# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_las _database_code_CSD 188251 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Veciana, Jaume' ; Institut de Ciencia de Materials de Barcelona (CSIC) Campus de la UAB E-08193 Bellaterra Spain ; 'Sporer, Christian' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Ruiz-Molina, Daniel' ; Institut de Ciencia de Materials de Barcelona (CSIC) Campus de la UAB E-08193 Bellaterra Spain ; 'Amabilino, David B.' ; Institut de Ciencia de Materials de Barcelona (CSIC) Campus de la UAB E-08193 Bellaterra Spain ; 'Wurst, Klaus' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Jaitner, Peter' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Kopacka, Holger' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; _publ_contact_author_name 'Prof J Veciana' _publ_contact_author_address ; Institut de Ciencia de Materials de Barcelona (CSIC) Campus Universitari de Bellaterra Cerdanyola 08193 SPAIN ; _publ_contact_author_phone '0034 935 801853' _publ_contact_author_fax ? _publ_contact_author_email vecianaj@icmab.es _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Spontaneous Resolution of a Mn(II) Polymeric Chain Incorporating Ferrocene-Based a-Nitronyl Nitroxide Radicals ; #============================================================================ _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H36 Cl2 F12 Fe Mn N4 O8' _chemical_formula_weight 1050.37 _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' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8382(4) _cell_length_b 19.9028(6) _cell_length_c 20.5120(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4424.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 11576 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method ? _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Kappa CCD' _diffrn_measurement_method 'phi and omega-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5752 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 22.48 _reflns_number_total 5752 _reflns_number_observed 5324 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement ? _computing_data_reduction 'Denzo and scalepak' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 2:1 disordering of three from four CF3-groups and 2:1 disordering of the solvent CH2Cl2 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+2.3254P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(15) _refine_ls_number_reflns 5647 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_obs 0.0318 _refine_ls_wR_factor_all 0.0766 _refine_ls_wR_factor_obs 0.0725 _refine_ls_goodness_of_fit_all 1.075 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group F1 F 0.4076(4) 0.2353(3) 0.1384(2) 0.184(3) Uani 1 d . . F2 F 0.3934(3) 0.3066(2) 0.2157(2) 0.1268(14) Uani 1 d . . F3 F 0.4823(4) 0.2165(2) 0.2293(2) 0.1206(13) Uani 1 d . . F4 F 0.8978(12) 0.2777(8) 0.0081(5) 0.140(7) Uani 0.67 d P . F5 F 0.7808(16) 0.3572(4) -0.0215(4) 0.130(5) Uani 0.67 d P . F6 F 0.7096(9) 0.2619(7) -0.0221(4) 