# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'M. Julve' 'Donatella Armentano' 'Juan Manuel Herrera' 'Francesc Lloret' 'Giovanni de Munno' 'M. Verdaguer' _publ_contact_author_name 'Prof M Julve' _publ_contact_author_address ; Departament de Quimica Inorganica, Facultat de Quimica de la Universitat de Valencia Dr.Moliner, 50 Valencia Burjassot 46100 SPAIN ; _publ_contact_author_phone '34 963864856' _publ_contact_author_fax '34 963864322' _publ_contact_author_email miguel.julve@uv.es _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; [MnII2(bpym)(H2O)8]4+ and [MIV(CN)8]4- (M=Mo and W) as building blocks in designing bpym- and cyanide-bridged bimetallic three-dimensional networks (bpym = 2,2' - bipyrimidine) ; data_(1) _database_code_CSD 188051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Mn2 Mo N12 O2' _chemical_formula_weight 608.18 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 14.539(3) _cell_length_b 12.620(2) _cell_length_c 12.114(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.400(10) _cell_angle_gamma 90.00 _cell_volume 2162.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.736 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2019 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1918 _reflns_number_gt 1630 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary patterson _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 1918 _refine_ls_number_parameters 156 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.996 _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 Mo1 Mo 1.0000 0.26664(3) 1.2500 0.01174(15) Uani 1 2 d S . . Mn1 Mn 0.76225(4) 0.51132(4) 0.94438(5) 0.01617(17) Uani 1 1 d . . . N1 N 0.6952(2) 0.6727(2) 0.8777(3) 0.0244(7) Uani 1 1 d . . . C1 C 0.6421(3) 0.6892(3) 0.7727(4) 0.0332(10) Uani 1 1 d . . . H1 H 0.6243 0.6316 0.7245 0.060 Uiso 1 1 calc R . . C2 C 0.6133(3) 0.7890(4) 0.7349(4) 0.0374(11) Uani 1 1 d . . . H2 H 0.5789 0.8005 0.6610 0.060 Uiso 1 1 calc R . . C3 C 0.6372(3) 0.8712(3) 0.8102(4) 0.0337(10) Uani 1 1 d . . . H3 H 0.6159 0.9390 0.7873 0.060 Uiso 1 1 calc R . . N2 N 0.6900(2) 0.8576(2) 0.9150(3) 0.0241(7) Uani 1 1 d . . . C4 C 0.7186(3) 0.7581(3) 0.9432(3) 0.0188(8) Uani 1 1 d . . . O1 O 0.6527(2) 0.4866(2) 1.0427(3) 0.0344(7) Uani 1 1 d D . . H1W H 0.623(3) 0.5524(19) 1.051(5) 0.060 Uiso 1 1 d D . . H2W H 0.600(2) 0.442(3) 1.012(5) 0.060 Uiso 1 1 d D . . N5 N 0.8723(2) 0.5685(3) 0.8633(3) 0.0288(8) Uani 1 1 d . . . C5 C 0.9162(3) 0.6247(3) 0.8228(3) 0.0200(8) Uani 1 1 d . . . N6 N 0.6724(2) 0.4109(3) 0.8149(3) 