data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Journaux, Yves' _publ_contact_author_email yves.journaux@upmc.fr _publ_section_title ; One dimensional assembly of Mn6 Single Molecule Magnets linked by oligothiophene bridges ; loop_ _publ_author_name Y.Journaux M.Haryono M.Kalisz R.Sibille R.Lescouzec C.Fave ; G.Trippe-Allard ; Y.Li M.Seuleiman H.Rousseliere M.Balkhy # Attachment '- mhp042publi.txt' ######################################################################### data_mhp042 _database_code_depnum_ccdc_archive 'CCDC 759086' #TrackingRef '- mhp042publi.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H43 Mn3 N3 O12 S, C2 H6 O' _chemical_formula_sum 'C38 H49 Mn3 N3 O13 S' _chemical_formula_weight 952.68 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' S S 0.1246 0.1234 '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 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5136(13) _cell_length_b 13.188(2) _cell_length_c 14.988(2) _cell_angle_alpha 100.797(13) _cell_angle_beta 93.295(11) _cell_angle_gamma 110.925(11) _cell_volume 2248.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 207 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40264 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12652 _reflns_number_gt 9212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; A model of disorder was introduced for some carbon atoms of solvent molecules (C34, C35 and C36). Moreover, C35 and C36 were refined isotropically. Because of residual density (another disordered solvent), the fonction SQUEEZE was used : # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 1.000 0.500 147 12 ' ' _platon_squeeze_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^)+(0.0541P)^2^+0.0493P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12652 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.04763(2) 0.59530(2) 0.095638(17) 0.01432(7) Uani 1 1 d . . . Mn2 Mn 0.27771(2) 0.55311(2) 0.170651(18) 0.01771(7) Uani 1 1 d . C . Mn3 Mn 0.02361(2) 0.35581(2) 0.145095(19) 0.01697(7) Uani 1 1 d . . . S1 S 0.03424(6) 0.84511(5) 0.46412(4) 0.03833(14) Uani 1 1 d . . . O1 O 0.11512(10) 0.50491(9) 0.14274(8) 0.0162(2) Uani 1 1 d . . . O2 O 0.15651(10) 0.32140(10) 0.17675(9) 0.0229(3) Uani 1 1 d . C . O3 O -0.07429(11) 0.20868(10) 0.14198(9) 0.0245(3) Uani 1 1 d . . . O4 O -0.09853(10) 0.46607(9) 0.05317(8) 0.0165(2) Uani 1 1 d . . . O5 O -0.00484(10) 0.68347(9) 0.02945(8) 0.0180(3) Uani 1 1 d . . . O6 O 0.29885(10) 0.68923(10) 0.13068(9) 0.0221(3) Uani 1 1 d . . . O7 O 0.43990(10) 0.59616(11) 0.19422(9) 0.0248(3) Uani 1 1 d . . . O8 O -0.01593(11) 