Supplementary Material (ESI) for Dalton Transactions this journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Miyasaka, Hitoshi' 'Chang, Ho-Chol' 'Clerac, Rodolphe' 'Ishii, Tomohiko' 'Kitagawa, Susumu' 'Yamashita, Masahiro' _publ_contact_author_name 'Dr Hitoshi Miyasaka' _publ_contact_author_address ; Department of Chemistry Tokyo Metropolitan University 1-1 Minamiohsawa Hachioji Tokyo JAPAN ; _publ_contact_author_email 'MIYASAKA@COMP.METRO-U.AC.JP' _publ_section_title ; Out-of-Plane dimers of Mn(III) quadridentate Schiff-Base complexes with saltmen2- and naphtmen2- ligands**: structure analysis and ferromagnetic exchange ; data_[Mn(saltmen)(H2O)]ClO4 _database_code_CSD 168755 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H48 Cl2 N4 Mn2 O14 ' _chemical_formula_moiety '?' _chemical_formula_weight 989.62 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 20.830(1) _cell_length_b 13.596(1) _cell_length_c 7.526(1) _cell_angle_alpha 90 _cell_angle_beta 89.818(8) _cell_angle_gamma 90 _cell_volume 2131.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024.00 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5264 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9996 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.30 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4900 _reflns_number_gt 2859 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1385 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4900 _refine_ls_number_parameters 280 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0502 _refine_diff_density_max 0.89 _refine_diff_density_min -0.76 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.44408(2) 0.00415(4) 0.33784(7) 0.0303(1) Uani 1.00 d . . . Cl(1) Cl 0.67328(5) -0.33346(8) -0.0205(2) 0.0540(3) Uani 1.00 d . . . O(1) O 0.5243(1) 0.0679(2) 0.3796(3) 0.0358(6) Uani 1.00 d . . . O(2) O 0.4817(1) -0.1058(2) 0.2283(3) 0.0383(7) Uani 1.00 d . . . O(3) O 0.4369(1) 0.0782(2) 0.0696(3) 0.0446(7) Uani 1.00 d . . . O(4) O 0.6328(2) -0.2605(3) -0.0863(6) 0.110(2) Uani 1.00 d . . . O(5) O 0.6463(3) -0.3857(5) 0.1210(7) 0.156(2) Uani 1.00 d . . . O(6) O 0.6819(4) -0.3994(4) -0.1471(9) 0.212(3) Uani 1.00 d . . . O(7) O 0.7304(3) -0.2962(5) 0.021(1) 0.250(4) Uani 1.00 d . . . N(1) N 0.3954(1) 0.1180(2) 0.4327(4) 0.0344(8) Uani 1.00 d . . . N(2) N 0.3574(1) -0.0551(2) 0.3374(4) 0.0327(8) Uani 1.00 d . . . C(1) C 0.5324(2) 0.1656(3) 0.3527(5) 0.0377(10) Uani 1.00 d . . . C(2) C 0.5920(2) 0.2008(3) 0.2958(6) 0.053(1) Uani 1.00 d . . . C(3) C 0.6028(2) 0.3004(4) 0.2809(7) 0.065(2) Uani 1.00 d . . . C(4) C 0.5555(3) 0.3676(3) 0.3217(7) 0.071(2) Uani 1.00 d . . . C(5) C 0.4961(2) 0.3354(3) 0.3737(6) 0.056(1) Uani 1.00 d . . . C(6) C 0.4834(2) 0.2333(3) 0.3886(5) 0.0396(10) Uani 1.00 d . . . C(7) C 0.4195(2) 0.2055(3) 0.4409(5) 0.040(1) Uani 1.00 d . . . C(8) C 0.3288(2) 0.0963(3) 0.4993(5) 0.0361(9) Uani 1.00 d . . . C(9) C 0.3366(2) 0.0623(3) 0.6923(5) 0.050(1) Uani 1.00 d . . . C(10) C 0.2854(2) 0.1875(3) 0.4949(6) 0.053(1) Uani 1.00 d . . . C(11) C 0.3023(2) 0.0146(3) 0.3754(5) 0.0369(9) Uani 1.00 d . . . C(12) C 0.2457(2) -0.0403(3) 0.4642(6) 0.053(1) Uani 1.00 d . . . C(13) C 0.2805(2) 0.0541(3) 0.1942(5) 0.049(1) Uani 1.00 d . . . C(14) C 0.3454(2) -0.1431(3) 0.2836(5) 0.042(1) Uani 1.00 d . . . C(15) C 0.3913(2) -0.2158(3) 0.2281(5) 0.042(1) Uani 1.00 d . . . C(16) C 0.3689(2) -0.3116(3) 0.1966(6) 0.063(1) Uani 1.00 d . . . C(17) C 0.4099(3) -0.3862(3) 0.1520(7) 0.076(2) Uani 1.00 d . . . C(18) C 0.4748(3) -0.3654(3) 0.1353(7) 0.066(2) Uani 1.00 d . . . C(19) C 0.4986(2) -0.2724(3) 0.1613(6) 0.052(1) Uani 1.00 d . . . C(20) C 0.4572(2) -0.1957(3) 0.2073(5) 0.040(1) Uani 1.00 d . . . H(1) H 0.6253 0.1559 0.2673 0.0631 Uiso 1.00 calc . . . H(2) H 0.6436 0.3230 0.2415 0.0770 Uiso 1.00 calc . . . H(3) H 0.5641 0.4360 0.3153 0.0840 Uiso 1.00 calc . . . H(4) H 0.4631 0.3818 0.3989 0.0669 Uiso 1.00 calc . . . H(5) H 0.3927 0.2563 0.4856 0.0481 Uiso 1.00 calc . . . H(6) H 0.3560 0.1132 0.7599 0.0595 Uiso 1.00 calc . . . H(7) H 0.2957 0.0472 0.7412 0.0595 Uiso 1.00 calc . . . H(8) H 0.3630 0.0053 0.6956 0.0595 Uiso 1.00 calc . . . H(9) H 0.3041 0.2384 0.5638 0.0628 Uiso 1.00 calc . . . H(10) H 0.2444 0.1712 0.5428 0.0628 Uiso 1.00 calc . . . H(11) H 0.2805 0.2091 0.3757 0.0628 Uiso 1.00 calc . . . H(12) H 0.2460 0.0990 0.2107 0.0581 Uiso 1.00 calc . . . H(13) H 0.2667 0.0010 0.1219 0.0581 Uiso 1.00 calc . . . H(14) H 0.3153 0.0870 0.1378 0.0581 Uiso 1.00 calc . . . H(15) H 0.2107 0.0038 0.4808 0.0631 Uiso 1.00 calc . . . H(16) H 0.2325 -0.0933 0.3904 0.0631 Uiso 1.00 calc . . . H(17) H 0.2588 -0.0653 0.5763 0.0631 Uiso 1.00 calc . . . H(18) H 0.3015 -0.1618 0.2798 0.0504 Uiso 1.00 calc . . . H(19) H 0.3244 -0.3252 0.2069 0.0748 Uiso 1.00 calc . . . H(20) H 0.3944 -0.4507 0.1330 0.0908 Uiso 1.00 calc . . . H(21) H 0.5036 -0.4169 0.1053 0.0784 Uiso 1.00 calc . . . H(22) H 0.5433 -0.2600 0.1478 0.0629 Uiso 1.00 calc . . . H(23) H 0.4520 0.0453 -0.0339 0.0531 Uiso 1.00 calc . . . H(24) H 0.4190 0.1422 0.0603 0.0531 Uiso 1.00 calc . . . 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 Mn(1) 0.0260(2) 0.0314(3) 0.0336(3) -0.0008(2) 0.0006(2) -0.0035(2) Cl(1) 0.0571(6) 0.0502(6) 0.0549(6) 0.0145(5) -0.0107(5) 0.0012(5) O(1) 0.030(1) 0.034(1) 0.044(1) -0.005(1) -0.003(1) 0.005(1) O(2) 0.037(1) 0.035(1) 0.044(1) 0.000(1) 0.006(1) -0.006(1) O(3) 0.050(2) 0.050(2) 0.034(1) 0.009(1) 0.003(1) 0.002(1) O(4) 0.082(3) 0.113(3) 0.135(4) 0.045(3) 0.014(3) 0.063(3) O(5) 0.133(4) 0.217(6) 0.119(4) 0.055(4) 0.024(3) 0.110(4) O(6) 0.36(1) 0.120(5) 0.157(6) 0.002(6) 0.107(6) -0.064(4) O(7) 0.157(6) 0.183(6) 0.41(1) -0.076(5) -0.205(7) 0.140(7) N(1) 0.033(2) 0.038(2) 0.033(2) 0.003(1) -0.002(1) -0.002(1) N(2) 0.030(1) 0.039(2) 0.029(1) 0.000(1) -0.001(1) -0.002(1) C(1) 0.040(2) 0.039(2) 0.035(2) -0.010(2) -0.011(2) 0.006(2) C(2) 0.039(2) 0.056(3) 0.062(3) -0.012(2) -0.007(2) 0.018(2) C(3) 0.055(3) 0.063(3) 0.076(3) -0.031(2) -0.015(2) 0.030(3) C(4) 0.083(4) 0.045(3) 0.084(4) -0.023(3) -0.026(3) 0.018(2) C(5) 0.065(3) 0.039(2) 0.064(3) -0.005(2) -0.011(2) 0.005(2) C(6) 0.044(2) 0.034(2) 0.041(2) -0.003(2) -0.006(2) 0.005(2) C(7) 0.047(2) 0.034(2) 0.039(2) 0.006(2) -0.005(2) -0.004(2) C(8) 0.031(2) 0.042(2) 0.036(2) 0.005(2) 0.002(1) -0.004(2) C(9) 0.052(2) 0.061(3) 0.037(2) 0.005(2) 0.007(2) -0.004(2) C(10) 0.044(2) 0.057(3) 0.057(3) 0.016(2) 0.004(2) -0.003(2) C(11) 0.027(2) 0.047(2) 0.037(2) 0.003(2) 0.002(1) -0.002(2) C(12) 0.034(2) 0.069(3) 0.055(3) -0.007(2) 0.009(2) -0.009(2) C(13) 0.035(2) 0.065(3) 0.046(2) 0.008(2) -0.008(2) 0.000(2) C(14) 0.040(2) 0.047(2) 0.040(2) -0.009(2) 0.004(2) -0.005(2) C(15) 0.053(2) 0.035(2) 0.039(2) -0.007(2) 0.006(2) -0.005(2) C(16) 0.076(3) 0.047(3) 0.065(3) -0.025(2) 0.014(2) -0.013(2) C(17) 0.119(5) 0.033(2) 0.075(4) -0.012(3) 0.014(3) -0.008(2) C(18) 0.101(4) 0.033(2) 0.064(3) 0.006(2) 0.008(3) -0.005(2) C(19) 0.066(3) 0.044(2) 0.047(2) 0.012(2) 0.004(2) -0.004(2) C(20) 0.056(2) 0.035(2) 0.029(2) 0.001(2) 0.005(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) O(1) 1.909(2) . . yes Mn(1) O(1) 2.434(2) . 3_656 yes Mn(1) O(2) 1.878(2) . . yes Mn(1) O(3) 2.261(3) . . yes Mn(1) N(1) 1.982(3) . . yes Mn(1) N(2) 1.978(3) . . yes Cl(1) O(4) 1.393(4) . . yes Cl(1) O(5) 1.397(4) . . yes Cl(1) O(6) 1.320(5) . . yes Cl(1) O(7) 1.332(5) . . yes O(1) C(1) 1.354(4) . . yes O(2) C(20) 1.333(4) . . yes N(1) C(7) 1.294(4) . . yes N(1) C(8) 1.503(4) . . yes N(2) C(11) 1.514(4) . . yes N(2) C(14) 1.288(5) . . yes C(1) C(2) 1.397(5) . . yes C(1) C(6) 1.400(5) . . yes C(2) C(3) 1.377(6) . . yes C(3) C(4) 1.378(7) . . yes C(4) C(5) 1.368(7) . . yes C(5) C(6) 1.417(5) . . yes C(6) C(7) 1.437(5) . . yes C(8) C(9) 1.533(5) . . yes C(8) C(10) 1.534(5) . . yes C(8) C(11) 1.553(5) . . yes C(11) C(12) 1.545(5) . . yes C(11) C(13) 1.536(5) . . yes C(14) C(15) 1.436(5) . . yes C(15) C(16) 1.404(5) . . yes C(15) C(20) 1.410(5) . . yes C(16) C(17) 1.367(7) . . yes C(17) C(18) 1.385(7) . . yes C(18) C(19) 1.372(6) . . yes C(19) C(20) 1.396(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(1) 78.42(10) . . 3_656 yes O(1) Mn(1) O(2) 94.0(1) . . . yes O(1) Mn(1) O(3) 90.3(1) . . . yes O(1) Mn(1) N(1) 91.9(1) . . . yes O(1) Mn(1) N(2) 170.0(1) . . . yes O(1) Mn(1) O(2) 87.09(10) 3_656 . . yes O(1) Mn(1) O(3) 167.94(9) 3_656 . . yes O(1) Mn(1) N(1) 98.0(1) 3_656 . . yes O(1) Mn(1) N(2) 95.02(10) 3_656 . . yes O(2) Mn(1) O(3) 89.5(1) . . . yes O(2) Mn(1) N(1) 172.9(1) . . . yes O(2) Mn(1) N(2) 93.1(1) . . . yes O(3) Mn(1) N(1) 86.5(1) . . . yes O(3) Mn(1) N(2) 96.7(1) . . . yes N(1) Mn(1) N(2) 81.5(1) . . . yes O(4) Cl(1) O(5) 113.0(3) . . . yes O(4) Cl(1) O(6) 107.9(4) . . . yes O(4) Cl(1) O(7) 110.8(3) . . . yes O(5) Cl(1) O(6) 105.0(4) . . . yes O(5) Cl(1) O(7) 111.9(4) . . . yes O(6) Cl(1) O(7) 107.9(6) . . . yes Mn(1) O(1) Mn(1) 101.58(10) . . 