# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 207/318 #============================================================================== data_2e #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Karl Anker Jorgensen ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structure of a chiral nitrido-manganese salen complex. The nitrogen analogue to the intermediate in the Jacobsen epoxidation reaction. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name ' Aase Sejr Jepsen' ' Mark Roberson ' ' Rita G. Hazell' ' Karl Anker Jorgensen' _publ_author_address ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; #============================================================================== # 4. TEXT _publ_section_references ; Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Burla,M.C., Polidori,G. & Camalli,M. (1994). J.Appl. Cryst. 27, 435. Burnett,M.N. & Johnson,C.K. (1996). ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Busing,W.T., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. ; #============================================================================== #============================================================================== #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; insert name here ; _chemical_formula_sum C38H42N3O2Mn _chemical_formula_weight 627.72 #================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' _cell_length_a 10.2919(8) _cell_length_b 12.0062(9) _cell_length_c 14.139(1) _cell_angle_alpha 88.543(1) _cell_angle_beta 76.608(1) _cell_angle_gamma 77.637(1) _cell_volume 1659.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 4475 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.97 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 6542 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 24 _diffrn_reflns_reduction_process 6542 _reflns_number_total 5284 _reflns_number_observed 4697 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996),KRYSTAL(Hazell,1995) ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; Pseudo center of symmetry except for the 2 asymmetric centers, therefore constrained rigid body refinement, TLS model, smae TL, opposite S for the 2 molecules, both relative to their Mn centres. Hydrogen atom positions recalculated each cycle, methyl groups with refined torsion angle. Ordered model refined to R=0.064, but difference map indicated disorder such that Mn and nitride was partly to be found on the opposite side of the plane of the salen group. Disorder was introduced for both molecules and occupation parameters were refined, showing that only molecule 2 was disordered. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic (1974)B-C ; _refine_ls_extinction_coef 0(15) _refine_ls_abs_structure_details ; Reversed structure gave significantly worse R ; _refine_ls_number_reflns 4697 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_number_constraints 487 _refine_ls_R_factor_obs 0.052 _refine_ls_wR_factor_obs 0.057 _refine_ls_goodness_of_fit_obs 2.79 _refine_ls_shift/esd_max 0.070 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 0.52(8) _refine_diff_density_min -0.60(8) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Mn 0.9008 0.7198 0.5014 0.0180(4) Uij 1.000 O(1) 1.0549(6) 0.7280(4) 0.3981(4) 0.0189(3) Uij 1.000 O(2) 0.8419(6) 0.6456(4) 0.4049(4) 0.0195(3) Uij 1.000 N(1) 1.0105(6) 0.7278(4) 0.5954(5) 0.0179(3) Uij 1.000 N(2) 0.8159(6) 0.6242(4) 0.6011(4) 0.0184(3) Uij 1.000 N 0.8000(6) 0.8365(5) 0.5179(4) 0.0189(3) Uij 1.000 C(1) 1.1560(9) 0.7770(6) 0.4024(6) 0.0194(3) Uij 1.000 C(2) 1.2366(9) 0.8076(6) 0.3130(6) 0.0221(3) Uij 1.000 C(3) 1.3449(9) 0.8618(6) 0.3216(7) 0.0236(4) Uij 1.000 C(4) 1.3770(9) 0.8847(6) 0.4052(7) 0.0230(5) Uij 1.000 C(5) 1.3030(9) 0.8515(6) 0.4913(6) 0.0210(4) Uij 1.000 C(6) 1.1941(9) 0.7970(6) 0.4891(6) 0.0191(3) Uij 1.000 C(7) 1.1213(8) 0.7648(6) 0.5823(6) 0.0186(3) Uij 1.000 C(8) 0.9398(7) 0.7078(5) 0.6972(5) 0.0193(3) Uij 1.000 C(9) 0.8711(7) 0.6060(5) 0.6895(5) 0.0194(3) Uij 1.000 C(10) 0.7116(7) 0.5837(5) 0.5937(5) 0.0195(3) Uij 1.000 C(11) 0.6563(8) 0.5864(6) 0.5116(6) 0.0204(3) Uij 1.000 C(12) 0.5284(8) 0.5498(6) 0.5266(7) 0.0228(4) Uij 1.000 C(13) 0.4720(9) 0.5396(7) 0.4488(7) 0.0253(4) Uij 1.000 C(14) 0.5413(9) 0.5631(7) 0.3563(7) 0.0259(4) Uij 1.000 C(15) 0.6706(9) 0.5931(7) 0.3381(7) 0.0237(3) Uij 1.000 C(16) 0.7251(9) 0.6112(7) 0.4173(7) 0.0207(3) Uij 1.000 C(17) 1.2077(9) 0.7859(7) 0.2146(7) 0.0249(4) Uij 1.000 C(18) 1.2190(9) 0.6594(6) 0.1995(6) 0.0264(16) Uij 1.000 C(19) 1.0610(9) 0.8518(7) 0.2134(6) 0.0265(11) Uij 1.000 C(20) 1.3043(9) 0.8283(7) 0.1307(7) 0.0307(14) Uij 1.000 C(21) 1.4909(9) 0.9458(6) 0.4056(6) 0.0263(6) Uij 1.000 C(22) 1.0239(8) 0.6913(6) 0.7733(6) 0.0217(3) Uij 1.000 C(23) 1.0000(8) 0.7732(6) 0.8439(5) 0.0269(10) Uij 1.000 C(24) 1.0742(9) 0.7604(7) 0.9149(6) 0.0310(11) Uij 1.000 C(25) 1.1752(9) 0.6633(7) 0.9148(7) 0.0297(7) Uij 1.000 C(26) 1.2003(8) 0.5794(6) 0.8430(5) 0.0292(10) Uij 1.000 C(27) 1.1241(8) 0.5943(6) 0.7737(6) 0.0253(10) Uij 1.000 C(28) 0.7655(9) 0.5939(7) 0.7812(7) 0.0221(3) Uij 1.000 C(29) 0.6541(7) 0.6821(6) 0.8156(5) 0.0262(7) Uij 1.000 C(30) 0.5552(8) 0.6686(6) 0.8971(5) 0.0302(7) Uij 1.000 C(31) 0.5631(8) 0.5664(7) 0.9449(6) 0.0306(6) Uij 1.000 C(32) 0.6715(8) 0.4784(6) 0.9124(6) 0.0319(8) Uij 1.000 C(33) 0.7743(8) 0.4906(6) 0.8282(5) 0.0278(8) Uij 1.000 C(34) 0.3398(9) 0.5014(7) 0.4615(7) 0.0290(6) Uij 1.000 C(35) 0.7428(9) 0.6181(6) 0.2327(6) 0.0265(4) Uij 1.000 C(36) 0.7491(10) 0.7468(7) 0.2232(6) 0.0364(16) Uij 1.000 C(37) 0.8874(9) 0.5451(7) 0.2078(6) 0.0364(11) Uij 1.000 C(38) 0.6698(10) 0.5900(7) 0.1565(7) 0.0415(18) Uij 1.000 Mn' 0.9553(1) 1.1073(1) 0.7037(1) 0.0180(4) Uij 0.880(2) O(2') 0.7999(6) 1.1062(4) 0.8077(4) 0.0189(3) Uij 1.000 O(1') 1.0230(6) 1.1778(4) 0.7950(4) 0.0195(3) Uij 1.000 N(2') 0.8340(7) 1.1292(4) 0.6121(5) 0.0179(3) Uij 1.000 N(1') 1.0674(6) 1.1742(4) 0.5966(4) 0.0184(3) Uij 1.000 N' 1.0270(7) 0.9810(5) 0.6900(5) 0.0189(3) Uij 0.880(2) C(16') 0.6939(9) 1.0582(6) 0.8056(6) 0.0195(3) Uij 1.000 C(15') 0.6085(9) 1.0295(7) 0.8937(6) 0.0221(3) Uij 1.000 C(14') 0.5030(9) 0.9803(7) 0.8877(7) 0.0236(4) Uij 1.000 C(13') 0.4684(9) 0.9617(6) 0.7955(6) 0.0229(4) Uij 1.000 C(12') 0.5476(9) 0.9934(6) 0.7155(6) 0.0208(4) Uij 1.000 C(11') 0.6629(9) 1.0418(6) 0.7136(6) 0.0190(3) Uij 1.000 C(10') 0.7240(8) 1.0862(6) 0.6277(6) 0.0185(3) Uij 1.000 C(9') 0.8771(7) 1.1920(5) 0.5238(5) 0.0192(3) Uij 1.000 C(8') 1.0332(7) 1.1637(6) 0.5017(5) 0.0195(3) Uij 1.000 C(7') 1.1768(7) 1.2121(5) 0.6009(5) 0.0196(3) Uij 1.000 C(6') 1.2193(8) 1.2306(6) 0.6871(6) 0.0205(3) Uij 1.000 C(5') 1.3425(8) 1.2686(6) 0.6772(6) 0.0229(4) Uij 1.000 C(4') 1.3868(9) 1.2914(7) 0.7547(7) 0.0253(5) Uij 1.000 C(3') 1.3045(9) 1.2769(7) 0.8471(7) 0.0258(4) Uij 1.000 C(2') 1.1862(9) 1.2394(7) 0.8664(7) 0.0238(3) Uij 1.000 C(1') 1.1389(9) 1.2147(7) 0.7808(6) 0.0206(3) Uij 1.000 C(35') 0.6359(9) 1.0560(7) 0.9919(6) 0.0249(4) Uij 1.000 C(36') 0.6175(9) 1.1874(6) 1.0034(6) 0.0254(4) Uij 1.000 C(37') 0.7760(9) 0.9970(6) 1.0029(6) 0.0256(4) Uij 1.000 C(38') 0.5323(9) 1.0184(7) 1.0780(7) 0.0298(6) Uij 1.000 C(34') 0.3466(8) 0.9100(6) 0.7935(7) 0.0260(6) Uij 1.000 C(28') 0.8156(8) 1.1778(6) 0.4407(5) 0.0216(3) Uij 1.000 C(29') 0.8408(8) 1.0739(6) 0.3886(5) 0.0232(4) Uij 1.000 C(30') 0.7835(9) 1.0648(7) 0.3131(6) 0.0272(6) Uij 1.000 C(31') 0.6979(9) 1.1576(7) 0.2843(7) 0.0297(7) Uij 1.000 C(32') 0.6677(8) 1.2613(6) 0.3322(6) 0.0279(6) Uij 1.000 C(33') 0.7287(8) 1.2707(6) 0.4111(6) 0.0238(4) Uij 1.000 C(22') 1.1010(9) 1.2308(7) 0.4206(7) 0.0222(3) Uij 1.000 C(23') 1.2038(8) 1.1774(6) 0.3456(5) 0.0251(4) Uij 1.000 C(24') 1.2680(8) 1.2426(6) 0.2730(6) 0.0292(6) Uij 1.000 C(25') 1.2258(8) 1.3589(6) 0.2735(6) 0.0305(6) Uij 1.000 C(26') 1.1199(7) 1.4138(6) 0.3484(5) 0.0277(5) Uij 1.000 C(27') 1.0574(7) 1.3503(6) 0.4217(5) 0.0235(4) Uij 1.000 C(21') 1.5197(9) 1.3351(7) 0.7447(7) 0.0293(6) Uij 1.000 C(17') 1.1024(9) 1.2326(6) 0.9674(6) 0.0263(4) Uij 1.000 C(18') 1.0972(9) 1.1091(6) 0.9902(6) 0.0266(4) Uij 1.000 C(19') 0.9562(9) 1.3057(6) 0.9827(6) 0.0261(4) Uij 1.000 C(20') 1.1693(9) 1.2719(6) 1.0459(6) 0.0318(6) Uij 1.000 Mn" 0.9077(9) 1.1865(9) 0.7022(6) 0.0191 Uiso 0.120(2) N" 0.8452(43) 1.2987(34) 0.7115(32) 0.0196 Uiso 0.120(2) H(3) 1.399 0.884 0.263 0.028 Uiso 1. H(5) 1.324 0.865 0.551 0.026 Uiso 1. H(7) 1.158 0.771 0.637 0.023 Uiso 1. H(8) 0.868 0.773 0.717 0.024 Uiso 1. H(9) 0.940 0.538 0.680 0.024 Uiso 1. H(10) 0.668 0.548 0.650 0.024 Uiso 1. H(12) 0.483 0.533 0.590 0.028 Uiso 1. H(14) 0.500 0.559 0.303 0.033 Uiso 1. H(23) 0.931 0.840 0.844 0.033 Uiso 1. H(24) 1.056 0.818 0.964 0.039 Uiso 1. H(25) 1.227 0.654 0.963 0.038 Uiso 1. H(26) 1.269 0.512 0.842 0.037 Uiso 1. H(27) 1.141 0.537 0.725 0.032 Uiso 1. H(29) 0.646 0.752 0.783 0.031 Uiso 1. H(30) 0.481 0.730 0.921 