# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Tamotsu Inabe' _publ_contact_author_email INABE@SCI.HOKUDAI.AC.JP _publ_section_title ; Variable mgnetotransport properties in the TPP[Fe(Pc)L2]2 system (TPP = tetraphenylphosphonium, Pc = phthalocyaninato, L = CN, Cl, and Br) ; loop_ _publ_author_name 'Tamotsu Inabe' 'Noriaki Hanasaki' 'Akira Kikuchi' 'Masaki Matsuda' 'Toshio Naito' 'Hiroyuki Tajima' ; T.Taketsugu ; 'Derrick Ethelbhert C. Yu' # Attachment 'FePctotal.cif' data__TPP[Fe(Pc)Cl2]2 _database_code_depnum_ccdc_archive 'CCDC 699209' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C88 H52 Cl4 Fe2 N16 P ' _chemical_formula_moiety 'C88 H52 Cl4 Fe2 N16 P ' _chemical_formula_weight 1617.97 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,1/2+X,1/2+Z 3 1/2-X,1/2-Y,+Z 4 1/2+Y,-X,1/2+Z 5 -X,-Y,-Z 6 +Y,1/2-X,1/2-Z 7 1/2+X,1/2+Y,-Z 8 1/2-Y,+X,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 21.49(2) _cell_length_b 21.49(2) _cell_length_c 7.472(10) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3450(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24551 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1654.00 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.936 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 26705 _diffrn_reflns_av_R_equivalents 0.116 _diffrn_reflns_theta_max 27.43 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3941 _reflns_number_gt 1979 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1288 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3941 _refine_ls_number_parameters 265 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0008Fo^2^ + 0.4000\s(Fo^2^) + 0.2000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.26 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.5000 0.0000 0.5000 0.02322(18) Uani 1.00 2 d S . . Cl(1) Cl 0.58771(5) -0.05196(4) 0.40458(13) 0.0373(2) Uani 1.00 1 d . . . P(1) P 0.2500 0.2500 0.7500 0.0235(3) Uani 1.00 4 d S . . N(1) N 0.48826(13) -0.06779(13) 0.6680(3) 0.0228(7) Uani 1.00 1 d . . . N(2) N 0.55674(13) -0.03488(13) 0.9069(3) 0.0231(7) Uani 1.00 1 d . . . N(3) N 0.55273(12) 0.04254(12) 0.6723(3) 0.0221(7) Uani 1.00 1 d . . . N(4) N 0.57780(12) 0.13637(12) 0.5069(3) 0.0226(7) Uani 1.00 1 d . . . C(1) C 0.51807(15) -0.07413(16) 0.8301(4) 0.0233(9) Uani 1.00 1 d . . . C(2) C 0.57208(15) 0.01912(15) 0.8327(4) 0.0226(9) Uani 1.00 1 d . . . C(3) C 0.61556(15) 0.06208(15) 0.9177(4) 0.0223(8) Uani 1.00 1 d . . . C(4) C 0.64789(15) 0.05988(16) 1.0782(4) 0.0261(9) Uani 1.00 1 d . . . C(5) C 0.68518(16) 0.11060(17) 1.1189(4) 0.0291(9) Uani 1.00 1 d . . . C(6) C 0.69069(16) 0.16119(16) 1.0038(4) 0.0275(9) Uani 1.00 1 d . . . C(7) C 0.65872(15) 0.16267(16) 0.8424(4) 0.0244(9) Uani 1.00 1 d . . . C(8) C 0.62127(15) 0.11257(15) 0.8007(4) 0.0220(8) Uani 1.00 1 d . . . C(9) C 0.58170(16) 0.09916(15) 0.6467(4) 0.0230(9) Uani 1.00 1 d . . . C(10) C 0.54401(15) 0.12222(16) 0.3640(4) 0.0237(9) Uani 1.00 1 d . . . C(11) C 0.53486(16) 0.16515(15) 0.2159(4) 0.0233(8) Uani 1.00 1 d . . . C(12) C 0.55514(16) 0.22609(15) 0.1883(4) 0.0257(9) Uani 1.00 1 d . . . C(13) C 0.53508(16) 0.25540(15) 0.0334(4) 0.0256(9) Uani 1.00 1 d . . . C(14) C 0.49699(16) 0.22536(16) -0.0899(4) 0.0270(9) Uani 1.00 1 d . . . C(15) C 0.47731(16) 0.16440(16) -0.0624(4) 0.0261(9) Uani 1.00 1 d . . . C(16) C 0.49614(15) 0.13523(15) 0.0930(4) 0.0232(8) Uani 1.00 1 d . . . C(17) C 0.31490(16) 0.26312(16) 0.6045(4) 0.0254(9) Uani 1.00 1 d . . . C(18) C 0.36519(16) 0.22239(19) 0.5997(5) 0.0341(10) Uani 1.00 1 d . . . C(19) C 0.41304(18) 0.2330(2) 0.4777(5) 0.0445(12) Uani 1.00 1 d . . . C(20) C 0.41023(19) 0.2829(2) 0.3617(5) 0.0423(12) Uani 1.00 1 d . . . C(21) C 0.35957(19) 0.32292(19) 0.3644(5) 0.0372(11) Uani 1.00 1 d . . . C(22) C 0.31214(17) 0.31308(17) 0.4848(5) 0.0324(10) Uani 1.00 1 d . . . H(1) H 0.6444 0.0252 1.1565 0.031 Uiso 1.00 1 c R . . H(2) H 0.7079 0.1107 1.2280 0.035 Uiso 1.00 1 c R . . H(3) H 0.7164 0.1953 1.0366 0.033 Uiso 1.00 1 c R . . H(4) H 0.6627 0.1969 0.7628 0.029 Uiso 1.00 1 c R . . H(5) H 0.5814 0.2465 0.2722 0.031 Uiso 1.00 1 c R . . H(6) H 0.5480 0.2969 0.0102 0.031 Uiso 1.00 1 c R . . H(7) H 0.4839 0.2468 -0.1945 0.032 Uiso 1.00 1 c R . . H(8) H 0.4518 0.1434 -0.1468 0.031 Uiso 1.00 1 c R . . H(9) H 0.3666 0.1878 0.6789 0.041 Uiso 1.00 1 c R . . H(10) H 0.4477 0.2056 0.4739 0.053 Uiso 1.00 1 c R . . H(11) H 0.4433 0.2899 0.2798 0.051 Uiso 1.00 1 c R . . H(12) H 0.3576 0.3573 0.2846 0.045 Uiso 1.00 1 c R . . H(13) H 0.2771 0.3400 0.4868 0.039 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0278(4) 0.0234(3) 0.0185(3) -0.0036(3) -0.0022(3) 0.0023(3) Cl(1) 0.0411(5) 0.0351(5) 0.0357(5) -0.0038(4) -0.0015(4) 0.0025(4) P(1) 0.0226(5) 0.0226(5) 0.0253(9) 0.0000 0.0000 0.0000 N(1) 0.0256(15) 0.0251(15) 0.0177(14) -0.0017(12) -0.0020(12) -0.0002(12) N(2) 0.0277(15) 0.0238(14) 0.0179(14) -0.0025(12) -0.0034(12) 0.0017(12) N(3) 0.0238(14) 0.0231(14) 0.0194(14) -0.0024(12) -0.0016(12) 0.0007(12) N(4) 0.0245(14) 0.0236(14) 0.0197(14) -0.0021(11) 0.0017(12) 0.0009(13) C(1) 0.0224(17) 0.0259(18) 0.0217(18) 0.0027(14) 0.0027(14) 0.0017(14) C(2) 0.0219(17) 0.0280(18) 0.0179(17) 0.0046(14) 0.0010(13) 0.0004(14) C(3) 0.0198(16) 0.0262(17) 0.0209(17) -0.0016(14) 0.0014(14) 0.0005(15) C(4) 0.0268(18) 0.0298(19) 0.0217(18) 0.0015(15) 0.0009(15) 0.0030(15) C(5) 0.0243(18) 0.037(2) 0.0257(19) -0.0025(16) -0.0064(15) 0.0018(16) C(6) 0.0299(18) 0.0264(17) 0.0262(17) -0.0036(15) -0.0057(16) 0.0001(16) C(7) 0.0251(18) 0.0233(17) 0.0248(18) 0.0028(15) 0.0005(14) 0.0031(14) C(8) 0.0208(17) 0.0267(18) 0.0186(17) 0.0020(14) 0.0012(13) 0.0005(14) C(9) 0.0238(18) 0.0227(17) 0.0226(18) 0.0022(14) -0.0001(14) -0.0005(14) C(10) 0.0213(17) 0.0272(18) 0.0228(19) 0.0001(15) 0.0026(14) -0.0031(14) C(11) 0.0260(17) 0.0235(17) 0.0205(18) 0.0026(14) 0.0004(14) 0.0015(14) C(12) 0.0274(18) 0.0234(17) 0.0262(19) -0.0025(15) -0.0008(15) -0.0007(15) C(13) 0.0292(18) 0.0205(17) 0.027(2) -0.0046(14) 0.0029(15) 0.0018(14) C(14) 0.0299(19) 0.0289(19) 0.0223(18) 0.0009(15) -0.0000(16) 0.0074(15) C(15) 0.0262(18) 0.0324(19) 0.0198(17) 0.0021(16) -0.0012(14) 0.0011(15) C(16) 0.0238(17) 0.0248(17) 0.0211(17) 0.0029(14) -0.0003(15) 0.0001(14) C(17) 0.0247(18) 0.0287(19) 0.0227(18) -0.0010(15) 0.0019(14) -0.0002(15) C(18) 0.031(2) 0.045(2) 0.027(2) 0.0062(17) -0.0031(17) 0.0011(18) C(19) 0.028(2) 0.072(3) 0.033(2) 0.014(2) 0.0022(18) -0.002(2) C(20) 0.033(2) 0.063(2) 0.030(2) -0.008(2) 0.0079(17) -0.007(2) C(21) 0.044(2) 0.035(2) 0.033(2) -0.0091(19) 0.0044(18) 0.0008(17) C(22) 0.0316(19) 0.0302(19) 0.036(2) -0.0012(15) 0.0040(18) -0.0026(17) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) Cl(1) 2.3037(10) yes . . Fe(1) Cl(1) 2.3037(10) yes . 5_656 Fe(1) N(1) 1.939(2) yes . . Fe(1) N(1) 1.939(2) yes . 5_656 Fe(1) N(3) 1.943(2) yes . . Fe(1) N(3) 1.943(2) yes . 5_656 P(1) C(17) 1.791(3) yes . . P(1) C(17) 1.791(3) yes . 3_555 P(1) C(17) 1.791(3) yes . 6_556 P(1) C(17) 1.791(3) yes . 8_556 N(1) C(1) 1.377(4) yes . . N(1) C(10) 1.380(4) yes . 5_656 N(2) C(1) 1.316(4) yes . . N(2) C(2) 1.328(4) yes . . N(3) C(2) 1.365(4) yes . . N(3) C(9) 1.380(4) yes . . N(4) C(9) 1.318(4) yes . . N(4) C(10) 1.327(4) yes . . C(1) C(16) 1.465(4) yes . 5_656 C(2) C(3) 1.459(4) yes . . C(3) C(4) 1.387(4) yes . . C(3) C(8) 1.399(4) yes . . C(4) C(5) 1.387(4) yes . . C(5) C(6) 1.392(5) yes . . C(6) C(7) 1.388(4) yes . . C(7) C(8) 1.380(4) yes . . C(8) C(9) 1.460(4) yes . . C(10) C(11) 1.454(4) yes . . C(11) C(12) 1.395(4) yes . . C(11) C(16) 1.396(4) yes . . C(12) C(13) 1.387(4) yes . . C(13) C(14) 1.391(4) yes . . C(14) C(15) 1.392(4) yes . . C(15) C(16) 1.380(4) yes . . C(17) C(18) 1.391(5) yes . . C(17) C(22) 1.399(5) yes . . C(18) C(19) 1.393(5) yes . . C(19) C(20) 1.380(6) yes . . C(20) C(21) 1.387(5) yes . . C(21) C(22) 1.375(5) yes . . C(4) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(13) H(6) 0.950 no . . C(14) H(7) 0.950 no . . C(15) H(8) 0.950 no . . C(18) H(9) 0.950 no . . C(19) H(10) 0.950 no . . C(20) H(11) 0.950 no . . C(21) H(12) 0.950 no . . C(22) H(13) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Fe(1) Cl(1) 180.00(4) yes . . 