# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1560 data_c003 #number 5 in manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code 'Ni_dmbp_Cl_c003_jan' _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date ? _chemical_name_systematic ;Aqua-dichloro(2,2'-dimethyl-4,4'-bipyrimidine)nickel(II) nitromethane (1:1) ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common '[(dmbp)(H2O)NiCl2] . CH3NO2' _chemical_formula_moiety '(C10 H10 N4), Cl2, Ni, (C H3 N O2), (H2 O)' _chemical_formula_sum 'C11 H15 Cl2 N5 Ni O3' _chemical_formula_weight 394.867 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 13.506(3) _cell_length_b 7.6665(10) _cell_length_c 15.374(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.69(2) _cell_angle_gamma 90.00 _cell_volume 1564.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 4979 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.85 _cell_special_details ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.6767(5) _exptl_crystal_density_method none _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.0770 -1 0 -1 0.1232 1 -1 -1 0.2310 -1 1 1 0.2695 1 1 -1 0.2695 -1 -2 2 0.2695 -1 0 2 0.2002 1 0 -1 0.2772 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 1.2 _diffr_source_voltage ? _diffr_source_current ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ? _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _diffrn_special_details ? _diffrn_reflns_number 9078 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.86 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.890 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.106 _reflns_number_total 3507 _reflns_number_gt 2685 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3507 _refine_ls_number_parameters 248 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details 'all H atoms with one common U' 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.32055(2) 0.21333(4) 0.64044(2) 0.01660(12) Uani 1 1 d . . . O91 O 0.2661(3) 0.2219(4) 0.7498(2) 0.0633(11) Uani 1 1 d D . . H911 H 0.221(3) 0.286(5) 0.757(3) 0.050(3) Uiso 1 1 d D . . H912 H 0.275(3) 0.153(5) 0.791(3) 0.050(3) Uiso 1 1 d D . . Cl1 Cl 0.39826(5) -0.04719(8) 0.69633(5) 0.02388(17) Uani 1 1 d . . . Cl2 Cl 0.22770(5) 0.46333(9) 0.59578(5) 0.02497(17) Uani 1 1 d . . . N1 N 0.30308(15) 0.1189(3) 0.51659(16) 0.0182(5) Uani 1 1 d . . . C1 C 0.22531(18) 0.0251(3) 0.4751(2) 0.0220(6) Uani 1 1 d . . . N2 N 0.21656(17) -0.0325(3) 0.39298(17) 0.0266(5) Uani 1 1 d . . . C2 C 0.2890(2) 0.0104(4) 0.3496(2) 0.0289(6) Uani 1 1 d D . . H2 H 0.286(3) -0.025(5) 0.2929(18) 0.050(3) Uiso 1 1 d D . . C3 C 0.3731(2) 0.1035(4) 0.3874(2) 0.0261(6) Uani 1 1 d D . . H3 H 0.421(2) 0.136(5) 0.357(3) 0.050(3) Uiso 1 1 d D . . C4 C 0.37813(19) 0.1549(3) 0.47356(19) 0.0198(6) Uani 1 1 d . . . C5 C 0.46281(18) 0.2506(3) 0.5266(2) 0.0191(6) Uani 1 1 d . . . N3 N 0.44801(15) 0.3031(3) 0.60651(16) 0.0184(5) Uani 1 1 d . . . C6 C 0.51873(18) 0.3976(3) 0.6573(2) 0.0221(6) Uani 1 1 d . . . N4 N 0.60734(16) 0.4372(3) 0.63556(18) 0.0267(6) Uani 1 1 d . . . C7 C 0.62219(19) 0.3792(4) 0.5577(2) 0.0278(7) Uani 1 1 d D . . H7 H 0.685(2) 0.400(5) 0.547(3) 0.050(3) Uiso 1 1 d D . . C8 C 0.55246(19) 0.2873(4) 0.4992(2) 0.0244(6) Uani 1 1 d D . . H8 H 0.567(3) 0.244(5) 0.448(2) 0.050(3) Uiso 1 1 d D . . C9 C 0.1454(2) -0.0186(4) 0.5256(2) 0.0315(7) Uani 1 1 d D . . H91 H 0.129(3) 0.076(4) 0.557(2) 0.050(3) Uiso 1 1 d D . . H92 H 0.167(3) -0.098(4) 0.570(2) 0.050(3) Uiso 1 1 d D . . H93 H 0.086(2) -0.045(5) 0.487(2) 0.050(3) Uiso 1 1 d D . . C10 C 0.4964(2) 0.4684(4) 0.7410(2) 0.0296(7) Uani 1 1 d D . . H101 H 0.550(2) 0.494(5) 0.786(2) 0.050(3) Uiso 1 1 d D . . H102 H 0.472(3) 0.384(4) 0.774(2) 0.050(3) Uiso 1 1 d D . . H103 H 0.443(2) 0.544(4) 0.728(3) 0.050(3) Uiso 1 1 d D . . N11 N 0.5800(2) 0.0854(4) 0.8841(2) 0.0366(6) Uani 1 1 d . . . O01 O 0.5316(2) 0.1984(3) 0.9121(2) 0.0510(7) Uani 1 1 d . . . O02 O 0.6474(2) 0.1150(4) 0.8451(3) 0.0716(10) Uani 1 1 d . . . C11 C 0.5554(3) -0.0954(4) 0.9011(3) 0.0374(8) Uani 1 1 d D . . H111 H 0.4881(14) -0.110(5) 0.875(3) 0.050(3) Uiso 1 1 d D . . H112 H 0.574(3) -0.114(5) 0.9612(12) 0.050(3) Uiso 1 1 d D . . H113 H 0.594(3) -0.171(5) 0.875(3) 0.050(3) Uiso 1 1 d D . . 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 Ni 0.01761(17) 0.01658(18) 0.0176(2) -0.00021(13) 0.00848(12) 0.00000(12) O91 0.107(2) 0.0511(17) 0.051(2) 0.0341(14) 0.0636(18) 0.0555(17) Cl1 0.0263(3) 0.0209(3) 0.0281(4) 0.0052(3) 0.0146(3) 0.0053(2) Cl2 0.0305(3) 0.0238(3) 0.0219(4) 0.0012(3) 0.0084(3) 0.0086(2) N1 0.0192(9) 0.0155(10) 0.0214(13) -0.0004(9) 0.0080(8) 0.0024(8) C1 0.0200(11) 0.0198(12) 0.0265(17) -0.0002(11) 0.0048(10) 0.0015(9) N2 0.0291(11) 0.0267(13) 0.0232(15) -0.0044(10) 0.0029(10) 0.0014(9) C2 0.0382(15) 0.0298(15) 0.0194(17) -0.0030(12) 0.0069(12) 0.0065(12) C3 0.0311(14) 0.0250(14) 0.0255(18) 0.0017(12) 0.0141(12) 0.0056(11) C4 0.0221(12) 0.0165(12) 0.0223(16) 0.0040(10) 0.0082(10) 0.0049(9) C5 0.0214(11) 0.0154(11) 0.0230(16) 0.0058(10) 0.0103(10) 0.0022(9) N3 0.0175(9) 0.0171(10) 0.0223(14) 0.0027(9) 0.0079(8) -0.0004(8) C6 0.0200(11) 0.0179(12) 0.0280(17) 0.0074(11) 0.0035(11) -0.0002(9) N4 0.0221(10) 0.0255(12) 0.0321(16) 0.0047(10) 0.0040(10) -0.0046(9) C7 0.0187(12) 0.0265(14) 0.040(2) 0.0105(13) 0.0111(12) 0.0009(10) C8 0.0204(12) 0.0237(14) 0.0322(19) 0.0062(12) 0.0127(11) 0.0032(10) C9 0.0254(13) 0.0352(17) 0.035(2) -0.0050(14) 0.0097(12) -0.0070(12) C10 0.0277(14) 0.0341(16) 0.0257(18) -0.0017(13) 0.0013(12) -0.0023(12) N11 0.0424(14) 0.0351(14) 0.0346(18) 0.0032(12) 0.0132(13) 0.0010(12) O01 0.0738(18) 0.0343(13) 0.0506(19) 0.0039(12) 0.0267(14) 0.0151(13) O02 0.0744(19) 0.065(2) 0.091(3) 0.0024(19) 0.0574(19) -0.0089(16) C11 0.0429(17) 0.0292(16) 0.038(2) 0.0018(15) 0.0032(15) 0.0025(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O91 1.957(3) . ? Ni N1 2.010(2) . ? Ni N3 2.010(2) . ? Ni Cl2 2.3234(8) . ? Ni Cl1 2.3441(7) . ? O91 H911 0.81(3) . ? O91 H912 0.82(3) . ? N1 C1 1.334(3) . ? N1 C4 1.338(3) . ? C1 N2 1.323(4) . ? C1 C9 1.480(4) . ? N2 C2 1.324(4) . ? C2 C3 1.376(4) . ? C2 H2 0.91(2) . ? C3 C4 1.371(4) . ? C3 H3 0.90(2) . ? C4 C5 1.472(4) . ? C5 N3 1.343(4) . ? C5 C8 1.383(4) . ? N3 C6 1.330(4) . ? C6 N4 1.336(3) . ? C6 C10 1.480(5) . ? N4 C7 1.327(4) . ? C7 C8 1.371(4) . ? C7 H7 0.91(2) . ? C8 H8 0.91(2) . ? C9 H91 0.926(16) . ? C9 H92 0.927(16) . ? C9 H93 0.925(16) . ? C10 H101 0.920(16) . ? C10 H102 0.920(16) . ? C10 H103 0.918(16) . ? N11 O02 1.201(4) . ? N11 O01 1.212(4) . ? N11 C11 1.460(4) . ? C11 H111 0.929(15) . ? C11 H112 0.921(15) . ? C11 H113 0.921(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O91 Ni N1 146.00(14) . . ? O91 Ni N3 133.45(14) . . ? N1 Ni N3 80.40(9) . . ? O91 Ni Cl2 87.59(7) . . ? N1 Ni Cl2 93.16(6) . . ? N3 Ni Cl2 94.71(6) . . ? O91 Ni Cl1 85.86(7) . . ? N1 Ni Cl1 90.36(6) . . ? N3 Ni Cl1 92.29(6) . . ? Cl2 Ni Cl1 172.60(3) . . ? Ni O91 H911 124(3) . . ? Ni O91 H912 128(3) . . ? H911 O91 H912 107(5) . . ? C1 N1 C4 118.5(3) . . ? C1 N1 Ni 126.20(19) . . ? C4 N1 Ni 115.31(18) . . ? N2 C1 N1 124.0(3) . . ? N2 C1 C9 118.7(2) . . ? N1 C1 C9 117.2(3) . . ? C1 N2 C2 117.1(2) . . ? N2 C2 C3 123.0(3) . . ? N2 C2 H2 120(3) . . ? C3 C2 H2 116(3) . . ? C4 C3 C2 116.5(3) . . ? C4 C3 H3 121(3) . . ? C2 C3 H3 122(3) . . ? N1 C4 C3 120.8(3) . . ? N1 C4 C5 114.3(3) . . ? C3 C4 C5 124.9(2) . . ? N3 C5 C8 120.4(3) . . ? N3 C5 C4 115.1(2) . . ? C8 C5 C4 124.5(3) . . ? C6 N3 C5 119.2(2) . . ? C6 N3 Ni 126.2(2) . . ? C5 N3 Ni 114.51(17) . . ? N3 C6 N4 123.8(3) . . ? N3 C6 C10 118.0(2) . . ? N4 C6 C10 118.1(3) . . ? C7 N4 C6 116.2(3) . . ? N4 C7 C8 124.3(3) . . ? N4 C7 H7 114(3) . . ? C8 C7 H7 122(3) . . ? C7 C8 C5 116.0(3) . . ? C7 C8 H8 121(3) . . ? C5 C8 H8 122(3) . . ? C1 C9 H91 112(3) . . ? C1 C9 H92 112(3) . . ? H91 C9 H92 101(4) . . ? C1 C9 H93 110(3) . . ? H91 C9 H93 104(3) . . ? H92 C9 H93 117(4) . . ? C6 C10 H101 118(3) . . ? C6 C10 H102 112(3) . . ? H101 C10 H102 93(4) . . ? C6 C10 H103 109(3) . . ? H101 C10 H103 120(4) . . ? H102 C10 H103 103(3) . . ? O02 N11 O01 123.5(3) . . ? O02 N11 C11 119.2(3) . . ? O01 N11 C11 117.3(3) . . ? N11 C11 H111 106(3) . . ? N11 C11 H112 107(3) . . ? H111 C11 H112 118(4) . . ? N11 C11 H113 111(3) . . ? H111 C11 H113 109(4) . . ? H112 C11 H113 106(4) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 N3 -6.