0.035 Uiso 1. H(31) 0.493 0.558 1.000 0.037 Uiso 1. H(32) 0.679 0.409 0.946 0.039 Uiso 1. H(33) 0.848 0.428 0.804 0.034 Uiso 1. H(18a) 1.205(2) 0.647(1) 0.137(1) 0.032 Uiso 1. H(18b) 1.152(2) 0.635(1) 0.248(1) 0.032 Uiso 1. H(18c) 1.308(1) 0.620(1) 0.204(2) 0.032 Uiso 1. H(19a) 1.039(1) 0.832(1) 0.155(1) 0.032 Uiso 1. H(19b) 1.058(1) 0.931(1) 0.216(1) 0.032 Uiso 1. H(19c) 0.999(1) 0.831(1) 0.268(1) 0.032 Uiso 1. H(20a) 1.395(1) 0.790(1) 0.130(1) 0.037 Uiso 1. H(20b) 1.295(2) 0.908(1) 0.139(1) 0.037 Uiso 1. H(20c) 1.282(1) 0.813(2) 0.072(1) 0.037 Uiso 1. H(21a) 1.575(1) 0.892(1) 0.394(1) 0.032 Uiso 1. H(21b) 1.475(1) 0.983(1) 0.467(1) 0.032 Uiso 1. H(21c) 1.493(1) 1.001(1) 0.356(1) 0.032 Uiso 1. H(34a) 0.288(1) 0.518(2) 0.526(1) 0.037 Uiso 1. H(34b) 0.359(1) 0.422(1) 0.449(1) 0.037 Uiso 1. H(34c) 0.290(1) 0.541(1) 0.417(1) 0.037 Uiso 1. H(36a) 0.797(2) 0.759(1) 0.159(1) 0.044 Uiso 1. H(36b) 0.795(2) 0.766(1) 0.269(1) 0.044 Uiso 1. H(36c) 0.659(1) 0.792(1) 0.235(2) 0.044 Uiso 1. H(37a) 0.927(1) 0.553(2) 0.141(1) 0.042 Uiso 1. H(37b) 0.883(1) 0.468(1) 0.221(2) 0.042 Uiso 1. H(37c) 0.940(1) 0.571(1) 0.246(1) 0.042 Uiso 1. H(38a) 0.728(1) 0.592(2) 0.094(1) 0.054 Uiso 1. H(38b) 0.587(1) 0.645(1) 0.162(1) 0.054 Uiso 1. H(38c) 0.651(2) 0.516(1) 0.168(1) 0.054 Uiso 1. H(14') 0.450 0.957 0.946 0.028 Uiso 1. H(12') 0.526 0.983 0.655 0.025 Uiso 1. H(10') 0.682 1.086 0.575 0.023 Uiso 1. H(9') 0.849 1.271 0.542 0.024 Uiso 1. H(8') 1.062 1.086 0.482 0.024 Uiso 1. H(7') 1.233 1.229 0.541 0.024 Uiso 1. H(5') 1.395 1.278 0.614 0.029 Uiso 1. H(3') 1.336 1.296 0.902 0.033 Uiso 1. H(29') 0.899 1.009 0.407 0.029 Uiso 1. H(30') 0.802 0.994 0.279 0.034 Uiso 1. H(31') 0.659 1.150 0.231 0.038 Uiso 1. H(32') 0.608 1.325 0.313 0.036 Uiso 1. H(33') 0.710 1.342 0.444 0.030 Uiso 1. H(23') 1.232 1.097 0.343 0.030 Uiso 1. H(24') 1.342 1.206 0.223 0.036 Uiso 1. H(25') 1.269 1.402 0.223 0.038 Uiso 1. H(26') 1.091 1.494 0.349 0.035 Uiso 1. H(27')) 0.985 1.388 0.473 0.029 Uiso 1. H(36a') 0.638(2) 1.204(1) 1.063(1) 0.030 Uiso 1. H(36b') 0.525(1) 1.223(1) 1.004(2) 0.030 Uiso 1. H(36c') 0.678(2) 1.214(1) 0.950(1) 0.030 Uiso 1. H(37a') 0.787(1) 1.018(1) 1.064(1) 0.031 Uiso 1. H(37b') 0.843(1) 1.020(1) 0.952(1) 0.031 Uiso 1. H(37c') 0.784(1) 0.917(1) 0.999(1) 0.031 Uiso 1. H(38a') 0.553(1) 1.036(2) 1.137(1) 0.036 Uiso 1. H(38b') 0.539(2) 0.939(1) 1.072(1) 0.036 Uiso 1. H(38c') 0.443(1) 1.058(1) 1.076(1) 0.036 Uiso 1. H(18a') 1.036(2) 1.106(1) 1.051(1) 0.033 Uiso 1. H(18b') 1.186(1) 1.068(1) 0.992(2) 0.033 Uiso 1. H(18c') 1.067(2) 1.077(1) 0.941(1) 0.033 Uiso 1. H(19a') 0.906(1) 1.295(1) 1.047(1) 0.032 Uiso 1. H(19b') 0.913(1) 1.283(1) 0.936(1) 0.032 Uiso 1. H(19c') 0.961(1) 1.384(1) 0.975(1) 0.032 Uiso 1. H(20a') 1.122(1) 1.254(2) 1.108(1) 0.040 Uiso 1. H(20b') 1.164(2) 1.352(1) 1.042(1) 0.040 Uiso 1. H(20c') 1.262(1) 1.233(1) 1.034(1) 0.040 Uiso 1. H(34a') 0.379(1) 0.837(1) 0.762(1) 0.032 Uiso 1. H(34b') 0.289(1) 0.958(1) 0.759(1) 0.032 Uiso 1. H(34c') 0.298(1) 0.903(2) 0.858(1) 0.032 Uiso 1. H(21a') 1.582(1) 1.282(1) 0.773(1) 0.037 Uiso 1. H(21b') 1.499(1) 1.407(1) 0.778(1) 0.037 Uiso 1. H(21c') 1.559(1) 1.343(2) 0.678(1) 0.037 Uiso 1. 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 0.0191(4) 0.0197(4) 0.0172(4) -0.0060(3) -0.0066(3) 0.0004(3) O(1) 0.0200(2) 0.0172(3) 0.0200(2) -0.0035(2) -0.0058(2) -0.0015(2) O(2) 0.0207(2) 0.0183(3) 0.0211(2) -0.0038(2) -0.0080(2) -0.0011(2) N(1) 0.0199(2) 0.0147(3) 0.0201(2) -0.0034(2) -0.0065(2) -0.0017(2) N(2) 0.0199(2) 0.0153(3) 0.0211(2) -0.0038(2) -0.0071(2) -0.0001(2) N(3) 0.0195(2) 0.0152(3) 0.0221(3) -0.0026(2) -0.0059(2) 0.0001(2) C(1) 0.0200(2) 0.0174(3) 0.0212(2) -0.0039(2) -0.0051(2) -0.0015(2) C(2) 0.0218(3) 0.0220(4) 0.0224(3) -0.0054(3) -0.0041(2) -0.0006(2) C(3) 0.0221(3) 0.0228(5) 0.0258(3) -0.0065(3) -0.0036(3) -0.0003(3) C(4) 0.0214(4) 0.0202(5) 0.0280(4) -0.0063(3) -0.0047(3) -0.0014(3) C(5) 0.0207(3) 0.0174(4) 0.0258(3) -0.0051(3) -0.0059(2) -0.0025(2) C(6) 0.0198(3) 0.0158(3) 0.0224(3) -0.0039(2) -0.0057(2) -0.0022(2) C(7) 0.0202(3) 0.0152(3) 0.0213(2) -0.0037(2) -0.0066(2) -0.0024(2) C(8) 0.0219(3) 0.0172(3) 0.0199(2) -0.0045(2) -0.0068(2) -0.0012(2) C(9) 0.0218(3) 0.0170(3) 0.0211(2) -0.0048(2) -0.0076(2) 0.0007(2) C(10) 0.0202(3) 0.0165(3) 0.0233(2) -0.0045(2) -0.0077(2) 0.0007(2) C(11) 0.0204(3) 0.0179(3) 0.0249(3) -0.0046(2) -0.0089(2) 0.0003(2) C(12) 0.0212(3) 0.0206(4) 0.0293(3) -0.0060(3) -0.0101(2) 0.0013(3) C(13) 0.0230(3) 0.0245(5) 0.0325(4) -0.0072(3) -0.0127(3) 0.0010(4) C(14) 0.0249(3) 0.0271(5) 0.0303(4) -0.0074(3) -0.0138(3) 0.0000(4) C(15) 0.0241(3) 0.0249(4) 0.0257(3) -0.0062(2) -0.0117(2) -0.0007(3) C(16) 0.0212(2) 0.0195(3) 0.0235(2) -0.0045(2) -0.0094(2) -0.0006(2) C(17) 0.0250(4) 0.0286(5) 0.0212(2) -0.0071(3) -0.0040(2) 0.0000(3) C(18) 0.0281(24) 0.0296(5) 0.0216(5) -0.0065(4) -0.0052(11) -0.0042(3) C(19) 0.0269(5) 0.0309(16) 0.0222(4) -0.0065(9) -0.0068(4) 0.0027(9) C(20) 0.0300(11) 0.0393(19) 0.0231(3) -0.0119(14) -0.0027(3) 0.0021(4) C(21) 0.0229(5) 0.0228(7) 0.0341(6) -0.0085(5) -0.0050(4) -0.0012(5) C(22) 0.0253(3) 0.0214(4) 0.0208(2) -0.0064(2) -0.0087(2) -0.0008(2) C(23) 0.0322(11) 0.0277(6) 0.0233(9) -0.0059(8) -0.0110(9) -0.0050(7) C(24) 0.0375(12) 0.0350(8) 0.0247(9) -0.0088(9) -0.0139(10) -0.0047(7) C(25) 0.0352(6) 0.0350(8) 0.0249(3) -0.0116(5) -0.0153(4) 0.0013(4) C(26) 0.0341(11) 0.0299(7) 0.0289(9) -0.0069(8) -0.0182(10) 0.0015(7) C(27) 0.0296(11) 0.0237(6) 0.0262(9) -0.0045(8) -0.0147(10) -0.0003(7) C(28) 0.0246(3) 0.0216(3) 0.0218(2) -0.0069(2) -0.0071(2) 0.0023(2) C(29) 0.0270(7) 0.0253(5) 0.0241(7) -0.0053(5) -0.0020(7) 0.0022(5) C(30) 0.0301(6) 0.0325(7) 0.0256(7) -0.0077(6) -0.0006(6) 0.0033(6) C(31) 0.0321(5) 0.0358(8) 0.0250(3) -0.0124(5) -0.0045(3) 0.0062(4) C(32) 0.0350(9) 0.0326(6) 0.0289(7) -0.0112(6) -0.0059(8) 0.0099(5) C(33) 0.0307(8) 0.0255(4) 0.0276(7) -0.0078(5) -0.0068(8) 0.0074(4) C(34) 0.0244(4) 0.0286(7) 0.0394(6) -0.0094(5) -0.0149(4) 0.0020(6) C(35) 0.0278(4) 0.0314(5) 0.0242(3) -0.0077(3) -0.0123(3) -0.0011(3) C(36) 0.0508(25) 0.0329(5) 0.0255(4) -0.0127(6) -0.0054(8) 0.0017(4) C(37) 0.0316(5) 0.0467(16) 0.0270(5) -0.0002(9) -0.0066(4) 0.0023(9) C(38) 0.0423(10) 0.0660(26) 0.0276(3) -0.0258(16) -0.0176(4) 0.0012(5) Mn' 0.0191(4) 0.0197(4) 0.0172(4) -0.0060(3) -0.0066(3) 0.0004(3) O(2') 0.0199(2) 0.0172(3) 0.0200(2) -0.0035(2) -0.0058(2) -0.0015(2) O(1') 0.0206(2) 0.0181(3) 0.0212(2) -0.0038(2) -0.0080(2) -0.0009(2) N(2') 0.0199(2) 0.0147(3) 0.0202(2) -0.0034(2) -0.0068(2) -0.0016(2) N(1') 0.0198(2) 0.0156(3) 0.0210(2) -0.0037(2) -0.0067(2) -0.0001(2) N' 0.0196(2) 0.0150(3) 0.0221(3) -0.0026(2) -0.0058(2) -0.0001(2) C(16') 0.0200(2) 0.0175(3) 0.0212(2) -0.0039(2) -0.0051(2) -0.0016(2) C(15') 0.0217(3) 0.0221(4) 0.0224(3) -0.0054(3) -0.0040(2) -0.0009(2) C(14') 0.0220(3) 0.0230(5) 0.0256(3) -0.0064(3) -0.0035(3) -0.0006(3) C(13') 0.0211(3) 0.0201(5) 0.0278(4) -0.0061(3) -0.0048(3) -0.0017(3) C(12') 0.0205(3) 0.0174(4) 0.0255(3) -0.0049(3) -0.0059(2) -0.0025(2) C(11') 0.0197(3) 0.0157(3) 0.0222(3) -0.0038(2) -0.0058(2) -0.0022(2) C(10') 0.0201(3) 0.0152(3) 0.0213(2) -0.0036(2) -0.0068(2) -0.0023(2) C(9') 0.0218(3) 0.0167(3) 0.0207(2) -0.0045(2) -0.0079(2) -0.0002(2) C(8') 0.0217(3) 0.0176(3) 0.0203(2) -0.0047(2) -0.0064(2) 0.0000(2) C(7') 0.0200(3) 0.0169(3) 0.0232(2) -0.0044(2) -0.0072(2) 0.0008(2) C(6') 0.0203(3) 0.0181(3) 0.0251(3) -0.0046(2) -0.0088(2) 0.0006(2) C(5') 0.0211(3) 0.0209(4) 0.0295(3) -0.0060(3) -0.0101(2) 0.0015(3) C(4') 0.0230(3) 0.0245(5) 0.0327(4) -0.0073(3) -0.0128(3) 0.0010(4) C(3') 0.0249(3) 0.0268(5) 0.0302(4) -0.0074(3) -0.0137(3) -0.0003(3) C(2') 0.0241(3) 0.0249(4) 0.0258(3) -0.0062(2) -0.0117(2) -0.0008(3) C(1') 0.0211(2) 0.0193(3) 0.0236(2) -0.0045(2) -0.0093(2) -0.0004(2) C(35') 0.0248(3) 0.0287(5) 0.0212(2) -0.0070(3) -0.0038(2) -0.0005(3) C(36') 0.0249(3) 0.0294(5) 0.0214(2) -0.0059(3) -0.0037(2) -0.0051(3) C(37') 0.0267(4) 0.0298(5) 0.0212(3) -0.0076(4) -0.0061(3) 0.0029(3) C(38') 0.0287(5) 0.0373(9) 0.0230(3) -0.0100(5) -0.0021(3) 0.0009(3) C(34') 0.0224(4) 0.0229(7) 0.0337(6) -0.0081(5) -0.0051(4) -0.0017(5) C(28') 0.0251(3) 0.0210(4) 0.0213(2) -0.0063(2) -0.0094(2) 0.0001(2) C(29') 0.0271(4) 0.0242(4) 0.0206(2) -0.0076(3) -0.0080(2) -0.0024(3) C(30') 0.0323(6) 0.0312(6) 0.0218(2) -0.0103(4) -0.0102(3) -0.0027(4) C(31') 0.0353(6) 0.0353(8) 0.0243(3) -0.0118(5) -0.0148(4) 0.0011(4) C(32') 0.0323(5) 0.0308(7) 0.0265(4) -0.0101(4) -0.0159(4) 0.0045(4) C(33') 0.0273(4) 0.0236(4) 0.0247(3) -0.0074(3) -0.0127(3) 0.0031(3) C(22') 0.0246(3) 0.0218(3) 0.0218(2) -0.0070(2) -0.0069(2) 0.0023(2) C(23') 0.0269(4) 0.0273(5) 0.0218(2) -0.0085(3) -0.0047(2) 0.0017(3) C(24') 0.0310(5) 0.0341(7) 0.0238(2) -0.0118(4) -0.0049(3) 0.0050(4) C(25') 0.0331(6) 0.0342(7) 0.0273(3) -0.0135(5) -0.0083(4) 0.0097(4) C(26') 0.0307(6) 0.0273(5) 