Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Pan, Long' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Kelly, Sean' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Huang, Xiaoying' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Li, Jing' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; _publ_contact_author_name 'Prof Jing Li' _publ_contact_author_address ; Department of Chemistry and Chemical Biology Rutgers University Wright-Rieman Labs 610 Taylor Road Piscataway New Jersey 08854 UNITED STATES OF AMERICA ; _publ_contact_author_email 'JINGLI@RUTCHEM.RUTGERS.EDU' _publ_contact_author_fax '+1(856)225-6506' _publ_contact_author_phone '+1(856)225-6160' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Unique 2D Metalloporphyrin Networks Constructed from Iron(II) and meso-tetra(4-pyridyl)porphyrin ; data_sk2-2e _database_code_CSD 179299 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Catena (mu4-meso-tetrkis(4-pyridyl)porphyrin-iron(II)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Fe(tpyp) _chemical_formula_sum 'C40 H24 Fe N8' _chemical_formula_weight 672.52 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z' 'x, -y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1, z+1/2' '-x+1/2, -y+1, z+1/2' '-x, -y, -z' 'x, -y, -z' '-x, y-1/2, -z-1/2' 'x, y-1/2, -z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x+1/2, y, -z-1/2' 'x+1/2, y, -z-1/2' _cell_length_a 18.1781(11) _cell_length_b 13.7783(8) _cell_length_c 13.7565(8) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3445.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 6292 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 _exptl_crystal_description 'square plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9043 _exptl_absorpt_correction_T_max 0.9999 _exptl_absorpt_process_details 'SADABS V2.03 (Bruker-AXS, 2001)' _exptl_special_details ; Frame time 20 sec Dark Current time 20 sec Frame width (omega) 0.3 deg Frame Size 512x512 Detector Distance 6.07 cm Hemisphere Array Collected ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX' _diffrn_measurement_method '0.3 deg omeg slices' _diffrn_detector_area_resol_mean .8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10497 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.56 _reflns_number_total 2152 _reflns_number_gt 1879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS, 2001)' _computing_cell_refinement 'SAINT+ V6.02A (Bruker-AXS, 2001)' _computing_data_reduction 'SAINT+ V6.02A (Bruker-AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio(MCI, 2001)' _computing_publication_material 'Window Word2000' _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^)+(0.0400P)^2^+7.3000P] 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 1879 _refine_ls_number_parameters 