5_656 Cl(1) Fe(1) N(1) 86.71(8) yes . . . Cl(1) Fe(1) N(1) 93.29(8) yes . . 5_656 Cl(1) Fe(1) N(3) 87.48(8) yes . . . Cl(1) Fe(1) N(3) 92.52(8) yes . . 5_656 Cl(1) Fe(1) N(1) 93.29(8) yes 5_656 . . Cl(1) Fe(1) N(1) 86.71(8) yes 5_656 . 5_656 Cl(1) Fe(1) N(3) 92.52(8) yes 5_656 . . Cl(1) Fe(1) N(3) 87.48(8) yes 5_656 . 5_656 N(1) Fe(1) N(1) 180.00(16) yes . . 5_656 N(1) Fe(1) N(3) 90.02(11) yes . . . N(1) Fe(1) N(3) 89.98(11) yes . . 5_656 N(1) Fe(1) N(3) 89.98(11) yes 5_656 . . N(1) Fe(1) N(3) 90.02(11) yes 5_656 . 5_656 N(3) Fe(1) N(3) 180.00(15) yes . . 5_656 C(17) P(1) C(17) 105.24(15) yes . . 3_555 C(17) P(1) C(17) 111.63(15) yes . . 6_556 C(17) P(1) C(17) 111.63(15) yes . . 8_556 C(17) P(1) C(17) 111.63(15) yes 3_555 . 6_556 C(17) P(1) C(17) 111.63(15) yes 3_555 . 8_556 C(17) P(1) C(17) 105.24(15) yes 6_556 . 8_556 Fe(1) N(1) C(1) 125.7(2) yes . . . Fe(1) N(1) C(10) 126.2(2) yes . . 5_656 C(1) N(1) C(10) 107.6(2) yes . . 5_656 C(1) N(2) C(2) 122.3(2) yes . . . Fe(1) N(3) C(2) 125.9(2) yes . . . Fe(1) N(3) C(9) 125.9(2) yes . . . C(2) N(3) C(9) 108.0(2) yes . . . C(9) N(4) C(10) 122.3(2) yes . . . N(1) C(1) N(2) 127.9(3) yes . . . N(1) C(1) C(16) 109.7(2) yes . . 5_656 N(2) C(1) C(16) 122.3(3) yes . . 5_656 N(2) C(2) N(3) 127.8(3) yes . . . N(2) C(2) C(3) 122.0(3) yes . . . N(3) C(2) C(3) 110.1(2) yes . . . C(2) C(3) C(4) 132.5(3) yes . . . C(2) C(3) C(8) 105.9(2) yes . . . C(4) C(3) C(8) 121.5(3) yes . . . C(3) C(4) C(5) 116.9(3) yes . . . C(4) C(5) C(6) 121.8(3) yes . . . C(5) C(6) C(7) 120.9(3) yes . . . C(6) C(7) C(8) 117.8(3) yes . . . C(3) C(8) C(7) 121.0(3) yes . . . C(3) C(8) C(9) 106.8(2) yes . . . C(7) C(8) C(9) 132.2(3) yes . . . N(3) C(9) N(4) 128.0(3) yes . . . N(3) C(9) C(8) 109.1(2) yes . . . N(4) C(9) C(8) 122.8(2) yes . . . N(1) C(10) N(4) 127.5(3) yes 5_656 . . N(1) C(10) C(11) 109.8(2) yes 5_656 . . N(4) C(10) C(11) 122.8(3) yes . . . C(10) C(11) C(12) 131.7(3) yes . . . C(10) C(11) C(16) 106.8(2) yes . . . C(12) C(11) C(16) 121.4(3) yes . . . C(11) C(12) C(13) 116.9(3) yes . . . C(12) C(13) C(14) 121.7(3) yes . . . C(13) C(14) C(15) 121.2(3) yes . . . C(14) C(15) C(16) 117.6(3) yes . . . C(1) C(16) C(11) 106.2(2) yes 5_656 . . C(1) C(16) C(15) 132.5(3) yes 5_656 . . C(11) C(16) C(15) 121.3(3) yes . . . P(1) C(17) C(18) 121.4(2) yes . . . P(1) C(17) C(22) 118.4(2) yes . . . C(18) C(17) C(22) 119.9(3) yes . . . C(17) C(18) C(19) 119.2(3) yes . . . C(18) C(19) C(20) 120.4(3) yes . . . C(19) C(20) C(21) 120.5(3) yes . . . C(20) C(21) C(22) 119.7(3) yes . . . C(17) C(22) C(21) 120.3(3) yes . . . C(3) C(4) H(1) 121.3 no . . . C(5) C(4) H(1) 121.8 no . . . C(4) C(5) H(2) 119.1 no . . . C(6) C(5) H(2) 119.1 no . . . C(5) C(6) H(3) 119.5 no . . . C(7) C(6) H(3) 119.6 no . . . C(6) C(7) H(4) 121.1 no . . . C(8) C(7) H(4) 121.1 no . . . C(11) C(12) H(5) 121.4 no . . . C(13) C(12) H(5) 121.7 no . . . C(12) C(13) H(6) 119.2 no . . . C(14) C(13) H(6) 119.1 no . . . C(13) C(14) H(7) 119.6 no . . . C(15) C(14) H(7) 119.2 no . . . C(14) C(15) H(8) 121.7 no . . . C(16) C(15) H(8) 120.8 no . . . C(17) C(18) H(9) 120.1 no . . . C(19) C(18) H(9) 120.8 no . . . C(18) C(19) H(10) 119.8 no . . . C(20) C(19) H(10) 119.9 no . . . C(19) C(20) H(11) 119.7 no . . . C(21) C(20) H(11) 119.9 no . . . C(20) C(21) H(12) 120.5 no . . . C(22) C(21) H(12) 119.8 no . . . C(17) C(22) H(13) 119.4 no . . . C(21) C(22) H(13) 120.3 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Fe(1) N(1) C(1) 81.3(2) ? . . . . Cl(1) Fe(1) N(1) C(10) -88.6(2) ? . . . 5_656 Cl(1) Fe(1) N(1) C(1) 98.7(2) ? . . 5_656 5_656 Cl(1) Fe(1) N(1) C(10) -91.4(2) ? . . 5_656 . Cl(1) Fe(1) N(3) C(2) -80.7(2) ? . . . . Cl(1) Fe(1) N(3) C(9) 92.9(2) ? . . . . Cl(1) Fe(1) N(3) C(2) -99.3(2) ? . . 5_656 5_656 Cl(1) Fe(1) N(3) C(9) 87.1(2) ? . . 5_656 5_656 Cl(1) Fe(1) N(1) C(1) -98.7(2) ? 5_656 . . . Cl(1) Fe(1) N(1) C(10) 91.4(2) ? 5_656 . . 5_656 Cl(1) Fe(1) N(1) C(1) -81.3(2) ? 5_656 . 5_656 5_656 Cl(1) Fe(1) N(1) C(10) 88.6(2) ? 5_656 . 5_656 . Cl(1) Fe(1) N(3) C(2) 99.3(2) ? 5_656 . . . Cl(1) Fe(1) N(3) C(9) -87.1(2) ? 5_656 . . . Cl(1) Fe(1) N(3) C(2) 80.7(2) ? 5_656 . 5_656 5_656 Cl(1) Fe(1) N(3) C(9) -92.9(2) ? 5_656 . 5_656 5_656 N(1) Fe(1) N(3) C(2) 6.0(2) ? . . . . N(1) Fe(1) N(3) C(9) 179.6(2) ? . . . . N(3) Fe(1) N(1) C(1) -6.2(2) ? . . . . N(3) Fe(1) N(1) C(10) -176.1(2) ? . . . 5_656 N(1) Fe(1) N(3) C(2) 174.0(2) ? . . 5_656 5_656 N(1) Fe(1) N(3) C(9) 0.4(2) ? . . 5_656 5_656 N(3) Fe(1) N(1) C(1) 173.8(2) ? 5_656 . . . N(3) Fe(1) N(1) C(10) 3.9(2) ? 5_656 . . 5_656 N(1) Fe(1) N(3) C(2) -174.0(2) ? 5_656 . . . N(1) Fe(1) N(3) C(9) -0.4(2) ? 5_656 . . . N(3) Fe(1) N(1) C(1) -173.8(2) ? . . 5_656 5_656 N(3) Fe(1) N(1) C(10) -3.9(2) ? . . 5_656 . N(1) Fe(1) N(3) C(2) -6.0(2) ? 5_656 . 5_656 5_656 N(1) Fe(1) N(3) C(9) -179.6(2) ? 5_656 . 5_656 5_656 N(3) Fe(1) N(1) C(1) 6.2(2) ? 5_656 . 5_656 5_656 N(3) Fe(1) N(1) C(10) 176.1(2) ? 5_656 . 5_656 . C(17) P(1) C(17) C(18) -115.4(3) ? . . 3_555 3_555 C(17) P(1) C(17) C(22) 59.9(3) ? . . 3_555 3_555 C(17) P(1) C(17) C(18) -115.4(3) ? 3_555 . . . C(17) P(1) C(17) C(22) 59.9(3) ? 3_555 . . . C(17) P(1) C(17) C(18) -123.3(3) ? . . 6_556 6_556 C(17) P(1) C(17) C(22) 61.4(3) ? . . 6_556 6_556 C(17) P(1) C(17) C(18) 5.9(3) ? 6_556 . . . C(17) P(1) C(17) C(22) -178.9(2) ? 6_556 . . . C(17) P(1) C(17) C(18) -5.9(3) ? . . 8_556 8_556 C(17) P(1) C(17) C(22) 178.9(2) ? . . 8_556 8_556 C(17) P(1) C(17) C(18) 123.3(3) ? 8_556 . . . C(17) P(1) C(17) C(22) -61.4(3) ? 8_556 . . . C(17) P(1) C(17) C(18) -5.9(3) ? 3_555 . 6_556 6_556 C(17) P(1) C(17) C(22) 178.9(2) ? 3_555 . 6_556 6_556 C(17) P(1) C(17) C(18) 123.3(3) ? 6_556 . 3_555 3_555 C(17) P(1) C(17) C(22) -61.4(3) ? 6_556 . 3_555 3_555 C(17) P(1) C(17) C(18) -123.3(3) ? 3_555 . 8_556 8_556 C(17) P(1) C(17) C(22) 61.4(3) ? 3_555 . 8_556 8_556 C(17) P(1) C(17) C(18) 5.9(3) ? 8_556 . 3_555 3_555 C(17) P(1) C(17) C(22) -178.9(2) ? 8_556 . 3_555 3_555 C(17) P(1) C(17) C(18) 115.4(3) ? 6_556 . 8_556 8_556 C(17) P(1) C(17) C(22) -59.9(3) ? 6_556 . 8_556 8_556 C(17) P(1) C(17) C(18) 115.4(3) ? 8_556 . 6_556 6_556 C(17) P(1) C(17) C(22) -59.9(3) ? 8_556 . 6_556 6_556 Fe(1) N(1) C(1) N(2) 4.2(5) ? . . . . Fe(1) N(1) C(1) C(16) -172.0(2) ? . . . 5_656 Fe(1) N(1) C(10) N(4) -6.9(4) ? . . 5_656 5_656 Fe(1) N(1) C(10) C(11) 171.8(2) ? . . 5_656 5_656 C(1) N(1) C(10) N(4) -178.3(3) ? . . 5_656 5_656 C(1) N(1) C(10) C(11) 0.3(3) ? . . 5_656 5_656 C(10) N(1) C(1) N(2) 175.7(3) ? 5_656 . . . C(10) N(1) C(1) C(16) -0.6(3) ? 5_656 . . 5_656 C(1) N(2) C(2) N(3) -0.9(5) ? . . . . C(1) N(2) C(2) C(3) -179.3(3) ? . . . . C(2) N(2) C(1) N(1) 0.6(5) ? . . . . C(2) N(2) C(1) C(16) 176.5(3) ? . . . 5_656 Fe(1) N(3) C(2) N(2) -3.7(4) ? . . . . Fe(1) N(3) C(2) C(3) 174.8(2) ? . . . . Fe(1) N(3) C(9) N(4) 2.9(4) ? . . . . Fe(1) N(3) C(9) C(8) -175.1(2) ? . . . . C(2) N(3) C(9) N(4) 177.5(3) ? . . . . C(2) N(3) C(9) C(8) -0.5(3) ? . . . . C(9) N(3) C(2) N(2) -178.3(3) ? . . . . C(9) N(3) C(2) C(3) 0.2(3) ? . . . . C(9) N(4) C(10) N(1) -4.1(5) ? . . . 5_656 C(9) N(4) C(10) C(11) 174.4(3) ? . . . . C(10) N(4) C(9) N(3) -1.1(5) ? . . . . C(10) N(4) C(9) C(8) 176.7(3) ? . . . . N(1) C(1) C(16) C(11) 0.6(3) ? . . 5_656 5_656 N(1) C(1) C(16) C(15) 178.5(3) ? . . 5_656 5_656 N(2) C(1) C(16) C(11) -175.9(3) ? . . 5_656 5_656 N(2) C(1) C(16) C(15) 2.0(5) ? . . 