# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1328 data_10 _audit_creation_method SHELXL _publ_contact_author_name 'D.S.Yufit' _publ_contact_author_address ; Department of Chemistry University of Durham South Rd. Durham DH1 3LE UK ; _publ_contact_author_email 'd.s.yufit@dur.ac.uk' _publ_requested_journal 'J.Chem.Soc.Chem.Commun.' _publ_contact_letter ; The CIF file contains 10K data for structure 1 from the paper "New type of metal squarates. Magnetic and multi-temperature X-ray study of di-hydroxy(\m^6^-squarato)manganese" by D.S.Yufit, D.J.Price, J.A.K.Howard, A.K.Powell, S.O.H.Gutschke and P.T.Wood, submitted in J.Chem.Soc.Chem.Commun.. Ref.N ; _chemical_name_systematic ; di-hydroxy-(\m^6^-squarato)manganese ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H2 Mn2 O6' _chemical_formula_weight 255.94 _chemical_melting_point ? _chemical_compound_source ? 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.3760(7) _cell_length_b 10.268(2) _cell_length_c 8.575(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.82(3) _cell_angle_gamma 90.00 _cell_volume 292.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 10(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 15.9 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 4.290 _exptl_absorpt_correction_type 'numerical from crystal shape' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; ? ; _diffrn_ambient_temperature 10(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FDDD' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 4 _diffrn_standards_interval_count 96 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2590 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 47.51 _reflns_number_total 2590 _reflns_number_observed 2256 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MAD (Allibon, 1996)' _computing_cell_refinement 'RAFIN (Filhol,Ellis, Pryor, 1987)' _computing_data_reduction 'C5N (Lehmann, Wilson, 1987)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0300P)^2^+0.1200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2588 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_obs 0.0234 _refine_ls_wR_factor_all 0.0579 _refine_ls_wR_factor_obs 0.0536 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.034 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.034 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.29022(4) 0.616000(11) 0.079947(13) 0.00560(3) Uani 1 d . . O1 O -0.1493(2) 0.61425(6) 0.26727(7) 0.00757(8) Uani 1 d . . O2 O 0.3243(2) 0.82130(6) 0.12119(7) 0.00776(8) Uani 1 d . . O3 O 0.2718(2) 0.40370(6) 0.07023(7) 0.00707(8) Uani 1 d . . C1 C 0.1449(2) 0.91823(7) 0.05437(8) 0.00646(9) Uani 1 d . . C2 C -0.0693(2) 0.55119(7) 0.39505(8) 0.00653(9) Uani 1 d . . H1 H 0.3140(61) 0.3651(20) 0.1495(29) 0.024(5) Uiso 