# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1910 data_Mn4(PO4)2(C2O4)(H2O)2 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 23 14:58:08 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.273(3) _cell_length_b 6.524(4) _cell_length_c 10.080(4) _cell_angle_alpha 89 _cell_angle_beta 116.83(2) _cell_angle_gamma 89 _cell_volume 602.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 493.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.7 _cell_measurement_theta_max 25.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.940 _exptl_crystal_density_meas ? _chemical_formula_weight 533.74 _chemical_formula_analytical ? _chemical_formula_sum 'C2 H4 Mn4 O14 P2 ' _chemical_formula_moiety 'C2 H4 Mn4 O14 P2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 516.00 _exptl_absorpt_coefficient_mu 4.438 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.512 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 493.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 -2 3 0 0 2 0 2 _diffrn_reflns_number 1575 _reflns_number_total 1496 _reflns_number_observed 1240 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.84 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.08263 _diffrn_orient_matrix_UB_12 0.06687 _diffrn_orient_matrix_UB_13 0.08619 _diffrn_orient_matrix_UB_21 -0.02468 _diffrn_orient_matrix_UB_22 -0.08008 _diffrn_orient_matrix_UB_23 0.07021 _diffrn_orient_matrix_UB_31 0.06680 _diffrn_orient_matrix_UB_32 -0.11230 _diffrn_orient_matrix_UB_33 0.00126 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn 0 8 0.337 0.728 'International Tables' P 0 4 0.102 0.094 'International Tables' O 0 28 0.011 0.006 'International Tables' C 0 4 0.003 0.002 'International Tables' H 0 8 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Mn(1) -0.11618(7) -0.85343(9) 0.02692(6) 0.0082(2) Uij ? ? Mn(2) 0.23426(7) -0.97430(9) 0.73259(6) 0.0098(2) Uij ? ? P(1) 0.1012(1) -0.8487(1) 0.3946(1) 0.0061(2) Uij ? ? O(1) 0.3282(3) -1.0910(4) 0.9635(3) 0.0116(7) Uij ? ? O(2) -0.0781(3) -1.1738(4) 0.0139(3) 0.0086(7) Uij ? ? O(3) 0.1566(3) -1.0337(4) 0.5025(3) 0.0095(7) Uij ? ? O(4) 0.2119(3) -0.7030(4) 0.8375(3) 0.0087(7) Uij ? ? O(5) -0.0460(3) -0.9015(4) 0.2607(3) 0.0105(7) Uij ? ? O(6) -0.2779(3) -0.8571(4) -0.2167(3) 0.0126(8) Uij ? ? O(7) 0.4691(3) -0.9312(5) 0.8196(3) 0.0144(8) Uij ? ? C(2) 0.4598(4) -1.0468(6) 1.0425(4) 0.0098(10) Uij ? ? H(1) -0.368(6) -0.883(8) -0.222(6) 0.03(2) Uij ? ? H(2) -0.277(7) -0.935(10) -0.282(7) 0.06(2) Uij ? ? 