Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 610298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dinitrosyl-bis[tris(hydroxymethyl)phoshine]iron(II) ; _chemical_name_common ? _chemical_formula_moiety 'C6 H18 Fe N2 O8 P2' _chemical_formula_sum 'C6 H18 Fe N2 O8 P2' _chemical_formula_weight 364.01 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8833(7) _cell_length_b 9.4457(9) _cell_length_c 11.4636(10) _cell_angle_alpha 89.368(11) _cell_angle_beta 72.801(11) _cell_angle_gamma 77.584(11) _cell_volume 694.25(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 30.25 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.7035 _exptl_absorpt_correction_T_max 0.7930 _exptl_special_details ; The crystals were "sticky" like honey and it was difficult to cut a single crystal from a large block to a suitable size for the X-ray measurement. The material was protected and cleaned in perfluorpolyetheroil, mounted on a glass fibre of a gonio- meterhead and subsequently transferred to the diffractometer. There the crystal was protected and cooled down to 153 K by a nitrogen stream of an Oxford Cryosystem. ; _diffrn_ambient_temperature 153(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 3.50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11490 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 30.27 _reflns_number_total 3765 _reflns_number_gt 3064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+2.6052P] 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 3765 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.30541(7) 0.74701(6) 0.38212(4) 0.01093(14) Uani 1 d . . . P1 P 0.53901(13) 0.56755(10) 0.25950(8) 0.01060(19) Uani 1 d . . . P2 P 0.20972(13) 0.90236(10) 0.24976(8) 0.01110(19) Uani 1 d . . . N1 N 0.0895(5) 0.6941(4) 0.4560(3) 0.0154(6) Uani 1 d . . . O1 O -0.0629(5) 0.6602(4) 0.5184(3) 0.0302(8) Uani 1 d . . . N2 N 0.4442(5) 0.8099(4) 0.4572(3) 0.0153(6) Uani 1 d . . . O2 O 0.5345(5) 0.8452(4) 0.5211(3) 0.0318(8) Uani 1 d . . . C1 C 0.4430(5) 0.4087(4) 0.2259(4) 0.0161(7) Uani 1 d . . . H1A H 0.5533 0.3459 0.1597 0.019 Uiso 1 calc R . . H1B H 0.4146 0.3517 0.2996 0.019 Uiso 1 calc R . . O3 O 0.2580(5) 0.4489(3) 0.1898(3) 0.0226(6) Uani 1 d . . . H3 H 0.2558 0.5284 0.1561 0.034 Uiso 1 calc R . . C2 C 0.6991(6) 0.6032(4) 0.1057(3) 0.0158(7) Uani 1 d . . . H2A H 0.8112 0.5161 0.0717 0.019 Uiso 1 calc R . . H2B H 0.6106 0.6222 0.0506 0.019 Uiso 1 calc R . . O4 O 0.7894(4) 0.7238(4) 0.1102(3) 0.0278(7) Uani 1 d . . . H4 H 0.6960 0.8006 0.1244 0.042 Uiso 1 calc R . . C3 C 0.7426(6) 0.4806(4) 0.3277(4) 0.0169(7) Uani 1 d . . . H3A H 0.8158 0.5543 0.3435 0.020 Uiso 1 calc R . . H3B H 0.6759 0.4434 0.4072 0.020 Uiso 1 calc R . . O5 O 0.8918(4) 0.3636(3) 0.2512(3) 0.0207(6) Uani 1 d . . . H5 H 1.0078 0.3865 0.2258 0.031 Uiso 1 calc R . . C4 C 0.2357(6) 0.8451(4) 0.0910(3) 0.0165(7) Uani 1 d . . . H4A H 0.1389 0.9174 0.0597 0.020 Uiso 1 calc R . . H4B H 0.3794 0.8435 0.0389 0.020 Uiso 1 calc R . . O6 O 0.1925(4) 0.7058(3) 0.0813(3) 0.0207(6) Uani 1 d . . . H6 H 0.0629 0.7136 0.1005 0.031 Uiso 1 calc R . . C5 C -0.0691(6) 0.9941(5) 0.3082(4) 0.0195(8) Uani 1 d . . . H5A H -0.1530 0.9192 0.3283 0.023 Uiso 1 calc R . . H5B H -0.0918 1.0510 0.3849 0.023 Uiso 1 calc R . . O7 O -0.1433(4) 1.0884(3) 0.2254(3) 0.0214(6) Uani 1 d . . . H7 H -0.1445 1.1744 0.2441 0.032 Uiso 1 calc R . . C6 C 0.3390(5) 1.0567(4) 0.2199(4) 0.0152(7) Uani 1 d . . . H6A H 0.2790 1.1239 0.1663 0.018 Uiso 1 calc R . . H6B H 0.3183 1.1108 0.2977 0.018 Uiso 1 calc R . . O8 O 0.5559(4) 1.0005(4) 0.1619(3) 0.0219(6) Uani 1 d . . . H8 H 0.6258 1.0398 0.1953 0.033 Uiso 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 0.0095(2) 0.0122(3) 0.0101(2) -0.00078(18) -0.00261(16) -0.00078(17) P1 0.0084(4) 0.0113(4) 0.0120(4) -0.0009(3) -0.0033(3) -0.0014(3) P2 0.0088(4) 0.0108(4) 0.0136(4) -0.0003(3) -0.0037(3) -0.0015(3) N1 0.0145(13) 0.0144(16) 0.0163(14) 0.0007(12) -0.0054(11) 0.0004(11) O1 0.0158(13) 0.042(2) 0.0313(16) 0.0075(15) -0.0014(12) -0.0113(13) N2 0.0145(13) 0.0130(16) 0.0160(14) -0.0015(12) -0.0040(11) 0.0011(11) O2 0.0271(16) 0.038(2) 0.0362(18) -0.0091(15) -0.0215(14) -0.0027(14) C1 0.0117(15) 0.0136(18) 0.0247(18) -0.0010(14) -0.0061(13) -0.0058(12) O3 0.0207(13) 0.0207(16) 0.0352(16) 0.0066(13) -0.0175(12) -0.0102(11) C2 0.0149(15) 0.0143(18) 0.0154(15) 0.0001(13) -0.0005(12) -0.0034(13) O4 0.0138(13) 0.0181(16) 0.0456(19) -0.0011(14) 0.0022(12) -0.0067(11) C3 0.0170(16) 0.0114(17) 0.0239(18) -0.0011(14) -0.0101(14) -0.0006(13) O5 0.0122(11) 0.0112(14) 0.0379(16) -0.0051(12) -0.0085(11) 0.0007(10) C4 0.0162(16) 0.022(2) 0.0135(15) 0.0003(14) -0.0068(12) -0.0053(13) O6 0.0189(13) 0.0176(15) 0.0283(15) -0.0032(12) -0.0117(11) -0.0029(11) C5 0.0110(15) 0.020(2) 0.0242(18) -0.0022(15) -0.0035(13) 0.0016(13) O7 0.0155(12) 0.0162(14) 0.0348(16) 0.0004(12) -0.0125(11) -0.0015(10) C6 0.0143(15) 0.0075(16) 0.0267(18) 0.0053(14) -0.0072(13) -0.0074(12) O8 0.0129(12) 0.0227(16) 0.0317(15) 0.0017(13) -0.0064(11) -0.0075(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.656(3) . yes Fe1 N2 1.658(3) . yes Fe1 P1 2.2313(10) . yes Fe1 P2 2.2396(11) . yes P1 C3 1.840(4) . yes P1 C1 1.850(4) . yes P1 C2 1.853(4) . yes P2 C6 1.844(4) . yes P2 C5 1.849(4) . yes P2 C4 1.851(4) . yes N1 O1 1.188(4) . yes N2 O2 1.182(4) . yes C1 O3 1.427(4) . yes C1 H1A 0.9900 . yes C1 H1B 0.9900 . yes O3 H3 0.8400 . yes C2 O4 1.418(5) . yes C2 H2A 0.9900 . yes C2 H2B 0.9900 . yes O4 H4 0.8400 . yes C3 O5 1.430(4) . yes C3 H3A 0.9900 . yes C3 H3B 0.9900 . yes O5 H5 0.8400 . yes C4 O6 1.422(5) . yes C4 H4A 0.9900 . yes C4 H4B 0.9900 . yes O6 H6 0.8400 . yes C5 O7 1.423(5) . yes C5 H5A 0.9900 . yes C5 H5B 0.9900 . yes O7 H7 0.8400 . yes C6 O8 1.426(4) . yes C6 H6A 0.9900 . yes C6 H6B 0.9900 . yes O8 H8 0.8400 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 121.10(16) . . yes N1 Fe1 P1 111.47(12) . . yes N2 Fe1 P1 103.08(11) . . yes N1 Fe1 P2 104.26(11) . . yes N2 Fe1 P2 112.81(12) . . yes P1 Fe1 P2 102.81(4) . . yes C3 P1 C1 101.04(18) . . yes C3 P1 C2 101.16(18) . . yes C1 P1 C2 101.98(17) . . yes C3 P1 Fe1 112.00(12) . . yes C1 P1 Fe1 116.86(12) . . yes C2 P1 Fe1 120.94(13) . . yes C6 P2 C5 102.39(18) . . yes C6 P2 C4 99.77(18) . . yes C5 P2 C4 102.26(17) . . yes C6 P2 Fe1 115.58(13) . . yes C5 P2 Fe1 111.51(14) . . yes C4 P2 Fe1 122.66(14) . . yes O1 N1 Fe1 174.1(3) . . yes O2 N2 Fe1 172.6(4) . . yes O3 C1 P1 112.7(3) . . yes O3 C1 H1A 109.1 . . yes P1 C1 H1A 109.1 . . yes O3 C1 H1B 109.1 . . yes P1 C1 H1B 109.1 . . yes H1A C1 H1B 107.8 . . yes C1 O3 H3 109.5 . . yes O4 C2 P1 111.5(3) . . yes O4 C2 H2A 109.3 . . yes P1 C2 H2A 109.3 . . yes O4 C2 H2B 109.3 . . yes P1 C2 H2B 109.3 . . yes H2A C2 H2B 108.0 . . yes C2 O4 H4 109.5 . . yes O5 C3 P1 112.8(3) . . yes O5 C3 H3A 109.0 . . yes P1 C3 H3A 109.0 . . yes O5 C3 H3B 109.0 . . yes P1 C3 H3B 109.0 . . yes H3A C3 H3B 107.8 . . yes C3 O5 H5 109.5 . . yes O6 C4 P2 112.9(3) . . yes O6 C4 H4A 109.0 . . yes P2 C4 H4A 109.0 . . yes O6 C4 H4B 109.0 . . yes P2 C4 H4B 109.0 . . yes H4A C4 H4B 107.8 . . yes C4 O6 H6 109.5 . . yes O7 C5 P2 114.4(3) . . yes O7 C5 H5A 108.7 . . yes P2 C5 H5A 108.7 . . yes O7 C5 H5B 108.7 . . yes P2 C5 H5B 108.7 . . yes H5A C5 H5B 107.6 . . yes C5 O7 H7 109.5 . . yes O8 C6 P2 108.0(2) . . yes O8 C6 H6A 110.1 . . yes P2 C6 H6A 110.1 . . yes O8 C6 H6B 110.1 . . yes P2 C6 H6B 110.1 . . yes H6A C6 H6B 108.4 . . yes C6 O8 H8 109.5 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 P1 C3 -100.64(19) . . . . yes N2 Fe1 P1 C3 30.8(2) . . . . yes P2 Fe1 P1 C3 148.21(15) . . . . yes N1 Fe1 P1 C1 15.22(19) . . . . yes N2 Fe1 P1 C1 146.62(19) . . . . yes P2 Fe1 P1 C1 -95.93(15) . . . . yes N1 Fe1 P1 C2 140.31(18) . . . . yes N2 Fe1 P1 C2 -88.30(19) . . . . yes P2 Fe1 P1 C2 29.16(15) . . . . yes N1 Fe1 P2 C6 145.08(18) . . . . yes N2 