# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email stuart.batten@sci.monash.edu.au _publ_contact_author_name 'Stuart Batten' loop_ _publ_author_name 'Anna Kutasi' 'David Turner' 'Boujemaa Moubaraki' 'Stuart Batten' 'Keith Murray' data_1 _database_code_depnum_ccdc_archive 'CCDC 836013' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Mn(bipy)2(HCTMCP)]2.2MeOH ; _chemical_name_common (Mn(bipy)2(HCTMCP))2.2MeOH _chemical_melting_point ? _chemical_formula_moiety 'C64 H32 Mn2 N20, 2(C H4 O)' _chemical_formula_sum 'C66 H40 Mn2 N20 O2' _chemical_formula_weight 1255.06 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2763(1) _cell_length_b 12.7033(2) _cell_length_c 12.8777(3) _cell_angle_alpha 90.936(1) _cell_angle_beta 92.611(1) _cell_angle_gamma 93.876(2) _cell_volume 1512.17(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27280 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9098 _exptl_absorpt_correction_T_max 0.9648 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27280 _diffrn_reflns_av_R_equivalents 0.1104 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6899 _reflns_number_gt 4159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.0940P)^2^+0.0000P] 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 6899 _refine_ls_number_parameters 405 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _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 0.03234(5) 0.77255(4) 0.76677(4) 0.01839(18) Uani 1 1 d . . . N1 N -0.1820(3) 0.7767(2) 0.6745(2) 0.0227(6) Uani 1 1 d . . . N2 N 0.0772(3) 0.8513(2) 0.6168(2) 0.0193(6) Uani 1 1 d . . . C10 C -0.3111(4) 0.7436(3) 0.7096(3) 0.0335(9) Uani 1 1 d . . . H10 H -0.3160 0.7220 0.7797 0.040 Uiso 1 1 calc R . . C11 C -0.4365(4) 0.7399(4) 0.6482(3) 0.0418(10) Uani 1 1 d . . . H11 H -0.5260 0.7153 0.6752 0.050 Uiso 1 1 calc R . . C12 C -0.4304(4) 0.7723(3) 0.5471(3) 0.0400(10) Uani 1 1 d . . . H12 H -0.5162 0.7718 0.5039 0.048 Uiso 1 1 calc R . . C13 C -0.2980(3) 0.8056(3) 0.5088(3) 0.0287(8) Uani 1 1 d . . . H13 H -0.2915 0.8271 0.4388 0.034 Uiso 1 1 calc R . . C14 C -0.1747(3) 0.8071(2) 0.5748(3) 0.0195(7) Uani 1 1 d . . . C15 C -0.0296(3) 0.8457(2) 0.5415(2) 0.0185(7) Uani 1 1 d . . . C16 C -0.0035(4) 0.8748(3) 0.4412(3) 0.0246(8) Uani 1 1 d . . . H16 H -0.0792 0.8686 0.3888 0.029 Uiso 1 1 calc R . . C17 C 0.1340(4) 0.9133(3) 0.4172(3) 0.0264(8) Uani 1 1 d . . . H17 H 0.1532 0.9331 0.3481 0.032 Uiso 1 1 calc R . . C18 C 0.2426(4) 0.9228(3) 0.4939(3) 0.0256(8) Uani 1 1 d . . . H18 H 0.3373 0.9501 0.4795 0.031 Uiso 1 1 calc R . . C19 C 0.2093(3) 0.8911(3) 0.5928(3) 0.0253(8) Uani 1 1 d . . . H19 H 0.2834 0.8979 0.6464 0.030 Uiso 1 1 calc R . . N3 N 0.0564(3) 0.6093(2) 0.6982(2) 0.0200(6) Uani 1 1 d . . . N4 N -0.0559(3) 0.6585(2) 0.8798(2) 0.0188(6) Uani 1 1 d . . . C20 C -0.1128(3) 0.6877(3) 0.9680(3) 0.0241(8) Uani 1 1 d . . . H20 H -0.0993 0.7597 0.9897 0.029 Uiso 1 1 calc R . . C21 C -0.1911(4) 0.6181(3) 1.0302(3) 0.0277(8) Uani 1 1 d . . . H21 H -0.2291 0.6412 1.0932 0.033 Uiso 1 1 calc R . . C22 C -0.2114(4) 0.5144(3) 0.9967(3) 0.0351(9) Uani 1 1 d . . . H22 H -0.2668 0.4650 1.0359 0.042 Uiso 1 1 calc R . . C23 C -0.1513(4) 0.4820(3) 0.9062(3) 0.0312(9) Uani 1 1 d . . . H23 H -0.1643 0.4105 0.8830 0.037 Uiso 1 1 calc R . . C24 C -0.0716(3) 0.5559(3) 0.8498(3) 0.0220(8) Uani 1 1 d . . . C25 C 0.0030(3) 0.5273(3) 0.7543(3) 0.0221(8) Uani 1 1 d . . . C26 C 0.0216(4) 0.4243(3) 0.7250(3) 0.0300(8) Uani 1 1 d . . . H26 H -0.0173 0.3676 0.7646 0.036 Uiso 1 1 calc R . . C27 C 0.0973(4) 0.4044(3) 0.6377(3) 0.0348(9) Uani 1 1 d . . . H27 H 0.1128 0.3340 0.6175 0.042 Uiso 1 1 calc R . . C28 C 0.1497(4) 0.4871(3) 0.5804(3) 0.0350(9) Uani 1 1 d . . . H28 H 0.2004 0.4753 0.5193 0.042 Uiso 1 1 calc R . . C29 C 0.1269(4) 0.5882(3) 0.6140(3) 0.0277(8) Uani 1 1 d . . . H29 H 0.1637 0.6457 0.5745 0.033 Uiso 1 1 calc R . . C101 C 0.5828(3) 0.8826(2) 0.9556(2) 0.0177(7) Uani 1 1 d . . . C110 C 0.4762(3) 0.7993(2) 0.9499(2) 0.0194(7) Uani 1 1 d . . . C111 C 0.3618(3) 0.7918(2) 0.8737(3) 0.0190(7) Uani 1 1 d . . . N112 N 0.2664(3) 0.7819(2) 0.8138(2) 0.0240(6) Uani 1 1 d . . . C113 C 0.4730(3) 0.7220(3) 1.0278(3) 0.0275(8) Uani 1 1 d . . . N114 N 0.4710(3) 0.6577(3) 1.0902(3) 0.0474(10) Uani 1 1 d . . . C102 C 0.6517(3) 0.9740(2) 0.9174(2) 0.0173(7) Uani 1 1 d . . . C120 C 0.6631(3) 1.0498(2) 0.8412(2) 0.0188(7) Uani 1 1 d . . . C121 C 0.5700(3) 1.0430(3) 0.7502(3) 0.0224(8) Uani 1 1 d . . . N122 N 0.4956(3) 1.0356(2) 0.6753(2) 0.0336(8) Uani 1 1 d . . . C123 C 0.7709(4) 1.1346(3) 0.8514(3) 0.0222(7) Uani 1 1 d . . . N124 N 0.8592(3) 1.2036(2) 0.8595(2) 0.0338(8) Uani 1 1 d . . . C103 C 0.6999(3) 0.9332(2) 1.0107(2) 0.0181(7) Uani 1 1 d . . . C130 C 0.7957(3) 0.9365(2) 1.0991(2) 0.0193(7) Uani 1 1 d . . . C131 C 0.7790(3) 0.8584(3) 1.1767(3) 0.0221(7) Uani 1 1 d . . . N132 N 0.7654(3) 0.7956(2) 1.2398(2) 0.0305(7) Uani 1 1 d . . . C133 C 0.9036(3) 1.0176(3) 1.1164(2) 0.0196(7) Uani 1 1 d . . . N134 N 0.9916(3) 1.0853(2) 1.1345(2) 0.0222(6) Uani 1 1 d . . . O2 O 0.5255(7) 0.4875(5) 0.2342(5) 0.080(3) Uiso 0.543(7) 1 d P A 1 C32 C 0.4984(10) 0.5529(7) 0.3225(8) 0.060(3) Uiso 0.543(7) 1 d P A 1 O1 O 0.3652(11) 0.6027(9) 0.3500(8) 0.116(4) Uiso 0.457(7) 1 d PD A 2 C31 C 0.435(2) 0.5189(14) 0.4023(16) 0.157(8) Uiso 0.457(7) 1 d PD A 2 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 0.0194(3) 0.0153(3) 0.0197(3) -0.0004(2) -0.0021(2) -0.00252(19) N1 0.0184(14) 0.0251(16) 0.0241(16) -0.0030(13) -0.0018(12) 0.0019(12) N2 0.0206(14) 0.0173(14) 0.0196(15) 0.0028(12) -0.0031(11) -0.0008(11) C10 0.0250(19) 0.049(3) 0.026(2) 0.0027(18) 0.0053(16) -0.0005(17) C11 0.0179(19) 0.071(3) 0.036(2) -0.004(2) 0.0018(17) -0.0013(18) C12 0.0222(19) 0.059(3) 0.038(2) -0.005(2) -0.0086(17) 0.0033(18) C13 0.0246(19) 0.038(2) 0.023(2) 0.0016(16) -0.0056(15) 0.0042(16) C14 0.0220(17) 0.0159(17) 0.0205(18) -0.0031(14) -0.0027(14) 0.0032(13) C15 0.0234(17) 0.0138(17) 0.0179(18) -0.0025(14) -0.0034(13) 0.0017(13) C16 0.0321(19) 0.0213(18) 0.0197(19) -0.0038(15) -0.0039(15) 0.0012(15) C17 0.039(2) 0.0212(19) 0.0192(19) 0.0024(15) 0.0070(16) 0.0005(15) C18 0.0243(18) 0.0242(19) 0.029(2) 0.0053(16) 0.0061(15) -0.0009(14) C19 0.0240(18) 0.0229(19) 0.028(2) 0.0017(16) -0.0040(15) -0.0034(14) N3 0.0213(14) 0.0171(15) 0.0212(16) -0.0024(12) -0.0027(12) 0.0020(11) N4 0.0232(14) 0.0164(15) 0.0162(15) -0.0021(12) 0.0021(11) -0.0020(11) C20 0.0264(18) 0.0193(18) 0.026(2) -0.0024(15) 0.0001(15) 0.0001(14) C21 0.0277(18) 0.030(2) 0.025(2) -0.0048(16) 0.0081(15) -0.0007(15) C22 0.036(2) 0.035(2) 0.033(2) 0.0034(18) 0.0102(17) -0.0139(17) C23 0.039(2) 0.0204(19) 0.032(2) -0.0054(16) 0.0034(17) -0.0124(16) C24 0.0237(17) 0.0173(18) 0.0241(19) 0.0019(15) -0.0019(14) -0.0036(14) C25 0.0242(17) 0.0169(18) 0.0241(19) -0.0021(15) -0.0049(14) -0.0031(14) C26 0.048(2) 0.0149(18) 0.027(2) -0.0005(15) -0.0013(17) 0.0008(16) C27 0.058(2) 0.020(2) 0.027(2) -0.0092(17) 0.0003(18) 0.0092(17) C28 0.053(2) 0.030(2) 0.023(2) -0.0019(17) 0.0074(18) 0.0129(18) C29 0.034(2) 0.028(2) 0.022(2) -0.0006(16) 0.0031(16) 0.0017(16) C101 0.0197(16) 0.0193(17) 0.0139(17) -0.0015(14) 0.0001(13) 0.0005(13) C110 0.0195(16) 0.0193(17) 0.0187(18) 0.0037(14) -0.0028(13) -0.0018(13) C111 0.0211(17) 0.0145(17) 0.0217(19) 0.0014(14) 0.0071(15) 0.0000(13) N112 0.0194(15) 0.0253(16) 0.0263(17) 0.0007(13) -0.0053(13) -0.0029(12) C113 0.0169(17) 0.031(2) 0.033(2) 0.0030(18) -0.0046(15) -0.0061(14) N114 0.0341(18) 0.054(2) 0.051(2) 0.028(2) -0.0125(16) -0.0158(16) C102 0.0173(16) 0.0165(17) 0.0181(18) -0.0023(14) 0.0011(13) 0.0014(13) C120 0.0218(17) 0.0181(17) 0.0156(17) -0.0027(14) 0.0000(13) -0.0029(13) C121 0.0226(17) 0.0235(19) 0.0208(19) 0.0049(15) 0.0039(15) -0.0025(14) N122 0.0329(17) 0.043(2) 0.0226(18) 0.0081(15) -0.0065(14) -0.0088(14) C123 0.0260(18) 0.0216(19) 0.0191(18) 0.0027(15) 0.0001(14) 0.0028(15) N124 0.0344(17) 0.0250(17) 0.041(2) 0.0059(15) -0.0034(14) -0.0074(14) C103 0.0185(16) 0.0156(17) 0.0198(18) -0.0016(14) 0.0010(13) -0.0007(12) C130 0.0233(17) 0.0182(17) 0.0154(17) -0.0009(14) -0.0029(13) -0.0034(13) C131 0.0216(17) 0.0220(19) 0.0216(19) -0.0061(16) -0.0033(14) -0.0025(14) N132 0.0359(17) 0.0246(17) 0.0297(18) 0.0053(15) -0.0087(14) -0.0018(13) C133 0.0234(17) 0.0190(18) 0.0170(18) -0.0022(14) -0.0005(14) 0.0064(15) N134 0.0255(15) 0.0171(15) 0.0232(16) -0.0056(12) -0.0039(12) -0.0003(12) _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 N4 2.214(3) . ? Mn1 N134 2.220(3) 2_677 ? Mn1 N112 2.222(3) . ? Mn1 N2 2.233(3) . ? Mn1 N3 2.270(3) . ? Mn1 N1 2.273(3) . ? N1 C10 1.343(4) . ? N1 C14 1.349(4) . ? N2 C19 1.344(4) . ? N2 C15 1.353(4) . ? C10 C11 1.374(5) . ? C10 H10 0.9500 . ? C11 C12 1.374(5) . ? C11 H11 0.9500 . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 C14 1.392(4) . ? C13 H13 0.9500 . ? C14 C15 1.486(4) . ? C15 C16 1.377(4) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C19 1.383(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? N3 C29 1.325(4) . ? N3 C25 1.356(4) . ? N4 C20 1.332(4) . ? N4 C24 1.350(4) . ? C20 C21 1.393(5) . ? C20 H20 0.9500 . ? C21 C22 1.377(5) . ? C21 H21 0.9500 . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.390(5) . ? C23 H23 0.9500 . ? C24 C25 1.490(5) . ? C25 C26 1.380(5) . ? C26 C27 1.382(5) . ? C26 H26 0.9500 . ? C27 C28 1.368(5) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C101 C103 1.384(4) . ? C101 C102 1.395(4) . ? C101 C110 1.398(4) . ? C110 C111 1.409(4) . ? C110 C113 1.415(5) . ? C111 N112 1.147(4) . ? C113 N114 1.156(4) . ? C102 C103 1.383(4) . ? C102 C120 1.388(4) . ? C120 C123 1.420(5) . ? C120 C121 1.422(4) . ? C121 N122 1.159(4) . ? C123 N124 1.159(4) . ? C103 C130 1.410(4) . ? C130 C133 1.395(5) . ? C130 C131 1.425(4) . ? C131 N132 1.154(4) . ? C133 N134 1.159(4) . ? N134 Mn1 2.220(3) 2_677 ? O2 C32 1.438(11) . ? O1 C31 1.445(5) . ? 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 N4 Mn1 N134 95.32(10) . 2_677 ? N4 Mn1 N112 101.22(10) . . ? N134 Mn1 N112 88.82(10) 2_677 . ? N4 Mn1 N2 161.00(10) . . ? N134 Mn1 N2 99.09(10) 2_677 . ? N112 Mn1 N2 91.43(10) . . ? N4 Mn1 N3 73.53(10) . . ? N134 Mn1 N3 167.89(9) 2_677 . ? N112 Mn1 N3 88.76(10) . . ? N2 Mn1 N3 92.83(10) . . ? N4 Mn1 N1 93.56(10) . . ? N134 Mn1 N1 96.78(10) 2_677 . ? N112 Mn1 N1 163.65(10) . . ? N2 Mn1 N1 72.55(9) . . ? N3 Mn1 N1 88.78(9) . . ? C10 N1 C14 118.8(3) . . ? C10 N1 Mn1 124.7(2) . . ? C14 N1 Mn1 116.32(19) . . ? C19 N2 C15 118.3(3) . . ? C19 N2 Mn1 123.4(2) . . ? C15 N2 Mn1 117.7(2) . . ? N1 C10 C11 122.6(3) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C14 118.8(3) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N1 C14 C13 121.4(3) . . ? N1 C14 C15 116.3(3) . . ? C13 C14 C15 122.4(3) . . ? N2 C15 C16 121.3(3) . . ? N2 C15 C14 115.5(3) . . ? C16 C15 C14 123.1(3) . