# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1249 # CIF for ms 8/06791K # Kinetically Inert Cryptate Systems; Solid State and Solution # NMR Studies. # DC Apperley, W. Clegg, S. Coles, JC Coyle, N Martin, B. # Maubert, V. McKee and J. Nelson data_qub1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 Cl2 Hg N8 O8' _chemical_formula_weight 757.99 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' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 6(3)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 8.94820(10) _cell_length_b 8.94820(10) _cell_length_c 18.37580(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1274.23(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 6.309 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.68790 _diffrn_radiation_type ? _diffrn_radiation_source 'synchrotron' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4494 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.26 _reflns_number_total 1724 _reflns_number_gt 1636 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0852P)^2^+1.4770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 1724 _refine_ls_number_parameters 112 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Hg Hg 0.3333 0.6667 0.41515(7) 0.0218(2) Uani 1 d S . . N1 N 0.3333 0.6667 0.577(2) 0.031(7) Uani 1 d S . . C1 C 0.2248(14) 0.7337(15) 0.6021(6) 0.034(2) Uani 1 d . . . H1A H 0.2653 0.7884 0.6504 0.041 Uiso 1 calc R . . H1B H 0.1049 0.6374 0.6076 0.041 Uiso 1 calc R . . C2 C 0.2276(16) 0.8661(15) 0.5488(7) 0.041(2) Uani 1 d . . . H2A H 0.1439 0.9013 0.5646 0.049 Uiso 1 calc R . . H2B H 0.3439 0.9699 0.5482 0.049 Uiso 1 calc R . . N11 N 0.1840(9) 0.7935(9) 0.4772(5) 0.0253(15) Uani 1 d . . . C3 C 0.0419(14) 0.7626(14) 0.4481(6) 0.033(2) Uani 1 d . . . H3 H -0.0304 0.7983 0.4709 0.040 Uiso 1 calc R . . C4 C -0.0073(10) 0.6695(11) 0.3775(5) 0.0199(14) Uani 1 d . . . H4 H -0.1084 0.6529 0.3534 0.024 Uiso 1 calc R . . N12 N 0.0782(11) 0.6143(11) 0.3499(5) 0.0329(18) Uani 1 d . . . C5 C 0.0300(10) 0.5255(11) 0.2793(6) 0.030(2) Uani 1 d . . . H5A H -0.0855 0.5046 0.2648 0.036 Uiso 1 calc R . . H5B H 0.0242 0.4124 0.2835 0.036 Uiso 1 calc R . . C6 C 0.1627(17) 0.6350(18) 0.2211(10) 0.056(4) Uani 1 d . . . H6A H 0.1298 0.5739 0.1738 0.067 Uiso 1 calc R . . H6B H 0.1652 0.7462 0.2154 0.067 Uiso 1 calc R . . N2 N 0.3333 0.6667 0.2426(16) 0.019(5) Uani 1 d S . . Cl1 Cl 0.6667 0.3333 0.5109(3) 0.0328(11) Uani 1 d S . . O11 O 0.6667 0.3333 0.4323(13) 0.071(9) Uani 1 d S . . O12 O 0.5049(12) 0.3057(11) 0.5372(8) 0.072(3) Uani 1 d . . . Cl2 Cl 0.0000 0.0000 0.2542(3) 0.0267(8) Uani 1 d S . . O21 O 0.0000 0.0000 0.3331(9) 0.041(4) Uani 1 d S . . O22 O -0.0701(11) 0.1016(12) 0.2289(5) 0.050(2) Uani 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 Hg 0.0177(2) 0.0177(2) 0.0300(4) 0.000 0.000 0.00885(10) N1 0.029(8) 0.029(8) 0.035(17) 0.000 0.000 0.014(4) C1 0.049(6) 0.061(7) 0.008(6) -0.001(5) -0.002(4) 0.040(6) C2 0.046(6) 0.045(5) 