5_656 5_656 N(2) C(2) C(3) C(4) -1.1(5) ? . . . . N(2) C(2) C(3) C(8) 178.8(3) ? . . . . N(3) C(2) C(3) C(4) -179.8(3) ? . . . . N(3) C(2) C(3) C(8) 0.2(3) ? . . . . C(2) C(3) C(4) C(5) -178.8(3) ? . . . . C(2) C(3) C(8) C(7) 179.0(3) ? . . . . C(2) C(3) C(8) C(9) -0.5(3) ? . . . . C(4) C(3) C(8) C(7) -1.0(5) ? . . . . C(4) C(3) C(8) C(9) 179.5(3) ? . . . . C(8) C(3) C(4) C(5) 1.2(4) ? . . . . C(3) C(4) C(5) C(6) -0.7(5) ? . . . . C(4) C(5) C(6) C(7) -0.0(5) ? . . . . C(5) C(6) C(7) C(8) 0.3(5) ? . . . . C(6) C(7) C(8) C(3) 0.2(4) ? . . . . C(6) C(7) C(8) C(9) 179.6(3) ? . . . . C(3) C(8) C(9) N(3) 0.6(3) ? . . . . C(3) C(8) C(9) N(4) -177.5(3) ? . . . . C(7) C(8) C(9) N(3) -178.8(3) ? . . . . C(7) C(8) C(9) N(4) 3.1(5) ? . . . . N(1) C(10) C(11) C(12) 177.0(3) ? 5_656 . . . N(1) C(10) C(11) C(16) -0.0(2) ? 5_656 . . . N(4) C(10) C(11) C(12) -1.7(5) ? . . . . N(4) C(10) C(11) C(16) -178.7(3) ? . . . . C(10) C(11) C(12) C(13) -176.7(3) ? . . . . C(10) C(11) C(16) C(1) 0.4(3) ? . . . 5_656 C(10) C(11) C(16) C(15) 178.6(3) ? . . . . C(12) C(11) C(16) C(1) -177.0(3) ? . . . 5_656 C(12) C(11) C(16) C(15) 1.2(5) ? . . . . C(16) C(11) C(12) C(13) -0.0(4) ? . . . . C(11) C(12) C(13) C(14) -0.6(5) ? . . . . C(12) C(13) C(14) C(15) 0.1(4) ? . . . . C(13) C(14) C(15) C(16) 1.0(5) ? . . . . C(14) C(15) C(16) C(1) 176.0(3) ? . . . 5_656 C(14) C(15) C(16) C(11) -1.7(5) ? . . . . P(1) C(17) C(18) C(19) 176.8(2) ? . . . . P(1) C(17) C(22) C(21) -176.7(2) ? . . . . C(18) C(17) C(22) C(21) -1.3(5) ? . . . . C(22) C(17) C(18) C(19) 1.5(5) ? . . . . C(17) C(18) C(19) C(20) -0.7(6) ? . . . . C(18) C(19) C(20) C(21) -0.4(6) ? . . . . C(19) C(20) C(21) C(22) 0.6(6) ? . . . . C(20) C(21) C(22) C(17) 0.2(5) ? . . . . #============================================================================== data__TPP[Fe(Pc)Br2]2 _database_code_depnum_ccdc_archive 'CCDC 699210' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C88 H52 Br4 Fe2 N16 P ' _chemical_formula_moiety 'C88 H52 Br4 Fe2 N16 P ' _chemical_formula_weight 1795.77 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,1/2+X,1/2+Z 3 1/2-X,1/2-Y,+Z 4 1/2+Y,-X,1/2+Z 5 -X,-Y,-Z 6 +Y,1/2-X,1/2-Z 7 1/2+X,1/2+Y,-Z 8 1/2-Y,+X,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 21.410(2) _cell_length_b 21.410(2) _cell_length_c 7.5777(7) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3473.6(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 34218 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1798.00 _exptl_absorpt_coefficient_mu 2.813 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.365 _exptl_absorpt_correction_T_max 0.755 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 31353 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3985 _reflns_number_gt 2673 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1091 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3985 _refine_ls_number_parameters 265 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.5000\s(Fo^2^) + 0.3000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.35 _refine_diff_density_min -1.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br -0.05605(2) -0.09304(2) -0.09372(5) 0.02338(9) Uani 1.00 1 d . . . Fe(1) Fe 0.0000 0.0000 0.0000 0.01070(14) Uani 1.00 2 d S . . P(1) P 0.2500 0.2500 0.2500 0.0141(2) Uani 1.00 4 d S . . N(1) N -0.04226(12) 0.05146(12) -0.1693(3) 0.0157(6) Uani 1.00 1 d . . . N(2) N -0.13741(12) 0.07686(12) -0.0113(3) 0.0161(6) Uani 1.00 1 d . . . N(3) N -0.06770(12) 0.01238(12) 0.1644(3) 0.0157(6) Uani 1.00 1 d . . . N(4) N -0.03500(12) -0.05546(13) 0.4025(3) 0.0169(6) Uani 1.00 1 d . . . C(1) C -0.01856(15) 0.07088(15) -0.3299(4) 0.0161(7) Uani 1.00 1 d . . . C(2) C -0.06202(15) 0.11441(15) -0.4148(4) 0.0157(7) Uani 1.00 1 d . . . C(3) C -0.05936(15) 0.14657(15) -0.5732(4) 0.0183(8) Uani 1.00 1 d . . . C(4) C -0.10994(17) 0.18362(16) -0.6164(4) 0.0210(8) Uani 1.00 1 d . . . C(5) C -0.16163(15) 0.18896(16) -0.5036(4) 0.0204(8) Uani 1.00 1 d . . . C(6) C -0.16349(15) 0.15722(15) -0.3426(4) 0.0177(8) Uani 1.00 1 d . . . C(7) C -0.11315(15) 0.11977(14) -0.3016(4) 0.0156(7) Uani 1.00 1 d . . . C(8) C -0.09929(15) 0.08095(15) -0.1481(4) 0.0158(7) Uani 1.00 1 d . . . C(9) C -0.12236(15) 0.04384(15) 0.1308(4) 0.0150(7) Uani 1.00 1 d . . . C(10) C -0.16584(15) 0.03523(15) 0.2771(4) 0.0157(7) Uani 1.00 1 d . . . C(11) C -0.22685(15) 0.05536(15) 0.3020(4) 0.0172(7) Uani 1.00 1 d . . . C(12) C -0.25686(15) 0.03595(16) 0.4547(4) 0.0196(8) Uani 1.00 1 d . . . C(13) C -0.22641(16) -0.00253(16) 0.5799(4) 0.0202(8) Uani 1.00 1 d . . . C(14) C -0.16556(16) -0.02227(15) 0.5535(4) 0.0185(8) Uani 1.00 1 d . . . C(15) C -0.13605(15) -0.00310(15) 0.3990(4) 0.0167(7) Uani 1.00 1 d . . . C(16) C -0.07453(15) -0.01688(14) 0.3249(4) 0.0153(7) Uani 1.00 1 d . . . C(17) C 0.18578(15) 0.23275(15) 0.3937(4) 0.0167(7) Uani 1.00 1 d . . . C(18) C 0.13149(16) 0.26777(17) 0.3926(4) 0.0221(8) Uani 1.00 1 d . . . C(19) C 0.08477(17) 0.25547(19) 0.5148(5) 0.0272(9) Uani 1.00 1 d . . . C(20) C 0.09205(18) 0.20797(18) 0.6373(4) 0.0267(9) Uani 1.00 1 d . . . C(21) C 0.14679(18) 0.17324(18) 0.6411(4) 0.0255(9) Uani 1.00 1 d . . . C(22) C 0.19372(17) 0.18553(16) 0.5214(4) 0.0211(8) Uani 1.00 1 d . . . H(1) H -0.0237 0.1442 -0.6473 0.022 Uiso 1.00 1 c R . . H(2) H -0.1103 0.2048 -0.7265 0.025 Uiso 1.00 1 c R . . H(3) H -0.1958 0.2145 -0.5378 0.024 Uiso 1.00 1 c R . . H(4) H -0.1974 0.1623 -0.2630 0.021 Uiso 1.00 1 c R . . H(5) H -0.2468 0.0822 0.2196 0.021 Uiso 1.00 1 c R . . H(6) H -0.2989 0.0482 0.4750 0.024 Uiso 1.00 1 c R . . H(7) H -0.2481 -0.0154 0.6831 0.024 Uiso 1.00 1 c R . . H(8) H -0.1443 -0.0472 0.6381 0.022 Uiso 1.00 1 c R . . H(9) H 0.1259 0.2999 0.3074 0.027 Uiso 1.00 1 c R . . H(10) H 0.0475 0.2796 0.5142 0.033 Uiso 1.00 1 c R . . H(11) H 0.0595 0.1991 0.7188 0.032 Uiso 1.00 1 c R . . H(12) H 0.1522 0.1405 0.7243 0.031 Uiso 1.00 1 c R . . H(13) H 0.2319 0.1630 0.5258 0.025 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.02121(19) 0.02139(19) 0.0276(2) 0.00032(14) -0.00011(15) -0.00110(15) Fe(1) 0.0090(2) 0.0111(3) 0.0121(2) 0.0015(2) 0.0015(2) 0.0018(2) P(1) 0.0134(4) 0.0134(4) 0.0157(7) 0.0000 0.0000 0.0000 N(1) 0.0123(12) 0.0180(13) 0.0167(13) 0.0015(10) 0.0023(11) 0.0027(11) N(2) 0.0129(12) 0.0179(13) 0.0176(13) 0.0017(10) 0.0038(11) 0.0017(11) N(3) 0.0160(13) 0.0144(13) 0.0168(13) 0.0004(10) -0.0005(11) 0.0018(11) N(4) 0.0151(13) 0.0179(13) 0.0177(14) 0.0005(11) 0.0036(11) 0.0035(11) C(1) 0.0158(15) 0.0144(15) 0.0181(16) -0.0011(12) 0.0016(13) 0.0009(13) C(2) 0.0148(15) 0.0128(14) 0.0195(16) 0.0006(11) 0.0017(13) 0.0004(13) C(3) 0.0168(15) 0.0191(16) 0.0189(16) -0.0006(13) 0.0040(13) 0.0011(14) C(4) 0.0258(17) 0.0195(16) 0.0176(16) -0.0010(14) 0.0007(14) 0.0044(14) C(5) 0.0184(16) 0.0188(16) 0.0241(17) 0.0038(13) -0.0032(15) 0.0047(15) C(6) 0.0171(15) 0.0164(15) 0.0196(16) -0.0006(12) 0.0003(13) 0.0013(13) C(7) 0.0162(15) 0.0135(14) 0.0170(15) -0.0033(12) 0.0015(13) -0.0012(13) C(8) 0.0152(15) 0.0129(15) 0.0192(16) 0.0006(12) -0.0002(13) 0.0007(13) C(9) 0.0111(14) 0.0142(15) 0.0198(16) 0.0007(11) 0.0009(12) -0.0022(12) C(10) 0.0150(15) 0.0172(15) 0.0149(15) -0.0027(12) 0.0016(13) -0.0024(13) C(11) 0.0189(16) 0.0155(15) 0.0173(16) 0.0012(12) -0.0006(13) -0.0013(13) C(12) 0.0134(15) 0.0215(16) 0.0240(18) 0.0005(12) 0.0036(13) -0.0044(14) C(13) 0.0202(16) 0.0221(17) 0.0185(16) -0.0003(13) 0.0053(14) 0.0011(14) C(14) 0.0201(16) 0.0162(15) 0.0191(16) 0.0006(13) 0.0025(13) 0.0011(13) C(15) 0.0163(15) 0.0142(14) 0.0196(16) -0.0002(12) 0.0029(13) -0.0001(13) C(16) 0.0159(15) 0.0137(15) 0.0164(15) 0.0002(11) 0.0014(12) 0.0002(12) C(17) 0.0143(14) 0.0185(16) 0.0174(16) -0.0007(12) 0.0009(13) -0.0030(13) C(18) 0.0224(17) 0.0235(17) 0.0206(17) 0.0024(14) -0.0026(14) -0.0015(15) C(19) 0.0176(16) 0.037(2) 0.0269(19) 0.0064(15) 0.0011(15) -0.0050(17) C(20) 0.0226(18) 0.036(2) 0.0212(18) -0.0066(15) 0.0060(15) -0.0027(16) C(21) 0.0305(19) 0.0252(19) 0.0207(18) -0.0043(15) 0.0036(15) 0.0014(15) C(22) 0.0216(17) 0.0190(16) 0.0226(17) 0.0009(13) 0.0008(14) 0.0007(14) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Fe(1) 2.4316(4) yes . . Fe(1) N(1) 1.918(2) yes . . Fe(1) N(1) 1.918(2) yes . 