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 Mn(1) 0.0097(3) 0.0056(3) 0.0108(3) 0.0004(2) 0.0058(3) 0.0009(2) Mn(2) 0.0083(3) 0.0122(3) 0.0095(3) -0.0011(2) 0.0046(3) -0.0019(2) P(1) 0.0072(5) 0.0044(5) 0.0074(5) 0.0004(4) 0.0039(4) 0.0002(3) O(1) 0.008(1) 0.016(1) 0.012(1) -0.001(1) 0.005(1) 0.001(1) O(2) 0.009(1) 0.006(1) 0.013(1) 0.001(1) 0.007(1) 0.001(1) O(3) 0.015(2) 0.004(1) 0.011(1) 0.000(1) 0.007(1) 0.002(1) O(4) 0.009(1) 0.008(1) 0.013(1) -0.001(1) 0.008(1) -0.002(1) O(5) 0.013(2) 0.010(1) 0.009(1) -0.002(1) 0.005(1) -0.002(1) O(6) 0.015(2) 0.012(2) 0.014(1) -0.002(1) 0.009(1) -0.001(1) O(7) 0.010(2) 0.022(2) 0.012(1) 0.000(1) 0.005(1) 0.001(1) C(2) 0.012(2) 0.006(2) 0.014(2) 0.003(2) 0.008(2) -0.001(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 19.18131 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1240 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0314 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0350 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.375 _refine_ls_shift/esd_max 0.2229 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.64 _refine_diff_density_max 0.62 #------------------------------------------------------------------------------ _geom_special_details ? 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 Mn(1) O(1) 2.253(3) ? ? yes Mn(1) O(2) 2.141(3) ? ? yes Mn(1) O(2) 2.219(3) ? ? yes Mn(1) O(3) 2.121(3) ? ? yes Mn(1) O(5) 2.153(3) ? ? yes Mn(1) O(6) 2.260(3) ? ? yes Mn(2) O(1) 2.214(3) ? ? yes Mn(2) O(3) 2.120(3) ? ? yes Mn(2) O(4) 2.127(3) ? ? yes Mn(2) O(5) 2.126(3) ? ? yes Mn(2) O(7) 2.181(3) ? ? yes P(1) O(2) 1.552(3) ? ? yes P(1) O(3) 1.551(3) ? ? yes P(1) O(4) 1.526(3) ? ? yes P(1) O(5) 1.544(3) ? ? yes O(1) C(2) 1.254(5) ? ? yes O(7) C(2) 1.253(5) ? ? yes C(2) C(2) 1.560(7) ? ? yes #------------------------------------------------------------------------------ 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 O(1) Mn(1) O(2) 93.0(1) ? ? ? yes O(1) Mn(1) O(2) 171.3(1) ? ? ? yes O(1) Mn(1) O(3) 91.9(1) ? ? ? yes O(1) Mn(1) O(5) 77.4(1) ? ? ? yes O(1) Mn(1) O(6) 78.1(1) ? ? ? yes O(2) Mn(1) O(2) 82.1(1) ? ? ? yes O(2) Mn(1) O(3) 168.8(1) ? ? ? yes O(2) Mn(1) O(5) 86.83(10) ? ? ? yes O(2) Mn(1) O(6) 89.3(1) ? ? ? yes O(2) Mn(1) O(3) 91.8(1) ? ? ? yes O(2) Mn(1) O(5) 109.3(1) ? ? ? yes O(2) Mn(1) O(6) 94.7(1) ? ? ? yes O(3) Mn(1) O(5) 104.1(1) ? ? ? yes O(3) Mn(1) O(6) 81.8(1) ? ? ? yes O(5) Mn(1) O(6) 155.0(1) ? ? ? yes O(1) Mn(2) O(3) 149.0(1) ? ? ? yes O(1) Mn(2) O(4) 81.8(1) ? ? ? yes O(1) Mn(2) O(5) 78.8(1) ? ? ? yes O(1) Mn(2) O(7) 75.1(1) ? ? ? yes O(3) Mn(2) O(4) 128.6(1) ? ? ? yes O(3) Mn(2) O(5) 93.8(1) ? ? ? yes O(3) Mn(2) O(7) 105.4(1) ? ? ? yes O(4) Mn(2) O(5) 89.8(1) ? ? ? yes O(4) Mn(2) O(7) 92.4(1) ? ? ? yes O(5) Mn(2) O(7) 153.3(1) ? ? ? yes O(2) P(1) O(3) 105.1(1) ? ? ? yes O(2) P(1) O(4) 113.7(2) ? ? ? yes O(2) P(1) O(5) 