Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Content-Length: 39868 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 989 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Zoe A D Lethbridge' 'Satish K Tiwary' 'Andrew Harrison' 'Philip Lightfoot' _publ_contact_author ; Dr Philip Lightfoot School of Chemistry University of St Andrews North Haugh St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_name 'Zoe A D Lethbridge' _publ_contact_author_email zadl@st-andrews.ac.uk data_[Mn2(HPO4)2(C2O4)(H2O)2](H3NC6H10NH3)_(1) _database_code_CSD 157825 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jul 1 16:06:10 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 5.9778(3) _cell_length_b 16.6747(8) _cell_length_c 8.4660(4) _cell_angle_alpha 90 _cell_angle_beta 90.384(1) _cell_angle_gamma 90 _cell_volume 843.85(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_meas ? _chemical_formula_weight 271.05 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H11 N Mn O7 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 552.00 _exptl_absorpt_coefficient_mu 1.767 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _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 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3727 _reflns_number_total 1272 _reflns_number_observed 883 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.90 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.29 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 16 0.003 0.002 'International Tables' N 0 4 0.006 0.003 'International Tables' H 0 44 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) 0.5153(1) 0.17646(4) 0.50446(10) 0.0171(2) Uij ? ? P(1) 1.0071(2) 0.24515(8) 0.3775(2) 0.0160(3) Uij ? ? O(1) 0.5287(7) 0.1610(3) 0.2400(5) 0.029(1) Uij ? ? O(2) 0.8234(6) 0.2440(2) 0.5008(4) 0.0216(10) Uij ? ? O(3) 0.7237(6) 0.0649(2) 0.5382(4) 0.024(1) Uij ? ? O(4) 0.7193(6) -0.0691(2) 0.5150(4) 0.023(1) Uij ? ? O(5) 1.0048(6) 0.1605(2) 0.2874(5) 0.024(1) Uij ? ? O(6) 1.2373(5) 0.2557(2) 0.4507(4) 0.0208(10) Uij ? ? O(7) 0.9585(6) 0.3068(2) 0.2502(4) 0.0209(10) Uij ? ? N(1) 1.0100(8) 0.1310(3) -0.2194(5) 0.022(1) Uij ? ? C(1) 1.0223(8) 0.0769(3) -0.0788(6) 0.018(1) Uij ? ? C(2) 0.8028(9) -0.0124(3) 0.1009(6) 0.024(2) Uij ? ? C(3) 0.7947(9) 0.0414(4) -0.0456(7) 0.026(2) Uij ? ? C(4) 0.6288(8) -0.0010(4) 0.5160(5) 0.019(1) Uij ? ? H(1) 0.44(1) 0.187(3) 0.175(7) 0.04(1) Uij ? ? H(2) 0.65(1) 0.167(4) 0.203(7) 0.04(1) Uij ? ? H(3) 1.04(1) 0.127(4) 0.333(7) 0.03(2) Uij ? ? H(4) 1.149(8) 0.152(3) -0.242(5) 0.01(1) Uij ? ? H(5) 0.95(1) 0.100(4) -0.301(7) 0.05(2) Uij ? ? H(6) 0.89(1) 0.180(4) -0.194(7) 