# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Braunstein, Pierre' 'Clerc, Guislaine' 'Morise, Xavier' _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Universite Louis Pasteur 4 rue Blaise Pascal F-67070 Strasbourg Cedex FRANCE ; _publ_contact_author_phone '+33/(0)3-90-24-13-08' _publ_contact_author_fax '+33/(0)3-90-24-13-22' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_requested_journal 'New Journal of Chemistry' _publ_requested_category FM _publ_section_title ; Cyclopropanation and Diels-Alder reactions catalyzed by the first heterobimetallic complexes with bridging phosphino-oxazoline ligands ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; data_st499 _database_code_CSD 177707 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C35 H32 Fe N2 O5 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H32 Fe N2 O5 P2' _chemical_formula_weight 678.45 _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 Fe ? 0.301 0.845 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 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall ' F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,+z 1/4+x,1/4-y,1/4+z 1/4-x,1/4+y,1/4+z +x,1/2+y,1/2+z -x,1/2-y,1/2+z 1/4+x,3/4-y,3/4+z 1/4-x,3/4+y,3/4+z 1/2+x,+y,1/2+z 1/2-x,-y,1/2+z 3/4+x,1/4-y,3/4+z 3/4-x,1/4+y,3/4+z 1/2+x,1/2+y,+z 1/2-x,1/2-y,+z 3/4+x,3/4-y,1/4+z 3/4-x,3/4+y,1/4+z _cell_length_a 41.966(1) _cell_length_b 34.575(1) _cell_length_c 9.741(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14133(2) _cell_formula_units_Z 16 _cell_measurement_temperature 173 _cell_measurement_reflns_used 17857 _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 'yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 5632 _exptl_absorpt_coefficient_mu 0.559 _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 ; 17857 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 = 8.50 Omega = 180.00 Kappa = 0.00 77 frames Set 2 Theta = -6.70 Kappa = -132.00 Phi = 0.00 13 frames Friedel pairs were not averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17857 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4422 _reflns_number_gt 2614 _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 0.10(3) _refine_ls_number_reflns 2614 _refine_ls_number_parameters 441 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.085 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_all 0.106 _refine_ls_wR_factor_ref 0.079 _refine_ls_goodness_of_fit_all 1.802 _refine_ls_goodness_of_fit_ref 1.361 _refine_ls_shift/su_max 0.022 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.175 _refine_diff_density_min -0.051 #=============================================================================== # 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 FE 0.70794(3) 0.12217(3) 0.13032(3) 0.0231(4) 1.000 Uani ? ? Fe C1 0.7063(2) 0.0740(2) 0.0711(8) 0.026(4) 1.000 Uani ? ? C O1 0.7047(1) 0.0422(2) 0.0307(7) 0.039(3) 1.000 Uani ? ? O C2 0.7010(2) 0.1603(2) 0.0114(8) 0.028(4) 1.000 Uani ? ? C O2 0.6969(1) 0.1840(2) -0.0675(7) 0.046(3) 1.000 Uani ? ? O C3 0.7148(2) 0.1322(3) 0.3082(9) 0.036(5) 1.000 Uani ? ? C O3 0.7205(2) 0.1387(2) 0.4205(6) 0.057(4) 1.000 Uani ? ? O P1 0.65673(5) 0.11958(5) 0.1761(2) 0.0234(9) 1.000 Uani ? ? P C4 0.6310(2) 0.1016(2) 0.0361(8) 0.030(4) 1.000 Uani ? ? C C5 0.6380(2) 0.1168(2) -0.1032(9) 0.036(5) 1.000 Uani ? ? C N1 0.6236(2) 0.1454(2) -0.1576(7) 0.048(5) 1.000 Uani ? ? N C6 0.6385(3) 