0.0290(4) -0.0112(4) -0.0110(4) 0.0094(4) C(27') 0.0263(4) 0.0219(3) 0.0254(3) -0.0080(3) -0.0098(3) 0.0053(3) C(21') 0.0246(4) 0.0288(7) 0.0400(6) -0.0096(5) -0.0151(4) 0.0019(6) C(17') 0.0276(4) 0.0308(5) 0.0243(3) -0.0076(3) -0.0121(2) -0.0019(3) C(18') 0.0278(4) 0.0324(5) 0.0233(3) -0.0077(3) -0.0121(3) 0.0022(3) C(19') 0.0277(4) 0.0296(5) 0.0238(3) -0.0070(3) -0.0099(2) -0.0060(3) C(20') 0.0333(5) 0.0402(8) 0.0276(3) -0.0107(4) -0.0157(3) -0.0030(4) Mn" 0.0191(4) 0.0197(4) 0.0172(4) -0.0060(3) -0.0066(3) 0.0004(3) N" 0.0196(2) 0.0150(3) 0.0221(3) -0.0026(2) -0.0058(2) -0.0001(2) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mn N 1.541(6) Mn O(1) 1.909(6) Mn O(2) 1.923(6) Mn N(1) 1.949(6) Mn N(2) 1.961(6) O(1) C(1) 1.314(9) O(2) C(16) 1.325(9) N(1) C(7) 1.283(9) N(1) C(8) 1.494(9) N(2) C(10) 1.296(8) N(2) C(9) 1.482(9) Mn' N' 1.533(7) Mn' O(1') 1.896(5) Mn' O(2') 1.907(6) Mn' N(1') 1.948(6) Mn' N(2') 1.974(7) Mn' Mn" 0.975(10) N(2') Mn" 1.842(10) N(1') Mn" 1.929(10) O(1') Mn" 1.949(10) O(2') Mn" 2.000(10) Mn" N" 1.357(42) O(2') C(16') 1.345(9) O(1') C(1') 1.330(9) N(2') C(10') 1.313(10) N(2') C(9') 1.470(8) N(1') C(7') 1.315(8) N(1') C(8') 1.479(9) C(16') C(15') 1.430(12) C(16') C(11') 1.436(12) O(1) C(1) 1.314(9) C(1) C(6) 1.410(12) C(1) C(2) 1.429(12) C(2) C(3) 1.435(11) C(2) C(17) 1.528(12) C(3) C(4) 1.348(12) C(4) C(5) 1.378(11) C(4) C(21) 1.512(11) C(5) C(6) 1.420(11) C(6) C(7) 1.446(11) N(1) C(7) 1.283(9) N(1) C(8) 1.494(9) C(8) C(22) 1.514(10) C(8) C(9) 1.556(8) N(2) C(9) 1.482(9) C(9) C(28) 1.512(11) N(2) C(10) 1.296(8) C(10) C(11) 1.403(11) C(11) C(16) 1.415(12) C(11) C(12) 1.444(11) C(12) C(13) 1.376(13) C(13) C(14) 1.391(12) C(13) C(34) 1.497(12) C(14) C(15) 1.418(12) C(15) C(16) 1.403(12) C(15) C(35) 1.556(12) O(2) C(16) 1.325(9) C(17) C(20) 1.515(12) C(17) C(18) 1.515(11) C(17) C(19) 1.550(12) C(22) C(23) 1.362(9) C(22) C(27) 1.381(10) C(23) C(24) 1.383(11) C(24) C(25) 1.385(11) C(25) C(26) 1.389(11) C(26) C(27) 1.376(11) C(28) C(33) 1.388(10) C(28) C(29) 1.386(10) C(29) C(30) 1.381(10) C(30) C(31) 1.381(10) C(31) C(32) 1.362(11) C(32) C(33) 1.426(10) C(35) C(38) 1.530(12) C(35) C(37) 1.523(12) C(35) C(36) 1.562(11) O(2') C(16') 1.345(9) O(1') C(1') 1.330(9) N(2') C(10') 1.313(10) N(2') C(9') 1.470(8) N(1') C(7') 1.315(8) N(1') C(8') 1.479(9) C(16') C(15') 1.430(12) C(16') C(11') 1.436(12) C(15') C(14') 1.361(11) C(15') C(35') 1.533(12) C(14') C(13') 1.464(12) C(13') C(12') 1.331(11) C(13') C(34') 1.519(11) C(12') C(11') 1.424(11) C(11') C(10') 1.382(11) C(9') C(28') 1.488(10) C(9') C(8') 1.528(9) C(8') C(22') 1.507(10) C(7') C(6') 1.424(11) C(6') C(1') 1.422(12) C(6') C(5') 1.413(10) C(5') C(4') 1.336(12) C(4') C(3') 1.412(13) C(4') C(21') 1.542(12) C(3') C(2') 1.355(12) C(2') C(1') 1.464(12) C(2') C(17') 1.497(12) C(35') C(37') 1.506(12) C(35') C(38') 1.549(12) C(35') C(36') 1.556(11) C(28') C(33') 1.394(10) C(28') C(29') 1.408(9) C(29') C(30') 1.351(10) C(30') C(31') 1.381(12) C(31') C(32') 1.373(11) C(32') C(33') 1.418(11) C(22') C(23') 1.371(11) C(22') C(27') 1.409(10) C(23') C(24') 1.404(9) C(24') C(25') 1.370(10) C(25') C(26') 1.393(10) C(26') C(27') 1.389(9) C(17') C(18') 1.518(10) C(17') C(19') 1.542(12) C(17') C(20') 1.564(12) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O(1) Mn N 110.0(3) O(2) Mn N 103.3(3) N(1) Mn N 101.9(3) N(2) Mn N 103.8(3) O(1) Mn O(2) 84.4(2) O(1) Mn N(1) 89.7(3) O(1) Mn N(2) 146.1(2) O(2) Mn N(1) 154.7(2) O(2) Mn N(2) 89.5(2) N(1) Mn N(2) 81.8(2) Mn O(1) C(1) 126.4(5) Mn O(2) C(16) 126.2(5) C(7) N(1) C(8) 118.0(6) Mn N(1) C(7) 127.8(6) Mn N(1) C(8) 113.2(4) C(9) N(2) C(10) 120.8(6) Mn N(2) C(10) 122.4(5) Mn N(2) C(9) 116.8(4) O(1') Mn' N' 109.6(3) O(2') Mn' N' 103.1(3) N(1') Mn' N' 101.2(3) N(2') Mn' N' 104.2(3) O(2') Mn' O(1') 85.7(2) O(1') Mn' N(1') 90.7(2) O(1') Mn' N(2') 146.2(2) O(2') Mn' N(1') 155.3(2) O(2') Mn' N(2') 89.0(3) N(2') Mn' N(1') 80.5(3) N(2') Mn" N(1') 84.4(4) O(1') Mn" N(2') 155.2(7) O(2') Mn" N(2') 90.0(4) O(1') Mn" N(1') 89.7(4) O(2') Mn" N(1') 146.8(7) O(2') Mn" O(1') 81.8(4) N(2') Mn" N" 104.1(19) N(1') Mn" N" 106.3(18) O(1') Mn" N" 100.7(19) O(2') Mn" N" 106.8(19) Mn' O(2') C(16') 126.5(5) Mn' O(1') C(1') 128.4(5) C(10') N(2') C(9') 122.2(7) Mn' N(2') C(10') 121.6(5) Mn' N(2') C(9') 116.1(4) C(8') N(1') C(7') 119.9(6) Mn' N(1') C(7') 125.4(5) Mn' N(1') C(8') 114.1(4) O(2') C(16') C(15') 120.7(8) O(2') C(16') C(11') 118.9(8) C(15') C(16') C(11') 120.2(8) C(15') C(16') C(11') 120.2(8) O(1) C(1) C(6) 124.4(8) O(1) C(1) C(2) 117.8(8) C(2) C(1) C(6) 117.8(8) C(1) C(2) C(3) 115.7(8) C(3) C(2) C(17) 122.1(8) C(1) C(2) C(17) 122.2(8) C(2) C(3) C(4) 126.0(8) C(3) C(4) C(5) 118.5(8) C(3) C(4) C(21) 121.4(8) C(5) C(4) C(2) 120.1(8) C(4) C(5) C(6) 119.0(8) C(1) C(6) C(5) 122.9(8) C(1) C(6) C(7) 121.4(8) C(5) C(6) C(7) 115.7(8) N(1) C(7) C(6) 124.0(8) N(1) C(8) C(22) 117.6(6) N(1) C(8) C(9) 105.4(5) C(9) C(8) C(22) 112.9(6) N(2) C(9) C(28) 114.1(6) N(2) C(9) C(8) 106.2(5) C(8) C(9) C(28) 112.1(6) N(2) C(10) C(11) 126.7(7) C(10) C(11) C(16) 123.6(7) C(10) C(11) C(12) 115.5(7) C(12) C(11) C(16) 120.5(8) C(11) C(12) C(13) 120.0(9) C(12) C(13) C(14) 118.9(9) C(12) C(13) C(34) 121.4(9) C(14) C(13) C(34) 119.6(8) C(13) C(14) C(15) 122.6(9) C(14) C(15) C(16) 118.9(8) C(16) C(15) C(35) 120.7(8) C(14) C(15) C(35) 120.0(8) O(2) C(16) C(15) 121.6(8) O(2) C(16) C(11) 119.7(8) C(11) C(16) C(15) 118.6(8) C(18) C(17) C(20) 109.1(7) C(2) C(17) C(20) 112.5(7) C(19) C(17) C(20) 107.0(7) C(2) C(17) C(18) 109.7(7) C(18) C(17) C(19) 109.7(7) C(2) C(17) C(19) 108.7(7) C(23) C(22) C(27) 118.7(7) C(8) C(22) C(23) 119.7(7) C(8) C(22) C(27) 121.6(6) C(22) C(23) C(24) 121.1(7) C(23) C(24) C(25) 120.0(7) C(24) C(25) C(26) 119.3(8) C(25) C(26) C(27) 119.3(7) C(22) C(27) C(26) 121.5(7) C(29) C(28) C(33) 119.0(7) C(9) C(28) C(33) 119.9(7) C(9) C(28) C(29) 121.0(7) C(28) C(29) C(30) 120.5(7) C(29) C(30) C(31) 121.0(7) C(30) C(31) C(32) 119.5(7) C(31) C(32) C(33) 120.3(7) C(28) C(33) C(32) 119.6(7) C(37) C(35) C(38) 107.3(7) C(15) C(35) C(38) 112.9(7) C(36) C(35) C(38) 107.3(7) C(15) C(35) C(37) 109.2(7) C(36) C(35) C(37) 109.4(7) C(15) C(35) C(36) 110.7(7) C(10') N(2') C(9') 122.2(7) C(8') N(1') C(7') 119.9(6) O(2') C(16') C(15') 120.7(8) O(2') C(16') C(11') 118.9(8) C(15') C(16') C(11') 120.2(8) C(16') C(15') C(14') 118.5(8) C(14') C(15') C(35') 121.7(8) C(16') C(15') C(35') 119.8(8) C(15') C(14') C(13') 122.9(8) C(14') C(13') C(12') 116.6(8) C(12') C(13') C(34') 122.8(8) C(14') C(13') C(34') 120.6(8) C(13') C(12') C(11') 124.9(9) C(12') C(11') C(10') 118.7(8) C(16') C(11') C(10') 123.6(7) C(16') C(11') C(12') 116.8(8) N(2') C(10') C(11') 126.7(8) N(2') C(9') C(28') 116.7(5) N(2') C(9') C(8') 105.1(5) C(8') C(9') C(28') 115.6(6) N(1') C(8') C(22') 115.7(6) N(1') C(8') C(9') 104.9(5) C(9') C(8') C(22') 114.6(6) N(1') C(7') C(6') 126.0(7) C(5') C(6') C(1') 120.6(8) C(7') C(6') C(1') 121.4(7) C(7') C(6') C(5') 118.0(7) C(6') C(5') C(4') 121.5(8) C(5') C(4') C(3') 117.1(8) C(5') C(4') C(21') 121.9(9) C(3') C(4') C(21') 121.0(8) C(4') C(3') C(2') 127.1(9) C(3') C(2') C(1') 115.2(9) C(3') C(2') C(17') 123.1(8) C(1') C(2') C(17') 121.6(8) O(1') C(1') C(6') 123.5(8) O(1') C(1') C(2') 118.1(8) C(6') C(1') C(2') 118.5(8) C(15') C(35') C(37') 113.0(7) C(37') C(35') C(38') 106.5(7) C(36') C(35') C(37') 109.9(7) C(15') C(35') C(38') 111.6(7) C(15') C(35') C(36') 108.7(7) C(36') C(35') C(38') 106.9(7) C(29') C(28') C(33') 117.1(7) C(9') C(28') C(33') 119.5(6) C(9') C(28') C(29') 123.3(7) C(28') C(29') C(30') 121.4(7) C(29') C(30') C(31') 120.9(7) C(30') C(31') C(32') 120.9(8) C(31') C(32') C(33') 118.1(7) C(28') C(33') C(32') 121.6(7) C(23') C(22') C(27') 119.4(7) C(8') C(22') C(23') 121.2(7) C(8') C(22') C(27') 119.4(7) C(22') C(23') C(24') 119.7(7) C(23') C(24') C(25') 121.1(7) C(24') C(25') C(26') 119.6(7) C(25') C(26') C(27') 119.8(7) C(22') C(27') C(26') 120.3(7) C(2') C(17') C(18') 109.7(6) C(2') C(17') C(19') 112.7(7) C(2') C(17') C(20') 111.9(7) C(18') C(17') C(19') 110.0(7) C(18') C(17') C(20') 104.8(6) C(19') C(17') C(20') 107.6(6) data_2f _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H52 Mn N3 O2' _chemical_formula_weight 613.