# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Dmitry Chernyshov' _publ_contact_author_email DMITRY.CHERNYSHOV@ESRF.FR _publ_section_title ; Chemical Disorder and Spin Crossover in Fe(II) complexes ; loop_ _publ_author_name 'Dmitry Chernyshov' 'H Burgi' 'Karl W Tornroos' 'Brita Vangdal' # # END OF FILE # # Attachment 'EtOH_2propanol_mix_16K_No_Laser.cif' # SUBMISSION DETAILS data_Ethanol_2propanol_mix_16K _database_code_depnum_ccdc_archive 'CCDC 714607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_name_common ;tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Fe N6, 0.744(C2 H6 O), 0.256(C3 H8 O), 2(Cl)' _chemical_formula_sum 'C20.25 H30.50 Cl2 Fe N6 O' _chemical_formula_weight 500.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'B 21/c' _symmetry_space_group_name_HALL '-B 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, -y-1/2, z' _cell_length_a 11.3341(12) _cell_length_b 21.512(2) _cell_length_c 19.3534(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.525(8) _cell_angle_gamma 90.00 _cell_volume 4696.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 16(2) _cell_measurement_reflns_used 13942 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 25.47 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details 'SADABS v.2.06 (Sheldrick, 2003)' _exptl_special_details ; Comment on the reduced completeness of data (0.988): the unique crystal axis nearly coincided with the (single) axis,(\f), of rotation and part of the detector was shadowed by the cryostat. However, a 359\% \f-scan corresponding to an almost a full sphere was collected. The program SADABS outputs only the ratio of minimum to maximum apparent transmission. Hence we have calulated the transmission from the geometry of the crystal, i.e. its dimension; T(max)=exp(-t(min)*mu) where t(min)=smallest crystal dimension and T(min)=exp(-t(max)*mu) where t(max)=body diagonal (d) of the crystal d=sqrt(a**2+b**2+c**2). N.B. that checkCIF only uses the largest crystal dimension to calculate T(min) which is an underestimate of the longest path length. ; _diffrn_ambient_temperature 16(2) _diffrn_radiation_wavelength 0.71058 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline BM1A, SNBL, ESRF, Grenoble, France' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'MAR345 Image plate' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean '150 \mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13843 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.45 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.539 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.066 _reflns_number_total 4295 _reflns_number_gt 4000 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'MARCCD control software (MAR, 2002)' _computing_cell_refinement 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.6.10. (Sheldrick, 2000)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Hydrogens were input as riding atoms with N---H(NH~2~) 0.92, C---H(CH) 0.95, C---H(CH~2~) 0.99, C---H(CH~3~) 0.98 and O---H 0.84 \%A. The isotropic displacement parameters of the H atoms were fixed at 1.2U~eq~ and 1.5U~eq~ (CH~3~, OH) of their parent atoms. The crystal consists of a mixture of ethanol (74%) and 2-propanol (26%) as non-coordinated solvent, which accounts for the discrepancy between the chemical formula calulated from the sum of occupancies in the output file and the chemical sum reported. The distances (carbon to carbon and carbon to oxygen) in the solvent molecules were restrained to be equal (SADI) within 0.02 Angstroems. The displacement parameters were also restrained to be equal (EADP). To avoid short intermolecular contacts, C3SB (2-propanol) was restrained (DFIX) to a position 3.12 Angstroms from its symmetry equivalent (1-x,1-y,1-z). The solvents were isotropically refined. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+12.3405P] 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 4295 _refine_ls_number_parameters 273 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.03807(2) 0.366855(11) 0.737428(13) 0.00401(8) Uani 1 1 d . . . Cl1 Cl -0.30059(4) 0.27259(2) 0.61567(2) 0.00886(11) Uani 1 1 d . . . Cl2 Cl 0.38278(4) 0.42981(2) 0.81991(2) 0.00670(10) Uani 1 1 d . . . N1 N 0.09825(13) 0.44855(7) 0.77799(8) 0.0061(3) Uani 1 1 d . . . H1A H 0.1760 0.4443 0.7954 0.007 Uiso 1 1 d R . . H1B H 0.0949 0.4785 0.7437 0.007 Uiso 1 1 d R . . N2 N -0.11256(13) 0.39710(7) 0.77218(8) 0.0064(3) Uani 1 1 d . . . N3 N -0.02735(13) 0.28388(7) 0.70146(8) 0.0069(3) Uani 1 1 d . . . H3A H -0.0940 0.2904 0.6717 0.008 Uiso 1 1 d R . . H3B H 0.0280 0.2639 0.6769 0.008 Uiso 1 1 d R . . N4 N 0.08199(13) 0.31558(7) 0.82225(8) 0.0061(3) Uani 1 1 d . . . N5 N 0.20068(13) 0.35273(7) 0.70583(8) 0.0073(3) Uani 1 1 d . . . H5A H 0.2568 0.3571 0.7430 0.009 Uiso 1 1 d R . . H5B H 0.2062 0.3132 0.6881 0.009 Uiso 1 1 d R . . N6 N 0.00700(13) 0.40035(7) 0.64166(8) 0.0071(3) Uani 1 1 d . . . C1 C 0.02574(15) 0.46842(8) 0.83360(10) 0.0073(4) Uani 1 1 d . . . H1C H 0.0271 0.5143 0.8377 0.009 Uiso 1 1 calc R . . H1D H 0.0584 0.4506 0.8786 0.009 Uiso 1 1 calc R . . C2 C -0.09938(16) 0.44631(8) 0.81606(10) 0.0073(4) Uani 1 1 d . . . C3 C -0.19423(17) 0.47452(9) 0.84376(10) 0.0113(4) Uani 1 1 d . . . H3 H -0.1814 0.5089 0.8744 0.014 Uiso 1 1 calc R . . C4 C -0.30811(16) 0.45222(9) 0.82637(11) 0.0116(4) Uani 1 1 d . . . H4A H -0.3743 0.4706 0.8451 0.014 Uiso 1 1 calc R . . C5 C -0.32266(16) 0.40243(9) 0.78089(10) 0.0102(4) Uani 1 1 d . . . H5 H -0.3996 0.3864 0.7674 0.012 Uiso 1 1 calc R . . C6 C -0.22449(16) 0.37628(9) 0.75538(10) 0.0081(4) Uani 1 1 d . . . H6A H -0.2359 0.3420 0.7245 0.010 Uiso 1 1 calc R . . C7 C -0.05637(16) 0.24496(8) 0.76054(10) 0.0076(4) Uani 1 1 d . . . H7A H -0.0508 0.2004 0.7483 0.009 Uiso 1 1 calc R . . H7B H -0.1385 0.2535 0.7712 0.009 Uiso 1 1 calc R . . C8 C 0.02871(15) 0.25922(8) 0.82283(10) 0.0065(4) Uani 1 1 d . . . C9 C 0.05094(16) 0.21721(8) 0.87699(10) 0.0079(4) Uani 1 1 d . . . H9A H 0.0109 0.1784 0.8760 0.009 Uiso 1 1 calc R . . C10 C 0.13234(16) 0.23263(9) 0.93266(10) 0.0091(4) Uani 1 1 d . . . H10A H 0.1471 0.2052 0.9710 0.011 Uiso 1 1 calc R . . C11 C 0.19164(16) 0.28900(9) 0.93095(10) 0.0085(4) Uani 1 1 d . . . H11A H 0.2503 0.3001 0.9673 0.010 Uiso 1 1 calc R . . C12 C 0.16419(15) 0.32881(8) 0.87568(9) 0.0065(4) Uani 1 1 d . . . H12A H 0.2050 0.3674 0.8752 0.008 Uiso 1 1 calc R . . C13 C 0.21941(16) 0.39853(9) 0.65072(10) 0.0091(4) Uani 1 1 d . . . H13A H 0.2814 0.3834 0.6221 0.011 Uiso 1 1 calc R . . H13B H 0.2456 0.4388 0.6718 0.011 Uiso 1 1 calc R . . C14 C 0.10432(16) 0.40661(8) 0.60647(10) 0.0083(4) Uani 1 1 d . . . C15 C 0.09680(18) 0.41870(9) 0.53615(10) 0.0115(4) Uani 1 1 d . . . H15A H 0.1669 0.4228 0.5133 0.014 Uiso 1 1 calc R . . C16 C -0.01368(19) 0.42479(9) 0.49894(11) 0.0131(4) Uani 1 1 d . . . H16A H -0.0207 0.4330 0.4505 0.016 Uiso 1 1 calc R . . C17 C -0.11340(18) 0.41852(9) 0.53461(11) 0.0133(4) Uani 1 1 d . . . H17A H -0.1903 0.4226 0.5108 0.016 Uiso 1 1 calc R . . C18 C -0.10023(17) 0.40632(8) 0.60499(10) 0.0096(4) Uani 1 1 d . . . H18A H -0.1694 0.4019 0.6287 0.012 Uiso 1 1 calc R . . O1SA O 0.4733(2) 0.61157(14) 0.39993(14) 0.0140(4) Uiso 0.744(6) 1 d PD A 1 H1SA H 0.4343 0.6445 0.3924 0.021 Uiso 0.744(6) 1 calc PR A 1 C1SA C 0.5068(4) 0.60526(16) 0.4738(2) 0.0179(4) Uiso 0.744(6) 1 d PD A 1 H1S1 H 0.5527 0.5665 0.4828 0.022 Uiso 0.744(6) 1 calc PR A 1 H1S2 H 0.4347 0.6027 0.4988 0.022 Uiso 0.744(6) 1 calc PR A 1 C2SA C 0.5815(3) 0.66094(17) 0.50044(18) 0.0179(4) Uiso 0.744(6) 1 d P A 1 H2S1 H 0.6507 0.6646 0.4741 0.027 Uiso 0.744(6) 1 calc PR A 1 H2S2 H 0.6078 0.6550 0.5497 0.027 Uiso 0.744(6) 1 calc PR A 1 H2S3 H 0.5338 0.6989 0.4946 0.027 Uiso 0.744(6) 1 calc PR A 1 O1SB O 0.4542(8) 0.6062(4) 0.4064(4) 0.0140(4) Uiso 0.256(6) 1 d PD A 2 H1SB H 0.4031 0.6340 0.3969 0.021 Uiso 0.256(6) 1 calc PR A 2 C1SB C 0.5145(11) 0.6180(4) 0.4714(6) 0.0179(4) Uiso 0.256(6) 1 d PD A 2 H1S3 H 0.4495 0.6192 0.5029 0.022 Uiso 0.256(6) 1 calc PR A 2 C2SB C 0.5779(8) 0.6785(5) 0.4861(5) 0.0179(4) Uiso 0.256(6) 1 d PD A 2 H2S4 H 0.6074 0.6804 0.5354 0.027 Uiso 0.256(6) 1 calc PR A 2 H2S5 H 0.5230 0.7130 0.4749 0.027 Uiso 0.256(6) 1 calc PR A 2 H2S6 H 0.6448 0.6815 0.4577 0.027 Uiso 0.256(6) 1 calc PR A 2 C3SB C 0.5731(7) 0.5600(3) 0.4891(4) 0.0179(4) Uiso 0.256(6) 1 d PD A 2 H3S1 H 0.5159 0.5259 0.4823 0.027 Uiso 0.256(6) 1 calc PR A 2 H3S2 H 0.6060 0.5611 0.5378 0.027 Uiso 0.256(6) 1 calc PR A 2 H3S3 H 0.6372 0.5536 0.4593 0.027 Uiso 0.256(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00315(13) 0.00322(14) 0.00524(14) -0.00019(10) -0.00170(9) 0.00059(9) Cl1 0.0091(2) 0.0087(2) 0.0083(2) 0.00129(17) -0.00200(16) -0.00296(16) Cl2 0.00445(19) 0.0070(2) 0.0084(2) 0.00144(16) -0.00098(15) -0.00021(15) N1 0.0045(7) 0.0067(7) 0.0069(8) 0.0007(6) -0.0008(6) 0.0010(6) N2 0.0059(7) 0.0054(7) 0.0073(8) 0.0020(6) -0.0021(6) 0.0005(6) N3 0.0061(7) 0.0066(8) 0.0075(8) 0.0003(6) -0.0018(6) 0.0014(6) N4 0.0047(7) 0.0055(7) 0.0081(8) -0.0015(6) 0.0010(6) 0.0009(6) N5 0.0078(7) 0.0063(7) 0.0074(8) -0.0008(6) -0.0019(6) 0.0011(6) N6 0.0090(7) 0.0012(7) 0.0106(8) -0.0018(6) -0.0023(6) 0.0002(6) C1 0.0055(8) 0.0063(9) 0.0102(9) -0.0030(7) 0.0010(7) -0.0004(7) C2 0.0069(8) 0.0054(9) 0.0094(9) 0.0002(7) -0.0004(7) -0.0004(7) C3 0.0098(9) 0.0085(9) 0.0157(10) -0.0034(8) 0.0016(8) -0.0006(7) C4 0.0061(8) 0.0096(9) 0.0196(11) -0.0015(8) 0.0042(7) 0.0021(7) C5 0.0055(8) 0.0090(9) 0.0155(10) 0.0014(8) -0.0012(7) -0.0010(7) C6 0.0069(8) 0.0060(9) 0.0108(9) 0.0003(7) -0.0017(7) -0.0010(7) C7 0.0084(9) 0.0051(9) 0.0089(9) -0.0003(7) -0.0016(7) -0.0023(7) C8 0.0036(8) 0.0063(9) 0.0097(9) -0.0013(7) 0.0013(7) 