22 0.7457(4) 0.03002(15) 0.78199(16) 0.0380(5) Uani d . 1 1 N N1 0.2648(4) 0.88914(13) -0.07174(13) 0.0408(4) Uani d . 1 1 H H1C 0.1180 0.9174 -0.0535 0.049 Uiso calc R 1 1 H H1D 0.3304 0.9325 -0.1289 0.049 Uiso calc R 1 1 N N2 0.7950(4) 0.84740(13) 0.14526(14) 0.0421(4) Uani d . 1 1 H H2A 0.9216 0.8903 0.1189 0.050 Uiso calc R 1 1 H H2B 0.7071 0.8643 0.1935 0.050 Uiso calc R 1 1 N N3 0.9570(4) 0.02365(15) 0.71937(13) 0.0466(5) Uani d . 1 1 H H3A 1.1067 0.0087 0.7416 0.056 Uiso calc R 1 1 O O1 0.5253(3) 0.04092(13) 0.75078(12) 0.0485(4) Uani d . 1 1 O O2 0.7879(3) 0.02260(11) 0.86767(11) 0.0427(3) Uani d . 1 1 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 0.04028(12) 0.04843(13) 0.05196(13) -0.00295(7) -0.01089(8) -0.01752(9) C1 0.0422(13) 0.0505(13) 0.0529(13) -0.0076(10) -0.0076(10) -0.0202(11) C2 0.0457(13) 0.0481(13) 0.0520(13) -0.0058(10) -0.0114(10) -0.0237(11) C3 0.0634(17) 0.0626(16) 0.0565(15) 0.0000(13) -0.0048(13) -0.0271(13) C4 0.0660(19) 0.092(2) 0.082(2) -0.0063(17) 0.0049(16) -0.0550(19) C5 0.0607(19) 0.090(2) 0.123(3) 0.0092(17) -0.021(2) -0.076(2) C6 0.090(2) 0.0589(18) 0.118(3) 0.0236(17) -0.051(2) -0.0405(19) C7 0.0736(19) 0.0557(16) 0.0671(17) 0.0033(14) -0.0224(15) -0.0194(14) C8 0.0394(12) 0.0503(13) 0.0541(14) -0.0004(10) -0.0124(10) -0.0170(11) C9 0.0383(12) 0.0437(12) 0.0446(12) 0.0037(9) -0.0138(10) -0.0114(10) C10 0.0589(16) 0.0533(15) 0.0533(14) -0.0044(12) -0.0027(12) -0.0199(12) C11 0.0725(19) 0.0494(15) 0.0709(18) -0.0042(13) -0.0139(15) -0.0240(13) C12 0.0535(16) 0.0459(14) 0.0745(18) -0.0083(12) -0.0150(14) -0.0056(13) C13 0.0504(15) 0.0660(18) 0.0691(18) -0.0071(13) 0.0057(13) -0.0164(14) C14 0.0517(15) 0.0584(16) 0.0608(16) -0.0029(12) -0.0037(12) -0.0244(13) C15 0.0509(15) 0.0737(18) 0.0482(14) -0.0044(13) -0.0109(11) -0.0141(13) C16 0.0680(19) 0.076(2) 0.0597(17) -0.0122(15) -0.0023(14) -0.0203(15) C17 0.0609(18) 0.0726(19) 0.0554(16) 0.0053(15) 0.0036(13) -0.0097(14) C18 0.0538(17) 0.093(2) 0.0601(17) 0.0114(16) -0.0175(13) -0.0103(16) C19 0.0461(14) 0.086(2) 0.0589(16) -0.0034(14) -0.0118(12) -0.0244(15) C20 0.0380(12) 0.0698(16) 0.0353(11) 0.0021(11) 0.0007(9) -0.0189(11) C21 0.0477(14) 0.0657(16) 