# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.P.Caradonna ;Department of Chemistry Boston University Boston, MA 02215 ; P.J.Cappillino ;Department of Chemistry Boston University Boston, MA 02215 ; J.R.Miecznikowski ;Department of Chemistry Fairfield University Fairfield CT 06824 ; L.A.Tyler ;Department of Chemistry Union College Schenectady NY 12308 ; W.Lo ;Department of Chemistry Boston College Chestnut Hill, MA 02467 ; ; W.H.Armstrong ; ;Department of Chemistry Boston College Chestnut Hill, MA 02467 ; _publ_contact_author_address ;Department of Chemistry Boston University Boston, MA 02215 ; _publ_contact_author_email caradonn@bu.edu _publ_contact_author_phone '(617) 353-1692 ' _publ_contact_author_name 'John P. Caradonna' #TrackingRef '- 1anew.cif' _publ_requested_category FA data_1a _database_code_depnum_ccdc_archive 'CCDC 829864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H33 Cl Fe N3 O6' _chemical_formula_weight 466.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5847(19) _cell_length_b 11.024(2) _cell_length_c 10.765(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.97(3) _cell_angle_gamma 90.00 _cell_volume 1093.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4542 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 23.31 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max .3 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .84 _exptl_absorpt_correction_T_max .92 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _chemical_absolute_configuration unk _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 Area _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4534 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.31 _reflns_number_total 2430 _reflns_number_gt 2129 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(3) _refine_ls_number_reflns 2430 _refine_ls_number_parameters 259 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.25066(6) 0.51269(7) 0.89494(6) 0.02317(18) Uani 1 1 d . . . Cl1 Cl 0.10777(15) 0.67364(12) 0.81215(13) 0.0372(4) Uani 1 1 d . . . O2 O 0.3698(3) 0.5932(3) 1.0547(3) 0.0276(8) Uani 1 1 d . . . O5 O 0.3988(4) 0.6421(3) 1.2610(3) 0.0370(9) Uani 1 1 d . . . O6 O 0.1151(4) 0.1956(3) 0.7175(4) 0.0530(12) Uani 1 1 d . . . O3 O 0.1370(4) 0.3884(3) 0.7792(3) 0.0315(10) Uani 1 1 d . . . O1 O 0.4154(3) 0.5299(4) 0.8193(3) 0.0339(9) Uani 1 1 d . . . O4 O 0.6537(3) 0.5041(5) 0.8596(3) 0.0499(10) Uani 1 1 d . . . C7 C 0.3301(6) 0.5972(5) 1.1595(5) 0.0265(11) Uani 1 1 d . . . N2 N 0.1369(4) 0.4538(4) 1.0397(4) 0.0300(11) Uani 1 1 d . . . C6 C 0.1828(5) 0.5407(5) 1.1478(5) 0.0380(15) Uani 1 1 d . . . H6A H 0.1856 0.4992 1.2279 0.046 Uiso 1 1 calc R . . H6B H 0.1110 0.6048 1.1361 0.046 Uiso 1 1 calc R . . C4 C 0.5331(5) 0.3866(5) 0.9826(5) 0.0374(14) Uani 1 1 d . . . H4A H 0.5900 0.3162 0.9730 0.045 Uiso 1 1 calc R . . H4B H 0.5756 0.4211 1.0674 0.045 Uiso 1 1 calc R . . C5 C 0.5366(5) 0.4800(5) 0.8788(5) 0.0338(15) Uani 1 1 d . . . C9 C 0.1825(5) 0.2768(5) 0.7823(5) 0.0319(13) Uani 1 1 d . . . C1 C 0.3532(5) 0.3170(5) 1.0941(5) 0.0362(14) Uani 1 1 d . . . H1A H 0.4079 0.3703 1.1618 0.043 Uiso 1 1 calc R . . H1B H 0.3844 0.2343 1.1170 0.043 Uiso 1 1 calc R . . N1 N 0.3809(4) 0.3492(4) 0.9708(4) 0.0286(10) Uani 1 1 d . . . C3 C -0.0241(5) 0.4506(5) 0.9921(5) 0.0411(15) Uani 1 1 d . . . H3A H -0.0529 0.3937 0.9222 0.062 Uiso 1 1 calc R . . H3B H -0.0597 0.5298 0.9623 0.062 Uiso 1 1 calc R . . H3C H -0.0636 0.4262 1.0610 0.062 Uiso 1 1 calc R . . C2 C 0.1916(5) 0.3289(5) 1.0822(5) 0.0375(14) Uani 1 1 d . . . H2A H 0.1382 0.2700 1.0202 0.045 Uiso 1 1 calc R . . H2B H 0.1744 0.3113 1.1651 0.045 Uiso 1 1 calc R . . C8 C 0.3310(5) 0.2524(4) 0.8721(5) 0.0349(14) Uani 1 1 d . . . H8A H 0.3291 0.1757 0.9157 0.042 Uiso 1 1 calc R . . H8B H 0.4001 0.2451 0.8215 0.042 Uiso 1 1 calc R . . N3 N 0.7383(4) 0.4105(4) 0.5051(4) 0.0269(11) Uani 1 1 d . . . C16 C 0.7864(5) 0.5096(6) 0.6056(4) 0.0356(12) Uani 1 1 d . . . H16A H 0.7439 0.4937 0.6760 0.043 Uiso 1 1 calc R . . H16B H 0.8910 0.5050 0.6404 0.043 Uiso 1 1 calc R . . C12 C 0.7838(5) 0.2920(5) 0.5757(5) 0.0314(13) Uani 1 1 d . . . H12A H 0.7369 0.2855 0.6446 0.038 Uiso 1 1 calc R . . H12B H 0.8877 0.2943 0.6154 0.038 Uiso 1 1 calc R . . C10 C 0.8079(6) 0.4261(5) 0.3965(5) 0.0395(14) Uani 1 1 d . . . H10A H 0.7778 0.5037 0.3552 0.047 Uiso 1 1 calc R . . H10B H 0.7713 0.3633 0.3327 0.047 Uiso 1 1 calc R . . C13 C 0.7484(6) 0.1792(5) 0.4923(5) 0.0467(15) Uani 1 1 d . . . H13A H 0.6451 0.1729 0.4568 0.070 Uiso 1 1 calc R . . H13B H 0.7838 0.1089 0.5439 0.070 Uiso 1 1 calc R . . H13C H 0.7938 0.1844 0.4233 0.070 Uiso 1 1 calc R . . C15 C 0.4857(5) 0.4042(5) 0.5423(6) 0.0489(17) Uani 1 1 d . . . H15A H 0.5115 0.3317 0.5928 0.073 Uiso 1 1 calc R . . H15B H 0.3848 0.4014 0.4957 0.073 Uiso 1 1 calc R . . H15C H 0.5035 0.4736 0.5984 0.073 Uiso 1 1 calc R . . C14 C 0.5772(5) 0.4138(5) 0.4467(5) 0.0408(15) Uani 1 1 d . . . H14A H 0.5506 0.3478 0.3852 0.049 Uiso 1 1 calc R . . H14B H 0.5526 0.4891 0.3990 0.049 Uiso 1 1 calc R . . C17 C 0.7467(7) 0.6372(5) 0.5572(6) 0.0585(19) Uani 1 1 d . . . H17A H 0.7838 0.6528 0.4845 0.088 Uiso 1 1 calc R . . H17B H 0.7880 0.6940 0.6248 0.088 Uiso 1 1 calc R . . H17C H 0.6430 0.6457 0.5314 0.088 Uiso 1 1 calc R . . C11 C 0.9722(6) 0.4209(6) 0.4360(6) 0.0573(19) Uani 1 1 d . . . H11A H 1.0102 0.4833 0.4983 0.086 Uiso 1 1 calc R . . H11B H 1.0070 0.4329 0.3614 0.086 Uiso 1 1 calc R . . H11C H 1.0036 0.3430 0.4733 0.086 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0248(3) 0.0202(4) 0.0248(4) 0.0005(4) 0.0074(3) 0.0017(4) Cl1 0.0413(8) 0.0275(8) 0.0428(8) 0.0079(7) 0.0117(7) 0.0111(7) O2 0.0270(18) 0.028(2) 0.029(2) -0.0015(16) 0.0111(16) -0.0052(16) O5 0.045(2) 0.036(2) 0.027(2) -0.0097(18) 