# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_FePc_TMP_0,5(Hexane)_150K_slow_cooling _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 Fe N8, C7 H17 N2, 0.5(C6 H14)' _chemical_formula_sum 'C42 H40 Fe N10' _chemical_formula_weight 740.69 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.694(5) _cell_length_b 17.544(5) _cell_length_c 17.590(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 113.591(5) _cell_angle_gamma 90.000(5) _cell_volume 6984(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8114 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.83 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_F_000 3104 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19592 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.322 _diffrn_reflns_theta_max 29.095 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.915 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.915 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 8567 _reflns_number_gt 6697 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8567 _refine_ls_number_parameters 510 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _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_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.76935(2) 0.09345(2) 0.16085(2) 0.01772(8) Uani 1 1 d . . . . . N1 N 0.70587(6) 0.04074(7) 0.07468(8) 0.0183(3) Uani 1 1 d . . . . . N2 N 0.82503(6) 0.04069(7) 0.12885(8) 0.0185(3) Uani 1 1 d . . . . . N3 N 0.83201(6) 0.15346(7) 0.23898(8) 0.0193(3) Uani 1 1 d . . . . . N4 N 0.71304(6) 0.15431(7) 0.18386(8) 0.0187(3) Uani 1 1 d . . . . . N6 N 0.76134(6) -0.05113(8) 0.02993(8) 0.0198(3) Uani 1 1 d . . . . . N7 N 0.91587(6) 0.10716(8) 0.21270(8) 0.0204(3) Uani 1 1 d . . . . . N8 N 0.77799(6) 0.22920(7) 0.30136(8) 0.0205(3) Uani 1 1 d . . . . . N5 N 0.62046(6) 0.10812(7) 0.07761(8) 0.0200(3) Uani 1 1 d . . . . . C1 C 0.64601(7) 0.05546(9) 0.04817(9) 0.0187(3) Uani 1 1 d . . . . . C2 C 0.61240(7) 0.00076(9) -0.01442(10) 0.0198(3) Uani 1 1 d . . . . . C3 C 0.65383(7) -0.05037(9) -0.02244(10) 0.0197(3) Uani 1 1 d . . . . . C4 C 0.71153(7) -0.02204(9) 0.03074(9) 0.0191(3) Uani 1 1 d . . . . . C5 C 0.81346(7) -0.01939(9) 0.07350(9) 0.0185(3) Uani 1 1 d . . . . . C6 C 0.86767(7) -0.04386(9) 0.06636(10) 0.0193(3) Uani 1 1 d . . . . . C7 C 0.91226(7) 0.00434(9) 0.11808(10) 0.0205(3) Uani 1 1 d . . . . . C8 C 0.88504(7) 0.05586(9) 0.15715(10) 0.0194(3) Uani 1 1 d . . . . . C9 C 0.89099(7) 0.15122(9) 0.25109(10) 0.0196(3) Uani 1 1 d . . . . . C10 C 0.92488(7) 0.20472(9) 0.31581(10) 0.0203(3) Uani 1 1 d . . . . . C11 C 0.88486(7) 0.23739(9) 0.34480(10) 0.0201(3) Uani 1 1 d . . . . . C12 C 0.82718(7) 0.20588(9) 0.29468(10) 0.0193(3) Uani 1 1 d . . . . . C13 C 0.72516(7) 0.20580(9) 0.24826(10) 0.0194(3) Uani 1 1 d . . . . . C14 C 0.67040(7) 0.23601(9) 0.24845(10) 0.0194(3) Uani 1 1 d . . . . . C15 C 0.62468(7) 0.20581(9) 0.17854(10) 0.0195(3) Uani 1 1 d . . . . . C16 C 0.65203(7) 0.15289(9) 0.14075(10) 0.0187(3) Uani 1 1 d . . . . . C17 C 0.55187(7) -0.00821(10) -0.06200(10) 0.0249(4) Uani 1 1 d . . . . . H17 H 0.5238 0.0264 -0.0571 0.030 Uiso 1 1 calc R U . . . C18 C 0.53410(8) -0.06930(10) -0.11662(11) 0.0276(4) Uani 1 1 d . . . . . H18 H 0.4933 -0.0759 -0.1504 0.033 Uiso 1 1 calc R U . . . C19 C 0.57515(8) -0.12160(10) -0.12310(11) 0.0272(4) Uani 1 1 d . . . . . H19 H 0.5616 -0.1635 -0.1602 0.033 Uiso 1 1 calc R U . . . C20 C 0.63518(8) -0.11298(9) -0.07620(10) 0.0236(4) Uani 1 1 d . . . . . H20 H 0.6629 -0.1485 -0.0804 0.028 Uiso 1 1 calc R U . . . C21 C 0.88014(8) -0.10137(9) 0.02110(10) 0.0235(4) Uani 1 1 d . . . . . H21 H 0.8501 -0.1350 -0.0131 0.028 Uiso 1 1 calc R U . . . C22 C 0.93794(8) -0.10786(10) 0.02764(11) 0.0279(4) Uani 1 1 d . . . . . H22 H 0.9476 -0.1464 -0.0029 0.033 Uiso 1 1 calc R U . . . C23 C 0.98231(8) -0.05848(11) 0.07854(11) 0.0307(4) Uani 1 1 d . . . . . H23 H 1.0213 -0.0637 0.0812 0.037 Uiso 1 1 calc R U . . . C24 C 0.97034(7) -0.00221(10) 0.12505(11) 0.0259(4) Uani 1 1 d . . . . . H24 H 1.0006 0.0306 0.1603 0.031 Uiso 1 1 calc R U . . . C25 C 0.98445(7) 0.22500(10) 0.34874(11) 0.0262(4) Uani 1 1 d . . . . . H25 H 1.0116 0.2020 0.3297 0.031 Uiso 1 1 calc R U . . . C26 C 1.00257(8) 0.28039(10) 0.41060(11) 0.0288(4) Uani 1 1 d . . . . . H26 H 1.0426 0.2967 0.4331 0.035 Uiso 1 1 calc R U . . . C27 C 0.96288(8) 0.31251(10) 0.44030(11) 0.0269(4) Uani 1 1 d . . . . . H27 H 0.9767 0.3500 0.4827 0.032 Uiso 1 1 calc R U . . . C28 C 0.90391(7) 0.29087(9) 0.40936(10) 0.0235(3) Uani 1 1 d . . . . . H28 H 0.8775 0.3115 0.4311 0.028 Uiso 1 1 calc R U . . . C29 C 0.65804(7) 0.28655(9) 0.30090(10) 0.0228(3) Uani 1 1 d . . . . . H29 H 0.6886 0.3054 0.3500 0.027 Uiso 1 1 calc R U . . . C30 C 0.59973(8) 0.30826(9) 0.27896(11) 0.0254(4) Uani 1 1 d . . . . . H30 H 0.5902 0.3424 0.3137 0.031 Uiso 1 1 calc R U . . . C31 C 0.55465(7) 0.28071(9) 0.20635(11) 0.0250(4) Uani 1 1 d . . . . . H31 H 0.5153 0.2983 0.1914 0.030 Uiso 1 1 calc R U . . . C32 C 0.56637(7) 0.22861(9) 0.15629(10) 0.0226(3) Uani 1 1 d . . . . . H32 H 0.5356 0.2089 0.1080 0.027 Uiso 1 1 calc R U . . . N21 N 0.78634(6) -0.00462(8) 0.27656(9) 0.0227(3) Uani 1 1 d . . . . . N22 N 0.67003(6) -0.04926(8) 0.27537(9) 0.0269(3) Uani 1 1 d . . . . . C201 C 0.75915(8) -0.07907(9) 0.24564(11) 0.0249(4) Uani 1 1 d . . . . . H20A H 0.7741 -0.1167 0.2913 0.030 Uiso 1 1 calc R U . . . H20B H 0.7712 -0.0963 0.2011 0.030 Uiso 1 1 calc R U . . . C202 C 0.69276(8) -0.07681(10) 0.21238(11) 0.0261(4) Uani 1 1 d . . . . . H20C H 0.6771 -0.1286 0.1938 0.031 Uiso 1 1 calc R U . . . H20D H 0.6777 -0.0428 0.1634 0.031 Uiso 1 1 calc R U . . . C203 C 0.76658(8) 0.02130(10) 0.34094(11) 0.0277(4) Uani 1 1 d . . . . . H20E H 0.7836 0.0722 0.3610 0.033 Uiso 1 1 calc R U . . . H20F H 0.7816 -0.0143 0.3885 0.033 Uiso 1 1 calc R U . . . C204 C 0.70048(8) 0.02583(10) 0.30955(12) 0.0289(4) Uani 1 1 d . . . . . H20G H 0.6859 0.0650 0.2654 0.035 Uiso 1 1 calc R U . . . H20H H 0.6896 0.0424 0.3554 0.035 Uiso 1 1 calc R U . . . C205 C 0.85110(8) -0.01489(11) 0.31559(12) 0.0336(4) Uani 1 1 d . . . . . H20I H 0.8701 0.0342 0.3368 0.050 Uiso 1 1 calc R U . . . H20J H 0.8650 -0.0344 0.2744 0.050 Uiso 1 1 calc R U . . . H20K H 0.8612 -0.0512 0.3615 0.050 Uiso 1 1 calc R U . . . C206 C 0.60484(9) -0.03578(13) 0.23290(15) 0.0452(5) Uani 1 1 d . . . . . H20L H 0.5970 0.0016 0.1883 0.068 Uiso 1 1 calc R U . . . H20M H 0.5900 -0.0163 0.2731 0.068 Uiso 1 1 calc R U . . . H20N H 0.5849 -0.0838 0.2095 0.068 Uiso 1 1 calc R U . . . C207 C 0.68064(9) -0.10625(11) 0.34234(13) 0.0359(5) Uani 1 1 d . . . . . H20O H 0.7232 -0.1156 0.3710 0.054 Uiso 1 1 calc R U . . . H20P H 0.6605 -0.1540 0.3182 0.054 Uiso 1 1 calc R U . . . H20Q H 0.6653 -0.0867 0.3820 0.054 Uiso 1 1 calc R U . . . C303 C 0.76648(7) 0.22310(12) -0.01636(13) 0.0335(5) Uani 0.330(3) 1 d D U P A 1 H30F H 0.7518 0.2314 -0.0770 0.040 Uiso 0.330(3) 1 calc R U P A 1 H30G H 0.7552 0.1706 -0.0081 0.040 Uiso 0.330(3) 1 calc R U P A 1 C301 C 0.86202(19) 0.1700(3) -0.0181(3) 0.0384(6) Uani 0.330(3) 1 d D U P A 1 H30A H 0.9050 0.1771 0.0077 0.058 Uiso 0.330(3) 1 calc R U P A 1 H30B H 0.8479 0.1783 -0.0780 0.058 Uiso 0.330(3) 1 calc R U P A 1 H30C H 0.8523 0.1180 -0.0076 0.058 Uiso 0.330(3) 1 calc R U P A 1 C302 C 0.83282(7) 0.2261(3) 0.0181(3) 0.0339(6) Uani 0.330(3) 1 d D U P A 1 H30D H 0.8448 0.2781 0.0093 0.041 Uiso 0.330(3) 1 calc R U P A 1 H30E H 0.8482 0.2174 0.0787 0.041 Uiso 0.330(3) 1 calc R U P A 1 C30C C 0.77298(5) 0.22850(11) 0.03509(10) 0.0335(5) Uani 0.670(3) 1 d D U P A 2 H30N H 0.7616 0.1740 0.0300 0.040 Uiso 0.670(3) 1 calc R U P A 2 H30O H 0.7727 0.2474 0.0880 0.040 Uiso 0.670(3) 1 calc R U P A 2 C30B C 0.83493(7) 0.23430(16) 0.03965(14) 0.0339(6) Uani 0.670(3) 