Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Christine McKenzie' 'Carole Baffert' 'Marie-Noelle Collomb' 'A. Deronzier' 'Sanne Kjaergaard Knudsen' ; J.-M.Latour ; 'Kirsten H. Lund' 'Martin Mortensen' 'Lars Preuss Nielsen' 'Niels Thorup' _publ_contact_author_name 'Dr Christine McKenzie' _publ_contact_author_address ; Department of Chemistry University of Southern Denmark Odense Campus Campusveh 55 Odense 5230 DENMARK ; _publ_contact_author_email CHK@CHEM.SDU.DK _publ_section_title ; Biologically relevant mono- and di-nuclear manganese II/III/IV complexes of mononegative pentadentate ligands ; data_cm6k _database_code_CSD 188989 _audit_creation_method 'manual editing of SHELXTL Ver. 5.10 cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H46 Mn2 N8 O6 (Cl O4)2' _chemical_formula_sum 'C34 H46 Cl2 Mn2 N8 O14' _chemical_formula_weight 971.57 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3686(9) _cell_length_b 9.8838(11) _cell_length_c 13.1867(14) _cell_angle_alpha 69.825(10) _cell_angle_beta 85.749(10) _cell_angle_gamma 78.412(10) _cell_volume 1002.92(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 927 _cell_measurement_theta_min 2.973 _cell_measurement_theta_max 26.378 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_preparation ; 'crystallized from aqueous solution' ; _exptl_crystal_F_000 502 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8635 _exptl_absorpt_correction_T_max 0.9672 _exptl_absorpt_process_details 'SADABS ver 2.03 (SHeldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Siemens/Bruker SMART 1K' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10572 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4106 _reflns_number_gt 3606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker-AXS, 1999)' _computing_cell_refinement 'SMART 5.054 (Bruker-AXS, 1999)' _computing_data_reduction 'SAINT 6.02a (Bruker-AXS, 2000)' _computing_structure_solution 'SHELXTL 5.10 (Bruker-AXS, 1997)' _computing_structure_refinement 'SHELXTL 5.10 (Bruker-AXS, 1997)' _computing_molecular_graphics ; 'SHELXTL 5.10 (Bruker-AXS, 1997) and PLATON (Spek, 1990)' ; _computing_publication_material ; 'SHELXTL 5.10 (Bruker-AXS, 1997) and PLATON (Spek, 1990)' ; _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^)+(0.0446P)^2^+1.2799P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4106 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Mn Mn 0.53260(4) 0.65864(4) 0.35586(3) 0.02110(11) Uani 1 1 d . . . O1 O 0.3244(2) 0.8415(2) 0.29925(17) 0.0363(4) Uani 1 1 d . . . H17A H 0.241(5) 0.814(4) 0.331(3) 0.051(10) Uiso 1 1 d . . . H17B H 0.303(4) 0.921(4) 0.253(3) 0.051(10) Uiso 1 1 d . . . O2 O 0.35347(18) 0.57485(18) 0.48495(12) 0.0230(3) Uani 1 1 d . . . O3 O 0.1097(2) 0.7002(2) 0.41639(15) 0.0412(5) Uani 1 1 d . . . N1 N 0.6718(2) 0.8338(2) 0.22246(15) 0.0240(4) Uani 1 1 