5_555 Fe(1) N(3) 1.929(2) yes . . Fe(1) N(3) 1.929(2) yes . 5_555 P(1) C(17) 1.792(3) yes . . P(1) C(17) 1.792(3) yes . 3_555 P(1) C(17) 1.792(3) yes . 6_555 P(1) C(17) 1.792(3) yes . 8_555 N(1) C(1) 1.383(4) yes . . N(1) C(8) 1.384(4) yes . . N(2) C(8) 1.322(4) yes . . N(2) C(9) 1.328(4) yes . . N(3) C(9) 1.374(4) yes . . N(3) C(16) 1.376(4) yes . . N(4) C(1) 1.314(4) yes . 5_555 N(4) C(16) 1.321(4) yes . . C(1) C(2) 1.466(4) yes . . C(2) C(3) 1.385(4) yes . . C(2) C(7) 1.396(4) yes . . C(3) C(4) 1.382(4) yes . . C(4) C(5) 1.403(4) yes . . C(5) C(6) 1.397(4) yes . . C(6) C(7) 1.379(4) yes . . C(7) C(8) 1.460(4) yes . . C(9) C(10) 1.459(4) yes . . C(10) C(11) 1.388(4) yes . . C(10) C(15) 1.391(4) yes . . C(11) C(12) 1.387(4) yes . . C(12) C(13) 1.416(4) yes . . C(13) C(14) 1.384(4) yes . . C(14) C(15) 1.392(4) yes . . C(15) C(16) 1.462(4) yes . . C(17) C(18) 1.383(4) yes . . C(17) C(22) 1.410(4) yes . . C(18) C(19) 1.389(5) yes . . C(19) C(20) 1.385(5) yes . . C(20) C(21) 1.388(5) yes . . C(21) C(22) 1.379(5) yes . . C(3) H(1) 0.950 no . . C(4) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(11) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(18) H(9) 0.950 no . . C(19) H(10) 0.950 no . . C(20) H(11) 0.950 no . . C(21) H(12) 0.950 no . . C(22) H(13) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Fe(1) Br(1) 180.0000 yes . . 5_555 Br(1) Fe(1) N(1) 92.43(7) yes . . . Br(1) Fe(1) N(1) 87.57(7) yes . . 5_555 Br(1) Fe(1) N(3) 86.00(7) yes . . . Br(1) Fe(1) N(3) 94.00(7) yes . . 5_555 Br(1) Fe(1) N(1) 87.57(7) yes 5_555 . . Br(1) Fe(1) N(1) 92.43(7) yes 5_555 . 5_555 Br(1) Fe(1) N(3) 94.00(7) yes 5_555 . . Br(1) Fe(1) N(3) 86.00(7) yes 5_555 . 5_555 N(1) Fe(1) N(1) 180.00(15) yes . . 5_555 N(1) Fe(1) N(3) 89.91(11) yes . . . N(1) Fe(1) N(3) 90.09(11) yes . . 5_555 N(1) Fe(1) N(3) 90.09(11) yes 5_555 . . N(1) Fe(1) N(3) 89.91(11) yes 5_555 . 5_555 N(3) Fe(1) N(3) 180.00(15) yes . . 5_555 C(17) P(1) C(17) 105.19(14) yes . . 3_555 C(17) P(1) C(17) 111.65(14) yes . . 6_555 C(17) P(1) C(17) 111.65(14) yes . . 8_555 C(17) P(1) C(17) 111.65(14) yes 3_555 . 6_555 C(17) P(1) C(17) 111.65(14) yes 3_555 . 8_555 C(17) P(1) C(17) 105.19(14) yes 6_555 . 8_555 Fe(1) N(1) C(1) 126.0(2) yes . . . Fe(1) N(1) C(8) 126.9(2) yes . . . C(1) N(1) C(8) 106.8(2) yes . . . C(8) N(2) C(9) 121.4(2) yes . . . Fe(1) N(3) C(9) 126.0(2) yes . . . Fe(1) N(3) C(16) 126.0(2) yes . . . C(9) N(3) C(16) 107.2(2) yes . . . C(1) N(4) C(16) 122.0(2) yes 5_555 . . N(1) C(1) N(4) 127.8(2) yes . . 5_555 N(1) C(1) C(2) 110.2(2) yes . . . N(4) C(1) C(2) 122.0(3) yes 5_555 . . C(1) C(2) C(3) 132.1(3) yes . . . C(1) C(2) C(7) 106.3(2) yes . . . C(3) C(2) C(7) 121.6(2) yes . . . C(2) C(3) C(4) 117.3(3) yes . . . C(3) C(4) C(5) 121.4(3) yes . . . C(4) C(5) C(6) 121.0(3) yes . . . C(5) C(6) C(7) 117.2(3) yes . . . C(2) C(7) C(6) 121.5(3) yes . . . C(2) C(7) C(8) 106.5(2) yes . . . C(6) C(7) C(8) 132.0(3) yes . . . N(1) C(8) N(2) 127.2(2) yes . . . N(1) C(8) C(7) 110.3(2) yes . . . N(2) C(8) C(7) 122.5(2) yes . . . N(2) C(9) N(3) 128.2(2) yes . . . N(2) C(9) C(10) 121.9(2) yes . . . N(3) C(9) C(10) 109.9(2) yes . . . C(9) C(10) C(11) 131.6(3) yes . . . C(9) C(10) C(15) 106.7(2) yes . . . C(11) C(10) C(15) 121.6(3) yes . . . C(10) C(11) C(12) 117.1(3) yes . . . C(11) C(12) C(13) 121.4(3) yes . . . C(12) C(13) C(14) 120.9(3) yes . . . C(13) C(14) C(15) 117.3(3) yes . . . C(10) C(15) C(14) 121.6(3) yes . . . C(10) C(15) C(16) 106.1(2) yes . . . C(14) C(15) C(16) 132.3(3) yes . . . N(3) C(16) N(4) 127.6(2) yes . . . N(3) C(16) C(15) 110.1(2) yes . . . N(4) C(16) C(15) 122.2(2) yes . . . P(1) C(17) C(18) 122.0(2) yes . . . P(1) C(17) C(22) 118.2(2) yes . . . C(18) C(17) C(22) 119.6(3) yes . . . C(17) C(18) C(19) 119.9(3) yes . . . C(18) C(19) C(20) 120.3(3) yes . . . C(19) C(20) C(21) 120.2(3) yes . . . C(20) C(21) C(22) 119.9(3) yes . . . C(17) C(22) C(21) 120.0(3) yes . . . C(2) C(3) H(1) 121.3 no . . . C(4) C(3) H(1) 121.4 no . . . C(3) C(4) H(2) 119.2 no . . . C(5) C(4) H(2) 119.4 no . . . C(4) C(5) H(3) 119.3 no . . . C(6) C(5) H(3) 119.8 no . . . C(5) C(6) H(4) 121.4 no . . . C(7) C(6) H(4) 121.4 no . . . C(10) C(11) H(5) 121.4 no . . . C(12) C(11) H(5) 121.4 no . . . C(11) C(12) H(6) 119.4 no . . . C(13) C(12) H(6) 119.2 no . . . C(12) C(13) H(7) 119.7 no . . . C(14) C(13) H(7) 119.4 no . . . C(13) C(14) H(8) 121.6 no . . . C(15) C(14) H(8) 121.0 no . . . C(17) C(18) H(9) 120.1 no . . . C(19) C(18) H(9) 120.0 no . . . C(18) C(19) H(10) 119.9 no . . . C(20) C(19) H(10) 119.8 no . . . C(19) C(20) H(11) 119.9 no . . . C(21) C(20) H(11) 119.9 no . . . C(20) C(21) H(12) 120.8 no . . . C(22) C(21) H(12) 119.2 no . . . C(17) C(22) H(13) 119.4 no . . . C(21) C(22) H(13) 120.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Fe(1) N(1) C(1) -100.4(2) ? . . . . Br(1) Fe(1) N(1) C(8) 86.2(2) ? . . . . Br(1) Fe(1) N(1) C(1) -79.6(2) ? . . 5_555 5_555 Br(1) Fe(1) N(1) C(8) 93.8(2) ? . . 5_555 5_555 Br(1) Fe(1) N(3) C(9) -87.7(2) ? . . . . Br(1) Fe(1) N(3) C(16) 81.0(2) ? . . . . Br(1) Fe(1) N(3) C(9) -92.3(2) ? . . 5_555 5_555 Br(1) Fe(1) N(3) C(16) 99.0(2) ? . . 5_555 5_555 Br(1) Fe(1) N(1) C(1) 79.6(2) ? 5_555 . . . Br(1) Fe(1) N(1) C(8) -93.8(2) ? 5_555 . . . Br(1) Fe(1) N(1) C(1) 100.4(2) ? 5_555 . 5_555 5_555 Br(1) Fe(1) N(1) C(8) -86.2(2) ? 5_555 . 5_555 5_555 Br(1) Fe(1) N(3) C(9) 92.3(2) ? 5_555 . . . Br(1) Fe(1) N(3) C(16) -99.0(2) ? 5_555 . . . Br(1) Fe(1) N(3) C(9) 87.7(2) ? 5_555 . 5_555 5_555 Br(1) Fe(1) N(3) C(16) -81.0(2) ? 5_555 . 5_555 5_555 N(1) Fe(1) N(3) C(9) 4.7(2) ? . . . . N(1) Fe(1) N(3) C(16) 173.4(2) ? . . . . N(3) Fe(1) N(1) C(1) 173.6(2) ? . . . . N(3) Fe(1) N(1) C(8) 0.2(2) ? . . . . N(1) Fe(1) N(3) C(9) 175.3(2) ? . . 5_555 5_555 N(1) Fe(1) N(3) C(16) 6.6(2) ? . . 5_555 5_555 N(3) Fe(1) N(1) C(1) -6.4(2) ? 5_555 . . . N(3) Fe(1) N(1) C(8) -179.8(2) ? 5_555 . . . N(1) Fe(1) N(3) C(9) -175.3(2) ? 5_555 . . . N(1) Fe(1) N(3) C(16) -6.6(2) ? 5_555 . . . N(3) Fe(1) N(1) C(1) 6.4(2) ? . . 5_555 5_555 N(3) Fe(1) N(1) C(8) 179.8(2) ? . . 5_555 5_555 N(1) Fe(1) N(3) C(9) -4.7(2) ? 5_555 . 5_555 5_555 N(1) Fe(1) N(3) C(16) -173.4(2) ? 5_555 . 5_555 5_555 N(3) Fe(1) N(1) C(1) -173.6(2) ? 5_555 . 5_555 5_555 N(3) Fe(1) N(1) C(8) -0.2(2) ? 5_555 . 5_555 5_555 C(17) P(1) C(17) C(18) 119.1(2) ? . . 3_555 3_555 C(17) P(1) C(17) C(22) -55.2(2) ? . . 3_555 3_555 C(17) P(1) C(17) C(18) 119.1(2) ? 3_555 . . . C(17) P(1) C(17) C(22) -55.2(2) ? 3_555 . . . C(17) P(1) C(17) C(18) 119.7(2) ? . . 6_555 6_555 C(17) P(1) C(17) C(22) -66.1(3) ? . . 6_555 6_555 C(17) P(1) C(17) C(18) -2.2(3) ? 6_555 . . . C(17) P(1) C(17) C(22) -176.5(2) ? 6_555 . . . C(17) P(1) C(17) C(18) 2.2(3) ? . . 8_555 8_555 C(17) P(1) C(17) C(22) 176.5(2) ? . . 8_555 8_555 C(17) P(1) C(17) C(18) -119.7(2) ? 8_555 . . . C(17) P(1) C(17) C(22) 66.1(2) ? 8_555 . . . C(17) P(1) C(17) C(18) 2.2(3) ? 3_555 . 6_555 6_555 C(17) P(1) C(17) C(22) 176.5(2) ? 3_555 . 6_555 6_555 C(17) P(1) C(17) C(18) -119.7(2) ? 6_555 . 3_555 3_555 C(17) P(1) C(17) C(22) 66.1(2) ? 6_555 . 3_555 3_555 C(17) P(1) C(17) C(18) 119.7(2) ? 3_555 . 8_555 8_555 C(17) P(1) C(17) C(22) -66.1(3) ? 3_555 . 8_555 8_555 C(17) P(1) C(17) C(18) -2.2(3) ? 8_555 . 3_555 3_555 C(17) P(1) C(17) C(22) -176.5(2) ? 8_555 . 3_555 3_555 C(17) P(1) C(17) C(18) -119.1(2) ? 6_555 . 8_555 8_555 C(17) P(1) C(17) C(22) 55.2(2) ? 6_555 . 8_555 8_555 C(17) P(1) C(17) C(18) -119.1(2) ? 8_555 . 6_555 6_555 C(17) P(1) C(17) C(22) 55.2(2) ? 8_555 . 6_555 6_555 Fe(1) N(1) C(1) C(2) -174.6(2) ? . . . . Fe(1) N(1) C(1) N(4) 4.3(4) ? . . . 