#------------------------------------------------------------------------------ #$Date: 2016-02-16 00:06:40 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176451 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/00/03/5000368.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_5000368 loop_ _publ_author_name 'Guillem Arom\'i' 'Michael J. Knapp' 'Juan-Pablo Claude' 'John C. Huffman' 'David N. Hendrickson' 'George Christou' _publ_section_title ; High-Spin Molecules: Hexanuclear MnIII Clusters with [Mn6O4X4]6+ (X = Cl-, Br-) Face-Capped Octahedral Cores and S= 12 Ground States ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 5489 _journal_page_last 5499 _journal_paper_doi 10.1021/ja983446c _journal_volume 121 _journal_year 1999 _chemical_formula_moiety ? _chemical_formula_sum 'C31 H24 Cl3 Mn O4' _chemical_formula_weight 621.825 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 102.689(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.888(3) _cell_length_b 8.3476(18) _cell_length_c 24.702(5) _cell_measurement_reflns_used 31 _cell_measurement_temperature 105.15 _cell_measurement_theta_max 11.19 _cell_measurement_theta_min 9.76 _cell_volume 2793.8(10) _diffrn_ambient_temperature 20 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 5167 _diffrn_reflns_theta_full 0 _diffrn_reflns_theta_max 25.0001 _diffrn_reflns_theta_min 2.58206 _diffrn_standards_decay_% 1.5 _diffrn_standards_interval_count 401 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 0.7946 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_crystal_colour 'red/dark brown' _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1272 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .22 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_extinction_coef -0.00000003(5) _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_extinction_method Zachariasen _refine_ls_goodness_of_fit_ref 1.4551 _refine_ls_hydrogen_treatment ? _refine_ls_matrix_type full _refine_ls_number_parameters 449 _refine_ls_number_reflns ? _refine_ls_R_factor_gt 0.0533 _refine_ls_shift/su_max 0.2711 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w^-1^=\s^2^(F)+(.03F)^2^ _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0456 _reflns_number_gt 3211 _reflns_number_total 4915 _reflns_threshold_expression F^2^>2.33\s(F^2^) _cod_depositor_comments ; The following automatic conversions were performed: '_cell_measurement_temperature' value '-168C' was changed to '105.