0.65737(11) 0.21552(9) 0.0254(3) Uani 1 1 d . . . O9 O 0.05825(13) 0.64227(11) 0.35099(9) 0.0336(3) Uani 1 1 d . . . O10 O 0.27629(12) 0.44640(11) 0.03173(9) 0.0280(3) Uani 1 1 d . . . H10A H 0.3209 0.4184 0.0059 0.042 Uiso 1 1 d R . . H10B H 0.2207 0.4342 -0.0101 0.042 Uiso 1 1 d R . . O11 O 0.27107(13) 0.63682(12) 0.31723(10) 0.0352(3) Uani 1 1 d . . . H110 H 0.1992 0.6341 0.3286 0.053 Uiso 1 1 d R C . O12 O 0.00379(13) 0.41743(11) 0.29062(9) 0.0295(3) Uani 1 1 d . B . H120 H 0.0205 0.4858 0.3079 0.044 Uiso 1 1 d R . . N1 N 0.25827(12) 0.41087(12) 0.21343(10) 0.0200(3) Uani 1 1 d . . . N2 N -0.11641(12) 0.38583(11) 0.10698(9) 0.0158(3) Uani 1 1 d . . . N3 N 0.20392(12) 0.71941(12) 0.12521(10) 0.0180(3) Uani 1 1 d . . . C1 C -0.17310(16) 0.18549(15) 0.17855(13) 0.0234(4) Uani 1 1 d . . . C2 C -0.20763(19) 0.09396(17) 0.22141(15) 0.0348(5) Uani 1 1 d . . . H2 H -0.1631 0.0505 0.2212 0.042 Uiso 1 1 calc R . . C3 C -0.3066(2) 0.0680(2) 0.26371(18) 0.0451(6) Uani 1 1 d . . . H3 H -0.3270 0.0082 0.2922 0.054 Uiso 1 1 calc R . . C4 C -0.3758(2) 0.1305(2) 0.26393(17) 0.0418(6) Uani 1 1 d . . . H4 H -0.4411 0.1138 0.2936 0.050 Uiso 1 1 calc R . . C5 C -0.34595(17) 0.21845(18) 0.21914(15) 0.0342(5) Uani 1 1 d . . . H5 H -0.3932 0.2591 0.2182 0.041 Uiso 1 1 calc R . . C6 C -0.24583(16) 0.24732(15) 0.17522(13) 0.0236(4) Uani 1 1 d . . . C7 C -0.22121(15) 0.33801(15) 0.12467(12) 0.0195(4) Uani 1 1 d . . . C8 C -0.31675(16) 0.37475(16) 0.09562(14) 0.0268(4) Uani 1 1 d . . . H8A H -0.3909 0.3149 0.0918 0.032 Uiso 1 1 calc R . . H8B H -0.3086 0.3908 0.0353 0.032 Uiso 1 1 calc R . . C9 C -0.3132(2) 0.4791(2) 0.16405(16) 0.0415(5) Uani 1 1 d . . . H9A H -0.3188 0.4640 0.2242 0.062 Uiso 1 1 calc R . . H9B H -0.3767 0.4986 0.1457 0.062 Uiso 1 1 calc R . . H9C H -0.2418 0.5397 0.1649 0.062 Uiso 1 1 calc R . . C10 C 0.02053(15) 0.79298(14) 0.06775(12) 0.0182(3) Uani 1 1 d . . . C11 C -0.06317(16) 0.83709(15) 0.04952(13) 0.0238(4) Uani 1 1 d . . . H11 H -0.1324 0.7912 0.0128 0.029 Uiso 1 1 calc R . . C12 C -0.04431(18) 0.94850(16) 0.08549(14) 0.0286(4) Uani 1 1 d . . . H12 H -0.1006 0.9764 0.0726 0.034 Uiso 1 1 calc R . . C13 C 0.05900(18) 1.01797(16) 0.14080(15) 0.0310(5) Uani 1 1 d . . . H13 H 0.0710 1.0917 0.1666 0.037 Uiso 1 1 calc R . . C14 C 0.14358(17) 0.97633(15) 0.15696(14) 0.0284(4) Uani 1 1 d . . . H14 H 0.2129 1.0238 0.1927 0.034 Uiso 1 1 calc R . . C15 C 0.12836(15) 0.86344(14) 0.12083(13) 0.0208(4) Uani 1 1 d . . . C16 C 0.22492(15) 0.82577(14) 0.13616(13) 0.0206(4) Uani 1 1 d . . . C17 C 0.34926(16) 0.90813(15) 0.15658(15) 0.0294(5) Uani 1 1 d . . . H17A