189 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.5000 0.0000 0.01638(13) Uani 1 4 d S . . N1 N 0.07749(8) 0.43086(10) 0.07563(10) 0.0238(3) Uani 1 1 d . . . N2 N 0.0000 0.10731(14) 0.40112(13) 0.0247(4) Uani 1 2 d S . . C1 C 0.15205(12) 0.44058(15) 0.06702(17) 0.0395(5) Uani 1 1 d . A . C2 C 0.18903(15) 0.3796(2) 0.1376(2) 0.0656(9) Uani 1 1 d . . . H2 H 0.2386(19) 0.375(2) 0.143(2) 0.079 Uiso 1 1 d . . . C3 C 0.13733(15) 0.3327(2) 0.1866(2) 0.0595(8) Uani 1 1 d . . . H3 H 0.1428(16) 0.290(2) 0.231(2) 0.071 Uiso 1 1 d . . . C4 C 0.06746(11) 0.36394(12) 0.14942(13) 0.0304(4) Uani 1 1 d . . . C5 C 0.0000 0.33215(16) 0.18349(16) 0.0271(5) Uani 1 2 d S . . C6 C 0.0000 0.25534(17) 0.26047(17) 0.0309(6) Uani 1 2 d S . . C7 C 0.0000 0.1586(2) 0.2352(2) 0.0726(15) Uani 1 2 d S . . H7 H 0.0000 0.141(3) 0.171(3) 0.087 Uiso 1 2 d S . . C8 C 0.0000 0.0879(2) 0.3064(2) 0.0669(14) Uani 1 2 d S . . H8 H 0.0000 0.024(3) 0.288(3) 0.080 Uiso 1 2 d S . . C9 C 0.0000 0.20097(18) 0.42568(18) 0.0308(6) Uani 1 2 d S . . H9 H 0.0000 0.215(2) 0.493(2) 0.037 Uiso 1 2 d S . . C10 C 0.0000 0.27590(19) 0.35859(19) 0.0364(7) Uani 1 2 d S . . H10 H 0.0000 0.342(3) 0.378(2) 0.044 Uiso 1 2 d S . . C11 C 0.18817(16) 0.5000 0.0000 0.0508(9) Uani 1 2 d SD . . C12A C 0.2696(4) 0.5257(7) 0.0142(5) 0.0338(16) Uani 0.33 1 d P A 1 C13A C 0.3202(4) 0.4535(6) -0.0063(6) 0.0407(17) Uani 0.33 1 d P A 1 H13A H 0.3046 0.3923 -0.0259 0.049 Uiso 0.33 1 calc PR A 1 C14A C 0.3969(5) 0.4747(6) 0.0030(18) 0.046(3) Uani 0.33 1 d PD A 1 H14A H 0.4308 0.4261 -0.0112 0.055 Uiso 0.33 1 calc PR A 1 N3A N 0.4221(4) 0.5623(6) 0.0316(9) 0.061(2) Uani 0.33 1 d PD A 1 C15A C 0.3708(5) 0.6266(7) 0.0542(9) 0.076(3) Uani 0.33 1 d P A 1 H15A H 0.3869 0.6870 0.0755 0.091 Uiso 0.33 1 calc PR A 1 C16A C 0.2964(4) 0.6127(5) 0.0492(7) 0.058(2) Uani 0.33 1 d P A 1 H16A H 0.2643 0.6613 0.0692 0.070 Uiso 0.33 1 calc PR A 1 C12B C 0.2695(3) 0.5166(12) 0.0399(9) 0.0338(16) Uani 0.17 1 d PGD A 2 C13B C 0.3194(7) 0.4873(11) -0.0307(7) 0.0407(17) Uani 0.17 1 d PG A 2 H13B H 0.3026 0.4635 -0.0899 0.049 Uiso 0.17 1 calc PR A 2 C14B C 0.3946(6) 0.4936(13) -0.0129(9) 0.046(3) Uani 0.17 1 d PG A 2 H14B H 0.4280 0.4740 -0.0601 0.055 Uiso 0.17 1 calc PR A 2 N3B N 0.4197(3) 0.5292(13) 0.0756(11) 0.071(6) Uani 0.17 1 d PG A 2 C15B C 0.3697(5) 0.5585(9) 0.1463(8) 0.070(5) Uani 0.17 1 d PG A 2 H15B H 0.3866 0.5823 0.2055 0.084 Uiso 0.17 1 calc PR A 2 C16B C 0.2946(4) 0.5522(10) 0.1284(8) 0.062(4) Uani 0.17 1 d PG A 2 H16B H 0.2612 0.5718 0.1757 0.074 Uiso 0.17 1 calc PR 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 0.0277(2) 0.0106(2) 0.0109(2) 0.00063(15) 0.000 0.000 N1 0.0331(8) 0.0164(6) 0.0217(7) 0.0042(5) -0.0060(6) -0.0024(6) N2 0.0464(12) 0.0142(9) 0.0135(8) 0.0010(7) 0.000 0.000 C1 0.0349(10) 0.0339(10) 