0.105(3) Uani 0.67 d P . F7 F 0.4445(10) 0.4685(5) 0.3309(6) 0.134(6) Uani 0.67 d P . F8 F 0.4411(12) 0.5706(6) 0.3001(5) 0.136(5) Uani 0.67 d P . F9 F 0.5751(11) 0.5337(5) 0.3620(5) 0.086(4) Uani 0.67 d P . F10 F 0.6200(21) 0.5094(5) 0.0278(4) 0.136(4) Uani 0.67 d P . F11 F 0.5292(13) 0.5845(8) 0.0748(5) 0.138(6) Uani 0.67 d P . F12 F 0.7267(12) 0.5870(7) 0.0632(5) 0.122(5) Uani 0.67 d P . F4A F 0.8904(13) 0.3113(13) -0.0028(8) 0.085(7) Uani 0.33 d P . F6A F 0.7829(26) 0.2272(7) 0.0037(8) 0.119(5) Uani 0.33 d P . F5A F 0.7154(24) 0.3188(21) -0.0286(6) 0.149(10) Uani 0.33 d P . F7A F 0.3950(13) 0.5287(12) 0.2879(8) 0.107(6) Uani 0.33 d P . F8A F 0.5476(28) 0.5627(14) 0.3467(15) 0.164(16) Uani 0.33 d P . F9A F 0.4835(21) 0.4647(11) 0.3458(10) 0.132(13) Uani 0.33 d P . F10A F 0.5244(23) 0.5305(34) 0.0510(11) 0.225(19) Uani 0.33 d P . F11A F 0.6146(35) 0.6177(7) 0.0929(8) 0.134(7) Uani 0.33 d P . F12A F 0.7077(25) 0.5454(24) 0.0366(10) 0.150(13) Uani 0.33 d P . Fe1 Fe 1.01064(5) 0.14964(3) 0.23146(2) 0.04020(15) Uani 1 d . . Mn1 Mn 0.79417(5) 0.39614(2) 0.20835(2) 0.03104(14) Uani 1 d . . O1 O 0.8728(2) 0.34471(12) 0.29050(11) 0.0379(6) Uani 1 d . . O2 O 0.7017(3) 0.13830(12) 0.34253(12) 0.0509(7) Uani 1 d . . O3 O 1.0211(2) -0.06312(11) 0.28994(11) 0.0363(5) Uani 1 d . . O4 O 0.9583(3) 0.12098(13) 0.42385(13) 0.0560(8) Uani 1 d . . N1 N 0.8163(3) 0.29629(13) 0.32293(13) 0.0317(7) Uani 1 d . . N2 N 0.7338(3) 0.19969(14) 0.34657(13) 0.0373(7) Uani 1 d . . N3 N 0.9783(3) -0.02353(14) 0.33581(12) 0.0343(7) Uani 1 d . . N4 N 0.9528(3) 0.06202(15) 0.40023(14) 0.0406(8) Uani 1 d . . O5 O 0.6397(2) 0.32733(13) 0.21106(12) 0.0440(6) Uani 1 d . . O6 O 0.8206(2) 0.34477(13) 0.11462(11) 0.0423(6) Uani 1 d . . O7 O 0.6755(2) 0.45600(12) 0.26960(11) 0.0394(6) Uani 1 d . . O8 O 0.7396(2) 0.47272(13) 0.13915(12) 0.0434(6) Uani 1 d . . C1 C 0.8529(3) 0.2058(2) 0.2425(2) 0.0360(9) Uani 1 d . . C2 C 0.8240(4) 0.1406(2) 0.2157(2) 0.0449(9) Uani 1 d . . H2 H 0.7722 0.1079 0.2342 0.054 Uiso 1 calc . . C3 C 0.8887(5) 0.1354(2) 0.1560(2) 0.0605(12) Uani 1 d . . H3 H 0.8858 0.0984 0.1276 0.073 Uiso 1 calc . . C4 C 0.9580(5) 0.1942(2) 0.1457(2) 0.0642(14) Uani 1 d . . H4 H 1.0092 0.2030 0.1097 0.077 Uiso 1 calc . . C5 C 0.9372(4) 0.2375(2) 0.1988(2) 0.0481(10) Uani 1 d . . H5 H 0.9729 0.2801 0.2045 0.058 Uiso 1 calc . . C6 C 1.0754(3) 0.0831(2) 0.3001(2) 0.0376(9) Uani 1 d . . C7 C 1.1178(4) 0.0659(2) 0.2359(2) 0.0468(10) Uani 1 d . . H7 H 1.1020 0.0256 0.2136 0.056 Uiso 1 calc . . C8 C 1.1880(4) 0.1210(2) 0.2123(2) 0.0606(12) Uani 1 d . . H8 H 1.2282 0.1230 0.1718 0.073 Uiso 1 calc . . C9 C 1.1872(4) 0.1719(2) 0.2596(2) 0.0615(12) Uani 1 d . . H9 H 1.2266 0.2138 0.2556 0.074 Uiso 1 calc . . C10 C 1.1184(3) 0.1504(2) 0.3138(2) 0.0477(10) Uani 1 d . . H10 H 1.1032 0.1753 0.3520 0.057 Uiso 1 calc . . C11 C 0.8039(3) 0.2332(2) 0.3021(2) 0.0326(8) Uani 1 d . . C12 C 0.7776(4) 0.3051(2) 0.3924(2) 0.0376(9) Uani 1 d . . C13 C 0.6844(4) 0.2457(2) 0.3982(2) 0.0387(9) Uani 1 d . . C14 C 1.0038(3) 0.0415(2) 