Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_gre45 _database_code_CSD 173902 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mulvey, R. E.' 'Gallagher, Daniel J.' 'Henderson, Kenneth W.' 'Kennedy, Alan R.' 'O'Hara, Charles T.' 'Rowlings, Rene B.' _publ_contact_author_name 'Prof R E Mulvey' _publ_contact_author_address ; Department of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email 'R.E.MULVEY@STRATH.AC.UK' _publ_requested_journal 'Chem. Commun.' _publ_contact_letter ; Dear Sir, The following file is submitted as the supplementary data for the paper "Hydride encapsulation in s-block metal inverse crown chemistry" by Gallacher, Henderson, Kennedy, O'Hara, Mulvey and Rowlings. This paper has recently been sent to you by normal mail. If there are any problems with the construction of this CIF please contact me. Yours, Alan Kennedy ; _publ_section_title ; Hydride Encapsulation in s-Block Metal Inverse Crown Chemistry ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H74 Mg2 N4 Na2' _chemical_formula_weight 681.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9353(4) _cell_length_b 12.1480(5) _cell_length_c 17.3141(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2089.71(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2050 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11817 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1912 _reflns_number_gt 1355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO & COLLECT' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.4478P] 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 'see text' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1912 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.5000 0.0000 0.08352(6) 0.0206(3) Uani 1 d S . . H1M H 0.614(3) 0.034(3) 0.0000 0.033(9) Uiso 1 d S . . Na1 Na 0.31813(13) 0.17954(11) 0.0000 0.0304(4) Uani 1 d S . . N1 N 0.40320(17) 0.13441(15) 0.13093(10) 0.0223(5) Uani 1 d . . . C1 C 0.4892(2) 0.21915(19) 0.16688(13) 0.0257(5) Uani 1 d . . . H1 H 0.5376 0.1844 0.2113 0.031 Uiso 1 calc R . . C2 C 0.5945(2) 0.2586(2) 0.10901(15) 0.0375(7) Uani 1 d . . . H2A H 0.6352 0.1949 0.0833 0.056 Uiso 1 calc R . . H2B H 0.6644 0.3003 0.1362 0.056 Uiso 1 calc R . . H2C H 0.5514 0.3059 0.0704 0.056 Uiso 1 calc R . . C3 C 0.4146(3) 0.3204(2) 0.19717(15) 0.0363(6) Uani 1 d . . . H3A H 0.3625 0.3536 0.1552 0.054 Uiso 1 calc R . . H3B H 0.4798 0.3740 0.2169 0.054 Uiso 1 calc R . . H3C H 0.3536 0.2983 0.2389 0.054 Uiso 1 calc R . . C4 C 0.2867(2) 0.1060(2) 0.17991(13) 0.0257(5) Uani 1 d . . . H4 H 0.2339 0.1749 0.1891 0.031 Uiso 1 calc R . . C5 C 0.1952(2) 0.0243(2) 0.13889(14) 0.0334(6) Uani 1 d . . . H5A H 0.1651 0.0557 0.0897 0.050 Uiso 1 calc R . . H5B H 0.1169 0.0085 0.1715 0.050 Uiso 1 calc R . . H5C H 0.2448 -0.0441 0.1291 0.050 Uiso 