Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Loeb, Stephen J.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; 'Davidson, Gregory J. E.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; 'Parekh, Neil A.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; 'Wisner, James A.' ; School of Physical Sciences Chemistry and Biochemistry University of Windsor Ontario N9B 3P4 Canada ; _publ_contact_author_name 'Prof Stephen Loeb' _publ_contact_author_address ; Chemistry & Biochemistry University of Windsor School of Physical Sciences Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email 'loeb@uwindsor.ca' _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; These structures are part of a study investigating the utility of anionic tranistion metal fragments [MBr3]- (M = Co(II), Mn(II)) as stoppers for rotaxanes ; _publ_section_title ; Zwitterionic [2]rotaxanes utilising anionic transition metal stoppers ; data_CoBr3_stoppered_[2]rotaxane _database_code_CSD 168751 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Br6 Co2 N4 O8' _chemical_formula_weight 1386.24 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca #(61) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.7244(2) _cell_length_b 14.7931(3) _cell_length_c 20.5958(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5400.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour 'emerald green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 5.105 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0533 _exptl_absorpt_correction_T_max 0.0886 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens SMART CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 18217 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4027 _reflns_number_gt 1857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL XP' _computing_publication_material 'Siemens SHELXTL XCIF' _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_number_reflns 4027 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1852 _refine_ls_R_factor_gt 0.1198 _refine_ls_wR_factor_ref 0.3532 _refine_ls_wR_factor_gt 0.3007 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.006 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 -0.08093(12) 0.60901(14) -0.13585(9) 0.0916(7) Uani 1 1 d . . . Br1 Br -0.14334(13) 0.46776(14) -0.12670(10) 0.1280(8) Uani 1 1 d . . . Br2 Br -0.10460(13) 0.71188(13) -0.04847(9) 0.1218(8) Uani 1 1 d . . . Br3 Br -0.09080(12) 0.67025(13) -0.24200(9) 0.1197(8) Uani 1 1 d . . . O1 O 0.5638(7) 0.6213(6) 0.1420(4) 