3_656 yes Mn(1) O(1) C(1) 122.0(2) . . . yes Mn(1) O(1) C(1) 119.4(2) 3_656 . . yes Mn(1) O(2) C(20) 128.5(2) . . . yes Mn(1) N(1) C(7) 122.5(2) . . . yes Mn(1) N(1) C(8) 116.0(2) . . . yes C(7) N(1) C(8) 121.5(3) . . . yes Mn(1) N(2) C(11) 115.9(2) . . . yes Mn(1) N(2) C(14) 123.8(3) . . . yes C(11) N(2) C(14) 119.5(3) . . . yes O(1) C(1) C(2) 119.5(3) . . . yes O(1) C(1) C(6) 121.7(3) . . . yes C(2) C(1) C(6) 118.8(3) . . . yes C(1) C(2) C(3) 120.4(4) . . . yes C(2) C(3) C(4) 121.1(4) . . . yes C(3) C(4) C(5) 119.9(4) . . . yes C(4) C(5) C(6) 120.3(4) . . . yes C(1) C(6) C(5) 119.5(4) . . . yes C(1) C(6) C(7) 123.6(3) . . . yes C(5) C(6) C(7) 116.8(4) . . . yes N(1) C(7) C(6) 126.0(3) . . . yes N(1) C(8) C(9) 105.9(3) . . . yes N(1) C(8) C(10) 112.1(3) . . . yes N(1) C(8) C(11) 105.6(3) . . . yes C(9) C(8) C(10) 109.2(3) . . . yes C(9) C(8) C(11) 113.1(3) . . . yes C(10) C(8) C(11) 110.8(3) . . . yes N(2) C(11) C(8) 106.9(3) . . . yes N(2) C(11) C(12) 110.9(3) . . . yes N(2) C(11) C(13) 106.1(3) . . . yes C(8) C(11) C(12) 111.0(3) . . . yes C(8) C(11) C(13) 112.9(3) . . . yes C(12) C(11) C(13) 109.0(3) . . . yes N(2) C(14) C(15) 127.0(3) . . . yes C(14) C(15) C(16) 117.9(4) . . . yes C(14) C(15) C(20) 123.1(3) . . . yes C(16) C(15) C(20) 119.0(4) . . . yes C(15) C(16) C(17) 121.5(4) . . . yes C(16) C(17) C(18) 118.6(4) . . . yes C(17) C(18) C(19) 121.9(4) . . . yes C(18) C(19) C(20) 120.1(4) . . . yes O(2) C(20) C(15) 122.6(3) . . . yes O(2) C(20) C(19) 118.6(4) . . . yes C(15) C(20) C(19) 118.9(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) O(3) 2.832(3) . 3_655 ? O(3) O(4) 2.875(5) . 3_655 ? O(3) C(20) 3.424(4) . 3_655 ? O(3) C(19) 3.432(5) . 3_655 ? O(3) C(9) 3.537(5) . 1_554 ? O(3) O(3) 3.538(5) . 3_655 ? O(4) C(7) 2.981(6) . 3_655 ? O(4) N(1) 3.302(5) . 3_655 ? O(4) C(6) 3.348(6) . 3_655 ? O(4) C(19) 3.359(6) . . ? O(4) C(13) 3.433(6) . 3_655 ? O(5) C(19) 3.454(7) . . ? O(5) C(12) 3.464(6) . 4_545 ? O(5) C(18) 3.586(8) . . ? O(6) C(12) 3.313(7) . 4_544 ? O(6) C(17) 3.486(8) . 3_645 ? O(7) C(14) 3.218(6) . 4_545 ? O(7) C(16) 3.499(7) . 4_545 ? C(3) C(17) 3.472(7) . 3_655 ? C(4) C(18) 3.499(7) . 3_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Mn(naphtmen)(H2O)]ClO4 _database_code_CSD 168756 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C58 H64 Cl2 N4 Mn2 O16 ' _chemical_formula_moiety '?' _chemical_formula_weight 1253.94 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.360(8) _cell_length_b 13.76(1) _cell_length_c 8.463(6) _cell_angle_alpha 101.76(7) _cell_angle_beta 94.45(7) _cell_angle_gamma 112.93(5) _cell_volume 1381(1) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.230 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_meas 1.500 _exptl_crystal_density_method ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652.00 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6726 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.52 _diffrn_measured_fraction_theta_max 0.9949 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.9949 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.92 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6299 _reflns_number_gt 4408 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2031 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6299 _refine_ls_number_parameters 370 _refine_ls_goodness_of_fit_ref 1.947 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05900(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 0.77 _refine_diff_density_min -1.48 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.04023(4) 0.13758(5) 0.10808(7) 0.0384(2) Uani 1.00 d . . . Cl(1) Cl 0.80222(10) 0.3377(1) 0.4368(1) 0.0574(3) Uani 1.00 d . . . O(1) O -0.0370(2) 0.0036(2) 0.1613(4) 0.0444(8) Uani 1.00 d . . . O(2) O 0.1804(2) 0.1461(2) 0.1762(3) 0.0448(8) Uani 1.00 d . . . O(3) O 0.0442(2) 0.2279(3) 0.3600(4) 0.0560(9) Uani 1.00 d . . . O(4) O 0.2239(3) 0.4027(3) 0.5406(5) 0.080(1) Uani 1.00 d . . . O(5) O 0.7017(7) 0.2646(7) 0.378(2) 0.332(6) Uani 1.00 d . . . O(6) O 0.8036(8) 0.3842(7) 0.5911(7) 0.204(4) Uani 1.00 d . . . O(7) O 0.8701(5) 0.2845(6) 0.4271(8) 0.146(3) Uani 1.00 d . . . O(8) O 0.8154(7) 0.4100(6) 0.3381(8) 0.161(3) Uani 1.00 d . . . N(1) N -0.0998(2) 0.1430(3) 0.0302(4) 0.0354(8) Uani 1.00 d . . . N(2) N 0.1004(2) 0.2537(3) -0.0042(4) 0.0361(8) Uani 1.00 d . . . C(1) C -0.1291(3) -0.0176(3) 0.2268(5) 0.0390(9) Uani 1.00 d . . . C(2) C -0.1461(3) -0.0830(3) 0.3401(5) 0.044(1) Uani 1.00 d . . . C(3) C -0.2433(3) -0.1187(3) 0.3961(5) 0.046(1) Uani 1.00 d . . . C(4) C -0.3308(3) -0.0919(3) 0.3443(5) 0.0416(10) Uani 1.00 d . . . C(5) C -0.4350(3) -0.1358(4) 0.3946(5) 0.052(1) Uani 1.00 d . . . C(6) C -0.5177(3) -0.1082(4) 0.3475(6) 0.056(1) Uani 1.00 d . . . C(7) C -0.5002(3) -0.0349(4) 0.2490(6) 0.055(1) Uani 1.00 d . . . C(8) C -0.4007(3) 0.0090(4) 0.1962(6) 0.050(1) Uani 1.00 d . . . C(9) C -0.3132(3) -0.0205(3) 0.2400(5) 0.0402(10) Uani 1.00 d . . . C(10) C -0.2083(3) 0.0196(3) 0.1835(5) 0.0375(9) Uani 1.00 d . . . C(11) C -0.1923(3) 0.0893(3) 0.0743(5) 0.0382(9) Uani 1.00 d . . . C(12) C -0.0959(3) 0.2079(3) -0.0940(4) 0.0361(9) Uani 1.00 d . . . C(13) C -0.1841(3) 0.2530(4) -0.0870(6) 0.049(1) Uani 1.00 d . . . C(14) C -0.1169(3) 0.1298(4) -0.2616(5) 0.050(1) Uani 1.00 d . . . C(15) C 0.0226(3) 0.3031(3) -0.0498(5) 0.0361(9) Uani 1.00 d . . . C(16) C 0.0520(3) 0.3549(3) -0.1930(5) 0.046(1) Uani 1.00 d . . . C(17) C 0.0337(3) 0.3909(3) 0.1016(5) 0.047(1) Uani 1.00 d . . . C(18) C 0.2013(3) 0.2935(3) -0.0304(5) 0.0374(9) Uani 1.00 d . . . C(19) C 0.2886(3) 0.2657(3) 0.0233(5) 0.0367(9) Uani 1.00 d . . . C(20) C 0.3945(3) 0.3142(3) -0.0273(5) 0.0399(10) Uani 1.00 d . . . C(21) C 0.4129(3) 0.3735(4) -0.1466(6) 0.048(1) Uani 1.00 d . . . C(22) C 0.5158(4) 0.4161(4) -0.1908(6) 0.060(1) Uani 1.00 d . . . C(23) C 0.6047(3) 0.4019(4) -0.1174(7) 0.062(1) Uani 1.00 d . . . C(24) C 0.5895(3) 0.3444(4) -0.0025(6) 0.056(1) Uani 1.00 d . . . C(25) C 0.4848(3) 0.2976(4) 0.0444(5) 0.046(1) Uani 1.00 d . . . C(26) C 0.4674(3) 0.2314(4) 0.1574(5) 0.050(1) Uani 1.00 d . . . C(27) C 0.3668(3) 0.1810(4) 0.1953(5) 0.048(1) Uani 1.00 d . . . C(28) C 0.2745(3) 0.1972(3) 0.1288(5) 0.0382(9) Uani 1.00 d . . . C(29) C 0.3172(5) 0.4399(6) 0.4696(8) 0.092(2) Uani 1.00 d . . . H(1) H -0.0890 -0.1023 0.3767 0.0526 Uiso 1.00 calc . . . H(2) H -0.2530 -0.1625 0.4720 0.0558 Uiso 1.00 calc . . . H(3) H -0.4471 -0.1856 0.4619 0.0630 Uiso 1.00 calc . . . H(4) H -0.5871 -0.1380 0.3818 0.0678 Uiso 1.00 calc . . . H(5) H -0.5581 -0.0155 0.2169 0.0649 Uiso 1.00 calc . . . H(6) H -0.3908 0.0594 0.1306 0.0593 Uiso 1.00 calc . . . H(7) H -0.2554 0.0973 0.0302 0.0455 Uiso 1.00 calc . . . H(8) H -0.1705 0.3022 0.0175 0.0594 Uiso 1.00 calc . . . H(9) H -0.2549 0.1947 -0.1030 0.0594 Uiso 1.00 calc . . . H(10) H -0.1817 0.2907 -0.1700 0.0594 Uiso 1.00 calc . . . H(11) H -0.1875 0.0710 -0.2779 0.0598 Uiso 1.00 calc . . . H(12) H -0.1150 0.1676 -0.3443 0.0598 Uiso 1.00 calc . . . H(13) H -0.0618 0.1025 -0.2662 0.0598 Uiso 1.00 calc . . . H(14) H 0.0040 0.3885 -0.2144 0.0551 Uiso 1.00 calc . . . H(15) H 0.0443 0.3002 -0.2882 0.0551 Uiso 1.00 calc . . . H(16) H 0.1262 0.4084 -0.1665 0.0551 Uiso 1.00 calc . . . H(17) H -0.0145 0.4238 0.0791 0.0566 Uiso 1.00 calc . . . H(18) H 0.1077 0.4445 0.1291 0.0566 Uiso 1.00 calc . . . H(19) H 0.0150 0.3586 0.1902 0.0566 Uiso 1.00 calc . . . H(20) H 0.2191 0.3472 -0.0911 0.0445 Uiso 1.00 calc . . . H(21) H 0.3539 0.3848 -0.1985 0.0585 Uiso 1.00 calc . . . H(22) H 0.5260 0.4556 -0.2725 0.0721 Uiso 1.00 calc . . . H(23) H 0.6754 0.4326 -0.1478 0.0748 Uiso 1.00 calc . . . H(24) H 0.6500 0.3350 0.0479 0.0675 Uiso 1.00 calc . . . H(25) H 0.5283 0.2226 0.2075 0.0603 Uiso 1.00 calc . . . H(26) H 0.3569 0.1341 0.2667 0.0566 Uiso 1.00 calc . . . H(27) H 0.2979 0.4482 0.3647 0.1093 Uiso 1.00 calc . . . H(28) H 0.3490 0.3879 0.4584 0.1093 Uiso 1.00 calc . . . H(29) H 0.3701 0.5079 0.5369 0.1093 Uiso 1.00 calc . . . H(30) H 0.1069 0.2505 0.4428 0.0668 Uiso 1.00 calc . . . H(31) H -0.0166 0.2439 0.3854 0.0668 Uiso 1.00 calc . . . H(32) H 0.2291 0.4286 0.6564 0.0950 Uiso 1.00 calc . . . 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 Mn(1) 0.0246(3) 0.0494(3) 0.0489(4) 0.0142(2) 0.0094(2) 0.0298(3) Cl(1) 0.0518(6) 0.0743(8) 0.0537(6) 0.0309(6) 0.0082(5) 0.0228(6) O(1) 0.032(1) 0.053(2) 0.060(2) 0.018(1) 0.018(1) 0.034(1) O(2) 0.031(1) 0.065(2) 0.052(2) 0.022(1) 0.014(1) 0.036(1) O(3) 0.045(2) 0.085(2) 0.044(2) 0.030(2) 0.010(1) 0.023(2) O(4) 0.065(2) 0.078(3) 0.089(3) 0.016(2) 0.025(2) 0.025(2) O(5) 0.143(7) 0.149(7) 0.58(2) 0.005(5) -0.19(1) 0.04(1) O(6) 0.39(1) 0.257(9) 0.077(4) 0.246(10) 0.067(6) 0.051(5) O(7) 0.154(5) 0.214(7) 0.170(6) 0.150(5) 0.079(4) 0.089(5) O(8) 0.263(8) 0.200(7) 0.145(5) 0.171(7) 0.122(5) 0.124(5) N(1) 0.026(1) 0.044(2) 0.042(2) 0.014(1) 0.009(1) 0.023(1) N(2) 0.025(1) 0.051(2) 0.040(2) 0.016(1) 0.010(1) 0.025(1) C(1) 0.028(2) 0.047(2) 0.042(2) 0.010(2) 0.009(1) 0.021(2) C(2) 0.040(2) 0.055(2) 0.044(2) 0.019(2) 0.011(2) 0.027(2) C(3) 0.044(2) 0.054(2) 0.042(2) 0.013(2) 0.012(2) 0.026(2) C(4) 0.037(2) 0.046(2) 0.037(2) 0.008(2) 0.012(2) 0.017(2) C(5) 0.038(2) 0.067(3) 0.045(2) 0.007(2) 0.015(2) 0.025(2) C(6) 0.033(2) 0.073(3) 0.051(2) 0.005(2) 0.015(2) 0.021(2) C(7) 0.033(2) 0.069(3) 0.064(3) 0.017(2) 0.017(2) 0.026(2) C(8) 0.036(2) 0.059(3) 0.060(3) 0.018(2) 0.017(2) 0.029(2) C(9) 0.027(2) 0.047(2) 0.044(2) 0.008(2) 0.011(1) 0.019(2) C(10) 0.029(2) 0.046(2) 0.041(2) 0.013(2) 0.012(1) 0.020(2) C(11) 0.026(2) 0.048(2) 0.043(2) 0.013(1) 0.007(1) 0.021(2) C(12) 0.026(2) 0.048(2) 0.041(2) 0.016(1) 0.007(1) 0.023(2) C(13) 0.031(2) 0.062(3) 0.069(3) 0.023(2) 0.012(2) 0.036(2) C(14) 0.041(2) 0.063(3) 0.044(2) 0.016(2) 0.002(2) 0.022(2) C(15) 0.026(2) 0.043(2) 0.047(2) 0.014(1) 0.008(1) 0.026(2) C(16) 0.035(2) 0.058(2) 0.056(2) 0.019(2) 0.013(2) 0.037(2) C(17) 0.039(2) 0.046(2) 0.060(3) 0.018(2) 0.009(2) 0.020(2) C(18) 0.024(2) 0.047(2) 0.043(2) 0.011(1) 0.006(1) 0.024(2) C(19) 0.024(2) 0.046(2) 0.041(2) 0.011(1) 0.006(1) 0.017(2) C(20) 0.025(2) 0.046(2) 0.045(2) 0.010(2) 0.007(1) 0.015(2) C(21) 0.029(2) 0.056(2) 0.060(3) 0.010(2) 0.012(2) 0.027(2) C(22) 0.037(2) 0.069(3) 0.075(3) 0.012(2) 0.023(2) 0.035(3) C(23) 0.028(2) 0.068(3) 0.086(4) 0.010(2) 0.022(2) 0.026(3) C(24) 0.024(2) 0.070(3) 0.073(3) 0.017(2) 0.009(2) 0.018(2) C(25) 0.025(2) 0.057(2) 0.053(2) 0.013(2) 0.004(2) 0.014(2) C(26) 0.030(2) 0.072(3) 0.052(2) 0.025(2) 0.000(2) 0.018(2) C(27) 0.035(2) 0.068(3) 0.048(2) 0.025(2) 0.005(2) 0.026(2) C(28) 0.025(2) 0.053(2) 0.040(2) 0.016(2) 0.005(1) 0.018(2) C(29) 0.075(4) 0.113(5) 0.093(5) 0.032(4) 0.035(3) 0.044(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) O(1) 1.896(3) . . yes Mn(1) O(1) 2.662(3) . 