############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # Copyright International Union of Crystallography # # # ############################################################################## data_I _audit_creation_method SHELXL97 _chemical_name_systematic ; Hexakis(\m~4~-2-amino-2-methylpropane-1,3-diolato)hexachloroheptairon(II,III) acetonitrile disolvate monohydrate ; _chemical_name_common ? _chemical_formula_moiety 'C24 H54 Cl6 Fe7 N6 O12 , 2C2 H3 N , H2 O' _chemical_formula_sum 'C28 H62 Cl6 Fe7 N8 O13' _chemical_formula_iupac '[Fe7 (C4 H9 N O2)6 Cl6] , 2C H3 C N , H2 O' _chemical_formula_weight 1322.51 _chemical_melting_point ? _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.4150(7) _cell_length_b 12.4150(7) _cell_length_c 28.030(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3741.5(5) _cell_formula_units_Z 3 _cell_measurement_reflns_used 3857 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _cell_measurement_temperature 153(2) _exptl_crystal_description brown _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_meas none _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2022 _exptl_absorpt_coefficient_mu 2.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(MULABS in PLATON; Spek, 2003)' _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 0.624 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\f oscillation' _diffrn_detector_area_resol_mean 0.81 _diffrn_reflns_number 9917 _diffrn_reflns_av_R_equivalents 0.1797 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.94 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 1622 _reflns_number_gt 916 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_gt 0.1560 _refine_ls_wR_factor_ref 0.1688 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.882 _refine_ls_number_reflns 1622 _refine_ls_number_parameters 105 _refine_ls_number_restraints 2 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0981P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.519 _refine_diff_density_min -1.119 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'EXPOSE in IPDS II (Stoe, 2000)' _computing_cell_refinement 'CELL in IPDS II' _computing_data_reduction 'INTEGRATE in IPDS II (Stoe, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL97 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 0.3333 0.6667 0.1667 0.0145(6) Uani d S 1 . . Fe Fe2 0.06706(10) 0.64746(11) 0.15927(3) 0.0269(4) Uani d . 1 . . Fe Cl1 -0.0502(2) 0.6934(3) 0.10790(7) 0.0521(7) Uani d . 