H 0.3524 0.9785 0.1929 0.035 Uiso 1 1 calc R . . H17B H 0.3951 0.8799 0.1920 0.035 Uiso 1 1 calc R . . C18 C 0.3993(2) 0.9266(2) 0.0685(2) 0.0539(7) Uani 1 1 d . . . H18A H 0.4032 0.8586 0.0354 0.081 Uiso 1 1 calc R . . H18B H 0.4754 0.9835 0.0828 0.081 Uiso 1 1 calc R . . H18C H 0.3508 0.9495 0.0315 0.081 Uiso 1 1 calc R . . C19 C 0.49396(15) 0.57895(16) 0.26692(13) 0.0231(4) Uani 1 1 d . C . C20 C 0.60255(17) 0.65962(18) 0.30828(15) 0.0329(5) Uani 1 1 d . . . H20 H 0.6324 0.7246 0.2869 0.039 Uiso 1 1 calc R . . C21 C 0.66555(19) 0.6444(2) 0.37965(15) 0.0408(6) Uani 1 1 d . . . H21 H 0.7373 0.6987 0.4053 0.049 Uiso 1 1 calc R . . C22 C 0.62194(19) 0.5476(2) 0.41368(16) 0.0432(6) Uani 1 1 d . . . H22 H 0.6641 0.5375 0.4621 0.052 Uiso 1 1 calc R . . C23 C 0.51482(18) 0.4670(2) 0.37415(15) 0.0357(5) Uani 1 1 d . C . H23 H 0.4863 0.4027 0.3966 0.043 Uiso 1 1 calc R . . C24 C 0.44783(16) 0.47970(17) 0.30092(13) 0.0262(4) Uani 1 1 d . . . C25 C 0.33554(16) 0.38891(15) 0.26060(13) 0.0229(4) Uani 1 1 d . C . C26 C 0.30949(18) 0.27071(17) 0.27228(15) 0.0329(5) Uani 1 1 d . . . H26A H 0.3818 0.2621 0.2869 0.039 Uiso 1 1 calc R C . H26B H 0.2713 0.2192 0.2145 0.039 Uiso 1 1 calc R . . C27 C 0.2340(3) 0.2396(2) 0.34657(18) 0.0555(7) Uani 1 1 d . C . H27A H 0.2741 0.2857 0.4051 0.083 Uiso 1 1 calc R . . H27B H 0.2169 0.1629 0.3475 0.083 Uiso 1 1 calc R . . H27C H 0.1633 0.2506 0.3340 0.083 Uiso 1 1 calc R . . C28 C 0.01341(16) 0.68847(15) 0.30134(13) 0.0231(4) Uani 1 1 d . . . C29 C -0.00660(17) 0.79058(15) 0.34694(12) 0.0247(4) Uani 1 1 d . . . C30 C -0.0502(2) 0.85460(17) 0.30757(14) 0.0350(5) Uani 1 1 d . . . H30 H -0.0767 0.8384 0.2453 0.042 Uiso 1 1 calc R . . C31 C -0.0514(2) 0.94905(19) 0.37096(15) 0.0430(6) Uani 1 1 d . . . H31 H -0.0795 1.0003 0.3544 0.052 Uiso 1 1 calc R . . C32 C -0.0069(2) 0.95692(16) 0.45878(13) 0.0306(5) Uani 1 1 d . . . C33 C -0.0051(2) 0.37104(19) 0.37072(14) 0.0388(5) Uani 1 1 d . . . H33A H 0.0654 0.4101 0.4135 0.047 Uiso 0.65 1 calc PR A 1 H33B H -0.0151 0.2932 0.3534 0.047 Uiso 0.65 1 calc PR A 1 H33C H -0.0119 0.2942 0.3522 0.047 Uiso 0.35 1 d PR A 2 H33D H -0.0751 0.3710 0.3953 0.047 Uiso 0.35 1 d PR A 2 C34A C -0.1070(4) 0.3814(4) 0.4163(3) 0.0576(12) Uani 0.65 1 d P B 1 H34A H -0.1017 0.4572 0.4265 0.086 Uiso 0.65 1 calc PR B 1 H34B H -0.1063 0.3597 0.4739 0.086 Uiso 0.65 1 calc PR B 1 H34C H -0.1775 0.3339 0.3773 0.086 Uiso 0.65 1 calc PR B 1 C34B C 0.0980(7) 0.4327(6) 0.4459(5) 0.054(2) Uani 0.35 1 d P B 2 H34D H 0.1684 0.4432 0.4197 0.081 Uiso 0.35 1 calc PR B 2 H34E H 0.0939 0.3898 0.4916 0.081 Uiso 0.35 1 calc PR B 2 