Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 10-11-03 _publ_contact_author_name 'Prof P Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Insitut Le Bel, Universite Louis Pasteur 4 Rue Blaise Pascal Strasbourg Cedex F-67070 FRANCE ; _publ_contact_author_email BRAUNST@CHIMIE.U-STRASBG.FR _publ_section_title ; Nickel and Iron Complexes with Oxazoline- or Pyridine-Phosphonite Ligands; Synthesis, Structure and Application for the Catalytic Oligomerisation of Ethylene ; _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. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; loop_ _publ_author_name 'P. Braunstein' 'L. Saussine' 'F. Speiser' data_st709 _database_code_depnum_ccdc_archive 'CCDC 224561' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C22 H33 Cl2 N2 Ni O4 P' _chemical_formula_sum 'C22 H33 Cl2 N2 Ni O4 P' _chemical_formula_weight 550.11 _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 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 Ni ? 0.285 1.113 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 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 18.2474(6) _cell_length_b 9.4918(2) _cell_length_c 15.6567(7) _cell_angle_alpha 90 _cell_angle_beta 102.837(5) _cell_angle_gamma 90 _cell_volume 2644.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 7156 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_method none _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _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 ; 10258 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 35. mm. Scan angle = 2.0 deg 1 scans of 30 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 5.90 Omega = 0.00 Kappa = 0.00 90 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10258 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.979 _reflns_number_total 6309 _reflns_number_gt 3781 _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 3781 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_all 0.107 _refine_ls_wR_factor_ref 0.048 _refine_ls_goodness_of_fit_all 1.242 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.330 _refine_diff_density_min -0.227 #=============================================================================== # 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 NI 0.77532(2) 0.18460(3) 0.19402(2) 0.0398(2) Uani ? ? Ni CL1 0.70355(4) 0.37724(6) 0.20365(5) 0.0532(4) Uani ? ? Cl CL2 0.87052(4) 0.10371(9) 0.13272(5) 0.0642(4) Uani ? ? Cl P 0.73477(3) 0.00747(6) 0.26395(4) 0.0324(3) Uani ? ? P C1 0.6440(1) -0.0050(2) 0.2904(2) 0.033(1) Uani ? ? C C2 0.6285(1) -0.1127(2) 0.3447(2) 0.044(1) Uani ? ? C C3 0.5588(2) -0.1235(3) 0.3634(2) 0.052(1) Uani ? ? C C4 0.5031(1) -0.0299(3) 0.3283(2) 