0.0267(8) Uani 1 1 d . . . C6 C 0.6133(3) 0.3485(3) 0.7878(3) 0.0178(8) Uani 1 1 d . . . N7 N 0.8483(2) 0.3928(3) 1.0479(3) 0.0271(8) Uani 1 1 d . . . C7 C 0.8988(3) 0.3473(3) 1.1171(3) 0.0200(8) Uani 1 1 d . . . C8 C 1.0105(3) 0.1960(3) 1.0909(3) 0.0202(8) Uani 1 1 d . . . N8 N 1.0149(3) 0.1600(3) 1.0043(3) 0.0321(9) 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 Mo1 0.0091(2) 0.0093(2) 0.0151(2) 0.000 -0.00051(16) 0.000 Mn1 0.0145(3) 0.0119(3) 0.0199(3) 0.0010(2) -0.0006(2) -0.0008(2) N1 0.0266(18) 0.0157(17) 0.0265(18) -0.0028(13) -0.0030(15) 0.0028(13) C1 0.040(3) 0.027(2) 0.026(2) -0.0045(19) -0.0046(19) -0.001(2) C2 0.046(3) 0.036(3) 0.021(2) 0.0002(19) -0.011(2) 0.007(2) C3 0.045(3) 0.022(2) 0.029(2) 0.0072(18) -0.003(2) 0.0041(19) N2 0.0291(18) 0.0160(16) 0.0232(18) 0.0006(13) -0.0020(14) 0.0003(14) C4 0.0178(18) 0.0153(18) 0.023(2) 0.0022(15) 0.0036(16) -0.0005(14) O1 0.0307(17) 0.0281(16) 0.047(2) -0.0120(14) 0.0151(15) -0.0026(13) N5 0.030(2) 0.0262(19) 0.0297(19) -0.0026(15) 0.0069(16) -0.0106(16) C5 0.0167(19) 0.0197(19) 0.0221(19) -0.0024(16) 0.0014(15) -0.0030(16) N6 0.0215(18) 0.0266(18) 0.0291(19) -0.0050(15) -0.0002(14) -0.0101(15) C6 0.0179(19) 0.0171(18) 0.0176(18) 0.0023(15) 0.0022(15) 0.0015(16) N7 0.0266(18) 0.0230(17) 0.0283(19) 0.0042(15) -0.0004(16) 0.0077(15) C7 0.0186(19) 0.0169(18) 0.023(2) -0.0007(16) 0.0021(16) 0.0014(16) C8 0.0162(19) 0.0171(18) 0.026(2) 0.0027(16) 0.0031(16) 0.0012(15) N8 0.030(2) 0.037(2) 0.030(2) -0.0054(16) 0.0072(16) 0.0053(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C5 2.155(4) 2_565 ? Mo1 C5 2.155(4) 5_767 ? Mo1 C8 2.161(4) . ? Mo1 C8 2.161(4) 6_758 ? Mo1 C6 2.164(4) 7_657 ? Mo1 C6 2.164(4) 4 ? Mo1 C7 2.166(4) 6_758 ? Mo1 C7 2.166(4) . ? Mn1 N7 2.155(3) . ? Mn1 N5 2.186(3) . ? Mn1 N6 2.196(3) . ? Mn1 O1 2.222(3) . ? Mn1 N1 2.321(3) . ? Mn1 N2 2.360(3) 7_667 ? N1 C4 1.335(5) . ? N1 C1 1.343(5) . ? C1 C2 1.372(6) . ? C2 C3 1.372(6) . ? C3 N2 1.333(5) . ? N2 C4 1.342(5) . ? N2 Mn1 2.360(3) 7_667 ? C4 C4 1.479(8) 7_667 ? N5 C5 1.137(5) . ? C5 Mo1 2.155(4) 5_767 ? N6 C6 1.156(5) . ? C6 Mo1 2.164(4) 7_657 ? N7 C7 1.135(5) . ? C8 N8 1.159(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 C5 Mo1 C5 101.0(2) 2_565 5_767 ? C5 Mo1 C8 142.30(14) 2_565 . ? C5 Mo1 C8 74.56(14) 5_767 . ? C5 Mo1 C8 74.56(14) 2_565 6_758 ? C5 Mo1 C8 142.30(14) 5_767 6_758 ? C8 Mo1 C8 131.3(2) . 6_758 ? C5 Mo1 C6 92.22(14) 2_565 7_657 ? C5 Mo1 C6 144.64(14) 5_767 7_657 ? C8 Mo1 C6 75.04(14) . 7_657 ? C8 Mo1 C6 72.81(14) 6_758 7_657 ? C5 Mo1 C6 144.64(14) 2_565 4 ? C5 Mo1 C6 92.22(14) 5_767 4 ? C8 Mo1 C6 72.81(14) . 