####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 620314' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Cl3 Cr Mn3 N12 O6' _chemical_formula_weight 1049.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 #No.148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 18.222(3) _cell_length_b 18.222(3) _cell_length_c 32.411(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9320(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 7.788 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min '0.4082 (relative)' _exptl_absorpt_correction_T_max '1.0000 (relative)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method '0.3 deg./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14112 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 59.95 _reflns_number_total 3039 _reflns_number_gt 2552 _reflns_threshold_expression >2sigma(I) _computing_data_collection SAINT _computing_cell_refinement SAINT _computing_data_reduction SAINT _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 w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+110.7076P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3039 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.6667 0.3333 0.12297(4) 0.0156(4) Uani 1 d S . . Mn1 Mn 0.48080(6) 0.17420(6) 0.07788(3) 0.0178(3) Uani 1 d . . . Cl1 Cl 0.41871(10) 0.18574(10) 0.01449(5) 0.0342(4) Uani 1 d . . . O1 O 0.5902(2) 0.2404(2) 0.16019(11) 0.0210(9) Uani 1 d . . . N2 N 0.5115(3) 0.1904(3) 0.14531(13) 0.0190(11) Uani 1 d . . . C3 C 0.4538(4) 0.1434(4) 0.17077(18) 0.0268(15) Uani 1 d . . . H3 H 0.4662 0.1400 0.1989 0.032 Uiso 1 calc R . . C4 C 0.3677(4) 0.0948(4) 0.15465(18) 0.0277(15) Uani 1 d . . . C5 C 0.2986(4) 0.0423(5) 0.1793(2) 0.0436(19) Uani 1 d . . . H5 H 0.3074 0.0353 0.2076 0.052 Uiso 1 calc R . . C6 C 0.2181(5) 0.0005(5) 0.1634(2) 0.049(2) Uani 1 d . . . H6 H 0.1707 -0.0350 0.1802 0.059 Uiso 1 calc R . . C7 C 0.2086(4) 0.0118(4) 0.1228(2) 0.0432(19) Uani 1 d . . . H7 H 0.1537 -0.0162 0.1108 0.052 Uiso 1 calc R . . C8 C 0.2787(4) 0.0641(4) 0.0984(2) 0.0325(16) Uani 1 d . . . H8 H 0.2705 0.0711 0.0701 0.039 Uiso 1 calc R . . N9 N 0.3575(3) 0.1047(3) 0.11407(16) 0.0258(12) Uani 1 d . . . O11 O 0.6857(2) 0.2560(2) 0.08566(11) 0.0207(9) Uani 1 d . . . N12 N 0.6122(3) 0.1852(3) 0.07588(13) 0.0162(10) Uani 1 d . . . C13 C 0.6160(4) 0.1210(4) 0.06556(17) 0.0219(14) Uani 1 d . . . H13 H 0.6691 0.1235 0.0628 0.026 Uiso 1 calc R . . C14 C 0.5346(4) 0.0397(3) 0.05763(16) 0.0168(13) Uani 1 d . . . C15 C 0.5369(4) -0.0325(4) 0.04610(16) 0.0221(14) Uani 1 d . . . H15 H 0.5891 -0.0320 0.0433 0.027 Uiso 1 calc R . . C16 C 0.4596(4) -0.1057(4) 0.03883(18) 0.0304(16) Uani 1 d . . . H16 H 0.4578 -0.1569 0.0312 0.037 Uiso 1 calc R . . C17 C 0.3855(4) -0.1030(4) 0.04283(17) 0.0304(16) Uani 1 d . . . H17 H 0.3321 -0.1522 0.0380 0.036 Uiso 1 calc R . . C18 C 0.3905(4) -0.0278(4) 0.05395(17) 0.0301(16) Uani 1 d . . . H18 H 0.3392 -0.0265 0.0564 0.036 Uiso 1 calc R . . N19 N 0.4649(3) 0.0450(3) 0.06162(13) 0.0203(11) Uani 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 Cr1 0.0151(6) 0.0151(6) 0.0166(8) 0.000 0.000 0.0076(3) Mn1 0.0150(5) 0.0166(5) 0.0212(5) -0.0007(4) -0.0012(4) 0.0074(4) Cl1 0.0420(10) 0.0301(9) 0.0318(8) -0.0040(7) -0.0123(7) 0.0191(8) O1 0.019(2) 0.021(2) 0.026(2) 0.0041(17) 0.0006(17) 0.012(2) N2 0.017(3) 0.014(3) 0.022(3) 0.002(2) 0.002(2) 0.005(2) C3 0.026(4) 0.023(4) 0.022(3) 0.001(3) 0.002(3) 0.005(3) C4 0.024(4) 0.019(3) 0.030(4) -0.006(3) 0.005(3) 0.003(3) C5 0.022(4) 0.050(5) 0.041(4) -0.009(4) 