2_555 yes Mn(1) O(2) 1.867(3) . . yes Mn(1) O(3) 2.224(3) . . yes Mn(1) N(1) 1.969(3) . . yes Mn(1) N(2) 1.959(3) . . yes Cl(1) O(5) 1.306(7) . . yes Cl(1) O(6) 1.327(6) . . yes Cl(1) O(7) 1.367(4) . . yes Cl(1) O(8) 1.393(5) . . yes O(1) C(1) 1.342(4) . . yes O(2) C(28) 1.319(4) . . yes O(4) C(29) 1.387(7) . . yes N(1) C(11) 1.299(4) . . yes N(1) C(12) 1.503(4) . . yes N(2) C(15) 1.513(4) . . yes N(2) C(18) 1.299(4) . . yes C(1) C(2) 1.417(5) . . yes C(1) C(10) 1.398(5) . . yes C(2) C(3) 1.359(5) . . yes C(3) C(4) 1.420(6) . . yes C(4) C(5) 1.423(5) . . yes C(4) C(9) 1.416(5) . . yes C(5) C(6) 1.360(6) . . yes C(6) C(7) 1.398(6) . . yes C(7) C(8) 1.382(5) . . yes C(8) C(9) 1.425(5) . . yes C(9) C(10) 1.452(4) . . yes C(10) C(11) 1.432(5) . . yes C(12) C(13) 1.532(5) . . yes C(12) C(14) 1.526(6) . . yes C(12) C(15) 1.566(5) . . yes C(15) C(16) 1.530(5) . . yes C(15) C(17) 1.524(6) . . yes C(18) C(19) 1.431(4) . . yes C(19) C(20) 1.451(5) . . yes C(19) C(28) 1.397(5) . . yes C(20) C(21) 1.401(5) . . yes C(20) C(25) 1.426(5) . . yes C(21) C(22) 1.384(5) . . yes C(22) C(23) 1.396(6) . . yes C(23) C(24) 1.353(7) . . yes C(24) C(25) 1.420(5) . . yes C(25) C(26) 1.423(6) . . yes C(26) C(27) 1.350(6) . . yes C(27) C(28) 1.429(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(1) 79.4(1) . . 2_555 yes O(1) Mn(1) O(2) 95.0(1) . . . yes O(1) Mn(1) O(3) 89.9(1) . . . yes O(1) Mn(1) N(1) 90.9(1) . . . yes O(1) Mn(1) N(2) 165.2(1) . . . yes O(1) Mn(1) O(2) 85.2(1) 2_555 . . yes O(1) Mn(1) O(3) 167.46(10) 2_555 . . yes O(1) Mn(1) N(1) 95.8(1) 2_555 . . yes O(1) Mn(1) N(2) 88.1(1) 2_555 . . yes O(2) Mn(1) O(3) 89.2(1) . . . yes O(2) Mn(1) N(1) 174.1(1) . . . yes O(2) Mn(1) N(2) 91.9(1) . . . yes O(3) Mn(1) N(1) 90.8(1) . . . yes O(3) Mn(1) N(2) 103.3(1) . . . yes N(1) Mn(1) N(2) 82.3(1) . . . yes O(5) Cl(1) O(6) 107.1(8) . . . yes O(5) Cl(1) O(7) 107.4(6) . . . yes O(5) Cl(1) O(8) 102.0(6) . . . yes O(6) Cl(1) O(7) 111.5(4) . . . yes O(6) Cl(1) O(8) 111.4(4) . . . yes O(7) Cl(1) O(8) 116.5(4) . . . yes Mn(1) O(1) Mn(1) 100.6(1) . . 2_555 yes Mn(1) O(1) C(1) 122.9(2) . . . yes Mn(1) O(1) C(1) 118.6(2) 2_555 . . yes Mn(1) O(2) C(28) 129.5(2) . . . yes Mn(1) N(1) C(11) 123.1(2) . . . yes Mn(1) N(1) C(12) 116.0(2) . . . yes C(11) N(1) C(12) 120.8(3) . . . yes Mn(1) N(2) C(15) 115.0(2) . . . yes Mn(1) N(2) C(18) 124.8(2) . . . yes C(15) N(2) C(18) 120.0(3) . . . yes O(1) C(1) C(2) 117.5(3) . . . yes O(1) C(1) C(10) 122.4(3) . . . yes C(2) C(1) C(10) 120.1(3) . . . yes C(1) C(2) C(3) 120.6(3) . . . yes C(2) C(3) C(4) 121.6(3) . . . yes C(3) C(4) C(5) 121.2(3) . . . yes C(3) C(4) C(9) 118.9(3) . . . yes C(5) C(4) C(9) 119.9(4) . . . yes C(4) C(5) C(6) 121.0(4) . . . yes C(5) C(6) C(7) 119.6(4) . . . yes C(6) C(7) C(8) 121.3(4) . . . yes C(7) C(8) C(9) 120.4(4) . . . yes C(4) C(9) C(8) 117.6(3) . . . yes C(4) C(9) C(10) 119.3(3) . . . yes C(8) C(9) C(10) 123.1(3) . . . yes C(1) C(10) C(9) 119.1(3) . . . yes C(1) C(10) C(11) 121.8(3) . . . yes C(9) C(10) C(11) 118.9(3) . . . yes N(1) C(11) C(10) 126.3(3) . . . yes N(1) C(12) C(13) 111.8(3) . . . yes N(1) C(12) C(14) 106.4(3) . . . yes N(1) C(12) C(15) 105.3(3) . . . yes C(13) C(12) C(14) 109.6(3) . . . yes C(13) C(12) C(15) 110.7(3) . . . yes C(14) C(12) C(15) 113.0(3) . . . yes N(2) C(15) C(12) 106.2(3) . . . yes N(2) C(15) C(16) 112.0(3) . . . yes N(2) C(15) C(17) 106.3(3) . . . yes C(12) C(15) C(16) 111.3(3) . . . yes C(12) C(15) C(17) 111.7(3) . . . yes C(16) C(15) C(17) 109.3(3) . . . yes N(2) C(18) C(19) 126.9(3) . . . yes C(18) C(19) C(20) 118.8(3) . . . yes C(18) C(19) C(28) 121.0(3) . . . yes C(20) C(19) C(28) 120.1(3) . . . yes C(19) C(20) C(21) 124.1(3) . . . yes C(19) C(20) C(25) 118.2(3) . . . yes C(21) C(20) C(25) 117.6(3) . . . yes C(20) C(21) C(22) 121.0(4) . . . yes C(21) C(22) C(23) 121.1(4) . . . yes C(22) C(23) C(24) 119.4(4) . . . yes C(23) C(24) C(25) 121.3(4) . . . yes C(20) C(25) C(24) 119.5(4) . . . yes C(20) C(25) C(26) 119.4(3) . . . yes C(24) C(25) C(26) 121.2(4) . . . yes C(25) C(26) C(27) 121.8(3) . . . yes C(26) C(27) C(28) 120.7(4) . . . yes O(2) C(28) C(19) 124.4(3) . . . yes O(2) C(28) C(27) 115.9(3) . . . yes C(19) C(28) C(27) 119.6(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Mn(1) O(1) 2.662(3) . 2_555 ? O(3) O(4) 2.705(5) . . ? O(3) O(7) 2.789(6) . 1_455 ? O(3) C(29) 3.571(8) . . ? O(4) O(8) 2.834(7) . 2_666 ? O(4) C(16) 3.320(6) . 1_556 ? O(4) O(6) 3.475(8) . 2_666 ? O(5) C(8) 3.21(1) . 1_655 ? O(5) C(26) 3.333(8) . . ? O(6) C(17) 3.416(10) . 2_666 ? O(6) C(29) 3.485(10) . 2_666 ? O(6) C(13) 3.588(7) . 1_656 ? O(7) C(11) 3.379(8) . 1_655 ? O(7) C(10) 3.501(8) . 1_655 ? O(7) C(16) 3.587(8) . 1_656 ? O(8) C(29) 3.462(9) . 2_666 ? O(8) C(16) 3.550(7) . 2_665 ? C(6) C(6) 3.37(1) . 2_456 ? C(6) C(7) 3.516(7) . 2_456 ? C(20) C(22) 3.466(7) . 2_665 ? C(21) C(22) 3.392(7) . 2_665 ? C(21) C(23) 3.526(7) . 2_665 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Mn(saltmen)(NCS)] _database_code_CSD 168757 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C21 H22 N3 Mn O2 S ' _chemical_formula_moiety 'C21 H22 N3 Mn O2 S ' _chemical_formula_weight 435.42 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.2800(6) _cell_length_b 19.873(2) _cell_length_c 12.1163(3) _cell_angle_alpha 90 _cell_angle_beta 95.7988(6) _cell_angle_gamma 90 _cell_volume 1983.5(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.080 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904.00 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.939 _exptl_absorpt_correction_T_max 0.939 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14364 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 27.39 _diffrn_measured_fraction_theta_max 0.9660 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.9660 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4354 _reflns_number_gt 3406 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1381 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4354 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.675 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0049 _refine_diff_density_max 0.52 _refine_diff_density_min -0.52 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.59507(4) 0.08485(2) 0.43605(3) 0.0384(1) Uani 1.00 d . . . S(1) S 0.89489(10) 0.16879(5) 0.13482(7) 0.0632(2) Uani 1.00 d . . . O(1) O 0.7649(2) 0.04192(10) 0.5223(2) 0.0496(5) Uani 1.00 d . . . O(2) O 0.5491(2) 0.00638(9) 0.3533(2) 0.0506(5) Uani 1.00 d . . . N(1) N 0.5920(2) 0.16097(10) 0.5425(2) 0.0353(5) Uani 1.00 d . . . N(2) N 0.3806(2) 0.12410(9) 0.3821(2) 0.0338(5) Uani 1.00 d . . . N(3) N 0.7348(3) 0.1295(1) 0.3149(2) 0.0594(8) Uani 1.00 d . . . C(1) C 0.8521(3) 0.0621(1) 0.6130(2) 0.0370(6) Uani 1.00 d . . . C(2) C 0.9815(3) 0.0208(1) 0.6575(2) 0.0426(7) Uani 1.00 d . . . C(3) C 1.0741(3) 0.0394(1) 0.7529(2) 0.0496(7) Uani 1.00 d . . . C(4) C 1.0452(4) 0.0989(2) 0.8077(2) 0.0570(9) Uani 1.00 d . . . C(5) C 0.9217(3) 0.1401(2) 0.7654(2) 0.0503(8) Uani 1.00 d . . . C(6) C 0.8223(3) 0.1229(1) 0.6677(2) 0.0394(6) Uani 1.00 d . . . C(7) C 0.6939(3) 0.1678(1) 0.6300(2) 0.0389(6) Uani 1.00 d . . . C(8) C 0.4667(3) 0.2143(1) 0.5097(2) 0.0378(6) Uani 1.00 d . . . C(9) C 0.4280(4) 0.2573(1) 0.6072(3) 0.0535(8) Uani 1.00 d . . . C(10) C 0.5382(4) 0.2587(1) 0.4233(3) 0.0506(8) Uani 1.00 d . . . C(11) C 0.3148(3) 0.1744(1) 0.4582(2) 0.0350(6) Uani 1.00 d . . . C(12) C 0.1875(3) 0.2209(1) 0.3978(2) 0.0472(7) Uani 1.00 d . . . C(13) C 0.2365(3) 0.1338(2) 0.5450(2) 0.0494(8) Uani 1.00 d . . . C(14) C 0.2989(3) 0.1052(1) 0.2911(2) 0.0379(6) Uani 1.00 d . . . C(15) C 0.3415(3) 0.0516(1) 0.2209(2) 0.0386(6) Uani 1.00 d . . . C(16) C 0.2478(3) 0.0433(1) 0.1179(2) 0.0471(7) Uani 1.00 d . . . C(17) C 0.2733(4) -0.0095(2) 0.0495(2) 0.0545(8) Uani 1.00 d . . . C(18) C 0.3961(4) -0.0556(1) 0.0828(2) 0.0528(8) Uani 1.00 d . . . C(19) C 0.4875(3) -0.0497(1) 0.1827(2) 0.0476(7) Uani 1.00 d . . . C(20) C 0.4629(3) 0.0038(1) 0.2545(2) 0.0387(6) Uani 1.00 d . . . C(21) C 0.8015(3) 0.1454(1) 0.2398(2) 0.0441(7) Uani 1.00 d . . . H(1) H 1.0043 -0.0200 0.6212 0.0511 Uiso 1.00 calc . . . H(2) H 1.1601 0.0109 0.7822 0.0595 Uiso 1.00 calc . . . H(3) H 1.1105 0.1109 0.8738 0.0685 Uiso 1.00 calc . . . H(4) H 0.9023 0.1810 0.8024 0.0603 Uiso 1.00 calc . . . H(5) H 0.6819 0.2067 0.6738 0.0466 Uiso 1.00 calc . . . H(6) H 0.5244 0.2784 0.6393 0.0642 Uiso 1.00 calc . . . H(7) H 0.3508 0.2907 0.5821 0.0642 Uiso 1.00 calc . . . H(8) H 0.3846 0.2298 0.6610 0.0642 Uiso 1.00 calc . . . H(9) H 0.6369 0.2782 0.4551 0.0607 Uiso 1.00 calc . . . H(10) H 0.5588 0.2321 0.3611 0.0607 Uiso 1.00 calc . . . H(11) H 0.4633 0.2934 0.4001 0.0607 Uiso 1.00 calc . . . H(12) H 0.1462 0.2505 0.4497 0.0566 Uiso 1.00 calc . . . H(13) H 0.2360 0.2464 0.3436 0.0566 Uiso 1.00 calc . . . H(14) H 0.1013 0.1946 0.3625 0.0566 Uiso 1.00 calc . . . H(15) H 0.1921 0.1636 0.5954 0.0593 Uiso 1.00 calc . . . H(16) H 0.1525 0.1065 0.5095 0.0593 Uiso 1.00 calc . . . H(17) H 0.3160 0.1060 0.5844 0.0593 Uiso 1.00 calc . . . H(18) H 0.2017 0.1291 0.2687 0.0454 Uiso 1.00 calc . . . H(19) H 0.1651 0.0751 0.0957 0.0565 Uiso 1.00 calc . . . H(20) H 0.2088 -0.0147 -0.0194 0.0653 Uiso 1.00 calc . . . H(21) H 0.4165 -0.0918 0.0349 0.0634 Uiso 1.00 calc . . . H(22) H 0.5687 -0.0823 0.2038 0.0571 Uiso 1.00 calc . . . 