0.094(3) Uani 1 1 d . . . O2 O 0.4247(7) 0.5156(8) 0.1564(6) 0.116(4) Uani 1 1 d . . . O3 O 0.3933(12) 0.3518(10) 0.1042(7) 0.171(8) Uani 1 1 d . . . O4 O 0.6292(7) 0.6710(7) 0.0351(6) 0.107(3) Uani 1 1 d . . . N1 N 0.0312(7) 0.5817(9) -0.1256(6) 0.090(3) Uani 1 1 d . . . N2 N 0.4113(6) 0.5538(7) -0.0292(5) 0.072(3) Uani 1 1 d . . . C1 C 0.0823(9) 0.6341(10) -0.1524(7) 0.084(4) Uani 1 1 d . . . H1A H 0.0672 0.6792 -0.1811 0.101 Uiso 1 1 calc R . . C2 C 0.1584(10) 0.6233(10) -0.1388(7) 0.092(5) Uani 1 1 d . . . H2A H 0.1933 0.6590 -0.1607 0.111 Uiso 1 1 calc R . . C3 C 0.1850(9) 0.5597(10) -0.0927(6) 0.081(4) Uani 1 1 d . . . C4 C 0.1301(9) 0.5073(10) -0.0636(7) 0.091(4) Uani 1 1 d . . . H4A H 0.1432 0.4649 -0.0322 0.109 Uiso 1 1 calc R . . C5 C 0.0537(10) 0.5187(11) -0.0820(8) 0.098(4) Uani 1 1 d . . . H5A H 0.0175 0.4813 -0.0634 0.117 Uiso 1 1 calc R . . C6 C 0.2639(8) 0.5593(8) -0.0720(7) 0.078(4) Uani 1 1 d . . . C7 C 0.3246(9) 0.5738(9) -0.1134(6) 0.081(4) Uani 1 1 d . . . H7A H 0.3155 0.5856 -0.1570 0.097 Uiso 1 1 calc R . . C8 C 0.3969(9) 0.5710(8) -0.0916(7) 0.079(4) Uani 1 1 d . . . H8A H 0.4365 0.5813 -0.1203 0.095 Uiso 1 1 calc R . . C9 C 0.3550(9) 0.5377(9) 0.0135(7) 0.084(4) Uani 1 1 d . . . H9A H 0.3656 0.5252 0.0568 0.100 Uiso 1 1 calc R . . C10 C 0.2827(9) 0.5402(9) -0.0078(6) 0.085(4) Uani 1 1 d . . . H10A H 0.2441 0.5286 0.0216 0.102 Uiso 1 1 calc R . . C11 C 0.4879(8) 0.5487(9) -0.0039(7) 0.088(4) Uani 1 1 d . . . H11A H 0.4903 0.5790 0.0378 0.106 Uiso 1 1 calc R . . H11B H 0.5221 0.5794 -0.0333 0.106 Uiso 1 1 calc R . . C12 C 0.6753(12) 0.6652(11) 0.0893(10) 0.102(5) Uani 1 1 d . . . C13 C 0.7487(13) 0.6857(11) 0.0885(10) 0.113(5) Uani 1 1 d . . . H13A H 0.7723 0.7043 0.0504 0.136 Uiso 1 1 calc R . . C14 C 0.7894(13) 0.6785(14) 0.1470(13) 0.135(7) Uani 1 1 d . . . H14A H 0.8411 0.6888 0.1469 0.162 Uiso 1 1 calc R . . C15 C 0.7550(15) 0.6569(14) 0.2029(11) 0.135(7) Uani 1 1 d . . . H15A H 0.7817 0.6575 0.2417 0.163 Uiso 1 1 calc R . . C16 C 0.6795(14) 0.6339(11) 0.2022(10) 0.116(5) Uani 1 1 d . . . H16A H 0.6563 0.6134 0.2399 0.139 Uiso 1 1 calc R . . C17 C 0.6384(9) 0.6415(10) 0.1452(9) 0.088(4) Uani 1 1 d . . . C18 C 0.5255(9) 0.6047(11) 0.2027(7) 0.100(5) Uani 1 1 d . . . H18A H 0.5342 0.6543 0.2325 0.120 Uiso 1 1 calc R . . H18B H 0.5441 0.5495 0.2224 0.120 Uiso 1 1 calc R . . C19 C 0.4449(11) 0.5965(11) 0.1885(7) 0.108(5) Uani 1 1 d . . . H19A H 0.4171 0.6001 0.2289 0.129 Uiso 1 1 calc R . . H19B H 0.4297 0.6473 0.1618 0.129 Uiso 1 1 calc R . . C20 C 0.3948(14) 