# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1800 data_global _publ_requested_journal ' Dalton Transactions' _publ_contact_author_name ; Hans-Conrad zur Loye ; _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina 730 South Main Street Columbia, South Carolina 29208 USA ; _publ_contact_author_email ' Hanno@psc.sc.edu' # TITLE AND AUTHOR LIST _publ_section_title ; Novel Hydrogen-Bonded Two- and Three-Dimensional Networks Generated from the Reaction of Metal Nitrate Hydrates (M = Cd, Co) with the Bidentate Linear Ligand 4,4'-Bipyridine ; loop_ _publ_author_name _publ_author_address ; Hans-Conrad zur Loye ; ; University of South Carolina Department of Chemistry and Biochemistry Columbia, SC 29208 USA ; ; Yu-Bin Dong ; ; University of South Carolina Department of Chemistry and Biochemistry Columbia, SC 29208 USA ; ; Mark D. Smith ; ; University of South Carolina Department of Chemistry and Biochemistry Columbia, SC 29208 USA ; ; Ralph C. Layland ; ; University of South Carolina Department of Chemistry and Biochemistry Columbia, SC 29208 USA ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; data_1 #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 20.669(3) _cell_length_b 23.430(5) _cell_length_c 7.533(1) _cell_angle_alpha 90 _cell_angle_beta 104.61(1) _cell_angle_gamma 90 _cell_volume 3530(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 9.89 _cell_measurement_theta_max 10.6 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m ' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' #----------------------------------------------------------------------- _exptl_crystal_description 'monoclinic block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 745.88 _chemical_formula_sum 'C25 H24 Cd F6 N6 O5 P ' _chemical_formula_moiety 'C25 H24 Cd F6 N6 O5 P ' _exptl_crystal_F_000 1492.00 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type 'DIFABS; Walker & Stuart, 1983' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.691 _exptl_special_details ; The scan width was (1.60+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 2 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.47 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 -1 0 2 -1 -2 -4 0 _diffrn_reflns_number 2183 _reflns_number_total 2113 _reflns_number_gt 1774 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.02177 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 21.53 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01414 _diffrn_orient_matrix_UB_12 -0.01444 _diffrn_orient_matrix_UB_13 -0.10903 _diffrn_orient_matrix_UB_21 0.04766 _diffrn_orient_matrix_UB_22 0.00676 _diffrn_orient_matrix_UB_23 0.06464 _diffrn_orient_matrix_UB_31 0.00305 _diffrn_orient_matrix_UB_32 -0.03958 _diffrn_orient_matrix_UB_33 0.05121 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd 4 -1.005 1.202 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 20 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 100 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P P 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 24 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cd 0.76512(3) 