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O91 H911 Cl1 0.81(4) 2.27(4) 3.071(4) 170(4) 4_667 ? O91 H912 Cl2 0.82(4) 2.27(4) 3.082(3) 171(4) 4_556 ? _geom_special_details ? #===END data_kplr #number 6 in dmbp-manuscript _audit_creation_method SHELXL _chemical_name_systematic ;(\m-2,2'-dimethyl-4,4'-bipyrimidine)-dinitrato-copper(II) ? ; _chemical_name_common '[Cu (N O3)2 (C10 H10 N4)]' _chemical_formula_moiety 'Cu, 2(N O3), (C10 H10 N4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H5 Cu0.50 N3 O3' _chemical_formula_weight 186.89 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.111(8) _cell_length_b 7.445(8) _cell_length_c 9.335(8) _cell_angle_alpha 82.29(8) _cell_angle_beta 83.07(8) _cell_angle_gamma 67.23(8) _cell_volume 387.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour blue-violet _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 189 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Syntex P21' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2009 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1759 _reflns_number_observed 1504 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1271P)^2^+0.5222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1756 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_obs 0.0726 _refine_ls_wR_factor_all 0.2087 _refine_ls_wR_factor_obs 0.1784 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_obs 1.033 _refine_ls_restrained_S_all 1.115 _refine_ls_restrained_S_obs 1.033 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.5000 0.0441(3) Uani 1 d S . N1 N 0.4944(7) 0.6819(5) 0.3138(4) 0.0440(8) Uani 1 d . . C1 C 0.3859(9) 0.6852(7) 0.1926(5) 0.0447(10) Uani 1 d . . C2 C 0.2592(11) 0.5457(8) 0.1921(6) 0.0581(12) Uani 1 d . . H21 H 0.1841(70) 0.5301(53) 0.2868(14) 0.080 Uiso 1 calc R . H22 H 0.3726(17) 0.4209(22) 0.1665(49) 0.080 Uiso 1 calc R . H23 H 0.1409(57) 0.5978(34) 0.1227(36) 0.080 Uiso 1 calc R . N2 N 0.3863(8) 0.8075(6) 0.0704(5) 0.0483(9) Uani 1 d . . C3 C 0.5025(8) 0.9331(6) 0.0691(5) 0.0452(10) Uani 1 d . . C4 C 0.6174(9) 0.9376(8) 0.1887(6) 0.0518(11) Uani 1 d . . H4 H 0.6970(9) 1.0221(8) 0.1867(6) 0.080 Uiso 1 calc R . C5 C 0.6075(9) 0.8097(7) 0.3113(5) 0.0499(10) Uani 1 d . . H5 H 0.6793(9) 0.8114(7) 0.3932(5) 0.080 Uiso 1 calc R . N10 N 0.8895(8) 0.2235(7) 0.3902(5) 0.0569(11) Uani 1 d . . O1 O 0.6608(7) 0.2605(5) 0.3882(4) 0.0557(9) Uani 1 d . . O2 O 0.9469(8) 0.3365(7) 0.4545(5) 0.0694(11) Uani 1 d . . O3 O 1.0346(9) 0.0824(8) 0.3281(7) 0.092(2) Uani 1 d . . 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 Cu1 0.0473(5) 0.0369(4) 0.0398(5) -0.0041(3) -0.0001(3) -0.0078(3) N1 0.046(2) 0.037(2) 0.039(2) -0.0013(14) 0.0005(15) -0.007(2) C1 0.049(2) 0.041(2) 0.037(2) -0.002(2) -0.001(2) -0.010(2) C2 0.061(3) 0.056(3) 0.057(3) -0.004(2) -0.004(2) -0.023(2) N2 0.054(2) 0.042(2) 0.044(2) -0.004(2) -0.003(2) -0.012(2) C3 0.047(2) 0.037(2) 0.045(2) -0.006(2) 0.000(2) -0.009(2) C4 0.055(3) 0.048(2) 0.049(3) -0.003(2) -0.005(2) -0.016(2) C5 0.057(3) 0.044(2) 0.046(2) 0.001(2) -0.007(2) -0.017(2) N10 0.051(2) 0.051(2) 0.058(3) -0.010(2) 0.001(2) -0.008(2) O1 0.054(2) 0.051(2) 0.057(2) -0.012(2) -0.002(2) -0.012(2) O2 0.069(3) 0.071(3) 0.073(3) -0.013(2) -0.009(2) -0.030(2) O3 0.068(3) 0.078(3) 0.102(4) -0.037(3) 0.011(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 2.032(4) . ? Cu1 O1 2.032(4) 2_666 ? Cu1 N1 2.051(4) . ? Cu1 N1 2.051(4) 2_666 ? Cu1 O2 2.531(6) 2_666 ? Cu1 O2 2.531(6) . ? N1 C1 1.371(6) . ? N1 C5 1.372(7) . ? C1 N2 1.361(6) . ? C1 C2 1.518(7) . ? C2 H21 0.96 . ? C2 H22 0.96 . ? C2 H23 0.96 . ? N2 C3 1.374(7) . ? C3 C4 1.398(7) . ? C3 C3 1.517(9) 2_675 ? C4 C5 1.398(7) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? N10 O3 1.243(6) . ? N10 O2 1.267(6) . ? N10 O1 1.318(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 180.0 . 2_666 ? O1 Cu1 N1 91.0(2) . . ? O1 Cu1 N1 89.0(2) 2_666 . ? O1 Cu1 N1 89.0(2) . 2_666 ? O1 Cu1 N1 91.0(2) 2_666 2_666 ? N1 Cu1 N1 180.0 . 2_666 ? O1 Cu1 O2 123.3(2) . 2_666 ? O1 Cu1 O2 56.7(2) 2_666 2_666 ? N1 Cu1 O2 90.9(2) . 2_666 ? N1 Cu1 O2 89.1(2) 2_666 2_666 ? O1 Cu1 O2 56.7(2) . . ? O1 Cu1 O2 123.3(2) 2_666 . ? N1 Cu1 O2 89.1(2) . . ? N1 Cu1 O2 90.9(2) 2_666 . ? O2 Cu1 O2 180.0 2_666 . ? C1 N1 C5 118.0(4) . . ? C1 N1 Cu1 124.9(3) . . ? C5 N1 Cu1 117.1(3) . . ? N2 C1 N1 123.3(4) . . ? N2 C1 C2 117.4(4) . . ? N1 C1 C2 119.2(4) . . ? C1 C2 H21 109.5(3) . . ? C1 C2 H22 109.5(3) . . ? H21 C2 H22 109.5 . . ? C1 C2 H23 109.5(3) . . ? H21 C2 H23 109.5 . . ? H22 C2 H23 109.5 . . ? C1 N2 C3 117.9(4) . . ? N2 C3 C4 121.9(4) . . ? N2 C3 C3 116.0(5) . 2_675 ? C4 C3 C3 122.2(6) . 2_675 ? C3 C4 C5 117.2(5) . . ? C3 C4 H4 121.4(3) . . ? C5 C4 H4 121.4(3) . . ? N1 C5 C4 121.6(5) . . ? N1 C5 H5 119.2(3) . . ? C4 C5 H5 119.2(3) . . ? O3 N10 O2 124.2(5) . . ? O3 N10 O1 118.4(5) . . ? O2 N10 O1 117.5(4) . . ? N10 O1 Cu1 103.7(3) . . ? N10 O2 Cu1 82.2(3) . . ? _refine_diff_density_max 0.943 _refine_diff_density_min -1.302 _refine_diff_density_rms 0.125 #===END data_c001 #number 8 in dmbp-manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code Cu2_dmbp_I2_c001_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date ? _chemical_name_systematic ;(\m-2,2'-dimethyl-4,4'-bipyrimidine)-di(\m3-iodo)-dicopper(I) ; _chemical_compound_source 'crystal provided by J. Janiak, Uni FR' _chemical_name_common [(dmbp)Cu2I2] _chemical_formula_moiety '(C10 H10 N4), Cu2, I2' _chemical_formula_sum 'C10 H10 Cu2 I2 N4' _chemical_formula_weight 567.114 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7509(12) _cell_length_b 10.5927(18) _cell_length_c 4.2001(7) _cell_angle_alpha 91.81(2) _cell_angle_beta 101.993(18) _cell_angle_gamma 88.544(19) _cell_volume 337.08(10) _cell_formula_units_Z 1 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 2985 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 27.85 _cell_special_details ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.7938(8) _exptl_crystal_density_method none _exptl_crystal_F_000 262 _exptl_absorpt_coefficient_mu 7.719 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3583 _exptl_absorpt_correction_T_max 0.5565 _exptl_absorpt_process_details 'XRed, rev. 1.06, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0693 -1 0 0 0.0693 0 1 0 0.0770 0 -1 0 0.0770 1 0 -1 0.0385 -1 0 1 0.0385 -1 -1 1 0.0500 1 1 -1 0.0500 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 1.2 _diffr_source_voltage ? _diffr_source_current ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ? _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 3494 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.89 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.601 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.170 _reflns_number_total 1492 _reflns_number_gt 1358 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1492 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.78437(3) -0.08075(2) 0.72059(5) 0.01407(9) Uani 1 1 d . . . Cu Cu 0.87631(6) 0.05871(4) 0.28710(11) 0.01858(12) Uani 1 1 d . . . N1 N 0.7322(4) 0.2217(3) 0.2079(8) 0.0156(6) Uani 1 1 d . . . C2 C 0.7774(5) 0.3338(3) 0.3552(8) 0.0140(7) Uani 1 1 d . . . C3 C 0.9389(5) 0.3390(4) 0.6212(10) 0.0198(7) Uiso 1 1 d . . . H31 H 1.029(6) 0.351(4) 0.528(11) 0.017(11) Uiso 1 1 d . . . H32 H 0.948(7) 0.258(5) 0.746(12) 0.031(13) Uiso 1 1 d . . . H33 H 0.942(7) 0.404(6) 0.778(14) 0.047(16) Uiso 1 1 d . . . N3 N 0.6904(4) 0.4425(3) 0.2815(7) 0.0161(6) Uani 1 1 d . . . C4 C 0.5460(5) 0.4390(3) 0.0416(8) 0.0140(7) Uani 1 1 d . . . C5 C 0.4868(5) 0.3280(3) -0.1150(10) 0.0204(8) Uani 1 1 d . . . H5 H 0.397(6) 0.328(4) -0.266(10) 0.011(10) Uiso 1 1 d . . . C6 C 0.5842(5) 0.2198(3) -0.0243(10) 0.0183(8) Uani 1 1 d . . . H6 H 0.542(5) 0.138(4) -0.131(9) 0.006(9) Uiso 1 1 d . . . 