Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global #=============================================================================== _audit_creation_date 3-07-01 _journal_coden_Cambridge 182 loop_ _publ_author_name 'de Cian, Andre' 'Ferlay, Sylvie' 'Hosseini, M.' 'Koenig, Stephanie' 'Kyritsakas, N.' 'Pansanel, Jerome' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof M Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg FRANCE ; _publ_contact_author_email 'HOSSEINI@CHIMIE.U-STRASBG.FR' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Design of 3-D Coordination Networks: Topology and Metrics ; data_st943A _database_code_CSD 172695 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C49 H43 Ag2 Cl3 F12 N6 O6 Sb2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C49 H43 Ag2 Cl3 F12 N6 O6 Sb2' _chemical_formula_weight 1605.51 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Ag ? -1.085 1.101 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Sb ? -0.816 1.546 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.2905(2) _cell_length_b 15.2386(2) _cell_length_c 25.6472(4) _cell_angle_alpha 90 _cell_angle_beta 94.269(5) _cell_angle_gamma 90 _cell_volume 5959.4(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12347 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.79 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9708 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12347 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.0 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 14 frames Set 2 Theta = -2.60 Kappa = -168.00 Phi = 0.00 39 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12347 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7021 _reflns_number_gt 4642 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4642 _refine_ls_number_parameters 366 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.055 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_all 9.890 _refine_ls_wR_factor_ref 0.065 _refine_ls_goodness_of_fit_all 9.990 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.425 _refine_diff_density_min -0.106 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol AG 0.73709(2) -0.15363(3) 0.56530(1) 0.0341(2) 1.000 Uani ? ? Ag C1 1.2142(3) -0.0725(3) 0.3816(2) 0.025(2) 1.000 Uani ? ? C O1 1.2111(2) 0.0210(2) 0.3759(1) 0.027(2) 1.000 Uani ? ? O C2 1.1337(3) -0.0991(3) 0.4105(2) 0.026(2) 1.000 Uani ? ? C C3 1.0623(3) -0.1449(3) 0.3862(2) 0.032(2) 1.000 Uani ? ? C C4 0.9875(3) -0.1605(3) 0.4132(2) 0.036(3) 1.000 Uani ? ? C C5 0.9854(3) -0.1312(3) 