Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name ; Prof C McAuliffe ; _publ_contact_author_address ; Department of Chemistry University of Manchester Institute of Science and Technology PO Box 88 Manchester M60 1QD England ; _publ_requested_journal 'Chem.Commun.' loop_ _publ_author_name 'Cross, Wendy' 'Godfrey, S. M.' 'McAuliffe, C.' 'Pritchard, Robin G.' _publ_section_title ; Anion and guest-molecule locations within the tunnels and cavities of micro-porous "chinese-lantern" crystals ; data_u _database_code_CSD 153090 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H128 I4 Mn2 O13 P8' _chemical_formula_weight 2583.41 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' 'P' 'P' 0.1023 0.0942 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.984(4) _cell_length_b 14.984(4) _cell_length_c 25.761(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5784(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7757 _exptl_absorpt_correction_T_max 0.9256 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4499 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.52 _reflns_number_total 4499 _reflns_number_gt 2103 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0470P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4499 _refine_ls_number_parameters 179 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.005 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.39617(16) 0.0491(11) Uani 0.375(3) 4 d SP . 2 Mn2 Mn 0.0000 0.0000 0.35631(7) 0.0320(5) Uani 0.625(3) 4 d SP . 1 P1 P 0.21799(4) 0.06133(5) 0.39051(3) 0.03474(17) Uani 1 1 d . . . O1 O 0.12046(11) 0.07356(11) 0.37917(7) 0.0421(5) Uani 1 1 d . . . C1 C 0.27751(18) 0.16617(19) 0.39032(11) 0.0429(7) Uani 1 1 d . . . C2 C 0.2443(2) 0.2373(2) 0.36313(15) 0.0634(10) Uani 1 1 d . . . H2A H 0.1884 0.2333 0.3477 0.076 Uiso 1 1 calc R . . C3 C 0.2941(3) 0.3163(2) 0.35843(17) 0.0851(13) Uani 1 1 d . . . H3A H 0.2710 0.3643 0.3399 0.102 Uiso 1 1 calc R . . C4 C 0.3751(3) 0.3231(3) 0.38061(19) 0.0934(14) Uani 1 1 d . . . H4A H 0.4079 0.3755 0.3774 0.112 Uiso 1 1 calc R . . C5 C 0.4092(3) 0.2521(3) 0.40816(18) 0.0929(14) Uani 1 1 d . . . H5A H 0.4649 0.2568 0.4239 0.112 Uiso 1 1 calc R . . C6 C 0.3614(2) 0.1744(2) 0.41247(15) 0.0719(10) Uani 1 1 d . . . H6A H 0.3856 0.1265 0.4306 0.086 Uiso 1 1 calc R . . C7 C 0.27401(19) -0.00470(17) 0.34194(11) 0.0436(7) Uani 1 1 d . . . C8 C 0.3604(2) -0.0358(2) 0.34882(14) 0.0601(9) Uani 1 1 d . . . H8A H 0.3900 -0.0240 0.3798 0.072 Uiso 1 1 calc R . . C9 C 0.4029(3) -0.0837(2) 0.31091(18) 0.0836(12) Uani 1 1 d . . . H9A H 0.4612 -0.1028 0.3163 0.100 Uiso 1 1 calc R . . C10 C 0.3619(3) -0.1033(3) 0.26646(19) 0.0912(14) Uani 1 1 d . . . H10A H 0.3910 -0.1375 0.2415 0.109 Uiso 1 1 calc R . . C11 C 0.2764(4) -0.0731(3) 0.25724(13) 0.0915(14) Uani 1 1 d . . . H11A H 0.2482 -0.0857 0.2259 0.110 Uiso 1 1 calc R . . C12 C 0.2316(2) -0.0223(2) 0.29607(12) 0.0637(9) Uani 1 1 d . . . H12A H 0.1740 -0.0013 0.2903 0.076 Uiso 1 1 calc R . . C13 C 0.23906(18) 0.00602(18) 0.45139(10) 0.0417(7) Uani 1 1 d . . . H13A H 0.2052 -0.0491 0.4520 0.050 Uiso 1 1 calc R . . H13B H 0.3018 -0.0097 0.4528 0.050 Uiso 1 1 calc R . . C14 C 