# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Martineau, Charlotte' _publ_contact_author_email charlotte.martineau@chimie.uvsq.fr loop_ _publ_author_name 'Martineau, Charlotte' 'Cadiau, Amandine' 'Bouchevreau, Boris' 'Senker, Jurgen' 'Taulelle, Francis' 'Adil, Karim' data_304 _database_code_depnum_ccdc_archive 'CCDC 871623' #TrackingRef '- Zn3Al2N24C12H24_SCD.cif' _audit_creation_date 2011-07-21T11:53:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H24 Al2 F12 N24 Zn3' _chemical_formula_sum 'C12 H24 Al2 F12 N24 Zn3' _chemical_formula_weight 982.62 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 12.5761(5) _cell_length_b 12.5761(5) _cell_length_c 17.6463(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2417.00(18) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 96 _cell_measurement_theta_min 4 _cell_measurement_theta_max 12 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS 2008/1, Bruker_AXS, Madison, WI.' _exptl_absorpt_correction_T_min 0.6462 _exptl_absorpt_correction_T_max 0.7454 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 30 settings' _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_number 4706 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.68 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.903 _reflns_number_total 1037 _reflns_number_gt 973 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2001) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+3.1368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method shelxl _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1037 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.331 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn1 Zn 0 0 0 0.02434(16) Uani 1 6 d S . . Zn2 Zn 0 0 0.20553(2) 0.02008(13) Uani 1 3 d S . . Al Al 0 0 0.36462(5) 0.0179(2) Uani 1 3 d S . . F1 F 0.08540(10) 0.13560(10) 0.41860(6) 0.0274(3) Uani 1 1 d . . . F2 F 0.12899(10) 0.04794(11) 0.29831(6) 0.0299(3) Uani 1 1 d . . . N2 N 0.09812(16) 0.16377(16) 0.07023(9) 0.0278(4) Uani 1 1 d . . . N1 N 0.11168(15) 0.15753(15) 0.14835(9) 0.0243(4) Uani 1 1 d . . . N3 N 0.21865(18) 0.34840(17) 0.11324(11) 0.0326(4) Uani 1 1 d . . . N4 N 0.22632(19) 0.30274(17) 0.24405(11) 0.0394(5) Uani 1 1 d . . . H4A H 0.2037 0.2472 0.2785 0.047 Uiso 1 1 calc R . . H4B H 0.2746 0.3786 0.2554 0.047 Uiso 1 1 calc R . . C1 C 0.1628(2) 0.27878(19) 0.05196(12) 0.0330(5) Uani 1 1 d . . . H1 H 0.1697 0.3092 0.0031 0.04 Uiso 1 1 calc R . . C2 C 0.18595(18) 0.27085(17) 0.17226(12) 0.0265(4) Uani 1 1 d . . . H3 H 0.264(2) 0.424(3) 0.1123(14) 0.04 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0270(2) 0.0270(2) 0.0190(3) 0 0 0.01350(10) Zn2 0.02080(16) 0.02080(16) 0.0186(2) 0 0 0.01040(8) Al 0.0171(3) 0.0171(3) 0.0193(5) 0 0 0.00856(15) F1 0.0260(6) 0.0209(6) 0.0324(7) -0.0061(5) -0.0051(5) 0.0095(5) F2 