0.007(3) 0.004(4) C6 0.030(5) 0.049(5) 0.040(4) -0.007(4) 0.026(3) -0.002(4) C7 0.011(4) 0.034(4) 0.069(5) -0.010(4) 0.005(3) 0.000(3) C8 0.019(4) 0.041(4) 0.032(4) -0.005(3) 0.003(3) 0.011(3) N9 0.011(3) 0.016(3) 0.042(3) -0.008(2) 0.003(2) 0.001(2) O11 0.017(2) 0.010(2) 0.029(2) -0.0030(17) 0.0009(17) 0.0029(18) N12 0.019(3) 0.011(3) 0.020(2) -0.004(2) 0.004(2) 0.009(2) C13 0.021(3) 0.023(4) 0.025(3) 0.006(3) 0.001(3) 0.014(3) C14 0.024(3) 0.012(3) 0.015(3) 0.005(2) 0.006(2) 0.009(3) C15 0.026(4) 0.021(4) 0.021(3) 0.006(3) -0.001(3) 0.013(3) C16 0.043(5) 0.021(4) 0.028(3) -0.004(3) -0.006(3) 0.017(3) C17 0.043(4) 0.019(4) 0.016(3) 0.002(3) -0.005(3) 0.006(3) C18 0.032(4) 0.035(4) 0.021(3) 0.000(3) 0.002(3) 0.014(3) N19 0.019(3) 0.018(3) 0.021(2) 0.001(2) -0.001(2) 0.007(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 Cr1 O1 1.976(4) 2_655 ? Cr1 O1 1.976(4) . ? Cr1 O1 1.976(4) 3_665 ? Cr1 O11 2.013(4) 3_665 ? Cr1 O11 2.013(4) 2_655 ? Cr1 O11 2.013(4) . ? Mn1 N2 2.239(5) . ? Mn1 O11 2.254(4) 3_665 ? Mn1 N9 2.277(5) . ? Mn1 N19 2.285(5) . ? Mn1 N12 2.300(5) . ? Mn1 Cl1 2.4050(17) . ? O1 N2 1.346(6) . ? N2 C3 1.273(7) . ? C3 C4 1.460(9) . ? C4 N9 1.353(8) . ? C4 C5 1.391(9) . ? C5 C6 1.372(10) . ? C6 C7 1.356(10) . ? C7 C8 1.394(9) . ? C8 N9 1.343(8) . ? O11 N12 1.353(6) . ? O11 Mn1 2.254(4) 2_655 ? N12 C13 1.253(7) . ? C13 C14 1.504(8) . ? C14 N19 1.328(7) . ? C14 C15 1.388(8) . ? C15 C16 1.393(9) . ? C16 C17 1.381(9) . ? C17 C18 1.375(9) . ? C18 N19 1.365(8) . ? 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 Cr1 O1 86.61(17) 2_655 . ? O1 Cr1 O1 86.61(17) 2_655 3_665 ? O1 Cr1 O1 86.61(17) . 3_665 ? O1 Cr1 O11 178.84(15) 2_655 3_665 ? O1 Cr1 O11 92.24(15) . 3_665 ? O1 Cr1 O11 93.50(15) 3_665 3_665 ? O1 Cr1 O11 93.50(15) 2_655 2_655 ? O1 Cr1 O11 178.84(16) . 2_655 ? O1 Cr1 O11 92.24(15) 3_665 2_655 ? O11 Cr1 O11 87.65(16) 3_665 2_655 ? O1 Cr1 O11 92.24(15) 2_655 . ? O1 Cr1 O11 93.50(15) . . ? O1 Cr1 O11 178.84(16) 3_665 . ? O11 Cr1 O11 87.65(16) 3_665 . ? O11 Cr1 O11 87.65(16) 2_655 . ? N2 Mn1 O11 75.49(15) . 3_665 ? N2 Mn1 N9 71.50(17) . . ? O11 Mn1 N9 121.76(16) 3_665 . ? N2 Mn1 N19 104.82(16) . . ? O11 Mn1 N19 147.14(16) 3_665 . ? N9 Mn1 N19 87.97(17) . . ? N2 Mn1 N12 80.52(16) . . ? O11 Mn1 N12 76.80(15) 3_665 . ? N9 Mn1 N12 139.27(17) . . ? N19 Mn1 N12 70.98(16) . . ? N2 Mn1 Cl1 156.93(13) . . ? O11 Mn1 Cl1 95.88(10) 3_665 . ? N9 Mn1 Cl1 96.43(14) . . ? N19 Mn1 Cl1 94.02(12) . . ? N12 Mn1 Cl1 118.86(12) . . ? N2 O1 Cr1 114.6(3) . . ? C3 N2 O1 117.7(5) . . ? C3 N2 Mn1 118.4(4) . . ? O1 N2 Mn1 123.4(3) . . ? N2 C3 C4 116.9(5) . . ? N9 C4 C5 120.9(6) . . ? N9 C4 C3 116.4(5) . . ? C5 C4 C3 122.7(6) . . ? C6 C5 C4 120.9(7) . . ? C7 C6 C5 117.6(6) . . ? C6 C7 C8 120.7(6) . . ? N9 C8 C7 121.7(6) . . ? C8 N9 C4 118.3(5) . . ? C8 N9 Mn1 126.7(4) . . ? C4 N9 Mn1 114.3(4) . . ? N12 O11 Cr1 111.9(3) . . ? N12 O11 Mn1 138.0(3) . 2_655 ? Cr1 O11 Mn1 109.70(16) . 2_655 ? C13 N12 O11 117.6(5) . . ? C13 N12 Mn1 117.9(4) . . ? O11 N12 Mn1 124.6(3) . . ? N12 C13 C14 118.6(5) . . ? N19 C14 C15 125.4(5) . . ? N19 C14 C13 114.8(5) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 117.2(6) . . ? C17 C16 C15 119.3(6) . . ? C18 C17 C16 118.7(6) . . ? N19 C18 C17 123.8(6) . . ? C14 N19 C18 115.6(5) . . ? C14 N19 Mn1 117.7(4) . . ? C18 N19 Mn1 126.7(4) . . ? _diffrn_measured_fraction_theta_max 0.328 _diffrn_reflns_theta_full 59.95 _diffrn_measured_fraction_theta_full 0.328 _refine_diff_density_max 0.522 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.101 #===END