0.2161(4) 0.0595(3) 0.5000 0.0693(15) Uani 1 2 d S . . H14A H 0.1530 0.0737 0.5000 0.083 Uiso 1 2 calc SR . . H14B H 0.2493 0.1151 0.5000 0.083 Uiso 1 2 calc SR . . I1 I 0.0000 0.0000 0.5000 0.0551(5) Uani 0.443(2) 8 d SP . . I2A I 0.0000 0.0000 0.24429(3) 0.0460(3) Uani 0.624(2) 4 d SP . . I2B I 0.0000 0.0000 0.2033(3) 0.106(3) Uani 0.126(2) 4 d SP . . I3 I 0.5000 0.0000 0.5000 0.0760(2) Uani 1.0013(18) 4 d SP . . O2 O 0.5000 0.5000 0.4400(12) 0.252(11) Uiso 0.50 4 d SPD . . C15 C 0.5000 0.5000 0.4825(9) 0.124(8) Uiso 0.50 4 d SPD . . C16 C 0.461(2) 0.583(2) 0.5000 0.260(14) Uiso 0.50 2 d SPD . . O17 O 0.2215(9) 0.3380(10) 0.5000 0.249(7) Uiso 0.415(5) 2 d SP . . C17 C 0.2215(9) 0.3380(10) 0.5000 0.249(7) Uiso 0.415(5) 2 d SP . . O18 O 0.2219(10) 0.4222(12) 0.5000 0.283(8) Uiso 0.415(5) 2 d SP . . C18 C 0.2219(10) 0.4222(12) 0.5000 0.283(8) Uiso 0.415(5) 2 d SP . . 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 Mn1 0.0313(9) 0.0313(9) 0.085(3) 0.000 0.000 0.000 Mn2 0.0279(5) 0.0279(5) 0.0402(10) 0.000 0.000 0.000 P1 0.0332(4) 0.0389(4) 0.0321(3) 0.0005(3) 0.0006(3) -0.0009(3) O1 0.0320(10) 0.0412(10) 0.0532(12) 0.0039(9) -0.0046(8) -0.0031(8) C1 0.0382(15) 0.0438(16) 0.0468(15) -0.0025(14) -0.0004(13) -0.0030(12) C2 0.0466(18) 0.056(2) 0.088(3) 0.0087(18) -0.0137(18) -0.0027(15) C3 0.081(3) 0.053(2) 0.122(4) 0.017(2) -0.012(3) -0.016(2) C4 0.077(3) 0.064(3) 0.139(4) -0.007(3) -0.006(3) -0.030(2) C5 0.062(2) 0.084(3) 0.133(4) 0.003(3) -0.033(2) -0.028(2) C6 0.055(2) 0.058(2) 0.103(3) 0.003(2) -0.027(2) -0.0068(17) C7 0.0525(18) 0.0410(16) 0.0373(15) 0.0000(12) 0.0092(13) -0.0076(13) C8 0.0516(19) 0.061(2) 0.067(2) -0.0088(18) 0.0155(17) 0.0021(15) C9 0.087(3) 0.072(3) 0.091(3) -0.010(2) 0.047(2) 0.001(2) C10 0.111(4) 0.075(3) 0.087(3) -0.004(2) 0.053(3) 0.003(3) C11 0.147(4) 0.088(3) 0.0398(19) -0.013(2) 0.011(2) -0.028(3) C12 0.080(2) 0.068(2) 0.0433(18) -0.0047(17) 0.0039(17) -0.0088(18) C13 0.0461(16) 0.0434(16) 0.0358(15) 0.0014(12) 0.0032(12) 0.0050(13) C14 0.116(4) 0.063(3) 0.029(2) 0.000 0.000 0.035(3) I1 0.0441(6) 0.0441(6) 0.0773(10) 0.000 0.000 0.000 I2A 0.0518(3) 0.0518(3) 0.0343(4) 0.000 0.000 0.000 I2B 0.091(3) 0.091(3) 0.137(7) 0.000 0.000 0.000 I3 0.0440(3) 0.1118(5) 0.0722(4) 0.000 0.000 0.0265(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 Mn1 O1 2.1597(19) 2 ? Mn1 O1 2.1597(19) . ? Mn1 O1 2.1597(19) 3 ? Mn1 O1 2.1597(19) 4 ? Mn1 I1 2.675(4) . ? Mn2 O1 2.1953(18) . ? Mn2 O1 2.1953(18) 3 ? Mn2 O1 2.1953(18) 2 ? Mn2 O1 2.1953(18) 4 ? Mn2 I2A 2.886(2) . ? P1 O1 1.5014(18) . ? P1 C13 1.802(3) . ? P1 C7 1.802(3) . ? P1 C1 1.806(3) . ? C1 C2 1.369(4) . ? C1 C6 1.386(4) . ? C2 C3 1.405(4) . ? C3 C4 1.344(5) . ? C4 C5 1.377(5) . ? C5 C6 1.371(5) . ? C7 C12 1.367(4) . ? C7 C8 1.387(4) . ? C8 C9 1.368(5) . ? C9 C10 1.332(6) . ? C10 C11 1.379(6) . ? C11 C12 1.425(5) . ? C13 C14 1.526(4) . ? C14 C13 1.526(4) 10_556 ? I1 Mn1 2.675(4) 9_556 ? I2A I2B 1.056(8) . ? O2 C15 1.10(3) . ? C15 C15 0.90(5) 9_666 ? C15 C16 1.44(3) 11_566 ? C15 C16 1.44(3) . ? C15 C16 1.44(3) 3_655 ? C15 C16 1.44(3) 9_666 ? C16 C15 1.44(3) 9_666 ? C16 C16 1.93(4) 3_655 ? C16 C16 1.93(4) 11_566 ? O17 O18 1.261(19) . ? 