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum 'C31 H24 Cl3 Mn1 O4' _cod_database_code 5000368 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z -x,-y,-z 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_disorder_group _atom_site_disorder_assembly MN1 MN 0.38002(5) 0.18395(10) 0.07304(3) 0.0162(3) Uani 1 0 . CL2 CL 0.27457(9) 0.40913(16) 0.05018(5) 0.0199(4) Uani 1 0 . O3 O 0.4996(2) 0.2939(4) 0.10216(13) 0.0195(12) Uani 1 0 . C4 C 0.5656(3) 0.3442(6) 0.0770(2) 0.0159(16) Uani 1 0 . C5 C 0.5621(4) 0.3173(6) 0.0209(2) 0.0171(16) Uani 1 0 . C6 C 0.4888(4) 0.2259(6) 0.98731(19) 0.0176(17) Uani 1 0 . O7 O 0.4177(2) 0.1577(4) 0.00429(13) 0.0202(12) Uani 1 0 . C8 C 0.6508(3) 0.4270(6) 0.1137(2) 0.0169(17) Uani 1 0 . C9 C 0.7241(4) 0.5066(7) 0.0938(2) 0.023(2) Uani 1 0 . C10 C 0.8012(4) 0.5806(7) 0.1302(2) 0.026(2) Uani 1 0 . C11 C 0.8062(4) 0.5771(7) 0.1863(2) 0.028(2) Uani 1 0 . C12 C 0.7351(4) 0.4998(8) 0.2069(2) 0.033(2) Uani 1 0 . C13 C 0.6567(4) 0.4251(8) 0.1710(2) 0.027(2) Uani 1 0 . C14 C 0.4877(3) 0.1947(6) 0.92750(19) 0.0172(16) Uani 1 0 . C15 C 0.5503(4) 0.2739(7) 0.8997(2) 0.024(2) Uani 1 0 . C16 C 0.5466(4) 0.2435(7) -0.1556(2) 0.0234(19) Uani 1 0 . C17 C 0.4801(4) 0.1342(7) 0.8159(2) 0.0227(19) Uani 1 0 . C18 C 0.4169(4) 0.0544(7) 0.8430(2) 0.0240(19) Uani 1 0 . C19 C 0.4205(4) 0.0852(7) 0.8987(2) 0.0219(19) Uani 1 0 . O20 O 0.2819(2) 0.0258(4) 0.04943(13) 0.0180(12) Uani 1 0 . C21 C 0.2176(4) 0.9763(6) 0.0760(2) 0.0183(17) Uani 1 0 . C22 C 0.2254(4) 0.0028(6) 0.1331(2) 0.0191(18) Uani 1 0 . C23 C 0.3051(4) 0.0821(6) 0.1669(2) 0.0175(17) Uani 1 0 . O24 O 0.3707(2) 0.1570(4) 0.14814(13) 0.0193(12) Uani 1 0 . C25 C 0.1353(4) 0.8807(6) 0.0443(2) 0.0173(17) Uani 1 0 . C26 C 0.1499(4) 0.7893(7) 0.9990(2) 0.0235(19) Uani 1 0 . C27 C 0.0734(4) 0.6994(7) 0.9686(2) 0.029(2) Uani 1 0 . C28 C 0.9822(4) 0.7014(7) 0.9814(2) 0.025(2) Uani 1 0 . C29 C 0.9656(4) 0.7916(6) 0.0256(2) 0.0200(18) Uani 1 0 . C30 C 0.0432(4) 0.8802(6) 0.0570(2) 0.0185(18) Uani 1 0 . C31 C 0.3208(4) 0.0809(6) 0.2284(2) 0.0171(17) Uani 1 0 . C32 C 0.4025(4) 0.1615(6) 0.2596(2) 0.0186(17) Uani 1 0 . C33 C 0.4196(4) 0.1614(7) 0.3171(2) 0.0216(18) Uani 1 0 . C34 C 0.3573(4) 0.0802(6) 0.3443(2) 0.0236(19) Uani 1 0 . C35 C 0.2761(4) 1.0006(7) 0.3138(2) 0.025(2) Uani 1 0 . C36 C 0.2585(4) 0.9987(7) 0.2566(2) 0.0242(19) Uani 1 0 . CL37 CL 1.02281(12) 1.1926(2) 0.18515(7) 0.0547(7) Uani 1 0 . C38 C 0.8966(6) 1.1745(9) 0.1768(4) 0.050(3) Uani 1 0 . CL39 CL 0.85123(13) 0.9864(2) 0.15180(8) 0.0580(8) Uani 1 0 . H1 H 0.615(3) 0.355(5) 0.0071(17) 0.006(12) Uiso 1 0 . H2 H 0.725(4) 0.501(7) 0.062(2) 0.028(18) Uiso 1 0 . H3 H 0.852(4) 0.623(7) 0.114(2) 0.041(18) Uiso 1 0 . H4 H 0.862(4) 0.625(6) 0.209(2) 0.025(15) Uiso 1 0 . H5 H 0.735(4) 0.490(7) 0.243(2) 0.043(19) Uiso 1 0 . H6 H 0.612(4) 0.373(7) 