0.0245(6) 0.0364(7) 0.0275(6) 0.0035(5) 0.0070(5) 0.0144(5) N2 0.0314(9) 0.0250(9) 0.0223(9) 0.0023(7) 0.0015(7) 0.0106(7) N1 0.0283(9) 0.0210(8) 0.0207(8) 0.0001(6) -0.0005(7) 0.0102(7) N3 0.0332(10) 0.0178(9) 0.0385(10) 0.0052(8) -0.0005(8) 0.0066(8) N4 0.0529(12) 0.0217(9) 0.0334(10) -0.0049(8) -0.0129(9) 0.0109(9) C1 0.0362(12) 0.0291(11) 0.0283(11) 0.0079(9) 0.0032(9) 0.0121(10) C2 0.0261(10) 0.0207(10) 0.0313(10) 0.0007(8) -0.0013(8) 0.0106(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn1 N2 2.1815(17) 10 ? Zn1 N2 2.1815(17) . ? Zn1 N2 2.1815(17) 2 ? Zn1 N2 2.1815(17) 3 ? Zn1 N2 2.1815(17) 11 ? Zn1 N2 2.1815(17) 12 ? Zn2 N1 2.0330(16) 2 ? Zn2 N1 2.0330(16) 3 ? Zn2 N1 2.0330(16) . ? Zn2 F2 2.1673(12) . ? Zn2 F2 2.1673(12) 2 ? Zn2 F2 2.1673(12) 3 ? Zn2 Al 2.8074(11) . ? Al F1 1.7713(12) . ? Al F1 1.7713(11) 2 ? Al F1 1.7713(11) 3 ? Al F2 1.8401(12) 3 ? Al F2 1.8401(12) . ? Al F2 1.8401(12) 2 ? N2 C1 1.296(3) . ? N2 N1 1.396(2) . ? N1 C2 1.323(3) . ? N3 C2 1.343(3) . ? N3 C1 1.347(3) . ? N4 C2 1.349(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N2 180.00(11) 10 . ? N2 Zn1 N2 89.09(6) 10 2 ? N2 Zn1 N2 90.91(6) . 2 ? N2 Zn1 N2 89.09(6) 10 3 ? N2 Zn1 N2 90.91(6) . 3 ? N2 Zn1 N2 90.91(6) 2 3 ? N2 Zn1 N2 90.91(6) 10 11 ? N2 Zn1 N2 89.09(6) . 11 ? N2 Zn1 N2 180.00(7) 2 11 ? N2 Zn1 N2 89.09(6) 3 11 ? N2 Zn1 N2 90.91(6) 10 12 ? N2 Zn1 N2 89.09(6) . 12 ? N2 Zn1 N2 89.09(6) 2 12 ? N2 Zn1 N2 180.00(10) 3 12 ? N2 Zn1 N2 90.91(6) 11 12 ? N1 Zn2 N1 97.50(6) 2 3 ? N1 Zn2 N1 97.50(6) 2 . ? N1 Zn2 N1 97.50(6) 3 . ? N1 Zn2 F2 160.30(6) 2 . ? N1 Zn2 F2 97.80(5) 3 . ? N1 Zn2 F2 92.72(5) . . ? N1 Zn2 F2 92.72(5) 2 2 ? N1 Zn2 F2 160.30(6) 3 2 ? N1 Zn2 F2 97.80(5) . 2 ? F2 Zn2 F2 69.15(5) . 2 ? N1 Zn2 F2 97.80(5) 2 3 ? N1 Zn2 F2 92.72(5) 3 3 ? N1 Zn2 F2 160.30(6) . 3 ? F2 Zn2 F2 69.15(5) . 3 ? F2 Zn2 F2 69.15(5) 2 3 ? N1 Zn2 Al 119.75(5) 2 . ? N1 Zn2 Al 119.75(5) 3 . ? N1 Zn2 Al 119.75(5) . . ? F2 Zn2 Al 40.94(3) . . ? F2 Zn2 Al 40.94(3) 2 . ? F2 Zn2 Al 40.94(3) 3 . ? F1 Al F1 93.79(6) . 2 ? F1 Al F1 93.79(6) . 3 ? F1 Al F1 93.79(6) 2 3 ? F1 Al F2 173.05(7) . 3 ? F1 Al F2 91.01(5) 2 3 ? F1 Al F2 90.90(5) 3 3 ? F1 Al F2 90.90(5) . . ? F1 Al F2 173.05(7) 2 . ? F1 Al F2 91.01(5) 3 . ? F2 Al F2 83.88(6) 3 . ? F1 Al F2 91.01(5) . 2 ? F1 Al F2 90.90(5) 2 2 ? F1 Al F2 173.05(7) 3 2 ? F2 Al F2 83.88(6) 3 2 ? F2 Al F2 83.88(6) . 2 ? F1 Al Zn2 122.53(5) . . ? F1 Al Zn2 122.53(5) 2 . ? F1 Al Zn2 122.53(5) 3 . ? F2 Al Zn2 50.51(4) 3 . ? F2 Al Zn2 50.51(4) . . ? F2 Al Zn2 50.51(4) 2 . ? Al F2 Zn2 88.55(5) . . ? C1 N2 N1 106.39(17) . . ? C1 N2 Zn1 130.93(15) . . ? N1 N2 Zn1 122.36(12) . . ? C2 N1 N2 107.14(16) . . ? C2 N1 Zn2 131.54(14) . . ? N2 N1 Zn2 120.04(12) . . ? C2 N3 C1 106.24(18) . . ? N2 C1 N3 110.97(19) . . ? N1 C2 N3 109.26(18) . . ? N1 C2 N4 125.30(18) . . ? N3 C2 N4 125.39(18) . . ?