0.4501(13) 0.1926(8) 0.140(7) Uani 1 1 d . . . H20A H 0.3551 0.4763 0.2189 0.168 Uiso 1 1 calc R . . H20B H 0.4335 0.4283 0.2219 0.168 Uiso 1 1 calc R . . C21 C 0.3636(14) 0.3727(13) 0.1585(14) 0.158(10) Uani 1 1 d . . . H21A H 0.3672 0.3206 0.1869 0.190 Uiso 1 1 calc R . . H21B H 0.3103 0.3842 0.1512 0.190 Uiso 1 1 calc R . . C22 C 0.346(3) 0.286(3) 0.068(2) 0.141(14) Uiso 0.50 1 d P . 1 H22A H 0.3425 0.2322 0.0941 0.169 Uiso 0.50 1 calc PR . 1 H22B H 0.2960 0.3116 0.0648 0.169 Uiso 0.50 1 calc PR . 1 C23 C 0.636(2) 0.738(2) -0.0136(17) 0.096(10) Uiso 0.50 1 d P . 1 H23A H 0.5878 0.7686 -0.0168 0.116 Uiso 0.50 1 calc PR . 1 H23B H 0.6727 0.7816 0.0010 0.116 Uiso 0.50 1 calc PR . 1 C24 C 0.401(2) 0.265(2) 0.0648(18) 0.111(11) Uiso 0.50 1 d P . 2 H24A H 0.3953 0.2111 0.0913 0.133 Uiso 0.50 1 calc PR . 2 H24B H 0.4476 0.2623 0.0404 0.133 Uiso 0.50 1 calc PR . 2 C25 C 0.674(2) 0.716(3) -0.018(2) 0.108(12) Uiso 0.50 1 d P . 2 H25A H 0.7102 0.6765 -0.0379 0.130 Uiso 0.50 1 calc PR . 2 H25B H 0.6977 0.7718 -0.0037 0.130 Uiso 0.50 1 calc PR . 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 0.0724(15) 0.1074(15) 0.0950(13) -0.0040(11) -0.0035(11) 0.0044(10) Br1 0.1172(17) 0.1346(16) 0.1322(15) -0.0117(11) 0.0162(12) -0.0232(12) Br2 0.1265(18) 0.1235(14) 0.1152(13) -0.0184(10) 0.0241(12) -0.0036(11) Br3 0.1231(17) 0.1289(15) 0.1071(12) -0.0020(10) -0.0260(11) 0.0118(10) O1 0.090(8) 0.107(7) 0.085(6) -0.003(5) 0.010(6) 0.002(6) O2 0.114(10) 0.121(8) 0.112(8) -0.029(7) 0.025(7) -0.029(7) O3 0.29(2) 0.123(11) 0.099(8) -0.005(8) -0.001(11) -0.063(12) O4 0.111(9) 0.112(8) 0.100(7) 0.004(6) 0.011(7) -0.020(6) N1 0.075(9) 0.104(8) 0.091(7) -0.006(7) -0.010(7) 0.011(7) N2 0.048(7) 0.078(6) 0.091(7) 0.010(6) 0.001(6) -0.001(5) C1 0.056(10) 0.091(9) 0.106(10) 0.004(8) 0.001(8) -0.002(7) C2 0.099(13) 0.093(10) 0.086(9) -0.014(8) 0.024(9) -0.016(8) C3 0.084(11) 0.094(9) 0.066(7) -0.004(7) -0.014(8) 0.011(8) C4 0.085(12) 0.089(9) 0.099(10) 0.030(8) 0.003(9) -0.005(8) C5 0.076(12) 0.108(11) 0.109(11) -0.001(10) 0.006(10) -0.011(9) C6 0.072(10) 0.074(8) 0.087(9) -0.009(7) -0.002(8) 0.005(7) C7 0.087(12) 0.086(9) 0.070(7) 0.010(7) 0.002(8) 0.005(7) C8 0.072(10) 0.081(8) 0.084(9) 0.022(7) 0.006(8) 0.009(7) C9 0.063(10) 0.101(10) 0.088(9) -0.001(8) -0.017(8) 0.003(8) C10 0.081(11) 0.094(9) 0.082(9) -0.002(7) 0.011(8) -0.001(8) C11 0.072(10) 0.098(9) 0.095(9) 0.003(8) -0.010(8) 0.009(8) C12 0.088(14) 0.097(11) 0.123(14) -0.011(10) 0.016(12) -0.004(9) C13 0.102(16) 0.115(12) 0.123(14) -0.028(11) 