0.0004(7) C9 0.0079(9) 0.0052(9) 0.0108(9) -0.0002(7) 0.0017(7) -0.0010(7) C10 0.0103(9) 0.0084(9) 0.0085(9) 0.0022(7) 0.0004(7) 0.0025(7) C11 0.0068(8) 0.0100(9) 0.0085(9) -0.0021(7) -0.0013(7) 0.0001(7) C12 0.0052(8) 0.0057(9) 0.0085(9) -0.0015(7) 0.0000(7) -0.0006(6) C13 0.0091(9) 0.0099(9) 0.0083(9) 0.0007(7) 0.0015(7) 0.0006(7) C14 0.0104(9) 0.0040(8) 0.0103(9) -0.0030(7) 0.0002(7) 0.0014(7) C15 0.0181(10) 0.0059(9) 0.0107(10) -0.0009(7) 0.0018(8) 0.0008(7) C16 0.0239(11) 0.0053(9) 0.0092(10) -0.0007(7) -0.0033(8) 0.0009(8) C17 0.0164(10) 0.0055(9) 0.0158(10) -0.0012(8) -0.0097(8) 0.0011(7) C18 0.0101(9) 0.0035(9) 0.0141(10) 0.0005(7) -0.0045(7) 0.0002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.9881(16) . ? Fe1 N4 2.0005(16) . ? Fe1 N2 2.0029(15) . ? Fe1 N1 2.0166(16) . ? Fe1 N5 2.0199(16) . ? Fe1 N3 2.0301(16) . ? N1 C1 1.479(2) . ? N1 H1A 0.9166 . ? N1 H1B 0.9238 . ? N2 C6 1.355(2) . ? N2 C2 1.356(2) . ? N3 C7 1.479(2) . ? N3 H3A 0.9153 . ? N3 H3B 0.9279 . ? N4 C12 1.354(2) . ? N4 C8 1.355(2) . ? N5 C13 1.482(2) . ? N5 H5A 0.9178 . ? N5 H5B 0.9215 . ? N6 C18 1.353(2) . ? N6 C14 1.358(2) . ? C1 C2 1.503(2) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.387(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4A 0.9500 . ? C5 C6 1.380(3) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.501(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.389(3) . ? C9 C10 1.389(3) . ? C9 H9A 0.9500 . ? C10 C11 1.388(3) . ? C10 H10A 0.9500 . ? C11 C12 1.382(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.500(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.380(3) . ? C15 C16 1.389(3) . ? C15 H15A 0.9500 . ? C16 C17 1.387(3) . ? C16 H16A 0.9500 . ? C17 C18 1.381(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O1SA C1SA 1.450(4) . ? O1SA H1SA 0.8400 . ? C1SA C2SA 1.527(4) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2SA H2S1 0.9800 . ? C2SA H2S2 0.9800 . ? C2SA H2S3 0.9800 . ? O1SB C1SB 1.397(11) . ? O1SB H1SB 0.8400 . ? C1SB C3SB 1.439(11) . ? C1SB C2SB 1.501(11) . ? C1SB H1S3 1.0000 . ? C2SB H2S4 0.9800 . ? C2SB H2S5 0.9800 . ? C2SB H2S6 0.9800 . ? C3SB H3S1 0.9800 . ? C3SB H3S2 0.9800 . ? C3SB H3S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 N4 166.55(6) . . ? N6 Fe1 N2 96.61(6) . . ? N4 Fe1 N2 93.23(6) . . ? N6 Fe1 N1 94.02(6) . . ? N4 Fe1 N1 96.48(6) . . ? N2 Fe1 N1 81.58(6) . . ? N6 Fe1 N5 81.78(6) . . ? N4 Fe1 N5 90.19(6) . . ? N2 Fe1 N5 169.30(6) . . ? N1 Fe1 N5 87.97(6) . . ? N6 Fe1 N3 88.45(6) . . ? N4 Fe1 N3 81.40(6) . . ? N2 Fe1 N3 96.07(6) . . ? N1 Fe1 N3 176.77(6) . . ? N5 Fe1 N3 94.46(6) . . ? C1 N1 Fe1 110.14(11) . . ? C1 N1 H1A 110.1 . . ? Fe1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? Fe1 N1 H1B 109.9 . . ? H1A N1 H1B 107.8 . . ? C6 N2 C2 116.89(16) . . ? C6 N2 Fe1 128.36(13) . . ? C2 N2 Fe1 114.69(12) . . ? C7 N3 Fe1 109.49(11) . . ? C7 N3 H3A 110.0 . . ? Fe1 N3 H3A 109.4 . . ? C7 N3 H3B 110.2 . . ? Fe1 N3 H3B 109.8 . . ? H3A N3 H3B 107.9 . . ? C12 N4 C8 117.15(16) . . ? C12 N4 Fe1 127.55(13) . . ? C8 N4 Fe1 115.10(12) . . ? C13 N5 Fe1 108.42(11) . . ? C13 N5 H5A 111.0 . . ? Fe1 N5 H5A 109.4 . . ? C13 N5 H5B 109.0 . . ? Fe1 N5 H5B 110.4 . . ? H5A N5 H5B 108.6 . . ? C18 N6 C14 117.36(17) . . ? C18 N6 Fe1 126.36(13) . . ? C14 N6 Fe1 115.09(12) . . ? N1 C1 C2 108.81(15) . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C3 122.74(17) . . ? N2 C2 C1 115.66(15) . . ? C3 C2 C1 121.60(17) . . ? C2 C3 C4 119.52(18) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.17(17) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C6 C5 C4 119.44(17) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N2 C6 C5 123.23(18) . . ? N2 C6 H6A 118.4 . . ? C5 C6 H6A 118.4 . . ? N3 C7 C8 109.36(14) . . ? N3 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 122.69(17) . . ? N4 C8 C7 115.38(16) . . ? C9 C8 C7 121.94(16) . . ? C8 C9 C10 119.24(17) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C11 C10 C9 118.50(17) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? C12 C11 C10 119.08(17) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? N4 C12 C11 123.23(17) . . ? N4 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N5 C13 C14 108.11(15) . . ? N5 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? N5 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N6 C14 C15 122.50(17) . . ? N6 C14 C13 113.96(16) . . ? C15 C14 C13 123.54(17) . . ? C14 C15 C16 119.74(19) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 118.03(19) . . ? C17 C16 H16A 121.0 . . ? C15 C16 H16A 121.0 . . ? C18 C17 C16 119.58(18) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? N6 C18 C17 122.79(18) . . ? N6 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? O1SA C1SA C2SA 110.1(3) . . ? O1SA C1SA H1S1 109.6 . . ? C2SA C1SA H1S1 109.6 . . ? O1SA C1SA H1S2 109.6 . . ? C2SA C1SA H1S2 109.6 . . ? H1S1 C1SA H1S2 108.2 . . ? C1SB O1SB H1SB 109.5 . . ? O1SB C1SB C3SB 103.4(8) . . ? O1SB C1SB C2SB 120.9(8) . . ? C3SB C1SB C2SB 120.3(9) . . ? O1SB C1SB H1S3 103.2 . . ? C3SB C1SB H1S3 103.2 . . ? C2SB C1SB H1S3 103.2 . . ? C1SB C2SB H2S4 109.5 . . ? C1SB C2SB H2S5 109.5 . . ? H2S4 C2SB H2S5 109.5 . . ? C1SB C2SB H2S6 109.5 . . ? H2S4 C2SB H2S6 109.5 . . ? H2S5 C2SB H2S6 109.5 . . ? C1SB C3SB H3S1 109.5 . . ? C1SB C3SB H3S2 109.5 . . ? H3S1 C3SB H3S2 109.5 . . ? C1SB C3SB H3S3 109.5 . . ? H3S1 C3SB H3S3 109.5 . . ? H3S2 C3SB H3S3 109.5 . . ? 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 N6 Fe1 N1 C1 121.45(12) . . . . ? N4 Fe1 N1 C1 -66.97(12) . . . . ? N2 Fe1 N1 C1 25.35(12) . . . . ? N5 Fe1 N1 C1 -156.93(12) . . . . ? N3 Fe1 N1 C1 -18.2(12) . . . . ? N6 Fe1 N2 C6 71.05(16) . . . . ? N4 Fe1 N2 C6 -99.77(16) . . . . ? N1 Fe1 N2 C6 164.15(17) . . . . ? N5 Fe1 N2 C6 151.8(3) . . . . ? N3 Fe1 N2 C6 -18.09(16) . . . . ? N6 Fe1 N2 C2 -106.20(13) . . . . ? N4 Fe1 N2 C2 82.98(13) . . . . ? N1 Fe1 N2 C2 -13.10(13) . . . . ? N5 Fe1 N2 C2 -25.5(4) . . . . ? N3 Fe1 N2 C2 164.66(13) . . . . ? N6 Fe1 N3 C7 -163.17(12) . . . . ? N4 Fe1 N3 C7 25.68(11) . . . . ? N2 Fe1 N3 C7 -66.68(12) . . . . ? N1 Fe1 N3 C7 -23.5(12) . . . . ? N5 Fe1 N3 C7 115.20(12) . . . . ? N6 Fe1 N4 C12 119.3(3) . . . . ? N2 Fe1 N4 C12 -103.67(15) . . . . ? N1 Fe1 N4 C12 -21.79(15) . . . . ? N5 Fe1 N4 C12 66.19(15) . . . . ? N3 Fe1 N4 C12 160.67(16) . . . . ? N6 Fe1 N4 C8 -55.4(3) . . . . ? N2 Fe1 N4 C8 81.66(13) . . . . ? N1 Fe1 N4 C8 163.54(12) . . . . ? N5 Fe1 N4 C8 -108.48(13) . . . . ? N3 Fe1 N4 C8 -14.00(12) . . . . ? N6 Fe1 N5 C13 26.30(12) . . . . ? N4 Fe1 N5 C13 -164.53(12) . . . . ? N2 Fe1 N5 C13 -55.8(4) . . . . ? N1 Fe1 N5 C13 -68.05(12) . . . . ? N3 Fe1 N5 C13 114.09(12) . . . . ? N4 Fe1 N6 C18 104.3(3) . . . . ? N2 Fe1 N6 C18 -32.51(16) . . . . ? N1 Fe1 N6 C18 -114.48(15) . . . . ? N5 Fe1 N6 C18 158.15(16) . . . . ? N3 Fe1 N6 C18 63.42(15) . . . . ? N4 Fe1 N6 C14 -62.8(3) . . . . ? N2 Fe1 N6 C14 160.37(13) . . . . ? N1 Fe1 N6 C14 78.41(13) . . . . ? N5 Fe1 N6 C14 -8.96(13) . . . . ? N3 Fe1 N6 C14 -103.69(13) . . . . ? Fe1 N1 C1 C2 -32.31(17) . . . . ? C6 N2 C2 C3 0.6(3) . . . . ? Fe1 N2 C2 C3 178.19(15) . . . . ? C6 N2 C2 C1 -179.88(16) . . . . ? Fe1 N2 C2 C1 -2.3(2) . . . . ? N1 C1 C2 N2 23.0(2) . . . . ? N1 C1 C2 C3 -157.50(17) . . . . ? N2 C2 C3 C4 -0.1(3) . . . . ? C1 C2 C3 C4 -179.61(18) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C2 N2 C6 C5 -0.3(3) . . . . ? Fe1 N2 C6 C5 -177.52(14) . . . . ? C4 C5 C6 N2 -0.5(3) . . . . ? Fe1 N3 C7 C8 -32.40(17) . . . . ? C12 N4 C8 C9 3.4(3) . . . . ? Fe1 N4 C8 C9 178.64(14) . . . . ? C12 N4 C8 C7 -176.46(15) . . . . ? Fe1 N4 C8 C7 -1.21(19) . . . . ? N3 C7 C8 N4 22.5(2) . . . . ? N3 C7 C8 C9 -157.30(16) . . . . ? N4 C8 C9 C10 -1.0(3) . . . . ? C7 C8 C9 C10 178.80(17) . . . . ? C8 C9 C10 C11 -2.1(3) . . . . ? C9 C10 C11 C12 2.7(3) . . . . ? C8 N4 C12 C11 -2.7(3) . . . . ? Fe1 N4 C12 C11 -177.28(13) . . . . ? C10 C11 C12 N4 -0.3(3) . . . . ? Fe1 N5 C13 C14 -37.90(17) . . . . ? C18 N6 C14 C15 0.1(3) . . . . ? Fe1 N6 C14 C15 168.44(14) . . . . ? C18 N6 C14 C13 -179.26(16) . . . . ? Fe1 N6 C14 C13 -10.93(19) . . . . ? N5 C13 C14 N6 32.5(2) . . . . ? N5 C13 C14 C15 -146.89(18) . . . . ? N6 C14 C15 C16 -0.1(3) . . . . ? C13 C14 C15 C16 179.23(17) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C15 C16 C17 C18 -0.3(3) . . . . ? C14 N6 C18 C17 -0.2(3) . . . . ? Fe1 N6 C18 C17 -167.08(14) . . . . ? C16 C17 C18 N6 0.3(3) . . . . ? # Attachment 'EtOH_2propanol_mix_16K_Laser.cif' # SUBMISSION DETAILS data_Ethanol_2propanol_mix_16K_Laser _database_code_depnum_ccdc_archive 'CCDC 714608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_name_common ;tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Fe N6, 0.744(C2 H6 O), 0.256(C3 H8 O), 2(Cl)' _chemical_formula_sum 'C20.25 H30.50 Cl2 Fe N6 O' _chemical_formula_weight 500.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'B 21/c' _symmetry_space_group_name_HALL '-B 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, -y-1/2, z' _cell_length_a 11.3823(15) _cell_length_b 21.839(2) _cell_length_c 19.462(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.688(11) _cell_angle_gamma 90.00 _cell_volume 4827.