Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jamie Manson' _publ_contact_author_address ; Department of Chemistry and Biochemistry Eastern Washington University 226 Science 526 5th Street WA 99004 UNITED STATES OF AMERICA ; _publ_contact_author_email JMANSON@EWU.EDU _publ_section_title ; Mn(dca)2(pym)2 and Mn(dca)2(pym)(H2O) {dca = dicyanamide; pym = pyrimidine}: New coordination polymers exhibiting 1- and 2D topologies based on double-bridged Mn-(NCNCN)2-Mn structural units ; loop_ _publ_author_name 'Jamie Manson' 'Cara L. Nygren' 'John A. Schlueter' # Attachment 'Mn(dca)2(pym)(H2O).cif' data_may8m _database_code_depnum_ccdc_archive 'CCDC 619247' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Mn(N3C2)2(N2C4H4)(H2O) _chemical_formula_sum 'C8 H6 Mn N8 O' _chemical_formula_weight 285.15 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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.3939(17) _cell_length_b 18.858(4) _cell_length_c 8.849(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.260(4) _cell_angle_gamma 90.00 _cell_volume 1164.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'BRUKER AXS CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12325 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2819 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'BRUKER SHELXTL' _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^)+(0.0402P)^2^+0.3670P] 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 2819 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.02603(2) 0.374019(10) 0.17496(2) 0.02107(8) Uani 1 1 d . . . O1 O -0.17476(15) 0.44513(6) 0.00439(13) 0.0324(2) Uani 1 1 d . . . H1A H -0.289(3) 0.4354(12) -0.022(3) 0.056(6) Uiso 1 1 d . . . H1B H -0.159(3) 0.4644(11) -0.071(2) 0.047(5) Uiso 1 1 d . . . N1 N 0.26441(17) 0.31617(6) 0.34313(15) 0.0329(3) Uani 1 1 d . . . N2 N 0.5597(2) 0.28359(12) 0.55393(18) 0.0691(6) Uani 1 1 d . . . N3 N 0.84361(17) 0.21655(6) 0.56155(15) 0.0317(3) Uani 1 1 d . . . N4 N 0.18665(17) 0.47465(6) 0.27962(14) 0.0301(2) Uani 1 1 d . . . N5 N 0.32505(19) 0.54253(10) 0.5259(2) 0.0574(5) Uani 1 1 d . . . N6 N 0.14942(18) 0.60960(7) 0.66959(15) 0.0332(3) Uani 1 1 d . . . N7 N 0.17797(16) 0.37157(6) -0.01248(14) 0.0250(2) Uani 1 1 d . . . N8 N 0.44543(16) 0.40691(7) -0.08631(15) 0.0312(2) Uani 1 1 d . . . C1 C 0.4078(2) 0.29885(8) 0.43488(17) 0.0320(3) Uani 1 1 d . . . C2 C 0.7047(2) 0.24731(7) 0.54775(16) 0.0309(3) Uani 1 1 d . . . C3 C 0.24412(18) 0.50750(7) 0.39535(16) 0.0271(3) Uani 1 1 d . . . C4 C 0.22425(19) 0.57749(8) 0.59700(16) 0.0307(3) Uani 1 1 d . . . C5 C 0.35353(18) 0.39840(7) 0.01825(16) 0.0284(3) Uani 1 1 d . . . H5A H 0.4189 0.4128 0.1253 0.034 Uiso 1 1 calc R . . C6 C 0.3527(2) 0.38620(8) -0.23708(18) 0.0322(3) Uani 1 1 d . . . H6A H 0.4131 0.3922 -0.3158 0.039 Uiso 1 1 calc R . . C7 C 0.1724(2) 0.35649(8) -0.28105(17) 0.0332(3) Uani 1 1 d . . . H7A H 0.1087 0.3410 -0.3875 0.040 Uiso 1 1 calc R . . C8 C 0.08866(19) 0.35024(8) -0.16370(16) 0.0291(3) Uani 1 1 d . . . H8A H -0.0359 0.3303 -0.1905 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01648(11) 0.02291(11) 0.02206(11) -0.00203(6) 0.00398(8) -0.00051(6) O1 0.0200(5) 0.0390(5) 0.0362(6) 0.0123(4) 0.0064(4) 0.0003(4) N1 0.0251(6) 0.0341(6) 0.0347(6) -0.0004(5) 0.0037(5) 0.0059(5) N2 0.0521(9) 0.1045(14) 0.0347(8) -0.0170(8) -0.0073(7) 0.0518(10) N3 0.0249(6) 0.0295(6) 0.0366(6) 0.0047(5) 0.0045(5) 0.0040(5) N4 0.0270(6) 0.0300(6) 0.0317(6) -0.0064(5) 0.0076(5) -0.0031(4) N5 0.0218(6) 0.0861(12) 0.0590(9) -0.0465(9) 0.0064(6) -0.0007(7) N6 0.0298(6) 0.0409(6) 0.0298(6) -0.0040(5) 0.0112(5) -0.0006(5) N7 0.0200(5) 0.0281(5) 0.0255(5) -0.0041(4) 0.0059(4) 0.0000(4) N8 0.0216(5) 0.0366(6) 0.0362(6) -0.0011(5) 0.0108(5) 0.0012(5) C1 0.0294(7) 0.0334(7) 0.0312(7) -0.0039(5) 0.0073(6) 0.0085(5) C2 0.0281(7) 0.0300(6) 0.0267(6) -0.0017(5) -0.0017(5) 0.0044(5) C3 0.0187(5) 0.0297(6) 0.0334(7) -0.0032(5) 0.0092(5) -0.0016(5) C4 0.0209(6) 0.0396(7) 0.0284(7) -0.0073(5) 0.0037(5) -0.0029(5) C5 0.0194(6) 0.0357(7) 0.0284(6) -0.0040(5) 0.0055(5) 0.0004(5) C6 0.0323(7) 0.0349(7) 0.0330(7) 0.0013(5) 0.0157(6) 0.0048(6) C7 0.0332(7) 0.0388(7) 0.0258(7) -0.0052(5) 0.0075(6) 0.0010(6) C8 0.0229(6) 0.0335(7) 0.0284(6) -0.0064(5) 0.0052(5) -0.0025(5) _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 2.1866(12) . ? Mn1 O1 2.1914(10) . ? Mn1 N6 2.2018(13) 3_566 ? Mn1 N3 2.2024(12) 4_465 ? Mn1 N4 2.2680(12) . ? Mn1 N7 2.2902(12) . ? N1 C1 1.1496(18) . ? N2 C2 1.288(2) . ? N2 C1 1.2939(19) . ? N3 C2 1.1503(18) . ? N3 Mn1 2.2024(12) 4_666 ? N4 C3 1.1516(18) . ? N5 C3 1.2931(19) . ? N5 C4 1.3023(19) . ? N6 C4 1.1488(19) . ? N6 Mn1 2.2018(13) 3_566 ? N7 C5 1.3349(17) . ? N7 C8 1.3438(17) . ? N8 C5 1.3261(18) . ? N8 C6 1.3413(19) . ? C6 C7 1.379(2) . ? C7 C8 1.378(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 N1 Mn1 O1 170.05(4) . . ? N1 Mn1 N6 98.83(5) . 3_566 ? O1 Mn1 N6 86.54(5) . 3_566 ? N1 Mn1 N3 99.11(5) . 4_465 ? O1 Mn1 N3 89.24(5) . 4_465 ? N6 Mn1 N3 89.72(5) 3_566 4_465 ? N1 Mn1 N4 86.76(5) . . ? O1 Mn1 N4 85.06(4) . . ? N6 Mn1 N4 87.97(5) 3_566 . ? N3 Mn1 N4 173.96(4) 4_465 . ? N1 Mn1 N7 90.29(5) . . ? O1 Mn1 N7 84.04(4) . . ? N6 Mn1 N7 170.47(4) 3_566 . ? N3 Mn1 N7 91.57(4) 4_465 . ? N4 Mn1 N7 89.81(4) . . ? C1 N1 Mn1 166.14(12) . . ? C2 N2 C1 126.51(15) . . ? C2 N3 Mn1 146.15(12) . 4_666 ? C3 N4 Mn1 143.44(11) . . ? C3 N5 C4 121.35(13) . . ? C4 N6 Mn1 156.20(13) . 