0.0000 -0.1692(1) 0.0432(3) 1 ST Uani d ? P(1) 0.5000 0.1586(7) -0.5000 0.257(6) 1 ST Uani d ? F(1) 0.5509(7) 0.205(1) -0.509(4) 0.35(1) 1 . Uani d ? F(2) 0.5523(6) 0.113(1) -0.500(2) 0.32(1) 1 . Uani d ? F(3) 0.5267(9) 0.162(1) -0.286(2) 0.34(1) 1 . Uani d ? O(1) 0.8726(4) 0.0000 0.054(1) 0.075(3) 1 ST Uani d ? O(2) 0.8040(5) 0.0000 0.224(2) 0.094(4) 1 ST Uani d ? O(3) 0.9086(5) 0.0000 0.344(1) 0.126(5) 1 ST Uani d ? O(4) 0.8529(4) 0.0000 -0.321(1) 0.073(3) 1 ST Uani d ? O(5) 0.7078(4) 0.0000 -0.477(1) 0.057(2) 1 ST Uani d ? N(1) 0.8624(5) 0.0000 0.209(1) 0.057(3) 1 ST Uani d ? N(2) 0.6568(4) 0.0000 -0.113(1) 0.042(3) 1 ST Uani d ? N(3) 0.7676(3) 0.0983(3) -0.1552(8) 0.056(2) 1 . Uani d ? N(4) 0.7750(6) 0.3943(3) -0.353(1) 0.085(3) 1 . Uani d ? C(1) 0.6511(5) 0.0000 0.053(2) 0.068(4) 1 ST Uani d ? C(2) 0.5911(6) 0.0000 0.105(2) 0.066(4) 1 ST Uani d ? C(3) 0.5334(5) 0.0000 -0.025(1) 0.044(3) 1 ST Uani d ? C(4) 0.5379(8) 0.0000 -0.199(2) 0.132(8) 1 ST Uani d ? C(5) 0.6000(6) 0.0000 -0.236(2) 0.126(7) 1 ST Uani d ? C(6) 0.8255(5) 0.1276(4) -0.133(2) 0.083(3) 1 . Uani d ? C(7) 0.8284(5) 0.1848(4) -0.160(2) 0.084(3) 1 . Uani d ? C(8) 0.7709(4) 0.2173(4) -0.213(1) 0.056(3) 1 . Uani d ? C(9) 0.7118(5) 0.1876(4) -0.230(1) 0.072(3) 1 . Uani d ? C(10) 0.7130(4) 0.1300(4) -0.200(1) 0.068(3) 1 . Uani d ? C(11) 0.7715(5) 0.2790(4) -0.256(1) 0.058(3) 1 . Uani d ? C(12) 0.8301(6) 0.3076(4) -0.244(2) 0.100(4) 1 . Uani d ? C(13) 0.8294(7) 0.3639(5) -0.297(2) 0.121(5) 1 . Uani d ? C(14) 0.7175(6) 0.3669(5) -0.360(2) 0.084(4) 1 . Uani d ? C(15) 0.7148(5) 0.3114(4) -0.314(1) 0.080(3) 1 . Uani d ? H(1) 0.6928 0.0000 0.1501 0.101 1 S Uiso d ? H(2) 0.5906 0.0000 0.2335 0.101 1 S Uiso d ? H(3) 0.4975 0.0000 -0.2950 0.101 1 S Uiso d ? H(4) 0.6011 0.0000 -0.3638 0.101 1 S Uiso d ? H(5) 0.8667 0.1068 -0.0982 0.101 1 . Uiso c ? H(6) 0.8708 0.2024 -0.1386 0.101 1 . Uiso c ? H(7) 0.6703 0.2079 -0.2620 0.101 1 . Uiso c ? H(8) 0.6715 0.1109 -0.2134 0.101 1 . Uiso c ? H(9) 0.8725 0.2887 -0.1970 0.101 1 . Uiso c ? H(10) 0.8710 0.3832 -0.2855 0.101 1 . Uiso c ? H(11) 0.6763 0.3880 -0.3977 0.101 1 . Uiso c ? H(12) 0.6716 0.2942 -0.3254 0.101 1 . Uiso c ? H(13) 0.7191 -0.0334 -0.5331 0.101 1 . Uiso c ? H(14) 0.8790 0.0331 -0.2862 0.101 1 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd 0.0435(6) 0.0434(6) 0.0429(6) 0.0000 0.0113(4) 0.0000 P(1) 0.052(4) 0.44(2) 0.28(1) 0.0000 0.056(6) 0.0000 F(1) 0.13(1) 0.40(3) 0.54(3) 0.03(1) 0.12(2) 0.16(2) F(2) 0.119(9) 0.58(4) 0.29(2) 0.02(1) 0.077(9) 0.12(2) F(3) 0.24(2) 0.55(4) 0.19(1) -0.08(2) 0.02(1) -0.06(2) O(1) 0.085(6) 0.094(7) 0.051(6) 0.0000 0.024(5) 0.0000 O(2) 0.059(6) 0.094(8) 0.14(1) 0.0000 0.041(6) 0.0000 O(3) 0.084(8) 0.24(2) 0.043(6) 0.0000 -0.009(6) 0.0000 O(4) 0.075(6) 0.084(6) 0.066(6) 0.0000 0.025(5) 0.0000 O(5) 0.063(5) 0.053(5) 0.057(5) 0.0000 0.019(4) 0.0000 N(1) 0.058(7) 0.061(6) 0.050(7) 0.0000 0.012(6) 0.0000 N(2) 0.043(5) 0.047(5) 0.038(5) 0.0000 0.012(4) 0.0000 N(3) 0.062(5) 0.051(4) 0.054(4) 0.002(4) 0.012(3) 0.005(3) N(4) 0.139(8) 0.049(5) 0.077(6) 0.020(6) 0.046(5) 0.016(4) C(1) 0.029(6) 0.12(1) 0.046(8) 0.0000 -0.002(5) 0.0000 