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 I 0.01327(12) 0.01455(12) 0.01403(12) 0.00093(8) 0.00185(8) -0.00070(8) Cu 0.0174(2) 0.0144(2) 0.0230(2) 0.00594(17) 0.00183(18) 0.00533(18) N1 0.0120(14) 0.0123(13) 0.0226(15) 0.0042(11) 0.0036(12) 0.0040(11) C2 0.0142(17) 0.0150(15) 0.0136(15) 0.0049(13) 0.0047(13) 0.0027(13) N3 0.0152(15) 0.0130(13) 0.0183(14) 0.0026(11) -0.0002(12) 0.0032(11) C4 0.0122(16) 0.0147(16) 0.0151(15) 0.0038(13) 0.0028(13) 0.0027(14) C5 0.0145(17) 0.0161(16) 0.0270(19) 0.0010(15) -0.0037(15) 0.0043(14) C6 0.0136(17) 0.0110(15) 0.0302(19) 0.0024(14) 0.0038(15) 0.0012(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I Cu 2.6014(7) . ? I Cu 2.6532(7) 2_756 ? I Cu 2.7347(8) 1_556 ? Cu N1 2.030(3) . ? Cu Cu 2.6488(10) 2_756 ? Cu I 2.6532(7) 2_756 ? Cu I 2.7347(8) 1_554 ? N1 C2 1.342(5) . ? N1 C6 1.342(5) . ? C2 N3 1.332(4) . ? C2 C3 1.495(5) . ? C3 H31 0.89(5) . ? C3 H32 1.01(5) . ? C3 H33 0.94(6) . ? N3 C4 1.342(4) . ? C4 C5 1.370(5) . ? C4 C4 1.477(6) 2_665 ? C5 C6 1.377(5) . ? C5 H5 0.84(4) . ? C6 H6 1.00(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu I Cu 60.53(2) . 2_756 ? Cu I Cu 103.80(2) . 1_556 ? Cu I Cu 82.61(2) 2_756 1_556 ? N1 Cu I 113.31(10) . . ? N1 Cu Cu 143.58(9) . 2_756 ? I Cu Cu 60.70(2) . 2_756 ? N1 Cu I 114.54(10) . 2_756 ? I Cu I 119.47(2) . 2_756 ? Cu Cu I 58.76(2) 2_756 2_756 ? N1 Cu I 105.03(9) . 1_554 ? I Cu I 103.80(2) . 1_554 ? Cu Cu I 111.30(3) 2_756 1_554 ? I Cu I 97.39(2) 2_756 1_554 ? C2 N1 C6 116.7(3) . . ? C2 N1 Cu 125.5(2) . . ? C6 N1 Cu 117.7(2) . . ? N3 C2 N1 125.1(3) . . ? N3 C2 C3 116.7(3) . . ? N1 C2 C3 118.2(3) . . ? C2 C3 H31 107(3) . . ? C2 C3 H32 109(3) . . ? H31 C3 H32 114(4) . . ? C2 C3 H33 116(3) . . ? H31 C3 H33 106(5) . . ? H32 C3 H33 105(4) . . ? C2 N3 C4 117.1(3) . . ? N3 C4 C5 121.8(3) . . ? N3 C4 C4 116.2(4) . 2_665 ? C5 C4 C4 122.0(4) . 2_665 ? C4 C5 C6 117.5(3) . . ? C4 C5 H5 120(3) . . ? C6 C5 H5 122(3) . . ? N1 C6 C5 121.8(3) . . ? N1 C6 H6 119(2) . . ? C5 C6 H6 119(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C4 C4 N3 -180.0(3) 180(2) . . 2_665 2_665 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C5 H5 N3 0.84(4) 2.51(4) 2.797(5) 102(3) 2_665 ? _geom_special_details ? #===END data_c025 #number 9 in dmbp-manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code Cu_dmbp1_I1_c025_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 19-Dec-1997 _chemical_name_systematic ;catena-(2,2'-dimethyl-4,4'-bipyrimidine)-\m-iodo-copper(I) ; _chemical_compound_source 'crystal provided by C. Janiak (Uni FR)' _chemical_name_common ;2,2'-dimethyl-4,4'-bipyrimidine.CuI ; _chemical_formula_moiety '(C10 H10 N4), Cu I ' _chemical_formula_sum 'C10 H10 Cu I N4' _chemical_formula_weight 376.664 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 33.463(2) _cell_length_b 35.0765(18) _cell_length_c 4.0449(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4747.8(4) _cell_formula_units_Z 16 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.9 _cell_special_details ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'red-blue (dichroitic)' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.10784(18) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 4.418 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6222 _exptl_absorpt_correction_T_max 0.9290 _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0192 0 1 0 0.0192 1 0 0 0.0077 -1 0 0 0.0077 0 0 1 0.3080 0 0 -1 0.3080 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.0 _diffr_source_voltage 40 _diffr_source_current 50 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ? _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _diffrn_special_details ? _diffrn_reflns_number 10123 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.84 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.179 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.086 _reflns_number_total 2811 _reflns_number_gt 2626 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.56(2) _refine_ls_number_reflns 2811 _refine_ls_number_parameters 163 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0501 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ; racemic twin, fraction of the main twin-component from refinement: 0.56, details of H atom refinement: 1 common U for all H atoms CH3 Hs geom pyrimidine Hs refxyz ; 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I -0.031149(6) 0.089388(6) -0.16800(7) 0.03200(6) Uani 1 1 d . . . Cu Cu 0.012506(10) 0.106426(9) 0.32318(13) 0.02902(9) Uani 1 1 d . . . N11 N 0.11214(9) 0.03687(8) 0.6510(9) 0.0400(9) Uani 1 1 d . . . C12 C 0.07866(10) 0.04812(9) 0.4974(9) 0.0311(8) Uani 1 1 d . . . N13 N 0.06907(7) 0.08454(7) 0.4334(7) 0.0254(5) Uani 1 1 d . . . C14 C 0.09552(8) 0.11173(8) 0.5215(8) 0.0243(6) Uani 1 1 d . . . C15 C 0.13107(10) 0.10233(10) 0.6781(10) 0.0364(8) Uani 1 1 d . . . H15 H 0.1491(12) 0.1195(11) 0.722(9) 0.031(10) Uiso 1 1 d . . . C16 C 0.13771(11) 0.06427(11) 0.7400(11) 0.0429(10) Uani 1 1 d . . . H16 H 0.1608(10) 0.0560(9) 0.854(12) 0.024(8) Uiso 1 1 d . . . C17 C 0.05000(11) 0.01782(9) 0.3895(13) 0.0448(11) Uani 1 1 d . . . H171 H 0.0621 0.0027 0.2189 0.120(11) Uiso 1 1 calc R . . H172 H 0.0261 0.0295 0.3058 0.120(11) Uiso 1 1 calc R . . H173 H 0.0434 0.0019 0.5745 0.120(11) Uiso 1 1 calc R . . N21 N 0.05842(10) 0.22265(8) 0.2620(10) 0.0447(9) Uani 1 1 d . . . C22 C 0.03454(10) 0.19218(9) 0.2562(8) 0.0325(8) Uani 1 1 d . . . N23 N 0.04589(7) 0.15640(6) 0.3382(9) 0.0270(5) Uani 1 1 d . . . C24 C 0.08376(9) 0.15153(9) 0.4381(8) 0.0264(6) Uani 1 1 d . . . C25 C 0.11035(11) 0.18173(10) 0.4601(11) 0.0413(9) Uani 1 1 d . . . H25 H 0.1358(12) 0.1804(11) 0.547(15) 0.038(10) Uiso 1 1 d . . . C26 C 0.09594(12) 0.21700(10) 0.3676(17) 0.0519(12) Uani 1 1 d . . . H26 H 0.1105(14) 0.2395(13) 0.382(15) 0.059(14) Uiso 1 1 d . . . C27 C -0.00770(11) 0.19809(11) 0.1475(13) 0.0476(11) Uani 1 1 d . . . H271 H -0.0171 0.2223 0.2269 0.120(11) Uiso 1 1 calc R . . H272 H -0.0242 0.1781 0.2354 0.120(11) Uiso 1 1 calc R . . H273 H -0.0090 0.1977 -0.0895 0.120(11) Uiso 1 1 calc 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 I 0.02243(8) 0.04674(11) 0.02682(9) 0.00141(10) -0.00288(9) -0.00298(8) Cu 0.01960(15) 0.03152(17) 0.0359(2) 0.0041(2) -0.00512(19) -0.00391(13) N11 0.0278(13) 0.0335(13) 0.059(3) 0.0112(14) -0.0058(14) 0.0044(11) C12 0.0242(14) 0.0264(13) 0.043(2) 