# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Mir Wais Hosseini' 'Pierre Dechambenoit' 'Sylvie Ferlay' 'Nathalie Kyritsakas' 'Jean-Marc Planeix' _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur Strasbourg F-67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Molecular tectonics: control of packing of hybrid 1-D and 2-D H-bonded molecular networks formed between bisamidinium dication and cyanometallate anions ; # Attachment 'B606265M_2-Co.cif' data_e470a _database_code_depnum_ccdc_archive 'CCDC 611940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Co N6)' _chemical_formula_sum 'C90 H132 Co2 N24' _chemical_formula_weight 1668.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 17.8434(6) _cell_length_b 17.8434(6) _cell_length_c 8.6540(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2386.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1738 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 25.71 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9801 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15160 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 30.05 _reflns_number_total 4646 _reflns_number_gt 2932 _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^)+(0.0724P)^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 4646 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 C1 C 0.60373(13) 0.05996(13) 0.2736(3) 0.0223(4) Uani 1 1 d . . . N1 N 0.67151(12) 0.13816(11) 0.2689(2) 0.0237(4) Uani 1 1 d . . . H1 H 0.6816 0.1690 0.1842 0.028 Uiso 1 1 calc R . . C2 C 0.73081(14) 0.17582(13) 0.3997(2) 0.0244(5) Uani 1 1 d . . . H2A H 0.7115 0.2082 0.4661 0.029 Uiso 1 1 calc R . . H2B H 0.7896 0.2170 0.3611 0.029 Uiso 1 1 calc R . . C3 C 0.73361(14) 0.10499(14) 0.4946(3) 0.0229(5) Uani 1 1 d . . . C4 C 0.63943(14) 0.03783(14) 0.5347(3) 0.0236(5) Uani 1 1 d . . . H4A H 0.6377 -0.0129 0.5848 0.028 Uiso 1 1 calc R . . H4B H 0.6161 0.0634 0.6086 0.028 Uiso 1 1 calc R . . C5 C 0.78353(16) 0.14770(15) 0.6438(3) 0.0299(5) Uani 1 1 d . . . H5A H 0.8411 0.1964 0.6148 0.036 Uiso 1 1 calc R . . H5B H 0.7524 0.1725 0.6991 0.036 Uiso 1 1 calc R . . C6 C 0.7967(2) 0.0896(2) 0.7548(4) 0.0603(9) Uani 1 1 d . . . H6A H 0.7396 0.0397 0.7824 0.072 Uiso 1 1 calc R . . H6B H 0.8305 0.0668 0.7025 0.072 Uiso 1 1 calc R . . C7 C 0.8430(2) 0.1357(2) 0.9007(3) 0.0636(10) Uani 1 1 d . . . H7A H 0.8988 0.1864 0.8741 0.095 Uiso 1 1 calc R . . H7B H 0.8528 0.0964 0.9655 0.095 Uiso 1 1 calc R . . H7C H 0.8076 0.1544 0.9574 0.095 Uiso 1 1 calc R . . C8 C 0.77295(14) 0.05928(15) 0.4023(3) 0.0277(5) Uani 1 1 d . . . H8A H 0.7717 0.0135 0.4688 0.033 Uiso 1 1 calc R . . H8B H 0.7346 0.0301 0.3130 0.033 Uiso 1 1 calc R . . C9 C 0.86419(17) 0.11397(18) 0.3418(4) 0.0456(7) Uani 1 1 d . . . H9A H 0.9017 0.1518 0.4258 0.055 Uiso 1 1 calc R . . H9B H 0.8643 0.1515 0.2575 0.055 Uiso 1 1 calc R . . C10 C 0.90117(19) 0.0587(2) 0.2812(4) 0.0530(8) Uani 1 1 d . . . H10A H 0.9060 0.0251 0.3664 0.080 Uiso 1 1 calc R . . H10B H 0.9586 0.0963 0.2367 0.080 Uiso 1 1 calc R . . H10C H 0.8627 0.0191 0.2016 0.080 Uiso 1 1 calc R . . N2 N 0.58572(11) 0.00989(11) 0.3958(2) 0.0249(4) Uani 1 1 d . . . H2 H 0.5398 -0.0422 0.3937 0.030 Uiso 1 1 calc R . . C11 C 0.54903(13) 0.02824(13) 0.1337(2) 0.0225(5) Uani 1 1 d . . . C12 C 0.52477(14) -0.05383(13) 0.0744(3) 0.0245(5) Uani 1 1 d . . . H12 H 0.5414 -0.0903 0.1258 0.029 Uiso 1 1 calc R . . C13 C 0.47613(14) -0.08120(14) -0.0604(3) 0.0254(5) Uani 1 1 d . . . H13 H 0.4601 -0.1364 -0.1025 0.030 Uiso 1 1 calc R . . Co1 Co 0.3333 0.6667 0.22239(6) 0.01800(15) Uani 1 3 d S . . C14 C 0.40115(13) 0.76782(13) 0.3440(2) 0.0200(4) Uani 1 1 d . . . N3 N 0.44527(12) 0.83046(12) 0.4104(2) 0.0271(4) Uani 1 1 d . . . C15 C 0.29738(13) 0.72729(13) 0.0907(3) 0.0218(4) Uani 1 1 d . . . N4 N 0.27472(13) 0.76102(13) 0.0046(2) 0.0317(5) 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 C1 0.0209(10) 0.0190(10) 0.0263(12) -0.0004(9) -0.0015(9) 0.0095(8) N1 0.0253(9) 0.0169(8) 0.0226(10) 0.0017(7) -0.0057(7) 0.0057(7) C2 0.0232(11) 0.0187(10) 0.0262(12) -0.0019(9) -0.0062(9) 0.0065(9) C3 0.0231(11) 0.0223(10) 0.0238(11) -0.0020(9) -0.0031(9) 0.0117(9) C4 0.0260(11) 0.0210(10) 0.0225(11) 0.0023(9) -0.0026(9) 0.0108(9) C5 0.0325(12) 0.0322(13) 0.0280(13) -0.0072(10) -0.0107(10) 0.0184(11) C6 0.090(3) 0.061(2) 0.0447(18) -0.0108(16) -0.0325(18) 0.049(2) C7 0.092(3) 0.096(3) 0.0372(17) -0.0172(17) -0.0251(17) 0.073(2) C8 0.0287(12) 0.0252(11) 0.0304(13) -0.0023(10) -0.0042(10) 0.0144(10) C9 0.0307(14) 0.0411(15) 0.0591(19) -0.0185(14) 0.0011(13) 0.0135(12) C10 0.0396(16) 0.0613(19) 0.063(2) -0.0107(16) 0.0060(14) 0.0286(15) N2 0.0213(9) 0.0184(9) 0.0278(10) 0.0021(8) -0.0025(8) 0.0045(7) C11 0.0194(10) 0.0184(10) 0.0249(11) 0.0010(9) -0.0022(9) 0.0058(8) C12 0.0242(11) 0.0195(10) 0.0273(12) 0.0004(9) -0.0056(9) 0.0092(9) C13 0.0249(11) 0.0185(10) 0.0307(12) -0.0018(9) -0.0038(10) 0.0093(9) Co1 0.01569(17) 0.01569(17) 0.0226(3) 0.000 0.000 0.00785(8) C14 0.0169(9) 0.0183(10) 0.0248(11) 0.0039(8) 0.0034(8) 0.0086(8) N3 0.0248(10) 0.0204(9) 0.0339(11) -0.0008(8) -0.0004(8) 0.0096(8) C15 0.0177(10) 0.0193(10) 0.0265(11) 0.0008(9) 0.0026(9) 0.0079(8) N4 0.0309(11) 0.0301(11) 0.0350(12) 0.0085(9) 0.0031(9) 0.0160(9) _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 C1 N1 1.313(3) . ? C1 N2 1.316(3) . ? C1 C11 1.479(3) . ? N1 C2 1.463(3) . ? N1 H1 0.8800 . ? C2 C3 1.529(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.536(3) . ? C3 C4 1.538(3) . ? C3 C8 1.539(3) . ? C4 N2 1.461(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.509(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.513(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.529(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2 H2 0.8800 . ? C11 C13 1.386(3) 4_655 ? C11 C12 1.401(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C11 1.386(3) 4_655 ? C13 H13 0.9500 . ? Co1 C15 1.891(2) 3_565 ? Co1 C15 1.891(2) . ? Co1 C15 1.891(2) 2_665 ? Co1 C14 1.909(2) . ? Co1 C14 1.909(2) 3_565 ? Co1 C14 1.909(2) 2_665 ? C14 N3 1.149(3) . ? C15 N4 1.151(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 C1 N2 121.9(2) . . ? N1 C1 C11 117.55(19) . . ? N2 C1 C11 120.49(18) . . ? C1 N1 C2 122.31(18) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 110.55(16) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C5 106.97(17) . . ? C2 C3 C4 106.88(17) . . ? C5 C3 C4 109.50(18) . . ? C2 C3 C8 111.77(18) . . ? C5 C3 C8 113.21(18) . . ? C4 C3 C8 108.31(17) . . ? N2 C4 C3 110.81(17) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C3 116.3(2) . . ? C6 C5 H5A 108.2 . . ? C3 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C3 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 112.8(3) . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 117.82(19) . . ? C9 C8 H8A 107.9 . . ? C3 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? C3 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 C10 112.0(2) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 N2 C4 122.24(17) . . ? C1 N2 H2 118.9 . . ? C4 N2 H2 118.9 . . ? C13 C11 C12 120.6(2) 4_655 . ? C13 C11 C1 119.39(19) 4_655 . ? C12 C11 C1 120.01(19) . . ? C13 C12 C11 119.2(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C11 C13 C12 120.2(2) 4_655 . ? C11 C13 H13 119.9 4_655 . ? C12 C13 H13 119.9 . . ? C15 Co1 C15 87.41(10) 3_565 . ? C15 Co1 C15 87.41(10) 3_565 2_665 ? C15 Co1 C15 87.41(10) . 2_665 ? C15 Co1 C14 88.42(9) 3_565 . ? C15 Co1 C14 91.58(9) . . ? C15 Co1 C14 175.74(9) 2_665 . ? C15 Co1 C14 91.58(9) 3_565 3_565 ? C15 Co1 C14 175.74(9) . 3_565 ? C15 Co1 C14 88.41(9) 2_665 3_565 ? C14 Co1 C14 92.53(9) . 3_565 ? C15 Co1 C14 175.74(9) 3_565 2_665 ? C15 Co1 C14 88.41(9) . 2_665 ? C15 Co1 C14 91.58(9) 2_665 2_665 ? C14 Co1 C14 92.53(9) . 2_665 ? C14 Co1 C14 92.53(9) 3_565 2_665 ? N3 C14 Co1 176.11(19) . . ? N4 C15 Co1 176.