Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shyamal Kumar Chattopadhyay' _publ_contact_author_address ; Department of Chemistry Bengal Engineering and Science University, Shibpur College Road, P. O. Botanic Garden Howrah West Bengal 711 103 INDIA ; _publ_contact_author_email SHCH20@HOTMAIL.COM _publ_section_title ; Synthesis, X-ray Crystal Structure and DFT Calculations of bis(N-(2-picolyl) picolinamido) Mn(III) Hexafluorophosphate ; loop_ _publ_author_name 'Shyamal Kumar Chattopadhyay' 'Hake M. Figgie' 'Serge Gorelsky' 'Sumita Hazra' 'Dipankar Mishra' ; S.Naskar ; 'W. Sheldrick' data_sn _database_code_depnum_ccdc_archive 'CCDC 637857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Mn N6 O2, F6 P' _chemical_formula_sum 'C24 H20 F6 Mn N6 O2 P' _chemical_formula_weight 624.37 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'P n' _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.9930(18) _cell_length_b 9.1411(18) _cell_length_c 16.002(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.17(3) _cell_angle_gamma 90.00 _cell_volume 1298.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description needle _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.83084 _exptl_absorpt_correction_T_max 0.93110 _exptl_absorpt_process_details ; XPREP. Sheldrick, G.M., (1995). SHELXTL, Release 5.03 for Siemens R3 crystallographic research system. Siemens Analytical X-Ray Instruments, Inc., Madison, USA. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 P4 4-circle' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 2427 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2427 _reflns_number_gt 1415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens R3m/V (Siemens, 1989)' _computing_cell_refinement 'Siemens R3m/V (Siemens, 1989)' _computing_data_reduction 'XDISK (Siemens, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS (Sheldrick, 1995)' _computing_publication_material 'SHELXL-97 (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^)+(0.1014P)^2^+1.8609P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_number_reflns 2427 _refine_ls_number_parameters 398 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2000 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.956 _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 0.3939(2) 0.8953(2) 0.52261(12) 0.0483(6) Uani 1 1 d . . . N1 N 0.3938(16) 0.8867(14) 0.6420(8) 0.063(4) Uani 1 1 d D . . C2 C 0.5193(15) 0.8377(17) 0.6967(6) 0.057(4) Uani 1 1 d D . . N2 N 0.6116(13) 0.8045(13) 0.5631(7) 