C(2) 0.053(8) 0.11(1) 0.038(7) 0.0000 0.009(6) 0.0000 C(3) 0.037(6) 0.057(7) 0.039(6) 0.0000 0.013(5) 0.0000 C(4) 0.07(1) 0.28(3) 0.039(8) 0.0000 -0.007(7) 0.0000 C(5) 0.022(7) 0.31(3) 0.047(8) 0.0000 0.010(6) 0.0000 C(6) 0.059(6) 0.051(6) 0.122(9) -0.007(5) -0.006(5) 0.012(6) C(7) 0.055(6) 0.056(6) 0.128(9) -0.009(5) -0.002(5) 0.019(6) C(8) 0.081(6) 0.046(5) 0.042(4) 0.000(5) 0.019(4) -0.003(4) C(9) 0.067(6) 0.056(6) 0.098(7) 0.011(5) 0.030(5) 0.008(5) C(10) 0.055(5) 0.050(6) 0.107(7) 0.002(4) 0.030(5) 0.007(5) C(11) 0.083(6) 0.047(5) 0.047(5) 0.003(5) 0.021(4) -0.006(4) C(12) 0.089(7) 0.056(7) 0.16(1) 0.004(6) 0.040(7) 0.023(7) C(13) 0.110(9) 0.061(8) 0.21(2) -0.001(7) 0.08(1) 0.030(9) C(14) 0.092(8) 0.056(7) 0.103(8) 0.011(6) 0.020(6) 0.008(6) C(15) 0.086(7) 0.054(6) 0.097(8) 0.008(5) 0.019(6) 0.009(5) #----------------------------------------------------------------------- _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^] ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1774 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_all 0.0822 _refine_ls_wR_factor_ref 0.0822 _refine_ls_goodness_of_fit_all 2.437 _refine_ls_goodness_of_fit_ref 2.437 _refine_ls_shift/su_max 0.0008 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.57 _refine_diff_density_max 1.47 #----------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd O(1) 2.425(9) . . yes Cd O(4) 2.377(8) . . yes Cd O(5) 2.321(8) . . yes Cd N(2) 2.382(8) . . yes Cd N(3) 2.306(7) . . yes Cd N(3) 2.306(7) . 2 yes P(1) F(1) 1.52(2) . . yes P(1) F(1) 1.52(2) . 4_654 yes P(1) F(2) 1.52(2) . . yes P(1) F(2) 1.52(2) . 4_654 yes P(1) F(3) 1.57(2) . . yes P(1) F(3) 1.57(2) . 4_654 yes O(1) N(1) 1.23(1) . . yes O(2) N(1) 1.24(1) . . yes O(3) N(1) 1.21(1) . . yes O(4) H(14) 0.94 . . no O(4) H(14) 0.94 . 2 no O(5) H(13) 0.95 . . no O(5) H(13) 0.95 . 2 no N(2) C(1) 1.29(1) . . yes N(2) C(5) 1.30(1) . . yes N(3) C(6) 1.35(1) . . yes N(3) C(10) 1.32(1) . . yes N(4) C(13) 1.31(1) . . yes N(4) C(14) 1.34(1) . . yes C(1) C(2) 1.39(2) . . yes C(1) H(1) 0.98 . . no C(2) C(3) 1.34(2) . . yes C(2) H(2) 0.97 . . no C(3) C(3) 1.52(2) . 3_655 yes C(3) C(4) 1.34(2) . . yes C(4) C(5) 1.38(2) . . yes C(4) H(3) 0.96 . . no C(5) H(4) 0.97 . . no C(6) C(7) 1.36(1) . . yes C(6) H(5) 0.96 . . no C(7) C(8) 1.38(1) . . yes C(7) H(6) 0.94 . . no C(8) C(9) 1.38(1) . . yes C(8) C(11) 1.48(1) . . yes C(9) C(10) 1.37(1) . . yes C(9) H(7) 0.96 . . no C(10) H(8) 0.95 . . no C(11) C(12) 1.37(1) . . yes C(11) C(15) 1.37(1) . . yes C(12) C(13) 1.38(1) . . yes C(12) H(9) 0.97 . . no C(13) H(10) 0.96 . . no C(14) C(15) 1.35(1) . . yes C(14) H(11) 0.96 . . no C(15) H(12) 0.96 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cd O(4) 70.0(3) . . . yes O(1) Cd O(5) 147.2(3) . . . yes O(1) Cd N(2) 127.9(3) . . . yes O(1) Cd N(3) 87.9(2) . . . yes O(1) Cd N(3) 87.9(2) . . 2 yes O(4) Cd O(5) 77.2(3) . . . yes O(4) Cd N(2) 162.1(3) . . . yes O(4) Cd N(3) 90.7(2) . . . yes O(4) Cd N(3) 90.7(2) . . 2 yes O(5) Cd N(2) 84.9(3) . . . yes O(5) Cd N(3) 92.6(2) . . . yes O(5) Cd N(3) 92.6(2) . . 2 yes N(2) Cd N(3) 90.1(2) . . . yes N(2) Cd N(3) 90.1(2) . . 