0.183(2) 0.037(18) Uiso 1 0 . H7 H 0.598(3) 0.324(5) 0.9169(18) 0.005(13) Uiso 1 0 . H8 H 0.588(3) 0.280(6) -0.173(2) 0.022(15) Uiso 1 0 . H9 H 0.479(3) 0.118(5) 0.7805(18) 0.005(12) Uiso 1 0 . H10 H 0.372(3) 0.973(6) 0.8230(19) 0.015(13) Uiso 1 0 . H11 H 0.383(4) 0.033(6) -0.084(2) 0.021(15) Uiso 1 0 . H12 H 0.176(3) 0.962(5) 0.1494(16) -0.007(10) Uiso 1 0 . H13 H 0.213(3) 0.793(5) 0.9908(16) 0.003(11) Uiso 1 0 . H14 H 0.085(4) 0.629(6) 0.938(2) 0.032(16) Uiso 1 0 . H15 H 0.930(4) 0.648(6) 0.965(2) 0.026(16) Uiso 1 0 . H16 H 0.901(3) 0.797(6) 0.0340(18) 0.018(13) Uiso 1 0 . H17 H 0.031(3) 0.947(6) 0.0862(18) 0.011(13) Uiso 1 0 . H18 H 0.445(4) 0.211(6) 0.241(2) 0.028(16) Uiso 1 0 . H19 H 0.474(4) 0.219(6) 0.339(2) 0.028(15) Uiso 1 0 . H20 H 0.366(3) 0.086(5) 0.3833(18) 0.007(12) Uiso 1 0 . H21 H 0.235(3) 0.941(5) 0.3311(17) 0.002(11) Uiso 1 0 . H22 H 0.204(3) -0.052(6) 0.2364(18) 0.009(12) Uiso 1 0 . H23 H 0.881(5) 1.195(10) 0.216(3) 0.10(3) Uiso 1 0 . H24 H 0.871(6) 1.229(10) 0.148(3) 0.09(3) Uiso 1 0 . 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 MN1 0.0175(15) 0.0189(7) 0.012(3) -0.0047(4) 0.0032(3) -0.0013(4) CL2 0.0206(18) 0.0204(9) 0.018(4) -0.0020(6) 0.0033(5) 0.0013(6) O3 0.021(3) 0.022(2) 0.016(4) -0.0060(17) 0.0043(15) -0.0019(17) C4 0.018(3) 0.009(3) 0.020(6) -0.002(2) 0.003(2) 0.002(2) C5 0.017(3) 0.016(3) 0.017(5) 0.000(3) 0.003(2) 0.004(2) C6 0.019(3) 0.016(3) 0.018(5) 0.001(2) 0.007(2) 0.004(2) O7 0.018(2) 0.025(2) 0.017(5) -0.0061(17) 0.0036(15) -0.0045(17) C8 0.014(3) 0.018(3) 0.018(5) 0.003(2) 0.000(2) -0.004(2) C9 0.027(4) 0.022(3) 0.019(6) -0.001(3) 0.006(3) -0.000(3) C10 0.023(4) 0.026(3) 0.027(7) -0.007(3) 0.003(3) -0.003(3) C11 0.018(3) 0.030(4) 0.032(8) -0.006(3) -0.002(3) -0.011(3) C12 0.028(4) 0.049(5) 0.020(6) -0.006(3) 0.002(3) -0.008(3) C13 0.019(3) 0.041(4) 0.022(6) -0.010(3) 0.004(2) -0.004(3) C14 0.018(3) 0.020(3) 0.014(4) 0.002(3) 0.004(2) 0.002(2) C15 0.019(3) 0.035(4) 0.017(5) -0.004(3) -0.000(2) -0.005(3) C16 0.024(4) 0.027(3) 0.022(6) 0.001(3) 0.011(3) 0.004(3) C17 0.032(4) 0.024(3) 0.012(4) 0.008(3) 0.005(2) 0.000(2) C18 0.021(3) 0.029(4) 0.021(6) -0.002(3) 0.000(2) -0.004(3) C19 0.024(4) 0.022(3) 0.021(6) -0.006(3) 0.007(2) -0.001(3) O20 0.020(3) 0.019(2) 0.017(4) -0.0054(17) 0.0066(16) -0.0034(17) C21 0.020(3) 0.013(3) 0.022(6) 0.001(2) 0.005(2) 0.004(2) C22 0.019(3) 0.023(3) 0.015(4) 0.000(2) 0.004(2) 0.004(2) C23 0.019(3) 0.014(3) 0.018(5) 0.005(2) 0.003(2) 0.002(2) O24 0.022(3) 0.021(2) 0.015(4) -0.0065(17) 0.0039(15) -0.0005(16) C25 0.019(3) 0.016(3) 0.015(4) -0.001(2) 0.001(2) 0.004(2) C26 0.017(3) 0.025(3) 0.027(7) 0.002(3) 0.003(2) -0.003(3) C27 