0.026(13) -0.002(11) C14 0.091(15) 0.138(16) 0.18(2) -0.043(15) 0.011(17) -0.020(11) C15 0.11(2) 0.157(17) 0.135(16) -0.013(14) -0.009(15) 0.038(14) C16 0.104(16) 0.114(12) 0.129(15) -0.001(11) 0.005(13) 0.011(11) C17 0.064(11) 0.089(9) 0.110(12) -0.014(8) -0.012(10) 0.001(8) C18 0.079(12) 0.125(12) 0.098(10) -0.021(9) 0.005(9) -0.002(9) C19 0.102(14) 0.135(13) 0.086(10) -0.004(10) 0.018(9) -0.013(11) C20 0.19(2) 0.137(15) 0.090(11) 0.025(12) 0.038(13) -0.005(15) C21 0.18(2) 0.099(13) 0.20(2) 0.008(16) -0.06(2) -0.065(14) _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 N1 2.039(13) . ? Co1 Br1 2.372(3) . ? Co1 Br3 2.373(3) . ? Co1 Br2 2.394(3) . ? O1 C17 1.357(18) . ? O1 C18 1.442(17) . ? O2 C20 1.333(18) . ? O2 C19 1.413(18) . ? O3 C21 1.28(3) . ? O3 C22 1.48(5) . ? O3 C24 1.53(4) . ? O4 C12 1.39(2) . ? O4 C23 1.41(3) . ? O4 C25 1.50(4) . ? N1 C1 1.315(17) . ? N1 C5 1.354(19) . ? N2 C8 1.334(16) . ? N2 C9 1.352(17) . ? N2 C11 1.457(17) . ? C1 C2 1.39(2) . ? C2 C3 1.416(19) . ? C3 C4 1.38(2) . ? C3 C6 1.46(2) . ? C4 C5 1.42(2) . ? C6 C7 1.389(19) . ? C6 C10 1.392(18) . ? C7 C8 1.36(2) . ? C9 C10 1.354(19) . ? C11 C11 1.51(3) 5_665 ? C12 C13 1.34(2) . ? C12 C17 1.37(2) . ? C13 C14 1.41(3) . ? C14 C15 1.34(3) . ? C15 C16 1.38(3) . ? C16 C17 1.39(2) . ? C18 C19 1.46(2) . ? C20 C21 1.45(3) . ? C22 C23 1.21(5) 5_665 ? C23 C22 1.21(5) 5_665 ? C24 C25 1.66(6) 5_665 ? C25 C24 1.66(6) 5_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 Br1 105.8(4) . . ? N1 Co1 Br3 104.1(4) . . ? Br1 Co1 Br3 112.04(11) . . ? N1 Co1 Br2 102.6(3) . . ? Br1 Co1 Br2 114.75(11) . . ? Br3 Co1 Br2 115.91(10) . . ? C17 O1 C18 117.0(12) . . ? C20 O2 C19 117.1(13) . . ? C21 O3 C22 112(3) . . ? C21 O3 C24 135(2) . . ? C22 O3 C24 40(2) . . ? C12 O4 C23 125(2) . . ? C12 O4 C25 107.8(19) . . ? C23 O4 C25 29.3(19) . . ? C1 N1 C5 118.8(14) . . ? C1 N1 Co1 120.7(11) . . ? C5 N1 Co1 119.5(11) . . ? C8 N2 C9 121.3(12) . . ? C8 N2 C11 122.2(12) . . ? C9 N2 C11 116.5(11) . . ? N1 C1 C2 121.1(14) . . ? C1 C2 C3 122.4(14) . . ? C4 C3 C2 115.4(14) . . ? C4 C3 C6 123.1(13) . . ? C2 C3 C6 121.0(14) . . ? C3 C4 C5 119.4(13) . . ? N1 C5 C4 122.7(14) . . ? C7 C6 C10 115.3(13) . . ? C7 C6 C3 124.2(13) . . ? C10 C6 C3 120.4(14) . . ? C8 C7 C6 121.6(12) . . ? N2 C8 C7 120.2(13) . . ? C10 C9 N2 118.8(13) . . ? C9 C10 C6 122.7(14) . . ? N2 C11 C11 110.5(15) . 