109.4(2) ? ? ? yes O(3) P(1) O(4) 109.7(2) ? ? ? yes O(3) P(1) O(5) 110.1(2) ? ? ? yes O(4) P(1) O(5) 108.8(1) ? ? ? yes Mn(1) O(1) Mn(2) 97.4(1) ? ? ? yes Mn(1) O(1) C(2) 142.7(2) ? ? ? yes Mn(2) O(1) C(2) 115.0(2) ? ? ? yes Mn(1) O(2) Mn(1) 97.9(1) ? ? ? yes Mn(1) O(2) P(1) 126.9(1) ? ? ? yes Mn(1) O(2) P(1) 124.1(2) ? ? ? yes Mn(1) O(3) Mn(2) 106.6(1) ? ? ? yes Mn(1) O(3) P(1) 132.9(2) ? ? ? yes Mn(2) O(3) P(1) 117.6(1) ? ? ? yes Mn(2) O(4) P(1) 129.6(2) ? ? ? yes Mn(1) O(5) Mn(2) 103.3(1) ? ? ? yes Mn(1) O(5) P(1) 129.5(2) ? ? ? yes Mn(2) O(5) P(1) 127.1(1) ? ? ? yes Mn(2) O(7) C(2) 114.6(2) ? ? ? yes O(1) C(2) O(7) 126.9(4) ? ? ? yes O(1) C(2) C(2) 115.3(4) ? ? ? yes O(7) C(2) C(2) 117.8(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr Philip Lightfoot School of Chemistry University of St Andrews Purdie Building North Haugh St Andrews Fife KY16 9ST UK pl@st-andrews.ac.uk 01334 463841 ; #===END data_Mn2(HPO4)2(C2O4)(H3N(CH2)3NH3)(H2O) #------------------------------------------------------------------------------ _audit_creation_date 'Wed Nov 24 17:05:05 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 5.474(2) _cell_length_b 15.737(2) _cell_length_c 9.056(2) _cell_angle_alpha 90 _cell_angle_beta 93.47(3) _cell_angle_gamma 90 _cell_volume 778.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 493.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 18.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.141 _exptl_crystal_density_meas ? _chemical_formula_weight 502.03 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H18 N2 Mn2 O14 P2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 508.00 _exptl_absorpt_coefficient_mu 1.906 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 493.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.14 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 2 1 -2 2 2 1 0 _diffrn_reflns_number 1592 _reflns_number_total 1439 _reflns_number_observed 1094 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.64 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.11171 _diffrn_orient_matrix_UB_12 -0.04621 _diffrn_orient_matrix_UB_13 -0.03058 _diffrn_orient_matrix_UB_21 0.10442 _diffrn_orient_matrix_UB_22 0.04312 _diffrn_orient_matrix_UB_23 -0.04726 _diffrn_orient_matrix_UB_31 0.10055 _diffrn_orient_matrix_UB_32 0.00656 _diffrn_orient_matrix_UB_33 0.09524 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn 0 4 0.337 0.728 'International Tables' P 0 4 0.102 0.094 'International Tables' O 0 28 0.011 0.006 'International Tables' C 0 10 0.003 0.002 'International Tables' N 0 4 0.006 0.003 'International Tables' H 0 36 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Mn(1) 0.3216(1) 