0.4643(2) 0.032(2) 1.000 Uani ? ? C C6 1.0582(3) -0.0879(3) 0.4894(2) 0.030(2) 1.000 Uani ? ? C C7 1.1303(3) -0.0718(3) 0.4617(2) 0.028(2) 1.000 Uani ? ? C C8 0.9089(3) -0.1446(3) 0.4930(2) 0.035(2) 1.000 Uani ? ? C N1 0.8501(3) -0.1532(3) 0.5172(2) 0.044(2) 1.000 Uani ? ? N C9 1.2999(3) -0.0932(3) 0.4142(2) 0.025(2) 1.000 Uani ? ? C C10 1.3073(3) -0.1635(3) 0.4477(2) 0.029(2) 1.000 Uani ? ? C C11 1.3848(3) -0.1810(3) 0.4765(2) 0.032(2) 1.000 Uani ? ? C C12 1.4564(3) -0.1258(3) 0.4714(2) 0.032(2) 1.000 Uani ? ? C C13 1.4503(3) -0.0571(3) 0.4358(2) 0.035(2) 1.000 Uani ? ? C C14 1.3726(3) -0.0407(3) 0.4078(2) 0.032(2) 1.000 Uani ? ? C C15 1.5370(3) -0.1405(3) 0.5030(2) 0.036(3) 1.000 Uani ? ? C N2 1.6009(3) -0.1504(3) 0.5284(2) 0.042(2) 1.000 Uani ? ? N C16 1.2176(3) -0.1169(3) 0.3283(2) 0.025(2) 1.000 Uani ? ? C C17 1.2323(3) -0.2069(3) 0.3246(2) 0.034(2) 1.000 Uani ? ? C C18 1.2373(3) -0.2475(3) 0.2767(2) 0.037(3) 1.000 Uani ? ? C C19 1.2268(3) -0.1980(3) 0.2312(2) 0.034(2) 1.000 Uani ? ? C C20 1.2109(4) -0.1080(4) 0.2337(2) 0.040(3) 1.000 Uani ? ? C C21 1.2070(4) -0.0694(3) 0.2819(2) 0.040(3) 1.000 Uani ? ? C C22 1.2320(3) -0.2396(4) 0.1812(2) 0.039(3) 1.000 Uani ? ? C N3 1.2347(3) -0.2736(3) 0.1418(2) 0.044(2) 1.000 Uani ? ? N SB 0.71009(2) 0.03073(2) 0.39727(1) 0.0363(2) 1.000 Uani ? ? Sb F1 0.6524(3) -0.0679(3) 0.3685(2) 0.076(2) 1.000 Uani ? ? F F2 0.6047(2) 0.0924(3) 0.3909(2) 0.083(3) 1.000 Uani ? ? F F3 0.6868(2) -0.0054(2) 0.4643(1) 0.056(2) 1.000 Uani ? ? F F4 0.7677(3) 0.1301(2) 0.4250(1) 0.066(2) 1.000 Uani ? ? F F5 0.8148(2) -0.0312(2) 0.4024(2) 0.073(2) 1.000 Uani ? ? F F6 0.7349(3) 0.0664(3) 0.3302(1) 0.062(2) 1.000 Uani ? ? F C23 1.0257(6) -0.0731(7) 0.6622(6) 0.138(8) 1.000 Uani ? ? C O2 0.9378(3) -0.0955(3) 0.6664(2) 0.081(3) 1.000 Uani ? ? O C24 1.0256(6) -0.3111(7) 0.6798(5) 0.128(7) 1.000 Uani ? ? C O3 0.9486(4) -0.2758(4) 0.6716(4) 0.117(5) 1.000 Uani ? ? O C25 1.0204(8) 0.383(1) 0.7676(5) 0.064(8) 0.500 Uani ? ? C CL1 1.0762(2) 0.4295(2) 0.7214(1) 0.155(2) 1.000 Uani ? ? Cl CL2 1.0000 0.2658(3) 0.7500 0.115(2) 0.500 Uani ? ? Cl H1 1.0647 -0.1655 0.3514 0.0421 1.000 Uiso calc C3 H H2 0.9387 -0.1908 0.3967 0.0472 1.000 Uiso calc C4 H H3 1.0575 -0.0699 0.5248 0.0393 1.000 Uiso calc C6 H H4 1.1790 -0.0413 0.4782 0.0359 1.000 Uiso calc C7 H H5 1.2581 -0.2007 0.4510 0.0379 1.000 Uiso calc C10 H H6 1.3895 -0.2299 0.4996 0.0423 1.000 Uiso calc C11 H H7 1.5001 -0.0216 0.4309 0.0463 1.000 Uiso calc C13 H H8 1.3682 0.0069 0.3838 0.0415 1.000 Uiso calc C14 H H9 1.2390 -0.2411 0.3556 0.0462 1.000 Uiso calc