0.058(3) Uani 1 1 d . . . O2 O 0.5277(15) 0.8400(12) 0.7741(5) 0.092(4) Uani 1 1 d D . . N3 N 0.1794(14) 0.9792(12) 0.5307(7) 0.057(3) Uani 1 1 d . . . C3 C 0.2650(16) 0.9403(16) 0.6796(8) 0.055(4) Uani 1 1 d . . . H3 H 0.2968 1.0185 0.7194 0.066 Uiso 1 1 calc R . . H31 H 0.2237 0.8617 0.7096 0.066 Uiso 1 1 calc R . . N4 N 0.3953(14) 0.9083(12) 0.4029(7) 0.048(3) Uani 1 1 d D . . N5 N 0.4817(13) 1.1177(13) 0.5137(7) 0.054(3) Uani 1 1 d . . . C5 C 0.4539(19) 1.0306(16) 0.3731(7) 0.070(5) Uani 1 1 d D . . O5 O 0.466(3) 1.053(2) 0.3010(9) 0.173(8) Uani 1 1 d D . . C6 C 0.3368(17) 0.8020(15) 0.3440(10) 0.060(4) Uani 1 1 d . . . H6 H 0.4132 0.7714 0.3112 0.071 Uiso 1 1 calc R . . H61 H 0.2521 0.8416 0.3055 0.071 Uiso 1 1 calc R . . N6 N 0.3037(13) 0.6848(12) 0.4777(7) 0.053(3) Uani 1 1 d . . . C21 C 0.6430(17) 0.7878(15) 0.6480(8) 0.062(4) Uani 1 1 d D . . C22 C 0.7735(19) 0.7279(15) 0.6888(10) 0.066(4) Uani 1 1 d . . . H22 H 0.7936 0.7190 0.7474 0.079 Uiso 1 1 calc R . . C23 C 0.876(2) 0.6801(18) 0.6365(13) 0.090(6) Uani 1 1 d . . . H23 H 0.9647 0.6348 0.6611 0.109 Uiso 1 1 calc R . . C24 C 0.8478(17) 0.6990(16) 0.5486(11) 0.070(5) Uani 1 1 d . . . H24 H 0.9156 0.6693 0.5137 0.083 Uiso 1 1 calc R . . C25 C 0.709(2) 0.7663(17) 0.5167(10) 0.071(4) Uani 1 1 d . . . H25 H 0.6869 0.7840 0.4588 0.085 Uiso 1 1 calc R . . C31 C 0.149(2) 0.9951(15) 0.6092(9) 0.066(4) Uani 1 1 d . . . C32 C 0.0105(17) 1.0587(19) 0.6219(10) 0.073(5) Uani 1 1 d . . . H32 H -0.0140 1.0672 0.6760 0.088 Uiso 1 1 calc R . . C33 C -0.085(2) 1.107(2) 0.5538(11) 0.089(6) Uani 1 1 d . . . H33 H -0.1750 1.1492 0.5622 0.106 Uiso 1 1 calc R . . C34 C -0.0557(19) 1.096(2) 0.4759(13) 0.088(6) Uani 1 1 d . . . H34 H -0.1224 1.1323 0.4303 0.106 Uiso 1 1 calc R . . C35 C 0.0731(19) 1.0299(19) 0.4644(9) 0.071(5) Uani 1 1 d . . . H35 H 0.0920 1.0179 0.4093 0.085 Uiso 1 1 calc R . . C51 C 0.5039(16) 1.1481(14) 0.4360(8) 0.056(4) Uani 1 1 d D . . C52 C 0.5656(19) 1.2828(19) 0.4106(11) 0.073(5) Uani 1 1 d . . . H52 H 0.5822 1.3017 0.3557 0.088 Uiso 1 1 calc R . . C53 C 0.598(2) 1.381(2) 0.4762(13) 0.088(5) Uani 1 1 d . . . H53 H 0.6354 1.4717 0.4641 0.106 Uiso 1 1 calc R . . C54 C 0.578(2) 1.354(2) 0.5600(13) 0.092(6) Uani 1 1 d . . . H54 H 0.6028 1.4218 0.6032 0.110 Uiso 1 1 calc R . . C55 C 0.517(2) 1.2170(17) 0.5734(11) 0.071(4) Uani 1 1 d . . . H55 H 0.4997 1.1945 0.6277 0.085 Uiso 1 1 calc R . . C61 C 0.2852(16) 0.6702(16) 0.3928(9) 0.056(4) Uani 1 1 d . . . C62 C 0.218(2) 0.5505(17) 0.3532(10) 0.070(4) Uani 1 1 d . . . H62 