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.913 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.077 # Attachment 'B606265M_2-Cr.cif' data_e485a _database_code_depnum_ccdc_archive 'CCDC 611941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Cr N6)' _chemical_formula_sum 'C90 H132 Cr2 N24' _chemical_formula_weight 1654.20 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.1638(14) _cell_length_b 18.1638(14) _cell_length_c 8.5506(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2443.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1865 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 23.36 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9729 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19843 _diffrn_reflns_av_R_equivalents 0.0862 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3753 _reflns_number_gt 2371 _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^)+(0.0799P)^2^+0.2526P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3753 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.60642(16) 0.06022(16) 0.2720(3) 0.0263(6) Uani 1 1 d . . . N1 N 0.67360(13) 0.13608(13) 0.2655(2) 0.0272(5) Uani 1 1 d . . . H1 H 0.6834 0.1661 0.1793 0.033 Uiso 1 1 calc R . . C2 C 0.73306(16) 0.17295(16) 0.3958(3) 0.0278(6) Uani 1 1 d . . . H2A H 0.7158 0.2062 0.4628 0.033 Uiso 1 1 calc R . . H2B H 0.7907 0.2121 0.3549 0.033 Uiso 1 1 calc R . . C3 C 0.73489(16) 0.10358(16) 0.4930(3) 0.0266(6) Uani 1 1 d . . . C4 C 0.64301(16) 0.03936(17) 0.5363(3) 0.0293(6) Uani 1 1 d . . . H4A H 0.6409 -0.0106 0.5874 0.035 Uiso 1 1 calc R . . H4B H 0.6214 0.0656 0.6115 0.035 Uiso 1 1 calc R . . C5 C 0.78521(18) 0.14600(18) 0.6439(3) 0.0339(6) Uani 1 1 d . . . H5A H 0.8419 0.1932 0.6135 0.041 Uiso 1 1 calc R . . H5B H 0.7555 0.1712 0.7001 0.041 Uiso 1 1 calc R . . C6 C 0.7978(3) 0.0891(3) 0.7563(4) 0.0628(11) Uani 1 1 d . . . H6A H 0.8300 0.0655 0.7030 0.075 Uiso 1 1 calc R . . H6B H 0.7416 0.0409 0.7860 0.075 Uiso 1 1 calc R . . C7 C 0.8451(3) 0.1351(3) 0.9028(4) 0.0737(13) Uani 1 1 d . . . H7A H 0.9020 0.1811 0.8747 0.111 Uiso 1 1 calc R . . H7B H 0.8500 0.0951 0.9728 0.111 Uiso 1 1 calc R . . H7C H 0.8139 0.1589 0.9558 0.111 Uiso 1 1 calc R . . C8 C 0.77262(17) 0.05750(17) 0.4001(3) 0.0305(6) Uani 1 1 d . . . H8A H 0.7675 0.0101 0.4652 0.037 Uiso 1 1 calc R . . H8B H 0.7370 0.0321 0.3060 0.037 Uiso 1 1 calc R . . C9 C 0.86375(19) 0.1094(2) 0.3476(4) 0.0462(8) Uani 1 1 d . . . H9A H 0.8991 0.1432 0.4371 0.055 Uiso 1 1 calc R . . H9B H 0.8678 0.1496 0.2654 0.055 Uiso 1 1 calc R . . C10 C 0.8990(2) 0.0547(2) 0.2838(4) 0.0552(9) Uani 1 1 d . . . H10A H 0.8979 0.0167 0.3664 0.083 Uiso 1 1 calc R . . H10B H 0.9577 0.0914 0.2487 0.083 Uiso 1 1 calc R . . H10C H 0.8641 0.0208 0.1956 0.083 Uiso 1 1 calc R . . N2 N 0.58876(14) 0.01174(14) 0.3964(2) 0.0302(5) Uani 1 1 d . . . H2 H 0.5429 -0.0389 0.3959 0.036 Uiso 1 1 calc R . . C11 C 0.55005(16) 0.02808(16) 0.1329(3) 0.0275(6) Uani 1 1 d . . . C12 C 0.52303(17) -0.05333(16) 0.0761(3) 0.0306(6) Uani 1 1 d . . . H12 H 0.5392 -0.0893 0.1278 0.037 Uiso 1 1 calc R . . C13 C 0.47242(16) -0.08158(16) -0.0564(3) 0.0302(6) Uani 1 1 d . . . H13 H 0.4531 -0.1374 -0.0949 0.036 Uiso 1 1 calc R . . Cr1 Cr 0.3333 0.6667 0.24323(8) 0.0236(2) Uani 1 3 d S . . C14 C 0.40667(16) 0.77561(16) 0.3750(3) 0.0260(6) Uani 1 1 d . . . N3 N 0.45131(15) 0.83899(14) 0.4374(3) 0.0345(6) Uani 1 1 d . . . C15 C 0.29340(16) 0.73010(17) 0.0964(3) 0.0287(6) Uani 1 1 d . . . N4 N 0.27068(16) 0.76166(16) 0.0074(3) 0.0390(6) 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 C1 0.0222(13) 0.0213(13) 0.0340(13) -0.0002(10) -0.0016(10) 0.0098(11) N1 0.0259(12) 0.0203(11) 0.0302(11) 0.0020(9) -0.0059(9) 0.0077(10) C2 0.0257(14) 0.0203(13) 0.0320(13) -0.0047(10) -0.0075(11) 0.0074(11) C3 0.0266(14) 0.0243(14) 0.0294(13) -0.0021(10) -0.0052(10) 0.0131(11) C4 0.0299(14) 0.0290(14) 0.0286(13) 0.0031(10) -0.0021(11) 0.0144(12) C5 0.0356(16) 0.0381(16) 0.0319(14) -0.0080(12) -0.0079(11) 0.0214(14) C6 0.088(3) 0.071(3) 0.0468(19) -0.0088(17) -0.0280(19) 0.053(2) C7 0.099(3) 0.117(4) 0.044(2) -0.018(2) -0.027(2) 0.083(3) C8 0.0306(15) 0.0283(14) 0.0346(14) -0.0017(11) -0.0032(11) 0.0160(12) C9 0.0330(17) 0.0445(19) 0.0559(19) -0.0159(15) -0.0022(14) 0.0154(15) C10 0.044(2) 0.061(2) 0.068(2) -0.0058(18) 0.0050(17) 0.0318(19) N2 0.0252(12) 0.0204(11) 0.0374(12) 0.0014(9) -0.0042(9) 0.0058(9) C11 0.0208(13) 0.0212(13) 0.0355(14) -0.0001(10) -0.0047(10) 0.0068(11) C12 0.0275(14) 0.0211(14) 0.0404(15) 0.0027(11) -0.0056(11) 0.0101(12) C13 0.0266(14) 0.0194(13) 0.0409(15) -0.0032(11) -0.0074(11) 0.0087(11) Cr1 0.0180(3) 0.0180(3) 0.0349(4) 0.000 0.000 0.00901(13) C14 0.0207(13) 0.0221(13) 0.0364(13) 0.0048(11) 0.0039(10) 0.0116(11) N3 0.0287(13) 0.0225(12) 0.0482(14) 0.0000(10) -0.0005(10) 0.0096(11) C15 0.0224(13) 0.0247(14) 0.0359(13) 0.0030(11) 0.0034(11) 0.0093(11) N4 0.0378(14) 0.0388(14) 0.0423(13) 0.0095(11) 0.0054(11) 0.0205(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 C1 N1 1.307(3) . ? C1 N2 1.314(3) . ? C1 C11 1.485(3) . ? N1 C2 1.461(3) . ? N1 H1 0.8800 . ? C2 C3 1.524(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.528(4) . ? C3 C8 1.541(4) . ? C3 C5 1.545(3) . ? C4 N2 1.469(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.506(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.527(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2 H2 0.8800 . ? C11 C13 1.391(4) 4_655 ? C11 C12 1.392(3) . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C11 1.391(4) 4_655 ? C13 H13 0.9500 . ? Cr1 C15 2.065(3) . ? Cr1 C15 2.065(3) 3_565 ? Cr1 C15 2.065(3) 2_665 ? Cr1 C14 2.079(3) 3_565 ? Cr1 C14 2.079(3) 2_665 ? Cr1 C14 2.079(3) . ? C14 N3 1.155(3) . ? C15 N4 1.147(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 C1 N2 121.8(2) . . ? N1 C1 C11 118.5(2) . . ? N2 C1 C11 119.7(2) . . ? C1 N1 C2 122.5(2) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 110.72(19) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 107.2(2) . . ? C2 C3 C8 111.5(2) . . ? C4 C3 C8 108.8(2) . . ? C2 C3 C5 107.1(2) . . ? C4 C3 C5 109.0(2) . . ? C8 C3 C5 112.9(2) . . ? N2 C4 C3 110.7(2) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C3 116.4(2) . . ? C6 C5 H5A 108.2 . . ? C3 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C3 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 112.8(3) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 117.5(2) . . ? C9 C8 H8A 107.9 . . ? C3 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? C3 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 C10 112.7(3) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 N2 C4 122.2(2) . . ? C1 N2 H2 118.9 . . ? C4 N2 H2 118.9 . . ? C13 C11 C12 120.4(2) 4_655 . ? C13 C11 C1 119.2(2) 4_655 . ? C12 C11 C1 120.3(2) . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C11 119.9(2) . 4_655 ? C12 C13 H13 120.1 . . ? C11 C13 H13 120.1 4_655 . ? C15 Cr1 C15 86.89(11) . 3_565 ? C15 Cr1 C15 86.89(11) . 2_665 ? C15 Cr1 C15 86.90(11) 3_565 2_665 ? C15 Cr1 C14 174.42(10) . 3_565 ? C15 Cr1 C14 92.01(10) 3_565 3_565 ? C15 Cr1 C14 87.58(10) 2_665 3_565 ? C15 Cr1 C14 87.58(10) . 2_665 ? C15 Cr1 C14 174.42(10) 3_565 2_665 ? C15 Cr1 C14 92.01(10) 2_665 2_665 ? C14 Cr1 C14 93.41(9) 3_565 2_665 ? C15 Cr1 C14 92.01(10) . . ? C15 Cr1 C14 87.58(10) 3_565 . ? C15 Cr1 C14 174.42(11) 2_665 . ? C14 Cr1 C14 93.41(9) 3_565 . ? C14 Cr1 C14 93.41(9) 2_665 . ? N3 C14 Cr1 174.4(2) . . ? N4 C15 Cr1 175.5(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.890 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.089 # Attachment 'B606265M_2-Fe(alternate).cif' data_e517a_B606265M_2-Fe(alternate).cif _database_code_depnum_ccdc_archive 'CCDC 611942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4),2(C6 Fe N6)' _chemical_formula_sum 'C90 H132 Fe2 N24' _chemical_formula_weight 1661.90 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' Fe Fe 0.3463 0.8444 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 17.9242(4) _cell_length_b 17.9242(4) _cell_length_c 8.6140(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2396.71(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2480 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 22.