0.052(1) Uani ? ? C C5 0.5174(1) 0.0761(3) 0.2751(2) 0.051(1) Uani ? ? C C6 0.5878(1) 0.0898(2) 0.2560(2) 0.042(1) Uani ? ? C O1 0.74243(9) -0.1377(2) 0.2139(1) 0.0419(8) Uani ? ? O C7 0.7079(2) -0.1734(2) 0.1241(2) 0.046(1) Uani ? ? C C8 0.7661(2) -0.2602(3) 0.0918(2) 0.074(2) Uani ? ? C C9 0.6370(2) -0.2588(3) 0.1247(2) 0.062(2) Uani ? ? C C10 0.6870(1) -0.0464(3) 0.0652(2) 0.043(1) Uani ? ? C N1 0.6948(1) 0.0845(2) 0.0814(1) 0.040(1) Uani ? ? N C11 0.6575(2) 0.1616(3) -0.0014(2) 0.050(1) Uani ? ? C C12 0.6458(2) 0.0425(4) -0.0685(2) 0.068(2) Uani ? ? C O2 0.6534(1) -0.0852(2) -0.0172(1) 0.061(1) Uani ? ? O C13 0.5835(2) 0.2197(4) 0.0102(2) 0.070(2) Uani ? ? C C14 0.7087(2) 0.2750(3) -0.0221(2) 0.073(2) Uani ? ? C O3 0.78578(8) -0.0249(2) 0.3585(1) 0.0359(8) Uani ? ? O C15 0.8667(1) -0.0038(2) 0.3860(2) 0.037(1) Uani ? ? C C16 0.9075(2) -0.1077(3) 0.3413(2) 0.061(2) Uani ? ? C C17 0.8822(2) -0.0257(3) 0.4845(2) 0.057(2) Uani ? ? C C18 0.8888(1) 0.1460(3) 0.3667(2) 0.041(1) Uani ? ? C N2 0.8563(1) 0.2342(2) 0.3109(1) 0.041(1) Uani ? ? N C19 0.9026(2) 0.3675(3) 0.3260(2) 0.054(2) Uani ? ? C C20 0.9771(2) 0.3107(3) 0.3786(3) 0.084(2) Uani ? ? C O4 0.9562(1) 0.1815(2) 0.4170(2) 0.065(1) Uani ? ? O C21 0.8656(2) 0.4673(3) 0.3803(3) 0.081(2) Uani ? ? C C22 0.9110(2) 0.4349(3) 0.2419(2) 0.080(2) Uani ? ? C H1 0.6666 -0.1789 0.3687 0.0583 Uiso calc C2 H H2 0.5491 -0.1963 0.4010 0.0671 Uiso calc C3 H H3 0.4547 -0.0387 0.3408 0.0702 Uiso calc C4 H H4 0.4788 0.1411 0.2511 0.0695 Uiso calc C5 H H5 0.5972 0.1643 0.2194 0.0555 Uiso calc C6 H H6 0.7466 -0.2872 0.0326 0.0951 Uiso calc C8 H H7 0.8103 -0.2058 0.0954 0.0951 Uiso calc C8 H H8 0.7777 -0.3421 0.1271 0.0951 Uiso calc C8 H H9 0.6132 -0.2837 0.0664 0.0840 Uiso calc C9 H H10 0.6503 -0.3419 0.1585 0.0840 Uiso calc C9 H H11 0.6036 -0.2040 0.1497 0.0840 Uiso calc C9 H H12 0.6827 0.0463 -0.1027 0.0951 Uiso calc C12 H H13 0.5971 0.0481 -0.1059 0.0951 Uiso calc C12 H H14 0.5924 0.2935 0.0522 0.0964 Uiso calc C13 H H15 0.5559 0.2553 -0.0442 0.0964 Uiso calc C13 H H16 0.5555 0.1469 0.0299 0.0964 Uiso calc C13 H H17 0.7144 0.3467 0.0212 0.0981 Uiso calc C14 H H18 0.7564 0.2355 -0.0226 0.0981 Uiso calc C14 H H19 0.6875 0.3142 -0.0779 0.0981 Uiso calc C14 H H20 0.9602 -0.0929 0.3598 0.0826 Uiso calc C16 H H21 0.8957 -0.2007 0.3562 0.0826 Uiso calc C16 H H22 0.8926 -0.0954 0.2797 0.0826 Uiso calc C16 H H23 0.9344 -0.0140 0.5087 0.0854 Uiso calc C17 H H24 0.8545 0.0412 0.5096 0.0854 Uiso calc C17 H H25 0.8674 -0.1182 0.4967 0.0854 Uiso calc C17 H H26 0.9998 0.3755 0.4228 0.1278 Uiso calc C20 H H27 1.0106 0.2917 0.3415 0.1278 Uiso calc C20 H H28 0.8937 0.5522 0.3907 0.1099 Uiso calc C21 H H29 0.8158 0.4878 0.3492 0.1099 