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 117.8(3) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? N2 C19 C18 123.2(3) . . ? N2 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C29 N3 C25 118.4(3) . . ? C29 N3 Mn1 125.6(2) . . ? C25 N3 Mn1 115.8(2) . . ? C20 N4 C24 118.7(3) . . ? C20 N4 Mn1 123.1(2) . . ? C24 N4 Mn1 117.4(2) . . ? N4 C20 C21 123.3(3) . . ? N4 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C22 C21 C20 117.5(3) . . ? C22 C21 H21 121.3 . . ? C20 C21 H21 121.3 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N4 C24 C23 121.4(3) . . ? N4 C24 C25 116.0(3) . . ? C23 C24 C25 122.6(3) . . ? N3 C25 C26 121.2(3) . . ? N3 C25 C24 115.9(3) . . ? C26 C25 C24 122.9(3) . . ? C25 C26 C27 119.4(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 119.4(3) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 118.2(4) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? N3 C29 C28 123.5(3) . . ? N3 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C103 C101 C102 59.7(2) . . ? C103 C101 C110 147.8(3) . . ? C102 C101 C110 152.5(3) . . ? C101 C110 C111 123.1(3) . . ? C101 C110 C113 120.0(3) . . ? C111 C110 C113 116.7(3) . . ? N112 C111 C110 177.1(3) . . ? C111 N112 Mn1 153.3(3) . . ? N114 C113 C110 178.9(4) . . ? C103 C102 C120 150.4(3) . . ? C103 C102 C101 59.7(2) . . ? C120 C102 C101 149.9(3) . . ? C102 C120 C123 120.5(3) . . ? C102 C120 C121 121.0(3) . . ? C123 C120 C121 118.4(3) . . ? N122 C121 C120 178.5(4) . . ? N124 C123 C120 179.8(4) . . ? C102 C103 C101 60.5(2) . . ? C102 C103 C130 151.2(3) . . ? C101 C103 C130 148.3(3) . . ? C133 C130 C103 122.0(3) . . ? C133 C130 C131 118.0(3) . . ? C103 C130 C131 120.0(3) . . ? N132 C131 C130 179.7(4) . . ? N134 C133 C130 177.4(4) . . ? C133 N134 Mn1 126.1(2) . 2_677 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.083 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.096 data_2Co _database_code_depnum_ccdc_archive 'CCDC 836014' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Co(2,2'-bipy)3](HCTMCP) ; _chemical_name_common (Co(2,2'-bipy)3)(HCTMCP) _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Co N6, C12 N6' _chemical_formula_sum 'C42 H24 Co N12' _chemical_formula_weight 755.66 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 13.0154(1) _cell_length_b 13.0154(1) _cell_length_c 17.9458(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2632.74(4) _cell_formula_units_Z 3 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 27912 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1161 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8210 _exptl_absorpt_correction_T_max 0.9233 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27912 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4022 _reflns_number_gt 3820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] 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_extinction_expression ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 4022 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.561472(18) 0.561472(18) 0.0000 0.01627(7) Uani 1 2 d S . . N10 N 0.69464(10) 0.68016(10) 0.07362(6) 0.0199(2) Uani 1 1 d . . . C11 C 0.69204(13) 0.67294(14) 0.14859(8) 0.0254(3) Uani 1 1 d . . . H11 H 0.6334 0.6019 0.1717 0.030 Uiso 1 1 calc R . . C12 C 0.77160(14) 0.76520(16) 0.19304(8) 0.0315(4) Uani 1 1 d . . . H12 H 0.7697 0.7564 0.2457 0.038 Uiso 1 1 calc R . . C13 C 0.85365(13) 0.87002(17) 0.16023(9) 0.0342(4) Uani 1 1 d . . . H13 H 0.9055 0.9362 0.1901 0.041 Uiso 1 1 calc R . . C14 C 0.85996(13) 0.87805(14) 0.08297(9) 0.0288(3) Uani 1 1 d . . . H14 H 0.9175 0.9487 0.0590 0.035 Uiso 1 1 calc R . . C15 C 0.78015(12) 0.78039(12) 0.04164(8) 0.0205(3) Uani 1 1 d . . . N20 N 0.46012(10) 0.64554(10) 0.02359(6) 0.0203(2) Uani 1 1 d . . . C21 C 0.47060(14) 0.74180(13) -0.01078(9) 0.0265(3) Uani 1 1 d . . . H21 H 0.5252 0.7751 -0.0509 0.032 Uiso 1 1 calc R . . C22 C 0.40544(15) 0.79457(14) 0.00957(10) 0.0320(4) Uani 1 1 d . . . H22 H 0.4141 0.8620 -0.0165 0.038 Uiso 1 1 calc R . . C23 C 0.32734(14) 0.74735(14) 0.06861(10) 0.0337(4) Uani 1 1 d . . . H23 H 0.2806 0.7812 0.0834 0.040 Uiso 1 1 calc R . . C24 C 0.31811(14) 0.65008(14) 0.10588(9) 0.0294(3) Uani 1 1 d . . . H24 H 0.2669 0.6181 0.1477 0.035 Uiso 1 1 calc R . . C25 C 0.38432(12) 0.59940(12) 0.08177(8) 0.0210(3) Uani 1 1 d . . . C26 C 0.37676(12) 0.49200(12) 0.11568(7) 0.0203(3) Uani 1 1 d . . . C27 C 0.30226(13) 0.43163(15) 0.17518(7) 0.0277(3) Uani 1 1 d . . . H27 H 0.2520 0.4579 0.1956 0.033 Uiso 1 1 calc R . . C28 C 0.30192(15) 0.33336(15) 0.20424(8) 0.0325(4) Uani 1 1 d . . . H28 H 0.2512 0.2909 0.2447 0.039 Uiso 1 1 calc R . . C29 C 0.37625(14) 0.29757(14) 0.17377(9) 0.0306(3) Uani 1 1 d . . . H29 H 0.3788 0.2312 0.1936 0.037 Uiso 1 1 calc R . . C30 C 0.44706(13) 0.35986(12) 0.11384(8) 0.0258(3) Uani 1 1 d . . . H30 H 0.4967 0.3339 0.0921 0.031 Uiso 1 1 calc R . . N30 N 0.44801(10) 0.45542(10) 0.08538(6) 0.0204(2) Uani 1 1 d . . . C101 C 0.58485(12) 0.60458(12) 0.46340(7) 0.0209(3) Uani 1 1 d . . . C110 C 0.62421(13) 0.67802(12) 0.40047(7) 0.0214(3) Uani 1 1 d . . . C111 C 0.55318(13) 0.65400(13) 0.33590(8) 0.0234(3) Uani 1 1 d . . . N112 N 0.49707(12) 0.63714(13) 0.28258(7) 0.0323(3) Uani 1 1 d . . . C113 C 0.73698(13) 0.78383(13) 0.40197(8) 0.0235(3) Uani 1 1 d . . . N114 N 0.82856(12) 0.86834(13) 0.40295(8) 0.0350(3) Uani 1 1 d . . . C102 C 0.50213(16) 0.50213(16) 0.5000 0.0215(4) Uani 1 2 d S . . C120 C 0.39388(16) 0.39388(16) 0.5000 0.0227(4) Uani 1 2 d S . . C121 C 0.32489(14) 0.34930(14) 0.43445(8) 0.0269(3) Uani 1 1 d . . . N122 N 0.26747(14) 0.31006(15) 0.38231(8) 0.0428(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01451(9) 0.01451(9) 0.01804(11) -0.00030(5) 0.00030(5) 0.00595(10) N10 0.0188(6) 0.0195(6) 0.0212(5) -0.0021(4) -0.0013(4) 0.0094(5) C11 0.0255(7) 0.0322(8) 0.0204(7) -0.0032(6) -0.0022(6) 0.0159(6) C12 0.0253(8) 0.0471(10) 0.0249(7) -0.0096(7) -0.0044(6) 0.0203(7) C13 0.0205(7) 0.0411(9) 0.0378(8) -0.0209(8) -0.0070(6) 0.0128(7) C14 0.0182(7) 0.0252(7) 0.0395(8) -0.0094(7) 0.0005(6) 0.0082(6) C15 0.0151(6) 0.0194(7) 0.0275(7) -0.0037(6) 0.0004(6) 0.0090(6) N20 0.0200(6) 0.0172(6) 0.0229(5) -0.0012(5) -0.0005(5) 0.0088(5) C21 0.0293(8) 0.0227(7) 0.0298(7) 0.0018(6) 0.0001(6) 0.0146(6) C22 0.0346(9) 0.0223(7) 0.0441(9) -0.0033(7) -0.0060(7) 0.0180(7) C23 0.0270(8) 0.0258(8) 0.0514(10) -0.0118(7) -0.0025(7) 0.0156(7) C24 0.0223(7) 0.0239(8) 0.0382(9) -0.0102(7) 0.0032(6) 0.0086(6) C25 0.0169(6) 0.0192(7) 0.0233(7) -0.0068(5) -0.0026(5) 0.0064(5) C26 0.0167(6) 0.0184(7) 0.0194(6) -0.0048(5) -0.0026(5) 0.0041(5) C27 0.0221(7) 0.0307(8) 0.0231(6) -0.0033(7) 0.0021(5) 0.0079(7) C28 0.0273(8) 0.0314(9) 0.0232(7) 0.0045(7) -0.0001(6) 0.0029(7) C29 0.0277(8) 0.0230(8) 0.0312(8) 0.0065(6) -0.0052(7) 0.0051(7) C30 0.0236(8) 0.0193(7) 0.0301(7) 0.0012(6) -0.0023(6) 0.0075(6) N30 0.0179(6) 0.0177(6) 0.0221(6) -0.0001(5) -0.0007(5) 0.0063(5) C101 0.0184(6) 0.0186(6) 0.0264(6) -0.0028(5) 0.0008(6) 0.0098(6) C110 0.0172(7) 0.0200(6) 0.0232(6) -0.0003(5) 0.0003(6) 0.0064(6) C111 0.0215(7) 0.0175(7) 0.0264(7) 0.0011(6) 0.0056(6) 0.0062(6) N112 0.0297(7) 0.0319(7) 0.0267(6) 0.0007(6) -0.0021(6) 0.0090(6) C113 0.0232(7) 0.0250(8) 0.0213(6) -0.0008(6) 0.0030(6) 0.0113(6) N114 0.0253(7) 0.0313(7) 0.0369(7) -0.0008(6) 0.0013(6) 0.0054(6) C102 0.0210(7) 0.0210(7) 0.0237(9) -0.0011(4) 0.0011(4) 0.0114(8) C120 0.0209(7) 0.0209(7) 0.0224(9) -0.0001(4) 0.0001(4) 0.0075(8) C121 0.0215(7) 0.0259(8) 0.0267(7) -0.0003(6) 0.0034(6) 0.0068(6) N122 0.0309(8) 0.0479(10) 0.0292(7) -0.0006(7) -0.0027(6) 0.0043(7) _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 Co1 N30 2.0965(11) 6 ? Co1 N30 2.0965(11) . ? Co1 N10 2.1115(11) . ? Co1 N10 2.1115(11) 6 ? Co1 N20 2.1354(11) 6 ? Co1 N20 2.1354(11) . ? N10 C15 1.3483(18) . ? N10 C11 1.3480(18) . ? C11 C12 1.381(2) . ? C11 H11 0.9500 . ? C12 C13 1.375(3) . ? C12 H12 0.9500 . ? C13 C14 1.390(2) . ? C13 H13 0.9500 . ? C14 C15 1.387(2) . ? C14 H14 0.9500 . ? C15 C15 1.494(3) 6 ? N20 C21 1.3408(18) . ? N20 C25 1.3534(18) . ? C21 C22 1.381(2) . ? C21 H21 0.9500 . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.383(2) . ? C23 H23 0.9500 . ? C24 C25 1.391(2) . ? C24 H24 0.9500 . ? C25 C26 1.482(2) . ? C26 N30 1.3506(19) . ? C26 C27 1.3913(19) . ? C27 C28 1.379(2) . ? C27 H27 0.9500 . ? C28 C29 1.379(3) . ? C28 H28 0.9500 . ? C29 C30 1.384(2) . ? C29 H29 0.9500 . ? C30 N30 1.3389(19) . ? C30 H30 0.9500 . ? C101 C101 1.387(3) 6_556 ? C101 C102 1.390(2) . ? C101 C110 1.4007(19) . ? C110 C111 1.416(2) . ? C110 C113 1.425(2) . ? C111 N112 1.156(2) . ? C113 N114 1.149(2) . ? C102 C101 1.390(2) 6_556 ? C102 C120 1.409(3) . ? C120 C121 1.4163(19) . ? C120 C121 1.4163(19) 6_556 ? C121 N122 1.146(2) . ? 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 N30 Co1 N30 94.10(6) 6 . ? N30 Co1 N10 169.46(5) 6 . ? N30 Co1 N10 94.28(4) . . ? N30 Co1 N10 94.28(4) 6 6 ? N30 Co1 N10 169.46(5) . 6 ? N10 Co1 N10 78.17(6) . 6 ? N30 Co1 N20 77.31(5) 6 6 ? N30 Co1 N20 98.51(5) . 6 ? N10 Co1 N20 95.12(5) . 6 ? N10 Co1 N20 89.57(4) 6 6 ? N30 Co1 N20 98.51(5) 6 . ? N30 Co1 N20 77.31(5) . . ? N10 Co1 N20 89.57(4) . . ? N10 Co1 N20 95.12(5) 6 . ? N20 Co1 N20 173.96(6) 6 . ? C15 N10 C11 118.17(12) . . ? C15 N10 Co1 114.83(9) . . ? C11 N10 Co1 126.21(10) . . ? N10 C11 C12 122.29(15) . . ? N10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 119.21(14) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 119.28(14) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 118.39(15) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N10 C15 C14 122.45(13) . . ? N10 C15 C15 115.17(8) . 6 ? C14 C15 C15 122.36(9) . 