1 d DG U P A 2 H30L H 0.8629 0.2198 0.0961 0.041 Uiso 0.670(3) 1 calc R U P A 2 H30M H 0.8430 0.2880 0.0304 0.041 Uiso 0.670(3) 1 calc R U P A 2 C30A C 0.8460(14) 0.18477(17) -0.02240(16) 0.0382(6) Uani 0.670(3) 1 d D U P A 2 H30H H 0.8887 0.1787 -0.0059 0.057 Uiso 0.670(3) 1 calc R U P A 2 H30I H 0.8286 0.2087 -0.0773 0.057 Uiso 0.670(3) 1 calc R U P A 2 H30K H 0.8279 0.1347 -0.0245 0.057 Uiso 0.670(3) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01312(12) 0.01997(13) 0.01844(13) -0.00352(9) 0.00461(9) -0.00052(9) N1 0.0178(7) 0.0188(7) 0.0179(6) -0.0017(5) 0.0069(5) -0.0004(5) N2 0.0150(6) 0.0215(7) 0.0177(7) -0.0016(5) 0.0051(5) -0.0011(5) N3 0.0176(7) 0.0192(7) 0.0196(7) -0.0014(5) 0.0058(5) 0.0000(5) N4 0.0169(7) 0.0189(7) 0.0189(7) -0.0025(5) 0.0055(5) -0.0004(5) N6 0.0176(7) 0.0219(7) 0.0188(7) -0.0022(5) 0.0059(5) -0.0005(5) N7 0.0159(7) 0.0219(7) 0.0214(7) -0.0019(5) 0.0055(5) -0.0007(5) N8 0.0176(7) 0.0202(7) 0.0215(7) -0.0033(6) 0.0055(5) 0.0001(5) N5 0.0156(7) 0.0223(7) 0.0201(7) -0.0012(5) 0.0051(5) 0.0005(5) C1 0.0165(8) 0.0214(8) 0.0161(7) 0.0005(6) 0.0043(6) -0.0019(6) C2 0.0182(8) 0.0224(8) 0.0183(8) -0.0011(6) 0.0067(6) -0.0023(6) C3 0.0179(8) 0.0232(8) 0.0176(8) -0.0003(6) 0.0068(6) -0.0030(6) C4 0.0190(8) 0.0214(8) 0.0163(7) -0.0019(6) 0.0064(6) -0.0023(6) C5 0.0196(8) 0.0183(8) 0.0167(7) 0.0005(6) 0.0064(6) 0.0021(6) C6 0.0175(8) 0.0203(8) 0.0176(8) 0.0014(6) 0.0044(6) 0.0026(6) C7 0.0183(8) 0.0221(8) 0.0191(8) 0.0016(6) 0.0052(6) 0.0026(6) C8 0.0154(8) 0.0226(8) 0.0191(8) 0.0002(6) 0.0057(6) 0.0002(6) C9 0.0145(7) 0.0217(8) 0.0194(8) 0.0001(6) 0.0034(6) -0.0007(6) C10 0.0174(8) 0.0201(8) 0.0195(8) -0.0008(6) 0.0034(6) -0.0003(6) C11 0.0169(8) 0.0195(8) 0.0186(8) 0.0013(6) 0.0016(6) 0.0013(6) C12 0.0189(8) 0.0175(8) 0.0193(8) -0.0011(6) 0.0054(6) -0.0006(6) C13 0.0181(8) 0.0178(8) 0.0212(8) -0.0015(6) 0.0067(6) -0.0012(6) C14 0.0182(8) 0.0166(8) 0.0235(8) 0.0000(6) 0.0086(6) -0.0013(6) C15 0.0192(8) 0.0176(8) 0.0226(8) -0.0004(6) 0.0093(6) -0.0009(6) C16 0.0150(7) 0.0206(8) 0.0197(8) 0.0003(6) 0.0060(6) 0.0009(6) C17 0.0182(8) 0.0286(9) 0.0251(9) -0.0013(7) 0.0057(7) -0.0010(7) C18 0.0195(8) 0.0298(9) 0.0281(9) -0.0028(7) 0.0039(7) -0.0058(7) C19 0.0258(9) 0.0270(9) 0.0266(9) -0.0073(7) 0.0081(7) -0.0088(7) C20 0.0225(9) 0.0240(8) 0.0248(9) -0.0037(7) 0.0101(7) -0.0038(7) C21 0.0225(8) 0.0256(9) 0.0195(8) -0.0019(7) 0.0053(7) 0.0033(7) C22 0.0260(9) 0.0302(10) 0.0248(9) -0.0061(7) 0.0074(7) 0.0077(7) C23 0.0173(8) 0.0378(10) 0.0353(10) -0.0045(8) 0.0086(7) 0.0049(7) C24 0.0175(8) 0.0279(9) 0.0295(9) -0.0044(7) 0.0066(7) -0.0001(7) C25 0.0173(8) 0.0308(9) 0.0270(9) -0.0032(7) 0.0051(7) -0.0010(7) C26 0.0174(8) 0.0298(9) 0.0309(10) -0.0036(8) 0.0010(7) -0.0032(7) C27 0.0258(9) 0.0227(9) 0.0224(9) -0.0046(7) -0.0006(7) -0.0007(7) C28 0.0208(8) 0.0232(8) 0.0211(8) -0.0011(7) 0.0027(7) 0.0037(7) C29 0.0215(8) 0.0221(8) 0.0260(9) -0.0031(7) 0.0107(7) -0.0041(6) C30 0.0272(9) 0.0223(9) 0.0321(9) -0.0056(7) 0.0175(8) -0.0012(7) C31 0.0168(8) 0.0270(9) 0.0329(9) 0.0018(7) 0.0118(7) 0.0022(7) C32 0.0184(8) 0.0256(9) 0.0228(8) -0.0001(7) 0.0070(7) -0.0011(6) N21 0.0170(7) 0.0263(7) 0.0230(7) -0.0022(6) 0.0064(6) -0.0008(6) N22 0.0204(7) 0.0297(8) 0.0319(8) 0.0032(6) 0.0121(6) 0.0004(6) C201 0.0250(9) 0.0213(8) 0.0291(9) -0.0015(7) 0.0114(7) 0.0011(7) C202 0.0241(9) 0.0274(9) 0.0256(9) -0.0034(7) 0.0086(7) -0.0047(7) C203 0.0327(10) 0.0282(9) 0.0219(9) -0.0034(7) 0.0106(7) -0.0052(7) C204 0.0355(11) 0.0237(9) 0.0353(10) -0.0020(8) 0.0224(9) 0.0009(7) C205 0.0194(9) 0.0420(11) 0.0338(10) 0.0126(9) 0.0049(8) 0.0014(8) C206 0.0206(10) 0.0536(13) 0.0614(15) 0.0118(11) 0.0165(10) 0.0045(9) C207 0.0411(12) 0.0320(10) 0.0399(11) 0.0090(9) 0.0217(10) -0.0017(8) C303 0.0423(11) 0.0290(12) 0.0294(12) -0.0024(11) 0.0144(11) -0.0107(9) C301 0.0378(16) 0.0354(15) 0.0390(12) -0.0017(11) 0.0124(12) -0.0024(12) C302 0.0416(10) 0.0333(11) 0.0221(14) -0.0017(10) 0.0078(9) -0.0069(9) C30C 0.0423(11) 0.0290(12) 0.0294(12) -0.0024(11) 0.0144(11) -0.0106(9) C30B 0.0416(10) 0.0333(11) 0.0221(14) -0.0017(10) 0.0078(9) -0.0069(9) C30A 0.0377(16) 0.0353(15) 0.0390(12) -0.0018(11) 0.0125(12) -0.0023(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 Fe1 N2 1.9193(13) . ? Fe1 N4 1.9204(13) . ? Fe1 N3 1.9207(13) . ? Fe1 N1 1.9256(13) . ? N1 C4 1.3845(19) . ? N1 C1 1.385(2) . ? N2 C5 1.385(2) . ? N2 C8 1.3870(19) . ? N3 C12 1.383(2) . ? N3 C9 1.386(2) . ? N4 C13 1.385(2) . ? N4 C16 1.390(2) . ? N6 C5 1.328(2) . ? N6 C4 1.337(2) . ? N7 C8 1.322(2) . ? N7 C9 1.328(2) . ? N8 C13 1.330(2) . ? N8 C12 1.331(2) . ? N5 C16 1.329(2) . ? N5 C1 1.335(2) . ? C1 C2 1.446(2) . ? C2 C17 1.399(2) . ? C2 C3 1.409(2) . ? C3 C20 1.402(2) . ? C3 C4 1.444(2) . ? C5 C6 1.458(2) . ? C6 C21 1.394(2) . ? C6 C7 1.398(2) . ? C7 C24 1.394(2) . ? C7 C8 1.453(2) . ? C9 C10 1.454(2) . ? C10 C25 1.394(2) . ? C10 C11 1.403(2) . ? C11 C28 1.401(2) . ? C11 C12 1.451(2) . ? C13 C14 1.454(2) . ? C14 C29 1.399(2) . ? C14 C15 1.399(2) . ? C15 C32 1.391(2) . ? C15 C16 1.456(2) . ? C17 C18 1.388(2) . ? C17 H17 0.9500 . ? C18 C19 1.405(3) . ? C18 H18 0.9500 . ? C19 C20 1.386(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.390(2) . ? C21 H21 0.9500 . ? C22 C23 1.403(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.392(2) . ? C25 H25 0.9500 . ? C26 C27 1.400(3) . ? C26 H26 0.9500 . ? C27 C28 1.388(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.386(2) . ? C29 H29 0.9500 . ? C30 C31 1.402(2) . ? C30 H30 0.9500 . ? C31 C32 1.378(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? N21 C201 1.470(2) . ? N21 C203 1.473(2) . ? N21 C205 1.477(2) . ? N22 C207 1.486(2) . ? N22 C206 1.498(2) . ? N22 C202 1.508(2) . ? N22 C204 1.517(2) . ? C201 C202 1.505(2) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.501(3) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 H20I 0.9800 . ? C205 H20J 0.9800 . ? C205 H20K 0.9800 . ? C206 H20L 0.9800 . ? C206 H20M 0.9800 . ? C206 H20N 0.9800 . ? C207 H20O 0.9800 . ? C207 H20P 0.9800 . ? C207 H20Q 0.9800 . ? C303 C303 1.5031(10) 7_655 ? C303 C302 1.5031(10) . ? C303 H30F 0.9900 . ? C303 H30G 0.9900 . ? C301 C302 1.5031(10) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 H30D 0.9900 . ? C302 H30E 0.9900 . ? C30C C30C 1.5031(10) 7_655 ? C30C C30B 1.5031 . ? C30C H30N 0.9900 . ? C30C H30O 0.9900 . ? C30B C30A 1.5031 . ? C30B H30L 0.9900 . ? C30B H30M 0.9900 . ? C30A H30H 0.9800 . ? C30A H30I 0.9800 . ? C30A H30K 0.9800 . ? 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 Fe1 N4 173.77(6) . . ? N2 Fe1 N3 90.43(6) . . ? N4 Fe1 N3 89.34(6) . . ? N2 Fe1 N1 89.46(6) . . ? N4 Fe1 N1 90.17(6) . . ? N3 Fe1 N1 174.46(5) . . ? C4 N1 C1 107.04(13) . . ? C4 N1 Fe1 126.10(11) . . ? C1 N1 Fe1 126.77(10) . . ? C5 N2 C8 106.77(13) . . ? C5 N2 Fe1 127.07(10) . . ? C8 N2 Fe1 126.16(11) . . ? C12 N3 C9 107.05(13) . . ? C12 N3 Fe1 126.73(11) . . ? C9 N3 Fe1 126.21(11) . . ? C13 N4 C16 106.88(12) . . ? C13 N4 Fe1 126.69(11) . . ? C16 N4 Fe1 126.39(10) . . ? C5 N6 C4 121.13(14) . . ? C8 N7 C9 121.68(14) . . ? C13 N8 C12 121.12(14) . . ? C16 N5 C1 121.55(14) . . ? N5 C1 N1 127.24(14) . . ? N5 C1 C2 122.58(14) . . ? N1 C1 C2 110.04(13) . . ? C17 C2 C3 120.86(15) . . ? C17 C2 C1 132.86(15) . . ? C3 C2 C1 106.28(14) . . ? C20 C3 C2 120.71(15) . . ? C20 C3 C4 132.79(15) . . ? C2 C3 C4 106.48(14) . . ? N6 C4 N1 127.48(14) . . ? N6 C4 C3 122.36(14) . . ? N1 C4 C3 109.97(14) . . ? N6 C5 N2 127.18(14) . . ? N6 C5 C6 122.53(14) . . ? N2 C5 C6 110.27(13) . . ? C21 C6 C7 120.87(15) . . ? C21 C6 C5 133.05(15) . . ? C7 C6 C5 106.08(14) . . ? C24 C7 C6 121.48(15) . . ? C24 C7 C8 131.60(15) . . ? C6 C7 C8 106.93(14) . . ? N7 C8 N2 127.75(14) . . ? N7 C8 C7 122.30(14) . . ? N2 C8 C7 