0.1510(3) -0.294(1) 0.061(7) 1.000 Uani ? ? C C7 0.6640(3) 0.1188(3) -0.304(1) 0.058(7) 1.000 Uani ? ? C O4 0.6603(1) 0.0977(2) -0.1749(6) 0.048(4) 1.000 Uani ? ? O C8 0.6378(2) 0.1651(2) 0.2281(8) 0.024(4) 1.000 Uani ? ? C C9 0.6158(2) 0.1852(2) 0.1486(9) 0.031(4) 1.000 Uani ? ? C C10 0.6031(2) 0.2203(2) 0.196(1) 0.040(5) 1.000 Uani ? ? C C11 0.6117(2) 0.2353(2) 0.316(1) 0.036(5) 1.000 Uani ? ? C C12 0.6338(2) 0.2159(2) 0.3962(9) 0.042(5) 1.000 Uani ? ? C C13 0.6468(2) 0.1812(2) 0.3541(9) 0.040(5) 1.000 Uani ? ? C C14 0.6445(2) 0.0862(2) 0.3142(8) 0.028(4) 1.000 Uani ? ? C C15 0.6137(2) 0.0880(3) 0.365(1) 0.049(5) 1.000 Uani ? ? C C16 0.6042(3) 0.0608(3) 0.465(1) 0.078(7) 1.000 Uani ? ? C C17 0.6272(3) 0.0311(3) 0.504(1) 0.070(7) 1.000 Uani ? ? C C18 0.6562(2) 0.0299(3) 0.4549(9) 0.053(6) 1.000 Uani ? ? C C19 0.6657(2) 0.0575(2) 0.3599(8) 0.032(4) 1.000 Uani ? ? C P2 0.76001(5) 0.12244(6) 0.0945(2) 0.024(1) 1.000 Uani ? ? P C20 0.7844(2) 0.0932(3) 0.2176(8) 0.037(5) 1.000 Uani ? ? C C21 0.7753(2) 0.0520(3) 0.2287(9) 0.050(5) 1.000 Uani ? ? C N2 0.7869(2) 0.0257(2) 0.1504(9) 0.053(5) 1.000 Uani ? ? N C22 0.7731(3) -0.0117(3) 0.194(1) 0.071(7) 1.000 Uani ? ? C C23 0.7467(3) 0.0007(3) 0.296(1) 0.062(6) 1.000 Uani ? ? C O5 0.7527(2) 0.0417(2) 0.3189(7) 0.065(4) 1.000 Uani ? ? O C24 0.7737(2) 0.1056(2) -0.0758(7) 0.029(4) 1.000 Uani ? ? C C25 0.8028(2) 0.0894(3) -0.0979(9) 0.049(5) 1.000 Uani ? ? C C26 0.8122(2) 0.0785(3) -0.229(1) 0.061(6) 1.000 Uani ? ? C C27 0.7933(2) 0.0844(3) -0.334(1) 0.057(6) 1.000 Uani ? ? C C28 0.7631(3) 0.1004(4) -0.316(1) 0.070(7) 1.000 Uani ? ? C C29 0.7536(2) 0.1108(3) -0.186(1) 0.056(6) 1.000 Uani ? ? C C30 0.7807(2) 0.1698(2) 0.1123(8) 0.028(4) 1.000 Uani ? ? C C31 0.7620(4) 0.2064(5) 0.146(2) 0.036(9) 0.500 Uani ? ? C C32 0.7765(4) 0.2414(5) 0.160(2) 0.04(1) 0.500 Uani ? ? C C33 0.8106(2) 0.2402(3) 0.142(1) 0.050(6) 1.000 Uani ? ? C C34 0.8272(4) 0.2094(5) 0.088(2) 0.05(1) 0.500 Uani ? ? C C35 0.8116(4) 0.1747(5) 0.072(2) 0.029(8) 0.500 Uani ? ? C C36 0.7878(4) 0.1897(5) 0.002(2) 0.038(9) 0.500 Uani ? ? C C37 0.7999(5) 0.2267(6) 0.020(2) 0.05(1) 0.500 Uani ? ? C C38 0.8038(4) 0.2161(6) 0.264(2) 0.05(1) 0.500 Uani ? ? C C39 0.7892(4) 0.1808(5) 0.252(2) 0.031(8) 0.500 Uani ? ? C H1 0.6096 0.1082 0.0579 0.0396 1.000 Uiso calc C4 H H2 0.6331 0.0742 0.0330 0.0396 1.000 Uiso calc C4 H H3 0.6481 0.1758 -0.2997 0.0857 1.000 Uiso calc C6 H H4 0.6231 0.1483 -0.3646 0.0857 1.000 Uiso calc C6 H H5 0.6848 0.1296 -0.3113 0.0876 1.000 Uiso calc C7 H H6 0.6601 0.1025 -0.3804 0.0876 1.000 Uiso calc C7 H H7 0.6094 0.1751 0.0622 0.0447 1.000 Uiso calc C9 H H8 0.5880 0.2336 0.1406 0.0548 1.000 Uiso calc C10 H H9 0.6027 0.2590 0.3464 0.0545 1.000 Uiso calc C11 H H10 0.6401 0.2266 0.4818 0.0557 1.000 Uiso calc C12 H H11 0.6619 0.1683 0.4106 0.0521 1.000 Uiso calc C13 H H12 0.5992 0.1071 0.3336 0.0649 1.000 Uiso calc C15 H H13 0.5837 0.0618 0.5058 0.1028 1.000 Uiso calc C16 H H14 0.6208 0.0117 0.5668 0.1038 1.000 Uiso calc C17 H H15 0.6706 0.0104 0.4843 0.0703 1.000 Uiso calc C18 H H16 0.6868 0.0570 0.3252 0.0426 1.000 Uiso calc C19 H H17 0.7824 0.1046 0.3060 0.0489 1.000 Uiso calc C20 H H18 0.8060 0.0944 0.1888 0.0489 1.000 Uiso calc C20 H H19 0.7886 -0.0274 0.2385 0.0941 1.000 Uiso calc C22 H H20 0.7643 -0.0253 0.1184 0.0941 1.000 Uiso calc C22 H H21 0.7483 -0.0134 0.3791 0.0825 1.000 Uiso calc C23 H H22 0.7262 -0.0031 0.2567 0.0825 1.000 Uiso calc