6 ? C21 N20 C25 118.72(12) . . ? C21 N20 Co1 125.97(10) . . ? C25 N20 Co1 115.18(9) . . ? N20 C21 C22 122.84(15) . . ? N20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C21 C22 C23 118.68(15) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C22 C23 C24 119.08(14) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 119.53(15) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N20 C25 C24 121.11(13) . . ? N20 C25 C26 115.17(12) . . ? C24 C25 C26 123.71(13) . . ? N30 C26 C27 121.16(14) . . ? N30 C26 C25 115.70(12) . . ? C27 C26 C25 123.14(13) . . ? C28 C27 C26 119.48(15) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 119.06(14) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 118.96(15) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? N30 C30 C29 122.31(15) . . ? N30 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 N30 C26 119.00(12) . . ? C30 N30 Co1 124.52(10) . . ? C26 N30 Co1 116.36(9) . . ? C101 C101 C102 60.08(7) 6_556 . ? C101 C101 C110 148.39(8) 6_556 . ? C102 C101 C110 151.53(13) . . ? C101 C110 C111 122.23(12) . . ? C101 C110 C113 119.53(13) . . ? C111 C110 C113 118.17(12) . . ? N112 C111 C110 178.34(16) . . ? N114 C113 C110 179.15(18) . . ? C101 C102 C101 59.84(14) 6_556 . ? C101 C102 C120 150.08(7) 6_556 . ? C101 C102 C120 150.08(7) . . ? C102 C120 C121 121.46(9) . . ? C102 C120 C121 121.46(9) . 6_556 ? C121 C120 C121 117.09(19) . 6_556 ? N122 C121 C120 178.04(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.202 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.034 data_2Fe _database_code_depnum_ccdc_archive 'CCDC 836015' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe(2,2'-bipy)3](HCTMCP) ; _chemical_name_common (Fe(2,2'-bipy)3)(HCTMCP) _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Fe N6, C12 N6' _chemical_formula_sum 'C42 H24 Fe N12' _chemical_formula_weight 752.58 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 12.92040(10) _cell_length_b 12.92040(10) _cell_length_c 17.7791(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2570.35(4) _cell_formula_units_Z 3 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 27330 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 27.47 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8348 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27330 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3932 _reflns_number_gt 3766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] 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_extinction_expression ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(10) _refine_ls_number_reflns 3932 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Fe1 Fe 0.56316(2) 0.56316(2) 0.0000 0.01237(7) Uani 1 2 d S . . N10 N 0.67187(10) 0.68475(10) 0.07208(6) 0.0149(2) Uani 1 1 d . . . C11 C 0.66032(13) 0.68301(13) 0.14774(8) 0.0185(3) Uani 1 1 d . . . H11 H 0.5885 0.6227 0.1700 0.022 Uiso 1 1 calc R . . C12 C 0.74932(15) 0.76588(14) 0.19381(8) 0.0229(3) Uani 1 1 d . . . H12 H 0.7373 0.7642 0.2466 0.027 Uiso 1 1 calc R . . C13 C 0.85595(15) 0.85124(14) 0.16239(9) 0.0259(3) Uani 1 1 d . . . H13 H 0.9202 0.9051 0.1936 0.031 Uiso 1 1 calc R . . C14 C 0.86799(14) 0.85731(13) 0.08484(8) 0.0232(3) Uani 1 1 d . . . H14 H 0.9396 0.9168 0.0618 0.028 Uiso 1 1 calc R . . C15 C 0.77339(13) 0.77482(12) 0.04154(8) 0.0168(3) Uani 1 1 d . . . N20 N 0.64451(10) 0.47167(10) 0.02074(6) 0.0147(2) Uani 1 1 d . . . C21 C 0.74291(13) 0.48359(14) -0.01366(8) 0.0203(3) Uani 1 1 d . . . H21 H 0.7776 0.5403 -0.0532 0.024 Uiso 1 1 calc R . . C22 C 0.79557(14) 0.41704(15) 0.00594(9) 0.0241(3) Uani 1 1 d . . . H22 H 0.8642 0.4272 -0.0201 0.029 Uiso 1 1 calc R . . C23 C 0.74683(14) 0.33520(14) 0.06419(9) 0.0247(3) Uani 1 1 d . . . H23 H 0.7808 0.2876 0.0782 0.030 Uiso 1 1 calc R . . C24 C 0.64816(13) 0.32407(13) 0.10137(9) 0.0214(3) Uani 1 1 d . . . H24 H 0.6149 0.2703 0.1424 0.026 Uiso 1 1 calc R . . C25 C 0.59747(13) 0.39198(12) 0.07852(8) 0.0160(3) Uani 1 1 d . . . C26 C 0.48928(12) 0.38369(12) 0.11132(7) 0.0157(3) Uani 1 1 d . . . C27 C 0.42555(14) 0.30837(13) 0.17058(7) 0.0207(3) Uani 1 1 d . . . H27 H 0.4506 0.2573 0.1922 0.025 Uiso 1 1 calc R . . C28 C 0.32557(14) 0.30860(14) 0.19764(8) 0.0241(3) Uani 1 1 d . . . H28 H 0.2807 0.2576 0.2380 0.029 Uiso 1 1 calc R . . C29 C 0.29191(13) 0.38449(14) 0.16490(8) 0.0230(3) Uani 1 1 d . . . H29 H 0.2239 0.3869 0.1829 0.028 Uiso 1 1 calc R . . C30 C 0.35824(12) 0.45677(14) 0.10576(8) 0.0189(3) Uani 1 1 d . . . H30 H 0.3337 0.5076 0.0831 0.023 Uiso 1 1 calc R . . N30 N 0.45594(11) 0.45790(10) 0.07910(6) 0.0152(2) Uani 1 1 d . . . C101 C 0.60850(12) 0.58879(13) 0.46301(7) 0.0181(3) Uani 1 1 d . . . C110 C 0.68181(12) 0.62779(14) 0.39935(8) 0.0191(3) Uani 1 1 d . . . C111 C 0.65376(13) 0.55422(14) 0.33458(8) 0.0202(3) Uani 1 1 d . . . N112 N 0.63276(13) 0.49530(13) 0.28151(7) 0.0269(3) Uani 1 1 d . . . C113 C 0.78837(14) 0.74145(14) 0.39980(8) 0.0218(3) Uani 1 1 d . . . N114 N 0.87300(13) 0.83395(13) 0.40074(8) 0.0332(3) Uani 1 1 d . . . C102 C 0.50552(16) 0.50552(16) 0.5000 0.0186(4) Uani 1 2 d S . . C120 C 0.39666(16) 0.39666(16) 0.5000 0.0189(4) Uani 1 2 d S . . C121 C 0.35295(14) 0.32642(14) 0.43374(8) 0.0221(3) Uani 1 1 d . . . N122 N 0.31588(14) 0.26914(13) 0.38058(8) 0.0336(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01174(10) 0.01174(10) 0.01303(11) 0.00004(5) -0.00004(5) 0.00541(11) N10 0.0146(6) 0.0156(6) 0.0158(5) -0.0014(4) -0.0021(4) 0.0085(5) C11 0.0220(7) 0.0193(7) 0.0155(6) -0.0015(5) -0.0024(5) 0.0113(6) C12 0.0331(8) 0.0211(7) 0.0173(7) -0.0029(6) -0.0069(6) 0.0156(7) C13 0.0307(8) 0.0168(7) 0.0281(7) -0.0060(6) -0.0140(7) 0.0103(7) C14 0.0202(7) 0.0158(7) 0.0303(8) -0.0007(6) -0.0046(6) 0.0066(6) C15 0.0157(7) 0.0145(6) 0.0207(7) 0.0002(6) -0.0012(5) 0.0079(6) N20 0.0132(6) 0.0142(5) 0.0160(5) -0.0007(5) -0.0012(4) 0.0062(4) C21 0.0172(7) 0.0221(7) 0.0220(7) 0.0017(6) 0.0022(6) 0.0100(6) C22 0.0180(7) 0.0276(8) 0.0307(8) -0.0013(6) 0.0003(6) 0.0145(6) C23 0.0214(8) 0.0219(8) 0.0337(8) -0.0021(6) -0.0084(6) 0.0131(7) C24 0.0195(7) 0.0168(7) 0.0252(7) 0.0020(6) -0.0059(6) 0.0070(6) C25 0.0149(7) 0.0145(6) 0.0158(6) -0.0007(5) -0.0036(5) 0.0053(5) C26 0.0157(7) 0.0143(6) 0.0147(6) -0.0014(5) -0.0030(5) 0.0056(6) C27 0.0229(8) 0.0180(7) 0.0171(6) 0.0023(5) -0.0017(6) 0.0073(6) C28 0.0227(8) 0.0233(8) 0.0179(7) 0.0016(6) 0.0036(6) 0.0051(6) C29 0.0162(7) 0.0235(8) 0.0231(7) -0.0030(6) 0.0048(6) 0.0053(6) C30 0.0154(6) 0.0192(7) 0.0205(6) -0.0016(6) 0.0009(5) 0.0075(6) N30 0.0144(6) 0.0147(6) 0.0142(5) -0.0013(4) -0.0009(4) 0.0056(5) C101 0.0176(6) 0.0164(7) 0.0215(7) 0.0003(6) -0.0033(5) 0.0095(6) C110 0.0174(6) 0.0172(7) 0.0204(6) 0.0018(6) 0.0000(5) 0.0069(6) C111 0.0157(7) 0.0197(7) 0.0218(7) 0.0060(6) 0.0016(5) 0.0064(6) N112 0.0259(7) 0.0283(7) 0.0221(6) -0.0006(6) 0.0001(6) 0.0103(6) C113 0.0233(8) 0.0223(8) 0.0194(7) 0.0032(6) 0.0002(6) 0.0111(7) N114 0.0291(8) 0.0242(7) 0.0351(8) 0.0028(6) 0.0003(6) 0.0050(7) C102 0.0198(8) 0.0198(8) 0.0182(9) 0.0014(3) -0.0014(3) 0.0112(8) C120 0.0186(7) 0.0186(7) 0.0176(9) 0.0011(4) -0.0011(4) 0.0079(9) C121 0.0221(8) 0.0186(7) 0.0229(7) 0.0043(6) -0.0001(6) 0.0081(6) N122 0.0414(9) 0.0255(7) 0.0230(7) -0.0002(6) -0.0021(6) 0.0085(7) _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 Fe1 N30 1.9653(12) 6 ? Fe1 N30 1.9653(12) . ? Fe1 N10 1.9689(12) . ? Fe1 N10 1.9689(12) 6 ? Fe1 N20 1.9700(11) . ? Fe1 N20 1.9700(11) 6 ? N10 C11 1.3523(18) . ? N10 C15 1.3576(18) . ? C11 C12 1.381(2) . ? C11 H11 0.9500 . ? C12 C13 1.381(2) . ? C12 H12 0.9500 . ? C13 C14 1.385(2) . ? C13 H13 0.9500 . ? C14 C15 1.386(2) . ? C14 H14 0.9500 . ? C15 C15 1.477(3) 6 ? N20 C21 1.3484(18) . ? N20 C25 1.3635(18) . ? C21 C22 1.382(2) . ? C21 H21 0.9500 . ? C22 C23 1.386(2) . ? C22 H22 0.9500 . ? C23 C24 1.378(2) . ? C23 H23 0.9500 . ? C24 C25 1.392(2) . ? C24 H24 0.9500 . ? C25 C26 1.468(2) . ? C26 N30 1.3587(18) . ? C26 C27 1.3906(19) . ? C27 C28 1.380(2) . ? C27 H27 0.9500 . ? C28 C29 1.384(2) . ? C28 H28 0.9500 . ? C29 C30 1.383(2) . ? C29 H29 0.9500 . ? C30 N30 1.3416(19) . ? C30 H30 0.9500 . ? C101 C101 1.387(3) 6_556 ? C101 C102 1.389(2) . ? C101 C110 1.3982(19) . ? C110 C111 1.420(2) . ? C110 C113 1.425(2) . ? C111 N112 1.156(2) . ? C113 N114 1.148(2) . ? C102 C101 1.389(2) 6_556 ? C102 C120 1.406(3) . ? C120 C121 1.4205(19) . ? C120 C121 1.4205(19) 6_556 ? C121 N122 1.147(2) . ? 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 N30 Fe1 N30 91.40(7) 6 . ? N30 Fe1 N10 173.90(5) 6 . ? N30 Fe1 N10 93.51(5) . . ? N30 Fe1 N10 93.51(5) 6 6 ? N30 Fe1 N10 173.90(5) . 6 ? N10 Fe1 N10 81.84(7) . 6 ? N30 Fe1 N20 95.73(5) 6 . ? N30 Fe1 N20 81.59(5) . . ? N10 Fe1 N20 88.57(5) . . ? N10 Fe1 N20 94.31(5) 6 . ? N30 Fe1 N20 81.59(5) 6 6 ? N30 Fe1 N20 95.73(5) . 6 ? N10 Fe1 N20 94.31(5) . 6 ? N10 Fe1 N20 88.57(5) 6 6 ? N20 Fe1 N20 176.19(7) . 6 ? C11 N10 C15 117.61(12) . . ? C11 N10 Fe1 127.26(10) . . ? C15 N10 Fe1 114.94(9) . . ? N10 C11 C12 122.32(14) . . ? N10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 119.39(13) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.12(14) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 118.59(14) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N10 C15 C14 122.66(13) . . ? N10 C15 C15 113.70(7) . 6 ? C14 C15 C15 123.60(9) . 6 ? C21 N20 C25 117.84(12) . . ? C21 N20 Fe1 127.01(10) . . ? C25 N20 Fe1 115.09(9) . . ? N20 C21 C22 122.95(14) . . ? N20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C21 C22 C23 119.08(14) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 118.80(14) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.75(14) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N20 C25 C24 121.55(13) . . ? N20 C25 C26 113.76(12) . . ? C24 C25 C26 124.67(13) . . ? N30 C26 C27 121.84(13) . . ? N30 C26 C25 114.04(12) . . ? C27 C26 C25 124.12(13) . . ? C28 C27 C26 119.35(14) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 118.75(14) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 119.35(14) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? N30 C30 C29 122.55(14) . . ? N30 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 N30 C26 118.16(12) . . ? C30 N30 Fe1 126.45(10) . . ? C26 N30 Fe1 115.31(10) . . ? C101 C101 C102 60.04(7) 6_556 . ? C101 C101 C110 148.74(8) 6_556 . ? C102 C101 C110 151.22(13) . . ? C101 C110 C111 121.00(13) . . ? C101 C110 C113 119.88(14) . . ? C111 C110 C113 119.09(13) . . ? N112 C111 C110 178.94(17) . . ? N114 C113 C110 178.70(19) . . ? C101 C102 C101 59.93(14) 6_556 . ? C101 C102 C120 150.04(7) 6_556 . ? C101 C102 C120 150.04(7) . . ? C102 C120 C121 121.22(10) . . ? C102 C120 C121 121.22(10) . 6_556 ? C121 C120 C121 117.57(19) . 