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 Mn1 O1 156.6(2) 2 . ? O1 Mn1 O1 87.64(5) 2 3 ? O1 Mn1 O1 87.64(5) . 3 ? O1 Mn1 O1 87.64(5) 2 4 ? O1 Mn1 O1 87.64(5) . 4 ? O1 Mn1 O1 156.6(2) 3 4 ? O1 Mn1 I1 101.70(11) 2 . ? O1 Mn1 I1 101.70(11) . . ? O1 Mn1 I1 101.70(11) 3 . ? O1 Mn1 I1 101.70(11) 4 . ? O1 Mn2 O1 85.87(3) . 3 ? O1 Mn2 O1 148.87(13) . 2 ? O1 Mn2 O1 85.87(3) 3 2 ? O1 Mn2 O1 85.87(3) . 4 ? O1 Mn2 O1 148.87(13) 3 4 ? O1 Mn2 O1 85.87(3) 2 4 ? O1 Mn2 I2A 105.56(7) . . ? O1 Mn2 I2A 105.56(7) 3 . ? O1 Mn2 I2A 105.56(7) 2 . ? O1 Mn2 I2A 105.56(7) 4 . ? O1 P1 C13 113.33(12) . . ? O1 P1 C7 112.66(12) . . ? C13 P1 C7 105.67(13) . . ? O1 P1 C1 111.96(11) . . ? C13 P1 C1 108.41(13) . . ? C7 P1 C1 104.21(12) . . ? P1 O1 Mn1 135.37(12) . . ? P1 O1 Mn2 142.29(11) . . ? Mn1 O1 Mn2 27.26(9) . . ? C2 C1 C6 118.1(3) . . ? C2 C1 P1 120.0(2) . . ? C6 C1 P1 121.6(2) . . ? C1 C2 C3 120.5(3) . . ? C4 C3 C2 120.4(4) . . ? C3 C4 C5 119.7(4) . . ? C6 C5 C4 120.2(4) . . ? C5 C6 C1 121.1(3) . . ? C12 C7 C8 118.6(3) . . ? C12 C7 P1 119.3(2) . . ? C8 C7 P1 122.0(2) . . ? C9 C8 C7 121.3(4) . . ? C10 C9 C8 121.0(4) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C12 119.5(4) . . ? C7 C12 C11 119.4(4) . . ? C14 C13 P1 115.7(2) . . ? C13 C14 C13 110.3(3) . 10_556 ? Mn1 I1 Mn1 180.0 9_556 . ? I2B I2A Mn2 180.0 . . ? C15 C15 O2 180.000(10) 9_666 . ? C15 C15 C16 71.8(11) 9_666 11_566 ? O2 C15 C16 108.2(11) . 11_566 ? C15 C15 C16 71.8(11) 9_666 . ? O2 C15 C16 108.2(11) . . ? C16 C15 C16 84.4(7) 11_566 . ? C15 C15 C16 71.8(11) 9_666 3_655 ? O2 C15 C16 108.2(11) . 3_655 ? C16 C15 C16 144(2) 11_566 3_655 ? C16 C15 C16 84.4(7) . 3_655 ? C15 C15 C16 71.8(11) 9_666 9_666 ? O2 C15 C16 108.2(11) . 9_666 ? C16 C15 C16 84.4(7) 11_566 9_666 ? C16 C15 C16 144(2) . 9_666 ? C16 C15 C16 84.4(7) 3_655 9_666 ? C15 C16 C15 36(2) 9_666 . ? C15 C16 C16 47.8(3) 9_666 3_655 ? C15 C16 C16 47.8(3) . 3_655 ? C15 C16 C16 47.8(3) 9_666 11_566 ? C15 C16 C16 47.8(3) . 11_566 ? C16 C16 C16 90.000(4) 3_655 11_566 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.823 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.063 #============================================================================== data_w11 _database_code_CSD 153091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H128 Cl4 Mn2 O13 P8' _chemical_formula_weight 2217.61 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' 'P' 'P' 0.1023 0.0942 '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' 'Mn' 'Mn' 0.3368 0.7283 '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 'tetragonal' _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.382(3) _cell_length_b 14.382(3) _cell_length_c 26.076(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5393(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square based pyramid' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.9114 _exptl_absorpt_correction_T_max 0.9728 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2645 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2441 _reflns_number_gt 1321 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] 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 0.00032(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2441 _refine_ls_number_parameters 180 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1530 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.40925(12) 0.0193(7) Uani 0.50 d SP . 