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 Mn(1) 0.0346(2) 0.0372(2) 0.0414(2) 0.0061(1) -0.0058(2) -0.0078(2) S(1) 0.0544(4) 0.0809(6) 0.0542(5) 0.0146(4) 0.0053(4) 0.0099(4) O(1) 0.0472(10) 0.048(1) 0.050(1) 0.0128(8) -0.0123(8) -0.0112(8) O(2) 0.055(1) 0.0408(10) 0.052(1) 0.0121(8) -0.0139(9) -0.0114(8) N(1) 0.0351(10) 0.0341(10) 0.036(1) 0.0021(8) -0.0015(8) -0.0022(8) N(2) 0.0323(9) 0.0308(10) 0.037(1) 0.0019(8) -0.0016(8) -0.0030(8) N(3) 0.054(1) 0.067(2) 0.057(2) 0.003(1) 0.009(1) -0.001(1) C(1) 0.032(1) 0.042(1) 0.036(1) -0.0014(10) 0.0006(9) 0.005(1) C(2) 0.037(1) 0.042(1) 0.048(1) 0.002(1) 0.000(1) 0.009(1) C(3) 0.039(1) 0.056(2) 0.052(2) 0.002(1) -0.007(1) 0.014(1) C(4) 0.054(2) 0.069(2) 0.044(2) 0.002(1) -0.016(1) 0.002(1) C(5) 0.048(1) 0.055(2) 0.044(2) 0.004(1) -0.011(1) -0.007(1) C(6) 0.035(1) 0.045(1) 0.038(1) -0.001(1) -0.0005(10) 0.003(1) C(7) 0.040(1) 0.039(1) 0.037(1) -0.002(1) 0.000(1) -0.0043(10) C(8) 0.041(1) 0.032(1) 0.038(1) 0.0047(10) -0.005(1) -0.0026(10) C(9) 0.055(2) 0.051(2) 0.052(2) 0.016(1) -0.009(1) -0.016(1) C(10) 0.055(2) 0.038(1) 0.057(2) -0.007(1) -0.003(1) 0.008(1) C(11) 0.032(1) 0.034(1) 0.037(1) 0.0053(9) -0.0031(9) -0.0032(9) C(12) 0.048(1) 0.042(1) 0.048(1) 0.014(1) -0.010(1) -0.004(1) C(13) 0.049(1) 0.049(2) 0.051(2) 0.000(1) 0.011(1) 0.002(1) C(14) 0.035(1) 0.038(1) 0.039(1) 0.0008(10) -0.0016(10) 0.000(1) C(15) 0.038(1) 0.039(1) 0.039(1) -0.003(1) 0.0022(10) -0.0035(10) C(16) 0.048(1) 0.050(2) 0.042(1) 0.002(1) -0.004(1) -0.003(1) C(17) 0.067(2) 0.055(2) 0.039(1) -0.005(1) -0.007(1) -0.008(1) C(18) 0.069(2) 0.042(1) 0.047(2) -0.002(1) 0.007(1) -0.013(1) C(19) 0.051(1) 0.038(1) 0.053(2) -0.001(1) 0.002(1) -0.006(1) C(20) 0.037(1) 0.038(1) 0.040(1) -0.0047(10) 0.0005(10) -0.006(1) C(21) 0.037(1) 0.044(1) 0.048(2) 0.008(1) -0.007(1) -0.007(1) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) O(1) 1.871(2) . . yes Mn(1) O(2) 1.872(2) . . yes Mn(1) N(1) 1.989(2) . . yes Mn(1) N(2) 1.988(2) . . yes Mn(1) N(3) 2.151(3) . . yes S(1) C(21) 1.622(3) . . yes O(1) C(1) 1.316(3) . . yes O(2) C(20) 1.331(3) . . yes N(1) C(7) 1.293(3) . . yes N(1) C(8) 1.507(3) . . yes N(2) C(11) 1.498(3) . . yes N(2) C(14) 1.290(3) . . yes N(3) C(21) 1.155(4) . . yes C(1) C(2) 1.413(3) . . yes C(1) C(6) 1.410(4) . . yes C(2) C(3) 1.372(4) . . yes C(3) C(4) 1.389(4) . . yes C(4) C(5) 1.368(4) . . yes C(5) C(6) 1.414(3) . . yes C(6) C(7) 1.428(3) . . yes C(8) C(9) 1.518(4) . . yes C(8) C(10) 1.534(4) . . yes C(8) C(11) 1.562(3) . . yes C(11) C(12) 1.531(3) . . yes C(11) C(13) 1.522(4) . . yes C(14) C(15) 1.430(4) . . yes C(15) C(16) 1.411(3) . . yes C(15) C(20) 1.413(3) . . yes C(16) C(17) 1.366(4) . . yes C(17) C(18) 1.398(4) . . yes C(18) C(19) 1.367(4) . . yes C(19) C(20) 1.402(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(2) 91.13(8) . . . yes O(1) Mn(1) N(1) 92.47(8) . . . yes O(1) Mn(1) N(2) 163.39(9) . . . yes O(1) Mn(1) N(3) 98.25(10) . . . yes O(2) Mn(1) N(1) 164.85(9) . . . yes O(2) Mn(1) N(2) 91.40(8) . . . yes O(2) Mn(1) N(3) 94.2(1) . . . yes N(1) Mn(1) N(2) 81.09(8) . . . yes N(1) Mn(1) N(3) 99.87(9) . . . yes N(2) Mn(1) N(3) 97.93(9) . . . yes Mn(1) O(1) C(1) 130.2(2) . . . yes Mn(1) O(2) C(20) 125.1(2) . . . yes Mn(1) N(1) C(7) 124.1(2) . . . yes Mn(1) N(1) C(8) 114.7(1) . . . yes C(7) N(1) C(8) 121.1(2) . . . yes Mn(1) N(2) C(11) 115.3(1) . . . yes Mn(1) N(2) C(14) 122.7(2) . . . yes C(11) N(2) C(14) 121.8(2) . . . yes Mn(1) N(3) C(21) 169.6(2) . . . yes O(1) C(1) C(2) 118.2(2) . . . yes O(1) C(1) C(6) 123.2(2) . . . yes C(2) C(1) C(6) 118.7(2) . . . yes C(1) C(2) C(3) 120.2(3) . . . yes C(2) C(3) C(4) 121.5(2) . . . yes C(3) C(4) C(5) 119.3(3) . . . yes C(4) C(5) C(6) 121.2(3) . . . yes C(1) C(6) C(5) 119.1(2) . . . yes C(1) C(6) C(7) 122.9(2) . . . yes C(5) C(6) C(7) 117.9(2) . . . yes N(1) C(7) C(6) 126.9(2) . . . yes N(1) C(8) C(9) 112.7(2) . . . yes N(1) C(8) C(10) 106.3(2) . . . yes N(1) C(8) C(11) 104.7(2) . . . yes C(9) C(8) C(10) 109.4(2) . . . yes C(9) C(8) C(11) 111.8(2) . . . yes C(10) C(8) C(11) 111.7(2) . . . yes N(2) C(11) C(8) 104.8(2) . . . yes N(2) C(11) C(12) 112.6(2) . . . yes N(2) C(11) C(13) 106.2(2) . . . yes C(8) C(11) C(12) 111.9(2) . . . yes C(8) C(11) C(13) 112.0(2) . . . yes C(12) C(11) C(13) 109.2(2) . . . yes N(2) C(14) C(15) 125.9(2) . . . yes C(14) C(15) C(16) 117.8(2) . . . yes C(14) C(15) C(20) 122.7(2) . . . yes C(16) C(15) C(20) 119.2(2) . . . yes C(15) C(16) C(17) 121.4(3) . . . yes C(16) C(17) C(18) 118.7(2) . . . yes C(17) C(18) C(19) 121.4(3) . . . yes C(18) C(19) C(20) 120.8(3) . . . yes O(2) C(20) C(15) 122.4(2) . . . yes O(2) C(20) C(19) 119.2(2) . . . yes C(15) C(20) C(19) 118.3(2) . . . yes S(1) C(21) N(3) 179.2(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Mn(1) O(2) 3.441(2) . 3_656 ? O(1) O(2) 3.279(3) . 3_656 ? O(1) C(2) 3.411(4) . 3_756 ? O(1) C(20) 3.568(3) . 3_656 ? O(1) C(13) 3.586(4) . 3_656 ? O(2) C(13) 3.462(3) . 3_656 ? C(1) C(20) 3.456(4) . 3_656 ? C(1) C(15) 3.519(4) . 3_656 ? C(2) C(13) 3.455(4) . 1_655 ? C(2) C(15) 3.492(4) . 3_656 ? C(2) C(14) 3.514(4) . 3_656 ? C(3) C(13) 3.515(4) . 1_655 ? C(6) C(19) 3.594(4) . 3_656 ? C(17) C(18) 3.553(5) . 3_655 ? C(18) C(18) 3.545(6) . 3_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Mn(naphtmen)(NCS)] _database_code_CSD 168758 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C29 H26 N3 Mn O2 S ' _chemical_formula_moiety 'C29 H26 N3 Mn O2 S ' _chemical_formula_weight 535.54 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 14.2464(3) _cell_length_b 13.1533(6) _cell_length_c 14.3675(3) _cell_angle_alpha 90 _cell_angle_beta 109.6759(5) _cell_angle_gamma 90 _cell_volume 2535.1(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112.00 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.950 _exptl_absorpt_correction_T_max 0.950 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5821 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.58 _diffrn_measured_fraction_theta_max 0.9893 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.9893 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5821 _reflns_number_gt 4245 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1821 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5821 _refine_ls_number_parameters 325 _refine_ls_goodness_of_fit_ref 1.726 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0655 _refine_diff_density_max 1.38 _refine_diff_density_min -0.60 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.93261(3) 0.37531(3) 0.05709(3) 0.0462(1) Uani 1.00 d . . . S(1) S 1.00372(8) 0.07140(10) 0.25750(9) 0.0918(4) Uani 1.00 d . . . O(1) O 0.9524(2) 0.3250(2) -0.0571(2) 0.0690(8) Uani 1.00 d . . . O(2) O 1.0680(1) 0.4086(2) 0.1142(2) 0.0641(7) Uani 1.00 d . . . N(1) N 0.7879(2) 0.3888(2) -0.0145(2) 0.0473(7) Uani 1.00 d . . . N(2) N 0.8981(2) 0.4645(2) 0.1505(2) 0.0494(7) Uani 1.00 d . . . N(3) N 0.9455(2) 0.2367(2) 0.1323(3) 0.0702(10) Uani 1.00 d . . . C(1) C 0.8887(2) 0.3029(2) -0.1440(2) 0.0535(9) Uani 1.00 d . . . C(2) C 0.9272(3) 0.2498(3) -0.2105(3) 0.065(1) Uani 1.00 d . . . C(3) C 0.8677(3) 0.2233(3) -0.3009(3) 0.068(1) Uani 1.00 d . . . C(4) C 0.7655(3) 0.2481(2) -0.3376(2) 0.0550(9) Uani 1.00 d . . . C(5) C 0.7047(3) 0.2216(3) -0.4343(3) 0.072(1) Uani 1.00 d . . . C(6) C 0.6076(3) 0.2485(4) -0.4701(3) 0.080(1) Uani 1.00 d . . . C(7) C 0.5678(3) 0.3025(3) -0.4099(3) 0.076(1) Uani 1.00 d . . . C(8) C 0.6232(2) 0.3291(3) -0.3163(2) 0.0588(10) Uani 1.00 d . . . C(9) C 0.7244(2) 0.3021(2) -0.2745(2) 0.0477(8) Uani 1.00 d . . . C(10) C 0.7873(2) 0.3258(2) -0.1749(2) 0.0447(8) Uani 1.00 d . . . C(11) C 0.7440(2) 0.3699(2) -0.1077(2) 0.0497(8) Uani 1.00 d . . . C(12) C 0.7297(2) 0.4260(3) 0.0491(2) 0.067(1) Uani 1.00 d . . . C(13) C 0.6247(2) 0.4539(3) -0.0060(3) 0.064(1) Uani 1.00 d . . . C(14) C 0.7261(3) 0.3318(3) 0.1216(4) 0.091(2) Uani 1.00 d . . . C(15) C 0.7913(2) 0.5062(3) 0.1122(3) 0.065(1) Uani 1.00 d . . . C(16) C 0.7602(2) 0.5365(3) 0.2017(2) 0.0563(9) Uani 1.00 