6_556 ? N122 C121 C120 178.95(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.216 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.052 data_3 _database_code_depnum_ccdc_archive 'CCDC 836016' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Co(phen)2(HCTMCP)(H2O)].H2O.0.5MeCN ; _chemical_name_common (Co(phen)2(HCTMCP)(H2O)).H2O.0.5MeCN _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Co N10 O, H2O, 0.5(C2 H3 N)' _chemical_formula_sum 'C37 H21.50 Co N10.50 O2' _chemical_formula_weight 704.08 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7130(4) _cell_length_b 13.0080(4) _cell_length_c 13.5422(6) _cell_angle_alpha 92.7190(10) _cell_angle_beta 95.0900(10) _cell_angle_gamma 91.710(2) _cell_volume 1876.51(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 26172 _cell_measurement_theta_min 1.51 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8436 _exptl_absorpt_correction_T_max 0.9284 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26172 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.1317 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8528 _reflns_number_gt 4446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 8528 _refine_ls_number_parameters 473 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1854 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.3170 _refine_ls_wR_factor_gt 0.2684 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.82829(8) 0.88262(5) 0.72273(5) 0.0340(3) Uani 1 1 d . . . N3 N 0.7966(5) 0.7410(3) 0.7915(3) 0.0336(11) Uani 1 1 d . . . N1 N 0.8394(5) 1.0290(3) 0.6576(3) 0.0349(11) Uani 1 1 d . . . N2 N 0.8376(4) 0.9870(3) 0.8493(3) 0.0288(10) Uani 1 1 d . . . N112 N 0.8763(5) 0.3056(3) 0.3429(4) 0.0458(13) Uani 1 1 d . . . N132 N 0.8222(5) 0.8049(3) 0.5834(3) 0.0413(12) Uani 1 1 d . . . N134 N 0.8496(5) 0.9391(3) 0.2997(4) 0.0443(13) Uani 1 1 d . . . N4 N 0.6310(5) 0.8807(4) 0.7238(4) 0.0430(12) Uani 1 1 d . . . C19 C 0.8362(6) 0.9656(4) 0.9445(4) 0.0370(14) Uani 1 1 d . . . H19 H 0.8318 0.8954 0.9608 0.044 Uiso 1 1 calc R . . N124 N 0.8405(6) 0.4173(4) 0.0836(4) 0.0605(16) Uani 1 1 d . . . C123 C 0.8397(6) 0.4928(5) 0.1204(5) 0.0470(16) Uani 1 1 d . . . C15 C 0.8552(7) 1.2728(4) 0.8685(5) 0.0468(16) Uani 1 1 d . . . H15 H 0.8598 1.3282 0.9171 0.056 Uiso 1 1 calc R . . C41 C 0.6737(7) 0.7202(5) 0.7992(4) 0.0468(16) Uani 1 1 d . . . C17 C 0.8483(6) 1.1431(5) 0.9990(4) 0.0446(15) Uani 1 1 d . . . H17 H 0.8529 1.1955 1.0506 0.054 Uiso 1 1 calc R . . C11 C 0.8466(7) 1.1477(4) 0.5292(4) 0.0527(18) Uani 1 1 d . . . H11 H 0.8473 1.1582 0.4603 0.063 Uiso 1 1 calc R . . C10 C 0.8403(6) 1.0491(4) 0.5624(4) 0.0448(16) Uani 1 1 d . . . H10 H 0.8363 0.9928 0.5147 0.054 Uiso 1 1 calc R . . C111 C 0.8613(6) 0.3847(4) 0.3771(5) 0.0437(15) Uani 1 1 d . . . C30 C 0.8756(7) 0.6722(4) 0.8231(4) 0.0430(15) Uani 1 1 d . . . H30 H 0.9626 0.6862 0.8193 0.052 Uiso 1 1 calc R . . C18 C 0.8409(6) 1.0405(4) 1.0204(4) 0.0429(15) Uani 1 1 d . . . H18 H 0.8391 1.0216 1.0871 0.051 Uiso 1 1 calc R . . C120 C 0.8403(7) 0.5953(4) 0.1639(5) 0.0487(17) Uani 1 1 d . . . C110 C 0.8410(6) 0.4856(4) 0.4197(4) 0.0446(15) Uani 1 1 d . . . C32 C 0.7177(8) 0.5575(5) 0.8698(5) 0.060(2) Uani 1 1 d . . . H32 H 0.6918 0.4950 0.8966 0.072 Uiso 1 1 calc R . . C102 C 0.8386(6) 0.6089(4) 0.2673(5) 0.0432(15) Uani 1 1 d . . . C31 C 0.8390(7) 0.5783(4) 0.8624(4) 0.0437(16) Uani 1 1 d . . . H31 H 0.9001 0.5306 0.8833 0.052 Uiso 1 1 calc R . . C13 C 0.8501(6) 1.2123(4) 0.6972(4) 0.0370(14) Uani 1 1 d . . . C20 C 0.8448(5) 1.0875(4) 0.8280(4) 0.0301(12) Uani 1 1 d . . . C14 C 0.8548(7) 1.2938(4) 0.7726(5) 0.0490(17) Uani 1 1 d . . . H14 H 0.8577 1.3635 0.7544 0.059 Uiso 1 1 calc R . . C113 C 0.8260(7) 0.5000(5) 0.5237(5) 0.0506(17) Uani 1 1 d . . . C39 C 0.5561(8) 0.9491(6) 0.6942(6) 0.066(2) Uani 1 1 d . . . H39 H 0.5890 1.0080 0.6652 0.080 Uiso 1 1 calc R . . C21 C 0.8444(5) 1.1096(4) 0.7251(4) 0.0310(12) Uani 1 1 d . . . C16 C 0.8488(6) 1.1683(4) 0.9004(4) 0.0376(14) Uani 1 1 d . . . C33 C 0.6269(7) 0.6294(5) 0.8372(5) 0.0581(19) Uani 1 1 d . . . C101 C 0.8386(6) 0.5713(4) 0.3596(5) 0.0423(15) Uani 1 1 d . . . C40 C 0.5842(7) 0.7951(5) 0.7645(5) 0.0518(17) Uani 1 1 d . . . C12 C 0.8519(6) 1.2291(4) 0.5953(4) 0.0453(16) Uani 1 1 d . . . H12 H 0.8567 1.2973 0.5732 0.054 Uiso 1 1 calc R . . C34 C 0.4928(8) 0.6187(7) 0.8454(7) 0.085(3) Uani 1 1 d . . . H34 H 0.4609 0.5595 0.8746 0.102 Uiso 1 1 calc R . . N114 N 0.8137(7) 0.5028(4) 0.6050(4) 0.071(2) Uani 1 1 d . . . C131 C 0.8251(6) 0.7891(4) 0.4977(5) 0.0446(15) Uani 1 1 d . . . N122 N 0.8234(7) 0.7545(4) 0.0585(4) 0.075(2) Uani 1 1 d . . . C130 C 0.8294(7) 0.7753(4) 0.3938(4) 0.0458(16) Uani 1 1 d . . . C103 C 0.8338(6) 0.6737(4) 0.3480(5) 0.0429(15) Uani 1 1 d . . . C133 C 0.8397(6) 0.8637(4) 0.3378(5) 0.0469(16) Uani 1 1 d . . . C121 C 0.8304(8) 0.6843(5) 0.1049(5) 0.062(2) Uani 1 1 d . . . C36 C 0.4551(7) 0.7795(6) 0.7733(6) 0.067(2) Uani 1 1 d . . . C37 C 0.3780(8) 0.8602(7) 0.7415(7) 0.079(2) Uani 1 1 d . . . H37 H 0.2905 0.8555 0.7484 0.094 Uiso 1 1 calc R . . C38 C 0.4249(8) 0.9408(7) 0.7028(7) 0.080(3) Uani 1 1 d . . . H38 H 0.3718 0.9938 0.6804 0.096 Uiso 1 1 calc R . . C35 C 0.4153(8) 0.6872(7) 0.8142(7) 0.083(3) Uani 1 1 d . . . H35 H 0.3282 0.6750 0.8191 0.100 Uiso 1 1 calc R . . O1 O 1.0243(4) 0.8726(3) 0.7404(3) 0.0356(9) Uani 1 1 d D . . H2O H 1.053(6) 0.818(3) 0.714(5) 0.06(2) Uiso 1 1 d D . . H1O H 1.074(5) 0.924(4) 0.731(5) 0.06(2) Uiso 1 1 d D . . C6 C 0.537(4) 0.847(3) 0.088(3) 0.074(12) Uiso 0.25 1 d P A 1 C5 C 0.497(3) 0.758(3) 0.135(3) 0.065(9) Uiso 0.25 1 d P A 1 N5 N 0.493(2) 0.6501(19) 0.1383(18) 0.059(6) Uiso 0.25 1 d P B 2 N6 N 0.504(3) 0.914(2) 0.046(2) 0.077(8) Uiso 0.25 1 d P A 1 O3 O 0.4154(19) 0.6019(16) 0.3273(16) 0.169(7) Uiso 0.50 1 d P . . O2 O 0.494(2) 0.7868(17) 0.4412(18) 0.189(9) Uiso 0.50 1 d P . . C6A C 0.506(4) 0.819(3) 0.061(3) 0.073(12) Uiso 0.25 1 d P B 2 C5A C 0.492(4) 0.723(3) 0.088(3) 0.083(11) Uiso 0.25 1 d P B 2 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 Co1 0.0585(6) 0.0180(4) 0.0262(4) 0.0061(3) 0.0040(3) 0.0019(3) N3 0.049(3) 0.024(2) 0.028(2) 0.0054(18) 0.003(2) 0.001(2) N1 0.066(3) 0.018(2) 0.021(2) 0.0053(17) 0.004(2) 0.004(2) N2 0.047(3) 0.021(2) 0.019(2) 0.0047(16) 0.0058(19) 0.004(2) N112 0.085(4) 0.018(2) 0.037(3) 0.004(2) 0.014(3) 0.006(2) N132 0.076(4) 0.023(2) 0.023(3) -0.0017(19) 0.001(2) 0.000(2) N134 0.063(4) 0.018(2) 0.052(3) 0.010(2) 0.003(3) 0.004(2) N4 0.049(3) 0.033(3) 0.047(3) 0.004(2) 0.003(2) 0.006(2) C19 0.056(4) 0.026(3) 0.030(3) 0.010(2) 0.007(3) 0.003(3) N124 0.095(5) 0.046(3) 0.041(3) -0.008(3) 0.016(3) 0.000(3) C123 0.067(5) 0.042(4) 0.032(3) -0.008(3) 0.012(3) 0.002(3) C15 0.077(5) 0.027(3) 0.036(3) -0.005(2) 0.008(3) -0.001(3) C41 0.066(5) 0.041(3) 0.034(3) 0.005(3) 0.005(3) -0.007(3) C17 0.068(4) 0.040(3) 0.025(3) -0.006(2) 0.005(3) 0.007(3) C11 0.100(6) 0.033(3) 0.027(3) 0.014(3) 0.010(3) 0.009(3) C10 0.084(5) 0.024(3) 0.027(3) 0.005(2) 0.007(3) 0.006(3) C111 0.061(4) 0.028(3) 0.044(4) 0.013(3) 0.009(3) 0.001(3) C30 0.073(5) 0.023(3) 0.034(3) 0.006(2) 0.009(3) 0.002(3) C18 0.066(4) 0.040(3) 0.026(3) 0.011(2) 0.014(3) 0.006(3) C120 0.084(5) 0.029(3) 0.035(3) 0.008(2) 0.010(3) 0.002(3) C110 0.070(4) 0.026(3) 0.038(3) 0.007(2) 0.003(3) 0.007(3) C32 0.095(6) 0.038(4) 0.047(4) 0.013(3) 0.003(4) -0.016(4) C102 0.056(4) 0.035(3) 0.038(3) 0.001(3) 0.003(3) 0.002(3) C31 0.075(5) 0.023(3) 0.034(3) 0.005(2) 0.006(3) 0.002(3) C13 0.059(4) 0.025(3) 0.029(3) 0.008(2) 0.009(3) 0.008(3) C20 0.043(3) 0.021(2) 0.027(3) 0.006(2) 0.003(2) 0.004(2) C14 0.082(5) 0.016(3) 0.050(4) 0.004(2) 0.009(3) 0.007(3) C113 0.081(5) 0.036(3) 0.036(4) 0.013(3) 0.003(3) 0.002(3) C39 0.077(6) 0.046(4) 0.077(5) 0.014(4) 0.001(4) 0.011(4) C21 0.051(4) 0.019(2) 0.023(3) 0.004(2) 0.007(2) 0.003(2) C16 0.053(4) 0.031(3) 0.030(3) 0.001(2) 0.007(3) 0.004(3) C33 0.079(5) 0.047(4) 0.047(4) 0.016(3) 0.000(4) -0.013(4) C101 0.051(4) 0.032(3) 0.045(4) 0.012(3) 0.005(3) -0.001(3) C40 0.067(5) 0.042(4) 0.046(4) 0.008(3) 0.004(3) 0.001(3) C12 0.077(5) 0.023(3) 0.038(3) 0.013(2) 0.006(3) 0.007(3) C34 0.072(6) 0.081(6) 0.103(7) 0.038(5) 0.003(5) -0.030(5) N114 0.139(6) 0.044(3) 0.032(3) 0.007(3) 0.017(3) 0.001(4) C131 0.062(4) 0.023(3) 0.047(4) 0.000(3) 0.000(3) 0.002(3) N122 0.139(6) 0.035(3) 0.054(4) 0.026(3) 0.018(4) 0.008(4) C130 0.078(5) 0.023(3) 0.036(3) 0.003(2) 0.004(3) 0.003(3) C103 0.049(4) 0.022(3) 0.056(4) -0.006(3) 0.004(3) 0.001(3) C133 0.056(4) 0.024(3) 0.060(4) -0.006(3) 0.005(3) 0.000(3) C121 0.090(6) 0.058(4) 0.041(4) 0.014(3) 0.016(4) 0.010(4) C36 0.049(5) 0.074(5) 0.079(6) 0.014(4) 0.005(4) -0.005(4) C37 0.060(5) 0.084(6) 0.093(7) 0.022(5) 0.000(5) 0.004(5) C38 0.055(5) 0.072(6) 0.115(8) 0.023(5) 0.001(5) 0.010(4) C35 0.062(5) 0.083(6) 0.107(7) 0.043(5) 0.005(5) 0.001(5) O1 0.058(3) 0.0164(19) 0.034(2) 0.0036(16) 0.0063(19) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N132 2.093(5) . ? Co1 O1 2.100(4) . ? Co1 N4 2.114(5) . ? Co1 N2 2.128(4) . ? Co1 N3 2.134(4) . ? Co1 N1 2.141(4) . ? N3 C30 1.311(7) . ? N3 C41 1.350(8) . ? N1 C10 1.329(7) . ? N1 C21 1.354(6) . ? N2 C19 1.333(6) . ? N2 C20 1.353(6) . ? N112 C111 1.131(7) . ? N132 C131 1.172(8) . ? N134 C133 1.136(7) . ? N4 C39 1.271(8) . ? N4 C40 1.368(8) . ? C19 C18 1.379(8) . ? N124 C123 1.081(7) . ? C123 C120 1.431(9) . ? C15 C14 1.339(8) . ? C15 C16 1.446(8) . ? C41 C33 1.407(9) . ? C41 C40 1.452(9) . ? C17 C18 1.381(8) . ? C17 C16 1.390(8) . ? C11 C12 1.350(9) . ? C11 C10 1.381(7) . ? C111 C110 1.438(8) . ? C30 C31 1.414(8) . ? C120 C102 1.405(8) . ? C120 C121 1.439(8) . ? C110 C101 1.411(8) . ? C110 C113 1.436(9) . ? C32 C31 1.333(10) . ? C32 C33 1.424(10) . ? C102 C103 1.354(8) . ? C102 C101 1.363(8) . ? C13 C21 1.406(7) . ? C13 C12 1.409(8) . ? C13 C14 1.434(8) . ? C20 C16 1.400(7) . ? C20 C21 1.437(7) . ? C113 N114 1.119(8) . ? C39 C38 1.422(11) . ? C33 C34 1.454(11) . ? C101 C103 1.350(8) . ? C40 C36 1.408(10) . ? C34 C35 1.296(11) . ? C131 C130 1.415(9) . ? N122 C121 1.133(8) . ? C130 C133 1.415(8) . ? C130 C103 1.437(8) . ? C36 C37 1.415(11) . ? C36 C35 1.416(11) . ? C37 C38 1.301(11) . ? C6 N6 1.10(4) . ? C6 C5 1.42(5) . ? N5 C5A 1.19(4) . ? C6A C5A 1.33(5) . ? 