2 yes N(3) Cd N(3) 174.8(3) . . 2 yes F(1) P(1) F(1) 90(2) . . 4_654 yes F(1) P(1) F(2) 89.9(9) . . . yes F(1) P(1) F(2) 178(1) . . 4_654 yes F(1) P(1) F(3) 87(1) . . . yes F(1) P(1) F(3) 89(1) . . 4_654 yes F(1) P(1) F(2) 178(1) 4_654 . . yes F(1) P(1) F(2) 89.9(9) 4_654 . 4_654 yes F(1) P(1) F(3) 89(1) 4_654 . . yes F(1) P(1) F(3) 87(1) 4_654 . 4_654 yes F(2) P(1) F(2) 91(2) . . 4_654 yes F(2) P(1) F(3) 88(1) . . . yes F(2) P(1) F(3) 96(1) . . 4_654 yes F(2) P(1) F(3) 96(1) 4_654 . . yes F(2) P(1) F(3) 88(1) 4_654 . 4_654 yes F(3) P(1) F(3) 174(2) . . 4_654 yes Cd O(1) N(1) 108.0(7) . . . yes Cd O(4) H(14) 108.5 . . . no Cd O(4) H(14) 108.5 . . 2 no H(14) O(4) H(14) 110.6 . . 2 no Cd O(5) H(13) 109.0 . . . no Cd O(5) H(13) 109.0 . . 2 no H(13) O(5) H(13) 111.6 . . 2 no O(1) N(1) O(2) 119(1) . . . yes O(1) N(1) O(3) 121(1) . . . yes O(2) N(1) O(3) 120(1) . . . yes Cd N(2) C(1) 119.5(7) . . . yes Cd N(2) C(5) 126.4(7) . . . yes C(1) N(2) C(5) 114.1(9) . . . yes Cd N(3) C(6) 121.3(6) . . . yes Cd N(3) C(10) 122.8(6) . . . yes C(6) N(3) C(10) 114.8(8) . . . yes C(13) N(4) C(14) 115.7(9) . . . yes N(2) C(1) C(2) 125(1) . . . yes N(2) C(1) H(1) 116.5 . . . no C(2) C(1) H(1) 118.2 . . . no C(1) C(2) C(3) 119(1) . . . yes C(1) C(2) H(2) 120.9 . . . no C(3) C(2) H(2) 119.8 . . . no C(2) C(3) C(3) 121(1) . . 3_655 yes C(2) C(3) C(4) 117(1) . . . yes C(3) C(3) C(4) 122(1) 3_655 . . yes C(3) C(4) C(5) 120(1) . . . yes C(3) C(4) H(3) 118.6 . . . no C(5) C(4) H(3) 121.6 . . . no N(2) C(5) C(4) 125(1) . . . yes N(2) C(5) H(4) 117.8 . . . no C(4) C(5) H(4) 117.3 . . . no N(3) C(6) C(7) 123.6(9) . . . yes N(3) C(6) H(5) 118.3 . . . no C(7) C(6) H(5) 118.1 . . . no C(6) C(7) C(8) 121.1(9) . . . yes C(6) C(7) H(6) 118.6 . . . no C(8) C(7) H(6) 120.2 . . . no C(7) C(8) C(9) 115.2(8) . . . yes C(7) C(8) C(11) 123.0(8) . . . yes C(9) C(8) C(11) 121.8(8) . . . yes C(8) C(9) C(10) 120.2(8) . . . yes C(8) C(9) H(7) 119.2 . . . no C(10) C(9) H(7) 120.6 . . . no N(3) C(10) C(9) 125.1(8) . . . yes N(3) C(10) H(8) 116.8 . . . no C(9) C(10) H(8) 118.1 . . . no C(8) C(11) C(12) 121.3(8) . . . yes C(8) C(11) C(15) 123.8(9) . . . yes C(12) C(11) C(15) 114.9(9) . . . yes C(11) C(12) C(13) 120(1) . . . yes C(11) C(12) H(9) 120.4 . . . no C(13) C(12) H(9) 119.3 . . . no N(4) C(13) C(12) 124(1) . . . yes N(4) C(13) H(10) 116.8 . . . no C(12) C(13) H(10) 119.0 . . . no N(4) C(14) C(15) 123(1) . . . yes N(4) C(14) H(11) 118.4 . . . no C(15) C(14) H(11) 118.5 . . . no C(11) C(15) C(14) 122(1) . . . yes C(11) C(15) H(12) 119.6 . . . no C(14) C(15) H(12) 118.6 . . . no #----------------------------------------------------------------------- #==END data_2 #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 17.918(2) _cell_length_b 11.397(1) _cell_length_c 23.071(2) _cell_angle_alpha 90 _cell_angle_beta 101.286(9) _cell_angle_gamma 90 _cell_volume 4620.