C23 H H23 0.8169 0.0855 -0.0228 0.0674 1.000 Uiso calc C25 H H24 0.8324 0.0668 -0.2426 0.0837 1.000 Uiso calc C26 H H25 0.8002 0.0777 -0.4241 0.0756 1.000 Uiso calc C27 H H26 0.7493 0.1041 -0.3922 0.0949 1.000 Uiso calc C28 H H27 0.7330 0.1215 -0.1720 0.0778 1.000 Uiso calc C29 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 FE 0.0194(4) 0.0246(4) 0.0259(4) -0.0003(5) 0.0026(4) -0.0034(5) Fe C1 0.017(4) 0.034(4) 0.032(4) -0.002(3) 0.003(3) 0.002(4) C O1 0.041(4) 0.025(3) 0.059(4) -0.005(3) 0.004(3) -0.011(3) O C2 0.026(4) 0.023(4) 0.036(4) -0.004(3) 0.008(3) -0.004(3) C O2 0.056(4) 0.033(3) 0.052(3) 0.007(3) 0.007(3) 0.010(3) O C3 0.027(4) 0.066(6) 0.027(4) 0.005(4) 0.001(4) -0.015(4) C O3 0.049(4) 0.115(6) 0.033(3) 0.013(4) -0.006(3) -0.016(4) O P1 0.0200(9) 0.0234(9) 0.027(1) 0.0015(8) 0.0027(8) 0.0016(8) P C4 0.022(4) 0.033(4) 0.037(4) 0.002(4) -0.004(3) 0.000(4) C C5 0.027(4) 0.042(5) 0.041(5) -0.001(4) -0.003(4) -0.003(4) C N1 0.049(5) 0.062(5) 0.037(4) 0.007(4) 0.003(4) 0.013(4) N C6 0.069(7) 0.094(8) 0.035(5) -0.002(7) -0.002(5) 0.015(5) C C7 0.061(7) 0.113(9) 0.028(5) -0.016(6) -0.002(5) -0.007(6) C O4 0.054(4) 0.077(4) 0.027(3) 0.019(3) -0.001(3) -0.003(3) O C8 0.014(3) 0.025(4) 0.037(4) -0.002(3) 0.006(3) 0.001(3) C C9 0.015(4) 0.037(4) 0.051(5) 0.001(3) 0.001(4) 0.004(4) C C10 0.038(5) 0.029(4) 0.060(5) 0.012(4) 0.006(4) 0.011(4) C C11 0.034(5) 0.019(4) 0.073(5) 0.003(4) 0.020(4) 0.006(4) C C12 0.050(5) 0.031(4) 0.048(5) -0.005(4) 0.023(4) -0.008(4) C C13 0.038(5) 0.036(5) 0.046(5) -0.004(4) 0.010(4) 0.002(4) C C14 0.032(4) 0.024(4) 0.029(4) -0.003(4) 0.006(4) -0.001(3) C C15 0.036(5) 0.050(5) 0.064(5) 0.002(4) 0.011(5) 0.024(5) C C16 0.065(6) 0.084(7) 0.088(6) -0.008(6) 0.045(5) 0.039(6) C C17 0.14(1) 0.047(6) 0.052(6) -0.013(7) 0.006(7) 0.027(5) C C18 0.067(6) 0.055(6) 0.040(5) 0.010(5) 0.019(5) 0.009(5) C C19 0.041(5) 0.029(4) 0.028(4) 0.004(4) -0.002(4) 0.004(3) C P2 0.0179(9) 0.028(1) 0.027(1) -0.0011(8) -0.0005(7) -0.0064(8) P C20 0.034(5) 0.044(5) 0.035(4) 0.001(4) -0.003(4) -0.004(4) C C21 0.036(5) 0.060(6) 0.058(5) -0.013(5) -0.014(4) 0.028(5) C N2 0.069(5) 0.034(4) 0.064(5) -0.003(4) 0.015(5) 0.007(4) N C22 0.091(8) 0.053(6) 0.073(7) -0.022(6) 0.003(7) 0.011(6) C C23 0.051(6) 0.055(5) 0.084(6) -0.007(5) -0.007(6) 0.035(5) C O5 0.062(4) 0.065(5) 0.068(4) 0.008(4) 0.007(4) 0.026(4) O C24 0.028(4) 0.032(4) 0.027(4) -0.004(4) 0.003(3) -0.006(3) C C25 0.034(5) 0.073(6) 0.048(5) 0.022(4) 0.011(4) -0.013(5) C C26 0.040(6) 0.095(8) 0.058(6) 0.002(6) 0.010(5) -0.033(5) C C27 0.048(5) 0.072(7) 0.054(6) -0.003(5) 0.025(4) -0.024(5) C C28 0.087(8) 0.088(8) 0.045(6) 0.026(7) 0.003(6) -0.014(6) C C29 0.058(6) 0.086(7) 0.036(5) 0.036(5) -0.002(5) -0.016(5) C C30 0.016(4) 0.034(4) 0.042(4) -0.008(3) 0.003(4) -0.008(4) C C31 0.032(8) 0.031(8) 0.045(9) -0.025(6) -0.003(8) -0.003(7) C C32 0.04(1) 0.021(8) 0.08(1) 0.000(8) -0.01(1) -0.015(9) C C33 0.048(6) 0.039(5) 0.068(6) -0.006(4) -0.004(5) -0.002(5) C C34 0.06(1) 0.04(1) 0.039(9) -0.032(8) 0.000(9) -0.002(8) C C35 0.019(7) 0.033(9) 0.040(8) -0.007(7) 0.000(7) 0.003(7) C C36 0.039(9) 0.034(9) 0.041(9) -0.022(8) 0.003(8) -0.007(8) C C37 0.07(1) 0.05(1) 0.05(1) -0.035(9) -0.00(1) 0.005(9) C C38 0.04(1) 0.05(1) 0.06(1) 0.006(9) -0.018(9) -0.017(9) C C39 0.023(8) 0.034(9) 0.040(8) -0.021(7) -0.003(7) -0.008(7) C # 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 FE C1 1.763(9) . . ? FE C2 