C17 H H10 1.2479 -0.3088 0.2749 0.0488 1.000 Uiso calc C18 H H11 1.2029 -0.0740 0.2027 0.0595 1.000 Uiso calc C20 H H12 1.1966 -0.0080 0.2836 0.0544 1.000 Uiso calc C21 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol AG 0.0296(2) 0.0488(2) 0.0275(2) -0.0042(2) 0.0038(1) 0.0038(2) Ag C1 0.028(2) 0.025(2) 0.023(2) -0.002(2) 0.004(2) -0.000(2) C O1 0.035(2) 0.020(2) 0.029(2) -0.002(1) 0.003(1) 0.000(1) O C2 0.029(2) 0.024(2) 0.026(2) 0.002(2) 0.001(2) -0.001(2) C C3 0.032(2) 0.039(3) 0.026(2) -0.004(2) 0.004(2) -0.006(2) C C4 0.033(2) 0.041(3) 0.035(3) -0.007(2) 0.006(2) -0.000(2) C C5 0.030(2) 0.028(2) 0.041(2) 0.003(2) 0.013(2) 0.004(2) C C6 0.037(2) 0.026(2) 0.028(2) 0.006(2) 0.004(2) -0.004(2) C C7 0.027(2) 0.027(2) 0.029(2) 0.001(2) 0.001(2) -0.002(2) C C8 0.038(2) 0.028(2) 0.041(3) 0.003(2) 0.011(2) 0.001(2) C N1 0.044(2) 0.042(3) 0.047(2) -0.000(2) 0.018(2) 0.001(2) N C9 0.025(2) 0.025(2) 0.025(2) -0.003(2) 0.003(2) -0.005(2) C C10 0.025(2) 0.028(2) 0.035(2) -0.004(2) 0.002(2) -0.004(2) C C11 0.031(2) 0.030(2) 0.036(3) 0.001(2) 0.001(2) 0.002(2) C C12 0.030(2) 0.032(2) 0.035(3) 0.003(2) 0.002(2) -0.005(2) C C13 0.026(2) 0.034(2) 0.047(3) -0.006(2) 0.004(2) -0.003(2) C C14 0.036(2) 0.031(2) 0.029(2) -0.007(2) 0.002(2) 0.002(2) C C15 0.035(2) 0.030(2) 0.045(3) 0.000(2) 0.001(2) -0.007(2) C N2 0.035(2) 0.035(2) 0.060(3) 0.001(2) -0.008(2) -0.002(2) N C16 0.025(2) 0.027(2) 0.023(2) -0.002(2) 0.005(2) -0.003(2) C C17 0.051(3) 0.033(3) 0.023(2) 0.000(2) 0.001(2) -0.001(2) C C18 0.047(3) 0.033(2) 0.033(3) 0.001(2) 0.001(2) -0.010(2) C C19 0.040(2) 0.037(3) 0.026(2) -0.000(2) 0.007(2) -0.007(2) C C20 0.078(3) 0.040(3) 0.021(2) 0.001(3) 0.014(2) 0.004(2) C C21 0.066(3) 0.029(3) 0.033(3) 0.001(3) 0.014(2) -0.001(2) C C22 0.044(2) 0.043(3) 0.031(2) 0.003(2) 0.011(2) -0.003(2) C N3 0.057(2) 0.049(3) 0.032(2) 0.001(2) 0.010(2) -0.008(2) N SB 0.0426(2) 0.0366(2) 0.0308(2) 0.0024(1) 0.0033(1) 0.0006(2) Sb F1 0.102(3) 0.064(2) 0.066(2) -0.026(2) 0.002(2) -0.016(2) F F2 0.066(2) 0.096(3) 0.089(3) 0.034(2) 0.002(2) 0.005(3) F F3 0.080(2) 0.060(2) 0.037(2) -0.013(2) 0.019(1) 0.001(2) F F4 0.102(3) 0.052(2) 0.054(2) -0.031(2) -0.003(2) 0.001(2) F F5 0.058(2) 0.080(3) 0.084(2) 0.027(2) 0.021(2) 0.029(2) F F6 0.116(3) 0.058(2) 0.036(2) 0.009(2) 0.015(2) 0.010(2) F C23 0.070(5) 0.119(7) 0.32(2) -0.012(6) -0.037(7) 0.081(9) C O2 0.057(2) 0.074(3) 0.124(4) 0.007(2) -0.019(3) 0.022(3) O C24 0.097(6) 0.127(7) 0.172(9) 0.046(6) -0.027(6) -0.049(7) C O3 0.075(3) 0.083(4) 0.258(9) 0.007(3) -0.001(5) -0.006(5) O C25 0.049(7) 0.12(1) 0.046(7) -0.001(8) -0.004(5) -0.001(8) C CL1 0.107(2) 0.221(3) 0.159(2) 0.010(2) 0.026(1) 0.113(2) Cl CL2 0.073(2) 0.126(3) 0.164(3) 0.0000 -0.033(2) 0.0000 Cl # 10. MOLECULAR GEOMETRY 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 AG N1 2.196(4) . . ? AG N2 2.222(4) . ._455 ? AG N3 2.257(5) . 