5_555 Fe(1) N(1) C(8) N(2) -3.9(4) ? . . . . Fe(1) N(1) C(8) C(7) 175.5(2) ? . . . . C(1) N(1) C(8) N(2) -178.4(3) ? . . . . C(1) N(1) C(8) C(7) 1.0(3) ? . . . . C(8) N(1) C(1) C(2) -0.0(3) ? . . . . C(8) N(1) C(1) N(4) 178.8(3) ? . . . 5_555 C(8) N(2) C(9) N(3) 3.0(5) ? . . . . C(8) N(2) C(9) C(10) -175.4(2) ? . . . . C(9) N(2) C(8) N(1) 2.9(5) ? . . . . C(9) N(2) C(8) C(7) -176.4(2) ? . . . . Fe(1) N(3) C(9) N(2) -7.2(4) ? . . . . Fe(1) N(3) C(9) C(10) 171.4(2) ? . . . . Fe(1) N(3) C(16) N(4) 4.7(4) ? . . . . Fe(1) N(3) C(16) C(15) -171.1(2) ? . . . . C(9) N(3) C(16) N(4) 175.2(3) ? . . . . C(9) N(3) C(16) C(15) -0.7(3) ? . . . . C(16) N(3) C(9) N(2) -177.7(3) ? . . . . C(16) N(3) C(9) C(10) 0.9(3) ? . . . . C(1) N(4) C(16) N(3) 0.1(4) ? 5_555 . . . C(1) N(4) C(16) C(15) 175.5(3) ? 5_555 . . . C(16) N(4) C(1) N(1) -0.3(5) ? . . 5_555 5_555 C(16) N(4) C(1) C(2) -179.1(3) ? . . 5_555 5_555 N(1) C(1) C(2) C(3) 179.4(3) ? . . . . N(1) C(1) C(2) C(7) -1.0(3) ? . . . . N(4) C(1) C(2) C(3) 0.4(5) ? 5_555 . . . N(4) C(1) C(2) C(7) -179.9(2) ? 5_555 . . . C(1) C(2) C(3) C(4) 178.6(3) ? . . . . C(1) C(2) C(7) C(6) -179.5(2) ? . . . . C(1) C(2) C(7) C(8) 1.5(3) ? . . . . C(3) C(2) C(7) C(6) 0.2(4) ? . . . . C(3) C(2) C(7) C(8) -178.8(3) ? . . . . C(7) C(2) C(3) C(4) -1.0(4) ? . . . . C(2) C(3) C(4) C(5) 0.6(5) ? . . . . C(3) C(4) C(5) C(6) 0.5(5) ? . . . . C(4) C(5) C(6) C(7) -1.2(4) ? . . . . C(5) C(6) C(7) C(2) 0.9(4) ? . . . . C(5) C(6) C(7) C(8) 179.6(3) ? . . . . C(2) C(7) C(8) N(1) -1.6(3) ? . . . . C(2) C(7) C(8) N(2) 177.8(2) ? . . . . C(6) C(7) C(8) N(1) 179.5(3) ? . . . . C(6) C(7) C(8) N(2) -1.0(5) ? . . . . N(2) C(9) C(10) C(11) 1.5(5) ? . . . . N(2) C(9) C(10) C(15) 177.9(2) ? . . . . N(3) C(9) C(10) C(11) -177.2(3) ? . . . . N(3) C(9) C(10) C(15) -0.8(3) ? . . . . C(9) C(10) C(11) C(12) 176.5(3) ? . . . . C(9) C(10) C(15) C(14) -178.0(3) ? . . . . C(9) C(10) C(15) C(16) 0.3(3) ? . . . . C(11) C(10) C(15) C(14) -1.1(5) ? . . . . C(11) C(10) C(15) C(16) 177.2(2) ? . . . . C(15) C(10) C(11) C(12) 0.4(4) ? . . . . C(10) C(11) C(12) C(13) 0.3(4) ? . . . . C(11) C(12) C(13) C(14) -0.3(5) ? . . . . C(12) C(13) C(14) C(15) -0.4(4) ? . . . . C(13) C(14) C(15) C(10) 1.1(4) ? . . . . C(13) C(14) C(15) C(16) -176.8(3) ? . . . . C(10) C(15) C(16) N(3) 0.2(3) ? . . . . C(10) C(15) C(16) N(4) -175.9(2) ? . . . . C(14) C(15) C(16) N(3) 178.3(3) ? . . . . C(14) C(15) C(16) N(4) 2.2(5) ? . . . . P(1) C(17) C(18) C(19) -175.4(2) ? . . . . P(1) C(17) C(22) C(21) 176.3(2) ? . . . . C(18) C(17) C(22) C(21) 1.9(5) ? . . . . C(22) C(17) C(18) C(19) -1.2(5) ? . . . . C(17) C(18) C(19) C(20) -0.4(5) ? . . . . C(18) C(19) C(20) C(21) 1.5(5) ? . . . . C(19) C(20) C(21) C(22) -0.8(5) ? . . . . C(20) C(21) C(22) C(17) -0.9(5) ? . . . . #============================================================================== data__PNP[Fe(Pc)Cl2]__________________ _database_code_depnum_ccdc_archive 'CCDC 699211' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C68 H46 Cl2 Fe N10 P ' _chemical_formula_moiety 'C68 H46 Cl2 Fe N10 P ' _chemical_formula_weight 1160.91 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.501(6) _cell_length_b 12.232(6) _cell_length_c 12.938(6) _cell_angle_alpha 85.71(3) _cell_angle_beta 68.16(4) _cell_angle_gamma 66.19(4) _cell_volume 1405.7(12) _cell_formula_units_Z 1 _cell_measurement_reflns_used 14503 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 273.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 599.00 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_T_max 0.875 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 13709 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6411 _reflns_number_gt 5140 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1380 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6411 _refine_ls_number_parameters 396 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 7.0000\s(Fo^2^) + 3.0000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.68 _refine_diff_density_min -1.84 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.0000 0.0000 0.0000 0.02135(14) Uani 1.00 2 d S . . Cl(1) Cl 0.01739(9) -0.06023(7) 0.16816(6) 0.03305(19) Uani 1.00 1 d . . . P(1) P -0.00199(9) 0.38776(7) 0.56340(6) 0.02730(19) Uani 1.00 1 d . . . N(1) N 0.1029(2) -0.1655(2) -0.06448(19) 0.0244(6) Uani 1.00 1 d . . . N(2) N 0.3597(2) -0.1836(2) -0.1431(2) 0.0281(6) Uani 1.00 1 d . . . N(3) N 0.1909(2) 0.0141(2) -0.04906(19) 0.0234(5) Uani 1.00 1 d . . . N(4) N 0.1076(2) 0.2216(2) 0.0177(2) 0.0290(6) Uani 1.00 1 d . . . N(5) N 0.0000 0.5000 0.5000 0.0468(12) Uani 1.00 2 d S . . C(1) C 0.2542(3) -0.2246(2) -0.1222(2) 0.0262(7) Uani 1.00 1 d . . . C(2) C 0.3278(3) -0.0729(2) -0.1084(2) 0.0254(7) Uani 1.00 1 d . . . C(3) C 0.4444(3) -0.0280(2) -0.1317(2) 0.0284(7) Uani 1.00 1 d . . . C(4) C 0.5988(3) -0.0813(3) -0.1873(2) 0.0370(8) Uani 1.00 1 d . . . C(5) C 0.6774(3) -0.0109(3) -0.1936(3) 0.0449(10) Uani 1.00 1 d . . . C(6) C 0.6035(3) 0.1082(3) -0.1499(2) 0.0449(10) Uani 1.00 1 d . . . C(7) C 0.4495(3) 0.1622(3) -0.0967(2) 0.0358(8) Uani 1.00 1 d . . . C(8) C 0.3702(3) 0.0913(2) -0.0870(2) 0.0264(7) Uani 1.00 1 d . . . C(9) C 0.2120(3) 0.1154(2) -0.0348(2) 0.0254(7) Uani 1.00 1 d . . . C(10) C -0.0362(3) 0.2425(2) 0.0635(2) 0.0258(7) Uani 1.00 1 d . . . C(11) C -0.1522(3) 0.3566(2) 0.1245(2) 0.0278(7) Uani 1.00 1 d . . . C(12) C -0.1451(4) 0.4637(2) 0.1475(3) 0.0406(9) Uani 1.00 1 d . . . C(13) C -0.2781(4) 0.5568(3) 0.2096(3) 0.0479(10) Uani 1.00 1 d . . . C(14) C -0.4149(4) 0.5443(3) 0.2477(3) 0.0456(9) Uani 1.00 1 d . . . C(15) C -0.4224(3) 0.4387(2) 0.2243(2) 0.0356(8) Uani 1.00 1 d . . . C(16) C -0.2877(3) 0.3447(2) 0.1617(2) 0.0276(7) Uani 1.00 1 d . . . C(17) C -0.1229(3) 0.4312(2) 0.7071(2) 0.0274(7) Uani 1.00 1 d . . . C(18) C -0.1437(3) 0.5383(3) 0.7561(2) 0.0389(9) Uani 1.00 1 d . . . C(19) C -0.2343(4) 0.5745(3) 0.8676(2) 0.0484(10) Uani 1.00 1 d . . . C(20) C -0.3028(4) 0.5031(3) 0.9306(2) 0.0460(9) Uani 1.00 1 d . . . C(21) C -0.2825(3) 0.3970(3) 0.8838(2) 0.0440(9) Uani 1.00 1 d . . . C(22) C -0.1927(3) 0.3604(2) 0.7720(2) 0.0342(8) Uani 1.00 1 d . . . C(23) C 0.1825(3) 0.2889(2) 0.5565(2) 0.0293(7) Uani 1.00 1 d . . . C(24) C 0.2065(4) 0.2215(3) 0.6436(2) 0.0442(9) Uani 1.00 1 d . . . C(25) C 0.3503(4) 0.1474(3) 0.6347(3) 0.0598(12) Uani 1.00 1 d . . . C(26) C 0.4713(4) 0.1401(4) 0.5390(3) 0.0624(13) Uani 1.00 1 d . . . C(27) C 0.4482(4) 0.2046(4) 0.4506(3) 0.0607(12) Uani 1.00 1 d . . . C(28) C 0.3049(3) 0.2801(3) 0.4594(3) 0.0456(10) Uani 1.00 1 d . . . C(29) C -0.0702(3) 0.3055(3) 0.5038(2) 0.0373(9) Uani 1.00 1 d . . . C(30) C 0.0063(4) 0.1845(4) 0.4723(4) 0.0648(14) Uani 1.00 1 d . . . C(31) C -0.0484(5) 0.1275(5) 0.4184(4) 0.0873(18) Uani 1.00 1 d . . . C(32) C -0.1725(6) 0.1901(5) 0.3973(3) 0.0786(18) Uani 1.00 1 d . . . C(33) C -0.2512(6) 0.3098(5) 0.4294(4) 0.084(2) Uani 1.00 1 d . . . C(34) C -0.1989(5) 0.3693(4) 0.4821(4) 0.0672(16) Uani 1.00 1 d . . . H(1) H 0.6482 -0.1619 -0.2194 0.042 Uiso 1.00 1 c R . . H(2) H 0.7837 -0.0448 -0.2284 0.052 Uiso 1.00 1 c R . . H(3) H 0.6600 0.1543 -0.1566 0.055 Uiso 1.00 1 c R . . H(4) H 0.3993 0.2442 -0.0682 0.044 Uiso 1.00 1 c R . . H(5) H -0.0521 0.4714 0.1217 0.050 Uiso 1.00 1 c R . . H(6) H -0.2770 0.6307 0.2264 0.057 Uiso 1.00 1 c R . . H(7) H -0.5044 0.6096 0.2907 0.048 Uiso 1.00 1 c R . . H(8) H -0.5151 0.4305 0.2491 0.038 Uiso 1.00 1 c R . . H(10) H -0.0945 0.5858 0.7120 0.047 Uiso 1.00 1 c R . . H(11) H -0.2482 0.6475 0.9004 0.055 Uiso 1.00 1 c R . . H(12) H -0.3657 0.5280 1.0070 0.048 Uiso 1.00 1 c R . . H(13) H -0.3296 0.3484 0.9281 0.050 Uiso 1.00 1 c R . . H(14) H -0.1790 0.2876 0.7391 0.039 Uiso 1.00 1 c R . . H(15) H 0.1227 0.2266 0.7090 0.048 Uiso 1.00 1 c R . . H(16) H 0.3665 0.1016 0.6947 0.065 Uiso 1.00 1 c R . . H(17) H 0.5707 0.0903 0.5335 0.070 Uiso 1.00 