0.0064(12) 0.0022(13) 0.0013(11) N13 0.0176(11) 0.0240(11) 0.0345(14) 0.0031(9) -0.0010(10) -0.0024(9) C14 0.0196(12) 0.0273(12) 0.0261(19) 0.0017(11) 0.0004(11) -0.0036(10) C15 0.0224(14) 0.0388(16) 0.048(2) 0.0031(15) -0.0054(14) -0.0083(13) C16 0.0240(15) 0.0475(19) 0.057(3) 0.0137(17) -0.0087(15) 0.0043(14) C17 0.0371(17) 0.0229(13) 0.074(4) 0.0048(17) -0.006(2) -0.0011(13) N21 0.0483(18) 0.0247(13) 0.061(3) 0.0088(14) 0.0091(17) -0.0008(12) C22 0.0353(16) 0.0291(14) 0.033(2) 0.0030(12) 0.0060(14) 0.0034(12) N23 0.0251(11) 0.0233(10) 0.0327(13) 0.0023(14) 0.0006(13) -0.0006(8) C24 0.0247(14) 0.0250(13) 0.0295(16) -0.0013(11) 0.0033(12) -0.0028(11) C25 0.0281(16) 0.0310(15) 0.065(3) -0.0009(15) 0.0021(16) -0.0091(14) C26 0.0446(19) 0.0283(14) 0.083(4) 0.003(2) 0.007(3) -0.0142(14) C27 0.041(2) 0.0376(17) 0.064(3) 0.0073(18) -0.007(2) 0.0113(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I Cu 2.5374(5) . ? I Cu 2.5937(5) 1_554 ? Cu N23 2.079(2) . ? Cu N13 2.091(2) . ? Cu I 2.5937(5) 1_556 ? N11 C16 1.336(5) . ? N11 C12 1.341(4) . ? C12 N13 1.342(4) . ? C12 C17 1.497(5) . ? N13 C14 1.349(4) . ? C14 C15 1.388(5) . ? C14 C24 1.489(4) . ? C15 C16 1.376(6) . ? C15 H15 0.87(4) . ? C16 H16 0.94(4) . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? N21 C22 1.334(4) . ? N21 C26 1.341(6) . ? C22 N23 1.353(4) . ? C22 C27 1.495(5) . ? N23 C24 1.341(4) . ? C24 C25 1.386(4) . ? C25 C26 1.379(6) . ? C25 H25 0.92(4) . ? C26 H26 0.93(5) . ? C27 H271 0.9600 . ? C27 H272 0.9600 . ? C27 H273 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu I Cu 104.050(13) . 1_554 ? N23 Cu N13 79.45(10) . . ? N23 Cu I 122.05(10) . . ? N13 Cu I 127.00(8) . . ? N23 Cu I 118.27(10) . 1_556 ? N13 Cu I 104.84(8) . 1_556 ? I Cu I 104.050(13) . 1_556 ? C16 N11 C12 116.6(3) . . ? N11 C12 N13 124.7(3) . . ? N11 C12 C17 117.5(3) . . ? N13 C12 C17 117.8(3) . . ? C12 N13 C14 117.7(3) . . ? C12 N13 Cu 127.4(2) . . ? C14 N13 Cu 113.00(19) . . ? N13 C14 C15 121.0(3) . . ? N13 C14 C24 115.4(3) . . ? C15 C14 C24 123.5(3) . . ? C16 C15 C14 116.9(3) . . ? C16 C15 H15 122(2) . . ? C14 C15 H15 121(2) . . ? N11 C16 C15 123.1(3) . . ? N11 C16 H16 115.8(19) . . ? C15 C16 H16 121(2) . . ? C12 C17 H171 109.5 . . ? C12 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C12 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C22 N21 C26 116.6(3) . . ? N21 C22 N23 124.8(3) . . ? N21 C22 C27 117.4(3) . . ? N23 C22 C27 117.8(3) . . ? C24 N23 C22 117.2(3) . . ? C24 N23 Cu 114.15(19) . . ? C22 N23 Cu 128.6(2) . . ? N23 C24 C25 121.9(3) . . ? N23 C24 C14 115.9(3) . . ? C25 C24 C14 122.2(3) . . ? C26 C25 C24 116.3(3) . . ? C26 C25 H25 118(2) . . ? C24 C25 H25 125(2) . . ? N21 C26 C25 123.1(3) . . ? N21 C26 H26 113(3) . . ? C25 C26 H26 124(3) . . ? C22 C27 H271 109.5 . . ? C22 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? C22 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 C14 C24 N23 10.9(4) . . . . ? #===END data_c046 #number 10 in dmbp-manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code Ag_dmbp_NO3_c046_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date ? _chemical_name_systematic ;\m-(2,2'-dimethyl-4,4'-bipyrimidine)-\m-nitrato-silver(I) ; _chemical_compound_source 'crstal provided by C. Janiak, Uni FR' _chemical_name_common [Ag(dmbp)(NO3)] _chemical_formula_moiety '(C10 H10 N4),(N O3),Ag' _chemical_formula_sum 'C10 H10 Ag N5 O3' _chemical_formula_weight 356.086 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' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 3.822(5) _cell_length_b 15.405(5) _cell_length_c 19.739(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1162.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 27.90 _cell_special_details ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035(3) _exptl_crystal_density_method none _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6961 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.1925 -1 0 0 0.1925 0 1 0 0.0096 0 -1 0 0.0096 0 0 1 0.0192 0 0 -1 0.0192 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.0 _diffr_source_voltage 50 _diffr_source_current 40 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation ? _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0 _kl_diffrn_detector_area_phi_end 118 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 6 _kl_diffrn_detector_area_plate_dist 60 _kl_diffrn_detector_area_eff_mos_spread ? _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min ? _kl_diffrn_detector_area_profile_max ? _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 5798 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.95 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.485 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.085 _reflns_number_total 1336 _reflns_number_gt 1040 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1336 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.0000 0.639033(17) 0.2500 0.02553(10) Uani 1 2 d S . . N5 N 0.3111(5) 0.59801(13) 0.46639(9) 0.0192(4) Uani 1 1 d . . . C6 C 0.1987(6) 0.63044(15) 0.40711(11) 0.0180(5) Uani 1 1 d . . . N1 N 0.2043(5) 0.58559(13) 0.34821(8) 0.0188(4) Uani 1 1 d . . . C4 C 0.4403(5) 0.51710(15) 0.46662(10) 0.0166(5) Uani 1 1 d . . . N8 N -0.5000 0.81977(19) 0.2500 0.0209(5) Uani 1 2 d S . . C7 C 0.0679(7) 0.72121(19) 0.40662(12) 0.0263(6) Uani 1 1 d . . . H71 H -0.094(10) 0.733(3) 0.377(2) 0.052(11) Uiso 1 1 d . . . H72 H -0.027(10) 0.740(3) 0.451(2) 0.061(12) Uiso 1 1 d . . . H73 H 0.242(14) 0.761(3) 0.397(2) 0.085(15) Uiso 1 1 d . . . O81 O -0.3355(7) 0.85963(16) 0.29377(12) 0.0479(6) Uani 1 1 d . . . O82 O -0.5000 0.73843(19) 0.2500 0.0426(7) Uani 1 2 d S . . C2 C 0.3355(7) 0.50545(17) 0.34909(11) 0.0204(5) Uani 1 1 d . . . H2 H 0.341(8) 0.4731(19) 0.3066(14) 0.023(7) Uiso 1 1 d . . . C3 C 0.4624(7) 0.46751(16) 0.40816(10) 0.0189(5) Uani 1 1 d . . . H3 H 0.549(8) 0.417(2) 0.4098(15) 0.028(8) Uiso 1 1 d . . . 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 Ag 0.03420(16) 0.02682(16) 0.01556(13) 0.000 -0.01050(10) 0.000 N5 0.0276(10) 0.0170(11) 0.0128(8) 0.0013(7) -0.0028(7) 0.0038(8) C6 0.0222(12) 0.0169(13) 0.0150(10) 0.0016(7) -0.0011(8) 0.0015(9) N1 0.0260(10) 0.0188(11) 0.0117(8) 0.0014(7) -0.0040(7) -0.0009(8) C4 0.0198(12) 0.0162(12) 0.0139(9) 0.0018(8) -0.0014(7) -0.0006(8) N8 0.0243(13) 0.0159(14) 0.0224(12) 0.000 -0.0020(12) 0.000 C7 0.0360(17) 0.0216(14) 0.0212(11) 0.0012(9) -0.0053(10) 0.0101(11) O81 0.0532(14) 0.0472(15) 0.0433(12) -0.0165(10) -0.0212(11) -0.0028(11) O82 0.0255(13) 0.0179(15) 0.084(2) 0.000 0.0023(15) 0.000 C2 0.0294(12) 0.0201(13) 0.0116(9) 0.0005(8) -0.0015(8) -0.0018(10) C3 0.0273(12) 0.0138(12) 0.0156(9) 0.0010(7) -0.0006(8) 0.0033(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.2461(18) 3 ? Ag N1 2.2461(18) . ? Ag O82 2.449(3) 1_655 ? Ag O82 2.449(3) . ? N5 C4 1.341(3) . ? N5 C6 1.343(3) . ? C6 N1 1.353(3) . ? C6 C7 1.485(4) . ? N1 C2 1.333(3) . ? C4 C3 1.386(3) . ? C4 C4 1.491(4) 5_666 ? N8 O81 1.232(3) . ? N8 O81 1.232(3) 3_455 ? N8 O82 1.253(4) . ? O82 Ag 2.449(3) 1_455 ? C2 C3 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N1 137.00(11) 3 . ? N1 Ag O82 120.03(5) 3 1_655 ? N1 Ag O82 87.59(7) . 1_655 ? N1 Ag O82 87.59(7) 3 . ? N1 Ag O82 120.03(5) . . ? O82 Ag O82 102.59(13) 1_655 . ? C4 N5 C6 117.82(19) . . ? N5 C6 N1 123.6(2) . . ? N5 C6 C7 117.6(2) . . ? N1 C6 C7 118.7(2) . . ? C2 N1 C6 117.89(18) . . ? C2 N1 Ag 118.79(14) . . ? C6 N1 Ag 123.31(16) . . ? N5 C4 C3 122.14(19) . . ? N5 C4 C4 116.4(2) . 