0.34300(15) 0.0340(8) Uani 1 d . . C15 C 0.8767(3) -0.0456(2) 0.3809(2) 0.0411(9) Uani 1 d . . C16 C 0.9005(4) 0.0043(2) 0.4374(2) 0.0440(9) Uani 1 d . . C17 C 0.5882(4) 0.2969(2) 0.1654(2) 0.0471(10) Uani 1 d . . C18 C 0.6305(4) 0.2878(2) 0.1030(2) 0.0599(13) Uani 1 d . . H18 H 0.5812 0.2640 0.0731 0.072 Uiso 1 calc . . C19 C 0.7450(4) 0.3127(2) 0.0826(2) 0.0454(10) Uani 1 d . . C20 C 0.5945(3) 0.4972(2) 0.2544(2) 0.0392(9) Uani 1 d . . C21 C 0.5749(4) 0.5278(2) 0.1938(2) 0.0488(10) Uani 1 d . . H21 H 0.5100 0.5587 0.1885 0.059 Uiso 1 calc . . C22 C 0.6511(4) 0.5125(2) 0.1414(2) 0.0440(10) Uani 1 d . . C121 C 0.8937(4) 0.2947(2) 0.4336(2) 0.0503(10) Uani 1 d . . H12A H 0.8734(7) 0.2999(13) 0.4794(2) 0.075 Uiso 1 calc R . H12B H 0.9553(10) 0.3278(9) 0.4215(9) 0.075 Uiso 1 calc R . H12C H 0.9261(15) 0.2499(5) 0.4260(10) 0.075 Uiso 1 calc R . C122 C 0.7223(4) 0.3738(2) 0.4036(2) 0.0542(11) Uani 1 d . . H12D H 0.7847(8) 0.4079(2) 0.3961(13) 0.081 Uiso 1 calc R . H12E H 0.6929(23) 0.3770(5) 0.4482(5) 0.081 Uiso 1 calc R . H12F H 0.6540(17) 0.3806(6) 0.3738(9) 0.081 Uiso 1 calc R . C131 C 0.6843(4) 0.2104(2) 0.4640(2) 0.0542(11) Uani 1 d . . H13A H 0.6227(19) 0.1751(10) 0.4640(5) 0.081 Uiso 1 calc R . H13B H 0.6652(27) 0.2427(4) 0.4980(2) 0.081 Uiso 1 calc R . H13C H 0.7650(9) 0.1911(13) 0.4721(7) 0.081 Uiso 1 calc R . C132 C 0.5539(4) 0.2645(2) 0.3783(2) 0.0576(11) Uani 1 d . . H13D H 0.5162(10) 0.2913(12) 0.4124(6) 0.086 Uiso 1 calc R . H13E H 0.5058(8) 0.2240(2) 0.3715(13) 0.086 Uiso 1 calc R . H13F H 0.5563(4) 0.2903(12) 0.3382(8) 0.086 Uiso 1 calc R . C151 C 0.7549(4) -0.0324(2) 0.3451(2) 0.0572(11) Uani 1 d . . H15A H 0.6863(4) -0.0457(13) 0.3726(6) 0.086 Uiso 1 calc R . H15B H 0.7531(12) -0.0583(11) 0.3050(7) 0.086 Uiso 1 calc R . H15C H 0.7483(13) 0.0150(3) 0.3349(12) 0.086 Uiso 1 calc R . C152 C 0.8882(4) -0.1195(2) 0.3984(2) 0.0550(11) Uani 1 d . . H15D H 0.8284(18) -0.1307(4) 0.4319(10) 0.083 Uiso 1 calc R . H15E H 0.9707(9) -0.1284(3) 0.4145(13) 0.083 Uiso 1 calc R . H15F H 0.8729(25) -0.1467(2) 0.3600(4) 0.083 Uiso 1 calc R . C161 C 0.7852(5) 0.0261(2) 0.4742(2) 0.0686(14) Uani 1 d . . H16A H 0.7438(17) -0.0131(3) 0.4918(14) 0.103 Uiso 1 calc R . H16B H 0.7300(14) 0.0496(14) 0.4447(4) 0.103 Uiso 1 calc R . H16C H 0.8083(6) 0.0559(13) 0.5097(10) 0.103 Uiso 1 calc R . C162 C 1.0025(5) -0.0192(2) 0.4839(2) 0.0647(12) Uani 1 d . . H16D H 0.9735(12) -0.0576(10) 0.5087(11) 0.097 Uiso 1 calc R . H16E H 1.0236(21) 0.0170(6) 0.5136(10) 0.097 Uiso 1 calc R . H16F H 1.0748(12) -0.0318(16) 0.4589(2) 0.097 Uiso 1 calc R . C171 C 0.4642(5) 0.2639(3) 0.1834(2) 0.078(2) Uani 1 d . . C191 C 0.7832(6) 0.2989(3) 0.0111(2) 0.0694(14) Uani 1 d . . C201 C 0.5089(5) 0.5168(3) 0.3111(2) 0.0608(12) Uani 1 d . . C221 C 0.6269(6) 0.5491(3) 0.0771(3) 0.073(2) Uani 1 d . . C23 C 0.3594(13) 0.5914(9) -0.1644(6) 0.074(4) Uani 0.67 d P 1 H23A H 0.4231 0.6068 -0.1948 0.089 Uiso 0.67 calc P 1 H23B H 0.3050 0.5606 -0.1881 0.089 Uiso 0.67 calc P 1 Cl1 Cl 0.2726(9) 0.6610(7) -0.1383(5) 