4 ? C8 Mo1 C6 75.04(14) 6_758 4 ? C6 Mo1 C6 95.67(19) 7_657 4 ? C5 Mo1 C7 75.40(14) 2_565 6_758 ? C5 Mo1 C7 69.77(14) 5_767 6_758 ? C8 Mo1 C7 132.89(14) . 6_758 ? C8 Mo1 C7 72.96(14) 6_758 6_758 ? C6 Mo1 C7 145.59(14) 7_657 6_758 ? C6 Mo1 C7 78.80(14) 4 6_758 ? C5 Mo1 C7 69.77(14) 2_565 . ? C5 Mo1 C7 75.40(14) 5_767 . ? C8 Mo1 C7 72.96(14) . . ? C8 Mo1 C7 132.89(14) 6_758 . ? C6 Mo1 C7 78.80(14) 7_657 . ? C6 Mo1 C7 145.59(14) 4 . ? C7 Mo1 C7 124.0(2) 6_758 . ? N7 Mn1 N5 95.96(14) . . ? N7 Mn1 N6 100.60(14) . . ? N5 Mn1 N6 104.23(13) . . ? N7 Mn1 O1 88.99(13) . . ? N5 Mn1 O1 168.06(12) . . ? N6 Mn1 O1 85.44(12) . . ? N7 Mn1 N1 162.11(13) . . ? N5 Mn1 N1 81.13(13) . . ? N6 Mn1 N1 97.22(12) . . ? O1 Mn1 N1 90.83(12) . . ? N7 Mn1 N2 91.86(13) . 7_667 ? N5 Mn1 N2 88.22(12) . 7_667 ? N6 Mn1 N2 161.22(13) . 7_667 ? O1 Mn1 N2 80.74(12) . 7_667 ? N1 Mn1 N2 70.47(11) . 7_667 ? C4 N1 C1 116.7(3) . . ? C4 N1 Mn1 118.2(2) . . ? C1 N1 Mn1 124.7(3) . . ? N1 C1 C2 121.5(4) . . ? C1 C2 C3 117.5(4) . . ? N2 C3 C2 122.5(4) . . ? C3 N2 C4 116.0(3) . . ? C3 N2 Mn1 127.2(3) . 7_667 ? C4 N2 Mn1 116.8(3) . 7_667 ? N1 C4 N2 125.7(3) . . ? N1 C4 C4 117.3(4) . 7_667 ? N2 C4 C4 117.0(4) . 7_667 ? C5 N5 Mn1 160.3(3) . . ? N5 C5 Mo1 178.6(3) . 5_767 ? C6 N6 Mn1 151.2(3) . . ? N6 C6 Mo1 175.5(3) . 7_657 ? C7 N7 Mn1 166.0(3) . . ? N7 C7 Mo1 177.2(4) . . ? N8 C8 Mo1 178.5(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 H1W N8 0.950(10) 2.06(3) 2.930(5) 152(4) 3_455 O1 H2W N8 0.953(10) 2.08(2) 3.006(5) 163(5) 7_657 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.608 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.106 #===END data_2 _database_code_CSD 188052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Mn2 N12 O2 W' _chemical_formula_weight 696.09 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 14.542(2) _cell_length_b 12.608(2) _cell_length_c 12.126(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.460(10) _cell_angle_gamma 90.00 _cell_volume 2162.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 6.499 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.270 _exptl_absorpt_correction_T_max 0.342 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2018 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1917 _reflns_number_gt 1782 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary patterson _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 1917 _refine_ls_number_parameters 156 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 W1 W 1.0000 