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.9 _cell_measurement_theta_max 11.1 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' #----------------------------------------------------------------------- _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow-orange' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1045.67 _chemical_formula_sum 'C40 H40 Co F12 N8 O4 P2 ' _exptl_crystal_F_000 2132.00 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type 'DIFABS; Walker & Stuart, 1983' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.596 _exptl_special_details ; The scan width was (1.50+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 2 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.05 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -1 0 -2 3 -1 -1 3 _diffrn_reflns_number 3320 _reflns_number_total 3192 _reflns_number_gt 2297 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01374 _diffrn_reflns_av_sigmaI/netI 0.030 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04358 _diffrn_orient_matrix_UB_12 -0.03389 _diffrn_orient_matrix_UB_13 0.01601 _diffrn_orient_matrix_UB_21 0.02270 _diffrn_orient_matrix_UB_22 0.03160 _diffrn_orient_matrix_UB_23 0.04002 _diffrn_orient_matrix_UB_31 -0.02914 _diffrn_orient_matrix_UB_32 0.07473 _diffrn_orient_matrix_UB_33 -0.00955 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 4 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 160 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P P 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Co 0.0000 -0.44799(7) -0.2500 0.0320(3) 1 ST Uani d ? P(1) 0.28129(9) -0.1139(1) -0.12402(6) 0.0567(5) 1 . Uani d ? F(1) 0.2096(2) -0.1883(4) -0.1202(2) 0.117(2) 1 . Uani d ? F(2) 0.2616(3) -0.1278(5) -0.1933(2) 0.127(2) 1 . Uani d ? F(3) 0.3341(3) -0.2232(4) -0.1206(2) 0.140(2) 1 . Uani d ? F(4) 0.2297(3) -0.0009(4) -0.1284(2) 0.123(2) 1 . Uani d ? F(5) 0.3515(3) -0.0334(4) -0.1317(2) 0.114(2) 1 . Uani d ? F(6) 0.3022(3) -0.0920(5) -0.0559(2) 0.131(2) 1 . Uani d ? O(1) 0.0265(2) -0.4494(3) -0.1593(1) 0.047(1) 1 . Uani d ? O(2) -0.1188(2) -0.4446(3) -0.2470(1) 0.044(1) 1 . Uani d ? N(1) 0.0000 -0.2594(4) -0.2500 0.029(2) 1 ST Uani d ? N(2) 0.0000 -0.6384(4) -0.2500 0.039(2) 1 ST Uani d ? N(3) 0.4277(3) 0.1444(4) 0.0853(2) 0.054(2) 1 . Uani d ? N(4) 0.2201(3) 0.4637(5) -0.1607(2) 0.067(2) 1 . Uani d ? N(5) 0.5312(3) 0.2523(4) -0.0869(2) 0.057(2) 1 . Uani d ? C(1) 0.0638(3) -0.1977(4) -0.2314(2) 0.037(1) 1 . Uani d ? C(2) 0.0662(3) -0.0769(4) -0.2311(2) 0.041(2) 1 . Uani d ? C(3) 0.0000 -0.0144(5) -0.2500 0.034(2) 1 ST Uani d ? C(4) 0.0000 0.1160(5) -0.2500 0.037(2) 1 ST Uani d ? C(5) 0.0529(3) 0.1798(4) -0.2739(2) 0.043(2) 1 . Uani d ? C(6) -0.0505(3) -0.7001(4) -0.2267(2) 0.044(2) 1 . Uani d ? C(7) 0.4181(4) 0.1063(5) 0.0295(3) 0.063(2) 1 . Uani d ? C(8) 0.3794(3) 0.1666(5) -0.0184(2) 0.053(2) 1 . Uani d ? C(9) 0.3472(3) 0.2737(4) -0.0112(2) 0.039(1) 1 . Uani d ? C(10) 0.3575(3) 0.3157(5) 0.0455(2) 0.051(2) 1 . Uani d ? C(11) 0.3979(3) 0.2491(5) 0.0921(2) 0.058(2) 1 . Uani d ? C(12) 0.3026(3) 0.3404(5) -0.0625(2) 0.043(2) 1 . Uani d ? C(13) 0.2735(3) 0.4510(5) -0.0569(2) 0.055(2) 1 . Uani d ? C(14) 0.2327(4) 0.5075(5) -0.1059(3) 0.067(2) 1 . Uani d ? C(15) 0.2480(4) 0.3584(7) -0.1652(2) 0.074(2) 1 . Uani d ? C(16) 0.2895(3) 0.2933(5) -0.1192(2) 0.064(2) 1 . Uani d ? C(17) 0.4844(3) 0.3403(5) -0.1086(2) 0.055(2) 