5_666 ? C3 C4 C4 121.5(3) . 5_666 ? O81 N8 O81 120.2(4) . 3_455 ? O81 N8 O82 119.89(18) . . ? O81 N8 O82 119.89(18) 3_455 . ? N8 O82 Ag 128.70(7) . 1_455 ? N8 O82 Ag 128.70(7) . . ? Ag O82 Ag 102.59(13) 1_455 . ? N1 C2 C3 122.1(2) . . ? C4 C3 C2 116.4(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C4 C4 N5 -180.00(19) . . 5_666 5_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C2 H2 O81 0.98(3) 2.59(3) 3.145(5) 116(2) 8_655 ? _geom_special_details ? #===END data_dmbp12 #number 11 in dmbp-manuscript _audit_creation_method SHELXL _chemical_name_systematic ;bis(\m3-2,2'-dimethyl-4,4'-bipyrimidine)-tris(\m3-nitrato)-trisilver(I) ; _chemical_name_common '[Ag3 (N O3)3 (C10 H10 N4)2]' _chemical_formula_moiety '3Ag, 3(N O3), 2(C10 H10 N4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Ag1.50 N5.50 O4.50' _chemical_formula_weight 441.04 _chemical_melting_point ? _chemical_compound_source 'C. Janiak, Uni Freiburg' 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' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pcna' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z+1/2' 'x+1/2, -y, z+1/2' 'x+1/2, y, -z' '-x, -y, -z' 'x, -y, -z-1/2' '-x-1/2, y, -z-1/2' '-x-1/2, -y, z' _cell_length_a 7.068(8) _cell_length_b 21.811(15) _cell_length_c 19.408(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2992.1(46) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.009 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Syntex P21' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3483 _diffrn_reflns_av_R_equivalents 0.5884 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3453 _reflns_number_observed 1130 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 46 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3407 _refine_ls_number_parameters 212 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2154 _refine_ls_R_factor_obs 0.0973 _refine_ls_wR_factor_all 0.3477 _refine_ls_wR_factor_obs 0.2336 _refine_ls_goodness_of_fit_all 1.454 _refine_ls_goodness_of_fit_obs 2.002 _refine_ls_restrained_S_all 1.652 _refine_ls_restrained_S_obs 2.065 _refine_ls_shift/esd_max 0.009 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.2500 0.0000 0.2500 0.0713(9) Uani 1 d S . Ag2 Ag -0.2500 0.5000 0.2500 0.0734(9) Uani 1 d S . Ag3 Ag 0.0001(4) 0.25052(5) 0.09145(6) 0.0809(4) Uani 1 d . . C11 C 0.2154(23) 0.0327(7) 0.0869(7) 0.066(5) Uani 1 d . . N11 N 0.1628(17) 0.0583(4) 0.1499(6) 0.054(4) Uani 1 d . . C12 C 0.0925(24) 0.1160(5) 0.1476(9) 0.059(5) Uani 1 d . . N12 N 0.0864(19) 0.1524(5) 0.0900(7) 0.064(4) Uani 1 d . . C13 C 0.1480(28) 0.1292(6) 0.0318(9) 0.077(6) Uani 1 d . . H13 H 0.1531(28) 0.1548(6) -0.0065(9) 0.080 Uiso 1 calc R . C14 C 0.2079(30) 0.0668(5) 0.0234(9) 0.076(6) Uani 1 d . . H14 H 0.2391(30) 0.0499(5) -0.0191(9) 0.080 Uiso 1 calc R . C15 C 0.0222(27) 0.1454(5) 0.2139(9) 0.079(6) Uani 1 d . . H151 H -0.0950(66) 0.1662(34) 0.2053(14) 0.080 Uiso 1 calc R . H152 H 0.1145(59) 0.1742(30) 0.2303(25) 0.080 Uiso 1 calc R . H153 H 0.0027(124) 0.1142(7) 0.2481(17) 0.080 Uiso 1 calc R . C21 C -0.2145(24) 0.4686(4) 0.0876(8) 0.061(5) Uani 1 d . . N21 N -0.1575(20) 0.4420(6) 0.1488(7) 0.068(4) Uani 1 d . . C22 C -0.0947(27) 0.3820(6) 0.1492(10) 0.067(6) Uani 1 d . . N22 N -0.0868(22) 0.3479(4) 0.0900(8) 0.073(5) Uani 1 d . . C23 C -0.1479(25) 0.3734(6) 0.0294(9) 0.067(5) Uani 1 d . . H23 H -0.1478(25) 0.3497(6) -0.0104(9) 0.080 Uiso 1 calc R . C24 C -0.2094(26) 0.4330(5) 0.0263(8) 0.064(5) Uani 1 d . . H24 H -0.2472(26) 0.4499(5) -0.0154(8) 0.080 Uiso 1 calc R . C25 C -0.0176(26) 0.3561(7) 0.2158(9) 0.082(6) Uani 1 d . . H251 H 0.1177(27) 0.3534(34) 0.2130(18) 0.080 Uiso 1 calc R . H252 H -0.0696(91) 0.3160(18) 0.2234(23) 0.080 Uiso 1 calc R . H253 H -0.0520(101) 0.3825(22) 0.2533(10) 0.080 Uiso 1 calc R . N1 N -0.5020(31) 0.2489(8) 0.1159(6) 0.086(3) Uani 1 d D . O1 O -0.3723(29) 0.2255(11) 0.1485(11) 0.218(11) Uani 1 d D . O2 O -0.6340(29) 0.2727(9) 0.1498(12) 0.192(10) Uani 1 d D . O3 O -0.4977(50) 0.2513(8) 0.0517(6) 0.188(9) Uani 1 d D . N2 N 0.7500 0.0000 0.1806(10) 0.041(7) Uani 0.50 d SPD . O4 O 0.6757(33) 0.0525(9) 0.1436(10) 0.090(8) Uani 0.50 d PD . O5 O 0.7500 0.0000 0.2488(17) 0.112(9) Uiso 1 d SD -1 N3 N 0.2500 0.5000 0.1652(22) 0.302(77) Uani 0.50 d SPD . O6 O 0.3332(41) 0.4466(13) 0.1392(12) 0.121(13) Uani 0.50 d PD . O7 O 0.2500 0.5000 0.2340(24) 0.162(20) Uiso 0.50 d SPD -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.099(2) 0.0419(11) 0.073(2) 0.000 0.000 0.000 Ag2 0.089(2) 0.0651(14) 0.066(2) 0.000 0.000 0.000 Ag3 0.0983(8) 0.0422(5) 0.1021(8) -0.0003(11) -0.001(2) 0.0182(4) C11 0.050(11) 0.092(11) 0.057(8) -0.016(8) 0.004(9) 0.021(9) N11 0.059(8) 0.015(3) 0.090(9) 0.011(5) 0.013(8) 0.002(5) C12 0.058(11) 0.042(6) 0.077(11) -0.002(8) -0.005(10) 0.007(7) N12 0.063(10) 0.049(6) 0.080(10) 0.004(7) 0.012(9) 0.016(6) C13 0.102(16) 0.043(7) 0.087(14) -0.017(9) -0.010(13) 0.012(9) C14 0.098(18) 0.050(7) 0.079(12) 0.003(9) 0.009(13) 0.013(10) C15 0.097(15) 0.028(5) 0.110(15) 0.006(8) 0.012(13) 0.011(9) C21 0.069(12) 0.017(5) 0.096(12) -0.006(6) 0.022(11) -0.007(6) N21 0.058(10) 0.082(8) 0.064(8) 0.015(8) 0.006(9) 0.006(8) C22 0.068(14) 0.041(7) 0.092(13) -0.009(9) -0.014(12) 0.003(8) N22 0.091(13) 0.024(5) 0.103(13) -0.008(7) 0.007(11) 0.009(6) C23 0.072(13) 0.052(7) 0.077(13) -0.018(9) -0.013(11) 0.010(8) C24 0.073(14) 0.047(6) 0.073(11) -0.002(8) 0.012(11) 0.009(9) C25 0.067(12) 0.092(11) 0.085(14) -0.005(11) -0.025(12) 0.014(11) N1 0.086(8) 0.078(8) 0.094(8) 0.015(13) -0.002(18) 0.017(6) O1 0.140(19) 0.323(23) 0.191(21) 0.154(19) 0.012(17) 0.092(19) O2 0.135(19) 0.232(17) 0.208(23) -0.124(17) -0.027(18) 0.063(17) O3 0.405(27) 0.097(9) 0.063(7) 0.000(11) 0.013(24) 0.070(12) N2 0.082(21) 0.020(9) 0.020(10) 0.000 0.000 -0.007(12) O4 0.063(17) 0.126(18) 0.080(16) -0.054(15) 0.019(15) -0.025(15) N3 0.140(75) 0.633(224) 0.131(69) 0.000 0.000 -0.214(109) O6 0.049(17) 0.248(36) 0.066(15) 0.077(22) 0.000(15) -0.015(22) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.403(11) 7_656 ? Ag1 N11 2.403(11) 8_655 ? Ag1 N11 2.403(11) . ? Ag1 N11 2.403(11) 6_556 ? Ag2 N21 2.426(13) 8_565 ? Ag2 N21 2.426(13) . ? Ag2 N21 2.426(13) 6_566 ? Ag2 N21 2.426(13) 7_556 ? Ag3 N22 2.212(10) . ? Ag3 N12 2.226(10) . ? C11 N11 1.39(2) . ? C11 C14 1.44(2) . ? C11 C11 1.51(3) 8_655 ? N11 C12 1.354(14) . ? C12 N12 1.37(2) . ? C12 C15 1.52(2) . ? N12 C13 1.31(2) . ? C13 C14 1.43(2) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H151 0.96 . ? C15 H152 0.96 . ? C15 H153 0.96 . ? C21 N21 1.38(2) . ? C21 C24 1.42(2) . ? C21 C21 1.46(2) 8_565 ? N21 C22 1.38(2) . ? C22 N22 1.37(2) . ? C22 C25 1.51(2) . ? N22 C23 1.37(2) . ? C23 C24 1.37(2) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 H251 0.96 . ? C25 H252 0.96 . ? C25 H253 0.96 . ? N1 O1 1.23(2) . ? N1 O3 1.247(15) . ? N1 O2 1.25(2) . ? N2 O5 1.32(3) . ? N2 O4 1.45(2) 8_755 ? N2 O4 1.45(2) . ? O5 N2 1.37(5) 6_556 ? N3 O7 1.34(2) . ? N3 O6 1.40(2) 8_665 ? N3 O6 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag1 N11 150.3(6) 7_656 8_655 ? N11 Ag1 N11 116.1(5) 7_656 . ? N11 Ag1 N11 72.1(5) 8_655 . ? N11 Ag1 N11 72.1(5) 7_656 6_556 ? N11 Ag1 N11 116.1(5) 8_655 6_556 ? N11 Ag1 N11 150.3(6) . 6_556 ? N21 Ag2 N21 71.8(6) 8_565 . ? N21 Ag2 N21 117.2(6) 8_565 6_566 ? N21 Ag2 N21 148.7(7) . 6_566 ? N21 Ag2 N21 148.7(7) 8_565 7_556 ? N21 Ag2 N21 117.2(6) . 7_556 ? N21 Ag2 N21 71.8(6) 6_566 7_556 ? N22 Ag3 N12 178.5(4) . . ? N11 C11 C14 122.2(12) . . ? N11 C11 C11 117.8(7) . 