1 c R . . H(18) H 0.5312 0.1977 0.3839 0.065 Uiso 1.00 1 c R . . H(19) H 0.2884 0.3258 0.3994 0.052 Uiso 1.00 1 c R . . H(20) H 0.0947 0.1397 0.4869 0.076 Uiso 1.00 1 c R . . H(21) H 0.0026 0.0436 0.3976 0.102 Uiso 1.00 1 c R . . H(22) H -0.2047 0.1504 0.3581 0.099 Uiso 1.00 1 c R . . H(23) H -0.3419 0.3526 0.4173 0.117 Uiso 1.00 1 c R . . H(24) H -0.2511 0.4532 0.5030 0.091 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0204(3) 0.0205(2) 0.0209(2) -0.0096(2) -0.0035(2) -0.0007(2) Cl(1) 0.0389(4) 0.0348(4) 0.0276(3) -0.0172(3) -0.0130(3) 0.0063(3) P(1) 0.0318(4) 0.0305(4) 0.0186(3) -0.0159(3) -0.0052(3) 0.0045(3) N(1) 0.0237(12) 0.0234(12) 0.0246(11) -0.0126(10) -0.0034(10) -0.0023(9) N(2) 0.0248(13) 0.0262(12) 0.0267(12) -0.0106(10) -0.0017(10) -0.0013(10) N(3) 0.0231(12) 0.0239(11) 0.0228(11) -0.0122(9) -0.0048(9) 0.0012(9) N(4) 0.0261(13) 0.0272(12) 0.0308(12) -0.0128(10) -0.0043(10) -0.0036(10) N(5) 0.050(2) 0.037(2) 0.042(2) -0.0192(19) -0.0061(19) 0.0205(19) C(1) 0.0252(14) 0.0248(14) 0.0253(13) -0.0101(11) -0.0057(11) 0.0003(11) C(2) 0.0222(14) 0.0273(14) 0.0241(13) -0.0116(11) -0.0040(11) 0.0002(11) C(3) 0.0236(15) 0.0333(16) 0.0271(14) -0.0149(12) -0.0044(11) 0.0026(12) C(4) 0.0273(17) 0.0384(18) 0.0378(17) -0.0141(14) -0.0025(14) -0.0032(14) C(5) 0.0274(18) 0.057(2) 0.045(2) -0.0235(16) -0.0002(15) -0.0009(17) C(6) 0.0354(19) 0.059(2) 0.0430(19) -0.0323(17) -0.0015(15) -0.0032(17) C(7) 0.0362(18) 0.0399(18) 0.0347(16) -0.0248(15) -0.0057(14) -0.0013(14) C(8) 0.0262(15) 0.0299(15) 0.0229(13) -0.0158(12) -0.0039(11) 0.0009(11) C(9) 0.0246(15) 0.0252(14) 0.0280(14) -0.0130(12) -0.0080(11) -0.0003(11) C(10) 0.0269(15) 0.0234(14) 0.0270(14) -0.0115(12) -0.0077(12) -0.0025(11) C(11) 0.0292(16) 0.0239(14) 0.0281(14) -0.0096(12) -0.0090(12) -0.0027(11) C(12) 0.043(2) 0.0307(17) 0.050(2) -0.0176(15) -0.0153(16) -0.0070(15) C(13) 0.057(2) 0.0292(17) 0.058(2) -0.0144(16) -0.0219(19) -0.0102(16) C(14) 0.044(2) 0.0306(17) 0.046(2) -0.0045(15) -0.0074(16) -0.0127(15) C(15) 0.0291(17) 0.0295(16) 0.0365(17) -0.0062(13) -0.0047(14) -0.0052(13) C(16) 0.0289(15) 0.0248(14) 0.0249(13) -0.0089(12) -0.0070(12) -0.0024(11) C(17) 0.0294(16) 0.0300(15) 0.0238(13) -0.0144(12) -0.0087(12) 0.0044(12) C(18) 0.052(2) 0.0417(18) 0.0239(14) -0.0261(16) -0.0059(14) -0.0022(13) C(19) 0.063(2) 0.047(2) 0.0286(16) -0.0221(18) -0.0082(16) -0.0093(15) C(20) 0.041(2) 0.054(2) 0.0236(15) -0.0107(17) 0.0001(14) -0.0047(15) C(21) 0.044(2) 0.057(2) 0.0240(15) -0.0256(17) 0.0004(14) 0.0060(15) C(22) 0.0384(18) 0.0342(16) 0.0253(14) -0.0176(14) -0.0042(13) 0.0052(13) C(23) 0.0326(16) 0.0299(15) 0.0228(13) -0.0137(13) -0.0057(12) -0.0016(12) C(24) 0.050(2) 0.0407(19) 0.0286(16) -0.0095(16) -0.0109(15) 0.0079(14) C(25) 0.060(2) 0.056(2) 0.046(2) -0.000(2) -0.028(2) 0.0088(19) C(26) 0.042(2) 0.068(2) 0.065(2) -0.008(2) -0.022(2) -0.002(2) C(27) 0.034(2) 0.071(2) 0.058(2) -0.017(2) -0.0011(18) 0.002(2) C(28) 0.0316(18) 0.059(2) 0.0385(18) -0.0192(17) -0.0053(15) 0.0096(17) C(29) 0.0384(18) 0.053(2) 0.0220(14) -0.0247(16) -0.0048(13) -0.0012(14) C(30) 0.041(2) 0.065(2) 0.083(3) -0.021(2) -0.013(2) -0.029(2) C(31) 0.060(3) 0.102(4) 0.092(3) -0.045(3) 0.006(2) -0.058(3) C(32) 0.071(3) 0.132(5) 0.046(2) -0.064(3) -0.004(2) -0.030(2) C(33) 0.091(4) 0.110(4) 0.091(3) -0.052(3) -0.064(3) 0.018(3) C(34) 0.082(3) 0.072(3) 0.074(3) -0.037(2) -0.053(2) 0.017(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) Cl(1) 2.2927(8) yes . . Fe(1) Cl(1) 2.2927(8) yes . 2_555 Fe(1) N(1) 1.943(2) yes . . Fe(1) N(1) 1.943(2) yes . 2_555 Fe(1) N(3) 1.941(2) yes . . Fe(1) N(3) 1.941(2) yes . 2_555 P(1) N(5) 1.5492(8) yes . . P(1) C(17) 1.788(2) yes . . P(1) C(23) 1.794(3) yes . . P(1) C(29) 1.797(4) yes . . N(1) C(1) 1.370(3) yes . . N(1) C(10) 1.379(4) yes . 2_555 N(2) C(1) 1.326(4) yes . . N(2) C(2) 1.326(4) yes . . N(3) C(2) 1.363(2) yes . . N(3) C(9) 1.380(4) yes . . N(4) C(9) 1.333(3) yes . . N(4) C(10) 1.320(4) yes . . C(1) C(16) 1.451(4) yes . 2_555 C(2) C(3) 1.462(5) yes . . C(3) C(4) 1.385(4) yes . . C(3) C(8) 1.394(4) yes . . C(4) C(5) 1.394(6) yes . . C(5) C(6) 1.389(5) yes . . C(6) C(7) 1.380(4) yes . . C(7) C(8) 1.397(6) yes . . C(8) C(9) 1.450(4) yes . . C(10) C(11) 1.460(3) yes . . C(11) C(12) 1.401(5) yes . . C(11) C(16) 1.387(5) yes . . C(12) C(13) 1.383(4) yes . . C(13) C(14) 1.403(6) yes . . C(14) C(15) 1.387(6) yes . . C(15) C(16) 1.397(3) yes . . C(17) C(18) 1.399(5) yes . . C(17) C(22) 1.393(4) yes . . C(18) C(19) 1.384(4) yes . . C(19) C(20) 1.382(6) yes . . C(20) C(21) 1.377(6) yes . . C(21) C(22) 1.387(4) yes . . C(23) C(24) 1.385(4) yes . . C(23) C(28) 1.396(4) yes . . C(24) C(25) 1.377(5) yes . . C(25) C(26) 1.383(5) yes . . C(26) C(27) 1.381(6) yes . . C(27) C(28) 1.377(5) yes . . C(29) C(30) 1.374(5) yes . . C(29) C(34) 1.384(6) yes . . C(30) C(31) 1.413(9) yes . . C(31) C(32) 1.337(8) yes . . C(32) C(33) 1.363(8) yes . . C(33) C(34) 1.404(10) yes . . C(4) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(13) H(6) 0.950 no . . C(14) H(7) 0.950 no . . C(15) H(8) 0.950 no . . C(18) H(10) 0.950 no . . C(19) H(11) 0.950 no . . C(20) H(12) 0.950 no . . C(21) H(13) 0.950 no . . C(22) H(14) 0.950 no . . C(24) H(15) 0.950 no . . C(25) H(16) 0.950 no . . C(26) H(17) 0.950 no . . C(27) H(18) 0.950 no . . C(28) H(19) 0.950 no . . C(30) H(20) 0.950 no . . C(31) H(21) 0.950 no . . C(32) H(22) 0.950 no . . C(33) H(23) 0.950 no . . C(34) H(24) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Fe(1) Cl(1) 180.00(4) yes . . 2_555 Cl(1) Fe(1) N(1) 90.81(7) yes . . . Cl(1) Fe(1) N(1) 89.19(7) yes . . 2_555 Cl(1) Fe(1) N(3) 91.07(7) yes . . . Cl(1) Fe(1) N(3) 88.93(7) yes . . 2_555 Cl(1) Fe(1) N(1) 89.19(7) yes 2_555 . . Cl(1) Fe(1) N(1) 90.81(7) yes 2_555 . 2_555 Cl(1) Fe(1) N(3) 88.93(7) yes 2_555 . . Cl(1) Fe(1) N(3) 91.07(7) yes 2_555 . 2_555 N(1) Fe(1) N(1) 180.00(15) yes . . 2_555 N(1) Fe(1) N(3) 90.15(10) yes . . . N(1) Fe(1) N(3) 89.85(10) yes . . 2_555 N(1) Fe(1) N(3) 89.85(10) yes 2_555 . . N(1) Fe(1) N(3) 90.15(10) yes 2_555 . 2_555 N(3) Fe(1) N(3) 180.00(14) yes . . 2_555 N(5) P(1) C(17) 110.29(10) yes . . . N(5) P(1) C(23) 111.31(12) yes . . . N(5) P(1) C(29) 110.50(12) yes . . . C(17) P(1) C(23) 108.60(14) yes . . . C(17) P(1) C(29) 108.09(16) yes . . . C(23) P(1) C(29) 107.97(16) yes . . . Fe(1) N(1) C(1) 125.7(2) yes . . . Fe(1) N(1) C(10) 126.16(16) yes . . 2_555 C(1) N(1) C(10) 108.1(2) yes . . 2_555 C(1) N(2) C(2) 122.0(2) yes . . . Fe(1) N(3) C(2) 126.0(2) yes . . . Fe(1) N(3) C(9) 126.36(15) yes . . . C(2) N(3) C(9) 107.6(2) yes . . . C(9) N(4) C(10) 122.0(3) yes . . . P(1) N(5) P(1) 180.00(0) yes . . 2_566 N(1) C(1) N(2) 128.0(2) yes . . . N(1) C(1) C(16) 109.6(3) yes . . 2_555 N(2) C(1) C(16) 122.4(2) yes . . 