0.0496(12) 0.0158(9) -0.0128(9) -0.0039(8) C2 0.0394(13) 0.0700(17) 0.087(2) 0.0444(16) -0.0287(13) -0.0081(12) C3 0.0533(15) 0.0584(15) 0.0667(16) 0.0406(14) -0.0303(13) -0.0110(12) C4 0.0443(11) 0.0216(8) 0.0253(8) 0.0088(6) -0.0131(8) -0.0051(8) C5 0.0530(16) 0.0138(10) 0.0145(10) 0.0023(8) 0.000 0.000 C6 0.0579(17) 0.0165(11) 0.0184(11) 0.0050(9) 0.000 0.000 C7 0.186(5) 0.0189(13) 0.0129(12) 0.0014(10) 0.000 0.000 C8 0.169(5) 0.0134(12) 0.0185(13) 0.0005(10) 0.000 0.000 C9 0.0567(17) 0.0199(11) 0.0158(11) -0.0002(9) 0.000 0.000 C10 0.072(2) 0.0163(12) 0.0211(12) 0.0012(9) 0.000 0.000 C11 0.0259(14) 0.0505(19) 0.076(2) 0.0277(18) 0.000 0.000 C12A 0.030(2) 0.031(3) 0.041(5) 0.002(3) 0.001(2) -0.0027(16) C13A 0.034(2) 0.052(5) 0.036(4) 0.003(3) -0.008(3) 0.014(3) C14A 0.036(2) 0.059(9) 0.043(4) -0.006(9) -0.002(4) 0.011(3) N3A 0.034(4) 0.054(5) 0.094(7) -0.022(5) 0.012(4) -0.019(3) C15A 0.043(4) 0.055(5) 0.130(9) -0.037(6) 0.011(5) -0.015(4) C16A 0.028(3) 0.038(4) 0.108(7) -0.020(4) 0.009(4) -0.010(3) C12B 0.030(2) 0.031(3) 0.041(5) 0.002(3) 0.001(2) -0.0027(16) C13B 0.034(2) 0.052(5) 0.036(4) 0.003(3) -0.008(3) 0.014(3) C14B 0.036(2) 0.059(9) 0.043(4) -0.006(9) -0.002(4) 0.011(3) N3B 0.028(7) 0.067(11) 0.119(18) -0.019(11) 0.023(9) -0.016(7) C15B 0.044(8) 0.087(13) 0.079(12) -0.030(10) -0.015(8) -0.009(8) C16B 0.047(8) 0.063(10) 0.075(11) -0.022(9) 0.003(8) -0.013(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 Fe1 N1 1.9935(14) 2 ? Fe1 N1 1.9935(14) 9_565 ? Fe1 N1 1.9935(14) . ? Fe1 N1 1.9935(14) 10_565 ? Fe1 N2 2.0090(19) 11_566 ? Fe1 N2 2.0090(19) 3_554 ? N1 C1 1.367(3) . ? N1 C4 1.383(2) . ? N2 C8 1.331(3) . ? N2 C9 1.334(3) . ? N2 Fe1 2.0090(19) 3 ? C1 C11 1.397(2) . ? C1 C2 1.449(3) . ? C2 C3 1.326(4) . ? C2 H2 0.91(3) . ? C3 C4 1.436(3) . ? C3 H3 0.85(3) . ? C4 C5 1.384(2) . ? C5 C4 1.384(2) 2 ? C5 C6 1.497(3) . ? C6 C7 1.377(4) . ? C6 C10 1.379(3) . ? C7 C8 1.381(4) . ? C7 H7 0.92(5) . ? C8 H8 0.91(4) . ? C9 C10 1.385(3) . ? C9 H9 0.94(3) . ? C10 H10 0.95(3) . ? C11 C1 1.397(2) 10_565 ? C11 C12A 1.535(7) . ? C11 C12B 1.593(2) . ? C12A C16A 1.381(10) . ? C12A C13A 1.383(10) . ? C13A C14A 1.430(10) . ? C13A H13A 0.9300 . ? C14A N3A 1.350(2) . ? C14A H14A 0.9300 . ? N3A C15A 1.322(12) . ? C15A C16A 1.366(10) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C12B C13B 1.3900 . ? C12B C16B 1.3900 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B N3B 1.3900 . ? C14B H14B 0.9300 . ? N3B C15B 1.3900 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? 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 Fe1 N1 90.08(8) 2 9_565 ? N1 Fe1 N1 89.92(8) 2 . ? N1 Fe1 N1 180.0 9_565 . ? N1 Fe1 N1 180.00(7) 2 10_565 ? N1 Fe1 N1 89.92(8) 9_565 10_565 ? N1 Fe1 N1 90.08(8) . 10_565 ? N1 Fe1 N2 89.91(5) 2 11_566 ? N1 Fe1 N2 90.09(5) 9_565 11_566 ? N1 Fe1 N2 89.91(5) . 