8_655 ? C14 C11 C11 120.0(8) . 8_655 ? C12 N11 C11 116.3(13) . . ? C12 N11 Ag1 127.8(11) . . ? C11 N11 Ag1 115.3(8) . . ? N11 C12 N12 125.2(15) . . ? N11 C12 C15 118.9(14) . . ? N12 C12 C15 115.9(11) . . ? C13 N12 C12 117.9(12) . . ? C13 N12 Ag3 118.2(10) . . ? C12 N12 Ag3 123.7(10) . . ? N12 C13 C14 124.1(16) . . ? N12 C13 H13 117.9(8) . . ? C14 C13 H13 117.9(11) . . ? C13 C14 C11 113.8(15) . . ? C13 C14 H14 123.1(11) . . ? C11 C14 H14 123.1(8) . . ? C12 C15 H151 109.5(9) . . ? C12 C15 H152 109.5(9) . . ? H151 C15 H152 109.5 . . ? C12 C15 H153 109.5(7) . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? N21 C21 C24 118.8(10) . . ? N21 C21 C21 119.7(7) . 8_565 ? C24 C21 C21 121.5(9) . 8_565 ? C21 N21 C22 119.8(14) . . ? C21 N21 Ag2 113.5(9) . . ? C22 N21 Ag2 125.1(11) . . ? N22 C22 N21 121.4(16) . . ? N22 C22 C25 120.0(13) . . ? N21 C22 C25 118.3(15) . . ? C23 N22 C22 119.2(11) . . ? C23 N22 Ag3 119.2(10) . . ? C22 N22 Ag3 121.4(11) . . ? N22 C23 C24 121.4(14) . . ? N22 C23 H23 119.3(7) . . ? C24 C23 H23 119.3(10) . . ? C23 C24 C21 119.3(15) . . ? C23 C24 H24 120.3(10) . . ? C21 C24 H24 120.3(8) . . ? C22 C25 H251 109.5(10) . . ? C22 C25 H252 109.5(9) . . ? H251 C25 H252 109.5 . . ? C22 C25 H253 109.5(9) . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? O1 N1 O3 121.1(25) . . ? O1 N1 O2 117.2(16) . . ? O3 N1 O2 121.6(25) . . ? O5 N2 O4 119.6(11) . 8_755 ? O5 N2 O4 119.6(11) . . ? O4 N2 O4 120.7(22) 8_755 . ? N2 O5 N2 180.000(1) . 6_556 ? O7 N3 O6 111.1(21) . 8_665 ? O7 N3 O6 111.1(21) . . ? O6 N3 O6 137.7(42) 8_665 . ? _refine_diff_density_max 1.295 _refine_diff_density_min -1.759 _refine_diff_density_rms 0.232 #===END data_c069 #number 12 in dmbp-manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code Ag_dmbp_BF4_c069_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 02-May-1998 _chemical_name_systematic ;tris(acetonitrile)-bis(\m-2,2'-dimethyl-4,4'-bipyrimidine)-trisilver(I) tetrafluoroborate ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common '[(C10 H10 N4)2 Ag3](BF4)3 . 3 CH3CN' _chemical_formula_moiety '2(C10 H10 N4), 3Ag, 3(B F4), 3(C2 H3 N)' _chemical_formula_sum 'C26 H29 Ag3 B3 F12 N11' _chemical_formula_weight 1079.601 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.1706(11) _cell_length_b 10.8107(7) _cell_length_c 21.3415(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.697(7) _cell_angle_gamma 90.00 _cell_volume 3729.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.95 _cell_special_details ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.9227(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.2002 0 0 1 0.1540 0 1 -3 0.1617 1 0 1 0.1155 0 1 1 0.2310 0 -3 -1 0.1925 -2 1 1 0.2695 2 -1 -1 0.2310 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.0 _diffr_source_voltage 50 _diffr_source_current 40 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.8 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0 _kl_diffrn_detector_area_phi_end 243.2 _kl_diffrn_detector_area_phi_incr 0.8 _kl_diffrn_detector_area_expos_time 0.6 _kl_diffrn_detector_area_plate_dist 60 _kl_diffrn_detector_area_eff_mos_spread 0.010 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 19 _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 21256 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.92 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.963 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.098 _reflns_number_total 4440 _reflns_number_gt 4054 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4440 _refine_ls_number_parameters 275 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ;aromatic H: geom, refU, CH3-H: constr, U(H) = 1.5*U(C(pivot)) The BF4 group with B2 is fourfold disordered and is an entity of apparent D2h symmetry. Inversion centre cryst., orientation of one of the mirror planes (-1 -1 3), other planes and directions of twofold axes have higher indices. The B2_F4 moiety is located inside a hydrophobic channel without well-defined bonding sites for an anion. 1 of 3 acetonitrile on a twofold axis, the hydrogen atoms are thus disordered. ; 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.089996(12) 0.405142(17) 0.226303(9) 0.02504(7) Uani 1 1 d . . . Ag2 Ag -0.2500 -0.14748(3) 0.5000 0.02742(8) Uani 1 2 d S . . N11 N 0.06109(13) 0.26385(19) 0.29131(10) 0.0216(4) Uani 1 1 d . . . C21 C 0.01163(15) 0.1659(2) 0.26756(12) 0.0211(4) Uani 1 1 d . . . N31 N -0.02601(13) 0.10236(18) 0.30290(10) 0.0200(4) Uani 1 1 d . . . C41 C -0.01312(14) 0.1368(2) 0.36602(11) 0.0183(4) Uani 1 1 d . . . C51 C 0.03983(15) 0.2327(2) 0.39517(11) 0.0218(4) Uani 1 1 d . . . H51 H 0.0506 0.2546 0.4394 0.025(7) Uiso 1 1 calc R . . C61 C 0.07619(15) 0.2947(2) 0.35531(12) 0.0232(5) Uani 1 1 d . . . H61 H 0.1122 0.3598 0.3734 0.019(7) Uiso 1 1 calc R . . C71 C -0.0032(2) 0.1264(3) 0.19735(13) 0.0337(6) Uani 1 1 d . . . H71A H 0.0270 0.0517 0.1972 0.051 Uiso 1 1 calc R . . H71B H 0.0151 0.1902 0.1743 0.051 Uiso 1 1 calc R . . H71C H -0.0612 0.1118 0.1754 0.051 Uiso 1 1 calc R . . N12 N -0.15479(13) -0.0585(2) 0.46125(10) 0.0224(4) Uani 1 1 d . . . C22 C -0.14079(16) -0.0998(2) 0.40629(12) 0.0221(5) Uani 1 1 d . . . N32 N -0.09421(12) -0.04078(19) 0.37678(10) 0.0200(4) Uani 1 1 d . . . C42 C -0.06099(14) 0.0688(2) 0.40182(11) 0.0184(4) Uani 1 1 d . . . C52 C -0.07312(16) 0.1186(2) 0.45809(12) 0.0225(5) Uani 1 1 d . . . H52 H -0.0501 0.1940 0.4759 0.029(8) Uiso 1 1 calc R . . C62 C -0.12118(16) 0.0501(2) 0.48610(12) 0.0237(5) Uani 1 1 d . . . H62 H -0.1304 0.0809 0.5237 0.032(9) Uiso 1 1 calc R . . C72 C -0.1811(2) -0.2180(3) 0.37586(15) 0.0361(6) Uani 1 1 d . . . H72A H -0.1650 -0.2377 0.3381 0.054 Uiso 1 1 calc R . . H72B H -0.2401 -0.2089 0.3619 0.054 Uiso 1 1 calc R . . H72C H -0.1640 -0.2833 0.4081 0.054 Uiso 1 1 calc R . . N18 N 0.2113(2) 0.4822(3) 0.31517(17) 0.0555(8) Uani 1 1 d . . . C18 C 0.2611(2) 0.5542(3) 0.32142(16) 0.0405(7) Uani 1 1 d . . . C28 C 0.3252(3) 0.6472(4) 0.3304(2) 0.0620(11) Uani 1 1 d . . . H28A H 0.3060 0.7252 0.3410 0.093 Uiso 1 1 calc R . . H28B H 0.3378 0.6552 0.2900 0.093 Uiso 1 1 calc R . . H28C H 0.3740 0.6227 0.3660 0.093 Uiso 1 1 calc R . . C19 C -0.2500 -0.4632(4) 0.5000 0.0382(9) Uani 1 2 d S . . N19 N -0.2500 -0.3577(3) 0.5000 0.0385(8) Uani 1 2 d S . . C29 C -0.2500 -0.5979(5) 0.5000 0.072(2) Uani 1 2 d S . . H29A H -0.2751 -0.6275 0.5311 0.109 Uiso 0.50 1 calc PR . . H29B H -0.1941 -0.6275 0.5127 0.109 Uiso 0.50 1 calc PR . . H29C H -0.2808 -0.6275 0.4562 0.109 Uiso 0.50 1 calc PR . . B2 B 0.5000 0.0000 0.0000 0.0560(16) Uani 1 2 d SD . . F12 F 0.5258(13) 0.1198(8) -0.0048(9) 0.096(4) Uiso 0.25 1 d PD . . F22 F 0.5573(9) -0.0945(11) 0.0278(6) 0.082(4) Uiso 0.25 1 d PD . . F32 F 0.4564(8) 0.0029(12) 0.0470(5) 0.073(3) Uiso 0.25 1 d PD . . F42 F 0.4416(7) -0.0519(13) -0.0569(5) 0.082(4) Uiso 0.25 1 d PD . . F52 F 0.5198(8) -0.1208(6) 0.0243(4) 0.0456(19) Uiso 0.25 1 d PD . . F62 F 0.4348(6) -0.0809(11) -0.0312(7) 0.068(3) Uiso 0.25 1 d PD . . F72 F 0.5026(9) 0.0105(13) 0.0672(4) 0.082(3) Uiso 0.25 1 d PD . . F82 F 0.5799(5) -0.0358(16) 0.0037(9) 0.106(4) Uiso 0.25 1 d PD . . B1 B 0.3302(2) 0.5877(3) 0.15140(16) 0.0326(7) Uani 1 1 d . . . F11 F 0.39956(13) 0.6148(2) 0.20531(11) 0.0550(6) Uani 1 1 d . . . F21 F 0.26329(13) 0.5737(3) 0.17312(12) 0.0608(6) Uani 1 1 d . . . F31 F 0.34254(12) 0.47696(18) 0.12194(9) 0.0438(4) Uani 1 1 d . . . F41 F 0.3133(2) 0.6789(2) 0.10402(13) 0.0802(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03307(12) 0.02117(11) 0.02579(11) 