5_665 ? C13 C12 O4 123.3(19) . . ? C13 C12 C17 122(2) . . ? O4 C12 C17 114.3(17) . . ? C12 C13 C14 118(2) . . ? C15 C14 C13 121(2) . . ? C14 C15 C16 119(2) . . ? C15 C16 C17 119.8(19) . . ? O1 C17 C12 118.8(16) . . ? O1 C17 C16 122.3(17) . . ? C12 C17 C16 118.8(18) . . ? O1 C18 C19 107.5(13) . . ? O2 C19 C18 114.3(15) . . ? O2 C20 C21 117.0(17) . . ? O3 C21 C20 117(2) . . ? C23 C22 O3 121(4) 5_665 . ? C22 C23 O4 118(4) 5_665 . ? O3 C24 C25 96(3) . 5_665 ? O4 C25 C24 95(3) . 5_665 ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.846 _refine_diff_density_max 0.975 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.192 #===END data_MnBr3_stoppered_[2]rotaxane _database_code_CSD 168752 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Br6 Mn2 N4 O8' _chemical_formula_weight 1378.26 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca #(61) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.893(2) _cell_length_b 14.854(2) _cell_length_c 20.799(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5528.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 4.844 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0483 _exptl_absorpt_correction_T_max 0.0796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens SMART CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 22700 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3964 _reflns_number_gt 2784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL XP' _computing_publication_material 'Siemens SHELXTL XCIF' _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^)+(0.0740P)^2^+1.9722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3964 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.004 _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 -0.08336(4) 0.61189(6) -0.13626(4) 0.0562(2) Uani 1 1 d . . . Br1 Br -0.14493(4) 0.46399(5) -0.12601(3) 0.0910(3) Uani 1 1 d . . . Br2 Br -0.10373(4) 0.71566(5) -0.04461(3) 0.0872(3) Uani 1 1 d . . . Br3 Br -0.08680(4) 0.67443(4) -0.24622(3) 0.0782(2) Uani 1 1 d . . . O1 O 0.56482(19) 0.6192(2) 0.14190(16) 0.0594(9) Uani 1 1 d . . . O2 O 0.4260(2) 0.5141(3) 0.1550(2) 0.0849(13) Uani 1 1 d . . . O3 O 0.3876(4) 0.3553(3) 0.1015(2) 0.138(2) Uani 1 1 d . . . O4 O 0.6298(2) 0.6709(3) 0.03569(19) 0.0750(11) Uani 1 1 d . . . N1 N 0.0361(2) 0.5809(3) -0.12414(19) 0.0505(10) Uani 1 1 d . . . N2 N 0.4117(2) 0.5543(2) -0.02809(18) 0.0438(9) Uani 1 1 d . . . C1 C 0.0875(3) 0.6311(3) -0.1518(2) 0.0508(12) Uani 1 1 d . . . H1A H 0.0723 0.6737 -0.1818 0.061 Uiso 1 1 calc R . . C2 C 0.1635(3) 0.6236(3) -0.1384(2) 0.0466(12) Uani 1 1 d . . . H2A H 0.1980 0.6587 -0.1604 0.056 Uiso 1 1 calc R . . C3 C 0.1869(2) 0.5635(3) -0.0920(2) 0.0416(11) Uani 1 1 d . . . C4 