109.93(13) . . ? N7 C9 N3 127.59(14) . . ? N7 C9 C10 122.38(14) . . ? N3 C9 C10 110.01(13) . . ? C25 C10 C11 121.61(15) . . ? C25 C10 C9 132.14(15) . . ? C11 C10 C9 106.25(14) . . ? C28 C11 C10 120.74(15) . . ? C28 C11 C12 132.60(15) . . ? C10 C11 C12 106.64(14) . . ? N8 C12 N3 127.41(14) . . ? N8 C12 C11 122.53(14) . . ? N3 C12 C11 109.98(14) . . ? N8 C13 N4 127.32(14) . . ? N8 C13 C14 122.55(14) . . ? N4 C13 C14 110.06(13) . . ? C29 C14 C15 120.51(15) . . ? C29 C14 C13 132.96(15) . . ? C15 C14 C13 106.51(14) . . ? C32 C15 C14 121.25(15) . . ? C32 C15 C16 132.22(15) . . ? C14 C15 C16 106.52(14) . . ? N5 C16 N4 127.75(14) . . ? N5 C16 C15 122.32(14) . . ? N4 C16 C15 109.82(13) . . ? C18 C17 C2 117.83(16) . . ? C18 C17 H17 121.1 . . ? C2 C17 H17 121.1 . . ? C17 C18 C19 121.45(16) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 120.98(16) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C3 118.12(16) . . ? C19 C20 H20 120.9 . . ? C3 C20 H20 120.9 . . ? C22 C21 C6 117.79(16) . . ? C22 C21 H21 121.1 . . ? C6 C21 H21 121.1 . . ? C21 C22 C23 121.08(16) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 121.30(16) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C7 117.46(16) . . ? C23 C24 H24 121.3 . . ? C7 C24 H24 121.3 . . ? C26 C25 C10 117.29(16) . . ? C26 C25 H25 121.4 . . ? C10 C25 H25 121.4 . . ? C25 C26 C27 121.22(16) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.66(16) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C11 117.39(16) . . ? C27 C28 H28 121.3 . . ? C11 C28 H28 121.3 . . ? C30 C29 C14 117.85(16) . . ? C30 C29 H29 121.1 . . ? C14 C29 H29 121.1 . . ? C29 C30 C31 121.08(15) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 121.17(16) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C15 117.99(16) . . ? C31 C32 H32 121.0 . . ? C15 C32 H32 121.0 . . ? C201 N21 C203 108.43(13) . . ? C201 N21 C205 108.23(14) . . ? C203 N21 C205 108.08(14) . . ? C207 N22 C206 108.35(14) . . ? C207 N22 C202 111.55(14) . . ? C206 N22 C202 109.03(15) . . ? C207 N22 C204 111.59(14) . . ? C206 N22 C204 108.90(14) . . ? C202 N22 C204 107.36(13) . . ? N21 C201 C202 112.69(14) . . ? N21 C201 H20A 109.1 . . ? C202 C201 H20A 109.1 . . ? N21 C201 H20B 109.1 . . ? C202 C201 H20B 109.1 . . ? H20A C201 H20B 107.8 . . ? C201 C202 N22 113.01(14) . . ? C201 C202 H20C 109.0 . . ? N22 C202 H20C 109.0 . . ? C201 C202 H20D 109.0 . . ? N22 C202 H20D 109.0 . . ? H20C C202 H20D 107.8 . . ? N21 C203 C204 112.30(14) . . ? N21 C203 H20E 109.1 . . ? C204 C203 H20E 109.1 . . ? N21 C203 H20F 109.1 . . ? C204 C203 H20F 109.1 . . ? H20E C203 H20F 107.9 . . ? C203 C204 N22 113.17(14) . . ? C203 C204 H20G 108.9 . . ? N22 C204 H20G 108.9 . . ? C203 C204 H20H 108.9 . . ? N22 C204 H20H 108.9 . . ? H20G C204 H20H 107.8 . . ? N21 C205 H20I 109.5 . . ? N21 C205 H20J 109.5 . . ? H20I C205 H20J 109.5 . . ? N21 C205 H20K 109.5 . . ? H20I C205 H20K 109.5 . . ? H20J C205 H20K 109.5 . . ? N22 C206 H20L 109.5 . . ? N22 C206 H20M 109.5 . . ? H20L C206 H20M 109.5 . . ? N22 C206 H20N 109.5 . . ? H20L C206 H20N 109.5 . . ? H20M C206 H20N 109.5 . . ? N22 C207 H20O 109.5 . . ? N22 C207 H20P 109.5 . . ? H20O C207 H20P 109.5 . . ? N22 C207 H20Q 109.5 . . ? H20O C207 H20Q 109.5 . . ? H20P C207 H20Q 109.5 . . ? C303 C303 C302 119.6(2) 7_655 . ? C303 C303 H30F 107.4 7_655 . ? C302 C303 H30F 107.4 . . ? C303 C303 H30G 107.4 7_655 . ? C302 C303 H30G 107.4 . . ? H30F C303 H30G 107.0 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C301 C302 C303 115.9(3) . . ? C301 C302 H30D 108.3 . . ? C303 C302 H30D 108.3 . . ? C301 C302 H30E 108.3 . . ? C303 C302 H30E 108.3 . . ? H30D C302 H30E 107.4 . . ? C30C C30C C30B 115.3(2) 7_655 . ? C30C C30C H30N 108.4 7_655 . ? C30B C30C H30N 108.4 . . ? C30C C30C H30O 108.4 7_655 . ? C30B C30C H30O 108.4 . . ? H30N C30C H30O 107.5 . . ? C30C C30B C30A 113.5(2) . . ? C30C C30B H30L 108.9 . . ? C30A C30B H30L 108.9 . . ? C30C C30B H30M 108.9 . . ? C30A C30B H30M 108.9 . . ? H30L C30B H30M 107.7 . . ? C30B C30A H30H 109.5 . . ? C30B C30A H30I 109.5 . . ? H30H C30A H30I 109.5 . . ? C30B C30A H30K 109.5 . . ? H30H C30A H30K 109.5 . . ? H30I C30A H30K 109.5 . . ? _refine_diff_density_max 0.447 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 931422' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_FePc_TMP_0,5(Hexane)_105K_slow_cooling _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 Fe N8, C7 H17 N2, 0.5(C6 H14)' _chemical_formula_sum 'C42 H40 Fe N10' _chemical_formula_weight 740.69 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.6749(4) _cell_length_b 17.5133(3) _cell_length_c 17.5399(3) _cell_angle_alpha 90 _cell_angle_beta 113.7680(10) _cell_angle_gamma 90 _cell_volume 6936.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 8820 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.42 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_F_000 3104 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32287 _diffrn_reflns_av_unetI/netI 0.0135 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.471 _diffrn_reflns_theta_max 29.424 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.927 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 8888 _reflns_number_gt 8053 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+9.1804P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8888 _refine_ls_number_parameters 487 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _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_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.76954(2) 0.09184(2) 0.16211(2) 0.01011(5) Uani 1 1 d . . . . . N1 N 0.70581(4) 0.03908(6) 0.07554(6) 0.01153(18) Uani 1 1 d . . . . . N2 N 0.82518(4) 0.03919(6) 0.12953(6) 0.01163(18) Uani 1 1 d . . . . . N3 N 0.83252(4) 0.15217(6) 0.24027(6) 0.01181(19) Uani 1 1 d . . . . . N4 N 0.71314(4) 0.15320(6) 0.18478(6) 0.01123(18) Uani 1 1 d . . . . . N6 N 0.76111(4) -0.05275(6) 0.03017(6) 0.01247(19) Uani 1 1 d . . . . . N7 N 0.91619(4) 0.10613(6) 0.21340(6) 0.01295(19) Uani 1 1 d . . . . . N8 N 0.77851(5) 0.22861(6) 0.30254(6) 0.01277(19) Uani 1 1 d . . . . . N5 N 0.62033(4) 0.10716(6) 0.07800(6) 0.01242(19) Uani 1 1 d . . . . . C1 C 0.64577(5) 0.05426(7) 0.04863(7) 0.0120(2) Uani 1 1 d . . . . . C2 C 0.61191(5) -0.00051(7) -0.01464(7) 0.0126(2) Uani 1 1 d . . . . . C3 C 0.65321(5) -0.05176(7) -0.02268(7) 0.0126(2) Uani 1 1 d . . . . . C4 C 0.71128(5) -0.02378(7) 0.03109(7) 0.0119(2) Uani 1 1 d . . . . . C5 C 0.81324(5) -0.02105(7) 0.07373(7) 0.0116(2) Uani 1 1 d . . . . . C6 C 0.86751(5) -0.04512(7) 0.06609(7) 0.0122(2) Uani 1 1 d . . . . . C7 C 0.91224(5) 0.00364(7) 0.11762(7) 0.0127(2) Uani 1 1 d . . . . . C8 C 0.88518(5) 0.05475(7) 0.15744(7) 0.0121(2) Uani 1 1 d . . . . . C9 C 0.89141(5) 0.15025(7) 0.25201(7) 0.0121(2) Uani 1 1 d . . . . . C10 C 0.92542(5) 0.20421(7) 0.31644(7) 0.0129(2) Uani 1 1 d . . . . . C11 C 0.88553(5) 0.23723(7) 0.34565(7) 0.0127(2) Uani 1 1 d . . . . . C12 C 0.82768(5) 0.20509(7) 0.29596(7) 0.0122(2) Uani 1 1 d . . . . . C13 C 0.72560(5) 0.20493(7) 0.24971(7) 0.0120(2) Uani 1 1 d . . . . . C14 C 0.67068(5) 0.23559(7) 0.24949(7) 0.0123(2) Uani 1 1 d . . . . . C15 C 0.62484(5) 0.20524(7) 0.17894(7) 0.0124(2) Uani 1 1 d . . . . . C16 C 0.65188(5) 0.15204(6) 0.14121(7) 0.0117(2) Uani 1 1 d . . . . . C17 C 0.55114(5) -0.00877(7) -0.06287(8) 0.0154(2) Uani 1 1 d . . . . . H17 H 0.5232 0.0261 -0.0580 0.019 Uiso 1 1 calc R U . . . C18 C 0.53315(6) -0.06987(8) -0.11816(8) 0.0180(2) Uani 1 1 d . . . . . H18 H 0.4923 -0.0762 -0.1524 0.022 Uiso 1 1 calc R U . . . C19 C 0.57427(6) -0.12261(7) -0.12449(8) 0.0177(2) Uani 1 1 d . . . . . H19 H 0.5605 -0.1645 -0.1619 0.021 Uiso 1 1 calc R U . . . C20 C 0.63451(6) -0.11439(7) -0.07699(8) 0.0150(2) Uani 1 1 d . . . . . H20 H 