0.05(1) Uij ? ? H(7) 1.076(7) 0.111(3) 0.015(5) 0.01(1) Uij ? ? H(8) 0.744(9) 0.013(3) -0.133(7) 0.03(1) Uij ? ? H(9) 0.689(8) 0.084(3) -0.035(5) 0.01(1) Uij ? ? H(10) 0.848(9) 0.019(3) 0.193(6) 0.02(1) Uij ? ? H(11) 0.663(9) -0.035(3) 0.128(6) 0.03(1) 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) 0.0173(4) 0.0180(4) 0.0160(4) 0.0002(4) -0.0003(3) 0.0001(4) P(1) 0.0162(7) 0.0170(7) 0.0148(7) 0.0001(6) -0.0008(5) 0.0002(6) O(1) 0.020(2) 0.045(3) 0.022(2) 0.003(2) 0.004(2) 0.002(2) O(2) 0.024(2) 0.021(2) 0.020(2) -0.005(2) 0.002(2) -0.002(2) O(3) 0.021(2) 0.016(2) 0.034(2) -0.001(2) -0.002(2) -0.004(2) O(4) 0.020(2) 0.017(2) 0.032(2) 0.002(2) -0.001(2) -0.001(2) O(5) 0.026(2) 0.023(2) 0.023(2) 0.002(2) -0.003(2) -0.004(2) O(6) 0.019(2) 0.019(2) 0.025(2) 0.001(2) -0.006(2) -0.003(2) O(7) 0.023(2) 0.024(2) 0.016(2) 0.003(2) 0.000(2) 0.000(2) N(1) 0.020(3) 0.024(3) 0.021(3) -0.003(2) 0.000(2) 0.004(2) C(1) 0.020(3) 0.021(3) 0.013(3) 0.000(2) -0.004(2) 0.001(2) C(2) 0.018(3) 0.029(3) 0.026(3) -0.003(2) 0.003(2) 0.004(3) C(3) 0.021(3) 0.026(3) 0.030(3) 0.006(3) -0.002(3) 0.000(3) C(4) 0.020(3) 0.022(3) 0.015(3) 0.001(3) -0.001(2) -0.001(2) #------------------------------------------------------------------------------ _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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 883 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0333 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.408 _refine_ls_shift/esd_max 0.8110 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.35 _refine_diff_density_max 0.34 #------------------------------------------------------------------------------ _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) 2.256(4) ? ? yes Mn(1) O(2) 2.159(3) ? ? yes Mn(1) O(3) 2.256(4) ? ? yes Mn(1) O(4) 2.279(4) ? ? yes Mn(1) O(6) 2.169(3) ? ? yes Mn(1) O(7) 2.128(3) ? ? yes P(1) O(2) 1.520(4) ? ? yes P(1) O(5) 1.605(4) ? ? yes P(1) O(6) 1.516(3) ? ? yes P(1) O(7) 1.516(4) ? ? yes O(3) C(4) 1.250(7) ? ? yes O(4) C(4) 1.258(7) ? ? yes N(1) C(1) 1.495(7) ? ? yes C(1) C(2) 1.512(7) ? ? yes C(1) C(3) 1.511(7) ? ? yes C(2) C(3) 1.532(8) ? ? yes C(4) C(4) 1.562(9) ? ? 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) 90.5(1) ? ? ? yes O(1) Mn(1) O(3) 90.5(1) ? ? ? yes O(1) Mn(1) O(4) 82.2(1) ? ? ? yes O(1) Mn(1) O(6) 83.9(1) ? ? ? yes O(1) Mn(1) O(7) 172.8(1) ? ? ? yes O(2) Mn(1) O(3) 87.8(1) ? ? ? yes O(2) Mn(1) O(4) 158.9(1) ? ? ? yes O(2) Mn(1) O(6) 109.4(1) ? ? ? yes O(2) Mn(1) O(7) 95.0(1) ? ? ? yes O(3) Mn(1) O(4) 72.6(1) ? ? ? yes O(3) Mn(1) O(6) 161.9(1) ? ? ? yes O(3) Mn(1) O(7) 94.3(1) ? ? ? yes