d . . . C(17) C 0.7882(3) 0.5988(3) 0.0430(3) 0.072(1) Uani 1.00 d . . . C(18) C 0.9626(2) 0.4970(3) 0.2309(3) 0.0550(9) Uani 1.00 d . . . C(19) C 1.0671(2) 0.4757(2) 0.2688(2) 0.0502(8) Uani 1.00 d . . . C(20) C 1.1245(2) 0.5068(2) 0.3685(2) 0.0521(9) Uani 1.00 d . . . C(21) C 1.0835(2) 0.5536(3) 0.4347(3) 0.063(1) Uani 1.00 d . . . C(22) C 1.1420(3) 0.5856(4) 0.5258(3) 0.076(1) Uani 1.00 d . . . C(23) C 1.2455(3) 0.5706(4) 0.5593(3) 0.081(1) Uani 1.00 d . . . C(24) C 1.2867(2) 0.5225(3) 0.4983(3) 0.070(1) Uani 1.00 d . . . C(25) C 1.2297(2) 0.4899(2) 0.4031(3) 0.0572(9) Uani 1.00 d . . . C(26) C 1.2732(2) 0.4430(3) 0.3391(3) 0.065(1) Uani 1.00 d . . . C(27) C 1.2198(2) 0.4154(3) 0.2457(3) 0.063(1) Uani 1.00 d . . . C(28) C 1.1139(2) 0.4319(2) 0.2075(3) 0.0537(9) Uani 1.00 d . . . C(29) C 0.9703(2) 0.1696(3) 0.1853(3) 0.0548(9) Uani 1.00 d . . . H(1) H 0.9961 0.2332 -0.1900 0.0784 Uiso 1.00 calc . . . H(2) H 0.8954 0.1861 -0.3421 0.0815 Uiso 1.00 calc . . . H(3) H 0.7327 0.1840 -0.4750 0.0862 Uiso 1.00 calc . . . H(4) H 0.5675 0.2307 -0.5355 0.0963 Uiso 1.00 calc . . . H(5) H 0.4996 0.3216 -0.4348 0.0907 Uiso 1.00 calc . . . H(6) H 0.5928 0.3670 -0.2778 0.0705 Uiso 1.00 calc . . . H(7) H 0.6753 0.3873 -0.1344 0.0597 Uiso 1.00 calc . . . H(8) H 0.5926 0.4735 0.0394 0.0770 Uiso 1.00 calc . . . H(9) H 0.6233 0.5090 -0.0492 0.0770 Uiso 1.00 calc . . . H(10) H 0.5910 0.3972 -0.0434 0.0770 Uiso 1.00 calc . . . H(11) H 0.6925 0.3528 0.1653 0.1093 Uiso 1.00 calc . . . H(12) H 0.6916 0.2761 0.0829 0.1093 Uiso 1.00 calc . . . H(13) H 0.7922 0.3117 0.1587 0.1093 Uiso 1.00 calc . . . H(14) H 0.8044 0.5872 0.2393 0.0676 Uiso 1.00 calc . . . H(15) H 0.6941 0.5625 0.1789 0.0676 Uiso 1.00 calc . . . H(16) H 0.7630 0.4785 0.2419 0.0676 Uiso 1.00 calc . . . H(17) H 0.8265 0.6530 0.0808 0.0861 Uiso 1.00 calc . . . H(18) H 0.8149 0.5792 -0.0066 0.0861 Uiso 1.00 calc . . . H(19) H 0.7211 0.6204 0.0127 0.0861 Uiso 1.00 calc . . . H(20) H 0.9379 0.5407 0.2700 0.0660 Uiso 1.00 calc . . . H(21) H 1.0134 0.5628 0.4150 0.0756 Uiso 1.00 calc . . . H(22) H 1.1121 0.6188 0.5676 0.0914 Uiso 1.00 calc . . . H(23) H 1.2859 0.5933 0.6229 0.0973 Uiso 1.00 calc . . . H(24) H 1.3565 0.5107 0.5210 0.0835 Uiso 1.00 calc . . . H(25) H 1.3430 0.4303 0.3627 0.0778 Uiso 1.00 calc . . . H(26) H 1.2523 0.3848 0.2050 0.0755 Uiso 1.00 calc . . . 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 Mn(1) 0.0413(3) 0.0461(3) 0.0561(3) 0.0073(2) 0.0229(2) -0.0047(2) S(1) 0.0739(6) 0.1005(9) 0.0828(8) -0.0030(6) 0.0026(6) 0.0384(7) O(1) 0.054(1) 0.095(2) 0.064(2) 0.023(1) 0.028(1) -0.010(1) O(2) 0.041(1) 0.075(2) 0.080(2) -0.001(1) 0.027(1) -0.023(1) N(1) 0.045(1) 0.054(1) 0.048(1) 0.012(1) 0.023(1) -0.004(1) N(2) 0.039(1) 0.053(1) 0.059(2) -0.001(1) 0.021(1) -0.014(1) N(3) 0.067(2) 0.051(2) 0.094(2) 0.011(1) 0.029(2) 0.013(2) C(1) 0.065(2) 0.050(2) 0.058(2) 0.013(1) 0.037(2) 0.003(1) C(2) 0.076(2) 0.067(2) 0.068(2) 0.027(2) 0.044(2) 0.004(2) C(3) 0.102(3) 0.058(2) 0.068(2) 0.019(2) 0.060(2) 0.003(2) C(4) 0.086(2) 0.039(2) 0.058(2) 0.001(2) 0.048(2) 0.003(1) C(5) 0.116(3) 0.056(2) 0.063(2) -0.009(2) 0.057(2) -0.015(2) C(6) 0.093(3) 0.096(3) 0.064(2) -0.034(3) 0.043(2) -0.026(2) C(7) 0.070(2) 0.103(3) 0.062(2) -0.029(2) 0.032(2) -0.023(2) C(8) 0.061(2) 0.068(2) 0.058(2) -0.016(2) 0.034(2) -0.016(2) C(9) 0.069(2) 0.035(1) 0.053(2) -0.006(1) 0.039(2) -0.001(1) C(10) 0.058(2) 0.037(1) 0.050(2) 0.005(1) 0.034(1) 0.004(1) C(11) 0.051(2) 0.053(2) 0.052(2) 0.010(1) 0.025(1) -0.002(1) C(12) 0.047(2) 0.103(3) 0.052(2) 0.020(2) 0.018(1) -0.022(2) C(13) 0.044(2) 0.089(3) 0.061(2) 0.009(2) 0.020(1) -0.025(2) C(14) 0.103(3) 0.056(2) 0.155(4) 0.001(2) 0.096(3) 0.010(2) C(15) 0.048(2) 0.078(2) 0.074(2) 0.011(2) 0.027(2) -0.019(2) C(16) 0.047(2) 0.068(2) 0.058(2) 0.006(1) 0.024(1) -0.019(2) C(17) 0.089(3) 0.049(2) 0.092(3) 0.026(2) 0.051(2) 0.026(2) C(18) 0.046(1) 0.057(2) 0.066(2) -0.001(1) 0.024(2) -0.015(2) C(19) 0.046(1) 0.044(2) 0.063(2) -0.002(1) 0.020(1) 0.003(1) C(20) 0.046(1) 0.050(2) 0.060(2) -0.007(1) 0.017(1) 0.011(1) C(21) 0.051(2) 0.079(2) 0.057(2) -0.010(2) 0.015(2) 0.003(2) C(22) 0.065(2) 0.104(3) 0.060(2) -0.013(2) 0.021(2) 0.001(2) C(23) 0.064(2) 0.115(4) 0.057(2) -0.027(2) 0.010(2) 0.013(2) C(24) 0.049(2) 0.080(3) 0.073(2) -0.011(2) 0.010(2) 0.025(2) C(25) 0.047(2) 0.052(2) 0.065(2) -0.009(1) 0.009(2) 0.020(2) C(26) 0.040(1) 0.058(2) 0.096(3) 0.004(1) 0.022(2) 0.018(2) C(27) 0.045(2) 0.050(2) 0.098(3) 0.004(1) 0.030(2) 0.000(2) C(28) 0.041(1) 0.041(2) 0.082(2) 0.000(1) 0.025(2) 0.001(2) C(29) 0.035(1) 0.065(2) 0.062(2) -0.004(1) 0.013(1) -0.004(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) O(1) 1.877(2) . . yes Mn(1) O(2) 1.877(2) . . yes Mn(1) N(1) 1.978(2) . . yes Mn(1) N(2) 1.966(2) . . yes Mn(1) N(3) 2.096(3) . . yes S(1) C(29) 1.625(4) . . yes O(1) C(1) 1.305(4) . . yes O(2) C(28) 1.314(4) . . yes N(1) C(11) 1.298(4) . . yes N(1) C(12) 1.506(4) . . yes N(2) C(15) 1.534(4) . . yes N(2) C(18) 1.283(4) . . yes N(3) C(29) 1.140(4) . . yes C(1) C(2) 1.432(4) . . yes C(1) C(10) 1.395(4) . . yes C(2) C(3) 1.337(5) . . yes C(3) C(4) 1.410(5) . . yes C(4) C(5) 1.410(5) . . yes C(4) C(9) 1.424(4) . . yes C(5) C(6) 1.351(6) . . yes C(6) C(7) 1.380(5) . . yes C(7) C(8) 1.357(5) . . yes C(8) C(9) 1.409(4) . . yes C(9) C(10) 1.443(4) . . yes C(10) C(11) 1.432(4) . . yes C(12) C(13) 1.484(4) . . yes C(12) C(14) 1.630(6) . . yes C(12) C(15) 1.474(5) . . yes C(15) C(16) 1.548(4) . . yes C(15) C(17) 1.563(5) . . yes C(18) C(19) 1.430(4) . . yes C(19) C(20) 1.449(5) . . yes C(19) C(28) 1.396(4) . . yes C(20) C(21) 1.413(5) . . yes C(20) C(25) 1.429(4) . . yes C(21) C(22) 1.361(5) . . yes C(22) C(23) 1.403(5) . . yes C(23) C(24) 1.364(6) . . yes C(24) C(25) 1.402(5) . . yes C(25) C(26) 1.413(5) . . yes C(26) C(27) 1.350(5) . . yes C(27) C(28) 1.437(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(2) 91.7(1) . . . yes O(1) Mn(1) N(1) 90.81(9) . . . yes O(1) Mn(1) N(2) 162.4(1) . . . yes O(1) Mn(1) N(3) 97.5(1) . . . yes O(2) Mn(1) N(1) 160.9(1) . . . yes O(2) Mn(1) N(2) 91.10(9) . . . yes O(2) Mn(1) N(3) 94.5(1) . . . yes N(1) Mn(1) N(2) 81.05(9) . . . yes N(1) Mn(1) N(3) 104.0(1) . . . yes N(2) Mn(1) N(3) 99.6(1) . . . yes Mn(1) O(1) C(1) 130.9(2) . . . yes Mn(1) O(2) C(28) 125.9(2) . . . yes Mn(1) N(1) C(11) 125.1(2) . . . yes Mn(1) N(1) C(12) 113.8(2) . . . yes C(11) N(1) C(12) 121.0(2) . . . yes Mn(1) N(2) C(15) 114.5(2) . . . yes Mn(1) N(2) C(18) 123.0(2) . . . yes C(15) N(2) C(18) 121.8(2) . . . yes Mn(1) N(3) C(29) 166.0(3) . . . yes O(1) C(1) C(2) 116.6(3) . . . yes O(1) C(1) C(10) 124.6(2) . . . yes C(2) C(1) C(10) 118.8(3) . . . yes C(1) C(2) C(3) 121.0(3) . . . yes C(2) C(3) C(4) 122.8(3) . . . yes C(3) C(4) C(5) 121.7(3) . . . yes C(3) C(4) C(9) 118.1(3) . . . yes C(5) C(4) C(9) 120.2(3) . . . yes C(4) C(5) C(6) 121.4(3) . . . yes C(5) C(6) C(7) 118.7(4) . . . yes C(6) C(7) C(8) 122.0(4) . . . yes C(7) C(8) C(9) 121.9(3) . . . yes C(4) C(9) C(8) 115.8(3) . . . yes C(4) C(9) C(10) 119.3(3) . . . yes C(8) C(9) C(10) 124.9(2) . . . yes C(1) C(10) C(9) 119.9(2) . . . yes C(1) C(10) C(11) 120.6(3) . . . yes C(9) C(10) C(11) 119.4(2) . . . yes N(1) C(11) C(10) 127.3(3) . . . yes N(1) C(12) C(13) 114.8(3) . . . yes N(1) C(12) C(14) 106.4(3) . . . yes N(1) C(12) C(15) 105.7(3) . . . yes C(13) C(12) C(14) 106.6(3) . . . yes C(13) C(12) C(15) 115.8(3) . . . yes C(14) C(12) C(15) 107.0(3) . . . yes N(2) C(15) C(12) 106.1(3) . . . yes N(2) C(15) C(16) 108.7(3) . . . yes N(2) C(15) C(17) 108.7(3) . . . yes C(12) C(15) C(16) 114.7(3) . . . yes C(12) C(15) C(17) 106.5(3) . . . yes C(16) C(15) C(17) 111.9(3) . . . yes N(2) C(18) C(19) 128.0(3) . . . yes C(18) C(19) C(20) 119.3(3) . . . yes C(18) C(19) C(28) 119.9(3) . . . yes C(20) C(19) C(28) 120.6(3) . . . yes C(19) C(20) C(21) 124.4(3) . . . yes C(19) C(20) C(25) 118.5(3) . . . yes C(21) C(20) C(25) 117.1(3) . . . yes C(20) C(21) C(22) 121.7(3) . . . yes C(21) C(22) C(23) 121.2(4) . . . yes C(22) C(23) C(24) 118.4(4) . . . yes C(23) C(24) C(25) 122.4(3) . . . yes C(20) C(25) C(24) 119.2(3) . . . yes C(20) C(25) C(26) 118.7(3) . . . yes C(24) C(25) C(26) 122.1(3) . . . yes C(25) C(26) C(27) 122.7(3) . . . yes C(26) C(27) C(28) 120.5(3) . . . yes O(2) C(28) C(19) 124.0(3) . . . yes O(2) C(28) C(27) 116.9(3) . . . yes C(19) C(28) C(27) 119.0(3) . . . yes S(1) C(29) N(3) 177.9(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 3.588(4) . 3_765 ? O(2) C(17) 3.524(4) . 3_765 ? C(1) C(19) 3.585(4) . 3_765 ? C(4) C(16) 3.488(4) . 2_645 ? C(4) C(25) 3.579(4) . 3_765 ? C(5) C(23) 3.473(5) . 3_765 ? C(5) C(24) 3.502(5) . 3_765 ? C(6) C(24) 3.451(5) . 3_765 ? C(8) C(26) 3.406(5) . 3_765 ? C(9) C(26) 3.482(4) . 3_765 ? C(9) C(25) 3.484(4) . 3_765 ? C(10) C(27) 3.545(4) . 3_765 ? C(10) C(28) 3.578(4) . 3_765 ? C(11) C(27) 3.586(5) . 