0.6622 -0.1500 -0.0811 0.018 Uiso 1 1 calc R U . . . C21 C 0.87990(6) -0.10273(7) 0.02036(8) 0.0149(2) Uani 1 1 d . . . . . H21 H 0.8498 -0.1366 -0.0138 0.018 Uiso 1 1 calc R U . . . C22 C 0.93783(6) -0.10881(8) 0.02667(8) 0.0183(2) Uani 1 1 d . . . . . H22 H 0.9474 -0.1473 -0.0041 0.022 Uiso 1 1 calc R U . . . C23 C 0.98234(6) -0.05908(8) 0.07770(9) 0.0200(3) Uani 1 1 d . . . . . H23 H 1.0214 -0.0642 0.0802 0.024 Uiso 1 1 calc R U . . . C24 C 0.97053(5) -0.00262(7) 0.12453(8) 0.0167(2) Uani 1 1 d . . . . . H24 H 1.0008 0.0304 0.1598 0.020 Uiso 1 1 calc R U . . . C25 C 0.98529(5) 0.22473(7) 0.34917(8) 0.0164(2) Uani 1 1 d . . . . . H25 H 1.0123 0.2014 0.3302 0.020 Uiso 1 1 calc R U . . . C26 C 1.00358(6) 0.28080(7) 0.41076(8) 0.0184(2) Uani 1 1 d . . . . . H26 H 1.0437 0.2972 0.4330 0.022 Uiso 1 1 calc R U . . . C27 C 0.96383(6) 0.31359(7) 0.44058(8) 0.0171(2) Uani 1 1 d . . . . . H27 H 0.9777 0.3516 0.4827 0.020 Uiso 1 1 calc R U . . . C28 C 0.90471(5) 0.29152(7) 0.40972(8) 0.0148(2) Uani 1 1 d . . . . . H28 H 0.8783 0.3125 0.4313 0.018 Uiso 1 1 calc R U . . . C29 C 0.65851(5) 0.28636(7) 0.30223(8) 0.0144(2) Uani 1 1 d . . . . . H29 H 0.6892 0.3050 0.3517 0.017 Uiso 1 1 calc R U . . . C30 C 0.59994(6) 0.30858(7) 0.27965(8) 0.0164(2) Uani 1 1 d . . . . . H30 H 0.5905 0.3430 0.3143 0.020 Uiso 1 1 calc R U . . . C31 C 0.55454(5) 0.28101(7) 0.20649(8) 0.0161(2) Uani 1 1 d . . . . . H31 H 0.5152 0.2987 0.1914 0.019 Uiso 1 1 calc R U . . . C32 C 0.56620(5) 0.22841(7) 0.15597(8) 0.0145(2) Uani 1 1 d . . . . . H32 H 0.5353 0.2088 0.1073 0.017 Uiso 1 1 calc R U . . . N21 N 0.21311(5) 0.00598(6) -0.27753(6) 0.01353(19) Uani 1 1 d . . . . . N22 N 0.32918(5) 0.04975(6) -0.27799(7) 0.0167(2) Uani 1 1 d . . . . . C201 C 0.24072(6) 0.08039(7) -0.24636(8) 0.0155(2) Uani 1 1 d . . . . . H20A H 0.2293 0.0974 -0.2011 0.019 Uiso 1 1 calc R U . . . H20B H 0.2254 0.1184 -0.2919 0.019 Uiso 1 1 calc R U . . . C202 C 0.30738(6) 0.07793(7) -0.21400(8) 0.0166(2) Uani 1 1 d . . . . . H20C H 0.3229 0.0441 -0.1647 0.020 Uiso 1 1 calc R U . . . H20D H 0.3233 0.1298 -0.1959 0.020 Uiso 1 1 calc R U . . . C203 C 0.23214(6) -0.02047(7) -0.34247(8) 0.0166(2) Uani 1 1 d . . . . . H20E H 0.2168 0.0150 -0.3904 0.020 Uiso 1 1 calc R U . . . H20F H 0.2149 -0.0715 -0.3621 0.020 Uiso 1 1 calc R U . . . C204 C 0.29870(6) -0.02524(7) -0.31172(8) 0.0180(2) Uani 1 1 d . . . . . H20G H 0.3090 -0.0419 -0.3582 0.022 Uiso 1 1 calc R U . . . H20H H 0.3136 -0.0644 -0.2674 0.022 Uiso 1 1 calc R U . . . C205 C 0.14821(6) 0.01694(8) -0.31621(9) 0.0208(3) Uani 1 1 d . . . . . H20I H 0.1288 -0.0320 -0.3376 0.031 Uiso 1 1 calc R U . . . H20J H 0.1380 0.0535 -0.3622 0.031 Uiso 1 1 calc R U . . . H20K H 0.1347 0.0366 -0.2745 0.031 Uiso 1 1 calc R U . . . C206 C 0.39471(6) 0.03628(10) -0.23603(11) 0.0290(3) Uani 1 1 d . . . . . H20L H 0.4030 -0.0011 -0.1912 0.043 Uiso 1 1 calc R U . . . H20M H 0.4148 0.0844 -0.2127 0.043 Uiso 1 1 calc R U . . . H20N H 0.4091 0.0168 -0.2768 0.043 Uiso 1 1 calc R U . . . C207 C 0.31799(7) 0.10696(8) -0.34599(9) 0.0228(3) Uani 1 1 d . . . . . H20O H 0.2753 0.1162 -0.3745 0.034 Uiso 1 1 calc R U . . . H20P H 0.3331 0.0873 -0.3859 0.034 Uiso 1 1 calc R U . . . H20Q H 0.3382 0.1549 -0.3220 0.034 Uiso 1 1 calc R U . . . C1S C 0.84751(7) 0.81623(9) 0.47687(10) 0.0269(3) Uani 1 1 d D . . . . H1S1 H 0.8884 0.8089 0.4828 0.040 Uiso 1 1 calc R U . A 1 H1S2 H 0.8415 0.8698 0.4876 0.040 Uiso 1 1 calc R U . A 1 H1S3 H 0.8202 0.8026 0.4202 0.040 Uiso 1 1 calc R U . A 1 C3S C 0.77311(6) 0.77206(8) 0.53604(9) 0.0161(5) Uani 0.870(7) 1 d D . P B 1 H3S1 H 0.7734 0.7525 0.5892 0.019 Uiso 0.870(7) 1 calc R U P B 1 H3S2 H 0.7615 0.8265 0.5313 0.019 Uiso 0.870(7) 1 calc R U P B 1 C3A C 0.7651(5) 0.7762(8) 0.4853(11) 0.043(5) Uiso 0.130(7) 1 d D . P B 2 H3A1 H 0.7552 0.7670 0.4255 0.052 Uiso 0.130(7) 1 calc R U P B 2 H3A2 H 0.7530 0.8289 0.4917 0.052 Uiso 0.130(7) 1 calc R U P B 2 C2S C 0.83582(6) 0.76589(8) 0.53868(9) 0.0231(3) Uani 1 1 d D . . . . H2S1 H 0.8502 0.7877 0.5955 0.028 Uiso 1 1 calc R U . B 1 H2S2 H 0.8498 0.7127 0.5402 0.028 Uiso 1 1 calc R U . B 1 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 Fe1 0.00886(9) 0.01139(9) 0.00988(9) -0.00205(6) 0.00355(7) -0.00030(5) N1 0.0118(5) 0.0128(4) 0.0104(4) -0.0010(3) 0.0049(4) -0.0001(3) N2 0.0108(4) 0.0129(4) 0.0107(4) -0.0010(3) 0.0038(4) -0.0003(3) N3 0.0114(4) 0.0119(4) 0.0120(5) -0.0012(3) 0.0046(4) 0.0003(3) N4 0.0107(4) 0.0118(4) 0.0106(4) -0.0010(3) 0.0038(4) -0.0006(3) N6 0.0126(5) 0.0138(4) 0.0112(5) -0.0015(3) 0.0049(4) -0.0004(4) N7 0.0114(4) 0.0142(4) 0.0130(5) -0.0011(4) 0.0047(4) -0.0002(4) N8 0.0126(5) 0.0129(4) 0.0123(5) -0.0017(4) 0.0045(4) -0.0004(4) N5 0.0117(4) 0.0136(4) 0.0118(5) -0.0005(4) 0.0045(4) -0.0004(4) C1 0.0117(5) 0.0136(5) 0.0100(5) -0.0003(4) 0.0038(4) -0.0013(4) C2 0.0134(5) 0.0137(5) 0.0110(5) -0.0007(4) 0.0052(4) -0.0019(4) C3 0.0132(5) 0.0149(5) 0.0104(5) -0.0001(4) 0.0055(4) -0.0019(4) C4 0.0133(5) 0.0131(5) 0.0095(5) -0.0012(4) 0.0047(4) -0.0015(4) C5 0.0133(5) 0.0127(5) 0.0094(5) 0.0002(4) 0.0051(4) 0.0018(4) C6 0.0116(5) 0.0143(5) 0.0100(5) 0.0011(4) 0.0035(4) 0.0021(4) C7 0.0129(5) 0.0133(5) 0.0116(5) 0.0004(4) 0.0047(4) 0.0016(4) C8 0.0109(5) 0.0139(5) 0.0117(5) 0.0006(4) 0.0047(4) 0.0011(4) C9 0.0109(5) 0.0128(5) 0.0114(5) -0.0003(4) 0.0032(4) -0.0007(4) C10 0.0127(5) 0.0126(5) 0.0118(5) -0.0004(4) 0.0032(4) 0.0001(4) C11 0.0118(5) 0.0129(5) 0.0112(5) 0.0007(4) 0.0024(4) 0.0008(4) C12 0.0127(5) 0.0118(5) 0.0107(5) -0.0007(4) 0.0035(4) -0.0004(4) C13 0.0133(5) 0.0115(5) 0.0123(5) -0.0006(4) 0.0063(4) -0.0001(4) C14 0.0122(5) 0.0117(5) 0.0143(5) 0.0000(4) 0.0066(4) -0.0007(4) C15 0.0142(5) 0.0118(5) 0.0128(5) -0.0003(4) 0.0069(4) -0.0008(4) C16 0.0113(5) 0.0122(5) 0.0124(5) 0.0009(4) 0.0054(4) 0.0008(4) C17 0.0128(5) 0.0168(5) 0.0157(6) -0.0005(4) 0.0047(5) -0.0009(4) C18 0.0135(6) 0.0201(6) 0.0171(6) -0.0021(5) 0.0028(5) -0.0040(5) C19 0.0178(6) 0.0177(6) 0.0164(6) -0.0053(4) 0.0057(5) -0.0059(5) C20 0.0158(6) 0.0153(5) 0.0148(6) -0.0019(4) 0.0072(5) -0.0019(4) C21 0.0149(5) 0.0161(5) 0.0122(5) -0.0015(4) 0.0038(4) 0.0024(4) C22 0.0166(6) 0.0209(6) 0.0164(6) -0.0041(5) 0.0057(5) 0.0048(5) C23 0.0127(6) 0.0252(6) 0.0218(6) -0.0040(5) 0.0066(5) 0.0031(5) C24 0.0123(5) 0.0194(6) 0.0180(6) -0.0028(5) 0.0057(5) -0.0004(4) C25 0.0124(5) 0.0187(6) 0.0163(6) -0.0019(4) 0.0040(5) -0.0005(4) C26 0.0125(5) 0.0196(6) 0.0183(6) -0.0027(5) 0.0011(5) -0.0024(4) C27 0.0173(6) 0.0150(5) 0.0133(6) -0.0025(4) 0.0003(5) -0.0003(4) C28 0.0153(6) 0.0141(5) 0.0126(5) -0.0006(4) 0.0030(4) 0.0023(4) C29 0.0152(6) 0.0140(5) 0.0153(6) -0.0024(4) 0.0077(5) -0.0032(4) C30 0.0176(6) 0.0155(5) 0.0200(6) -0.0036(4) 0.0117(5) -0.0009(4) C31 0.0128(5) 0.0172(6) 0.0206(6) 0.0002(5) 0.0092(5) 0.0013(4) C32 0.0126(5) 0.0164(5) 0.0145(5) -0.0003(4) 0.0054(4) -0.0006(4) N21 0.0119(5) 0.0159(5) 0.0128(5) -0.0007(4) 0.0050(4) -0.0002(4) N22 0.0141(5) 0.0180(5) 0.0198(5) 0.0034(4) 0.0088(4) 0.0003(4) C201 0.0173(6) 0.0133(5) 0.0172(6) -0.0009(4) 0.0083(5) 0.0010(4) C202 0.0175(6) 0.0177(6) 0.0142(6) -0.0018(4) 0.0060(5) -0.0034(4) C203 0.0208(6) 0.0173(6) 0.0123(5) -0.0023(4) 0.0073(5) -0.0028(5) C204 0.0233(6) 0.0152(6) 0.0208(6) -0.0002(5) 0.0145(5) 0.0014(5) C205 0.0122(6) 0.0263(6) 0.0214(6) 0.0090(5) 0.0042(5) 0.0016(5) C206 0.0135(6) 0.0362(8) 0.0374(8) 0.0092(7) 0.0104(6) 0.0027(6) C207 0.0266(7) 0.0212(6) 0.0244(7) 0.0076(5) 0.0143(6) -0.0010(5) C1S 0.0301(7) 0.0265(7) 0.0254(7) 0.0036(6) 0.0124(6) 0.0059(6) C3S 0.0192(7) 0.0153(7) 0.0137(8) -0.0007(5) 0.0066(6) 0.0015(5) C2S 0.0226(7) 0.0207(6) 0.0248(7) -0.0021(5) 0.0085(6) 0.0021(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 Fe1 N3 1.9219(10) . ? Fe1 N2 1.9220(10) . ? Fe1 