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 0.00547(5) 0.00532(4) 0.00592(4) -0.00026(3) 0.00068(3) -0.00005(3) O1 0.0082(2) 0.0080(2) 0.0063(2) 0.00143(15) 0.00042(14) 0.0002(2) O2 0.0084(2) 0.0060(2) 0.0084(2) 0.00077(15) 0.00008(15) 0.00092(15) O3 0.0074(2) 0.0069(2) 0.0067(2) 0.00092(14) 0.00060(14) 0.00013(15) C1 0.0066(3) 0.0060(2) 0.0066(2) 0.0001(2) 0.0006(2) -0.0001(2) C2 0.0064(2) 0.0067(2) 0.0065(2) 0.0001(2) 0.0009(2) -0.0003(2) _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 O3 2.1132(9) 3_565 ? Mn1 O3 2.1297(8) 3_665 ? Mn1 O2 2.1374(7) . ? Mn1 O3 2.1820(7) . ? Mn1 O1 2.2638(10) 1_655 ? Mn1 O1 2.3653(9) . ? Mn1 Mn1 3.1974(6) 3_665 ? Mn1 Mn1 3.2370(6) 3_565 ? O1 C2 1.2617(9) . ? O1 Mn1 2.2637(10) 1_455 ? O2 C1 1.2518(10) . ? O3 Mn1 2.1132(9) 3_565 ? O3 Mn1 2.1297(8) 3_665 ? C1 C2 1.4666(11) 4_575 ? C1 C2 1.4678(10) 2 ? C2 C1 1.4666(11) 4_576 ? C2 C1 1.4679(11) 2_545 ? 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 O3 Mn1 O3 105.44(3) 3_565 3_665 ? O3 Mn1 O2 102.28(2) 3_565 . ? O3 Mn1 O2 99.82(2) 3_665 . ? O3 Mn1 O3 82.20(2) 3_565 . ? O3 Mn1 O3 84.27(2) 3_665 . ? O2 Mn1 O3 172.77(2) . . ? O3 Mn1 O1 170.62(2) 3_565 1_655 ? O3 Mn1 O1 81.13(3) 3_665 1_655 ? O2 Mn1 O1 82.85(2) . 1_655 ? O3 Mn1 O1 91.95(2) . 1_655 ? O3 Mn1 O1 79.11(3) 3_565 . ? O3 Mn1 O1 172.12(2) 3_665 . ? O2 Mn1 O1 85.26(2) . . ? O3 Mn1 O1 90.07(2) . . ? O1 Mn1 O1 93.63(3) 1_655 . ? O3 Mn1 Mn1 94.86(2) 3_565 3_665 ? O3 Mn1 Mn1 42.77(2) 3_665 3_665 ? O2 Mn1 Mn1 142.23(2) . 3_665 ? O3 Mn1 Mn1 41.51(2) . 3_665 ? O1 Mn1 Mn1 85.44(2) 1_655 3_665 ? O1 Mn1 Mn1 131.35(2) . 3_665 ? O3 Mn1 Mn1 41.90(2) 3_565 3_565 ? O3 Mn1 Mn1 96.12(2) 3_665 3_565 ? O2 Mn1 Mn1 143.85(2) . 3_565 ? O3 Mn1 Mn1 40.30(2) . 3_565 ? O1 Mn1 Mn1 131.84(2) 1_655 3_565 ? O1 Mn1 Mn1 82.97(2) . 3_565 ? Mn1 Mn1 Mn1 63.290(14) 3_665 3_565 ? C2 O1 Mn1 130.50(6) . 1_455 ? C2 O1 Mn1 121.85(5) . . ? Mn1 O1 Mn1 93.63(3) 1_455 . ? C1 O2 Mn1 134.44(6) . . ? Mn1 O3 Mn1 105.44(3) 3_565 3_665 ? Mn1 O3 Mn1 97.80(2) 3_565 . ? Mn1 O3 Mn1 95.72(2) 3_665 . ? O2 C1 C2 136.04(7) . 4_575 ? O2 C1 C2 134.35(7) . 2 ? C2 C1 C2 89.61(6) 4_575 2 ? O1 C2 C1 134.23(7) . 4_576 ? O1 C2 C1 135.38(7) . 2_545 ? C1 C2 C1 90.39(6) 4_576 2_545 ? _refine_diff_density_max 0.651 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.128 #=== END data_20 _audit_creation_method SHELXL _publ_contact_author_name 'D.S.Yufit' _publ_contact_author_address ; Department of Chemistry University of Durham South Rd. Durham DH1 3LE UK ; _publ_contact_author_email 'd.s.yufit@dur.ac.uk' _publ_requested_journal 'J.Chem.Soc.Chem.Commun.' _publ_contact_letter ; The CIF file contains 20K data for structure 1 from the paper "New type of metal squarates. Magnetic and multi-temperature X-ray study of di-hydroxy(\m^6^-squarato)manganese" by D.S.Yufit, D.J.Price, J.A.K.Howard, A.K.Powell, S.O.H.Gutschke and P.T.Wood, submitted in J.Chem.Soc.Chem.Commun.. Ref.N ; _chemical_name_systematic ; di-hydroxy-(\m^6^-squarato)manganese ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H2 Mn2 O6' _chemical_formula_weight 255.94 _chemical_melting_point ? _chemical_compound_source ? 