Fe1 P2 C6 11.83(18) . . . . yes P1 Fe1 P2 C6 -98.50(14) . . . . yes N1 Fe1 P2 C5 28.69(19) . . . . yes N2 Fe1 P2 C5 -104.55(18) . . . . yes P1 Fe1 P2 C5 145.12(15) . . . . yes N1 Fe1 P2 C4 -92.89(18) . . . . yes N2 Fe1 P2 C4 133.87(18) . . . . yes P1 Fe1 P2 C4 23.54(15) . . . . yes C3 P1 C1 O3 170.3(3) . . . . yes C2 P1 C1 O3 -85.6(3) . . . . yes Fe1 P1 C1 O3 48.6(3) . . . . yes C3 P1 C2 O4 -76.2(3) . . . . yes C1 P1 C2 O4 179.8(3) . . . . yes Fe1 P1 C2 O4 48.1(3) . . . . yes C1 P1 C3 O5 53.8(3) . . . . yes C2 P1 C3 O5 -50.9(3) . . . . yes Fe1 P1 C3 O5 179.0(2) . . . . yes C6 P2 C4 O6 166.2(3) . . . . yes C5 P2 C4 O6 -88.7(3) . . . . yes Fe1 P2 C4 O6 37.1(3) . . . . yes C6 P2 C5 O7 59.2(3) . . . . yes C4 P2 C5 O7 -43.8(3) . . . . yes Fe1 P2 C5 O7 -176.6(2) . . . . yes C5 P2 C6 O8 -174.0(3) . . . . yes C4 P2 C6 O8 -69.0(3) . . . . yes Fe1 P2 C6 O8 64.6(3) . . . . yes _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 30.27 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 2.127 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.161 data_4 _database_code_depnum_ccdc_archive 'CCDC 610300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dinitrosyl-(1,2-bis(hydroxymethylphosphino)ethane)iron(II) ; _chemical_name_common ? _chemical_formula_moiety 'C6 H16 Fe N2 O6 P2' _chemical_formula_sum 'C6 H16 Fe N2 O6 P2' _chemical_formula_weight 330.00 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6992(10) _cell_length_b 8.5741(11) _cell_length_c 11.2515(15) _cell_angle_alpha 95.919(15) _cell_angle_beta 106.994(15) _cell_angle_gamma 109.827(14) _cell_volume 651.11(18) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 30.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.6009 _exptl_absorpt_correction_T_max 0.7201 _exptl_special_details ; All positions of H-atoms were calculated after each refinement cycle except of two hydroxyl H-atoms which were freely refined because they belong to strong hydrogen bonding systems. ; _diffrn_ambient_temperature 183(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.40 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13195 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 30.39 _reflns_number_total 3544 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0611P] 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 3544 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.15588(3) 0.75961(3) 0.40203(2) 0.01298(7) Uani 1 d . . . P1 P 0.18729(5) 0.91923(5) 0.25741(4) 0.01357(9) Uani 1 d . . . P2 P -0.14151(5) 0.60141(5) 0.26103(4) 0.01309(9) Uani 1 d . . . N1 N 0.1458(2) 0.87262(17) 0.52665(14) 0.0190(3) Uani 1 d . . . O1 O 0.1409(2) 0.94500(19) 0.62114(15) 0.0321(3) Uani 1 d . . . N2 N 0.26553(19) 0.62287(17) 0.41146(13) 0.0165(3) Uani 1 d . . . O2 O 0.3260(2) 0.51375(18) 0.42513(15) 0.0297(3) Uani 1 d . . . C1 C -0.0556(2) 0.85527(19) 0.13046(16) 0.0169(3) Uani 1 d . . . H1A H -0.1313 0.9168 0.1564 0.020 Uiso 1 calc R . . H1B H -0.0375 0.8849 0.0510 0.020 Uiso 1 calc R . . C2 C -0.1695(2) 0.66227(19) 0.10687(16) 0.0170(3) Uani 1 d . . . H2A H -0.1176 0.6004 0.0563 0.020 Uiso 1 calc R . . H2B H -0.3108 0.6318 0.0582 0.020 Uiso 1 calc R . . C3 C 0.3510(2) 0.9122(2) 0.16699(18) 0.0207(3) Uani 1 d . . . H3A H 0.3515 0.9943 0.1112 0.025 Uiso 1 calc R . . H3B H 0.4872 0.9472 0.2274 0.025 Uiso 1 calc R . . O3 O 0.2903(2) 0.74676(17) 0.09088(13) 0.0262(3) Uani 1 d . . . H3 H 0.3397 0.6888 0.1349 0.039 Uiso 1 calc R . . C4 C 0.2687(2) 1.15128(19) 0.31135(17) 0.0188(3) Uani 1 d . . . H4A H 0.2022 1.1740 0.3703 0.023 Uiso 1 calc R . . H4B H 0.4123 1.2007 0.3592 0.023 Uiso 1 calc R . . O4 O 0.22705(18) 1.23332(14) 0.20824(13) 0.0193(2) Uani 1 d . . . H4 H 0.137(4) 1.254(3) 0.203(3) 0.034(7) Uiso 1 d . . . C5 C -0.3479(2) 0.6245(2) 0.30140(17) 0.0184(3) Uani 1 d . . . H5A H -0.3604 0.5714 0.3742 0.022 Uiso 1 calc R . . H5B H -0.3184 0.7470 0.3287 0.022 Uiso 1 calc R . . O5 O -0.53160(16) 0.54812(16) 0.19692(13) 0.0195(2) Uani 1 d . . . H5 H -0.586(4) 0.469(4) 0.210(3) 0.041(8) Uiso 1 d . . . C6 C -0.2183(3) 0.3676(2) 0.22179(18) 0.0209(3) Uani 1 d . . . H6A H -0.2080 0.3251 0.3011 0.025 Uiso 1 calc R . . H6B H -0.3580 0.3148 0.1647 0.025 Uiso 1 calc R . . O6 O -0.1008(2) 0.31782(17) 0.16125(13) 0.0256(3) Uani 1 d . . . H6 H -0.1524 0.3022 0.0819 0.038 Uiso 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 0.01397(11) 0.01203(11) 0.01094(14) 0.00242(8) 0.00194(8) 0.00475(8) P1 0.01429(17) 0.01018(16) 0.0132(2) 0.00200(13) 0.00298(13) 0.00288(13) P2 0.01359(16) 0.01100(16) 0.0124(2) 0.00305(13) 0.00330(13) 0.00304(12) N1 0.0222(6) 0.0160(6) 0.0168(8) 0.0030(5) 0.0038(5) 0.0080(5) O1 0.0458(8) 0.0308(7) 0.0219(9) -0.0020(6) 0.0138(6) 0.0180(6) N2 0.0166(6) 0.0193(6) 0.0121(7) 0.0036(5) 0.0029(5) 0.0071(5) O2 0.0393(7) 0.0330(7) 0.0298(8) 0.0122(6) 0.0133(6) 0.0271(6) C1 0.0179(7) 0.0143(6) 0.0138(8) 0.0046(5) 0.0018(5) 0.0034(5) C2 0.0175(6) 0.0150(7) 0.0113(8) 0.0018(5) 0.0024(5) 0.0003(5) C3 0.0230(7) 0.0198(7) 0.0224(10) 0.0052(6) 0.0115(6) 0.0089(6) O3 0.0377(7) 0.0269(6) 0.0177(7) 0.0016(5) 0.0053(5) 0.0215(6) C4 0.0225(7) 0.0119(6) 0.0177(9) 0.0023(5) 0.0040(6) 0.0044(5) O4 0.0216(5) 0.0131(5) 0.0225(7) 0.0064(4) 0.0069(4) 0.0061(4) C5 0.0149(6) 0.0192(7) 0.0182(9) 0.0021(6) 0.0042(5) 0.0050(5) O5 0.0133(5) 0.0186(6) 0.0227(7) 0.0071(5) 0.0031(4) 0.0036(4) C6 0.0264(8) 0.0127(6) 0.0226(10) 0.0039(6) 0.0083(6) 0.0066(6) O6 0.0310(6) 0.0288(6) 0.0187(7) 0.0006(5) 0.0030(5) 0.0201(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.6563(13) . yes Fe1 N1 1.6567(16) . yes Fe1 P2 2.2193(7) . yes Fe1 P1 2.2459(6) . yes P1 C4 1.8446(16) . yes P1 C3 1.8481(18) . yes P1 C1 1.8493(16) . yes P2 C2 1.8363(17) . yes P2 C5 1.8404(17) . yes P2 C6 1.8503(16) . yes N1 O1 1.192(2) . yes N2 O2 1.1827(18) . yes C1 C2 1.538(2) . yes C1 H1A 0.9900 . yes C1 H1B 0.9900 . yes C2 H2A 0.9900 . yes C2 H2B 0.9900 . yes C3 O3 1.425(2) . yes C3 H3A 0.9900 . yes C3 H3B 0.9900 . yes O3 H3 0.8400 . yes C4 O4 1.431(2) . yes C4 H4A 0.9900 . yes C4 H4B 0.9900 . yes O4 H4 0.76(3) . yes C5 O5 1.433(2) . yes C5 H5A 0.9900 . yes C5 H5B 0.9900 . yes O5 H5 0.72(3) . yes C6 O6 1.424(2) . yes C6 H6A 0.9900 . yes C6 H6B 0.9900 . yes O6 H6 0.8400 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 124.28(7) . . yes N2 Fe1 P2 101.74(5) . . yes N1 Fe1 P2 112.17(5) . . yes N2 Fe1 P1 116.96(5) . . yes N1 Fe1 P1 108.63(5) . . yes P2 Fe1 P1 85.80(2) . . yes C4 P1 C3 100.31(8) . . yes C4 P1 C1 104.09(7) . . yes C3 P1 C1 103.04(8) . . yes C4 P1 Fe1 117.87(6) . . yes C3 P1 Fe1 120.43(6) . . yes C1 P1 Fe1 109.05(5) . . yes C2 P2 C5 103.90(8) . . yes C2 P2 C6 104.61(8) . . yes C5 P2 C6 102.24(8) . . yes C2 P2 Fe1 110.48(5) . . yes C5 P2 Fe1 115.14(6) . . yes C6 P2 Fe1 118.92(6) . . yes O1 N1 Fe1 175.11(13) . . yes O2 N2 Fe1 171.14(14) . . yes C2 C1 P1 109.38(10) . . yes C2 C1 H1A 109.8 . . yes P1 C1 H1A 109.8 . . yes C2 C1 H1B 109.8 . . yes P1 C1 H1B 109.8 . . yes H1A C1 H1B 108.2 . . yes C1 C2 P2 109.07(11) . . yes C1 C2 H2A 109.9 . . yes P2 C2 H2A 109.9 . . yes C1 C2 H2B 109.9 . . yes P2 C2 H2B 109.9 . . yes H2A C2 H2B 108.3 . . yes O3 C3 P1 112.00(12) . . yes O3 C3 H3A 109.2 . . yes P1 C3 H3A 109.2 . . yes O3 C3 H3B 109.2 . . yes P1 C3 H3B 109.2 . . yes H3A C3 H3B 107.9 . . yes C3 O3 H3 109.5 . . yes O4 C4 P1 112.85(11) . . yes O4 C4 H4A 109.0 . . yes P1 C4 H4A 109.0 . . yes O4 C4 H4B 109.0 . . yes P1 C4 H4B 109.0 . . yes H4A C4 H4B 107.8 . . yes C4 O4 H4 111(2) . . yes O5 C5 P2 112.81(12) . . yes O5 C5 H5A 109.0 . . yes P2 C5 H5A 109.0 . . yes O5 C5 H5B 109.0 . . yes P2 C5 H5B 109.0 . . yes H5A C5 H5B 107.8 . . yes C5 O5 H5 106(2) . . yes O6 C6 P2 112.07(12) . . yes O6 C6 H6A 109.2 . . yes P2 C6 H6A 109.2 . . yes O6 C6 H6B 109.2 . . yes P2 C6 H6B 109.2 . . yes H6A C6 H6B 107.9 . . yes C6 O6 H6 109.5 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 P1 C4 -129.46(8) . . . . yes N1 Fe1 P1 C4 17.50(8) . . . . yes P2 Fe1 P1 C4 129.50(6) . . . . yes N2 Fe1 P1 C3 -6.42(9) . . . . yes N1 Fe1 P1 C3 140.55(9) . . . . yes P2 Fe1 P1 C3 -107.45(7) . . . . yes N2 Fe1 P1 C1 112.25(8) . . . . yes N1 Fe1 P1 C1 -100.79(8) . . . . yes P2 Fe1 P1 C1 11.21(6) . . . . yes N2 Fe1 P2 C2 -106.19(8) . . . . yes N1 Fe1 P2 C2 118.92(8) . . . . yes P1 Fe1 P2 C2 10.50(6) . . . . yes N2 Fe1 P2 C5 136.52(8) . . . . yes N1 Fe1 P2 C5 1.63(8) . . . . yes P1 Fe1 P2 C5 -106.79(6) . . . . yes N2 Fe1 P2 C6 14.74(9) . . . . yes N1 Fe1 P2 C6 -120.15(9) . . . . yes P1 Fe1 P2 C6 131.42(7) . . . . yes C4 P1 C1 C2 -161.90(12) . . . . yes C3 P1 C1 C2 93.77(13) . . . . yes Fe1 P1 C1 C2 -35.28(13) . . . . yes P1 C1 C2 P2 43.54(14) . . . . yes C5 P2 C2 C1 89.26(12) . . . . yes C6 P2 C2 C1 -163.87(11) . . . . yes Fe1 P2 C2 C1 -34.76(12) . . . . yes C4 P1 C3 O3 -167.20(12) . . . . yes C1 P1 C3 O3 -59.98(13) . . . . yes Fe1 P1 C3 O3 61.66(14) . . . . yes C3 P1 C4 O4 65.10(13) . . . . yes C1 P1 C4 O4 -41.28(14) . . . . yes Fe1 P1 C4 O4 -162.17(9) . . . . yes C2 P2 C5 O5 47.01(13) . . . . yes C6 P2 C5 O5 -61.63(13) . . . . yes Fe1 P2 C5 O5 167.96(9) . . . . yes C2 P2 C6 O6 59.34(14) . . . . yes C5 P2 C6 O6 167.43(12) . . . . yes Fe1 P2 C6 O6 -64.52(14) . . . . yes _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 30.39 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.558 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.089 data_6 _database_code_depnum_ccdc_archive 'CCDC 610301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(dinitrosyl-2-aminoethanethiol) hydrochloride S-bridged dinuclear iron(II) ; _chemical_name_common ? _chemical_formula_moiety 'C4 H14 Fe2 N6 O4 S2, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C4 H18 Cl2 Fe2 N6 O6 S2' _chemical_formula_weight 492.98 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' 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6305(9) _cell_length_b 7.9844(12) _cell_length_c 9.7216(14) _cell_angle_alpha 106.336(17) _cell_angle_beta 90.782(17) _cell_angle_gamma 113.684(16) _cell_volume 447.57(14) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 30.3 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 250 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.6452 _exptl_absorpt_correction_T_max 0.8802 _exptl_special_details ; The positions of H atoms were from difference Fourier calculations. Finally the H atomic positions of the CH2 groups and NH3 group were calculated after each refinement cycle. The water hydrogen atomic positions were fixed, their isotropic displacement parameters were freely refined. ; _diffrn_ambient_temperature 153(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7924 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 30.30 _reflns_number_total 2446 _reflns_number_gt 1859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] 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 2446 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.46265(8) 0.15989(7) 0.05279(6) 0.01600(17) Uani 1 d . . . S1 S 0.76994(14) 0.14502(13) -0.03747(10) 0.0174(2) Uani 1 d . . . Cl1 Cl 0.97300(16) 0.19187(13) 0.35479(11) 0.0251(2) Uani 1 d . . . N1 N 0.7817(6) 0.3722(5) -0.3683(4) 0.0224(7) Uani 1 d . . . H1A H 0.8323 0.4972 -0.3663 0.034 Uiso 1 calc R . . H1B H 0.6326 0.3107 -0.3993 0.034 Uiso 1 calc R . . H1C H 0.8525 0.3131 -0.4300 0.034 Uiso 1 calc R . . C1 C 0.7435(6) 0.1562(5) -0.2220(4) 0.0195(7) Uani 1 d . . . H1D H 0.8309 0.0952 -0.2809 0.023 Uiso 1 calc R . . H1E H 0.5856 0.0843 -0.2670 0.023 Uiso 1 calc R . . C2 C 0.8272(6) 0.3650(6) -0.2198(4) 0.0199(7) Uani 1 d . . . H2A H 0.7517 0.4303 -0.1523 0.024 Uiso 1 calc R . . H2B H 0.9892 0.4333 -0.1853 0.024 Uiso 1 calc R . . N2 N 0.5398(6) 0.2903(5) 0.2284(4) 0.0221(7) Uani 1 d . . . N3 N 0.3492(5) 0.2393(5) -0.0548(4) 0.0209(7) Uani 1 d . . . O1 O 0.5825(6) 0.3983(5) 0.3444(3) 0.0371(8) Uani 1 d . . . O2 O 0.2835(5) 0.3215(5) -0.1122(4) 0.0306(7) Uani 1 d . . . O3 O 0.3318(5) 0.1674(5) 0.5556(4) 0.0365(8) Uani 1 d . . . H8 H 0.2524 0.2030 0.4980 0.042(16) Uiso 1 d . . . H9 H 0.2356 0.0951 0.6214 0.16(5) Uiso 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 Fe1 0.0187(3) 0.0130(2) 0.0164(3) 0.0050(2) 0.00337(18) 0.00646(19) S1 0.0170(4) 0.0160(4) 0.0176(4) 0.0057(3) 0.0028(3) 0.0051(3) Cl1 0.0263(4) 0.0189(4) 0.0293(5) 0.0090(4) 0.0040(4) 0.0078(3) N1 0.0275(16) 0.0173(14) 0.0215(16) 0.0084(13) 0.0055(13) 0.0069(12) C1 0.0242(17) 0.0167(15) 0.0156(16) 0.0040(14) 0.0019(13) 0.0074(13) C2 0.0233(17) 0.0187(16) 0.0163(17) 0.0054(14) 0.0049(13) 0.0074(13) N2 0.0253(15) 0.0176(14) 0.0236(16) 0.0085(13) 0.0059(12) 0.0078(12) N3 0.0179(14) 0.0185(14) 0.0259(17) 0.0066(13) 0.0043(12) 0.0075(12) O1 0.055(2) 0.0275(16) 0.0201(15) -0.0020(14) 0.0026(14) 0.0150(15) O2 0.0324(15) 0.0327(16) 0.0379(18) 0.0196(14) 0.0036(13) 0.0188(13) O3 0.0266(15) 0.0372(18) 0.042(2) 0.0225(16) -0.0033(14) 0.0030(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.672(4) . yes Fe1 N2 1.676(4) . yes Fe1 S1 2.2585(12) 2_655 yes Fe1 S1 2.2628(11) . yes Fe1 Fe1 2.7154(11) 2_655 yes S1 C1 1.831(4) . yes S1 Fe1 2.2585(12) 2_655 yes N1 C2 1.493(5) . yes N1 H1A 0.9100 . yes N1 H1B 0.9100 . yes N1 H1C 0.9100 . yes C1 C2 1.524(5) . yes C1 H1D 0.9900 . yes C1 H1E 0.9900 . yes C2 H2A 0.9900 . yes C2 H2B 0.9900 . yes N2 O1 1.160(5) . yes N3 O2 1.167(5) . yes O3 H8 0.935 . yes O3 H9 1.035 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N2 117.62(16) . . yes N3 Fe1 S1 109.87(12) . 2_655 yes N2 Fe1 S1 108.23(13) . 2_655 yes N3 Fe1 S1 106.95(12) . . yes N2 Fe1 S1 107.40(12) . . yes S1 Fe1 S1 106.18(4) 2_655 . yes N3 Fe1 Fe1 121.71(11) . 2_655 yes N2 Fe1 Fe1 120.62(12) . 2_655 yes S1 Fe1 Fe1 53.16(3) 2_655 2_655 yes S1 Fe1 Fe1 53.02(3) . 2_655 yes C1 S1 Fe1 104.84(13) . 2_655 yes C1 S1 Fe1 105.90(13) . . yes Fe1 S1 Fe1 73.82(4) 2_655 . yes C2 N1 H1A 109.5 . . yes C2 N1 H1B 109.5 . . yes H1A N1 H1B 109.5 . . yes C2 N1 H1C 109.5 . . yes H1A N1 H1C 109.5 . . yes H1B N1 H1C 109.5 . . yes C2 C1 S1 110.2(2) . . yes C2 C1 H1D 109.6 . . yes S1 C1 H1D 109.6 . . yes C2 C1 H1E 109.6 . . yes S1 C1 H1E 109.6 . . yes H1D C1 H1E 108.1 . . yes N1 C2 C1 109.9(3) . . yes N1 C2 H2A 109.7 . . yes C1 C2 H2A 109.7 . . yes N1 C2 H2B 109.7 . . yes C1 C2 H2B 109.7 . . yes H2A C2 H2B 108.2 . . yes O1 N2 Fe1 170.1(3) . . yes O2 N3 Fe1 169.3(3) . . yes H8 O3 H9 113.0 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 S1 C1 -16.05(17) . . . . yes N2 Fe1 S1 C1 -143.16(18) . . . . yes S1 Fe1 S1 C1 101.23(13) 2_655 . . . yes Fe1 Fe1 S1 C1 101.23(13) 2_655 . . . yes N3 Fe1 S1 Fe1 -117.28(12) . . . 2_655 yes N2 Fe1 S1 Fe1 115.61(13) . . . 2_655 yes S1 Fe1 S1 Fe1 0.0 2_655 . . 