0.041(8) -0.001(5) 0.008(5) 0.029(5) N11 0.033(4) 0.026(3) 0.022(5) 0.006(3) 0.007(3) 0.018(3) C3 0.048(6) 0.036(5) 0.031(6) 0.017(4) 0.017(5) 0.033(5) C4 0.016(3) 0.016(3) 0.028(4) 0.008(3) 0.000(3) 0.008(3) N12 0.034(4) 0.032(4) 0.035(5) -0.006(4) -0.008(4) 0.018(3) C5 0.016(3) 0.030(4) 0.033(6) -0.002(4) -0.005(3) 0.003(3) C6 0.038(6) 0.049(7) 0.070(12) 0.007(7) -0.009(6) 0.013(5) N2 0.021(7) 0.021(7) 0.016(13) 0.000 0.000 0.010(4) Cl1 0.0289(14) 0.0289(14) 0.041(4) 0.000 0.000 0.0144(7) O11 0.087(10) 0.087(10) 0.04(3) 0.000 0.000 0.044(5) O12 0.045(5) 0.060(6) 0.111(10) -0.009(6) -0.013(5) 0.025(4) Cl2 0.0238(10) 0.0238(10) 0.032(3) 0.000 0.000 0.0119(5) O21 0.040(4) 0.040(4) 0.044(12) 0.000 0.000 0.020(2) O22 0.050(5) 0.059(5) 0.057(7) 0.004(4) -0.001(4) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg N12 2.409(8) . y Hg N12 2.409(8) 3_565 ? Hg N12 2.409(8) 2_665 ? Hg N11 2.427(7) . y Hg N11 2.427(7) 3_565 ? Hg N11 2.427(7) 2_665 ? N1 C1 1.447(15) . y N1 C1 1.447(15) 3_565 ? N1 C1 1.447(15) 2_665 ? C1 C2 1.528(15) . y C2 N11 1.432(15) . y N11 C3 1.276(13) . y C3 C4 1.484(13) . y C4 N12 1.211(12) . y N12 C5 1.469(13) . y C5 C6 1.532(18) . y C6 N2 1.462(16) . y N2 C6 1.462(16) 3_565 ? N2 C6 1.462(16) 2_665 ? Cl1 O12 1.425(11) 2_655 ? Cl1 O12 1.425(11) 3_665 ? Cl1 O12 1.425(11) . ? Cl1 O11 1.45(3) . ? Cl2 O22 1.416(8) 2 ? Cl2 O22 1.416(8) 3 ? Cl2 O22 1.416(8) . ? Cl2 O21 1.451(17) . ? 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 N12 Hg N12 97.3(3) . 3_565 y N12 Hg N12 97.3(3) . 2_665 ? N12 Hg N12 97.3(3) 3_565 2_665 ? N12 Hg N11 68.6(3) . . y N12 Hg N11 96.9(3) 3_565 . y N12 Hg N11 161.1(3) 2_665 . ? N12 Hg N11 161.1(3) . 3_565 y N12 Hg N11 68.6(3) 3_565 3_565 ? N12 Hg N11 96.9(3) 2_665 3_565 ? N11 Hg N11 99.7(2) . 3_565 y N12 Hg N11 96.9(3) . 2_665 ? N12 Hg N11 161.1(2) 3_565 2_665 ? N12 Hg N11 68.6(3) 2_665 2_665 ? N11 Hg N11 99.7(2) . 2_665 ? N11 Hg N11 99.7(2) 3_565 2_665 ? C1 N1 C1 110.6(14) . 3_565 ? C1 N1 C1 110.6(14) . 2_665 ? C1 N1 C1 110.6(14) 3_565 2_665 ? N1 C1 C2 111.5(14) . . ? N11 C2 C1 110.0(9) . . ? C3 N11 C2 120.0(9) . . ? C3 N11 Hg 115.1(7) . . ? C2 N11 Hg 123.7(6) . . ? N11 C3 C4 118.2(8) . . ? N12 C4 C3 121.7(8) . . ? C4 N12 C5 121.1(8) . . ? C4 N12 Hg 116.3(7) . . ? C5 N12 Hg 122.6(6) . . ? N12 C5 C6 110.3(9) . . ? N2 C6 C5 109.6(14) . . ? C6 N2 C6 113.0(12) . 3_565 ? C6 N2 C6 113.0(12) . 2_665 ? C6 N2 C6 113.0(12) 3_565 2_665 ? O12 Cl1 O12 109.1(6) 2_655 3_665 ? O12 Cl1 O12 109.1(6) 2_655 . ? O12 Cl1 O12 109.1(6) 3_665 . ? O12 Cl1 O11 109.8(6) 2_655 . ? O12 Cl1 O11 109.8(6) 3_665 . ? O12 Cl1 O11 109.8(6) . . ? O22 Cl2 O22 109.8(5) 2 3 ? O22 Cl2 O22 109.8(5) 2 . ? O22 Cl2 O22 109.8(4) 3 . ? O22 Cl2 O21 109.1(5) 2 . ? O22 Cl2 O21 109.1(5) 3 . ? O22 Cl2 O21 109.1(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 N11 C3 C4 N12 4.5(12) . . . . y _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 1.689 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.236