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 N132 Co1 O1 90.52(18) . . ? N132 Co1 N4 93.7(2) . . ? O1 Co1 N4 171.73(16) . . ? N132 Co1 N2 169.26(16) . . ? O1 Co1 N2 89.62(16) . . ? N4 Co1 N2 87.59(18) . . ? N132 Co1 N3 90.75(17) . . ? O1 Co1 N3 93.53(16) . . ? N4 Co1 N3 79.30(18) . . ? N2 Co1 N3 99.96(16) . . ? N132 Co1 N1 91.51(16) . . ? O1 Co1 N1 92.45(17) . . ? N4 Co1 N1 94.56(18) . . ? N2 Co1 N1 77.76(15) . . ? N3 Co1 N1 173.58(18) . . ? C30 N3 C41 117.0(5) . . ? C30 N3 Co1 130.5(4) . . ? C41 N3 Co1 112.5(4) . . ? C10 N1 C21 118.1(4) . . ? C10 N1 Co1 128.6(4) . . ? C21 N1 Co1 113.3(3) . . ? C19 N2 C20 117.3(4) . . ? C19 N2 Co1 128.4(3) . . ? C20 N2 Co1 114.3(3) . . ? C131 N132 Co1 161.1(4) . . ? C39 N4 C40 119.1(6) . . ? C39 N4 Co1 127.8(5) . . ? C40 N4 Co1 113.0(4) . . ? N2 C19 C18 123.1(5) . . ? N124 C123 C120 176.7(7) . . ? C14 C15 C16 122.1(5) . . ? N3 C41 C33 123.9(6) . . ? N3 C41 C40 118.1(5) . . ? C33 C41 C40 118.0(7) . . ? C18 C17 C16 118.7(5) . . ? C12 C11 C10 119.7(5) . . ? N1 C10 C11 123.2(5) . . ? N112 C111 C110 179.3(8) . . ? N3 C30 C31 123.8(6) . . ? C19 C18 C17 119.8(5) . . ? C102 C120 C123 118.8(5) . . ? C102 C120 C121 118.6(5) . . ? C123 C120 C121 122.3(6) . . ? C101 C110 C113 119.6(5) . . ? C101 C110 C111 119.9(5) . . ? C113 C110 C111 120.4(5) . . ? C31 C32 C33 119.8(6) . . ? C103 C102 C101 59.6(4) . . ? C103 C102 C120 148.7(6) . . ? C101 C102 C120 151.8(6) . . ? C32 C31 C30 119.2(6) . . ? C21 C13 C12 117.4(5) . . ? C21 C13 C14 119.1(5) . . ? C12 C13 C14 123.4(5) . . ? N2 C20 C16 123.3(5) . . ? N2 C20 C21 116.8(4) . . ? C16 C20 C21 119.9(4) . . ? C15 C14 C13 120.6(5) . . ? N114 C113 C110 174.3(7) . . ? N4 C39 C38 122.5(7) . . ? N1 C21 C13 122.1(5) . . ? N1 C21 C20 117.8(4) . . ? C13 C21 C20 120.0(5) . . ? C17 C16 C20 117.8(5) . . ? C17 C16 C15 123.9(5) . . ? C20 C16 C15 118.3(5) . . ? C41 C33 C32 116.3(7) . . ? C41 C33 C34 118.2(7) . . ? C32 C33 C34 125.4(7) . . ? C103 C101 C102 59.9(4) . . ? C103 C101 C110 151.4(6) . . ? C102 C101 C110 148.7(6) . . ? N4 C40 C36 122.0(6) . . ? N4 C40 C41 117.1(6) . . ? C36 C40 C41 120.9(6) . . ? C11 C12 C13 119.5(5) . . ? C35 C34 C33 122.2(7) . . ? N132 C131 C130 177.2(6) . . ? C133 C130 C131 118.4(5) . . ? C133 C130 C103 121.0(5) . . ? C131 C130 C103 120.4(5) . . ? C101 C103 C102 60.6(4) . . ? C101 C103 C130 147.8(6) . . ? C102 C103 C130 151.6(6) . . ? N134 C133 C130 174.6(7) . . ? N122 C121 C120 179.6(9) . . ? C40 C36 C37 115.7(7) . . ? C40 C36 C35 117.8(7) . . ? C37 C36 C35 126.5(8) . . ? C38 C37 C36 121.0(8) . . ? C37 C38 C39 119.6(8) . . ? C34 C35 C36 122.7(8) . . ? N6 C6 C5 144(4) . . ? N5 C5A C6A 161(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2O N112 0.85(2) 1.96(2) 2.809(6) 178(7) 2_766 O1 H1O N134 0.86(2) 2.02(3) 2.860(6) 166(6) 2_776 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.428 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.129 data_4 _database_code_depnum_ccdc_archive 'CCDC 836017' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Mn(phen)(HCTMCP)(MeOH)(H2O)] ; _chemical_name_common (Mn(phen)(HCTMCP)(MeOH)(H2O)) _chemical_melting_point ? _chemical_formula_moiety 'C25 H14 Mn N8 O2' _chemical_formula_sum 'C25 H14 Mn N8 O2' _chemical_formula_weight 513.38 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6839(3) _cell_length_b 16.3826(6) _cell_length_c 18.9623(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.4790(10) _cell_angle_gamma 90.00 _cell_volume 2354.42(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 31515 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9535 _exptl_absorpt_correction_T_max 0.9822 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31515 _diffrn_reflns_av_R_equivalents 0.1681 _diffrn_reflns_av_sigmaI/netI 0.1964 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5377 _reflns_number_gt 2417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 5377 _refine_ls_number_parameters 348 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2069 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.35656(6) 0.29687(3) 0.32612(3) 0.02394(18) Uani 1 1 d . . . O1 O 0.1199(3) 0.33643(18) 0.36364(16) 0.0344(7) Uani 1 1 d D . . O2 O 0.5931(3) 0.25558(16) 0.28470(14) 0.0318(7) Uani 1 1 d D . . N10 N 0.4644(3) 0.42538(17) 0.32801(16) 0.0244(7) Uani 1 1 d . . . N20 N 0.5146(3) 0.31330(18) 0.43505(15) 0.0235(7) Uani 1 1 d . . . N112 N 0.2968(4) 0.16881(19) 0.34655(15) 0.0268(8) Uani 1 1 d . . . N114 N 0.0041(4) -0.0163(2) 0.20923(18) 0.0408(9) Uani 1 1 d . . . N122 N -0.2154(4) -0.19311(19) 0.28372(17) 0.0304(8) Uani 1 1 d . . . N124 N -0.0588(4) -0.2628(2) 0.50965(18) 0.0366(9) Uani 1 1 d . . . N132 N 0.4489(4) 0.0960(2) 0.57726(16) 0.0334(8) Uani 1 1 d . . . N134 N 0.2263(4) -0.1360(2) 0.63246(17) 0.0378(9) Uani 1 1 d . . . C2 C 0.6992(5) 0.3016(3) 0.2440(2) 0.0496(12) Uani 1 1 d . . . H2A H 0.6211 0.3299 0.2056 0.056(13) Uiso 1 1 d R . . H2B H 0.7779 0.2650 0.2231 0.071(15) Uiso 1 1 d R . . H2C H 0.7696 0.3418 0.2746 0.15(3) Uiso 1 1 d R . . C10 C 0.4378(4) 0.4809(2) 0.2764(2) 0.0291(9) Uani 1 1 d . . . H10 H 0.3653 0.4667 0.2326 0.023(10) Uiso 1 1 d R . . C11 C 0.5110(5) 0.5587(2) 0.2828(2) 0.0340(10) Uani 1 1 d . . . H11 H 0.4877 0.5966 0.2445 0.040(11) Uiso 1 1 d R . . C12 C 0.6176(5) 0.5799(2) 0.3454(2) 0.0346(10) Uani 1 1 d . . . H12 H 0.6695 0.6326 0.3509 0.056(13) Uiso 1 1 d R . . C13 C 0.6496(4) 0.5235(2) 0.4014(2) 0.0262(9) Uani 1 1 d . . . C14 C 0.7537(4) 0.5421(3) 0.4689(2) 0.0377(11) Uani 1 1 d . . . H14 H 0.8070 0.5943 0.4764 0.040(11) Uiso 1 1 d R . . C15 C 0.7770(4) 0.4867(3) 0.5224(2) 0.0361(11) Uani 1 1 d . . . H15 H 0.8475 0.5003 0.5669 0.044(11) Uiso 1 1 d R . . C16 C 0.6979(4) 0.4079(2) 0.5133(2) 0.0275(9) Uani 1 1 d . . . C17 C 0.7144(4) 0.3490(3) 0.5675(2) 0.0348(10) Uani 1 1 d . . . H17 H 0.7843 0.3602 0.6126 0.040(11) Uiso 1 1 d R . . C18 C 0.6309(4) 0.2757(3) 0.5556(2) 0.0351(11) Uani 1 1 d . . . H18 H 0.6392 0.2359 0.5925 0.040(11) Uiso 1 1 d R . . C19 C 0.5335(4) 0.2604(2) 0.4885(2) 0.0293(9) Uani 1 1 d . . . H19 H 0.4766 0.2089 0.4805 0.031(10) Uiso 1 1 d R . . C20 C 0.5953(4) 0.3872(2) 0.44761(19) 0.0229(9) Uani 1 1 d . . . C21 C 0.5692(4) 0.4472(2) 0.39075(19) 0.0211(9) Uani 1 1 d . . . C101 C 0.1408(4) -0.0239(2) 0.39360(19) 0.0196(9) Uani 1 1 d . . . C102 C 0.0751(4) -0.0951(2) 0.41790(18) 0.0209(9) Uani 1 1 d . . . C103 C 0.1807(4) -0.0443(2) 0.46546(19) 0.0195(9) Uani 1 1 d . . . C110 C 0.1507(4) 0.0282(2) 0.33509(19) 0.0203(8) Uani 1 1 d . . . C111 C 0.2317(4) 0.1052(2) 0.34330(18) 0.0231(9) Uani 1 1 d . . . C113 C 0.0693(4) 0.0043(2) 0.2655(2) 0.0276(10) Uani 1 1 d . . . C120 C -0.0291(4) -0.1658(2) 0.40605(18) 0.0202(8) Uani 1 1 d . . . C121 C -0.1316(4) -0.1812(2) 0.3386(2) 0.0254(9) Uani 1 1 d . . . C123 C -0.0472(4) -0.2186(2) 0.4634(2) 0.0256(9) Uani 1 1 d . . . C130 C 0.2593(4) -0.0301(2) 0.53588(19) 0.0208(9) Uani 1 1 d . . . C131 C 0.3634(4) 0.0395(2) 0.55756(19) 0.0239(9) Uani 1 1 d . . . C133 C 0.2413(4) -0.0880(2) 0.5889(2) 0.0247(9) Uani 1 1 d . . . H1O H 0.075(6) 0.314(3) 0.3980(19) 0.11(2) Uiso 1 1 d D . . H2O H 0.037(4) 0.371(2) 0.348(2) 0.065(15) Uiso 1 1 d D . . H3O H 0.656(4) 0.2214(18) 0.3127(17) 0.049(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0313(3) 0.0197(3) 0.0196(3) 0.0020(3) 0.0004(2) -0.0025(3) O1 0.0390(17) 0.0342(19) 0.0323(19) 0.0094(15) 0.0123(14) 0.0074(14) O2 0.0337(15) 0.0279(17) 0.0343(18) 0.0110(14) 0.0071(13) 0.0021(13) N10 0.0315(17) 0.0210(19) 0.022(2) 0.0014(16) 0.0071(14) -0.0011(14) N20 0.0283(16) 0.021(2) 0.0186(19) 0.0038(15) -0.0030(13) 0.0004(14) N112 0.0393(18) 0.019(2) 0.022(2) 0.0015(15) 0.0038(14) -0.0030(15) N114 0.051(2) 0.044(2) 0.027(2) 0.0007(19) 0.0015(17) -0.0163(17) N122 0.0378(19) 0.031(2) 0.021(2) -0.0025(17) 0.0027(15) -0.0046(15) N124 0.049(2) 0.033(2) 0.028(2) 0.0050(18) 0.0063(16) -0.0109(16) N132 0.0316(18) 0.034(2) 0.034(2) -0.0065(18) 0.0029(15) -0.0035(16) N134 0.0383(19) 0.042(2) 0.031(2) 0.0068(19) 0.0007(16) 0.0022(16) C2 0.054(3) 0.061(3) 0.038(3) 0.016(3) 0.018(2) 0.010(3) C10 0.034(2) 0.025(3) 0.029(3) 0.005(2) 0.006(2) 0.0009(19) C11 0.040(2) 0.022(3) 0.043(3) 0.012(2) 0.017(2) 0.0019(19) C12 0.036(2) 0.023(3) 0.048(3) -0.001(2) 0.016(2) -0.003(2) C13 0.027(2) 0.021(2) 0.031(3) -0.004(2) 0.0074(18) -0.0016(18) C14 0.034(2) 0.031(3) 0.049(3) -0.012(2) 0.009(2) -0.009(2) C15 0.027(2) 0.042(3) 0.036(3) -0.014(2) -0.002(2) -0.004(2) C16 0.023(2) 0.032(3) 0.027(3) -0.005(2) 0.0025(17) -0.0004(18) C17 0.027(2) 0.048(3) 0.026(3) -0.003(2) -0.0072(19) 0.005(2) C18 0.036(2) 0.048(3) 0.019(2) 0.008(2) -0.0007(18) 0.005(2) C19 0.036(2) 0.025(3) 0.026(3) 0.003(2) 0.0012(18) 0.0027(19) C20 0.0221(19) 0.023(2) 0.024(2) -0.0034(19) 0.0053(16) 0.0001(17) C21 0.0238(19) 0.019(2) 0.022(2) -0.0041(19) 0.0074(17) -0.0016(16) C101 0.0155(19) 0.018(2) 0.024(2) -0.0017(19) -0.0010(16) 0.0039(16) C102 0.0186(19) 0.021(2) 0.024(2) 0.0058(19) 0.0056(16) 0.0055(17) C103 0.0145(18) 0.024(2) 0.020(2) 0.0042(19) 0.0021(16) 0.0022(16) C110 0.027(2) 0.016(2) 0.018(2) -0.0004(18) 0.0025(16) -0.0041(16) C111 0.026(2) 0.029(3) 0.014(2) 0.0034(19) 0.0040(16) 0.0033(19) C113 0.033(2) 0.024(2) 0.025(3) 0.002(2) 0.0038(19) -0.0041(18) C120 0.028(2) 0.019(2) 0.013(2) 0.0042(18) 0.0022(16) -0.0027(17) C121 0.030(2) 0.012(2) 0.037(3) 0.0021(19) 0.015(2) 0.0013(17) C123 0.028(2) 0.022(3) 0.026(3) -0.003(2) 0.0029(17) -0.0030(17) C130 0.023(2) 0.022(2) 0.017(2) 0.0013(19) 0.0001(16) -0.0012(17) C131 0.023(2) 0.032(3) 0.017(2) 0.002(2) 0.0047(17) 0.0101(19) C133 0.021(2) 0.030(3) 0.023(3) -0.004(2) 0.0002(17) 0.0022(18) _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 2.158(3) . ? Mn1 N122 2.190(3) 2 ? Mn1 N112 2.196(3) . ? Mn1 O2 2.202(2) . ? Mn1 N20 2.233(3) . ? Mn1 N10 2.261(3) . ? O2 C2 1.428(4) . ? N10 C10 1.327(4) . ? N10 C21 1.370(4) . ? N20 C19 1.323(4) . ? N20 C20 1.364(4) . ? N112 C111 1.153(4) . ? N114 C113 1.151(4) . ? N122 C121 1.147(4) . ? N122 Mn1 2.190(3) 2_545 ? N124 C123 1.153(4) . ? N132 C131 1.161(4) . ? N134 C133 1.160(4) . ? C10 C11 1.390(5) . ? C11 C12 1.371(5) . ? C12 C13 1.398(5) . ? C13 C21 1.394(5) . ? C13 C14 1.425(5) . ? C14 C15 1.352(5) . ? C15 C16 1.424(5) . ? C16 C17 1.400(5) . ? C16 C20 1.402(4) . ? C17 C18 1.363(5) . ? C18 C19 1.389(5) . ? C20 C21 1.448(5) . ? C101 C102 1.380(4) . ? C101 C103 1.387(5) . ? C101 C110 1.412(5) . ? C102 C103 1.387(4) . ? C102 C120 1.404(4) . ? C103 C130 1.391(4) . ? C110 C111 1.405(5) . ? C110 C113 1.420(5) . ? C120 C121 1.410(5) . ? C120 C123 1.414(5) . ? C130 C133 1.405(5) . ? C130 C131 1.415(5) . ? 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 N122 88.79(11) . 2 ? O1 Mn1 N112 90.97(11) . . ? N122 Mn1 N112 98.87(11) 2 . ? O1 Mn1 O2 178.26(11) . . ? N122 Mn1 O2 89.56(10) 2 . ? N112 Mn1 O2 88.74(10) . . ? O1 Mn1 N20 91.04(10) . . ? N122 Mn1 N20 168.29(11) 2 . ? N112 Mn1 N20 92.84(11) . . ? O2 Mn1 N20 90.69(10) . . ? O1 Mn1 N10 92.38(10) . . ? N122 Mn1 N10 93.91(11) 2 . ? N112 Mn1 N10 166.85(10) . . ? O2 Mn1 N10 88.28(10) . . ? N20 Mn1 N10 74.40(11) . . ? C2 O2 Mn1 127.6(2) . . ? C10 N10 C21 117.3(3) . . ? C10 N10 Mn1 128.0(2) . . ? C21 N10 Mn1 114.7(2) . . ? C19 N20 C20 117.3(3) . . ? C19 N20 Mn1 127.1(2) . . ? C20 N20 Mn1 115.5(2) . . ? C111 N112 Mn1 162.8(3) . . ? C121 N122 Mn1 172.7(3) . 