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.9795(4) _cell_length_b 13.4234(6) _cell_length_c 14.6685(6) _cell_angle_alpha 63.1440(10) _cell_angle_beta 78.5960(10) _cell_angle_gamma 71.5410(10) _cell_volume 1659.37(12) _cell_formula_units_Z 2 _cell_measurement_temperature 122(2) _cell_measurement_reflns_used 16219 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.9 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.048 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.98 _diffrn_ambient_temperature 122(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9514 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.92 _reflns_number_total 9514 _reflns_number_gt 8212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Siemens, 1995' _computing_cell_refinement 'SAINT, Siemens, 1995' _computing_data_reduction 'SAINT, Siemens, 1995' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+3.1889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 9514 _refine_ls_number_parameters 757 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.628 _refine_ls_shift/su_mean 0.042 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.99839(7) -0.08819(6) -1.39780(6) 0.0152(3) Uani 1 1 d . . . N1 N -1.1463(7) -0.0089(6) -1.3961(5) 0.0245(15) Uani 1 1 d . . . O1 O -0.9104(5) -0.0875(5) -1.2936(4) 0.0163(12) Uani 1 1 d . . . O2 O -0.9870(5) -0.2449(5) -1.3034(4) 0.0208(13) Uani 1 1 d . . . N2 N -0.8823(6) 0.0096(5) -1.5046(5) 0.0152(14) Uani 1 1 d U . . N3 N -1.0147(6) -0.1236(5) -1.5101(5) 0.0167(15) Uani 1 1 d . . . Mn2 Mn -0.44631(7) -0.11973(7) -0.61804(6) 0.0143(3) Uani 1 1 d . . . O3 O -0.4611(5) 0.0384(5) -0.7136(4) 0.0174(13) Uani 1 1 d . . . N4 N -0.2921(6) -0.1879(5) -0.6215(5) 0.0177(14) Uani 1 1 d U . . O4 O -0.5316(6) -0.1211(5) -0.7212(4) 0.0191(13) Uani 1 1 d . . . N5 N -0.4615(6) -0.0751(5) -0.5050(5) 0.0134(14) Uani 1 1 d U . . N6 N -0.5364(6) -0.2384(5) -0.5130(5) 0.0134(13) Uani 1 1 d . . . C1 C -0.8598(7) -0.0079(7) -1.2967(6) 0.0142(17) Uani 1 1 d U . . C2 C -0.8555(7) 0.0054(6) -1.2079(6) 0.0133(17) Uani 1 1 d . . . C3 C -0.7752(8) 0.0757(6) -1.2144(6) 0.0170(18) Uani 1 1 d . . . H3A H -0.7660 0.0788 -1.1525 0.020 Uiso 1 1 calc R . . C4 C -0.7065(7) 0.1425(6) -1.3027(6) 0.0141(17) Uani 1 1 d . . . C5 C -0.7280(7) 0.1406(7) -1.3909(6) 0.0155(18) Uani 1 1 d U . . H5A H -0.6915 0.1905 -1.4542 0.019 Uiso 1 1 calc R . . C6 C -0.8018(7) 0.0681(7) -1.3918(6) 0.0175(19) Uani 1 1 d . . . C7 C -0.8121(7) 0.0666(6) -1.4894(6) 0.0126(16) Uani 1 1 d . . . H7A H -0.7622 0.1121 -1.5476 0.015 Uiso 1 1 calc R . . C8 C -0.8695(6) 0.0072(5) -1.6067(4) 0.0155(11) Uani 1 1 d . . . H8A H -0.7844 -0.0559 -1.6093 0.019 Uiso 1 1 calc R . . C9 C -0.8561(8) 0.1178(7) -1.6964(6) 0.0200(19) Uani 1 1 d . . . H9A H -0.7665 0.1343 -1.6955 0.024 Uiso 1 1 calc R . . H9B H -0.9357 0.1827 -1.6927 0.024 Uiso 1 1 calc R . . C10 C -0.8576(6) 0.1053(5) -1.7967(4) 0.0213(12) Uani 1 1 d . . . H10A H -0.8557 0.1799 -1.8562 0.026 Uiso 1 1 calc R . . H10B H -0.7713 0.0466 -1.8036 0.026 Uiso 1 1 calc R . . C11 C -0.9889(6) 0.0695(5) -1.7984(5) 0.0204(14) Uani 1 1 d . . . H11A H -1.0751 0.1318 -1.7992 0.024 Uiso 1 1 calc R . . H11B H -0.9826 0.0580 -1.8614 0.024 Uiso 1 1 calc R . . C12 C -0.9992(8) -0.0408(7) -1.7058(6) 0.0179(18) Uani 1 1 d . . . H12A H -0.9166 -0.1046 -1.7080 0.021 Uiso 1 1 calc R . . H12B H -1.0860 -0.0611 -1.7065 0.021 Uiso 1 1 calc R . . C13 C -1.0031(7) -0.0265(5) -1.6087(4) 0.0202(14) Uani 1 1 d . . . H13A H -1.0863 0.0396 -1.6103 0.024 Uiso 1 1 calc R . . C14 C -1.0395(8) -0.2137(7) -1.5035(6) 0.0177(18) Uani 1 1 d U . . H14A H -1.0476 -0.2161 -1.5659 0.021 Uiso 1 1 calc R . . C15 C -1.0565(8) -0.3140(7) -1.4091(6) 0.0187(19) Uani 1 1 d . . . C16 C -1.1049(8) -0.3967(7) -1.4165(6) 0.0155(17) Uani 1 1 d . . . H16A H -1.1253 -0.3863 -1.4813 0.019 Uiso 1 1 calc R . . C17 C -1.1235(8) -0.4947(7) -1.3290(6) 0.0177(18) Uani 1 1 d U . . C18 C -1.0872(8) -0.5079(7) -1.2358(6) 0.0191(19) Uani 1 1 d U . . H18A H -1.0968 -0.5760 -1.1767 0.023 Uiso 1 1 calc R . . C19 C -1.0381(8) -0.4286(7) -1.2234(6) 0.0167(18) Uani 1 1 d . . . C20 C -1.0279(8) -0.3236(7) -1.3128(7) 0.0163(18) Uani 1 1 d . . . C21 C -0.9438(8) -0.0528(7) -1.1123(6) 0.0198(18) Uani 1 1 d . . . C22 C -0.8927(8) -0.1841(6) -1.0691(6) 0.0187(18) Uani 1 1 d . . . H22A H -0.9518 -0.2180 -1.0075 0.028 Uiso 1 1 calc R . . H22B H -0.7941 -0.2088 -1.0516 0.028 Uiso 1 1 calc R . . H22C H -0.8992 -0.2098 -1.1205 0.028 Uiso 1 1 calc R . . C23 C -1.1010(8) -0.0150(7) -1.1399(7) 0.025(2) Uani 1 1 d . . . H23A H -1.1590 -0.0519 -1.0787 0.038 Uiso 1 1 calc R . . H23B H -1.1061 -0.0387 -1.1930 0.038 Uiso 1 1 calc R . . H23C H -1.1363 0.0692 -1.1653 0.038 Uiso 1 1 calc R . . C24 C -0.9456(9) -0.0133(8) -1.0279(6) 0.028(2) Uani 1 1 d . . . H24A H -1.0031 -0.0527 -0.9676 0.043 Uiso 1 1 calc R . . H24B H -0.9863 0.0705 -1.0535 0.043 Uiso 1 1 calc R . . H24C H -0.8487 -0.0327 -1.0091 0.043 Uiso 1 1 calc R . . C25 C -0.6131(8) 0.2114(7) -1.2969(6) 0.0215(19) Uani 1 1 d . . . C26 C -0.6753(9) 0.2620(9) -1.2199(7) 0.033(2) Uani 1 1 d . . . H26A H -0.6892 0.2000 -1.1528 0.050 Uiso 1 1 calc R . . H26B H -0.7666 0.3179 -1.2416 0.050 Uiso 1 1 calc R . . H26C H -0.6106 0.3010 -1.2152 0.050 Uiso 1 1 calc R . . C27 C -0.4677(8) 0.1290(7) -1.2644(8) 0.029(2) Uani 1 1 d . . . H27A H -0.4257 0.0961 -1.3143 0.043 Uiso 1 1 calc R . . H27B H -0.4781 0.0666 -1.1968 0.043 Uiso 1 1 calc R . . H27C H -0.4062 0.1715 -1.2614 0.043 Uiso 1 1 calc R . . C28 C -0.5919(9) 0.3088(7) -1.4006(7) 0.030(2) Uani 1 1 d U . . H28A H -0.5509 0.2768 -1.4512 0.044 Uiso 1 1 calc R . . H28B H -0.5278 0.3479 -1.3952 0.044 Uiso 1 1 calc R . . H28C H -0.6834 0.3645 -1.4221 0.044 Uiso 1 1 calc R . . C29 C -1.1760(8) -0.5869(7) -1.3360(6) 0.0181(18) Uani 1 1 d . . . C30 C -1.2731(9) -0.5343(8) -1.4261(8) 0.031(2) Uani 1 1 d . . . H30A H -1.3040 -0.5957 -1.4280 0.046 Uiso 1 1 calc R . . H30B H -1.2204 -0.4980 -1.4907 0.046 Uiso 1 1 calc R . . H30C H -1.3560 -0.4761 -1.4163 0.046 Uiso 1 1 calc R . . C31 C -1.2591(10) -0.6489(9) -1.2369(8) 0.041(3) Uani 1 1 d . . . H31A H -1.2907 -0.7071 -1.2440 0.061 Uiso 1 1 calc R . . H31B H -1.3417 -0.5925 -1.2241 0.061 Uiso 1 1 calc R . . H31C H -1.1980 -0.6869 -1.1794 0.061 Uiso 1 1 calc R . . C32 C -1.0470(8) -0.6769(7) -1.3545(8) 0.033(2) Uani 1 1 d . . . H32A H -1.0789 -0.7363 -1.3591 0.049 Uiso 1 1 calc R . . H32B H -0.9852 -0.7130 -1.2976 0.049 Uiso 1 1 calc R . . H32C H -0.9945 -0.6388 -1.4186 0.049 Uiso 1 1 calc R . . C33 C -1.0030(8) -0.4498(7) -1.1196(7) 0.023(2) Uani 1 1 d . . . C34 C -1.0101(10) -0.5721(7) -1.0348(7) 0.030(2) Uani 1 1 d . . . H34A H -0.9863 -0.5805 -0.9695 0.045 Uiso 1 1 calc R . . H34B H -0.9424 -0.6316 -1.0540 0.045 Uiso 1 1 calc R . . H34C H -1.1059 -0.5809 -1.0277 0.045 Uiso 1 1 calc R . . C35 C -0.8499(7) -0.4414(7) -1.1239(7) 0.0221(18) Uani 1 1 d . . . H35A H -0.8288 -0.4554 -1.0560 0.033 Uiso 1 1 calc R . . H35B H -0.8416 -0.3640 -1.1732 0.033 Uiso 1 1 calc R . . H35C H -0.7826 -0.4994 -1.1452 0.033 Uiso 1 1 calc R . . C36 C -1.1070(8) -0.3594(8) -1.0852(7) 0.027(2) Uani 1 1 d . . . H36A H -1.0840 -0.3735 -1.0178 0.040 Uiso 1 1 calc R . . H36B H -1.2037 -0.3651 -1.0811 0.040 Uiso 1 1 calc R . . H36C H -1.0997 -0.2819 -1.1348 0.040 Uiso 1 1 calc R . . C41 C -0.4188(8) 0.1158(7) -0.7033(6) 0.0173(19) Uani 1 1 d U . . C42 C -0.4022(8) 0.2194(7) -0.7915(7) 0.020(2) Uani 1 1 d . . . C43 C -0.3516(7) 0.2945(7) -0.7772(6) 0.0172(18) Uani 1 1 d U . . H43A H -0.3392 0.3619 -0.8361 0.021 Uiso 1 1 calc R . . C44 C -0.3160(8) 0.2814(7) -0.6831(7) 0.0187(19) Uani 1 1 d . . . C45 C -0.3410(8) 0.1871(7) -0.6020(7) 0.0201(19) Uani 1 1 d U . . H45A H -0.3248 0.1764 -0.5362 0.024 Uiso 1 1 calc R . . C46 C -0.3904(8) 0.1014(6) -0.6087(6) 0.0146(17) Uani 1 1 d . . . C47 C -0.4230(7) 0.0134(7) -0.5149(6) 0.0176(18) Uani 1 1 d . . . H47A H -0.4163 0.0193 -0.4539 0.021 Uiso 1 1 calc R . . C48 C -0.5152(7) -0.1544(5) -0.4041(4) 0.0183(13) Uani 1 1 d . . . H48A H -0.6193 -0.1197 -0.3976 0.022 Uiso 1 1 calc R . . C49 C -0.4536(10) -0.1697(8) -0.3097(7) 0.026(2) Uani 1 1 d . . . H49A H -0.4730 -0.0940 -0.3070 0.031 Uiso 1 1 calc R . . H49B H -0.3499 -0.2028 -0.3124 0.031 Uiso 1 1 calc R . . C50 C -0.5237(7) -0.2515(5) -0.2148(5) 0.0229(14) Uani 1 1 d . . . H50A H -0.4777 -0.2691 -0.1534 0.027 Uiso 1 1 calc R . . H50B H -0.6245 -0.2116 -0.2072 0.027 Uiso 1 1 calc R . . C51 C -0.5149(7) -0.3636(5) -0.2193(4) 0.0226(13) Uani 1 1 d . . . H51A H -0.4146 -0.4084 -0.2184 0.027 Uiso 1 1 calc R . . H51B H -0.5670 -0.4101 -0.1581 0.027 Uiso 1 1 calc R . . C52 C -0.5762(8) -0.3422(7) -0.3141(6) 0.0199(19) Uani 1 1 d . . . H52A H -0.6784 -0.3027 -0.3130 0.024 Uiso 1 1 calc R . . H52B H -0.5656 -0.4167 -0.3168 0.024 Uiso 1 1 calc R . . C53 C -0.4983(6) -0.2663(5) -0.4091(4) 0.0170(11) Uani 1 1 d . . . H53A H -0.3952 -0.3072 -0.4046 0.020 Uiso 1 1 calc R . . C54 C -0.6151(8) -0.2892(6) -0.5280(7) 0.0180(18) Uani 1 1 d . . . H54A H -0.6588 -0.3395 -0.4691 0.022 Uiso 1 1 calc R . . C55 C -0.6414(7) -0.2767(6) -0.6228(6) 0.0148(18) Uani 1 1 d . . . C56 C -0.7225(8) -0.3469(7) -0.6240(6) 0.0169(18) Uani 1 1 d U . . H56A H -0.7645 -0.3935 -0.5616 0.020 Uiso 1 1 calc R . . C57 C -0.7405(7) -0.3479(7) -0.7145(7) 0.021(2) Uani 1 1 d . . . C58 C -0.6687(7) -0.2807(6) -0.8071(6) 0.0165(18) Uani 1 1 d . . . H58A H -0.6764 -0.2835 -0.8693 0.020 Uiso 1 1 calc R . . C59 C -0.5897(8) -0.2130(7) -0.8081(6) 0.0195(19) Uani 1 1 d U . . C60 C -0.5852(8) -0.2026(7) -0.7151(6) 