1.78(1) . . ? FE C3 1.79(1) . . ? FE P1 2.197(3) . . ? FE P2 2.213(3) . . ? C1 O1 1.17(1) . . ? C2 O2 1.14(1) . . ? C3 O3 1.14(1) . . ? P1 C4 1.848(9) . . ? P1 C8 1.835(9) . . ? P1 C14 1.844(9) . . ? C4 C5 1.48(1) . . ? C5 N1 1.28(1) . . ? C5 C6 2.20(2) . . ? C5 C7 2.24(2) . . ? C5 O4 1.34(1) . . ? N1 C6 1.48(1) . . ? C6 C7 1.55(2) . . ? C7 O4 1.46(1) . . ? C8 C9 1.39(1) . . ? C8 C13 1.40(1) . . ? C9 C10 1.40(1) . . ? C10 C11 1.33(2) . . ? C11 C12 1.39(1) . . ? C12 C13 1.38(1) . . ? C14 C15 1.39(1) . . ? C14 C19 1.40(1) . . ? C15 C16 1.41(1) . . ? C16 C17 1.46(2) . . ? C17 C18 1.31(2) . . ? C18 C19 1.39(1) . . ? P2 C20 1.87(1) . . ? P2 C24 1.850(9) . . ? P2 C30 1.860(9) . . ? C20 C21 1.48(1) . . ? C21 N2 1.28(1) . . ? C21 C22 2.23(2) . . ? C21 C23 2.24(2) . . ? C21 O5 1.34(1) . . ? N2 C22 1.48(1) . . ? N2 O5 2.25(1) . . ? C22 C23 1.54(2) . . ? C23 O5 1.46(2) . . ? C24 C25 1.36(1) . . ? C24 C29 1.38(1) . . ? C25 C26 1.39(2) . . ? C26 C27 1.31(2) . . ? C27 C28 1.39(2) . . ? C28 C29 1.38(2) . . ? C30 C31 1.53(2) . . ? C30 C35 1.36(2) . . ? C30 C36 1.31(2) . . ? C30 C39 1.45(2) . . ? C31 C32 1.36(2) . . ? C31 C36 1.86(3) . . ? C31 C37 2.13(3) . . ? C31 C38 2.12(3) . . ? C31 C39 1.77(3) . . ? C32 C33 1.44(2) . . ? C32 C37 1.76(3) . . ? C32 C38 1.76(3) . . ? C33 C34 1.38(3) . . ? C33 C37 1.35(3) . . ? C33 C38 1.47(3) . . ? C34 C35 1.38(2) . . ? C34 C36 1.97(3) . . ? C34 C37 1.45(3) . . ? C34 C38 1.98(3) . . ? C35 C36 1.31(3) . . ? C35 C37 1.93(3) . . ? C35 C39 1.99(3) . . ? C36 C37 1.39(3) . . ? C38 C39 1.37(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 C1 FE C2 118.7(4) . . . ? C1 FE C3 120.4(5) . . . ? C1 FE P1 89.4(3) . . . ? C1 FE P2 89.5(3) . . . ? C2 FE C3 120.9(5) . . . ? C2 FE P1 90.1(3) . . . ? C2 FE P2 93.3(3) . . . ? C3 FE P1 88.2(3) . . . ? C3 FE P2 89.6(3) . . . ? P1 FE P2 176.6(1) . . . ? FE C1 O1 178.9(8) . . . ? FE C2 O2 177.9(8) . . . ? FE C3 O3 177.2(9) . . . ? FE P1 C4 115.8(3) . . . ? FE P1 C8 116.3(3) . . . ? FE P1 C14 116.4(3) . . . ? C4 P1 C8 103.9(4) . . . ? C4 P1 C14 99.5(4) . . . ? C8 P1 C14 102.5(4) . . . ? P1 C4 C5 116.1(6) . . . ? C4 C5 N1 124.1(9) . . . ? C4 C5 C6 164.4(9) . . . ? C4 C5 C7 154.8(8) . . . ? C4 C5 O4 116.1(8) . . . ? N1 C5 C6 40.2(6) . . . ? N1 C5 C7 81.0(7) . . . ? N1 C5 O4 119.7(9) . . . ? C6 C5 C7 40.8(5) . . . ? C6 C5 O4 79.5(7) . . . ? C7 C5 O4 38.8(6) . . . ? C5 N1 C6 105.9(9) . . . ? C5 C6 N1 33.9(5) . . . ? C5 C6 C7 71.0(7) . . . ? N1 C6 C7 104(1) . . . ? C5 C7 C6 68.2(7) . . . ? C5 C7 O4 35.1(5) . . . ? C6 C7 O4 103.3(9) . . . ? C5 O4 C7 106.1(9) . . . ? P1 C8 C9 124.2(7) . . . ? P1 C8 C13 117.8(7) . . . ? C9 C8 C13 117.9(9) . . . ? C8 C9 C10 120.2(9) . . . ? C9 C10 C11 121.4(9) . . . ? C10 C11 C12 119.3(9) . . . ? C11 C12 C13 121(1) . . . ? C8 C13 C12 119(1) . . . ? P1 C14 C15 119.6(7) . . . ? P1 C14 C19 119.9(7) . . . ? C15 C14 C19 120.4(8) . . . ? C14 C15 C16 118(1) . . . ? C15 C16 C17 117(1) . . . ? C16 C17 C18 123(1) . . . ? C17 C18 C19 119(1) . . . ? C14 C19 C18 121.1(9) . . . ? FE P2 C20 115.9(3) . . . ? FE P2 C24 116.5(3) . . . ? FE P2 C30 116.7(3) . . . ? C20 P2 C24 103.6(4) . . . ? C20 P2 C30 99.2(4) . . . ? C24 P2 C30 102.5(4) . . . ? P2 C20 C21 115.2(7) . . . ? C20 C21 N2 122(1) . . . ? C20 C21 C22 162(1) . . . ? C20 C21 C23 157(1) . . . ? C20 C21 O5 119(1) . . . ? N2 C21 C22 39.4(6) . . . ? N2 C21 C23 79.4(8) . . . ? N2 C21 O5 118(1) . . . ? C22 C21 C23 40.4(5) . . . ? C22 C21 O5 78.9(7) . . . ? C23 