1 calc R . . C6 C 0.3240(2) 0.0576(2) 0.25868(13) 0.0309(6) Uani 1 d . . . H6A H 0.3755 -0.0103 0.2513 0.046 Uiso 1 calc R . . H6B H 0.2417 0.0414 0.2878 0.046 Uiso 1 calc R . . H6C H 0.3786 0.1109 0.2874 0.046 Uiso 1 calc R . . C7 C 0.2232(4) 0.4875(3) 0.0000 0.0448(10) Uani 1 d S . . H7A H 0.1786 0.5495 0.0256 0.067 Uiso 0.50 calc PR . . H7B H 0.2450 0.5076 -0.0533 0.067 Uiso 0.50 calc PR . . H7C H 0.3061 0.4690 0.0278 0.067 Uiso 0.50 calc PR . . C8 C 0.1304(3) 0.3892(3) 0.0000 0.0311(8) Uani 1 d S . . C9 C 0.0846(2) 0.3424(2) 0.06899(14) 0.0341(6) Uani 1 d . . . H9 H 0.1147 0.3717 0.1168 0.041 Uiso 1 calc R . . C10 C -0.0036(3) 0.2542(2) 0.06895(14) 0.0376(6) Uani 1 d . . . H10 H -0.0335 0.2240 0.1166 0.045 Uiso 1 calc R . . C11 C -0.0487(4) 0.2098(3) 0.0000 0.0378(9) Uani 1 d S . . H11 H -0.1098 0.1496 0.0000 0.045 Uiso 1 calc SR . . 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 Mg1 0.0237(6) 0.0185(6) 0.0195(5) 0.000 0.000 0.0006(5) Na1 0.0343(8) 0.0299(8) 0.0271(7) 0.000 0.000 0.0055(6) N1 0.0228(10) 0.0228(10) 0.0213(10) -0.0024(8) 0.0016(8) -0.0015(8) C1 0.0311(13) 0.0208(12) 0.0253(11) -0.0039(10) -0.0016(11) -0.0004(11) C2 0.0382(15) 0.0296(15) 0.0448(16) -0.0118(13) 0.0054(12) -0.0105(12) C3 0.0390(15) 0.0275(14) 0.0424(15) -0.0104(12) 0.0001(12) -0.0005(12) C4 0.0260(12) 0.0244(13) 0.0267(12) -0.0032(11) 0.0016(10) 0.0030(10) C5 0.0277(13) 0.0379(16) 0.0346(13) -0.0038(12) 0.0050(11) -0.0064(11) C6 0.0310(13) 0.0323(15) 0.0295(13) 0.0010(11) 0.0068(11) 0.0003(12) C7 0.039(2) 0.040(2) 0.055(2) 0.000 0.000 -0.0037(19) C8 0.0286(19) 0.028(2) 0.036(2) 0.000 0.000 0.0071(16) C9 0.0367(14) 0.0371(15) 0.0283(13) -0.0048(12) -0.0023(11) 0.0045(12) C10 0.0430(15) 0.0383(16) 0.0315(13) 0.0056(12) 0.0029(13) 0.0012(13) C11 0.039(2) 0.030(2) 0.045(2) 0.000 0.000 0.0015(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N1 2.0651(18) 2_655 ? Mg1 N1 2.0651(18) . ? Mg1 Mg1 2.8921(19) 5_655 ? Mg1 Na1 3.1801(12) . ? Mg1 Na1 3.1801(12) 5_655 ? Mg1 H1M 1.89(2) . ? Na1 N1 2.4807(18) 6 ? Na1 N1 2.4807(18) . ? Na1 Mg1 3.1801(12) 5_655 ? N1 C1 1.476(3) . ? N1 C4 1.476(3) . ? C1 C2 1.525(3) . ? C1 C3 1.529(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.522(3) . ? C4 C6 1.531(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.507(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.399(3) . ? C8 C9 1.399(3) 6 ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C10 1.385(3) 6 ? C11 H11 0.9500 . ? 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 Mg1 N1 133.16(11) 2_655 . ? N1 Mg1 Mg1 113.42(5) 2_655 5_655 ? N1 Mg1 Mg1 113.42(5) . 5_655 ? N1 Mg1 Na1 170.98(6) 2_655 . ? N1 Mg1 Na1 51.24(5) . . ? Mg1 Mg1 Na1 62.953(18) 5_655 . ? N1 Mg1 Na1 51.24(5) 2_655 5_655 ? N1 Mg1 Na1 170.98(6) . 5_655 ? Mg1 Mg1 Na1 62.953(19) 5_655 5_655 ? Na1 Mg1 Na1 125.91(4) . 