data_[NH(prol)3][MnCr(ox)3](H2O)2 _audit_creation_date '2009-02-05' _audit_creation_method 'by CrystalStructure 3.8.0' _publ_contact_author_name 'Hiroshi Kitagawa' _publ_contact_author_address ; Department of Chemistry Graduate School of Science Kyoto University Kitashirakawa-Oiwakecho Sakyo-ku, Kyoto 606-8502 Japan ; _publ_contact_author_email 'kitagawa@kuchem.kyoto-u.ac.jp' _publ_contact_author_fax '+81-92-642-2319' _publ_contact_author_phone '+81-92-642-2319' _publ_section_title ; Oxalate-bridged Bimetallic Complexes {NH(prol)3}[MCr(ox)3] (M = MnII, FeII, CoII; NH(prol)3+ = Tri(3-hydroxypropyl)ammonium) Exhibiting Coexistent Ferromagnetism and Proton Conduction ; loop_ _publ_author_name 'Hisashi Okawa' 'Akihito Shigematsu' 'Masaaki Sadakiyo' 'Takuya Miyakawa' 'Masaaki Ohba' 'Hiroshi Kitagawa' _publ_author_address ; Department of Chemistry Faculty of Science Kyushu University Hakozaki 6-10-1, Higashi-ku Fukuoka 812-8581, Japan ; _publ_requested_journal 'Journal of the American Chemical Society' _chemical_name_systematic ; {NH(prol)3}[MnCr(ox)3](H2O)2 ; _chemical_name_common '{NH(prol)3}[MnCr(ox)3](H2O)2' _chemical_melting_point ? _chemical_formula_moiety 'C6 Cr Mn O12, C9 N O3' _chemical_formula_sum 'C15 H26 Cr Mn N O17' _chemical_formula_weight 599.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' _cell_length_a 9.3808(14) _cell_length_b 9.3808(14) _cell_length_c 15.8006(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1204.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode with a mirror focusing unit' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD-detector' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number NONE _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4310 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_max 21.92 _reflns_number_total 959 _reflns_number_gt 915 _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^)+(0.1450P)^2^+1.6547P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(11) _refine_ls_number_reflns 959 _refine_ls_number_parameters 113 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2283 _refine_ls_wR_factor_gt 0.2190 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.5424(8) 0.205(4) Uani 1 3 d S . . Cr1 Cr 0.6667 0.3333 0.54365(14) 0.0427(8) Uani 1 3 d S . . O5 O 0.635(5) -0.072(4) 0.379(3) 0.306(18) Uani 1 1 d . . . O1 O 0.4836(9) 0.1646(9) 0.4761(5) 0.068(2) Uani 1 1 d . . . O2 O 0.2062(11) 0.0209(10) 0.4767(11) 0.138(6) Uani 1 1 d . . . O3 O 0.6823(7) 0.1621(8) 0.6138(5) 0.0645(19) Uani 1 1 d . . . O4 O 0.8178(10) 0.0257(8) 0.6151(9) 0.104(3) Uani 1 1 d . . . O6 O 1.0000 0.0000 0.2584(18) 0.191(12) Uani 1 3 d S . . O7 O 0.654(9) 0.269(4) -0.030(2) 0.120(12) Uani 0.33 1 d P . . N1 N 0.6667 0.3333 0.2285(17) 0.152(13) Uani 1 3 d S . . C1 C 0.3507(16) 0.1322(12) 0.5054(10) 0.078(4) Uani 1 1 d . . . C2 C 0.7784(14) 0.1210(12) 0.5824(8) 0.066(3) Uani 1 1 d . . . C5 C 0.708(6) -0.077(6) 0.292(3) 0.246(18) Uani 1 1 d . . . C3 C 0.599(5) 0.149(5) 0.2726(18) 0.215(15) Uani 1 1 d . . . C4 C 0.682(5) 0.080(4) 0.274(2) 0.217(17) 