0.0160(18) Uani 1 1 d U . . C61 C -0.4359(8) 0.2411(7) -0.8985(6) 0.0194(18) Uani 1 1 d . . . C62 C -0.3310(8) 0.1495(8) -0.9331(7) 0.026(2) Uani 1 1 d . . . H62A H -0.2339 0.1522 -0.9337 0.039 Uiso 1 1 calc R . . H62B H -0.3508 0.1660 -1.0021 0.039 Uiso 1 1 calc R . . H62C H -0.3421 0.0724 -0.8855 0.039 Uiso 1 1 calc R . . C63 C -0.4217(9) 0.3594(8) -0.9781(7) 0.031(2) Uani 1 1 d . . . H63A H -0.3246 0.3641 -0.9820 0.047 Uiso 1 1 calc R . . H63B H -0.4877 0.4193 -0.9587 0.047 Uiso 1 1 calc R . . H63C H -0.4436 0.3710 -1.0450 0.047 Uiso 1 1 calc R . . C64 C -0.5878(8) 0.2397(7) -0.8968(7) 0.0248(19) Uani 1 1 d . . . H64A H -0.6019 0.1645 -0.8462 0.037 Uiso 1 1 calc R . . H64B H -0.6075 0.2526 -0.9647 0.037 Uiso 1 1 calc R . . H64C H -0.6521 0.3010 -0.8783 0.037 Uiso 1 1 calc R . . C65 C -0.2592(8) 0.3719(7) -0.6768(6) 0.0207(19) Uani 1 1 d . . . C66 C -0.1706(8) 0.3148(8) -0.5846(7) 0.0263(19) Uani 1 1 d . . . H66A H -0.0909 0.2529 -0.5916 0.039 Uiso 1 1 calc R . . H66B H -0.2292 0.2823 -0.5221 0.039 Uiso 1 1 calc R . . H66C H -0.1344 0.3725 -0.5804 0.039 Uiso 1 1 calc R . . C67 C -0.1646(8) 0.4243(7) -0.7727(7) 0.0255(19) Uani 1 1 d . . . H67A H -0.2194 0.4616 -0.8335 0.038 Uiso 1 1 calc R . . H67B H -0.0836 0.3629 -0.7793 0.038 Uiso 1 1 calc R . . H67C H -0.1306 0.4818 -0.7666 0.038 Uiso 1 1 calc R . . C68 C -0.3837(8) 0.4694(7) -0.6669(7) 0.030(2) Uani 1 1 d . . . H68A H -0.4404 0.5056 -0.7266 0.045 Uiso 1 1 calc R . . H68B H -0.3475 0.5273 -0.6634 0.045 Uiso 1 1 calc R . . H68C H -0.4427 0.4375 -0.6045 0.045 Uiso 1 1 calc R . . C69 C -0.8334(8) -0.4158(7) -0.7215(6) 0.0199(18) Uani 1 1 d . . . C70 C -0.7694(9) -0.4684(8) -0.8003(8) 0.031(2) Uani 1 1 d . . . H70A H -0.8321 -0.5107 -0.8023 0.046 Uiso 1 1 calc R . . H70B H -0.6762 -0.5216 -0.7801 0.046 Uiso 1 1 calc R . . H70C H -0.7596 -0.4063 -0.8682 0.046 Uiso 1 1 calc R . . C71 C -0.9791(9) -0.3303(9) -0.7553(8) 0.037(2) Uani 1 1 d . . . H71A H -1.0412 -0.3709 -0.7607 0.056 Uiso 1 1 calc R . . H71B H -0.9667 -0.2672 -0.8220 0.056 Uiso 1 1 calc R . . H71C H -1.0216 -0.2986 -0.7046 0.056 Uiso 1 1 calc R . . C72 C -0.8506(11) -0.5169(9) -0.6173(7) 0.047(3) Uani 1 1 d . . . H72A H -0.9102 -0.5589 -0.6236 0.071 Uiso 1 1 calc R . . H72B H -0.8951 -0.4866 -0.5660 0.071 Uiso 1 1 calc R . . H72C H -0.7573 -0.5695 -0.5962 0.071 Uiso 1 1 calc R . . C73 C -0.4942(7) -0.1572(7) -0.9057(6) 0.0180(18) Uani 1 1 d U . . C74 C -0.3417(8) -0.2004(8) -0.8748(7) 0.029(2) Uani 1 1 d . . . H74A H -0.3364 -0.1787 -0.8204 0.043 Uiso 1 1 calc R . . H74B H -0.2800 -0.1655 -0.9342 0.043 Uiso 1 1 calc R . . H74C H -0.3108 -0.2847 -0.8498 0.043 Uiso 1 1 calc R . . C75 C -0.5434(9) -0.0242(8) -0.9494(7) 0.030(2) Uani 1 1 d . . . H75A H -0.5409 0.0009 -0.8967 0.045 Uiso 1 1 calc R . . H75B H -0.6402 0.0021 -0.9707 0.045 Uiso 1 1 calc R . . H75C H -0.4803 0.0089 -1.0086 0.045 Uiso 1 1 calc R . . C76 C -0.5000(8) -0.1916(7) -0.9901(7) 0.0231(19) Uani 1 1 d . . . H76A H -0.5973 -0.1642 -1.0108 0.035 Uiso 1 1 calc R . . H76B H -0.4689 -0.2760 -0.9648 0.035 Uiso 1 1 calc R . . H76C H -0.4376 -0.1568 -1.0491 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0114(6) 0.0180(6) 0.0167(6) -0.0074(5) 0.0000(4) -0.0048(5) N1 0.014(3) 0.034(4) 0.026(4) -0.017(3) -0.001(2) -0.001(3) O1 0.013(3) 0.020(3) 0.019(3) -0.006(3) -0.002(2) -0.011(2) O2 0.025(3) 0.022(3) 0.022(3) -0.010(3) 0.002(2) -0.014(2) N2 0.014(3) 0.021(3) 0.015(3) -0.012(2) -0.0026(19) -0.001(2) N3 0.013(3) 0.018(3) 0.017(3) -0.004(2) 0.000(2) -0.006(2) Mn2 0.0105(5) 0.0169(6) 0.0153(6) -0.0071(5) 0.0005(4) -0.0036(4) O3 0.016(3) 0.020(3) 0.015(3) -0.004(2) -0.004(2) -0.005(2) N4 0.009(3) 0.020(3) 0.018(3) -0.006(2) 0.003(2) -0.002(2) O4 0.020(3) 0.019(3) 0.017(3) -0.008(3) 0.000(2) -0.003(2) N5 0.012(3) 0.016(3) 0.014(3) -0.008(2) -0.002(2) -0.002(2) N6 0.016(3) 0.010(3) 0.012(3) -0.004(2) 0.006(2) -0.005(2) C1 0.003(3) 0.016(3) 0.018(3) -0.005(3) -0.002(2) 0.003(2) C2 0.013(3) 0.008(3) 0.017(4) -0.004(3) -0.004(3) 0.000(3) C3 0.017(4) 0.016(4) 0.013(4) -0.008(3) -0.003(3) 0.005(3) C4 0.014(4) 0.012(4) 0.012(4) -0.002(3) 0.003(3) -0.007(3) C5 0.005(3) 0.016(3) 0.020(4) -0.003(3) 0.002(3) -0.003(3) C6 0.007(4) 0.019(4) 0.021(5) -0.009(4) 0.003(3) 0.004(3) C7 0.008(3) 0.013(3) 0.015(4) -0.006(3) -0.001(2) 0.000(3) C8 0.010(3) 0.017(3) 0.019(3) -0.008(2) 0.000(2) -0.004(2) C9 0.015(4) 0.026(4) 0.023(4) -0.012(3) -0.005(3) -0.006(3) C10 0.019(3) 0.022(3) 0.018(3) -0.002(2) -0.002(2) -0.008(3) C11 0.013(3) 0.031(3) 0.017(3) -0.008(3) -0.003(3) -0.007(3) C12 0.007(4) 0.027(4) 0.020(4) -0.010(4) -0.002(3) -0.004(3) C13 0.012(3) 0.026(3) 0.026(3) -0.013(3) 0.000(3) -0.008(3) C14 0.012(3) 0.022(3) 0.018(3) -0.006(3) -0.004(2) -0.004(3) C15 0.007(4) 0.031(5) 0.020(5) -0.015(4) 0.004(3) -0.005(3) C16 0.014(3) 0.024(4) 0.016(4) -0.016(3) -0.002(3) -0.002(3) C17 0.011(3) 0.019(3) 0.021(4) -0.009(3) 0.003(3) -0.003(3) C18 0.016(3) 0.018(3) 0.020(3) -0.008(3) 0.001(2) -0.001(3) C19 0.009(4) 0.021(4) 0.021(5) -0.010(4) -0.002(3) -0.002(3) C20 0.007(3) 0.023(4) 0.025(4) -0.017(3) -0.002(3) -0.002(3) C21 0.016(4) 0.028(4) 0.022(4) -0.013(3) -0.003(3) -0.010(3) C22 0.026(4) 0.017(4) 0.016(4) -0.004(3) -0.006(3) -0.011(3) C23 0.013(4) 0.031(5) 0.026(5) -0.007(4) 0.005(3) -0.010(3) C24 0.023(4) 0.043(5) 0.013(4) -0.011(4) 0.004(3) -0.005(4) C25 0.021(4) 0.025(4) 0.020(5) -0.006(4) -0.004(3) -0.011(3) C26 0.034(5) 0.049(6) 0.034(6) -0.027(5) 0.004(4) -0.021(4) C27 0.016(4) 0.030(4) 0.046(6) -0.015(4) -0.006(4) -0.013(3) C28 0.030(2) 0.030(2) 0.030(2) -0.0122(12) -0.0030(10) -0.0092(11) C29 0.017(4) 0.021(4) 0.021(4) -0.009(4) 0.002(3) -0.011(3) C30 0.025(4) 0.025(4) 0.050(6) -0.020(4) -0.016(4) -0.001(3) C31 0.047(5) 0.055(6) 0.048(6) -0.039(5) 0.021(4) -0.037(4) C32 0.021(4) 0.021(4) 0.062(6) -0.027(5) -0.005(4) 0.001(3) C33 0.018(4) 0.023(4) 0.025(5) -0.008(4) 0.000(3) -0.005(3) C34 0.042(5) 0.024(4) 0.024(5) -0.006(4) 0.002(4) -0.019(4) C35 0.014(4) 0.022(4) 0.028(5) -0.008(4) -0.006(3) -0.003(3) C36 0.018(4) 0.034(5) 0.028(5) -0.013(4) 0.004(3) -0.010(4) C41 0.014(3) 0.017(3) 0.018(4) -0.004(3) 0.002(3) -0.008(3) C42 0.008(4) 0.025(5) 0.024(5) -0.010(4) 0.004(3) -0.005(3) C43 0.010(3) 0.016(3) 0.024(3) -0.007(3) 0.003(2) -0.005(2) C44 0.009(3) 0.023(4) 0.028(4) -0.017(3) 0.001(3) -0.001(3) C45 0.017(3) 0.023(3) 0.018(4) -0.006(3) 0.000(3) -0.007(3) C46 0.011(4) 0.010(4) 0.023(5) -0.008(3) -0.003(3) -0.001(3) C47 0.013(3) 0.022(4) 0.019(4) -0.014(3) -0.002(3) 0.004(3) C48 0.018(3) 0.027(3) 0.009(3) -0.005(2) 0.006(2) -0.012(3) C49 0.033(5) 0.026(5) 0.023(5) -0.013(4) -0.001(4) -0.008(4) C50 0.017(4) 0.031(3) 0.017(3) -0.007(3) 0.000(3) -0.007(3) C51 0.021(3) 0.022(3) 0.019(3) -0.004(3) -0.002(2) -0.005(3) C52 0.021(4) 0.015(3) 0.013(4) 0.003(3) 0.003(3) -0.007(3) C53 0.012(3) 0.019(3) 0.017(3) -0.007(2) 0.002(2) -0.003(2) C54 0.013(4) 0.009(3) 0.026(4) -0.006(3) 0.005(3) -0.002(3) C55 0.014(4) 0.014(4) 0.019(5) -0.008(4) -0.004(3) -0.004(3) C56 0.015(3) 0.016(3) 0.018(3) -0.007(3) 0.002(3) -0.004(3) C57 0.010(4) 0.020(4) 0.035(5) -0.017(4) -0.006(3) 0.004(3) C58 0.013(4) 0.020(4) 0.021(5) -0.010(4) -0.002(3) -0.007(3) C59 0.013(3) 0.018(3) 0.021(4) -0.005(3) 0.000(3) 0.000(3) C60 0.014(3) 0.014(3) 0.021(3) -0.009(3) -0.003(2) -0.001(2) C61 0.024(4) 0.030(5) 0.011(4) -0.008(4) -0.001(3) -0.017(4) C62 0.021(4) 0.038(5) 0.029(5) -0.023(4) 0.001(3) -0.010(4) C63 0.034(5) 0.040(5) 0.022(5) -0.007(4) -0.009(3) -0.015(4) C64 0.028(4) 0.030(4) 0.019(4) -0.007(4) -0.003(3) -0.015(4) C65 0.023(4) 0.019(4) 0.022(5) -0.013(4) 0.001(3) -0.001(3) C66 0.025(4) 0.036(5) 0.032(5) -0.024(4) 0.009(3) -0.018(4) C67 0.025(4) 0.023(4) 0.024(4) -0.002(3) -0.003(3) -0.012(3) C68 0.028(4) 0.026(4) 0.033(5) -0.011(4) 0.004(3) -0.007(4) C69 0.015(4) 0.024(4) 0.025(5) -0.013(4) 0.000(3) -0.007(3) C70 0.027(5) 0.027(5) 0.051(7) -0.026(5) 0.003(4) -0.012(4) C71 0.020(4) 0.055(6) 0.055(7) -0.041(5) -0.005(4) -0.006(4) C72 0.073(6) 0.055(5) 0.028(4) -0.002(3) -0.007(3) -0.057(4) C73 0.016(3) 0.021(3) 0.014(3) -0.004(3) 0.008(3) -0.010(3) C74 0.022(4) 0.039(5) 0.029(5) -0.017(4) 0.005(3) -0.013(4) C75 0.029(5) 0.039(5) 0.021(5) -0.012(4) 0.002(4) -0.011(4) C76 0.026(4) 0.021(4) 0.033(5) -0.015(4) 0.007(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 1.526(6) . ? Mn1 O2 1.907(6) . ? Mn1 O1 1.912(5) . ? Mn1 N3 1.957(7) . ? Mn1 N2 1.976(7) . ? O1 C1 1.300(9) . ? O2 C20 1.314(10) . ? N2 C7 1.298(9) . ? N2 C8 1.491(8) . ? N3 C14 1.267(10) . ? N3 C13 1.459(9) . ? Mn2 N4 1.525(6) . ? Mn2 O4 1.886(6) . ? Mn2 O3 1.920(6) . ? Mn2 N6 1.965(6) . ? Mn2 N5 1.967(6) . ? O3 C41 1.313(10) . ? O4 C60 1.325(9) . ? N5 C47 1.300(10) . ? N5 C48 1.495(8) . ? N6 C54 1.293(10) . ? N6 C53 1.494(8) . ? C1 C2 1.403(12) . ? C1 C6 1.445(12) . ? C2 C3 1.382(11) . ? C2 C21 1.520(12) . ? C3 C4 1.393(11) . ? C4 C5 1.365(12) . ? C4 