2_655 yes Fe1 S1 C1 C2 160.9(2) 2_655 . . . yes Fe1 S1 C1 C2 83.9(3) . . . . yes S1 C1 C2 N1 -173.7(2) . . . . yes N2 Fe1 N3 O2 15.4(18) . . . . yes S1 Fe1 N3 O2 139.8(17) 2_655 . . . yes S1 Fe1 N3 O2 -105.4(18) . . . . yes Fe1 Fe1 N3 O2 -161.9(17) 2_655 . . . yes _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 30.30 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.595 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.163 data_7 _database_code_depnum_ccdc_archive 'CCDC 610302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[dinitrosyl-cysteamine-iron(II)] iodide water ; _chemical_name_common ? _chemical_formula_moiety 'C4 H16 Fe2 N6 O4 S2, H2 O, 2(I)' _chemical_formula_sum 'C4 H18 Fe2 I2 N6 O5 S2' _chemical_formula_weight 659.88 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3097(5) _cell_length_b 6.8752(5) _cell_length_c 24.5366(17) _cell_angle_alpha 90.403(8) _cell_angle_beta 93.515(8) _cell_angle_gamma 116.319(8) _cell_volume 951.58(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 5.011 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.2970 _exptl_absorpt_correction_T_max 0.6612 _exptl_special_details ; see text ; _diffrn_ambient_temperature 153(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 3.50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10041 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.02 _reflns_number_total 4195 _reflns_number_gt 3491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] 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 4195 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.32750(8) 1.15415(8) 0.033333(18) 0.01325(11) Uani 1 d . . . I1 I 0.05737(4) 1.17775(4) 0.182667(8) 0.02047(8) Uani 1 d . . . S1 S -0.52575(14) 0.79746(14) 0.04908(3) 0.01551(16) Uani 1 d . . . H1 H -0.4216 0.6878 0.0523 0.019 Uiso 1 calc R . . N1 N -0.0459(5) 1.2041(5) 0.02644(11) 0.0177(6) Uani 1 d . . . O1 O 0.1570(4) 1.2579(5) 0.02703(13) 0.0331(7) Uani 1 d . . . N2 N -0.3737(5) 1.3025(5) 0.08146(11) 0.0179(6) Uani 1 d . . . O2 O -0.3582(5) 1.4224(5) 0.11712(11) 0.0309(6) Uani 1 d . . . C1 C -0.7538(6) 0.7590(6) 0.09593(13) 0.0185(7) Uani 1 d . . . H1A H -0.8151 0.8673 0.0893 0.022 Uiso 1 calc R . . H1B H -0.8874 0.6124 0.0895 0.022 Uiso 1 calc R . . C2 C -0.6504(6) 0.7847(6) 0.15467(13) 0.0187(7) Uani 1 d . . . H2A H -0.5686 0.6915 0.1599 0.022 Uiso 1 calc R . . H2B H -0.5328 0.9374 0.1627 0.022 Uiso 1 calc R . . N3 N -0.8436(5) 0.7221(5) 0.19245(11) 0.0194(6) Uani 1 d . . . H3A H -0.9152 0.8110 0.1883 0.029 Uiso 1 calc R . . H3B H -0.7819 0.7347 0.2275 0.029 Uiso 1 calc R . . H3C H -0.9521 0.5822 0.1846 0.029 Uiso 1 calc R . . Fe2 Fe 0.82367(8) 0.83373(8) 0.470231(17) 0.01197(11) Uani 1 d . . . I2 I 0.44653(4) 0.79306(4) 0.322853(9) 0.01939(8) Uani 1 d . . . S2 S 0.98916(13) 0.81707(14) 0.55334(3) 0.01387(16) Uani 1 d . . . H2 H 1.0983 0.7122 0.5583 0.017 Uiso 1 calc R . . N4 N 0.5428(5) 0.7834(5) 0.47810(11) 0.0166(6) Uani 1 d . . . O3 O 0.3394(4) 0.7274(5) 0.47781(13) 0.0329(7) Uani 1 d . . . N5 N 0.8656(5) 0.6752(5) 0.42415(11) 0.0167(6) Uani 1 d . . . O4 O 0.8507(5) 0.5525(5) 0.38961(11) 0.0287(6) Uani 1 d . . . C3 C 0.7702(6) 0.7889(6) 0.60211(13) 0.0197(7) Uani 1 d . . . H3D H 0.6891 0.8780 0.5905 0.024 Uiso 1 calc R . . H3E H 0.6493 0.6355 0.6013 0.024 Uiso 1 calc R . . C4 C 0.8772(6) 0.8576(6) 0.66014(13) 0.0176(7) Uani 1 d . . . H4A H 0.9833 1.0155 0.6620 0.021 Uiso 1 calc R . . H4B H 0.7487 0.8302 0.6846 0.021 Uiso 1 calc R . . N6 N 1.0149(5) 0.7385(5) 0.67976(11) 0.0162(5) Uani 1 d . . . H6A H 0.9292 0.5943 0.6711 0.024 Uiso 1 calc R . . H6B H 1.0447 0.7584 0.7167 0.024 Uiso 1 calc R . . H6C H 1.1544 0.7905 0.6635 0.024 Uiso 1 calc R . . O5 O -0.2895(5) 0.4690(5) 0.25330(13) 0.0392(8) Uani 1 d . . . H51 H -0.4318 0.3833 0.2310 0.08(2) Uiso 1 d . . . H52 H -0.2726 0.5812 0.2775 0.07(2) Uiso 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 Fe1 0.0115(2) 0.0153(3) 0.0124(2) -0.00015(18) 0.00224(16) 0.00527(19) I1 0.03065(14) 0.01854(15) 0.01647(12) 0.00062(9) 0.00371(9) 0.01451(11) S1 0.0161(3) 0.0173(4) 0.0144(3) 0.0032(3) 0.0044(3) 0.0081(3) N1 0.0165(13) 0.0188(16) 0.0169(13) -0.0007(12) 0.0033(10) 0.0068(12) O1 0.0141(12) 0.0349(18) 0.0489(17) -0.0060(14) 0.0050(12) 0.0094(12) N2 0.0170(13) 0.0212(16) 0.0160(12) -0.0010(12) 0.0030(10) 0.0089(12) O2 0.0350(15) 0.0349(18) 0.0258(13) -0.0097(13) 0.0031(11) 0.0183(14) C1 0.0178(15) 0.0225(19) 0.0142(14) 0.0037(13) 0.0054(12) 0.0074(14) C2 0.0208(15) 0.0194(19) 0.0156(14) 0.0060(13) 0.0061(12) 0.0080(15) N3 0.0262(14) 0.0200(16) 0.0153(12) 0.0058(12) 0.0068(11) 0.0125(13) Fe2 0.0120(2) 0.0134(3) 0.0109(2) 0.00046(18) 0.00201(16) 0.00579(19) I2 0.01723(12) 0.01638(14) 0.02043(12) 0.00149(9) -0.00029(8) 0.00393(10) S2 0.0160(3) 0.0154(4) 0.0120(3) 0.0030(3) 0.0033(3) 0.0083(3) N4 0.0162(13) 0.0140(15) 0.0182(13) 0.0019(11) 0.0034(10) 0.0051(12) O3 0.0148(12) 0.0388(19) 0.0454(17) -0.0026(14) 0.0058(11) 0.0120(12) N5 0.0186(13) 0.0177(16) 0.0166(12) 0.0025(11) 0.0029(10) 0.0104(12) O4 0.0371(15) 0.0277(16) 0.0265(13) -0.0075(12) 0.0023(11) 0.0193(13) C3 0.0187(15) 0.028(2) 0.0147(14) 0.0043(14) 0.0051(12) 0.0113(15) C4 0.0213(15) 0.0220(19) 0.0144(14) 0.0046(13) 0.0066(12) 0.0133(15) N6 0.0175(13) 0.0145(15) 0.0154(12) 0.0029(11) 0.0036(10) 0.0056(12) O5 0.0340(16) 0.041(2) 0.0447(18) -0.0092(16) 0.0017(14) 0.0192(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.673(3) . ? Fe1 N2 1.676(3) . ? Fe1 S1 2.2540(10) . ? Fe1 S1 2.2606(9) 2_475 ? Fe1 Fe1 2.7075(10) 2_475 ? S1 C1 1.825(3) . ? S1 Fe1 2.2607(9) 2_475 ? S1 H1 1.2000 . ? N1 O1 1.163(4) . ? N2 O2 1.167(4) . ? C1 C2 1.521(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N3 1.487(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? Fe2 N4 1.673(3) . ? Fe2 N5 1.677(3) . ? Fe2 S2 2.2544(10) 2_776 ? Fe2 S2 2.2606(8) . ? Fe2 Fe2 2.7122(10) 2_776 ? S2 C3 1.829(3) . ? S2 Fe2 2.2544(10) 2_776 ? S2 H2 1.2000 . ? N4 O3 1.165(4) . ? N5 O4 1.161(4) . ? C3 C4 1.515(4) . ? C3 H3D 0.9900 . ? C3 H3E 0.9900 . ? C4 N6 1.498(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N6 H6C 0.9100 . ? O5 H51 0.958 . ? O5 H52 0.934 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 116.70(14) . . ? N1 Fe1 S1 106.42(11) . . ? N2 Fe1 S1 110.40(11) . . ? N1 Fe1 S1 106.82(10) . 2_475 ? N2 Fe1 S1 109.65(10) . 2_475 ? S1 Fe1 S1 106.30(3) . 2_475 ? N1 Fe1 Fe1 118.48(10) . 2_475 ? N2 Fe1 Fe1 124.82(10) . 2_475 ? S1 Fe1 Fe1 53.27(3) . 2_475 ? S1 Fe1 Fe1 53.04(3) 2_475 2_475 ? C1 S1 Fe1 108.77(13) . . ? C1 S1 Fe1 105.40(11) . 2_475 ? Fe1 S1 Fe1 73.70(3) . 2_475 ? C1 S1 H1 119.9 . . ? Fe1 S1 H1 119.9 . . ? Fe1 S1 H1 119.9 2_475 . ? O1 N1 Fe1 171.4(3) . . ? O2 N2 Fe1 166.6(3) . . ? C2 C1 S1 109.9(2) . . ? C2 C1 H1A 109.7 . . ? S1 C1 H1A 109.7 . . ? C2 C1 H1B 109.7 . . ? S1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N3 C2 C1 109.6(3) . . ? N3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 N3 H3A 109.5 . . ? C2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? N4 Fe2 N5 116.53(14) . . ? N4 Fe2 S2 106.16(11) . 2_776 ? N5 Fe2 S2 109.40(11) . 2_776 ? N4 Fe2 S2 107.44(10) . . ? N5 Fe2 S2 110.59(10) . . ? S2 Fe2 S2 106.16(3) 2_776 . ? N4 Fe2 Fe2 118.75(10) . 2_776 ? N5 Fe2 Fe2 124.69(10) . 2_776 ? S2 Fe2 Fe2 53.18(3) 2_776 2_776 ? S2 Fe2 Fe2 52.98(3) . 2_776 ? C3 S2 Fe2 109.44(13) . 2_776 ? C3 S2 Fe2 105.99(11) . . ? Fe2 S2 Fe2 73.84(3) 2_776 . ? C3 S2 H2 119.5 . . ? Fe2 S2 H2 119.5 2_776 . ? Fe2 S2 H2 119.5 . . ? O3 N4 Fe2 170.7(3) . . ? O4 N5 Fe2 167.4(3) . . ? C4 C3 S2 113.3(2) . . ? C4 C3 H3D 108.9 . . ? S2 C3 H3D 108.9 . . ? C4 C3 H3E 108.9 . . ? S2 C3 H3E 108.9 . . ? H3D C3 H3E 107.7 . . ? N6 C4 C3 112.2(3) . . ? N6 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N6 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 N6 H6A 109.5 . . ? C4 N6 H6B 109.5 . . ? H6A N6 H6B 109.5 . . ? C4 N6 H6C 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? H51 O5 H52 123.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 S1 C1 145.28(15) . . . . ? N2 Fe1 S1 C1 17.73(15) . . . . ? S1 Fe1 S1 C1 -101.12(11) 2_475 . . . ? Fe1 Fe1 S1 C1 -101.12(11) 2_475 . . . ? N1 Fe1 S1 Fe1 -113.60(10) . . . 2_475 ? N2 Fe1 S1 Fe1 118.85(10) . . . 2_475 ? S1 Fe1 S1 Fe1 0.0 2_475 . . 2_475 ? N1 Fe1 N2 O2 -3.2(13) . . . . ? S1 Fe1 N2 O2 118.5(13) . . . . ? S1 Fe1 N2 O2 -124.8(13) 2_475 . . . ? Fe1 Fe1 N2 O2 177.2(12) 2_475 . . . ? Fe1 S1 C1 C2 -87.4(2) . . . . ? Fe1 S1 C1 C2 -165.0(2) 2_475 . . . ? S1 C1 C2 N3 -171.8(2) . . . . ? N4 Fe2 S2 C3 -7.14(18) . . . . ? N5 Fe2 S2 C3 -135.33(18) . . . . ? S2 Fe2 S2 C3 106.11(14) 2_776 . . . ? Fe2 Fe2 S2 C3 106.11(14) 2_776 . . . ? N4 Fe2 S2 Fe2 -113.24(11) . . . 2_776 ? N5 Fe2 S2 Fe2 118.57(12) . . . 2_776 ? S2 Fe2 S2 Fe2 0.0 2_776 . . 2_776 ? N4 Fe2 N5 O4 10.0(14) . . . . ? S2 Fe2 N5 O4 -110.4(13) 2_776 . . . ? S2 Fe2 N5 O4 133.1(13) . . . . ? Fe2 Fe2 N5 O4 -168.4(13) 2_776 . . . ? Fe2 S2 C3 C4 -80.5(3) 2_776 . . . ? Fe2 S2 C3 C4 -158.6(2) . . . . ? S2 C3 C4 N6 -55.