0.150(4) Uani 0.67 d P 1 Cl2 Cl 0.4321(3) 0.5463(2) -0.09869(14) 0.0799(9) Uani 0.67 d P 1 C23A C 0.3302(32) 0.6205(20) -0.1789(18) 0.080(9) Uani 0.33 d P 2 H23C H 0.4009 0.6421 -0.2001 0.096 Uiso 0.33 calc P 2 H23D H 0.2718 0.6061 -0.2126 0.096 Uiso 0.33 calc P 2 Cl2A Cl 0.3795(8) 0.5506(4) -0.1314(5) 0.115(3) Uani 0.33 d P 2 Cl1A Cl 0.2677(9) 0.6695(9) -0.1311(5) 0.083(3) Uani 0.33 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.119(3) 0.357(7) 0.074(2) -0.040(3) 0.008(2) -0.165(4) F2 0.056(2) 0.156(3) 0.168(4) -0.009(3) 0.032(2) -0.026(2) F3 0.119(3) 0.130(3) 0.113(3) 0.028(2) 0.009(2) -0.066(2) F4 0.129(10) 0.229(15) 0.064(4) -0.023(6) 0.010(4) 0.093(10) F5 0.249(16) 0.105(5) 0.037(4) 0.001(3) 0.017(5) -0.045(7) F6 0.113(6) 0.142(8) 0.061(4) -0.058(5) 0.015(4) -0.055(7) F7 0.087(6) 0.125(9) 0.190(10) -0.045(7) 0.083(6) -0.058(7) F8 0.169(11) 0.164(9) 0.076(5) 0.013(6) 0.025(6) 0.131(8) F9 0.087(4) 0.123(10) 0.048(3) -0.011(5) 0.015(3) 0.015(7) F10 0.207(11) 0.147(6) 0.055(4) -0.005(4) -0.061(8) 0.050(8) F11 0.122(9) 0.222(12) 0.069(6) 0.065(6) 0.009(6) 0.120(10) F12 0.153(10) 0.148(7) 0.066(5) 0.063(5) -0.012(5) -0.047(8) F4A 0.037(8) 0.170(18) 0.049(8) -0.054(10) 0.027(6) -0.055(10) F6A 0.181(17) 0.086(9) 0.090(9) -0.054(7) 0.039(10) -0.030(11) F5A 0.158(20) 0.261(31) 0.028(6) -0.033(16) -0.033(10) 0.076(22) F7A 0.055(7) 0.192(19) 0.073(8) 0.005(11) 0.023(6) 0.086(10) F8A 0.211(37) 0.113(18) 0.168(28) -0.102(17) 0.138(23) -0.094(19) F9A 0.122(17) 0.153(20) 0.120(11) 0.111(14) 0.106(11) 0.108(17) F10A 0.082(14) 0.522(60) 0.070(13) 0.075(21) -0.043(11) -0.021(25) F11A 0.194(19) 0.097(11) 0.111(12) 0.061(8) -0.016(16) 0.043(12) F12A 0.094(13) 0.305(36) 0.052(12) 0.082(15) 0.035(10) 0.128(19) Fe1 0.0411(3) 0.0370(3) 0.0426(3) 0.0090(2) 0.0133(2) 0.0072(3) Mn1 0.0315(3) 0.0309(3) 0.0307(3) 0.0015(2) -0.0010(2) -0.0010(2) O1 0.0373(13) 0.0361(13) 0.0403(13) 0.0082(12) -0.0036(11) -0.0054(11) O2 0.060(2) 0.036(2) 0.056(2) 0.0034(11) 0.0081(13) -0.0101(14) O3 0.0350(13) 0.0391(13) 0.0346(12) -0.0053(11) 0.0024(11) 0.0054(11) O4 0.067(2) 0.040(2) 0.061(2) -0.0110(13) 0.0164(14) 0.0011(14) N1 0.033(2) 0.030(2) 0.0324(15) 0.0081(13) -0.0011(13) -0.0006(14) N2 0.040(2) 0.034(2) 0.038(2) 0.0046(13) 0.0031(14) -0.0039(15) N3 0.032(2) 0.035(2) 0.037(2) 0.0022(12) 0.0027(13) 0.0058(14) N4 0.046(2) 0.036(2) 0.040(2) -0.0008(14) 0.0080(14) 0.0057(15) O5 0.0398(15) 0.054(2) 0.0379(14) -0.0034(12) 0.0007(12) -0.0151(12) O6 0.0383(15) 0.050(2) 0.0382(13) -0.0094(12) 0.0000(11) -0.0066(14) O7 0.0394(15) 0.0395(14) 0.0393(13) 0.0035(11) 0.0001(11) 0.0086(13) O8 0.044(2) 0.0460(15) 0.0406(14) 0.0069(11) 0.0014(12) 0.0071(14) C1 0.039(2) 0.033(2) 0.036(2) 0.003(2) 0.002(2) 0.007(2) C2 0.048(2) 0.043(2) 0.043(2) -0.005(2) -0.003(2) 0.008(2) C3 0.082(3) 0.055(3) 0.044(2) -0.008(2) 0.000(2) 0.024(3) C4 0.088(4) 0.064(3) 0.041(2) 0.017(2) 0.024(2) 0.032(3) C5 0.052(3) 0.046(2) 0.046(2) 0.016(2) 0.016(2) 0.014(2) C6 0.031(2) 0.038(2) 0.044(2) 0.008(2) 0.005(2) 0.004(2) C7 0.041(2) 