3_765 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Mn(saltmen)(Cl)] _database_code_CSD 168759 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H22 Cl N2 Mn O2 ' _chemical_formula_moiety '?' _chemical_formula_weight 412.80 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 20.1584(5) _cell_length_b 21.9138(5) _cell_length_c 8.6859(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3836.9(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 52562 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712.00 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.943 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 34410 _diffrn_reflns_av_R_equivalents 0.096 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.2796 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.2796 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4931 _reflns_number_gt 2982 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0777 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4931 _refine_ls_number_parameters 470 _refine_ls_goodness_of_fit_ref 0.570 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04700(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0054 _refine_diff_density_max 0.59 _refine_diff_density_min -0.61 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.44(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.73162(4) 0.15000(4) 0.7265(1) 0.0188(2) Uani 1.00 d . . . Mn(2) Mn 0.37976(5) 0.09747(4) 0.6154(1) 0.0184(2) Uani 1.00 d . . . Cl(1) Cl 0.73141(9) 0.07809(7) 0.5249(2) 0.0309(4) Uani 1.00 d . . . Cl(2) Cl 0.28297(7) 0.10501(7) 0.7745(2) 0.0272(4) Uani 1.00 d . . . O(1) O 0.7158(2) 0.2222(2) 0.6131(5) 0.026(1) Uani 1.00 d . . . O(2) O 0.8233(2) 0.1629(2) 0.7257(5) 0.0231(9) Uani 1.00 d . . . O(3) O 0.4295(2) 0.0341(2) 0.7071(5) 0.029(1) Uani 1.00 d . . . O(4) O 0.4287(2) 0.1558(2) 0.7250(5) 0.0220(10) Uani 1.00 d . . . N(1) N 0.6361(2) 0.1416(2) 0.7742(6) 0.019(1) Uani 1.00 d . . . N(2) N 0.7391(2) 0.1022(2) 0.9187(5) 0.019(1) Uani 1.00 d . . . N(3) N 0.3479(2) 0.0420(2) 0.4502(6) 0.019(1) Uani 1.00 d . . . N(4) N 0.3579(2) 0.1590(2) 0.4556(5) 0.016(1) Uani 1.00 d . . . C(1) C 0.6619(3) 0.2331(2) 0.5303(7) 0.022(1) Uani 1.00 d . . . C(2) C 0.6651(3) 0.2762(3) 0.4108(8) 0.027(2) Uani 1.00 d . . . C(3) C 0.6107(4) 0.2883(3) 0.3216(7) 0.030(2) Uani 1.00 d . . . C(4) C 0.5503(3) 0.2594(3) 0.3465(8) 0.032(2) Uani 1.00 d . . . C(5) C 0.5454(3) 0.2188(3) 0.4656(7) 0.026(2) Uani 1.00 d . . . C(6) C 0.6002(3) 0.2046(3) 0.5594(7) 0.021(1) Uani 1.00 d . . . C(7) C 0.5902(3) 0.1639(3) 0.6877(7) 0.022(1) Uani 1.00 d . . . C(8) C 0.6199(3) 0.0984(3) 0.9047(7) 0.023(1) Uani 1.00 d . . . C(9) C 0.5536(3) 0.1142(3) 0.9815(8) 0.035(2) Uani 1.00 d . . . C(10) C 0.6154(4) 0.0348(3) 0.8387(7) 0.031(2) Uani 1.00 d . . . C(11) C 0.6789(3) 0.1054(3) 1.0188(7) 0.025(1) Uani 1.00 d . . . C(12) C 0.6799(3) 0.1686(3) 1.0947(8) 0.037(2) Uani 1.00 d . . . C(13) C 0.6785(3) 0.0569(3) 1.1426(8) 0.035(2) Uani 1.00 d . . . C(14) C 0.7916(3) 0.0728(2) 0.9568(7) 0.019(1) Uani 1.00 d . . . C(15) C 0.8536(3) 0.0744(2) 0.8757(7) 0.020(1) Uani 1.00 d . . . C(16) C 0.9031(3) 0.0329(3) 0.9160(7) 0.027(2) Uani 1.00 d . . . C(17) C 0.9649(3) 0.0351(3) 0.8487(8) 0.032(2) Uani 1.00 d . . . C(18) C 0.9777(3) 0.0785(3) 0.7365(8) 0.034(2) Uani 1.00 d . . . C(19) C 0.9296(3) 0.1199(3) 0.6937(7) 0.028(2) Uani 1.00 d . . . C(20) C 0.8669(3) 0.1196(2) 0.7629(7) 0.022(1) Uani 1.00 d . . . C(21) C 0.4205(3) -0.0255(3) 0.6937(8) 0.024(1) Uani 1.00 d . . . C(22) C 0.4512(3) -0.0647(3) 0.8012(8) 0.031(2) Uani 1.00 d . . . C(23) C 0.4434(3) -0.1267(3) 0.7894(9) 0.035(2) Uani 1.00 d . . . C(24) C 0.4053(3) -0.1530(3) 0.6741(8) 0.033(2) Uani 1.00 d . . . C(25) C 0.3751(3) -0.1159(2) 0.5682(7) 0.026(1) Uani 1.00 d . . . C(26) C 0.3822(3) -0.0522(2) 0.5759(7) 0.022(1) Uani 1.00 d . . . C(27) C 0.3503(3) -0.0169(2) 0.4582(7) 0.021(1) Uani 1.00 d . . . C(28) C 0.3122(3) 0.0724(3) 0.3178(7) 0.021(1) Uani 1.00 d . . . C(29) C 0.3148(4) 0.0339(3) 0.1704(8) 0.031(2) Uani 1.00 d . . . C(30) C 0.2401(3) 0.0810(3) 0.3702(7) 0.028(1) Uani 1.00 d . . . C(31) C 0.3485(3) 0.1348(2) 0.2960(7) 0.020(1) Uani 1.00 d . . . C(32) C 0.4179(3) 0.1261(3) 0.2283(8) 0.027(1) Uani 1.00 d . . . C(33) C 0.3095(3) 0.1782(3) 0.1926(7) 0.027(2) Uani 1.00 d . . . C(34) C 0.3536(3) 0.2165(2) 0.4859(7) 0.019(1) Uani 1.00 d . . . C(35) C 0.3714(3) 0.2442(2) 0.6298(7) 0.019(1) Uani 1.00 d . . . C(36) C 0.3563(3) 0.3071(3) 0.6508(7) 0.025(1) Uani 1.00 d . . . C(37) C 0.3790(3) 0.3383(3) 0.7764(7) 0.030(2) Uani 1.00 d . . . C(38) C 0.4181(3) 0.3076(3) 0.8860(8) 0.030(2) Uani 1.00 d . . . C(39) C 0.4332(3) 0.2472(3) 0.8684(7) 0.024(1) Uani 1.00 d . . . C(40) C 0.4106(3) 0.2141(2) 0.7407(7) 0.020(1) Uani 1.00 d . . . H(1) H 0.7055 0.2972 0.3916 0.0322 Uiso 1.00 calc . . . H(2) H 0.6143 0.3171 0.2404 0.0360 Uiso 1.00 calc . . . H(3) H 0.5132 0.2678 0.2825 0.0383 Uiso 1.00 calc . . . H(4) H 0.5040 0.1996 0.4853 0.0315 Uiso 1.00 calc . . . H(5) H 0.5458 0.1524 0.7104 0.0270 Uiso 1.00 calc . . . H(6) H 0.5557 0.1542 1.0230 0.0422 Uiso 1.00 calc . . . H(7) H 0.5190 0.1121 0.9073 0.0422 Uiso 1.00 calc . . . H(8) H 0.5449 0.0858 1.0619 0.0422 Uiso 1.00 calc . . . H(9) H 0.6057 0.0067 0.9188 0.0369 Uiso 1.00 calc . . . H(10) H 0.5812 0.0334 0.7635 0.0369 Uiso 1.00 calc . . . H(11) H 0.6565 0.0243 0.7922 0.0369 Uiso 1.00 calc . . . H(12) H 0.7192 0.1728 1.1541 0.0446 Uiso 1.00 calc . . . H(13) H 0.6788 0.1992 1.0174 0.0446 Uiso 1.00 calc . . . H(14) H 0.6423 0.1728 1.1597 0.0446 Uiso 1.00 calc . . . H(15) H 0.6405 0.0620 1.2058 0.0419 Uiso 1.00 calc . . . H(16) H 0.6775 0.0177 1.0960 0.0419 Uiso 1.00 calc . . . H(17) H 0.7174 0.0606 1.2036 0.0419 Uiso 1.00 calc . . . H(18) H 0.7893 0.0479 1.0462 0.0224 Uiso 1.00 calc . . . H(19) H 0.8940 0.0025 0.9912 0.0325 Uiso 1.00 calc . . . H(20) H 0.9985 0.0072 0.8790 0.0385 Uiso 1.00 calc . . . H(21) H 1.0200 0.0798 0.6885 0.0405 Uiso 1.00 calc . . . H(22) H 0.9391 0.1491 0.6160 0.0333 Uiso 1.00 calc . . . H(23) H 0.4774 -0.0481 0.8819 0.0373 Uiso 1.00 calc . . . H(24) H 0.4647 -0.1523 0.8624 0.0424 Uiso 1.00 calc . . . H(25) H 0.4003 -0.1960 0.6686 0.0401 Uiso 1.00 calc . . . H(26) H 0.3490 -0.1335 0.4887 0.0314 Uiso 1.00 calc . . . H(27) H 0.3289 -0.0389 0.3783 0.0255 Uiso 1.00 calc . . . H(28) H 0.2944 -0.0045 0.1886 0.0368 Uiso 1.00 calc . . . H(29) H 0.2918 0.0546 0.0903 0.0368 Uiso 1.00 calc . . . H(30) H 0.3597 0.0279 0.1409 0.0368 Uiso 1.00 calc . . . H(31) H 0.2391 0.1059 0.4597 0.0330 Uiso 1.00 calc . . . H(32) H 0.2155 0.1000 0.2904 0.0330 Uiso 1.00 calc . . . H(33) H 0.2212 0.0423 0.3930 0.0330 Uiso 1.00 calc . . . H(34) H 0.4422 0.0983 0.2903 0.0327 Uiso 1.00 calc . . . H(35) H 0.4143 0.1105 0.1266 0.0327 Uiso 1.00 calc . . . H(36) H 0.4403 0.1643 0.2259 0.0327 Uiso 1.00 calc . . . H(37) H 0.3319 0.2163 0.1871 0.0329 Uiso 1.00 calc . . . H(38) H 0.3060 0.1612 0.0924 0.0329 Uiso 1.00 calc . . . H(39) H 0.2664 0.1841 0.2341 0.0329 Uiso 1.00 calc . . . H(40) H 0.3373 0.2425 0.4069 0.0225 Uiso 1.00 calc . . . H(41) H 0.3299 0.3277 0.5764 0.0297 Uiso 1.00 calc . . . H(42) H 0.3685 0.3802 0.7896 0.0359 Uiso 1.00 calc . . . H(43) H 0.4343 0.3291 0.9732 0.0356 Uiso 1.00 calc . . . H(44) H 0.4595 0.2273 0.9441 0.0291 Uiso 1.00 calc . . . 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 Mn(1) 0.0173(4) 0.0202(4) 0.0189(4) -0.0020(4) -0.0009(4) 0.0031(4) Mn(2) 0.0200(4) 0.0179(4) 0.0173(4) -0.0012(4) -0.0042(4) 0.0025(4) Cl(1) 0.0402(9) 0.0290(7) 0.0236(7) -0.0054(8) 0.0010(8) -0.0054(6) Cl(2) 0.0279(7) 0.0336(8) 0.0202(7) -0.0069(7) 0.0020(7) 0.0011(7) O(1) 0.024(2) 0.021(2) 0.034(2) -0.004(2) -0.007(2) 0.009(2) O(2) 0.019(1) 0.022(2) 0.027(2) -0.005(2) -0.001(2) 0.007(2) O(3) 0.031(2) 0.020(2) 0.034(3) 0.003(2) -0.017(2) 0.007(2) O(4) 0.025(2) 0.018(2) 0.022(2) -0.001(2) -0.007(2) -0.004(2) N(1) 0.018(2) 0.025(2) 0.015(2) 0.000(2) 0.002(2) 0.005(2) N(2) 0.018(2) 0.020(2) 0.019(2) -0.001(2) 0.001(2) 0.000(2) N(3) 0.019(3) 0.021(2) 0.017(2) -0.005(2) -0.001(2) 0.002(2) N(4) 0.013(2) 0.021(2) 0.014(2) 0.000(2) -0.002(2) 0.002(2) C(1) 0.027(2) 0.015(3) 0.024(3) 0.002(2) -0.003(2) -0.002(2) C(2) 0.033(3) 0.018(3) 0.029(3) -0.003(3) 0.006(3) 0.003(3) C(3) 0.044(3) 0.024(3) 0.022(3) 0.004(3) 0.000(3) 0.011(3) C(4) 0.034(3) 0.040(4) 0.022(3) 0.009(3) -0.008(3) 0.004(3) C(5) 0.021(3) 0.035(3) 0.023(3) 0.001(3) -0.003(3) 0.000(3) C(6) 0.024(3) 0.022(3) 0.018(3) 0.005(2) 0.000(2) 0.000(2) C(7) 0.018(3) 0.030(3) 0.020(3) 0.000(3) -0.003(2) 0.003(2) C(8) 0.021(2) 0.028(2) 0.019(3) 0.000(3) 0.003(2) 0.011(2) C(9) 0.020(3) 0.056(4) 0.030(3) 0.008(3) 0.005(3) 0.014(4) C(10) 0.035(4) 0.031(3) 0.026(3) -0.009(3) 0.000(3) 0.007(3) C(11) 0.021(2) 0.037(3) 0.016(3) 0.003(3) 0.003(2) 0.002(2) C(12) 0.035(4) 0.045(4) 0.032(4) 0.005(3) 0.000(3) -0.014(3) C(13) 0.027(3) 0.054(4) 0.024(4) 0.006(3) 0.000(3) 0.020(3) C(14) 0.022(2) 0.018(3) 0.016(3) -0.004(2) -0.004(2) 0.003(2) C(15) 0.020(2) 0.023(3) 0.018(3) -0.002(2) -0.006(2) -0.005(2) C(16) 0.027(3) 0.028(3) 0.026(3) 0.006(2) -0.005(3) -0.003(3) C(17) 0.025(3) 0.033(3) 0.038(4) 0.004(3) -0.008(3) -0.006(3) C(18) 0.019(3) 0.049(4) 0.034(4) 0.002(3) 0.003(3) 0.000(3) C(19) 0.021(3) 0.035(3) 0.027(3) -0.007(2) -0.001(2) 0.006(3) C(20) 0.020(2) 0.024(2) 0.023(3) -0.003(2) -0.005(2) -0.002(2) C(21) 0.020(3) 0.021(2) 0.030(3) 0.003(2) 0.002(3) 0.002(2) C(22) 0.029(3) 0.028(2) 0.036(4) 0.005(3) -0.005(3) 0.011(3) C(23) 0.031(4) 0.028(2) 0.047(4) 0.010(3) -0.004(3) 0.013(3) C(24) 0.043(4) 0.019(3) 0.038(4) 0.008(3) 0.010(3) 0.004(3) C(25) 0.027(3) 0.021(2) 0.030(3) 0.001(3) 0.008(3) -0.002(2) C(26) 0.019(3) 0.020(2) 0.026(3) 