C21 O5 38.7(6) . . . ? C21 N2 C22 107(1) . . . ? C21 N2 O5 31.7(6) . . . ? C22 N2 O5 75.7(7) . . . ? C21 C22 N2 33.3(5) . . . ? C21 C22 C23 70.1(8) . . . ? N2 C22 C23 102(1) . . . ? C21 C23 C22 69.5(7) . . . ? C21 C23 O5 35.2(5) . . . ? C22 C23 O5 104.3(9) . . . ? C21 O5 N2 30.1(6) . . . ? C21 O5 C23 106(1) . . . ? N2 O5 C23 75.9(7) . . . ? P2 C24 C25 123.3(7) . . . ? P2 C24 C29 117.9(7) . . . ? C25 C24 C29 118.7(8) . . . ? C24 C25 C26 120(1) . . . ? C25 C26 C27 120(1) . . . ? C26 C27 C28 120(1) . . . ? C27 C28 C29 119(1) . . . ? C24 C29 C28 120(1) . . . ? P2 C30 C31 120.7(8) . . . ? P2 C30 C35 121(1) . . . ? P2 C30 C36 119(1) . . . ? P2 C30 C39 115.6(9) . . . ? C31 C30 C35 116(1) . . . ? C31 C30 C36 81(1) . . . ? C31 C30 C39 72(1) . . . ? C35 C30 C36 58(1) . . . ? C35 C30 C39 89(1) . . . ? C36 C30 C39 124(1) . . . ? C30 C31 C32 122(1) . . . ? C30 C31 C36 44.0(9) . . . ? C30 C31 C37 76(1) . . . ? C30 C31 C38 79(1) . . . ? C30 C31 C39 51(1) . . . ? C32 C31 C36 95(1) . . . ? C32 C31 C37 55(1) . . . ? C32 C31 C38 55(1) . . . ? C32 C31 C39 95(1) . . . ? C36 C31 C37 40.0(9) . . . ? C36 C31 C38 88(1) . . . ? C36 C31 C39 84(1) . . . ? C37 C31 C38 68(1) . . . ? C37 C31 C39 90(1) . . . ? C38 C31 C39 40.0(9) . . . ? C31 C32 C33 113(1) . . . ? C31 C32 C37 85(1) . . . ? C31 C32 C38 84(1) . . . ? C33 C32 C37 48(1) . . . ? C33 C32 C38 53(1) . . . ? C37 C32 C38 86(1) . . . ? C32 C33 C34 124(1) . . . ? C32 C33 C37 77(1) . . . ? C32 C33 C38 74(1) . . . ? C34 C33 C37 64(1) . . . ? C34 C33 C38 88(1) . . . ? C37 C33 C38 116(1) . . . ? C33 C34 C35 118(1) . . . ? C33 C34 C36 90(1) . . . ? C33 C34 C37 57(1) . . . ? C33 C34 C38 47(1) . . . ? C35 C34 C36 41(1) . . . ? C35 C34 C37 86(1) . . . ? C35 C34 C38 87(1) . . . ? C36 C34 C37 44(1) . . . ? C36 C34 C38 89(1) . . . ? C37 C34 C38 87(1) . . . ? C30 C35 C34 122(1) . . . ? C30 C35 C36 58(1) . . . ? C30 C35 C37 87(1) . . . ? C30 C35 C39 46.9(8) . . . ? C34 C35 C36 94(1) . . . ? C34 C35 C37 48(1) . . . ? C34 C35 C39 91(1) . . . ? C36 C35 C37 45(1) . . . ? C36 C35 C39 93(1) . . . ? C37 C35 C39 90(1) . . . ? C30 C36 C31 54(1) . . . ? C30 C36 C34 91(1) . . . ? C30 C36 C35 62(1) . . . ? C30 C36 C37 117(1) . . . ? C31 C36 C34 93(1) . . . ? C31 C36 C35 99(1) . . . ? C31 C36 C37 80(1) . . . ? C34 C36 C35 43(1) . . . ? C34 C36 C37 47(1) . . . ? C35 C36 C37 91(1) . . . ? C31 C37 C32 39.5(9) . . . ? C31 C37 C33 81(1) . . . ? C31 C37 C34 100(1) . . . ? C31 C37 C35 74(1) . . . ? C31 C37 C36 59(1) . . . ? C32 C37 C33 53(1) . . . ? C32 C37 C34 101(1) . . . ? C32 C37 C35 101(1) . . . ? C32 C37 C36 99(1) . . . ? C33 C37 C34 58(1) . . . ? C33 C37 C35 90(1) . . . ? C33 C37 C36 123(1) . . . ? C34 C37 C35 45(1) . . . ? C34 C37 C36 88(1) . . . ? C35 C37 C36 42(1) . . . ? C31 C38 C32 39.7(9) . . . ? C31 C38 C33 79(1) . . . ? C31 C38 C34 85(1) . . . ? C31 C38 C39 56(1) . . . ? C32 C38 C33 52(1) . . . ? C32 C38 C34 83(1) . . . ? C32 C38 C39 95(1) . . . ? C33 C38 C34 43(1) . . . ? C33 C38 C39 121(1) . . . ? C34 C38 C39 92(1) . . . ? C30 C39 C31 55(1) . . . ? C30 C39 C35 43.2(8) . . . ? C30 C39 C38 115(1) . . . ? C31 C39 C35 81(1) . . . ? C31 C39 C38 83(1) . . . ? C35 C39 C38 87(1) . . . ? data_st341 _database_code_CSD 177708 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2 1.5 CH2Cl2' _chemical_formula_moiety 'C73 H70 B2 Cl6 Cu2 F8 Fe2 N4 O10 P4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C73 H70 B2 Cl6 Cu2 F8 Fe2 N4 O10 P4' _chemical_formula_weight 1912.39 _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 0.001 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 Fe ? 