2_545 ? N10 C10 C11 123.6(4) . . ? C12 C11 C10 118.9(4) . . ? C11 C12 C13 119.7(4) . . ? C21 C13 C12 117.6(3) . . ? C21 C13 C14 119.4(4) . . ? C12 C13 C14 122.9(4) . . ? C15 C14 C13 121.1(4) . . ? C14 C15 C16 121.0(4) . . ? C17 C16 C20 117.0(4) . . ? C17 C16 C15 123.4(4) . . ? C20 C16 C15 119.6(4) . . ? C18 C17 C16 120.2(4) . . ? C17 C18 C19 118.6(4) . . ? N20 C19 C18 123.9(4) . . ? N20 C20 C16 122.9(3) . . ? N20 C20 C21 118.0(3) . . ? C16 C20 C21 119.1(3) . . ? N10 C21 C13 122.9(3) . . ? N10 C21 C20 117.3(3) . . ? C13 C21 C20 119.8(3) . . ? C102 C101 C103 60.2(2) . . ? C102 C101 C110 147.5(3) . . ? C103 C101 C110 152.4(3) . . ? C101 C102 C103 60.2(2) . . ? C101 C102 C120 150.9(3) . . ? C103 C102 C120 148.8(3) . . ? C102 C103 C101 59.6(2) . . ? C102 C103 C130 147.1(3) . . ? C101 C103 C130 153.3(3) . . ? C111 C110 C101 122.4(3) . . ? C111 C110 C113 118.0(3) . . ? C101 C110 C113 119.5(3) . . ? N112 C111 C110 176.7(4) . . ? N114 C113 C110 179.0(4) . . ? C102 C120 C121 120.8(3) . . ? C102 C120 C123 120.5(3) . . ? C121 C120 C123 118.4(3) . . ? N122 C121 C120 179.4(4) . . ? N124 C123 C120 178.3(4) . . ? C103 C130 C133 119.7(3) . . ? C103 C130 C131 123.3(3) . . ? C133 C130 C131 117.0(3) . . ? N132 C131 C130 178.2(4) . . ? N134 C133 C130 179.8(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2O N114 0.861(18) 2.14(3) 2.865(4) 141(3) 2 O1 H1O N124 0.863(19) 1.97(2) 2.796(5) 161(5) 3_556 O2 H3O N134 0.865(18) 1.88(2) 2.741(4) 172(3) 3_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.426 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.106 data_5 _database_code_depnum_ccdc_archive 'CCDC 836018' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Mn(pypzH)(HCTMCP)(MeOH)(H2O)] ; _chemical_name_common (Mn(pypzH)(HCTMCP)(MeOH)(H2O)) _chemical_melting_point ? _chemical_formula_moiety 'C21 H13 Mn N9 O2' _chemical_formula_sum 'C21 H13 Mn N9 O2' _chemical_formula_weight 478.34 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.53130(10) _cell_length_b 15.9150(3) _cell_length_c 18.2438(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.7100(10) _cell_angle_gamma 90.00 _cell_volume 2161.50(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 26166 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8756 _exptl_absorpt_correction_T_max 0.9203 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26166 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4942 _reflns_number_gt 3411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 4942 _refine_ls_number_parameters 315 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.46170(5) 0.18102(2) 0.348283(18) 0.02148(11) Uani 1 1 d . . . O1 O 0.7363(2) 0.14258(11) 0.38654(10) 0.0314(4) Uani 1 1 d D . . O2 O 0.1852(2) 0.22606(11) 0.31148(10) 0.0375(4) Uani 1 1 d D . . N1 N 0.3996(2) 0.16494(11) 0.46379(10) 0.0232(4) Uani 1 1 d . . . N2 N 0.4137(3) 0.20913(14) 0.52807(12) 0.0322(5) Uani 1 1 d . . . N3 N 0.3503(2) 0.04944(11) 0.35380(10) 0.0228(4) Uani 1 1 d . . . N112 N 0.5389(3) 0.31321(11) 0.35740(10) 0.0259(4) Uani 1 1 d . . . N114 N 0.6814(3) 0.51042(12) 0.20308(11) 0.0336(5) Uani 1 1 d . . . N122 N 0.9953(3) 0.67253(11) 0.27041(11) 0.0265(4) Uani 1 1 d . . . N124 N 1.0620(3) 0.75295(12) 0.50749(11) 0.0317(5) Uani 1 1 d . . . N132 N 0.5960(3) 0.36999(14) 0.56807(12) 0.0382(5) Uani 1 1 d . . . N134 N 0.8907(3) 0.61039(14) 0.64377(12) 0.0409(6) Uani 1 1 d . . . C2 C 0.0547(4) 0.19807(18) 0.25376(17) 0.0471(7) Uani 1 1 d . . . H2A H 0.0862 0.2167 0.2062 0.071 Uiso 1 1 calc R . . H2B H -0.0625 0.2213 0.2601 0.071 Uiso 1 1 calc R . . H2C H 0.0491 0.1366 0.2546 0.071 Uiso 1 1 calc R . . C3 C 0.3471(3) 0.16338(18) 0.58247(13) 0.0404(7) Uani 1 1 d . . . H3 H 0.3422 0.1808 0.6319 0.048 Uiso 1 1 calc R . . C4 C 0.2887(3) 0.08684(15) 0.55063(13) 0.0289(5) Uani 1 1 d . . . H4 H 0.2361 0.0415 0.5735 0.035 Uiso 1 1 calc R . . C5 C 0.3245(3) 0.09127(13) 0.47784(12) 0.0217(5) Uani 1 1 d . . . C6 C 0.2965(3) 0.02806(13) 0.41861(12) 0.0219(5) Uani 1 1 d . . . C7 C 0.2229(3) -0.05057(14) 0.42781(14) 0.0311(6) Uani 1 1 d . . . H7 H 0.1861 -0.0653 0.4737 0.037 Uiso 1 1 calc R . . C8 C 0.2039(4) -0.10599(17) 0.37083(15) 0.0410(7) Uani 1 1 d . . . H8 H 0.1529 -0.1598 0.3764 0.049 Uiso 1 1 calc R . . C9 C 0.2570(3) -0.08479(15) 0.30709(15) 0.0360(6) Uani 1 1 d . . . H9 H 0.2444 -0.1232 0.2668 0.043 Uiso 1 1 calc R . . C10 C 0.3286(3) -0.00851(14) 0.30029(13) 0.0275(5) Uani 1 1 d . . . H10 H 0.3664 0.0052 0.2544 0.033 Uiso 1 1 calc R . . C101 C 0.7736(3) 0.52744(13) 0.46928(12) 0.0199(5) Uani 1 1 d . . . C102 C 0.8349(3) 0.58075(13) 0.41872(11) 0.0189(5) Uani 1 1 d . . . C103 C 0.7419(3) 0.50900(13) 0.39434(12) 0.0195(5) Uani 1 1 d . . . C110 C 0.6674(3) 0.45790(13) 0.33515(11) 0.0202(5) Uani 1 1 d . . . C111 C 0.5963(3) 0.37846(14) 0.34742(11) 0.0211(5) Uani 1 1 d . . . C113 C 0.6749(3) 0.48469(13) 0.26173(13) 0.0236(5) Uani 1 1 d . . . C120 C 0.9290(3) 0.65334(13) 0.40264(12) 0.0195(5) Uani 1 1 d . . . C121 C 0.9668(3) 0.66564(13) 0.33020(12) 0.0206(5) Uani 1 1 d . . . C123 C 1.0043(3) 0.70847(13) 0.46041(12) 0.0209(5) Uani 1 1 d . . . C130 C 0.7553(3) 0.50784(13) 0.54241(12) 0.0223(5) Uani 1 1 d . . . C131 C 0.6680(3) 0.43244(15) 0.55835(12) 0.0260(5) Uani 1 1 d . . . C133 C 0.8277(3) 0.56308(15) 0.59948(13) 0.0268(5) Uani 1 1 d . . . H1N H 0.469(4) 0.2582(18) 0.5302(15) 0.050(9) Uiso 1 1 d . . . H1O H 0.813(3) 0.1747(16) 0.4131(15) 0.055(9) Uiso 1 1 d D . . H2O H 0.791(4) 0.1062(16) 0.3648(16) 0.063(10) Uiso 1 1 d D . . H3O H 0.159(5) 0.2752(13) 0.3232(19) 0.080(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0288(2) 0.01618(17) 0.01897(18) 0.00094(14) 0.00192(14) -0.00185(15) O1 0.0307(10) 0.0305(10) 0.0308(10) -0.0146(8) -0.0029(8) 0.0031(8) O2 0.0365(11) 0.0336(10) 0.0378(10) -0.0118(8) -0.0093(8) 0.0087(9) N1 0.0306(11) 0.0190(10) 0.0198(10) -0.0026(7) 0.0033(8) 0.0012(8) N2 0.0325(12) 0.0264(11) 0.0353(13) -0.0098(10) -0.0025(10) 0.0023(10) N3 0.0288(11) 0.0186(9) 0.0204(10) 0.0010(8) 0.0015(8) -0.0024(8) N112 0.0346(11) 0.0197(10) 0.0225(10) 0.0016(8) 0.0012(8) -0.0038(9) N114 0.0507(14) 0.0265(11) 0.0232(11) -0.0025(9) 0.0049(10) -0.0106(10) N122 0.0333(11) 0.0228(10) 0.0229(11) -0.0010(8) 0.0026(9) -0.0043(9) N124 0.0372(12) 0.0276(11) 0.0288(11) -0.0045(9) 0.0004(10) -0.0044(9) N132 0.0344(12) 0.0362(13) 0.0458(14) 0.0147(10) 0.0119(11) 0.0040(11) N134 0.0428(14) 0.0458(14) 0.0317(12) -0.0134(11) -0.0018(11) 0.0121(11) C2 0.0403(17) 0.0395(16) 0.0560(19) -0.0008(14) -0.0101(14) -0.0047(13) C3 0.0354(15) 0.0660(19) 0.0186(13) -0.0076(13) 0.0003(11) 0.0220(14) C4 0.0318(14) 0.0295(13) 0.0260(13) 0.0078(10) 0.0066(11) 0.0030(11) C5 0.0239(12) 0.0203(11) 0.0199(11) 0.0032(9) 0.0007(10) 0.0032(10) C6 0.0228(12) 0.0202(11) 0.0220(12) 0.0030(9) 0.0013(9) 0.0018(9) C7 0.0334(14) 0.0260(13) 0.0341(14) 0.0071(11) 0.0053(11) -0.0020(11) C8 0.0449(17) 0.0311(14) 0.0445(17) -0.0014(13) -0.0016(13) -0.0008(13) C9 0.0358(15) 0.0248(13) 0.0454(17) -0.0046(12) 0.0003(13) 0.0020(11) C10 0.0295(13) 0.0293(13) 0.0231(12) -0.0057(10) 0.0014(10) -0.0004(11) C101 0.0178(11) 0.0183(11) 0.0230(12) -0.0012(9) 0.0013(9) 0.0042(9) C102 0.0210(12) 0.0171(11) 0.0184(11) -0.0016(9) 0.0022(9) 0.0038(9) C103 0.0197(11) 0.0182(11) 0.0208(11) 0.0010(9) 0.0038(9) 0.0018(9) C110 0.0260(12) 0.0164(11) 0.0180(11) 0.0008(9) 0.0026(9) -0.0024(9) C111 0.0240(12) 0.0239(12) 0.0146(11) -0.0028(9) 0.0008(9) 0.0025(10) C113 0.0262(13) 0.0166(11) 0.0278(13) -0.0068(10) 0.0033(10) -0.0052(9) C120 0.0232(12) 0.0154(10) 0.0192(11) -0.0017(9) 0.0005(9) -0.0004(9) C121 0.0227(12) 0.0156(11) 0.0221(13) -0.0020(9) -0.0009(10) -0.0011(9) C123 0.0235(12) 0.0187(11) 0.0205(12) 0.0023(9) 0.0030(10) 0.0010(9) C130 0.0228(12) 0.0227(11) 0.0214(12) 0.0016(9) 0.0034(9) 0.0040(9) C131 0.0242(13) 0.0306(13) 0.0239(12) 0.0054(10) 0.0057(10) 0.0095(11) C133 0.0288(13) 0.0312(13) 0.0207(12) 0.0002(10) 0.0049(10) 0.0108(11) _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 2.1683(18) . ? Mn1 N112 2.1822(19) . ? Mn1 O2 2.2089(18) . ? Mn1 N1 2.2413(18) . ? Mn1 N122 2.2415(19) 2_645 ? Mn1 N3 2.2639(18) . ? O1 H1O 0.864(17) . ? O1 H2O 0.842(17) . ? O2 C2 1.400(3) . ? O2 H3O 0.842(18) . ? N1 C5 1.343(3) . ? N1 N2 1.358(3) . ? N2 C3 1.385(3) . ? N2 H1N 0.88(3) . ? N3 C10 1.335(3) . ? N3 C6 1.350(3) . ? N112 C111 1.150(3) . ? N114 C113 1.154(3) . ? N122 C121 1.149(3) . ? N122 Mn1 2.2415(19) 2_655 ? N124 C123 1.147(3) . ? N132 C131 1.159(3) . ? N134 C133 1.153(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.392(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(3) . ? C4 H4 0.9500 . ? C5 C6 1.468(3) . ? C6 C7 1.389(3) . ? C7 C8 1.354(3) . ? C7 H7 0.9500 . ? C8 C9 1.329(4) . ? C8 H8 0.9500 . ? C9 C10 1.342(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C101 C102 1.383(3) . ? C101 C103 1.383(3) . ? C101 C130 1.397(3) . ? C102 C103 1.378(3) . ? C102 C120 1.409(3) . ? C103 C110 1.400(3) . ? C110 C111 1.404(3) . ? C110 C113 1.415(3) . ? C120 C121 1.407(3) . ? C120 C123 1.421(3) . ? C130 C133 1.408(3) . ? C130 C131 1.419(3) . ? 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 N112 90.99(7) . . ? O1 Mn1 O2 177.33(7) . . ? N112 Mn1 O2 86.47(7) . . ? O1 Mn1 N1 89.42(7) . . ? N112 Mn1 N1 97.44(7) . . ? O2 Mn1 N1 90.08(7) . . ? O1 Mn1 N122 91.36(7) . 2_645 ? N112 Mn1 N122 93.21(7) . 2_645 ? O2 Mn1 N122 89.62(7) . 2_645 ? N1 Mn1 N122 169.30(7) . 2_645 ? O1 Mn1 N3 93.82(7) . . ? N112 Mn1 N3 169.94(7) . . ? O2 Mn1 N3 88.56(7) . . ? N1 Mn1 N3 73.80(6) . . ? N122 Mn1 N3 95.50(7) 2_645 . ? Mn1 O1 H1O 123(2) . . ? Mn1 O1 H2O 123(2) . . ? H1O O1 H2O 110(3) . . ? C2 O2 Mn1 130.35(16) . . ? C2 O2 H3O 109(2) . . ? Mn1 O2 H3O 118(2) . . ? C5 N1 N2 105.51(18) . . ? C5 N1 Mn1 115.66(14) . . ? N2 N1 Mn1 138.83(15) . . ? N1 N2 C3 110.9(2) . . ? N1 N2 H1N 118.1(18) . . ? C3 N2 H1N 130.8(18) . . ? C10 N3 C6 116.53(18) . . ? C10 N3 Mn1 127.71(15) . . ? C6 N3 Mn1 115.75(14) . . ? C111 N112 Mn1 163.90(17) . . ? C121 N122 Mn1 176.79(18) . 