0.029(4) 0.023(3) 0.032(8) -0.006(3) 0.001(3) -0.012(3) C28 0.027(4) 0.014(3) 0.031(8) -0.005(3) -0.001(3) 0.002(3) C29 0.021(3) 0.018(3) 0.019(5) -0.002(3) 0.001(2) 0.009(2) C30 0.024(4) 0.013(3) 0.017(5) 0.002(2) 0.002(2) 0.005(2) C31 0.019(3) 0.017(3) 0.016(5) 0.002(2) 0.004(2) 0.003(2) C32 0.019(3) 0.017(3) 0.018(5) 0.001(2) 0.002(2) 0.001(2) C33 0.019(3) 0.024(3) 0.020(5) 0.001(3) -0.001(2) -0.002(3) C34 0.040(5) 0.015(3) 0.015(5) 0.008(3) 0.004(3) 0.000(2) C35 0.033(4) 0.023(3) 0.021(6) -0.007(3) 0.009(3) 0.005(3) C36 0.025(4) 0.024(3) 0.022(6) -0.007(3) 0.002(3) -0.001(3) CL37 0.038(3) 0.075(3) 0.053(13) -0.0120(10) 0.0147(8) -0.0292(11) C38 0.056(7) 0.023(4) 0.069(17) -0.003(4) 0.009(4) -0.008(4) CL39 0.058(5) 0.0458(18) 0.080(19) -0.0220(10) 0.0353(10) -0.0325(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MN Mn 0.295 0.729 'International Tables Vol. IV (1974) Table 2.2B' CL Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' 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 MN1 CL2 2.3735(16) . . no MN1 O3 1.896(3) . . no MN1 O7 1.896(3) . . no MN1 O20 1.895(3) . . no MN1 O24 1.901(3) . . no CL37 C38 1.726(8) . . no CL39 C38 1.754(7) . . no O3 C4 1.285(5) . . no O7 C6 1.288(6) . 1_554 no O20 C21 1.287(6) . 1_545 no O24 C23 1.273(6) . . no C4 C5 1.393(6) . . no C4 C8 1.493(6) . . no C5 C6 1.392(7) . 1_554 no C6 C14 1.497(6) . . no C8 C9 1.392(7) . . no C8 C13 1.400(7) . . no C9 C10 1.383(7) . . no C10 C11 1.375(8) . . no C11 C12 1.367(8) . . no C12 C13 1.392(7) . . no C14 C15 1.389(7) . . no C14 C19 1.386(7) . . no C15 C16 1.379(7) . 1_556 no C16 C17 1.376(8) . 1_554 no C17 C18 1.386(7) . . no C18 C19 1.389(7) . . no C21 C22 1.407(7) . 1_565 no C21 C25 1.472(7) . . no C22 C23 1.398(7) . . no C23 C31 1.487(6) . . no C25 C26 1.406(7) . 1_554 no C25 C30 1.382(7) . . no C26 C27 1.380(7) . . no C27 C28 1.372(7) . 1_455 no C28 C29 1.386(7) . 1_556 no C29 C30 1.394(7) . 1_655 no C31 C32 1.397(7) . . no C31 C36 1.404(7) . 1_545 no C32 C33 1.387(7) . . no C33 C34 1.384(7) . . no C34 C35 1.381(7) . 1_545 no C35 C36 1.379(7) . . no C5 H1 0.93(4) . . no C9 H2 0.78(5) . . no C10 H3 0.96(5) . . no C11 H4 0.94(5) . . no C12 H5 0.89(6) . . no C13 H6 0.87(5) . . no C15 H7 0.81(4) . . no C16 H8 0.85(5) . . no C17 H9 0.88(4) . . no C18 H10 0.98(5) . 1_545 no C19 H11 0.87(5) . 1_556 no C22 H12 0.93(4) . 1_545 no C26 H13 0.94(4) . . no C27 H14 0.99(5) . . no C28 H15 0.88(5) . . no C29 H16 0.97(4) . . no C30 H17 0.95(4) . . no C32 H18 0.93(5) . . no C33 H19 0.95(5) . . no C34 H20 0.94(4) . . no C35 H21 0.93(4) . . no C36 H22 0.92(4) . 1_565 no C38 H23 1.05(7) . . no C38 H24 0.85(7) . . no