# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Natarajan, Srinivasan' _publ_contact_author_email snatarajan@sscu.iisc.ernet.in _publ_section_title ; CoMn2O4 Spinel from a MOF: Synthesis, structure and magnetic Studies ; _publ_author_name S.Natarajan # Attachment '- CIF.txt' data_Compound(I) _database_code_depnum_ccdc_archive 'CCDC 775632' #TrackingRef '- CIF.txt' #============================================================================================== _chemical_name_systematic ; ? ; _chemical_name_common 'Cobalt-Manganese carboxylate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 Co1 Mn2 N0 O12' _chemical_formula_weight 583.04 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.330(6) _cell_length_b 6.557(3) _cell_length_c 11.330(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.84 _cell_angle_gamma 90.00 _cell_volume 786.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1486 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.10 _exptl_crystal_description Rectangular _exptl_crystal_colour Light-pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 2.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.8125 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4806 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.1520 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.10 _reflns_number_total 1486 _reflns_number_gt 925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0296P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1486 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.32187(9) 0.21146(17) 0.22659(10) 0.0158(3) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 0.5000 0.0168(4) Uani 1 2 d S . . O1 O 0.0019(4) 0.3251(7) 0.7148(5) 0.0233(13) Uani 1 1 d . . . O2 O 0.2337(4) 0.4957(7) 0.4227(4) 0.0227(12) Uani 1 1 d . . . O3 O 0.3827(4) 0.2653(7) 0.4365(4) 0.0152(10) Uani 1 1 d . . . O5 O 0.6611(4) 0.4533(7) 0.7782(4) 0.0165(8) Uani 1 1 d . . . O6 O 0.1186(4) 0.3812(8) 0.9148(4) 0.0225(12) Uani 1 1 d . . . C1 C 0.2242(6) 0.3442(10) 0.7716(6) 0.0120(14) Uani 1 1 d . . . C2 C 0.3402(6) 0.3397(10) 0.8715(6) 0.0148(15) Uani 1 1 d . . . H2 H 0.3431 0.3375 0.9545 0.018 Uiso 1 1 calc R . . C3 C 0.4508(6) 0.3384(10) 0.8459(6) 0.0164(15) Uani 1 1 d . . . H3 H 0.5278 0.3373 0.9128 0.020 Uiso 1 1 calc R . . C4 C 0.4501(5) 0.3386(10) 0.7234(6) 0.0119(14) Uani 1 1 d . . . C5 C 0.3328(6) 0.3512(10) 0.6219(6) 0.0132(14) Uani 1 1 d . . . C6 C 0.2224(6) 0.3573(10) 0.6495(6) 0.0143(15) Uani 1 1 d . . . H6 H 0.1453 0.3706 0.5836 0.017 Uiso 1 1 calc R . . C7 C 0.1039(6) 0.3512(10) 0.8022(7) 0.0177(15) Uani 1 1 d . . . C8 C 0.5792(6) 0.3255(10) 0.7162(6) 0.0138(15) Uani 1 1 d . . . C9 C 0.3173(6) 0.3732(11) 0.4838(6) 0.0161(15) Uani 1 1 d . . . O4 O 0.6102(4) 0.1823(7) 0.6593(4) 0.0165(8) 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 0.0051(5) 0.0264(6) 0.0182(5) -0.0048(5) 0.0068(4) -0.0018(4) Co1 0.0097(6) 0.0259(8) 0.0187(7) 0.0012(6) 0.0097(5) 0.0001(5) O1 0.005(2) 0.039(4) 0.030(3) -0.001(2) 0.011(2) -0.001(2) O2 0.012(2) 0.038(3) 0.018(3) 0.010(2) 0.0057(19) 0.010(2) O3 0.011(2) 0.024(3) 0.015(2) 0.0014(19) 0.0102(18) 0.0047(19) O5 0.0044(14) 0.028(2) 0.0181(17) -0.0027(15) 0.0055(12) 0.0002(13) O6 0.018(2) 0.037(3) 0.022(3) -0.002(2) 0.018(2) 0.004(2) C1 0.008(3) 0.013(3) 0.019(3) 0.001(3) 0.010(3) -0.001(2) C2 