C 0.1326(3) 0.5099(4) -0.0635(2) 0.0548(13) Uani 1 1 d . . . H4A H 0.1457 0.4678 -0.0324 0.066 Uiso 1 1 calc R . . C5 C 0.0585(3) 0.5200(4) -0.0820(3) 0.0609(14) Uani 1 1 d . . . H5A H 0.0229 0.4821 -0.0639 0.073 Uiso 1 1 calc R . . C6 C 0.2657(2) 0.5596(3) -0.0706(2) 0.0402(11) Uani 1 1 d . . . C7 C 0.3247(3) 0.5767(3) -0.1118(2) 0.0477(12) Uani 1 1 d . . . H7A H 0.3153 0.5915 -0.1545 0.057 Uiso 1 1 calc R . . C8 C 0.3967(3) 0.5721(3) -0.0901(2) 0.0484(12) Uani 1 1 d . . . H8A H 0.4359 0.5813 -0.1187 0.058 Uiso 1 1 calc R . . C9 C 0.3549(3) 0.5393(3) 0.0128(2) 0.0521(12) Uani 1 1 d . . . H9A H 0.3653 0.5274 0.0558 0.063 Uiso 1 1 calc R . . C10 C 0.2827(3) 0.5412(3) -0.0073(2) 0.0506(12) Uani 1 1 d . . . H10A H 0.2445 0.5299 0.0219 0.061 Uiso 1 1 calc R . . C11 C 0.4891(2) 0.5489(3) -0.0044(3) 0.0505(12) Uani 1 1 d . . . H11A H 0.4932 0.5804 0.0363 0.061 Uiso 1 1 calc R . . H11B H 0.5226 0.5774 -0.0349 0.061 Uiso 1 1 calc R . . C12 C 0.6736(3) 0.6651(3) 0.0886(3) 0.0614(15) Uani 1 1 d . . . C13 C 0.7491(4) 0.6838(4) 0.0879(4) 0.0832(19) Uani 1 1 d . . . H13A H 0.7725 0.6999 0.0497 0.100 Uiso 1 1 calc R . . C14 C 0.7898(4) 0.6784(5) 0.1443(5) 0.104(3) Uani 1 1 d . . . H14A H 0.8407 0.6913 0.1438 0.125 Uiso 1 1 calc R . . C15 C 0.7556(4) 0.6540(5) 0.2017(4) 0.097(2) Uani 1 1 d . . . H15A H 0.7831 0.6519 0.2396 0.117 Uiso 1 1 calc R . . C16 C 0.6807(4) 0.6330(4) 0.2019(3) 0.0770(17) Uani 1 1 d . . . H16A H 0.6579 0.6150 0.2399 0.092 Uiso 1 1 calc R . . C17 C 0.6390(3) 0.6383(3) 0.1461(3) 0.0570(14) Uani 1 1 d . . . C18 C 0.5258(3) 0.6041(4) 0.2016(3) 0.0700(16) Uani 1 1 d . . . H18A H 0.5342 0.6542 0.2307 0.084 Uiso 1 1 calc R . . H18B H 0.5440 0.5497 0.2220 0.084 Uiso 1 1 calc R . . C19 C 0.4451(4) 0.5954(4) 0.1876(3) 0.0785(17) Uani 1 1 d . . . H19A H 0.4176 0.5982 0.2277 0.094 Uiso 1 1 calc R . . H19B H 0.4296 0.6461 0.1614 0.094 Uiso 1 1 calc R . . C20 C 0.3959(5) 0.4503(5) 0.1900(3) 0.103(2) Uani 1 1 d . . . H20A H 0.3573 0.4775 0.2163 0.123 Uiso 1 1 calc R . . H20B H 0.4341 0.4280 0.2191 0.123 Uiso 1 1 calc R . . C21 C 0.3641(5) 0.3752(6) 0.1583(4) 0.124(3) Uani 1 1 d . . . H21A H 0.3718 0.3228 0.1854 0.148 Uiso 1 1 calc R . . H21B H 0.3107 0.3851 0.1556 0.148 Uiso 1 1 calc R . . C22 C 0.3356(12) 0.2910(10) 0.0712(9) 0.089(5) Uani 0.50 1 d P . 1 H22A H 0.3268 0.2408 0.1001 0.107 Uiso 0.50 1 calc PR . 1 H22B H 0.2881 0.3203 0.0631 0.107 Uiso 0.50 1 calc PR . 1 C23 C 0.6356(12) 0.7401(14) -0.0149(12) 0.067(5) Uani 0.50 1 d P . 1 H23A H 0.5863 0.7646 -0.0230 0.080 Uiso 0.50 1 calc PR . 