2_555 N(2) C(2) N(3) 128.1(3) yes . . . N(2) C(2) C(3) 121.9(2) yes . . . N(3) C(2) C(3) 110.0(2) yes . . . C(2) C(3) C(4) 132.0(3) yes . . . C(2) C(3) C(8) 106.0(2) yes . . . C(4) C(3) C(8) 121.9(3) yes . . . C(3) C(4) C(5) 116.7(3) yes . . . C(4) C(5) C(6) 121.4(3) yes . . . C(5) C(6) C(7) 121.9(4) yes . . . C(6) C(7) C(8) 117.1(3) yes . . . C(3) C(8) C(7) 120.9(2) yes . . . C(3) C(8) C(9) 106.6(3) yes . . . C(7) C(8) C(9) 132.4(2) yes . . . N(3) C(9) N(4) 127.5(2) yes . . . N(3) C(9) C(8) 109.7(2) yes . . . N(4) C(9) C(8) 122.8(3) yes . . . N(1) C(10) N(4) 128.0(2) yes 2_555 . . N(1) C(10) C(11) 108.8(2) yes 2_555 . . N(4) C(10) C(11) 123.1(3) yes . . . C(10) C(11) C(12) 131.9(3) yes . . . C(10) C(11) C(16) 106.8(3) yes . . . C(12) C(11) C(16) 121.3(2) yes . . . C(11) C(12) C(13) 117.5(3) yes . . . C(12) C(13) C(14) 121.0(4) yes . . . C(13) C(14) C(15) 121.6(2) yes . . . C(14) C(15) C(16) 117.2(3) yes . . . C(1) C(16) C(11) 106.7(2) yes 2_555 . . C(1) C(16) C(15) 132.0(3) yes 2_555 . . C(11) C(16) C(15) 121.4(3) yes . . . P(1) C(17) C(18) 118.4(2) yes . . . P(1) C(17) C(22) 122.2(2) yes . . . C(18) C(17) C(22) 119.3(2) yes . . . C(17) C(18) C(19) 120.5(3) yes . . . C(18) C(19) C(20) 119.4(4) yes . . . C(19) C(20) C(21) 120.9(2) yes . . . C(20) C(21) C(22) 120.2(3) yes . . . C(17) C(22) C(21) 119.8(3) yes . . . P(1) C(23) C(24) 122.2(2) yes . . . P(1) C(23) C(28) 118.3(2) yes . . . C(24) C(23) C(28) 119.5(3) yes . . . C(23) C(24) C(25) 120.1(3) yes . . . C(24) C(25) C(26) 120.2(4) yes . . . C(25) C(26) C(27) 120.1(3) yes . . . C(26) C(27) C(28) 120.0(3) yes . . . C(23) C(28) C(27) 120.1(3) yes . . . P(1) C(29) C(30) 122.4(3) yes . . . P(1) C(29) C(34) 117.8(3) yes . . . C(30) C(29) C(34) 119.5(4) yes . . . C(29) C(30) C(31) 119.3(4) yes . . . C(30) C(31) C(32) 120.7(5) yes . . . C(31) C(32) C(33) 120.9(7) yes . . . C(32) C(33) C(34) 119.8(5) yes . . . C(29) C(34) C(33) 119.8(4) yes . . . C(3) C(4) H(1) 121.4 no . . . C(5) C(4) H(1) 121.9 no . . . C(4) C(5) H(2) 119.5 no . . . C(6) C(5) H(2) 119.1 no . . . C(5) C(6) H(3) 119.5 no . . . C(7) C(6) H(3) 118.6 no . . . C(6) C(7) H(4) 121.6 no . . . C(8) C(7) H(4) 121.4 no . . . C(11) C(12) H(5) 121.0 no . . . C(13) C(12) H(5) 121.5 no . . . C(12) C(13) H(6) 119.5 no . . . C(14) C(13) H(6) 119.5 no . . . C(13) C(14) H(7) 119.2 no . . . C(15) C(14) H(7) 119.2 no . . . C(14) C(15) H(8) 121.6 no . . . C(16) C(15) H(8) 121.2 no . . . C(17) C(18) H(10) 119.2 no . . . C(19) C(18) H(10) 120.4 no . . . C(18) C(19) H(11) 120.1 no . . . C(20) C(19) H(11) 120.5 no . . . C(19) C(20) H(12) 119.6 no . . . C(21) C(20) H(12) 119.6 no . . . C(20) C(21) H(13) 120.1 no . . . C(22) C(21) H(13) 119.7 no . . . C(17) C(22) H(14) 119.6 no . . . C(21) C(22) H(14) 120.5 no . . . C(23) C(24) H(15) 119.2 no . . . C(25) C(24) H(15) 120.7 no . . . C(24) C(25) H(16) 119.9 no . . . C(26) C(25) H(16) 119.8 no . . . C(25) C(26) H(17) 120.2 no . . . C(27) C(26) H(17) 119.7 no . . . C(26) C(27) H(18) 120.0 no . . . C(28) C(27) H(18) 119.9 no . . . C(23) C(28) H(19) 119.5 no . . . C(27) C(28) H(19) 120.4 no . . . C(29) C(30) H(20) 120.3 no . . . C(31) C(30) H(20) 120.4 no . . . C(30) C(31) H(21) 120.0 no . . . C(32) C(31) H(21) 119.3 no . . . C(31) C(32) H(22) 119.2 no . . . C(33) C(32) H(22) 120.0 no . . . C(32) C(33) H(23) 120.2 no . . . C(34) C(33) H(23) 120.0 no . . . C(29) C(34) H(24) 119.6 no . . . C(33) C(34) H(24) 120.7 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Fe(1) N(1) C(1) -93.2(2) ? . . . . Cl(1) Fe(1) N(1) C(10) 89.1(2) ? . . . 2_555 Cl(1) Fe(1) N(1) C(1) -86.8(2) ? . . 2_555 2_555 Cl(1) Fe(1) N(1) C(10) 90.9(2) ? . . 2_555 . Cl(1) Fe(1) N(3) C(2) 92.6(2) ? . . . . Cl(1) Fe(1) N(3) C(9) -90.6(2) ? . . . . Cl(1) Fe(1) N(3) C(2) 87.4(2) ? . . 2_555 2_555 Cl(1) Fe(1) N(3) C(9) -89.4(2) ? . . 2_555 2_555 Cl(1) Fe(1) N(1) C(1) 86.8(2) ? 2_555 . . . Cl(1) Fe(1) N(1) C(10) -90.9(2) ? 2_555 . . 2_555 Cl(1) Fe(1) N(1) C(1) 93.2(2) ? 2_555 . 2_555 2_555 Cl(1) Fe(1) N(1) C(10) -89.1(2) ? 2_555 . 2_555 . Cl(1) Fe(1) N(3) C(2) -87.4(2) ? 2_555 . . . Cl(1) Fe(1) N(3) C(9) 89.4(2) ? 2_555 . . . Cl(1) Fe(1) N(3) C(2) -92.6(2) ? 2_555 . 2_555 2_555 Cl(1) Fe(1) N(3) C(9) 90.6(2) ? 2_555 . 2_555 2_555 N(1) Fe(1) N(3) C(2) 1.8(2) ? . . . . N(1) Fe(1) N(3) C(9) 178.6(2) ? . . . . N(3) Fe(1) N(1) C(1) -2.2(2) ? . . . . N(3) Fe(1) N(1) C(10) -179.8(2) ? . . . 2_555 N(1) Fe(1) N(3) C(2) 178.2(2) ? . . 2_555 2_555 N(1) Fe(1) N(3) C(9) 1.4(2) ? . . 2_555 2_555 N(3) Fe(1) N(1) C(1) 177.8(2) ? 2_555 . . . N(3) Fe(1) N(1) C(10) 0.2(2) ? 2_555 . . 2_555 N(1) Fe(1) N(3) C(2) -178.2(2) ? 2_555 . . . N(1) Fe(1) N(3) C(9) -1.4(2) ? 2_555 . . . N(3) Fe(1) N(1) C(1) -177.8(2) ? . . 2_555 2_555 N(3) Fe(1) N(1) C(10) -0.2(2) ? . . 2_555 . N(1) Fe(1) N(3) C(2) -1.8(2) ? 2_555 . 2_555 2_555 N(1) Fe(1) N(3) C(9) -178.6(2) ? 2_555 . 2_555 2_555 N(3) Fe(1) N(1) C(1) 2.2(2) ? 2_555 . 2_555 2_555 N(3) Fe(1) N(1) C(10) 179.8(2) ? 2_555 . 2_555 . N(5) P(1) C(17) C(18) -28.0(3) ? . . . . N(5) P(1) C(17) C(22) 154.0(2) ? . . . . N(5) P(1) C(23) C(24) 146.2(3) ? . . . . N(5) P(1) C(23) C(28) -34.2(3) ? . . . . N(5) P(1) C(29) C(30) 128.4(3) ? . . . . N(5) P(1) C(29) C(34) -46.8(3) ? . . . . C(17) P(1) C(23) C(24) 24.6(4) ? . . . . C(17) P(1) C(23) C(28) -155.8(3) ? . . . . C(23) P(1) C(17) C(18) 94.2(3) ? . . . . C(23) P(1) C(17) C(22) -83.7(3) ? . . . . C(17) P(1) C(29) C(30) -110.8(3) ? . . . . C(17) P(1) C(29) C(34) 74.0(3) ? . . . . C(29) P(1) C(17) C(18) -148.9(2) ? . . . . C(29) P(1) C(17) C(22) 33.1(3) ? . . . . C(23) P(1) C(29) C(30) 6.5(3) ? . . . . C(23) P(1) C(29) C(34) -168.7(2) ? . . . . C(29) P(1) C(23) C(24) -92.4(3) ? . . . . C(29) P(1) C(23) C(28) 87.3(3) ? . . . . Fe(1) N(1) C(1) N(2) 2.0(4) ? . . . . Fe(1) N(1) C(1) C(16) -177.3(2) ? . . . 2_555 Fe(1) N(1) C(10) N(4) -1.6(4) ? . . 2_555 2_555 Fe(1) N(1) C(10) C(11) 177.8(2) ? . . 2_555 2_555 C(1) N(1) C(10) N(4) -179.6(3) ? . . 2_555 2_555 C(1) N(1) C(10) C(11) -0.2(3) ? . . 2_555 2_555 C(10) N(1) C(1) N(2) 179.9(2) ? 2_555 . . . C(10) N(1) C(1) C(16) 0.7(3) ? 2_555 . . 2_555 C(1) N(2) C(2) N(3) 0.0(4) ? . . . . C(1) N(2) C(2) C(3) -179.9(2) ? . . . . C(2) N(2) C(1) N(1) -0.5(5) ? . . . . C(2) N(2) C(1) C(16) 178.7(2) ? . . . 2_555 Fe(1) N(3) C(2) N(2) -1.1(4) ? . . . . Fe(1) N(3) C(2) C(3) 178.8(2) ? . . . . Fe(1) N(3) C(9) N(4) 2.1(4) ? . . . . Fe(1) N(3) C(9) C(8) -177.7(2) ? . . . . C(2) N(3) C(9) N(4) 179.4(3) ? . . . . C(2) N(3) C(9) C(8) -0.4(3) ? . . . . C(9) N(3) C(2) N(2) -178.4(3) ? . . . . C(9) N(3) C(2) C(3) 1.5(3) ? . . . . C(9) N(4) C(10) N(1) -1.3(5) ? . . . 2_555 C(9) N(4) C(10) C(11) 178.0(3) ? . . . . C(10) N(4) C(9) N(3) -0.6(5) ? . . . . C(10) N(4) C(9) C(8) 179.1(3) ? . . . . N(1) C(1) C(16) C(11) -0.9(3) ? . . 2_555 2_555 N(1) C(1) C(16) C(15) 179.4(3) ? . . 2_555 2_555 N(2) C(1) C(16) C(11) 179.8(3) ? . . 2_555 2_555 N(2) C(1) C(16) C(15) 0.1(4) ? . . 2_555 2_555 N(2) C(2) C(3) C(4) -0.9(5) ? . . . . N(2) C(2) C(3) C(8) 177.9(2) ? . . . . N(3) C(2) C(3) C(4) 179.2(3) ? . . . . N(3) C(2) C(3) C(8) -2.0(3) ? . . . . C(2) C(3) C(4) C(5) -179.7(3) ? . . . . C(2) C(3) C(8) C(7) -178.8(3) ? . . . . C(2) C(3) C(8) C(9) 1.7(3) ? . . . . C(4) C(3) C(8) C(7) 0.1(3) ? . . . . C(4) C(3) C(8) C(9) -179.4(3) ? . . . . C(8) C(3) C(4) C(5) 1.8(5) ? . . . . C(3) C(4) C(5) C(6) -2.3(5) ? . . . . C(4) C(5) C(6) C(7) 1.0(6) ? . . . . C(5) C(6) C(7) C(8) 0.9(5) ? . . . . C(6) C(7) C(8) C(3) -1.5(5) ? . . . . C(6) C(7) C(8) C(9) 177.9(3) ? . . . . C(3) C(8) C(9) N(3) -0.9(3) ? . . . . C(3) C(8) C(9) N(4) 179.3(3) ? . . . . C(7) C(8) C(9) N(3) 179.7(3) ? . . . . C(7) C(8) C(9) N(4) -0.1(4) ? . . . . N(1) C(10) C(11) C(12) -179.6(3) ? 2_555 . . . N(1) C(10) C(11) C(16) 0.4(3) ? 2_555 . . . N(4) C(10) C(11) C(12) 0.9(5) ? . . . . N(4) C(10) C(11) C(16) -179.0(3) ? . . . . C(10) C(11) C(12) C(13) -179.4(3) ? . . . . C(10) C(11) C(16) C(1) -0.8(3) ? . . . 2_555 C(10) C(11) C(16) C(15) 179.5(3) ? . . . . C(12) C(11) C(16) C(1) 179.3(3) ? . . . 2_555 C(12) C(11) C(16) C(15) -0.5(5) ? . . . . C(16) C(11) C(12) C(13) 0.6(5) ? . . . . C(11) C(12) C(13) C(14) -0.2(5) ? . . . . C(12) C(13) C(14) C(15) -0.2(5) ? . . . . C(13) C(14) C(15) C(16) 0.4(5) ? . . . . C(14) C(15) C(16) C(1) -179.7(3) ? . . . 2_555 C(14) C(15) C(16) C(11) -0.0(4) ? . . . . P(1) C(17) C(18) C(19) -178.9(3) ? . . . . P(1) C(17) C(22) C(21) 178.4(2) ? . . . . C(18) C(17) C(22) C(21) 0.5(5) ? . . . . C(22) C(17) C(18) C(19) -0.9(5) ? . . . . C(17) C(18) C(19) C(20) 0.8(6) ? . . . . C(18) C(19) C(20) C(21) -0.2(5) ? . . . . C(19) C(20) C(21) C(22) -0.2(5) ? . . . . C(20) C(21) C(22) C(17) 0.1(4) ? . . . . P(1) C(23) C(24) C(25) -179.6(3) ? . . . . P(1) C(23) C(28) C(27) -179.6(3) ? . . . . C(24) C(23) C(28) C(27) 0.1(5) ? . . . . C(28) C(23) C(24) C(25) 0.7(6) ? . . . . C(23) C(24) C(25) C(26) 0.1(5) ? . . . . C(24) C(25) C(26) C(27) -1.8(8) ? . . . . C(25) C(26) C(27) C(28) 2.6(8) ? . . . . C(26) C(27) C(28) C(23) -1.8(7) ? . . . . P(1) C(29) C(30) C(31) -175.3(3) ? . . . . P(1) C(29) C(34) C(33) 176.2(3) ? . . . . C(30) C(29) C(34) C(33) 0.8(6) ? . . . . C(34) C(29) C(30) C(31) -0.2(5) ? . . . . C(29) C(30) C(31) C(32) 0.6(7) ? . . . . C(30) C(31) C(32) C(33) -1.5(8) ? . . . . C(31) C(32) C(33) C(34) 2.1(8) ? . . . . C(32) C(33) C(34) C(29) -1.8(7) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(22) 3.556(3) ? . 