0.0040(17) -0.0006(19) O6 0.041(2) 0.034(3) 0.068(3) -0.028(2) -0.012(2) 0.004(2) O3 0.032(2) 0.026(2) 0.033(2) -0.0035(17) 0.0022(17) 0.0036(17) O1 0.0307(18) 0.040(2) 0.0327(18) -0.003(2) 0.0112(15) 0.005(2) O4 0.0280(18) 0.063(3) 0.062(2) -0.006(3) 0.0186(16) -0.004(3) C7 0.036(3) 0.014(3) 0.028(3) -0.001(2) 0.007(3) 0.004(2) N2 0.025(2) 0.026(3) 0.039(3) 0.000(2) 0.008(2) -0.004(2) C6 0.039(3) 0.039(4) 0.041(3) -0.009(3) 0.021(2) 0.000(3) C4 0.033(3) 0.028(3) 0.046(3) -0.004(3) 0.002(3) 0.006(3) C5 0.032(3) 0.040(4) 0.031(3) -0.017(3) 0.011(2) -0.001(3) C9 0.028(3) 0.028(4) 0.036(3) -0.003(3) 0.004(3) 0.007(3) C1 0.040(3) 0.021(3) 0.041(3) 0.006(3) -0.002(3) 0.005(3) N1 0.024(2) 0.027(3) 0.029(2) 0.001(2) -0.0010(19) 0.001(2) C3 0.025(3) 0.045(4) 0.055(4) 0.004(3) 0.013(3) -0.010(3) C2 0.039(3) 0.036(4) 0.035(3) 0.005(3) 0.007(3) -0.007(3) C8 0.033(3) 0.018(3) 0.047(4) -0.014(3) -0.001(3) 0.002(3) N3 0.035(3) 0.020(3) 0.022(2) 0.0014(18) 0.002(2) 0.000(2) C16 0.040(3) 0.037(3) 0.026(2) -0.008(3) 0.004(2) -0.006(4) C12 0.033(3) 0.031(3) 0.030(3) 0.015(3) 0.007(2) 0.005(3) C10 0.071(4) 0.025(3) 0.027(3) 0.003(3) 0.021(3) -0.005(3) C13 0.061(4) 0.034(4) 0.053(4) 0.011(3) 0.028(3) 0.003(3) C15 0.031(3) 0.041(4) 0.065(4) 0.007(3) -0.003(3) 0.006(3) C14 0.042(3) 0.031(4) 0.037(3) -0.005(3) -0.010(3) 0.005(3) C17 0.083(5) 0.033(4) 0.053(4) -0.013(3) 0.008(4) -0.010(4) C11 0.065(4) 0.061(5) 0.058(4) -0.004(3) 0.038(4) -0.022(4) _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 O3 1.967(3) . ? Fe1 O1 1.975(3) . ? Fe1 O2 1.992(3) . ? Fe1 N1 2.216(4) . ? Fe1 N2 2.231(4) . ? Fe1 Cl1 2.2685(15) . ? O2 C7 1.287(6) . ? O5 C7 1.215(6) . ? O6 C9 1.207(6) . ? O3 C9 1.303(6) . ? O1 C5 1.286(5) . ? O4 C5 1.225(5) . ? C7 C6 1.515(7) . ? N2 C6 1.478(6) . ? N2 C3 1.486(5) . ? N2 C2 1.499(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C4 N1 1.487(6) . ? C4 C5 1.526(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C9 C8 1.508(6) . ? C1 N1 1.467(6) . ? C1 C2 1.524(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? N1 C8 1.489(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N3 C14 1.499(6) . ? N3 C10 1.507(7) . ? N3 C12 1.514(6) . ? N3 C16 1.517(7) . ? C16 C17 1.512(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C12 C13 1.516(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 C11 1.516(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C14 1.528(7) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? 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 O3 Fe1 O1 99.92(15) . . ? O3 Fe1 O2 160.60(14) . . ? O1 Fe1 O2 88.83(13) . . ? O3 Fe1 N1 79.91(14) . . ? O1 Fe1 N1 78.28(16) . . ? O2 Fe1 N1 85.03(14) . . ? O3 Fe1 N2 87.00(14) . . ? O1 Fe1 N2 156.39(14) . . ? O2 Fe1 N2 78.53(14) . . ? N1 Fe1 N2 80.80(15) . . ? O3 Fe1 Cl1 97.27(11) . . ? O1 Fe1 Cl1 103.15(12) . . ? O2 Fe1 Cl1 97.53(10) . . ? N1 Fe1 Cl1 177.06(12) . . ? N2 Fe1 Cl1 98.26(11) . . ? C7 O2 Fe1 122.3(3) . . ? C9 O3 Fe1 121.2(3) . . ? C5 O1 Fe1 117.9(3) . . ? O5 C7 O2 125.7(5) . . ? O5 C7 C6 120.3(5) . . ? O2 C7 C6 114.0(4) . . ? C6 N2 C3 110.1(4) . . ? C6 N2 C2 110.6(4) . . ? C3 N2 C2 109.0(4) . . ? C6 N2 Fe1 105.3(3) . . ? C3 N2 Fe1 115.3(3) . . ? C2 N2 Fe1 106.4(3) . . ? N2 C6 C7 113.7(4) . . ? N2 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N1 C4 C5 110.1(4) . . ? N1 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? O4 C5 O1 124.6(5) . . ? O4 C5 C4 118.4(5) . . ? O1 C5 C4 117.0(4) . . ? O6 C9 O3 124.3(5) . . ? O6 C9 C8 119.9(5) . . ? O3 C9 C8 115.8(5) . . ? N1 C1 C2 109.7(4) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 N1 C4 114.1(4) . . ? C1 N1 C8 111.7(4) . . ? C4 N1 C8 112.0(4) . . ? C1 N1 Fe1 107.8(3) . . ? C4 N1 Fe1 104.3(3) . . ? C8 N1 Fe1 106.4(3) . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C2 C1 111.5(4) . . ? N2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C8 C9 113.0(4) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C14 N3 C10 107.3(4) . . ? C14 N3 C12 110.7(4) . . ? C10 N3 C12 111.1(4) . . ? C14 N3 C16 110.9(4) . . ? C10 N3 C16 111.0(4) . . ? C12 N3 C16 105.9(4) . . ? C17 C16 N3 115.2(4) . . ? C17 C16 H16A 108.5 . . ? N3 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? N3 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N3 C12 C13 115.1(4) . . ? N3 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? N3 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? N3 C10 C11 115.2(4) . . ? N3 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N3 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C14 C15 115.6(4) . . ? N3 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? N3 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.234 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.053 # Attachment '- 1cnew.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 829865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Fe3 N4 O19' _chemical_formula_sum 'C20 H40 Fe3 N4 O19' _chemical_formula_weight 808.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.726(3) _cell_length_b 11.2284(17) _cell_length_c 14.423(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.109(2) _cell_angle_gamma 90.00 _cell_volume 3123.