#------------------------------------------------------------------------------ #$Date: 2020-11-08 04:17:25 +0200 (Sun, 08 Nov 2020) $ #$Revision: 259042 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/94/4339483.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_4339483 loop_ _publ_author_name 'Feng, Patrick L.' 'Beedle, Christopher C.' 'Wernsdorfer, Wolfgang' 'Koo, Changhyun' 'Nakano, Motohiro' 'Hill, Stephen' 'Hendrickson, David N.' _publ_section_title ; Heterometallic cubane single-molecule magnets. ; _journal_issue 20 _journal_name_full 'Inorganic chemistry' _journal_page_first 8126 _journal_page_last 8128 _journal_paper_doi 10.1021/ic7012107 _journal_volume 46 _journal_year 2007 _chemical_formula_moiety 'C41 H35 Cl6 Mn3 N12 Ni1 O10' _chemical_formula_sum 'C41 H35 Cl6 Mn3 N12 Ni O10' _chemical_formula_weight 1292.015 _space_group.centring_type P _space_group_crystal_system rhombohedral _space_group_IT_number 161 _space_group_name_Hall 'R 3 -2"c' _space_group_name_H-M_alt 'R 3 c :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 15.453(4) _cell_length_b 15.453 _cell_length_c 38.060(10) _cell_measurement_reflns_used 17761 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.02 _cell_measurement_theta_min 2.63 _cell_volume 7871(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ORTEP32 _computing_publication_material WINGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_refln_scan_rate 10 _diffrn_refln_scan_width 0.3 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 17761 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 2.63 _exptl_absorpt_coefficient_mu 1.430 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour red-brown _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3816 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _platon_squeeze_details ; SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent contributions. Total electron count found = 673/unit cell. Calculated for 2 chloroform (the re'xtal solvent) = 696/unit cell. The intensive properties (density, F(000), etc.) reflect these contributions. ; _refine_diff_density_max 0.337 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 3097 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0367 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+2.4088P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0990 _refine_ls_wR_factor_ref 0.1002 _reflns_number_gt 2870 _reflns_number_total 3097 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic7012107-file001.cif _cod_data_source_block import _cod_depositor_comments ; Removed the _space_group.IT_number data item since it had an incorrect value, changed the value of the _symmetry_cell_setting data item from 