11_566 ? N1 Fe1 N2 90.09(5) 10_565 11_566 ? N1 Fe1 N2 90.09(5) 2 3_554 ? N1 Fe1 N2 89.91(5) 9_565 3_554 ? N1 Fe1 N2 90.09(5) . 3_554 ? N1 Fe1 N2 89.91(5) 10_565 3_554 ? N2 Fe1 N2 180.00(8) 11_566 3_554 ? C1 N1 C4 105.04(15) . . ? C1 N1 Fe1 127.48(12) . . ? C4 N1 Fe1 127.47(13) . . ? C8 N2 C9 116.2(2) . . ? C8 N2 Fe1 121.04(17) . 3 ? C9 N2 Fe1 122.72(16) . 3 ? N1 C1 C11 125.49(19) . . ? N1 C1 C2 110.19(19) . . ? C11 C1 C2 124.3(2) . . ? C3 C2 C1 107.2(2) . . ? C3 C2 H2 129.3(19) . . ? C1 C2 H2 123.5(19) . . ? C2 C3 C4 107.41(19) . . ? C2 C3 H3 128(2) . . ? C4 C3 H3 124(2) . . ? N1 C4 C5 125.19(17) . . ? N1 C4 C3 110.19(18) . . ? C5 C4 C3 124.62(17) . . ? C4 C5 C4 124.8(2) . 2 ? C4 C5 C6 117.60(11) . . ? C4 C5 C6 117.60(11) 2 . ? C7 C6 C10 116.5(2) . . ? C7 C6 C5 120.4(2) . . ? C10 C6 C5 123.2(2) . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 120(3) . . ? C8 C7 H7 120(3) . . ? N2 C8 C7 123.6(3) . . ? N2 C8 H8 118(3) . . ? C7 C8 H8 118(3) . . ? N2 C9 C10 123.5(2) . . ? N2 C9 H9 116.3(19) . . ? C10 C9 H9 120(2) . . ? C6 C10 C9 119.9(2) . . ? C6 C10 H10 118(2) . . ? C9 C10 H10 122(2) . . ? C1 C11 C1 123.9(3) . 10_565 ? C1 C11 C12A 120.3(3) . . ? C1 C11 C12A 113.7(3) 10_565 . ? C1 C11 C12B 107.0(6) . . ? C1 C11 C12B 125.4(6) 10_565 . ? C16A C12A C13A 117.4(6) . . ? C16A C12A C11 125.8(7) . . ? C13A C12A C11 116.7(7) . . ? C12A C13A C14A 118.9(7) . . ? C12A C13A H13A 120.6 . . ? C14A C13A H13A 120.6 . . ? N3A C14A C13A 122.6(7) . . ? N3A C14A H14A 118.7 . . ? C13A C14A H14A 118.7 . . ? C15A N3A C14A 115.4(8) . . ? N3A C15A C16A 126.3(8) . . ? N3A C15A H15A 116.9 . . ? C16A C15A H15A 116.9 . . ? C15A C16A C12A 119.2(7) . . ? C15A C16A H16A 120.4 . . ? C12A C16A H16A 120.4 . . ? C13B C12B C16B 120.0 . . ? C13B C12B C11 108.9(8) . . ? C16B C12B C11 131.1(8) . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B N3B 120.0 . . ? C13B C14B H14B 120.0 . . ? N3B C14B H14B 120.0 . . ? C14B N3B C15B 120.0 . . ? C16B C15B N3B 120.0 . . ? C16B C15B H15B 120.0 . . ? N3B C15B H15B 120.0 . . ? C15B C16B C12B 120.0 . . ? C15B C16B H16B 120.0 . . ? C12B C16B H16B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C1 -179.00(14) 2 . . . ? N1 Fe1 N1 C1 -11(100) 9_565 . . . ? N1 Fe1 N1 C1 1.00(14) 10_565 . . . ? N2 Fe1 N1 C1 -89.10(17) 11_566 . . . ? N2 Fe1 N1 C1 90.90(17) 3_554 . . . ? N1 Fe1 N1 C4 -0.28(17) 2 . . . ? N1 Fe1 N1 C4 168(100) 9_565 . . . ? N1 Fe1 N1 C4 179.72(17) 10_565 . . . ? N2 Fe1 N1 C4 89.62(14) 11_566 . . . ? N2 Fe1 N1 C4 -90.38(14) 3_554 . . . ? C4 N1 C1 C11 178.93(18) . . . . ? Fe1 N1 C1 C11 -2.1(3) . . . . ? C4 N1 C1 C2 -0.8(3) . . . . ? Fe1 N1 C1 C2 178.18(18) . . . . ? N1 C1 C2 C3 1.1(4) . . . . ? C11 C1 C2 C3 -178.6(2) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? C1 N1 C4 C5 179.6(2) . . . . ? Fe1 N1 C4 C5 0.7(3) . . . . ? C1 N1 C4 C3 0.2(2) . . . . ? Fe1 N1 C4 C3 -178.71(16) . . . . ? C2 C3 C4 N1 0.4(3) . . . . ? C2 C3 C4 C5 -179.0(3) . . . . ? N1 C4 C5 C4 -1.0(4) . . . 