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2766 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max .08 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786468 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Area _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14847 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2763 _reflns_number_gt 2335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SMART (Bruker, 2003)' _computing_data_reduction 'SAINTPLUS (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+49.3856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2763 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2661(3) 0.0139(5) 0.1563(4) 0.0195(12) Uani 1 1 d . . . H1A H 0.2177 0.0232 0.1260 0.023 Uiso 1 1 calc R . . H1B H 0.2700 -0.0526 0.2001 0.023 Uiso 1 1 calc R . . C2 C 0.3082(3) -0.0114(5) 0.0821(4) 0.0188(12) Uani 1 1 d . . . H2A H 0.2929 -0.0861 0.0509 0.023 Uiso 1 1 calc R . . H2B H 0.2999 0.0510 0.0346 0.023 Uiso 1 1 calc R . . C3 C 0.4010(3) -0.1357(5) 0.1715(4) 0.0213(12) Uani 1 1 d . . . H3A H 0.4477 -0.1583 0.1673 0.026 Uiso 1 1 calc R . . H3B H 0.3695 -0.1960 0.1391 0.026 Uiso 1 1 calc R . . C4 C 0.3959(3) -0.1315(5) 0.2754(4) 0.0203(12) Uani 1 1 d . . . C5 C 0.2682(3) 0.2314(5) 0.1511(4) 0.0242(13) Uani 1 1 d . . . H5A H 0.2481 0.2870 0.1892 0.029 Uiso 1 1 calc R . . H5B H 0.2322 0.2090 0.0972 0.029 Uiso 1 1 calc R . . C6 C 0.3258(3) 0.2939(5) 0.1152(4) 0.0216(13) Uani 1 1 d . . . C7 C 0.2759(3) 0.1350(5) 0.3021(4) 0.0208(12) Uani 1 1 d . . . H7A H 0.2764 0.0571 0.3312 0.025 Uiso 1 1 calc R . . H7B H 0.2299 0.1686 0.2967 0.025 Uiso 1 1 calc R . . C8 C 0.3294(3) 0.2156(5) 0.3650(4) 0.0167(11) Uani 1 1 d . . . C9 C 0.4245(3) -0.0047(6) 0.0485(4) 0.0248(13) Uani 1 1 d . . . H9A H 0.4132 -0.0679 0.0031 0.037 Uiso 1 1 calc R . . H9B H 0.4731 -0.0076 0.0768 0.037 Uiso 1 1 calc R . . H9C H 0.4137 0.0705 0.0172 0.037 Uiso 1 1 calc R . . C10 C 0.5815(4) 0.5038(6) 0.2236(5) 0.0334(15) Uani 1 1 d . . . H10A H 0.5591 0.4282 0.2254 0.050 Uiso 1 1 calc R . . H10B H 0.5777 0.5494 0.2786 0.050 Uiso 1 1 calc R . . H10C H 0.6295 0.4915 0.2230 0.050 Uiso 1 1 calc R . . Fe1 Fe 0.40852(4) 0.11601(6) 0.23507(5) 0.0098(2) Uani 1 1 d . . . Fe2 Fe 0.5000 0.5000 0.0000 0.0337(4) Uani 1 2 d S . . N1 N 0.2912(2) 0.1232(4) 0.2087(3) 0.0186(10) Uani 1 1 d . . . N2 N 0.3836(2) -0.0186(4) 0.1232(3) 0.0185(10) Uani 1 1 d . . . O1 O 0.3112(2) 0.3861(4) 0.0696(3) 0.0315(11) Uani 1 1 d . . . O2 O 0.38599(18) 0.2473(3) 0.1361(3) 0.0188(8) Uani 1 1 d . . . O3 O 0.3143(2) 0.2692(4) 0.4318(3) 0.0227(9) Uani 1 1 d . . . O4 O 0.38924(19) 0.2185(3) 0.3424(3) 0.0172(8) Uani 1 1 d . . . O5 O 0.3995(2) -0.0297(3) 0.3129(3) 0.0198(9) Uani 1 1 d . . . O6 O 0.3885(2) -0.2256(4) 0.3177(3) 0.0310(10) Uani 1 1 d . . . O7 O 0.5000 0.1306(5) 0.2500 0.0163(11) Uani 1 2 d S . . O8 O 0.5489(3) 0.5672(4) 0.1399(3) 0.0369(12) Uani 1 1 d . . . O9 O 0.3988(2) 0.5524(4) 0.0232(3) 0.0312(11) Uani 1 1 d . . . H9 H 0.3761 0.4927 0.0291 0.047 Uiso 1 1 calc R . . O10 O 0.4928(2) 0.3246(4) 0.0556(3) 0.0257(9) Uani 1 1 d . . . H10 H 0.4730 0.3277 0.1001 0.039 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.009(2) 0.024(3) 0.023(3) -0.002(2) -0.001(2) -0.005(2) C2 0.011(3) 0.027(3) 0.016(3) -0.003(2) -0.003(2) -0.004(2) C3 0.022(3) 0.016(3) 0.027(3) -0.003(2) 0.007(2) 0.000(2) C4 0.013(3) 0.018(3) 0.027(3) 0.004(2) -0.004(2) 0.000(2) C5 0.017(3) 0.023(3) 0.031(3) 0.011(3) 0.000(2) 0.003(2) C6 0.020(3) 0.022(3) 0.018(3) 0.003(2) -0.006(2) -0.005(2) C7 0.016(3) 0.024(3) 0.023(3) -0.002(2) 0.005(2) -0.001(2) C8 0.019(3) 0.008(2) 0.020(3) 0.005(2) -0.002(2) 0.003(2) C9 0.020(3) 0.039(4) 0.015(3) -0.009(3) 0.003(2) -0.006(3) C10 0.035(4) 0.032(4) 0.035(4) 0.000(3) 0.011(3) 0.000(3) Fe1 0.0080(4) 0.0099(4) 0.0097(4) 0.0011(3) -0.0021(3) -0.0005(3) Fe2 0.0325(8) 0.0301(8) 0.0348(8) 0.0061(6) -0.0010(6) -0.0048(6) N1 0.012(2) 0.020(2) 0.022(2) 0.001(2) 0.0012(19) -0.0027(18) N2 0.015(2) 0.026(3) 0.014(2) -0.003(2) 0.0023(18) -0.0034(19) O1 0.022(2) 0.025(2) 0.041(3) 0.021(2) -0.0054(19) -0.0036(18) O2 0.0130(19) 0.0178(19) 0.022(2) 0.0083(16) -0.0052(15) -0.0016(15) O3 0.027(2) 0.021(2) 0.022(2) -0.0063(17) 0.0096(17) 0.0037(17) O4 0.0157(19) 0.0172(19) 0.0188(19) -0.0048(16) 0.0042(15) -0.0024(15) O5 0.020(2) 0.020(2) 0.0165(19) 0.0042(16) -0.0028(16) -0.0018(16) O6 0.036(3) 0.018(2) 0.037(3) 0.0112(19) 0.002(2) 0.0007(19) O7 0.007(2) 0.022(3) 0.018(3) 0.000 -0.003(2) 0.000 O8 0.053(3) 0.025(2) 0.029(2) 0.003(2) 0.001(2) -0.008(2) O9 0.029(2) 0.025(2) 0.036(3) 0.012(2) -0.002(2) -0.0106(19) O10 0.020(2) 0.028(2) 0.029(2) 0.0072(19) 0.0030(18) -0.0016(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.470(7) . ? C1 C2 1.513(8) . ? C2 N2 1.484(7) . ? C3 N2 1.494(7) . ? C3 C4 1.523(8) . ? C4 O6 1.243(7) . ? C4 O5 1.260(7) . ? C5 N1 1.489(7) . ? C5 C6 1.517(8) . ? C6 O1 1.228(7) . ? C6 O2 1.274(7) . ? C7 N1 1.447(7) . ? C7 C8 1.533(8) . ? C8 O3 1.224(7) . ? C8 O4 1.290(7) . ? C9 N2 1.484(7) . ? C10 O8 1.433(8) . ? Fe1 O7 1.7795(9) . ? Fe1 O5 2.013(4) . ? Fe1 O4 2.028(4) . ? Fe1 O2 2.035(4) . ? Fe1 N2 2.190(5) . ? Fe1 N1 2.267(5) . ? Fe2 O10 2.143(4) . ? Fe2 O10 2.143(4) 5_665 ? Fe2 O9 2.174(5) . ? Fe2 O9 2.174(5) 5_665 ? Fe2 O8 2.180(5) 5_665 ? Fe2 O8 2.180(5) . ? O7 Fe1 1.7795(9) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.2(4) . . ? N2 C2 C1 112.4(4) . . ? N2 C3 C4 112.1(4) . . ? O6 C4 O5 124.2(6) . . ? O6 C4 C3 119.6(5) . . ? O5 C4 C3 116.1(5) . . ? N1 C5 C6 113.9(5) . . ? O1 C6 O2 125.2(6) . . ? O1 C6 C5 117.6(5) . . ? O2 C6 C5 117.2(5) . . ? N1 C7 C8 110.7(5) . . ? O3 C8 O4 124.9(5) . . ? O3 C8 C7 120.4(5) . . ? O4 C8 C7 114.7(5) . . ? O7 Fe1 O5 102.29(18) . . ? O7 Fe1 O4 101.73(15) . . ? O5 Fe1 O4 89.02(16) . . ? O7 Fe1 O2 94.88(16) . . ? O5 Fe1 O2 161.45(15) . . ? O4 Fe1 O2 94.37(16) . . ? O7 Fe1 N2 102.56(17) . . ? O5 Fe1 N2 79.48(17) . . ? O4 Fe1 N2 154.83(16) . . ? O2 Fe1 N2 90.06(17) . . ? O7 Fe1 N1 172.3(2) . . ? O5 Fe1 N1 85.18(16) . . ? O4 Fe1 N1 76.08(16) . . ? O2 Fe1 N1 77.99(16) . . ? N2 Fe1 N1 80.66(17) . . ? O10 Fe2 O10 180.0(2) . 5_665 ? O10 Fe2 O9 93.19(16) . . ? O10 Fe2 O9 86.81(16) 5_665 . ? O10 Fe2 O9 86.81(16) . 5_665 ? O10 Fe2 O9 93.19(16) 5_665 5_665 ? O9 Fe2 O9 180.0(2) . 5_665 ? O10 Fe2 O8 88.67(17) . 5_665 ? O10 Fe2 O8 91.33(17) 5_665 5_665 ? O9 Fe2 O8 89.65(18) . 