N4 1.9224(10) . ? Fe1 N1 1.9255(10) . ? N1 C4 1.3867(15) . ? N1 C1 1.3874(15) . ? N2 C8 1.3862(15) . ? N2 C5 1.3877(15) . ? N3 C9 1.3834(15) . ? N3 C12 1.3862(15) . ? N4 C13 1.3892(15) . ? N4 C16 1.3923(15) . ? N6 C5 1.3246(15) . ? N6 C4 1.3361(15) . ? N7 C8 1.3240(15) . ? N7 C9 1.3277(15) . ? N8 C13 1.3268(15) . ? N8 C12 1.3295(15) . ? N5 C16 1.3256(15) . ? N5 C1 1.3335(15) . ? C1 C2 1.4500(16) . ? C2 C17 1.4008(16) . ? C2 C3 1.4070(16) . ? C3 C20 1.4033(16) . ? C3 C4 1.4470(16) . ? C5 C6 1.4607(16) . ? C6 C21 1.3971(16) . ? C6 C7 1.4001(16) . ? C7 C24 1.3982(16) . ? C7 C8 1.4529(16) . ? C9 C10 1.4526(16) . ? C10 C25 1.3991(16) . ? C10 C11 1.4044(16) . ? C11 C28 1.4007(16) . ? C11 C12 1.4530(16) . ? C13 C14 1.4561(16) . ? C14 C29 1.4001(16) . ? C14 C15 1.4019(16) . ? C15 C32 1.3967(16) . ? C15 C16 1.4515(16) . ? C17 C18 1.3913(17) . ? C17 H17 0.9500 . ? C18 C19 1.4091(19) . ? C18 H18 0.9500 . ? C19 C20 1.3879(17) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.3926(17) . ? C21 H21 0.9500 . ? C22 C23 1.4049(19) . ? C22 H22 0.9500 . ? C23 C24 1.3894(18) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3936(17) . ? C25 H25 0.9500 . ? C26 C27 1.4066(19) . ? C26 H26 0.9500 . ? C27 C28 1.3907(17) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.3912(17) . ? C29 H29 0.9500 . ? C30 C31 1.4057(18) . ? C30 H30 0.9500 . ? C31 C32 1.3864(17) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? N21 C201 1.4701(15) . ? N21 C203 1.4710(16) . ? N21 C205 1.4785(16) . ? N22 C207 1.4958(17) . ? N22 C206 1.5008(17) . ? N22 C202 1.5096(16) . ? N22 C204 1.5105(17) . ? C201 C202 1.5091(17) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.5104(18) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 H20I 0.9800 . ? C205 H20J 0.9800 . ? C205 H20K 0.9800 . ? C206 H20L 0.9800 . ? C206 H20M 0.9800 . ? C206 H20N 0.9800 . ? C207 H20O 0.9800 . ? C207 H20P 0.9800 . ? C207 H20Q 0.9800 . ? C1S C2S 1.513(2) . ? C1S C3A 2.212(8) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C3A C2S 1.624(12) . ? C3A C3A 1.404(18) 7_666 ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C3S C3S 1.528(3) 7_666 ? C3S C2S 1.533(2) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N2 90.38(4) . . ? N3 Fe1 N4 89.41(4) . . ? N2 Fe1 N4 173.25(4) . . ? N3 Fe1 N1 174.23(4) . . ? N2 Fe1 N1 89.40(4) . . ? N4 Fe1 N1 90.13(4) . . ? C4 N1 C1 107.07(9) . . ? C4 N1 Fe1 126.21(8) . . ? C1 N1 Fe1 126.66(8) . . ? C8 N2 C5 106.95(10) . . ? C8 N2 Fe1 126.16(8) . . ? C5 N2 Fe1 126.90(8) . . ? C9 N3 C12 107.17(9) . . ? C9 N3 Fe1 126.27(8) . . ? C12 N3 Fe1 126.56(8) . . ? C13 N4 C16 106.98(9) . . ? C13 N4 Fe1 126.49(8) . . ? C16 N4 Fe1 126.48(8) . . ? C5 N6 C4 121.22(10) . . ? C8 N7 C9 121.76(11) . . ? C13 N8 C12 121.20(10) . . ? C16 N5 C1 121.73(10) . . ? N5 C1 N1 127.30(11) . . ? N5 C1 C2 122.66(11) . . ? N1 C1 C2 109.91(10) . . ? C17 C2 C3 121.05(11) . . ? C17 C2 C1 132.60(11) . . ? C3 C2 C1 106.35(10) . . ? C20 C3 C2 120.89(11) . . ? C20 C3 C4 132.49(11) . . ? C2 C3 C4 106.60(10) . . ? N6 C4 N1 127.36(11) . . ? N6 C4 C3 122.54(11) . . ? N1 C4 C3 109.88(10) . . ? N6 C5 N2 127.32(11) . . ? N6 C5 C6 122.63(11) . . ? N2 C5 C6 110.02(10) . . ? C21 C6 C7 120.88(11) . . ? C21 C6 C5 132.98(11) . . ? C7 C6 C5 106.14(10) . . ? C24 C7 C6 121.59(11) . . ? C24 C7 C8 131.50(11) . . ? C6 C7 C8 106.90(10) . . ? N7 C8 N2 127.67(11) . . ? N7 C8 C7 122.34(11) . . ? N2 C8 C7 109.97(10) . . ? N7 C9 N3 127.60(11) . . ? N7 C9 C10 122.35(11) . . ? N3 C9 C10 110.04(10) . . ? C25 C10 C11 121.60(11) . . ? C25 C10 C9 132.03(11) . . ? C11 C10 C9 106.37(10) . . ? C28 C11 C10 120.81(11) . . ? C28 C11 C12 132.60(11) . . ? C10 C11 C12 106.57(10) . . ? N8 C12 N3 127.53(11) . . ? N8 C12 C11 122.55(11) . . ? N3 C12 C11 109.81(10) . . ? N8 C13 N4 127.35(11) . . ? N8 C13 C14 122.64(11) . . ? N4 C13 C14 109.89(10) . . ? C29 C14 C15 120.82(11) . . ? C29 C14 C13 132.82(11) . . ? C15 C14 C13 106.34(10) . . ? C32 C15 C14 121.20(11) . . ? C32 C15 C16 131.92(11) . . ? C14 C15 C16 106.87(10) . . ? N5 C16 N4 127.55(11) . . ? N5 C16 C15 122.62(11) . . ? N4 C16 C15 109.71(10) . . ? C18 C17 C2 117.61(12) . . ? C18 C17 H17 121.2 . . ? C2 C17 H17 121.2 . . ? C17 C18 C19 121.43(12) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 121.04(11) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C3 117.91(11) . . ? C19 C20 H20 121.0 . . ? C3 C20 H20 121.0 . . ? C22 C21 C6 117.68(11) . . ? C22 C21 H21 121.2 . . ? C6 C21 H21 121.2 . . ? C21 C22 C23 121.14(12) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 121.43(12) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C7 117.26(11) . . ? C23 C24 H24 121.4 . . ? C7 C24 H24 121.4 . . ? C26 C25 C10 117.22(12) . . ? C26 C25 H25 121.4 . . ? C10 C25 H25 121.4 . . ? C25 C26 C27 121.30(12) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.40(11) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C11 117.59(11) . . ? C27 C28 H28 121.2 . . ? C11 C28 H28 121.2 . . ? C30 C29 C14 117.67(11) . . ? C30 C29 H29 121.2 . . ? C14 C29 H29 121.2 . . ? C29 C30 C31 121.20(11) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 121.15(11) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C15 117.80(11) . . ? C31 C32 H32 121.1 . . ? C15 C32 H32 121.1 . . ? C201 N21 C203 108.81(10) . . ? C201 N21 C205 108.02(10) . . ? C203 N21 C205 108.08(10) . . ? C207 N22 C206 108.21(11) . . ? C207 N22 C202 111.54(10) . . ? C206 N22 C202 108.85(11) . . ? C207 N22 C204 111.55(11) . . ? C206 N22 C204 108.87(11) . . ? C202 N22 C204 107.77(9) . . ? N21 C201 C202 112.71(10) . . ? N21 C201 H20A 109.0 . . ? C202 C201 H20A 109.0 . . ? N21 C201 H20B 109.0 . . ? C202 C201 H20B 109.0 . . ? H20A C201 H20B 107.8 . . ? C201 C202 N22 113.00(10) . . ? C201 C202 H20C 109.0 . . ? N22 C202 H20C 109.0 . . ? C201 C202 H20D 109.0 . . ? N22 C202 H20D 109.0 . . ? H20C C202 H20D 107.8 . . ? N21 C203 C204 112.42(10) . . ? N21 C203 H20E 109.1 . . ? C204 C203 H20E 109.1 . . ? N21 C203 H20F 109.1 . . ? C204 C203 H20F 109.1 . . ? H20E C203 H20F 107.9 . . ? C203 C204 N22 112.95(10) . . ? C203 C204 H20G 109.0 . . ? N22 C204 H20G 109.0 . . ? C203 C204 H20H 109.0 . . ? N22 C204 H20H 109.0 . . ? H20G C204 H20H 107.8 . . ? N21 C205 H20I 109.5 . . ? N21 C205 H20J 109.5 . . ? H20I C205 H20J 109.5 . . ? N21 C205 H20K 109.5 . . ? H20I C205 H20K 109.5 . . ? H20J C205 H20K 109.5 . . ? N22 C206 H20L 109.5 . . ? N22 C206 H20M 109.5 . . ? H20L C206 H20M 109.5 . . ? N22 C206 H20N 109.5 . . ? H20L C206 H20N 109.5 . . ? H20M C206 H20N 109.5 . . ? N22 C207 H20O 109.5 . . ? N22 C207 H20P 109.5 . . ? H20O C207 H20P 109.5 . . ? N22 C207 H20Q 109.5 . . ? H20O C207 H20Q 109.5 . . ? H20P C207 H20Q 109.5 . . ? C2S C1S C3A 47.2(4) . . ? C2S C1S H1S1 109.5 . . ? C3A C1S H1S1 152.5 . . ? C2S C1S H1S2 109.5 . . ? C3A C1S H1S2 94.4 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? C3A C1S H1S3 73.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S C3A C3A 108.8(14) . 7_666 ? C2S C3A C1S 43.1(2) . . ? C3A C3A C1S 150.4(14) 7_666 . ? C2S C3A H3A1 109.9 . . ? C3A C3A H3A1 109.9 7_666 . ? C1S C3A H3A1 79.7 . . ? C2S C3A H3A2 109.9 . . ? C3A C3A H3A2 109.9 7_666 . ? C1S C3A H3A2 92.2 . . ? H3A1 C3A H3A2 108.3 . . ? C3S C3S C2S 113.40(15) 7_666 . ? C3S C3S H3S1 108.9 7_666 . ? C2S C3S H3S1 108.9 . . ? C3S C3S H3S2 108.9 7_666 . ? C2S C3S H3S2 108.9 . . ? H3S1 C3S H3S2 107.7 . . ? C1S C2S C3S 114.76(12) . . ? C1S C2S C3A 89.6(4) . . ? C1S C2S H2S1 113.7 . . ? C3A C2S H2S1 113.7 . . ? C1S C2S H2S2 113.7 . . ? C3A C2S H2S2 113.7 . . ? H2S1 C2S H2S2 111.0 . . ? _refine_diff_density_max 0.501 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 931420' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_CoPc_TMP_150K _audit_creation_date ; 'Tue Nov 13 14:26:21 2012' ; _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 Co N8, C7 H17 N2' _chemical_formula_sum 'C39 H33 Co N10' _chemical_formula_weight 700.68 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_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4374(12) _cell_length_b 16.7909(14) _cell_length_c 16.8616(17) _cell_angle_alpha 90.00 _cell_angle_beta 106.284(10) _cell_angle_gamma 90.00 _cell_volume 3380.