0.301 0.845 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 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,+y,-z -x,-y,-z +x,-y,+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,+z _cell_length_a 24.4623(7) _cell_length_b 14.3872(6) _cell_length_c 12.4708(4) _cell_angle_alpha 90 _cell_angle_beta 111.598(4) _cell_angle_gamma 90 _cell_volume 4080.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13114 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 32.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 1.213 _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 ; 13114 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 29. mm. Scan angle = 2.0 deg 1 scans of 71 sec per frame. Data collection was divided into 1 sets with the following starting angles and number of frames : Set 1 Theta = 8.85 Omega = 180.00 Kappa = 0.00 76 frames Friedel pairs were not averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13114 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 32.51 _reflns_number_total 6229 _reflns_number_gt 4571 _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 4571 _refine_ls_number_parameters 276 _refine_ls_number_restraints 49 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_all 0.062 _refine_ls_wR_factor_ref 0.057 _refine_ls_goodness_of_fit_all 1.254 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_shift/su_max 0.004 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.691 _refine_diff_density_min -0.093 #=============================================================================== # 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 FE 0.88136(2) 0.0000 0.11455(4) 0.0236(2) 0.500 Uani ? ? Fe CU 0.85943(2) 0.0000 0.29876(4) 0.0373(2) 0.500 Uani ? ? Cu C1 0.9428(2) 0.0000 0.2492(3) 0.033(1) 0.500 Uani ? ? C O1 0.9854(1) 0.0000 0.3307(3) 0.046(2) 0.500 Uani ? ? O C2 0.8044(2) 0.0000 0.0842(3) 0.029(1) 0.500 Uani ? ? C O2 0.7538(1) 0.0000 0.0615(2) 0.037(1) 0.500 Uani ? ? O C3 0.9092(1) 0.0000 0.0007(3) 0.027(1) 0.500 Uani ? ? C O3 0.9279(1) 0.0000 -0.0708(2) 0.040(1) 0.500 Uani ? ? O P1 0.87618(2) 0.15476(4) 0.10841(5) 0.0240(2) 1.000 Uani ? ? P C4 0.9452(1) 0.2183(2) 0.1694(2) 0.0261(9) 1.000 Uani ? ? C C5 0.9510(1) 0.3004(2) 0.2315(2) 0.035(1) 1.000 Uani ? ? C C6 1.0039(1) 0.3493(2) 0.2692(2) 0.038(1) 1.000 Uani ? ? C C7 1.0510(1) 0.3170(2) 0.2446(2) 0.038(1) 1.000 Uani ? ? C C8 1.0462(1) 0.2349(2) 0.1850(2) 0.042(1) 1.000 Uani ? ? C C9 0.9939(1) 0.1851(2) 0.1483(2) 0.035(1) 1.000 Uani ? ? C C10 0.8423(1) 0.2052(2) -0.0364(2) 0.0270(9) 1.000 Uani ? ? C C11 0.8457(1) 0.3009(2) -0.0527(2) 0.031(1) 1.000 Uani ? ? C C12 0.8217(1) 0.3393(2) -0.1620(2) 0.034(1) 1.000 Uani ? ? C C13 0.7944(1) 0.2829(2) -0.2564(2) 0.034(1) 1.000 Uani ? ? C C14 0.7902(1) 0.1887(2) -0.2419(2) 0.033(1) 1.000 Uani ? ? C C15 0.8135(1) 0.1494(2) -0.1318(2) 0.030(1) 1.000 Uani ? ? C C16 0.8286(1) 0.2100(2) 0.1759(2) 0.0269(9) 1.000 Uani ? ? C C17 0.8472(1) 0.1988(2) 0.3033(2) 0.0295(9) 1.000 Uani ? ? C O4 0.85073(9) 0.2781(1) 0.3622(1) 0.0383(9) 1.000 Uani ? ? O C18 0.8709(2) 0.2521(2) 0.4833(3) 0.053(2) 1.000 Uani ? ? C C19 0.8711(1) 0.1470(2) 0.4830(2) 0.044(1) 1.000 Uani ? ? C N 0.8582(1) 0.1235(2) 0.3603(2) 0.0355(9) 1.000 Uani ? ? N B 0.7858(2) 0.5000 0.5649(4) 0.041(2) 0.500 Uani ? ? B F1 0.8454(2) 0.5000 0.6302(4) 0.088(2) 0.500 Uani ? ? F F2 0.7559(1) 0.5000 0.6387(2) 0.058(1) 0.500 Uani ? ? F F3 0.7737(1) 0.4211(2) 0.4991(2) 0.076(1) 1.000 Uani ? ? F C20 0.8488(2) 0.5000 0.3529(3) 0.041(2) 0.500 Uani ? ? C CL2 0.92568(5) 0.5000 0.4264(1) 0.0555(6) 0.500 Uani ? ? Cl CL1 0.83088(6) 0.5000 0.2011(1) 0.0533(6) 0.500 Uani ? ? Cl CL3 0.94173(9) 0.5000 0.0052(3) 0.110(2) 0.500 Uani ? ? Cl C21 1.0000 0.543(1) 0.0000 0.132(9) 0.250 Uani ? ? C H1 0.9186 0.3232 0.2484 0.0456 1.000 Uiso calc C5 H H2 1.0074 0.4051 0.3120 0.0509 1.000 Uiso calc C6 H H3 1.0867 0.3512 0.2688 0.0508 1.000 Uiso calc C7 H H4 1.0788 0.2122 0.1689 0.0550 1.000 Uiso calc C8 H H5 0.9912 0.1279 0.1085 0.0453 1.000 Uiso calc C9 H H6 0.8646 0.3399 0.0118 0.0406 1.000 Uiso calc C11 H H7 0.8240 0.4044 -0.1721 0.0445 1.000 Uiso calc C12 H H8 0.7786 0.3092 -0.3314 0.0441 1.000 Uiso calc C13 H H9 0.7714 0.1502 -0.3069 0.0434 1.000 Uiso calc C14 H H10 0.8098 0.0846 -0.1220 0.0388 1.000 Uiso calc C15 H H11 0.7904 0.1842 0.1413 0.0348 1.000 Uiso calc C16 H H12 0.8272 0.2747 0.1597 0.0348 1.000 Uiso calc C16 H H13 0.8449 0.2751 0.5178 0.0793 1.000 Uiso calc C18 H H14 0.9094 0.2754 0.5237 0.0793 1.000 Uiso calc C18 H H15 0.8415 0.1232 0.5079 0.0595 1.000 Uiso calc C19 H H16 0.9083 0.1235 0.5310 0.0595 1.000 Uiso calc C19 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 FE 0.0237(2) 0.0219(2) 0.0252(2) 0.0000 0.0101(1) 0.0000 Fe CU 0.0553(2) 0.0272(2) 0.0346(2) 0.0000 0.0226(1) 0.0000 Cu C1 0.035(2) 0.027(1) 0.036(1) 0.0000 0.014(1) 0.0000 C O1 0.041(2) 0.056(2) 0.042(1) 0.0000 0.001(1) 0.0000 O C2 0.036(1) 0.023(1) 0.029(1) 0.0000 0.013(1) 0.0000 C O2 0.027(1) 0.043(1) 0.045(1) 0.0000 0.0136(9) 0.0000 O C3 0.028(1) 0.023(1) 0.032(1) 0.0000 0.0136(9) 0.0000 C O3 0.042(1) 0.040(1) 0.038(1) 0.0000 0.0236(8) 0.0000 O P1 0.0234(2) 0.0229(2) 0.0257(2) -0.0000(2) 0.0101(2) -0.0011(2) P C4 0.0240(9) 0.027(1) 0.0275(8) -0.0010(8) 0.0100(6) 0.0001(8) C C5 0.031(1) 0.033(1) 0.042(1) -0.002(1) 0.0140(8) -0.008(1) C C6 0.037(1) 0.036(1) 0.042(1) -0.008(1) 0.0118(9) -0.012(1) C C7 0.032(1) 0.046(1) 0.038(1) -0.010(1) 0.0102(9) -0.005(1) C C8 0.029(1) 0.053(2) 0.049(1) -0.007(1) 0.0191(8) -0.010(1) C C9 0.031(1) 0.037(1) 0.039(1) -0.004(1) 0.0153(7) -0.009(1) C C10 0.0255(9) 0.028(1) 0.0276(8) 0.0013(8) 0.0115(6) 0.0018(8) C C11 0.034(1) 0.027(1) 0.033(1) -0.0001(9) 0.0125(8) 0.0004(9) C C12 0.035(1) 0.030(1) 0.039(1) 0.0035(9) 0.0153(8) 0.007(1) C C13 0.029(1) 0.042(1) 0.0322(9) 0.005(1) 0.0130(7) 0.009(1) C C14 0.031(1) 0.039(1) 0.029(1) 0.001(1) 0.0093(8) -0.002(1) C C15 0.027(1) 0.029(1) 0.032(1) 0.0010(9) 0.0103(7) 0.0002(9) C C16 0.0238(9) 0.027(1) 0.0297(9) 0.0008(8) 0.0107(7) -0.0017(8) C C17 0.0279(9) 0.029(1) 0.0316(9) -0.0015(8) 0.0137(7) -0.0060(9) C O4 0.053(1) 0.0324(9) 0.0331(8) 0.0042(8) 0.0124(7) -0.0072(7) O C18 0.097(2) 0.046(2) 0.033(1) 0.009(2) 0.016(1) -0.009(1) C C19 0.063(2) 0.047(2) 0.030(1) 0.004(1) 0.0190(9) -0.003(1) C N 0.046(1) 0.032(1) 0.0301(8) 0.0004(9) 0.0188(7) -0.0036(8) N B 0.052(2) 0.031(2) 0.041(2) 0.0000 0.021(1) 0.0000 B F1 0.058(2) 0.111(3) 0.106(3) 0.0000 0.020(2) 0.0000 F F2 0.075(1) 0.046(1) 0.056(1) 0.0000 0.0399(8) 0.0000 F F3 0.135(2) 0.052(1) 0.0638(9) -0.023(1) 0.0554(8) -0.0238(9) F C20 0.039(2) 0.040(2) 0.045(2) 0.0000 0.017(1) 0.0000 C CL2 0.0433(5) 0.0750(8) 0.0528(6) 0.0000 0.0101(4) 0.0000 Cl CL1 0.0610(6) 0.0533(6) 0.0466(5) 0.0000 0.0103(5) 0.0000 Cl CL3 0.064(1) 0.090(1) 0.233(3) 0.0000 0.003(2) 0.0000 Cl C21 0.22(1) 0.042(6) 0.25(1) 0.0000 0.180(7) 0.0000 C # 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 FE CU 2.5441(7) . . ? FE CU 2.5441(7) . 