2_655 ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 106.7(2) . . ? N2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C3 C4 C5 105.0(2) . . ? C3 C4 H4 127.5 . . ? C5 C4 H4 127.5 . . ? N1 C5 C4 111.91(19) . . ? N1 C5 C6 118.39(18) . . ? C4 C5 C6 129.7(2) . . ? N3 C6 C7 120.7(2) . . ? N3 C6 C5 116.30(18) . . ? C7 C6 C5 123.0(2) . . ? C8 C7 C6 119.4(2) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.3(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N3 C10 C9 124.3(2) . . ? N3 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? C102 C101 C103 59.73(15) . . ? C102 C101 C130 149.9(2) . . ? C103 C101 C130 150.4(2) . . ? C103 C102 C101 60.14(15) . . ? C103 C102 C120 149.3(2) . . ? C101 C102 C120 150.6(2) . . ? C102 C103 C101 60.13(15) . . ? C102 C103 C110 148.8(2) . . ? C101 C103 C110 151.0(2) . . ? C103 C110 C111 121.21(19) . . ? C103 C110 C113 119.10(19) . . ? C111 C110 C113 119.55(19) . . ? N112 C111 C110 179.6(2) . . ? N114 C113 C110 176.7(2) . . ? C121 C120 C102 119.27(18) . . ? C121 C120 C123 119.74(19) . . ? C102 C120 C123 120.55(19) . . ? N122 C121 C120 177.3(2) . . ? N124 C123 C120 178.7(2) . . ? C101 C130 C133 118.9(2) . . ? C101 C130 C131 120.0(2) . . ? C133 C130 C131 121.0(2) . . ? N132 C131 C130 177.0(2) . . ? N134 C133 C130 176.8(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2O N114 0.842(17) 1.99(2) 2.791(3) 157(3) 2_645 O1 H1O N124 0.864(17) 1.974(19) 2.814(3) 164(3) 3_766 O2 H3O N134 0.842(18) 1.972(19) 2.812(3) 177(4) 3_666 N2 H1N N132 0.88(3) 2.09(3) 2.944(3) 163(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.590 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.064 data_6Co _database_code_depnum_ccdc_archive 'CCDC 836019' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Co(pypzH)(HCTMCP)(MeOH)2] ; _chemical_name_common (Co(pypzH)(HCTMCP)(MeOH)2) _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 Co N9 O2' _chemical_formula_sum 'C22 H15 Co N9 O2' _chemical_formula_weight 496.36 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0169(2) _cell_length_b 15.3911(3) _cell_length_c 18.0902(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.7400(10) _cell_angle_gamma 90.00 _cell_volume 2206.21(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 24344 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8093 _exptl_absorpt_correction_T_max 0.8871 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24344 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5018 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 5018 _refine_ls_number_parameters 321 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.37187(6) 0.33342(3) 0.34801(3) 0.01992(14) Uani 1 1 d . . . O1 O 0.1639(3) 0.36874(17) 0.39973(14) 0.0263(6) Uani 1 1 d D . . O2 O 0.5845(3) 0.29065(18) 0.30208(15) 0.0316(6) Uani 1 1 d D . . N1 N 0.5276(4) 0.33877(19) 0.45315(15) 0.0225(6) Uani 1 1 d . . . N2 N 0.5729(5) 0.2878(3) 0.5135(2) 0.0385(9) Uani 1 1 d . . . N3 N 0.4744(4) 0.46010(19) 0.34698(16) 0.0229(7) Uani 1 1 d . . . N112 N 0.3023(4) 0.2042(2) 0.35631(16) 0.0268(7) Uani 1 1 d . . . N114 N -0.0613(6) 0.0619(4) 0.2083(2) 0.0783(16) Uani 1 1 d . . . N122 N -0.2291(4) -0.15594(19) 0.25979(16) 0.0245(7) Uani 1 1 d . . . N124 N -0.1029(5) -0.2635(2) 0.48440(19) 0.0397(9) Uani 1 1 d . . . N132 N 0.4471(5) 0.1147(3) 0.5589(2) 0.0522(11) Uani 1 1 d . . . N134 N 0.2687(5) -0.1439(3) 0.6287(2) 0.0528(11) Uani 1 1 d . . . C1 C -0.0072(6) 0.3621(4) 0.3631(3) 0.0569(14) Uani 1 1 d . . . H1A H -0.0235 0.3061 0.3372 0.085 Uiso 1 1 calc R . . H1B H -0.0312 0.4093 0.3268 0.085 Uiso 1 1 calc R . . H1C H -0.0837 0.3662 0.4004 0.085 Uiso 1 1 calc R . . C2 C 0.6395(6) 0.3142(3) 0.2348(3) 0.0507(13) Uani 1 1 d . . . H2A H 0.6677 0.3762 0.2361 0.076 Uiso 1 1 calc R . . H2B H 0.5496 0.3027 0.1929 0.076 Uiso 1 1 calc R . . H2C H 0.7397 0.2802 0.2286 0.076 Uiso 1 1 calc R . . C3 C 0.6988(6) 0.3288(4) 0.5649(2) 0.0554(14) Uani 1 1 d . . . H3 H 0.7529 0.3061 0.6112 0.067 Uiso 1 1 calc R . . C4 C 0.7282(5) 0.4109(3) 0.5331(2) 0.0342(9) Uani 1 1 d . . . H4 H 0.8040 0.4551 0.5537 0.041 Uiso 1 1 calc R . . C5 C 0.6206(4) 0.4118(2) 0.4647(2) 0.0239(8) Uani 1 1 d . . . C6 C 0.5952(4) 0.4781(2) 0.40555(19) 0.0236(8) Uani 1 1 d . . . C7 C 0.6861(5) 0.5544(3) 0.4067(3) 0.0385(10) Uani 1 1 d . . . H7 H 0.7693 0.5675 0.4484 0.046 Uiso 1 1 calc R . . C8 C 0.6578(7) 0.6096(3) 0.3497(3) 0.0553(13) Uani 1 1 d . . . H8 H 0.7213 0.6618 0.3505 0.066 Uiso 1 1 calc R . . C9 C 0.5429(6) 0.5920(3) 0.2930(3) 0.0476(12) Uani 1 1 d . . . H9 H 0.5232 0.6308 0.2518 0.057 Uiso 1 1 calc R . . C10 C 0.4531(5) 0.5195(2) 0.2931(2) 0.0305(9) Uani 1 1 d . . . H10 H 0.3674 0.5094 0.2516 0.037 Uiso 1 1 calc R . . C101 C 0.1272(4) -0.0003(2) 0.38815(19) 0.0211(7) Uani 1 1 d . . . C102 C 0.0626(4) -0.0787(2) 0.40774(18) 0.0205(7) Uani 1 1 d . . . C103 C 0.1742(4) -0.0333(2) 0.45954(19) 0.0209(7) Uani 1 1 d . . . C110 C 0.1314(5) 0.0650(2) 0.33472(19) 0.0254(8) Uani 1 1 d . . . C111 C 0.2269(4) 0.1407(2) 0.34915(19) 0.0215(7) Uani 1 1 d . . . C113 C 0.0243(6) 0.0617(3) 0.2650(2) 0.0427(11) Uani 1 1 d . . . C120 C -0.0464(4) -0.1492(2) 0.38853(19) 0.0205(7) Uani 1 1 d . . . C121 C -0.1471(4) -0.1530(2) 0.3175(2) 0.0200(7) Uani 1 1 d . . . C123 C -0.0763(5) -0.2120(2) 0.4419(2) 0.0258(8) Uani 1 1 d . . . C130 C 0.2666(5) -0.0235(2) 0.5309(2) 0.0263(8) Uani 1 1 d . . . C131 C 0.3681(5) 0.0519(3) 0.5479(2) 0.0339(10) Uani 1 1 d . . . C133 C 0.2679(5) -0.0896(3) 0.5851(2) 0.0335(9) Uani 1 1 d . . . H1N H 0.521(7) 0.236(4) 0.513(3) 0.067(17) Uiso 1 1 d . . . H1O H 0.165(6) 0.334(3) 0.4374(19) 0.055(15) Uiso 1 1 d D . . H2O H 0.640(5) 0.247(2) 0.319(2) 0.052(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0231(3) 0.0186(2) 0.0181(2) 0.0006(2) 0.00307(17) -0.0032(2) O1 0.0264(14) 0.0288(14) 0.0248(14) 0.0038(11) 0.0071(11) -0.0001(11) O2 0.0332(16) 0.0333(16) 0.0307(15) 0.0086(12) 0.0126(12) 0.0099(13) N1 0.0259(16) 0.0208(15) 0.0197(14) 0.0021(13) -0.0001(12) 0.0001(13) N2 0.040(2) 0.040(2) 0.038(2) 0.0116(17) 0.0131(17) 0.0067(17) N3 0.0275(17) 0.0209(16) 0.0212(15) 0.0016(12) 0.0062(13) -0.0042(13) N112 0.0301(17) 0.0245(17) 0.0249(16) 0.0043(13) 0.0015(13) -0.0039(14) N114 0.071(3) 0.119(4) 0.037(2) 0.013(3) -0.014(2) -0.046(3) N122 0.0296(17) 0.0223(17) 0.0208(16) -0.0029(13) 0.0007(13) -0.0025(13) N124 0.053(2) 0.034(2) 0.0337(19) 0.0093(16) 0.0105(17) -0.0071(17) N132 0.032(2) 0.062(3) 0.063(3) -0.034(2) 0.0108(19) -0.011(2) N134 0.057(3) 0.060(3) 0.042(2) 0.019(2) 0.0102(19) 0.026(2) C1 0.035(3) 0.084(4) 0.053(3) 0.016(3) 0.010(2) 0.009(3) C2 0.055(3) 0.062(3) 0.041(3) 0.007(2) 0.025(2) 0.011(2) C3 0.053(3) 0.095(4) 0.018(2) 0.013(2) 0.007(2) 0.035(3) C4 0.028(2) 0.045(3) 0.028(2) -0.0090(19) -0.0019(17) -0.0029(18) C5 0.0232(19) 0.026(2) 0.0232(18) -0.0050(15) 0.0060(15) 0.0003(15) C6 0.0238(19) 0.025(2) 0.0238(18) -0.0030(15) 0.0083(15) -0.0008(15) C7 0.039(3) 0.031(2) 0.047(3) -0.005(2) 0.011(2) -0.0059(19) C8 0.070(4) 0.046(3) 0.053(3) 0.004(2) 0.020(3) 0.001(3) C9 0.049(3) 0.034(3) 0.064(3) 0.004(2) 0.022(3) 0.000(2) C10 0.033(2) 0.032(2) 0.028(2) 0.0106(17) 0.0081(17) 0.0021(17) C101 0.0194(18) 0.0211(18) 0.0229(18) -0.0028(14) 0.0039(14) -0.0015(14) C102 0.0204(18) 0.0227(19) 0.0189(17) 0.0012(14) 0.0041(14) 0.0020(14) C103 0.0200(18) 0.0219(18) 0.0219(18) -0.0030(14) 0.0065(14) 0.0020(14) C110 0.029(2) 0.025(2) 0.0218(18) 0.0044(15) 0.0018(15) -0.0088(16) C111 0.0195(18) 0.0251(19) 0.0195(17) 0.0049(14) 0.0021(14) 0.0008(15) C113 0.046(3) 0.051(3) 0.030(2) 0.006(2) 0.001(2) -0.022(2) C120 0.0232(18) 0.0189(19) 0.0203(17) 0.0016(14) 0.0057(14) -0.0021(14) C121 0.0221(18) 0.0147(18) 0.0249(18) -0.0006(14) 0.0090(15) -0.0021(13) C123 0.027(2) 0.025(2) 0.0248(19) -0.0046(16) 0.0034(16) -0.0024(16) C130 0.0219(19) 0.034(2) 0.0229(19) -0.0041(16) 0.0040(15) 0.0032(16) C131 0.021(2) 0.048(3) 0.032(2) -0.0162(19) 0.0055(17) 0.0030(19) C133 0.030(2) 0.046(3) 0.024(2) -0.0002(19) 0.0010(17) 0.0159(18) _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 Co1 N112 2.078(3) . ? Co1 O1 2.104(2) . ? Co1 O2 2.112(3) . ? Co1 N122 2.112(3) 2 ? Co1 N1 2.112(3) . ? Co1 N3 2.117(3) . ? O1 C1 1.433(5) . ? O1 H1O 0.866(19) . ? O2 C2 1.403(5) . ? O2 H2O 0.843(19) . ? N1 C5 1.347(5) . ? N1 N2 1.349(4) . ? N2 C3 1.412(6) . ? N2 H1N 0.90(5) . ? N3 C10 1.329(4) . ? N3 C6 1.351(4) . ? N112 C111 1.146(4) . ? N114 C113 1.145(6) . ? N122 C121 1.147(4) . ? N122 Co1 2.112(3) 2_545 ? N124 C123 1.147(5) . ? N132 C131 1.156(5) . ? N134 C133 1.149(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.423(7) . ? C3 H3 0.9500 . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.469(5) . ? C6 C7 1.381(5) . ? C7 C8 1.328(6) . ? C7 H7 0.9500 . ? C8 C9 1.299(7) . ? C8 H8 0.9500 . ? C9 C10 1.329(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C101 C102 1.380(5) . ? C101 C103 1.386(5) . ? C101 C110 1.398(5) . ? C102 C103 1.383(5) . ? C102 C120 1.403(5) . ? C103 C130 1.395(5) . ? C110 C111 1.397(5) . ? C110 C113 1.415(5) . ? C120 C121 1.411(5) . ? C120 C123 1.413(5) . ? C130 C133 1.411(6) . ? C130 C131 1.424(6) . ? 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 N112 Co1 O1 88.60(11) . . ? N112 Co1 O2 88.38(12) . . ? O1 Co1 O2 175.77(10) . . ? N112 Co1 N122 91.56(12) . 2 ? O1 Co1 N122 92.05(11) . 2 ? O2 Co1 N122 90.99(11) . 2 ? N112 Co1 N1 95.78(11) . . ? O1 Co1 N1 89.40(11) . . ? O2 Co1 N1 87.96(11) . . ? N122 Co1 N1 172.55(11) 2 . ? N112 Co1 N3 172.43(12) . . ? O1 Co1 N3 95.80(11) . . ? O2 Co1 N3 86.89(11) . . ? N122 Co1 N3 94.42(11) 2 . ? N1 Co1 N3 78.16(11) . . ? C1 O1 Co1 122.9(3) . . ? C1 O1 H1O 102(3) . . ? Co1 O1 H1O 106(3) . . ? C2 O2 Co1 129.8(3) . . ? C2 O2 H2O 107(3) . . ? Co1 O2 H2O 122(3) . . ? C5 N1 N2 106.6(3) . . ? C5 N1 Co1 114.1(2) . . ? N2 N1 Co1 139.1(3) . . ? N1 N2 C3 110.5(4) . . ? N1 N2 H1N 116(3) . . ? C3 N2 H1N 133(3) . . ? C10 N3 C6 115.6(3) . . ? C10 N3 Co1 129.3(3) . . ? C6 N3 Co1 114.5(2) . . ? C111 N112 Co1 162.0(3) . . ? C121 N122 Co1 177.0(3) . 2_545 ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 106.1(3) . . ? N2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? C5 C4 C3 104.4(4) . . ? C5 C4 H4 127.8 . . ? C3 C4 H4 127.8 . . ? N1 C5 C4 112.4(3) . . ? N1 C5 C6 117.0(3) . . ? C4 C5 C6 130.5(4) . . ? N3 C6 C7 120.0(3) . . ? N3 C6 C5 115.6(3) . . ? C7 C6 C5 124.4(4) . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.8(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.6(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 N3 124.7(4) . . ? C9 C10 H10 117.7 . . ? N3 C10 H10 117.7 . . ? C102 C101 C103 60.0(2) . . ? C102 C101 C110 148.8(3) . . ? C103 C101 C110 151.2(3) . . ? C101 C102 C103 60.2(2) . . ? C101 C102 C120 148.9(3) . . ? C103 C102 C120 150.8(3) . . ? C102 C103 C101 59.8(2) . . ? C102 C103 C130 151.6(3) . . ? C101 C103 C130 148.6(3) . . ? C111 C110 C101 122.7(3) . . ? C111 C110 C113 115.9(3) . . ? C101 C110 C113 121.0(3) . . ? N112 C111 C110 175.7(4) . . ? N114 C113 C110 177.7(5) . . ? C102 C120 C121 120.4(3) . . ? C102 C120 C123 121.6(3) . . ? C121 C120 C123 117.5(3) . . ? N122 C121 C120 179.8(4) . . ? N124 C123 C120 178.8(4) . . ? C103 C130 C133 120.7(3) . . ? C103 C130 C131 119.6(3) . . ? C133 C130 C131 119.5(3) . . ? N132 C131 C130 177.0(5) . . ? N134 C133 C130 179.4(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1N N132 0.90(5) 2.16(6) 3.006(6) 156(5) . O1 H1O N124 0.866(19) 1.91(2) 2.751(4) 165(5) 3_556 O2 H2O N134 0.843(19) 1.93(2) 2.759(5) 168(5) 3_656 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.079 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.084 data_6Fe _database_code_depnum_ccdc_archive 'CCDC 836020' #TrackingRef '- Batten.