H 0.2030 0.5436 0.2945 0.083 Uiso 1 1 calc R . . C63 C 0.1738(19) 0.442(2) 0.4006(12) 0.081(5) Uani 1 1 d . . . H63 H 0.1277 0.3589 0.3743 0.097 Uiso 1 1 calc R . . C64 C 0.196(2) 0.4512(19) 0.4858(11) 0.076(5) Uani 1 1 d . . . H64 H 0.1693 0.3735 0.5180 0.092 Uiso 1 1 calc R . . C65 C 0.2573(17) 0.5768(18) 0.5253(9) 0.066(4) Uani 1 1 d . . . H65 H 0.2666 0.5869 0.5838 0.079 Uiso 1 1 calc R . . P1 P 0.7670(7) 0.5971(6) 0.2702(3) 0.0952(17) Uani 1 1 d D . . F1 F 0.835(4) 0.743(3) 0.307(3) 0.25(2) Uani 0.50 1 d PDU . . F1' F 0.910(4) 0.687(4) 0.261(3) 0.23(2) Uani 0.50 1 d PDU . . F2 F 0.832(4) 0.457(2) 0.2386(18) 0.209(19) Uani 0.50 1 d PDU . . F2' F 0.910(2) 0.558(3) 0.2307(14) 0.118(11) Uani 0.50 1 d PD . . F3 F 0.696(3) 0.750(2) 0.2934(14) 0.090(7) Uani 0.50 1 d PD . . F3' F 0.637(3) 0.632(3) 0.3184(18) 0.18(2) Uani 0.50 1 d PD . . F4 F 0.702(3) 0.444(2) 0.2379(18) 0.098(9) Uani 0.50 1 d PD . . F4' F 0.622(3) 0.515(4) 0.284(3) 0.204(19) Uani 0.50 1 d PDU . . F5 F 0.702(2) 0.6511(18) 0.1798(8) 0.201(9) Uani 1 1 d DU . . F6 F 0.8405(16) 0.5380(19) 0.3580(7) 0.152(6) Uani 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 0.0561(12) 0.0523(11) 0.0343(9) 0.0016(12) 0.0003(8) 0.0075(14) N1 0.083(11) 0.069(10) 0.034(7) 0.001(6) -0.001(7) 0.001(8) C2 0.064(10) 0.071(10) 0.035(7) 0.001(7) 0.003(7) 0.011(8) N2 0.052(7) 0.052(7) 0.062(7) -0.016(6) -0.015(6) -0.005(6) O2 0.140(11) 0.082(7) 0.038(5) -0.009(5) -0.033(6) 0.019(8) N3 0.066(8) 0.058(7) 0.051(7) 0.001(6) 0.019(6) -0.005(6) C3 0.056(9) 0.058(9) 0.051(8) -0.007(7) 0.010(7) 0.007(7) N4 0.060(9) 0.042(7) 0.041(7) 0.007(5) 0.004(6) 0.002(6) N5 0.063(7) 0.050(7) 0.051(6) 0.002(6) 0.014(5) 0.008(7) C5 0.098(13) 0.093(12) 0.026(7) 0.007(8) 0.029(7) 0.030(10) O5 0.24(2) 0.154(17) 0.139(15) 0.001(12) 0.073(16) 0.040(16) C6 0.043(8) 0.045(8) 0.093(12) 0.008(8) 0.018(8) 0.014(7) N6 0.066(8) 0.045(7) 0.045(6) 0.003(5) -0.005(6) 0.008(6) C21 0.089(12) 0.046(8) 0.041(7) 0.016(6) -0.021(8) -0.012(8) C22 0.076(11) 0.043(8) 0.071(10) 0.003(7) -0.013(9) 0.005(8) C23 0.074(12) 0.060(11) 0.117(15) -0.007(11) -0.048(12) 0.009(9) C24 0.047(10) 0.055(9) 0.098(14) -0.013(9) -0.016(8) 0.013(8) C25 0.083(12) 0.067(10) 0.061(9) -0.024(8) 0.001(9) 0.006(10) C31 0.102(13) 0.049(8) 0.049(8) 0.011(7) 0.015(9) -0.007(9) C32 0.055(9) 0.106(14) 0.064(10) -0.005(9) 0.030(8) 0.009(9) C33 0.065(12) 0.129(16) 0.079(12) 0.000(11) 0.036(11) 0.011(12) C34 0.046(10) 0.107(14) 0.113(15) 0.010(12) 0.013(10) 0.023(11) C35 0.075(12) 0.096(12) 0.038(8) -0.003(8) 