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 1.500 _refine_diff_density_min -1.582 _refine_diff_density_rms 0.167 data_9 _database_code_depnum_ccdc_archive 'CCDC 610303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[(\m-pyrimidine-2-thionate)dinitrosyl-iron] ; _chemical_name_common ? _chemical_formula_moiety 'C8 H8 Fe2 N8 O4 S2' _chemical_formula_sum 'C8 H8 Fe2 N8 O4 S2' _chemical_formula_weight 456.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4219(13) _cell_length_b 7.626(2) _cell_length_c 8.345(2) _cell_angle_alpha 75.61(3) _cell_angle_beta 80.83(3) _cell_angle_gamma 85.15(3) _cell_volume 390.37(17) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6822 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 30.3 _exptl_crystal_description block _exptl_crystal_colour 'red (opaque)' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 228 _exptl_absorpt_coefficient_mu 2.159 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.5542 _exptl_absorpt_correction_T_max 0.6845 _exptl_special_details ; see text ; _diffrn_ambient_temperature 183(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 3.8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6823 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 30.33 _reflns_number_total 2102 _reflns_number_gt 1752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^] 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 2102 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.06459(5) 0.00121(4) 0.64747(5) 0.01615(13) Uani 1 d . . . S1 S 0.07603(9) -0.23830(8) 0.53007(8) 0.01885(16) Uani 1 d . . . H1 H 0.2442 -0.3053 0.4853 0.023 Uiso 1 calc R . . N1 N -0.1091(3) -0.0432(3) 0.8231(3) 0.0225(5) Uani 1 d . . . N2 N 0.3149(3) 0.0368(3) 0.6604(3) 0.0233(5) Uani 1 d . . . O1 O -0.2057(3) -0.0750(4) 0.9579(3) 0.0380(6) Uani 1 d . . . O2 O 0.4788(3) 0.0559(4) 0.6940(4) 0.0414(6) Uani 1 d . . . N3 N -0.0584(4) -0.4849(3) 0.7979(4) 0.0306(6) Uani 1 d . . . N4 N -0.3098(4) -0.3806(3) 0.6088(3) 0.0260(5) Uani 1 d . . . C1 C -0.1246(4) -0.3819(3) 0.6601(3) 0.0186(5) Uani 1 d . . . C2 C -0.4452(4) -0.5008(4) 0.7085(4) 0.0290(6) Uani 1 d . . . H2 H -0.5795 -0.5070 0.6768 0.035 Uiso 1 calc R . . C3 C -0.3955(4) -0.6150(4) 0.8547(4) 0.0280(6) Uani 1 d . . . H3 H -0.4923 -0.6992 0.9240 0.034 Uiso 1 calc R . . C4 C -0.1982(5) -0.6013(4) 0.8959(4) 0.0327(7) Uani 1 d . . . H4 H -0.1604 -0.6768 0.9970 0.039 Uiso 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 0.01355(18) 0.01816(19) 0.0168(2) -0.00259(13) -0.00340(12) -0.00380(11) S1 0.0153(3) 0.0165(3) 0.0240(4) -0.0033(2) -0.0028(2) -0.00104(19) N1 0.0189(9) 0.0244(10) 0.0234(12) -0.0021(9) -0.0031(8) -0.0065(8) N2 0.0170(9) 0.0264(11) 0.0267(13) -0.0040(9) -0.0048(8) -0.0054(8) O1 0.0329(11) 0.0538(14) 0.0240(12) -0.0051(10) 0.0060(9) -0.0147(10) O2 0.0204(9) 0.0587(15) 0.0496(16) -0.0141(12) -0.0124(9) -0.0103(9) N3 0.0295(12) 0.0287(12) 0.0307(14) 0.0054(10) -0.0125(10) -0.0078(9) N4 0.0209(10) 0.0265(11) 0.0292(14) 0.0001(9) -0.0071(9) -0.0065(8) C1 0.0194(10) 0.0154(10) 0.0216(13) -0.0048(9) -0.0037(9) -0.0019(8) C2 0.0222(12) 0.0296(14) 0.0348(17) -0.0043(12) -0.0042(10) -0.0090(10) C3 0.0278(13) 0.0235(12) 0.0301(16) -0.0029(11) 0.0022(11) -0.0087(10) C4 0.0384(15) 0.0282(14) 0.0285(17) 0.0053(12) -0.0099(12) -0.0110(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.674(2) . yes Fe1 N2 1.677(2) . yes Fe1 S1 2.2578(11) 2_556 yes Fe1 S1 2.2684(10) . yes Fe1 Fe1 2.7242(10) 2_556 yes S1 C1 1.800(3) . yes S1 Fe1 2.2578(11) 2_556 yes S1 H1 1.2000 . yes N1 O1 1.173(3) . yes N2 O2 1.161(3) . yes N3 C1 1.330(4) . yes N3 C4 1.343(4) . yes N4 C1 1.325(3) . yes N4 C2 1.347(3) . yes C2 C3 1.377(4) . yes C2 H2 0.9500 . yes C3 C4 1.383(4) . yes C3 H3 0.9500 . yes C4 H4 0.9500 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 118.80(12) . . yes N1 Fe1 S1 106.69(8) . 2_556 yes N2 Fe1 S1 110.75(9) . 2_556 yes N1 Fe1 S1 107.16(9) . . yes N2 Fe1 S1 106.72(9) . . yes S1 Fe1 S1 105.99(3) 2_556 . yes N1 Fe1 Fe1 118.93(8) . 2_556 yes N2 Fe1 Fe1 122.22(9) . 2_556 yes S1 Fe1 Fe1 53.17(3) 2_556 2_556 yes S1 Fe1 Fe1 52.82(3) . 2_556 yes C1 S1 Fe1 111.64(8) . 2_556 yes C1 S1 Fe1 104.51(9) . . yes Fe1 S1 Fe1 74.01(3) 2_556 . yes C1 S1 H1 119.2 . . yes Fe1 S1 H1 119.2 2_556 . yes Fe1 S1 H1 119.2 . . yes O1 N1 Fe1 170.2(2) . . yes O2 N2 Fe1 170.1(3) . . yes C1 N3 C4 115.2(2) . . yes C1 N4 C2 115.3(2) . . yes N4 C1 N3 128.1(2) . . yes N4 C1 S1 119.3(2) . . yes N3 C1 S1 112.55(18) . . yes N4 C2 C3 122.3(3) . . yes N4 C2 H2 118.9 . . yes C3 C2 H2 118.9 . . yes C2 C3 C4 117.0(3) . . yes C2 C3 H3 121.5 . . yes C4 C3 H3 121.5 . . yes N3 C4 C3 122.2(3) . . yes N3 C4 H4 118.9 . . yes C3 C4 H4 118.9 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 S1 C1 4.86(12) . . . . yes N2 Fe1 S1 C1 133.11(12) . . . . yes S1 Fe1 S1 C1 -108.79(9) 2_556 . . . yes Fe1 Fe1 S1 C1 -108.79(9) 2_556 . . . yes N1 Fe1 S1 Fe1 113.65(8) . . . 2_556 yes N2 Fe1 S1 Fe1 -118.09(9) . . . 2_556 yes S1 Fe1 S1 Fe1 0.0 2_556 . . 2_556 yes C2 N4 C1 N3 -1.0(5) . . . . yes C2 N4 C1 S1 175.7(2) . . . . yes C4 N3 C1 N4 0.0(5) . . . . yes C4 N3 C1 S1 -176.9(2) . . . . yes Fe1 S1 C1 N4 23.1(3) 2_556 . . . yes Fe1 S1 C1 N4 101.4(2) . . . . yes Fe1 S1 C1 N3 -159.6(2) 2_556 . . . yes Fe1 S1 C1 N3 -81.4(2) . . . . yes C1 N4 C2 C3 1.0(5) . . . . yes N4 C2 C3 C4 0.0(5) . . . . yes C1 N3 C4 C3 1.1(5) . . . . yes C2 C3 C4 N3 -1.1(5) . . . . yes _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 30.33 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.550 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.119 data_10 _database_code_depnum_ccdc_archive 'CCDC 610304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Iodo-2-mercaptopyrimidine-dinitrosyl-iron(-I) diethylether ; _chemical_name_common ? _chemical_formula_moiety 'C4 H4 Fe I N4 O2 S, C4 H10 O' _chemical_formula_sum 'C8 H14 Fe I N4 O3 S' _chemical_formula_weight 429.05 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' S S 0.1246 0.1234 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0648(4) _cell_length_b 11.4932(7) _cell_length_c 18.8432(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.237(7) _cell_angle_gamma 90.00 _cell_volume 1529.66(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 30.3 _exptl_crystal_description block _exptl_crystal_colour 'red, opaque' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 3.145 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.4952 _exptl_absorpt_correction_T_max 0.7438 _exptl_special_details ; The crystals were opaque or black, only at their rim it was possible to observe extinction under polarized light. The material was grown as large prism or blocks, the example crystal had to be cut to a suitable size for the X-ray experiment. ; _diffrn_ambient_temperature 153(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.40 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17573 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.31 _reflns_number_total 4499 _reflns_number_gt 2709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] 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 4499 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1312 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.47748(6) 0.71489(4) 0.33622(2) 0.03031(13) Uani 1 d . . . Fe1 Fe 0.78775(12) 0.83547(8) 0.34126(4) 0.0260(2) Uani 1 d . . . S1 S 0.9646(2) 0.78440(15) 0.44126(7) 0.0272(3) Uani 1 d . . . N1 N 0.9323(8) 0.7951(6) 0.2751(3) 0.0393(14) Uani 1 d . . . O1 O 1.0328(8) 0.7945(7) 0.2282(3) 0.066(2) Uani 1 d . . . N2 N 0.7257(8) 0.9774(5) 0.3387(3) 0.0346(12) Uani 1 d . . . O2 O 0.7040(8) 1.0761(5) 0.3255(3) 0.0536(14) Uani 1 d . . . O3 O 1.1687(6) 0.6303(4) 0.5978(3) 0.0352(10) Uani 1 d . . . N3 N 0.9393(7) 0.8200(5) 0.5779(3) 0.0261(10) Uani 1 d . . . N4 N 0.7514(7) 0.9468(4) 0.5075(3) 0.0259(10) Uani 1 d . . . C1 C 0.8754(8) 0.8565(5) 