0.046(2) 0.053(2) 0.011(2) 0.013(2) 0.015(2) C8 0.045(2) 0.059(3) 0.078(3) 0.025(2) 0.031(2) 0.012(2) C9 0.038(2) 0.052(3) 0.095(3) 0.014(2) 0.015(2) -0.004(2) C10 0.033(2) 0.046(2) 0.064(3) 0.008(2) 0.003(2) -0.003(2) C11 0.031(2) 0.032(2) 0.035(2) 0.0070(15) -0.001(2) -0.001(2) C12 0.044(2) 0.039(2) 0.030(2) 0.0009(15) -0.002(2) 0.004(2) C13 0.040(2) 0.040(2) 0.036(2) 0.004(2) 0.007(2) 0.006(2) C14 0.032(2) 0.033(2) 0.037(2) 0.0024(14) 0.003(2) 0.008(2) C15 0.040(2) 0.038(2) 0.045(2) 0.008(2) 0.013(2) 0.002(2) C16 0.054(3) 0.038(2) 0.040(2) 0.003(2) 0.012(2) 0.003(2) C17 0.036(2) 0.062(3) 0.043(2) -0.001(2) -0.002(2) -0.018(2) C18 0.051(3) 0.085(3) 0.043(2) -0.014(2) -0.005(2) -0.026(3) C19 0.047(3) 0.054(2) 0.035(2) -0.004(2) -0.001(2) -0.002(2) C20 0.028(2) 0.043(2) 0.046(2) 0.000(2) 0.002(2) 0.002(2) C21 0.039(2) 0.054(3) 0.053(3) 0.012(2) 0.002(2) 0.013(2) C22 0.037(2) 0.050(2) 0.045(2) 0.011(2) -0.004(2) 0.000(2) C121 0.056(3) 0.051(2) 0.043(2) 0.002(2) -0.007(2) -0.005(2) C122 0.070(3) 0.046(2) 0.047(2) -0.004(2) 0.003(2) 0.015(2) C131 0.063(3) 0.057(3) 0.042(2) 0.009(2) 0.015(2) -0.003(2) C132 0.040(3) 0.071(3) 0.061(3) 0.002(2) 0.007(2) 0.007(2) C151 0.036(2) 0.064(3) 0.072(3) 0.004(2) 0.001(2) -0.003(2) C152 0.056(3) 0.040(2) 0.069(3) 0.010(2) 0.021(2) 0.001(2) C161 0.076(3) 0.065(3) 0.065(3) 0.004(2) 0.040(3) 0.003(3) C162 0.089(4) 0.067(3) 0.038(2) 0.009(2) -0.008(3) -0.001(3) C171 0.061(3) 0.126(5) 0.048(3) -0.021(3) 0.005(3) -0.037(3) C191 0.079(5) 0.084(4) 0.046(3) -0.021(3) -0.004(3) -0.009(4) C201 0.054(3) 0.071(3) 0.058(3) 0.007(3) 0.009(3) 0.022(3) C221 0.073(4) 0.083(4) 0.064(4) 0.029(3) 0.010(3) 0.029(4) C23 0.063(9) 0.117(16) 0.043(8) -0.011(7) 0.013(6) -0.010(9) Cl1 0.136(6) 0.178(7) 0.135(7) 0.012(6) -0.011(5) 0.018(5) Cl2 0.087(2) 0.069(2) 0.084(2) -0.0014(14) 0.0181(13) -0.022(2) C23A 0.068(17) 0.112(26) 0.061(17) 0.011(14) -0.013(11) 0.013(15) Cl2A 0.108(6) 0.081(4) 0.155(9) 0.020(6) 0.045(5) 0.015(5) Cl1A 0.052(4) 0.155(9) 0.044(4) -0.015(4) 0.001(3) 0.000(5) _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 F1 C171 1.246(5) . ? F2 C171 1.323(6) . ? F3 C171 1.347(6) . ? F4 F4A 0.71(3) . ? F4 C191 1.313(12) . ? F4 F6A 1.60(2) . ? F5 F5A 1.05(4) . ? F5 C191 1.339(10) . ? F5 F4A 1.55(2) . ? F6 F5A 1.14(3) . ? F6 F6A 1.18(2) . ? F6 C191 1.282(8) . ? F7 F9A 0.53(3) . ? F7 C201 1.257(9) . ? F7 F7A 1.58(2) . ? F8 F7A 1.00(2) . ? F8 C201 1.317(9) . ? F8 F8A 1.51(3) . ? F9 F8A 0.72(3) . ? F9 C201 1.311(11) . ? F9 F9A 1.73(3) . ? F10 F12A 1.20(4) . ? F10 F10A 1.21(3) . ? F10 C221 1.286(9) . ? F11 F10A 1.18(5) . ? F11 F11A 1.20(2) . ? F11 C221 1.272(10) . ? F12 F12A 1.01(4) . ? F12 C221 1.349(10) . ? F12 F11A 1.49(2) . ? F4A C191 1.222(13) . ? F6A C191 1.435(14) . ? F5A C191 1.167(15) . ? F7A C201 1.34(2) . ? F8A C201 1.24(2) . ? F9A C201 1.29(2) . ? F10A C221 1.29(2) . ? F11A C221 1.41(2) . ? F12A C221 1.209(13) . ? Fe1 C7 2.033(4) . ? Fe1 C5 2.034(4) . ? Fe1 C8 2.043(4) . ? Fe1 C9 2.047(5) . ? Fe1 C4 2.051(4) . ? Fe1 C10 2.054(4) . ? Fe1 