2 Mn2 Mn 0.0000 0.0000 0.36826(13) 0.0236(7) Uani 0.50 d SP . 1 P1 P 0.22504(8) 0.06320(8) 0.39329(5) 0.0246(3) Uani 1 d . . . O1 O 0.1226(2) 0.0784(2) 0.38575(13) 0.0286(8) Uani 1 d . . . C1 C 0.2891(3) 0.1694(3) 0.39152(19) 0.0257(10) Uani 1 d . . . C2 C 0.2536(4) 0.2436(4) 0.3638(2) 0.0380(13) Uani 1 d . . . H2A H 0.1951 0.2388 0.3489 0.046 Uiso 1 calc R . . C3 C 0.3042(4) 0.3244(4) 0.3581(3) 0.0506(16) Uani 1 d . . . H3A H 0.2797 0.3739 0.3396 0.061 Uiso 1 calc R . . C4 C 0.3895(4) 0.3315(4) 0.3796(3) 0.0535(18) Uani 1 d . . . H4A H 0.4235 0.3861 0.3759 0.064 Uiso 1 calc R . . C5 C 0.4265(4) 0.2583(4) 0.4070(3) 0.0530(18) Uani 1 d . . . H5A H 0.4855 0.2634 0.4214 0.064 Uiso 1 calc R . . C6 C 0.3762(4) 0.1779(4) 0.4130(2) 0.0391(14) Uani 1 d . . . H6A H 0.4012 0.1288 0.4317 0.047 Uiso 1 calc R . . C7 C 0.2757(4) -0.0054(4) 0.3428(2) 0.0361(14) Uani 1 d . . . C8 C 0.3655(4) -0.0385(4) 0.3465(2) 0.0472(16) Uani 1 d . . . H8A H 0.4003 -0.0256 0.3757 0.057 Uiso 1 calc R . . C9 C 0.4038(5) -0.0896(5) 0.3082(3) 0.068(2) Uani 1 d . . . H9A H 0.4641 -0.1122 0.3115 0.081 Uiso 1 calc R . . C10 C 0.3548(6) -0.1076(5) 0.2656(3) 0.078(3) Uani 1 d . . . H10A H 0.3819 -0.1423 0.2394 0.093 Uiso 1 calc R . . C11 C 0.2645(6) -0.0753(4) 0.2599(2) 0.072(2) Uani 1 d . . . H11A H 0.2309 -0.0884 0.2303 0.086 Uiso 1 calc R . . C12 C 0.2243(5) -0.0224(4) 0.2998(2) 0.0484(16) Uani 1 d . . . H12A H 0.1640 0.0004 0.2968 0.058 Uiso 1 calc R . . C13 C 0.2514(3) 0.0065(3) 0.45233(18) 0.0263(11) Uani 1 d . . . H13A H 0.2153 -0.0504 0.4543 0.032 Uiso 1 calc R . . H13B H 0.3166 -0.0109 0.4521 0.032 Uiso 1 calc R . . C14 C 0.2325(5) 0.0637(5) 0.5000 0.0249(15) Uani 1 d S . . H14A H 0.1683 0.0842 0.5000 0.030 Uiso 1 calc SR . . H14B H 0.2720 0.1184 0.5000 0.030 Uiso 1 calc SR . . Cl1 Cl 0.0000 0.0000 0.5000 0.0317(9) Uani 1 d S . . Cl2A Cl 0.0000 0.0000 0.2746(2) 0.0333(13) Uani 0.50 d SP . . Cl3 Cl 0.5000 0.0000 0.5000 0.0692(11) Uani 1 d S . . O2 O 0.5000 0.5000 0.444(2) 0.24(2) Uiso 0.50 d SPD . . C15 C 0.5000 0.5000 0.489(3) 0.16(2) Uiso 0.50 d SPD . . C16 C 0.431(5) 0.558(6) 0.5000 0.31(4) Uiso 0.50 d SPD . . O17 O 0.2252(8) 0.3414(8) 0.5000 0.112(4) Uani 0.50 d SP . . C17 C 0.2252(8) 0.3414(8) 0.5000 0.112(4) Uani 0.50 d SP . . O18 O 0.1993(10) 0.4219(8) 0.4829(6) 0.131(8) Uani 0.25 d P . . C18 C 0.1993(10) 0.4219(8) 0.4829(6) 0.131(8) Uani 0.25 d P . . 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 Mn1 0.0179(10) 0.0179(10) 0.0222(17) 0.000 0.000 0.000 Mn2 0.0177(11) 0.0177(11) 0.035(2) 0.000 0.000 0.000 P1 0.0221(7) 0.0248(7) 0.0270(6) 0.0004(7) 0.0010(6) -0.0009(5) O1 0.0200(16) 0.0248(17) 0.041(2) 0.0041(17) -0.0051(17) -0.0033(13) C1 0.024(2) 0.027(3) 0.026(2) -0.005(2) 0.000(3) 0.000(2) C2 0.025(3) 0.038(3) 0.051(3) 0.004(3) -0.001(3) -0.006(2) C3 0.044(4) 0.037(3) 0.071(4) 0.011(3) 0.001(3) -0.006(3) C4 0.037(3) 0.038(3) 0.086(5) 0.008(3) 0.006(4) -0.016(3) C5 0.027(3) 0.054(4) 0.077(5) 0.002(4) -0.004(3) -0.015(3) C6 