1 . Uani d ? C(18) 0.4725(3) 0.4386(5) -0.0769(2) 0.050(2) 1 . Uani d ? C(19) 0.5069(3) 0.4490(4) -0.0183(2) 0.042(1) 1 . Uani d ? C(20) 0.5563(3) 0.3584(5) 0.0037(3) 0.063(2) 1 . Uani d ? C(21) 0.5655(4) 0.2655(5) -0.0313(3) 0.070(2) 1 . Uani d ? H(1) 0.1103 -0.2408 -0.2169 0.063 1 . Uiso c ? H(2) 0.1140 -0.0357 -0.2173 0.063 1 . Uiso c ? H(3) 0.0057 -0.3801 -0.1444 0.063 1 . Uiso c ? H(4) 0.0039 -0.5164 -0.1447 0.063 1 . Uiso c ? H(5) 0.0926 0.1390 -0.2891 0.063 1 . Uiso c ? H(6) -0.0881 -0.6573 -0.2095 0.063 1 . Uiso c ? H(7) 0.4399 0.0289 0.0230 0.063 1 . Uiso c ? H(8) 0.3747 0.1355 -0.0581 0.063 1 . Uiso c ? H(9) -0.1299 -0.3757 -0.2260 0.063 1 . Uiso c ? H(10) 0.3363 0.3913 0.0535 0.063 1 . Uiso c ? H(11) 0.4047 0.2797 0.1318 0.063 1 . Uiso c ? H(12) -0.1317 -0.5121 -0.2262 0.063 1.000 . Uiso c ? H(13) 0.2816 0.4882 -0.0183 0.063 1 . Uiso c ? H(14) 0.2103 0.5847 -0.1005 0.063 1 . Uiso c ? H(15) 0.2399 0.3219 -0.2044 0.063 1 . Uiso c ? H(16) 0.3101 0.2165 -0.1266 0.063 1 . Uiso c ? H(17) 0.4576 0.3349 -0.1490 0.063 1 . Uiso c ? H(18) 0.4393 0.5023 -0.0962 0.063 1 . Uiso c ? H(20) 0.5832 0.3619 0.0446 0.063 1 . Uiso c ? H(21) 0.6011 0.2045 -0.0143 0.063 1 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0361(7) 0.0266(5) 0.0324(5) 0.0000 0.0047(4) 0.0000 P(1) 0.047(1) 0.072(1) 0.0518(9) -0.0034(9) 0.0116(7) -0.0109(8) F(1) 0.087(3) 0.131(4) 0.139(4) -0.046(3) 0.038(3) -0.017(3) F(2) 0.119(4) 0.190(5) 0.069(3) -0.004(4) 0.015(2) -0.033(3) F(3) 0.116(4) 0.117(4) 0.176(5) 0.049(3) 0.006(3) 0.003(3) F(4) 0.108(4) 0.099(3) 0.166(4) 0.028(3) 0.033(3) -0.026(3) F(5) 0.102(3) 0.140(4) 0.114(3) -0.050(3) 0.057(3) -0.037(3) F(6) 0.119(4) 0.213(5) 0.060(2) -0.025(4) 0.017(2) -0.013(3) O(1) 0.068(3) 0.035(2) 0.035(2) 0.002(2) 0.005(2) -0.001(1) O(2) 0.045(2) 0.034(2) 0.055(2) -0.002(2) 0.012(2) 0.001(2) N(1) 0.029(4) 0.028(3) 0.028(3) 0.0000 -0.001(2) 0.0000 N(2) 0.046(4) 0.032(3) 0.038(3) 0.0000 0.009(3) 0.0000 N(3) 0.052(3) 0.067(3) 0.043(3) 0.003(3) 0.006(2) 0.010(2) N(4) 0.054(4) 0.078(4) 0.067(3) 0.011(3) 0.005(3) 0.022(3) N(5) 0.057(3) 0.060(3) 0.058(3) -0.004(3) 0.020(3) -0.012(2) C(1) 0.036(3) 0.034(3) 0.040(3) 0.002(2) 0.003(2) 0.002(2) C(2) 0.039(3) 0.029(3) 0.051(3) -0.005(2) 0.003(2) -0.004(2) C(3) 0.035(5) 0.029(4) 0.037(4) 0.0000 0.004(3) 0.0000 C(4) 0.046(5) 0.028(4) 0.033(4) 0.0000 0.001(3) 0.0000 C(5) 0.046(3) 0.032(3) 0.057(3) 0.002(2) 0.022(3) -0.004(2) C(6) 0.049(4) 0.035(3) 0.054(3) 0.006(3) 0.022(3) 0.000(2) C(7) 0.071(5) 0.054(3) 0.062(4) 0.013(3) 0.012(3) 0.009(3) C(8) 0.066(4) 0.054(3) 0.039(3) 0.005(3) 0.011(3) 0.005(2) C(9) 0.030(3) 0.048(3) 0.040(3) -0.005(3) 0.012(2) 0.005(2) C(10) 0.049(4) 0.054(3) 0.050(3) 0.005(3) 0.011(3) -0.002(3) C(11) 0.064(4) 0.071(4) 0.037(3) 0.002(3) 0.002(3) -0.001(3) C(12) 0.029(3) 0.057(3) 0.042(3) -0.006(3) 0.009(2) 0.006(2) C(13) 0.046(4) 0.063(4) 0.054(3) 0.009(3) 0.007(3) 0.009(3) C(14) 0.056(4) 0.058(4) 0.087(5) 0.013(3) 0.013(4) 0.015(3) C(15) 0.067(5) 0.106(5) 0.044(3) 0.009(4) 0.001(3) 0.008(3) C(16) 0.066(4) 0.069(4) 0.052(4) 0.014(3) 0.000(3) 0.003(3) C(17) 0.058(4) 0.070(4) 0.042(3) -0.003(3) 0.023(3) -0.005(3) C(18) 