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.3770(7) _cell_length_b 10.268(2) _cell_length_c 8.576(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.81(3) _cell_angle_gamma 90.00 _cell_volume 293.0(1) _cell_formula_units_Z 2 _cell_measurement_temperature 20(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 15.9 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 4.288 _exptl_absorpt_correction_type 'numerical from crystal shape' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Fddd' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 4 _diffrn_standards_interval_count 96 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1231 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 506 _reflns_number_observed 476 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MAD (Allibon, 1996)' _computing_cell_refinement 'RAFIN (Filhol,Ellis, Pryor, 1987)' _computing_data_reduction 'C5N (Lehmann, Wilson, 1987)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0090P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.005(1) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 504 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_obs 0.0138 _refine_ls_wR_factor_all 0.0358 _refine_ls_wR_factor_obs 0.0325 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.28955(8) 0.61597(2) 0.08002(3) 0.00446(12) Uani 1 d . . O1 O -0.1499(4) 0.61401(12) 0.26732(15) 0.0065(3) Uani 1 d . . O2 O 0.3236(4) 0.82134(12) 0.12141(15) 0.0070(3) Uani 1 d . . O3 O 0.2726(4) 0.40385(13) 0.0697(2) 0.0066(3) Uani 1 d . . C1 C 0.1438(5) 0.9187(2) 0.0542(2) 0.0057(4) Uani 1 d . . C2 C -0.0688(5) 0.5512(2) 0.3954(2) 0.0058(4) Uani 1 d . . H1 H 0.3295(84) 0.3687(26) 0.1536(37) 0.034(8) Uiso 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 0.0045(2) 0.0032(2) 0.0057(2) -0.00012(11) 0.00096(11) -0.00002(10) O1 0.0062(7) 0.0071(6) 0.0063(6) 0.0011(5) 0.0014(5) 0.0010(5) O2 0.0072(7) 0.0049(6) 0.0088(6) 0.0007(5) 0.0013(5) 0.0007(5) O3 0.0079(7) 0.0060(7) 0.0061(7) 0.0017(5) 0.0015(5) 0.0009(5) C1 0.0013(9) 0.0069(9) 0.0096(9) -0.0005(8) 0.0025(7) -0.0022(7) C2 0.0034(9) 0.0061(9) 0.0086(9) -0.0002(7) 0.0033(7) 0.0020(7) _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 O3 2.1128(15) 3_565 ? Mn1 O3 2.1271(15) 3_665 ? Mn1 O2 2.1383(14) . ? Mn1 O3 2.1802(14) . ? Mn1 O1 2.2645(15) 1_655 ? Mn1 O1 2.3655(14) . ? Mn1 Mn1 3.2000(7) 3_665 ? Mn1 Mn1 3.2349(8) 3_565 ? O1 C2 1.263(2) . ? O1 Mn1 2.2645(15) 1_455 ? O2 C1 1.257(2) . ? O3 Mn1 2.1128(15) 3_565 ? O3 Mn1 2.1270(14) 3_665 ? C1 C2 1.460(3) 4_575 ? C1 C2 1.463(3) 2 ? C2 C1 1.460(3) 4_576 ? C2 C1 1.463(3) 2_545 ? 