O(4) Mn(1) O(6) 89.6(1) ? ? ? yes O(4) Mn(1) O(7) 94.1(1) ? ? ? yes O(6) Mn(1) O(7) 89.9(1) ? ? ? yes O(2) P(1) O(5) 108.2(2) ? ? ? yes O(2) P(1) O(6) 112.3(2) ? ? ? yes O(2) P(1) O(7) 111.2(2) ? ? ? yes O(5) P(1) O(6) 107.5(2) ? ? ? yes O(5) P(1) O(7) 104.9(2) ? ? ? yes O(6) P(1) O(7) 112.4(2) ? ? ? yes Mn(1) O(2) P(1) 129.5(2) ? ? ? yes Mn(1) O(3) C(4) 117.1(3) ? ? ? yes Mn(1) O(4) C(4) 116.4(3) ? ? ? yes Mn(1) O(6) P(1) 135.1(2) ? ? ? yes Mn(1) O(7) P(1) 138.8(2) ? ? ? yes N(1) C(1) C(2) 111.2(4) ? ? ? yes N(1) C(1) C(3) 110.2(4) ? ? ? yes C(2) C(1) C(3) 111.7(4) ? ? ? yes C(1) C(2) C(3) 109.6(4) ? ? ? yes C(1) C(3) C(2) 110.9(4) ? ? ? yes O(3) C(4) O(4) 126.9(4) ? ? ? yes O(3) C(4) C(4) 117.0(6) ? ? ? yes O(4) C(4) C(4) 116.2(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_[Mn2(HPO4)2(C2O4)(H2O)2](H3N(CH2)2NH3)_(2) _database_code_CSD 157826 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Dec 6 16:01:00 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 5.4573(4) _cell_length_b 8.9650(7) _cell_length_c 15.253(1) _cell_angle_alpha 90 _cell_angle_beta 98.924(1) _cell_angle_gamma 90 _cell_volume 737.22(8) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_meas ? _chemical_formula_weight 488.00 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H16 N2 Mn2 O14 P2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 492.00 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _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 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3230 _reflns_number_total 1136 _reflns_number_observed 808 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.35 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.26 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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' H 0 32 0.000 0.000 'International Tables' C 0 8 0.003 0.002 'International Tables' N 0 4 0.006 0.003 '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) 0.1010(1) 0.48380(6) 0.81816(4) 0.0173(2) Uij ? ? P(1) -0.3903(2) 0.2596(1) 0.81943(7) 0.0155(3) Uij ? ? O(1) -0.2249(5) 0.6014(3) 1.0434(2) 0.0232(8) Uij ? ? O(2) -0.1476(5) 0.3016(3) 0.7899(2) 0.0209(7) Uij ? ? O(3) -0.0463(5) 0.5956(3) 0.6988(2) 0.0218(8) Uij ? ? O(4) 0.3711(6) 0.6762(4) 0.8505(2) 0.0292(10) Uij ? ? O(5) -0.1248(5) 0.6057(3) 0.9073(2) 0.0199(8) Uij ? ? O(6) 0.3975(5) 0.3602(3) 0.7795(2) 0.0211(8) Uij ? ? O(7) -0.3452(8) 0.2784(5) 0.9252(3) 0.0241(9) Uij ? ? N(1) -0.0578(8) 0.9267(4) 0.8829(2) 0.024(1) Uij ? ? C(1) -0.1010(7) 0.5598(4) 0.9858(3) 0.016(1) Uij ? ? C(2) 0.0765(8) 1.0043(5) 0.9623(3) 0.026(1) Uij ? ? H(1) 0.37(1) 0.720(7) 0.810(4) 0.08(2) Uij ? ? H(2) 0.51(1) 0.646(7) 0.871(4) 0.07(2) Uij ? ? H(3) 0.032(8) 0.924(4) 0.837(3) 0.03(1) Uij ? ? H(4) -0.10(1) 0.824(7) 0.898(4) 0.08(2) Uij ? ? H(5) 0.231(7) 0.955(4) 0.979(2) 0.014(9) Uij ? ? H(7) 0.082(8) 1.105(5) 0.947(3) 0.03(1) Uij ? ? H(8) -0.195(9) 0.978(5) 0.859(3) 0.04(1) Uij ? ? H(9) -0.46(2) 0.29(1) 0.933(6) 0.10(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) 0.0169(3) 0.0177(4) 0.0171(3) 0.0024(3) 0.0022(2) -0.0003(3) P(1) 0.0163(5) 0.0144(6) 0.0156(5) 0.0004(4) 0.0015(4) -0.0008(4) O(1) 0.023(2) 0.029(2) 0.018(2) 0.008(1) 0.004(1) 0.000(1) O(2) 0.020(1) 0.022(2) 0.021(1) -0.003(1) 0.005(1) -0.004(1) O(3) 0.028(2) 0.013(1) 0.023(2) 0.002(1) -0.001(1) 0.003(1) O(4) 0.023(2) 0.028(2) 0.033(2) -0.001(1) -0.005(1) 0.007(2) O(5) 0.022(1) 0.022(2) 0.015(2) 0.003(1) 0.003(1) 0.003(1) O(6) 0.022(2) 0.020(2) 0.022(2) 0.007(1) 0.004(1) 0.001(1) O(7) 0.022(2) 0.031(2) 0.019(2) 0.001(2) 0.000(1) 0.000(1) N(1) 0.030(2) 0.023(2) 0.017(2) 0.005(2) 0.001(2) -0.003(2) C(1) 0.014(2) 0.016(2) 0.018(2) -0.004(2) 0.003(2) -0.004(2) C(2) 0.027(3) 0.026(3) 0.023(2) 0.004(2) 0.000(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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 808 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0239 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0270 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.334 _refine_ls_shift/esd_max 5.1720 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.37 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ _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) 2.249(3) ? ? yes Mn(1) O(2) 2.125(3) ? ? yes Mn(1) O(3) 2.123(3) ? ? yes Mn(1) O(4) 2.273(3) ? ? yes Mn(1) O(5) 2.254(3) ? ? yes Mn(1) O(6) 2.119(3) ? ? yes P(1) O(2) 1.511(3) ? ? yes P(1) O(3) 1.526(3) ? ? yes P(1) O(6) 1.519(3) ? ? yes P(1) O(7) 1.602(4) ? ? yes O(1) C(1) 1.246(4) ? ? yes O(5) C(1) 1.254(4) ? ? yes N(1) C(2) 1.487(5) ? ? yes C(1) C(1) 1.551(7) ? ? yes C(2) C(2) 1.525(8) ? ? 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) 91.1(1) ? ? ? yes O(1) Mn(1) O(3) 169.71(10) ? ? ? yes O(1) Mn(1) O(4) 87.9(1) ? ? ? yes O(1) Mn(1) O(5) 73.23(9) ? ? ? yes O(1) Mn(1) O(6) 87.2(1) ? ? ? yes O(2) Mn(1) O(3) 92.5(1) ? ? ? yes O(2) Mn(1) O(4) 178.9(1) ? ? ? yes O(2) Mn(1) O(5) 95.93(10) ? ? ? yes O(2) Mn(1) O(6) 91.89(10) ? ? ? yes O(3) Mn(1) O(4) 88.5(1) ? ? ? yes O(3) Mn(1) O(5) 96.80(10) ? ? ? yes O(3) Mn(1) O(6) 102.3(1) ? ? ? yes O(4) Mn(1) O(5) 84.1(1) ? ? ? yes O(4) Mn(1) O(6) 87.7(1) ? ? ? yes O(5) Mn(1) O(6) 159.04(10) ? ? ? yes O(2) P(1) O(3) 111.7(2) ? ? ? yes O(2) P(1) O(6) 112.4(2) ? ? ? yes O(2) P(1) O(7) 