5_665 ? O9 Fe2 O8 90.35(18) 5_665 5_665 ? O10 Fe2 O8 91.33(17) . . ? O10 Fe2 O8 88.67(17) 5_665 . ? O9 Fe2 O8 90.34(18) . . ? O9 Fe2 O8 89.66(18) 5_665 . ? O8 Fe2 O8 179.998(1) 5_665 . ? C7 N1 C1 116.3(4) . . ? C7 N1 C5 110.2(5) . . ? C1 N1 C5 111.3(4) . . ? C7 N1 Fe1 104.6(3) . . ? C1 N1 Fe1 106.1(3) . . ? C5 N1 Fe1 107.6(3) . . ? C2 N2 C9 110.9(4) . . ? C2 N2 C3 110.3(4) . . ? C9 N2 C3 109.0(5) . . ? C2 N2 Fe1 107.9(3) . . ? C9 N2 Fe1 113.0(3) . . ? C3 N2 Fe1 105.7(3) . . ? C6 O2 Fe1 121.3(4) . . ? C8 O4 Fe1 120.4(3) . . ? C4 O5 Fe1 120.1(4) . . ? Fe1 O7 Fe1 169.5(3) 2_655 . ? C10 O8 Fe2 129.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.801 _refine_diff_density_min -2.183 _refine_diff_density_rms 0.164 # Attachment '- 2anew.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 829866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common (NMe4)(FeCl23N2O2) _chemical_melting_point ? _chemical_formula_moiety 'C16 H34 Cl2 Fe N3 O4' _chemical_formula_sum 'C16 H34 Cl2 Fe N3 O4' _chemical_formula_weight 459.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0936(6) _cell_length_b 10.2705(8) _cell_length_c 25.975(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.228(2) _cell_angle_gamma 90.00 _cell_volume 2153.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3798 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .829234 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 Area _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12245 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3798 _reflns_number_gt 3039 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3798 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.819 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4411(3) 0.8302(3) 0.77155(11) 0.0356(6) Uani 1 1 d . . . H1A H 0.4726 0.9199 0.7659 0.043 Uiso 1 1 calc R . . H1B H 0.3367 0.8143 0.7518 0.043 Uiso 1 1 calc R . . C2 C 0.5716(3) 0.7410(3) 0.75284(10) 0.0346(6) Uani 1 1 d . . . H2A H 0.5358 0.6513 0.7559 0.042 Uiso 1 1 calc R . . H2B H 0.5849 0.7584 0.7167 0.042 Uiso 1 1 calc R . . C3 C 0.8154(3) 0.8803(3) 0.76851(11) 0.0409(7) Uani 1 1 d . . . H3A H 0.7825 0.9000 0.7327 0.049 Uiso 1 1 calc R . . H3B H 0.9343 0.8668 0.7714 0.049 Uiso 1 1 calc R . . C4 C 0.7752(3) 0.9954(3) 0.80134(11) 0.0400(7) Uani 1 1 d . . . C5 C 0.8385(4) 0.6451(3) 0.77261(13) 0.0504(8) Uani 1 1 d . . . H5A H 0.8516 0.6393 0.7363 0.076 Uiso 1 1 calc R . . H5B H 0.7871 0.5671 0.7840 0.076 Uiso 1 1 calc R . . H5C H 0.9452 0.6553 0.7909 0.076 Uiso 1 1 calc R . . C6 C 0.3350(3) 0.6851(2) 0.83603(12) 0.0363(6) Uani 1 1 d . . . H6A H 0.2628 0.6641 0.8057 0.044 Uiso 1 1 calc R . . H6B H 0.2664 0.6952 0.8648 0.044 Uiso 1 1 calc R . . C7 C 0.3212(4) 0.9200(3) 0.84561(13) 0.0451(7) Uani 1 1 d . . . H7A H 0.2155 0.9229 0.8263 0.068 Uiso 1 1 calc R . . H7B H 0.3793 1.0002 0.8409 0.068 Uiso 1 1 calc R . . H7C H 0.3052 0.9084 0.8816 0.068 Uiso 1 1 calc R . . C8 C 0.4540(3) 0.5735(3) 0.84724(10) 0.0364(6) Uani 1 1 d . . . C9A C 0.6817(6) 0.1870(4) 0.94686(19) 0.0394(12) Uani 0.625(4) 1 d P A 1 H9A1 H 0.7102 0.1040 0.9320 0.047 Uiso 0.625(4) 1 calc PR A 1 H9A2 H 0.6831 0.1748 0.9839 0.047 Uiso 0.625(4) 1 calc PR A 1 C10A C 0.7699(6) 0.4188(4) 0.9595(2) 0.0396(12) Uani 0.625(4) 1 d P A 1 H10A H 0.8590 0.4797 0.9547 0.048 Uiso 0.625(4) 1 calc PR A 1 H10B H 0.6719 0.4509 0.9398 0.048 Uiso 0.625(4) 1 calc PR A 1 C11A C 0.8225(6) 0.3033(5) 0.87941(18) 0.0409(12) Uani 0.625(4) 1 d P A 1 H11A H 0.7203 0.3451 0.8665 0.049 Uiso 0.625(4) 1 calc PR A 1 H11B H 0.8270 0.2187 0.8629 0.049 Uiso 0.625(4) 1 calc PR A 1 C12A C 0.9759(6) 0.2418(5) 0.9634(2) 0.0431(12) Uani 0.625(4) 1 d P A 1 H12A H 0.9588 0.2258 0.9995 0.052 Uiso 0.625(4) 1 calc PR A 1 H12B H 1.0561 0.3116 0.9620 0.052 Uiso 0.625(4) 1 calc PR A 1 C13A C 0.509(3) 0.219(2) 0.9276(8) 0.052(4) Uani 0.625(4) 1 d P A 1 H13A H 0.4740 0.2962 0.9445 0.077 Uiso 0.625(4) 1 calc PR A 1 H13B H 0.4376 0.1479 0.9348 0.077 Uiso 0.625(4) 1 calc PR A 1 H13C H 0.5052 0.2336 0.8910 0.077 Uiso 0.625(4) 1 calc PR A 1 C14A C 0.7362(12) 0.4189(8) 1.0160(3) 0.0451(18) Uani 0.625(4) 1 d P A 1 H14A H 0.6475 0.3596 1.0215 0.068 Uiso 0.625(4) 1 calc PR A 1 H14B H 0.7055 0.5051 1.0261 0.068 Uiso 0.625(4) 1 calc PR A 1 H14C H 0.8342 0.3922 1.0364 0.068 Uiso 0.625(4) 1 calc PR A 1 C15A C 0.9679(12) 0.3848(9) 0.8637(5) 0.056(2) Uani 0.625(4) 1 d P A 1 H15A H 0.9561 0.4726 0.8756 0.084 Uiso 0.625(4) 1 calc PR A 1 H15B H 0.9697 0.3844 0.8268 0.084 Uiso 0.625(4) 1 calc PR A 1 H15C H 1.0695 0.3487 0.8789 0.084 Uiso 0.625(4) 1 calc PR A 1 C16A C 1.0453(16) 0.1201(13) 0.9403(4) 0.061(2) Uani 0.625(4) 1 d P A 1 H16A H 0.9695 0.0491 0.9436 0.091 Uiso 0.625(4) 1 calc PR A 1 H16B H 1.1500 0.0991 0.9582 0.091 Uiso 0.625(4) 1 calc PR A 1 H16C H 1.0604 0.1347 0.9045 0.091 Uiso 0.625(4) 1 calc PR A 1 C9B C 0.6709(9) 0.2819(7) 0.8979(3) 0.0358(18) Uani 0.375(4) 1 d P A 2 H9B1 H 0.7026 0.2394 0.8668 0.043 Uiso 0.375(4) 1 calc PR A 2 H9B2 H 0.6419 0.3712 0.8890 0.043 Uiso 0.375(4) 1 calc PR A 2 C10B C 0.7898(10) 0.3147(8) 0.9891(3) 0.045(2) Uani 0.375(4) 1 d P A 2 H10C H 0.8943 0.3108 1.0099 0.053 Uiso 0.375(4) 1 calc PR A 2 H10D H 0.7162 0.2503 1.0023 0.053 Uiso 0.375(4) 1 calc PR A 2 C11B C 0.9512(10) 0.3688(8) 0.9148(4) 0.049(2) Uani 0.375(4) 1 d P A 2 H11C H 0.9075 0.4567 0.9119 0.059 Uiso 0.375(4) 1 calc PR A 2 H11D H 1.0447 0.3712 0.9403 0.059 Uiso 0.375(4) 1 calc PR A 2 C12B C 0.8887(10) 0.1358(7) 0.9355(3) 0.044(2) Uani 0.375(4) 1 d P A 2 H12C H 0.8109 0.0790 0.9511 0.052 Uiso 0.375(4) 1 calc PR A 2 H12D H 0.8924 0.1092 0.8997 0.052 Uiso 0.375(4) 1 calc PR A 2 C13B C 0.519(3) 0.214(3) 0.9155(13) 0.037(5) Uani 0.375(4) 1 d P A 2 H13D H 0.5428 0.1240 0.9216 0.055 Uiso 0.375(4) 1 calc PR A 2 H13E H 0.4295 0.2224 0.8892 0.055 Uiso 0.375(4) 1 