8_445 ? C1 O1 1.433(6) . . ? C1 C2 1.538(6) . . ? C1 C9 1.532(6) . . ? C1 C16 1.531(6) . . ? C2 C3 1.401(7) . . ? C2 C7 1.383(6) . . ? C3 C4 1.401(7) . . ? C4 C5 1.387(7) . . ? C5 C6 1.408(7) . . ? C5 C8 1.441(7) . . ? C6 C7 1.377(7) . . ? C8 N1 1.138(6) . . ? C9 C10 1.373(7) . . ? C9 C14 1.390(6) . . ? C10 C11 1.376(7) . . ? C11 C12 1.395(7) . . ? C12 C13 1.388(8) . . ? C12 C15 1.442(7) . . ? C13 C14 1.365(7) . . ? C15 N2 1.144(7) . . ? C16 C17 1.394(7) . . ? C16 C21 1.391(7) . . ? C17 C18 1.382(7) . . ? C18 C19 1.389(8) . . ? C19 C20 1.396(8) . . ? C19 C22 1.437(7) . . ? C20 C21 1.375(7) . . ? C22 N3 1.139(7) . . ? SB F1 1.867(4) . . ? SB F2 1.863(4) . . ? SB F3 1.865(3) . . ? SB F4 1.866(4) . . ? SB F5 1.855(4) . . ? SB F6 1.869(4) . . ? C23 O2 1.40(1) . . ? C24 O3 1.30(1) . . ? C25 C25 1.06(3) . 2_756 ? C25 CL1 1.67(2) . . ? C25 CL1 1.68(2) . 2_756 ? C25 CL2 1.86(2) . . ? C25 CL2 1.86(2) . 2_756 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 N1 AG N2 120.8(2) . . ._455 ? N1 AG N3 123.7(2) . . 8_445 ? N2 AG N3 107.8(2) ._455 . 8_445 ? O1 C1 C2 106.8(4) . . . ? O1 C1 C9 106.3(4) . . . ? O1 C1 C16 110.5(4) . . . ? C2 C1 C9 111.5(4) . . . ? C2 C1 C16 113.3(4) . . . ? C9 C1 C16 108.2(4) . . . ? C1 C2 C3 122.9(4) . . . ? C1 C2 C7 117.7(4) . . . ? C3 C2 C7 119.3(4) . . . ? C2 C3 C4 120.2(5) . . . ? C3 C4 C5 119.3(5) . . . ? C4 C5 C6 120.6(4) . . . ? C4 C5 C8 120.9(5) . . . ? C6 C5 C8 118.5(5) . . . ? C5 C6 C7 119.0(4) . . . ? C2 C7 C6 121.6(4) . . . ? C5 C8 N1 177.2(6) . . . ? C1 C9 C10 121.9(4) . . . ? C1 C9 C14 118.4(4) . . . ? C10 C9 C14 119.6(4) . . . ? C9 C10 C11 121.0(4) . . . ? C10 C11 C12 118.9(5) . . . ? C11 C12 C13 120.2(5) . . . ? C11 C12 C15 119.8(5) . . . ? C13 C12 C15 120.0(5) . . . ? C12 C13 C14 119.8(5) . . . ? C9 C14 C13 120.3(5) . . . ? C12 C15 N2 178.6(6) . . . ? C1 C16 C17 120.7(4) . . . ? C1 C16 C21 121.6(4) . . . ? C17 C16 C21 117.6(5) . . . ? C16 C17 C18 121.3(5) . . . ? C17 C18 C19 119.6(5) . . . ? C18 C19 C20 120.3(5) . . . ? C18 C19 C22 120.0(5) . . . ? C20 C19 C22 119.8(5) . . . ? C19 C20 C21 118.8(5) . . . ? C16 C21 C20 122.4(5) . . . ? C19 C22 N3 178.5(6) . . . ? F1 SB F2 89.5(2) . . . ? F1 SB F3 90.5(2) . . . ? F1 SB F4 179.2(2) . . . ? F1 SB F5 89.9(2) . . . ? F1 SB F6 89.6(2) . . . ? F2 SB F3 90.4(2) . . . ? F2 SB F4 90.3(2) . . . ? F2 SB F5 179.0(2) . . . ? F2 SB F6 90.4(2) . . . ? F3 SB F4 90.3(2) . . . ? F3 SB F5 90.4(2) . . . ? F3 SB F6 179.3(2) . . . ? F4 SB F5 90.3(2) . . . ? F4 SB F6 89.6(2) . . . ? F5 SB F6 88.8(2) . . . ? C25 C25 CL1 72(1) 2_756 . . ? C25 C25 CL1 70(1) 2_756 . 