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 16(2) _cell_measurement_reflns_used 13862 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 25.46 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS v.2.06 (Sheldrick, 2003)' _exptl_special_details ; Comment on the reduced completeness of data (0.981): the unique crystal axis nearly coincided with the (single) axis,(\f), of rotation and part of the detector was shadowed by the cryostat. However, a 359\% \f-scan corresponding to an almost a full sphere was collected. The program SADABS outputs only the ratio of minimum to maximum apparent transmission. Hence we have calulated the transmission from the geometry of the crystal, i.e. its dimension; T(max)=exp(-t(min)*mu) where t(min)=smallest crystal dimension and T(min)=exp(-t(max)*mu) where t(max)=body diagonal (d) of the crystal d=sqrt(a**2+b**2+c**2). N.B. that checkCIF only uses the largest crystal dimension to calculate T(min) which is an underestimate of the longest path length. ; _diffrn_ambient_temperature 16(2) _diffrn_radiation_wavelength 0.71058 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline BM1A, SNBL, ESRF, Grenoble, France' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'MAR345 Image plate' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean '150 \mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13603 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.45 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.518 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.078 _reflns_number_total 4386 _reflns_number_gt 4038 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'MARCCD control software (MAR, 2002)' _computing_cell_refinement 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.6.10. (Sheldrick, 2000)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections except for 5 which were found systematically in error. Hydrogens were input as riding atoms with N---H(NH~2~) 0.92, C---H(CH) 0.95, C---H(CH~2~) 0.99, C---H(CH~3~) 0.98 and O---H 0.84 \%A. The isotropic displacement parameters of the H atoms were fixed at 1.2U~eq~ and 1.5U~eq~ (CH~3~, OH) of their parent atoms. The crystal consists of a mixture of ethanol (74%) and 2-propanol (26%) as non-coordinated solvent, which accounts for the discrepancy between the chemical formula calulated from the sum of occupancies in the output file and the chemical sum reported. The distances (carbon to carbon and carbon to oxygen) in the solvent molecules were restrained to be equal (SADI) within 0.02 Angstroems. The displacement parameters were also restrained to be equal (EADP). To avoid short intermolecular contacts, C3SB (2-propanol) was restrained (DFIX) to a position 3.10 Angstroms from its symmetry equivalent (1-x,1-y,1-z). The solvents were isotropically refined. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+15.8747P] 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 4386 _refine_ls_number_parameters 273 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04142(2) 0.365063(13) 0.735619(15) 0.00640(10) Uani 1 1 d . . . Cl1 Cl -0.29931(4) 0.27224(2) 0.62154(3) 0.01061(12) Uani 1 1 d . . . Cl2 Cl 0.37551(4) 0.43225(2) 0.82187(3) 0.00867(12) Uani 1 1 d . . . N1 N 0.09441(15) 0.45182(8) 0.78305(9) 0.0093(4) Uani 1 1 d . . . H1A H 0.1721 0.4476 0.8005 0.011 Uiso 1 1 d R . . H1B H 0.0910 0.4818 0.7488 0.011 Uiso 1 1 d R . . N2 N -0.12153(15) 0.40114(8) 0.77718(9) 0.0087(4) Uani 1 1 d . . . N3 N -0.03263(16) 0.27614(8) 0.70593(9) 0.0089(4) Uani 1 1 d . . . H3A H -0.0993 0.2827 0.6762 0.011 Uiso 1 1 d R . . H3B H 0.0227 0.2562 0.6814 0.011 Uiso 1 1 d R . . N4 N 0.08982(15) 0.30527(8) 0.82453(9) 0.0079(4) Uani 1 1 d . . . N5 N 0.21698(16) 0.36232(8) 0.69681(9) 0.0095(4) Uani 1 1 d . . . H5A H 0.2731 0.3667 0.7339 0.011 Uiso 1 1 d R . . H5B H 0.2225 0.3228 0.6790 0.011 Uiso 1 1 d R . . N6 N 0.01137(16) 0.39616(8) 0.62849(10) 0.0105(4) Uani 1 1 d . . . C1 C 0.01803(18) 0.46902(10) 0.83806(11) 0.0112(4) Uani 1 1 d . . . H1C H 0.0210 0.5139 0.8449 0.013 Uiso 1 1 calc R . . H1D H 0.0468 0.4492 0.8817 0.013 Uiso 1 1 calc R . . C2 C -0.10730(19) 0.44951(9) 0.81977(11) 0.0101(4) Uani 1 1 d . . . C3 C -0.20181(19) 0.47999(10) 0.84563(11) 0.0109(4) Uani 1 1 d . . . H3 H -0.1890 0.5142 0.8753 0.013 Uiso 1 1 calc R . . C4 C -0.31530(19) 0.45994(10) 0.82771(12) 0.0115(4) Uani 1 1 d . . . H4A H -0.3813 0.4799 0.8451 0.014 Uiso 1 1 calc R . . C5 C -0.33056(19) 0.41011(10) 0.78381(11) 0.0119(4) Uani 1 1 d . . . H5 H -0.4073 0.3955 0.7706 0.014 Uiso 1 1 calc R . . C6 C -0.23261(19) 0.38204(10) 0.75963(11) 0.0100(4) Uani 1 1 d . . . H6A H -0.2436 0.3480 0.7295 0.012 Uiso 1 1 calc R . . C7 C -0.05817(18) 0.23950(9) 0.76655(11) 0.0103(4) Uani 1 1 d . . . H7A H -0.0561 0.1955 0.7546 0.012 Uiso 1 1 calc R . . H7B H -0.1383 0.2493 0.7802 0.012 Uiso 1 1 calc R . . C8 C 0.03046(18) 0.25216(9) 0.82654(11) 0.0085(4) Uani 1 1 d . . . C9 C 0.04830(18) 0.21052(10) 0.88033(11) 0.0099(4) Uani 1 1 d . . . H9A H 0.0052 0.1733 0.8804 0.012 Uiso 1 1 calc R . . C10 C 0.12995(19) 0.22439(10) 0.93373(11) 0.0106(4) Uani 1 1 d . . . H10A H 0.1423 0.1973 0.9717 0.013 Uiso 1 1 calc R . . C11 C 0.19364(19) 0.27851(10) 0.93113(11) 0.0108(4) Uani 1 1 d . . . H11A H 0.2516 0.2886 0.9667 0.013 Uiso 1 1 calc R . . C12 C 0.17115(18) 0.31734(10) 0.87595(11) 0.0095(4) Uani 1 1 d . . . H12A H 0.2150 0.3542 0.8742 0.011 Uiso 1 1 calc R . . C13 C 0.22353(19) 0.40830(10) 0.64181(11) 0.0104(4) Uani 1 1 d . . . H13A H 0.2900 0.3985 0.6133 0.012 Uiso 1 1 calc R . . H13B H 0.2378 0.4493 0.6625 0.012 Uiso 1 1 calc R . . C14 C 0.11012(19) 0.40915(9) 0.59702(11) 0.0091(4) Uani 1 1 d . . . C15 C 0.1078(2) 0.42408(10) 0.52761(11) 0.0125(4) Uani 1 1 d . . . H15A H 0.1787 0.4334 0.5066 0.015 Uiso 1 1 calc R . . C16 C 0.0010(2) 0.42524(10) 0.48937(12) 0.0156(5) Uani 1 1 d . . . H16A H -0.0024 0.4356 0.4419 0.019 Uiso 1 1 calc R . . C17 C -0.1007(2) 0.41101(10) 0.52136(12) 0.0141(5) Uani 1 1 d . . . H17A H -0.1751 0.4110 0.4962 0.017 Uiso 1 1 calc R . . C18 C -0.09181(19) 0.39674(10) 0.59096(12) 0.0125(4) Uani 1 1 d . . . H18A H -0.1615 0.3870 0.6130 0.015 Uiso 1 1 calc R . . O1SA O 0.4597(3) 0.61134(14) 0.40270(15) 0.0143(5) Uiso 0.739(6) 1 d PD A 1 H1SA H 0.4126 0.6403 0.3939 0.021 Uiso 0.739(6) 1 calc PR A 1 C1SA C 0.4953(5) 0.6116(2) 0.4741(2) 0.0192(5) Uiso 0.739(6) 1 d PD A 1 H1S1 H 0.5419 0.5744 0.4861 0.023 Uiso 0.739(6) 1 calc PR A 1 H1S2 H 0.4252 0.6118 0.5017 0.023 Uiso 0.739(6) 1 calc PR A 1 C2SA C 0.5729(3) 0.67133(18) 0.4906(2) 0.0192(5) Uiso 0.739(6) 1 d P A 1 H2S1 H 0.6432 0.6702 0.4640 0.029 Uiso 0.739(6) 1 calc PR A 1 H2S2 H 0.5966 0.6726 0.5399 0.029 Uiso 0.739(6) 1 calc PR A 1 H2S3 H 0.5265 0.7079 0.4780 0.029 Uiso 0.739(6) 1 calc PR A 1 O1SB O 0.4820(8) 0.6168(4) 0.3956(4) 0.0143(5) Uiso 0.261(6) 1 d PD A 2 H1SB H 0.4539 0.6506 0.3821 0.021 Uiso 0.261(6) 1 calc PR A 2 C1SB C 0.5035(16) 0.6179(6) 0.4682(7) 0.0192(5) Uiso 0.261(6) 1 d PD A 2 H1S3 H 0.4246 0.6196 0.4880 0.023 Uiso 0.261(6) 1 calc PR A 2 C2SB C 0.5733(10) 0.6564(5) 0.5055(6) 0.0192(5) Uiso 0.261(6) 1 d PD A 2 H2S4 H 0.5839 0.6414 0.5530 0.029 Uiso 0.261(6) 1 calc PR A 2 H2S5 H 0.5372 0.6972 0.5054 0.029 Uiso 0.261(6) 1 calc PR A 2 H2S6 H 0.6501 0.6589 0.4856 0.029 Uiso 0.261(6) 1 calc PR A 2 C3SB C 0.5566(8) 0.5639(3) 0.4919(5) 0.0192(5) Uiso 0.261(6) 1 d PD A 2 H3S1 H 0.4975 0.5312 0.4918 0.029 Uiso 0.261(6) 1 calc PR A 2 H3S2 H 0.5910 0.5699 0.5388 0.029 Uiso 0.261(6) 1 calc PR A 2 H3S3 H 0.6186 0.5524 0.4616 0.029 Uiso 0.261(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00643(16) 0.00333(15) 0.00906(17) -0.00012(11) -0.00237(11) 0.00009(11) Cl1 0.0099(2) 0.0091(2) 0.0124(3) 0.00117(19) -0.00228(19) -0.00203(19) Cl2 0.0064(2) 0.0070(2) 0.0124(3) 0.00088(18) -0.00171(18) 0.00010(17) N1 0.0062(8) 0.0071(8) 0.0142(9) -0.0008(7) -0.0006(7) 0.0015(7) N2 0.0064(8) 0.0071(8) 0.0120(9) 0.0010(7) -0.0024(7) 0.0007(7) N3 0.0084(8) 0.0081(8) 0.0097(9) 0.0000(7) -0.0035(7) 0.0008(7) N4 0.0086(8) 0.0053(8) 0.0096(9) -0.0009(7) -0.0010(7) 0.0002(7) N5 0.0108(9) 0.0074(9) 0.0098(9) -0.0010(7) -0.0046(7) 0.0032(7) N6 0.0118(9) 0.0028(8) 0.0164(10) -0.0004(7) -0.0045(7) 0.0009(7) C1 0.0086(10) 0.0106(10) 0.0142(11) -0.0053(8) -0.0010(8) 0.0002(8) C2 0.0094(10) 0.0058(10) 0.0147(11) 0.0013(8) -0.0019(8) -0.0004(8) C3 0.0123(11) 0.0092(10) 0.0110(11) -0.0015(8) -0.0006(8) 0.0013(8) C4 0.0081(10) 0.0095(10) 0.0173(11) 0.0016(9) 0.0035(8) 0.0019(8) C5 0.0090(10) 0.0106(10) 0.0157(11) 0.0028(9) -0.0015(8) -0.0017(8) C6 0.0108(10) 0.0068(10) 0.0120(11) 0.0009(8) -0.0023(8) -0.0013(8) C7 0.0087(10) 0.0059(10) 0.0158(11) 0.0011(8) -0.0028(8) -0.0020(8) C8 0.0071(10) 0.0061(10) 0.0122(11) -0.0006(8) 0.0001(8) 0.0004(8) C9 0.0093(10) 0.0066(10) 0.0138(11) 0.0002(8) 0.0011(8) -0.0014(8) C10 0.0131(11) 0.0093(10) 0.0093(10) 0.0026(8) -0.0005(8) 0.0010(8) C11 0.0112(10) 0.0105(10) 0.0101(10) -0.0014(8) -0.0032(8) 0.0004(8) C12 0.0094(10) 0.0075(10) 0.0113(11) -0.0018(8) -0.0007(8) -0.0019(8) C13 0.0114(10) 0.0088(10) 0.0107(11) -0.0012(8) -0.0002(8) 0.0003(8) C14 0.0136(10) 0.0022(9) 0.0112(10) -0.0009(8) -0.0003(8) 0.0018(8) C15 0.0197(12) 0.0062(10) 0.0115(11) -0.0025(8) -0.0001(9) 0.0025(9) C16 0.0280(13) 0.0048(10) 0.0134(11) -0.0014(8) -0.0028(10) 0.0020(9) C17 0.0191(12) 0.0071(10) 0.0146(11) -0.0007(8) -0.0112(9) -0.0009(8) C18 0.0121(11) 0.0071(10) 0.0175(12) 0.0005(8) -0.0055(9) -0.0001(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 2.1758(18) . ? Fe1 N3 2.1800(18) . ? Fe1 N5 2.1820(18) . ? Fe1 N6 2.1984(19) . ? Fe1 N4 2.2090(18) . ? Fe1 N2 2.2155(18) . ? N1 C1 1.471(3) . ? N1 H1A 0.9312 . ? N1 H1B 0.9340 . ? N2 C2 1.346(3) . ? N2 C6 1.354(3) . ? N3 C7 1.470(3) . ? N3 H3A 0.9349 . ? N3 H3B 0.9240 . ? N4 C8 1.344(3) . ? N4 C12 1.345(3) . ? N5 C13 1.473(3) . ? N5 H5A 0.9384 . ? N5 H5B 0.9334 . ? N6 C18 1.343(3) . ? N6 C14 1.345(3) . ? C1 C2 1.509(3) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.387(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4A 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.518(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.392(3) . ? C9 C10 1.383(3) . ? C9 H9A 0.9500 . ? C10 C11 1.389(3) . ? C10 H10A 0.9500 . ? C11 C12 