H34F H 0.0966 0.5039 0.4736 0.081 Uiso 0.35 1 calc PR B 2 C35A C 0.3553(7) 0.7575(7) 0.3555(5) 0.0473(19) Uiso 0.40 1 d P C 4 H35A H 0.3205 0.8097 0.3442 0.057 Uiso 0.40 1 calc PR C 4 H35B H 0.4257 0.7726 0.3275 0.057 Uiso 0.40 1 calc PR C 4 C36A C 0.3811(10) 0.7671(9) 0.4615(8) 0.097(3) Uiso 0.40 1 d P C 4 H36A H 0.3118 0.7259 0.4835 0.146 Uiso 0.40 1 calc PR C 4 H36B H 0.4083 0.8440 0.4930 0.146 Uiso 0.40 1 calc PR C 4 H36C H 0.4391 0.7374 0.4725 0.146 Uiso 0.40 1 calc PR C 4 C35B C 0.3488(5) 0.7320(5) 0.3757(4) 0.0510(14) Uiso 0.60 1 d P C 5 H35C H 0.3132 0.7865 0.3888 0.061 Uiso 0.60 1 calc PR C 5 H35D H 0.4156 0.7633 0.3455 0.061 Uiso 0.60 1 calc PR C 5 C36B C 0.3893(7) 0.7092(6) 0.4675(5) 0.100(2) Uiso 0.60 1 d P C 5 H36D H 0.3233 0.6746 0.4961 0.150 Uiso 0.60 1 calc PR C 5 H36E H 0.4386 0.7783 0.5075 0.150 Uiso 0.60 1 calc PR C 5 H36F H 0.4311 0.6607 0.4554 0.150 Uiso 0.60 1 calc PR C 5 O13 O 0.43110(14) 0.35608(14) -0.04270(12) 0.0476(4) Uani 1 1 d . . . H130 H 0.4708 0.3786 -0.0844 0.071 Uiso 1 1 d R . . C37 C 0.3863(2) 0.2367(2) -0.0682(2) 0.0593(8) Uani 1 1 d . . . H37A H 0.4434 0.2116 -0.0957 0.071 Uiso 1 1 calc R . . H37B H 0.3177 0.2103 -0.1130 0.071 Uiso 1 1 calc R . . C38 C 0.3570(2) 0.1906(3) 0.0154(3) 0.0827(12) Uani 1 1 d . . . H38A H 0.4258 0.2144 0.0584 0.124 Uiso 1 1 calc R . . H38B H 0.3247 0.1107 -0.0019 0.124 Uiso 1 1 calc R . . H38C H 0.3019 0.2171 0.0431 0.124 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 0.01612(13) 0.01069(12) 0.01545(13) -0.00026(10) 0.00063(10) 0.00603(10) Mn2 0.01626(13) 0.01600(13) 0.02141(15) 0.00252(11) 0.00066(11) 0.00780(10) Mn3 0.01732(13) 0.01292(13) 0.02126(14) 0.00313(10) 0.00169(11) 0.00684(10) S1 0.0723(4) 0.0334(3) 0.0188(2) -0.0043(2) -0.0018(3) 0.0374(3) O1 0.0163(6) 0.0120(5) 0.0201(6) 0.0014(5) 0.0013(5) 0.0063(5) O2 0.0213(6) 0.0161(6) 0.0304(7) 0.0023(5) -0.0033(5) 0.0083(5) O3 0.0264(7) 0.0142(6) 0.0331(8) 0.0058(5) 0.0052(6) 0.0075(5) O4 0.0200(6) 0.0141(6) 0.0159(6) 0.0031(5) 0.0011(5) 0.0075(5) O5 0.0228(6) 0.0119(5) 0.0186(6) -0.0009(5) -0.0007(5) 0.0083(5) O6 0.0165(6) 0.0196(6) 0.0327(7) 0.0057(6) 0.0034(5) 0.0098(5) O7 0.0174(6) 0.0270(7) 0.0315(8) 0.0089(6) 0.0016(5) 0.0093(5) O8 0.0323(7) 0.0240(7) 0.0191(7) -0.0039(5) 0.0057(6) 0.0136(6) O9 0.0533(9) 0.0290(7) 0.0247(7) -0.0006(6) 0.0035(7) 0.0263(7) O10 0.0305(7) 0.0328(7) 0.0233(7) -0.0004(6) 0.0021(6) 0.0186(6) O11 0.0333(8) 0.0384(8) 0.0284(8) -0.0069(7) 0.0003(6) 0.0147(7) O12 0.0478(9) 0.0221(7) 0.0202(7) 0.0036(6) 0.0075(6) 0.0150(6) N1 0.0193(7) 0.0189(7) 0.0219(8) 0.0015(6) 0.0017(6) 0.0090(6) N2 0.0207(7) 