0.17405(5) 1.01095(8) 0.0175(2) Uij 1 ? P(1) -0.1547(2) 0.17836(9) 1.2432(1) 0.0173(4) Uij 1 ? O(1) 0.0439(8) 0.1468(3) 0.8203(5) 0.028(1) Uij 1 ? O(2) 0.2546(6) 0.0416(2) 1.0890(4) 0.025(1) Uij 1 ? O(3) 0.4084(6) -0.0899(2) 1.0954(4) 0.023(1) Uij 1 ? O(4) -0.1357(7) 0.0775(2) 1.2469(5) 0.027(1) Uij 1 ? O(5) 0.0366(6) 0.2127(2) 1.1452(4) 0.028(1) Uij 1 ? O(6) -0.4144(6) 0.2004(2) 1.1871(4) 0.026(1) Uij 1 ? O(7) -0.1144(7) 0.2081(2) 1.4030(4) 0.028(1) Uij 1 ? N(1) 0.851(2) 0.3455(6) 0.977(1) 0.021(2) Uij 0.5 ? N(2) 0.815(2) 0.3674(7) 1.045(1) 0.042(3) Uij 0.5 ? C(1) 0.4019(9) -0.0145(3) 1.0539(6) 0.019(1) Uij 1 ? C(2) 0.861(2) 0.4440(8) 0.960(1) 0.039(3) Uij 0.5 ? C(3) 1.0000 0.5000 1.0000 0.090(4) Uij 1 ? C(4) 0.953(3) 0.4178(10) 1.055(2) 0.055(4) Uij 0.5 ? H(1) 0.04(1) 0.198(5) 0.762(9) 0.10(2) Uij 1 ? H(2) -0.06(1) 0.131(5) 0.849(8) 0.06(2) Uij 1 ? H(3) -0.02(1) 0.053(5) 1.224(8) 0.08(2) Uij 1 ? H(4) 0.8492 0.4535 0.8572 0.0507 Uij 0.5 ? H(5) 0.7161 0.4630 1.0027 0.0507 Uij 0.5 ? H(6) 1.1548 0.4726 1.0017 0.0507 Uij 0.25 ? H(7) 0.9580 0.5109 1.0985 0.0507 Uij 0.25 ? H(8) 0.8452 0.5274 0.9983 0.0507 Uij 0.25 ? H(9) 1.0419 0.4891 0.9015 0.0507 Uij 0.25 ? H(10) 1.0957 0.3894 1.0331 0.0507 Uij 0.5 ? H(11) 0.9497 0.4295 1.1571 0.0507 Uij 0.5 ? H(12) 0.9853 0.3205 0.9311 0.0507 Uij 0.5 ? H(13) 0.7019 0.3254 0.9267 0.0507 Uij 0.5 ? H(14) 0.8086 0.3448 0.9462 0.0507 Uij 0.5 ? H(15) 0.6624 0.3850 1.0701 0.0507 Uij 0.5 ? H(16) 0.8722 0.3213 1.1104 0.0507 Uij 0.5 ? H(17) 0.8532 0.3299 1.0770 0.0507 Uij 0.5 ? 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 Mn(1) 0.0156(4) 0.0186(4) 0.0185(4) -0.0002(4) 0.0028(3) 0.0001(4) P(1) 0.0151(7) 0.0189(7) 0.0180(7) 0.0025(6) 0.0019(6) -0.0015(6) O(1) 0.022(2) 0.032(3) 0.031(2) -0.008(2) 0.000(2) 0.007(2) O(2) 0.023(2) 0.021(2) 0.031(2) 0.002(2) 0.013(2) -0.001(2) O(3) 0.022(2) 0.014(2) 0.032(2) 0.001(2) 0.010(2) 0.001(2) O(4) 0.028(2) 0.019(2) 0.035(2) 0.003(2) 0.013(2) 0.000(2) O(5) 0.024(2) 0.022(2) 0.041(2) 0.003(2) 0.015(2) 0.002(2) O(6) 0.016(2) 0.031(2) 0.030(2) 0.005(2) -0.004(2) -0.008(2) O(7) 0.035(2) 0.027(2) 0.021(2) 0.010(2) -0.005(2) -0.007(2) C(1) 0.013(3) 0.022(3) 0.021(3) -0.003(2) 0.003(2) -0.004(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1094 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0408 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0388 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.670 _refine_ls_shift/esd_max 0.0180 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.85 _refine_diff_density_max 1.41 #------------------------------------------------------------------------------ _geom_special_details ? 