2_756 ? C25 C25 CL2 73.5(4) 2_756 . . ? CL1 C25 CL1 116(1) . . 2_756 ? CL1 C25 CL2 108.7(8) . . . ? CL1 C25 CL2 108.2(8) 2_756 . . ? C25 CL1 C25 36.9(9) . . 2_756 ? C25 CL2 C25 33.1(8) . . 2_756 ? #=============================================================================== data_st855 _database_code_CSD 172696 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C22 H13 N3 O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H13 N3 O' _chemical_formula_weight 335.37 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 25.1606(7) _cell_length_b 9.3019(3) _cell_length_c 15.4356(7) _cell_angle_alpha 90 _cell_angle_beta 91.112(5) _cell_angle_gamma 90 _cell_volume 3611.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7184 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.23 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 7184 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 91 frames Set 2 Theta = -4.80 Kappa = -170.00 Phi = 0.00 21 frames Friedel pairs were averaged. Internal R = 0.00 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7184 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4308 _reflns_number_gt 1835 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1835 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.108 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.098 _refine_ls_wR_factor_ref 0.049 _refine_ls_goodness_of_fit_all 1.970 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.064 _refine_diff_density_min -0.094 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol C1 0.64711(6) 0.1638(2) 0.2834(1) 0.035(1) Uani ? ? C O 0.68860(4) 0.0670(2) 0.25982(8) 0.0450(8) Uani ? ? O C2 0.59871(6) 0.0811(2) 0.3154(1) 0.031(1) Uani ? ? C C3 0.59517(7) -0.0663(2) 0.3061(1) 0.041(1) Uani ? ? C C4 0.55024(8) -0.1403(2) 0.3310(1) 0.044(1) Uani ? ? C C5 0.50827(7) -0.0660(2) 0.3666(1) 0.037(1) Uani ? ? C C6 0.51115(6) 0.0809(2) 0.3765(1) 0.040(1) Uani ? ? C C7 0.55595(6) 0.1539(2) 0.3510(1) 0.038(1) Uani ? ? C C8 0.46087(8) -0.1419(2) 0.3905(1) 0.048(1) Uani ? ? C N1 0.42253(7) -0.2004(2) 0.4079(1) 0.069(1) Uani ? ? N C9 0.67002(6) 0.2682(2) 0.3510(1) 0.035(1) Uani ? ? C C10 0.66304(6) 0.2464(2) 0.4387(1) 0.038(1) Uani ? ? C C11 0.68639(6) 0.3353(2) 0.4999(1) 0.040(1) Uani ? ? C