C25 1.543(11) . ? C5 C6 1.399(11) . ? C6 C7 1.466(12) . ? C8 C9 1.499(10) . ? C8 C13 1.547(7) . ? C9 C10 1.559(10) . ? C10 C11 1.539(8) . ? C11 C12 1.507(10) . ? C12 C13 1.513(10) . ? C14 C15 1.458(12) . ? C15 C16 1.396(11) . ? C15 C20 1.438(12) . ? C16 C17 1.395(12) . ? C17 C18 1.403(12) . ? C17 C29 1.536(11) . ? C18 C19 1.395(11) . ? C19 C20 1.444(12) . ? C19 C33 1.510(12) . ? C21 C22 1.523(11) . ? C21 C24 1.546(11) . ? C21 C23 1.564(10) . ? C25 C26 1.508(12) . ? C25 C28 1.522(12) . ? C25 C27 1.529(10) . ? C29 C32 1.538(10) . ? C29 C31 1.537(12) . ? C29 C30 1.553(12) . ? C33 C36 1.533(12) . ? C33 C35 1.555(11) . ? C33 C34 1.562(11) . ? C41 C46 1.387(12) . ? C41 C42 1.439(12) . ? C42 C43 1.368(11) . ? C42 C61 1.547(12) . ? C43 C44 1.413(12) . ? C44 C45 1.342(12) . ? C44 C65 1.538(11) . ? C45 C46 1.434(11) . ? C46 C47 1.411(12) . ? C48 C53 1.492(8) . ? C48 C49 1.529(10) . ? C49 C50 1.533(11) . ? C50 C51 1.511(9) . ? C51 C52 1.502(10) . ? C52 C53 1.541(9) . ? C54 C55 1.392(12) . ? C55 C60 1.405(12) . ? C55 C56 1.430(11) . ? C56 C57 1.381(12) . ? C57 C58 1.445(12) . ? C57 C69 1.536(11) . ? C58 C59 1.372(11) . ? C59 C60 1.443(12) . ? C59 C73 1.569(11) . ? C61 C64 1.517(11) . ? C61 C63 1.519(12) . ? C61 C62 1.550(11) . ? C65 C66 1.519(12) . ? C65 C68 1.531(10) . ? C65 C67 1.539(12) . ? C69 C72 1.541(12) . ? C69 C71 1.546(11) . ? C69 C70 1.550(12) . ? C73 C76 1.521(11) . ? C73 C74 1.528(11) . ? C73 C75 1.540(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn1 O2 112.5(3) . . ? N1 Mn1 O1 103.1(3) . . ? O2 Mn1 O1 83.1(2) . . ? N1 Mn1 N3 98.8(3) . . ? O2 Mn1 N3 90.3(3) . . ? O1 Mn1 N3 158.0(2) . . ? N1 Mn1 N2 106.4(3) . . ? O2 Mn1 N2 141.1(2) . . ? O1 Mn1 N2 90.3(2) . . ? N3 Mn1 N2 81.7(3) . . ? C1 O1 Mn1 129.0(5) . . ? C20 O2 Mn1 128.9(5) . . ? C7 N2 C8 120.0(6) . . ? C7 N2 Mn1 124.8(5) . . ? C8 N2 Mn1 115.0(4) . . ? C14 N3 C13 121.7(7) . . ? C14 N3 Mn1 127.5(6) . . ? C13 N3 Mn1 110.7(4) . . ? N4 Mn2 O4 106.2(3) . . ? N4 Mn2 O3 108.2(3) . . ? O4 Mn2 O3 82.4(2) . . ? N4 Mn2 N6 102.4(3) . . ? O4 Mn2 N6 90.2(3) . . ? O3 Mn2 N6 149.4(2) . . ? N4 Mn2 N5 103.9(3) . . ? O4 Mn2 N5 149.8(2) . . ? O3 Mn2 N5 89.3(3) . . ? N6 Mn2 N5 82.2(3) . . ? C41 O3 Mn2 127.4(5) . . ? C60 O4 Mn2 127.8(5) . . ? C47 N5 C48 121.8(6) . . ? C47 N5 Mn2 123.4(5) . . ? C48 N5 Mn2 114.8(4) . . ? C54 N6 C53 123.0(6) . . ? C54 N6 Mn2 126.9(5) . . ? C53 N6 Mn2 110.0(4) . . ? O1 C1 C2 121.4(7) . . ? O1 C1 C6 121.0(7) . . ? C2 C1 C6 117.6(7) . . ? C3 C2 C1 117.3(7) . . ? C3 C2 C21 123.7(7) . . ? C1 C2 C21 118.9(7) . . ? C2 C3 C4 126.4(7) . . ? C5 C4 C3 115.2(7) . . ? C5 C4 C25 124.3(7) . . ? C3 C4 C25 120.5(7) . . ? C4 C5 C6 122.6(7) . . ? C5 C6 C1 119.9(7) . . ? C5 C6 C7 118.8(7) . . ? C1 C6 C7 121.2(8) . . ? N2 C7 C6 126.7(7) . . ? N2 C8 C9 114.9(5) . . ? N2 C8 C13 104.6(5) . . ? C9 C8 C13 111.9(5) . . ? C8 C9 C10 108.7(6) . . ? C11 C10 C9 112.4(5) . . ? C12 C11 C10 110.5(5) . . ? C11 C12 C13 110.4(6) . . ? N3 C13 C12 118.9(6) . . ? N3 C13 C8 105.7(5) . . ? C12 C13 C8 110.5(5) . . ? N3 C14 C15 126.1(8) . . ? C16 C15 C20 122.3(8) . . ? C16 C15 C14 117.4(7) . . ? C20 C15 C14 120.3(8) . . ? C17 C16 C15 120.3(7) . . ? C16 C17 C18 117.6(8) . . ? C16 C17 C29 120.8(7) . . ? C18 C17 C29 121.5(7) . . ? C19 C18 C17 124.9(8) . . ? C18 C19 C20 117.4(7) . . ? C18 C19 C33 121.2(7) . . ? C20 C19 C33 121.4(8) . . ? O2 C20 C15 123.5(8) . . ? O2 C20 C19 119.2(7) . . ? C15 C20 C19 117.3(8) . . ? C2 C21 C22 112.1(6) . . ? C2 C21 C24 111.9(7) . . ? C22 C21 C24 109.2(7) . . ? C2 C21 C23 108.7(6) . . ? C22 C21 C23 108.7(7) . . ? C24 C21 C23 106.0(6) . . ? C26 C25 C28 108.8(7) . . ? C26 C25 C27 108.6(7) . . ? C28 C25 C27 107.8(7) . . ? C26 C25 C4 111.7(7) . . ? C28 C25 C4 111.6(7) . . ? C27 C25 C4 108.2(6) . . ? C32 C29 C17 108.6(6) . . ? C32 C29 C31 108.6(7) . . ? C17 C29 C31 111.7(7) . . ? C32 C29 C30 107.9(7) . . ? C17 C29 C30 112.0(6) . . ? C31 C29 C30 108.0(7) . . ? C19 C33 C36 109.7(7) . . ? C19 C33 C35 110.6(7) . . ? C36 C33 C35 108.9(7) . . ? C19 C33 C34 113.4(8) . . ? C36 C33 C34 107.8(7) . . ? C35 C33 C34 106.3(7) . . ? O3 C41 C46 121.8(7) . . ? O3 C41 C42 120.0(8) . . ? C46 C41 C42 118.3(8) . . ? C43 C42 C41 117.5(8) . . ? C43 C42 C61 122.1(8) . . ? C41 C42 C61 120.4(8) . . ? C42 C43 C44 126.2(8) . . ? C45 C44 C43 114.2(8) . . ? C45 C44 C65 124.3(8) . . ? C43 C44 C65 121.4(7) . . ? C44 C45 C46 124.1(8) . . ? C41 C46 C47 123.7(7) . . ? C41 C46 C45 119.5(7) . . ? C47 C46 C45 116.4(7) . . ? N5 C47 C46 125.5(8) . . ? N5 C48 C53 107.9(5) . . ? N5 C48 C49 115.9(6) . . ? C53 C48 C49 112.9(5) . . ? C48 C49 C50 107.8(6) . . ? C51 C50 C49 113.4(6) . . ? C52 C51 C50 111.4(5) . . ? C51 C52 C53 109.2(6) . . ? C48 C53 N6 107.3(5) . . ? C48 C53 C52 109.2(5) . . ? N6 C53 C52 118.9(5) . . ? N6 C54 C55 125.8(8) . . ? C54 C55 C60 122.0(7) . . ? C54 C55 C56 117.8(7) . . ? C60 C55 C56 120.1(7) . . ? C57 C56 C55 120.9(7) . . ? C56 C57 C58 117.9(7) . . ? C56 C57 C69 123.3(8) . . ? C58 C57 C69 118.8(7) . . ? C59 C58 C57 122.3(7) . . ? C58 C59 C60 119.0(7) . . ? C58 C59 C73 120.6(7) . . ? C60 C59 C73 120.1(7) . . ? O4 C60 C55 122.9(7) . . ? O4 C60 C59 118.3(7) . . ? C55 C60 C59 118.8(7) . . ? C64 C61 C63 106.6(7) . . ? C64 C61 C42 110.3(7) . . ? C63 C61 C42 111.1(7) . . ? C64 C61 C62 111.1(7) . . ? C63 C61 C62 107.6(7) . . ? C42 C61 C62 110.2(7) . . ? C66 C65 C68 110.0(7) . . ? C66 C65 C67 107.8(7) . . ? C68 C65 C67 108.7(7) . . ? C66 C65 C44 109.4(6) . . ? C68 C65 C44 109.4(6) . . ? C67 C65 C44 111.4(7) . . ? C57 C69 C72 110.9(7) . . ? C57 C69 C71 107.3(6) . . ? C72 C69 C71 110.4(8) . . ? C57 C69 C70 112.3(6) . . ? C72 C69 C70 107.0(7) . . ? C71 C69 C70 109.0(7) . . ? C76 C73 C74 108.6(6) . . ? C76 C73 C75 107.4(7) . . ? C74 C73 C75 110.5(7) . . ? C76 C73 C59 111.6(6) . . ? C74 C73 C59 107.9(7) . . ? C75 C73 C59 110.8(6) . . ? _diffrn_measured_fraction_theta_max 0.805 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.805 _refine_diff_density_max 0.553 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.073 data_2i #================================== # 5. CHEMICAL DATA _chemical_formula_sum C28H34N3O2Br2Mn _chemical_formula_weight 661.39 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,1/2+y,-z' _cell_length_a 12.2876(5) _cell_length_b 9.1876(4) _cell_length_c 24.399(1) _cell_angle_alpha 90 _cell_angle_beta 90.518(1) _cell_angle_gamma 90 _cell_volume 2754.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 7416 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max .88 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.59 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 3.42 _exptl_absorpt_correction_type 'multi-scan, SADABS' _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.69 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 55917 _diffrn_reflns_av_R_equivalents 0.239 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process 55917 _reflns_number_total 15788 _reflns_number_observed 3748 _reflns_observed_criterion I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; Pseudo center of symmetry except for the 2 cyclohexane rings, (space group nearly P21/n), therefore constrained rigid body refinement, TLS model, for all atoms other than Mn and Br; same TL, opposite S for the 2 molecules, both relative to their Mn centres. Thermal parameters for the heavy atoms also constrained to be the same for related atoms. Hydrogen atom positions recalculated each cycle, methyl groups with refined torsion angle. Initial constraints on the geometry of the molecules were released at the end, but the correlations are large, so that only average distances can be trusted. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method ; Type 1 Lorentzian isotropic; Becker and Coppens (1974) ; _refine_ls_extinction_coef 14(13) _refine_ls_abs_structure_details ; Rogers (1981) parameter refined to 1.10 (9), reset to 1.0. 