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 Mn1 0.0353(12) 0.0353(12) 0.545(12) 0.000 0.000 0.0176(6) Cr1 0.0346(9) 0.0346(9) 0.0590(12) 0.000 0.000 0.0173(5) O5 0.34(4) 0.17(2) 0.36(5) 0.05(3) 0.01(4) 0.10(2) O1 0.040(4) 0.057(4) 0.099(5) -0.017(4) -0.005(4) 0.020(3) O2 0.064(5) 0.047(5) 0.301(17) -0.052(7) -0.083(7) 0.026(4) O3 0.052(4) 0.054(4) 0.087(4) 0.020(3) 0.003(3) 0.027(3) O4 0.057(4) 0.043(4) 0.208(10) 0.038(5) -0.004(6) 0.021(4) O6 0.210(19) 0.210(19) 0.15(2) 0.000 0.000 0.105(9) O7 0.17(3) 0.05(2) 0.16(2) 0.004(13) -0.05(3) 0.07(3) N1 0.19(2) 0.19(2) 0.078(15) 0.000 0.000 0.094(11) C1 0.068(9) 0.030(5) 0.136(9) -0.013(6) -0.032(7) 0.025(6) C2 0.044(5) 0.035(5) 0.132(8) 0.005(6) -0.004(6) 0.029(5) C5 0.27(5) 0.21(4) 0.21(3) -0.09(3) -0.04(3) 0.09(3) C3 0.34(4) 0.31(4) 0.15(2) 0.00(2) 0.03(2) 0.27(4) C4 0.32(5) 0.14(2) 0.17(2) 0.033(17) -0.06(3) 0.10(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 O2 2.117(15) 5 ? Mn1 O2 2.117(15) . ? Mn1 O2 2.117(15) 3 ? Mn1 O4 2.171(14) 5_665 ? Mn1 O4 2.171(14) 1_455 ? Mn1 O4 2.171(14) 3_545 ? Cr1 O1 1.968(7) 3_655 ? Cr1 O1 1.968(7) . ? Cr1 O1 1.968(7) 5_665 ? Cr1 O3 2.017(7) . ? Cr1 O3 2.017(7) 3_655 ? Cr1 O3 2.017(7) 5_665 ? O5 C5 1.55(6) . ? O1 C1 1.217(15) . ? O2 C1 1.311(15) . ? O3 C2 1.247(13) . ? O4 C2 1.239(12) . ? O4 Mn1 2.171(14) 1_655 ? O7 O7 0.97(4) 5_665 ? O7 O7 0.97(4) 3_655 ? N1 C3 1.66(4) 3_655 ? N1 C3 1.66(4) . ? N1 C3 1.66(4) 5_665 ? C1 C2 1.500(17) 5_665 ? C2 C1 1.500(17) 3_655 ? C5 C4 1.63(6) . ? C3 C4 1.24(4) . ? 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 O2 Mn1 O2 98.0(6) 5 . ? O2 Mn1 O2 98.0(6) 5 3 ? O2 Mn1 O2 98.0(6) . 3 ? O2 Mn1 O4 169.6(3) 5 5_665 ? O2 Mn1 O4 76.5(3) . 5_665 ? O2 Mn1 O4 91.6(4) 3 5_665 ? O2 Mn1 O4 91.6(4) 5 1_455 ? O2 Mn1 O4 169.6(3) . 1_455 ? O2 Mn1 O4 76.5(3) 3 1_455 ? O4 Mn1 O4 94.6(6) 5_665 1_455 ? O2 Mn1 O4 76.5(3) 5 3_545 ? O2 Mn1 O4 91.6(4) . 3_545 ? O2 Mn1 O4 169.6(3) 3 3_545 ? O4 Mn1 O4 94.6(6) 5_665 3_545 ? O4 Mn1 O4 94.6(6) 1_455 3_545 ? O1 Cr1 O1 93.4(3) 3_655 . ? O1 Cr1 O1 93.4(3) 3_655 5_665 ? O1 Cr1 O1 93.4(3) . 5_665 ? O1 Cr1 O3 82.1(3) 3_655 . ? O1 Cr1 O3 92.3(3) . . ? O1 Cr1 O3 173.0(3) 5_665 . ? O1 Cr1 O3 92.3(3) 3_655 3_655 ? O1 Cr1 O3 173.0(3) . 3_655 ? O1 Cr1 O3 82.1(3) 5_665 3_655 ? O3 Cr1 O3 92.7(3) . 3_655 ? O1 Cr1 O3 173.0(3) 3_655 5_665 ? O1 Cr1 O3 82.1(3) . 5_665 ? O1 Cr1 O3 92.3(3) 5_665 5_665 ? O3 Cr1 O3 92.7(3) . 5_665 ? O3 Cr1 O3 92.7(3) 3_655 5_665 ? C1 O1 Cr1 111.6(7) . . ? C1 O2 Mn1 115.9(12) . . ? C2 O3 Cr1 112.2(7) . . ? C2 O4 Mn1 113.2(10) . 1_655 ? O7 O7 O7 60.000(2) 5_665 3_655 ? C3 N1 C3 103.7(15) 3_655 . ? C3 N1 C3 103.7(15) 3_655 5_665 ? C3 N1 C3 103.7(15) . 5_665 ? O1 C1 O2 126.1(14) . . ? O1 C1 C2 120.0(9) . 5_665 ? O2 C1 C2 113.9(14) . 5_665 ? O4 C2 O3 125.4(13) . . ? O4 C2 C1 120.1(12) . 3_655 ? O3 C2 C1 113.9(8) . 3_655 ? O5 C5 C4 82(3) . . ? C4 C3 N1 122(4) . . ? C3 C4 C5 153(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.92 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.208 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.154