0.002(2) 0.006(2) 0.004(2) C(27) 0.021(3) 0.022(2) 0.021(3) -0.003(2) 0.007(3) 0.001(2) C(28) 0.024(3) 0.021(3) 0.018(3) -0.002(2) -0.003(2) 0.005(2) C(29) 0.048(4) 0.024(3) 0.020(3) -0.006(3) -0.005(3) 0.002(2) C(30) 0.023(3) 0.037(3) 0.023(3) -0.008(3) -0.006(3) 0.002(3) C(31) 0.028(3) 0.019(3) 0.015(2) 0.000(2) -0.002(2) -0.001(2) C(32) 0.030(3) 0.026(3) 0.026(3) -0.002(3) 0.008(3) 0.001(3) C(33) 0.038(4) 0.024(3) 0.021(3) 0.003(3) -0.008(3) 0.003(3) C(34) 0.013(3) 0.021(2) 0.022(3) 0.008(2) 0.000(3) 0.001(2) C(35) 0.017(3) 0.020(2) 0.019(3) 0.001(2) 0.007(2) 0.000(2) C(36) 0.025(3) 0.024(2) 0.026(3) 0.006(3) 0.006(3) -0.002(2) C(37) 0.039(3) 0.024(3) 0.027(3) 0.004(3) 0.005(3) -0.007(2) C(38) 0.038(4) 0.030(3) 0.020(3) 0.000(3) 0.001(3) -0.014(3) C(39) 0.022(3) 0.029(2) 0.022(3) 0.000(2) -0.003(3) -0.002(3) C(40) 0.018(3) 0.021(2) 0.020(3) -0.001(2) 0.005(2) 0.000(2) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) Cl(1) 2.356(1) . . yes Mn(1) O(1) 1.890(3) . . yes Mn(1) O(2) 1.870(3) . . yes Mn(1) N(1) 1.979(3) . . yes Mn(1) N(2) 1.977(3) . . yes Mn(2) Cl(2) 2.397(1) . . yes Mn(2) O(3) 1.889(3) . . yes Mn(2) O(4) 1.874(3) . . yes Mn(2) N(3) 1.986(4) . . yes Mn(2) N(4) 1.985(3) . . yes O(1) C(1) 1.325(5) . . yes O(2) C(20) 1.335(5) . . yes O(3) C(21) 1.322(5) . . yes O(4) C(40) 1.337(5) . . yes N(1) C(7) 1.287(5) . . yes N(1) C(8) 1.512(5) . . yes N(2) C(11) 1.494(5) . . yes N(2) C(14) 1.283(5) . . yes N(3) C(27) 1.294(5) . . yes N(3) C(28) 1.511(5) . . yes N(4) C(31) 1.496(5) . . yes N(4) C(34) 1.289(5) . . yes C(1) C(2) 1.405(6) . . yes C(1) C(6) 1.415(6) . . yes C(2) C(3) 1.370(7) . . yes C(3) C(4) 1.388(7) . . yes C(4) C(5) 1.369(6) . . yes C(5) C(6) 1.407(6) . . yes C(6) C(7) 1.442(6) . . yes C(8) C(9) 1.534(6) . . yes C(8) C(10) 1.510(6) . . yes C(8) C(11) 1.556(6) . . yes C(11) C(12) 1.533(6) . . yes C(11) C(13) 1.512(6) . . yes C(14) C(15) 1.435(6) . . yes C(15) C(16) 1.395(6) . . yes C(15) C(20) 1.418(6) . . yes C(16) C(17) 1.378(7) . . yes C(17) C(18) 1.386(7) . . yes C(18) C(19) 1.379(6) . . yes C(19) C(20) 1.399(6) . . yes C(21) C(22) 1.412(6) . . yes C(21) C(26) 1.409(6) . . yes C(22) C(23) 1.370(6) . . yes C(23) C(24) 1.388(7) . . yes C(24) C(25) 1.370(6) . . yes C(25) C(26) 1.407(5) . . yes C(26) C(27) 1.434(6) . . yes C(28) C(29) 1.534(6) . . yes C(28) C(30) 1.534(6) . . yes C(28) C(31) 1.561(6) . . yes C(31) C(32) 1.530(6) . . yes C(31) C(33) 1.525(6) . . yes C(34) C(35) 1.436(6) . . yes C(35) C(36) 1.423(6) . . yes C(35) C(40) 1.410(6) . . yes C(36) C(37) 1.366(6) . . yes C(37) C(38) 1.408(7) . . yes C(38) C(39) 1.366(6) . . yes C(39) C(40) 1.401(6) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Mn(1) O(1) 99.9(1) . . . yes Cl(1) Mn(1) O(2) 95.8(1) . . . yes Cl(1) Mn(1) N(1) 95.2(1) . . . yes Cl(1) Mn(1) N(2) 105.9(1) . . . yes O(1) Mn(1) O(2) 92.1(1) . . . yes O(1) Mn(1) N(1) 91.3(1) . . . yes O(1) Mn(1) N(2) 153.7(1) . . . yes O(2) Mn(1) N(1) 167.7(2) . . . yes O(2) Mn(1) N(2) 90.5(1) . . . yes N(1) Mn(1) N(2) 81.3(1) . . . yes Cl(2) Mn(2) O(3) 103.9(1) . . . yes Cl(2) Mn(2) O(4) 95.1(1) . . . yes Cl(2) Mn(2) N(3) 101.3(1) . . . yes Cl(2) Mn(2) N(4) 100.1(1) . . . yes O(3) Mn(2) O(4) 90.5(1) . . . yes O(3) Mn(2) N(3) 91.5(1) . . . yes O(3) Mn(2) N(4) 155.8(2) . . . yes O(4) Mn(2) N(3) 162.6(1) . . . yes O(4) Mn(2) N(4) 90.5(1) . . . yes N(3) Mn(2) N(4) 80.7(1) . . . yes Mn(1) O(1) C(1) 124.9(3) . . . yes Mn(1) O(2) C(20) 122.8(3) . . . yes Mn(2) O(3) C(21) 128.1(3) . . . yes Mn(2) O(4) C(40) 124.1(3) . . . yes Mn(1) N(1) C(7) 122.8(3) . . . yes Mn(1) N(1) C(8) 115.1(3) . . . yes C(7) N(1) C(8) 121.4(3) . . . yes Mn(1) N(2) C(11) 113.8(3) . . . yes Mn(1) N(2) C(14) 123.2(3) . . . yes C(11) N(2) C(14) 122.9(4) . . . yes Mn(2) N(3) C(27) 124.0(3) . . . yes Mn(2) N(3) C(28) 115.7(2) . . . yes C(27) N(3) C(28) 119.9(4) . . . yes Mn(2) N(4) C(31) 115.8(2) . . . yes Mn(2) N(4) C(34) 122.4(3) . . . yes C(31) N(4) C(34) 121.8(4) . . . yes O(1) C(1) C(2) 119.0(4) . . . yes O(1) C(1) C(6) 123.0(4) . . . yes C(2) C(1) C(6) 118.0(4) . . . yes C(1) C(2) C(3) 120.7(4) . . . yes C(2) C(3) C(4) 121.8(4) . . . yes C(3) C(4) C(5) 118.5(4) . . . yes C(4) C(5) C(6) 121.7(4) . . . yes C(1) C(6) C(5) 119.3(4) . . . yes C(1) C(6) C(7) 122.2(4) . . . yes C(5) C(6) C(7) 118.4(4) . . . yes N(1) C(7) C(6) 125.9(4) . . . yes N(1) C(8) C(9) 111.9(3) . . . yes N(1) C(8) C(10) 107.8(4) . . . yes N(1) C(8) C(11) 104.6(3) . . . yes C(9) C(8) C(10) 108.7(4) . . . yes C(9) C(8) C(11) 111.5(4) . . . yes C(10) C(8) C(11) 112.3(4) . . . yes N(2) C(11) C(8) 104.2(3) . . . yes N(2) C(11) C(12) 106.4(4) . . . yes N(2) C(11) C(13) 112.6(4) . . . yes C(8) C(11) C(12) 111.9(4) . . . yes C(8) C(11) C(13) 112.3(4) . . . yes C(12) C(11) C(13) 109.2(4) . . . yes N(2) C(14) C(15) 125.4(4) . . . yes C(14) C(15) C(16) 118.9(4) . . . yes C(14) C(15) C(20) 121.4(4) . . . yes C(16) C(15) C(20) 119.6(4) . . . yes C(15) C(16) C(17) 121.1(5) . . . yes C(16) C(17) C(18) 119.5(4) . . . yes C(17) C(18) C(19) 120.6(4) . . . yes C(18) C(19) C(20) 121.1(4) . . . yes O(2) C(20) C(15) 122.7(4) . . . yes O(2) C(20) C(19) 119.2(4) . . . yes C(15) C(20) C(19) 118.1(4) . . . yes O(3) C(21) C(22) 118.9(4) . . . yes O(3) C(21) C(26) 123.2(4) . . . yes C(22) C(21) C(26) 117.9(4) . . . yes C(21) C(22) C(23) 120.2(5) . . . yes C(22) C(23) C(24) 122.0(5) . . . yes C(23) C(24) C(25) 119.0(4) . . . yes C(24) C(25) C(26) 120.8(5) . . . yes C(21) C(26) C(25) 120.2(4) . . . yes C(21) C(26) C(27) 122.7(4) . . . yes C(25) C(26) C(27) 117.1(4) . . . yes N(3) C(27) C(26) 126.4(4) . . . yes N(3) C(28) C(29) 112.2(3) . . . yes N(3) C(28) C(30) 106.2(3) . . . yes N(3) C(28) C(31) 104.8(3) . . . yes C(29) C(28) C(30) 110.3(4) . . . yes C(29) C(28) C(31) 111.4(4) . . . yes C(30) C(28) C(31) 111.9(4) . . . yes N(4) C(31) C(28) 104.9(3) . . . yes N(4) C(31) C(32) 106.5(4) . . . yes N(4) C(31) C(33) 112.9(3) . . . yes C(28) C(31) C(32) 111.5(3) . . . yes C(28) C(31) C(33) 112.1(4) . . . yes C(32) C(31) C(33) 108.8(4) . . . yes N(4) C(34) C(35) 125.0(4) . . . yes C(34) C(35) C(36) 117.9(4) . . . yes C(34) C(35) C(40) 122.5(4) . . . yes C(36) C(35) C(40) 119.1(4) . . . yes C(35) C(36) C(37) 121.0(4) . . . yes C(36) C(37) C(38) 119.2(4) . . . yes C(37) C(38) C(39) 120.8(4) . . . yes C(38) C(39) C(40) 121.1(4) . . . yes O(4) C(40) C(35) 122.0(4) . . . yes O(4) C(40) C(39) 119.2(4) . . . yes C(35) C(40) C(39) 118.7(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(14) 3.391(4) . 2_654 ? Cl(1) C(13) 3.519(5) . 1_554 ? O(1) C(34) 3.202(5) . 3_556 ? O(1) C(33) 3.343(6) . 3_556 ? O(2) C(34) 3.276(5) . 3_556 ? O(2) C(36) 3.401(6) . 3_556 ? O(2) C(33) 3.564(5) . 3_556 ? O(4) C(7) 3.277(5) . . ? O(4) C(9) 3.484(6) . . ? O(4) C(5) 3.537(6) . . ? C(3) C(12) 3.565(7) . 1_554 ? C(9) C(32) 3.485(7) . 1_556 ? C(13) C(16) 3.496(7) . 2_655 ? C(13) C(15) 3.578(7) . 2_655 ? C(14) C(37) 3.503(6) . 3_557 ? C(15) C(38) 3.559(6) . 3_557 ? C(20) C(38) 3.594(6) . 3_557 ? C(23) C(38) 3.491(7) . 4_646 ? C(25) C(30) 3.586(6) . 2_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Mn(naphtmen)(Cl)] _database_code_CSD 168760 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H26 Cl N2 Mn O2 ' _chemical_formula_moiety 'C28 H26 Cl N2 Mn O2 ' _chemical_formula_weight 512.92 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 13.481(3) _cell_length_b 12.266(1) _cell_length_c 14.388(3) _cell_angle_alpha 90 _cell_angle_beta 97.754(3) _cell_angle_gamma 90 _cell_volume 2357.4(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10691 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.080 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064.00 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.945 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11145 _diffrn_reflns_av_R_equivalents 0.129 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.8689 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.8689 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4698 _reflns_number_gt 2371 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.2350 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4698 _refine_ls_number_parameters 307 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.08200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0091 _refine_diff_density_max 1.13 _refine_diff_density_min -1.75 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Mn(1) Mn 0.53351(8) 0.07429(9) 0.62812(7) 0.0186(3) Uani 1.00 d . . . Cl(1) Cl 0.5508(1) 0.0714(2) 0.7951(1) 0.0299(5) Uani 1.00 d . . . O(1) O 0.3951(4) 0.0487(4) 0.6050(4) 0.024(1) Uani 1.00 d . . . O(2) O 0.5585(4) -0.0758(4) 0.6117(3) 0.025(1) Uani 1.00 d . . . N(1) N 0.5150(4) 0.2323(5) 0.6094(4) 0.018(2) Uani 1.00 d . . . N(2) N 0.6706(4) 0.1107(4) 0.6061(4) 0.017(2) Uani 1.00 d . . . C(1) C 0.3201(6) 0.1190(6) 0.6040(5) 0.024(2) Uani 1.00 d . . . C(2) C 0.2229(6) 0.0733(7) 0.6030(5) 0.031(2) Uani 1.00 d . . . C(3) C 0.1416(6) 0.1365(7) 0.5991(5) 0.029(2) Uani 1.00 d . . . C(4) C 0.1479(6) 0.2532(6) 0.5970(5) 0.026(2) Uani 1.00 d . . . C(5) C 0.0623(6) 0.3193(7) 0.5938(6) 0.034(2) Uani 1.00 d . . . C(6) C 0.0681(6) 0.4293(7) 0.5919(6) 0.037(2) Uani 1.00 d . . . C(7) C 0.1627(7) 0.4782(7) 0.5938(6) 0.038(3) Uani 1.00 d . . . C(8) C 