0.000(8) -0.002(10) C51 0.057(9) 0.054(9) 0.058(9) 0.011(7) 0.017(7) 0.005(7) C52 0.073(11) 0.075(13) 0.072(11) 0.008(10) 0.009(9) 0.012(10) C53 0.107(15) 0.063(11) 0.097(14) 0.011(11) 0.029(12) -0.001(11) C54 0.108(16) 0.076(13) 0.093(14) -0.035(11) 0.023(11) 0.015(12) C55 0.091(12) 0.051(9) 0.076(10) -0.020(8) 0.027(9) 0.015(9) C61 0.049(8) 0.061(9) 0.054(8) 0.005(7) -0.003(6) 0.006(7) C62 0.098(13) 0.060(10) 0.049(8) -0.007(7) 0.006(8) -0.007(9) C63 0.070(12) 0.074(13) 0.096(14) -0.030(10) 0.001(10) -0.014(9) C64 0.089(14) 0.062(10) 0.075(12) -0.004(9) 0.006(10) -0.017(11) C65 0.068(10) 0.081(12) 0.046(7) -0.013(8) -0.003(7) 0.015(9) P1 0.128(5) 0.094(4) 0.061(3) 0.009(3) 0.007(3) 0.004(4) F1 0.37(5) 0.18(3) 0.17(3) -0.08(3) 0.01(3) -0.14(4) F1' 0.21(4) 0.23(4) 0.26(4) 0.08(3) 0.10(3) 0.02(3) F2 0.36(5) 0.14(3) 0.12(2) 0.04(2) 0.01(3) 0.17(3) F2' 0.124(19) 0.18(3) 0.065(13) -0.010(17) 0.061(14) -0.06(2) F3 0.13(2) 0.064(13) 0.076(14) 0.005(10) 0.012(14) -0.010(14) F3' 0.19(4) 0.26(5) 0.097(19) 0.02(3) 0.06(2) 0.19(4) F4 0.091(16) 0.098(18) 0.116(18) -0.051(15) 0.052(15) -0.032(15) F4' 0.13(3) 0.22(4) 0.25(4) 0.10(3) -0.03(3) -0.07(3) F5 0.31(2) 0.181(16) 0.104(10) 0.041(10) 0.001(12) 0.131(15) F6 0.144(11) 0.235(17) 0.074(7) 0.036(9) 0.005(7) 0.018(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 N1 1.913(12) . ? Mn1 N4 1.921(11) . ? Mn1 N3 2.099(12) . ? Mn1 N2 2.130(12) . ? Mn1 N6 2.166(11) . ? Mn1 N5 2.193(12) . ? N1 C2 1.387(14) . ? N1 C3 1.471(19) . ? C2 O2 1.228(9) . ? C2 C21 1.527(15) . ? N2 C25 1.283(18) . ? N2 C21 1.352(16) . ? N3 C31 1.335(17) . ? N3 C35 1.390(19) . ? C3 C31 1.50(2) . ? C3 H3 0.9700 . ? C3 H31 0.9700 . ? N4 C5 1.354(14) . ? N4 C6 1.397(18) . ? N5 C51 1.320(16) . ? N5 C55 1.319(17) . ? C5 O5 1.195(10) . ? C5 C51 1.491(15) . ? C6 C61 1.55(2) . ? C6 H6 0.9700 . ? C6 H61 0.9700 . ? N6 C61 1.350(16) . ? N6 C65 1.353(19) . ? C21 C22 1.36(2) . ? C22 C23 1.41(2) . ? C22 H22 0.9300 . ? C23 C24 1.40(2) . ? C23 H23 0.9300 . ? C24 C25 1.41(2) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C32 1.42(2) . ? C32 C33 1.35(2) . ? C32 H32 0.9300 . ? C33 C34 1.32(2) . ? C33 H33 0.9300 . ? C34 C35 1.34(2) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C51 C52 1.44(2) . ? C52 C53 1.38(2) . ? C52 H52 0.9300 . ? C53 C54 1.40(2) . ? C53 H53 0.9300 . ? C54 C55 1.40(2) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C61 C62 1.36(2) . ? C62 C63 1.35(2) . ? C62 H62 0.9300 . ? C63 C64 1.35(2) . ? C63 H63 0.9300 . ? C64 C65 