0.0121(6) 0.0130(7) 0.0014(5) 0.0019(6) 0.0050(6) N3 0.0168(7) 0.0166(7) 0.0207(8) 0.0018(6) 0.0003(6) 0.0080(6) C1 0.0236(9) 0.0190(9) 0.0229(10) 0.0026(8) 0.0000(8) 0.0039(7) C2 0.0396(12) 0.0272(11) 0.0386(13) 0.0143(10) 0.0074(10) 0.0101(9) C3 0.0491(14) 0.0364(12) 0.0497(15) 0.0259(11) 0.0138(12) 0.0067(11) C4 0.0326(11) 0.0444(13) 0.0460(14) 0.0208(11) 0.0144(10) 0.0047(10) C5 0.0260(10) 0.0391(12) 0.0401(13) 0.0162(10) 0.0119(9) 0.0105(9) C6 0.0226(9) 0.0213(9) 0.0231(10) 0.0048(8) 0.0031(8) 0.0037(8) C7 0.0192(8) 0.0209(9) 0.0181(9) 0.0019(7) 0.0034(7) 0.0083(7) C8 0.0193(9) 0.0336(11) 0.0313(11) 0.0124(9) 0.0068(8) 0.0114(8) C9 0.0496(14) 0.0533(14) 0.0389(13) 0.0129(11) 0.0185(11) 0.0364(12) C10 0.0256(9) 0.0132(8) 0.0174(9) 0.0012(7) 0.0043(7) 0.0099(7) C11 0.0268(9) 0.0193(9) 0.0247(10) -0.0011(8) -0.0023(8) 0.0117(8) C12 0.0360(11) 0.0244(10) 0.0314(11) 0.0030(8) -0.0002(9) 0.0209(9) C13 0.0407(12) 0.0153(9) 0.0381(12) -0.0003(8) 0.0000(10) 0.0158(9) C14 0.0298(10) 0.0132(8) 0.0368(12) -0.0019(8) -0.0025(9) 0.0062(8) C15 0.0250(9) 0.0150(8) 0.0232(9) 0.0028(7) 0.0022(7) 0.0093(7) C16 0.0215(9) 0.0162(8) 0.0208(9) -0.0001(7) 0.0007(7) 0.0056(7) C17 0.0217(9) 0.0172(9) 0.0446(13) 0.0016(9) -0.0005(9) 0.0051(8) C18 0.0378(13) 0.0533(16) 0.0651(18) 0.0245(14) 0.0157(13) 0.0036(12) C19 0.0203(9) 0.0282(10) 0.0218(9) -0.0003(8) 0.0012(7) 0.0134(8) C20 0.0243(10) 0.0344(11) 0.0350(12) 0.0012(9) 0.0008(9) 0.0089(9) C21 0.0273(11) 0.0501(14) 0.0317(12) -0.0048(11) -0.0064(9) 0.0072(10) C22 0.0328(12) 0.0615(16) 0.0293(12) 0.0079(11) -0.0089(10) 0.0137(11) C23 0.0320(11) 0.0461(13) 0.0302(11) 0.0119(10) -0.0002(9) 0.0151(10) C24 0.0236(9) 0.0339(11) 0.0218(10) 0.0032(8) 0.0012(8) 0.0134(8) C25 0.0248(9) 0.0251(9) 0.0212(9) 0.0051(8) 0.0002(8) 0.0126(8) C26 0.0348(11) 0.0289(11) 0.0370(12) 0.0110(9) -0.0064(9) 0.0143(9) C27 0.0747(19) 0.0401(14) 0.0427(15) 0.0163(12) 0.0059(14) 0.0078(13) C28 0.0274(9) 0.0180(9) 0.0222(10) -0.0019(7) 0.0066(8) 0.0093(8) C29 0.0363(11) 0.0229(9) 0.0160(9) -0.0023(7) 0.0065(8) 0.0152(8) C30 0.0615(14) 0.0355(11) 0.0153(9) -0.0020(8) 0.0017(9) 0.0310(11) C31 0.0836(18) 0.0402(12) 0.0227(11) 0.0018(9) 0.0036(11) 0.0472(13) C32 0.0521(13) 0.0257(10) 0.0202(10) -0.0017(8) 0.0043(9) 0.0252(10) C33 0.0565(14) 0.0338(12) 0.0230(11) 0.0063(9) 0.0024(10) 0.0138(11) C34A 0.058(3) 0.069(3) 0.0261(19) 0.0049(19) 0.0167(18) 0.002(2) C34B 0.077(5) 0.040(4) 0.038(4) 0.008(3) -0.006(4) 0.016(4) O13 0.0504(10) 0.0485(10) 0.0598(11) 0.0230(9) 0.0269(9) 0.0291(8) C37 0.0506(16) 0.0526(16) 0.082(2) 0.0210(16) 0.0222(15) 0.0227(14) C38 0.0389(15) 