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 O3 Mn1 O3 105.59(6) 3_565 3_665 ? O3 Mn1 O2 102.31(5) 3_565 . ? O3 Mn1 O2 99.86(5) 3_665 . ? O3 Mn1 O3 82.22(5) 3_565 . ? O3 Mn1 O3 84.04(5) 3_665 . ? O2 Mn1 O3 172.86(5) . . ? O3 Mn1 O1 170.50(5) 3_565 1_655 ? O3 Mn1 O1 81.05(5) 3_665 1_655 ? O2 Mn1 O1 82.88(5) . 1_655 ? O3 Mn1 O1 91.88(5) . 1_655 ? O3 Mn1 O1 79.01(5) 3_565 . ? O3 Mn1 O1 172.02(5) 3_665 . ? O2 Mn1 O1 85.29(4) . . ? O3 Mn1 O1 90.22(5) . . ? O1 Mn1 O1 93.64(5) 1_655 . ? O3 Mn1 Mn1 94.96(4) 3_565 3_665 ? O3 Mn1 Mn1 42.66(4) 3_665 3_665 ? O2 Mn1 Mn1 142.17(4) . 3_665 ? O3 Mn1 Mn1 41.39(4) . 3_665 ? O1 Mn1 Mn1 85.35(4) 1_655 3_665 ? O1 Mn1 Mn1 131.36(3) . 3_665 ? O3 Mn1 Mn1 41.89(4) 3_565 3_565 ? O3 Mn1 Mn1 96.06(4) 3_665 3_565 ? O2 Mn1 Mn1 143.90(4) . 3_565 ? O3 Mn1 Mn1 40.32(4) . 3_565 ? O1 Mn1 Mn1 131.78(4) 1_655 3_565 ? O1 Mn1 Mn1 82.99(3) . 3_565 ? Mn1 Mn1 Mn1 63.31(2) 3_665 3_565 ? C2 O1 Mn1 130.74(12) . 1_455 ? C2 O1 Mn1 121.78(11) . . ? Mn1 O1 Mn1 93.64(5) 1_455 . ? C1 O2 Mn1 134.40(12) . . ? Mn1 O3 Mn1 105.59(6) 3_565 3_665 ? Mn1 O3 Mn1 97.78(5) 3_565 . ? Mn1 O3 Mn1 95.96(5) 3_665 . ? O2 C1 C2 135.9(2) . 4_575 ? O2 C1 C2 134.3(2) . 2 ? C2 C1 C2 89.77(15) 4_575 2 ? O1 C2 C1 134.6(2) . 4_576 ? O1 C2 C1 135.2(2) . 2_545 ? C1 C2 C1 90.23(15) 4_576 2_545 ? _refine_diff_density_max 0.301 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.059 #=== END data_45 _audit_creation_method SHELXL _publ_contact_author_name 'D.S.Yufit' _publ_contact_author_address ; Department of Chemistry University of Durham South Rd. Durham DH1 3LE UK ; _publ_contact_author_email 'd.s.yufit@dur.ac.uk' _publ_requested_journal 'J.Chem.Soc.Chem.Commun.' _publ_contact_letter ; The CIF file contains 45K data for structure 1 from the paper "New type of metal squarates. Magnetic and multi-temperature X-ray study of di-hydroxy(\m^6^-squarato)manganese" by D.S.Yufit, D.J.Price, J.A.K.Howard, A.K.Powell, S.O.H.Gutschke and P.T.Wood, submitted in J.Chem.Soc.Chem.Commun.. Ref.N ; _chemical_name_systematic ; di-hydroxy-(\m^6^-squarato)manganese ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H2 Mn2 O6' _chemical_formula_weight 255.94 _chemical_melting_point ? _chemical_compound_source ? 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.3770(7) _cell_length_b 10.269(2) _cell_length_c 8.573(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.80(3) _cell_angle_gamma 90.00 _cell_volume 293.0(1) _cell_formula_units_Z 2 _cell_measurement_temperature 45(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 15.9 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 4.289 _exptl_absorpt_correction_type 'numerical from