calc PR A 2 H13F H 0.4874 0.2540 0.9468 0.055 Uiso 0.375(4) 1 calc PR A 2 C14B C 0.716(2) 0.4468(16) 0.9940(5) 0.059(4) Uani 0.375(4) 1 d P A 2 H14D H 0.7891 0.5110 0.9815 0.088 Uiso 0.375(4) 1 calc PR A 2 H14E H 0.6994 0.4639 1.0296 0.088 Uiso 0.375(4) 1 calc PR A 2 H14F H 0.6112 0.4505 0.9740 0.088 Uiso 0.375(4) 1 calc PR A 2 C15B C 1.018(2) 0.3344(16) 0.8632(7) 0.063(4) Uani 0.375(4) 1 d P A 2 H15D H 1.0641 0.2483 0.8650 0.095 Uiso 0.375(4) 1 calc PR A 2 H15E H 1.1024 0.3957 0.8556 0.095 Uiso 0.375(4) 1 calc PR A 2 H15F H 0.9295 0.3377 0.8365 0.095 Uiso 0.375(4) 1 calc PR A 2 C16B C 1.061(3) 0.114(2) 0.9629(6) 0.060(4) Uani 0.375(4) 1 d P A 2 H16D H 1.1436 0.1522 0.9429 0.090 Uiso 0.375(4) 1 calc PR A 2 H16E H 1.0815 0.0225 0.9668 0.090 Uiso 0.375(4) 1 calc PR A 2 H16F H 1.0658 0.1544 0.9964 0.090 Uiso 0.375(4) 1 calc PR A 2 Cl1 Cl 0.94664(9) 0.74948(9) 0.89378(3) 0.0520(2) Uani 1 1 d . . . Cl2 Cl 0.58305(9) 0.83603(8) 0.94518(3) 0.0470(2) Uani 1 1 d . . . Fe1 Fe 0.67501(4) 0.78818(3) 0.866334(14) 0.02977(15) Uani 1 1 d . . . N1 N 0.4196(3) 0.8099(2) 0.82719(9) 0.0322(5) Uani 1 1 d . . . N2 N 0.7331(3) 0.7588(2) 0.78293(9) 0.0334(5) Uani 1 1 d . . . N3 N 0.8178(3) 0.2835(2) 0.93646(9) 0.0342(5) Uani 1 1 d . . . O1 O 0.7061(2) 0.96974(17) 0.84338(7) 0.0380(5) Uani 1 1 d . . . O2 O 0.8082(3) 1.1055(2) 0.78731(8) 0.0546(6) Uani 1 1 d . . . O3 O 0.6041(2) 0.60503(17) 0.86170(8) 0.0384(4) Uani 1 1 d . . . O4 O 0.4037(3) 0.46191(19) 0.84335(9) 0.0552(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0359(14) 0.0391(13) 0.0308(15) 0.0054(12) -0.0046(12) -0.0003(12) C2 0.0344(14) 0.0469(15) 0.0221(14) -0.0024(12) -0.0014(11) -0.0053(12) C3 0.0355(14) 0.0597(18) 0.0283(15) -0.0038(14) 0.0077(12) -0.0138(13) C4 0.0387(15) 0.0536(16) 0.0274(15) 0.0024(13) -0.0002(12) -0.0160(13) C5 0.0412(16) 0.065(2) 0.0449(19) -0.0196(17) 0.0030(14) 0.0106(15) C6 0.0296(13) 0.0418(14) 0.0379(16) 0.0007(13) 0.0059(12) -0.0042(11) C7 0.0421(16) 0.0447(16) 0.0486(19) -0.0002(15) 0.0055(14) 0.0096(13) C8 0.0427(16) 0.0388(15) 0.0274(14) 0.0055(12) 0.0009(12) -0.0046(12) C9A 0.051(3) 0.034(2) 0.033(3) 0.000(2) 0.007(2) -0.012(2) C10A 0.050(3) 0.034(2) 0.035(3) -0.005(2) 0.003(2) -0.006(2) C11A 0.051(3) 0.046(3) 0.026(3) 0.000(2) 0.008(2) -0.003(2) C12A 0.045(3) 0.045(3) 0.039(3) -0.001(2) -0.006(2) -0.001(2) C13A 0.055(7) 0.062(6) 0.038(8) 0.006(5) 0.003(5) -0.016(4) C14A 0.057(4) 0.047(4) 0.032(4) -0.007(3) 0.007(3) -0.005(3) C15A 0.060(6) 0.062(5) 0.048(4) 0.006(4) 0.025(4) -0.009(4) C16A 0.054(5) 0.055(4) 0.072(7) 0.003(6) -0.005(6) 0.023(3) C9B 0.037(4) 0.037(4) 0.032(4) 0.006(3) -0.006(3) 0.000(3) C10B 0.041(4) 0.063(5) 0.029(4) -0.002(4) -0.003(3) -0.006(4) C11B 0.046(5) 0.048(4) 0.055(6) 0.002(4) 0.012(4) -0.017(4) C12B 0.046(5) 0.042(4) 0.042(5) 0.000(4) -0.004(4) 0.002(3) C13B 0.023(6) 0.045(7) 0.041(14) 0.006(7) 0.001(6) -0.007(5) C14B 0.074(8) 0.067(9) 0.037(9) -0.011(7) 0.010(8) -0.002(6) C15B 0.067(11) 0.084(12) 0.040(7) 0.000(9) 0.016(7) -0.022(8) C16B 0.050(7) 0.065(7) 0.061(10) 0.008(9) -0.018(9) 0.004(5) Cl1 0.0314(4) 0.0853(6) 0.0379(4) -0.0074(4) -0.0060(3) 0.0024(4) Cl2 0.0539(4) 0.0615(5) 0.0271(4) 0.0004(3) 0.0124(3) -0.0066(4) Fe1 0.0293(2) 0.0367(2) 0.0233(2) 0.00029(16) 0.00148(16) -0.00216(15) N1 0.0306(11) 0.0349(11) 0.0314(13) 0.0028(10) 0.0036(10) 0.0010(9) N2 0.0288(11) 0.0452(12) 0.0264(12) -0.0060(10) 0.0031(10) -0.0008(10) N3 0.0390(12) 0.0357(12) 0.0275(12) 0.0031(10) -0.0004(10) -0.0073(10) O1 0.0486(11) 0.0388(10) 0.0275(11) -0.0024(8) 0.0089(9) -0.0098(9) O2 0.0745(15) 0.0533(13) 0.0364(12) 0.0043(11) 0.0059(11) -0.0261(11) O3 0.0364(10) 0.0339(9) 0.0437(12) 0.0047(9) -0.0054(9) 0.0008(8) O4 0.0636(14) 0.0373(11) 0.0626(15) 0.0085(11) -0.0103(12) -0.0114(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.483(4) . ? C1 C2 1.506(4) . ? C2 N2 1.484(3) . ? C3 N2 1.476(4) . ? C3 C4 1.508(4) . ? C4 O2 1.223(4) . ? C4 O1 1.290(3) . ? C5 N2 1.482(4) . ? C6 N1 1.479(3) . ? C6 C8 1.511(4) . ? C7 N1 1.483(3) . ? C8 O4 1.218(3) . ? C8 O3 1.286(3) . ? C9A C13A 1.48(2) . ? C9A N3 1.520(4) . ? C10A C14A 1.513(8) . ? C10A N3 1.573(5) . ? C11A N3 1.499(5) . ? C11A C15A 1.523(11) . ? C12A N3 1.476(5) . ? C12A C16A 1.513(13) . ? C9B N3 1.497(8) . ? C9B C13B 1.51(3) . ? C10B N3 1.438(8) . ? C10B C14B 1.493(19) . ? C11B C15B 1.523(19) . ? C11B N3 1.530(7) . ? C12B C16B 1.535(19) . ? C12B N3 1.622(8) . ? Cl1 Fe1 2.2953(8) . ? Cl2 Fe1 2.2835(8) . ? Fe1 O3 1.9677(18) . ? Fe1 O1 1.9795(18) . ? Fe1 N1 2.246(2) . ? Fe1 N2 2.271(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.4(2) . . ? N2 C2 C1 111.5(2) . . ? N2 C3 C4 113.5(2) . . ? O2 C4 O1 124.0(3) . . ? O2 C4 C3 119.7(2) . . ? O1 C4 C3 116.3(2) . . ? N1 C6 C8 113.0(2) . . ? O4 C8 O3 124.3(3) . . ? O4 C8 C6 119.6(3) . . ? O3 C8 C6 116.1(2) . . ? C13A C9A N3 118.1(10) . . ? C14A C10A N3 115.9(5) . . ? N3 C11A C15A 114.5(6) . . ? N3 C12A C16A 112.7(5) . . ? N3 C9B C13B 115.3(12) . . ? N3 C10B C14B 112.1(8) . . ? C15B C11B N3 119.8(9) . . ? C16B C12B N3 116.0(11) . . ? O3 Fe1 O1 157.69(8) . . ? O3 Fe1 N1 79.21(8) . . ? O1 Fe1 N1 84.46(8) . . ? O3 Fe1 N2 83.95(8) . . ? O1 Fe1 N2 78.34(8) . . ? N1 Fe1 N2 80.19(8) . . ? O3 Fe1 Cl2 98.50(6) . . ? O1 Fe1 Cl2 97.16(6) . . ? N1 Fe1 Cl2 91.99(6) . . ? N2 Fe1 Cl2 171.27(6) . . ? O3 Fe1 Cl1 96.99(6) . . ? O1 Fe1 Cl1 96.69(6) . . ? N1 Fe1 Cl1 170.43(6) . . ? N2 Fe1 Cl1 90.71(6) . . ? Cl2 Fe1 Cl1 97.28(3) . . ? C6 N1 C1 111.2(2) . . ? C6 N1 C7 110.2(2) . . ? C1 N1 C7 108.1(2) . . ? C6 N1 Fe1 105.36(16) . . ? C1 N1 Fe1 106.55(15) . . ? C7 N1 Fe1 115.32(18) . . ? C3 N2 C5 110.1(2) . . ? C3 N2 C2 111.5(2) . . ? C5 N2 C2 107.7(2) . . ? C3 N2 Fe1 105.01(16) . . ? C5 N2 Fe1 116.08(19) . . ? C2 N2 Fe1 106.42(15) . . ? C10B N3 C12A 78.8(4) . . ? C10B N3 C9B 