0.093(2) 0.131(3) 0.077(2) 0.0084(18) 0.0175(16) _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 O1 1.8970(12) . ? Mn1 O5 1.9156(12) . ? Mn1 O4 1.9718(12) . ? Mn1 N3 2.0106(15) . ? Mn1 O8 2.1470(13) . ? Mn1 O4 2.4271(13) 2_565 ? Mn2 O7 1.8936(12) . ? Mn2 O1 1.8967(12) . ? Mn2 O6 1.9322(13) . ? Mn2 N1 2.0327(15) . ? Mn2 O10 2.2795(14) . ? Mn2 O11 2.2869(15) . ? Mn3 O3 1.8787(13) . ? Mn3 O1 1.8977(12) . ? Mn3 O2 1.9302(12) . ? Mn3 N2 2.0045(15) . ? Mn3 O12 2.2409(14) . ? S1 C29 1.7390(19) . ? S1 C32 1.740(2) . ? O2 N1 1.3854(19) . ? O3 C1 1.339(2) . ? O4 N2 1.4112(17) . ? O4 Mn1 2.4271(13) 2_565 ? O5 C10 1.363(2) . ? O6 N3 1.3838(18) . ? O7 C19 1.347(2) . ? O8 C28 1.264(2) . ? O9 C28 1.267(2) . ? O10 H10A 0.8467 . ? O10 H10B 0.8568 . ? O11 C35B 1.381(6) . ? O11 C35A 1.538(8) . ? O11 H110 0.9144 . ? O12 C33 1.439(2) . ? O12 H120 0.8337 . ? N1 C25 1.310(2) . ? N2 C7 1.304(2) . ? N3 C16 1.307(2) . ? C1 C2 1.416(3) . ? C1 C6 1.427(3) . ? C2 C3 1.386(3) . ? C2 H2 0.9300 . ? C3 C4 1.392(3) . ? C3 H3 0.9300 . ? C4 C5 1.396(3) . ? C4 H4 0.9300 . ? C5 C6 1.413(3) . ? C5 H5 0.9300 . ? C6 C7 1.484(3) . ? C7 C8 1.512(2) . ? C8 C9 1.539(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.404(2) . ? C10 C15 1.422(2) . ? C11 C12 1.395(3) . ? C11 H11 0.9300 . ? C12 C13 1.394(3) . ? C12 H12 0.9300 . ? C13 C14 1.384(3) . ? C13 H13 0.9300 . ? C14 C15 1.425(2) . ? C14 H14 0.9300 . ? C15 C16 1.483(2) . ? C16 C17 1.519(2) . ? C17 C18 1.517(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.409(3) . ? C19 C24 1.432(3) . ? C20 C21 1.379(3) . ? C20 H20 0.9300 . ? C21 C22 1.402(3) . ? C21 H21 0.9300 . ? C22 C23 1.390(3) . ? C22 H22 0.9300 . ? C23 C24 1.414(3) . ? C23 H23 0.9300 . ? C24 C25 1.484(3) . ? C25 C26 1.521(3) . ? C26 C27 1.522(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.503(2) . ? C29 C30 1.355(3) . ? C30 C31 1.423(3) . ? C30 H30 0.9300 . ? C31 C32 1.370(3) . ? C31 H31 0.9300 . ? C32 C32 1.468(4) 2_576 ? C33 C34A 1.517(5) . ? C33 C34B 1.528(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C33 H33D 0.9700 . ? C34A H33D 0.5609 . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C34B H34D 0.9600 . ? C34B H34E 0.9600 . ? C34B H34F 0.9600 . ? C35A C36A 1.575(13) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C35B C36B 1.556(9) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36B H36D 0.9600 . ? C36B H36E 0.9600 . ? C36B H36F 0.9600 . ? O13 C37 1.434(3) . ? O13 H130 0.8525 . ? C37 C38 1.501(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O5 169.37(5) . . ? O1 Mn1 O4 90.59(5) . . ? O5 Mn1 O4 91.45(5) . . ? O1 Mn1 N3 87.98(5) . . ? O5 Mn1 N3 88.71(6) . . ? O4 Mn1 N3 172.92(6) . . ? O1 Mn1 O8 100.27(5) . . ? O5 Mn1 O8 90.04(5) . . ? O4 Mn1 O8 92.74(5) . . ? N3 Mn1 O8 94.34(6) . . ? O1 Mn1 O4 88.32(5) . 