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7810 _cell_measurement_theta_min 1.7023 _cell_measurement_theta_max 29.4023 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8342 _exptl_absorpt_correction_T_max 0.9623 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(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 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4752 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22160 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 29.47 _reflns_number_total 8127 _reflns_number_gt 5880 _reflns_threshold_expression >2sigma(I) _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.7539P] 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 8127 _refine_ls_number_parameters 558 _refine_ls_number_restraints 481 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.006 _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 Co1 Co 0.0000 0.0000 0.0000 0.01924(11) Uani 1 2 d S . . N101 N 0.11368(15) 0.00054(9) 0.10090(11) 0.0208(4) Uani 1 1 d . . . N102 N -0.10743(15) -0.02312(10) 0.05769(11) 0.0223(4) Uani 1 1 d . . . N103 N 0.00858(16) -0.02886(12) 0.19924(11) 0.0278(4) Uani 1 1 d . . . N104 N 0.27787(15) 0.03018(11) 0.05434(11) 0.0237(4) Uani 1 1 d . . . C5 C -0.08797(18) -0.03348(13) 0.14197(13) 0.0257(5) Uani 1 1 d . . . C6 C 0.22669(18) 0.01594(12) 0.11221(13) 0.0228(4) Uani 1 1 d . . . C7 C 0.28668(19) 0.01486(12) 0.19860(13) 0.0244(5) Uani 1 1 d . . . C8 C -0.22144(18) -0.03352(12) 0.02380(13) 0.0228(4) Uani 1 1 d . . . C9 C 0.10232(19) -0.01256(12) 0.17925(13) 0.0246(5) Uani 1 1 d . . . C11 C -0.19201(19) -0.05158(14) 0.16201(14) 0.0299(5) Uani 1 1 d . . . C13 C -0.27534(19) -0.05080(13) 0.08781(13) 0.0264(5) Uani 1 1 d . . . C14 C -0.3866(2) -0.06637(14) 0.08450(14) 0.0312(5) Uani 1 1 d . . . H14 H -0.4438 -0.0662 0.0335 0.037 Uiso 1 1 calc R . . C17 C 0.3513(2) 0.00439(14) 0.36822(15) 0.0337(6) Uani 1 1 d . . . H17 H 0.3756 0.0007 0.4268 0.040 Uiso 1 1 calc R . . C18 C 0.39842(19) 0.02980(14) 0.24007(14) 0.0289(5) Uani 1 1 d . . . H18 H 0.4513 0.0431 0.2110 0.035 Uiso 1 1 calc R . . C21 C 0.2404(2) -0.01011(14) 0.32726(14) 0.0315(5) Uani 1 1 d . . . H21 H 0.1877 -0.0234 0.3564 0.038 Uiso 1 1 calc R . . C23 C 0.20878(19) -0.00444(12) 0.24126(14) 0.0263(5) Uani 1 1 d . . . C25 C 0.4292(2) 0.02453(15) 0.32492(15) 0.0328(5) Uani 1 1 d . . . H25 H 0.5047 0.0347 0.3550 0.039 Uiso 1 1 calc R . . C30 C -0.4107(2) -0.08210(16) 0.15823(15) 0.0393(6) Uani 1 1 d . . . H30 H -0.4859 -0.0926 0.1579 0.047 Uiso 1 1 calc R . . C33 C -0.3269(2) -0.08282(18) 0.23270(16) 0.0449(7) Uani 1 1 d . . . H33 H -0.3460 -0.0938 0.2823 0.054 Uiso 1 1 calc R . . C35 C -0.2163(2) -0.06797(16) 0.23627(15) 0.0386(6) Uani 1 1 d . . . H35 H -0.1591 -0.0689 0.2873 0.046 Uiso 1 1 calc R . . Co2 Co 0.0000 0.5000 0.0000 0.01876(11) Uani 1 2 d S . . N201 N 0.12044(14) 0.42665(10) 0.02596(10) 0.0213(4) Uani 1 1 d . . . N202 N -0.10274(14) 0.41449(10) -0.00782(11) 0.0222(4) Uani 1 1 d . A . N203 N 0.02242(15) 0.30075(10) 0.02254(11) 0.0254(4) Uani 1 1 d . A . N204 N -0.28010(15) 0.48499(10) -0.04248(11) 0.0227(4) Uani 1 1 d . . . C3 C 0.11318(18) 0.34461(12) 0.03335(13) 0.0230(4) Uani 1 1 d . . . C4 C -0.07769(18) 0.33377(12) 0.00270(13) 0.0245(5) Uani 1 1 d D . . C10 C -0.21843(17) 0.41964(13) -0.02711(13) 0.0236(4) Uani 1 1 d D . . C12 C 0.23353(18) 0.44393(13) 0.04115(12) 0.0224(4) Uani 1 1 d . . . C15 C 0.22391(18) 0.30899(13) 0.05379(13) 0.0248(5) Uani 1 1 d . . . C19 C 0.29892(18) 0.37145(13) 0.05712(13) 0.0241(5) Uani 1 1 d . . . C24 C 0.2601(2) 0.23023(14) 0.06763(15) 0.0302(5) Uani 1 1 d . . . H24 H 0.2082 0.1879 0.0642 0.036 Uiso 1 1 calc R . . C27 C 0.41352(19) 0.35651(14) 0.07495(14) 0.0306(5) Uani 1 1 d . . . H27 H 0.4654 0.3984 0.0766 0.037 Uiso 1 1 calc R . . C28 C 0.3732(2) 0.21597(15) 0.08633(16) 0.0361(6) Uani 1 1 d . . . H28 H 0.4005 0.1631 0.0968 0.043 Uiso 1 1 calc R . . C29 C 0.4487(2) 0.27877(15) 0.09005(16) 0.0365(6) Uani 1 1 d . . . H29 H 0.5266 0.2674 0.1034 0.044 Uiso 1 1 calc R . . C21A C -0.2706(8) 0.3379(6) -0.0249(11) 0.0222(19) Uani 0.56(4) 1 d P A 1 C22A C -0.3806(8) 0.3116(8) -0.0381(10) 0.0291(19) Uani 0.56(4) 1 d PU A 1 H26 H -0.4418 0.3478 -0.0491 0.035 Uiso 0.56(4) 1 calc PR A 1 C23A C -0.3963(9) 0.2305(8) -0.0344(10) 0.0313(17) Uani 0.56(4) 1 d PU A 1 H31 H -0.4702 0.2106 -0.0433 0.038 Uiso 0.56(4) 1 calc PR A 1 C24A C -0.3066(11) 0.1765(7) -0.0178(10) 0.0307(17) Uani 0.56(4) 1 d PU A 1 H38 H -0.3219 0.1212 -0.0167 0.037 Uiso 0.56(4) 1 calc PR A 1 C25A C -0.1970(11) 0.2013(7) -0.0028(10) 0.0279(18) Uani 0.56(4) 1 d PU A 1 H34 H -0.1361 0.1649 0.0088 0.033 Uiso 0.56(4) 1 calc PR A 1 C26A C -0.1812(8) 0.2839(7) -0.0060(12) 0.0234(18) Uani 0.56(4) 1 d PU A 1 C21B C -0.2628(9) 0.3456(8) -0.0319(14) 0.026(3) Uani 0.44(4) 1 d PGDU A 2 C22B C -0.3728(8) 0.3187(10) -0.0507(12) 0.028(2) Uani 0.44(4) 1 d PGU A 2 H22B H -0.4327 0.3559 -0.0616 0.033 Uiso 0.44(4) 1 calc PR A 2 C23B C -0.3951(11) 0.2375(11) -0.0537(12) 0.033(2) Uani 0.44(4) 1 d PGU A 2 H23B H -0.4703 0.2192 -0.0665 0.039 Uiso 0.44(4) 1 calc PR A 2 C24B C -0.3074(14) 0.1831(8) -0.0378(12) 0.033(2) Uani 0.44(4) 1 d PGU A 2 H24B H -0.3227 0.1276 -0.0399 0.039 Uiso 0.44(4) 1 calc PR A 2 C25B C -0.1974(12) 0.2099(7) -0.0190(12) 0.027(2) Uani 0.44(4) 1 d PGU A 2 H25B H -0.1375 0.1727 -0.0082 0.032 Uiso 0.44(4) 1 calc PR A 2 C26B C -0.1751(9) 0.2911(7) -0.0161(14) 0.024(2) Uani 0.44(4) 1 d PGDU A 2 N301 N 0.9474(3) 0.70761(16) 0.21868(17) 0.0567(6) Uani 0.909(2) 1 d PU B 1 N302 N 1.1785(3) 0.69878(19) 0.2113(2) 0.0670(7) Uani 0.909(2) 1 d PU B 1 C304 C 1.0134(4) 0.7789(2) 0.2054(3) 0.0695(8) Uani 0.909(2) 1 d PU B 1 H30A H 0.9877 0.8264 0.2297 0.083 Uiso 0.909(2) 1 calc PR B 1 H30B H 0.9985 0.7883 0.1453 0.083 Uiso 0.909(2) 1 calc PR B 1 C303 C 1.1368(4) 0.7690(2) 0.2430(3) 0.0738(8) Uani 0.909(2) 1 d PU B 1 H30C H 1.1763 0.8167 0.2308 0.089 Uiso 0.909(2) 1 calc PR B 1 H30D H 1.1529 0.7645 0.3037 0.089 Uiso 0.909(2) 1 calc PR B 1 C301 C 0.9988(3) 0.63542(19) 0.1911(2) 0.0516(7) Uani 0.909(2) 1 d PU B 1 H30E H 0.9629 0.5871 0.2058 0.062 Uiso 0.909(2) 1 calc PR B 1 H30F H 0.9829 0.6368 0.1302 0.062 Uiso 0.909(2) 1 calc PR B 1 C306 C 0.8285(3) 0.7152(2) 0.1693(2) 0.0688(10) Uani 0.909(2) 1 d PU B 1 H30G H 0.8246 0.7204 0.1106 0.103 Uiso 0.909(2) 1 calc PR B 1 H30H H 0.7955 0.7625 0.1872 0.103 Uiso 0.909(2) 1 calc PR B 1 H30I H 0.7869 0.6677 0.1773 0.103 Uiso 0.909(2) 1 calc PR B 1 C302 C 1.1231(3) 0.6296(2) 0.2289(3) 0.0596(8) Uani 0.909(2) 1 d PU B 1 H30J H 1.1394 0.6232 0.2895 0.071 Uiso 0.909(2) 1 calc PR B 1 H30K H 1.1520 0.5820 0.2069 0.071 Uiso 0.909(2) 1 calc PR B 1 C305 C 0.9498(4) 0.7000(3) 0.3074(2) 0.0713(10) Uani 0.909(2) 1 d PU B 1 H30L H 1.0276 0.6951 0.3414 0.107 Uiso 0.909(2) 1 calc PR B 1 H30M H 0.9077 0.6526 0.3147 0.107 Uiso 0.909(2) 1 calc PR B 1 H30N H 0.9158 0.7474 0.3243 0.107 Uiso 0.909(2) 1 calc PR B 1 C307 C 1.2992(4) 0.6916(3) 0.2433(3) 0.0899(13) Uani 0.909(2) 1 d PU B 1 H30O H 1.3349 0.7398 0.2299 0.135 Uiso 0.909(2) 1 calc PR B 1 H30P H 1.3248 0.6453 0.2183 0.135 Uiso 0.909(2) 1 calc PR B 1 H30Q H 1.3193 0.6848 0.3034 0.135 Uiso 0.909(2) 1 calc PR B 1 N32A N 0.8551(14) 0.7547(10) 0.2173(12) 0.0626(13) Uani 0.091(2) 1 d PGU B 2 C32A C 0.9172(16) 0.7106(14) 0.2870(11) 0.0630(13) Uani 0.091(2) 1 d PGU B 2 H32A H 0.9115 0.6531 0.2734 0.076 Uiso 