117.7(5) . . ? C12A N3 C9B 158.8(4) . . ? C10B N3 C11A 157.9(4) . . ? C12A N3 C11A 115.1(3) . . ? C9B N3 C11A 54.3(3) . . ? C10B N3 C9A 79.0(4) . . ? C12A N3 C9A 109.9(3) . . ? C9B N3 C9A 64.0(3) . . ? C11A N3 C9A 109.6(3) . . ? C10B N3 C11B 112.8(5) . . ? C12A N3 C11B 74.4(4) . . ? C9B N3 C11B 107.9(5) . . ? C11A N3 C11B 59.2(4) . . ? C9A N3 C11B 168.2(4) . . ? C10B N3 C10A 51.7(4) . . ? C12A N3 C10A 107.8(3) . . ? C9B N3 C10A 93.3(4) . . ? C11A N3 C10A 106.3(3) . . ? C9A N3 C10A 107.8(3) . . ? C11B N3 C10A 80.5(4) . . ? C10B N3 C12B 107.7(5) . . ? C12A N3 C12B 56.0(3) . . ? C9B N3 C12B 104.1(4) . . ? C11A N3 C12B 94.4(4) . . ? C9A N3 C12B 69.9(3) . . ? C11B N3 C12B 105.6(4) . . ? C10A N3 C12B 158.3(4) . . ? C4 O1 Fe1 121.36(18) . . ? C8 O3 Fe1 121.53(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.410 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.060 # Attachment '- 2cnew.cif' data_2c _database_code_depnum_ccdc_archive 'CCDC 829867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(m2-Oxo)-bis(N,N'-dimethylethylenediamine-diacetato-N,N',O,O')-diiron(iii) ; _chemical_name_common ;'(m2-Oxo)-bis(N,N'-dimethylethylenediamine-diacetato- N,N',O,O')-diiron(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C17 H32 Fe2 N4 O10' _chemical_formula_sum 'C17 H32 Fe2 N4 O10' _chemical_formula_weight 564.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 12.8820(5) _cell_length_b 12.8820(5) _cell_length_c 13.7401(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2280.11(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4025 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 24.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max .4 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828423 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193 _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 Area _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12731 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2013 _reflns_number_gt 1971 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; disordered hydrogen atoms on solvent atom C100 were omitted ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 2013 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.314 _refine_ls_restrained_S_all 1.314 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2657(3) 0.2205(3) 0.1499(3) 0.0300(8) Uani 1 1 d . . . H1A H 0.2134 0.2622 0.1174 0.036 Uiso 1 1 calc R . . H1B H 0.3325 0.2537 0.1402 0.036 Uiso 1 1 calc R . . C2 C 0.2423(3) 0.2159(3) 0.2558(3) 0.0323(9) Uani 1 1 d . . . H2A H 0.2409 0.2854 0.2828 0.039 Uiso 1 1 calc R . . H2B H 0.2957 0.1766 0.2892 0.039 Uiso 1 1 calc R . . C3 C 0.1326(3) 0.1175(4) 0.3661(3) 0.0355(9) Uani 1 1 d . . . H3A H 0.0613 0.0993 0.3813 0.043 Uiso 1 1 calc R . . H3B H 0.1568 0.1665 0.4147 0.043 Uiso 1 1 calc R . . C4 C 0.2010(4) 0.0194(4) 0.3677(3) 0.0372(11) Uani 1 1 d . . . C5 C 0.0536(4) 0.2409(4) 0.2588(5) 0.0484(13) Uani 1 1 d . . . C6 C 0.2460(3) 0.1217(3) 0.0014(3) 0.0217(7) Uani 1 1 d . . . H6A H 0.2691 0.0589 -0.0311 0.026 Uiso 1 1 calc R . . H6B H 0.2828 0.1802 -0.0266 0.026 Uiso 1 1 calc R . . C7 C 0.3689(3) 0.0628(4) 0.1210(3) 0.0346(9) Uani 1 1 d . . . C8 C 0.1283(3) 0.1355(3) -0.0126(3) 0.0215(7) Uani 1 1 d . . . C100 C 0.5000 1.0000 0.3855(7) 0.109(5) Uani 1 2 d S . . Fe1 Fe 0.12810(3) 0.03114(3) 0.17275(4) 0.0194(2) Uani 1 1 d . . . N1 N 0.2677(2) 0.1148(2) 0.1062(2) 0.0229(7) Uani 1 1 d . . . N2 N 0.1380(3) 0.1642(3) 0.2701(2) 0.0286(7) Uani 1 1 d . . . O1 O 0.2141(2) -0.0241(2) 0.2836(2) 0.0290(6) Uani 1 1 d . . . O2 O 0.2377(3) -0.0113(4) 0.4440(2) 0.0583(11) Uani 1 1 d . . . O3 O 0.0712(2) 0.1178(2) 0.0575(2) 0.0213(5) Uani 1 1 d . . . O4 O 0.0984(2) 0.1649(2) -0.0960(2) 0.0246(6) Uani 1 1 d . . . O5 O 0.0000 0.0000 0.2148(3) 0.0266(8) Uani 1 2 d S . . O100 O 0.4228(6) 0.9049(6) 0.4355(6) 0.116(2) Uani 1 1 d . . . H100 H 0.3616 0.9195 0.4265 0.173 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0291(19) 0.0247(18) 0.036(2) -0.0044(16) -0.0039(18) -0.0111(14) C2 0.034(2) 0.032(2) 0.031(2) -0.0073(17) -0.0005(17) -0.0131(16) C3 0.031(2) 0.052(3) 0.0241(18) -0.0150(18) 0.0043(17) -0.0124(18) C4 0.036(2) 0.056(3) 0.019(2) 0.0031(19) -0.0053(17) -0.020(2) C5 0.042(3) 0.050(3) 0.053(3) -0.024(2) 0.000(2) 0.022(2) C6 0.0190(16) 0.0254(17) 0.0206(19) 0.0014(15) 0.0001(14) -0.0031(13) C7 0.0224(19) 0.052(2) 0.029(2) 0.0068(18) -0.0065(17) -0.0018(16) C8 0.0228(17) 0.0174(16) 0.0243(18) -0.0001(15) 0.0005(16) 0.0000(13) C100 0.141(11) 0.149(12) 0.037(4) 0.000 0.000 0.085(10) Fe1 0.0188(3) 0.0223(3) 0.0170(3) -0.00127(18) -0.0010(2) -0.00316(19) N1 0.0212(15) 0.0250(15) 0.0226(17) -0.0009(13) -0.0023(12) -0.0039(12) N2 0.0236(16) 0.0322(17) 0.0298(18) -0.0122(14) -0.0010(13) -0.0034(13) O1 0.0286(14) 0.0347(15) 0.0237(14) 0.0054(11) -0.0036(12) -0.0035(11) O2 0.068(2) 0.084(3) 0.0232(16) 0.0117(19) -0.0111(17) -0.018(2) O3 0.0219(12) 0.0217(12) 0.0205(12) -0.0001(11) 0.0010(11) -0.0019(9) O4 0.0237(12) 0.0286(13) 0.0216(13) 0.0079(11) -0.0031(11) -0.0032(10) O5 0.0239(18) 0.037(2) 0.0190(18) 0.000 0.000 -0.0076(15) O100 0.123(6) 0.116(6) 0.108(5) 0.008(4) -0.008(5) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.489(5) . ? C1 C2 1.487(6) . ? C2 N2 1.512(5) . ? C3 N2 1.452(6) . ? C3 C4 1.541(8) . ? C4 O2 1.216(6) . ? C4 O1 1.295(6) . ? C5 N2 1.478(6) . ? C6 N1 1.470(5) . ? C6 C8 1.538(5) . ? C7 N1 1.479(5) . ? C8 O3 1.233(5) . ? C8 O4 1.267(5) . ? C100 O100 1.720(7) . ? C100 O100 1.720(7) 2_675 ? Fe1 O5 1.7940(13) . ? Fe1 O1 2.014(3) . ? Fe1 O4 2.030(3) 3 ? Fe1 O3 2.071(3) . ? Fe1 N2 2.178(3) . ? Fe1 N1 2.287(3) . ? O4 Fe1 2.030(3) 4 ? O5 Fe1 1.7940(13) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.2(3) . . ? C1 C2 N2 109.0(3) . . ? N2 C3 C4 109.0(3) . . ? O2 C4 O1 125.3(5) . . ? O2 C4 C3 120.1(4) . . ? O1 C4 C3 114.6(4) . . ? N1 C6 C8 108.5(3) . . ? O3 C8 O4 125.5(4) . . ? O3 C8 C6 117.9(3) . . ? O4 C8 C6 116.5(3) . . ? O100 C100 O100 133.0(8) . 