C1 2.055(3) . ? Fe1 C3 2.055(5) . ? Fe1 C6 2.056(3) . ? Fe1 C2 2.057(4) . ? Mn1 O1 2.148(2) . ? Mn1 O7 2.157(2) . ? Mn1 O3 2.161(2) 3_755 ? Mn1 O5 2.164(2) . ? Mn1 O8 2.165(2) . ? Mn1 O6 2.196(2) . ? O1 N1 1.321(3) . ? O2 N2 1.273(4) . ? O3 N3 1.312(3) . ? O3 Mn1 2.161(2) 3_745 ? O4 N4 1.271(4) . ? N1 C11 1.332(4) . ? N1 C12 1.496(4) . ? N2 C11 1.362(4) . ? N2 C13 1.498(4) . ? N3 C14 1.333(4) . ? N3 C15 1.504(4) . ? N4 C14 1.360(4) . ? N4 C16 1.491(5) . ? O5 C17 1.247(4) . ? O6 C19 1.229(4) . ? O7 C20 1.241(4) . ? O8 C22 1.244(4) . ? C1 C5 1.427(5) . ? C1 C11 1.441(5) . ? C1 C2 1.444(5) . ? C2 C3 1.415(6) . ? C3 C4 1.406(7) . ? C4 C5 1.408(6) . ? C6 C14 1.435(5) . ? C6 C7 1.437(5) . ? C6 C10 1.446(5) . ? C7 C8 1.418(6) . ? C8 C9 1.402(6) . ? C9 C10 1.406(6) . ? C12 C122 1.510(5) . ? C12 C121 1.530(5) . ? C12 C13 1.559(5) . ? C13 C132 1.520(6) . ? C13 C131 1.522(5) . ? C15 C152 1.519(5) . ? C15 C151 1.534(5) . ? C15 C16 1.549(5) . ? C16 C161 1.523(6) . ? C16 C162 1.533(6) . ? C17 C18 1.371(6) . ? C17 C171 1.541(6) . ? C18 C19 1.400(6) . ? C19 C191 1.549(6) . ? C20 C21 1.401(5) . ? C20 C201 1.538(5) . ? C21 C22 1.389(5) . ? C22 C221 1.529(6) . ? C23 Cl1 1.76(2) . ? C23 Cl2 1.80(2) . ? C23A Cl1A 1.54(5) . ? C23A Cl2A 1.78(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F4A F4 C191 66.8(16) . . ? F4A F4 F6A 119.1(20) . . ? C191 F4 F6A 58.0(8) . . ? F5A F5 C191 56.9(12) . . ? F5A F5 F4A 97.1(15) . . ? C191 F5 F4A 49.4(7) . . ? F5A F6 F6A 126.7(16) . . ? F5A F6 C191 57.2(9) . . ? F6A F6 C191 71.2(9) . . ? F9A F7 C201 81.3(26) . . ? F9A F7 F7A 134.6(31) . . ? C201 F7 F7A 55.1(8) . . ? F7A F8 C201 69.2(12) . . ? F7A F8 F8A 116.8(18) . . ? C201 F8 F8A 51.6(9) . . ? F8A F9 C201 68.4(24) . . ? F8A F9 F9A 108.3(29) . . ? C201 F9 F9A 47.8(7) . . ? F12A F10 F10A 114.2(22) . . ? F12A F10 C221 58.0(10) . . ? F10A F10 C221 61.9(16) . . ? F10A F11 F11A 131.7(19) . . ? F10A F11 C221 63.2(12) . . ? F11A F11 C221 69.5(11) . . ? F12A F12 C221 59.6(13) . . ? F12A F12 F11A 113.0(16) . . ? C221 F12 F11A 59.3(8) . . ? F4 F4A C191 81.0(17) . . ? F4 F4A F5 136.1(19) . . ? C191 F4A F5 56.4(9) . . ? F6 F6A C191 57.7(8) . . ? F6 F6A F4 100.5(11) . . ? C191 F6A F4 50.9(7) . . ? F5 F5A F6 137.8(21) . . ? F5 F5A C191 74.0(15) . . ? F6 F5A C191 67.4(15) . . ? F8 F7A C201 66.5(13) . . ? F8 F7A F7 108.9(17) . . ? C201 F7A F7 50.1(7) . . ? F9 F8A C201 79.0(24) . . ? F9 F8A F8 132.6(33) . . ? C201 F8A F8 56.3(12) . . ? F7 F9A C201 74.8(21) . . ? F7 F9A F9 117.5(31) . . ? C201 F9A F9 48.9(10) . . ? F11 F10A F10 116.1(29) . . ? F11 F10A C221 61.9(20) . . ? F10 F10A C221 61.8(11) . . ? F11 F11A C221 57.7(9) . . ? F11 F11A F12 106.0(15) . . ? C221 F11A F12 55.3(9) . . ? F12 F12A F10 136.7(16) . . ? F12 F12A C221 74.1(15) . . ? F10 F12A C221 64.4(13) . . ? C7 Fe1 C5 160.47(15) . . ? C7 Fe1 C8 40.7(2) . . ? C5 Fe1 C8 123.0(2) . . ? C7 Fe1 C9 68.3(2) . . ? C5 Fe1 C9 105.8(2) . . ? C8 Fe1 C9 40.1(2) . . ? C7 Fe1 C4 123.5(2) . . ? C5 Fe1 C4 40.3(2) . . ? C8 Fe1 C4 102.6(2) . . ? C9 Fe1 C4 114.1(2) . . ? C7 