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16699 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3684 _reflns_number_gt 2613 _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^)+(0.0712P)^2^+0.1118P] 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 3684 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 C1 C 0.39545(13) 0.93962(12) 0.7735(2) 0.0235(4) Uani 1 1 d . . . N1 N 0.41319(11) 0.98923(11) 0.89666(19) 0.0251(4) Uani 1 1 d . . . H1 H 0.4590 1.0410 0.8951 0.030 Uiso 1 1 calc R . . C2 C 0.35934(13) 0.96117(13) 1.0357(2) 0.0257(5) Uani 1 1 d . . . H2A H 0.3612 1.0116 1.0866 0.031 Uiso 1 1 calc R . . H2B H 0.3821 0.9353 1.1098 0.031 Uiso 1 1 calc R . . C3 C 0.26531(13) 0.89465(13) 0.9946(2) 0.0245(4) Uani 1 1 d . . . C4 C 0.26874(13) 0.82448(12) 0.8985(2) 0.0251(5) Uani 1 1 d . . . H4A H 0.2878 0.7922 0.9652 0.030 Uiso 1 1 calc R . . H4B H 0.2104 0.7835 0.8592 0.030 Uiso 1 1 calc R . . N2 N 0.32775(11) 0.86185(10) 0.76821(19) 0.0251(4) Uani 1 1 d . . . H2 H 0.3177 0.8313 0.6829 0.030 Uiso 1 1 calc R . . C5 C 0.22691(13) 0.94058(14) 0.9015(3) 0.0284(5) Uani 1 1 d . . . H5A H 0.2296 0.9872 0.9672 0.034 Uiso 1 1 calc R . . H5B H 0.2645 0.9683 0.8105 0.034 Uiso 1 1 calc R . . C6 C 0.13539(15) 0.88663(16) 0.8436(3) 0.0456(7) Uani 1 1 d . . . H6A H 0.0985 0.8500 0.9294 0.055 Uiso 1 1 calc R . . H6B H 0.1339 0.8482 0.7596 0.055 Uiso 1 1 calc R . . C7 C 0.09897(17) 0.94237(19) 0.7821(3) 0.0537(7) Uani 1 1 d . . . H7A H 0.1371 0.9811 0.7012 0.081 Uiso 1 1 calc R . . H7B H 0.0951 0.9765 0.8674 0.081 Uiso 1 1 calc R . . H7C H 0.0415 0.9051 0.7386 0.081 Uiso 1 1 calc R . . C8 C 0.21564(15) 0.85181(14) 1.1438(2) 0.0309(5) Uani 1 1 d . . . H8A H 0.1586 0.8030 1.1145 0.037 Uiso 1 1 calc R . . H8B H 0.2470 0.8276 1.1999 0.037 Uiso 1 1 calc R . . C9 C 0.2018(2) 0.9098(2) 1.2550(3) 0.0607(9) Uani 1 1 d . . . H9A H 0.2583 0.9597 1.2832 0.073 Uiso 1 1 calc R . . H9B H 0.1679 0.9321 1.2019 0.073 Uiso 1 1 calc R . . C10 C 0.1552(2) 0.8633(2) 1.4015(3) 0.0671(10) Uani 1 1 d . . . H10A H 0.1914 0.8466 1.4604 0.101 Uiso 1 1 calc R . . H10B H 0.1009 0.8116 1.3740 0.101 Uiso 1 1 calc R . . H10C H 0.1432 0.9014 1.4649 0.101 Uiso 1 1 calc R . . C11 C 0.45046(13) 0.97136(13) 0.6336(2) 0.0242(4) Uani 1 1 d . . . C12 C 0.47576(13) 1.05354(12) 0.5752(2) 0.0254(5) Uani 1 1 d . . . H12 H 0.4593 1.0899 0.6271 0.030 Uiso 1 1 calc R . . C13 C 0.52488(13) 1.08144(13) 0.4415(2) 0.0262(5) Uani 1 1 d . . . H13 H 0.5418 1.1369 0.4009 0.031 Uiso 1 1 calc R . . Fe2 Fe 0.3333 0.6667 0.27136(6) 0.01903(16) Uani 1 3 d S . . C14 C 0.40304(12) 0.76985(12) 0.1477(2) 0.0209(4) Uani 1 1 d . . . N3 N 0.44732(11) 0.83293(11) 0.0825(2) 0.0291(4) Uani 1 1 d . . . C15 C 0.29637(12) 0.72765(12) 0.4075(2) 0.0231(4) Uani 1 1 d . . . N4 N 0.27353(12) 0.76061(12) 0.4950(2) 0.0331(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0226(10) 0.0198(10) 0.0276(11) 0.0001(9) 0.0022(9) 0.0103(8) N1 0.0221(9) 0.0181(8) 0.0281(9) -0.0022(7) 0.0015(7) 0.0047(7) C2 0.0281(11) 0.0241(10) 0.0236(10) -0.0021(9) 0.0026(9) 0.0120(9) C3 0.0251(11) 0.0216(10) 0.0268(11) 0.0015(9) 0.0055(9) 0.0115(9) C4 0.0228(10) 0.0196(10) 0.0295(11) 0.0027(9) 0.0057(9) 0.0081(8) N2 0.0256(9) 0.0184(8) 0.0252(9) -0.0015(7) 0.0055(7) 0.0064(7) C5 0.0288(11) 0.0264(11) 0.0307(11) 0.0024(9) 0.0036(9) 0.0144(9) C6 0.0332(13) 0.0418(14) 0.0556(16) 0.0170(13) -0.0022(12) 0.0140(11) C7 0.0406(15) 0.0616(18) 0.0636(18) 0.0101(15) -0.0031(14) 0.0291(14) C8 0.0336(12) 0.0335(12) 0.0287(11) 0.0050(10) 0.0071(10) 0.0190(10) C9 0.090(2) 0.0656(19) 0.0441(16) 0.0091(15) 0.0292(16) 0.0525(19) C10 0.096(3) 0.101(3) 0.0389(15) 0.0210(17) 0.0293(16) 0.076(2) C11 0.0206(10) 0.0208(10) 0.0259(11) -0.0003(8) 0.0014(8) 0.0063(8) C12 0.0256(11) 0.0204(10) 0.0298(11) -0.0025(9) 0.0043(9) 0.0113(9) C13 0.0253(11) 0.0181(10) 0.0326(11) 0.0030(9) 0.0043(9) 0.0088(8) Fe2 0.01651(18) 0.01651(18) 0.0241(3) 0.000 0.000 0.00826(9) C14 0.0176(9) 0.0206(10) 0.0255(10) -0.0018(8) -0.0025(8) 0.0103(8) N3 0.0270(9) 0.0234(9) 0.0351(10) 0.0015(8) 0.0009(8) 0.0113(8) C15 0.0191(10) 0.0200(10) 0.0278(10) -0.0012(8) -0.0037(8) 0.0081(8) N4 0.0318(10) 0.0327(10) 0.0363(10) -0.0089(9) -0.0028(9) 0.0174(9) _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 C1 N2 1.314(2) . ? C1 N1 1.317(2) . ? C1 C11 1.479(3) . ? N1 C2 1.461(3) . ? N1 H1 0.8800 . ? C2 C3 1.542(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.533(3) . ? C3 C8 1.533(3) . ? C3 C5 1.537(3) . ? C4 N2 1.456(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.513(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.535(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.389(3) 4_676 ? C11 C12 1.400(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C11 1.389(3) 4_676 ? C13 H13 0.9500 . ? Fe2 C15 1.932(2) . ? Fe2 C15 1.932(2) 3_565 ? Fe2 C15 1.932(2) 2_665 ? Fe2 C14 1.951(2) . ? Fe2 C14 1.951(2) 3_565 ? Fe2 C14 1.951(2) 2_665 ? C14 N3 1.152(2) . ? C15 N4 1.152(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 N2 C1 N1 121.84(19) . . ? N2 C1 C11 117.66(18) . . ? N1 C1 C11 120.48(18) . . ? C1 N1 C2 122.22(17) . . ? C1 N1 H1 118.9 . . ? C2 N1 H1 118.9 . . ? N1 C2 C3 110.88(16) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C8 107.07(16) . . ? C4 C3 C5 111.71(17) . . ? C8 C3 C5 113.72(17) . . ? C4 C3 C2 106.38(16) . . ? C8 C3 C2 109.36(17) . . ? C5 C3 C2 108.34(16) . . ? N2 C4 C3 110.92(16) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C1 N2 C4 122.32(17) . . ? C1 N2 H2 118.8 . . ? C4 N2 H2 118.8 . . ? C6 C5 C3 117.55(18) . . ? C6 C5 H5A 107.9 . . ? C3 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C3 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 112.1(2) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 115.96(19) . . ? C9 C8 H8A 108.3 . . ? C3 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C3 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 112.4(2) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 120.23(19) 4_676 . ? C13 C11 C1 119.73(18) 4_676 . ? C12 C11 C1 120.02(18) . . ? C13 C12 C11 119.50(19) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C11 120.26(19) . 4_676 ? C12 C13 H13 119.9 . . ? C11 C13 H13 119.9 4_676 . ? C15 Fe2 C15 86.99(9) . 3_565 ? C15 Fe2 C15 86.99(9) . 2_665 ? C15 Fe2 C15 86.99(9) 3_565 2_665 ? C15 Fe2 C14 91.91(8) . . ? C15 Fe2 C14 87.99(8) 3_565 . ? C15 Fe2 C14 174.91(8) 2_665 . ? C15 Fe2 C14 174.91(8) . 3_565 ? C15 Fe2 C14 91.91(8) 3_565 3_565 ? C15 Fe2 C14 87.99(8) 2_665 3_565 ? C14 Fe2 C14 93.02(8) . 3_565 ? C15 Fe2 C14 87.99(8) . 2_665 ? C15 Fe2 C14 174.91(8) 3_565 2_665 ? C15 Fe2 C14 91.91(8) 2_665 2_665 ? C14 Fe2 C14 93.02(8) . 2_665 ? C14 Fe2 C14 93.02(8) 3_565 2_665 ? N3 C14 Fe2 175.83(18) . . ? N4 C15 Fe2 176.13(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.377 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.093 # Attachment 'B606265M_2-Fe.cif' data_e517a _database_code_depnum_ccdc_archive 'CCDC 611943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Fe N6)' _chemical_formula_sum 'C90 H132 Fe2 N24' _chemical_formula_weight 1661.90 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' Fe Fe 0.3463 0.8444 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 17.9242(4) _cell_length_b 17.9242(4) _cell_length_c 8.6140(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2396.71(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2480 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 22.