0.029(3) 0.034(3) 0.054(4) 0.007(3) -0.003(3) -0.003(2) C7 0.046(4) 0.033(3) 0.029(3) 0.005(3) 0.009(3) -0.005(3) C8 0.052(4) 0.034(3) 0.056(4) -0.006(3) 0.027(3) -0.005(3) C9 0.079(5) 0.056(4) 0.067(5) -0.014(4) 0.042(4) -0.003(4) C10 0.124(7) 0.045(4) 0.064(5) -0.011(4) 0.055(5) 0.000(5) C11 0.136(7) 0.048(4) 0.032(4) 0.002(3) 0.007(5) -0.031(4) C12 0.082(5) 0.038(3) 0.026(3) 0.000(3) -0.002(3) -0.006(3) C13 0.019(2) 0.025(3) 0.035(3) -0.006(2) 0.001(2) -0.003(2) C14 0.026(4) 0.029(4) 0.019(3) 0.000 0.000 -0.006(3) Cl1 0.0338(13) 0.0338(13) 0.028(2) 0.000 0.000 0.000 Cl2A 0.0306(18) 0.0306(18) 0.039(3) 0.000 0.000 0.000 Cl3 0.0276(17) 0.077(3) 0.103(3) 0.000 0.000 0.0118(17) O17 0.106(8) 0.101(8) 0.130(9) 0.000 0.000 0.000(7) C17 0.106(8) 0.101(8) 0.130(9) 0.000 0.000 0.000(7) O18 0.164(12) 0.065(7) 0.16(2) 0.086(10) 0.108(13) 0.057(8) C18 0.164(12) 0.065(7) 0.16(2) 0.086(10) 0.108(13) 0.057(8) _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 Mn1 O1 2.181(3) 2 ? Mn1 O1 2.181(3) . ? Mn1 O1 2.181(3) 3 ? Mn1 O1 2.181(3) 4 ? Mn1 Cl1 2.366(3) . ? Mn2 O1 2.142(3) 3 ? Mn2 O1 2.142(3) 2 ? Mn2 O1 2.142(3) . ? Mn2 O1 2.142(3) 4 ? Mn2 Cl2A 2.441(6) . ? P1 O1 1.502(3) . ? P1 C13 1.783(5) . ? P1 C1 1.784(5) . ? P1 C7 1.798(5) . ? C1 C6 1.378(7) . ? C1 C2 1.386(7) . ? C2 C3 1.379(8) . ? C3 C4 1.353(8) . ? C4 C5 1.379(8) . ? C5 C6 1.373(7) . ? C7 C12 1.367(7) . ? C7 C8 1.380(7) . ? C8 C9 1.357(8) . ? C9 C10 1.342(10) . ? C10 C11 1.388(10) . ? C11 C12 1.412(9) . ? C13 C14 1.515(6) . ? C14 C13 1.515(6) 10_556 ? Cl1 Mn1 2.366(3) 9_556 ? O2 C15 1.16(7) . ? O2 C15 1.74(12) 9_666 ? C15 C15 0.58(16) 9_666 ? C15 C16 1.33(5) 11_566 ? C15 C16 1.33(5) 9_666 ? C15 C16 1.33(5) 3_655 ? C15 C16 1.33(5) . ? C15 O2 1.74(12) 9_666 ? C16 C15 1.33(5) 9_666 ? C16 C16 1.84(8) 11_566 ? C16 C16 1.84(8) 3_655 ? O17 C18 1.295(13) 10_556 ? O17 O18 1.295(13) 10_556 ? O17 O18 1.295(13) . ? O18 C18 0.89(3) 10_556 ? O18 O18 0.89(3) 10_556 ? 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 Mn1 O1 147.4(2) 2 . ? O1 Mn1 O1 85.47(7) 2 3 ? O1 Mn1 O1 85.47(7) . 3 ? O1 Mn1 O1 85.47(7) 2 4 ? O1 Mn1 O1 85.47(7) . 4 ? O1 Mn1 O1 147.4(2) 3 4 ? O1 Mn1 Cl1 106.31(12) 2 . ? O1 Mn1 Cl1 106.31(12) . . ? O1 Mn1 Cl1 106.31(12) 3 . ? O1 Mn1 Cl1 106.31(12) 4 . ? O1 Mn2 O1 87.40(5) 3 2 ? O1 Mn2 O1 87.40(5) 3 . ? O1 Mn2 O1 155.4(3) 2 . ? O1 Mn2 O1 155.4(3) 3 4 ? O1 Mn2 O1 87.40(5) 2 4 ? O1 Mn2 O1 87.40(5) . 4 ? O1 Mn2 Cl2A 102.29(13) 3 . ? O1 Mn2 Cl2A 102.29(13) 2 . ? O1 Mn2 Cl2A 102.29(13) . . ? O1 Mn2 Cl2A 102.29(13) 4 . ? O1 P1 C13 112.9(2) . . ? O1 P1 C1 112.23(19) . . ? C13 P1 C1 107.7(2) . . ? O1 P1 C7 112.4(2) . . ? C13 P1 C7 107.1(2) . . ? C1 P1 C7 103.9(2) . . ? P1 O1 Mn2 139.30(19) . . ? P1 O1 Mn1 132.88(19) . . ? Mn2 O1 Mn1 28.61(10) . . ? C6 C1 C2 118.6(5) . . ? C6 C1 P1 122.4(4) . . ? C2 C1 P1 118.8(4) . . ? C3 C2 C1 120.7(5) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C5 120.5(5) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 C1 120.5(5) . . ? C12 C7 C8 120.1(6) . . ? C12 C7 P1 118.7(5) . . ? C8 C7 P1 121.2(4) . . ? C9 C8 C7 121.0(6) . . ? C10 C9 C8 120.1(7) . . ? C9 C10 C11 121.0(7) . . ? C10 C11 C12 119.1(7) . . ? C7 C12 C11 118.6(7) . . ? C14 C13 P1 114.9(3) . . ? C13 C14 C13 110.2(6) . 