1 H23B H 0.6669 0.7887 0.0007 0.080 Uiso 0.50 1 calc PR . 1 C24 C 0.3983(13) 0.2670(11) 0.0665(8) 0.101(5) Uani 0.50 1 d P . 2 H24A H 0.3897 0.2151 0.0939 0.122 Uiso 0.50 1 calc PR . 2 H24B H 0.4469 0.2624 0.0461 0.122 Uiso 0.50 1 calc PR . 2 C25 C 0.6719(12) 0.7159(16) -0.0129(12) 0.080(6) Uani 0.50 1 d P . 2 H25A H 0.7112 0.6781 -0.0304 0.096 Uiso 0.50 1 calc PR . 2 H25B H 0.6931 0.7720 0.0024 0.096 Uiso 0.50 1 calc PR . 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 0.0383(5) 0.0700(5) 0.0602(5) -0.0050(4) -0.0032(4) 0.0037(4) Br1 0.0925(5) 0.0870(5) 0.0935(5) -0.0140(4) 0.0237(4) -0.0272(4) Br2 0.0965(5) 0.0840(5) 0.0810(4) -0.0202(4) 0.0296(4) -0.0094(4) Br3 0.0929(5) 0.0826(4) 0.0590(4) -0.0046(3) -0.0261(3) 0.0137(3) O1 0.047(2) 0.070(2) 0.061(2) 0.0012(18) 0.0017(17) -0.0108(18) O2 0.090(3) 0.083(3) 0.082(3) -0.012(2) 0.025(2) -0.036(2) O3 0.275(8) 0.081(3) 0.058(3) -0.003(3) 0.003(4) -0.074(4) O4 0.088(3) 0.074(3) 0.063(2) -0.009(2) 0.014(2) -0.028(2) N1 0.037(2) 0.059(3) 0.056(2) 0.001(2) -0.005(2) 0.004(2) N2 0.033(2) 0.043(2) 0.055(2) 0.0013(18) -0.0046(19) 0.0025(17) C1 0.044(3) 0.056(3) 0.052(3) 0.008(2) -0.011(2) 0.001(3) C2 0.043(3) 0.050(3) 0.046(3) 0.007(2) -0.002(2) -0.004(2) C3 0.034(3) 0.048(3) 0.042(3) -0.004(2) 0.002(2) 0.002(2) C4 0.041(3) 0.063(3) 0.060(3) 0.013(3) -0.004(2) 0.006(3) C5 0.038(3) 0.071(4) 0.073(4) 0.016(3) 0.006(3) -0.009(3) C6 0.031(3) 0.042(3) 0.048(3) 0.000(2) 0.001(2) 0.005(2) C7 0.041(3) 0.056(3) 0.047(3) 0.006(2) -0.006(2) 0.008(2) C8 0.038(3) 0.053(3) 0.054(3) 0.004(2) 0.006(2) 0.001(2) C9 0.042(3) 0.068(3) 0.046(3) 0.007(2) -0.003(2) 0.006(3) C10 0.039(3) 0.066(3) 0.046(3) 0.010(2) 0.004(2) 0.008(2) C11 0.031(3) 0.054(3) 0.066(3) 0.000(3) -0.008(2) 0.001(2) C12 0.059(4) 0.049(3) 0.076(4) -0.023(3) 0.009(3) -0.009(3) C13 0.068(5) 0.074(4) 0.107(5) -0.035(4) 0.026(4) -0.015(4) C14 0.049(4) 0.091(5) 0.173(9) -0.041(5) 0.004(5) -0.005(4) C15 0.071(5) 0.098(5) 0.122(6) -0.019(5) -0.041(5) 0.008(4) C16 0.076(5) 0.078(4) 0.078(4) 0.003(3) -0.011(3) -0.003(3) C17 0.053(4) 0.047(3) 0.071(4) -0.008(3) -0.002(3) 0.001(3) C18 0.080(4) 0.066(4) 0.063(3) -0.008(3) 0.004(3) -0.010(3) C19 0.074(4) 0.078(4) 0.084(4) -0.015(3) 0.022(3) -0.012(3) C20 0.151(7) 0.099(5) 0.059(4) 0.001(4) 0.015(4) -0.037(5) C21 0.160(8) 0.118(6) 0.093(6) 0.023(5) -0.012(6) -0.074(6) C22 0.123(14) 0.061(9) 0.082(12) 0.003(8) -0.006(11) -0.047(10) C23 0.078(15) 0.042(10) 0.080(12) -0.007(8) 0.000(12) -0.009(9) C24 0.161(18) 0.082(11) 0.060(10) 0.013(8) 