Fe1 C10 69.2(2) . . ? C5 Fe1 C10 119.1(2) . . ? C8 Fe1 C10 68.0(2) . . ? C9 Fe1 C10 40.1(2) . . ? C4 Fe1 C10 149.4(2) . . ? C7 Fe1 C1 156.38(15) . . ? C5 Fe1 C1 40.83(15) . . ? C8 Fe1 C1 162.9(2) . . ? C9 Fe1 C1 129.0(2) . . ? C4 Fe1 C1 68.2(2) . . ? C10 Fe1 C1 112.22(15) . . ? C7 Fe1 C3 106.8(2) . . ? C5 Fe1 C3 67.6(2) . . ? C8 Fe1 C3 114.9(2) . . ? C9 Fe1 C3 147.5(2) . . ? C4 Fe1 C3 40.0(2) . . ? C10 Fe1 C3 170.5(2) . . ? C1 Fe1 C3 67.8(2) . . ? C7 Fe1 C6 41.15(15) . . ? C5 Fe1 C6 155.8(2) . . ? C8 Fe1 C6 68.3(2) . . ? C9 Fe1 C6 68.1(2) . . ? C4 Fe1 C6 163.9(2) . . ? C10 Fe1 C6 41.2(2) . . ? C1 Fe1 C6 123.95(13) . . ? C3 Fe1 C6 130.3(2) . . ? C7 Fe1 C2 119.8(2) . . ? C5 Fe1 C2 68.8(2) . . ? C8 Fe1 C2 150.5(2) . . ? C9 Fe1 C2 169.4(2) . . ? C4 Fe1 C2 68.2(2) . . ? C10 Fe1 C2 133.60(14) . . ? C1 Fe1 C2 41.12(14) . . ? C3 Fe1 C2 40.2(2) . . ? C6 Fe1 C2 112.78(15) . . ? O1 Mn1 O7 92.46(9) . . ? O1 Mn1 O3 78.38(8) . 3_755 ? O7 Mn1 O3 109.64(9) . 3_755 ? O1 Mn1 O5 89.15(9) . . ? O7 Mn1 O5 82.71(9) . . ? O3 Mn1 O5 162.60(9) 3_755 . ? O1 Mn1 O8 163.38(9) . . ? O7 Mn1 O8 80.22(9) . . ? O3 Mn1 O8 89.99(9) 3_755 . ? O5 Mn1 O8 104.53(10) . . ? O1 Mn1 O6 114.41(9) . . ? O7 Mn1 O6 147.63(9) . . ? O3 Mn1 O6 93.92(9) 3_755 . ? O5 Mn1 O6 80.13(9) . . ? O8 Mn1 O6 77.84(10) . . ? N1 O1 Mn1 124.0(2) . . ? N3 O3 Mn1 122.8(2) . 3_745 ? O1 N1 C11 124.9(3) . . ? O1 N1 C12 121.6(3) . . ? C11 N1 C12 112.8(3) . . ? O2 N2 C11 125.4(3) . . ? O2 N2 C13 122.3(3) . . ? C11 N2 C13 111.9(3) . . ? O3 N3 C14 126.1(3) . . ? O3 N3 C15 121.6(3) . . ? C14 N3 C15 111.6(3) . . ? O4 N4 C14 125.9(3) . . ? O4 N4 C16 122.3(3) . . ? C14 N4 C16 111.4(3) . . ? C17 O5 Mn1 129.4(2) . . ? C19 O6 Mn1 128.5(2) . . ? C20 O7 Mn1 129.8(2) . . ? C22 O8 Mn1 129.4(2) . . ? C5 C1 C11 127.0(3) . . ? C5 C1 C2 107.3(3) . . ? C11 C1 C2 125.7(3) . . ? C5 C1 Fe1 68.8(2) . . ? C11 C1 Fe1 127.3(2) . . ? C2 C1 Fe1 69.5(2) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 Fe1 69.8(3) . . ? C1 C2 Fe1 69.4(2) . . ? C4 C3 C2 109.5(3) . . ? C4 C3 Fe1 69.8(3) . . ? C2 C3 Fe1 69.9(2) . . ? C3 C4 C5 107.9(4) . . ? C3 C4 Fe1 70.1(2) . . ? C5 C4 Fe1 69.2(2) . . ? C4 C5 C1 108.6(4) . . ? C4 C5 Fe1 70.5(2) . . ? C1 C5 Fe1 70.4(2) . . ? C14 C6 C7 126.7(3) . . ? C14 C6 C10 126.1(3) . . ? C7 C6 C10 107.2(3) . . ? C14 C6 Fe1 127.4(3) . . ? C7 C6 Fe1 68.6(2) . . ? C10 C6 Fe1 69.3(2) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 Fe1 70.0(2) . . ? C6 C7 Fe1 70.3(2) . . ? C9 C8 C7 108.6(4) . . ? C9 C8 Fe1 70.1(2) . . ? C7 C8 Fe1 69.3(2) . . ? C8 C9 C10 109.3(4) . . ? C8 C9 Fe1 69.8(3) . . ? C10 C9 Fe1 70.2(2) . . ? C9 C10 C6 107.4(4) . . ? C9 C10 Fe1 69.7(2) . . ? C6 C10 Fe1 69.5(2) . . ? N1 C11 N2 107.7(3) . . ? N1 C11 C1 126.3(3) . . ? N2 C11 C1 126.0(3) . . ? N1 C12 C122 111.2(3) . . ? N1 C12 C121 106.2(3) . . ? C122 C12 C121 111.4(3) . . ? N1 C12 C13 99.5(3) . . ? C122 C12 C13 114.7(3) . . ? C121 C12 C13 112.9(3) . . ? N2 C13 C132 107.1(3) . . ? N2 C13 C131 110.2(3) . . ? C132 C13 C131 110.6(3) . . ? N2 C13 C12 100.3(3) . . ? C132 C13 