'trigonal' to 'rhombohedral' and renamed several space group related data items. Antanas Vaitkus, 2020-11-08 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according to /usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius The following automatic conversions were performed: '_space_group.centring_type' value 'primitive' was replaced with the value 'P' as specified in the replacement file '/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'. Automatic conversion script Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas ; _cod_original_cell_volume 7870(3) _cod_original_sg_symbol_H-M R3c _cod_original_formula_sum 'C41 H35 Cl6 Mn3 N12 Ni1 O10' _cod_database_code 4339483 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, z+1/2' '-x+y, -x, z' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, -x+1/3, z+1/3' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, -x+2/3, z+2/3' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 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 N3 N 0.2004(3) 0.2682(3) 0.92904(10) 0.0602(10) Uani 1 1 d . Ni1 Ni 0.3333 0.6667 0.98881(2) 0.0336(2) Uani 1 3 d S Mn1 Mn 0.25634(4) 0.53631(4) 0.918217(14) 0.03466(17) Uani 1 1 d . O4 O 0.21516(18) 0.59927(18) 0.95439(10) 0.0352(5) Uani 1 1 d . O3 O 0.3333 0.6667 0.89958(13) 0.0351(10) Uani 1 3 d S O2 O 0.3210(2) 0.48311(18) 0.88881(7) 0.0418(7) Uani 1 1 d . N1 N 0.1824(2) 0.4076(2) 0.94167(9) 0.0412(8) Uani 1 1 d . N2 N 0.1931(3) 0.3374(2) 0.93435(9) 0.0425(8) Uani 1 1 d . N4 N 0.2262(2) 0.6795(2) 1.01544(8) 0.0349(6) Uani 1 1 d . O1 O 0.13510(19) 0.5217(2) 0.88499(8) 0.0443(6) Uani 1 1 d . C009 C 0.0487(3) 0.6068(3) 1.02153(10) 0.0406(8) Uani 1 1 d . H009 H -0.0154 0.5605 1.0140 0.049 Uiso 1 1 calc R C010 C 0.1325(2) 0.6176(2) 1.00388(11) 0.0349(8) Uani 1 1 d . C011 C 0.2376(3) 0.7359(3) 1.04377(11) 0.0417(9) Uani 1 1 d . H011 H 0.3018 0.7798 1.0518 0.050 Uiso 1 1 calc R C012 C 0.4405(3) 0.4600(3) 0.85854(10) 0.0435(9) Uani 1 1 d . C013 C 0.4044(4) 0.2980(3) 0.83931(13) 0.0589(12) Uani 1 1 d . H013 H 0.3615 0.2292 0.8386 0.071 Uiso 1 1 calc R C014 C 0.0628(3) 0.6661(3) 1.05024(11) 0.0471(10) Uani 1 1 d . H014 H 0.0080 0.6617 1.0620 0.057 Uiso 1 1 calc R C015 C 0.5280(3) 0.5017(3) 0.83993(13) 0.0557(12) Uani 1 1 d . H015 H 0.5692 0.5707 0.8398 0.067 Uiso 1 1 calc R C016 C 0.1232(3) 0.5566(3) 0.97206(12) 0.0403(9) Uani 1 1 d . H01A H 0.1034 0.4888 0.9790 0.048 Uiso 1 1 calc R H01B H 0.0723 0.5541 0.9565 0.048 Uiso 1 1 calc R C017 C 0.4124(3) 0.5267(3) 0.87909(10) 0.0414(9) Uani 1 1 d . C018 C 0.4933(4) 0.3387(4) 0.82170(13) 0.0633(13) Uani 1 1 d . H018 H 0.5115 0.2972 0.8101 0.076 Uiso 1 1 calc R C019 C 0.1568(3) 0.7312(3) 1.06149(11) 0.0450(9) Uani 1 1 d . H019 H 0.1670 0.7720 1.0808 0.054 Uiso 1 1 calc R C020 C 0.5568(3) 0.4417(3) 0.82099(14) 0.0609(13) Uani 1 1 d . H020 H 0.6164 0.4702 0.8084 0.073 Uiso 1 1 calc R C021 C 0.3766(3) 0.3574(3) 0.85823(12) 0.0551(11) Uani 1 1 d . H021 H 0.3164 0.3289 0.8704 0.066 Uiso 1 1 calc R 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 N3 0.082(3) 0.046(2) 0.069(2) 0.0056(18) 0.013(2) 0.044(2) Ni1 0.0249(3) 0.0249(3) 0.0510(5) 0.000 0.000 0.01244(13) Mn1 0.0262(3) 0.0255(3) 0.0524(3) -0.0018(2) 0.0002(3) 0.0131(2) O4 0.0279(14) 0.0293(13) 0.0524(14) -0.0020(11) 0.0007(12) 0.0173(12) O3 0.0297(15) 0.0297(15) 0.046(3) 0.000 0.000 0.0149(7) O2 0.0377(14) 0.0316(14) 0.0554(16) -0.0068(11) 0.0013(12) 0.0169(13) N1 0.0327(17) 0.0287(17) 0.062(2) 0.0011(15) 0.0026(15) 0.0152(15) N2 0.0390(18) 0.0292(18) 0.058(2) 0.0011(15) 0.0026(16) 0.0164(15) N4 0.0311(16) 0.0269(16) 0.0472(17) 0.0042(13) 0.0018(13) 0.0148(14) O1 0.0337(14) 0.0325(14) 0.0717(18) -0.0044(12) -0.0122(12) 0.0204(12) C009 0.0280(18) 0.0359(19) 0.060(2) 0.0042(17) 0.0033(16) 0.0173(16) C010 0.0285(17) 0.0211(17) 0.056(2) 0.0028(15) -0.0002(16) 0.0127(14) C011 0.044(2) 0.0269(18) 0.052(2) 0.0053(16) -0.0020(18) 0.0164(17) C012 0.043(2) 0.039(2) 0.048(2) -0.0066(17) 0.0012(18) 0.0203(19) C013 0.061(3) 0.029(2) 0.074(3) -0.011(2) 0.017(2) 0.013(2) C014 0.045(2) 0.046(2) 0.057(2) 0.0066(19) 0.008(2) 0.028(2) C015 0.043(2) 0.038(2) 0.078(3) -0.008(2) 0.011(2) 0.0137(19) C016 0.024(2) 0.037(2) 0.058(2) -0.0025(17) 0.0021(17) 0.0148(16) C017 0.034(2) 0.047(2) 0.048(2) -0.0032(18) -0.0001(17) 0.0242(19) C018 0.066(3) 0.057(3) 0.065(3) -0.018(2) 0.008(2) 0.029(2) C019 0.045(2) 0.047(2) 0.049(2) -0.0001(18) 0.0017(18) 0.027(2) C020 0.050(3) 0.047(3) 0.072(3) -0.007(2) 0.016(2) 0.014(2) C021 0.047(2) 0.044(2) 0.063(3) 0.000(2) 0.010(2) 0.014(2) 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' Mn Mn 0.3368 0.7283 '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' Ni Ni 0.3393 1.1124 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N4 Ni1 N4 97.31(12) . 4_565 N4 Ni1 N4 97.31(12) . 2_665 N4 Ni1 N4 97.31(12) 4_565 2_665 N4 Ni1 O4 78.87(12) . . N4 Ni1 O4 161.16(11) 4_565 . N4 Ni1 O4 101.47(11) 2_665 . N4 Ni1 O4 101.47(11) . 4_565 N4 Ni1 O4 78.87(12) 4_565 4_565 N4 Ni1 O4 161.16(11) 2_665 4_565 O4 Ni1 O4 83.80(14) . 4_565 N4 Ni1 O4 161.16(11) . 2_665 N4 Ni1 O4 101.47(11) 4_565 2_665 N4 Ni1 O4 78.87(12) 2_665 2_665 O4 Ni1 O4 83.80(14) . 2_665 O4 Ni1 O4 83.80(14) 4_565 2_665 O3 Mn1 O2 92.98(12) . . O3 Mn1 N1 174.62(19) . . O2 Mn1 N1 89.70(12) . . O3 Mn1 O4 85.55(15) . . O2 Mn1 O4 168.05(12) . . N1 Mn1 O4 90.85(14) . . O3 Mn1 O1 86.75(11) . . O2 Mn1 O1 102.72(12) . . N1 Mn1 O1 97.21(13) . . O4 Mn1 O1 89.06(12) . . O3 Mn1 O4 74.82(14) . 