2_565 ? O5 Mn1 O4 81.51(5) . 2_565 ? O4 Mn1 O4 84.32(5) . 2_565 ? N3 Mn1 O4 88.70(5) . 2_565 ? O8 Mn1 O4 170.96(5) . 2_565 ? O7 Mn2 O1 177.48(5) . . ? O7 Mn2 O6 90.02(5) . . ? O1 Mn2 O6 90.91(5) . . ? O7 Mn2 N1 89.06(6) . . ? O1 Mn2 N1 90.01(5) . . ? O6 Mn2 N1 179.07(6) . . ? O7 Mn2 O10 89.86(6) . . ? O1 Mn2 O10 87.71(5) . . ? O6 Mn2 O10 97.38(5) . . ? N1 Mn2 O10 82.76(6) . . ? O7 Mn2 O11 91.46(6) . . ? O1 Mn2 O11 90.86(5) . . ? O6 Mn2 O11 90.76(6) . . ? N1 Mn2 O11 89.12(6) . . ? O10 Mn2 O11 171.75(5) . . ? O3 Mn3 O1 176.29(5) . . ? O3 Mn3 O2 90.29(6) . . ? O1 Mn3 O2 93.01(5) . . ? O3 Mn3 N2 88.25(6) . . ? O1 Mn3 N2 88.38(5) . . ? O2 Mn3 N2 177.33(6) . . ? O3 Mn3 O12 93.24(6) . . ? O1 Mn3 O12 88.16(5) . . ? O2 Mn3 O12 94.74(6) . . ? N2 Mn3 O12 87.57(6) . . ? C29 S1 C32 91.89(9) . . ? Mn2 O1 Mn1 120.70(6) . . ? Mn2 O1 Mn3 118.24(6) . . ? Mn1 O1 Mn3 120.37(6) . . ? N1 O2 Mn3 116.75(9) . . ? C1 O3 Mn3 121.75(11) . . ? N2 O4 Mn1 112.83(9) . . ? N2 O4 Mn1 112.07(8) . 2_565 ? Mn1 O4 Mn1 95.68(5) . 2_565 ? C10 O5 Mn1 119.65(10) . . ? N3 O6 Mn2 116.81(10) . . ? C19 O7 Mn2 123.69(12) . . ? C28 O8 Mn1 139.04(12) . . ? Mn2 O10 H10A 137.2 . . ? Mn2 O10 H10B 116.8 . . ? H10A O10 H10B 105.7 . . ? C35B O11 Mn2 130.9(3) . . ? C35A O11 Mn2 118.1(3) . . ? C35B O11 H110 106.2 . . ? C35A O11 H110 106.9 . . ? Mn2 O11 H110 114.2 . . ? C33 O12 Mn3 133.65(12) . . ? C33 O12 H120 107.9 . . ? Mn3 O12 H120 116.5 . . ? C25 N1 O2 115.94(14) . . ? C25 N1 Mn2 128.04(13) . . ? O2 N1 Mn2 115.28(10) . . ? C7 N2 O4 117.19(14) . . ? C7 N2 Mn3 127.30(12) . . ? O4 N2 Mn3 115.49(10) . . ? C16 N3 O6 116.68(14) . . ? C16 N3 Mn1 126.33(12) . . ? O6 N3 Mn1 116.94(10) . . ? O3 C1 C2 118.17(17) . . ? O3 C1 C6 123.25(16) . . ? C2 C1 C6 118.57(18) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 120.7(2) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.60(18) . . ? C5 C6 C7 119.45(17) . . ? C1 C6 C7 121.93(16) . . ? N2 C7 C6 119.08(16) . . ? N2 C7 C8 120.96(16) . . ? C6 C7 C8 119.95(16) . . ? C7 C8 C9 111.08(16) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O5 C10 C11 117.25(15) . . ? O5 C10 C15 122.86(15) . . ? C11 C10 C15 119.83(15) . . ? C12 C11 C10 121.15(17) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 119.93(17) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 119.44(17) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 122.44(17) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C10 C15 C14 