0.051(4) 0.058(3) 0.043(3) 0.003(3) 0.020(3) 0.001(3) C(19) 0.034(3) 0.048(3) 0.048(3) -0.011(3) 0.015(2) -0.007(2) C(20) 0.060(4) 0.061(4) 0.060(4) 0.009(3) -0.010(3) -0.018(3) C(21) 0.068(5) 0.059(4) 0.071(4) 0.013(3) -0.012(3) -0.014(3) #----------------------------------------------------------------------- _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^] ; _refine_ls_hydrogen_treatment calc _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000006(3) _refine_ls_extinction_expression ; equ(3) Acta Cryst.(1968) A24, p213. ; _refine_ls_number_reflns 2297 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_all 0.0621 _refine_ls_wR_factor_ref 0.0621 _refine_ls_goodness_of_fit_all 2.718 _refine_ls_goodness_of_fit_ref 2.718 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.39 _refine_diff_density_max 0.55 #----------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O(1) 2.053(3) . . yes Co O(1) 2.053(3) . 2_554 yes Co O(2) 2.144(3) . . yes Co O(2) 2.144(3) . 2_554 yes Co N(1) 2.150(5) . . yes Co N(2) 2.170(5) . . yes P(1) F(1) 1.556(5) . . yes P(1) F(2) 1.577(4) . . yes P(1) F(3) 1.558(5) . . yes P(1) F(4) 1.577(5) . . yes P(1) F(5) 1.594(5) . . yes P(1) F(6) 1.563(4) . . yes O(1) H(3) 0.96 . . no O(1) H(4) 0.96 . . no O(2) H(9) 0.96 . . no O(2) H(12) 0.96 . . no N(1) C(1) 1.339(5) . . yes N(1) C(1) 1.339(5) . 2_554 yes N(2) C(6) 1.339(6) . . yes N(2) C(6) 1.339(6) . 2_554 yes N(3) C(7) 1.338(7) . . yes N(3) C(11) 1.328(8) . . yes N(4) C(14) 1.336(9) . . yes N(4) C(15) 1.312(9) . . yes N(5) C(17) 1.341(7) . . yes N(5) C(21) 1.318(7) . . yes C(1) C(2) 1.378(6) . . yes C(1) H(1) 0.97 . . no C(2) C(3) 1.379(6) . . yes C(2) H(2) 0.97 . . no C(3) C(4) 1.486(9) . . yes C(4) C(5) 1.392(6) . . yes C(4) C(5) 1.392(6) . 2_554 yes C(5) C(6) 1.369(7) . 2_564 yes C(5) H(5) 0.97 . . no C(6) H(6) 0.98 . . no C(7) C(8) 1.370(7) . . yes C(7) H(7) 0.99 . . no C(8) C(9) 1.373(7) . . yes C(8) H(8) 0.97 . . no C(9) C(10) 1.371(7) . . yes C(9) C(12) 1.500(6) . . yes C(10) C(11) 1.395(7) . . yes C(10) H(10) 0.97 . . no C(11) H(11) 0.97 . . no C(12) C(13) 1.380(8) . . yes C(12) C(16) 1.390(7) . . yes C(13) C(14) 1.379(8) . . yes C(13) H(13) 0.97 . . no C(14) H(14) 0.99 . . no C(15) C(16) 1.387(8) . . yes C(15) H(15) 0.98 . . no C(16) H(16) 0.98 . . no C(17) C(18) 1.378(8) . . yes C(17) H(17) 0.96 . . no C(18) C(19) 1.377(6) . . yes C(18) H(18) 0.99 . . no C(19) C(19) 1.49(1) . 3_665 yes C(19) C(20) 1.389(7) . . yes C(20) C(21) 1.362(9) . . yes C(20) H(20) 0.97 . . no C(21) H(21) 0.97 . . no #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Co O(1) 179.1(2) . . 2_554 yes O(1) Co O(2) 90.0(1) . . . yes O(1) Co O(2) 90.0(1) . . 2_554 yes O(1) Co N(1) 90.44(9) . . . yes O(1) Co N(2) 89.56(9) . . . yes O(1) Co O(2) 90.0(1) 2_554 . . yes O(1) Co O(2) 90.0(1) 2_554 . 2_554 yes O(1) Co N(1) 90.44(9) 2_554 . . yes O(1) Co N(2) 89.56(9) 2_554 . . yes O(2) Co O(2) 177.9(2) . . 