1.38(2) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? P1 F3' 1.533(16) . ? P1 F2 1.531(18) . ? P1 F1 1.545(19) . ? P1 F6 1.551(11) . ? P1 F4' 1.550(19) . ? P1 F5 1.553(11) . ? P1 F1' 1.56(2) . ? P1 F4 1.569(16) . ? P1 F2' 1.561(17) . ? P1 F3 1.604(16) . ? F1 F1' 1.20(3) . ? F1 F3 1.23(3) . ? F1' F2' 1.27(3) . ? F2 F2' 1.18(3) . ? F2 F4 1.17(3) . ? F3 F3' 1.29(3) . ? F3' F4' 1.20(3) . ? F4 F4' 1.29(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 N1 Mn1 N4 178.8(5) . . ? N1 Mn1 N3 78.8(5) . . ? N4 Mn1 N3 101.0(5) . . ? N1 Mn1 N2 80.1(5) . . ? N4 Mn1 N2 100.1(5) . . ? N3 Mn1 N2 158.9(5) . . ? N1 Mn1 N6 103.6(5) . . ? N4 Mn1 N6 77.6(5) . . ? N3 Mn1 N6 92.6(5) . . ? N2 Mn1 N6 91.8(4) . . ? N1 Mn1 N5 99.3(5) . . ? N4 Mn1 N5 79.5(4) . . ? N3 Mn1 N5 90.6(4) . . ? N2 Mn1 N5 93.3(5) . . ? N6 Mn1 N5 157.1(4) . . ? C2 N1 C3 117.6(12) . . ? C2 N1 Mn1 120.9(10) . . ? C3 N1 Mn1 121.4(9) . . ? O2 C2 N1 122.9(13) . . ? O2 C2 C21 125.9(12) . . ? N1 C2 C21 111.1(10) . . ? C25 N2 C21 119.9(13) . . ? C25 N2 Mn1 127.5(11) . . ? C21 N2 Mn1 112.6(10) . . ? C31 N3 C35 117.6(14) . . ? C31 N3 Mn1 115.2(11) . . ? C35 N3 Mn1 127.0(10) . . ? N1 C3 C31 107.7(12) . . ? N1 C3 H3 110.2 . . ? C31 C3 H3 110.2 . . ? N1 C3 H31 110.2 . . ? C31 C3 H31 110.2 . . ? H3 C3 H31 108.5 . . ? C5 N4 C6 117.5(12) . . ? C5 N4 Mn1 117.8(9) . . ? C6 N4 Mn1 124.6(10) . . ? C51 N5 C55 118.9(13) . . ? C51 N5 Mn1 111.5(9) . . ? C55 N5 Mn1 129.6(10) . . ? O5 C5 N4 125.6(16) . . ? O5 C5 C51 117.7(16) . . ? N4 C5 C51 116.7(11) . . ? N4 C6 C61 108.2(13) . . ? N4 C6 H6 110.1 . . ? C61 C6 H6 110.1 . . ? N4 C6 H61 110.1 . . ? C61 C6 H61 110.1 . . ? H6 C6 H61 108.4 . . ? C61 N6 C65 119.6(12) . . ? C61 N6 Mn1 113.7(9) . . ? C65 N6 Mn1 126.5(9) . . ? N2 C21 C22 123.6(14) . . ? N2 C21 C2 115.3(11) . . ? C22 C21 C2 121.1(12) . . ? C21 C22 C23 115.7(15) . . ? C21 C22 H22 122.2 . . ? C23 C22 H22 122.2 . . ? C22 C23 C24 122.0(16) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C25 115.1(16) . . ? C23 C24 H24 122.5 . . ? C25 C24 H24 122.5 . . ? N2 C25 C24 123.7(15) . . ? N2 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N3 C31 C32 119.7(15) . . ? N3 C31 C3 116.7(15) . . ? C32 C31 C3 123.5(13) . . ? C33 C32 C31 118.5(15) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 123.0(19) . . ? C34 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 C34 C35 118.0(18) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? C34 C35 N3 123.2(15) . . ? C34 C35 H35 118.4 . . ? N3 C35 H35 118.4 . . ? N5 C51 C52 124.8(13) . . ? N5 C51 C5 114.2(12) . . ? C52 C51 C5 