0.5125(3) 0.0230(11) Uani 1 d . . . C2 C 0.6969(9) 0.9967(6) 0.5665(3) 0.0291(13) Uani 1 d . . . H2 H 0.6112 1.0602 0.5627 0.035 Uiso 1 calc R . . C3 C 0.7574(8) 0.9622(6) 0.6348(3) 0.0293(13) Uani 1 d . . . H3 H 0.7146 1.0003 0.6762 0.035 Uiso 1 calc R . . C4 C 0.8814(8) 0.8705(6) 0.6385(3) 0.0289(13) Uani 1 d . . . H4 H 0.9263 0.8427 0.6833 0.035 Uiso 1 calc R . . C5 C 0.9087(13) 0.5487(9) 0.6603(5) 0.066(3) Uani 1 d . . . H5A H 0.9458 0.5966 0.7013 0.099 Uiso 1 calc R . . H5B H 0.8554 0.4750 0.6767 0.099 Uiso 1 calc R . . H5C H 0.8135 0.5903 0.6314 0.099 Uiso 1 calc R . . C6 C 1.0780(13) 0.5249(7) 0.6167(6) 0.063(3) Uani 1 d . . . H6A H 1.1679 0.4752 0.6440 0.076 Uiso 1 calc R . . H6B H 1.0388 0.4822 0.5732 0.076 Uiso 1 calc R . . C7 C 1.3334(10) 0.6103(8) 0.5557(5) 0.052(2) Uani 1 d . . . H7A H 1.2941 0.5804 0.5084 0.063 Uiso 1 calc R . . H7B H 1.4156 0.5513 0.5790 0.063 Uiso 1 calc R . . C8 C 1.4382(10) 0.7191(8) 0.5479(4) 0.0474(19) Uani 1 d . . . H8A H 1.3529 0.7794 0.5290 0.071 Uiso 1 calc R . . H8B H 1.5421 0.7073 0.5150 0.071 Uiso 1 calc R . . H8C H 1.4897 0.7435 0.5942 0.071 Uiso 1 calc R . . H1 H 1.0866 0.7890 0.4385 0.008(12) Uiso 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 I1 0.0320(2) 0.0352(2) 0.02367(19) -0.00491(19) -0.00115(13) -0.00458(19) Fe1 0.0288(4) 0.0305(5) 0.0188(4) -0.0033(4) 0.0008(3) -0.0017(4) S1 0.0294(7) 0.0304(7) 0.0217(7) -0.0058(6) -0.0008(5) 0.0037(7) N1 0.034(3) 0.057(4) 0.027(3) -0.010(3) 0.001(2) -0.007(3) O1 0.044(3) 0.133(6) 0.021(2) -0.015(3) 0.012(2) -0.006(4) N2 0.038(3) 0.034(3) 0.031(3) 0.003(2) -0.001(2) -0.001(2) O2 0.051(3) 0.038(3) 0.072(4) 0.011(3) 0.004(3) -0.001(3) O3 0.030(2) 0.035(3) 0.041(3) 0.005(2) 0.0094(19) 0.0035(19) N3 0.025(2) 0.031(3) 0.023(2) 0.005(2) -0.0021(18) -0.006(2) N4 0.031(2) 0.025(3) 0.022(2) -0.001(2) -0.0011(19) 0.001(2) C1 0.022(2) 0.025(3) 0.022(3) -0.002(2) -0.001(2) -0.004(2) C2 0.032(3) 0.030(3) 0.025(3) -0.003(3) -0.001(2) 0.005(3) C3 0.031(3) 0.034(3) 0.023(3) -0.005(3) 0.002(2) -0.003(3) C4 0.028(3) 0.039(4) 0.020(3) 0.000(3) 0.001(2) -0.006(3) C5 0.066(5) 0.064(6) 0.069(6) 0.001(5) 0.015(5) -0.030(5) C6 0.062(5) 0.027(4) 0.101(8) 0.000(4) 0.024(5) -0.003(4) C7 0.035(4) 0.052(5) 0.070(6) -0.014(4) 0.012(4) 0.006(3) C8 0.039(4) 0.071(6) 0.032(3) 0.004(4) 0.003(3) -0.009(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 I1 Fe1 2.5934(9) . yes Fe1 N2 1.690(6) . yes Fe1 N1 1.693(5) . yes Fe1 S1 2.3139(17) . yes S1 C1 1.709(6) . yes S1 H1 0.8665 . yes N1 O1 1.145(7) . yes N2 O2 1.171(8) . yes O3 C6 1.420(9) . yes O3 C7 1.440(8) . yes N3 C4 1.353(8) . yes N3 C1 1.369(7) . yes N4 C2 1.317(8) . yes N4 C1 1.360(8) . yes C2 C3 1.404(9) . yes C2 H2 0.9500 . yes C3 C4 1.371(9) . yes C3 H3 0.9500 . yes C4 H4 0.9500 . yes C5 C6 1.491(12) . yes C5 H5A 0.9800 . yes C5 H5B 0.9800 . yes C5 H5C 0.9800 . yes C6 H6A 0.9900 . yes C6 H6B 0.9900 . yes C7 C8 1.462(12) . yes C7 H7A 0.9900 . yes C7 H7B 0.9900 . yes C8 H8A 0.9800 . yes C8 H8B 0.9800 . yes C8 H8C 0.9800 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 113.8(3) . . yes N2 Fe1 S1 113.8(2) . . yes N1 Fe1 S1 101.9(2) . . yes N2 Fe1 I1 107.25(19) . . yes N1 Fe1 I1 110.5(2) . . yes S1 Fe1 I1 109.59(5) . . yes C1 S1 Fe1 108.4(2) . . yes C1 S1 H1 113.7 . . yes Fe1 S1 H1 117.13 . . yes O1 N1 Fe1 164.5(7) . . yes O2 N2 Fe1 167.0(6) . . yes C6 O3 C7 112.1(6) . . yes C4 N3 C1 122.0(5) . . yes C2 N4 C1 118.3(5) . . yes N4 C1 N3 119.7(5) . . yes N4 C1 S1 124.3(4) . . yes N3 C1 S1 116.0(4) . . yes N4 C2 C3 124.2(6) . . yes N4 C2 H2 117.9 . . yes C3 C2 H2 117.9 . . yes C4 C3 C2 116.5(6) . . yes C4 C3 H3 121.8 . . yes C2 C3 H3 121.8 . . yes N3 C4 C3 119.4(6) . . yes N3 C4 H4 120.3 . . yes C3 C4 H4 120.3 . . yes C6 C5 H5A 109.5 . . yes C6 C5 H5B 109.5 . . yes H5A C5 H5B 109.5 . . yes C6 C5 H5C 109.5 . . yes H5A C5 H5C 109.5 . . yes H5B C5 H5C 109.5 . . yes O3 C6 C5 110.7(7) . . yes O3 C6 H6A 109.5 . . yes C5 C6 H6A 109.5 . . yes O3 C6 H6B 109.5 . . yes C5 C6 H6B 109.5 . . yes H6A C6 H6B 108.1 . . yes O3 C7 C8 109.6(6) . . yes O3 C7 H7A 109.7 . . yes C8 C7 H7A 109.7 . . yes O3 C7 H7B 109.7 . . yes C8 C7 H7B 109.7 . . yes H7A C7 H7B 108.2 . . yes C7 C8 H8A 109.5 . . yes C7 C8 H8B 109.5 . . yes H8A C8 H8B 109.5 . . yes C7 C8 H8C 109.5 . . yes H8A C8 H8C 109.5 . . yes H8B C8 H8C 109.5 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 S1 C1 39.3(3) . . . . yes N1 Fe1 S1 C1 162.2(3) . . . . yes I1 Fe1 S1 C1 -80.8(2) . . . . yes N2 Fe1 N1 O1 12(2) . . . . yes S1 Fe1 N1 O1 -111(2) . . . . yes I1 Fe1 N1 O1 132(2) . . . . yes N1 Fe1 N2 O2 0(3) . . . . yes S1 Fe1 N2 O2 116(2) . . . . yes I1 Fe1 N2 O2 -122(2) . . . . yes C2 N4 C1 N3 0.2(8) . . . . yes C2 N4 C1 S1 -178.4(5) . . . . yes C4 N3 C1 N4 0.7(8) . . . . yes C4 N3 C1 S1 179.3(4) . . . . yes Fe1 S1 C1 N4 -13.4(5) . . . . yes Fe1 S1 C1 N3 168.0(4) . . . . yes C1 N4 C2 C3 -0.6(9) . . . . yes N4 C2 C3 C4 0.2(10) . . . . yes C1 N3 C4 C3 -1.1(9) . . . . yes C2 C3 C4 N3 0.6(9) . . . . yes C7 O3 C6 C5 179.9(8) . . . . yes C6 O3 C7 C8 -170.7(8) . . . . yes _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.31 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.080 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.169 data_11 _database_code_depnum_ccdc_archive 'CCDC 610305' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trinitrosyl(tris(hydroxymethyl)phosphino)iron(II) hexafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety 'C3 H9 Fe N3 O6 P, F6 P' _chemical_formula_sum 'C3 H9 F6 Fe N3 O6 P2' _chemical_formula_weight 414.92 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P na21' 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' _cell_length_a 24.693(3) _cell_length_b 6.6317(10) _cell_length_c 8.2556(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1351.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 30.5 _exptl_crystal_description 'tiny irregular shaped plate' _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.454 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Due to instability of the green crystals at room temperature a tiny crystal of arbitrary plate-like shape had immediately been mounted with protecting oil and cooled to 183 K on the goniometer of the IPDS diffractometer using an Oxford Cryogenic System. It was not possible to measure crystal faces for the absorption correction because of the tiny piece of crystal, and also the centering procedure was difficult and probably also introduced systematic errors to the data set. Systematic extinction revealed orthorhombic space groups Pnma or Pna21. A triclinic solution (in P-1) clearly showed mirror symmetry m of two Fe-complexes and two PF6 counterions but the refinement of the Pnma solution resulted in problems with disordered PF6 and disordered CH2OH groups and calculation of H-atom positions of the disordered parts. Therefore the space group Pna21 was finally chosen. The structure was solved with Patterson method implemented in SHELXS-97. The refinement resulted in one disordered OH position. Shift limiting restraints (damping) had to be introduced and 23 distance restraints for N=O and C-OH, and also for P-F and F..F distances were used to achieve stable refinement. Finally, one cycle with "DAMP 0 0" was used to get more realistic standard uncertainties for the bond distances and angles. It should be noted that only 50% of the unique data are considered "observed" by criterion I>2s(I). The Flack parameter was 0.05(15) at convergence. To improve the relatively bad R-values, a secondary extintion correction was applied in the refinement. ; _diffrn_ambient_temperature 183(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 6.0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6204 _diffrn_reflns_av_R_equivalents 0.1438 _diffrn_reflns_av_sigmaI/netI 0.1162 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 