3_566 ? C5 N7 C8 116.22(12) . . ? C5 N7 Mn1 121.41(9) . . ? C8 N7 Mn1 122.00(9) . . ? C5 N8 C6 116.59(12) . . ? N1 C1 N2 171.46(16) . . ? N3 C2 N2 171.78(16) . . ? N4 C3 N5 174.47(15) . . ? N6 C4 N5 174.31(15) . . ? N8 C5 N7 126.25(12) . . ? N8 C6 C7 121.89(13) . . ? C8 C7 C6 117.07(13) . . ? N7 C8 C7 121.96(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mn1 N1 C1 21.1(7) . . . . ? N6 Mn1 N1 C1 -101.1(5) 3_566 . . . ? N3 Mn1 N1 C1 167.8(5) 4_465 . . . ? N4 Mn1 N1 C1 -13.6(5) . . . . ? N7 Mn1 N1 C1 76.2(5) . . . . ? N1 Mn1 N4 C3 -63.03(18) . . . . ? O1 Mn1 N4 C3 122.63(18) . . . . ? N6 Mn1 N4 C3 35.93(18) 3_566 . . . ? N3 Mn1 N4 C3 103.4(4) 4_465 . . . ? N7 Mn1 N4 C3 -153.33(18) . . . . ? N1 Mn1 N7 C5 -57.09(11) . . . . ? O1 Mn1 N7 C5 114.72(11) . . . . ? N6 Mn1 N7 C5 106.1(3) 3_566 . . . ? N3 Mn1 N7 C5 -156.21(10) 4_465 . . . ? N4 Mn1 N7 C5 29.67(10) . . . . ? N1 Mn1 N7 C8 130.15(11) . . . . ? O1 Mn1 N7 C8 -58.04(11) . . . . ? N6 Mn1 N7 C8 -66.6(3) 3_566 . . . ? N3 Mn1 N7 C8 31.04(11) 4_465 . . . ? N4 Mn1 N7 C8 -143.09(11) . . . . ? Mn1 N1 C1 N2 79.5(15) . . . . ? C2 N2 C1 N1 175.8(12) . . . . ? Mn1 N3 C2 N2 62.9(14) 4_666 . . . ? C1 N2 C2 N3 178(100) . . . . ? Mn1 N4 C3 N5 108.7(18) . . . . ? C4 N5 C3 N4 -178(100) . . . . ? Mn1 N6 C4 N5 -107.0(18) 3_566 . . . ? C3 N5 C4 N6 176.2(18) . . . . ? C6 N8 C5 N7 -0.3(2) . . . . ? C8 N7 C5 N8 1.2(2) . . . . ? Mn1 N7 C5 N8 -171.94(11) . . . . ? C5 N8 C6 C7 -1.0(2) . . . . ? N8 C6 C7 C8 1.4(2) . . . . ? C5 N7 C8 C7 -0.8(2) . . . . ? Mn1 N7 C8 C7 172.32(11) . . . . ? C6 C7 C8 N7 -0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.499 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.050 # Attachment 'mndca2pym2.cif' data_rtdatac _database_code_depnum_ccdc_archive 'CCDC 619248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Mn N10' _chemical_formula_weight 347.22 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.6213(16) _cell_length_b 7.5799(9) _cell_length_c 14.7671(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1524.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'BRUKER CCD area diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9318 _diffrn_reflns_av_R_equivalents 0.1996 _diffrn_reflns_av_sigmaI/netI 0.1504 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1825 _reflns_number_gt 800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^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 1825 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2042 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2239 _refine_ls_wR_factor_gt 0.1759 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.5000 0.11115(13) 0.7500 0.0367(4) Uani 1 2 d S . . N1 N 0.4432(4) 0.3195(6) 0.8409(4) 0.0497(14) Uani 1 1 d . . . N2 N 0.4082(4) 0.6104(6) 0.9010(4) 0.0601(17) Uani 1 1 d . . . N3 N 0.4425(4) 0.9036(6) 0.8396(3) 0.0498(14) Uani 1 1 d . . . C1 C 