Uiso calc C21 H H30 0.8642 0.4240 0.4346 0.1099 Uiso calc C21 H H31 0.9404 0.5181 0.2546 0.1030 Uiso calc C22 H H32 0.9351 0.3711 0.2104 0.1030 Uiso calc C22 H H33 0.8627 0.4583 0.2076 0.1030 Uiso calc C22 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 NI 0.0348(2) 0.0448(2) 0.0406(2) 0.0064(1) 0.0125(1) 0.0128(1) Ni CL1 0.0460(3) 0.0451(3) 0.0728(5) 0.0115(3) 0.0066(3) 0.0065(3) Cl CL2 0.0451(3) 0.1031(5) 0.0568(4) 0.0077(4) 0.0225(3) -0.0024(4) Cl P 0.0284(3) 0.0362(3) 0.0331(3) 0.0036(3) 0.0058(2) 0.0027(3) P C1 0.028(1) 0.039(1) 0.034(1) -0.003(1) 0.004(1) -0.004(1) C C2 0.037(1) 0.047(1) 0.050(1) 0.002(1) 0.008(1) 0.007(1) C C3 0.046(1) 0.051(1) 0.061(2) -0.007(1) 0.018(1) 0.010(1) C C4 0.032(1) 0.069(2) 0.062(2) -0.008(1) 0.014(1) -0.002(2) C C5 0.034(1) 0.061(1) 0.065(2) 0.013(1) 0.010(1) 0.009(1) C C6 0.037(1) 0.045(1) 0.046(1) 0.003(1) 0.009(1) 0.007(1) C O1 0.0469(9) 0.0354(7) 0.0444(9) 0.0075(8) 0.0083(8) -0.0004(7) O C7 0.053(1) 0.042(1) 0.044(1) 0.008(1) 0.010(1) -0.006(1) C C8 0.083(2) 0.071(2) 0.067(2) 0.028(2) 0.021(2) -0.016(2) C C9 0.073(2) 0.050(1) 0.066(2) -0.017(1) 0.006(2) -0.001(1) C C10 0.042(1) 0.052(1) 0.036(1) 0.000(1) 0.012(1) -0.005(1) C N1 0.042(1) 0.0477(9) 0.032(1) 0.0058(9) 0.0083(9) 0.0073(9) N C11 0.053(2) 0.066(1) 0.035(1) 0.000(1) 0.003(1) 0.015(1) C C12 0.082(2) 0.093(2) 0.041(2) -0.002(2) 0.005(2) 0.005(2) C O2 0.086(1) 0.069(1) 0.038(1) -0.005(1) 0.002(1) -0.005(1) O C13 0.059(2) 0.091(2) 0.065(2) 0.014(2) -0.003(2) 0.023(2) C C14 0.085(2) 0.083(2) 0.054(2) -0.003(2) 0.008(2) 0.035(1) C O3 0.0261(8) 0.0480(8) 0.0369(9) -0.0013(7) 0.0022(7) 0.0119(7) O C15 0.022(1) 0.051(1) 0.047(1) 0.002(1) 0.003(1) 0.017(1) C C16 0.044(1) 0.058(1) 0.090(2) 0.012(1) 0.018(2) 0.017(2) C C17 0.034(1) 0.103(2) 0.053(2) -0.004(2) -0.006(1) 0.033(2) C C18 0.027(1) 0.053(1) 0.049(1) -0.002(1) 0.001(1) 0.005(1) C N2 0.033(1) 0.0420(9) 0.048(1) -0.0008(9) 0.0085(9) 0.007(1) N C19 0.045(1) 0.050(1) 0.069(2) -0.014(1) 0.002(1) 0.007(1) C C20 0.057(2) 0.073(2) 0.142(3) -0.023(2) -0.026(2) 0.037(2) C O4 0.041(1) 0.071(1) 0.096(2) -0.0154(9) -0.022(1) 0.028(1) O C21 0.109(3) 0.063(2) 0.078(2) -0.027(2) 0.012(2) -0.005(2) C C22 0.068(2) 0.072(2) 0.103(2) -0.015(2) 0.030(2) 0.026(2) 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 NI CL1 2.2736(7) . . ? NI CL2 2.2954(8) . . ? NI P 2.2210(7) . . ? NI N1 2.241(2) . . ? NI N2 2.133(2) . . ? P C1 1.799(3) . . ? P O1 1.606(2) . . ? P O3 1.593(2) . . ? C1 C2 1.398(4) . . ? C1 C6 1.380(3) . . ? C2 C3 1.371(4) . . ? C3 C4 1.370(4) . . ? C4 C5 1.367(4) . . ? C5 C6 1.387(4) . . ? O1 C7 1.448(3) . . ? C7 C8 1.517(4) . . ? C7 C9 1.528(4) . . ? C7 C10 1.515(4) . . ? C10 N1 1.269(3) . . ? C10 O2 1.350(3) . . ? N1 C11 1.512(3) . . ? C11 C12 1.526(4) . . ? C11 C13 1.506(5) . . ? C11 C14 1.507(5) . . ? C12 O2 1.444(4) . . ? O3 C15 1.458(3) . . ? C15 C16 1.499(4) . . ? C15 C17 1.519(4) . . ? C15 C18 1.527(4) . . ? C18 N2 1.259(3) . . ? C18 O4 1.348(3) . . ? N2 C19 1.511(3) . . ? C19 C20 1.523(4) . . ? C19 C21 1.526(5) . . ? C19 C22 1.502(5) . . ? C20 O4 1.454(4) . . ? 