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16699 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3684 _reflns_number_gt 2613 _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^)+(0.0712P)^2^+0.1118P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3684 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _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 C1 C 0.60455(13) 0.06038(12) 0.7265(2) 0.0235(4) Uani 1 1 d . . . N1 N 0.58681(11) 0.01077(11) 0.60334(19) 0.0251(4) Uani 1 1 d . . . H1 H 0.5410 -0.0410 0.6049 0.030 Uiso 1 1 calc R . . C2 C 0.64066(13) 0.03883(13) 0.4643(2) 0.0257(5) Uani 1 1 d . . . H2A H 0.6179 0.0647 0.3902 0.031 Uiso 1 1 calc R . . H2B H 0.6388 -0.0116 0.4134 0.031 Uiso 1 1 calc R . . C3 C 0.73469(13) 0.10535(13) 0.5054(2) 0.0245(4) Uani 1 1 d . . . C4 C 0.73126(13) 0.17552(12) 0.6015(2) 0.0251(5) Uani 1 1 d . . . H4A H 0.7896 0.2165 0.6408 0.030 Uiso 1 1 calc R . . H4B H 0.7122 0.2078 0.5348 0.030 Uiso 1 1 calc R . . N2 N 0.67225(11) 0.13815(10) 0.73179(19) 0.0251(4) Uani 1 1 d . . . H2 H 0.6823 0.1687 0.8171 0.030 Uiso 1 1 calc R . . C5 C 0.77309(13) 0.05942(14) 0.5985(3) 0.0284(5) Uani 1 1 d . . . H5A H 0.7355 0.0317 0.6895 0.034 Uiso 1 1 calc R . . H5B H 0.7704 0.0128 0.5328 0.034 Uiso 1 1 calc R . . C6 C 0.86461(15) 0.11337(16) 0.6564(3) 0.0456(7) Uani 1 1 d . . . H6A H 0.8661 0.1518 0.7404 0.055 Uiso 1 1 calc R . . H6B H 0.9015 0.1500 0.5706 0.055 Uiso 1 1 calc R . . C7 C 0.90103(17) 0.05763(19) 0.7179(3) 0.0537(7) Uani 1 1 d . . . H7A H 0.8629 0.0189 0.7988 0.081 Uiso 1 1 calc R . . H7B H 0.9585 0.0949 0.7614 0.081 Uiso 1 1 calc R . . H7C H 0.9049 0.0235 0.6326 0.081 Uiso 1 1 calc R . . C8 C 0.78436(15) 0.14819(14) 0.3562(2) 0.0309(5) Uani 1 1 d . . . H8A H 0.7530 0.1724 0.3001 0.037 Uiso 1 1 calc R . . H8B H 0.8414 0.1970 0.3855 0.037 Uiso 1 1 calc R . . C9 C 0.7982(2) 0.0902(2) 0.2450(3) 0.0607(9) Uani 1 1 d . . . H9A H 0.8321 0.0679 0.2981 0.073 Uiso 1 1 calc R . . H9B H 0.7417 0.0403 0.2168 0.073 Uiso 1 1 calc R . . C10 C 0.8448(2) 0.1367(2) 0.0985(3) 0.0671(10) Uani 1 1 d . . . H10A H 0.8086 0.1534 0.0396 0.101 Uiso 1 1 calc R . . H10B H 0.8568 0.0986 0.0351 0.101 Uiso 1 1 calc R . . H10C H 0.8991 0.1884 0.1260 0.101 Uiso 1 1 calc R . . C11 C 0.54954(13) 0.02864(13) 0.8664(2) 0.0242(4) Uani 1 1 d . . . C12 C 0.52424(13) -0.05354(12) 0.9248(2) 0.0254(5) Uani 1 1 d . . . H12 H 0.5407 -0.0899 0.8729 0.030 Uiso 1 1 calc R . . C13 C 0.47512(13) -0.08144(13) 1.0585(2) 0.0262(5) Uani 1 1 d . . . H13 H 0.4582 -0.1369 1.0991 0.031 Uiso 1 1 calc R . . Fe2 Fe 0.6667 0.3333 0.22864(6) 0.01903(16) Uani 1 3 d S . . C14 C 0.59696(12) 0.23015(12) 0.3523(2) 0.0209(4) Uani 1 1 d . . . N3 N 0.55268(11) 0.16707(11) 0.4175(2) 0.0291(4) Uani 1 1 d . . . C15 C 0.70363(12) 0.27235(12) 0.0925(2) 0.0231(4) Uani 1 1 d . . . N4 N 0.72647(12) 0.23939(12) 0.0050(2) 0.0331(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0226(10) 0.0198(10) 0.0276(11) 0.0001(9) 0.0022(9) 0.0103(8) N1 0.0221(9) 0.0181(8) 0.0281(9) -0.0022(7) 0.0015(7) 0.0047(7) C2 0.0281(11) 0.0241(10) 0.0236(10) -0.0021(9) 0.0026(9) 0.0120(9) C3 0.0251(11) 0.0216(10) 0.0268(11) 0.0015(9) 0.0055(9) 0.0115(9) C4 0.0228(10) 0.0196(10) 0.0295(11) 0.0027(9) 0.0057(9) 0.0081(8) N2 0.0256(9) 0.0184(8) 0.0252(9) -0.0015(7) 0.0055(7) 0.0064(7) C5 0.0288(11) 0.0264(11) 0.0307(11) 0.0024(9) 0.0036(9) 0.0144(9) C6 0.0332(13) 0.0418(14) 0.0556(16) 0.0170(13) -0.0022(12) 0.0140(11) C7 0.0406(15) 0.0616(18) 0.0636(18) 0.0101(15) -0.0031(14) 0.0291(14) C8 0.0336(12) 0.0335(12) 0.0287(11) 0.0050(10) 0.0071(10) 0.0190(10) C9 0.090(2) 0.0656(19) 0.0441(16) 0.0091(15) 0.0292(16) 0.0525(19) C10 0.096(3) 0.101(3) 0.0389(15) 0.0210(17) 0.0293(16) 0.076(2) C11 0.0206(10) 0.0208(10) 0.0259(11) -0.0003(8) 0.0014(8) 0.0063(8) C12 0.0256(11) 0.0204(10) 0.0298(11) -0.0025(9) 0.0043(9) 0.0113(9) C13 0.0253(11) 0.0181(10) 0.0326(11) 0.0030(9) 0.0043(9) 0.0088(8) Fe2 0.01651(18) 0.01651(18) 0.0241(3) 0.000 0.000 0.00826(9) C14 0.0176(9) 0.0206(10) 0.0255(10) -0.0018(8) -0.0025(8) 0.0103(8) N3 0.0270(9) 0.0234(9) 0.0351(10) 0.0015(8) 0.0009(8) 0.0113(8) C15 0.0191(10) 0.0200(10) 0.0278(10) -0.0012(8) -0.0037(8) 0.0081(8) N4 0.0318(10) 0.0327(10) 0.0363(10) -0.0089(9) -0.0028(9) 0.0174(9) _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 C1 N2 1.314(2) . ? C1 N1 1.317(2) . ? C1 C11 1.479(3) . ? N1 C2 1.461(3) . ? N1 H1 0.8800 . ? C2 C3 1.542(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.533(3) . ? C3 C8 1.533(3) . ? C3 C5 1.537(3) . ? C4 N2 1.456(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.513(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.535(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.389(3) 4_657 ? C11 C12 1.400(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C11 1.389(3) 4_657 ? C13 H13 0.9500 . ? Fe2 C15 1.932(2) 3_665 ? Fe2 C15 1.932(2) 2_655 ? Fe2 C15 1.932(2) . ? Fe2 C14 1.951(2) 2_655 ? Fe2 C14 1.951(2) 3_665 ? Fe2 C14 1.951(2) . ? C14 N3 1.152(2) . ? C15 N4 1.152(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 N2 C1 N1 121.84(19) . . ? N2 C1 C11 117.66(18) . . ? N1 C1 C11 120.48(17) . . ? C1 N1 C2 122.22(17) . . ? C1 N1 H1 118.9 . . ? C2 N1 H1 118.9 . . ? N1 C2 C3 110.88(16) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C8 107.07(16) . . ? C4 C3 C5 111.71(17) . . ? C8 C3 C5 113.72(17) . . ? C4 C3 C2 106.38(16) . . ? C8 C3 C2 109.36(17) . . ? C5 C3 C2 108.34(16) . . ? N2 C4 C3 110.92(16) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C1 N2 C4 122.32(17) . . ? C1 N2 H2 118.8 . . ? C4 N2 H2 118.8 . . ? C6 C5 C3 117.55(18) . . ? C6 C5 H5A 107.9 . . ? C3 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C3 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 112.1(2) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 115.96(19) . . ? C9 C8 H8A 108.3 . . ? C3 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C3 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 112.4(2) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 120.23(19) 4_657 . ? C13 C11 C1 119.73(18) 4_657 . ? C12 C11 C1 120.02(18) . . ? C13 C12 C11 119.50(19) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C11 120.26(19) . 4_657 ? C12 C13 H13 119.9 . . ? C11 C13 H13 119.9 4_657 . ? C15 Fe2 C15 86.99(9) 3_665 2_655 ? C15 Fe2 C15 86.99(9) 3_665 . ? C15 Fe2 C15 86.99(9) 2_655 . ? C15 Fe2 C14 174.91(8) 3_665 2_655 ? C15 Fe2 C14 91.91(8) 2_655 2_655 ? C15 Fe2 C14 87.99(8) . 2_655 ? C15 Fe2 C14 91.91(8) 3_665 3_665 ? C15 Fe2 C14 87.99(8) 2_655 3_665 ? C15 Fe2 C14 174.91(8) . 3_665 ? C14 Fe2 C14 93.02(8) 2_655 3_665 ? C15 Fe2 C14 87.99(8) 3_665 . ? C15 Fe2 C14 174.91(8) 2_655 . ? C15 Fe2 C14 91.91(8) . . ? C14 Fe2 C14 93.02(8) 2_655 . ? C14 Fe2 C14 93.02(8) 3_665 . ? N3 C14 Fe2 175.83(18) . . ? N4 C15 Fe2 176.13(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.377 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.093 # Attachment 'B606265M_2-HCl_rev.cif' data_e290a _database_code_depnum_ccdc_archive 'CCDC 611944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C26 H48 Cl2 N4 O2' _chemical_formula_weight 519.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1738(6) _cell_length_b 9.4718(6) _cell_length_c 17.6898(13) _cell_angle_alpha 100.914(3) _cell_angle_beta 92.932(4) _cell_angle_gamma 103.963(4) _cell_volume 1457.13(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1566 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description needdle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9753 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13497 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.31 _reflns_number_total 6500 _reflns_number_gt 3766 _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^)+(0.0456P)^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 6500 _refine_ls_number_parameters 325 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 C1 C 0.1136(3) 0.6332(3) 0.12591(14) 0.0222(6) Uani 1 1 d . . . N1 N 0.0601(2) 0.7320(2) 0.17148(12) 0.0228(5) Uani 1 1 d . . . H1 H 0.0699 0.8200 0.1600 0.027 Uiso 1 1 calc . . . C2 C -0.0148(3) 0.7026(3) 0.24022(14) 0.0240(6) Uani 1 1 d . . . H2A H -0.1255 0.6724 0.2268 0.029 Uiso 1 1 calc R . . H2B H 0.0100 0.7948 0.2808 0.029 Uiso 1 1 calc R . . C3 C 0.0346(3) 0.5798(3) 0.27168(14) 0.0201(5) Uani 1 1 d . . . C4 C 0.0183(3) 0.4497(3) 0.20251(14) 0.0248(6) Uani 1 1 d . . . H4A H 0.0585 0.3712 0.2192 0.030 Uiso 1 1 calc R . . H4B H -0.0900 0.4066 0.1841 0.030 Uiso 1 1 calc R . . N2 N 0.0996(2) 0.4983(2) 0.13893(12) 0.0232(5) Uani 1 1 d . . . H2 H 0.1398 0.4360 0.1088 0.028 Uiso 1 1 calc . . . C5 C -0.0749(3) 0.5255(3) 