C12 113.3(3) . . ? C131 C13 C12 114.6(3) . . ? N3 C14 N4 107.6(3) . . ? N3 C14 C6 127.2(3) . . ? N4 C14 C6 125.1(3) . . ? N3 C15 C152 111.6(3) . . ? N3 C15 C151 106.5(3) . . ? C152 C15 C151 110.5(4) . . ? N3 C15 C16 98.7(3) . . ? C152 C15 C16 115.6(3) . . ? C151 C15 C16 113.1(3) . . ? N4 C16 C161 110.3(3) . . ? N4 C16 C162 106.2(3) . . ? C161 C16 C162 111.7(3) . . ? N4 C16 C15 100.1(3) . . ? C161 C16 C15 114.7(4) . . ? C162 C16 C15 112.9(3) . . ? O5 C17 C18 128.0(4) . . ? O5 C17 C171 114.7(3) . . ? C18 C17 C171 117.2(4) . . ? C17 C18 C19 121.8(4) . . ? O6 C19 C18 128.0(3) . . ? O6 C19 C191 114.8(4) . . ? C18 C19 C191 117.2(4) . . ? O7 C20 C21 128.1(3) . . ? O7 C20 C201 113.8(3) . . ? C21 C20 C201 118.0(3) . . ? C22 C21 C20 120.1(4) . . ? O8 C22 C21 128.7(3) . . ? O8 C22 C221 113.8(4) . . ? C21 C22 C221 117.4(4) . . ? F1 C171 F2 112.2(5) . . ? F1 C171 F3 105.7(5) . . ? F2 C171 F3 100.6(4) . . ? F1 C171 C17 116.6(4) . . ? F2 C171 C17 110.6(4) . . ? F3 C171 C17 109.8(5) . . ? F5A C191 F4A 111.5(15) . . ? F5A C191 F6 55.4(17) . . ? F4A C191 F6 125.7(8) . . ? F5A C191 F4 132.2(11) . . ? F4A C191 F4 32.3(12) . . ? F6 C191 F4 112.2(8) . . ? F5A C191 F5 49.1(19) . . ? F4A C191 F5 74.2(12) . . ? F6 C191 F5 102.7(8) . . ? F4 C191 F5 105.9(9) . . ? F5A C191 F6A 105.2(17) . . ? F4A C191 F6A 100.2(12) . . ? F6 C191 F6A 51.0(8) . . ? F4 C191 F6A 71.1(10) . . ? F5 C191 F6A 143.9(8) . . ? F5A C191 C19 115.7(9) . . ? F4A C191 C19 116.1(7) . . ? F6 C191 C19 116.0(5) . . ? F4 C191 C19 110.8(7) . . ? F5 C191 C19 108.4(5) . . ? F6A C191 C19 106.0(6) . . ? F8A C201 F7 124.0(14) . . ? F8A C201 F9A 109.7(15) . . ? F7 C201 F9A 23.9(12) . . ? F8A C201 F9 32.6(16) . . ? F7 C201 F9 104.1(8) . . ? F9A C201 F9 83.2(13) . . ? F8A C201 F8 72.1(15) . . ? F7 C201 F8 111.6(9) . . ? F9A C201 F8 129.0(9) . . ? F9 C201 F8 103.5(8) . . ? F8A C201 F7A 112.9(16) . . ? F7 C201 F7A 74.8(11) . . ? F9A C201 F7A 98.1(13) . . ? F9 C201 F7A 137.7(9) . . ? F8 C201 F7A 44.3(8) . . ? F8A C201 C20 115.4(13) . . ? F7 C201 C20 112.6(6) . . ? F9A C201 C20 110.0(9) . . ? F9 C201 C20 109.7(6) . . ? F8 C201 C20 114.4(5) . . ? F7A C201 C20 109.4(7) . . ? F12A C221 F11 127.7(8) . . ? F12A C221 F10 57.6(18) . . ? F11 C221 F10 105.2(9) . . ? F12A C221 F10A 108.8(16) . . ? F11 C221 F10A 54.9(24) . . ? F10 C221 F10A 56.3(18) . . ? F12A C221 F12 46.3(21) . . ? F11 C221 F12 110.6(9) . . ? F10 C221 F12 102.9(9) . . ? F10A C221 F12 139.9(13) . . ? F12A C221 F11A 106.7(19) . . ? F11 C221 F11A 52.8(9) . . ? F10 C221 F11A 140.4(8) . . ? F10A C221 F11A 107.1(23) . . ? F12 C221 F11A 65.4(12) . . ? F12A C221 C22 116.0(7) . . ? F11 C221 C22 116.0(6) . . ? F10 C221 C22 113.3(5) . . ? F10A C221 C22 111.6(15) . . ? F12 C221 C22 108.1(6) . . ? F11A C221 C22 106.2(8) . . ? Cl1 C23 Cl2 113.5(8) . . ? Cl1A C23A Cl2A 106.2(20) . . ? _refine_diff_density_max 0.315 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.039 #============================================================================ _eof # End of Crystallographic Information File