d . . . N2 N 0.7665(2) 0.5164(2) 0.31225(15) 0.0241(4) Uani 1 1 d . . . N3 N 0.4584(2) 0.5628(2) 0.23511(16) 0.0265(4) Uani 1 1 d . . . N4 N 0.6440(2) 0.7756(2) 0.44323(15) 0.0241(4) Uani 1 1 d . . . C1 C 0.8420(3) 0.7576(3) 0.21902(19) 0.0270(5) Uani 1 1 d . . . H1A H 0.9007 0.7492 0.2840 0.032 Uiso 1 1 calc R . . H1B H 0.8982 0.8150 0.1546 0.032 Uiso 1 1 calc R . . C2 C 0.8449(3) 0.6062(3) 0.21460(19) 0.0288(5) Uani 1 1 d . . . H2A H 0.7866 0.6148 0.1494 0.035 Uiso 1 1 calc R . . H2B H 0.9592 0.5573 0.2096 0.035 Uiso 1 1 calc R . . C3 C 0.8810(3) 0.4559(3) 0.4027(2) 0.0313(6) Uani 1 1 d . . . H3A H 0.9321 0.5354 0.4078 0.038 Uiso 1 1 calc R . . H3B H 0.9686 0.3810 0.3882 0.038 Uiso 1 1 calc R . . C4 C 0.7146(3) 0.3956(3) 0.2903(2) 0.0309(5) Uani 1 1 d . . . H4A H 0.6937 0.3202 0.3596 0.037 Uiso 1 1 calc R . . H4B H 0.8036 0.3494 0.2523 0.037 Uiso 1 1 calc R . . C5 C 0.5639(3) 0.4477(3) 0.22295(19) 0.0280(5) Uani 1 1 d . . . C6 C 0.5323(4) 0.3752(3) 0.1554(2) 0.0379(7) Uani 1 1 d . . . H6 H 0.6099 0.2948 0.1477 0.045 Uiso 1 1 calc R . . C7 C 0.3887(4) 0.4204(4) 0.1002(2) 0.0436(8) Uani 1 1 d . . . H7 H 0.3637 0.3697 0.0557 0.052 Uiso 1 1 calc R . . C8 C 0.2806(3) 0.5400(4) 0.1099(2) 0.0425(8) Uani 1 1 d . . . H8 H 0.1812 0.5750 0.0708 0.051 Uiso 1 1 calc R . . C9 C 0.3198(3) 0.6087(3) 0.1781(2) 0.0343(6) Uani 1 1 d . . . H9 H 0.2454 0.6917 0.1846 0.041 Uiso 1 1 calc R . . C10 C 0.6598(3) 0.7304(3) 0.55124(19) 0.0257(5) Uani 1 1 d . . . H10 H 0.6251 0.6418 0.5934 0.031 Uiso 1 1 calc R . . C11 C 0.7236(3) 0.8060(3) 0.6037(2) 0.0309(5) Uani 1 1 d . . . H11 H 0.7301 0.7717 0.6803 0.037 Uiso 1 1 calc R . . C12 C 0.7779(4) 0.9327(3) 0.5425(2) 0.0353(6) Uani 1 1 d . . . H12 H 0.8236 0.9870 0.5762 0.042 Uiso 1 1 calc R . . C13 C 0.7645(3) 0.9791(3) 0.4317(2) 0.0333(6) Uani 1 1 d . . . H13 H 0.8035 1.0648 0.3879 0.040 Uiso 1 1 calc R . . C14 C 0.6941(3) 0.9002(3) 0.38437(19) 0.0264(5) Uani 1 1 d . . . C15 C 0.6660(3) 0.9543(3) 0.26437(19) 0.0297(5) Uani 1 1 d . . . H15A H 0.5582 1.0202 0.2480 0.036 Uiso 1 1 calc R . . H15B H 0.7502 1.0121 0.2272 0.036 Uiso 1 1 calc R . . C16 C 0.6043(3) 0.8952(3) 0.11193(19) 0.0304(5) Uani 1 1 d . . . H16A H 0.4906 0.9439 0.1141 0.046 Uiso 1 1 calc R . . H16B H 0.6095 0.8158 0.0826 0.046 Uiso 1 1 calc R . . H16C H 0.6683 0.9665 0.0658 0.046 Uiso 1 1 calc R . . C17 C 0.2002(3) 0.6130(3) 0.49065(19) 0.0266(5) Uani 1 1 d . . . Cl Cl 0.07004(8) 1.17290(7) 0.12711(5) 0.03251(16) Uani 1 1 d . . . O4 O 0.2449(3) 1.1214(3) 0.1389(2) 0.0621(7) Uani 1 1 d . . . O5 O 0.0008(3) 1.1342(4) 0.2312(2) 0.0705(8) Uani 1 1 d . . . O6 O 0.0421(4) 1.3260(3) 0.0780(3) 0.1125(15) Uani 1 1 d . . . O7 O -0.0039(6) 1.1131(5) 0.0659(3) 0.1219(16) Uani 1 1 d . . . 