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 Mn(1) O(1) 2.271(4) ? ? yes Mn(1) O(2) 2.238(4) ? ? yes Mn(1) O(3) 2.245(3) ? ? yes Mn(1) O(5) 2.124(3) ? ? yes Mn(1) O(6) 2.128(4) ? ? yes Mn(1) O(7) 2.135(4) ? ? yes P(1) O(4) 1.591(4) ? ? yes P(1) O(5) 1.513(4) ? ? yes P(1) O(6) 1.520(4) ? ? yes P(1) O(7) 1.524(4) ? ? yes O(2) C(1) 1.250(6) ? ? yes O(3) C(1) 1.244(6) ? ? yes N(1) N(2) 0.75(1) ? ? yes N(1) C(2) 1.56(2) ? ? yes N(1) C(4) 1.44(2) ? ? yes N(2) C(2) 1.46(2) ? ? yes N(2) C(4) 1.09(2) ? ? yes C(1) C(1) 1.562(9) ? ? yes C(2) C(3) 1.21(1) ? ? yes C(2) C(4) 1.06(2) ? ? yes C(3) C(4) 1.42(2) ? ? yes C(3) C(4) 1.42(2) ? ? yes #------------------------------------------------------------------------------ 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 O(1) Mn(1) O(2) 87.1(2) ? ? ? yes O(1) Mn(1) O(3) 89.4(2) ? ? ? yes O(1) Mn(1) O(5) 90.5(2) ? ? ? yes O(1) Mn(1) O(6) 179.1(1) ? ? ? yes O(1) Mn(1) O(7) 86.4(2) ? ? ? yes O(2) Mn(1) O(3) 73.2(1) ? ? ? yes O(2) Mn(1) O(5) 86.9(1) ? ? ? yes O(2) Mn(1) O(6) 93.5(1) ? ? ? yes O(2) Mn(1) O(7) 171.1(1) ? ? ? yes O(3) Mn(1) O(5) 160.0(1) ? ? ? yes O(3) Mn(1) O(6) 90.1(1) ? ? ? yes O(3) Mn(1) O(7) 100.7(1) ? ? ? yes O(5) Mn(1) O(6) 90.2(1) ? ? ? yes O(5) Mn(1) O(7) 99.2(1) ? ? ? yes O(6) Mn(1) O(7) 92.9(1) ? ? ? yes O(4) P(1) O(5) 108.8(2) ? ? ? yes O(4) P(1) O(6) 107.1(2) ? ? ? yes O(4) P(1) O(7) 106.3(2) ? ? ? yes O(5) P(1) O(6) 112.9(2) ? ? ? yes O(5) P(1) O(7) 112.4(2) ? ? ? yes O(6) P(1) O(7) 109.0(2) ? ? ? yes Mn(1) O(2) C(1) 117.2(3) ? ? ? yes Mn(1) O(3) C(1) 116.2(3) ? ? ? yes Mn(1) O(5) P(1) 142.4(2) ? ? ? yes Mn(1) O(6) P(1) 141.7(2) ? ? ? yes Mn(1) O(7) P(1) 133.1(2) ? ? ? yes N(2) N(1) C(2) 68(1) ? ? ? yes N(2) N(1) C(4) 48(1) ? ? ? yes C(2) N(1) C(4) 41.1(7) ? ? ? yes N(1) N(2) C(2) 82(1) ? ? ? yes N(1) N(2) C(4) 100(1) ? ? ? yes C(2) N(2) C(4) 46(1) ? ? ? yes O(2) C(1) O(3) 127.2(4) ? ? ? yes O(2) C(1) C(1) 115.6(6) ? ? ? yes O(3) C(1) C(1) 117.3(6) ? ? ? yes N(1) C(2) N(2) 28.5(5) ? ? ? yes N(1) C(2) C(3) 136(1) ? ? ? yes N(1) C(2) C(4) 63(1) ? ? ? yes N(2) C(2) C(3) 124(1) ? ? ? yes N(2) C(2) C(4) 48(1) ? ? ? yes C(3) C(2) C(4) 77(1) ? ? ? yes C(2) C(3) C(2) 180.0 ? ? ? yes C(2) C(3) C(4) 46.7(8) ? ? ? yes C(2) C(3) C(4) 133.3(8) ? ? ? yes C(2) C(3) C(4) 133.3(8) ? ? ? yes C(2) C(3) C(4) 46.7(8) ? ? ? yes C(4) C(3) C(4) 180.0 ? ? ? yes N(1) C(4) N(2) 30.8(8) ? ? ? yes N(1) C(4) C(2) 75(1) ? ? ? yes N(1) C(4) C(3) 128(1) ? ? ? yes N(2) C(4) C(2) 85(1) ? ? ? yes N(2) C(4) C(3) 140(1) ? ? ? yes C(2) C(4) C(3) 56(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr Philip Lightfoot School of Chemistry University of St Andrews Purdie Building North Haugh St Andrews Fife KY16 9ST UK pl@st-andrews.ac.uk 01334 463841 ;