1.379(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.510(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.388(3) . ? C15 C16 1.384(3) . ? C15 H15A 0.9500 . ? C16 C17 1.385(3) . ? C16 H16A 0.9500 . ? C17 C18 1.387(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O1SA C1SA 1.422(5) . ? O1SA H1SA 0.8400 . ? C1SA C2SA 1.597(6) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2SA H2S1 0.9800 . ? C2SA H2S2 0.9800 . ? C2SA H2S3 0.9800 . ? O1SB C1SB 1.419(13) . ? O1SB H1SB 0.8400 . ? C1SB C2SB 1.339(15) . ? C1SB C3SB 1.391(15) . ? C1SB H1S3 1.0000 . ? C2SB H2S4 0.9800 . ? C2SB H2S5 0.9800 . ? C2SB H2S6 0.9800 . ? C3SB H3S1 0.9800 . ? C3SB H3S2 0.9800 . ? C3SB H3S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N3 168.53(7) . . ? N1 Fe1 N5 86.32(7) . . ? N3 Fe1 N5 103.35(7) . . ? N1 Fe1 N6 98.93(7) . . ? N3 Fe1 N6 89.42(7) . . ? N5 Fe1 N6 76.72(7) . . ? N1 Fe1 N4 97.71(7) . . ? N3 Fe1 N4 75.74(7) . . ? N5 Fe1 N4 93.85(7) . . ? N6 Fe1 N4 160.25(7) . . ? N1 Fe1 N2 75.59(6) . . ? N3 Fe1 N2 95.45(7) . . ? N5 Fe1 N2 160.56(7) . . ? N6 Fe1 N2 98.83(7) . . ? N4 Fe1 N2 95.55(6) . . ? C1 N1 Fe1 111.74(13) . . ? C1 N1 H1A 110.6 . . ? Fe1 N1 H1A 107.4 . . ? C1 N1 H1B 110.0 . . ? Fe1 N1 H1B 108.1 . . ? H1A N1 H1B 108.9 . . ? C2 N2 C6 118.07(18) . . ? C2 N2 Fe1 115.69(14) . . ? C6 N2 Fe1 126.04(15) . . ? C7 N3 Fe1 111.43(13) . . ? C7 N3 H3A 112.7 . . ? Fe1 N3 H3A 108.2 . . ? C7 N3 H3B 109.6 . . ? Fe1 N3 H3B 107.0 . . ? H3A N3 H3B 107.8 . . ? C8 N4 C12 118.07(18) . . ? C8 N4 Fe1 115.62(14) . . ? C12 N4 Fe1 126.31(14) . . ? C13 N5 Fe1 108.85(13) . . ? C13 N5 H5A 115.2 . . ? Fe1 N5 H5A 108.9 . . ? C13 N5 H5B 110.7 . . ? Fe1 N5 H5B 103.8 . . ? H5A N5 H5B 108.7 . . ? C18 N6 C14 118.55(19) . . ? C18 N6 Fe1 126.59(15) . . ? C14 N6 Fe1 114.43(14) . . ? N1 C1 C2 110.50(18) . . ? N1 C1 H1C 109.6 . . ? C2 C1 H1C 109.6 . . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C3 122.3(2) . . ? N2 C2 C1 116.19(19) . . ? C3 C2 C1 121.50(19) . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C6 C5 C4 119.1(2) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N2 C6 C5 122.6(2) . . ? N2 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? N3 C7 C8 111.23(17) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C9 122.44(19) . . ? N4 C8 C7 116.42(18) . . ? C9 C8 C7 121.14(18) . . ? C10 C9 C8 118.74(19) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C11 119.1(2) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 118.7(2) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? N4 C12 C11 122.91(19) . . ? N4 C12 H12A 118.5 . . ? C11 C12 H12A 118.5 . . ? N5 C13 C14 110.27(17) . . ? N5 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N5 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N6 C14 C15 121.9(2) . . ? N6 C14 C13 116.29(18) . . ? C15 C14 C13 121.8(2) . . ? C16 C15 C14 119.2(2) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C17 119.0(2) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C16 C17 C18 118.6(2) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? N6 C18 C17 122.7(2) . . ? N6 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? O1SA C1SA C2SA 108.6(3) . . ? O1SA C1SA H1S1 110.0 . . ? C2SA C1SA H1S1 110.0 . . ? O1SA C1SA H1S2 110.0 . . ? C2SA C1SA H1S2 110.0 . . ? H1S1 C1SA H1S2 108.4 . . ? C1SB O1SB H1SB 109.5 . . ? C2SB C1SB C3SB 97.1(12) . . ? C2SB C1SB O1SB 127.6(12) . . ? C3SB C1SB O1SB 110.9(11) . . ? C2SB C1SB H1S3 106.5 . . ? C3SB C1SB H1S3 106.5 . . ? O1SB C1SB H1S3 106.5 . . ? C1SB C2SB H2S4 109.5 . . ? C1SB C2SB H2S5 109.5 . . ? H2S4 C2SB H2S5 109.5 . . ? C1SB C2SB H2S6 109.5 . . ? H2S4 C2SB H2S6 109.5 . . ? H2S5 C2SB H2S6 109.5 . . ? C1SB C3SB H3S1 109.5 . . ? C1SB C3SB H3S2 109.5 . . ? H3S1 C3SB H3S2 109.5 . . ? C1SB C3SB H3S3 109.5 . . ? H3S1 C3SB H3S3 109.5 . . ? H3S2 C3SB H3S3 109.5 . . ? 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 N1 C1 -14.0(4) . . . . ? N5 Fe1 N1 C1 -161.73(14) . . . . ? N6 Fe1 N1 C1 122.34(14) . . . . ? N4 Fe1 N1 C1 -68.34(14) . . . . ? N2 Fe1 N1 C1 25.44(14) . . . . ? N1 Fe1 N2 C2 -11.31(15) . . . . ? N3 Fe1 N2 C2 161.40(15) . . . . ? N5 Fe1 N2 C2 -33.3(3) . . . . ? N6 Fe1 N2 C2 -108.34(15) . . . . ? N4 Fe1 N2 C2 85.24(15) . . . . ? N1 Fe1 N2 C6 163.40(18) . . . . ? N3 Fe1 N2 C6 -23.89(18) . . . . ? N5 Fe1 N2 C6 141.4(2) . . . . ? N6 Fe1 N2 C6 66.38(18) . . . . ? N4 Fe1 N2 C6 -100.05(17) . . . . ? N1 Fe1 N3 C7 -29.8(4) . . . . ? N5 Fe1 N3 C7 117.01(14) . . . . ? N6 Fe1 N3 C7 -166.79(14) . . . . ? N4 Fe1 N3 C7 26.39(13) . . . . ? N2 Fe1 N3 C7 -67.97(14) . . . . ? N1 Fe1 N4 C8 154.60(14) . . . . ? N3 Fe1 N4 C8 -15.79(14) . . . . ? N5 Fe1 N4 C8 -118.60(15) . . . . ? N6 Fe1 N4 C8 -58.2(3) . . . . ? N2 Fe1 N4 C8 78.44(15) . . . . ? N1 Fe1 N4 C12 -24.88(18) . . . . ? N3 Fe1 N4 C12 164.72(18) . . . . ? N5 Fe1 N4 C12 61.91(17) . . . . ? N6 Fe1 N4 C12 122.3(2) . . . . ? N2 Fe1 N4 C12 -101.05(17) . . . . ? N1 Fe1 N5 C13 -72.10(13) . . . . ? N3 Fe1 N5 C13 114.16(13) . . . . ? N6 Fe1 N5 C13 27.98(13) . . . . ? N4 Fe1 N5 C13 -169.59(13) . . . . ? N2 Fe1 N5 C13 -50.8(3) . . . . ? N1 Fe1 N6 C18 -115.30(17) . . . . ? N3 Fe1 N6 C18 56.80(18) . . . . ? N5 Fe1 N6 C18 160.66(18) . . . . ? N4 Fe1 N6 C18 97.6(3) . . . . ? N2 Fe1 N6 C18 -38.63(18) . . . . ? N1 Fe1 N6 C14 72.42(15) . . . . ? N3 Fe1 N6 C14 -115.48(14) . . . . ? N5 Fe1 N6 C14 -11.62(14) . . . . ? N4 Fe1 N6 C14 -74.7(3) . . . . ? N2 Fe1 N6 C14 149.09(14) . . . . ? Fe1 N1 C1 C2 -35.6(2) . . . . ? C6 N2 C2 C3 -0.2(3) . . . . ? Fe1 N2 C2 C3 174.96(16) . . . . ? C6 N2 C2 C1 179.82(19) . . . . ? Fe1 N2 C2 C1 -5.0(2) . . . . ? N1 C1 C2 N2 26.9(3) . . . . ? N1 C1 C2 C3 -153.1(2) . . . . ? N2 C2 C3 C4 0.5(3) . . . . ? C1 C2 C3 C4 -179.5(2) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C2 N2 C6 C5 -0.2(3) . . . . ? Fe1 N2 C6 C5 -174.76(16) . . . . ? C4 C5 C6 N2 0.2(3) . . . . ? Fe1 N3 C7 C8 -33.4(2) . . . . ? C12 N4 C8 C9 1.6(3) . . . . ? Fe1 N4 C8 C9 -177.95(16) . . . . ? C12 N4 C8 C7 -178.39(18) . . . . ? Fe1 N4 C8 C7 2.1(2) . . . . ? N3 C7 C8 N4 20.9(3) . . . . ? N3 C7 C8 C9 -159.10(19) . . . . ? N4 C8 C9 C10 0.1(3) . . . . ? C7 C8 C9 C10 -179.89(19) . . . . ? C8 C9 C10 C11 -1.7(3) . . . . ? C9 C10 C11 C12 1.5(3) . . . . ? C8 N4 C12 C11 -1.8(3) . . . . ? Fe1 N4 C12 C11 177.69(15) . . . . ? C10 C11 C12 N4 0.3(3) . . . . ? Fe1 N5 C13 C14 -40.00(19) . . . . ? C18 N6 C14 C15 1.2(3) . . . . ? Fe1 N6 C14 C15 174.12(15) . . . . ? C18 N6 C14 C13 179.56(18) . . . . ? Fe1 N6 C14 C13 -7.5(2) . . . . ? N5 C13 C14 N6 32.3(2) . . . . ? N5 C13 C14 C15 -149.34(19) . . . . ? N6 C14 C15 C16 -0.5(3) . . . . ? C13 C14 C15 C16 -178.78(19) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C15 C16 C17 C18 0.7(3) . . . . ? C14 N6 C18 C17 -0.9(3) . . . . ? Fe1 N6 C18 C17 -172.92(16) . . . . ? C16 C17 C18 N6 0.0(3) . . . . ? # # END OF FILE # # Attachment 'EtOH_2propanol_mix_118K.cif' # SUBMISSION DETAILS data_Ethanol_2propanol_mix_118K _database_code_depnum_ccdc_archive 'CCDC 714609' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_name_common ;tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Fe N6, 0.744(C2 H6 O), 0.256(C3 H8 O), 2(Cl)' _chemical_formula_sum 'C20.25 H30.50 Cl2 Fe N6 O' _chemical_formula_weight 500.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'B 21/c' _symmetry_space_group_name_HALL '-B 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, -y-1/2, z' _cell_length_a 11.3976(14) _cell_length_b 21.667(2) _cell_length_c 19.454(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.540(10) _cell_angle_gamma 90.00 _cell_volume 4781.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 16063 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 25.43 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details 'SADABS v.2.06 (Sheldrick, 2003)' _exptl_special_details ; Comment on the reduced completeness of data (0.992): the unique crystal axis nearly coincided with the (single) axis,(\f), of rotation and part of the detector was shadowed by the cryostat. However, a 359\% \f-scan corresponding to an almost a full sphere was collected. The program SADABS outputs only the ratio of minimum to maximum apparent transmission. Hence we have calulated the transmission from the geometry of the crystal, i.e. its dimension; T(max)=exp(-t(min)*mu) where t(min)=smallest crystal dimension and T(min)=exp(-t(max)*mu) where t(max)=body diagonal (d) of the crystal d=sqrt(a**2+b**2+c**2). N.B. that checkCIF only uses the largest crystal dimension to calculate T(min) which is an underestimate of the longest path length. ; _diffrn_ambient_temperature 118(2) _diffrn_radiation_wavelength 0.71058 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline BM1A, SNBL, ESRF, Grenoble, France' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'MAR345 Image plate' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean '150 \mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 15797 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.43 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.754 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.054 _reflns_number_total 4374 _reflns_number_gt 3954 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'MARCCD control software (MAR, 2002)' _computing_cell_refinement 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.6.10. (Sheldrick, 2000)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Hydrogens were input as riding atoms with N---H(NH~2~) 0.92, C---H(CH) 0.95, C---H(CH~2~) 0.99, C---H(CH~3~) 0.98 and O---H 0.84 \%A. The isotropic displacement parameters of the H atoms were fixed at 1.2U~eq~ and 1.5U~eq~ (CH~3~, OH) of their parent atoms. The crystal consists of a mixture of ethanol (74%) and 2-propanol (26%) as non-coordinated solvent, which accounts for the discrepancy between the chemical formula calulated from the sum of occupancies in the output file and the chemical sum reported. The ratio beteween the solvents is based upon the ratio determinad at 16K. The two solvent molecules also suffers from two-fold disorder; ethanol in the ratio 0.52(A) and 0.22(C); 2-propanol in the ratio 0.12(B) and 0.14(D). The distances (carbon to carbon and carbon to oxygen) in the solvent molecules were restrained to be equal (SADI) within 0.02 Angstroems. The displacement parameters were also restrained to be equal (EADP). To avoid short intermolecular contacts, H3S6 (2-propanol) was restrained (DFIX) to a position 2.11 Angstroems from H15A (1-x,1-y,1-z). In addition, the restrain BUMP was applied. The solvents were isotropically refined. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+9.0272P] 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 4374 _refine_ls_number_parameters 296 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.03774(2) 0.366301(12) 0.736124(14) 0.01478(9) Uani 1 1 d . . . Cl1 Cl -0.30354(4) 0.27292(2) 0.61777(3) 0.02455(12) Uani 1 1 d . . . Cl2 Cl 0.38079(4) 0.43002(2) 0.81848(3) 0.02085(12) Uani 1 1 d . . . N1 N 0.09646(14) 0.44911(7) 0.77911(9) 0.0188(3) Uani 1 1 d . . . H1A H 0.1742 0.4449 0.7965 0.023 Uiso 1 1 d R . . H1B H 0.0931 0.4791 0.7448 0.023 Uiso 1 1 d R . . N2 N -0.11515(14) 0.39801(7) 0.77343(8) 0.0174(3) Uani 1 1 d . . . N3 N -0.03122(14) 0.28160(7) 0.70229(8) 0.0183(3) Uani 1 1 d . . . H3A H -0.0979 0.2882 0.6725 0.022 Uiso 1 1 d R . . H3B H 0.0242 0.2617 0.6777 0.022 Uiso 1 1 d R . . N4 N 0.08413(15) 0.31238(8) 0.82186(8) 0.0210(4) Uani 1 1 d . . . N5 N 0.20153(17) 0.35527(9) 0.70218(10) 0.0349(5) Uani 1 1 d . . . H5A H 0.2577 0.3597 0.7393 0.042 Uiso 1 1 d R . . H5B H 0.2071 0.3158 0.6844 0.042 Uiso 1 1 d R . . N6 N 0.00382(16) 0.39915(8) 0.63742(10) 0.0253(4) Uani 1 1 d . . . C1 C 0.02400(17) 0.46829(9) 0.83403(11) 0.0213(4) Uani 1 1 d . . . H1C H 0.0256 0.5138 0.8385 0.026 Uiso 1 1 calc R . . H1D H 0.0564 0.4503 0.8787 0.026 Uiso 1 1 calc R . . C2 C -0.10050(17) 0.44676(9) 0.81676(10) 0.0191(4) Uani 1 1 d . . . C3 C -0.19447(18) 0.47514(10) 0.84436(12) 0.0259(5) Uani 1 1 d . . . H3 H -0.1811 0.5093 0.8747 0.031 Uiso 1 1 calc R . . C4 C -0.30770(18) 0.45347(10) 0.82745(12) 0.0280(5) Uani 1 1 d . . . H4A H -0.3730 0.4722 0.8461 0.034 Uiso 1 1 calc R . . C5 C -0.32361(18) 0.40390(10) 0.78267(11) 0.0250(5) Uani 1 1 d . . . H5 H -0.4003 0.3881 0.7698 0.030 Uiso 1 1 calc R . . C6 C -0.22647(17) 0.37787(9) 0.75711(11) 0.0211(4) Uani 1 1 d . . . H6A H -0.2384 0.3439 0.7263 0.025 Uiso 1 1 calc R . . C7 C -0.05788(17) 0.24355(9) 0.76173(11) 0.0211(4) Uani 1 1 d . . . H7A H -0.0533 0.1993 0.7497 0.025 Uiso 1 1 calc R . . H7B H -0.1390 0.2524 0.7732 0.025 Uiso 1 1 calc R . . C8 C 0.02842(17) 0.25738(9) 0.82310(10) 0.0187(4) Uani 1 1 d . . . C9 C 0.04814(18) 0.21623(9) 0.87761(11) 0.0227(4) Uani 1 1 d . . . H9A H 0.0063 0.1783 0.8773 0.027 Uiso 1 1 calc R . . C10 C 0.1294(2) 0.23121(10) 0.93234(11) 0.0263(5) Uani 1 1 d . . . H10A H 0.1427 0.2042 0.9708 0.032 Uiso 1 1 calc R . . C11 C 0.19134(19) 0.28611(10) 0.93036(11) 0.0257(5) Uani 1 1 d . . . H11A H 0.2500 0.2967 0.9665 0.031 Uiso 1 1 calc R . . C12 C 0.16615(19) 0.32518(10) 0.87479(10) 0.0249(5) Uani 1 1 d . . . H12A H 0.2085 0.3629 0.8737 0.030 Uiso 1 1 calc R . . C13 C 0.2155(2) 0.40040(12) 0.64681(12) 0.0350(6) Uani 1 1 d . . . H13A H 0.2773 0.3862 0.6180 0.042 Uiso 1 1 calc R . . H13B H 0.2399 0.4408 0.6672 0.042 Uiso 1 1 calc R . . C14 C 0.1003(2) 0.40700(9) 0.60300(12) 0.0270(5) Uani 1 1 d . . . C15 C 0.0921(2) 0.41956(11) 0.53292(13) 0.0362(6) Uani 1 1 d . . . H15A H 0.1614 0.4248 0.5101 0.043 Uiso 1 1 calc R . . C16 C -0.0177(3) 0.42444(11) 0.49644(14) 0.0417(6) Uani 1 1 d . . . H16A H -0.0251 0.4329 0.4483 0.050 Uiso 1 1 calc R . . C17 C -0.1166(2) 0.41674(11) 0.53162(15) 0.0425(7) Uani 1 1 d . . . H17A H -0.1933 0.4200 0.5079 0.051 Uiso 1 1 calc R . . C18 C -0.1026(2) 0.40431(10) 0.60148(13) 0.0334(5) Uani 1 1 d . . . H18A H -0.1710 0.3992 0.6252 0.040 Uiso 1 1 calc R . . O1SA O 0.4668(4) 0.6085(3) 0.4043(2) 0.0316(7) Uiso 0.523(4) 1 d PD A 1 H1SA H 0.4207 0.6387 0.3979 0.047 Uiso 0.523(4) 1 calc PR A 1 C1SA C 0.5119(7) 0.6055(3) 0.4771(4) 0.0347(8) Uiso 0.523(4) 1 d PD A 1 H1S1 H 0.5651 0.5696 0.4856 0.042 Uiso 0.523(4) 1 calc PR A 1 H1S2 H 0.4462 0.6015 0.5065 0.042 Uiso 0.523(4) 1 calc PR A 1 C2SA C 0.5814(6) 0.6678(3) 0.4938(4) 0.0347(8) Uiso 0.523(4) 1 d PD A 1 H2S1 H 0.6337 0.6759 0.4577 0.052 Uiso 0.523(4) 1 calc PR A 1 H2S2 H 0.6284 0.6642 0.5385 0.052 Uiso 0.523(4) 1 calc PR A 1 H2S3 H 0.5252 0.7019 0.4955 0.052 Uiso 0.523(4) 1 calc PR A 1 O1SB O 0.3984(11) 0.6011(6) 0.4604(7) 0.0316(7) Uiso 0.125(2) 1 d PD B 2 H1SB H 0.3835 0.6061 0.5015 0.047 Uiso 0.125(2) 1 calc PR B 2 C1SB C 0.5211(14) 0.6152(10) 0.4545(12) 0.0347(8) Uiso 0.125(2) 1 d PD B 2 H1S3 H 0.5376 0.6251 0.4062 0.042 Uiso 0.125(2) 1 calc PR B 2 C2SB C 0.577(3) 0.6550(9) 0.5032(19) 0.0347(8) Uiso 0.125(2) 1 d PD B 2 H2S4 H 0.5725 0.6974 0.4854 0.052 Uiso 0.125(2) 1 calc PR B 2 H2S5 H 0.6604 0.6431 0.5123 0.052 Uiso 0.125(2) 1 calc PR B 2 H2S6 H 0.5391 0.6527 0.5461 0.052 Uiso 0.125(2) 1 calc PR B 2 C3SB C 0.5699(15) 0.5601(6) 0.4780(7) 0.0347(8) Uiso 0.125(2) 1 d PD B 2 H3S1 H 0.5189 0.5260 0.4606 0.052 Uiso 0.125(2) 1 calc PR B 2 H3S2 H 0.5775 0.5598 0.5286 0.052 Uiso 0.125(2) 1 calc PR B 2 H3S3 H 0.6479 0.5553 0.4615 0.052 Uiso 0.125(2) 1 calc PR B 2 O1SC O 0.4857(9) 0.6186(5) 0.3952(6) 0.0316(7) Uiso 0.217(4) 1 d PD C 3 H1SC H 0.4430 0.6492 0.3836 0.047 Uiso 0.217(4) 1 calc PR C 3 C1SC C 0.4910(15) 0.6099(10) 0.4714(7) 0.0347(8) Uiso 0.217(4) 1 d PD C 3 H1S4 H 0.5107 0.5663 0.4825 0.042 Uiso 0.217(4) 1 calc PR C 3 H1S5 H 0.4122 0.6184 0.4867 0.042 Uiso 0.217(4) 1 calc PR C 3 C2SC C 0.5815(17) 0.6514(8) 0.5117(10) 0.0347(8) Uiso 0.217(4) 1 d PD C 3 H2S7 H 0.5530 0.6628 0.5559 0.052 Uiso 0.217(4) 1 calc PR C 3 H2S8 H 0.5931 0.6889 0.4848 0.052 Uiso 0.217(4) 1 calc PR C 3 H2S9 H 0.6566 0.6294 0.5202 0.052 Uiso 0.217(4) 1 calc PR C 3 O1SD O 0.4369(14) 0.6055(8) 0.4136(8) 0.0316(7) Uiso 0.135(2) 1 d PD D 4 H1SD H 0.4443 0.6302 0.3810 0.047 Uiso 0.135(2) 1 calc PR D 4 C1SD C 0.512(2) 0.6259(7) 0.4756(11) 0.0347(8) Uiso 0.135(2) 1 d PD D 4 H1S6 H 0.4555 0.6283 0.5118 0.042 Uiso 0.135(2) 1 calc PR D 4 C2SD C 0.5675(19) 0.6838(9) 0.4800(12) 0.0347(8) Uiso 0.135(2) 1 d PD D 4 H2SX H 0.5102 0.7159 0.4650 0.052 Uiso 0.135(2) 1 calc PR D 4 H2SY H 0.6322 0.6843 0.4503 0.052 Uiso 0.135(2) 1 calc PR D 4 H2SZ H 0.5988 0.6916 0.5280 0.052 Uiso 0.135(2) 1 calc PR D 4 C3SD C 0.5862(11) 0.5777(5) 0.4982(10) 0.0347(8) Uiso 0.135(2) 1 d PD D 4 H3S4 H 0.5429 0.5387 0.4933 0.052 Uiso 0.135(2) 1 calc PR D 4 H3S5 H 0.6145 0.5841 0.5469 0.052 Uiso 0.135(2) 1 calc PR D 4 H3S6 H 0.6535 0.5764 0.4705 0.052 Uiso 0.135(2) 1 calc PRD D 4 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 0.01532(14) 0.01203(14) 0.01628(15) -0.00051(10) -0.00215(10) 0.00196(10) Cl1 0.0244(3) 0.0267(3) 0.0216(3) 0.0039(2) -0.00295(19) -0.0076(2) Cl2 0.0134(2) 0.0219(2) 0.0269(3) 0.00731(19) 0.00017(18) 0.00102(18) N1 0.0136(8) 0.0190(8) 0.0241(9) 0.0058(7) 0.0027(7) 0.0023(6) N2 0.0135(8) 0.0178(8) 0.0205(8) 0.0018(7) -0.0001(6) -0.0002(6) N3 0.0138(8) 0.0201(8) 0.0201(9) -0.0019(7) -0.0027(6) 0.0014(6) N4 0.0227(9) 0.0226(9) 0.0177(8) -0.0012(7) 0.0020(7) -0.0087(7) N5 0.0356(11) 0.0380(11) 0.0282(10) -0.0137(9) -0.0120(8) 0.0226(9) N6 0.0237(9) 0.0115(8) 0.0386(11) -0.0016(7) -0.0079(8) 0.0017(7) C1 0.0163(10) 0.0194(10) 0.0283(11) -0.0042(8) 0.0025(8) -0.0009(8) C2 0.0160(9) 0.0169(9) 0.0244(11) 0.0023(8) 0.0025(8) 0.0011(7) C3 0.0219(11) 0.0219(11) 0.0345(12) -0.0058(9) 0.0065(9) 0.0008(8) C4 0.0167(10) 0.0265(11) 0.0423(13) -0.0014(10) 0.0099(9) 0.0032(8) C5 0.0133(9) 0.0251(11) 0.0365(12) 0.0019(9) 0.0018(8) -0.0026(8) C6 0.0169(10) 0.0198(10) 0.0261(11) 0.0019(8) 0.0001(8) -0.0016(8) C7 0.0183(10) 0.0166(10) 0.0277(11) 0.0007(8) -0.0020(8) -0.0038(8) C8 0.0164(9) 0.0183(10) 0.0216(10) -0.0013(8) 0.0031(8) -0.0024(8) C9 0.0231(10) 0.0187(10) 0.0262(11) 0.0009(8) 0.0012(8) -0.0023(8) C10 0.0310(12) 0.0240(11) 0.0234(11) 0.0048(9) -0.0002(9) 0.0011(9) C11 0.0244(11) 0.0319(12) 0.0199(10) -0.0015(9) -0.0030(8) -0.0048(9) C12 0.0258(11) 0.0285(11) 0.0202(10) -0.0003(8) 0.0015(8) -0.0106(9) C13 0.0233(11) 0.0484(15) 0.0334(13) -0.0145(11) 0.0035(10) 0.0097(10) C14 0.0312(12) 0.0174(10) 0.0312(12) -0.0090(9) -0.0024(9) 0.0058(9) C15 0.0475(15) 0.0257(12) 0.0346(13) -0.0070(10) 0.0005(11) 0.0065(11) C16 0.0664(19) 0.0199(12) 0.0349(14) -0.0013(10) -0.0142(13) 0.0038(11) C17 0.0452(15) 0.0215(12) 0.0551(17) 0.0086(11) -0.0253(13) -0.0037(10) C18 0.0275(12) 0.0190(11) 0.0500(15) 0.0094(10) -0.0157(10) -0.0018(9) _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 N6 2.0493(19) . ? Fe1 N5 2.053(2) . ? Fe1 N4 2.0631(17) . ? Fe1 N1 2.0636(17) . ? Fe1 N2 2.0687(16) . ? Fe1 N3 2.0782(16) . ? N1 C1 1.472(2) . ? N1 H1A 0.9217 . ? N1 H1B 0.9295 . ? N2 C6 1.350(3) . ? N2 C2 1.352(3) . ? N3 C7 1.475(3) . ? N3 H3A 0.9203 . ? N3 H3B 0.9334 . ? N4 C12 1.351(3) . ? N4 C8 1.352(3) . ? N5 C13 1.475(3) . ? N5 H5A 0.9225 . ? N5 H5B 0.9278 . ? N6 C18 1.345(3) . ? N6 C14 1.353(3) . ? C1 C2 1.501(3) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.387(3) . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4A 0.9500 . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.502(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.387(3) . ? C9 C10 1.381(3) . ? C9 H9A 0.9500 . ? C10 C11 1.385(3) . ? C10 H10A 0.9500 . ? C11 C12 1.381(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.501(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.385(3) . ? C15 C16 1.382(4) . ? C15 H15A 0.9500 . ? C16 C17 1.384(4) . ? C16 H16A 0.9500 . ? C17 C18 1.380(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O1SA C1SA 1.461(7) . ? O1SA H1SA 0.8400 . ? C1SA C2SA 1.583(9) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2SA H2S1 0.9800 . ? C2SA H2S2 0.9800 . ? C2SA H2S3 0.9800 . ? O1SB C1SB 1.447(14) . ? O1SB H1SB 0.8400 . ? C1SB C3SB 1.376(19) . ? C1SB C2SB 1.39(2) . ? C1SB H1S3 1.0000 . ? C2SB H2S4 0.9800 . ? C2SB H2S5 0.9800 . ? C2SB H2S6 0.9800 . ? C3SB H3S1 0.9800 . ? C3SB H3S2 0.9800 . ? C3SB H3S3 0.9800 . ? O1SC C1SC 1.490(13) . ? O1SC H1SC 0.8400 . ? C1SC C2SC 1.527(15) . ? C1SC H1S4 0.9900 . ? C1SC H1S5 0.9900 . ? C2SC H2S7 0.9800 . ? C2SC H2S8 0.9800 . ? C2SC H2S9 0.9800 . ? O1SD C1SD 1.477(15) . ? O1SD H1SD 0.8400 . ? C1SD C3SD 1.389(18) . ? C1SD C2SD 1.403(19) . ? C1SD H1S6 1.0000 . ? C2SD H2SX 0.9800 . ? C2SD H2SY 0.9800 . ? C2SD H2SZ 0.9800 . ? C3SD H3S4 0.9800 . ? C3SD H3S5 0.9800 . ? C3SD H3S6 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 N5 80.46(7) . . ? N6 Fe1 N4 164.72(7) . . ? N5 Fe1 N4 91.38(7) . . ? N6 Fe1 N1 95.86(7) . . ? N5 Fe1 N1 87.83(7) . . ? N4 Fe1 N1 96.72(7) . . ? N6 Fe1 N2 97.13(7) . . ? N5 Fe1 N2 166.97(7) . . ? N4 Fe1 N2 93.63(7) . . ? N1 Fe1 N2 79.65(6) . . ? N6 Fe1 N3 88.77(7) . . ? N5 Fe1 N3 97.07(7) . . ? N4 Fe1 N3 79.37(6) . . ? N1 Fe1 N3 173.77(7) . . ? N2 Fe1 N3 95.67(6) . . ? C1 N1 Fe1 110.91(12) . . ? C1 N1 H1A 110.4 . . ? Fe1 N1 H1A 109.0 . . ? C1 N1 H1B 109.7 . . ? Fe1 N1 H1B 109.1 . . ? H1A N1 H1B 107.7 . . ? C6 N2 C2 117.12(17) . . ? C6 N2 Fe1 127.91(14) . . ? C2 N2 Fe1 114.89(13) . . ? C7 N3 Fe1 110.20(12) . . ? C7 N3 H3A 111.0 . . ? Fe1 N3 H3A 109.1 . . ? C7 N3 H3B 110.0 . . ? Fe1 N3 H3B 108.5 . . ? H3A N3 H3B 107.9 . . ? C12 N4 C8 117.33(18) . . ? C12 N4 Fe1 127.19(14) . . ? C8 N4 Fe1 115.43(13) . . ? C13 N5 Fe1 108.86(13) . . ? C13 N5 H5A 112.8 . . ? Fe1 N5 H5A 108.7 . . ? C13 N5 H5B 108.9 . . ? Fe1 N5 H5B 108.9 . . ? H5A N5 H5B 108.6 . . ? C18 N6 C14 117.9(2) . . ? C18 N6 Fe1 126.52(17) . . ? C14 N6 Fe1 114.75(14) . . ? N1 C1 C2 109.54(16) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.2 . . ? N2 C2 C3 122.29(18) . . ? N2 C2 C1 116.08(17) . . ? C3 C2 C1 121.62(18) . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.41(19) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C6 C5 C4 118.95(19) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N2 C6 C5 123.5(2) . . ? N2 C6 H6A 118.2 . . ? C5 C6 H6A 118.2 . . ? N3 C7 C8 110.06(16) . . ? N3 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N3 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 122.58(18) . . ? N4 C8 C7 115.75(17) . . ? C9 C8 C7 121.67(18) . . ? C10 C9 C8 119.05(19) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 119.1(2) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 118.7(2) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? N4 C12 C11 123.16(19) . . ? N4 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N5 C13 C14 109.1(2) . . ? N5 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N5 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N6 C14 C15 122.1(2) . . ? N6 C14 C13 114.5(2) . . ? C15 C14 C13 123.4(2) . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 118.5(2) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? C18 C17 C16 119.2(2) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? N6 C18 C17 122.8(2) . . ? N6 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? O1SA C1SA C2SA 106.5(6) . . ? O1SA C1SA H1S1 110.4 . . ? C2SA C1SA H1S1 110.4 . . ? O1SA C1SA H1S2 110.4 . . ? C2SA C1SA H1S2 110.4 . . ? H1S1 C1SA H1S2 108.6 . . ? C1SA C2SA H2S1 109.5 . . ? C1SA C2SA H2S2 109.5 . . ? H2S1 C2SA H2S2 109.5 . . ? C1SA C2SA H2S3 109.5 . . ? H2S1 C2SA H2S3 109.5 . . ? H2S2 C2SA H2S3 109.5 . . ? C1SB O1SB H1SB 109.5 . . ? C3SB C1SB C2SB 99.7(16) . . ? C3SB C1SB O1SB 98.8(16) . . ? C2SB C1SB O1SB 118(2) . . ? C3SB C1SB H1S3 113.0 . . ? C2SB C1SB H1S3 113.0 . . ? O1SB C1SB H1S3 113.0 . . ? C1SB C2SB H2S4 109.5 . . ? C1SB C2SB H2S5 109.5 . . ? H2S4 C2SB H2S5 109.5 . . ? C1SB C2SB H2S6 109.5 . . ? H2S4 C2SB H2S6 109.5 . . ? H2S5 C2SB H2S6 109.5 . . ? C1SB C3SB H3S1 109.5 . . ? C1SB C3SB H3S2 109.5 . . ? H3S1 C3SB H3S2 109.5 . . ? C1SB C3SB H3S3 109.5 . . ? H3S1 C3SB H3S3 109.5 . . ? H3S2 C3SB H3S3 109.5 . . ? O1SC C1SC C2SC 113.3(14) . . ? O1SC C1SC H1S4 108.9 . . ? C2SC C1SC H1S4 108.9 . . ? O1SC C1SC H1S5 108.9 . . ? C2SC C1SC H1S5 108.9 . . ? H1S4 C1SC H1S5 107.7 . . ? C1SC C2SC H2S7 109.5 . . ? C1SC C2SC H2S8 109.5 . . ? H2S7 C2SC H2S8 109.5 . . ? C1SC C2SC H2S9 109.5 . . ? H2S7 C2SC H2S9 109.5 . . ? H2S8 C2SC H2S9 109.5 . . ? C3SD C1SD C2SD 113.3(19) . . ? C3SD C1SD O1SD 108.7(14) . . ? C2SD C1SD O1SD 122.7(17) . . ? C3SD C1SD H1S6 103.2 . . ? C2SD C1SD H1S6 103.2 . . ? O1SD C1SD H1S6 103.2 . . ? C1SD C2SD H2SX 109.5 . . ? C1SD C2SD H2SY 109.5 . . ? H2SX C2SD H2SY 109.5 . . ? C1SD C2SD H2SZ 109.5 . . ? H2SX C2SD H2SZ 109.5 . . ? H2SY C2SD H2SZ 109.5 . . ? C1SD C3SD H3S4 109.5 . . ? C1SD C3SD H3S5 109.5 . . ? H3S4 C3SD H3S5 109.5 . . ? C1SD C3SD H3S6 109.5 . . ? H3S4 C3SD H3S6 109.5 . . ? H3S5 C3SD H3S6 109.5 . . ? 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 N6 Fe1 N1 C1 120.90(13) . . . . ? N5 Fe1 N1 C1 -158.92(14) . . . . ? N4 Fe1 N1 C1 -67.79(13) . . . . ? N2 Fe1 N1 C1 24.69(13) . . . . ? N3 Fe1 N1 C1 -17.0(7) . . . . ? N6 Fe1 N2 C6 69.65(17) . . . . ? N5 Fe1 N2 C6 148.1(3) . . . . ? N4 Fe1 N2 C6 -99.49(17) . . . . ? N1 Fe1 N2 C6 164.33(18) . . . . ? N3 Fe1 N2 C6 -19.82(17) . . . . ? N6 Fe1 N2 C2 -106.88(14) . . . . ? N5 Fe1 N2 C2 -28.4(4) . . . . ? N4 Fe1 N2 C2 83.98(14) . . . . ? N1 Fe1 N2 C2 -12.20(14) . . . . ? N3 Fe1 N2 C2 163.65(14) . . . . ? N6 Fe1 N3 C7 -163.87(13) . . . . ? N5 Fe1 N3 C7 115.91(13) . . . . ? N4 Fe1 N3 C7 25.83(12) . . . . ? N1 Fe1 N3 C7 -25.7(6) . . . . ? N2 Fe1 N3 C7 -66.82(13) . . . . ? N6 Fe1 N4 C12 122.8(3) . . . . ? N5 Fe1 N4 C12 65.58(18) . . . . ? N1 Fe1 N4 C12 -22.39(18) . . . . ? N2 Fe1 N4 C12 -102.38(18) . . . . ? N3 Fe1 N4 C12 162.52(19) . . . . ? N6 Fe1 N4 C8 -54.6(3) . . . . ? N5 Fe1 N4 C8 -111.86(15) . . . . ? N1 Fe1 N4 C8 160.17(14) . . . . ? N2 Fe1 N4 C8 80.18(14) . . . . ? N3 Fe1 N4 C8 -14.92(14) . . . . ? N6 Fe1 N5 C13 26.21(14) . . . . ? N4 Fe1 N5 C13 -166.77(15) . . . . ? N1 Fe1 N5 C13 -70.10(15) . . . . ? N2 Fe1 N5 C13 -54.1(4) . . . . ? N3 Fe1 N5 C13 113.76(15) . . . . ? N5 Fe1 N6 C18 159.72(19) . . . . ? N4 Fe1 N6 C18 101.2(3) . . . . ? N1 Fe1 N6 C18 -113.49(18) . . . . ? N2 Fe1 N6 C18 -33.23(19) . . . . ? N3 Fe1 N6 C18 62.33(18) . . . . ? N5 Fe1 N6 C14 -9.51(14) . . . . ? N4 Fe1 N6 C14 -68.0(3) . . . . ? N1 Fe1 N6 C14 77.28(15) . . . . ? N2 Fe1 N6 C14 157.54(14) . . . . ? N3 Fe1 N6 C14 -106.89(15) . . . . ? Fe1 N1 C1 C2 -32.43(19) . . . . ? C6 N2 C2 C3 0.6(3) . . . . ? Fe1 N2 C2 C3 177.54(16) . . . . ? C6 N2 C2 C1 -179.94(18) . . . . ? Fe1 N2 C2 C1 -3.0(2) . . . . ? N1 C1 C2 N2 23.5(2) . . . . ? N1 C1 C2 C3 -157.05(19) . . . . ? N2 C2 C3 C4 -0.1(3) . . . . ? C1 C2 C3 C4 -179.5(2) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C2 N2 C6 C5 -0.6(3) . . . . ? Fe1 N2 C6 C5 -177.10(16) . . . . ? C4 C5 C6 N2 0.1(3) . . . . ? Fe1 N3 C7 C8 -32.32(19) . . . . ? C12 N4 C8 C9 3.4(3) . . . . ? Fe1 N4 C8 C9 -178.86(15) . . . . ? C12 N4 C8 C7 -177.16(18) . . . . ? Fe1 N4 C8 C7 0.5(2) . . . . ? N3 C7 C8 N4 21.3(2) . . . . ? N3 C7 C8 C9 -159.29(18) . . . . ? N4 C8 C9 C10 -1.3(3) . . . . ? C7 C8 C9 C10 179.35(19) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? C9 C10 C11 C12 2.5(3) . . . . ? C8 N4 C12 C11 -2.6(3) . . . . ? Fe1 N4 C12 C11 179.96(16) . . . . ? C10 C11 C12 N4 -0.3(3) . . . . ? Fe1 N5 C13 C14 -37.8(2) . . . . ? C18 N6 C14 C15 -0.4(3) . . . . ? Fe1 N6 C14 C15 169.79(17) . . . . ? C18 N6 C14 C13 -179.91(19) . . . . ? Fe1 N6 C14 C13 -9.7(2) . . . . ? N5 C13 C14 N6 31.7(3) . . . . ? N5 C13 C14 C15 -147.8(2) . . . . ? N6 C14 C15 C16 0.1(3) . . . . ? C13 C14 C15 C16 179.5(2) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C14 N6 C18 C17 0.4(3) . . . . ? Fe1 N6 C18 C17 -168.50(17) . . . . ? C16 C17 C18 N6 -0.1(4) . . . . ? # # END OF FILE # # Attachment 'EtOH_2propanol_mix_200K.cif' # SUBMISSION DETAILS data_Ethanol_2propanol_mix_200K _database_code_depnum_ccdc_archive 'CCDC 714610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_name_common ;tris(2-Picolylamine)-iron(ii) chloride ethanol 2-propanol solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Fe N6, 0.744(C2 H6 O), 0.256(C3 H8 O), 2(Cl)' _chemical_formula_sum 'C20.25 H30.50 Cl2 Fe N6 O' _chemical_formula_weight 500.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'B 21/c' _symmetry_space_group_name_HALL '-B 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, -y-1/2, z' _cell_length_a 11.4808(8) _cell_length_b 21.9300(12) _cell_length_c 19.6473(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.923(5) _cell_angle_gamma 90.00 _cell_volume 4928.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 16547 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.45 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'SADABS v.2.06 (Sheldrick, 2003)' _exptl_special_details ; Comment on the reduced completeness of data (0.991): the unique crystal axis nearly coincided with the (single) axis,(\f), of rotation and part of the detector was shadowed by the cryostat. However, a 359\% \f-scan corresponding to an almost a full sphere was collected. The program SADABS outputs only the ratio of minimum to maximum apparent transmission. Hence we have calulated the transmission from the geometry of the crystal, i.e. its dimension; T(max)=exp(-t(min)*mu) where t(min)=smallest crystal dimension and T(min)=exp(-t(max)*mu) where t(max)=body diagonal (d) of the crystal d=sqrt(a**2+b**2+c**2). N.B. that checkCIF only uses the largest crystal dimension to calculate T(min) which is an underestimate of the longest path length. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71058 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline BM1A, SNBL, ESRF, Grenoble, France' _diffrn_radiation_monochromator 'Si (111)' _diffrn_measurement_device_type 'MAR345 Image plate' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean '150 \mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 16277 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.45 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.446 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.048 _reflns_number_total 4519 _reflns_number_gt 3912 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'MARCCD control software (MAR, 2002)' _computing_cell_refinement 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlis 1.171 (Oxford Diffraction, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.6.10. (Sheldrick, 2000)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Hydrogens were input as riding atoms with N---H(NH~2~) 0.92, C---H(CH) 0.95, C---H(CH~2~) 0.99, C---H(CH~3~) 0.98 and O---H 0.84 \%A. The isotropic displacement parameters of the H atoms were fixed at 1.2U~eq~ and 1.5U~eq~ (CH~3~, OH) of their parent atoms. The crystal consists of a mixture of ethanol (74%) and 2-propanol (26%) as non-coordinated solvent, which accounts for the discrepancy between the chemical formula calulated from the sum of occupancies in the output file and the chemical sum reported. The ratio beteween the solvents is based upon the ratio determinad at 16K. The two solvent molecules also suffers from two-fold disorder; ethanol in the ratio 0.48(A) and 0.26(C); 2-propanol in the ratio 0.12(B) and 0.14(D). The distances (carbon to carbon and carbon to oxygen) in the solvent molecules were restrained to be equal (SADI) within 0.02 Angstroems. The displacement parameters were also restrained to be equal (EADP). To avoid short intermolecular contacts, H3S3 (2-propanol) was restrained (DFIX) to a position 2.10 Angstroems from H13A (1-x,1-y,1-z). In addition, the restrain BUMP was applied. The solvents were isotropically refined. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+7.5377P] 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 4519 _refine_ls_number_parameters 295 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.032 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04023(2) 0.365654(12) 0.735717(14) 0.02317(8) Uani 1 1 d . . . Cl1 Cl -0.30301(5) 0.27246(3) 0.62407(3) 0.03996(14) Uani 1 1 d . . . Cl2 Cl 0.37796(4) 0.43144(2) 0.81932(3) 0.03001(12) Uani 1 1 d . . . N1 N 0.09513(14) 0.45199(7) 0.78267(9) 0.0262(4) Uani 1 1 d . . . H1A H 0.1728 0.4478 0.8001 0.031 Uiso 1 1 d R . . H1B H 0.0917 0.4820 0.7484 0.031 Uiso 1 1 d R . . N2 N -0.11921(14) 0.40156(8) 0.77736(9) 0.0284(4) Uani 1 1 d . . . N3 N -0.03411(15) 0.27716(7) 0.70620(9) 0.0299(4) Uani 1 1 d . . . H3A H -0.1007 0.2837 0.6765 0.036 Uiso 1 1 d R . . H3B H 0.0213 0.2572 0.6817 0.036 Uiso 1 1 d R . . N4 N 0.09131(14) 0.30567(7) 0.82352(8) 0.0273(4) Uani 1 1 d . . . N5 N 0.21193(14) 0.36255(8) 0.69593(9) 0.0306(4) Uani 1 1 d . . . H5A H 0.2681 0.3669 0.7331 0.037 Uiso 1 1 d R . . H5B H 0.2175 0.3230 0.6782 0.037 Uiso 1 1 d R . . N6 N 0.00467(15) 0.39643(8) 0.62975(9) 0.0306(4) Uani 1 1 d . . . C1 C 0.02113(18) 0.47028(10) 0.83631(12) 0.0354(5) Uani 1 1 d . . . H1C H 0.0234 0.5152 0.8414 0.042 Uiso 1 1 calc R . . H1D H 0.0517 0.4520 0.8803 0.042 Uiso 1 1 calc R . . C2 C -0.10324(17) 0.44992(9) 0.81908(11) 0.0294(4) Uani 1 1 d . . . C3 C -0.19599(19) 0.47927(10) 0.84629(12) 0.0391(5) Uani 1 1 d . . . H3 H -0.1823 0.5133 0.8758 0.047 Uiso 1 1 calc R . . C4 C -0.3082(2) 0.45832(11) 0.82987(13) 0.0423(6) Uani 1 1 d . . . H4A H -0.3729 0.4776 0.8480 0.051 Uiso 1 1 calc R . . C5 C -0.32508(19) 0.40895(11) 0.78673(13) 0.0407(5) Uani 1 1 d . . . H5 H -0.4015 0.3938 0.7744 0.049 Uiso 1 1 calc R . . C6 C -0.22936(18) 0.38200(10) 0.76181(12) 0.0349(5) Uani 1 1 d . . . H6A H -0.2416 0.3479 0.7322 0.042 Uiso 1 1 calc R . . C7 C -0.05729(19) 0.24048(10) 0.76596(12) 0.0363(5) Uani 1 1 d . . . H7A H -0.0544 0.1967 0.7541 0.044 Uiso 1 1 calc R . . H7B H -0.1368 0.2497 0.7791 0.044 Uiso 1 1 calc R . . C8 C 0.03090(17) 0.25336(9) 0.82571(11) 0.0286(4) Uani 1 1 d . . . C9 C 0.0473(2) 0.21307(10) 0.88014(12) 0.0374(5) Uani 1 1 d . . . H9A H 0.0033 0.1764 0.8805 0.045 Uiso 1 1 calc R . . C10 C 0.1282(2) 0.22716(11) 0.93353(12) 0.0432(6) Uani 1 1 d . . . H10A H 0.1392 0.2008 0.9719 0.052 Uiso 1 1 calc R . . C11 C 0.1934(2) 0.27995(10) 0.93087(11) 0.0392(5) Uani 1 1 d . . . H11A H 0.2513 0.2900 0.9666 0.047 Uiso 1 1 calc R . . C12 C 0.17252(19) 0.31754(10) 0.87536(11) 0.0328(5) Uani 1 1 d . . . H12A H 0.2176 0.3537 0.8734 0.039 Uiso 1 1 calc R . . C13 C 0.21517(19) 0.40690(10) 0.64051(11) 0.0363(5) Uani 1 1 d . . . H13A H 0.2786 0.3960 0.6116 0.044 Uiso 1 1 calc R . . H13B H 0.2321 0.4479 0.6600 0.044 Uiso 1 1 calc R . . C14 C 0.1007(2) 0.40825(9) 0.59745(11) 0.0323(5) Uani 1 1 d . . . C15 C 0.0942(3) 0.42221(11) 0.52851(12) 0.0466(6) Uani 1 1 d . . . H15A H 0.1633 0.4304 0.5067 0.056 Uiso 1 1 calc R . . C16 C -0.0132(3) 0.42414(12) 0.49188(13) 0.0562(7) Uani 1 1 d . . . H16A H -0.0193 0.4340 0.4446 0.067 Uiso 1 1 calc R . . C17 C -0.1113(3) 0.41163(11) 0.52438(14) 0.0537(7) Uani 1 1 d . . . H17A H -0.1863 0.4124 0.4999 0.064 Uiso 1 1 calc R . . C18 C -0.0999(2) 0.39781(10) 0.59332(13) 0.0426(6) Uani 1 1 d . . . H18A H -0.1681 0.3890 0.6156 0.051 Uiso 1 1 calc R . . O1SA O 0.4620(6) 0.6102(3) 0.4049(3) 0.0546(7) Uiso 0.478(9) 1 d PD A 1 H1SA H 0.4311 0.6439 0.3943 0.082 Uiso 0.478(9) 1 calc PR A 1 C1SA C 0.5068(8) 0.6110(4) 0.4793(4) 0.0546(7) Uiso 0.478(9) 1 d PD A 1 H1S1 H 0.4405 0.6099 0.5083 0.066 Uiso 0.478(9) 1 calc PR A 1 H1S2 H 0.5569 0.5750 0.4902 0.066 Uiso 0.478(9) 1 calc PR A 1 C2SA C 0.5758(6) 0.6683(4) 0.4925(5) 0.0546(7) Uiso 0.478(9) 1 d PD A 1 H2S1 H 0.6340 0.6719 0.4590 0.082 Uiso 0.478(9) 1 calc PR A 1 H2S2 H 0.6155 0.6670 0.5386 0.082 Uiso 0.478(9) 1 calc PR A 1 H2S3 H 0.5231 0.7035 0.4884 0.082 Uiso 0.478(9) 1 calc PR A 1 O1SB O 0.3927(13) 0.6098(8) 0.4582(10) 0.0546(7) Uiso 0.121(3) 1 d PD B 2 H1SB H 0.3909 0.6000 0.4994 0.082 Uiso 0.121(3) 1 calc PR B 2 C1SB C 0.5165(16) 0.6159(9) 0.4420(15) 0.0546(7) Uiso 0.121(3) 1 d PD B 2 H1S3 H 0.5215 0.6113 0.3916 0.066 Uiso 0.121(3) 1 calc PR B 2 C2SB C 0.568(3) 0.6737(13) 0.4650(16) 0.0546(7) Uiso 0.121(3) 1 d PD B 2 H2S4 H 0.5289 0.7072 0.4393 0.082 Uiso 0.121(3) 1 calc PR B 2 H2S5 H 0.6516 0.6738 0.4576 0.082 Uiso 0.121(3) 1 calc PR B 2 H2S6 H 0.5592 0.6790 0.5138 0.082 Uiso 0.121(3) 1 calc PR B 2 C3SB C 0.5658(18) 0.5624(7) 0.4774(8) 0.0546(7) Uiso 0.121(3) 1 d PD B 2 H3S1 H 0.5212 0.5262 0.4618 0.082 Uiso 0.121(3) 1 calc PR B 2 H3S2 H 0.5620 0.5675 0.5267 0.082 Uiso 0.121(3) 1 calc PR B 2 H3S3 H 0.6476 0.5576 0.4675 0.082 Uiso 0.121(3) 1 calc PRD B 2 O1SC O 0.4895(10) 0.6230(5) 0.3939(5) 0.0546(7) Uiso 0.262(9) 1 d PD C 3 H1SC H 0.5264 0.6552 0.3873 0.082 Uiso 0.262(9) 1 calc PR C 3 C1SC C 0.4866(14) 0.6128(8) 0.4684(7) 0.0546(7) Uiso 0.262(9) 1 d PD C 3 H1S4 H 0.4979 0.5688 0.4778 0.066 Uiso 0.262(9) 1 calc PR C 3 H1S5 H 0.4081 0.6240 0.4815 0.066 Uiso 0.262(9) 1 calc PR C 3 C2SC C 0.5756(10) 0.6474(7) 0.5125(7) 0.0546(7) Uiso 0.262(9) 1 d PD C 3 H2S7 H 0.5858 0.6284 0.5578 0.082 Uiso 0.262(9) 1 calc PR C 3 H2S8 H 0.5494 0.6897 0.5171 0.082 Uiso 0.262(9) 1 calc PR C 3 H2S9 H 0.6503 0.6470 0.4918 0.082 Uiso 0.262(9) 1 calc PR C 3 O1SD O 0.4209(15) 0.6073(8) 0.4195(9) 0.0546(7) Uiso 0.139(3) 1 d PD D 4 H1SD H 0.3813 0.6358 0.4007 0.082 Uiso 0.139(3) 1 calc PR D 4 C1SD C 0.5129(17) 0.6330(7) 0.4689(11) 0.0546(7) Uiso 0.139(3) 1 d PD D 4 H1S6 H 0.4585 0.6432 0.5044 0.066 Uiso 0.139(3) 1 calc PR D 4 C2SD C 0.577(2) 0.6895(9) 0.4754(15) 0.0546(7) Uiso 0.139(3) 1 d PD D 4 H2SX H 0.5229 0.7237 0.4660 0.082 Uiso 0.139(3) 1 calc PR D 4 H2SY H 0.6365 0.6901 0.4426 0.082 Uiso 0.139(3) 1 calc PR D 4 H2SZ H 0.6146 0.6932 0.5218 0.082 Uiso 0.139(3) 1 calc PR D 4 C3SD C 0.5538(18) 0.5750(4) 0.5011(11) 0.0546(7) Uiso 0.139(3) 1 d PD D 4 H3S4 H 0.4884 0.5463 0.5007 0.082 Uiso 0.139(3) 1 calc PR D 4 H3S5 H 0.5848 0.5826 0.5484 0.082 Uiso 0.139(3) 1 calc PR D 4 H3S6 H 0.6155 0.5576 0.4755 0.082 Uiso 0.139(3) 1 calc PR D 4 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 0.02114(14) 0.02043(14) 0.02736(15) 0.00069(11) -0.00126(10) -0.00010(11) Cl1 0.0363(3) 0.0378(3) 0.0441(3) 0.0075(2) -0.0062(2) -0.0080(2) Cl2 0.0218(2) 0.0303(3) 0.0370(3) 0.0051(2) -0.00338(19) -0.00077(19) N1 0.0198(8) 0.0231(8) 0.0355(9) 0.0013(7) 0.0003(7) 0.0004(6) N2 0.0223(8) 0.0275(9) 0.0353(10) 0.0001(7) 0.0016(7) 0.0007(7) N3 0.0259(9) 0.0283(9) 0.0341(10) -0.0014(7) -0.0053(7) -0.0003(7) N4 0.0270(8) 0.0242(8) 0.0300(9) 0.0022(7) -0.0008(7) -0.0032(7) N5 0.0276(9) 0.0293(9) 0.0341(9) -0.0036(7) -0.0015(7) 0.0042(7) N6 0.0338(9) 0.0255(9) 0.0310(9) 0.0004(7) -0.0060(7) 0.0000(7) C1 0.0273(11) 0.0373(12) 0.0417(13) -0.0109(10) 0.0029(9) -0.0025(9) C2 0.0266(10) 0.0277(10) 0.0339(11) -0.0007(9) 0.0032(8) 0.0016(8) C3 0.0345(12) 0.0352(12) 0.0485(14) -0.0060(10) 0.0089(10) 0.0043(10) C4 0.0280(11) 0.0438(13) 0.0567(15) -0.0022(11) 0.0135(10) 0.0049(10) C5 0.0237(11) 0.0394(13) 0.0595(15) 0.0014(11) 0.0062(10) -0.0041(9) C6 0.0255(10) 0.0303(11) 0.0487(14) -0.0014(9) 0.0025(9) -0.0033(8) C7 0.0328(12) 0.0266(11) 0.0476(13) 0.0038(10) -0.0076(10) -0.0070(9) C8 0.0259(10) 0.0234(10) 0.0362(11) -0.0001(8) 0.0009(8) -0.0018(8) C9 0.0418(13) 