0.0452(13) 0.0019(12) -0.0011(11) -0.0239(12) C22 0.0315(11) 0.0367(11) 0.0444(12) -0.0021(8) -0.0026(9) -0.0128(9) N1 0.0351(9) 0.0420(10) 0.0435(10) -0.0008(8) -0.0033(8) -0.0135(8) N2 0.0378(10) 0.0424(10) 0.0497(11) -0.0046(8) -0.0054(8) -0.0198(8) N3 0.0321(9) 0.0639(12) 0.0397(10) 0.0034(9) -0.0036(8) -0.0145(9) O1 0.0299(8) 0.0635(10) 0.0544(9) -0.0016(7) -0.0067(7) -0.0232(8) O2 0.0350(8) 0.0537(9) 0.0405(8) -0.0037(7) -0.0031(6) -0.0179(7) 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' Ag Ag -0.8971 1.1015 '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' O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2 Ag1 N1 175.96(7) N1 C1 C2 111.10(18) N1 C1 H1A 109.4 C2 C1 H1A 109.4 N1 C1 H1B 109.4 C2 C1 H1B 109.4 H1A C1 H1B 108.0 C7 C2 C3 118.6(3) C7 C2 C1 121.3(2) C3 C2 C1 120.1(2) C4 C3 C2 121.0(3) C4 C3 H3 119.5 C2 C3 H3 119.5 C5 C4 C3 119.8(3) C5 C4 H4 120.1 C3 C4 H4 120.1 C4 C5 C6 120.1(3) C4 C5 H5 120.0 C6 C5 H5 120.0 C5 C6 C7 120.5(3) C5 C6 H6 119.7 C7 C6 H6 119.7 C2 C7 C6 120.0(3) C2 C7 H7 120.0 C6 C7 H7 120.0 N2 C8 C9 112.28(18) N2 C8 H8A 109.1 C9 C8 H8A 109.1 N2 C8 H8B 109.1 C9 C8 H8B 109.1 H8A C8 H8B 107.9 C10 C9 C14 118.1(2) C10 C9 C8 120.6(2) C14 C9 C8 121.3(2) C9 C10 C11 120.9(3) C9 C10 H10 119.6 C11 C10 H10 119.6 C12 C11 C10 120.2(3) C12 C11 H11 119.9 C10 C11 H11 119.9 C13 C12 C11 119.6(3) C13 C12 H12 120.2 C11 C12 H12 120.2 C12 C13 C14 120.4(3) C12 C13 H13 119.8 C14 C13 H13 119.8 C13 C14 C9 120.9(3) C13 C14 H14 119.6 C9 C14 H14 119.6 C20 C15 C16 121.6(3) C20 C15 H15 119.2 C16 C15 H15 119.2 C17 C16 C15 120.2(3) C17 C16 H16 119.9 C15 C16 H16 119.9 C18 C17 C16 119.1(3) C18 C17 H17 120.5 C16 C17 H17 120.5 C17 C18 C19 120.7(3) C17 C18 H18 119.7 C19 C18 H18 119.7 C18 C19 C20 120.9(3) C18 C19 H19 119.6 C20 C19 H19 119.6 C15 C20 C19 117.5(3) C15 C20 C21 121.1(2) C19 C20 C21 121.4(3) N3 C21 C20 114.1(2) N3 C21 H21A 108.7 C20 C21 H21A 108.7 N3 C21 H21B 108.7 C20 C21 H21B 108.7 H21A C21 H21B 107.6 O1 C22 O2 125.1(2) O1 C22 N3 117.7(2) O2 C22 N3 117.16(19) C1 N1 Ag1 121.93(14) C1 N1 H1C 106.8 Ag1 N1 H1C 106.8 C1 N1 H1D 106.8 Ag1 N1 H1D 106.8 H1C N1 H1D 106.7 C8 N2 Ag1 122.49(14) C8 N2 H2A 106.7 Ag1 N2 H2A 106.7 C8 N2 H2B 106.7 Ag1 N2 H2B 106.7 H2A N2 H2B 106.6 C22 N3 C21 122.13(19) C22 N3 H3A 118.9 C21 N3 H3A 118.