2_554 yes O(2) Co N(1) 88.97(8) . . . yes O(2) Co N(2) 91.03(8) . . . yes O(2) Co N(1) 88.97(8) 2_554 . . yes O(2) Co N(2) 91.03(8) 2_554 . . yes N(1) Co N(2) 180.00 . . . yes F(1) P(1) F(2) 88.8(3) . . . yes F(1) P(1) F(3) 93.5(3) . . . yes F(1) P(1) F(4) 88.2(3) . . . yes F(1) P(1) F(5) 176.1(2) . . . yes F(1) P(1) F(6) 93.9(3) . . . yes F(2) P(1) F(3) 89.1(3) . . . yes F(2) P(1) F(4) 90.3(3) . . . yes F(2) P(1) F(5) 88.3(2) . . . yes F(2) P(1) F(6) 176.5(3) . . . yes F(3) P(1) F(4) 178.2(3) . . . yes F(3) P(1) F(5) 88.9(3) . . . yes F(3) P(1) F(6) 93.0(3) . . . yes F(4) P(1) F(5) 89.4(3) . . . yes F(4) P(1) F(6) 87.5(3) . . . yes F(5) P(1) F(6) 88.9(3) . . . yes Co O(1) H(3) 109.2 . . . no Co O(1) H(4) 109.6 . . . no H(3) O(1) H(4) 108.0 . . . no Co O(2) H(9) 109.5 . . . no Co O(2) H(12) 109.9 . . . no H(9) O(2) H(12) 107.9 . . . no Co N(1) C(1) 121.6(3) . . . yes Co N(1) C(1) 121.6(3) . . 2_554 yes C(1) N(1) C(1) 116.8(5) . . 2_554 yes Co N(2) C(6) 121.7(3) . . . yes Co N(2) C(6) 121.7(3) . . 2_554 yes C(6) N(2) C(6) 116.6(6) . . 2_554 yes C(7) N(3) C(11) 115.2(4) . . . yes C(14) N(4) C(15) 114.9(5) . . . yes C(17) N(5) C(21) 114.6(5) . . . yes N(1) C(1) C(2) 123.3(4) . . . yes N(1) C(1) H(1) 117.9 . . . no C(2) C(1) H(1) 118.8 . . . no C(1) C(2) C(3) 119.4(4) . . . yes C(1) C(2) H(2) 120.5 . . . no C(3) C(2) H(2) 120.1 . . . no C(2) C(3) C(2) 117.8(6) . . 2_554 yes C(2) C(3) C(4) 121.1(3) . . . yes C(2) C(3) C(4) 121.1(3) 2_554 . . yes C(3) C(4) C(5) 121.5(3) . . . yes C(3) C(4) C(5) 121.5(3) . . 2_554 yes C(5) C(4) C(5) 116.9(6) . . 2_554 yes C(4) C(5) C(6) 119.6(5) . . 2_564 yes C(4) C(5) H(5) 119.8 . . . no C(6) C(5) H(5) 120.6 2_564 . . no N(2) C(6) C(5) 123.6(5) . . 2_544 yes N(2) C(6) H(6) 118.3 . . . no C(5) C(6) H(6) 118.0 2_544 . . no N(3) C(7) C(8) 124.2(5) . . . yes N(3) C(7) H(7) 117.1 . . . no C(8) C(7) H(7) 118.6 . . . no C(7) C(8) C(9) 120.5(5) . . . yes C(7) C(8) H(8) 121.0 . . . no C(9) C(8) H(8) 118.6 . . . no C(8) C(9) C(10) 116.4(4) . . . yes C(8) C(9) C(12) 121.7(4) . . . yes C(10) C(9) C(12) 121.9(5) . . . yes C(9) C(10) C(11) 119.8(5) . . . yes C(9) C(10) H(10) 120.3 . . . no C(11) C(10) H(10) 119.9 . . . no N(3) C(11) C(10) 123.9(5) . . . yes N(3) C(11) H(11) 117.1 . . . no C(10) C(11) H(11) 118.9 . . . no C(9) C(12) C(13) 122.8(4) . . . yes C(9) C(12) C(16) 120.9(5) . . . yes C(13) C(12) C(16) 116.3(5) . . . yes C(12) C(13) C(14) 119.9(5) . . . yes C(12) C(13) H(13) 119.6 . . . no C(14) C(13) H(13) 120.5 . . . no N(4) C(14) C(13) 124.4(6) . . . yes N(4) C(14) H(14) 117.1 . . . no C(13) C(14) H(14) 118.5 . . . no N(4) C(15) C(16) 125.7(6) . . . yes N(4) C(15) H(15) 118.2 . . . no C(16) C(15) H(15) 116.1 . . . no C(12) C(16) C(15) 118.7(6) . . . yes C(12) C(16) H(16) 120.8 . . . no C(15) C(16) H(16) 120.5 . . . no N(5) C(17) C(18) 124.1(5) . . . yes N(5) C(17) H(17) 118.1 . . . no C(18) C(17) H(17) 117.8 . . . no C(17) C(18) C(19) 120.4(5) . . . yes C(17) C(18) H(18) 120.0 . . . no C(19) C(18) H(18) 119.7 . . . no C(18) C(19) C(19) 122.1(5) . . 3_665 yes C(18) C(19) C(20) 115.3(5) . . . yes C(19) C(19) C(20) 122.6(5) 3_665 . . yes C(19) C(20) C(21) 120.2(5) . . . yes C(19) C(20) H(20) 118.9 . . . no C(21) C(20) H(20) 120.9 . . . no N(5) C(21) C(20) 125.4(5) . . . yes N(5) C(21) H(21) 117.1 . . . no C(20) C(21) H(21) 117.5 . . . no #==END