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 Mn 0.01844(18) 0.0253(2) 0.02020(18) -0.00877(14) 0.00038(13) -0.00390(14) O1 0.0263(10) 0.0308(11) 0.0389(11) -0.0005(9) 0.0055(8) 0.0013(8) O2 0.0170(8) 0.0268(8) 0.0231(8) -0.0069(7) -0.0024(6) -0.0012(6) O3 0.0215(9) 0.0492(12) 0.0348(10) 0.0104(9) -0.0089(8) -0.0069(8) N1 0.0210(10) 0.0292(11) 0.0183(9) -0.0045(8) -0.0026(7) -0.0020(8) N2 0.0185(9) 0.0264(10) 0.0220(10) -0.0032(8) 0.0000(7) -0.0011(8) N3 0.0230(10) 0.0369(12) 0.0217(10) -0.0108(9) 0.0010(8) -0.0091(9) N4 0.0267(10) 0.0241(10) 0.0208(9) -0.0061(8) -0.0005(8) -0.0059(8) C1 0.0195(11) 0.0351(13) 0.0206(11) -0.0013(10) -0.0018(9) -0.0055(10) C2 0.0199(11) 0.0344(13) 0.0247(12) -0.0039(10) 0.0032(9) -0.0005(10) C3 0.0162(11) 0.0368(14) 0.0298(13) 0.0002(11) -0.0029(9) 0.0005(10) C4 0.0343(14) 0.0267(13) 0.0284(12) -0.0097(10) 0.0053(10) 0.0001(10) C5 0.0358(13) 0.0291(13) 0.0211(11) -0.0083(10) 0.0078(10) -0.0133(11) C6 0.0592(19) 0.0360(15) 0.0253(13) -0.0132(11) 0.0122(12) -0.0239(13) C7 0.0594(19) 0.061(2) 0.0253(13) -0.0195(13) 0.0131(13) -0.0398(17) C8 0.0335(15) 0.077(2) 0.0229(13) -0.0127(14) 0.0018(11) -0.0325(15) C9 0.0220(12) 0.0556(17) 0.0259(13) -0.0120(12) 0.0001(10) -0.0117(12) C10 0.0275(12) 0.0271(12) 0.0211(11) -0.0060(9) 0.0020(9) -0.0065(10) C11 0.0340(14) 0.0364(14) 0.0237(12) -0.0128(11) 0.0008(10) -0.0052(11) C12 0.0452(16) 0.0337(14) 0.0344(14) -0.0186(12) -0.0002(12) -0.0113(12) C13 0.0424(15) 0.0249(12) 0.0348(14) -0.0110(11) 0.0028(11) -0.0107(11) C14 0.0291(12) 0.0238(12) 0.0245(12) -0.0062(10) -0.0001(9) -0.0046(10) C15 0.0357(14) 0.0248(12) 0.0244(12) -0.0016(10) -0.0020(10) -0.0077(10) C16 0.0254(12) 0.0393(14) 0.0185(11) -0.0023(10) -0.0045(9) -0.0003(11) C17 0.0202(11) 0.0288(13) 0.0274(12) -0.0042(10) -0.0050(9) -0.0048(10) Cl 0.0385(3) 0.0297(3) 0.0280(3) -0.0072(2) 0.0029(2) -0.0089(3) O4 0.0448(13) 0.0431(13) 0.0743(17) 0.0003(12) 0.0227(12) 0.0016(10) O5 0.0455(14) 0.113(2) 0.0454(13) -0.0302(15) 0.0093(11) 0.0040(14) O6 0.072(2) 0.0440(15) 0.179(4) 0.0363(19) -0.068(2) -0.0244(14) O7 0.172(4) 0.161(4) 0.093(3) -0.084(3) 0.024(3) -0.103(3) _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 Mn O1 2.204(2) . ? Mn O2 2.2313(16) . ? Mn N4 2.246(2) . ? Mn N3 2.290(2) . ? Mn N2 2.329(2) . ? Mn N1 2.419(2) . ? Mn O2 2.5908(16) 2_666 ? O1 H17A 0.83(4) . ? O1 H17B 0.80(4) . ? O2 C17 1.266(3) . ? O3 C17 1.241(3) . ? N1 C15 1.468(3) . ? N1 C1 1.477(3) . ? N1 C16 1.478(3) . ? N2 C3 1.464(3) . ? N2 C4 1.471(3) . ? N2 C2 1.483(3) . ? N3 C9 1.341(3) . ? N3 C5 1.342(3) . ? N4 C14 1.340(3) . ? N4 C10 1.346(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C17 1.513(3) 2_666 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.495(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.389(4) . ? C6 C7 1.365(5) . ? C6 H6 0.9500 . ? C7 C8 1.375(5) . ? C7 H7 0.9500 . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.375(3) . ? C10 H10 0.9500 . ? C11 C12 1.379(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(4) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.505(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C3 1.513(3) 2_666 ? Cl O7 1.391(3) . ? Cl O6 1.403(3) . ? Cl O5 1.405(2) . ? Cl O4 1.451(2) . ? 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 O1 Mn O2 81.49(7) . . ? O1 Mn N4 92.80(8) . . ? O2 Mn N4 96.38(7) . . ? O1 Mn N3 88.22(8) . . ? O2 Mn N3 96.85(6) . . ? N4 Mn N3 166.73(7) . . ? O1 Mn N2 147.95(7) . . ? O2 Mn N2 125.28(7) . . ? N4 Mn N2 100.28(7) . . ? N3 Mn N2 72.64(7) . . ? O1 Mn N1 80.83(7) . . ? O2 Mn N1 158.64(7) . . ? N4 Mn N1 72.66(7) . . ? N3 Mn N1 94.48(7) . . ? N2 Mn N1 75.47(7) . . ? O1 Mn O2 144.81(7) . 2_666 ? O2 Mn O2 64.11(6) . 2_666 ? N4 Mn O2 84.32(6) . 2_666 ? N3 Mn O2 102.36(7) . 2_666 ? N2 Mn O2 66.24(6) . 2_666 ? N1 Mn O2 130.55(6) . 2_666 ? Mn O1 H17A 108(3) . . ? Mn O1 H17B 140(3) . . ? H17A O1 H17B 112(3) . . ? C17 O2 Mn 131.37(15) . . ? C15 N1 C1 110.14(19) . . ? C15 N1 C16 108.76(19) . . ? C1 N1 C16 109.21(18) . . ? C15 N1 Mn 105.64(14) . . ? C1 N1 Mn 106.15(14) . . ? C16 N1 Mn 116.79(15) . . ? C3 N2 C4 109.4(2) . . ? C3 N2 C2 110.13(18) . . ? C4 N2 C2 109.79(19) . . ? C3 N2 Mn 110.55(15) . . ? C4 N2 Mn 107.02(14) . . ? C2 N2 Mn 109.88(14) . . ? C9 N3 C5 117.8(2) . . ? C9 N3 Mn 126.33(18) . . ? C5 N3 Mn 115.83(16) . . ? C14 N4 C10 117.9(2) . . ? C14 N4 Mn 117.95(15) . . ? C10 N4 Mn 124.14(16) . . ? N1 C1 C2 110.02(19) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 110.6(2) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C17 112.67(19) . 2_666 ? N2 C3 H3A 109.1 . . ? C17 C3 H3A 109.1 2_666 . ? N2 C3 H3B 109.1 . . ? C17 C3 H3B 109.1 2_666 . ? H3A C3 H3B 107.8 . . ? N2 C4 C5 111.8(2) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 122.2(3) . . ? N3 C5 C4 116.7(2) . . ? C6 C5 C4 121.1(2) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.2(3) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C7 C8 C9 118.6(3) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N3 C9 C8 122.7(3) . . ? N3 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N4 C10 C11 123.4(2) . . ? N4 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 118.5(2) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 118.7(2) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 119.7(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? N4 C14 C13 121.8(2) . . ? N4 C14 C15 117.3(2) . . ? C13 C14 C15 120.9(2) . . ? N1 C15 C14 112.31(19) . . ? N1 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O2 126.1(2) . . ? O3 C17 C3 116.8(2) . 2_666 ? O2 C17 C3 117.1(2) . 2_666 ? O7 Cl O6 109.0(3) . . ? O7 Cl O5 108.1(2) . . ? O6 Cl O5 110.3(2) . . ? O7 Cl O4 114.1(2) . . ? O6 Cl O4 107.78(16) . . ? O5 Cl O4 107.52(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.983 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.065