1 . . Cl N1 0.2415(7) 0.9585(7) 0.1115(3) 0.0409(18) Uani d D 1 . . N H1 0.161(3) 0.924(8) 0.105(3) 0.049 Uiso d D 1 . . H H2 0.264(8) 1.035(4) 0.102(3) 0.049 Uiso d D 1 . . H N2 0.0000 1.0000 0.2987(6) 0.067(4) Uani d S 1 . . N O1 0.2420(5) 0.7474(5) 0.12845(16) 0.0298(12) Uani d . 1 . . O O2 0.4639(5) 0.9850(5) 0.13216(16) 0.0352(13) Uani d . 1 . . O C1 0.3060(8) 0.9262(8) 0.0735(2) 0.035(2) Uani d . 1 . . C C2 0.2578(8) 0.7853(8) 0.0788(2) 0.0345(19) Uani d . 1 . . C H2A 0.1771 0.7380 0.0621 0.041 Uiso calc R 1 . . H H2B 0.3174 0.7651 0.0635 0.041 Uiso calc R 1 . . H C3 0.4419(8) 1.0029(8) 0.0839(3) 0.043(2) Uani d . 1 . . C H3A 0.4891 0.9781 0.0625 0.052 Uiso calc R 1 . . H H3B 0.4704 1.0919 0.0782 0.052 Uiso calc R 1 . . H C4 0.2787(9) 0.9527(9) 0.0231(3) 0.054(3) Uani d . 1 . . C H4C 0.3174 1.0428 0.0184 0.081 Uiso calc R 1 . . H H4A 0.1885 0.9138 0.0186 0.081 Uiso calc R 1 . . H H4B 0.3126 0.9186 -0.0002 0.081 Uiso calc R 1 . . H C5 0.0000 1.0000 0.2598(7) 0.050(4) Uani d S 1 . . C C6 0.0000 1.0000 0.2062(6) 0.076(6) Uani d S 1 . . C H6A -0.0805 0.9859 0.1946 0.114 Uiso calc PR 0.33 . . H H6B 0.0141 0.9337 0.1946 0.114 Uiso calc PR 0.33 . . H H6C 0.0663 1.0805 0.1946 0.114 Uiso calc PR 0.33 . . H O1WA 0.0000 1.0000 0.0492(12) 0.026(8) Uiso d SP 0.25 A 1 O O1WB 0.0000 1.0000 0.0203(12) 0.028(8) Uiso d SP 0.25 . 2 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0169(8) 0.0169(8) 0.0099(10) 0.0084(4) 0.000 0.000 Fe2 0.0290(7) 0.0448(8) 0.0131(5) 0.0231(6) 0.0000(4) 0.0002(4) Cl1 0.0451(14) 0.102(2) 0.0293(10) 0.0515(15) -0.0016(9) 0.0024(11) N1 0.048(5) 0.032(4) 0.043(4) 0.021(4) 0.000(4) 0.007(3) N2 0.066(7) 0.066(7) 0.068(11) 0.033(4) 0.000 0.000 O1 0.039(3) 0.037(3) 0.018(2) 0.022(3) 0.006(2) 0.006(2) O2 0.036(3) 0.037(3) 0.027(3) 0.015(3) 0.002(2) 0.008(2) C1 0.066(6) 0.038(5) 0.012(3) 0.035(5) -0.004(4) 0.004(3) C2 0.044(5) 0.046(5) 0.016(3) 0.025(5) 0.002(3) 0.005(3) C3 0.052(6) 0.041(6) 0.028(4) 0.017(5) 0.006(4) 0.017(4) C4 0.084(8) 0.057(6) 0.026(4) 0.038(6) -0.013(4) 0.012(4) C5 0.044(7) 0.044(7) 0.060(11) 0.022(3) 0.000 0.000 C6 0.086(10) 0.086(10) 0.056(11) 0.043(5) 0.000 0.000 _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 O1 13_565 2.138(5) ? Fe1 O1 . 2.138(5) y Fe1 O1 2_665 2.138(5) ? Fe1 O1 3_565 2.138(5) ? Fe1 O1 15 2.138(5) ? Fe1 O1 14_455 2.138(5) ? Fe2 O1 15 2.203(5) y Fe2 O1 . 2.076(5) y Fe2 O2 15 1.994(5) y Fe2 O2 2_665 2.005(5) y Fe2 N1 15 2.168(7) y N1 Fe2 14_455 2.168(7) ? Fe2 Cl1 . 2.313(2) y N1 C1 . 1.501(11) ? N1 H1 . 0.89(2) ? N1 H2 . 0.89(2) ? N2 C5 . 1.09(2) ? O1 C2 . 1.451(8) ? O1 Fe2 14_455 2.203(5) ? O2 C3 . 