2_675 ? O5 Fe1 O1 100.57(13) . . ? O5 Fe1 O4 101.42(10) . 3 ? O1 Fe1 O4 88.50(12) . 3 ? O5 Fe1 O3 92.38(12) . . ? O1 Fe1 O3 164.46(11) . . ? O4 Fe1 O3 97.40(11) 3 . ? O5 Fe1 N2 91.83(11) . . ? O1 Fe1 N2 77.37(12) . . ? O4 Fe1 N2 162.23(12) 3 . ? O3 Fe1 N2 93.78(12) . . ? O5 Fe1 N1 163.23(9) . . ? O1 Fe1 N1 92.07(11) . . ? O4 Fe1 N1 89.79(12) 3 . ? O3 Fe1 N1 73.67(11) . . ? N2 Fe1 N1 80.13(12) . . ? C6 N1 C7 109.2(3) . . ? C6 N1 C1 109.7(3) . . ? C7 N1 C1 112.0(3) . . ? C6 N1 Fe1 105.7(2) . . ? C7 N1 Fe1 115.1(2) . . ? C1 N1 Fe1 104.8(2) . . ? C3 N2 C5 109.7(4) . . ? C3 N2 C2 110.0(3) . . ? C5 N2 C2 110.3(4) . . ? C3 N2 Fe1 103.2(2) . . ? C5 N2 Fe1 114.8(3) . . ? C2 N2 Fe1 108.6(2) . . ? C4 O1 Fe1 116.8(3) . . ? C8 O3 Fe1 119.1(2) . . ? C8 O4 Fe1 130.5(2) . 4 ? Fe1 O5 Fe1 142.4(2) 2 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.610 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.121 # Attachment '- 3anew.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 829868' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (PSH)(FeCl3N2O1) _chemical_formula_moiety 'C21 H34 Cl3 Fe N4 O2' _chemical_formula_sum 'C21 H34 Cl3 Fe N4 O2' _chemical_melting_point ? _chemical_formula_weight 536.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6852(15) _cell_length_b 10.9015(11) _cell_length_c 15.4710(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.284(2) _cell_angle_gamma 90.00 _cell_volume 2563.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4025 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.648159 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Area _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14432 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4512 _reflns_number_gt 3494 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Corresp. distances and ADP in two parts of disorder were restrained with SADI, SIMU and DELU ; _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^)+(0.1218P)^2^+12.7617P] 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 4512 _refine_ls_number_parameters 289 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.2692 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8975(10) 0.4841(12) 0.2520(10) 0.125(5) Uani 1 1 d U . . H1A H 0.9211 0.5667 0.2551 0.150 Uiso 1 1 calc R . . H1B H 0.9434 0.4317 0.2866 0.150 Uiso 1 1 calc R . . C2 C 0.8798(7) 0.4465(12) 0.1654(7) 0.096(3) Uani 1 1 d U . . H2A H 0.9354 0.4370 0.1493 0.115 Uiso 1 1 calc R . . H2B H 0.8478 0.5118 0.1286 0.115 Uiso 1 1 calc R . . C5 C 0.7873(6) 0.3356(10) 0.0459(6) 0.082(3) Uani 1 1 d D . . H5A H 0.8319 0.3387 0.0133 0.123 Uiso 1 1 calc R . . H5B H 0.7512 0.4077 0.0331 0.123 Uiso 1 1 calc R . . H5C H 0.7515 0.2640 0.0285 0.123 Uiso 1 1 calc R . . C6 C 0.7802(8) 0.6015(9) 0.2889(8) 0.098(3) Uani 1 1 d D . . H6A H 0.7385 0.5989 0.3251 0.147 Uiso 1 1 calc R . . H6B H 0.7499 0.6175 0.2281 0.147 Uiso 1 1 calc R . . H6C H 0.8223 0.6654 0.3100 0.147 Uiso 1 1 calc R . . C50 C 0.5852(5) 1.0152(8) 0.3791(6) 0.067(2) Uani 1 1 d . . . H50A H 0.5999 1.0292 0.4423 0.101 Uiso 1 1 calc R . . H50B H 0.5226 1.0209 0.3561 0.101 Uiso 1 1 calc R . . H50C H 0.6135 1.0758 0.3508 0.101 Uiso 1 1 calc R . . C51 C 0.5867(6) 0.8597(9) 0.2644(5) 0.074(2) Uani 1 1 d . . . H51A H 0.6100 0.9186 0.2302 0.111 Uiso 1 1 calc R . . H51B H 0.5236 0.8604 0.2458 0.111 Uiso 1 1 calc R . . H51C H 0.6080 0.7794 0.2552 0.111 Uiso 1 1 calc R . . C52 C 0.5636(6) 0.6009(8) 0.4134(7) 0.074(3) Uani 1 1 d . . . H52A H 0.6012 0.5868 0.3740 0.111 Uiso 1 1 calc R . . H52B H 0.5037 0.6078 0.3792 0.111 Uiso 1 1 calc R . . H52C H 0.5685 0.5334 0.4542 0.111 Uiso 1 1 calc R . . C53 C 0.5334(5) 0.7384(8) 0.5248(5) 0.059(2) Uani 1 1 d . . . H53A H 0.5360 0.6694 0.5638 0.088 Uiso 1 1 calc R . . H53B H 0.4738 0.7502 0.4908 0.088 Uiso 1 1 calc R . . H53C H 0.5532 0.8106 0.5595 0.088 Uiso 1 1 calc R . . C60 C 0.6837(5) 0.7147(6) 0.5056(5) 0.0465(16) Uani 1 1 d . . . C61 C 0.7187(6) 0.6401(7) 0.5760(6) 0.061(2) Uani 1 1 d . . . H61 H 0.6818 0.5897 0.5991 0.073 Uiso 1 1 calc R . . C62 C 0.8089(6) 0.6382(8) 0.6138(6) 0.069(2) Uani 1 1 d . . . H62 H 0.8312 0.5875 0.6625 0.083 Uiso 1 1 calc R . . C63 C 0.8640(6) 0.7074(7) 0.5817(5) 0.060(2) Uani 1 1 d . . . H63 H 0.9240 0.7043 0.6081 0.072 Uiso 1 1 calc R . . C64 C 0.8894(5) 0.8579(7) 0.4713(6) 0.059(2) Uani 1 1 d . . . H64 H 0.9497 0.8523 0.4955 0.071 Uiso 1 1 calc R . . C65 C 0.8586(5) 0.9347(7) 0.4025(6) 0.0583(19) Uani 1 1 d . . . H65 H 0.8979 0.9812 0.3798 0.070 Uiso 1 1 calc R . . C66 C 0.7680(5) 0.9452(7) 0.3648(5) 0.0530(18) Uani 1 1 d . . . H66 H 0.7471 0.9990 0.3177 0.064 Uiso 1 1 calc R . . C67 C 0.7106(4) 0.8758(6) 0.3976(4) 0.0415(15) Uani 1 1 d . . . C68 C 0.7393(4) 0.7926(6) 0.4694(4) 0.0388(14) Uani 1 1 d . . . C69 C 0.8320(5) 0.7858(6) 0.5076(5) 0.0469(16) Uani 1 1 d . . . C3A C 0.8893(9) 0.2297(14) 0.1687(10) 0.086(4) Uiso 0.80 1 d PD A 1 H3A1 H 0.9472 0.2538 0.1632 0.103 Uiso 0.80 1 calc PR A 1 H3A2 H 0.8703 0.1600 0.1298 0.103 Uiso 0.80 1 calc PR A 1 C4A C 0.8947(8) 0.1918(11) 0.2670(8) 0.071(3) Uiso 0.80 1 d PD A 1 C7A C 0.8612(11) 0.4689(16) 0.3949(10) 0.107(5) Uiso 0.80 1 d PD B 1 H7A1 H 0.8813 0.3862 0.4078 0.161 Uiso 0.80 1 calc PR B 1 H7A2 H 0.8155 0.4865 0.4244 0.161 Uiso 0.80 1 calc PR B 1 H7A3 H 0.9094 0.5245 0.4157 0.161 Uiso 0.80 1 calc PR B 1 C3B C 0.887(3) 0.428(3) 0.369(3) 0.085(15) Uiso 0.20 1 d PD B 2 H3B1 H 0.8755 0.4579 0.4243 0.102 Uiso 0.20 1 calc PR B 2 H3B2 H 0.9464 0.4525 0.3686 0.102 Uiso 0.20 1 calc PR B 2 C4B C 0.882(3) 0.285(3) 0.368(3) 0.093(16) Uiso 0.20 1 d PD B 2 C7B C 