0.4294(4) 0.4617(8) 0.8644(4) 0.0377(14) Uani 1 1 d . . . C2 C 0.4296(4) 0.7620(8) 0.8636(4) 0.0360(14) Uani 1 1 d . . . N4 N 0.3564(3) 0.1093(6) 0.6729(3) 0.0435(12) Uani 1 1 d . . . N5 N 0.1812(4) 0.1091(8) 0.6748(4) 0.0658(16) Uani 1 1 d . . . C3 C 0.2689(6) 0.1163(8) 0.7118(5) 0.0591(18) Uani 1 1 d . . . H3 H 0.2696 0.1281 0.7745 0.071 Uiso 1 1 calc R . . C4 C 0.1823(6) 0.0980(11) 0.5840(5) 0.074(2) Uani 1 1 d . . . H4 H 0.1229 0.0951 0.5529 0.088 Uiso 1 1 calc R . . C5 C 0.2658(5) 0.0911(10) 0.5371(5) 0.084(3) Uani 1 1 d . . . H5 H 0.2648 0.0813 0.4743 0.101 Uiso 1 1 calc R . . C6 C 0.3516(5) 0.0986(10) 0.5819(5) 0.063(2) Uani 1 1 d . . . H6 H 0.4098 0.0962 0.5489 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0444(8) 0.0279(6) 0.0378(7) 0.000 0.0011(7) 0.000 N1 0.063(3) 0.037(3) 0.049(3) -0.001(3) 0.002(3) 0.000(3) N2 0.102(5) 0.029(2) 0.050(3) -0.002(3) 0.039(3) 0.001(3) N3 0.070(4) 0.025(2) 0.054(3) 0.004(3) 0.010(3) 0.001(3) C1 0.040(3) 0.037(3) 0.037(4) -0.001(3) 0.008(3) -0.002(3) C2 0.040(3) 0.043(3) 0.025(3) -0.014(3) 0.004(3) 0.007(3) N4 0.047(3) 0.044(3) 0.040(3) -0.004(3) 0.005(3) -0.004(2) N5 0.041(3) 0.088(4) 0.068(4) -0.011(4) 0.003(3) -0.004(3) C3 0.070(5) 0.067(4) 0.040(4) -0.005(3) 0.005(4) 0.003(4) C4 0.053(4) 0.114(6) 0.054(5) -0.008(5) -0.011(4) -0.015(4) C5 0.054(5) 0.150(8) 0.047(4) 0.001(5) -0.002(4) -0.028(5) C6 0.047(4) 0.096(6) 0.047(4) -0.002(4) 0.005(3) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N3 2.199(5) 1_545 ? Mn1 N3 2.199(5) 3_646 ? Mn1 N1 2.213(5) . ? Mn1 N1 2.213(5) 3_656 ? Mn1 N4 2.263(5) . ? Mn1 N4 2.263(5) 3_656 ? N1 C1 1.147(6) . ? N2 C1 1.284(7) . ? N2 C2 1.308(7) . ? N3 C2 1.144(6) . ? N3 Mn1 2.199(5) 1_565 ? N4 C3 1.324(8) . ? N4 C6 1.348(8) . ? N5 C3 1.315(9) . ? N5 C4 1.345(9) . ? C4 C5 1.333(10) . ? C5 C6 1.344(9) . ? 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 N3 Mn1 N3 88.7(2) 1_545 3_646 ? N3 Mn1 N1 91.23(17) 1_545 . ? N3 Mn1 N1 179.5(2) 3_646 . ? N3 Mn1 N1 179.5(2) 1_545 3_656 ? N3 Mn1 N1 91.23(17) 3_646 3_656 ? N1 Mn1 N1 88.9(3) . 3_656 ? N3 Mn1 N4 89.45(19) 1_545 . ? N3 Mn1 N4 90.03(19) 3_646 . ? N1 Mn1 N4 90.43(18) . . ? N1 Mn1 N4 90.09(19) 3_656 . ? N3 Mn1 N4 90.03(19) 1_545 3_656 ? N3 Mn1 N4 89.45(19) 3_646 3_656 ? N1 Mn1 N4 90.09(19) . 3_656 ? N1 Mn1 N4 90.43(18) 3_656 3_656 ? N4 Mn1 N4 179.3(2) . 3_656 ? C1 N1 Mn1 155.6(5) . . ? C1 N2 C2 122.9(5) . . ? C2 N3 Mn1 155.9(5) . 1_565 ? N1 C1 N2 171.5(7) . . ? N3 C2 N2 171.7(6) . . ? C3 N4 C6 113.1(6) . . ? C3 N4 Mn1 124.0(5) . . ? C6 N4 Mn1 122.9(4) . . ? C3 N5 C4 114.1(6) . . ? N5 C3 N4 129.5(7) . . ? C5 C4 N5 122.0(7) . . ? C4 C5 C6 119.0(7) . . ? C5 C6 N4 122.4(6) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.332 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.112