0.003(12) -0.045(13) C25 0.101(19) 0.062(14) 0.077(12) -0.012(10) 0.023(14) -0.019(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 N1 2.202(4) . ? Mn1 Br1 2.4669(11) . ? Mn1 Br3 2.4693(10) . ? Mn1 Br2 2.4784(10) . ? O1 C17 1.361(6) . ? O1 C18 1.443(6) . ? O2 C20 1.310(7) . ? O2 C19 1.427(7) . ? O3 C21 1.287(9) . ? O3 C22 1.476(16) . ? O3 C24 1.51(2) . ? O4 C12 1.354(7) . ? O4 C25 1.43(2) . ? O4 C23 1.47(2) . ? N1 C1 1.316(6) . ? N1 C5 1.321(6) . ? N2 C8 1.344(6) . ? N2 C9 1.344(6) . ? N2 C11 1.472(5) . ? C1 C2 1.392(6) . ? C2 C3 1.379(6) . ? C3 C4 1.389(6) . ? C3 C6 1.480(6) . ? C4 C5 1.388(7) . ? C6 C10 1.379(6) . ? C6 C7 1.383(6) . ? C7 C8 1.367(6) . ? C9 C10 1.358(6) . ? C11 C11 1.515(9) 5_665 ? C12 C13 1.379(8) . ? C12 C17 1.403(8) . ? C13 C14 1.383(10) . ? C14 C15 1.390(10) . ? C15 C16 1.377(9) . ? C16 C17 1.381(8) . ? C18 C19 1.478(8) . ? C20 C21 1.416(9) . ? C22 C23 1.36(3) 5_665 ? C23 C22 1.36(3) 5_665 ? C24 C25 1.70(3) 5_665 ? C25 C24 1.70(3) 5_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn1 Br1 103.74(12) . . ? N1 Mn1 Br3 102.06(11) . . ? Br1 Mn1 Br3 113.83(4) . . ? N1 Mn1 Br2 100.65(11) . . ? Br1 Mn1 Br2 114.95(4) . . ? Br3 Mn1 Br2 118.34(4) . . ? C17 O1 C18 116.8(4) . . ? C20 O2 C19 116.5(5) . . ? C21 O3 C22 109.5(9) . . ? C21 O3 C24 132.9(8) . . ? C22 O3 C24 46.5(8) . . ? C12 O4 C25 107.5(10) . . ? C12 O4 C23 125.7(10) . . ? C25 O4 C23 29.6(8) . . ? C1 N1 C5 117.8(4) . . ? C1 N1 Mn1 120.7(3) . . ? C5 N1 Mn1 120.9(3) . . ? C8 N2 C9 119.3(4) . . ? C8 N2 C11 121.4(4) . . ? C9 N2 C11 119.4(4) . . ? N1 C1 C2 123.3(4) . . ? C3 C2 C1 119.3(4) . . ? C2 C3 C4 117.2(4) . . ? C2 C3 C6 121.7(4) . . ? C4 C3 C6 121.1(4) . . ? C5 C4 C3 119.2(4) . . ? N1 C5 C4 123.2(5) . . ? C10 C6 C7 117.4(4) . . ? C10 C6 C3 120.4(4) . . ? C7 C6 C3 122.3(4) . . ? C8 C7 C6 120.4(4) . . ? N2 C8 C7 121.0(4) . . ? N2 C9 C10 121.4(4) . . ? C9 C10 C6 120.5(4) . . ? N2 C11 C11 109.6(5) . 5_665 ? O4 C12 C13 123.1(6) . . ? O4 C12 C17 117.1(5) . . ? C13 C12 C17 119.9(6) . . ? C14 C13 C12 119.7(7) . . ? C13 C14 C15 120.8(7) . . ? C16 C15 C14 119.3(7) . . ? C15 C16 C17 120.7(7) . . ? O1 C17 C16 124.6(5) . . ? O1 C17 C12 115.8(5) . . ? C16 C17 C12 119.6(6) . . ? O1 C18 C19 108.5(5) . . ? O2 C19 C18 113.7(5) . . ? O2 C20 C21 118.4(6) . . ? O3 C21 C20 118.5(7) . . ? C23 C22 O3 110.4(17) 5_665 . ? C22 C23 O4 113.9(15) 5_665 . ? O3 C24 C25 95.3(15) . 5_665 ? O4 C25 C24 98.3(15) . 5_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.655 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.067 #===END