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 CL1 NI CL2 142.87(3) . . . ? CL1 NI P 108.43(3) . . . ? CL1 NI N1 96.11(6) . . . ? CL1 NI N2 93.74(6) . . . ? CL2 NI P 108.60(3) . . . ? CL2 NI N1 87.38(6) . . . ? CL2 NI N2 89.31(6) . . . ? P NI N1 80.48(6) . . . ? P NI N2 89.28(6) . . . ? N1 NI N2 167.60(8) . . . ? C1 P O1 103.9(1) . . . ? C1 P O3 98.7(1) . . . ? O1 P O3 101.02(9) . . . ? P C1 C2 120.5(2) . . . ? P C1 C6 120.7(2) . . . ? C2 C1 C6 118.8(2) . . . ? C1 C2 C3 120.4(2) . . . ? C2 C3 C4 120.4(3) . . . ? C3 C4 C5 119.8(3) . . . ? C4 C5 C6 120.7(2) . . . ? C1 C6 C5 119.8(2) . . . ? P O1 C7 127.5(1) . . . ? O1 C7 C8 105.4(2) . . . ? O1 C7 C9 107.7(2) . . . ? O1 C7 C10 113.7(2) . . . ? C8 C7 C9 111.7(2) . . . ? C8 C7 C10 109.2(3) . . . ? C9 C7 C10 109.2(2) . . . ? C7 C10 N1 130.9(2) . . . ? C7 C10 O2 111.3(2) . . . ? N1 C10 O2 117.7(2) . . . ? C10 N1 C11 107.0(2) . . . ? N1 C11 C12 101.5(2) . . . ? N1 C11 C13 108.6(2) . . . ? N1 C11 C14 110.3(2) . . . ? C12 C11 C13 111.3(3) . . . ? C12 C11 C14 112.3(3) . . . ? C13 C11 C14 112.3(3) . . . ? C11 C12 O2 104.9(2) . . . ? C10 O2 C12 105.7(2) . . . ? P O3 C15 126.3(2) . . . ? O3 C15 C16 110.3(2) . . . ? O3 C15 C17 103.2(2) . . . ? O3 C15 C18 111.3(2) . . . ? C16 C15 C17 112.6(2) . . . ? C16 C15 C18 109.9(2) . . . ? C17 C15 C18 109.3(2) . . . ? C15 C18 N2 130.7(2) . . . ? C15 C18 O4 111.3(2) . . . ? N2 C18 O4 117.9(2) . . . ? C18 N2 C19 106.7(2) . . . ? N2 C19 C20 100.9(2) . . . ? N2 C19 C21 107.9(3) . . . ? N2 C19 C22 112.4(3) . . . ? C20 C19 C21 111.8(3) . . . ? C20 C19 C22 111.8(3) . . . ? C21 C19 C22 111.5(3) . . . ? C19 C20 O4 103.8(3) . . . ? C18 O4 C20 104.9(2) . . . ? data_st805 _database_code_depnum_ccdc_archive 'CCDC 224562' _audit_creation_date 10-11-03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl4 Fe2 N2 O4' _chemical_formula_sum 'C16 H28 Cl4 Fe2 N2 O4' _chemical_formula_weight 565.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5227(3) _cell_length_b 9.4272(2) _cell_length_c 20.3311(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2400.17(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2970 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2752 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2752 _reflns_number_gt 2152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.7409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2752 