0.868(2) 0.198(2) 0.141(2) 0.045(8) Uiso 0.20 1 d PD A 2 H7B1 H 0.9180 0.2002 0.1165 0.067 Uiso 0.20 1 calc PR A 2 H7B2 H 0.8238 0.1444 0.1058 0.067 Uiso 0.20 1 calc PR A 2 H7B3 H 0.8847 0.1673 0.2012 0.067 Uiso 0.20 1 calc PR A 2 Cl1 Cl 0.67281(15) 0.14743(18) 0.16361(15) 0.0661(6) Uani 1 1 d . . . Cl2 Cl 0.66288(17) 0.3321(2) 0.34427(16) 0.0747(7) Uani 1 1 d . . . Cl3 Cl 0.64255(15) 0.4585(2) 0.13600(17) 0.0805(7) Uani 1 1 d . . . Fe1 Fe 0.73609(7) 0.32490(9) 0.23331(7) 0.0480(4) Uani 1 1 d D . . H99 H 0.591(5) 0.846(7) 0.390(5) 0.040(19) Uiso 1 1 d . . . N1 N 0.8255(5) 0.4842(6) 0.2943(5) 0.0671(18) Uani 1 1 d D B . N2 N 0.8286(4) 0.3302(6) 0.1413(4) 0.0548(15) Uani 1 1 d D A . N30 N 0.6153(4) 0.8918(6) 0.3607(4) 0.0457(14) Uani 1 1 d . . . N31 N 0.5901(4) 0.7157(5) 0.4639(4) 0.0469(14) Uani 1 1 d . . . O1A O 0.8429(11) 0.237(2) 0.3118(14) 0.161(15) Uiso 0.80 1 d PDU A 1 O2A O 0.9571(7) 0.1257(10) 0.3023(7) 0.108(3) Uiso 0.80 1 d PD A 1 O1B O 0.8327(6) 0.2244(9) 0.3020(7) 0.016(3) Uiso 0.40(3) 1 d PDU B 2 O2B O 0.936(2) 0.233(3) 0.427(2) 0.116(13) Uiso 0.20 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.162(12) 0.089(8) 0.148(9) -0.044(8) 0.082(10) -0.063(8) C2 0.084(7) 0.114(9) 0.089(6) 0.006(6) 0.021(6) -0.044(6) C5 0.083(6) 0.109(8) 0.056(5) -0.005(5) 0.020(5) -0.004(6) C6 0.136(10) 0.053(5) 0.103(8) -0.016(5) 0.023(7) 0.020(6) C50 0.051(4) 0.060(5) 0.085(6) 0.000(4) 0.008(4) 0.005(4) C51 0.086(6) 0.084(6) 0.044(4) 0.005(4) 0.001(4) -0.016(5) C52 0.071(5) 0.059(5) 0.099(7) -0.035(5) 0.037(5) -0.019(4) C53 0.059(5) 0.058(5) 0.067(5) -0.011(4) 0.031(4) -0.006(4) C60 0.063(4) 0.032(3) 0.051(4) -0.004(3) 0.025(3) -0.002(3) C61 0.079(6) 0.042(4) 0.068(5) 0.012(4) 0.031(4) 0.006(4) C62 0.084(6) 0.053(5) 0.071(5) 0.022(4) 0.020(5) 0.021(4) C63 0.062(5) 0.051(4) 0.064(5) 0.001(4) 0.007(4) 0.016(4) C64 0.048(4) 0.057(5) 0.074(5) -0.009(4) 0.022(4) 0.003(4) C65 0.057(5) 0.056(4) 0.070(5) 0.001(4) 0.031(4) -0.007(4) C66 0.067(5) 0.048(4) 0.049(4) 0.010(3) 0.024(4) 0.001(3) C67 0.048(4) 0.040(3) 0.039(3) -0.006(3) 0.015(3) -0.001(3) C68 0.052(4) 0.030(3) 0.035(3) -0.007(3) 0.013(3) -0.001(3) C69 0.052(4) 0.039(4) 0.050(4) -0.007(3) 0.012(3) 0.006(3) Cl1 0.0807(14) 0.0494(11) 0.0684(13) -0.0051(9) 0.0189(10) -0.0078(9) Cl2 0.1050(17) 0.0566(12) 0.0787(14) 0.0009(10) 0.0532(13) 0.0089(11) Cl3 0.0689(13) 0.0804(15) 0.0903(16) 0.0291(13) 0.0158(12) 0.0330(12) Fe1 0.0577(7) 0.0361(6) 0.0524(6) 0.0054(4) 0.0176(5) 0.0088(4) N1 0.082(5) 0.047(4) 0.076(5) 0.003(3) 0.025(4) 0.003(3) N2 0.055(4) 0.057(4) 0.052(4) 0.009(3) 0.011(3) 0.011(3) N30 0.050(3) 0.045(3) 0.042(3) 0.004(3) 0.011(3) -0.009(3) N31 0.057(3) 0.037(3) 0.053(3) -0.007(3) 0.024(3) -0.008(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 C1 C2 1.362(16) . ? C1 N1 1.439(13) . ? C2 N2 1.498(12) . ? C5 N2 1.459(10) . ? C6 N1 1.455(11) . ? C50 N30 1.477(10) . ? C51 N30 1.487(10) . ? C52 N31 1.481(9) . ? C53 N31 1.467(9) . ? C60 C61 1.362(11) . ? C60 C68 1.427(9) . ? C60 N31 1.451(9) . ? C61 C62 1.392(12) . ? C62 C63 1.332(12) . ? C63 C69 1.419(10) . ? C64 C65 1.347(11) . ? C64 C69 1.411(11) . ? C65 C66 1.402(11) . ? C66 C67 1.365(10) . ? C67 C68 1.418(9) . ? C67 N30 1.473(9) . ? C68 C69 1.430(10) . ? C3A N2 1.445(14) . ? C3A C4A 1.558(18) . ? C4A O2A 1.230(14) . ? C4A O1A 1.29(2) . ? C7A N1 1.527(15) . ? C3B N1 1.45(2) . ? C3B C4B 1.56(3) . ? C4B O2B 1.22(2) . ? C4B O1B 1.30(3) . ? C7B N2 1.57(2) . ? Cl1 Fe1 2.316(2) . ? Cl2 Fe1 2.290(2) . ? Cl3 Fe1 2.335(2) . ? Fe1 O1B 1.957(8) . ? Fe1 O1A 2.051(13) . ? Fe1 N2 2.271(6) . ? Fe1 N1 2.285(7) . ? 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 C2 C1 N1 117.1(12) . . ? C1 C2 N2 117.8(9) . . ? C61 C60 C68 120.3(7) . . ? C61 C60 N31 121.6(6) . . ? C68 C60 N31 118.1(6) . . ? C60 C61 C62 120.8(7) . . ? C63 C62 C61 121.4(8) . . ? C62 C63 C69 120.7(8) . . ? C65 C64 C69 121.4(7) . . ? C64 C65 C66 120.5(7) . . ? C67 C66 C65 119.6(7) . . ? C66 C67 C68 122.3(6) . . ? C66 C67 N30 119.3(6) . . ? C68 C67 N30 118.3(6) . . ? C67 C68 C60 125.5(6) . . ? C67 C68 C69 116.8(6) . . ? C60 C68 C69 117.7(6) . . ? C64 C69 C63 121.6(7) . . ? C64 C69 C68 119.3(7) . . ? C63 C69 C68 119.1(7) . . ? N2 C3A C4A 111.2(11) . . ? O2A C4A O1A 121.5(13) . . ? O2A C4A C3A 115.7(11) . . ? O1A C4A C3A 122.4(12) . . ? N1 C3B C4B 113(3) . . ? O2B C4B O1B 121(2) . . ? O2B C4B C3B 115(2) . . ? O1B C4B C3B 122(3) . . ? O1B Fe1 O1A 6.1(8) . . ? O1B Fe1 N2 80.0(3) . . ? O1A Fe1 N2 80.1(6) . . ? O1B Fe1 N1 83.5(4) . . ? O1A Fe1 N1 77.5(7) . . ? N2 Fe1 N1 79.5(3) . . ? O1B Fe1 Cl2 94.4(3) . . ? O1A Fe1 Cl2 93.4(6) . . ? N2 Fe1 Cl2 170.20(18) . . ? N1 Fe1 Cl2 91.96(19) . . ? O1B Fe1 Cl1 88.3(3) . . ? O1A Fe1 Cl1 94.4(7) . . ? N2 Fe1 Cl1 89.78(18) . . ? N1 Fe1 Cl1 167.5(2) . . ? Cl2 Fe1 Cl1 98.11(9) . . ? O1B Fe1 Cl3 168.1(3) . . ? O1A Fe1 Cl3 165.1(6) . . ? N2 Fe1 Cl3 88.67(16) . . ? N1 Fe1 Cl3 90.93(19) . . ? Cl2 Fe1 Cl3 96.34(9) . . ? Cl1 Fe1 Cl3 95.28(10) . . ? C1 N1 C3B 85(2) . . ? C1 N1 C6 113.7(9) . . ? C3B N1 C6 129.6(19) . . ? C1 N1 C7A 109.3(10) . . ? C3B N1 C7A 30(2) . . ? C6 N1 C7A 101.9(9) . . ? C1 N1 Fe1 106.4(6) . . ? C3B N1 Fe1 103.2(16) . . ? C6 N1 Fe1 113.8(6) . . ? C7A N1 Fe1 111.8(7) . . ? C3A N2 C5 115.1(8) . . ? C3A N2 C2 107.1(9) . . ? C5 N2 C2 107.2(7) . . ? C3A N2 C7B 22.1(13) . . ? C5 N2 C7B 96.4(12) . . ? C2 N2 C7B 126.5(16) . . ? C3A N2 Fe1 105.8(7) . . ? C5 N2 Fe1 116.2(5) . . ? C2 N2 Fe1 104.6(6) . . ? C7B N2 Fe1 106.6(14) . . ? C67 N30 C50 112.0(6) . . ? C67 N30 C51 112.8(6) . . ? C50 N30 C51 112.0(7) . . ? C60 N31 C53 115.0(6) . . ? C60 N31 C52 110.5(6) . . ? C53 N31 C52 110.2(6) . . ? C4A O1A Fe1 113.0(13) . . ? C4B O1B Fe1 111.9(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.702 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.132