0.2468(6) 0.4178(6) 0.5965(5) 0.030(2) Uani 1.00 d . . . C(9) C 0.2437(5) 0.3024(6) 0.5982(5) 0.024(2) Uani 1.00 d . . . C(10) C 0.3323(5) 0.2325(6) 0.6022(5) 0.019(2) Uani 1.00 d . . . C(11) C 0.4283(5) 0.2825(6) 0.6025(5) 0.019(2) Uani 1.00 d . . . C(12) C 0.6102(5) 0.2975(6) 0.6133(5) 0.019(2) Uani 1.00 d . . . C(13) C 0.6468(6) 0.3198(6) 0.7173(5) 0.028(2) Uani 1.00 d . . . C(14) C 0.5932(5) 0.4055(6) 0.5594(5) 0.024(2) Uani 1.00 d . . . C(15) C 0.6845(5) 0.2228(5) 0.5679(5) 0.016(2) Uani 1.00 d . . . C(16) C 0.6556(5) 0.2149(6) 0.4614(5) 0.021(2) Uani 1.00 d . . . C(17) C 0.7905(5) 0.2628(6) 0.5894(6) 0.025(2) Uani 1.00 d . . . C(18) C 0.7438(5) 0.0399(6) 0.6118(5) 0.023(2) Uani 1.00 d . . . C(19) C 0.7384(5) -0.0745(6) 0.6343(5) 0.021(2) Uani 1.00 d . . . C(20) C 0.8310(6) -0.1367(6) 0.6492(5) 0.025(2) Uani 1.00 d . . . C(21) C 0.9270(6) -0.0912(6) 0.6566(6) 0.034(2) Uani 1.00 d . . . C(22) C 1.0121(6) -0.1552(8) 0.6658(7) 0.040(3) Uani 1.00 d . . . C(23) C 1.0039(7) -0.2683(8) 0.6744(7) 0.043(3) Uani 1.00 d . . . C(24) C 0.9134(7) -0.3154(7) 0.6698(6) 0.039(3) Uani 1.00 d . . . C(25) C 0.8240(6) -0.2525(6) 0.6579(5) 0.027(2) Uani 1.00 d . . . C(26) C 0.7273(6) -0.2998(6) 0.6560(5) 0.029(2) Uani 1.00 d . . . C(27) C 0.6412(6) -0.2417(6) 0.6433(5) 0.024(2) Uani 1.00 d . . . C(28) C 0.6457(6) -0.1259(6) 0.6305(5) 0.022(2) Uani 1.00 d . . . H(1) H 0.2154 -0.0034 0.6046 0.0358 Uiso 1.00 calc . . . H(2) H 0.0780 0.1029 0.5980 0.0342 Uiso 1.00 calc . . . H(3) H -0.0013 0.2854 0.5925 0.0388 Uiso 1.00 calc . . . H(4) H 0.0092 0.4720 0.5888 0.0445 Uiso 1.00 calc . . . H(5) H 0.1669 0.5553 0.5937 0.0470 Uiso 1.00 calc . . . H(6) H 0.3093 0.4538 0.5972 0.0352 Uiso 1.00 calc . . . H(7) H 0.4292 0.3598 0.5974 0.0227 Uiso 1.00 calc . . . H(8) H 0.6595 0.2521 0.7493 0.0337 Uiso 1.00 calc . . . H(9) H 0.7066 0.3613 0.7228 0.0337 Uiso 1.00 calc . . . H(10) H 0.5968 0.3586 0.7441 0.0337 Uiso 1.00 calc . . . H(11) H 0.6542 0.4450 0.5644 0.0283 Uiso 1.00 calc . . . H(12) H 0.5699 0.3910 0.4956 0.0283 Uiso 1.00 calc . . . H(13) H 0.5445 0.4476 0.5858 0.0283 Uiso 1.00 calc . . . H(14) H 0.6636 0.2843 0.4337 0.0257 Uiso 1.00 calc . . . H(15) H 0.6975 0.1633 0.4365 0.0257 Uiso 1.00 calc . . . H(16) H 0.5878 0.1925 0.4478 0.0257 Uiso 1.00 calc . . . H(17) H 0.8085 0.2682 0.6557 0.0299 Uiso 1.00 calc . . . H(18) H 0.8346 0.2132 0.5650 0.0299 Uiso 1.00 calc . . . H(19) H 0.7965 0.3326 0.5620 0.0299 Uiso 1.00 calc . . . H(20) H 0.8072 0.0665 0.5997 0.0283 Uiso 1.00 calc . . . H(21) H 0.9340 -0.0141 0.6555 0.0406 Uiso 1.00 calc . . . H(22) H 1.0763 -0.1232 0.6659 0.0467 Uiso 1.00 calc . . . H(23) H 1.0623 -0.3118 0.6848 0.0521 Uiso 1.00 calc . . . H(24) H 0.9090 -0.3920 0.6744 0.0447 Uiso 1.00 calc . . . H(25) H 0.7230 -0.3760 0.6643 0.0370 Uiso 1.00 calc . . . H(26) H 0.5785 -0.2776 0.6428 0.0281 Uiso 1.00 calc . . . 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 Mn(1) 0.0144(5) 0.0201(6) 0.0219(6) 0.0001(5) 0.0043(4) 0.0011(5) Cl(1) 0.036(1) 0.032(1) 0.0228(10) -0.0037(9) 0.0076(8) 0.0030(8) O(1) 0.014(3) 0.023(3) 0.034(3) -0.001(2) 0.002(2) -0.004(2) O(2) 0.022(3) 0.022(3) 0.031(3) -0.002(2) 0.006(2) 0.003(2) N(1) 0.017(3) 0.024(3) 0.013(3) 0.000(2) 0.001(2) 0.001(2) N(2) 0.017(3) 0.014(3) 0.020(3) -0.002(2) 0.004(2) 0.006(2) C(1) 0.021(4) 0.026(4) 0.023(4) 0.002(3) 0.000(3) -0.003(3) C(2) 0.020(4) 0.035(5) 0.040(5) -0.006(4) 0.009(3) -0.006(4) C(3) 0.023(4) 0.036(5) 0.032(4) -0.002(3) 0.014(3) 0.001(3) C(4) 0.017(4) 0.036(5) 0.023(4) 0.008(3) 0.003(3) 0.001(3) C(5) 0.012(4) 0.047(6) 0.042(5) 0.004(3) 0.004(3) -0.002(4) C(6) 0.024(4) 0.044(6) 0.043(5) 0.014(4) 0.006(4) -0.006(4) C(7) 0.037(5) 0.037(5) 0.042(5) 0.008(4) 0.010(4) 0.005(4) C(8) 0.032(5) 0.021(4) 0.037(4) -0.003(3) 0.003(3) 0.006(3) C(9) 0.010(4) 0.035(5) 0.028(4) 0.001(3) 0.003(3) -0.001(3) C(10) 0.015(4) 0.021(4) 0.020(4) -0.004(3) 0.003(3) -0.002(3) C(11) 0.020(4) 0.026(4) 0.013(3) 0.002(3) 0.005(3) 0.004(3) C(12) 0.018(4) 0.014(4) 0.025(4) -0.006(3) 0.003(3) -0.001(3) C(13) 0.026(4) 0.030(5) 0.029(4) -0.004(3) 0.008(3) -0.004(3) C(14) 0.015(4) 0.034(5) 0.023(4) -0.005(3) 0.007(3) 0.002(3) C(15) 0.018(4) 0.014(4) 0.016(3) 0.000(2) 0.000(3) 0.006(2) C(16) 0.021(4) 0.023(4) 0.020(4) 0.005(3) 0.004(3) 0.000(3) C(17) 0.018(4) 0.017(4) 0.040(5) -0.002(3) 0.007(3) 0.003(3) C(18) 0.018(4) 0.031(4) 0.020(4) 0.001(3) 0.003(3) 0.009(3) C(19) 0.023(4) 0.012(4) 0.028(4) 0.003(3) 0.002(3) 0.000(3) C(20) 0.028(4) 0.026(5) 0.022(4) 0.007(3) 0.006(3) -0.005(3) C(21) 0.022(4) 0.031(5) 0.048(5) 0.005(3) 0.006(4) 0.006(4) C(22) 0.021(5) 0.046(6) 0.054(6) 0.005(4) 0.005(4) 0.011(4) C(23) 0.027(5) 0.051(6) 0.050(6) 0.025(4) -0.004(4) 0.009(4) C(24) 0.048(6) 0.037(5) 0.030(5) 0.017(4) 0.000(4) 0.000(3) C(25) 0.025(5) 0.035(5) 0.020(4) 0.010(3) 0.001(3) 0.002(3) C(26) 0.041(5) 0.021(4) 0.026(4) 0.001(3) 0.002(3) 0.005(3) C(27) 0.027(4) 0.026(4) 0.020(4) -0.001(3) 0.005(3) 0.001(3) C(28) 0.026(4) 0.024(4) 0.017(4) 0.002(3) 0.003(3) 0.005(3) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Mn(1) Cl(1) 2.383(2) . . yes Mn(1) O(1) 1.877(5) . . yes Mn(1) O(2) 1.894(5) . . yes Mn(1) N(1) 1.968(6) . . yes Mn(1) N(2) 1.968(6) . . yes O(1) C(1) 1.329(8) . . yes O(2) C(28) 1.322(9) . . yes N(1) C(11) 1.314(9) . . yes N(1) C(12) 1.508(8) . . yes N(2) C(15) 1.503(8) . . yes N(2) C(18) 1.312(9) . . yes C(1) C(2) 1.42(1) . . yes C(1) C(10) 1.403(10) . . yes C(2) C(3) 1.33(1) . . yes C(3) C(4) 1.44(1) . . yes C(4) C(5) 1.40(1) . . yes C(4) C(9) 1.42(1) . . yes C(5) C(6) 1.35(1) . . yes C(6) C(7) 1.40(1) . . yes C(7) C(8) 1.35(1) . . yes C(8) C(9) 1.42(1) . . yes C(9) C(10) 1.468(10) . . yes C(10) C(11) 1.430(9) . . yes C(12) C(13) 1.533(10) . . yes C(12) C(14) 1.538(10) . . yes C(12) C(15) 1.566(9) . . yes C(15) C(16) 1.531(9) . . yes C(15) C(17) 1.506(9) . . yes C(18) C(19) 1.44(1) . . yes C(19) C(20) 1.454(10) . . yes C(19) C(28) 1.39(1) . . yes C(20) C(21) 1.40(1) . . yes C(20) C(25) 1.43(1) . . yes C(21) C(22) 1.39(1) . . yes C(22) C(23) 1.39(1) . . yes C(23) C(24) 1.34(1) . . yes C(24) C(25) 1.42(1) . . yes C(25) C(26) 1.43(1) . . yes C(26) C(27) 1.35(1) . . yes C(27) C(28) 1.44(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Mn(1) O(1) 97.8(2) . . . yes Cl(1) Mn(1) O(2) 96.7(2) . . . yes Cl(1) Mn(1) N(1) 98.5(2) . . . yes Cl(1) Mn(1) N(2) 101.5(2) . . . yes O(1) Mn(1) O(2) 90.2(2) . . . yes O(1) Mn(1) N(1) 92.1(2) . . . yes O(1) Mn(1) N(2) 160.4(2) . . . yes O(2) Mn(1) N(1) 164.2(2) . . . yes O(2) Mn(1) N(2) 90.9(2) . . . yes N(1) Mn(1) N(2) 81.8(2) . . . yes Mn(1) O(1) C(1) 129.1(5) . . . yes Mn(1) O(2) C(28) 126.2(5) . . . yes Mn(1) N(1) C(11) 124.6(5) . . . yes Mn(1) N(1) C(12) 115.2(4) . . . yes C(11) N(1) C(12) 119.9(6) . . . yes Mn(1) N(2) C(15) 115.8(4) . . . yes Mn(1) N(2) C(18) 123.8(5) . . . yes C(15) N(2) C(18) 119.8(6) . . . yes O(1) C(1) C(2) 116.6(7) . . . yes O(1) C(1) C(10) 123.3(7) . . . yes C(2) C(1) C(10) 120.1(7) . . . yes C(1) C(2) C(3) 121.7(8) . . . yes C(2) C(3) C(4) 121.9(8) . . . yes C(3) C(4) C(5) 121.7(8) . . . yes C(3) C(4) C(9) 118.2(7) . . . yes C(5) C(4) C(9) 120.1(7) . . . yes C(4) C(5) C(6) 121.7(8) . . . yes C(5) C(6) C(7) 118.9(8) . . . yes C(6) C(7) C(8) 121.5(9) . . . yes C(7) C(8) C(9) 121.2(8) . . . yes C(4) C(9) C(8) 116.6(7) . . . yes C(4) C(9) C(10) 119.5(7) . . . yes C(8) C(9) C(10) 123.9(7) . . . yes C(1) C(10) C(9) 118.7(7) . . . yes C(1) C(10) C(11) 122.7(7) . . . yes C(9) C(10) C(11) 118.6(6) . . . yes N(1) C(11) C(10) 126.2(7) . . . yes N(1) C(12) C(13) 107.0(5) . . . yes N(1) C(12) C(14) 111.6(6) . . . yes N(1) C(12) C(15) 105.3(5) . . . yes C(13) C(12) C(14) 110.2(6) . . . yes C(13) C(12) C(15) 111.8(6) . . . yes C(14) C(12) C(15) 110.7(5) . . . yes N(2) C(15) C(12) 105.1(5) . . . yes N(2) C(15) C(16) 106.3(5) . . . yes N(2) C(15) C(17) 112.7(5) . . . yes C(12) C(15) C(16) 111.4(5) . . . yes C(12) C(15) C(17) 111.6(6) . . . yes C(16) C(15) C(17) 109.7(6) . . . yes N(2) C(18) C(19) 126.6(7) . . . yes C(18) C(19) C(20) 118.2(7) . . . yes C(18) C(19) C(28) 120.2(7) . . . yes C(20) C(19) C(28) 121.1(7) . . . yes C(19) C(20) C(21) 124.7(8) . . . yes C(19) C(20) C(25) 118.0(7) . . . yes C(21) C(20) C(25) 117.3(8) . . . yes C(20) C(21) C(22) 121.7(8) . . . yes C(21) C(22) C(23) 119.7(9) . . . yes C(22) C(23) C(24) 120.5(8) . . . yes C(23) C(24) C(25) 121.5(9) . . . yes C(20) C(25) C(24) 119.1(8) . . . yes C(20) C(25) C(26) 118.1(7) . . . yes C(24) C(25) C(26) 122.8(8) . . . yes C(25) C(26) C(27) 124.0(8) . . . yes C(26) C(27) C(28) 118.9(8) . . . yes O(2) C(28) C(19) 124.7(7) . . . yes O(2) C(28) C(27) 115.4(7) . . . yes C(19) C(28) C(27) 119.8(7) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Mn(1) O(2) 3.507(5) . 3_656 ? Cl(1) C(8) 3.503(8) . 2_646 ? O(1) O(2) 3.281(7) . 3_656 ? O(1) C(16) 3.414(9) . 3_656 ? O(1) C(28) 3.494(9) . 3_656 ? O(1) C(18) 3.583(9) . 3_656 ? O(2) C(16) 3.394(9) . 3_656 ? C(1) C(19) 3.458(10) . 3_656 ? C(1) C(28) 3.475(10) . 3_656 ? C(2) C(18) 3.47(1) . 3_656 ? C(2) C(19) 3.520(10) . 3_656 ? C(3) C(24) 3.55(1) . 2_656 ? C(4) C(25) 3.49(1) . 2_656 ? C(6) C(6) 3.47(2) . 3_566 ? C(10) C(27) 3.599(10) . 3_656 ? C(11) C(27) 3.570(10) . 3_656 ? C(13) C(16) 3.52(1) . 4_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END