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.50699(3) 0.48545(4) -0.078707(15) 0.02236(13) Uani 1 1 d . . . Cl1 Cl 0.38658(5) 0.61707(7) -0.12933(3) 0.03381(18) Uani 1 1 d . . . Cl2 Cl 0.65568(5) 0.49611(7) -0.13861(3) 0.03507(18) Uani 1 1 d . . . O1 O 0.62729(14) 0.91417(19) 0.08594(7) 0.0301(4) Uani 1 1 d . . . O2 O 0.55474(13) 0.60292(17) -0.00309(7) 0.0243(4) Uani 1 1 d . . . N N 0.53674(17) 0.7166(2) 0.11050(9) 0.0255(5) Uani 1 1 d . . . C6 C 0.6031(2) 0.9289(3) 0.15624(12) 0.0369(7) Uani 1 1 d . . . H6A H 0.5676 1.0184 0.1649 0.044 Uiso 1 1 calc . . . H6B H 0.6679 0.9243 0.1822 0.044 Uiso 1 1 calc . . . C7 C 0.4136(2) 0.8524(3) 0.18212(14) 0.0428(7) Uani 1 1 d . . . H7A H 0.3916 0.9070 0.1446 0.064 Uiso 1 1 calc . . . H7B H 0.4090 0.9099 0.2210 0.064 Uiso 1 1 calc . . . H7C H 0.3679 0.7713 0.1868 0.064 Uiso 1 1 calc . . . C3 C 0.5801(2) 0.8382(3) -0.05085(12) 0.0336(6) Uani 1 1 d . . . H3A H 0.5965 0.8017 -0.0938 0.050 Uiso 1 1 calc . . . H3B H 0.6173 0.9261 -0.0442 0.050 Uiso 1 1 calc . . . H3C H 0.5046 0.8540 -0.0474 0.050 Uiso 1 1 calc . . . C4 C 0.59027(19) 0.7879(3) 0.06848(11) 0.0249(5) Uani 1 1 d . . . C1 C 0.61491(19) 0.7318(3) 0.00104(10) 0.0248(5) Uani 1 1 d . . . C5 C 0.5287(2) 0.8031(3) 0.17257(12) 0.0311(6) Uani 1 1 d . . . C2 C 0.7347(2) 0.7009(3) -0.00258(11) 0.0338(6) Uani 1 1 d . . . H2A H 0.7521 0.6645 -0.0454 0.051 Uiso 1 1 calc . . . H2B H 0.7533 0.6320 0.0302 0.051 Uiso 1 1 calc . . . H2C H 0.7740 0.7868 0.0051 0.051 Uiso 1 1 calc . . . C8 C 0.5672(3) 0.7170(3) 0.23019(14) 0.0524(9) Uani 1 1 d . . . H8A H 0.6395 0.6874 0.2226 0.079 Uiso 1 1 calc . . . H8B H 0.5225 0.6350 0.2354 0.079 Uiso 1 1 calc . . . H8C H 0.5642 0.7737 0.2694 0.079 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0298(2) 0.0214(2) 0.01591(19) 0.00015(13) 0.00167(13) -0.00233(14) Cl1 0.0361(4) 0.0367(4) 0.0287(3) 0.0015(3) -0.0033(3) 0.0051(3) Cl2 0.0344(4) 0.0379(4) 0.0330(3) -0.0074(3) 0.0101(3) -0.0061(3) O1 0.0414(10) 0.0216(10) 0.0274(9) -0.0045(7) 0.0036(7) -0.0062(8) O2 0.0336(10) 0.0212(9) 0.0181(8) -0.0003(6) 0.0011(7) -0.0076(8) N 0.0348(12) 0.0224(12) 0.0191(10) -0.0051(8) 0.0021(9) -0.0033(9) C6 0.0445(16) 0.0362(17) 0.0301(13) -0.0144(12) 0.0056(12) -0.0043(13) C7 0.0463(17) 0.0374(18) 0.0447(16) -0.0119(14) 0.0121(14) -0.0044(14) C3 0.0467(16) 0.0257(15) 0.0283(13) 0.0058(11) -0.0013(12) -0.0048(12) C4 0.0275(13) 0.0218(14) 0.0254(12) 0.0011(10) -0.0038(10) 0.0005(10) C1 0.0329(14) 0.0205(13) 0.0209(12) -0.0016(10) 0.0022(10) -0.0046(11) C5 0.0461(16) 0.0241(14) 0.0232(12) -0.0043(10) 0.0031(11) -0.0012(12) C2 0.0315(15) 0.0369(16) 0.0330(14) -0.0082(11) 0.0046(11) -0.0041(12) C8 