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe(pypzH)(HCTMCP)(MeOH)2] ; _chemical_name_common (Fe(pypzH)(HCTMCP)(MeOH)2) _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 Fe N9 O2' _chemical_formula_sum 'C22 H15 Fe N9 O2' _chemical_formula_weight 493.28 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9896(16) _cell_length_b 15.532(3) _cell_length_c 18.130(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.89(3) _cell_angle_gamma 90.00 _cell_volume 2222.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 25397 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 27.49 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7719 _exptl_absorpt_correction_T_max 0.8696 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25397 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5098 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 5098 _refine_ls_number_parameters 321 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Fe1 Fe 0.36886(5) 0.33352(2) 0.34802(2) 0.01914(12) Uani 1 1 d . . . O1 O 0.1573(2) 0.36808(13) 0.39948(11) 0.0247(4) Uani 1 1 d D . . O2 O 0.5858(3) 0.28993(14) 0.30299(11) 0.0279(5) Uani 1 1 d D . . N1 N 0.5282(3) 0.34099(15) 0.45484(12) 0.0216(5) Uani 1 1 d . . . N2 N 0.5735(4) 0.29148(19) 0.51618(15) 0.0340(6) Uani 1 1 d . . . N3 N 0.4795(3) 0.46072(15) 0.34729(12) 0.0213(5) Uani 1 1 d . . . N112 N 0.2950(3) 0.20369(15) 0.35560(13) 0.0251(5) Uani 1 1 d . . . N114 N -0.0682(5) 0.0592(3) 0.20964(18) 0.0655(11) Uani 1 1 d . . . N122 N -0.2254(3) -0.15638(15) 0.26201(13) 0.0238(5) Uani 1 1 d . . . N124 N -0.0949(4) -0.26391(18) 0.48562(15) 0.0366(6) Uani 1 1 d . . . N132 N 0.4452(4) 0.1191(2) 0.55763(18) 0.0446(8) Uani 1 1 d . . . N134 N 0.2820(4) -0.1398(2) 0.63002(17) 0.0472(8) Uani 1 1 d . . . C1 C -0.0146(4) 0.3612(3) 0.3616(2) 0.0493(10) Uani 1 1 d . . . H1A H -0.0309 0.3050 0.3369 0.074 Uiso 1 1 calc R . . H1B H -0.0369 0.4070 0.3242 0.074 Uiso 1 1 calc R . . H1C H -0.0929 0.3668 0.3980 0.074 Uiso 1 1 calc R . . C2 C 0.6356(5) 0.3097(3) 0.23345(19) 0.0439(9) Uani 1 1 d . . . H2A H 0.6548 0.3718 0.2303 0.066 Uiso 1 1 calc R . . H2B H 0.5462 0.2921 0.1930 0.066 Uiso 1 1 calc R . . H2C H 0.7404 0.2788 0.2288 0.066 Uiso 1 1 calc R . . C3 C 0.6962(5) 0.3333(3) 0.56687(17) 0.0439(9) Uani 1 1 d . . . H3 H 0.7484 0.3120 0.6140 0.053 Uiso 1 1 calc R . . C4 C 0.7278(4) 0.4129(2) 0.53494(16) 0.0294(7) Uani 1 1 d . . . H4 H 0.8043 0.4566 0.5554 0.035 Uiso 1 1 calc R . . C5 C 0.6211(3) 0.41321(18) 0.46615(15) 0.0209(6) Uani 1 1 d . . . C6 C 0.5993(3) 0.47861(17) 0.40672(15) 0.0202(5) Uani 1 1 d . . . C7 C 0.6937(4) 0.5535(2) 0.40864(19) 0.0337(7) Uani 1 1 d . . . H7 H 0.7763 0.5658 0.4509 0.040 Uiso 1 1 calc R . . C8 C 0.6689(5) 0.6086(2) 0.3511(2) 0.0469(9) Uani 1 1 d . . . H8 H 0.7338 0.6600 0.3523 0.056 Uiso 1 1 calc R . . C9 C 0.5530(5) 0.5908(2) 0.2926(2) 0.0415(8) Uani 1 1 d . . . H9 H 0.5358 0.6287 0.2509 0.050 Uiso 1 1 calc R . . C10 C 0.4607(4) 0.5191(2) 0.29260(17) 0.0285(6) Uani 1 1 d . . . H10 H 0.3756 0.5090 0.2508 0.034 Uiso 1 1 calc R . . C101 C 0.1256(3) 0.00016(17) 0.38989(15) 0.0199(5) Uani 1 1 d . . . C102 C 0.0650(3) -0.07811(17) 0.41020(14) 0.0193(5) Uani 1 1 d . . . C103 C 0.1772(3) -0.03166(17) 0.46118(15) 0.0198(5) Uani 1 1 d . . . C110 C 0.1262(4) 0.06423(18) 0.33588(15) 0.0247(6) Uani 1 1 d . . . C111 C 0.2207(3) 0.14012(18) 0.34952(15) 0.0216(6) Uani 1 1 d . . . C113 C 0.0183(4) 0.0598(2) 0.26628(18) 0.0382(8) Uani 1 1 d . . . C120 C -0.0415(3) -0.14935(17) 0.39092(15) 0.0197(5) Uani 1 1 d . . . C121 C -0.1428(3) -0.15329(17) 0.32010(15) 0.0196(5) Uani 1 1 d . . . C123 C -0.0689(4) -0.21233(18) 0.44406(16) 0.0237(6) Uani 1 1 d . . . C130 C 0.2716(3) -0.02055(19) 0.53222(15) 0.0232(6) Uani 1 1 d . . . C131 C 0.3696(4) 0.0556(2) 0.54773(17) 0.0295(7) Uani 1 1 d . . . C133 C 0.2776(4) -0.0860(2) 0.58625(17) 0.0309(7) Uani 1 1 d . . . H1N H 0.525(5) 0.240(3) 0.516(2) 0.052(12) Uiso 1 1 d . . . H1O H 0.156(5) 0.336(2) 0.4377(17) 0.060(13) Uiso 1 1 d D . . H2O H 0.631(5) 0.2440(18) 0.321(2) 0.056(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0211(2) 0.0179(2) 0.01775(19) -0.00035(16) 0.00120(14) -0.00322(15) O1 0.0246(10) 0.0272(11) 0.0222(10) 0.0032(9) 0.0032(8) -0.0012(8) O2 0.0286(11) 0.0293(12) 0.0267(11) 0.0045(9) 0.0068(9) 0.0054(9) N1 0.0254(12) 0.0192(11) 0.0189(11) 0.0017(9) -0.0003(9) -0.0006(9) N2 0.0347(15) 0.0340(15) 0.0341(15) 0.0117(12) 0.0081(12) 0.0042(12) N3 0.0251(12) 0.0197(11) 0.0190(11) 0.0000(9) 0.0033(9) -0.0030(9) N112 0.0308(13) 0.0206(12) 0.0229(12) 0.0034(10) 0.0008(10) -0.0039(10) N114 0.064(2) 0.092(3) 0.0334(17) 0.0069(18) -0.0138(16) -0.033(2) N122 0.0279(12) 0.0208(12) 0.0217(12) -0.0010(10) 0.0003(10) -0.0019(10) N124 0.0476(17) 0.0308(15) 0.0320(14) 0.0068(12) 0.0083(12) -0.0072(12) N132 0.0302(15) 0.0515(19) 0.0525(18) -0.0263(16) 0.0078(13) -0.0093(14) N134 0.0493(18) 0.056(2) 0.0355(16) 0.0150(15) 0.0038(13) 0.0228(15) C1 0.0311(18) 0.072(3) 0.045(2) 0.011(2) 0.0056(15) 0.0079(18) C2 0.048(2) 0.054(2) 0.0332(18) 0.0009(16) 0.0164(16) 0.0057(17) C3 0.045(2) 0.068(3) 0.0183(14) 0.0080(16) 0.0037(13) 0.0212(19) C4 0.0252(15) 0.0345(17) 0.0256(15) -0.0087(13) -0.0055(12) 0.0008(12) C5 0.0172(12) 0.0242(14) 0.0211(13) -0.0040(11) 0.0025(10) -0.0005(10) C6 0.0203(13) 0.0203(13) 0.0206(13) -0.0033(11) 0.0049(10) -0.0001(10) C7 0.0340(17) 0.0271(16) 0.0407(18) -0.0061(14) 0.0081(14) -0.0056(13) C8 0.060(2) 0.0351(19) 0.048(2) 0.0043(17) 0.0154(19) -0.0021(17) C9 0.044(2) 0.0286(17) 0.055(2) 0.0039(16) 0.0153(17) -0.0011(15) C10 0.0280(15) 0.0320(16) 0.0251(15) 0.0104(13) 0.0029(12) 0.0026(12) C101 0.0192(13) 0.0200(13) 0.0204(13) -0.0021(11) 0.0023(10) -0.0014(10) C102 0.0181(12) 0.0213(13) 0.0185(13) 0.0000(11) 0.0024(10) 0.0018(10) C103 0.0186(12) 0.0203(13) 0.0209(13) -0.0025(11) 0.0037(10) 0.0006(10) C110 0.0271(14) 0.0235(14) 0.0219(14) 0.0022(12) -0.0014(11) -0.0080(12) C111 0.0210(13) 0.0238(14) 0.0188(13) 0.0051(11) -0.0005(10) 0.0010(11) C113 0.0394(18) 0.044(2) 0.0295(17) 0.0059(15) -0.0014(14) -0.0190(15) C120 0.0222(13) 0.0179(13) 0.0189(13) 0.0008(10) 0.0032(10) -0.0022(10) C121 0.0220(13) 0.0158(13) 0.0218(13) -0.0014(10) 0.0058(11) -0.0026(10) C123 0.0271(14) 0.0219(14) 0.0219(14) -0.0031(12) 0.0032(11) -0.0042(11) C130 0.0215(13) 0.0279(15) 0.0198(13) -0.0034(11) 0.0017(10) 0.0032(11) C131 0.0193(14) 0.0417(19) 0.0267(15) -0.0119(14) 0.0017(11) 0.0016(13) C133 0.0257(15) 0.0417(18) 0.0237(15) -0.0011(14) -0.0014(12) 0.0130(13) _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 Fe1 N112 2.112(2) . ? Fe1 O1 2.122(2) . ? Fe1 O2 2.137(2) . ? Fe1 N122 2.147(2) 2 ? Fe1 N1 2.150(2) . ? Fe1 N3 2.165(2) . ? O1 C1 1.441(4) . ? O1 H1O 0.859(19) . ? O2 C2 1.413(4) . ? O2 H2O 0.839(19) . ? N1 C5 1.343(4) . ? N1 N2 1.354(3) . ? N2 C3 1.396(5) . ? N2 H1N 0.89(4) . ? N3 C10 1.335(4) . ? N3 C6 1.355(3) . ? N112 C111 1.149(4) . ? N114 C113 1.146(4) . ? N122 C121 1.154(4) . ? N122 Fe1 2.147(2) 2_545 ? N124 C123 1.141(4) . ? N132 C131 1.156(4) . ? N134 C133 1.150(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.405(5) . ? C3 H3 0.9500 . ? C4 C5 1.398(4) . ? C4 H4 0.9500 . ? C5 C6 1.471(4) . ? C6 C7 1.383(4) . ? C7 C8 1.341(5) . ? C7 H7 0.9500 . ? C8 C9 1.325(5) . ? C8 H8 0.9500 . ? C9 C10 1.336(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C101 C102 1.380(4) . ? C101 C103 1.386(4) . ? C101 C110 1.397(4) . ? C102 C103 1.387(4) . ? C102 C120 1.407(4) . ? C103 C130 1.399(4) . ? C110 C111 1.401(4) . ? C110 C113 1.415(4) . ? C120 C121 1.409(4) . ? C120 C123 1.413(4) . ? C130 C133 1.407(4) . ? C130 C131 1.422(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N112 Fe1 O1 87.90(9) . . ? N112 Fe1 O2 88.48(9) . . ? O1 Fe1 O2 175.09(8) . . ? N112 Fe1 N122 90.90(9) . 2 ? O1 Fe1 N122 92.46(9) . 2 ? O2 Fe1 N122 90.92(9) . 2 ? N112 Fe1 N1 97.21(9) . . ? O1 Fe1 N1 89.51(8) . . ? O2 Fe1 N1 87.64(9) . . ? N122 Fe1 N1 171.72(9) 2 . ? N112 Fe1 N3 171.98(9) . . ? O1 Fe1 N3 97.22(8) . . ? O2 Fe1 N3 86.03(9) . . ? N122 Fe1 N3 95.02(9) 2 . ? N1 Fe1 N3 76.75(9) . . ? C1 O1 Fe1 122.5(2) . . ? C1 O1 H1O 102(3) . . ? Fe1 O1 H1O 109(3) . . ? C2 O2 Fe1 129.0(2) . . ? C2 O2 H2O 111(3) . . ? Fe1 O2 H2O 117(3) . . ? C5 N1 N2 106.1(2) . . ? C5 N1 Fe1 114.76(18) . . ? N2 N1 Fe1 139.0(2) . . ? N1 N2 C3 110.3(3) . . ? N1 N2 H1N 117(3) . . ? C3 N2 H1N 133(3) . . ? C10 N3 C6 115.8(2) . . ? C10 N3 Fe1 128.7(2) . . ? C6 N3 Fe1 114.91(18) . . ? C111 N112 Fe1 163.8(2) . . ? C121 N122 Fe1 176.9(2) . 2_545 ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 106.9(3) . . ? N2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 C3 104.3(3) . . ? C5 C4 H4 127.9 . . ? C3 C4 H4 127.9 . . ? N1 C5 C4 112.3(3) . . ? N1 C5 C6 117.7(2) . . ? C4 C5 C6 130.0(3) . . ? N3 C6 C7 120.5(3) . . ? N3 C6 C5 115.5(2) . . ? C7 C6 C5 124.0(3) . . ? C8 C7 C6 120.2(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 N3 124.6(3) . . ? C9 C10 H10 117.7 . . ? N3 C10 H10 117.7 . . ? C102 C101 C103 60.19(19) . . ? C102 C101 C110 148.7(3) . . ? C103 C101 C110 151.1(3) . . ? C101 C102 C103 60.12(19) . . ? C101 C102 C120 148.3(3) . . ? C103 C102 C120 151.5(3) . . ? C101 C103 C102 59.69(19) . . ? C101 C103 C130 148.8(3) . . ? C102 C103 C130 151.5(3) . . ? C101 C110 C111 122.4(3) . . ? C101 C110 C113 121.5(3) . . ? C111 C110 C113 115.8(3) . . ? N112 C111 C110 175.3(3) . . ? N114 C113 C110 177.7(4) . . ? C102 C120 C121 120.0(2) . . ? C102 C120 C123 121.8(2) . . ? C121 C120 C123 117.6(2) . . ? N122 C121 C120 179.8(3) . . ? N124 C123 C120 178.1(3) . . ? C103 C130 C133 120.5(3) . . ? C103 C130 C131 119.1(3) . . ? C133 C130 C131 120.3(3) . . ? N132 C131 C130 177.0(4) . . ? N134 C133 C130 179.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1N N132 0.89(4) 2.15(4) 3.004(4) 160(4) . O1 H1O N124 0.859(19) 1.90(2) 2.744(3) 166(4) 3_556 O2 H2O N134 0.839(19) 1.93(2) 2.762(4) 173(4) 3_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.035 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.075