121.1(13) . . ? C53 C52 C51 112.7(15) . . ? C53 C52 H52 123.6 . . ? C51 C52 H52 123.6 . . ? C52 C53 C54 124.9(18) . . ? C52 C53 H53 117.5 . . ? C54 C53 H53 117.5 . . ? C55 C54 C53 114.6(16) . . ? C55 C54 H54 122.7 . . ? C53 C54 H54 122.7 . . ? N5 C55 C54 124.1(16) . . ? N5 C55 H55 118.0 . . ? C54 C55 H55 118.0 . . ? N6 C61 C62 121.7(14) . . ? N6 C61 C6 115.6(13) . . ? C62 C61 C6 122.7(13) . . ? C63 C62 C61 118.8(14) . . ? C63 C62 H62 120.6 . . ? C61 C62 H62 120.6 . . ? C62 C63 C64 120.7(16) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C63 C64 C65 120.0(17) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? N6 C65 C64 119.1(14) . . ? N6 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? F3' P1 F2 134.9(16) . . ? F3' P1 F1 84.9(18) . . ? F2 P1 F1 134.6(18) . . ? F3' P1 F6 82.4(13) . . ? F2 P1 F6 82.9(13) . . ? F1 P1 F6 82(2) . . ? F3' P1 F4' 45.8(11) . . ? F2 P1 F4' 91.0(16) . . ? F1 P1 F4' 130.7(19) . . ? F6 P1 F4' 87.1(18) . . ? F3' P1 F5 101.3(14) . . ? F2 P1 F5 93.9(12) . . ? F1 P1 F5 99(2) . . ? F6 P1 F5 176.3(10) . . ? F4' P1 F5 94.9(19) . . ? F3' P1 F1' 130.4(18) . . ? F2 P1 F1' 92.5(16) . . ? F1 P1 F1' 45.5(12) . . ? F6 P1 F1' 92(2) . . ? F4' P1 F1' 176.2(18) . . ? F5 P1 F1' 86(2) . . ? F3' P1 F4 94.6(13) . . ? F2 P1 F4 44.4(11) . . ? F1 P1 F4 176(2) . . ? F6 P1 F4 94.0(14) . . ? F4' P1 F4 48.8(11) . . ? F5 P1 F4 84.9(14) . . ? F1' P1 F4 135.0(15) . . ? F3' P1 F2' 173.8(16) . . ? F2 P1 F2' 45.0(11) . . ? F1 P1 F2' 92.9(14) . . ? F6 P1 F2' 91.6(11) . . ? F4' P1 F2' 135.6(15) . . ? F5 P1 F2' 84.8(13) . . ? F1' P1 F2' 48.0(11) . . ? F4 P1 F2' 87.2(12) . . ? F3' P1 F3 48.6(10) . . ? F2 P1 F3 174.1(14) . . ? F1 P1 F3 46.0(12) . . ? F6 P1 F3 102.8(11) . . ? F4' P1 F3 90.8(15) . . ? F5 P1 F3 80.4(10) . . ? F1' P1 F3 85.9(16) . . ? F4 P1 F3 135.5(14) . . ? F2' P1 F3 132.4(14) . . ? F1' F1 F3 125(4) . . ? F1' F1 P1 67.7(14) . . ? F3 F1 P1 69.6(13) . . ? F1 F1' F2' 132(2) . . ? F1 F1' P1 66.8(14) . . ? F2' F1' P1 66.2(13) . . ? F2' F2 F4 133(2) . . ? F2' F2 P1 68.9(13) . . ? F4 F2 P1 69.5(13) . . ? F2 F2' F1' 131(2) . . ? F2 F2' P1 66.2(12) . . ? F1' F2' P1 65.7(12) . . ? F1 F3 F3' 111(3) . . ? F1 F3 P1 64.4(13) . . ? F3' F3 P1 62.8(10) . . ? F4' F3' F3 129(3) . . ? F4' F3' P1 67.8(12) . . ? F3 F3' P1 68.6(12) . . ? F2 F4 F4' 127(2) . . ? F2 F4 P1 66.1(12) . . ? F4' F4 P1 64.8(11) . . ? F3' F4' F4 133(2) . . ? F3' F4' P1 66.3(13) . . ? F4 F4' P1 66.4(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.663 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.075