5_655 ? N1 Mg1 H1M 101.4(10) 2_655 . ? N1 Mg1 H1M 114.3(10) . . ? Mg1 Mg1 H1M 39.9(7) 5_655 . ? Na1 Mg1 H1M 80.9(9) . . ? Na1 Mg1 H1M 57.3(10) 5_655 . ? N1 Na1 N1 132.08(10) 6 . ? N1 Na1 Mg1 40.47(5) 6 5_655 ? N1 Na1 Mg1 94.04(6) . 5_655 ? N1 Na1 Mg1 94.04(6) 6 . ? N1 Na1 Mg1 40.47(5) . . ? Mg1 Na1 Mg1 54.09(4) 5_655 . ? C1 N1 C4 112.03(17) . . ? C1 N1 Mg1 116.70(13) . . ? C4 N1 Mg1 114.12(14) . . ? C1 N1 Na1 115.37(13) . . ? C4 N1 Na1 108.04(12) . . ? Mg1 N1 Na1 88.29(7) . . ? N1 C1 C2 109.82(18) . . ? N1 C1 C3 115.12(19) . . ? C2 C1 C3 107.8(2) . . ? N1 C1 H1 108.0 . . ? C2 C1 H1 108.0 . . ? C3 C1 H1 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 110.66(18) . . ? N1 C4 C6 114.32(18) . . ? C5 C4 C6 108.1(2) . . ? N1 C4 H4 107.9 . . ? C5 C4 H4 107.9 . . ? C6 C4 H4 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C9 117.2(3) . 6 ? C9 C8 C7 121.37(16) . . ? C9 C8 C7 121.37(16) 6 . ? C10 C9 C8 121.3(2) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C10 119.1(4) 6 . ? C10 C11 H11 120.4 6 . ? C10 C11 H11 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mg1 Na1 N1 -75.3(4) 2_655 . . 6 ? N1 Mg1 Na1 N1 162.24(11) . . . 6 ? Mg1 Mg1 Na1 N1 -6.99(5) 5_655 . . 6 ? Na1 Mg1 Na1 N1 -6.99(5) 5_655 . . 6 ? N1 Mg1 Na1 N1 122.5(4) 2_655 . . . ? Mg1 Mg1 Na1 N1 -169.23(7) 5_655 . . . ? Na1 Mg1 Na1 N1 -169.23(7) 5_655 . . . ? N1 Mg1 Na1 Mg1 -68.3(4) 2_655 . . 5_655 ? N1 Mg1 Na1 Mg1 169.23(7) . . . 5_655 ? Na1 Mg1 Na1 Mg1 0.0 5_655 . . 5_655 ? N1 Mg1 N1 C1 72.75(14) 2_655 . . . ? Mg1 Mg1 N1 C1 -107.25(14) 5_655 . . . ? Na1 Mg1 N1 C1 -117.70(16) . . . . ? Na1 Mg1 N1 C1 -42.8(5) 5_655 . . . ? N1 Mg1 N1 C4 -60.52(13) 2_655 . . . ? Mg1 Mg1 N1 C4 119.48(13) 5_655 . . . ? Na1 Mg1 N1 C4 109.03(15) . . . . ? Na1 Mg1 N1 C4 -176.1(3) 5_655 . . . ? N1 Mg1 N1 Na1 -169.55(7) 2_655 . . . ? Mg1 Mg1 N1 Na1 10.45(7) 5_655 . . . ? Na1 Mg1 N1 Na1 74.9(4) 5_655 . . . ? N1 Na1 N1 C1 94.71(18) 6 . . . ? Mg1 Na1 N1 C1 110.18(14) 5_655 . . . ? Mg1 Na1 N1 C1 118.91(16) . . . . ? N1 Na1 N1 C4 -139.06(13) 6 . . . ? Mg1 Na1 N1 C4 -123.58(13) 5_655 . . . ? Mg1 Na1 N1 C4 -114.85(15) . . . . ? N1 Na1 N1 Mg1 -24.20(15) 6 . . . ? Mg1 Na1 N1 Mg1 -8.73(6) 5_655 . . . ? C4 N1 C1 C2 -171.00(19) . . . . ? Mg1 N1 C1 C2 54.8(2) . . . . ? Na1 N1 C1 C2 -46.8(2) . . . . ? C4 N1 C1 C3 -49.2(3) . . . . ? Mg1 N1 C1 C3 176.65(16) . . . . ? Na1 N1 C1 C3 75.0(2) . . . . ? C1 N1 C4 C5 176.20(19) . . . . ? Mg1 N1 C4 C5 -48.4(2) . . . . ? Na1 N1 C4 C5 48.0(2) . . . . ? C1 N1 C4 C6 -61.5(2) . . . . ? Mg1 N1 C4 C6 73.9(2) . . . . ? Na1 N1 C4 C6 170.32(16) . . . . ? C9 C8 C9 C10 -0.8(5) 6 . . . ? C7 C8 C9 C10 178.1(3) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C9 C10 C11 C10 0.5(5) . . . 6 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.186 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.047