117.13(16) . . ? C10 C15 C16 123.09(15) . . ? C14 C15 C16 119.73(16) . . ? N3 C16 C15 119.70(15) . . ? N3 C16 C17 119.17(16) . . ? C15 C16 C17 120.93(15) . . ? C18 C17 C16 110.78(18) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 C20 118.52(18) . . ? O7 C19 C24 122.51(16) . . ? C20 C19 C24 118.90(18) . . ? C21 C20 C19 121.6(2) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 120.3(2) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.1(2) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 122.1(2) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C23 C24 C19 117.95(18) . . ? C23 C24 C25 119.13(18) . . ? C19 C24 C25 122.88(17) . . ? N1 C25 C24 119.41(17) . . ? N1 C25 C26 119.59(17) . . ? C24 C25 C26 121.00(16) . . ? C25 C26 C27 113.89(19) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O8 C28 O9 126.09(17) . . ? O8 C28 C29 115.79(17) . . ? O9 C28 C29 118.12(16) . . ? C30 C29 C28 128.26(17) . . ? C30 C29 S1 111.09(14) . . ? C28 C29 S1 120.58(14) . . ? C29 C30 C31 113.30(18) . . ? C29 C30 H30 123.4 . . ? C31 C30 H30 123.4 . . ? C32 C31 C30 113.25(19) . . ? C32 C31 H31 123.4 . . ? C30 C31 H31 123.4 . . ? C31 C32 C32 128.5(2) . 2_576 ? C31 C32 S1 110.46(14) . . ? C32 C32 S1 121.0(2) 2_576 . ? O12 C33 C34A 109.9(2) . . ? O12 C33 C34B 113.9(3) . . ? C34A C33 C34B 104.0(4) . . ? O12 C33 H33A 109.7 . . ? C34A C33 H33A 109.7 . . ? O12 C33 H33B 109.7 . . ? C34A C33 H33B 109.7 . . ? C34B C33 H33B 109.5 . . ? H33A C33 H33B 108.2 . . ? O12 C33 H33C 108.3 . . ? C34A C33 H33C 112.2 . . ? C34B C33 H33C 108.6 . . ? H33A C33 H33C 107.0 . . ? O12 C33 H33D 108.9 . . ? C34B C33 H33D 109.3 . . ? H33A C33 H33D 115.0 . . ? H33B C33 H33D 105.2 . . ? H33C C33 H33D 107.7 . . ? C33 C34A H34A 109.5 . . ? H33D C34A H34A 116.2 . . ? C33 C34A H34B 109.5 . . ? H33D C34A H34B 112.0 . . ? C33 C34A H34C 109.5 . . ? H33D C34A H34C 99.7 . . ? C33 C34B H34D 109.5 . . ? C33 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? O11 C35A C36A 105.0(6) . . ? O11 C35A H35A 110.7 . . ? C36A C35A H35A 110.7 . . ? O11 C35A H35B 110.7 . . ? C36A C35A H35B 110.7 . . ? H35A C35A H35B 108.8 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? O11 C35B C36B 112.5(5) . . ? O11 C35B H35C 109.1 . . ? C36B C35B H35C 109.1 . . ? O11 C35B H35D 109.1 . . ? C36B C35B H35D 109.1 . . ? H35C C35B H35D 107.8 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C37 O13 H130 106.2 . . ? O13 C37 C38 109.4(3) . . ? O13 C37 H37A 109.8 . . ? C38 C37 H37A 109.8 . . ? O13 C37 H37B 109.8 . . ? C38 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.626 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.071