0.014(3) 0.020(4) 0.012(3) 0.005(3) 0.007(3) 0.000(3) C3 0.013(3) 0.023(4) 0.016(3) 0.004(3) 0.008(3) 0.004(3) C4 0.004(3) 0.021(4) 0.011(3) -0.002(3) 0.003(2) -0.001(2) C5 0.011(3) 0.017(4) 0.012(3) 0.000(3) 0.004(2) -0.001(3) C6 0.010(3) 0.015(4) 0.017(3) -0.001(3) 0.004(2) 0.000(3) C7 0.011(3) 0.012(4) 0.032(4) 0.003(3) 0.010(3) 0.001(3) C8 0.008(3) 0.026(4) 0.010(3) 0.003(3) 0.005(2) -0.006(3) C9 0.008(3) 0.027(4) 0.015(3) 0.002(3) 0.007(2) -0.006(3) O4 0.0044(14) 0.028(2) 0.0181(17) -0.0027(15) 0.0055(12) 0.0002(13) _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 2.105(5) 4_665 ? Mn1 O2 2.121(5) 2_545 ? Mn1 O5 2.209(5) 3_666 ? Mn1 O3 2.256(5) . ? Mn1 O4 2.349(5) 4_565 ? Mn1 O5 2.363(5) 4_565 ? Co1 O6 2.066(5) 2_546 ? Co1 O6 2.066(5) 4_665 ? Co1 O3 2.152(5) . ? Co1 O3 2.152(5) 3_656 ? Co1 O4 2.155(5) 3_656 ? Co1 O4 2.155(5) . ? O1 C7 1.237(8) . ? O1 Mn1 2.105(5) 4_566 ? O2 C9 1.247(8) . ? O2 Mn1 2.121(5) 2 ? O3 C9 1.273(8) . ? O5 C8 1.262(8) . ? O5 Mn1 2.209(5) 3_666 ? O5 Mn1 2.363(5) 4_666 ? O6 C7 1.241(9) . ? O6 Co1 2.066(5) 2_556 ? C1 C6 1.379(9) . ? C1 C2 1.397(9) . ? C1 C7 1.523(9) . ? C2 C3 1.383(8) . ? C3 C4 1.385(9) . ? C4 C5 1.417(8) . ? C4 C8 1.495(8) . ? C5 C6 1.393(8) . ? C5 C9 1.518(9) . ? C8 O4 1.258(8) . ? O4 Mn1 2.349(5) 4_666 ? 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 O2 83.86(19) 4_665 2_545 ? O1 Mn1 O5 90.96(18) 4_665 3_666 ? O2 Mn1 O5 130.38(19) 2_545 3_666 ? O1 Mn1 O3 98.35(18) 4_665 . ? O2 Mn1 O3 146.87(19) 2_545 . ? O5 Mn1 O3 82.73(17) 3_666 . ? O1 Mn1 O4 156.03(19) 4_665 4_565 ? O2 Mn1 O4 87.68(18) 2_545 4_565 ? O5 Mn1 O4 77.59(16) 3_666 4_565 ? O3 Mn1 O4 100.93(16) . 4_565 ? O1 Mn1 O5 144.44(18) 4_665 4_565 ? O2 Mn1 O5 81.72(19) 2_545 4_565 ? O5 Mn1 O5 122.86(14) 3_666 4_565 ? O3 Mn1 O5 77.53(16) . 4_565 ? O4 Mn1 O5 55.10(16) 4_565 4_565 ? O6 Co1 O6 180.0 2_546 4_665 ? O6 Co1 O3 91.94(19) 2_546 . ? O6 Co1 O3 88.06(19) 4_665 . ? O6 Co1 O3 88.06(19) 2_546 3_656 ? O6 Co1 O3 91.94(19) 4_665 3_656 ? O3 Co1 O3 180.000(1) . 3_656 ? O6 Co1 O4 84.41(19) 2_546 3_656 ? O6 Co1 O4 95.59(19) 4_665 3_656 ? O3 Co1 O4 93.64(17) . 3_656 ? O3 Co1 O4 86.36(17) 3_656 3_656 ? O6 Co1 O4 95.59(19) 2_546 . ? O6 Co1 O4 84.41(19) 4_665 . ? O3 Co1 O4 86.36(17) . . ? O3 Co1 O4 93.64(17) 3_656 . ? O4 Co1 O4 180.000(1) 3_656 . ? C7 O1 Mn1 127.9(5) . 4_566 ? C9 O2 Mn1 145.5(5) . 2 ? C9 O3 Co1 133.8(4) . . ? C9 O3 Mn1 121.7(4) . . ? Co1 O3 Mn1 98.43(18) . . ? C8 O5 Mn1 134.5(4) . 3_666 ? C8 O5 Mn1 92.2(4) . 4_666 ? Mn1 O5 Mn1 111.53(19) 3_666 4_666 ? C7 O6 Co1 131.9(5) . 2_556 ? C6 C1 C2 119.2(6) . . ? C6 C1 C7 122.1(6) . . ? C2 C1 C7 118.5(6) . . ? C3 C2 C1 119.4(6) . . ? C2 C3 C4 121.8(6) . . ? C3 C4 C5 118.8(6) . . ? C3 C4 C8 113.4(5) . . ? C5 C4 C8 127.7(6) . . ? C6 C5 C4 118.5(6) . . ? C6 C5 C9 116.4(5) . . ? C4 C5 C9 125.0(6) . . ? C1 C6 C5 121.9(6) . . ? O1 C7 O6 126.2(7) . . ? O1 C7 C1 118.0(7) . . ? O6 C7 C1 115.8(5) . . ? O4 C8 O5 119.7(6) . . ? O4 C8 C4 121.9(6) . . ? O5 C8 C4 118.1(6) . . ? O2 C9 O3 124.4(6) . . ? O2 C9 C5 114.9(6) . . ? O3 C9 C5 120.6(6) . . ? C8 O4 Co1 131.2(4) . . ? C8 O4 Mn1 93.0(4) . 4_666 ? Co1 O4 Mn1 131.1(2) . 4_666 ? _diffrn_measured_fraction_theta_max 0.774 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.774 _refine_diff_density_max 0.730 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.132