0.00701(6) 0.01637(8) 0.00178(7) Ag2 0.03236(15) 0.02552(15) 0.03375(15) 0.000 0.02347(12) 0.000 N11 0.0238(10) 0.0200(9) 0.0231(9) 0.0045(8) 0.0105(8) 0.0000(8) C21 0.0246(11) 0.0186(10) 0.0225(10) 0.0016(8) 0.0109(9) 0.0016(9) N31 0.0240(10) 0.0173(9) 0.0215(9) 0.0005(7) 0.0112(8) 0.0002(8) C41 0.0207(10) 0.0172(10) 0.0198(10) 0.0033(8) 0.0105(8) 0.0032(9) C51 0.0267(11) 0.0203(11) 0.0194(10) -0.0001(8) 0.0091(9) -0.0001(9) C61 0.0259(11) 0.0205(11) 0.0232(11) 0.0018(9) 0.0083(9) -0.0043(9) C71 0.0510(17) 0.0314(13) 0.0261(12) -0.0049(11) 0.0228(12) -0.0108(13) N12 0.0255(10) 0.0227(10) 0.0234(9) 0.0019(8) 0.0142(8) 0.0021(8) C22 0.0261(11) 0.0194(11) 0.0244(11) 0.0005(9) 0.0131(9) 0.0001(9) N32 0.0222(9) 0.0186(9) 0.0233(9) 0.0001(7) 0.0132(7) 0.0001(8) C42 0.0198(10) 0.0169(10) 0.0204(10) 0.0008(8) 0.0092(8) 0.0023(8) C52 0.0275(12) 0.0209(11) 0.0221(11) -0.0031(9) 0.0122(9) -0.0015(10) C62 0.0300(12) 0.0237(11) 0.0211(10) -0.0006(9) 0.0138(9) 0.0007(10) C72 0.0510(17) 0.0276(13) 0.0435(15) -0.0103(12) 0.0340(14) -0.0142(13) N18 0.0454(16) 0.0493(18) 0.0593(18) 0.0074(15) 0.0009(14) -0.0134(15) C18 0.0377(16) 0.0416(17) 0.0379(15) -0.0029(13) 0.0072(12) -0.0041(14) C28 0.062(2) 0.066(3) 0.066(2) -0.028(2) 0.032(2) -0.031(2) C19 0.056(3) 0.028(2) 0.0316(19) 0.000 0.0153(18) 0.000 N19 0.054(2) 0.0244(17) 0.0405(19) 0.000 0.0207(17) 0.000 C29 0.129(6) 0.022(2) 0.067(4) 0.000 0.034(4) 0.000 B2 0.059(4) 0.037(3) 0.062(4) -0.018(3) 0.007(3) 0.008(3) B1 0.0313(15) 0.0367(17) 0.0316(15) -0.0019(12) 0.0129(12) 0.0032(13) F11 0.0336(10) 0.0685(14) 0.0573(12) -0.0196(11) 0.0081(9) -0.0102(10) F21 0.0406(11) 0.0926(18) 0.0569(13) -0.0292(12) 0.0265(10) -0.0159(11) F31 0.0421(10) 0.0404(10) 0.0460(10) -0.0068(8) 0.0111(8) 0.0083(8) F41 0.133(3) 0.0507(14) 0.0629(15) 0.0212(12) 0.0411(16) 0.0292(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.2290(19) . ? Ag1 N32 2.3009(19) 4_455 ? Ag1 N31 2.383(2) 4_455 ? Ag1 N18 2.442(3) . ? Ag2 N19 2.272(4) . ? Ag2 N12 2.279(2) 2_456 ? Ag2 N12 2.279(2) . ? N11 C61 1.344(3) . ? N11 C21 1.345(3) . ? C21 N31 1.337(3) . ? C21 C71 1.495(3) . ? N31 C41 1.342(3) . ? N31 Ag1 2.383(2) 4_445 ? C41 C51 1.381(3) . ? C41 C42 1.491(3) . ? C51 C61 1.386(3) . ? N12 C62 1.336(3) . ? N12 C22 1.350(3) . ? C22 N32 1.335(3) . ? C22 C72 1.493(4) . ? N32 C42 1.345(3) . ? N32 Ag1 2.3009(19) 4_445 ? C42 C52 1.394(3) . ? C52 C62 1.385(3) . ? N18 C18 1.131(5) . ? C18 C28 1.455(5) . ? C19 N19 1.141(6) . ? C19 C29 1.456(6) . ? B2 F12 1.384(6) . ? B2 F12 1.384(6) 5_655 ? B2 F62 1.399(5) 5_655 ? B2 F62 1.399(5) . ? B2 F82 1.401(6) 5_655 ? B2 F82 1.401(6) . ? B2 F22 1.404(6) 5_655 ? B2 F22 1.404(6) . ? B2 F52 1.405(5) 5_655 ? B2 F52 1.405(5) . ? B2 F42 1.405(6) 5_655 ? B2 F42 1.405(6) . ? B1 F41 1.372(4) . ? B1 F11 1.380(4) . ? B1 F21 1.384(4) . ? B1 F31 1.401(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag1 N32 148.71(8) . 4_455 ? N11 Ag1 N31 126.59(7) . 4_455 ? N32 Ag1 N31 71.51(7) 4_455 4_455 ? N11 Ag1 N18 93.49(9) . . ? N32 Ag1 N18 111.25(10) 4_455 . ? N31 Ag1 N18 95.45(10) 4_455 . ? N19 Ag2 N12 114.98(5) . 2_456 ? N19 Ag2 N12 114.98(5) . . ? N12 Ag2 N12 130.05(11) 2_456 . ? C61 N11 C21 117.4(2) . . ? C61 N11 Ag1 117.08(16) . . ? C21 N11 Ag1 123.34(15) . . ? N31 C21 N11 123.8(2) . . ? N31 C21 C71 117.8(2) . . ? N11 C21 C71 118.4(2) . . ? C21 N31 C41 118.4(2) . . ? C21 N31 Ag1 125.47(16) . 4_445 ? C41 N31 Ag1 114.60(15) . 4_445 ? N31 C41 C51 121.4(2) . . ? N31 C41 C42 116.4(2) . . ? C51 C41 C42 122.2(2) . . ? C41 C51 C61 116.8(2) . . ? N11 C61 C51 122.1(2) . . ? C62 N12 C22 117.1(2) . . ? C62 N12 Ag2 119.58(16) . . ? C22 N12 Ag2 122.34(17) . . ? N32 C22 N12 124.2(2) . . ? N32 C22 C72 117.8(2) . . ? N12 C22 C72 118.0(2) . . ? C22 N32 C42 118.3(2) . . ? C22 N32 Ag1 123.12(16) . 4_445 ? C42 N32 Ag1 117.25(15) . 4_445 ? N32 C42 C52 121.1(2) . . ? N32 C42 C41 117.65(19) . . ? C52 C42 C41 121.3(2) . . ? C62 C52 C42 116.7(2) . . ? N12 C62 C52 122.6(2) . . ? C18 N18 Ag1 137.7(3) . . ? N18 C18 C28 179.2(4) . . ? N19 C19 C29 180.000(1) . . ? C19 N19 Ag2 180.000(1) . . ? F41 B1 F11 111.7(3) . . ? F41 B1 F21 109.4(3) . . ? F11 B1 F21 108.9(3) . . ? F41 B1 F31 108.0(3) . . ? F11 B1 F31 109.7(3) . . ? F21 B1 F31 109.0(3) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 C41 C42 N32 18.2(3) . . . . ? _geom_special_details ? #===END data_c068 #number 13 in dmbp-manuscript _audit_author_name 'Piotrowski, H.' _audit_block_code Ag_dmbp_PF6_c068_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 01-May-98 _chemical_name_systematic ;tris(acetonitrile)-bis(\m-2,2'-dimethyl-4,4'-bipyrimidine)-trisilver(I) hexafluorophosphate ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common '[(C10 H10 N4)2 Ag3](PF6)3 . 3 CH3CN' _chemical_formula_moiety '2(C10 H10 N4), 3Ag, 3(P F6), 3(C2 H3 N)' _chemical_formula_sum 'C26 H29 Ag3 P3 F18 N11' _chemical_formula_weight 1254.080 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.3846(11) _cell_length_b 10.9689(10) _cell_length_c 21.9716(14) _cell_angle_alpha 90.00 _cell_angle_beta 105.148(7) _cell_angle_gamma 90.00 _cell_volume 4044.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.95 _cell_special_details ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.0597(3) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 1.678 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.1925 0 0 1 0.1925 1 0 0 0.2695 0 -1 1 0.2695 -1 0 -1 0.2310 0 1 -2 0.2695 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.0 _diffr_source_voltage 50 _diffr_source_current 40 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.8 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0 _kl_diffrn_detector_area_phi_end 180.8 _kl_diffrn_detector_area_phi_incr 0.8 _kl_diffrn_detector_area_expos_time 0.6 _kl_diffrn_detector_area_plate_dist 60 _kl_diffrn_detector_area_eff_mos_spread 0.012 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 15 _kl_diffrn_detector_area_profile_max 19 _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 17161 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.88 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.001 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.122 _reflns_number_total 4568 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4568 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_special_details ;aromatic H: geom, refU, CH3-H: constr, U(H) = 1.5*U(C(pivot)). The PF6 group with P1 is twofold disordered. A form is transformed to its respective counterpart by the action of a C2h symmmetry group. The mirror plane coincides approximately with the crystal (8 1 3) plane. The P1_F6 moiety is located inside a hydrophobic channel without well-defined bonding sites for an anion. 