30.52 _reflns_number_total 2046 _reflns_number_gt 1023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.045(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(15) _refine_ls_number_reflns 2046 _refine_ls_number_parameters 199 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1627 _refine_ls_R_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.2612 _refine_ls_wR_factor_gt 0.2201 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.67802(5) 0.5002(3) 0.4996(6) 0.0379(5) Uani 1 d . . . P1 P 0.58854(10) 0.5937(5) 0.4974(10) 0.0361(6) Uani 1 d . . . N1 N 0.7030(6) 0.597(3) 0.662(2) 0.044(4) Uani 1 d . . . O1 O 0.7246(9) 0.667(4) 0.786(2) 0.070(6) Uani 1 d . . . N2 N 0.6771(4) 0.2428(17) 0.497(4) 0.044(2) Uani 1 d . . . O2 O 0.6785(5) 0.0714(16) 0.494(4) 0.062(3) Uani 1 d . . . N3 N 0.7022(10) 0.613(4) 0.325(3) 0.059(6) Uani 1 d . . . O3 O 0.7217(12) 0.669(4) 0.211(4) 0.078(7) Uani 1 d . . . C1 C 0.5729(7) 0.765(4) 0.335(2) 0.055(6) Uani 1 d D . . H1A H 0.5930 0.8927 0.3502 0.066 Uiso 1 calc R . . H1B H 0.5839 0.7052 0.2303 0.066 Uiso 1 calc R . . O4 O 0.5144(8) 0.805(4) 0.335(3) 0.088(8) Uani 1 d D . . H4 H 0.4979 0.7048 0.3729 0.132 Uiso 1 calc R . . C2 C 0.5411(6) 0.397(2) 0.5622(19) 0.046(3) Uani 1 d D . . H2A H 0.5456 0.3729 0.6798 0.055 Uiso 1 calc R . . H2B H 0.5036 0.4436 0.5436 0.055 Uiso 1 calc R . . O5 O 0.5493(5) 0.2098(16) 0.477(3) 0.060(5) Uani 1 d D . . H5 H 0.5295 0.2072 0.3942 0.090 Uiso 1 calc R . . C3 C 0.5638(8) 0.719(5) 0.683(5) 0.090(11) Uani 1 d D . . H3A H 0.5778 0.6477 0.7798 0.109 Uiso 1 calc R A 1 H3B H 0.5766 0.8600 0.6863 0.109 Uiso 1 calc R A 1 O61 O 0.5039(7) 0.713(3) 0.682(3) 0.042(4) Uani 0.57(3) d PD B 1 H61 H 0.4922 0.7828 0.6044 0.062 Uiso 0.57(3) calc PR B 1 O62 O 0.5233(10) 0.875(4) 0.641(4) 0.042(4) Uani 0.43(3) d PD B 2 H62 H 0.4999 0.8257 0.5789 0.062 Uiso 0.43(3) calc PR B 2 P2 P 0.85934(12) 0.6837(6) 0.5012(10) 0.0468(8) Uani 1 d D . . F1 F 0.9145(4) 0.5580(16) 0.498(3) 0.079(3) Uani 1 d D . . F2 F 0.8044(4) 0.8099(17) 0.497(3) 0.095(4) Uani 1 d D . . F3 F 0.8413(10) 0.588(4) 0.659(2) 0.22(2) Uani 1 d D . . F4 F 0.8312(7) 0.516(3) 0.404(3) 0.157(12) Uani 1 d D . . F5 F 0.8871(9) 0.854(3) 0.596(3) 0.23(2) Uani 1 d D . . F6 F 0.8772(8) 0.778(3) 0.340(2) 0.155(12) Uani 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0231(5) 0.0378(7) 0.0527(9) -0.0005(18) 0.0000(17) -0.0001(7) P1 0.0265(10) 0.0362(13) 0.0456(14) 0.001(3) -0.001(3) -0.0001(11) N1 0.021(6) 0.029(7) 0.082(13) -0.011(8) -0.011(7) -0.014(6) O1 0.051(11) 0.107(18) 0.051(10) -0.011(10) -0.014(8) -0.011(12) N2 0.025(3) 0.048(5) 0.058(6) 0.002(13) -0.013(9) -0.002(4) O2 0.056(5) 0.041(4) 0.090(9) -0.004(15) 0.013(12) -0.003(5) N3 0.052(12) 0.080(15) 0.044(9) 0.003(10) -0.002(8) 0.016(12) O3 0.077(17) 0.060(13) 0.098(17) 0.016(11) 0.004(13) -0.005(13) C1 0.051(9) 0.075(14) 0.039(8) 0.039(10) 0.018(7) 0.023(10) O4 0.075(13) 0.107(17) 0.082(13) 0.065(13) 0.025(11) 0.051(13) C2 0.028(5) 0.053(9) 0.057(8) -0.015(7) -0.002(5) 0.003(7) O5 0.046(5) 0.038(5) 0.098(14) -0.024(8) -0.017(8) 0.001(4) C3 0.054(13) 0.094(19) 0.12(2) 0.046(18) 0.011(13) 0.046(14) O61 0.032(7) 0.024(6) 0.068(12) 0.016(7) 0.011(6) -0.002(6) O62 0.032(7) 0.024(6) 0.068(12) 0.016(7) 0.011(6) -0.002(6) P2 0.0368(13) 0.055(2) 0.0489(16) 0.000(4) -0.002(3) -0.0032(14) F1 0.051(5) 0.090(8) 0.097(7) -0.021(16) 0.000(13) 0.010(5) F2 0.054(6) 0.071(7) 0.160(12) -0.027(16) -0.025(15) 0.015(6) F3 0.19(3) 0.34(5) 0.133(19) 0.16(3) 0.10(2) 0.15(3) F4 0.062(10) 0.138(15) 0.27(3) -0.137(18) -0.044(13) 0.003(11) F5 0.124(19) 0.099(13) 0.46(6) -0.15(2) -0.16(3) 0.032(14) F6 0.092(13) 0.24(3) 0.133(14) 0.152(19) 0.006(12) -0.010(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.610(18) . ? Fe1 N2 1.708(12) . ? Fe1 N3 1.73(2) . ? Fe1 P1 2.295(3) . ? P1 C1 1.798(17) . ? P1 C2 1.835(17) . ? P1 C3 1.85(4) . ? N1 O1 1.25(2) . ? N2 O2 1.137(15) . ? N3 O3 1.12(3) . ? C1 O4 1.469(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O4 H4 0.8400 . ? C2 O5 1.439(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O5 H5 0.8400 . ? C3 O61 1.480(15) . ? C3 O62 1.481(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O61 H61 0.8400 . ? O62 H62 0.8400 . ? P2 F3 1.514(13) . ? P2 F5 1.535(13) . ? P2 F6 1.536(13) . ? P2 F4 1.539(12) . ? P2 F2 1.595(9) . ? P2 F1 1.597(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 114.4(12) . . ? N1 Fe1 N3 112.9(7) . . ? N2 Fe1 N3 115.4(14) . . ? N1 Fe1 P1 105.5(7) . . ? N2 Fe1 P1 104.9(3) . . ? N3 Fe1 P1 102.0(8) . . ? C1 P1 C2 122.0(9) . . ? C1 P1 C3 105.3(9) . . ? C2 P1 C3 82.3(10) . . ? C1 P1 Fe1 112.6(6) . . ? C2 P1 Fe1 114.8(5) . . ? C3 P1 Fe1 115.7(7) . . ? O1 N1 Fe1 176.9(19) . . ? O2 N2 Fe1 177.4(15) . . ? O3 N3 Fe1 172(3) . . ? O4 C1 P1 109.1(10) . . ? O4 C1 H1A 109.9 . . ? P1 C1 H1A 109.9 . . ? O4 C1 H1B 109.9 . . ? P1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 O4 H4 109.5 . . ? O5 C2 P1 112.4(11) . . ? O5 C2 H2A 109.1 . . ? P1 C2 H2A 109.1 . . ? O5 C2 H2B 109.1 . . ? P1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C2 O5 H5 109.5 . . ? O61 C3 O62 48.8(13) . . ? O61 C3 P1 108(2) . . ? O62 C3 P1 110(2) . . ? O61 C3 H3A 110.0 . . ? O62 C3 H3A 139.1 . . ? P1 C3 H3A 110.0 . . ? O61 C3 H3B 110.0 . . ? O62 C3 H3B 63.8 . . ? P1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C3 O61 H61 109.5 . . ? C3 O62 H62 109.5 . . ? F3 P2 F5 90.1(13) . . ? F3 P2 F6 179.2(14) . . ? F5 P2 F6 90.7(13) . . ? F3 P2 F4 90.9(13) . . ? F5 P2 F4 178.7(14) . . ? F6 P2 F4 88.2(12) . . ? F3 P2 F2 89.3(11) . . ? F5 P2 F2 90.3(8) . . ? F6 P2 F2 90.6(10) . . ? F4 P2 F2 89.0(8) . . ? F3 P2 F1 92.8(10) . . ? F5 P2 F1 90.8(9) . . ? F6 P2 F1 87.2(10) . . ? F4 P2 F1 89.9(8) . . ? F2 P2 F1 177.6(13) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.961 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.175 #======================================END============================= data_3 _database_code_depnum_ccdc_archive 'CCDC 610299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dinitrosyl-bis(1,3,5-triaza-7-phosphatricyclo[3,3,1,1]decane) iron(II) tetrahydrofurane ; _chemical_name_common ; Dinitrosyl-bis(1,3,5-triaza-7-phosphatricyclo(3,3,1,1)decane) iron(ii) tetrahydrofurane ; _chemical_formula_moiety 'C12 H24 Fe N8 O2 P2, C4 H8 O' _chemical_formula_sum 'C16 H32 Fe N8 O3 P2' _chemical_formula_weight 502.29 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 19.4660(9) _cell_length_b 6.5409(4) _cell_length_c 19.0131(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.104(5) _cell_angle_gamma 90.00 _cell_volume 2192.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.3 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.8054 _exptl_absorpt_correction_T_max 0.9180 _exptl_special_details ; During publication a referee correctly found the THF oxygen O21 misplaced. Atoms O21 and C91 had to change places in order to prevent intermolecular H...H collision of 1.69 \%A between old H91 and adjacent H3B atom. The refinement was repeated with correctly assigned atoms in the THF molecule. The refinement improved (R1old=0.0518, wR2old=0.1310; the new values are those of this CIF, which was resent to Cambridge for replacement under the same CCDC number: 610299. The center of gravity of the THF molecule lies on a center of inversion and was therefore set sof=1/2 for each atom. The calculation of H-atoms for the THF molecule was possible with FREE instructions. To stabilize the refinement, nine distance restraints (two O21-C, three C-C, two O21...C and two C...C with distances 1.495(0.015), 1.545(0.015) and 2.200(0.025) \%A) were used. ; _diffrn_ambient_temperature 153(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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 5.0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12492 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 