C12 0.71749(6) 0.4490(2) 0.4732(1) 0.039(1) Uani ? ? C C13 0.72519(7) 0.4729(3) 0.3861(1) 0.054(1) Uani ? ? C C14 0.70198(7) 0.3820(3) 0.3257(1) 0.051(1) Uani ? ? C C15 0.74372(7) 0.5388(2) 0.5381(1) 0.046(1) Uani ? ? C N2 0.76508(6) 0.6036(2) 0.5915(1) 0.059(1) Uani ? ? N C16 0.62948(6) 0.2385(2) 0.1991(1) 0.035(1) Uani ? ? C C17 0.60136(8) 0.3663(2) 0.2013(1) 0.045(1) Uani ? ? C C18 0.58266(8) 0.4313(2) 0.1260(1) 0.049(1) Uani ? ? C C19 0.59280(7) 0.3676(2) 0.0468(1) 0.041(1) Uani ? ? C C20 0.62104(7) 0.2402(2) 0.0435(1) 0.042(1) Uani ? ? C C21 0.63870(6) 0.1761(2) 0.1195(1) 0.040(1) Uani ? ? C C22 0.57331(8) 0.4347(2) -0.0319(1) 0.048(1) Uani ? ? C N3 0.55771(8) 0.4853(2) -0.0948(1) 0.060(1) Uani ? ? N H01 0.6981(8) 0.020(3) 0.306(2) 0.105(8) Uiso ? ? H H1 0.6240 -0.1177 0.2823 0.0544 Uiso calc C3 H H2 0.5482 -0.2416 0.3236 0.0592 Uiso calc C4 H H3 0.4823 0.1320 0.4008 0.0522 Uiso calc C6 H H4 0.5577 0.2553 0.3577 0.0497 Uiso calc C7 H H5 0.6417 0.1684 0.4572 0.0509 Uiso calc C10 H H6 0.6812 0.3186 0.5599 0.0540 Uiso calc C11 H H7 0.7463 0.5515 0.3679 0.0753 Uiso calc C13 H H8 0.7079 0.3975 0.2658 0.0743 Uiso calc C14 H H9 0.5948 0.4104 0.2555 0.0608 Uiso calc C17 H H10 0.5631 0.5185 0.1286 0.0670 Uiso calc C18 H H11 0.6282 0.1969 -0.0108 0.0570 Uiso calc C20 H H12 0.6575 0.0877 0.1170 0.0540 Uiso calc C21 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol C1 0.0287(8) 0.053(1) 0.029(1) 0.0053(9) 0.0029(8) -0.000(1) C O 0.0398(6) 0.076(1) 0.0301(8) 0.0173(7) 0.0031(6) 0.0037(8) O C2 0.0328(8) 0.038(1) 0.024(1) 0.0036(8) -0.0023(8) 0.002(1) C C3 0.047(1) 0.046(1) 0.033(1) 0.011(1) 0.0009(9) 0.000(1) C C4 0.064(1) 0.033(1) 0.039(1) -0.000(1) -0.002(1) 0.004(1) C C5 0.047(1) 0.039(1) 0.027(1) -0.0060(9) 0.0019(8) 0.003(1) C C6 0.0373(9) 0.044(1) 0.040(1) -0.0015(9) 0.0048(9) -0.005(1) C C7 0.037(1) 0.033(1) 0.044(1) -0.0012(8) 0.0027(9) -0.003(1) C C8 0.069(1) 0.048(1) 0.033(1) -0.014(1) 0.010(1) -0.001(1) C N1 0.084(1) 0.070(1) 0.056(1) -0.030(1) 0.021(1) -0.004(1) N C9 0.0273(9) 0.061(1) 0.026(1) -0.0015(9) 0.0008(8) 0.004(1) C C10 0.0331(9) 0.051(1) 0.033(1) -0.0039(9) 0.0007(8) 0.006(1) C C11 0.0375(9) 0.059(1) 0.028(1) 0.0006(9) 0.0014(8) 0.004(1) C C12 0.0300(8) 0.063(1) 0.032(1) -0.0038(9) -0.0044(8) 0.001(1) C C13 0.044(1) 0.089(2) 0.041(1) -0.030(1) -0.0022(9) 0.007(1) C C14 0.047(1) 0.095(2) 0.030(1) -0.028(1) 0.0010(9) 0.007(1) C C15 0.038(1) 0.061(1) 0.041(1) 0.000(1) -0.0033(9) 0.007(1) C N2 0.0583(9) 0.071(1) 0.049(1) -0.0040(9) -0.0192(8) -0.002(1) N C16 0.0317(9) 0.047(1) 0.028(1) -0.0056(9) 