10_556 ? Mn1 Cl1 Mn1 180.0 9_556 . ? C15 O2 C15 0.000(8) . 9_666 ? C15 C15 O2 180.00(2) 9_666 . ? C15 C15 C16 77(4) 9_666 11_566 ? O2 C15 C16 103(4) . 11_566 ? C15 C15 C16 77(4) 9_666 9_666 ? O2 C15 C16 103(4) . 9_666 ? C16 C15 C16 87.3(15) 11_566 9_666 ? C15 C15 C16 77(4) 9_666 3_655 ? O2 C15 C16 103(4) . 3_655 ? C16 C15 C16 155(7) 11_566 3_655 ? C16 C15 C16 87.3(15) 9_666 3_655 ? C15 C15 C16 77(4) 9_666 . ? O2 C15 C16 103(4) . . ? C16 C15 C16 87.3(15) 11_566 . ? C16 C15 C16 155(7) 9_666 . ? C16 C15 C16 87.3(15) 3_655 . ? C15 C15 O2 0.00(3) 9_666 9_666 ? O2 C15 O2 180.000(6) . 9_666 ? C16 C15 O2 77(4) 11_566 9_666 ? C16 C15 O2 77(4) 9_666 9_666 ? C16 C15 O2 77(4) 3_655 9_666 ? C16 C15 O2 77(4) . 9_666 ? C15 C16 C15 25(7) 9_666 . ? C15 C16 C16 46.4(8) 9_666 11_566 ? C15 C16 C16 46.4(8) . 11_566 ? C15 C16 C16 46.4(8) 9_666 3_655 ? C15 C16 C16 46.4(7) . 3_655 ? C16 C16 C16 90.000(11) 11_566 3_655 ? C18 O17 O18 0.0(15) 10_556 10_556 ? C18 O17 O18 40.2(14) 10_556 . ? O18 O17 O18 40.2(14) 10_556 . ? C18 O18 O18 0(3) 10_556 10_556 ? C18 O18 O17 69.9(7) 10_556 . ? O18 O18 O17 69.9(7) 10_556 . ? _diffrn_measured_fraction_theta_max 0.497 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.497 _refine_diff_density_max 0.756 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.075 #============================================================================== data_w12a _database_code_CSD 153092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H128 Br4 Mn2 O13 P8' _chemical_formula_weight 2395.45 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' 'P' 'P' 0.1023 0.0942 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.523(4) _cell_length_b 14.523(4) _cell_length_c 25.874(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5457(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 1.874 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.6032 _exptl_absorpt_correction_T_max 0.7056 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2750 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2750 _reflns_number_gt 1500 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] 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 0.00001(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2750 _refine_ls_number_parameters 180 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.40688(18) 0.0200(10) Uani 0.50 d SP . 2 Mn2 Mn 0.0000 0.0000 0.36574(19) 0.0230(11) Uani 0.50 d SP . 1 P1 P 0.22324(12) 0.06383(12) 0.39223(7) 0.0228(4) Uani 1 d . . . O1 O 0.1221(3) 0.0785(3) 0.38415(19) 0.0274(11) Uani 1 d . . . C1 C 0.2850(4) 0.1702(4) 0.3902(3) 0.0219(15) Uani 1 d . . . C2 C 0.2498(6) 0.2421(6) 0.3633(2) 0.0326(16) Uani 1 d . . . H2A H 0.1912 0.2371 0.3481 0.039 Uiso 1 calc R . . C3 C 0.3001(6) 0.3236(5) 0.3580(3) 0.046(2) Uani 1 d . . . H3A H 0.2747 0.3738 0.3400 0.055 Uiso 1 calc R . . C4 C 0.3850(5) 0.3304(5) 0.3787(3) 0.044(2) Uani 1 d . . . H4A H 0.4186 0.3853 0.3746 0.053 Uiso 1 calc R . . C5 C 0.4236(5) 0.2571(5) 0.4059(3) 0.044(2) Uani 1 d . . . H5A H 0.4830 0.2620 0.4202 0.053 Uiso 1 calc R . . C6 C 0.3730(5) 0.1773(5) 0.4117(3) 0.0341(19) Uani 1 d . . . H6A