105.6(2) ? ? ? yes O(3) P(1) O(6) 111.2(2) ? ? ? yes O(3) P(1) O(7) 106.3(2) ? ? ? yes O(6) P(1) O(7) 109.2(2) ? ? ? yes Mn(1) O(1) C(1) 116.3(2) ? ? ? yes Mn(1) O(2) P(1) 133.9(2) ? ? ? yes Mn(1) O(3) P(1) 131.0(2) ? ? ? yes Mn(1) O(5) C(1) 115.6(2) ? ? ? yes Mn(1) O(6) P(1) 140.1(2) ? ? ? yes O(1) C(1) O(5) 126.1(3) ? ? ? yes O(1) C(1) C(1) 116.8(4) ? ? ? yes O(5) C(1) C(1) 117.2(4) ? ? ? yes N(1) C(2) C(2) 109.4(5) ? ? ? yes #------------------------------------------------------------------------------ _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_[Mn4(HPO4)2(C2O4)3(H2O)2](H3N(CH2)2NH3)(H2O)2_(3) _database_code_CSD 157827 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Dec 14 17:31:59 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 7.830(4) _cell_length_b 8.041(4) _cell_length_c 9.652(7) _cell_angle_alpha 76.29(5) _cell_angle_beta 78.47(6) _cell_angle_gamma 86.36(6) _cell_volume 578.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_meas ? _chemical_formula_weight 401.95 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H7 N Mn2 O12 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 398.00 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _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 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 2923 _reflns_number_total 1637 _reflns_number_observed 1343 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.87 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.26 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 2 0.102 0.094 'International Tables' C 0 8 0.003 0.002 'International Tables' O 0 24 0.011 0.006 'International Tables' N 0 2 0.006 0.003 'International Tables' H 0 14 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) 1.19076(9) -0.68967(9) 0.61460(8) 0.0203(2) Uij ? ? Mn(2) 0.84283(9) -0.96611(9) 0.74818(8) 0.0173(2) Uij ? ? P(1) 1.0778(2) -0.2671(2) 0.5903(1) 0.0161(3) Uij ? ? O(1) 1.4157(4) -0.6399(4) 0.7039(4) 0.026(1) Uij ? ? O(2) 1.3444(4) -0.9384(4) 0.6493(4) 0.027(1) Uij ? ? O(3) 1.0311(4) -0.8415(4) 0.8382(3) 0.0215(9) Uij ? ? O(4) 1.0744(4) -0.4595(4) 0.6350(4) 0.0235(10) Uij ? ? O(5) 1.3454(5) -0.6416(6) 0.3914(5) 0.031(1) Uij ? ? O(6) 0.8138(4) -1.0985(4) 0.9836(4) 0.0256(10) Uij ? ? O(7) 0.5904(4) -1.0531(4) 0.7169(4) 0.0245(10) Uij ? ? O(8) 1.6538(4) -0.7610(4) 0.7830(4) 0.027(1) Uij ? ? O(9) 1.2748(4) -0.2141(5) 0.5650(4) 0.027(1) Uij ? ? O(10) 0.9717(4) -0.1893(4) 0.7099(3) 0.0210(9) Uij ? ? O(11) 1.0166(4) -0.1985(4) 0.4458(3) 0.0204(9) Uij ? ? O(12) 0.5254(10) -0.675(1) 1.0501(9) 0.129(3) Uij ? ? N(1) 0.8169(6) -0.4842(7) 0.8976(5) 0.044(2) Uij ? ? C(1) 1.5196(6) -0.7620(6) 