30.28 _reflns_number_total 3253 _reflns_number_gt 2151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^] 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 3253 _refine_ls_number_parameters 131 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.912 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.59342(7) 0.2500 0.01710(14) Uani 1 d S . . P1 P 0.55391(3) 0.38823(9) 0.19427(3) 0.01566(15) Uani 1 d . . . N1 N 0.57223(14) 0.7128(3) 0.31816(15) 0.0296(5) Uani 1 d . . . O1 O 0.62313(14) 0.8105(4) 0.36410(17) 0.0582(8) Uani 1 d . . . N2 N 0.69049(12) 0.2320(4) 0.20446(13) 0.0252(5) Uani 1 d . . . N3 N 0.57457(12) 0.0434(3) 0.12096(13) 0.0198(4) Uani 1 d . . . N4 N 0.60326(14) 0.3745(3) 0.07709(13) 0.0231(5) Uani 1 d . . . C1 C 0.68151(16) 0.3526(4) 0.13606(17) 0.0280(6) Uani 1 d . . . H1A H 0.7027 0.4907 0.1535 0.034 Uiso 1 calc R . . H1B H 0.7119 0.2880 0.1116 0.034 Uiso 1 calc R . . C2 C 0.65415(15) 0.0317(4) 0.17824(16) 0.0247(5) Uani 1 d . . . H2A H 0.6833 -0.0456 0.1552 0.030 Uiso 1 calc R . . H2B H 0.6566 -0.0458 0.2240 0.030 Uiso 1 calc R . . C3 C 0.57061(16) 0.1682(4) 0.05565(15) 0.0232(5) Uani 1 d . . . H3A H 0.5168 0.1815 0.0182 0.028 Uiso 1 calc R . . H3B H 0.5975 0.0959 0.0290 0.028 Uiso 1 calc R . . C4 C 0.55781(15) 0.4979(4) 0.10655(14) 0.0203(5) Uani 1 d . . . H4A H 0.5055 0.5102 0.0653 0.024 Uiso 1 calc R . . H4B H 0.5796 0.6371 0.1187 0.024 Uiso 1 calc R . . C5 C 0.65656(15) 0.3398(4) 0.25002(15) 0.0238(5) Uani 1 d . . . H5A H 0.6830 0.4720 0.2681 0.029 Uiso 1 calc R . . H5B H 0.6644 0.2573 0.2965 0.029 Uiso 1 calc R . . C6 C 0.52609(15) 0.1254(3) 0.15646(15) 0.0207(5) Uani 1 d . . . H6A H 0.5296 0.0347 0.1995 0.025 Uiso 1 calc R . . H6B H 0.4727 0.1261 0.1172 0.025 Uiso 1 calc R . . C91 C 0.7344(4) 0.5746(13) -0.0257(6) 0.0426(8) Uiso 0.50 d PD . . H91A H 0.7513 0.4755 0.0177 0.051 Uiso 0.50 calc PR . . H91B H 0.7035 0.5014 -0.0746 0.051 Uiso 0.50 calc PR . . C81 C 0.6893(4) 0.7438(11) -0.0122(5) 0.0426(8) Uiso 0.50 d PD . . H81A H 0.6684 0.7006 0.0248 0.051 Uiso 0.50 calc PR . . H81B H 0.6470 0.7866 -0.0614 0.051 Uiso 0.50 calc PR . . O21 O 0.7992(3) 0.6718(10) -0.0307(3) 0.0585(14) Uiso 0.50 d PD . . C82 C 0.8212(4) 0.8296(12) 0.0277(4) 0.0426(8) Uiso 0.50 d PD . . H82A H 0.8512 0.9373 0.0168 0.051 Uiso 0.50 calc PR . . H82B H 0.8515 0.7725 0.0800 0.051 Uiso 0.50 calc PR . . C92 C 0.7460(4) 0.9137(13) 0.0214(6) 0.0426(8) Uiso 0.50 d PD . . H92A H 0.7308 1.0349 -0.0130 0.051 Uiso 0.50 calc PR . . H92B H 0.7500 0.9536 0.0732 0.051 Uiso 0.50 calc PR . . 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 0.0207(3) 0.0110(2) 0.0228(3) 0.000 0.0124(2) 0.000 P1 0.0196(3) 0.0120(3) 0.0183(3) 0.0008(2) 0.0109(2) -0.0004(2) N1 0.0296(12) 0.0194(10) 0.0418(14) -0.0075(10) 0.0172(11) 0.0004(9) O1 0.0369(13) 0.0466(15) 0.0710(19) -0.0308(14) 0.0036(13) -0.0073(12) N2 0.0206(11) 0.0277(11) 0.0281(11) -0.0088(9) 0.0111(9) -0.0012(9) N3 0.0239(10) 0.0116(9) 0.0243(10) -0.0014(8) 0.0104(9) 0.0004(7) N4 0.0361(12) 0.0173(10) 0.0227(10) -0.0031(8) 0.0190(10) -0.0050(8) C1 0.0301(14) 0.0274(13) 0.0347(14) -0.0108(11) 0.0217(12) -0.0104(11) C2 0.0270(13) 0.0189(11) 0.0287(13) -0.0017(10) 0.0122(11) 0.0039(10) C3 0.0303(13) 0.0178(11) 0.0205(12) -0.0045(9) 0.0098(11) -0.0024(10) C4 0.0315(13) 0.0115(10) 0.0206(11) 0.0006(8) 0.0136(10) -0.0017(9) C5 0.0219(12) 0.0261(12) 0.0218(12) -0.0036(10) 0.0078(10) 0.0025(10) C6 0.0224(12) 0.0117(10) 0.0289(12) 0.0017(9) 0.0120(10) -0.0023(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.649(2) . ? Fe1 N1 1.649(2) 2_655 ? Fe1 P1 2.2290(6) . ? Fe1 P1 2.2291(6) 2_655 ? P1 C4 1.846(2) . ? P1 C5 1.849(3) . ? P1 C6 1.853(2) . ? N1 O1 1.191(3) . ? N2 C1 1.467(4) . ? N2 C5 1.473(3) . ? N2 C2 1.472(3) . ? N3 C3 1.461(3) . ? N3 C2 1.470(3) . ? N3 C6 1.475(3) . ? N4 C1 1.466(4) . ? N4 C4 1.472(3) . ? N4 C3 1.473(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C91 O21 1.449(8) . ? C91 C81 1.501(9) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C81 C92 1.505(9) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? O21 C82 1.441(8) . ? C82 C92 1.520(9) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 123.49(17) . 2_655 ? N1 Fe1 P1 104.02(8) . . ? N1 Fe1 P1 109.14(9) 2_655 . ? N1 Fe1 P1 109.14(9) . 2_655 ? N1 Fe1 P1 104.01(8) 2_655 2_655 ? P1 Fe1 P1 105.96(4) . 2_655 ? C4 P1 C5 97.80(12) . . ? C4 P1 C6 97.30(11) . . ? C5 P1 C6 97.49(12) . . ? C4 P1 Fe1 113.80(8) . . ? C5 P1 Fe1 116.28(8) . . ? C6 P1 Fe1 128.60(9) . . ? O1 N1 Fe1 175.5(3) . . ? C1 N2 C5 110.5(2) . . ? C1 N2 C2 108.6(2) . . ? C5 N2 C2 110.8(2) . . ? C3 N3 C2 108.5(2) . . ? C3 N3 C6 111.88(19) . . ? C2 N3 C6 111.0(2) . . ? C1 N4 C4 111.1(2) . . ? C1 N4 C3 108.0(2) . . ? C4 N4 C3 110.4(2) . . ? N4 C1 N2 115.2(2) . . ? N4 C1 H1A 108.5 . . ? N2 C1 H1A 108.5 . . ? N4 C1 H1B 108.5 . . ? N2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N3 C2 N2 114.1(2) . . ? N3 C2 H2A 108.7 . . ? N2 C2 H2A 108.7 . . ? N3 C2 H2B 108.7 . . ? N2 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N3 C3 N4 114.6(2) . . ? N3 C3 H3A 108.6 . . ? N4 C3 H3A 108.6 . . ? N3 C3 H3B 108.6 . . ? N4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? N4 C4 P1 113.11(16) . . ? N4 C4 H4A 109.0 . . ? P1 C4 H4A 109.0 . . ? N4 C4 H4B 109.0 . . ? P1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N2 C5 P1 112.96(17) . . ? N2 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N3 C6 P1 112.12(16) . . ? N3 C6 H6A 109.2 . . ? P1 C6 H6A 109.2 . . ? N3 C6 H6B 109.2 . . ? P1 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O21 C91 C81 106.0(6) . . ? O21 C91 H91A 110.5 . . ? C81 C91 H91A 110.5 . . ? O21 C91 H91B 110.5 . . ? C81 C91 H91B 110.5 . . ? H91A C91 H91B 108.7 . . ? C91 C81 C92 103.9(5) . . ? C91 C81 H81A 111.0 . . ? C92 C81 H81A 111.0 . . ? C91 C81 H81B 111.0 . . ? C92 C81 H81B 111.0 . . ? H81A C81 H81B 109.0 . . ? C82 O21 C91 104.4(6) . . ? O21 C82 C92 103.7(6) . . ? O21 C82 H82A 111.0 . . ? C92 C82 H82A 111.0 . . ? O21 C82 H82B 111.0 . . ? C92 C82 H82B 111.0 . . ? H82A C82 H82B 109.0 . . ? C82 C92 C81 106.0(6) . . ? C82 C92 H92A 110.5 . . ? C81 C92 H92A 110.5 . . ? C82 C92 H92B 110.5 . . ? C81 C92 H92B 110.5 . . ? H92A C92 H92B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 P1 C4 -95.18(13) . . . . ? N1 Fe1 P1 C4 38.35(13) 2_655 . . . ? P1 Fe1 P1 C4 149.81(10) 2_655 . . . ? N1 Fe1 P1 C5 17.36(14) . . . . ? N1 Fe1 P1 C5 150.88(13) 2_655 . . . ? P1 Fe1 P1 C5 -97.66(10) 2_655 . . . ? N1 Fe1 P1 C6 142.83(14) . . . . ? N1 Fe1 P1 C6 -83.65(14) 2_655 . . . ? P1 Fe1 P1 C6 27.81(11) 2_655 . . . ? N1 Fe1 N1 O1 -22(3) 2_655 . . . ? P1 Fe1 N1 O1 103(3) . . . . ? P1 Fe1 N1 O1 -144(3) 2_655 . . . ? C4 N4 C1 N2 66.9(3) . . . . ? C3 N4 C1 N2 -54.2(3) . . . . ? C5 N2 C1 N4 -67.4(3) . . . . ? C2 N2 C1 N4 54.2(3) . . . . ? C3 N3 C2 N2 55.1(3) . . . . ? C6 N3 C2 N2 -68.2(3) . . . . ? C1 N2 C2 N3 -54.1(3) . . . . ? C5 N2 C2 N3 67.4(3) . . . . ? C2 N3 C3 N4 -55.8(3) . . . . ? C6 N3 C3 N4 67.0(3) . . . . ? C1 N4 C3 N3 55.0(3) . . . . ? C4 N4 C3 N3 -66.6(3) . . . . ? C1 N4 C4 P1 -59.0(2) . . . . ? C3 N4 C4 P1 60.8(2) . . . . ? C5 P1 C4 N4 48.3(2) . . . . ? C6 P1 C4 N4 -50.4(2) . . . . ? Fe1 P1 C4 N4 171.56(14) . . . . ? C1 N2 C5 P1 60.1(3) . . . . ? C2 N2 C5 P1 -60.3(3) . . . . ? C4 P1 C5 N2 -49.0(2) . . . . ? C6 P1 C5 N2 49.5(2) . . . . ? Fe1 P1 C5 N2 -170.44(16) . . . . ? C3 N3 C6 P1 -60.2(2) . . . . ? C2 N3 C6 P1 61.2(2) . . . . ? C4 P1 C6 N3 49.3(2) . . . . ? C5 P1 C6 N3 -49.6(2) . . . . ? Fe1 P1 C6 N3 177.79(12) . . . . ? O21 C91 C81 C92 -22.1(11) . . . . ? C81 C91 O21 C82 39.0(8) . . . . ? C91 O21 C82 C92 -39.2(7) . . . . ? O21 C82 C92 C81 25.1(9) . . . . ? C91 C81 C92 C82 -1.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.892 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.104 #===============================END of CIF=============================