2_665 O2 Mn1 O4 90.24(11) . 2_665 N1 Mn1 O4 100.52(12) . 2_665 O4 Mn1 O4 77.92(15) . 2_665 O1 Mn1 O4 158.06(9) . 2_665 O3 Mn1 Mn1 36.59(8) . 2_665 O2 Mn1 Mn1 82.51(8) . 2_665 N1 Mn1 Mn1 139.55(10) . 2_665 O4 Mn1 Mn1 89.35(8) . 2_665 O1 Mn1 Mn1 123.23(8) . 2_665 O4 Mn1 Mn1 40.31(7) 2_665 2_665 O3 Mn1 Mn1 36.59(8) . 4_565 O2 Mn1 Mn1 129.23(8) . 4_565 N1 Mn1 Mn1 141.06(10) . 4_565 O4 Mn1 Mn1 51.40(9) . 4_565 O1 Mn1 Mn1 75.70(7) . 4_565 O4 Mn1 Mn1 82.39(6) 2_665 4_565 Mn1 Mn1 Mn1 60.000(11) 2_665 4_565 C016 O4 Mn1 127.2(2) . . C016 O4 Ni1 111.5(3) . . Mn1 O4 Ni1 105.74(10) . . C016 O4 Mn1 124.9(2) . 4_565 Mn1 O4 Mn1 88.29(13) . 4_565 Ni1 O4 Mn1 92.46(9) . 4_565 Mn1 O3 Mn1 106.81(15) 4_565 2_665 Mn1 O3 Mn1 106.81(15) 4_565 . Mn1 O3 Mn1 106.81(15) 2_665 . C017 O2 Mn1 127.8(2) . . N2 N1 Mn1 122.5(3) . . N3 N2 N1 176.2(4) . . C011 N4 C010 117.9(3) . . C011 N4 Ni1 128.0(3) . . C010 N4 Ni1 113.9(2) . . C017 O1 Mn1 125.9(2) 4_565 . C014 C009 C010 118.5(4) . . N4 C010 C009 122.1(3) . . N4 C010 C016 116.2(3) . . C009 C010 C016 121.6(3) . . N4 C011 C019 122.3(4) . . C015 C012 C021 120.3(4) . . C015 C012 C017 119.8(4) . . C021 C012 C017 119.9(4) . . C018 C013 C021 121.3(4) . . C019 C014 C009 120.0(4) . . C012 C015 C020 121.2(4) . . O4 C016 C010 109.6(3) . . O1 C017 O2 127.9(4) 2_665 . O1 C017 C012 118.0(3) 2_665 . O2 C017 C012 114.0(3) . . C013 C018 C020 120.5(4) . . C014 C019 C011 119.2(4) . . C018 C020 C015 117.9(4) . . C012 C021 C013 118.7(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N3 N2 1.148(5) . Ni1 N4 2.033(3) . Ni1 N4 2.033(3) 4_565 Ni1 N4 2.033(3) 2_665 Ni1 O4 2.058(3) . Ni1 O4 2.058(3) 4_565 Ni1 O4 2.058(3) 2_665 Mn1 O3 1.8919(19) . Mn1 O2 1.936(3) . Mn1 N1 1.946(3) . Mn1 O4 1.966(3) . Mn1 O1 2.176(3) . Mn1 O4 2.375(3) 2_665 Mn1 Mn1 3.0380(11) 2_665 Mn1 Mn1 3.0380(10) 4_565 O4 C016 1.403(5) . O4 Mn1 2.375(3) 4_565 O3 Mn1 1.8919(19) 4_565 O3 Mn1 1.8919(19) 2_665 O2 C017 1.278(5) . N1 N2 1.207(5) . N4 C011 1.342(5) . N4 C010 1.349(4) . O1 C017 1.233(5) 4_565 C009 C014 1.371(6) . C009 C010 1.394(5) . C010 C016 1.497(6) . C011 C019 1.388(6) . C012 C015 1.369(6) . C012 C021 1.386(6) . C012 C017 1.519(5) . C013 C018 1.367(7) . C013 C021 1.393(6) . C014 C019 1.358(6) . C015 C020 1.410(7) . C017 O1 1.233(5) 2_665 C018 C020 1.391(6) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.103 332.4 111.9 2 0.000 0.000 0.437 14.3 -0.8 3 0.000 0.000 0.603 332.4 112.4 4 0.000 0.000 0.937 14.3 -0.8 5 0.333 0.667 0.270 334.5 112.3 6 0.333 0.667 0.770 334.5 111.9 7 0.333 0.667 0.103 15.1 -0.8 8 0.333 0.667 0.603 15.1 -0.8 9 0.667 0.333 0.436 332.9 112.0 10 0.667 0.333 0.936 332.9 112.5 11 0.666 0.333 0.270 14.9 -0.8 12 0.666 0.333 0.770 14.9 -0.8