2 ? C3 C4 C5 C4 178.3(2) . . . 2 ? N1 C4 C5 C6 176.85(18) . . . . ? C3 C4 C5 C6 -3.9(3) . . . . ? C4 C5 C6 C7 -89.00(18) . . . . ? C4 C5 C6 C7 89.00(18) 2 . . . ? C4 C5 C6 C10 91.00(18) . . . . ? C4 C5 C6 C10 -91.00(18) 2 . . . ? C10 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C8 180.0 . . . . ? C9 N2 C8 C7 0.0 . . . . ? Fe1 N2 C8 C7 180.0 3 . . . ? C6 C7 C8 N2 0.0 . . . . ? C8 N2 C9 C10 0.0 . . . . ? Fe1 N2 C9 C10 180.0 3 . . . ? C7 C6 C10 C9 0.0 . . . . ? C5 C6 C10 C9 180.0 . . . . ? N2 C9 C10 C6 0.0 . . . . ? N1 C1 C11 C1 1.11(16) . . . 10_565 ? C2 C1 C11 C1 -179.2(3) . . . 10_565 ? N1 C1 C11 C12A 163.8(4) . . . . ? C2 C1 C11 C12A -16.5(5) . . . . ? N1 C1 C11 C12B 160.5(6) . . . . ? C2 C1 C11 C12B -19.8(6) . . . . ? C1 C11 C12A C16A -102.3(8) . . . . ? C1 C11 C12A C16A 62.1(9) 10_565 . . . ? C12B C11 C12A C16A -89(3) . . . . ? C1 C11 C12A C13A 74.9(7) . . . . ? C1 C11 C12A C13A -120.8(6) 10_565 . . . ? C12B C11 C12A C13A 88(4) . . . . ? C16A C12A C13A C14A -4.4(16) . . . . ? C11 C12A C13A C14A 178.2(12) . . . . ? C12A C13A C14A N3A 0(2) . . . . ? C13A C14A N3A C15A 3(2) . . . . ? C14A N3A C15A C16A -1(2) . . . . ? N3A C15A C16A C12A -2.7(19) . . . . ? C13A C12A C16A C15A 5.5(14) . . . . ? C11 C12A C16A C15A -177.4(8) . . . . ? C1 C11 C12B C13B 123.8(7) . . . . ? C1 C11 C12B C13B -77.1(9) 10_565 . . . ? C12A C11 C12B C13B -44(3) . . . . ? C1 C11 C12B C16B -55.4(11) . . . . ? C1 C11 C12B C16B 103.6(9) 10_565 . . . ? C12A C11 C12B C16B 137(4) . . . . ? C16B C12B C13B C14B 0.0 . . . . ? C11 C12B C13B C14B -179.3(12) . . . . ? C12B C13B C14B N3B 0.0 . . . . ? C13B C14B N3B C15B 0.0 . . . . ? C14B N3B C15B C16B 0.0 . . . . ? N3B C15B C16B C12B 0.0 . . . . ? C13B C12B C16B C15B 0.0 . . . . ? C11 C12B C16B C15B 179.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.500 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.064 data_sk2-2e-t _database_code_CSD 190853 _audit_creation_method SHELXL-97 _publ_section_title ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Fe(tpyp) _chemical_formula_sum 'C40 H24 Fe N8' _chemical_formula_weight 672.52 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 13.758(2) _cell_length_b 13.758(2) _cell_length_c 36.606(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6928.9(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.74 _cell_measurement_theta_max 11.91 _exptl_crystal_description Square-plate _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% +-3.0 _diffrn_reflns_number 3286 _diffrn_reflns_av_R_equivalents 0.1739 _diffrn_reflns_av_sigmaI/netI 0.1462 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1701 _reflns_number_gt 593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4/PC' _computing_cell_refinement 'CAD4/PC' _computing_data_reduction 'XCAD4/PC' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Material Studio' _computing_publication_material 'Windows Word2000' _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^)+(0.0150P)^2^+15.0000P] 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 593 _refine_ls_number_parameters 105 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.2239 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.137 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.0000 0.2500 0.1250 0.0199(3) Uani 1 4 d S . . N1 N -0.0741(5) 0.1791(5) 0.08647(11) 0.0298(11) Uani 1 1 d . . . N2 N -0.3967(3) -0.1467(3) 0.1250 0.0324(15) Uani 1 2 d S . . C1 C -0.1464(7) 0.1109(7) 0.09154(15) 0.0379(15) Uani 1 1 d U . . C2 C -0.1811(7) 0.0788(8) 0.05673(16) 0.069(2) Uani 1 1 d U . . H2A H -0.2290 0.0323 0.0527 0.083 Uiso 1 1 calc R . . C3 C -0.1327(8) 0.1273(8) 0.03106(17) 0.076(2) Uani 1 1 d U . . H3A H -0.1418 0.1220 0.0060 0.091 Uiso 1 1 calc R . . C4 C -0.0637(7) 0.1891(8) 0.04914(15) 0.0463(15) Uani 1 1 d U A . C5 C 0.0000 0.2500 0.03166(17) 0.0480(18) Uani 1 2 d SU . . C6 C -0.1753(4) 0.0747(4) 0.1250 0.0360(18) Uani 1 2 d SU . . C7 C -0.2516(6) -0.0016(6) 0.1250 0.0363(15) Uani 1 2 d SU . . C8 C -0.3476(4) 0.0193(4) 0.1185(3) 0.053(2) Uani 1 1 d U . . H8A H -0.3667 0.0827 0.1135 0.063 Uiso 1 1 calc R . . C9 C -0.4161(4) -0.0550(4) 0.1195(3) 0.055(2) Uani 1 1 d U . . H9A H -0.4808 -0.0380 0.1159 0.066 Uiso 1 1 calc R . . C10A C 0.0262(17) 0.2304(15) -0.0100(3) 0.047(4) Uiso 0.30 1 d PGU A 1 C11A C 0.0644(15) 0.1412(14) -0.0206(5) 0.078(7) Uiso 0.30 1 d PGU A 1 H11A H 0.0906 0.0995 -0.0032 0.094 Uiso 0.30 1 calc PR A 1 C12A C 0.0633(15) 0.1143(10) -0.0572(5) 0.129(11) Uiso 0.30 1 d PGU A 1 H12A H 0.0889 0.0546 -0.0643 0.155 Uiso 0.30 1 calc PR A 1 N3A N 0.0241(14) 0.1766(11) -0.0832(4) 0.069(6) Uiso 0.30 1 d PG A 1 C13A C -0.0141(17) 0.2658(12) -0.0726(4) 0.062(5) Uiso 0.30 1 d PGU A 1 H13A H -0.0403 0.3075 -0.0899 0.074 Uiso 0.30 1 calc PR A 1 C14A C -0.013(2) 0.2927(12) -0.0360(4) 0.056(5) Uiso 0.30 1 d PGU A 1 H14A H -0.0385 0.3524 -0.0289 0.067 Uiso 0.30 1 calc PR A 1 C10B C 0.016(2) 0.254(3) -0.0087(4) 0.047(4) Uiso 0.20 1 d PGU A 2 C11B C 0.105(2) 0.231(3) -0.0245(7) 0.078(7) Uiso 0.20 1 d PGU A 2 H11B H 0.1574 0.2138 -0.0098 0.094 Uiso 0.20 1 calc PR A 2 C12B C 0.1160(14) 0.234(2) -0.0622(7) 0.129(11) Uiso 0.20 1 d PGU A 2 H12B H 0.1755 0.2188 -0.0727 0.155 Uiso 0.20 1 calc PR A 2 N3B N 0.0379(18) 0.260(2) -0.0842(5) 0.069(6) Uiso 0.20 1 d PG A 2 C13B C -0.0511(16) 0.283(2) -0.0685(7) 0.062(5) Uiso 0.20 1 d PGU A 2 H13B H -0.1034 0.3008 -0.0832 0.074 Uiso 0.20 1 calc PR A 2 C14B C -0.0620(18) 0.280(3) -0.0307(7) 0.056(5) Uiso 0.20 1 d PGU A 2 H14B H -0.1216 0.2958 -0.0202 0.067 Uiso 0.20 1 calc PR 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 Fe 0.0146(4) 0.0146(4) 0.0306(7) 0.000 0.000 -0.0017(12) N1 0.022(5) 0.025(6) 0.042(3) 0.004(4) -0.009(4) -0.0035(17) N2 0.023(2) 0.023(2) 0.051(4) 0.000(6) 0.000(6) 0.009(3) C1 0.034(6) 0.031(6) 0.048(3) 0.001(4) -0.007(4) -0.010(3) C2 0.080(7) 0.078(7) 0.049(4) 0.000(6) -0.017(6) -0.048(4) C3 0.090(8) 0.095(8) 0.042(4) 0.000(6) -0.017(6) -0.048(4) C4 0.041(6) 0.057(7) 0.040(3) -0.013(5) -0.001(5) -0.014(3) C5 0.053(9) 0.056(9) 0.035(4) 0.000 0.000 -0.025(6) C6 0.031(3) 0.031(3) 0.047(4) 0.006(6) -0.006(6) -0.005(3) C7 0.0288(18) 0.0288(18) 0.051(4) 0.001(5) -0.001(5) -0.002(3) C8 0.036(3) 0.031(4) 0.091(7) 0.000(5) -0.011(5) -0.004(3) C9 0.037(3) 0.034(3) 0.095(7) 0.018(5) -0.027(5) -0.007(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 Fe N1 1.995(4) 10_454 ? Fe N1 1.995(4) . ? Fe N1 1.995(4) 8 ? Fe N1 1.995(4) 15_444 ? Fe N2 2.010(5) 20_566 ? Fe N2 2.010(5) 27 ? N1 C4 1.381(6) . ? N1 C1 1.380(6) . ? N2 C9 1.305(6) . ? N2 C9 1.305(6) 15_444 ? N2 Fe 2.010(5) 27_455 ? C1 C6 1.381(6) . ? C1 C2 1.430(7) . ? C2 C3 1.331(8) . ? C3 C4 1.436(7) . ? C4 C5 1.371(6) . ? C5 C4 1.371(6) 10_454 ? C5 C10B 1.496(17) . ? C5 C10A 1.589(14) . ? C6 C1 1.381(6) 15_444 ? C6 C7 1.485(14) . ? C7 C8 1.372(8) . ? C7 C8 1.372(8) 15_444 ? C8 C9 1.391(7) . ? C10A C11A 1.3900 . ? C10A C14A 1.3900 . ? C11A C12A 1.3900 . ? C12A N3A 1.3900 . ? N3A C13A 1.3900 . ? C13A C14A 1.3900 . ? C10B C11B 1.3900 . ? C10B C14B 1.3900 . ? C11B C12B 1.3900 . ? C12B N3B 1.3900 . ? N3B C13B 1.3900 . ? C13B C14B 1.3900 . ? 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 Fe N1 90.0(2) 10_454 . ? N1 Fe N1 90.0(2) 10_454 8 ? N1 Fe N1 178.2(5) . 8 ? N1 Fe N1 178.2(5) 10_454 15_444 ? N1 Fe N1 90.0(2) . 15_444 ? N1 Fe N1 90.0(2) 8 15_444 ? N1 Fe N2 90.9(3) 10_454 20_566 ? N1 Fe N2 89.1(3) . 20_566 ? N1 Fe N2 89.1(3) 8 20_566 ? N1 Fe N2 90.9(3) 15_444 20_566 ? N1 Fe N2 89.1(3) 10_454 27 ? N1 Fe N2 90.9(3) . 27 ? N1 Fe N2 90.9(3) 8 27 ? N1 Fe N2 89.1(3) 15_444 27 ? N2 Fe N2 180.0 20_566 27 ? C4 N1 C1 106.0(4) . . ? C4 N1 Fe 126.7(3) . . ? C1 N1 Fe 127.3(4) . . ? C9 N2 C9 114.8(7) . 15_444 ? C9 N2 Fe 122.6(3) . 27_455 ? C9 N2 Fe 122.6(3) 15_444 27_455 ? N1 C1 C6 124.9(5) . . ? N1 C1 C2 109.3(5) . . ? C6 C1 C2 125.7(5) . . ? C3 C2 C1 107.9(5) . . ? C2 C3 C4 107.6(5) . . ? C5 C4 N1 126.1(5) . . ? C5 C4 C3 124.7(5) . . ? N1 C4 C3 109.2(5) . . ? C4 C5 C4 124.4(7) 10_454 . ? C4 C5 C10B 125.5(14) . . ? C4 C5 C10A 119.3(9) . . ? C1 C6 C1 125.5(7) . 15_444 ? C1 C6 C7 117.3(3) . . ? C1 C6 C7 117.3(3) 15_444 . ? C8 C7 C8 115.7(10) . 