0.266616(19) 1.2500 0.01315(10) Uani 1 2 d S . . Mn1 Mn 0.76237(5) 0.51115(5) 0.94396(6) 0.01772(17) Uani 1 1 d . . . N1 N 0.6955(3) 0.6727(3) 0.8773(3) 0.0238(9) Uani 1 1 d . . . C1 C 0.6430(4) 0.6893(4) 0.7731(5) 0.0335(12) Uani 1 1 d . . . H1 H 0.6264 0.6319 0.7243 0.060 Uiso 1 1 calc R . . C2 C 0.6127(4) 0.7896(4) 0.7358(5) 0.0372(14) Uani 1 1 d . . . H2 H 0.5773 0.8010 0.6624 0.060 Uiso 1 1 calc R . . C3 C 0.6365(4) 0.8709(4) 0.8105(5) 0.0351(13) Uani 1 1 d . . . H3 H 0.6147 0.9386 0.7877 0.060 Uiso 1 1 calc R . . N2 N 0.6900(3) 0.8576(3) 0.9152(3) 0.0233(9) Uani 1 1 d . . . C4 C 0.7187(3) 0.7579(4) 0.9435(4) 0.0216(10) Uani 1 1 d . . . O1 O 0.6522(3) 0.4872(3) 1.0423(3) 0.0359(9) Uani 1 1 d D . . H1W H 0.614(3) 0.547(3) 1.050(6) 0.060 Uiso 1 1 d D . . H2W H 0.603(3) 0.436(3) 1.014(6) 0.060 Uiso 1 1 d D . . N5 N 0.8730(3) 0.5679(3) 0.8640(4) 0.0314(10) Uani 1 1 d . . . C5 C 0.9169(3) 0.6249(4) 0.8229(4) 0.0204(10) Uani 1 1 d . . . N6 N 0.6722(3) 0.4103(3) 0.8154(4) 0.0280(10) Uani 1 1 d . . . C6 C 0.6133(3) 0.3485(4) 0.7878(4) 0.0193(10) Uani 1 1 d . . . N7 N 0.8478(3) 0.3931(3) 1.0477(4) 0.0283(10) Uani 1 1 d . . . C7 C 0.8982(3) 0.3469(4) 1.1161(4) 0.0212(10) Uani 1 1 d . . . C8 C 1.0108(3) 0.1962(4) 1.0901(4) 0.0209(10) Uani 1 1 d . . . N8 N 1.0147(3) 0.1597(4) 1.0045(4) 0.0327(10) 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 W1 0.01202(14) 0.01146(15) 0.01519(15) 0.000 0.00161(9) 0.000 Mn1 0.0171(4) 0.0146(4) 0.0201(4) 0.0009(3) 0.0016(3) -0.0007(3) N1 0.028(2) 0.017(2) 0.025(2) -0.0037(16) 0.0032(18) -0.0025(16) C1 0.042(3) 0.027(3) 0.027(3) -0.007(2) -0.002(2) -0.001(2) C2 0.046(4) 0.034(3) 0.024(3) 0.003(2) -0.006(2) 0.003(3) C3 0.050(4) 0.022(3) 0.027(3) 0.004(2) -0.002(3) 0.004(2) N2 0.031(2) 0.017(2) 0.019(2) 0.0004(16) 0.0015(17) 0.0008(17) C4 0.023(2) 0.019(2) 0.022(3) 0.0039(18) 0.005(2) -0.0011(18) O1 0.035(2) 0.032(2) 0.045(2) -0.0131(18) 0.0195(19) -0.0071(17) N5 0.037(3) 0.030(2) 0.029(2) -0.0016(19) 0.012(2) -0.007(2) C5 0.021(2) 0.018(2) 0.023(2) -0.0020(19) 0.006(2) -0.0060(19) N6 0.031(2) 0.026(2) 0.025(2) -0.0022(18) 0.0036(18) -0.0092(19) C6 0.020(2) 0.022(2) 0.015(2) -0.0045(18) 0.0029(18) -0.004(2) N7 0.031(2) 0.024(2) 0.028(2) 0.0030(18) 0.003(2) 0.0088(18) C7 0.022(2) 0.019(2) 0.022(2) 0.000(2) 0.005(2) -0.0007(19) C8 0.020(2) 0.023(2) 0.020(3) 0.002(2) 0.0067(19) 0.0039(19) N8 0.038(3) 0.036(3) 0.027(2) -0.005(2) 0.012(2) 0.004(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 W1 C5 2.146(4) 2_565 ? W1 C5 2.146(5) 5_767 ? W1 C6 2.163(5) 7_657 ? W1 C6 2.163(5) 