2_556 C(3) C(7) 3.595(4) ? . 2_655 C(5) C(8) 3.593(4) ? . 2_655 C(5) C(9) 3.536(5) ? . 2_655 C(7) C(3) 3.595(4) ? . 2_655 C(8) C(5) 3.593(4) ? . 2_655 C(9) C(5) 3.536(5) ? . 2_655 C(11) C(20) 3.464(5) ? . 1_554 C(16) C(20) 3.458(4) ? . 1_554 C(16) C(21) 3.589(4) ? . 1_554 C(16) C(33) 3.599(7) ? . . C(20) C(11) 3.464(5) ? . 1_556 C(20) C(16) 3.458(4) ? . 1_556 C(21) C(16) 3.589(4) ? . 1_556 C(22) Cl(1) 3.556(3) ? . 2_556 C(26) C(26) 3.395(7) ? . 2_656 C(33) C(16) 3.599(7) ? . . Cl(1) H(2) 3.186 ? . 2_655 Cl(1) H(3) 3.054 ? . 2_655 Cl(1) H(14) 3.043 ? . 2_556 Cl(1) H(15) 3.004 ? . 2_556 Cl(1) H(21) 3.241 ? . . Cl(1) H(22) 3.154 ? . . N(1) H(13) 3.468 ? . 2_556 N(1) H(22) 3.555 ? . 2_555 N(2) H(13) 3.304 ? . 2_556 N(2) H(18) 2.884 ? . 2_655 N(3) H(16) 3.471 ? . 1_554 N(4) H(2) 3.585 ? . 2_655 N(4) H(11) 3.033 ? . 2_566 C(1) H(13) 3.029 ? . 2_556 C(1) H(18) 3.377 ? . 2_655 C(1) H(22) 3.285 ? . 2_555 C(2) H(3) 3.532 ? . 2_655 C(2) H(16) 3.213 ? . 1_554 C(2) H(18) 3.506 ? . 2_655 C(3) H(16) 2.830 ? . 1_554 C(4) H(11) 3.371 ? . 1_644 C(4) H(16) 3.338 ? . 1_554 C(5) H(21) 3.301 ? . 2_655 C(6) H(13) 3.574 ? . 1_654 C(7) H(6) 3.230 ? . 2_565 C(7) H(11) 3.042 ? . 2_566 C(7) H(16) 3.341 ? . 1_554 C(8) H(16) 2.832 ? . 1_554 C(9) H(2) 3.462 ? . 2_655 C(9) H(16) 3.249 ? . 1_554 C(11) H(12) 3.162 ? . 1_554 C(11) H(23) 3.572 ? . . C(12) H(5) 3.549 ? . 2_565 C(12) H(10) 3.466 ? . 2_566 C(12) H(12) 3.276 ? . 1_554 C(13) H(4) 3.075 ? . 2_565 C(13) H(12) 3.168 ? . 1_554 C(13) H(23) 3.594 ? . . C(14) H(4) 3.358 ? . 2_565 C(14) H(12) 2.969 ? . 1_554 C(14) H(23) 3.152 ? . . C(15) H(12) 2.877 ? . 1_554 C(15) H(18) 3.562 ? . 1_455 C(15) H(23) 2.918 ? . . C(16) H(12) 2.962 ? . 1_554 C(16) H(13) 3.208 ? . 1_554 C(16) H(22) 3.455 ? . . C(16) H(23) 3.142 ? . . C(17) H(8) 3.314 ? . 2_466 C(18) H(1) 3.392 ? . 1_466 C(18) H(5) 2.988 ? . 2_566 C(18) H(8) 3.473 ? . 2_466 C(19) H(1) 3.234 ? . 1_466 C(19) H(4) 3.012 ? . 2_566 C(19) H(5) 2.883 ? . 2_566 C(19) H(8) 3.509 ? . 2_466 C(20) H(4) 3.272 ? . 2_566 C(20) H(8) 3.391 ? . 2_466 C(20) H(12) 3.442 ? . 2_467 C(20) H(13) 3.336 ? . 2_467 C(21) H(3) 3.371 ? . 1_456 C(21) H(8) 3.239 ? . 2_466 C(21) H(12) 3.172 ? . 2_467 C(22) H(3) 3.366 ? . 1_456 C(22) H(7) 3.441 ? . 2_466 C(22) H(8) 3.197 ? . 2_466 C(24) H(6) 3.019 ? . 2_566 C(25) H(6) 3.034 ? . 2_566 C(25) H(17) 3.396 ? . 2_656 C(26) H(17) 3.274 ? . 2_656 C(26) H(22) 3.383 ? . 1_655 C(27) H(22) 3.175 ? . 1_655 C(27) H(23) 3.274 ? . 1_655 C(28) H(1) 3.306 ? . 2_655 C(28) H(8) 3.548 ? . 1_655 C(30) H(2) 3.212 ? . 2_655 C(30) H(21) 3.166 ? . 2_556 C(31) H(2) 2.794 ? . 2_655 C(31) H(20) 3.557 ? . 2_556 C(31) H(21) 3.094 ? . 2_556 C(32) H(2) 3.561 ? . 2_655 C(32) H(17) 3.266 ? . 1_455 C(32) H(18) 3.143 ? . 1_455 C(33) H(7) 3.500 ? . 2_466 C(33) H(18) 3.331 ? . 1_455 C(34) H(7) 3.326 ? . 2_466 H(1) C(18) 3.392 ? . 1_644 H(1) C(19) 3.234 ? . 1_644 H(1) C(28) 3.306 ? . 2_655 H(1) H(10) 3.083 ? . 1_644 H(1) H(11) 2.772 ? . 1_644 H(1) H(18) 3.473 ? . 2_655 H(1) H(19) 2.890 ? . 2_655 H(1) H(20) 3.583 ? . 2_655 H(2) Cl(1) 3.186 ? . 2_655 H(2) N(4) 3.585 ? . 2_655 H(2) C(9) 3.462 ? . 2_655 H(2) C(30) 3.212 ? . 2_655 H(2) C(31) 2.794 ? . 2_655 H(2) C(32) 3.561 ? . 2_655 H(2) H(20) 3.219 ? . 2_655 H(2) H(21) 2.488 ? . 2_655 H(3) Cl(1) 3.054 ? . 2_655 H(3) C(2) 3.532 ? . 2_655 H(3) C(21) 3.371 ? . 1_654 H(3) C(22) 3.366 ? . 1_654 H(3) H(7) 3.401 ? . 2_565 H(3) H(13) 2.744 ? . 1_654 H(3) H(14) 2.745 ? . 1_654 H(4) C(13) 3.075 ? . 2_565 H(4) C(14) 3.358 ? . 2_565 H(4) C(19) 3.012 ? . 2_566 H(4) C(20) 3.272 ? . 2_566 H(4) H(6) 2.843 ? . 2_565 H(4) H(7) 3.341 ? . 2_565 H(4) H(11) 2.271 ? . 2_566 H(4) H(12) 2.801 ? . 2_566 H(4) H(13) 3.542 ? . 1_654 H(5) C(12) 3.549 ? . 2_565 H(5) C(18) 2.988 ? . 2_566 H(5) C(19) 2.883 ? . 2_566 H(5) H(5) 3.054 ? . 2_565 H(5) H(10) 2.975 ? . 2_566 H(5) H(11) 2.798 ? . 2_566 H(6) C(7) 3.230 ? . 2_565 H(6) C(24) 3.019 ? . 2_566 H(6) C(25) 3.034 ? . 2_566 H(6) H(4) 2.843 ? . 2_565 H(6) H(15) 3.144 ? . 2_566 H(6) H(16) 3.155 ? . 2_566 H(7) C(22) 3.441 ? . 2_466 H(7) C(33) 3.500 ? . 2_466 H(7) C(34) 3.326 ? . 2_466 H(7) H(3) 3.401 ? . 2_565 H(7) H(4) 3.341 ? . 2_565 H(7) H(12) 3.462 ? . 1_554 H(7) H(14) 3.207 ? . 2_466 H(7) H(23) 3.529 ? . . H(7) H(23) 3.494 ? . 2_466 H(7) H(24) 3.239 ? . 2_466 H(8) C(17) 3.314 ? . 2_466 H(8) C(18) 3.473 ? . 2_466 H(8) C(19) 3.509 ? . 2_466 H(8) C(20) 3.391 ? . 2_466 H(8) C(21) 3.239 ? . 2_466 H(8) C(22) 3.197 ? . 2_466 H(8) C(28) 3.548 ? . 1_455 H(8) H(12) 3.316 ? . 1_554 H(8) H(18) 3.186 ? . 1_455 H(8) H(19) 2.907 ? . 1_455 H(8) H(23) 3.191 ? . . H(8) H(24) 3.216 ? . 2_466 H(10) C(12) 3.466 ? . 2_566 H(10) H(1) 3.083 ? . 1_466 H(10) H(5) 2.975 ? . 2_566 H(11) N(4) 3.033 ? . 2_566 H(11) C(4) 3.371 ? . 1_466 H(11) C(7) 3.042 ? . 2_566 H(11) H(1) 2.772 ? . 1_466 H(11) H(4) 2.271 ? . 2_566 H(11) H(5) 2.798 ? . 2_566 H(12) C(11) 3.162 ? . 1_556 H(12) C(12) 3.276 ? . 1_556 H(12) C(13) 3.168 ? . 1_556 H(12) C(14) 2.969 ? . 1_556 H(12) C(15) 2.877 ? . 1_556 H(12) C(16) 2.962 ? . 1_556 H(12) C(20) 3.442 ? . 2_467 H(12) C(21) 3.172 ? . 2_467 H(12) H(4) 2.801 ? . 2_566 H(12) H(7) 3.462 ? . 1_556 H(12) H(8) 3.316 ? . 1_556 H(12) H(12) 3.228 ? . 2_467 H(12) H(13) 2.741 ? . 2_467 H(13) N(1) 3.468 ? . 2_556 H(13) N(2) 3.304 ? . 2_556 H(13) C(1) 3.029 ? . 2_556 H(13) C(6) 3.574 ? . 1_456 H(13) C(16) 3.208 ? . 1_556 H(13) C(20) 3.336 ? . 2_467 H(13) H(3) 2.744 ? . 1_456 H(13) H(4) 3.542 ? . 1_456 H(13) H(12) 2.741 ? . 2_467 H(14) Cl(1) 3.043 ? . 2_556 H(14) H(3) 2.745 ? . 1_456 H(14) H(7) 3.207 ? . 2_466 H(15) Cl(1) 3.004 ? . 2_556 H(15) H(6) 3.144 ? . 2_566 H(16) N(3) 3.471 ? . 1_556 H(16) C(2) 3.213 ? . 1_556 H(16) C(3) 2.830 ? . 1_556 H(16) C(4) 3.338 ? . 1_556 H(16) C(7) 3.341 ? . 1_556 H(16) C(8) 2.832 ? . 1_556 H(16) C(9) 3.249 ? . 1_556 H(16) H(6) 3.155 ? . 2_566 H(16) H(18) 3.487 ? . 2_656 H(17) C(25) 3.396 ? . 2_656 H(17) C(26) 3.274 ? . 2_656 H(17) C(32) 3.266 ? . 1_655 H(17) H(17) 3.423 ? . 2_656 H(17) H(20) 3.431 ? . 2_656 H(17) H(22) 2.902 ? . 1_655 H(18) N(2) 2.884 ? . 2_655 H(18) C(1) 3.377 ? . 2_655 H(18) C(2) 3.506 ? . 2_655 H(18) C(15) 3.562 ? . 1_655 H(18) C(32) 3.143 ? . 1_655 H(18) C(33) 3.331 ? . 1_655 H(18) H(1) 3.473 ? . 2_655 H(18) H(8) 3.186 ? . 1_655 H(18) H(16) 3.487 ? . 2_656 H(18) H(22) 2.486 ? . 1_655 H(18) H(23) 2.853 ? . 1_655 H(19) H(1) 2.890 ? . 2_655 H(19) H(8) 2.907 ? . 1_655 H(20) C(31) 3.557 ? . 2_556 H(20) H(1) 3.583 ? . 2_655 H(20) H(2) 3.219 ? . 2_655 H(20) H(17) 3.431 ? . 2_656 H(20) H(21) 2.918 ? . 2_556 H(21) Cl(1) 3.241 ? . . H(21) C(5) 3.301 ? . 2_655 H(21) C(30) 3.166 ? . 2_556 H(21) C(31) 3.094 ? . 2_556 H(21) H(2) 2.488 ? . 2_655 H(21) H(20) 2.918 ? . 2_556 H(21) H(21) 2.772 ? . 2_556 H(22) Cl(1) 3.154 ? . . H(22) N(1) 3.555 ? . 2_555 H(22) C(1) 3.285 ? . 2_555 H(22) C(16) 3.455 ? . . H(22) C(26) 3.383 ? . 1_455 H(22) C(27) 3.175 ? . 1_455 H(22) H(17) 2.902 ? . 1_455 H(22) H(18) 2.486 ? . 1_455 H(23) C(11) 3.572 ? . . H(23) C(13) 3.594 ? . . H(23) C(14) 3.152 ? . . H(23) C(15) 2.918 ? . . H(23) C(16) 3.142 ? . . H(23) C(27) 3.274 ? . 1_455 H(23) H(7) 3.529 ? . . H(23) H(7) 3.494 ? . 2_466 H(23) H(8) 3.191 ? . . H(23) H(18) 2.853 ? . 1_455 H(24) H(7) 3.239 ? . 2_466 H(24) H(8) 3.216 ? . 2_466 #============================================================================== # End of CIF #==============================================================================