0.32915(14) 0.0243(6) Uani 1 1 d . . . H5A H -0.1783 0.4921 0.3022 0.029 Uiso 1 1 calc R . . H5B H -0.0499 0.4375 0.3437 0.029 Uiso 1 1 calc R . . C6 C -0.0760(3) 0.6375(3) 0.40303(16) 0.0361(7) Uani 1 1 d . . . H6A H 0.0281 0.6773 0.4289 0.043 Uiso 1 1 calc R . . H6B H -0.1110 0.7216 0.3897 0.043 Uiso 1 1 calc R . . C7 C -0.1780(3) 0.5680(3) 0.45829(16) 0.0406(8) Uani 1 1 d . . . H7A H -0.2821 0.5330 0.4337 0.061 Uiso 1 1 calc R . . H7B H -0.1735 0.6424 0.5057 0.061 Uiso 1 1 calc R . . H7C H -0.1444 0.4839 0.4711 0.061 Uiso 1 1 calc R . . C8 C 0.1995(3) 0.6378(3) 0.30841(14) 0.0227(6) Uani 1 1 d . . . H8A H 0.2640 0.6679 0.2680 0.027 Uiso 1 1 calc R . . H8B H 0.2071 0.7282 0.3487 0.027 Uiso 1 1 calc R . . C9 C 0.2629(3) 0.5290(3) 0.34484(17) 0.0360(7) Uani 1 1 d . . . H9A H 0.2715 0.4454 0.3037 0.043 Uiso 1 1 calc R . . H9B H 0.1923 0.4877 0.3804 0.043 Uiso 1 1 calc R . . C10 C 0.4174(3) 0.6032(4) 0.38947(18) 0.0496(9) Uani 1 1 d . . . H10A H 0.4886 0.6407 0.3540 0.074 Uiso 1 1 calc R . . H10B H 0.4537 0.5304 0.4129 0.074 Uiso 1 1 calc R . . H10C H 0.4094 0.6860 0.4302 0.074 Uiso 1 1 calc R . . C11 C 0.1922(3) 0.6777(3) 0.05931(13) 0.0203(6) Uani 1 1 d . . . C12 C 0.1414(3) 0.7741(3) 0.01953(14) 0.0249(6) Uani 1 1 d . . . H12 H 0.0554 0.8078 0.0342 0.030 Uiso 1 1 calc R . . C13 C 0.2153(3) 0.8206(3) -0.04079(14) 0.0241(6) Uani 1 1 d . . . H13 H 0.1804 0.8862 -0.0674 0.029 Uiso 1 1 calc R . . C14 C 0.3415(3) 0.7710(3) -0.06274(13) 0.0199(5) Uani 1 1 d . . . C15 C 0.3906(3) 0.6737(3) -0.02393(14) 0.0249(6) Uani 1 1 d . . . H15 H 0.4755 0.6387 -0.0393 0.030 Uiso 1 1 calc R . . C16 C 0.3173(3) 0.6274(3) 0.03692(14) 0.0242(6) Uani 1 1 d . . . H16 H 0.3521 0.5614 0.0633 0.029 Uiso 1 1 calc R . . C17 C 0.4214(3) 0.8222(3) -0.12741(14) 0.0205(5) Uani 1 1 d . . . N3 N 0.4676(2) 0.7265(2) -0.17816(12) 0.0221(5) Uani 1 1 d . . . H3 H 0.4533 0.6347 -0.1713 0.027 Uiso 1 1 calc . . . C18 C 0.5421(3) 0.7649(3) -0.24590(14) 0.0227(6) Uani 1 1 d . . . H18A H 0.5124 0.6783 -0.2898 0.027 Uiso 1 1 calc R . . H18B H 0.6529 0.7887 -0.2337 0.027 Uiso 1 1 calc R . . C19 C 0.4988(3) 0.8987(3) -0.26925(14) 0.0198(5) Uani 1 1 d . . . C20 C 0.5249(3) 1.0196(3) -0.19501(14) 0.0236(6) Uani 1 1 d . . . H20A H 0.6343 1.0548 -0.1778 0.028 Uiso 1 1 calc R . . H20B H 0.4896 1.1053 -0.2059 0.028 Uiso 1 1 calc R . . N4 N 0.4445(2) 0.9628(2) -0.13360(12) 0.0231(5) Uani 1 1 d . . . H4 H 0.4102 1.0241 -0.0995 0.028 Uiso 1 1 calc . . . C21 C 0.6073(3) 0.9587(3) -0.32603(14) 0.0251(6) Uani 1 1 d . . . H21A H 0.5863 1.0520 -0.3354 0.030 Uiso 1 1 calc R . . H21B H 0.7117 0.9844 -0.3007 0.030 Uiso 1 1 calc R . . C22 C 0.6006(3) 0.8556(3) -0.40401(15) 0.0338(7) Uani 1 1 d . . . H22A H 0.6334 0.7668 -0.3960 0.041 Uiso 1 1 calc R . . H22B H 0.4949 0.8217 -0.4281 0.041 Uiso 1 1 calc R . . C23 C 0.6999(3) 0.9310(3) -0.45840(16) 0.0398(7) Uani 1 1 d . . . H23A H 0.6651 1.0165 -0.4682 0.060 Uiso 1 1 calc R . . H23B H 0.6941 0.8603 -0.5074 0.060 Uiso 1 1 calc R . . H23C H 0.8046 0.9650 -0.4347 0.060 Uiso 1 1 calc R . . C24 C 0.3313(3) 0.8543(3) -0.30308(14) 0.0229(6) Uani 1 1 d . . . H24A H 0.3159 0.7666 -0.3460 0.028 Uiso 1 1 calc R . . H24B H 0.2681 0.8231 -0.2625 0.028 Uiso 1 1 calc R . . C25 C 0.2739(3) 0.9740(3) -0.33331(16) 0.0348(7) Uani 1 1 d . . . H25A H 0.2794 1.0586 -0.2898 0.042 Uiso 1 1 calc R . . H25B H 0.3403 1.0111 -0.3715 0.042 Uiso 1 1 calc R . . C26 C 0.1125(3) 0.9158(4) -0.37102(18) 0.0432(8) Uani 1 1 d . . . H26A H 0.1063 0.8312 -0.4137 0.065 Uiso 1 1 calc R . . H26B H 0.0814 0.9949 -0.3911 0.065 Uiso 1 1 calc R . . H26C H 0.0456 0.8839 -0.3326 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.04477(7) 0.05457(7) 0.16759(4) 0.03143(18) Uani 1 1 d . . . Cl2 Cl 0.42366(7) 0.38702(7) 0.80932(4) 0.03195(18) Uani 1 1 d . . . O1 O 0.2232(2) 0.2705(2) 0.06676(12) 0.0341(5) Uani 1 1 d D . . O2 O 0.2647(2) 0.1722(2) 0.91177(12) 0.0321(5) Uani 1 1 d D . . H1A H 0.183(3) 0.205(3) 0.0898(16) 0.052(7) Uiso 1 1 d D . . H1B H 0.233(3) 0.240(3) 0.0202(11) 0.052(7) Uiso 1 1 d D . . H2C H 0.186(3) 0.118(3) 0.8846(17) 0.072(9) Uiso 1 1 d D . . H2D H 0.297(4) 0.231(3) 0.8840(17) 0.072(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0222(13) 0.0205(14) 0.0214(14) 0.0043(11) -0.0018(11) 0.0016(10) N1 0.0292(11) 0.0162(11) 0.0265(12) 0.0102(9) 0.0079(9) 0.0070(9) C2 0.0255(13) 0.0217(14) 0.0268(15) 0.0106(12) 0.0070(11) 0.0051(11) C3 0.0246(13) 0.0103(12) 0.0243(14) 0.0051(10) 0.0045(11) 0.0010(10) C4 0.0294(14) 0.0165(13) 0.0250(15) 0.0055(11) 0.0028(11) -0.0018(11) N2 0.0330(12) 0.0117(11) 0.0244(12) 0.0037(9) 0.0068(9) 0.0041(9) C5 0.0241(13) 0.0184(13) 0.0303(15) 0.0079(12) 0.0045(11) 0.0024(11) C6 0.0461(17) 0.0283(16) 0.0365(17) 0.0097(14) 0.0196(14) 0.0087(13) C7 0.0439(17) 0.049(2) 0.0356(17) 0.0151(15) 0.0189(14) 0.0170(15) C8 0.0258(13) 0.0156(13) 0.0236(14) 0.0026(11) 0.0033(11) 0.0000(10) C9 0.0358(16) 0.0349(17) 0.0420(18) 0.0154(14) 0.0022(13) 0.0124(13) C10 0.0381(18) 0.067(2) 0.046(2) 0.0155(18) -0.0052(15) 0.0180(17) C11 0.0242(13) 0.0142(13) 0.0189(13) 0.0007(10) -0.0005(11) 0.0010(10) C12 0.0264(13) 0.0254(15) 0.0254(15) 0.0071(12) 0.0035(11) 0.0100(11) C13 0.0307(14) 0.0212(14) 0.0241(14) 0.0099(11) 0.0014(12) 0.0098(11) C14 0.0242(13) 0.0142(13) 0.0191(13) 0.0036(10) 0.0004(10) 0.0011(10) C15 0.0269(13) 0.0231(14) 0.0260(15) 0.0070(12) 0.0036(11) 0.0074(11) C16 0.0280(14) 0.0189(14) 0.0280(15) 0.0086(11) 0.0014(12) 0.0075(11) C17 0.0202(12) 0.0181(13) 0.0224(14) 0.0059(11) -0.0013(10) 0.0030(10) N3 0.0302(11) 0.0136(11) 0.0244(12) 0.0062(9) 0.0052(9) 0.0068(9) C18 0.0253(13) 0.0203(14) 0.0228(14) 0.0047(11) 0.0066(11) 0.0054(11) C19 0.0253(13) 0.0107(12) 0.0217(13) 0.0045(10) 0.0041(11) -0.0003(10) C20 0.0286(13) 0.0151(13) 0.0234(14) 0.0035(11) 0.0034(11) -0.0012(10) N4 0.0316(12) 0.0129(11) 0.0236(12) 0.0026(9) 0.0057(9) 0.0036(9) C21 0.0294(14) 0.0182(13) 0.0248(14) 0.0070(11) 0.0054(11) -0.0018(11) C22 0.0433(16) 0.0243(15) 0.0316(16) 0.0041(13) 0.0117(13) 0.0039(13) C23 0.0460(17) 0.0405(19) 0.0331(17) 0.0118(14) 0.0123(14) 0.0067(14) C24 0.0253(13) 0.0168(13) 0.0231(14) 0.0026(11) 0.0040(11) -0.0004(10) C25 0.0379(16) 0.0279(16) 0.0384(17) 0.0102(13) -0.0030(13) 0.0067(13) C26 0.0353(16) 0.048(2) 0.051(2) 0.0174(16) -0.0013(14) 0.0145(14) Cl1 0.0362(4) 0.0174(3) 0.0418(4) 0.0099(3) 0.0028(3) 0.0063(3) Cl2 0.0364(4) 0.0165(3) 0.0425(4) 0.0093(3) 0.0012(3) 0.0041(3) O1 0.0409(12) 0.0252(11) 0.0358(13) 0.0063(10) 0.0112(10) 0.0060(9) O2 0.0369(11) 0.0227(11) 0.0360(12) 0.0087(9) 0.0054(9) 0.0040(9) _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 C1 N2 1.318(3) . ? C1 N1 1.320(3) . ? C1 C11 1.488(3) . ? N1 C2 1.466(3) . ? N1 H1 0.8800 . ? C2 C3 1.530(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.536(3) . ? C3 C5 1.536(3) . ? C3 C8 1.541(3) . ? C4 N2 1.466(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.518(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.393(3) . ? C11 C12 1.401(3) . ? C12 C13 1.378(3) . ? C12 H12 0.9500 . ? C13 C14 1.397(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(3) . ? C14 C17 1.485(3) . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N3 1.313(3) . ? C17 N4 1.324(3) . ? N3 C18 1.471(3) . ? N3 H3 0.8800 . ? C18 C19 1.536(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.536(3) . ? C19 C21 1.539(3) . ? C19 C24 1.548(3) . ? C20 N4 1.458(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N4 H4 0.8800 . ? C21 C22 1.521(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.529(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.519(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O1 H1A 0.827(17) . ? O1 H1B 0.836(17) . ? O2 H2C 0.840(17) . ? O2 H2D 0.824(18) . ? 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 N2 C1 N1 121.3(2) . . ? N2 C1 C11 120.2(2) . . ? N1 C1 C11 118.5(2) . . ? C1 N1 C2 123.4(2) . . ? C1 N1 H1 118.3 . . ? C2 N1 H1 118.3 . . ? N1 C2 C3 111.31(19) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 106.6(2) . . ? C2 C3 C5 109.04(19) . . ? C4 C3 C5 107.60(19) . . ? C2 C3 C8 109.81(19) . . ? C4 C3 C8 111.05(19) . . ? C5 C3 C8 112.6(2) . . ? N2 C4 C3 111.3(2) . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C1 N2 C4 121.4(2) . . ? C1 N2 H2 119.3 . . ? C4 N2 H2 119.3 . . ? C6 C5 C3 116.4(2) . . ? C6 C5 H5A 108.2 . . ? C3 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C3 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C7 C6 C5 111.8(2) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 115.8(2) . . ? C9 C8 H8A 108.3 . . ? C3 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C3 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 C10 111.8(2) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.5(2) . . ? C16 C11 C1 121.0(2) . . ? C12 C11 C1 119.5(2) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.6(2) . . ? C15 C14 C17 120.7(2) . . ? C13 C14 C17 119.7(2) . . ? C16 C15 C14 120.7(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 119.8(2) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? N3 C17 N4 120.8(2) . . ? N3 C17 C14 119.3(2) . . ? N4 C17 C14 119.9(2) . . ? C17 N3 C18 123.4(2) . . ? C17 N3 H3 118.3 . . ? C18 N3 H3 118.3 . . ? N3 C18 C19 111.18(19) . . ? N3 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N3 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 106.17(19) . . ? C18 C19 C21 109.2(2) . . ? C20 C19 C21 107.61(19) . . ? C18 C19 C24 110.18(19) . . ? C20 C19 C24 110.74(19) . . ? C21 C19 C24 112.7(2) . . ? N4 C20 C19 111.02(19) . . ? N4 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? N4 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C17 N4 C20 122.2(2) . . ? C17 N4 H4 118.9 . . ? C20 N4 H4 118.9 . . ? C22 C21 C19 116.4(2) . . ? C22 C21 H21A 108.2 . . ? C19 C21 H21A 108.2 . . ? C22 C21 H21B 108.2 . . ? C19 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C23 C22 C21 112.1(2) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C19 116.2(2) . . ? C25 C24 H24A 108.2 . . ? C19 C24 H24A 108.2 . . ? C25 C24 H24B 108.2 . . ? C19 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C24 112.1(2) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H1A O1 H1B 115(3) . . ? H2C O2 H2D 102(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.378 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.064 # Attachment 'B606265M_2-Ni.cif' data_e305a _database_code_depnum_ccdc_archive 'CCDC 611945' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, C4 N4 Ni' _chemical_formula_sum 'C30 H44 N8 Ni' _chemical_formula_weight 575.44 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2020(2) _cell_length_b 9.5615(2) _cell_length_c 10.9335(3) _cell_angle_alpha 68.098(2) _cell_angle_beta 84.4370(10) _cell_angle_gamma 84.4120(10) _cell_volume 790.07(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5509 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.84 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8818 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12610 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 29.91 _reflns_number_total 4524 _reflns_number_gt 3920 _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^)+(0.0473P)^2^+0.1186P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4524 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.63651(16) 0.30377(13) 0.86549(12) 0.0189(2) Uani 1 1 d . . . N1 N 0.66214(14) 0.15875(11) 0.93736(10) 0.0217(2) Uani 1 1 d . . . H1 H 0.6301 0.1263 1.0219 0.026 Uiso 1 1 calc R . . C2 C 0.74218(17) 0.04962(13) 0.88136(12) 0.0215(3) Uani 1 1 d . . . H2A H 0.6575 -0.0017 0.8582 0.026 Uiso 1 1 calc R . . H2B H 0.8092 -0.0281 0.9481 0.026 Uiso 1 1 calc R . . C3 C 0.85227(16) 0.12912(13) 0.75750(12) 0.0194(2) Uani 1 1 d . . . C4 C 0.74339(16) 0.25962(13) 0.66725(12) 0.0205(2) Uani 1 1 d . . . H4A H 0.8094 0.3188 0.5870 0.025 Uiso 1 1 calc R . . H4B H 0.6534 0.2185 0.6395 0.025 Uiso 1 1 calc R . . N2 N 0.67412(13) 0.35818(11) 0.73784(10) 0.0198(2) Uani 1 1 d . . . H2 H 0.6575 0.4557 0.6935 0.024 Uiso 1 1 calc R . . C5 C 0.90750(18) 0.01736(14) 0.68668(13) 0.0251(3) Uani 1 1 d . . . H5A H 0.8122 0.0034 0.6443 0.030 Uiso 1 1 calc R . . H5B H 0.9920 0.0638 0.6156 0.030 Uiso 1 1 calc R . . C6 C 0.9771(2) -0.13847(15) 0.77499(15) 0.0312(3) Uani 1 1 d . . . H6A H 1.0679 -0.1259 0.8227 0.037 Uiso 1 1 calc R . . H6B H 0.8903 -0.1902 0.8415 0.037 Uiso 1 1 calc R . . C7 C 1.0408(2) -0.23663(18) 0.69505(19) 0.0456(4) Uani 1 1 d . . . H7A H 0.9519 -0.2474 0.6461 0.068 Uiso 1 1 calc R . . H7B H 1.0799 -0.3366 0.7551 0.068 Uiso 1 1 calc R . . H7C H 1.1314 -0.1888 0.6328 0.068 Uiso 1 1 calc R . . C8 C 1.00038(17) 0.18824(14) 0.79648(13) 0.0240(3) Uani 1 1 d . . . H8A H 0.9605 0.2304 0.8649 0.029 Uiso 1 1 calc R . . H8B H 1.0785 0.1010 0.8375 0.029 Uiso 1 1 calc R . . C9 C 1.0946(2) 0.30829(18) 0.68561(16) 0.0355(3) Uani 1 1 d . . . H9A H 1.1299 0.2704 0.6138 0.043 Uiso 1 1 calc R . . H9B H 1.0210 0.4004 0.6490 0.043 Uiso 1 1 calc R . . C10 C 1.2446(2) 0.3482(2) 0.7346(2) 0.0443(4) Uani 1 1 d . . . H10A H 1.2101 0.3850 0.8063 0.066 Uiso 1 1 calc R . . H10B H 1.3003 0.4272 0.6618 0.066 Uiso 1 1 calc R . . H10C H 1.3200 0.2582 0.7673 0.066 Uiso 1 1 calc R . . C11 C 0.56513(16) 0.40605(13) 0.93393(12) 0.0190(2) Uani 1 1 d . . . C12 C 0.43515(17) 0.36192(14) 1.02849(13) 0.0236(3) Uani 1 1 d . . . H12 H 0.3910 0.2672 1.0478 0.028 Uiso 1 1 calc R . . C13 C 0.63067(17) 0.54487(14) 0.90500(13) 0.0234(3) Uani 1 1 d . . . H13 H 0.7195 0.5754 0.8404 0.028 Uiso 1 1 calc R . . Ni1 Ni 0.5000 0.0000 0.5000 0.01982(8) Uani 1 2 d S . . C14 C 0.44094(18) 0.20622(15) 0.44654(12) 0.0263(3) Uani 1 1 d . . . N3 N 0.40363(19) 0.33370(14) 0.41414(13) 0.0380(3) Uani 1 1 d . . . C15 C 0.57326(17) 0.02571(13) 0.32651(13) 0.0237(3) Uani 1 1 d . . . N4 N 0.61488(16) 0.04128(13) 0.21868(11) 0.0306(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0214(6) 0.0170(5) 0.0173(5) -0.0058(4) 0.0003(5) -0.0007(4) N1 0.0315(6) 0.0162(5) 0.0140(5) -0.0036(4) 0.0032(4) 0.0014(4) C2 0.0299(7) 0.0149(5) 0.0177(6) -0.0049(4) 0.0007(5) 0.0022(5) C3 0.0246(6) 0.0172(5) 0.0157(5) -0.0059(4) -0.0012(5) 0.0018(4) C4 0.0263(7) 0.0194(5) 0.0147(5) -0.0059(4) -0.0017(5) 0.0018(5) N2 0.0269(6) 0.0140(4) 0.0152(5) -0.0026(4) -0.0008(4) 0.0024(4) C5 0.0313(7) 0.0224(6) 0.0234(6) -0.0118(5) 0.0011(5) 0.0004(5) C6 0.0368(8) 0.0232(6) 0.0336(8) -0.0130(6) 0.0034(6) 0.0034(6) C7 0.0593(12) 0.0301(8) 0.0496(10) -0.0219(7) 0.0066(9) 0.0069(7) C8 0.0255(7) 0.0232(6) 0.0242(6) -0.0101(5) -0.0037(5) 0.0021(5) C9 0.0302(8) 0.0394(8) 0.0354(8) -0.0112(7) 0.0014(6) -0.0087(6) C10 0.0313(9) 0.0402(9) 0.0648(12) -0.0217(8) -0.0048(8) -0.0073(7) C11 0.0234(6) 0.0158(5) 0.0165(5) -0.0051(4) -0.0007(5) 0.0012(4) C12 0.0282(7) 0.0180(5) 0.0237(6) -0.0073(5) 0.0035(5) -0.0044(5) C13 0.0254(7) 0.0210(6) 0.0216(6) -0.0067(5) 0.0057(5) -0.0031(5) Ni1 0.02766(14) 0.01474(11) 0.01221(11) -0.00025(8) -0.00012(8) 0.00098(8) C14 0.0366(8) 0.0231(6) 0.0141(6) -0.0021(5) 0.0003(5) 0.0007(5) N3 0.0603(9) 0.0222(6) 0.0243(6) -0.0026(5) -0.0009(6) 0.0055(6) C15 0.0291(7) 0.0166(5) 0.0205(6) -0.0019(5) -0.0016(5) 0.0022(5) N4 0.0384(7) 0.0284(6) 0.0194(6) -0.0042(5) 0.0006(5) 0.0031(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 C1 N2 1.3115(16) . ? C1 N1 1.3216(15) . ? C1 C11 1.4861(16) . ? N1 C2 1.4696(15) . ? N1 H1 0.8800 . ? C2 C3 1.5348(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5373(17) . ? C3 C8 1.5462(18) . ? C3 C5 1.5497(16) . ? C4 N2 1.4696(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.5317(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.532(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.529(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.3900(18) . ? C11 C13 1.3941(17) . ? C12 C13 1.3885(17) 2_667 ? C12 H12 0.9500 . ? C13 C12 1.3885(17) 2_667 ? C13 H13 0.9500 . ? Ni1 C14 1.8637(13) 2_656 ? Ni1 C14 1.8637(13) . ? Ni1 C15 1.8653(14) . ? Ni1 C15 1.8653(14) 2_656 ? C14 N3 1.1537(18) . ? C15 N4 1.1530(18) . ? 