H 0.3979 0.1274 0.4301 0.041 Uiso 1 calc R . . C7 C 0.2745(5) -0.0056(5) 0.3426(3) 0.033(2) Uani 1 d . . . C8 C 0.3644(6) -0.0367(5) 0.3475(3) 0.051(3) Uani 1 d . . . H8A H 0.3989 -0.0229 0.3772 0.061 Uiso 1 calc R . . C9 C 0.4025(7) -0.0883(6) 0.3079(4) 0.065(3) Uani 1 d . . . H9A H 0.4629 -0.1108 0.3112 0.078 Uiso 1 calc R . . C10 C 0.3544(10) -0.1066(7) 0.2651(4) 0.084(4) Uani 1 d . . . H10A H 0.3818 -0.1419 0.2388 0.100 Uiso 1 calc R . . C11 C 0.2641(10) -0.0743(6) 0.2584(3) 0.078(4) Uani 1 d . . . H11A H 0.2309 -0.0874 0.2280 0.094 Uiso 1 calc R . . C12 C 0.2252(7) -0.0226(5) 0.2979(3) 0.052(2) Uani 1 d . . . H12A H 0.1653 0.0010 0.2942 0.062 Uiso 1 calc R . . C13 C 0.2484(5) 0.0080(5) 0.4516(2) 0.0240(15) Uani 1 d . . . H13A H 0.2096 -0.0469 0.4544 0.029 Uiso 1 calc R . . H13B H 0.3127 -0.0126 0.4508 0.029 Uiso 1 calc R . . C14 C 0.2341(7) 0.0674(6) 0.5000 0.022(2) Uani 1 d S . . H14A H 0.2780 0.1187 0.5000 0.026 Uiso 1 calc SR . . H14B H 0.1717 0.0931 0.5000 0.026 Uiso 1 calc SR . . Br1 Br 0.0000 0.0000 0.5000 0.0347(6) Uani 1 d S . . Br2A Br 0.0000 0.0000 0.26392(11) 0.0304(8) Uani 0.50 d SP . . Br3 Br 0.5000 0.0000 0.5000 0.0496(5) Uani 1 d S . . O2 O 0.5000 0.5000 0.435(2) 0.179(19) Uiso 0.50 d SPD . . C15 C 0.5000 0.5000 0.479(2) 0.102(19) Uiso 0.50 d SPD . . C16 C 0.443(4) 0.571(3) 0.5000 0.17(2) Uiso 0.50 d SPD . . O17 O 0.2260(10) 0.3340(9) 0.5000 0.102(5) Uani 0.50 d SP . . C17 C 0.2260(10) 0.3340(9) 0.5000 0.102(5) Uani 0.50 d SP . . O18 O 0.2099(11) 0.4226(9) 0.4867(10) 0.108(11) Uani 0.25 d P . . C18 C 0.2099(11) 0.4226(9) 0.4867(10) 0.108(11) Uani 0.25 d P . . 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 Mn1 0.0172(15) 0.0172(15) 0.026(3) 0.000 0.000 0.000 Mn2 0.0183(16) 0.0183(16) 0.032(3) 0.000 0.000 0.000 P1 0.0207(9) 0.0244(10) 0.0232(9) 0.0013(9) -0.0023(9) -0.0027(8) O1 0.023(2) 0.022(2) 0.037(3) 0.007(2) -0.008(3) -0.005(2) C1 0.021(3) 0.020(4) 0.025(4) 0.007(3) -0.001(3) -0.003(3) C2 0.027(4) 0.032(5) 0.039(4) 0.004(4) 0.000(4) -0.002(4) C3 0.040(5) 0.026(5) 0.072(6) 0.006(4) 0.001(5) -0.009(4) C4 0.034(5) 0.027(4) 0.072(6) -0.007(5) 0.013(5) -0.014(4) C5 0.035(5) 0.042(5) 0.055(6) 0.000(4) -0.002(4) -0.015(4) C6 0.026(4) 0.031(4) 0.046(5) 0.007(4) -0.003(4) -0.009(4) C7 0.038(5) 0.029(4) 0.031(4) 0.000(4) 0.010(4) -0.012(4) C8 0.061(6) 0.029(5) 0.062(6) -0.010(4) 0.035(5) -0.009(5) C9 0.088(8) 0.041(6) 0.067(7) -0.013(5) 0.045(6) -0.009(5) C10 0.150(12) 0.046(7) 0.056(8) -0.003(6) 0.042(8) -0.018(8) C11 0.173(12) 0.046(6) 0.016(5) 0.003(5) -0.001(7) -0.030(7) C12 0.084(7) 0.037(5) 0.035(5) 0.002(4) 0.003(5) -0.015(5) C13 0.017(3) 0.028(4) 0.027(3) 0.004(4) 0.004(4) 0.005(3) C14 0.025(6) 0.021(6) 0.019(5) 0.000 0.000 0.003(5) Br1 0.0328(9) 0.0328(9) 0.0385(14) 0.000 0.000 0.000 Br2A 0.0316(11) 0.0316(11) 0.0282(17) 0.000 0.000 0.000 Br3 0.0262(10) 0.0641(13) 0.0585(13) 0.000 0.000 0.0103(10) O17 0.116(12) 0.079(10) 0.111(11) 0.000 0.000 0.009(9) C17 0.116(12) 0.079(10) 0.111(11) 0.000 0.000 0.009(9) O18 0.113(12) 0.059(9) 0.15(3) 0.064(14) 0.099(18) 0.040(9) C18 0.113(12) 0.059(9) 0.15(3) 0.064(14) 0.099(18) 0.040(9) _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 Mn1 O1 