0.091(2) 1 calc PR B 2 H32B H 0.8846 0.7193 0.3335 0.076 Uiso 0.091(2) 1 calc PR B 2 C33A C 0.8997(15) 0.7410(14) 0.1490(9) 0.0649(11) Uani 0.091(2) 1 d PGU B 2 H33A H 0.8551 0.7707 0.1000 0.078 Uiso 0.091(2) 1 calc PR B 2 H33B H 0.8952 0.6836 0.1351 0.078 Uiso 0.091(2) 1 calc PR B 2 C37A C 0.7358(14) 0.7354(15) 0.1954(17) 0.066(3) Uani 0.091(2) 1 d PGU B 2 H37A H 0.6958 0.7668 0.1472 0.099 Uiso 0.091(2) 1 calc PR B 2 H37B H 0.7061 0.7477 0.2420 0.099 Uiso 0.091(2) 1 calc PR B 2 H37C H 0.7254 0.6785 0.1822 0.099 Uiso 0.091(2) 1 calc PR B 2 N31A N 1.0935(14) 0.7249(11) 0.2447(12) 0.0690(11) Uani 0.091(2) 1 d PGU B 2 C34A C 1.0199(16) 0.7680(14) 0.1704(11) 0.0692(12) Uani 0.091(2) 1 d PGU B 2 H34A H 1.0232 0.8259 0.1818 0.083 Uiso 0.091(2) 1 calc PR B 2 H34B H 1.0494 0.7589 0.1224 0.083 Uiso 0.091(2) 1 calc PR B 2 C31A C 1.0366(16) 0.7343(15) 0.3126(9) 0.0666(16) Uani 0.091(2) 1 d PGU B 2 H31A H 1.0768 0.7015 0.3606 0.080 Uiso 0.091(2) 1 calc PR B 2 H31B H 1.0422 0.7906 0.3307 0.080 Uiso 0.091(2) 1 calc PR B 2 C36A C 1.2064(14) 0.7606(16) 0.2694(17) 0.072(2) Uani 0.091(2) 1 d PGU B 2 H36A H 1.2006 0.8172 0.2817 0.108 Uiso 0.091(2) 1 calc PR B 2 H36B H 1.2412 0.7549 0.2243 0.108 Uiso 0.091(2) 1 calc PR B 2 H36C H 1.2524 0.7333 0.3187 0.108 Uiso 0.091(2) 1 calc PR B 2 C35A C 1.1077(18) 0.6396(12) 0.227(2) 0.062(2) Uani 0.091(2) 1 d PGU B 2 H35A H 1.0342 0.6137 0.2103 0.093 Uiso 0.091(2) 1 calc PR B 2 H35B H 1.1547 0.6137 0.2768 0.093 Uiso 0.091(2) 1 calc PR B 2 H35C H 1.1435 0.6352 0.1824 0.093 Uiso 0.091(2) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0197(2) 0.0200(2) 0.0187(2) 0.00089(15) 0.00650(16) -0.00092(15) N101 0.0208(9) 0.0208(8) 0.0213(9) 0.0009(7) 0.0065(7) 0.0007(7) N102 0.0242(10) 0.0220(8) 0.0217(9) 0.0006(7) 0.0079(7) 0.0001(7) N103 0.0266(10) 0.0345(10) 0.0233(9) 0.0024(8) 0.0088(8) -0.0017(8) N104 0.0241(10) 0.0239(9) 0.0242(9) 0.0003(8) 0.0083(8) -0.0016(8) C5 0.0266(12) 0.0290(11) 0.0234(11) 0.0027(9) 0.0104(9) -0.0008(9) C6 0.0243(11) 0.0193(10) 0.0247(11) 0.0000(8) 0.0065(9) -0.0005(8) C7 0.0261(12) 0.0239(11) 0.0232(11) -0.0006(9) 0.0068(9) 0.0017(9) C8 0.0226(11) 0.0221(10) 0.0257(11) -0.0007(9) 0.0100(9) -0.0022(9) C9 0.0263(12) 0.0253(11) 0.0224(11) 0.0008(9) 0.0073(9) 0.0006(9) C11 0.0271(12) 0.0360(12) 0.0292(12) 0.0005(10) 0.0123(10) -0.0026(10) C13 0.0275(12) 0.0272(11) 0.0271(11) 0.0003(9) 0.0120(9) -0.0022(9) C14 0.0270(12) 0.0373(13) 0.0308(12) -0.0036(10) 0.0104(10) -0.0046(10) C17 0.0311(13) 0.0467(15) 0.0210(11) 0.0012(10) 0.0035(10) 0.0052(11) C18 0.0236(12) 0.0319(12) 0.0309(12) 0.0007(10) 0.0070(10) 0.0011(10) C21 0.0269(12) 0.0436(14) 0.0249(11) 0.0036(10) 0.0087(10) 0.0040(10) C23 0.0262(12) 0.0274(11) 0.0253(11) 0.0004(9) 0.0070(9) 0.0028(9) C25 0.0247(12) 0.0394(13) 0.0317(13) 0.0001(11) 0.0037(10) 0.0025(10) C30 0.0315(13) 0.0539(16) 0.0376(14) -0.0047(12) 0.0180(11) -0.0110(12) C33 0.0401(15) 0.0686(19) 0.0325(14) -0.0005(13) 0.0208(12) -0.0113(14) C35 0.0330(14) 0.0563(16) 0.0287(13) 0.0033(12) 0.0123(11) -0.0067(12) Co2 0.0171(2) 0.01818(19) 0.0212(2) 0.00001(15) 0.00578(16) -0.00026(15) N201 0.0197(9) 0.0216(8) 0.0232(9) -0.0005(7) 0.0072(7) -0.0005(7) N202 0.0203(9) 0.0222(9) 0.0248(9) -0.0003(7) 0.0075(7) -0.0006(7) N203 0.0232(10) 0.0217(9) 0.0317(10) 0.0024(8) 0.0084(8) 0.0001(7) N204 0.0186(9) 0.0252(9) 0.0248(9) -0.0029(7) 0.0070(7) -0.0011(7) C3 0.0240(11) 0.0217(10) 0.0234(11) 0.0019(9) 0.0070(9) 0.0034(9) C4 0.0252(12) 0.0200(10) 0.0290(11) 0.0004(9) 0.0088(9) -0.0013(9) C10 0.0203(11) 0.0266(11) 0.0256(11) -0.0022(9) 0.0091(9) -0.0014(9) C12 0.0212(11) 0.0267(11) 0.0201(10) -0.0014(9) 0.0069(8) 0.0003(9) C15 0.0237(11) 0.0271(11) 0.0238(11) 0.0006(9) 0.0071(9) 0.0017(9) C19 0.0227(11) 0.0266(11) 0.0230(11) -0.0010(9) 0.0064(9) 0.0026(9) C24 0.0290(13) 0.0249(11) 0.0372(13) 0.0026(10) 0.0099(10) 0.0022(10) C27 0.0220(12) 0.0328(12) 0.0371(13) -0.0010(10) 0.0086(10) 0.0009(10) C28 0.0340(14) 0.0281(12) 0.0465(15) 0.0072(11) 0.0120(12) 0.0110(11) C29 0.0230(12) 0.0364(13) 0.0497(16) 0.0018(12) 0.0095(11) 0.0070(11) C21A 0.024(3) 0.013(3) 0.033(4) 0.000(2) 0.012(3) -0.005(2) C22A 0.021(2) 0.030(4) 0.042(4) 0.001(3) 0.018(2) -0.005(2) C23A 0.031(2) 0.027(3) 0.041(5) 0.003(3) 0.019(3) -0.011(2) C24A 0.035(2) 0.022(2) 0.038(4) 0.003(3) 0.015(3) -0.008(2) C25A 0.034(3) 0.017(2) 0.035(5) 0.011(2) 0.012(3) -0.002(2) C26A 0.022(2) 0.025(3) 0.028(4) 0.004(2) 0.014(2) -0.008(2) C21B 0.022(4) 0.028(4) 0.034(5) 0.000(3) 0.017(3) -0.007(3) C22B 0.027(3) 0.018(3) 0.045(5) 0.007(3) 0.021(3) -0.005(3) C23B 0.027(3) 0.032(4) 0.046(5) 0.006(4) 0.020(3) -0.009(3) C24B 0.039(3) 0.022(3) 0.042(5) 0.004(3) 0.019(4) -0.010(3) C25B 0.029(3) 0.022(4) 0.035(5) 0.008(3) 0.019(3) 0.000(3) C26B 0.030(3) 0.018(3) 0.026(5) 0.005(3) 0.013(3) -0.003(3) N301 0.0780(14) 0.0469(12) 0.0484(12) -0.0025(10) 0.0228(11) -0.0050(11) N302 0.0741(15) 0.0625(14) 0.0650(14) 0.0029(12) 0.0207(12) -0.0127(12) C304 0.0860(16) 0.0508(13) 0.0706(15) 0.0006(13) 0.0202(14) -0.0076(13) C303 0.0831(17) 0.0569(14) 0.0776(16) -0.0003(14) 0.0164(15) -0.0151(15) C301 0.0720(17) 0.0424(14) 0.0425(14) -0.0024(12) 0.0197(13) -0.0031(13) C306 0.078(2) 0.067(2) 0.062(2) -0.0071(17) 0.0196(17) 0.0040(18) C302 0.0735(17) 0.0521(15) 0.0519(15) -0.0002(14) 0.0155(14) -0.0032(14) C305 0.093(2) 0.076(2) 0.0501(19) -0.0126(17) 0.0281(18) -0.005(2) C307 0.074(3) 0.109(3) 0.081(3) 0.002(2) 0.013(2) -0.018(2) N32A 0.079(2) 0.054(2) 0.056(2) -0.003(2) 0.022(2) -0.004(2) C32A 0.080(2) 0.056(2) 0.055(2) -0.004(2) 0.022(2) -0.005(2) C33A 0.0811(19) 0.0527(18) 0.0613(19) -0.0016(18) 0.0207(18) -0.0056(18) C37A 0.077(4) 0.060(4) 0.062(4) -0.004(4) 0.020(4) 0.000(4) N31A 0.0811(18) 0.0569(17) 0.0683(17) -0.0001(16) 0.0196(17) -0.0099(16) C34A 0.083(2) 0.0542(19) 0.069(2) -0.0003(19) 0.0196(19) -0.0091(19) C31A 0.081(3) 0.059(2) 0.061(2) -0.003(2) 0.022(2) -0.007(2) C36A 0.079(4) 0.062(4) 0.072(4) 0.001(3) 0.017(3) -0.009(4) C35A 0.075(3) 0.054(3) 0.057(3) 0.000(3) 0.019(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N101 1.8827(18) 3 ? Co1 N101 1.8827(18) . ? Co1 N102 1.9002(17) 3 ? Co1 N102 1.9003(17) . ? N101 C9 1.385(3) . ? N101 C6 1.389(3) . ? N102 C8 1.383(3) . ? N102 C5 1.384(3) . ? N103 C5 1.315(3) . ? N103 C9 1.330(3) . ? N104 C8 1.309(3) 3 ? N104 C6 1.328(3) . ? C5 C11 1.458(3) . ? C6 C7 1.439(3) . ? C7 C18 1.392(3) . ? C7 C23 1.397(3) . ? C8 N104 1.309(3) 3 ? C8 C13 1.451(3) . ? C9 C23 1.445(3) . ? C11 C13 1.383(3) . ? C11 C35 1.396(3) . ? C13 C14 1.394(3) . ? C14 C30 1.383(3) . ? C14 H14 0.9500 . ? C17 C21 1.380(3) . ? C17 C25 1.408(3) . ? C17 H17 0.9500 . ? C18 C25 1.376(3) . ? C18 H18 0.9500 . ? C21 C23 1.395(3) . ? C21 H21 0.9500 . ? C25 H25 0.9500 . ? C30 C33 1.389(4) . ? C30 H30 0.9500 . ? C33 C35 1.382(3) . ? C33 H33 0.9500 . ? C35 H35 0.9500 . ? Co2 N201 1.8933(17) . ? Co2 N201 1.8933(17) 3_565 ? Co2 N202 1.9018(17) 3_565 ? Co2 N202 1.9019(17) . ? N201 C3 1.388(3) . ? N201 C12 1.388(3) . ? N202 C10 1.386(3) . ? N202 C4 1.391(3) . ? N203 C3 1.317(3) . ? N203 C4 1.318(3) . ? N204 C10 1.322(3) . ? N204 C12 1.324(3) 3_565 ? C3 C15 1.452(3) . ? C4 C26B 1.366(15) . ? C4 C26A 1.507(13) . ? C10 C21B 1.354(15) . ? C10 C21A 1.523(13) . ? C12 N204 1.324(3) 3_565 ? C12 C19 1.446(3) . ? C15 C19 1.394(3) . ? C15 C24 1.395(3) . ? C19 C27 1.394(3) . ? C24 C28 1.374(3) . ? C24 H24 0.9500 . ? C27 C29 1.378(3) . ? C27 H27 0.9500 . ? C28 C29 1.402(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C21A C22A 1.395(7) . ? C21A C26A 1.400(6) . ? C22A C23A 1.379(7) . ? C22A H26 0.9500 . ? C23A C24A 1.403(7) . ? C23A H31 0.9500 . ? C24A C25A 1.380(7) . ? C24A H38 0.9500 . ? C25A C26A 1.404(7) . ? C25A H34 0.9500 . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B H22B 0.9500 . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? N301 C306 1.486(5) . ? N301 C305 1.493(4) . ? N301 C304 1.503(5) . ? N301 C301 1.503(4) . ? N302 C302 1.424(5) . ? N302 C307 1.450(5) . ? N302 C303 1.450(5) . ? C304 C303 1.497(6) . ? C304 H30A 0.9900 . ? C304 H30B 0.9900 . ? C303 H30C 0.9900 . ? C303 H30D 0.9900 . ? C301 C302 1.502(5) . ? C301 H30E 0.9900 . ? C301 H30F 0.9900 . ? C306 H30G 0.9800 . ? C306 H30H 0.9800 . ? C306 H30I 0.9800 . ? C302 H30J 0.9900 . ? C302 H30K 0.9900 . ? C305 H30L 0.9800 . ? C305 H30M 0.9800 . ? C305 H30N 0.9800 . ? C307 H30O 0.9800 . ? C307 H30P 0.9800 . ? C307 H30Q 0.9800 . ? N32A C32A 1.4198 . ? N32A C33A 1.4317 . ? N32A C37A 1.4612 . ? C32A C31A 1.4801 . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.5055 . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? N31A C36A 1.4747 . ? N31A C35A 1.4825 . ? N31A C34A 1.5127 . ? N31A C31A 1.5135 . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? 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 N101 Co1 N101 180.0 3 . ? N101 Co1 N102 89.77(8) 3 3 ? N101 Co1 N102 90.23(8) . 3 ? N101 Co1 N102 90.23(8) 3 . ? N101 Co1 N102 89.77(8) . . ? N102 Co1 N102 180.0 3 . ? C9 N101 C6 105.58(17) . . ? C9 N101 Co1 127.56(15) . . ? C6 N101 Co1 126.84(14) . . ? C8 N102 C5 105.79(17) . . ? C8 N102 Co1 126.93(14) . . ? C5 N102 Co1 127.28(15) . . ? C5 N103 C9 120.72(19) . . ? C8 N104 C6 121.01(19) 3 . ? N103 C5 N102 127.4(2) . . ? N103 C5 C11 121.94(19) . . ? N102 C5 C11 110.67(19) . . ? N104 C6 N101 127.5(2) . . ? N104 C6 C7 121.8(2) . . ? N101 C6 C7 110.75(18) . . ? C18 C7 C23 121.5(2) . . ? C18 C7 C6 131.9(2) . . ? C23 C7 C6 106.66(19) . . ? N104 C8 N102 127.50(19) 3 . ? N104 C8 C13 121.89(19) 3 . ? N102 C8 C13 110.61(18) . . ? N103 C9 N101 127.3(2) . . ? N103 C9 C23 121.8(2) . . ? N101 C9 C23 110.94(19) . . ? C13 C11 C35 121.2(2) . . ? C13 C11 C5 106.09(19) . . ? C35 C11 C5 132.7(2) . . ? C11 C13 C14 121.2(2) . . ? C11 C13 C8 106.83(19) . . ? C14 C13 C8 131.9(2) . . ? C30 C14 C13 117.6(2) . . ? C30 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C21 C17 C25 121.3(2) . . ? C21 C17 H17 119.4 . . ? C25 C17 H17 119.4 . . ? C25 C18 C7 117.2(2) . . ? C25 C18 H18 121.4 . . ? C7 C18 H18 121.4 . . ? C17 C21 C23 117.3(2) . . ? C17 C21 H21 121.3 . . ? C23 C21 H21 121.3 . . ? C21 C23 C7 121.1(2) . . ? C21 C23 C9 132.8(2) . . ? C7 C23 C9 106.04(19) . . ? C18 C25 C17 121.6(2) . . ? C18 C25 H25 119.2 . . ? C17 C25 H25 119.2 . . ? C14 C30 C33 121.2(2) . . ? C14 C30 H30 119.4 . . ? C33 C30 H30 119.4 . . ? C35 C33 C30 121.5(2) . . ? C35 C33 H33 119.2 . . ? C30 C33 H33 119.2 . . ? C33 C35 C11 117.4(2) . . ? C33 C35 H35 121.3 . . ? C11 C35 H35 121.3 . . ? N201 Co2 N201 180.0 . 3_565 ? N201 Co2 N202 90.14(7) . 3_565 ? N201 Co2 N202 89.86(7) 3_565 3_565 ? N201 Co2 N202 89.86(7) . . ? N201 Co2 N202 90.14(7) 3_565 . ? N202 Co2 N202 180.0 3_565 . ? C3 N201 C12 106.20(17) . . ? C3 N201 Co2 126.80(14) . . ? C12 N201 Co2 127.00(14) . . ? C10 N202 C4 105.74(17) . . ? C10 N202 Co2 127.04(14) . . ? C4 N202 Co2 127.20(14) . . ? C3 N203 C4 120.80(18) . . ? C10 N204 C12 121.18(19) . 3_565 ? N203 C3 N201 128.11(19) . . ? N203 C3 C15 121.45(19) . . ? N201 C3 C15 110.42(18) . . ? N203 C4 C26B 123.5(3) . . ? N203 C4 N202 127.19(19) . . ? C26B C4 N202 109.2(3) . . ? N203 C4 C26A 120.7(3) . . ? C26B C4 C26A 7.6(14) . . ? N202 C4 C26A 112.0(3) . . ? N204 C10 C21B 123.1(3) . . ? N204 C10 N202 127.21(19) . . ? C21B C10 N202 109.6(2) . . ? N204 C10 C21A 121.7(3) . . ? C21B C10 C21A 5.3(15) . . ? N202 C10 C21A 111.1(3) . . ? N204 C12 N201 127.41(19) 3_565 . ? N204 C12 C19 122.33(19) 3_565 . ? N201 C12 C19 110.26(18) . . ? C19 C15 C24 121.7(2) . . ? C19 C15 C3 106.21(18) . . ? C24 C15 C3 132.1(2) . . ? C27 C19 C15 120.4(2) . . ? C27 C19 C12 132.8(2) . . ? C15 C19 C12 106.88(19) . . ? C28 C24 C15 117.7(2) . . ? C28 C24 H24 121.2 . . ? C15 C24 H24 121.2 . . ? C29 C27 C19 117.6(2) . . ? C29 C27 H27 121.2 . . ? C19 C27 H27 121.2 . . ? C24 C28 C29 120.6(2) . . ? C24 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C27 C29 C28 122.0(2) . . ? C27 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C22A C21A C26A 120.8(5) . . ? C22A C21A C10 133.4(5) . . ? C26A C21A C10 105.8(5) . . ? C23A C22A C21A 116.7(5) . . ? C23A C22A H26 121.6 . . ? C21A C22A H26 121.6 . . ? C22A C23A C24A 122.2(5) . . ? C22A C23A H31 118.9 . . ? C24A C23A H31 118.9 . . ? C25A C24A C23A 122.1(5) . . ? C25A C24A H38 119.0 . . ? C23A C24A H38 119.0 . . ? C24A C25A C26A 115.7(5) . . ? C24A C25A H34 122.2 . . ? C26A C25A H34 122.2 . . ? C25A C26A C21A 122.5(5) . . ? C25A C26A C4 132.0(5) . . ? C21A C26A C4 105.4(5) . . ? C10 C21B C22B 132.0(3) . . ? C10 C21B C26B 107.9(3) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B H22B 120.0 . . ? C21B C22B H22B 120.0 . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C4 C26B C25B 132.7(3) . . ? C4 C26B C21B 107.3(3) . . ? C25B C26B C21B 120.0 . . ? C306 N301 C305 107.8(3) . . ? C306 N301 C304 110.3(3) . . ? C305 N301 C304 111.0(3) . . ? C306 N301 C301 109.8(3) . . ? C305 N301 C301 110.5(3) . . ? C304 N301 C301 107.4(3) . . ? C302 N302 C307 111.4(3) . . ? C302 N302 C303 110.0(3) . . ? C307 N302 C303 111.7(3) . . ? N301 C304 C303 112.8(3) . . ? N301 C304 H30A 109.0 . . ? C303 C304 H30A 109.0 . . ? N301 C304 H30B 109.0 . . ? C303 C304 H30B 109.0 . . ? H30A C304 H30B 107.8 . . ? N302 C303 C304 111.4(3) . . ? N302 C303 H30C 109.4 . . ? C304 C303 H30C 109.4 . . ? N302 C303 H30D 109.4 . . ? C304 C303 H30D 109.4 . . ? H30C C303 H30D 108.0 . . ? C302 C301 N301 113.5(3) . . ? C302 C301 H30E 108.9 . . ? N301 C301 H30E 108.9 . . ? C302 C301 H30F 108.9 . . ? N301 C301 H30F 108.9 . . ? H30E C301 H30F 107.7 . . ? N301 C306 H30G 109.5 . . ? N301 C306 H30H 109.5 . . ? H30G C306 H30H 109.5 . . ? N301 C306 H30I 109.5 . . ? H30G C306 H30I 109.5 . . ? H30H C306 H30I 109.5 . . ? N302 C302 C301 111.1(3) . . ? N302 C302 H30J 109.4 . . ? C301 C302 H30J 109.4 . . ? N302 C302 H30K 109.4 . . ? C301 C302 H30K 109.4 . . ? H30J C302 H30K 108.0 . . ? N301 C305 H30L 109.5 . . ? N301 C305 H30M 109.5 . . ? H30L C305 H30M 109.5 . . ? N301 C305 H30N 109.5 . . ? H30L C305 H30N 109.5 . . ? H30M C305 H30N 109.5 . . ? N302 C307 H30O 109.5 . . ? N302 C307 H30P 109.5 . . ? H30O C307 H30P 109.5 . . ? N302 C307 H30Q 109.5 . . ? H30O C307 H30Q 109.5 . . ? H30P C307 H30Q 109.5 . . ? C32A N32A C33A 109.8 . . ? C32A N32A C37A 111.9 . . ? C33A N32A C37A 110.9 . . ? N32A C32A C31A 111.8 . . ? N32A C32A H32A 109.3 . . ? C31A C32A H32A 109.3 . . ? N32A C32A H32B 109.3 . . ? C31A C32A H32B 109.3 . . ? H32A C32A H32B 107.9 . . ? N32A C33A C34A 110.0 . . ? N32A C33A H33A 109.7 . . ? C34A C33A H33A 109.7 . . ? N32A C33A H33B 109.7 . . ? C34A C33A H33B 109.7 . . ? H33A C33A H33B 108.2 . . ? N32A C37A H37A 109.5 . . ? N32A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? N32A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C36A N31A C35A 106.9 . . ? C36A N31A C34A 110.3 . . ? C35A N31A C34A 112.0 . . ? C36A N31A C31A 110.7 . . ? C35A N31A C31A 111.1 . . ? C34A N31A C31A 105.9 . . ? C33A C34A N31A 112.6 . . ? C33A C34A H34A 109.1 . . ? N31A C34A H34A 109.1 . . ? C33A C34A H34B 109.1 . . ? N31A C34A H34B 109.1 . . ? H34A C34A H34B 107.8 . . ? C32A C31A N31A 113.3 . . ? C32A C31A H31A 108.9 . . ? N31A C31A H31A 108.9 . . ? C32A C31A H31B 108.9 . . ? N31A C31A H31B 108.9 . . ? H31A C31A H31B 107.7 . . ? N31A C36A H36A 109.5 . . ? N31A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? N31A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? N31A C35A H35A 109.5 . . ? N31A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? N31A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.594 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 931416'