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 N2 C1 N1 121.85(11) . . ? N2 C1 C11 120.15(10) . . ? N1 C1 C11 117.99(11) . . ? C1 N1 C2 122.45(10) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 110.76(10) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 105.81(10) . . ? C2 C3 C8 109.75(10) . . ? C4 C3 C8 111.33(10) . . ? C2 C3 C5 109.09(10) . . ? C4 C3 C5 108.84(10) . . ? C8 C3 C5 111.82(11) . . ? N2 C4 C3 109.94(10) . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C1 N2 C4 121.38(10) . . ? C1 N2 H2 119.3 . . ? C4 N2 H2 119.3 . . ? C6 C5 C3 115.53(11) . . ? C6 C5 H5A 108.4 . . ? C3 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C3 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 111.85(13) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 116.78(11) . . ? C9 C8 H8A 108.1 . . ? C3 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C3 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 111.63(14) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 120.10(11) . . ? C12 C11 C1 119.94(11) . . ? C13 C11 C1 119.95(11) . . ? C13 C12 C11 120.55(11) 2_667 . ? C13 C12 H12 119.7 2_667 . ? C11 C12 H12 119.7 . . ? C12 C13 C11 119.35(12) 2_667 . ? C12 C13 H13 120.3 2_667 . ? C11 C13 H13 120.3 . . ? C14 Ni1 C14 180.0 2_656 . ? C14 Ni1 C15 90.21(5) 2_656 . ? C14 Ni1 C15 89.80(5) . . ? C14 Ni1 C15 89.80(5) 2_656 2_656 ? C14 Ni1 C15 90.20(5) . 2_656 ? C15 Ni1 C15 180.0 . 2_656 ? N3 C14 Ni1 179.55(14) . . ? N4 C15 Ni1 178.41(13) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.91 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.450 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.057 # Attachment 'B606265M_2-Pd.cif' data_e321a _database_code_depnum_ccdc_archive 'CCDC 611946' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, C4 N4 Pd' _chemical_formula_sum 'C30 H44 N8 Pd' _chemical_formula_weight 623.13 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' N N 0.0061 0.0033 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2700(17) _cell_length_b 9.5086(19) _cell_length_c 10.937(2) _cell_angle_alpha 70.10(3) _cell_angle_beta 85.07(3) _cell_angle_gamma 85.64(3) _cell_volume 804.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 326 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9703 _exptl_absorpt_correction_T_max 0.9761 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9334 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.07 _reflns_number_total 4619 _reflns_number_gt 4428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0447P)^2^+0.2441P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4619 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 C1 C 0.6396(2) 0.30273(19) 0.86529(16) 0.0199(3) Uani 1 1 d . . . N1 N 0.6657(2) 0.16064(17) 0.93465(14) 0.0226(3) Uani 1 1 d . . . H1 H 0.6340 0.1299 1.0180 0.027 Uiso 1 1 calc R . . C2 C 0.7458(2) 0.05134(19) 0.87827(16) 0.0221(3) Uani 1 1 d . . . H2A H 0.6624 -0.0024 0.8544 0.026 Uiso 1 1 calc R . . H2B H 0.8120 -0.0232 0.9439 0.026 Uiso 1 1 calc R . . C3 C 0.8550(2) 0.12923(19) 0.75698(16) 0.0198(3) Uani 1 1 d . . . C4 C 0.7474(2) 0.25595(19) 0.66881(16) 0.0210(3) Uani 1 1 d . . . H4A H 0.8132 0.3144 0.5905 0.025 Uiso 1 1 calc R . . H4B H 0.6589 0.2126 0.6399 0.025 Uiso 1 1 calc R . . N2 N 0.67783(18) 0.35502(16) 0.73941(14) 0.0206(3) Uani 1 1 d . . . H2 H 0.6614 0.4512 0.6967 0.025 Uiso 1 1 calc R . . C5 C 0.9094(2) 0.0167(2) 0.68562(18) 0.0258(4) Uani 1 1 d . . . H5A H 0.8155 0.0017 0.6418 0.031 Uiso 1 1 calc R . . H5B H 0.9945 0.0620 0.6170 0.031 Uiso 1 1 calc R . . C6 C 0.9754(3) -0.1370(2) 0.7713(2) 0.0321(4) Uani 1 1 d . . . H6A H 1.0647 -0.1233 0.8204 0.038 Uiso 1 1 calc R . . H6B H 0.8880 -0.1877 0.8352 0.038 Uiso 1 1 calc R . . C7 C 1.0386(4) -0.2361(3) 0.6909(3) 0.0460(6) Uani 1 1 d . . . H7A H 0.9501 -0.2512 0.6432 0.069 Uiso 1 1 calc R . . H7B H 1.0793 -0.3332 0.7491 0.069 Uiso 1 1 calc R . . H7C H 1.1268 -0.1873 0.6289 0.069 Uiso 1 1 calc R . . C8 C 1.0018(2) 0.1914(2) 0.79708(18) 0.0240(3) Uani 1 1 d . . . H8A H 0.9622 0.2354 0.8648 0.029 Uiso 1 1 calc R . . H8B H 1.0784 0.1062 0.8376 0.029 Uiso 1 1 calc R . . C9 C 1.0963(3) 0.3089(3) 0.6892(2) 0.0365(5) Uani 1 1 d . . . H9A H 1.1312 0.2692 0.6179 0.044 Uiso 1 1 calc R . . H9B H 1.0244 0.3993 0.6533 0.044 Uiso 1 1 calc R . . C10 C 1.2453(3) 0.3518(3) 0.7392(3) 0.0466(6) Uani 1 1 d . . . H10A H 1.2114 0.3888 0.8113 0.070 Uiso 1 1 calc R . . H10B H 1.3003 0.4305 0.6686 0.070 Uiso 1 1 calc R . . H10C H 1.3200 0.2638 0.7698 0.070 Uiso 1 1 calc R . . C11 C 0.5669(2) 0.40568(19) 0.93395(16) 0.0199(3) Uani 1 1 d . . . C12 C 0.4405(2) 0.35886(19) 1.02905(18) 0.0235(3) Uani 1 1 d . . . H12 H 0.4001 0.2622 1.0486 0.028 Uiso 1 1 calc R . . C13 C 0.6266(2) 0.5472(2) 0.90454(17) 0.0233(3) Uani 1 1 d . . . H13 H 0.7126 0.5794 0.8395 0.028 Uiso 1 1 calc R . . Pd1 Pd 0.5000 0.0000 0.5000 0.01986(7) Uani 1 2 d S . . C14 C 0.4354(3) 0.2183(2) 0.44472(17) 0.0275(4) Uani 1 1 d . . . N3 N 0.3976(3) 0.3436(2) 0.41241(18) 0.0392(4) Uani 1 1 d . . . C15 C 0.5799(2) 0.0251(2) 0.31699(17) 0.0244(3) Uani 1 1 d . . . N4 N 0.6218(2) 0.0400(2) 0.21079(16) 0.0322(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0233(8) 0.0162(7) 0.0196(7) -0.0059(6) 0.0003(6) 0.0007(6) N1 0.0325(8) 0.0165(7) 0.0156(6) -0.0031(5) 0.0031(5) 0.0022(6) C2 0.0311(9) 0.0142(7) 0.0188(7) -0.0043(6) 0.0013(6) 0.0026(6) C3 0.0253(8) 0.0168(7) 0.0171(7) -0.0062(6) -0.0009(6) 0.0022(6) C4 0.0273(8) 0.0187(8) 0.0160(7) -0.0054(6) -0.0012(6) 0.0019(6) N2 0.0271(7) 0.0148(6) 0.0166(6) -0.0025(5) -0.0001(5) 0.0036(5) C5 0.0337(9) 0.0223(8) 0.0230(8) -0.0114(7) 0.0014(7) 0.0019(7) C6 0.0397(11) 0.0209(9) 0.0350(10) -0.0112(8) 0.0026(8) 0.0047(8) C7 0.0595(16) 0.0303(12) 0.0511(14) -0.0221(11) 0.0046(12) 0.0101(10) C8 0.0264(8) 0.0235(8) 0.0238(8) -0.0105(7) -0.0041(6) 0.0032(7) C9 0.0317(10) 0.0396(12) 0.0378(11) -0.0115(9) 0.0003(8) -0.0092(9) C10 0.0337(12) 0.0415(13) 0.0700(18) -0.0240(12) -0.0067(11) -0.0054(10) C11 0.0247(8) 0.0161(7) 0.0175(7) -0.0048(6) 0.0005(6) 0.0017(6) C12 0.0285(9) 0.0162(8) 0.0241(8) -0.0057(6) 0.0046(6) -0.0027(6) C13 0.0269(8) 0.0194(8) 0.0217(8) -0.0058(6) 0.0057(6) -0.0024(6) Pd1 0.02723(11) 0.01489(10) 0.01289(9) 0.00052(6) -0.00038(6) 0.00140(6) C14 0.0400(10) 0.0211(8) 0.0167(7) -0.0013(6) -0.0002(7) 0.0019(7) N3 0.0618(13) 0.0225(8) 0.0264(9) -0.0013(7) -0.0010(8) 0.0062(8) C15 0.0300(9) 0.0193(8) 0.0193(8) -0.0012(6) -0.0019(6) 0.0025(6) N4 0.0405(9) 0.0291(9) 0.0209(7) -0.0028(6) 0.0008(6) 0.0055(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.314(2) . ? C1 N1 1.317(2) . ? C1 C11 1.489(2) . ? N1 C2 1.470(2) . ? N1 H1 0.8800 . ? C2 C3 1.533(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.538(2) . ? C3 C5 1.547(2) . ? C3 C8 1.547(2) . ? C4 N2 1.467(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.531(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.531(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.526(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.526(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.392(2) . ? C11 C12 1.393(2) . ? C12 C13 1.389(2) 2_667 ? C12 H12 0.9500 . ? C13 C12 1.389(2) 2_667 ? C13 H13 0.9500 . ? Pd1 C15 1.9929(19) 2_656 ? Pd1 C15 1.9929(19) . ? Pd1 C14 1.998(2) 2_656 ? Pd1 C14 1.998(2) . ? C14 N3 1.148(3) . ? C15 N4 1.147(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 N2 C1 N1 121.97(16) . . ? N2 C1 C11 119.95(15) . . ? N1 C1 C11 118.08(15) . . ? C1 N1 C2 122.55(15) . . ? C1 N1 H1 118.7 . . ? C2 N1 H1 118.7 . . ? N1 C2 C3 110.87(14) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 105.75(14) . . ? C2 C3 C5 109.09(14) . . ? C4 C3 C5 108.88(14) . . ? C2 C3 C8 109.74(14) . . ? C4 C3 C8 111.38(14) . . ? C5 C3 C8 111.81(15) . . ? N2 C4 C3 110.29(13) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 121.18(14) . . ? C1 N2 H2 119.4 . . ? C4 N2 H2 119.4 . . ? C6 C5 C3 115.78(15) . . ? C6 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 112.00(19) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 116.85(16) . . ? C9 C8 H8A 108.1 . . ? C3 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C3 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 111.6(2) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 120.18(16) . . ? C13 C11 C1 120.11(15) . . ? C12 C11 C1 119.71(15) . . ? C13 C12 C11 120.33(16) 2_667 . ? C13 C12 H12 119.8 2_667 . ? C11 C12 H12 119.8 . . ? C12 C13 C11 119.49(15) 2_667 . ? C12 C13 H13 120.3 2_667 . ? C11 C13 H13 120.3 . . ? C15 Pd1 C15 180.0 2_656 . ? C15 Pd1 C14 89.41(8) 2_656 2_656 ? C15 Pd1 C14 90.59(8) . 