15_444 ? C8 C7 C6 122.1(5) . . ? C8 C7 C6 122.1(5) 15_444 . ? C7 C8 C9 119.6(7) . . ? N2 C9 C8 125.2(6) . . ? C11A C10A C14A 120.0 . . ? C11A C10A C5 120.3(12) . . ? C14A C10A C5 117.6(12) . . ? C10A C11A C12A 120.0 . . ? N3A C12A C11A 120.0 . . ? C12A N3A C13A 120.0 . . ? C14A C13A N3A 120.0 . . ? C13A C14A C10A 120.0 . . ? C11B C10B C14B 120.0 . . ? C11B C10B C5 122(2) . . ? C14B C10B C5 118(2) . . ? C12B C11B C10B 120.0 . . ? C11B C12B N3B 120.0 . . ? C13B N3B C12B 120.0 . . ? N3B C13B C14B 120.0 . . ? C13B C14B C10B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe N1 C4 0.0(8) 10_454 . . . ? N1 Fe N1 C4 90.9(9) 8 . . . ? N1 Fe N1 C4 -178.2(11) 15_444 . . . ? N2 Fe N1 C4 90.9(9) 20_566 . . . ? N2 Fe N1 C4 -89.1(9) 27 . . . ? N1 Fe N1 C1 -179.5(12) 10_454 . . . ? N1 Fe N1 C1 -88.6(10) 8 . . . ? N1 Fe N1 C1 2.3(8) 15_444 . . . ? N2 Fe N1 C1 -88.6(10) 20_566 . . . ? N2 Fe N1 C1 91.4(10) 27 . . . ? C4 N1 C1 C6 175.5(10) . . . . ? Fe N1 C1 C6 -4.9(17) . . . . ? C4 N1 C1 C2 -0.2(13) . . . . ? Fe N1 C1 C2 179.4(8) . . . . ? N1 C1 C2 C3 -1.1(15) . . . . ? C6 C1 C2 C3 -176.8(12) . . . . ? C1 C2 C3 C4 1.9(16) . . . . ? C1 N1 C4 C5 179.6(11) . . . . ? Fe N1 C4 C5 0.1(17) . . . . ? C1 N1 C4 C3 1.3(14) . . . . ? Fe N1 C4 C3 -178.3(8) . . . . ? C2 C3 C4 C5 179.6(12) . . . . ? C2 C3 C4 N1 -2.0(17) . . . . ? N1 C4 C5 C4 0.0(9) . . . 10_454 ? C3 C4 C5 C4 178.0(15) . . . 10_454 ? N1 C4 C5 C10B 175(2) . . . . ? C3 C4 C5 C10B -7(3) . . . . ? N1 C4 C5 C10A 161.3(12) . . . . ? C3 C4 C5 C10A -20.7(17) . . . . ? N1 C1 C6 C1 2.5(9) . . . 15_444 ? C2 C1 C6 C1 177.6(15) . . . 15_444 ? N1 C1 C6 C7 -177.5(9) . . . . ? C2 C1 C6 C7 -2.4(15) . . . . ? C1 C6 C7 C8 -74.9(7) . . . . ? C1 C6 C7 C8 105.1(7) 15_444 . . . ? C1 C6 C7 C8 105.1(7) . . . 15_444 ? C1 C6 C7 C8 -74.9(7) 15_444 . . 15_444 ? C8 C7 C8 C9 1.0(7) 15_444 . . . ? C6 C7 C8 C9 -179.0(7) . . . . ? C9 N2 C9 C8 1.2(8) 15_444 . . . ? Fe N2 C9 C8 -178.8(8) 27_455 . . . ? C7 C8 C9 N2 -2.3(17) . . . . ? C4 C5 C10A C11A -56.7(17) . . . . ? C4 C5 C10A C14A -90.2(12) 10_454 . . . ? C4 C5 C10A C14A 106.7(13) . . . . ? C14A C10A C11A C12A 0.0 . . . . ? C5 C10A C11A C12A 163.0(18) . . . . ? C10A C11A C12A N3A 0.0 . . . . ? C11A C12A N3A C13A 0.0 . . . . ? C12A N3A C13A C14A 0.0 . . . . ? N3A C13A C14A C10A 0.0 . . . . ? C11A C10A C14A C13A 0.0 . . . . ? C5 C10A C14A C13A -163.4(17) . . . . ? C4 C5 C10B C11B 59(3) 10_454 . . . ? C4 C5 C10B C11B -116.6(17) . . . . ? C4 C5 C10B C14B -122.6(16) 10_454 . . . ? C4 C5 C10B C14B 62(3) . . . . ? C14B C10B C11B C12B 0.0 . . . . ? C5 C10B C11B C12B 179(3) . . . . ? C10B C11B C12B N3B 0.0 . . . . ? C11B C12B N3B C13B 0.0 . . . . ? C12B N3B C13B C14B 0.0 . . . . ? N3B C13B C14B C10B 0.0 . . . . ? C11B C10B C14B C13B 0.0 . . . . ? C5 C10B C14B C13B -179(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.557 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.081