2.189(4) 2 ? Mn1 O1 2.189(4) 4 ? Mn1 O1 2.189(4) . ? Mn1 O1 2.189(4) 3 ? Mn1 Br1 2.409(5) . ? Mn2 O1 2.162(4) 2 ? Mn2 O1 2.162(4) . ? Mn2 O1 2.162(4) 4 ? Mn2 O1 2.162(4) 3 ? Mn2 Br2A 2.634(6) . ? P1 O1 1.499(4) . ? P1 C13 1.774(6) . ? P1 C1 1.787(6) . ? P1 C7 1.794(8) . ? C1 C2 1.355(9) . ? C1 C6 1.397(9) . ? C2 C3 1.399(10) . ? C3 C4 1.347(10) . ? C4 C5 1.396(10) . ? C5 C6 1.381(9) . ? C7 C12 1.384(11) . ? C7 C8 1.387(10) . ? C8 C9 1.385(10) . ? C9 C10 1.337(14) . ? C10 C11 1.403(15) . ? C11 C12 1.389(12) . ? C13 C14 1.536(8) . ? C14 C13 1.536(8) 10_556 ? Br1 Mn1 2.409(5) 9_556 ? O2 C15 1.14(5) . ? C15 C15 1.09(10) 9_666 ? C15 C16 1.44(4) 3_655 ? C15 C16 1.44(4) 9_666 ? C15 C16 1.44(4) 11_566 ? C15 C16 1.44(4) . ? C16 C15 1.44(4) 9_666 ? C16 C16 1.88(6) 3_655 ? C16 C16 1.88(6) 11_566 ? O17 O18 1.351(17) . ? O17 C18 1.351(17) 10_556 ? O17 O18 1.351(17) 10_556 ? O18 C18 0.69(5) 10_556 ? O18 O18 0.69(5) 10_556 ? 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 Mn1 O1 85.86(9) 2 4 ? O1 Mn1 O1 148.8(3) 2 . ? O1 Mn1 O1 85.86(9) 4 . ? O1 Mn1 O1 85.86(9) 2 3 ? O1 Mn1 O1 148.8(3) 4 3 ? O1 Mn1 O1 85.86(9) . 3 ? O1 Mn1 Br1 105.58(17) 2 . ? O1 Mn1 Br1 105.58(17) 4 . ? O1 Mn1 Br1 105.58(17) . . ? O1 Mn1 Br1 105.58(17) 3 . ? O1 Mn2 O1 154.5(4) 2 . ? O1 Mn2 O1 87.22(8) 2 4 ? O1 Mn2 O1 87.22(8) . 4 ? O1 Mn2 O1 87.22(8) 2 3 ? O1 Mn2 O1 87.22(8) . 3 ? O1 Mn2 O1 154.5(4) 4 3 ? O1 Mn2 Br2A 102.73(18) 2 . ? O1 Mn2 Br2A 102.73(18) . . ? O1 Mn2 Br2A 102.73(18) 4 . ? O1 Mn2 Br2A 102.73(18) 3 . ? O1 P1 C13 112.8(3) . . ? O1 P1 C1 111.4(3) . . ? C13 P1 C1 108.5(3) . . ? O1 P1 C7 112.8(3) . . ? C13 P1 C7 106.1(3) . . ? C1 P1 C7 104.9(3) . . ? P1 O1 Mn2 139.4(3) . . ? P1 O1 Mn1 133.0(3) . . ? Mn2 O1 Mn1 28.31(14) . . ? C2 C1 C6 119.6(7) . . ? C2 C1 P1 119.4(6) . . ? C6 C1 P1 120.7(5) . . ? C1 C2 C3 120.3(8) . . ? C4 C3 C2 120.1(8) . . ? C3 C4 C5 120.8(7) . . ? C6 C5 C4 118.7(7) . . ? C5 C6 C1 120.4(7) . . ? C12 C7 C8 120.3(8) . . ? C12 C7 P1 119.0(7) . . ? C8 C7 P1 120.6(6) . . ? C9 C8 C7 119.1(9) . . ? C10 C9 C8 120.8(11) . . ? C9 C10 C11 121.7(11) . . ? C12 C11 C10 118.0(10) . . ? C7 C12 C11 120.1(10) . . ? C14 C13 P1 114.9(5) . . ? C13 C14 C13 109.4(7) 10_556 . ? Mn1 Br1 Mn1 180.0 9_556 . ? C15 C15 O2 180.000(14) 9_666 . ? C15 C15 C16 68(2) 9_666 3_655 ? O2 C15 C16 112(2) . 3_655 ? C15 C15 C16 68(2) 9_666 9_666 ? O2 C15 C16 112(2) . 9_666 ? C16 C15 C16 81.7(16) 3_655 9_666 ? C15 C15 C16 68(2) 9_666 11_566 ? O2 C15 C16 112(2) . 11_566 ? C16 C15 C16 135(5) 3_655 11_566 ? C16 C15 C16 81.7(16) 9_666 11_566 ? C15 C15 C16 68(2) 9_666 . ? O2 C15 C16 112(2) . . ? C16 C15 C16 81.7(16) 3_655 . ? C16 C15 C16 135(5) 9_666 . ? C16 C15 C16 81.7(16) 11_566 . ? C15 C16 C15 45(5) 9_666 . ? C15 C16 C16 49.2(8) 9_666 3_655 ? C15 C16 C16 49.2(8) . 3_655 ? C15 C16 C16 49.2(8) 9_666 11_566 ? C15 C16 C16 49.2(8) . 11_566 ? C16 C16 C16 90.000(8) 3_655 11_566 ? O18 O17 C18 30(2) . 10_556 ? O18 O17 O18 30(2) . 10_556 ? C18 O17 O18 0(2) 10_556 10_556 ? C18 O18 O18 0(4) 10_556 10_556 ? C18 O18 O17 75.2(11) 10_556 . ? O18 O18 O17 75.2(11) 10_556 . ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.582 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.106