2_656 ? C15 Pd1 C14 90.59(8) 2_656 . ? C15 Pd1 C14 89.41(8) . . ? C14 Pd1 C14 180.0 2_656 . ? N3 C14 Pd1 179.6(2) . . ? N4 C15 Pd1 178.26(18) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.228 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.085 # Attachment 'B606265M_2-Pt.cif' data_e307a _database_code_depnum_ccdc_archive 'CCDC 611947' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, C4 N4 Pt' _chemical_formula_sum 'C30 H44 N8 Pt' _chemical_formula_weight 711.82 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2909(2) _cell_length_b 9.4857(2) _cell_length_c 10.9177(2) _cell_angle_alpha 70.1910(10) _cell_angle_beta 84.9360(10) _cell_angle_gamma 85.7130(10) _cell_volume 803.74(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7301 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 29.97 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 4.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4062 _exptl_absorpt_correction_T_max 0.6676 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15935 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 29.50 _reflns_number_total 4520 _reflns_number_gt 4519 _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^)+(0.0265P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4520 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0427 _refine_ls_wR_factor_gt 0.0427 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 C1 C 0.64036(19) 0.30262(19) 0.86442(17) 0.0195(3) Uani 1 1 d . . . N1 N 0.66620(19) 0.16031(17) 0.93396(15) 0.0222(3) Uani 1 1 d . . . H1 H 0.6342 0.1295 1.0174 0.027 Uiso 1 1 calc R . . C2 C 0.7468(2) 0.05091(19) 0.87704(18) 0.0218(3) Uani 1 1 d . . . H2A H 0.6638 -0.0028 0.8527 0.026 Uiso 1 1 calc R . . H2B H 0.8124 -0.0239 0.9427 0.026 Uiso 1 1 calc R . . C3 C 0.8563(2) 0.12904(19) 0.75626(17) 0.0194(3) Uani 1 1 d . . . C4 C 0.7500(2) 0.2557(2) 0.66751(17) 0.0205(3) Uani 1 1 d . . . H4A H 0.8164 0.3145 0.5896 0.025 Uiso 1 1 calc R . . H4B H 0.6623 0.2122 0.6378 0.025 Uiso 1 1 calc R . . N2 N 0.67895(17) 0.35485(17) 0.73855(15) 0.0201(3) Uani 1 1 d . . . H2 H 0.6620 0.4511 0.6958 0.024 Uiso 1 1 calc R . . C5 C 0.9116(2) 0.0164(2) 0.68447(19) 0.0256(3) Uani 1 1 d . . . H5A H 0.8185 0.0013 0.6401 0.031 Uiso 1 1 calc R . . H5B H 0.9971 0.0619 0.6161 0.031 Uiso 1 1 calc R . . C6 C 0.9766(3) -0.1371(2) 0.7703(2) 0.0316(4) Uani 1 1 d . . . H6A H 0.8890 -0.1879 0.8342 0.038 Uiso 1 1 calc R . . H6B H 1.0654 -0.1234 0.8196 0.038 Uiso 1 1 calc R . . C7 C 1.0399(3) -0.2365(3) 0.6897(3) 0.0454(6) Uani 1 1 d . . . H7A H 0.9530 -0.2486 0.6393 0.068 Uiso 1 1 calc R . . H7B H 1.0765 -0.3350 0.7482 0.068 Uiso 1 1 calc R . . H7C H 1.1309 -0.1894 0.6299 0.068 Uiso 1 1 calc R . . C8 C 1.0023(2) 0.1918(2) 0.79712(19) 0.0238(3) Uani 1 1 d . . . H8A H 0.9621 0.2362 0.8647 0.029 Uiso 1 1 calc R . . H8B H 1.0784 0.1065 0.8381 0.029 Uiso 1 1 calc R . . C9 C 1.0972(3) 0.3092(3) 0.6891(2) 0.0359(4) Uani 1 1 d . . . H9A H 1.0257 0.3999 0.6533 0.043 Uiso 1 1 calc R . . H9B H 1.1319 0.2693 0.6176 0.043 Uiso 1 1 calc R . . C10 C 1.2461(3) 0.3522(3) 0.7390(3) 0.0459(6) Uani 1 1 d . . . H10A H 1.2122 0.3907 0.8105 0.069 Uiso 1 1 calc R . . H10B H 1.3020 0.4299 0.6679 0.069 Uiso 1 1 calc R . . H10C H 1.3196 0.2636 0.7706 0.069 Uiso 1 1 calc R . . C11 C 0.56719(19) 0.40563(19) 0.93343(17) 0.0196(3) Uani 1 1 d . . . C12 C 0.4409(2) 0.3581(2) 1.02874(19) 0.0234(3) Uani 1 1 d . . . H12 H 0.4006 0.2612 1.0480 0.028 Uiso 1 1 calc R . . C13 C 0.6266(2) 0.5478(2) 0.90410(18) 0.0233(3) Uani 1 1 d . . . H13 H 0.7124 0.5803 0.8389 0.028 Uiso 1 1 calc R . . Pt1 Pt 0.5000 0.0000 0.5000 0.01901(3) Uani 1 2 d S . . C14 C 0.4345(2) 0.2181(2) 0.44471(18) 0.0266(3) Uani 1 1 d . . . N3 N 0.3972(3) 0.3435(2) 0.4130(2) 0.0394(4) Uani 1 1 d . . . C15 C 0.5800(2) 0.0250(2) 0.31710(19) 0.0243(3) Uani 1 1 d . . . N4 N 0.6223(2) 0.0399(2) 0.21041(18) 0.0320(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0209(7) 0.0167(7) 0.0197(8) -0.0051(6) -0.0002(5) 0.0006(5) N1 0.0298(7) 0.0171(7) 0.0163(7) -0.0030(6) 0.0032(5) 0.0022(5) C2 0.0281(8) 0.0144(7) 0.0206(8) -0.0041(6) 0.0012(6) 0.0026(6) C3 0.0217(7) 0.0181(7) 0.0181(7) -0.0060(6) -0.0019(5) 0.0020(5) C4 0.0249(7) 0.0201(8) 0.0152(7) -0.0046(6) -0.0015(5) 0.0018(6) N2 0.0247(6) 0.0153(6) 0.0171(7) -0.0022(5) -0.0004(5) 0.0025(5) C5 0.0314(8) 0.0218(8) 0.0249(9) -0.0108(7) 0.0000(6) 0.0027(6) C6 0.0378(10) 0.0219(9) 0.0346(11) -0.0114(8) 0.0017(8) 0.0051(7) C7 0.0567(14) 0.0309(12) 0.0523(16) -0.0229(12) 0.0034(11) 0.0099(10) C8 0.0242(7) 0.0237(8) 0.0253(9) -0.0104(7) -0.0047(6) 0.0025(6) C9 0.0292(9) 0.0401(12) 0.0380(12) -0.0111(10) -0.0003(8) -0.0101(8) C10 0.0298(10) 0.0417(13) 0.0713(19) -0.0235(14) -0.0086(10) -0.0063(9) C11 0.0220(7) 0.0161(7) 0.0189(7) -0.0048(6) 0.0009(5) 0.0018(5) C12 0.0264(8) 0.0177(8) 0.0246(9) -0.0064(7) 0.0053(6) -0.0033(6) C13 0.0247(7) 0.0187(8) 0.0240(8) -0.0055(7) 0.0059(6) -0.0021(6) Pt1 0.02293(5) 0.01545(5) 0.01406(5) 0.00064(3) -0.00096(3) 0.00064(3) C14 0.0347(9) 0.0226(9) 0.0173(8) -0.0008(7) -0.0004(6) 0.0016(7) N3 0.0593(12) 0.0228(9) 0.0284(10) -0.0009(8) -0.0009(8) 0.0080(8) C15 0.0268(8) 0.0201(8) 0.0209(8) -0.0009(7) -0.0014(6) 0.0024(6) N4 0.0377(9) 0.0315(9) 0.0201(8) -0.0019(7) 0.0009(6) 0.0042(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.312(2) . ? C1 N1 1.317(2) . ? C1 C11 1.490(2) . ? N1 C2 1.473(2) . ? N1 H1 0.8800 . ? C2 C3 1.530(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.537(2) . ? C3 C5 1.548(2) . ? C3 C8 1.550(2) . ? C4 N2 1.471(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.529(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.532(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.525(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.527(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.394(2) . ? C11 C13 1.394(2) . ? C12 C13 1.394(2) 2_667 ? C12 H12 0.9500 . ? C13 C12 1.394(2) 2_667 ? C13 H13 0.9500 . ? Pt1 C15 1.9880(19) . ? Pt1 C15 1.9880(19) 2_656 ? Pt1 C14 1.996(2) . ? Pt1 C14 1.996(2) 2_656 ? C14 N3 1.146(3) . ? C15 N4 1.150(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 N2 C1 N1 122.02(15) . . ? N2 C1 C11 120.03(16) . . ? N1 C1 C11 117.94(16) . . ? C1 N1 C2 122.35(15) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 110.90(14) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 105.93(13) . . ? C2 C3 C5 109.11(15) . . ? C4 C3 C5 108.72(14) . . ? C2 C3 C8 109.74(14) . . ? C4 C3 C8 111.33(14) . . ? C5 C3 C8 111.82(14) . . ? N2 C4 C3 110.17(13) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 121.29(15) . . ? C1 N2 H2 119.4 . . ? C4 N2 H2 119.4 . . ? C6 C5 C3 115.62(16) . . ? C6 C5 H5A 108.4 . . ? C3 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C3 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 111.8(2) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 116.65(16) . . ? C9 C8 H8A 108.1 . . ? C3 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C3 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10 111.7(2) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 120.28(14) . . ? C12 C11 C1 119.64(15) . . ? C13 C11 C1 120.07(15) . . ? C11 C12 C13 120.26(16) . 2_667 ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 2_667 . ? C11 C13 C12 119.46(16) . 2_667 ? C11 C13 H13 120.3 . . ? C12 C13 H13 120.3 2_667 . ? C15 Pt1 C15 180.0 . 2_656 ? C15 Pt1 C14 89.41(8) . . ? C15 Pt1 C14 90.59(8) 2_656 . ? C15 Pt1 C14 90.59(8) . 2_656 ? C15 Pt1 C14 89.41(8) 2_656 2_656 ? C14 Pt1 C14 179.999(1) . 2_656 ? N3 C14 Pt1 179.8(2) . . ? N4 C15 Pt1 178.25(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.631 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.089