1.419(9) ? O2 Fe2 14_455 1.994(5) ? O2 Fe2 3_565 2.005(5) ? C1 C3 . 1.495(12) ? C1 C4 . 1.528(9) ? C1 C2 . 1.548(11) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 H4C . 0.9800 ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C5 C6 . 1.50(2) ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? O1WB O1WB 10_575 1.14(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Fe1 O1 13_565 . 180 y O1 Fe1 O1 13_565 2_665 82.91(16) y O1 Fe1 O1 . 2_665 97.09(16) y O1 Fe1 O1 13_565 3_565 82.91(16) ? O1 Fe1 O1 . 3_565 97.09(16) ? O1 Fe1 O1 2_665 3_565 97.09(16) ? O1 Fe1 O1 13_565 15 97.09(16) ? O1 Fe1 O1 . 15 82.91(16) ? O1 Fe1 O1 2_665 15 82.91(16) ? O1 Fe1 O1 3_565 15 180 ? O1 Fe1 O1 13_565 14_455 97.09(16) ? O1 Fe1 O1 . 14_455 82.91(16) ? O1 Fe1 O1 2_665 14_455 180 ? O1 Fe1 O1 3_565 14_455 82.91(16) ? O1 Fe1 O1 15 14_455 97.09(16) ? O2 Fe2 O2 15 2_665 161.6(2) y O2 Fe2 O1 15 . 79.1(2) y O2 Fe2 O1 2_665 . 99.2(2) y O2 Fe2 O1 15 15 85.7(2) y O2 Fe2 O1 2_665 15 75.8(2) y O1 Fe2 O1 . 15 82.8(3) y O2 Fe2 N1 15 15 79.9(2) ? O2 Fe2 N1 2_665 15 94.2(3) y O1 Fe2 N1 . 15 150.5(2) y N1 Fe2 O1 15 15 75.2(2) y O1 Fe2 Cl1 . . 101.15(15) y N1 Fe2 Cl1 15 . 103.4(2) y O1 Fe2 Cl1 15 . 171.65(16) y O2 Fe2 Cl1 15 . 102.20(17) y O2 Fe2 Cl1 2_665 . 96.16(16) y C1 N1 Fe2 . 14_455 99.2(5) ? C1 N1 H1 . . 111(6) ? Fe2 N1 H1 14_455 . 123(6) ? C1 N1 H2 . . 99(6) ? Fe2 N1 H2 14_455 . 125(6) ? H1 N1 H2 . . 97(8) ? C2 O1 Fe2 . . 121.6(5) ? C2 O1 Fe1 . . 128.0(4) ? Fe2 O1 Fe1 . . 98.8(2) y C2 O1 Fe2 . 14_455 109.1(4) ? Fe2 O1 Fe2 . 14_455 97.57(19) y Fe1 O1 Fe2 . 14_455 94.96(19) y C3 O2 Fe2 . 14_455 114.9(5) ? C3 O2 Fe2 . 3_565 129.6(5) ? Fe2 O2 Fe2 14_455 3_565 107.3(2) y C3 C1 N1 . . 105.9(6) ? C3 C1 C4 . . 110.1(7) ? N1 C1 C4 . . 113.2(7) ? C3 C1 C2 . . 112.1(7) ? N1 C1 C2 . . 106.1(6) ? C4 C1 C2 . . 109.3(6) ? O1 C2 C1 . . 111.8(6) ? O1 C2 H2A . . 109.3 ? C1 C2 H2A . . 109.3 ? O1 C2 H2B . . 109.3 ? C1 C2 H2B . . 109.3 ? H2A C2 H2B . . 107.9 ? O2 C3 C1 . . 109.3(6) ? O2 C3 H3A . . 109.8 ? C1 C3 H3A . . 109.8 ? O2 C3 H3B . . 109.8 ? C1 C3 H3B . . 109.8 ? H3A C3 H3B . . 108.3 ? C1 C4 H4C . . 109.5 ? C1 C4 H4A . . 109.5 ? H4C C4 H4A . . 109.5 ? C1 C4 H4B . . 109.5 ? H4C C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? N2 C5 C6 . . 180.000(6) ? C5 C6 H6A . . 109.5 ? C5 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C5 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O2 Fe2 O1 C2 15 . . . -121.6(5) ? O2 Fe2 O1 C2 2_665 . . . 77.0(5) ? N1 Fe2 O1 C2 15 . . . -166.9(6) ? O1 Fe2 O1 C2 15 . . . 151.4(5) ? Cl1 Fe2 O1 C2 . . . . -21.2(5) ? O2 Fe2 O1 Fe1 15 . . . 