0.0018(8) 0.001(1) C C17 0.062(1) 0.046(1) 0.032(1) -0.003(1) -0.002(1) -0.002(1) C C18 0.073(1) 0.040(1) 0.042(1) 0.000(1) -0.010(1) 0.001(1) C C19 0.050(1) 0.044(1) 0.031(1) -0.0120(9) -0.0064(9) 0.005(1) C C20 0.043(1) 0.061(1) 0.027(1) -0.002(1) -0.0006(8) -0.001(1) C C21 0.0334(9) 0.057(1) 0.034(1) 0.005(1) 0.0014(8) 0.000(1) C C22 0.073(1) 0.039(1) 0.038(1) -0.011(1) -0.008(1) 0.003(1) C N3 0.108(1) 0.043(1) 0.047(1) -0.008(1) -0.020(1) 0.009(1) N # 10. MOLECULAR GEOMETRY 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 C1 O 1.431(2) . . ? C1 C2 1.531(3) . . ? C1 C9 1.530(3) . . ? C1 C16 1.533(3) . . ? C1 H01 1.8842 . . ? O H01 0.87(3) . . ? C2 C3 1.381(3) . . ? C2 C7 1.393(3) . . ? C3 C4 1.384(3) . . ? C4 C5 1.385(3) . . ? C5 C6 1.377(3) . . ? C5 C8 1.440(3) . . ? C6 C7 1.380(3) . . ? C8 N1 1.144(3) . . ? C9 C10 1.383(3) . . ? C9 C14 1.391(3) . . ? C10 C11 1.378(3) . . ? C11 C12 1.383(3) . . ? C12 C13 1.379(3) . . ? C12 C15 1.454(3) . . ? C13 C14 1.380(3) . . ? C15 N2 1.146(3) . . ? N2 H01 2.1514 . 7_656 ? C16 C17 1.384(3) . . ? C16 C21 1.383(3) . . ? C17 C18 1.384(3) . . ? C18 C19 1.387(3) . . ? C19 C20 1.383(3) . . ? C19 C22 1.443(3) . . ? C20 C21 1.382(3) . . ? C22 N3 1.141(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 C1 C2 110.8(2) . . . ? O C1 C9 107.8(1) . . . ? O C1 C16 105.7(2) . . . ? O C1 H01 25.93 . . . ? C2 C1 C9 113.0(2) . . . ? C2 C1 C16 106.4(1) . . . ? C2 C1 H01 97.24 . . . ? C9 C1 C16 113.0(2) . . . ? C9 C1 H01 94.62 . . . ? C16 C1 H01 131.55 . . . ? C1 O H01 107.4(17) . . . ? C1 C2 C3 121.1(2) . . . ? C1 C2 C7 120.5(2) . . . ? C3 C2 C7 118.3(2) . . . ? C2 C3 C4 121.1(2) . . . ? C3 C4 C5 119.7(2) . . . ? C4 C5 C6 120.0(2) . . . ? C4 C5 C8 119.9(2) . . . ? C6 C5 C8 120.0(2) . . . ? C5 C6 C7 119.9(2) . . . ? C2 C7 C6 121.0(2) . . . ? C5 C8 N1 178.3(3) . . . ? C1 C9 C10 121.4(2) . . . ? C1 C9 C14 120.2(2) . . . ? C10 C9 C14 118.2(2) . . . ? C9 C10 C11 121.5(2) . . . ? C10 C11 C12 119.4(2) . . . ? C11 C12 C13 120.3(2) . . . ? C11 C12 C15 119.1(2) . . . ? C13 C12 C15 120.5(2) . . . ? C12 C13 C14 119.6(2) . . . ? C9 C14 C13 121.0(2) . . . ? C12 C15 N2 176.6(3) . . . ? C15 N2 H01 116.08 . . 7_656 ? C1 C16 C17 120.6(2) . . . ? C1 C16 C21 120.9(2) . . . ? C17 C16 C21 118.5(2) . . . ? C16 C17 C18 121.4(2) . . . ? C17 C18 C19 119.2(2) . . . ? C18 C19 C20 120.1(2) . . . ? C18 C19 C22 119.5(2) . . . ? C20 C19 C22 120.4(2) . . . ? C19 C20 C21 119.7(2) . . . ? C16 C21 C20 121.1(2) . . . ? C19 C22 N3 178.7(3) . . . ? C1 H01 O 46.33 . . . ? C1 H01 N2 142.76 . . 7_656 ? O H01 N2 169.84 . . 7_656 ?