0.7308(5) 0.021(1) Uij ? ? C(2) 1.4817(6) -0.9330(6) 0.6951(5) 0.020(1) Uij ? ? C(3) 1.0639(6) -0.9265(6) 0.9589(5) 0.019(1) Uij ? ? C(4) 0.9043(8) -0.5198(8) 1.0242(6) 0.035(2) Uij ? ? H(1) 1.413(9) -0.585(9) 0.367(8) 0.05(2) Uij ? ? H(2) 1.381(8) -0.735(8) 0.364(7) 0.04(2) Uij ? ? H(3) 0.8585 -0.3806 0.8326 0.0552 Uij ? ? H(4) 0.6956 -0.4787 0.9275 0.0552 Uij ? ? H(5) 0.8460 -0.5759 0.8470 0.0552 Uij ? ? H(6) 0.845(6) -0.460(6) 1.086(6) 0.02(1) Uij ? ? H(7) 0.888(7) -0.647(7) 1.076(6) 0.04(1) Uij ? ? H(8) 1.284(7) -0.126(7) 0.585(6) 0.02(1) 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) 0.0183(4) 0.0170(4) 0.0275(5) 0.0018(3) -0.0084(3) -0.0060(3) Mn(2) 0.0172(4) 0.0175(4) 0.0180(4) 0.0016(3) -0.0057(3) -0.0040(3) P(1) 0.0160(6) 0.0155(6) 0.0177(7) 0.0009(5) -0.0054(5) -0.0039(5) O(1) 0.021(2) 0.020(2) 0.043(2) 0.005(2) -0.015(2) -0.011(2) O(2) 0.022(2) 0.024(2) 0.041(2) 0.002(2) -0.014(2) -0.012(2) O(3) 0.024(2) 0.024(2) 0.014(2) -0.004(2) -0.006(1) 0.002(2) O(4) 0.027(2) 0.017(2) 0.027(2) 0.004(1) -0.008(2) -0.004(2) O(5) 0.027(2) 0.026(2) 0.038(2) -0.003(2) -0.001(2) -0.009(2) O(6) 0.025(2) 0.032(2) 0.020(2) -0.007(2) -0.010(2) 0.000(2) O(7) 0.022(2) 0.018(2) 0.035(2) 0.005(2) -0.009(2) -0.009(2) O(8) 0.025(2) 0.027(2) 0.037(2) 0.006(2) -0.016(2) -0.015(2) O(9) 0.019(2) 0.032(2) 0.036(2) -0.002(2) -0.004(2) -0.017(2) O(10) 0.024(2) 0.019(2) 0.019(2) 0.004(1) -0.001(1) -0.006(1) O(11) 0.023(2) 0.020(2) 0.018(2) -0.004(1) -0.006(1) 0.000(1) O(12) 0.115(6) 0.144(7) 0.122(6) -0.018(5) -0.004(5) -0.030(5) N(1) 0.040(3) 0.052(3) 0.030(3) -0.002(3) -0.003(2) 0.004(2) C(1) 0.020(3) 0.022(3) 0.019(3) -0.001(2) -0.001(2) -0.005(2) C(2) 0.021(3) 0.022(3) 0.018(3) -0.004(2) -0.003(2) -0.003(2) C(3) 0.019(3) 0.020(3) 0.018(3) 0.004(2) -0.001(2) -0.009(2) C(4) 0.041(3) 0.038(4) 0.021(3) 0.005(3) -0.002(3) -0.003(3) #------------------------------------------------------------------------------ _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 1343 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0301 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0383 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.788 _refine_ls_shift/esd_max 0.0755 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.54 _refine_diff_density_max 0.32 #------------------------------------------------------------------------------ _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) 2.205(3) ? ? yes Mn(1) O(2) 2.257(3) ? ? yes Mn(1) O(3) 2.362(3) ? ? yes Mn(1) O(4) 2.045(3) ? ? yes Mn(1) O(5) 2.208(4) ? ? yes Mn(1) O(11) 2.144(3) ? ? yes Mn(2) O(3) 2.246(3) ? ? yes Mn(2) O(6) 2.242(3) ? ? yes