crystal shape' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; ? ; _diffrn_ambient_temperature 45(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Fddd' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 4 _diffrn_standards_interval_count 96 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1231 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 506 _reflns_number_observed 473 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MAD (Allibon, 1996)' _computing_cell_refinement 'RAFIN (Filhol,Ellis, Pryor, 1987)' _computing_data_reduction 'C5N (Lehmann, Wilson, 1987)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0090P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(1) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 504 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_obs 0.0144 _refine_ls_wR_factor_all 0.0357 _refine_ls_wR_factor_obs 0.0327 _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.169 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.28885(8) 0.61593(3) 0.08019(3) 0.00482(13) Uani 1 d . . O1 O -0.1494(4) 0.61415(13) 0.2674(2) 0.0072(3) Uani 1 d . . O2 O 0.3237(4) 0.82114(13) 0.1212(2) 0.0072(3) Uani 1 d . . O3 O 0.2727(4) 0.40386(13) 0.0699(2) 0.0067(3) Uani 1 d . . C1 C 0.1440(6) 0.9187(2) 0.0544(2) 0.0055(4) Uani 1 d . . C2 C -0.0686(6) 0.5514(2) 0.3953(2) 0.0064(4) Uani 1 d . . H1 H 0.3283(80) 0.3659(26) 0.1563(35) 0.024(7) Uiso 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 0.0049(2) 0.0037(2) 0.0058(2) -0.00024(11) 0.00081(11) -0.00003(11) O1 0.0072(7) 0.0076(6) 0.0066(6) 0.0015(6) 0.0007(5) 0.0003(5) O2 0.0076(7) 0.0044(6) 0.0091(6) 0.0005(6) 0.0004(5) 0.0008(5) O3 0.0084(7) 0.0059(7) 0.0055(7) 0.0014(6) 0.0008(5) 0.0004(5) C1 0.0028(9) 0.0058(9) 0.0088(9) -0.0005(8) 0.0029(7) -0.0023(7) C2 0.0033(9) 0.0075(10) 0.0091(9) -0.0016(8) 0.0034(7) 0.0014(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 O3 2.112(2) 3_565 ? Mn1 O3 2.1301(15) 3_665 ? Mn1 O2 2.1364(14) . ? Mn1 O3 2.1799(15) . ? Mn1 O1 2.267(2) 1_655 ? Mn1 O1 2.3608(15) . ? Mn1 Mn1 3.2033(8) 3_665 ? Mn1 Mn1 3.2330(8) 3_565 ? O1 C2 1.261(2) . ? O1 Mn1 2.267(2) 1_455 ? O2 C1 1.258(3) . ? O3 Mn1 2.112(2) 3_565 ? O3 Mn1 2.1301(15) 3_665 ? C1 C2 1.462(3) 4_575 ? C1 C2 1.464(3) 2 ? C2 C1 1.462(3) 4_576 ? C2 C1 1.464(3) 2_545 ? 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 O3 Mn1 O3 105.50(6) 3_565 3_665 ? O3 Mn1 O2 102.34(5) 3_565 . ? O3 Mn1 O2 99.73(5) 3_665 . ? O3 Mn1 O3 82.27(6) 3_565 . ? O3 Mn1 O3 83.99(6) 3_665 . ? O2 Mn1 O3 172.94(5) . . ? O3 Mn1 O1 170.68(5) 3_565 1_655 ? O3 Mn1 O1 80.95(5) 3_665 1_655 ? O2 Mn1 O1 82.85(5) . 1_655 ? O3 Mn1 O1 91.88(5) . 1_655 ? O3 Mn1 O1 79.14(5) 3_565 . ? O3 Mn1 O1 172.04(5) 3_665 . ? O2 Mn1 O1 85.36(5) . . ? O3 Mn1 O1 90.32(5) . . ? O1 Mn1 O1 93.71(5) 1_655 . ? O3 Mn1 Mn1 94.94(4) 3_565 3_665 ? O3 Mn1 Mn1 42.59(4) 3_665 3_665 ? O2 Mn1 Mn1 141.98(4) . 