0.0265(11) 0.0432(13) 0.0078(9) 0.0002(10) -0.0060(9) C10 0.0564(15) 0.0336(12) 0.0382(13) 0.0124(10) -0.0039(11) -0.0023(11) C11 0.0434(13) 0.0371(12) 0.0347(12) 0.0042(10) -0.0100(10) -0.0035(10) C12 0.0339(11) 0.0285(11) 0.0350(12) 0.0013(9) -0.0027(9) -0.0058(9) C13 0.0331(12) 0.0369(12) 0.0399(13) -0.0027(10) 0.0099(9) 0.0016(9) C14 0.0459(13) 0.0201(10) 0.0311(11) -0.0027(8) 0.0038(9) 0.0021(9) C15 0.0727(18) 0.0362(13) 0.0313(12) -0.0002(10) 0.0058(12) 0.0055(12) C16 0.100(2) 0.0345(13) 0.0320(13) 0.0009(10) -0.0070(14) 0.0031(14) C17 0.0722(19) 0.0323(13) 0.0498(16) 0.0005(11) -0.0342(14) -0.0010(12) C18 0.0431(13) 0.0321(12) 0.0491(15) 0.0050(10) -0.0163(11) -0.0030(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.1757(16) . ? Fe1 N3 2.1786(17) . ? Fe1 N5 2.1832(17) . ? Fe1 N6 2.1933(17) . ? Fe1 N4 2.2083(16) . ? Fe1 N2 2.2129(17) . ? N1 C1 1.465(3) . ? N1 H1A 0.9323 . ? N1 H1B 0.9399 . ? N2 C2 1.343(3) . ? N2 C6 1.346(3) . ? N3 C7 1.466(3) . ? N3 H3A 0.9332 . ? N3 H3B 0.9384 . ? N4 C8 1.343(3) . ? N4 C12 1.346(3) . ? N5 C13 1.463(3) . ? N5 H5A 0.9361 . ? N5 H5B 0.9389 . ? N6 C14 1.344(3) . ? N6 C18 1.344(3) . ? C1 C2 1.507(3) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.390(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.379(3) . ? C4 H4A 0.9500 . ? C5 C6 1.374(3) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.510(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.387(3) . ? C9 C10 1.376(3) . ? C9 H9A 0.9500 . ? C10 C11 1.382(3) . ? C10 H10A 0.9500 . ? C11 C12 1.372(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.501(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.384(3) . ? C15 C16 1.373(4) . ? C15 H15A 0.9500 . ? C16 C17 1.370(4) . ? C16 H16A 0.9500 . ? C17 C18 1.383(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O1SA C1SA 1.507(7) . ? O1SA H1SA 0.8400 . ? C1SA C2SA 1.496(10) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2SA H2S1 0.9800 . ? C2SA H2S2 0.9800 . ? C2SA H2S3 0.9800 . ? O1SB C1SB 1.489(15) . ? O1SB H1SB 0.8400 . ? C1SB C3SB 1.454(17) . ? C1SB C2SB 1.455(18) . ? C1SB H1S3 1.0000 . ? C2SB H2S4 0.9800 . ? C2SB H2S5 0.9800 . ? C2SB H2S6 0.9800 . ? C3SB H3S1 0.9800 . ? C3SB H3S2 0.9800 . ? C3SB H3S3 0.9800 . ? O1SC C1SC 1.484(12) . ? O1SC H1SC 0.8400 . ? C1SC C2SC 1.490(13) . ? C1SC H1S4 0.9900 . ? C1SC H1S5 0.9900 . ? C2SC H2S7 0.9800 . ? C2SC H2S8 0.9800 . ? C2SC H2S9 0.9800 . ? O1SD C1SD 1.483(15) . ? O1SD H1SD 0.8400 . ? C1SD C2SD 1.442(15) . ? C1SD C3SD 1.479(13) . ? C1SD H1S6 1.0000 . ? C2SD H2SX 0.9800 . ? C2SD H2SY 0.9800 . ? C2SD H2SZ 0.9800 . ? C3SD H3S4 0.9800 . ? C3SD H3S5 0.9800 . ? C3SD H3S6 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N3 168.74(7) . . ? N1 Fe1 N5 86.63(6) . . ? N3 Fe1 N5 102.83(7) . . ? N1 Fe1 N6 99.10(6) . . ? N3 Fe1 N6 89.13(6) . . ? N5 Fe1 N6 76.70(7) . . ? N1 Fe1 N4 98.01(6) . . ? N3 Fe1 N4 75.46(6) . . ? N5 Fe1 N4 94.23(6) . . ? N6 Fe1 N4 160.07(6) . . ? N1 Fe1 N2 75.66(6) . . ? N3 Fe1 N2 95.61(6) . . ? N5 Fe1 N2 160.81(6) . . ? N6 Fe1 N2 98.57(6) . . ? N4 Fe1 N2 95.50(6) . . ? C1 N1 Fe1 112.23(12) . . ? C1 N1 H1A 111.0 . . ? Fe1 N1 H1A 107.6 . . ? C1 N1 H1B 109.5 . . ? Fe1 N1 H1B 108.2 . . ? H1A N1 H1B 108.2 . . ? C2 N2 C6 117.82(18) . . ? C2 N2 Fe1 115.63(13) . . ? C6 N2 Fe1 126.42(15) . . ? C7 N3 Fe1 111.68(13) . . ? C7 N3 H3A 113.0 . . ? Fe1 N3 H3A 108.1 . . ? C7 N3 H3B 109.5 . . ? Fe1 N3 H3B 106.6 . . ? H3A N3 H3B 107.8 . . ? C8 N4 C12 117.84(17) . . ? C8 N4 Fe1 115.51(13) . . ? C12 N4 Fe1 126.59(13) . . ? C13 N5 Fe1 109.10(12) . . ? C13 N5 H5A 116.9 . . ? Fe1 N5 H5A 107.5 . . ? C13 N5 H5B 109.3 . . ? Fe1 N5 H5B 104.7 . . ? H5A N5 H5B 108.7 . . ? C14 N6 C18 118.4(2) . . ? C14 N6 Fe1 114.47(14) . . ? C18 N6 Fe1 126.69(16) . . ? N1 C1 C2 110.74(17) . . ? N1 C1 H1C 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C3 122.10(19) . . ? N2 C2 C1 116.63(18) . . ? C3 C2 C1 121.27(19) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.0(2) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C6 C5 C4 118.8(2) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N2 C6 C5 123.1(2) . . ? N2 C6 H6A 118.4 . . ? C5 C6 H6A 118.4 . . ? N3 C7 C8 111.36(17) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C9 122.17(19) . . ? N4 C8 C7 116.65(18) . . ? C9 C8 C7 121.17(18) . . ? C10 C9 C8 118.9(2) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C11 119.5(2) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C12 C11 C10 118.4(2) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N4 C12 C11 123.2(2) . . ? N4 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N5 C13 C14 110.84(18) . . ? N5 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N6 C14 C15 121.8(2) . . ? N6 C14 C13 116.37(18) . . ? C15 C14 C13 121.8(2) . . ? C16 C15 C14 119.4(3) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C17 C16 C15 119.1(2) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C16 C17 C18 119.2(2) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? N6 C18 C17 122.1(3) . . ? N6 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C2SA C1SA O1SA 108.0(6) . . ? C2SA C1SA H1S1 110.1 . . ? O1SA C1SA H1S1 110.1 . . ? C2SA C1SA H1S2 110.1 . . ? O1SA C1SA H1S2 110.1 . . ? H1S1 C1SA H1S2 108.4 . . ? C1SA C2SA H2S1 109.5 . . ? C1SA C2SA H2S2 109.5 . . ? H2S1 C2SA H2S2 109.5 . . ? C1SA C2SA H2S3 109.5 . . ? H2S1 C2SA H2S3 109.5 . . ? H2S2 C2SA H2S3 109.5 . . ? C1SB O1SB H1SB 109.5 . . ? C3SB C1SB C2SB 115(2) . . ? C3SB C1SB O1SB 99.5(16) . . ? C2SB C1SB O1SB 113(2) . . ? C3SB C1SB H1S3 109.8 . . ? C2SB C1SB H1S3 109.8 . . ? O1SB C1SB H1S3 109.8 . . ? C1SB C2SB H2S4 109.5 . . ? C1SB C2SB H2S5 109.5 . . ? H2S4 C2SB H2S5 109.5 . . ? C1SB C2SB H2S6 109.5 . . ? H2S4 C2SB H2S6 109.5 . . ? H2S5 C2SB H2S6 109.5 . . ? C1SB C3SB H3S1 109.5 . . ? C1SB C3SB H3S2 109.5 . . ? H3S1 C3SB H3S2 109.5 . . ? C1SB C3SB H3S3 109.5 . . ? H3S1 C3SB H3S3 109.5 . . ? H3S2 C3SB H3S3 109.5 . . ? O1SC C1SC C2SC 115.2(11) . . ? O1SC C1SC H1S4 108.5 . . ? C2SC C1SC H1S4 108.5 . . ? O1SC C1SC H1S5 108.5 . . ? C2SC C1SC H1S5 108.5 . . ? H1S4 C1SC H1S5 107.5 . . ? C1SC C2SC H2S7 109.5 . . ? C1SC C2SC H2S8 109.5 . . ? H2S7 C2SC H2S8 109.5 . . ? C1SC C2SC H2S9 109.5 . . ? H2S7 C2SC H2S9 109.5 . . ? H2S8 C2SC H2S9 109.5 . . ? C2SD C1SD C3SD 124.2(17) . . ? C2SD C1SD O1SD 135.4(18) . . ? C3SD C1SD O1SD 97.8(14) . . ? C2SD C1SD H1S6 95.2 . . ? C3SD C1SD H1S6 95.2 . . ? O1SD C1SD H1S6 95.2 . . ? C1SD C2SD H2SX 109.5 . . ? C1SD C2SD H2SY 109.5 . . ? H2SX C2SD H2SY 109.5 . . ? C1SD C2SD H2SZ 109.5 . . ? H2SX C2SD H2SZ 109.5 . . ? H2SY C2SD H2SZ 109.5 . . ? C1SD C3SD H3S4 109.5 . . ? C1SD C3SD H3S5 109.5 . . ? H3S4 C3SD H3S5 109.5 . . ? C1SD C3SD H3S6 109.5 . . ? H3S4 C3SD H3S6 109.5 . . ? H3S5 C3SD H3S6 109.5 . . ? 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 N1 C1 -15.8(4) . . . . ? N5 Fe1 N1 C1 -163.36(14) . . . . ? N6 Fe1 N1 C1 120.69(14) . . . . ? N4 Fe1 N1 C1 -69.56(14) . . . . ? N2 Fe1 N1 C1 24.10(13) . . . . ? N1 Fe1 N2 C2 -10.78(14) . . . . ? N3 Fe1 N2 C2 161.98(14) . . . . ? N5 Fe1 N2 C2 -34.0(3) . . . . ? N6 Fe1 N2 C2 -108.06(15) . . . . ? N4 Fe1 N2 C2 86.10(15) . . . . ? N1 Fe1 N2 C6 165.07(19) . . . . ? N3 Fe1 N2 C6 -22.17(18) . . . . ? N5 Fe1 N2 C6 141.8(2) . . . . ? N6 Fe1 N2 C6 67.79(18) . . . . ? N4 Fe1 N2 C6 -98.04(18) . . . . ? N1 Fe1 N3 C7 -29.1(4) . . . . ? N5 Fe1 N3 C7 117.55(14) . . . . ? N6 Fe1 N3 C7 -166.30(14) . . . . ? N4 Fe1 N3 C7 26.46(13) . . . . ? N2 Fe1 N3 C7 -67.78(14) . . . . ? N1 Fe1 N4 C8 153.71(14) . . . . ? N3 Fe1 N4 C8 -16.93(14) . . . . ? N5 Fe1 N4 C8 -119.10(15) . . . . ? N6 Fe1 N4 C8 -57.3(3) . . . . ? N2 Fe1 N4 C8 77.46(15) . . . . ? N1 Fe1 N4 C12 -23.52(18) . . . . ? N3 Fe1 N4 C12 165.84(18) . . . . ? N5 Fe1 N4 C12 63.67(18) . . . . ? N6 Fe1 N4 C12 125.5(2) . . . . ? N2 Fe1 N4 C12 -99.77(18) . . . . ? N1 Fe1 N5 C13 -73.45(14) . . . . ? N3 Fe1 N5 C13 112.72(14) . . . . ? N6 Fe1 N5 C13 26.73(13) . . . . ? N4 Fe1 N5 C13 -171.25(13) . . . . ? N2 Fe1 N5 C13 -50.9(3) . . . . ? N1 Fe1 N6 C14 73.67(14) . . . . ? N3 Fe1 N6 C14 -114.05(14) . . . . ? N5 Fe1 N6 C14 -10.65(14) . . . . ? N4 Fe1 N6 C14 -75.2(2) . . . . ? N2 Fe1 N6 C14 150.40(14) . . . . ? N1 Fe1 N6 C18 -114.21(18) . . . . ? N3 Fe1 N6 C18 58.07(18) . . . . ? N5 Fe1 N6 C18 161.47(19) . . . . ? N4 Fe1 N6 C18 96.9(2) . . . . ? N2 Fe1 N6 C18 -37.48(19) . . . . ? Fe1 N1 C1 C2 -33.5(2) . . . . ? C6 N2 C2 C3 0.4(3) . . . . ? Fe1 N2 C2 C3 176.67(17) . . . . ? C6 N2 C2 C1 179.24(19) . . . . ? Fe1 N2 C2 C1 -4.5(2) . . . . ? N1 C1 C2 N2 25.2(3) . . . . ? N1 C1 C2 C3 -156.0(2) . . . . ? N2 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C4 -179.0(2) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C2 N2 C6 C5 -0.3(3) . . . . ? Fe1 N2 C6 C5 -176.03(17) . . . . ? C4 C5 C6 N2 -0.1(4) . . . . ? Fe1 N3 C7 C8 -32.5(2) . . . . ? C12 N4 C8 C9 2.1(3) . . . . ? Fe1 N4 C8 C9 -175.38(17) . . . . ? C12 N4 C8 C7 -178.41(19) . . . . ? Fe1 N4 C8 C7 4.1(2) . . . . ? N3 C7 C8 N4 18.9(3) . . . . ? N3 C7 C8 C9 -161.6(2) . . . . ? N4 C8 C9 C10 -0.1(3) . . . . ? C7 C8 C9 C10 -179.6(2) . . . . ? C8 C9 C10 C11 -1.8(4) . . . . ? C9 C10 C11 C12 1.8(4) . . . . ? C8 N4 C12 C11 -2.2(3) . . . . ? Fe1 N4 C12 C11 174.97(17) . . . . ? C10 C11 C12 N4 0.3(4) . . . . ? Fe1 N5 C13 C14 -38.7(2) . . . . ? C18 N6 C14 C15 0.6(3) . . . . ? Fe1 N6 C14 C15 173.46(16) . . . . ? C18 N6 C14 C13 179.28(19) . . . . ? Fe1 N6 C14 C13 -7.9(2) . . . . ? N5 C13 C14 N6 31.7(3) . . . . ? N5 C13 C14 C15 -149.6(2) . . . . ? N6 C14 C15 C16 0.0(3) . . . . ? C13 C14 C15 C16 -178.5(2) . . . . ? C14 C15 C16 C17 -0.6(4) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C14 N6 C18 C17 -0.8(3) . . . . ? Fe1 N6 C18 C17 -172.62(17) . . . . ? C16 C17 C18 N6 0.2(4) . . . . ? # # END OF FILE #