4 ? W1 C8 2.171(5) 6_758 ? W1 C8 2.171(5) . ? W1 C7 2.175(5) 6_758 ? W1 C7 2.175(5) . ? Mn1 N7 2.148(4) . ? Mn1 N5 2.183(4) . ? Mn1 N6 2.194(4) . ? Mn1 O1 2.229(4) . ? Mn1 N1 2.319(4) . ? Mn1 N2 2.363(4) 7_667 ? N1 C1 1.331(7) . ? N1 C4 1.337(6) . ? C1 C2 1.380(8) . ? C2 C3 1.358(8) . ? C3 N2 1.337(7) . ? N2 C4 1.343(6) . ? N2 Mn1 2.363(4) 7_667 ? C4 C4 1.472(10) 7_667 ? N5 C5 1.150(6) . ? C5 W1 2.146(4) 5_767 ? N6 C6 1.149(6) . ? C6 W1 2.163(5) 7_657 ? N7 C7 1.132(6) . ? C8 N8 1.149(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 C5 W1 C5 100.9(3) 2_565 5_767 ? C5 W1 C6 92.34(18) 2_565 7_657 ? C5 W1 C6 144.49(17) 5_767 7_657 ? C5 W1 C6 144.49(17) 2_565 4 ? C5 W1 C6 92.34(18) 5_767 4 ? C6 W1 C6 95.7(3) 7_657 4 ? C5 W1 C8 74.23(18) 2_565 6_758 ? C5 W1 C8 142.47(18) 5_767 6_758 ? C6 W1 C8 72.82(17) 7_657 6_758 ? C6 W1 C8 75.29(17) 4 6_758 ? C5 W1 C8 142.47(17) 2_565 . ? C5 W1 C8 74.23(18) 5_767 . ? C6 W1 C8 75.29(17) 7_657 . ? C6 W1 C8 72.82(17) 4 . ? C8 W1 C8 131.7(3) 6_758 . ? C5 W1 C7 75.33(18) 2_565 6_758 ? C5 W1 C7 70.15(18) 5_767 6_758 ? C6 W1 C7 145.35(18) 7_657 6_758 ? C6 W1 C7 78.57(18) 4 6_758 ? C8 W1 C7 72.68(17) 6_758 6_758 ? C8 W1 C7 132.73(18) . 6_758 ? C5 W1 C7 70.15(17) 2_565 . ? C5 W1 C7 75.33(18) 5_767 . ? C6 W1 C7 78.57(18) 7_657 . ? C6 W1 C7 145.35(18) 4 . ? C8 W1 C7 132.73(18) 6_758 . ? C8 W1 C7 72.68(17) . . ? C7 W1 C7 124.5(2) 6_758 . ? N7 Mn1 N5 95.85(18) . . ? N7 Mn1 N6 100.56(17) . . ? N5 Mn1 N6 104.75(16) . . ? N7 Mn1 O1 88.99(17) . . ? N5 Mn1 O1 167.84(15) . . ? N6 Mn1 O1 85.22(15) . . ? N7 Mn1 N1 161.97(16) . . ? N5 Mn1 N1 81.37(16) . . ? N6 Mn1 N1 97.37(16) . . ? O1 Mn1 N1 90.58(15) . . ? N7 Mn1 N2 91.71(15) . 7_667 ? N5 Mn1 N2 88.23(15) . 7_667 ? N6 Mn1 N2 160.97(16) . 7_667 ? O1 Mn1 N2 80.46(14) . 7_667 ? N1 Mn1 N2 70.47(14) . 7_667 ? C1 N1 C4 116.9(4) . . ? C1 N1 Mn1 124.8(3) . . ? C4 N1 Mn1 118.0(3) . . ? N1 C1 C2 121.6(5) . . ? C3 C2 C1 117.4(5) . . ? N2 C3 C2 122.7(5) . . ? C3 N2 C4 115.9(4) . . ? C3 N2 Mn1 127.4(3) . 7_667 ? C4 N2 Mn1 116.7(3) . 7_667 ? N1 C4 N2 125.4(4) . . ? N1 C4 C4 117.7(5) . 7_667 ? N2 C4 C4 116.9(5) . 7_667 ? C5 N5 Mn1 159.9(4) . . ? N5 C5 W1 178.6(4) . 5_767 ? C6 N6 Mn1 151.9(4) . . ? N6 C6 W1 175.1(4) . 7_657 ? C7 N7 Mn1 166.7(4) . . ? N7 C7 W1 176.6(4) . . ? N8 C8 W1 178.6(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 H2W N8 0.959(10) 2.07(2) 3.001(6) 163(6) 7_657 O1 H1W N8 0.960(10) 2.00(3) 2.917(6) 158(6) 3_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.007 _refine_diff_density_min -2.645 _refine_diff_density_rms 0.138