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ag1 N2 2.1504(19) Ag1 N1 2.1527(18) C1 N1 1.478(3) C1 C2 1.506(3) C1 H1A 0.9700 C1 H1B 0.9700 C2 C7 1.371(4) C2 C3 1.382(4) C3 C4 1.382(4) C3 H3 0.9300 C4 C5 1.359(5) C4 H4 0.9300 C5 C6 1.361(5) C5 H5 0.9300 C6 C7 1.391(5) C6 H6 0.9300 C7 H7 0.9300 C8 N2 1.478(3) C8 C9 1.504(3) C8 H8A 0.9700 C8 H8B 0.9700 C9 C10 1.374(4) C9 C14 1.382(3) C10 C11 1.386(4) C10 H10 0.9300 C11 C12 1.366(4) C11 H11 0.9300 C12 C13 1.364(4) C12 H12 0.9300 C13 C14 1.378(4) C13 H13 0.9300 C14 H14 0.9300 C15 C20 1.373(4) C15 C16 1.375(4) C15 H15 0.9300 C16 C17 1.373(4) C16 H16 0.9300 C17 C18 1.364(5) C17 H17 0.9300 C18 C19 1.378(4) C18 H18 0.9300 C19 C20 1.387(3) C19 H19 0.9300 C20 C21 1.505(4) C21 N3 1.449(3) C21 H21A 0.9700 C21 H21B 0.9700 C22 O1 1.260(3) C22 O2 1.269(3) C22 N3 1.372(3) N1 H1C 0.9000 N1 H1D 0.9000 N2 H2A 0.9000 N2 H2B 0.9000 N3 H3A 0.8600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N3 H3A O1 1_655 0.86 2.29 3.087(2) 153.6 N2 H2B O1 2_666 0.90 2.10 2.931(2) 154.0 N2 H2A O2 2_766 0.90 2.12 2.943(2) 151.3 N1 H1D O1 1_564 0.90 2.12 3.011(2) 170.5 N1 H1C O2 1_464 0.90 2.32 3.037(2) 136.2 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N1 C1 C2 C7 101.7(3) N1 C1 C2 C3 -76.7(3) C7 C2 C3 C4 -0.2(4) C1 C2 C3 C4 178.2(2) C2 C3 C4 C5 0.3(5) C3 C4 C5 C6 -0.1(5) C4 C5 C6 C7 -0.1(5) C3 C2 C7 C6 0.0(4) C1 C2 C7 C6 -178.5(3) C5 C6 C7 C2 0.2(5) N2 C8 C9 C10 109.3(2) N2 C8 C9 C14 -70.1(3) C14 C9 C10 C11 0.4(4) C8 C9 C10 C11 -179.0(2) C9 C10 C11 C12 -0.2(4) C10 C11 C12 C13 -0.2(4) C11 C12 C13 C14 0.5(4) C12 C13 C14 C9 -0.3(4) C10 C9 C14 C13 -0.1(4) C8 C9 C14 C13 179.2(2) C20 C15 C16 C17 -0.2(4) C15 C16 C17 C18 -1.1(4) C16 C17 C18 C19 1.3(5) C17 C18 C19 C20 -0.2(5) C16 C15 C20 C19 1.3(4) C16 C15 C20 C21 -179.0(2) C18 C19 C20 C15 -1.0(4) C18 C19 C20 C21 179.2(3) C15 C20 C21 N3 47.1(3) C19 C20 C21 N3 -133.2(2) C2 C1 N1 Ag1 -58.7(2) N2 Ag1 N1 C1 -23.4(10) C9 C8 N2 Ag1 -46.1(3) N1 Ag1 N2 C8 29.8(10) O1 C22 N3 C21 7.9(3) O2 C22 N3 C21 -173.4(2) C20 C21 N3 C22 77.1(3) _journal_paper_doi 10.1107/S0108768112030212