Mn(2) O(7) 2.237(4) ? ? yes Mn(2) O(8) 2.186(3) ? ? yes Mn(2) O(10) 2.076(3) ? ? yes Mn(2) O(11) 2.158(3) ? ? yes P(1) O(4) 1.505(3) ? ? yes P(1) O(9) 1.582(4) ? ? yes P(1) O(10) 1.519(3) ? ? yes P(1) O(11) 1.532(3) ? ? yes O(1) C(1) 1.247(6) ? ? yes O(2) C(2) 1.248(6) ? ? yes O(3) C(3) 1.269(6) ? ? yes O(6) C(3) 1.247(6) ? ? yes O(7) C(2) 1.254(6) ? ? yes O(8) C(1) 1.254(6) ? ? yes N(1) C(4) 1.478(8) ? ? yes C(1) C(2) 1.554(7) ? ? yes C(3) C(3) 1.555(10) ? ? yes C(4) C(4) 1.51(1) ? ? 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) 74.1(1) ? ? ? yes O(1) Mn(1) O(3) 95.5(1) ? ? ? yes O(1) Mn(1) O(4) 92.6(1) ? ? ? yes O(1) Mn(1) O(5) 92.0(2) ? ? ? yes O(1) Mn(1) O(11) 166.0(1) ? ? ? yes O(2) Mn(1) O(3) 78.7(1) ? ? ? yes O(2) Mn(1) O(4) 163.9(1) ? ? ? yes O(2) Mn(1) O(5) 84.8(1) ? ? ? yes O(2) Mn(1) O(11) 93.0(1) ? ? ? yes O(3) Mn(1) O(4) 93.8(1) ? ? ? yes O(3) Mn(1) O(5) 159.3(1) ? ? ? yes O(3) Mn(1) O(11) 76.0(1) ? ? ? yes O(4) Mn(1) O(5) 105.1(2) ? ? ? yes O(4) Mn(1) O(11) 99.1(1) ? ? ? yes O(5) Mn(1) O(11) 92.5(1) ? ? ? yes O(3) Mn(2) O(6) 73.7(1) ? ? ? yes O(3) Mn(2) O(7) 159.9(1) ? ? ? yes O(3) Mn(2) O(8) 89.0(1) ? ? ? yes O(3) Mn(2) O(10) 104.0(1) ? ? ? yes O(3) Mn(2) O(11) 78.3(1) ? ? ? yes O(6) Mn(2) O(7) 96.1(1) ? ? ? yes O(6) Mn(2) O(8) 95.4(1) ? ? ? yes O(6) Mn(2) O(10) 85.0(1) ? ? ? yes O(6) Mn(2) O(11) 151.2(1) ? ? ? yes O(7) Mn(2) O(8) 74.4(1) ? ? ? yes O(7) Mn(2) O(10) 92.1(1) ? ? ? yes O(7) Mn(2) O(11) 112.7(1) ? ? ? yes O(8) Mn(2) O(10) 166.5(1) ? ? ? yes O(8) Mn(2) O(11) 91.0(1) ? ? ? yes O(10) Mn(2) O(11) 95.0(1) ? ? ? yes O(4) P(1) O(9) 106.8(2) ? ? ? yes O(4) P(1) O(10) 110.6(2) ? ? ? yes O(4) P(1) O(11) 112.0(2) ? ? ? yes O(9) P(1) O(10) 108.9(2) ? ? ? yes O(9) P(1) O(11) 106.8(2) ? ? ? yes O(10) P(1) O(11) 111.4(2) ? ? ? yes Mn(1) O(1) C(1) 116.6(3) ? ? ? yes Mn(1) O(2) C(2) 115.1(3) ? ? ? yes Mn(1) O(3) Mn(2) 97.6(1) ? ? ? yes Mn(1) O(3) C(3) 137.1(3) ? ? ? yes Mn(2) O(3) C(3) 114.5(3) ? ? ? yes Mn(1) O(4) P(1) 148.7(2) ? ? ? yes Mn(2) O(6) C(3) 114.1(3) ? ? ? yes Mn(2) O(7) C(2) 112.8(3) ? ? ? yes Mn(2) O(8) C(1) 114.7(3) ? ? ? yes Mn(2) O(10) P(1) 142.6(2) ? ? ? yes Mn(1) O(11) Mn(2) 107.5(1) ? ? ? yes Mn(1) O(11) P(1) 123.1(2) ? ? ? yes Mn(2) O(11) P(1) 127.3(2) ? ? ? yes O(1) C(1) O(8) 126.6(5) ? ? ? yes O(1) C(1) C(2) 117.4(4) ? ? ? yes O(8) C(1) C(2) 116.0(4) ? ? ? yes O(2) C(2) O(7) 126.2(5) ? ? ? yes O(2) C(2) C(1) 116.7(4) ? ? ? yes O(7) C(2) C(1) 117.1(4) ? ? ? yes O(3) C(3) O(6) 126.2(4) ? ? ? yes O(3) C(3) C(3) 115.6(5) ? ? ? yes O(6) C(3) C(3) 118.2(5) ? ? ? yes N(1) C(4) C(4) 110.4(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;