0.086(3) 0.0406(19) 0.0311(15) -0.0037(13) -0.0119(16) 0.0057(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2 1.9869(15) . ? Fe O2 2.0142(15) 5_665 ? Fe N 2.085(2) 5_665 ? Fe Cl1 2.2074(7) . ? Fe Cl2 2.2273(7) . ? O1 C4 1.326(3) . ? O1 C6 1.468(3) . ? O2 C1 1.432(3) . ? O2 Fe 2.0141(15) 5_665 ? N C4 1.277(3) . ? N C5 1.505(3) . ? N Fe 2.085(2) 5_665 ? C6 C5 1.544(4) . ? C7 C5 1.527(4) . ? C3 C1 1.519(3) . ? C4 C1 1.501(3) . ? C1 C2 1.530(4) . ? C5 C8 1.504(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe O2 72.97(7) . 5_665 ? O2 Fe N 145.92(7) . 5_665 ? O2 Fe N 77.13(7) 5_665 5_665 ? O2 Fe Cl1 104.66(5) . . ? O2 Fe Cl1 110.81(5) 5_665 . ? N Fe Cl1 100.94(6) 5_665 . ? O2 Fe Cl2 98.42(5) . . ? O2 Fe Cl2 142.28(5) 5_665 . ? N Fe Cl2 95.24(6) 5_665 . ? Cl1 Fe Cl2 106.90(3) . . ? C4 O1 C6 105.86(19) . . ? C1 O2 Fe 132.58(12) . . ? C1 O2 Fe 120.29(12) . 5_665 ? Fe O2 Fe 107.03(7) . 5_665 ? C4 N C5 108.1(2) . . ? C4 N Fe 114.26(16) . 5_665 ? C5 N Fe 137.47(16) . 5_665 ? O1 C6 C5 105.15(19) . . ? N C4 O1 118.5(2) . . ? N C4 C1 122.3(2) . . ? O1 C4 C1 119.2(2) . . ? O2 C1 C4 104.12(18) . . ? O2 C1 C3 111.62(19) . . ? C4 C1 C3 110.1(2) . . ? O2 C1 C2 110.6(2) . . ? C4 C1 C2 108.21(19) . . ? C3 C1 C2 111.9(2) . . ? C8 C5 N 109.9(2) . . ? C8 C5 C7 111.6(2) . . ? N C5 C7 109.5(2) . . ? C8 C5 C6 112.9(2) . . ? N C5 C6 101.27(19) . . ? C7 C5 C6 111.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe O2 C1 -176.2(2) 5_665 . . . ? N Fe O2 C1 154.09(19) 5_665 . . . ? Cl1 Fe O2 C1 -68.5(2) . . . . ? Cl2 Fe O2 C1 41.6(2) . . . . ? O2 Fe O2 Fe 0.0 5_665 . . 5_665 ? N Fe O2 Fe -29.74(17) 5_665 . . 5_665 ? Cl1 Fe O2 Fe 107.70(7) . . . 5_665 ? Cl2 Fe O2 Fe -142.28(7) . . . 5_665 ? C4 O1 C6 C5 -10.0(3) . . . . ? C5 N C4 O1 0.7(3) . . . . ? Fe N C4 O1 -175.84(16) 5_665 . . . ? C5 N C4 C1 179.1(2) . . . . ? Fe N C4 C1 2.5(3) 5_665 . . . ? C6 O1 C4 N 6.2(3) . . . . ? C6 O1 C4 C1 -172.2(2) . . . . ? Fe O2 C1 C4 161.16(15) . . . . ? Fe O2 C1 C4 -14.6(2) 5_665 . . . ? Fe O2 C1 C3 42.5(3) . . . . ? Fe O2 C1 C3 -133.30(17) 5_665 . . . ? Fe O2 C1 C2 -82.8(2) . . . . ? Fe O2 C1 C2 101.42(18) 5_665 . . . ? N C4 C1 O2 7.3(3) . . . . ? O1 C4 C1 O2 -174.4(2) . . . . ? N C4 C1 C3 127.0(3) . . . . ? O1 C4 C1 C3 -54.7(3) . . . . ? N C4 C1 C2 -110.4(3) . . . . ? O1 C4 C1 C2 67.9(3) . . . . ? C4 N C5 C8 -126.4(3) . . . . ? Fe N C5 C8 49.0(3) 5_665 . . . ? C4 N C5 C7 110.7(2) . . . . ? Fe N C5 C7 -73.9(3) 5_665 . . . ? C4 N C5 C6 -6.9(3) . . . . ? Fe N C5 C6 168.5(2) 5_665 . . . ? O1 C6 C5 C8 127.4(2) . . . . ? O1 C6 C5 N 10.0(3) . . . . ? O1 C6 C5 C7 -106.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.447 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.073