3_665 ? O3 Mn1 Mn1 41.40(4) . 3_665 ? O1 Mn1 Mn1 85.28(4) 1_655 3_665 ? O1 Mn1 Mn1 131.48(4) . 3_665 ? O3 Mn1 Mn1 41.92(4) 3_565 3_565 ? O3 Mn1 Mn1 95.97(4) 3_665 3_565 ? O2 Mn1 Mn1 143.97(4) . 3_565 ? O3 Mn1 Mn1 40.34(4) . 3_565 ? O1 Mn1 Mn1 131.82(4) 1_655 3_565 ? O1 Mn1 Mn1 83.15(4) . 3_565 ? Mn1 Mn1 Mn1 63.29(2) 3_665 3_565 ? C2 O1 Mn1 130.59(12) . 1_455 ? C2 O1 Mn1 121.83(12) . . ? Mn1 O1 Mn1 93.71(5) 1_455 . ? C1 O2 Mn1 134.61(12) . . ? Mn1 O3 Mn1 105.50(6) 3_565 3_665 ? Mn1 O3 Mn1 97.73(6) 3_565 . ? Mn1 O3 Mn1 96.01(6) 3_665 . ? O2 C1 C2 135.6(2) . 4_575 ? O2 C1 C2 134.6(2) . 2 ? C2 C1 C2 89.8(2) 4_575 2 ? O1 C2 C1 134.7(2) . 4_576 ? O1 C2 C1 135.1(2) . 2_545 ? C1 C2 C1 90.2(2) 4_576 2_545 ? _refine_diff_density_max 0.399 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.061 #=== END data_120 _audit_creation_method SHELXL _publ_contact_author_name 'D.S.Yufit' _publ_contact_author_address ; Department of Chemistry University of Durham South Rd. Durham DH1 3LE UK ; _publ_contact_author_email 'd.s.yufit@dur.ac.uk' _publ_requested_journal 'J.Chem.Soc.Chem.Commun.' _publ_contact_letter ; The CIF file contains 120K data for structure 1 from the paper "New type of metal squarates. Magnetic and multi-temperature X-ray study of di-hydroxy(\m^6^-squarato)manganese" by D.S.Yufit, D.J.Price, J.A.K.Howard, A.K.Powell, S.O.H.Gutschke and P.T.Wood, submitted in J.Chem.Soc.Chem.Commun.. Ref.N ; _chemical_name_systematic ; di-hydroxy-(\m^6^-squarato)manganese ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H2 Mn2 O6' _chemical_formula_weight 255.94 _chemical_melting_point ? _chemical_compound_source ? 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.381(1) _cell_length_b 10.268(5) _cell_length_c 8.579(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.85(3) _cell_angle_gamma 90.00 _cell_volume 293.4(1) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 15.9 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 4.282 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Fddd' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 4 _diffrn_standards_interval_count 96 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1235 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 24.99 _reflns_number_total 506 _reflns_number_observed 474 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MAD (Allibon, 1996)' _computing_cell_refinement 'RAFIN (Filhol,Ellis, Pryor, 1987)' _computing_data_reduction 'C5N (Lehmann, Wilson, 1987)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0300P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.001(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 504 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_obs 