1712 Bijvoet pairs in refinement. ; _refine_ls_abs_structure_Rogers 1.0 _refine_ls_number_reflns 3748 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 38 _refine_ls_R_factor_obs 0.060 _refine_ls_wR_factor_obs 0.068 _refine_ls_goodness_of_fit_obs 0.745 _refine_ls_shift/esd_max 0.161 _refine_ls_shift/esd_mean 0.009 _refine_diff_density_max 1.4(2) _refine_diff_density_min -1.2(2) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Br(1) 0.1317(4) -0.6274 0.1859(1) 0.0290(8) Uij Br(2) 0.1194(4) -0.3448(7) 0.3680(1) 0.0217(7) Uij Br(1') -0.6293(4) -0.1781(2) 0.3189(2) 0.0290(8) Uij Br(2') -0.6209(4) -0.4617(7) 0.1382(1) 0.0217(7) Uij Mn -0.1878(5) -0.6141(9) 0.2964(2) 0.0143(10) Uij Mn' -0.3121(5) -0.2043(8) 0.2091(2) 0.0143(10) Uij O(1) -0.0862(15) -0.5971(20) 0.2358(7) 0.0138(8) Uij O(2) -0.0919(14) -0.4657(19) 0.3245(7) 0.0136(8) Uij N -0.1582(16) -0.7450(20) 0.3305(6) 0.0128(9) Uij N(1) -0.3036(15) -0.6883(17) 0.2480(7) 0.0142(9) Uij C(8) -0.4055(15) -0.7027(21) 0.2786(8) 0.0153(10) Uij C(21) -0.5033(20) -0.7432(26) 0.2468(10) 0.0173(14) Uij C(22) -0.6068(16) -0.7454(22) 0.2840(8) 0.0195(21) Uij N(2) -0.3138(20) -0.5312(21) 0.3352(9) 0.0143(8) Uij C(9) -0.4223(16) -0.5572(21) 0.3069(8) 0.0158(10) Uij C(24) -0.5154(28) -0.5600(29) 0.3484(11) 0.0174(14) Uij C(23) -0.6173(16) -0.5974(21) 0.3143(8) 0.0199(21) Uij C(1) -0.1009(26) -0.6614(34) 0.1910(10) 0.0142(7) Uij C(2) -0.0064(27) -0.6835(29) 0.1576(10) 0.0150(10) Uij C(3) -0.0147(29) -0.7653(35) 0.1058(12) 0.0158(11) Uij C(4) -0.1104(29) -0.8040(31) 0.0844(11) 0.0160(10) Uij C(5) -0.2051(27) -0.7901(33) 0.1155(12) 0.0154(10) Uij C(6) -0.1942(27) -0.7200(34) 0.1657(12) 0.0146(8) Uij C(7) -0.2965(19) -0.7276(22) 0.1977(9) 0.0147(9) Uij C(17) -0.1113(26) -0.8802(32) 0.0245(12) 0.0175(14) Uij C(18) -0.1911(27) -0.7792(32) -0.0130(12) 0.0229(52) Uij C(19) -0.0036(30) -0.9059(37) 0.0004(14) 0.0214(55) Uij C(20) -0.1716(27) -1.0253(33) 0.0282(11) 0.0203(54) Uij C(16) -0.1041(31) -0.4269(31) 0.3772(13) 0.0136(8) Uij C(15) -0.0089(27) -0.3705(34) 0.4093(11) 0.0143(10) Uij C(14) -0.0168(25) -0.3476(35) 0.4604(12) 0.0146(10) Uij C(13) -0.1050(28) -0.3672(35) 0.4943(12) 0.0145(9) Uij C(12) -0.1969(30) -0.3953(32) 0.4646(13) 0.0143(9) Uij C(11) -0.1969(27) -0.4346(32) 0.4095(12) 0.0138(8) Uij C(10) -0.3074(22) -0.4649(29) 0.3818(11) 0.0144(9) Uij C(25) -0.0988(27) -0.3547(35) 0.5558(12) 0.0155(13) Uij C(26) -0.0617(28) -0.2014(36) 0.5725(11) 0.0239(67) Uij C(27) -0.2113(21) -0.3767(35) 0.5845(11) 0.0236(70) Uij C(28) -0.0199(25) -0.4651(38) 0.5763(11) 0.0231(51) Uij C(1') -0.4028(26) -0.1449(34) 0.3156(10) 0.0141(7) Uij C(2') -0.4924(27) -0.1113(29) 0.3476(10) 0.0149(10) Uij C(3') -0.4920(29) -0.0515(36) 0.3957(13) 0.0157(11) Uij C(4') -0.3915(28) 0.0103(31) 0.4189(11) 0.0158(10) Uij C(5') -0.3029(27) -0.0261(32) 0.3885(12) 0.0154(9) Uij C(6') -0.2971(27) -0.0904(34) 0.3359(12) 0.0145(8) Uij C(7') -0.2006(19) -0.1204(23) 0.3071(9) 0.0148(9) Uij C(17') -0.3763(25) 0.0781(31) 0.4720(12) 0.0171(13) Uij C(18') -0.3169(29) 0.2258(33) 0.4651(11) 0.0251(65) Uij C(19') -0.4873(31) 0.1083(40) 0.4982(15) 0.0263(67) Uij C(20') -0.3209(28) -0.0147(32) 0.5107(12) 0.0265(58) Uij C(16') -0.3947(31) -0.3931(33) 0.1259(13) 0.0136(8) Uij C(15') -0.4862(27) -0.4386(32) 0.0979(11) 0.0142(9) Uij C(14') -0.4932(24) -0.4662(36) 0.0408(12) 0.0147(10) Uij C(13') -0.4008(29) -0.4458(35) 0.0095(12) 0.0145(9) Uij C(12') -0.3062(30) -0.4016(32) 0.0349(13) 0.0142(9) Uij C(11') -0.2957(27) -0.3859(33) 0.0939(12) 0.0138(8) Uij C(10') -0.2047(22) -0.3279(28) 0.1147(11) 0.0142(9) Uij C(25') -0.4118(26) -0.4554(35) -0.0543(12) 0.0156(13) Uij C(26') -0.4970(24) -0.3458(35) -0.0743(11) 0.0189(45) Uij C(27') -0.3086(22) -0.4202(31) -0.0826(11) 0.0189(57) Uij C(28') -0.4533(26) -0.6109(35) -0.0692(10) 0.0195(59) Uij O(1')) -0.4013(15) -0.2249(20) 0.2703(7) 0.0138(7) Uij O(2') -0.3938(14) -0.3601(19) 0.1764(7) 0.0136(8) Uij N(' -0.3401(16) -0.0570(20) 0.1854(6) 0.0128(9) Uij N(1') -0.1884(15) -0.1635(17) 0.2590(7) 0.0144(9) Uij C(8') -0.0782(15) -0.1908(21) 0.2370(7) 0.0158(10) Uij C(21') 0.0166(21) -0.0954(24) 0.2594(10) 0.0176(15) Uij C(22') 0.1169(15) -0.1437(22) 0.2296(8) 0.0199(21) Uij N(2') -0.1930(20) -0.2568(21) 0.1602(8) 0.0141(8) Uij C(9') -0.0906(15) -0.1833(21) 0.1769(8) 0.0152(10) Uij C(24') 0.0185(28) -0.2311(30) 0.1493(11) 0.0174(15) Uij C(23') 0.1101(16) -0.1436(22) 0.1701(8) 0.0195(21) Uij H(3) 0.0548 -0.7554 0.0860 0.0169(16) Uij H(5) -0.2639 -0.8291 0.1011 0.0161(12) Uij H(7) -0.3602 -0.7637 0.1799 0.0157(11) Uij H(8) -0.3982 -0.7755 0.3065 0.0150(11) Uij H(9) -0.4338 -0.4883 0.2818 0.0166(11) Uij H(10) -0.3722 -0.4342 0.3993 0.0154(11) Uij H(12) -0.2651 -0.4112 0.4851 0.0149(12) Uij H(14) 0.0524 -0.3200 0.4792 0.0154(14) Uij H(18a) -0.2021(41) -0.8242(33) -0.0477(9) 0.0243(52) Uij H(18b) -0.1587(23) -0.6863(23) -0.0180(21) 0.0250(94) Uij H(18c) -0.2591(18) -0.7681(56) 0.0047(12) 0.0240(66) Uij H(19a) -0.0122(3) -0.9534(80) -0.0340(16) 0.0222(51) Uij H(19b) 0.0386(24) -0.9654(74) 0.0243(16) 0.0221(71) Uij H(19c) 0.0324(27) -0.8155(6) -0.0048(31) 0.0236(68) Uij H(20a) -0.1871(45) -1.0603(33) -0.0076 0.0215(50) Uij H(20b) -0.2378(24) -1.0119(14) 0.0474(22) 0.0214(63) Uij H(20c) -0.1276(21) -1.0941(20) 0.0472(22) 0.0210(96) Uij H(21a) -0.5003 -0.8341 0.2293 0.0174(16) Uij H(21b) -0.5195 -0.6703 0.2173 0.0182(16) Uij H(22a) -0.5977 -0.8195 0.3083 0.0193(21) Uij H(22b) -0.6700 -0.7567 0.2615 0.0215(27) Uij H(23a) -0.6334 -0.5263 0.2892 0.0208(23) Uij H(23b) -0.6780 -0.6130 0.3388 0.0216(27) Uij H(24a) -0.5273 -0.4698 0.3635 0.0180(16) Uij H(24b) -0.5064 -0.6333 0.3755 0.0171(15) Uij H(26a) -0.0554(52) -0.1961(21) 0.6113(1) 0.0246(66) Uij H(26b) -0.1135(27) -0.1320(6) 0.5600(24) 0.0272(99) Uij H(26c) 0.0070(25) -0.1812(28) 0.5566(22) 0.0272(75) Uij H(27a) -0.2050(13) -0.3504(63) 0.6220(6) 0.0242(70) Uij H(27b) -0.2325(24) -0.4758(13) 0.5817(22) 0.0265(77) Uij H(27c) -0.2645(11) -0.3171(50) 0.5671(16) 0.0270(98) Uij H(28a) -0.0081(44) -0.4516(48) 0.6145(6) 0.0243(52) Uij H(28b) 0.0471(18) -0.4545(50) 0.5576(21) 0.0262(82) Uij H(28c) -0.0482(25) -0.5599(1) 0.5699(26) 0.0259(92) Uij H(3') -0.5508 -0.0241 0.4157 0.0166(15) Uij H(5') -0.2283 0.0087 0.4007 0.0160(12) Uij H(7') -0.1351 -0.1057 0.3273 0.0159(11) Uij H(8') -0.0640 -0.2909 0.2453 0.0166(11) Uij H(9') -0.1010 -0.0811 0.1675 0.0150(11) Uij H(10') -0.1408 -0.3402 0.0935 0.0150(11) Uij H(12') -0.2432 -0.3924 0.0154 0.0148(12) Uij H(14') -0.5593 -0.4902 0.0242 0.0154(14) Uij H(18a') -0.3127(47) 0.2739(32) 0.4996(5) 0.0261(68) Uij H(18b') -0.3561(28) 0.2849(27) 0.4398(20) 0.0278(119) Uij H(18c') -0.2456(18) 0.2093(5) 0.4518(25) 0.0285(76) Uij H(19a') -0.4770(5) 0.1626(81) 0.5310(19) 0.0272(67) Uij H(19b') -0.5220(31) 0.0187 0.5065(32) 0.0305(83) Uij H(19c') -0.5315(25) 0.1624(81) 0.4734(14) 0.0291(83) Uij H(20a') -0.3263(46) 0.0257(37) 0.5464(4) 0.0274(64) Uij H(20b') -0.2464(11) -0.0226(57) 0.5010(16) 0.0299(66) Uij H(20c') -0.3533(34) -0.1086(20) 0.5102(19) 0.0306(111) Uij H(21a') 0.0223 -0.1141 0.2976 0.0182(16) Uij H(21b') 0.0008 0.0006 0.2522 0.0171(15) Uij H(22a') 0.1348 -0.2424 0.2414 0.0209(23) Uij H(22b') 0.1752 -0.0824 0.2420 0.0216(27) Uij H(23a') 0.0982 -0.0417 0.1587 0.0193(21) Uij H(23b') 0.1742 -0.1759 0.1544 0.0214(27) Uij H(24a') 0.0077 -0.2148 0.1089 0.0172(16) Uij H(24b') 0.0276 -0.3299 0.1544 0.0179(15) Uij H(26a') -0.5047(39) -0.3528(51) -0.1129(3) 0.0200(46) Uij H(26b') -0.4744(26) -0.2501(6) -0.0647(24) 0.0198(77) Uij H(26c') -0.5648(13) -0.3662(45) -0.0575(21) 0.0203(75) Uij H(27a') -0.3195(12) -0.4266(62) -0.1211(1) 0.0197(56) Uij H(27b') -0.2538(12) -0.4873(39) -0.0716(18) 0.0203(85) Uij H(27c') -0.2865(25) -0.3243(23) -0.0732(19) 0.0199(64) Uij H(28a') -0.4711(49) -0.6148(20) -0.1072(5) 0.0204(58) Uij H(28b') -0.5161(31) -0.6326(27) -0.0484(19) 0.0209(66) Uij H(28c') -0.3980(19) -0.6801(7) -0.0612(25) 0.0209(89) Uij 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 Br(1) 0.0113(7) 0.0368(7) 0.0391(10) -0.0060(6) 0.0047(6) -0.0089(7) Br(2) 0.0146(6) 0.0242(6) 0.0263(9) -0.0033(5) 0.0066(6) 0.0036(7) Br(1') 0.0113(7) 0.0368(7) 0.0391(10) -0.0060(6) 0.0047(6) -0.0089(7) Br(2') 0.0146(6) 0.0242(6) 0.0263(9) -0.0033(5) 0.0066(6) 0.0036(7) Mn 0.0109(9) 0.0136(10) 0.0184(12) -0.0010(8) 0.0038(9) 0.0017(9) Mn' 0.0109(9) 0.0136(10) 0.0184(12) -0.0010(8) 0.0038(9) 0.0017(9) O(1) 0.0093(8) 0.0121(8) 0.0201(6) -0.0009(7) 0.0031(5) 0.0015(6) O(2) 0.0092(8) 0.0113(8) 0.0204(7) -0.0003(7) 0.0017(6) 0.0013(6) N 0.0073(11) 0.0120(8) 0.0193(7) -0.0011(8) 0.0024(7) 0.0008(6) N(1) 0.0080(8) 0.0158(10) 0.0190(7) 0.0000(7) 0.0021(6) -0.0002(7) C(8) 0.0075(8) 0.0188(12) 0.0197(9) -0.0001(9) 0.0020(6) -0.0017(9) C(21) 0.0077(9) 0.0234(20) 0.0209(13) 0.0000(12) 0.0016(8) -0.0036(13) C(22) 0.0073(10) 0.0284(29) 0.0230(18) -0.0005(15) 0.0021(9) -0.0061(18) N(2) 0.0082(7) 0.0153(10) 0.0193(7) 0.0011(7) 0.0013(5) -0.0003(7) C(9) 0.0082(7) 0.0192(13) 0.0200(10) 0.0018(9) 0.0011(6) -0.0018(9) C(24) 0.0079(8) 0.0232(20) 0.0213(13) 0.0017(12) 0.0015(7) -0.0037(13) C(23) 0.0078(8) 0.0288(31) 0.0232(18) 0.0021(14) 0.0011(8) -0.0061(18) C(1) 0.0098(8) 0.0129(8) 0.0198(6) -0.0011(7) 0.0036(5) 0.0014(6) C(2) 0.0109(8) 0.0132(13) 0.0211(8) -0.0021(9) 0.0050(7) 0.0013(8) C(3) 0.0121(10) 0.0145(14) 0.0209(9) -0.0023(9) 0.0058(7) 0.0010(8) C(4) 0.0127(11) 0.0155(11) 0.0197(7) -0.0015(8) 0.0048(7) 0.0007(7) C(5) 0.0113(9) 0.0160(12) 0.0191(7) -0.0008(7) 0.0034(6) 0.0004(7) C(6) 0.0100(8) 0.0146(10) 0.0191(7) -0.0006(6) 0.0031(6) 0.0008(6) C(7) 0.0089(8) 0.0163(12) 0.0190(7) -0.0001(7) 0.0022(6) -0.0002(7) C(17) 0.0152(16) 0.0174(15) 0.0198(8) -0.0018(11) 0.0056(8) 0.0002(9) C(18) 0.0259(79) 0.0231(40) 0.0199(12) 0.0043(57) 0.0020(28) -0.0011(20) C(19) 0.0165(19) 0.0249(90) 0.0229(23) -0.0031(16) 0.0078(11) -0.0033(44) C(20) 0.0207(89) 0.0201(26) 