4_555 ? FE C1 1.795(4) . . ? FE C1 1.795(4) . 4_555 ? FE C2 1.777(4) . . ? FE C2 1.777(4) . 4_555 ? FE C3 1.786(4) . . ? FE C3 1.786(4) . 4_555 ? FE P1 2.2298(6) . . ? FE P1 2.2298(6) . 4_555 ? CU C1 2.339(4) . . ? CU C1 2.339(4) . 4_555 ? CU C2 2.514(4) . . ? CU C2 2.514(4) . 4_555 ? CU N 1.939(2) . . ? CU N 1.939(2) . 4_555 ? C1 O1 1.157(5) . . ? C1 O1 1.157(5) . 4_555 ? C2 O2 1.164(5) . . ? C2 O2 1.164(5) . 4_555 ? C3 O3 1.142(4) . . ? C3 O3 1.142(4) . 4_555 ? P1 C4 1.822(3) . . ? P1 C10 1.837(2) . . ? P1 C16 1.848(2) . . ? C4 C5 1.391(4) . . ? C4 C9 1.394(4) . . ? C5 C6 1.393(4) . . ? C6 C7 1.379(4) . . ? C7 C8 1.377(4) . . ? C8 C9 1.390(4) . . ? C10 C11 1.399(3) . . ? C10 C15 1.392(4) . . ? C11 C12 1.384(4) . . ? C12 C13 1.382(4) . . ? C13 C14 1.377(4) . . ? C14 C15 1.397(4) . . ? C16 C17 1.491(3) . . ? C17 O4 1.342(3) . . ? C17 N 1.270(3) . . ? O4 C18 1.455(4) . . ? C18 C19 1.511(5) . . ? C19 N 1.483(3) . . ? B F1 1.382(7) . . ? B F1 1.382(7) . 4_565 ? B F2 1.371(6) . . ? B F2 1.371(6) . 4_565 ? B F3 1.367(3) . . ? B F3 1.367(3) . 4_565 ? C20 CL2 1.762(5) . . ? C20 CL2 1.762(5) . 4_565 ? C20 CL1 1.779(5) . . ? C20 CL1 1.779(5) . 4_565 ? CL3 C21 1.576(6) . . ? CL3 C21 1.576(6) . 3_765 ? CL3 C21 1.576(6) . 2_755 ? CL3 C21 1.576(6) . 4_565 ? C21 C21 1.23(3) . 3_765 ? C21 C21 1.23(3) . 4_565 ? 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 CU FE C1 62.4(1) . . . ? CU FE C2 68.5(1) . . . ? CU FE C3 170.5(1) . . . ? CU FE P1 90.16(2) . . . ? CU FE P1 90.16(2) . . 4_555 ? C1 FE C2 131.0(2) . . . ? C1 FE C3 108.1(2) . . . ? C1 FE P1 92.84(2) . . . ? C1 FE P1 92.84(2) . . 4_555 ? C2 FE C3 121.0(2) . . . ? C2 FE P1 87.16(2) . . . ? C2 FE P1 87.16(2) . . 4_555 ? C3 FE P1 90.36(2) . . . ? C3 FE P1 90.36(2) . . 4_555 ? P1 FE P1 173.75(4) . . 4_555 ? FE CU C1 42.9(1) . . . ? FE CU C2 41.14(9) . . . ? FE CU N 113.33(7) . . . ? FE CU N 113.33(7) . . 4_555 ? C1 CU C2 84.0(1) . . . ? C1 CU N 104.25(8) . . . ? C1 CU N 104.25(8) . . 4_555 ? C2 CU N 109.94(7) . . . ? C2 CU N 109.94(7) . . 4_555 ? N CU N 132.7(1) . . 4_555 ? C4 P1 C10 103.0(1) . . . ? C4 P1 C16 103.7(1) . . . ? C10 P1 C16 98.4(1) . . . ? P1 C4 C5 123.2(2) . . . ? P1 C4 C9 118.3(2) . . . ? C5 C4 C9 118.5(2) . . . ? C4 C5 C6 120.6(2) . . . ? C5 C6 C7 120.2(3) . . . ? C6 C7 C8 119.8(3) . . . ? C7 C8 C9 120.4(3) . . . ? C4 C9 C8 120.5(3) . . . ? P1 C10 C11 120.2(2) . . . ? P1 C10 C15 121.1(2) . . . ? C11 C10 C15 118.8(2) . . . ? C10 C11 C12 120.6(2) . . . ? C11 C12 C13 120.1(2) . . . ? C12 C13 C14 120.1(2) . . . ? C13 C14 C15 120.2(3) . . . ? C10 C15 C14 120.1(2) . . . ? P1 C16 C17 116.3(2) . . . ? C16 C17 O4 115.1(2) . . . ? C16 C17 N 127.4(2) . . . ? O4 C17 N 117.5(2) . . . ? C17 O4 C18 106.1(2) . . . ? O4 C18 C19 104.8(2) . . . ? C18 C19 N 103.4(2) . . . ? C17 N C19 107.6(2) . . . ? F1 B F2 108.2(4) . . . ? F1 B F3 107.6(3) . . . ? F1 B F3 107.6(3) . . 4_565 ? F2 B F3 110.6(3) . . . ? F2 B F3 110.6(3) . . 4_565 ? F3 B F3 112.2(4) . . 4_565 ? CL2 C20 CL1 110.6(2) . . . ? C21 CL3 C21 46.0(9) . . 3_765 ? CL3 C21 CL3 134.0(9) . . 3_765 ? CL3 C21 C21 67.0(5) . . 3_765 ? CL3 C21 C21 67.0(5) . 3_765 3_765 ? #===============================================================================