1 of 3 acetonitrile on a twofold axis, the hydrogen atoms are thus disordered. ; 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.2500 0.33292(2) 0.5000 0.03721(6) Uani 1 2 d S . . Ag2 Ag 0.092575(11) 0.903529(15) 0.229837(8) 0.03313(4) Uani 1 1 d . . . N11 N 0.05347(11) 0.76069(16) 0.28874(8) 0.0276(4) Uani 1 1 d . . . C21 C 0.00817(13) 0.66374(18) 0.26600(10) 0.0263(4) Uani 1 1 d . . . N31 N -0.02941(11) 0.59588(15) 0.30029(8) 0.0245(4) Uani 1 1 d . . . C41 C -0.01955(12) 0.62471(18) 0.36099(9) 0.0237(4) Uani 1 1 d . . . C51 C 0.02976(13) 0.7192(2) 0.38907(10) 0.0288(5) Uani 1 1 d . . . H51 H 0.0388 0.7372 0.4327 0.027(6) Uiso 1 1 calc R . . C61 C 0.06537(13) 0.7862(2) 0.35031(10) 0.0302(5) Uani 1 1 d . . . H61 H 0.0993 0.8523 0.3679 0.029(6) Uiso 1 1 calc R . . C71 C -0.00058(16) 0.6274(2) 0.19913(10) 0.0349(5) Uani 1 1 d . . . H71A H 0.0017 0.7002 0.1738 0.052 Uiso 1 1 calc R . . H71B H -0.0519 0.5864 0.1828 0.052 Uiso 1 1 calc R . . H71C H 0.0427 0.5718 0.1969 0.052 Uiso 1 1 calc R . . N12 N -0.15708(11) 0.41956(17) 0.45720(9) 0.0297(4) Uani 1 1 d . . . C22 C -0.14444(13) 0.38544(19) 0.40158(10) 0.0281(4) Uani 1 1 d . . . N32 N -0.09986(10) 0.44802(16) 0.37135(8) 0.0254(4) Uani 1 1 d . . . C42 C -0.06639(12) 0.55261(18) 0.39689(9) 0.0241(4) Uani 1 1 d . . . C52 C -0.07659(14) 0.5943(2) 0.45398(10) 0.0302(5) Uani 1 1 d . . . H52 H -0.0528 0.6680 0.4726 0.054(9) Uiso 1 1 calc R . . C62 C -0.12318(14) 0.5234(2) 0.48241(10) 0.0322(5) Uani 1 1 d . . . H62 H -0.1313 0.5497 0.5214 0.051(9) Uiso 1 1 calc R . . C72 C -0.18421(16) 0.2720(2) 0.37112(12) 0.0416(6) Uani 1 1 d . . . H72A H -0.2387 0.2911 0.3470 0.062 Uiso 1 1 calc R . . H72B H -0.1857 0.2116 0.4037 0.062 Uiso 1 1 calc R . . H72C H -0.1543 0.2389 0.3427 0.062 Uiso 1 1 calc R . . C28 C 0.32325(18) 1.1334(3) 0.33291(15) 0.0519(8) Uani 1 1 d . . . H28A H 0.3747 1.0932 0.3370 0.078 Uiso 1 1 calc R . . H28B H 0.3234 1.1740 0.3727 0.078 Uiso 1 1 calc R . . H28C H 0.3143 1.1939 0.2990 0.078 Uiso 1 1 calc R . . C18 C 0.25991(18) 1.0429(3) 0.31825(13) 0.0456(7) Uani 1 1 d . . . N18 N 0.21046(18) 0.9733(3) 0.30586(14) 0.0600(8) Uani 1 1 d . . . N19 N -0.2500 0.1287(3) 0.5000 0.0708(11) Uani 1 2 d S . . C19 C -0.2500 0.0262(4) 0.5000 0.0619(11) Uani 1 2 d S . . C29 C -0.2500 -0.1053(4) 0.5000 0.095(2) Uani 1 2 d S . . H29A H -0.2857 -0.1351 0.4606 0.143 Uiso 0.50 1 calc PR . . H29B H -0.2685 -0.1351 0.5358 0.143 Uiso 0.50 1 calc PR . . H29C H -0.1958 -0.1351 0.5036 0.143 Uiso 0.50 1 calc PR . . P1 P 0.0000 0.5000 0.0000 0.0419(2) Uani 1 2 d S . . F11A F -0.0434(3) 0.4845(4) 0.0562(2) 0.0658(10) Uiso 0.50 1 d P . . F21A F 0.0817(4) 0.4431(7) 0.0372(3) 0.113(2) Uiso 0.50 1 d P . . F31A F 0.0217(3) 0.6381(5) 0.0189(3) 0.0887(14) Uiso 0.50 1 d P . . F11B F 0.0689(4) 0.5973(5) 0.0221(3) 0.0934(16) Uiso 0.50 1 d P . . F21B F -0.0545(3) 0.6178(5) -0.0135(2) 0.0755(12) Uiso 0.50 1 d P . . F31B F -0.0051(2) 0.4915(3) 0.07109(18) 0.0544(9) Uiso 0.50 1 d P . . P2 P 0.33458(4) 0.10145(6) 0.15017(3) 0.03362(14) Uani 1 1 d . . . F12 F 0.33150(11) -0.03374(15) 0.12211(9) 0.0549(4) Uani 1 1 d . . . F22 F 0.25548(10) 0.07656(17) 0.17176(9) 0.0526(4) Uani 1 1 d . . . F32 F 0.28211(11) 0.14640(18) 0.08332(8) 0.0572(5) Uani 1 1 d . . . F42 F 0.41382(10) 0.12430(17) 0.12726(9) 0.0547(4) Uani 1 1 d . . . F52 F 0.38769(13) 0.0547(3) 0.21589(9) 0.0855(7) Uani 1 1 d . . . F62 F 0.33828(11) 0.23565(17) 0.17761(11) 0.0696(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04414(11) 0.03310(11) 0.04524(11) 0.000 0.03103(9) 0.000 Ag2 0.04448(9) 0.02868(8) 0.03171(8) 0.00889(6) 0.01969(7) 0.00297(6) N11 0.0346(8) 0.0239(8) 0.0281(7) 0.0033(6) 0.0151(7) -0.0002(7) C21 0.0333(9) 0.0241(9) 0.0251(8) 0.0044(7) 0.0138(8) 0.0055(7) N31 0.0289(8) 0.0247(8) 0.0231(7) 0.0016(6) 0.0123(6) 0.0020(6) C41 0.0270(8) 0.0232(8) 0.0245(8) 0.0022(7) 0.0129(7) 0.0033(7) C51 0.0359(10) 0.0289(9) 0.0241(8) -0.0018(7) 0.0122(8) -0.0033(8) C61 0.0357(10) 0.0259(9) 0.0317(9) -0.0006(8) 0.0137(9) -0.0034(8) C71 0.0488(12) 0.0355(11) 0.0249(9) 0.0011(8) 0.0173(9) -0.0013(10) N12 0.0343(8) 0.0306(8) 0.0303(8) 0.0031(7) 0.0194(7) 0.0022(7) C22 0.0313(9) 0.0253(9) 0.0314(9) 0.0014(7) 0.0147(8) 0.0024(7) N32 0.0299(8) 0.0231(7) 0.0278(7) 0.0001(6) 0.0155(6) 0.0012(6) C42 0.0271(8) 0.0240(8) 0.0245(8) 0.0012(7) 0.0128(7) 0.0024(7) C52 0.0362(10) 0.0325(10) 0.0256(9) -0.0033(7) 0.0148(8) -0.0031(8) C62 0.0368(10) 0.0382(11) 0.0263(9) -0.0021(8) 0.0164(8) -0.0014(9) C72 0.0549(12) 0.0310(10) 0.0480(12) -0.0076(9) 0.0299(10) -0.0119(10) C28 0.0402(14) 0.0612(16) 0.0527(15) -0.0144(14) 0.0093(13) -0.0022(13) C18 0.0445(14) 0.0463(14) 0.0412(13) 0.0025(11) 0.0027(12) 0.0089(12) N18 0.0558(16) 0.0475(13) 0.0644(16) 0.0040(12) -0.0064(14) -0.0001(12) N19 0.104(3) 0.0324(16) 0.099(3) 0.000 0.068(2) 0.000 C19 0.091(2) 0.0366(19) 0.080(2) 0.000 0.0611(19) 0.000 C29 0.135(5) 0.033(2) 0.144(5) 0.000 0.084(4) 0.000 P1 0.0566(5) 0.0353(4) 0.0358(4) 0.0123(3) 0.0155(4) 0.0048(4) P2 0.0292(3) 0.0378(3) 0.0343(3) -0.0043(2) 0.0092(2) 0.0035(2) F12 0.0591(9) 0.0367(8) 0.0758(10) -0.0080(7) 0.0300(8) 0.0019(7) F22 0.0446(8) 0.0597(10) 0.0619(9) -0.0024(8) 0.0287(7) -0.0026(7) F32 0.0531(10) 0.0671(10) 0.0476(9) 0.0151(8) 0.0063(8) 0.0111(8) F42 0.0375(7) 0.0647(10) 0.0675(10) -0.0210(8) 0.0239(7) -0.0091(7) F52 0.0653(11) 0.1489(19) 0.0388(9) 0.0052(11) 0.0072(9) 0.0525(12) F62 0.0461(9) 0.0578(9) 0.1091(14) -0.0435(9) 0.0276(9) -0.0086(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N19 2.240(4) . ? Ag1 N12 2.2783(19) 2_456 ? Ag1 N12 2.2783(19) . ? Ag2 N11 2.2476(18) . ? Ag2 N32 2.3119(18) 4_455 ? Ag2 N31 2.3908(17) 4_455 ? Ag2 N18 2.406(3) . ? N11 C21 1.340(3) . ? N11 C61 1.343(3) . ? C21 N31 1.344(3) . ? C21 C71 1.491(3) . ? N31 C41 1.337(3) . ? N31 Ag2 2.3908(17) 4_445 ? C41 C51 1.383(3) . ? C41 C42 1.499(3) . ? C51 C61 1.388(3) . ? N12 C62 1.335(3) . ? N12 C22 1.350(3) . ? C22 N32 1.335(3) . ? C22 C72 1.494(3) . ? N32 C42 1.341(3) . ? N32 Ag2 2.3119(17) 4_445 ? C42 C52 1.389(3) . ? C52 C62 1.384(3) . ? C28 C18 1.455(4) . ? C18 N18 1.128(4) . ? N19 C19 1.124(6) . ? C19 C29 1.443(6) . ? P1 F21A 1.571(7) 5_565 ? P1 F21A 1.571(7) . ? P1 F11B 1.583(6) . ? P1 F11B 1.583(6) 5_565 ? P1 F21B 1.584(5) . ? P1 F21B 1.584(5) 5_565 ? P1 F31B 1.590(4) . ? P1 F31B 1.590(4) 5_565 ? P1 F31A 1.590(6) . ? P1 F31A 1.590(6) 5_565 ? P1 F11A 1.616(5) . ? P1 F11A 1.616(5) 5_565 ? P2 F52 1.583(2) . ? P2 F62 1.5856(19) . ? P2 F22 1.5911(18) . ? P2 F32 1.5914(18) . ? P2 F12 1.6015(18) . ? P2 F42 1.6050(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N19 Ag1 N12 114.65(5) . 2_456 ? N19 Ag1 N12 114.65(5) . . ? N12 Ag1 N12 130.69(10) 2_456 . ? N11 Ag2 N32 143.30(6) . 4_455 ? N11 Ag2 N31 126.05(7) . 4_455 ? N32 Ag2 N31 71.58(6) 4_455 4_455 ? N11 Ag2 N18 98.81(9) . . ? N32 Ag2 N18 110.47(9) 4_455 . ? N31 Ag2 N18 99.07(8) 4_455 . ? C21 N11 C61 117.51(19) . . ? C21 N11 Ag2 125.12(14) . . ? C61 N11 Ag2 116.37(14) . . ? N11 C21 N31 123.71(19) . . ? N11 C21 C71 118.58(19) . . ? N31 C21 C71 117.71(19) . . ? C41 N31 C21 118.28(18) . . ? C41 N31 Ag2 114.50(13) . 4_445 ? C21 N31 Ag2 126.08(14) . 4_445 ? N31 C41 C51 121.67(19) . . ? N31 C41 C42 117.02(17) . . ? C51 C41 C42 121.27(18) . . ? C41 C51 C61 116.57(19) . . ? N11 C61 C51 122.1(2) . . ? C62 N12 C22 116.98(19) . . ? C62 N12 Ag1 117.94(15) . . ? C22 N12 Ag1 123.97(15) . . ? N32 C22 N12 124.12(19) . . ? N32 C22 C72 117.8(2) . . ? N12 C22 C72 118.1(2) . . ? C22 N32 C42 118.46(18) . . ? C22 N32 Ag2 123.70(14) . 4_445 ? C42 N32 Ag2 117.13(14) . 4_445 ? N32 C42 C52 121.04(19) . . ? N32 C42 C41 117.85(18) . . ? C52 C42 C41 121.09(18) . . ? C62 C52 C42 116.7(2) . . ? N12 C62 C52 122.7(2) . . ? N18 C18 C28 178.8(3) . . ? C18 N18 Ag2 147.1(3) . . ? C19 N19 Ag1 180.000(1) . . ? N19 C19 C29 180.000(2) . . ? F52 P2 F62 89.89(13) . . ? F52 P2 F22 90.91(11) . . ? F62 P2 F22 89.90(10) . . ? F52 P2 F32 178.75(13) . . ? F62 P2 F32 91.14(11) . . ? F22 P2 F32 89.81(10) . . ? F52 P2 F12 90.22(13) . . ? F62 P2 F12 179.44(12) . . ? F22 P2 F12 90.65(10) . . ? F32 P2 F12 88.74(10) . . ? F52 P2 F42 89.60(11) . . ? F62 P2 F42 91.23(10) . . ? F22 P2 F42 178.76(10) . . ? F32 P2 F42 89.66(11) . . ? F12 P2 F42 88.22(10) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 C41 C42 N32 15.2(3) . . . . ? _geom_special_details ? #===END