0.0202(12) -0.0059(49) 0.0069(26) -0.0020(14) C(16) 0.0092(8) 0.0113(7) 0.0205(7) 0.0001(7) 0.0010(6) 0.0010(6) C(15) 0.0099(10) 0.0109(10) 0.0221(9) -0.0004(9) 0.0006(7) 0.0007(8) C(14) 0.0104(11) 0.0112(10) 0.0221(9) 0.0001(9) -0.0003(7) 0.0003(8) C(13) 0.0108(12) 0.0120(9) 0.0207(7) 0.0008(8) -0.0004(7) 0.0001(7) C(12) 0.0100(10) 0.0129(11) 0.0199(7) 0.0011(8) 0.0004(6) 0.0000(7) C(11) 0.0091(8) 0.0126(9) 0.0197(7) 0.0009(6) 0.0008(6) 0.0004(6) C(10) 0.0087(8) 0.0151(11) 0.0195(8) 0.0014(8) 0.0011(6) -0.0004(8) C(25) 0.0127(17) 0.0129(12) 0.0209(7) 0.0011(11) -0.0011(8) -0.0004(8) C(26) 0.0344(114) 0.0149(15) 0.0224(10) -0.0049(39) -0.0023(11) -0.0009(11) C(27) 0.0146(21) 0.0361(119) 0.0200(7) -0.0025(27) 0.0002(9) -0.0024(12) C(28) 0.0254(70) 0.0224(53) 0.0215(8) 0.0117(63) -0.0033(14) -0.0013(12) C(1') 0.0097(8) 0.0129(8) 0.0199(6) -0.0012(7) 0.0037(5) 0.0013(6) C(2') 0.0105(8) 0.0132(13) 0.0211(8) -0.0021(9) 0.0050(6) 0.0012(8) C(3') 0.0119(10) 0.0144(14) 0.0210(9) -0.0023(9) 0.0058(7) 0.0010(9) C(4') 0.0123(11) 0.0154(11) 0.0198(8) -0.0017(8) 0.0049(7) 0.0006(7) C(5') 0.0112(9) 0.0158(11) 0.0191(7) -0.0009(7) 0.0035(6) 0.0004(7) C(6') 0.0098(8) 0.0147(10) 0.0191(7) -0.0006(6) 0.0030(6) 0.0007(6) C(7') 0.0091(7) 0.0164(12) 0.0190(7) 0.0002(8) 0.0020(6) -0.0001(7) C(17') 0.0145(16) 0.0172(14) 0.0197(9) -0.0018(11) 0.0054(8) 0.0001(9) C(18') 0.0322(108) 0.0231(32) 0.0201(11) -0.0123(57) 0.0072(17) -0.0023(12) C(19') 0.0158(19) 0.0374(112) 0.0257(27) -0.0032(15) 0.0077(10) -0.0095(54) C(20') 0.0358(97) 0.0224(24) 0.0212(13) 0.0066(44) -0.0014(34) -0.0021(16) C(16') 0.0092(8) 0.0113(7) 0.0205(7) 0.0002(7) 0.0010(6) 0.0010(6) C(15') 0.0097(9) 0.0109(10) 0.0220(9) -0.0004(9) 0.0006(7) 0.0007(8) C(14') 0.0104(11) 0.0113(11) 0.0222(9) 0.0000(9) -0.0004(8) 0.0003(9) C(13') 0.0108(12) 0.0120(9) 0.0208(7) 0.0007(8) -0.0004(7) 0.0001(7) C(12') 0.0100(10) 0.0129(11) 0.0198(7) 0.0009(8) 0.0005(6) 0.0001(7) C(11') 0.0091(8) 0.0127(9) 0.0197(7) 0.0009(7) 0.0008(6) 0.0004(6) C(10') 0.0085(8) 0.0147(11) 0.0194(7) 0.0010(8) 0.0012(6) -0.0003(7) C(25') 0.0128(18) 0.0129(13) 0.0210(7) 0.0011(11) -0.0012(9) -0.0003(9) C(26') 0.0180(58) 0.0170(52) 0.0217(8) 0.0053(55) -0.0028(14) -0.0007(13) C(27') 0.0146(23) 0.0221(96) 0.0199(7) -0.0009(30) -0.0001(9) -0.0010(10) C(28') 0.0221(99) 0.0138(16) 0.0226(10) -0.0013(36) -0.0026(12) -0.0009(11) O(1') 0.0093(8) 0.0122(8) 0.0200(6) -0.0008(7) 0.0030(5) 0.0015(6) O(2') 0.0092(8) 0.0114(8) 0.0203(6) -0.0001(7) 0.0016(6) 0.0013(6) N' 0.0073(12) 0.0120(8) 0.0193(7) -0.0012(8) 0.0025(8) 0.0008(6) N(1') 0.0083(7) 0.0160(11) 0.0191(7) 0.0004(7) 0.0018(5) -0.0002(7) C(8') 0.0081(7) 0.0195(13) 0.0199(9) 0.0012(9) 0.0012(6) -0.0018(9) C(21') 0.0078(8) 0.0239(21) 0.0211(13) 0.0004(12) 0.0014(8) -0.0038(13) C(22') 0.0076(8) 0.0290(31) 0.0231(18) 0.0012(14) 0.0011(8) -0.0061(18) N(2') 0.0079(7) 0.0151(10) 0.0192(7) 0.0006(7) 0.0016(5) -0.0002(7) C(9') 0.0075(8) 0.0185(12) 0.0197(9) 0.0003(9) 0.0019(6) -0.0017(9) C(24') 0.0077(8) 0.0232(20) 0.0212(13) 0.0010(12) 0.0019(8) -0.0038(13) C(23') 0.0074(9) 0.0282(30) 0.0230(18) -0.0001(14) 0.0025(9) -0.0060(18) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br(1) C(2) 1.899(32) Br(2) C(15) 1.893(33) Br(1') C(2') 1.917(31) Br(2') C(15') 1.944(33) Mn O(1) 1.951(20) Mn' O(1') 1.868(20) Mn O(2) 1.925(20) Mn' O(2') 1.918(19) Mn N 1.505(18) Mn' N' 1.510(18) Mn N(1) 1.963(19) Mn' N(1') 1.975(19) Mn N(2) 1.975(24) Mn' N(2') 1.957(24) O(1) C(1) 1.254(30) O(2) C(16) 1.345(34) N(1) C(7) 1.284(25) N(1) C(8) 1.470(25) C(8) C(9) 1.520(26) C(8) C(21) 1.472(30) C(21) C(22) 1.570(30) C(22) C(23) 1.554(27) N(2) C(10) 1.292(30) N(2) C(9) 1.515(28) C(9) C(24) 1.535(34) C(24) C(23) 1.535(36) C(1) C(6) 1.405(41) C(1) C(2) 1.439(41) C(2) C(3) 1.472(38) C(3) C(4) 1.331(46) C(4) C(5) 1.401(42) C(4) C(17) 1.620(39) C(5) C(6) 1.387(39) C(6) C(7) 1.487(39) C(17) C(18) 1.626(43) C(17) C(19) 1.473(45) C(17) C(20) 1.529(37) C(16) C(11) 1.394(45) C(16) C(15) 1.495(44) C(15) C(14) 1.269(35) C(14) C(13) 1.381(41) C(13) C(12) 1.361(43) C(13) C(25) 1.505(39) C(12) C(11) 1.390(44) C(11) C(10) 1.536(40) C(25) C(26) 1.534(41) C(25) C(27) 1.568(38) C(25) C(28) 1.486(41) C(1') O(1') 1.328(30) C(1') C(6') 1.473(43) C(1') C(2') 1.391(40) C(2') C(3') 1.296(36) C(3') C(4') 1.468(46) C(4') C(5') 1.365(42) C(4') C(17') 1.448(38) C(5') C(6') 1.415(40) C(6') C(7') 1.411(38) C(7') N(1') 1.249(25) C(17') C(18') 1.551(37) C(17') C(19') 1.537(45) C(17') C(20') 1.439(41) C(16') O(2') 1.268(33) C(16') C(11') 1.453(45) C(16') C(15') 1.376(44) C(15') C(14') 1.416(36) C(14') C(13') 1.388(41) C(13') C(12') 1.375(44) C(13') C(25') 1.563(39) C(12') C(11') 1.450(44) C(11') C(10') 1.335(41) C(10') N(2') 1.295(30) C(25') C(26') 1.528(41) C(25') C(27') 1.484(38) C(25') C(28') 1.558(41) N(1') C(8') 1.483(24) C(8') C(9') 1.474(25) C(8') C(21') 1.552(31) C(21') C(22') 1.503(29) C(22') C(23') 1.453(26) N(2') C(9') 1.483(29) C(9') C(24') 1.568(36) C(24') C(23') 1.470(35) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O(1) Mn O(2) 79.6(8) O(1) Mn N 109.3(9) O(1) Mn N(1) 92.1(8) O(1) Mn N(2) 147.4(8) O(2) Mn N 103.0(8) O(2) Mn N(1) 154.0(7) O(2) Mn N(2) 92.1(8) N Mn N(1) 103.0(8) N Mn N(2) 103.3(9) N(1) Mn N(2) 81.7(9) O(1') Mn' O(2') 87.1(9) O(1') Mn' N' 105.3(9) O(1') Mn' N(1') 88.9(8) O(1') Mn' N(2') 155.4(8) O(2') Mn' N' 113.2(8) O(2') Mn' N(1') 142.7(7) O(2') Mn' N(2') 87.3(9) N' Mn' N(1') 103.7(8) N' Mn' N(2') 99.0(9) N(1') Mn' N(2') 81.2(9) Mn O(1) C(1) 122.3(19) Mn O(2) C(16) 117.1(18) Mn N(1) C(7) 128.2(16) Mn N(1) C(8) 110.0(13) C(8) N(1) C(7) 121.7(18) N(1) C(8) C(9) 105.7(15) N(1) C(8) C(21) 116.7(18) C(21) C(8) C(9) 110.4(17) C(8) C(21) C(22) 111.1(18) C(21) C(22) C(23) 109.6(17) Mn N(2) C(9) 114.2(14) Mn N(2) C(10) 124.2(19) C(9) N(2) C(10) 121.5(21) C(8) C(9) N(2) 102.9(15) N(2) C(9) C(24) 111.1(19) C(8) C(9) C(24) 113.0(17) C(9) C(24) C(23) 104.8(19) C(22) C(23) C(24) 112.5(18) O(1) C(1) C(6) 132.4(29) O(1) C(1) C(2) 116.7(28) C(2) C(1) C(6) 110.9(25) C(1) C(2) C(3) 120.5(29) Br(1) C(2) C(1) 118.6(19) Br(1) C(2) C(3) 120.4(23) C(2) C(3) C(4) 121.8(31) C(3) C(4) C(5) 119.9(28) C(5) C(4) C(17) 121.9(29) C(3) C(4) C(17) 117.9(29) C(4) C(5) C(6) 116.5(30) C(1) C(6) C(5) 129.6(31) C(5) C(6) C(7) 111.4(27) C(1) C(6) C(7) 118.5(25) N(1) C(7) C(6) 123.6(23) C(18) C(17 C(19) 113.9(26) C(18) C(17) C(20) 103.9(25) C(19) C(17) C(20) 108.8(27) C(4) C(17) C(18) 105.1(24) C(4) C(17) C(19) 115.6(27) C(4) C(17) C(20) 108.8(22) O(2) C(16) C(11) 128.8(31) O(2) C(16) C(15) 119.9(30) C(15) C(16) C(11) 111.2(29) C(16) C(15) C(14) 120.3(31) Br(2) C(15) C(16) 114.6(21) Br(2) C(15) C(14) 125.0(25) C(15) C(14) C(13) 129.4(32) C(14) C(13) C(12) 110.9(28) C(12) C(13) C(25) 125.5(29) C(14) C(13) C(25) 123.6(30) C(13) C(12) C(11) 123.9(33) C(16) C(11) C(12) 122.7(32) C(12) C(11) C(10) 117.7(29) C(16) C(11) C(10) 119.0(28) N(2) C(10) C(11) 121.3(25) C(26) C(25) C(27) 105.1(25) C(26) C(25) C(28) 110.2(28) C(27) C(25) C(28) 109.7(25) C(13) C(25) C(26) 110.3(25) C(13) C(25) C(27) 113.4(26) C(13) C(25) C(28) 108.1(25) C(6') C(1') O(1') 116.7(26) C(2') C(1') O(1') 127.5(29) C(2') C(1') C(6') 115.8(24) C(1') C(2') C(3') 127.4(32) Br(1') C(2') C(1') 114.8(20) Br(1') C(2') C(3') 117.6(25) C(2') C(3') C(4') 120.6(31) C(3') C(4') C(5') 111.6(27) C(5') C(4') C(17') 119.7(31) C(3') C(4') C(17') 127.7(29) C(4') C(5') C(6') 130.0(32) C(1') C(6') C(5') 113.3(28) C(5') C(6') C(7') 125.6(29) C(1') C(6') C(7') 120.5(25) C(6') C(7') N(1') 129.7(24) C(18') C(17') C(19') 107.9(26) C(18') C(17') C(20') 111.7(28) C(19') C(17') C(20') 104.5(26) C(4') C(17') C(18') 109.7(23) C(4') C(17') C(19') 110.1(28) C(4') C(17') C(20') 112.9(27) C(11') C(16') O(2') 120.7(31) C(15') C(16') O(2') 123.7(32) C(15') C(16') C(11') 115.5(30) C(16') C(15') C(14') 125.8(30) Br(2') C(15') C(16') 118.5(22) Br(2') C(15') C(14') 115.7(22) C(15') C(14') C(13') 118.4(28) C(14') C(13') C(12') 118.9(28) C(12') C(13') C(25') 122.1(28) C(14') C(13') C(25') 118.5(29) C(13') C(12') C(11') 123.0(32) C(16') C(11') C(12') 117.5(30) C(12') C(11') C(10') 118.9(31) C(16') C(11') C(10') 121.1(30) C(11') C(10') N(2') 127.9(28) C(26') C(25') C(27') 107.1(24) C(26') C(25') C(28') 108.0(27) C(27') C(25') C(28') 111.7(26) C(13') C(25') C(26') 109.4(24) C(13') C(25') C(27') 112.6(26) C(13') C(25') C(28') 108.0(24) Mn' O(1') C(1') 128.4(18) Mn' O(2') C(16') 125.6(19) Mn' N(1') C(7') 122.8(17) Mn' N(1') C(8') 116.4(13) C(7') N(1') C(8') 120.8(18) N(1') C(8') C(9') 105.4(15) N(1') C(8') C(21') 117.5(16) C(21') C(8') C(9') 113.2(17) C(8') C(21') C(22') 106.2(18) C(21') C(22') C(23') 116.3(18) Mn' N(2') C(10') 124.7(20) Mn' N(2') C(9') 110.9(14) C(10') N(2') C(9') 123.6(23) C(8') C(9') N(2') 109.4(16) N(2') C(9') C(24') 118.7(18) C(8') C(9') C(24') 109.5(17) C(9') C(24') C(23') 110.7(20) C(22') C(23') C(24') 112.4(19)