0.0189 _refine_ls_wR_factor_all 0.0522 _refine_ls_wR_factor_obs 0.0482 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.28882(10) 0.61601(3) 0.08010(4) 0.0068(2) Uani 1 d . . O1 O -0.1510(5) 0.61441(14) 0.2675(2) 0.0088(4) Uani 1 d . . O2 O 0.3223(5) 0.8212(2) 0.1211(2) 0.0091(4) Uani 1 d . . O3 O 0.2729(5) 0.4041(2) 0.0693(2) 0.0087(4) Uani 1 d . . C1 C 0.1439(7) 0.9185(2) 0.0543(3) 0.0076(5) Uani 1 d . . C2 C -0.0703(6) 0.5512(2) 0.3951(3) 0.0069(5) Uani 1 d . . H1 H 0.3092(102) 0.3643(33) 0.1381(46) 0.027(11) Uiso 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 0.0067(3) 0.0077(2) 0.0057(2) -0.00057(13) 0.00029(15) 0.00000(12) O1 0.0092(9) 0.0103(8) 0.0065(8) 0.0025(6) 0.0002(7) 0.0005(6) O2 0.0101(8) 0.0072(8) 0.0091(8) 0.0006(7) -0.0007(6) 0.0009(6) O3 0.0094(9) 0.0102(9) 0.0063(8) 0.0029(7) 0.0005(7) 0.0004(6) C1 0.0051(12) 0.0112(11) 0.0066(10) -0.0003(9) 0.0015(9) -0.0028(8) C2 0.0035(11) 0.0103(11) 0.0072(10) -0.0012(9) 0.0016(9) 0.0013(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 O3 2.111(2) 3_565 ? Mn1 O3 2.128(2) 3_665 ? Mn1 O2 2.136(2) . ? Mn1 O3 2.179(2) . ? Mn1 O1 2.265(2) 1_655 ? Mn1 O1 2.369(2) . ? Mn1 Mn1 3.2055(8) 3_665 ? Mn1 Mn1 3.2342(9) 3_565 ? O1 C2 1.262(3) . ? O1 Mn1 2.265(2) 1_455 ? O2 C1 1.253(3) . ? O3 Mn1 2.111(2) 3_565 ? O3 Mn1 2.128(2) 3_665 ? C1 C2 1.464(3) 2 ? C1 C2 1.466(3) 4_575 ? C2 C1 1.464(3) 2_545 ? C2 C1 1.466(3) 4_576 ? 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 O3 Mn1 O3 105.77(8) 3_565 3_665 ? O3 Mn1 O2 102.30(7) 3_565 . ? O3 Mn1 O2 99.89(7) 3_665 . ? O3 Mn1 O3 82.16(7) 3_565 . ? O3 Mn1 O3 83.82(7) 3_665 . ? O2 Mn1 O3 173.06(7) . . ? O3 Mn1 O1 170.44(7) 3_565 1_655 ? O3 Mn1 O1 80.96(6) 3_665 1_655 ? O2 Mn1 O1 82.87(6) . 1_655 ? O3 Mn1 O1 91.99(6) . 1_655 ? O3 Mn1 O1 78.90(6) 3_565 . ? O3 Mn1 O1 171.98(6) 3_665 . ? O2 Mn1 O1 85.23(6) . . ? O3 Mn1 O1 90.47(6) . . ? O1 Mn1 O1 93.67(6) 1_655 . ? O3 Mn1 Mn1 95.03(5) 3_565 3_665 ? O3 Mn1 Mn1 42.51(5) 3_665 3_665 ? O2 Mn1 Mn1 142.07(5) . 3_665 ? O3 Mn1 Mn1 41.31(5) . 3_665 ? O1 Mn1 Mn1 85.36(4) 1_655 3_665 ? O1 Mn1 Mn1 131.53(4) . 3_665 ? O3 Mn1 Mn1 41.86(5) 3_565 3_565 ? O3 Mn1 Mn1 96.02(5) 3_665 3_565 ? O2 Mn1 Mn1 143.88(5) . 3_565 ? O3 Mn1 Mn1 40.30(5) . 3_565 ? O1 Mn1 Mn1 131.84(4) 1_655 3_565 ? O1 Mn1 Mn1 83.10(4) . 3_565 ? Mn1 Mn1 Mn1 63.34(2) 3_665 3_565 ? C2 O1 Mn1 130.52(15) . 1_455 ? C2 O1 Mn1 121.64(14) . . ? Mn1 O1 Mn1 93.67(6) 1_455 . ? C1 O2 Mn1 134.6(2) . . ? Mn1 O3 Mn1 105.77(8) 3_565 3_665 ? Mn1 O3 Mn1 97.84(7) 3_565 . ? Mn1 O3 Mn1 96.18(7) 3_665 . ? O2 C1 C2 134.3(2) . 2 ? O2 C1 C2 135.9(2) . 4_575 ? C2 C1 C2 89.8(2) 2 4_575 ? O1 C2 C1 135.6(2) . 2_545 ? O1 C2 C1 134.3(2) . 4_576 ? C1 C2 C1 90.2(2) 2_545 4_576 ? _refine_diff_density_max 0.417 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.082