92.6(2) ? O2 Fe2 O1 Fe1 2_665 . . . -68.7(2) ? N1 Fe2 O1 Fe1 15 . . . 47.3(6) ? O1 Fe2 O1 Fe1 15 . . . 5.59(19) ? Cl1 Fe2 O1 Fe1 . . . . -166.94(15) ? O2 Fe2 O1 Fe2 15 . . 14_455 -3.6(2) ? O2 Fe2 O1 Fe2 2_665 . . 14_455 -164.98(19) ? N1 Fe2 O1 Fe2 15 . . 14_455 -48.9(6) ? O1 Fe2 O1 Fe2 15 . . 14_455 -90.7(2) ? Cl1 Fe2 O1 Fe2 . . . 14_455 96.80(16) ? O1 Fe1 O1 C2 2_665 . . . -66.4(5) ? O1 Fe1 O1 C2 3_565 . . . 31.7(6) ? O1 Fe1 O1 C2 15 . . . -148.3(6) ? O1 Fe1 O1 C2 14_455 . . . 113.6(5) ? O1 Fe1 O1 Fe2 2_665 . . . 76.1(3) ? O1 Fe1 O1 Fe2 3_565 . . . 174.24(18) ? O1 Fe1 O1 Fe2 15 . . . -5.76(18) ? O1 Fe1 O1 Fe2 14_455 . . . -103.9(3) ? O1 Fe1 O1 Fe2 2_665 . . 14_455 174.62(19) ? O1 Fe1 O1 Fe2 3_565 . . 14_455 -87.3(3) ? O1 Fe1 O1 Fe2 15 . . 14_455 92.7(3) ? O1 Fe1 O1 Fe2 14_455 . . 14_455 -5.38(19) ? Fe2 N1 C1 C3 14_455 . . . -56.8(6) ? Fe2 N1 C1 C4 14_455 . . . -177.6(6) ? Fe2 N1 C1 C2 14_455 . . . 62.6(6) ? Fe2 O1 C2 C1 . . . . 106.0(7) ? Fe1 O1 C2 C1 . . . . -118.9(6) ? Fe2 O1 C2 C1 14_455 . . . -6.1(8) ? C3 C1 C2 O1 . . . . 77.0(8) ? N1 C1 C2 O1 . . . . -38.3(8) ? C4 C1 C2 O1 . . . . -160.6(7) ? Fe2 O2 C3 C1 14_455 . . . -18.3(8) ? Fe2 O2 C3 C1 3_565 . . . 125.7(6) ? N1 C1 C3 O2 . . . . 52.3(8) ? C4 C1 C3 O2 . . . . 175.1(7) ? C2 C1 C3 O2 . . . . -63.0(8) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1 Cl1 . 0.89(2) 2.75(6) 3.470(8) 139(8) N1 H2 Cl1 2_675 0.89(2) 2.52(4) 3.370(8) 158(8) data_global _journal_date_recd_electronic 2005-02-18 _journal_date_accepted 2005-02-21 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2005 _journal_volume 61 _journal_issue 4 _journal_page_first m611 _journal_page_last m613 _journal_paper_category EM _publ_contact_author_name 'Dr Gael Labat' _publ_contact_author_address ; Institut de Chimie Universite de Neuchatel Avenue de Bellevaux 51 CH-2000 Neuchatel Switzerland ; _publ_contact_author_email gael.labat@unine.ch _publ_contact_author_fax '+41 32 718 25 11' _publ_contact_author_phone '+41 32 718 38 85' _publ_section_title ; Hexakis(\m~4~-2-amino-2-methylpropane-1,3-diolato)hexachloroheptairon(II,III) acetonitrile disolvate monohydrate ; loop_ _publ_author_name _publ_author_address 'Ga\"el Labat' ; Institut de Chimie Universit\'e de Neuch\^atel Avenue de Bellevaux 51 CH-2007 Neuch\^atel Switzerland ; 'Colette Boscovic' ; Departement f\"ur Chemie und Biochemie Universit\"at Bern Freiestra\&se 3 CH-3012 Bern Switzerland ; 'Hans U. G\"udel' ; Departement f\"ur Chemie und Biochemie Universit\"at Bern Freiestra\&se 3 CH-3012 Bern Switzerland ;