# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1145 data_1 _publ_contact_author ; Alan Kennedy Dept of P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL ; _publ_requested_coeditor_name 'A Kybett' _publ_contact_author_phone ' 0141 548 4241 ' _publ_contact_author_fax ' 0141 552 5664 ' _publ_contact_author_email ' a.r.kennedy@ccsun.strath.ac.uk ' #----------------------------------------------------------------------- _audit_creation_date 'Wed Dec 9 13:13:40 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 11.102(4) _cell_length_b 12.907(6) _cell_length_c 8.906(3) _cell_angle_alpha 107.63(3) _cell_angle_beta 100.47(3) _cell_angle_gamma 96.34(4) _cell_volume 1177.3(10) _cell_formula_units_Z 1 _cell_measurement_temperature 123 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 16.70 _cell_measurement_theta_max 22.35 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _exptl_crystal_description 'rhomb' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 800.34 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H72 K2 N4 Mg2 O2 Si8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 434.00 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.925 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.25 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5673 _reflns_number_total 5394 _reflns_number_observed 5156 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0108 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.04150 _diffrn_orient_matrix_UB_12 -0.01934 _diffrn_orient_matrix_UB_13 -0.09303 _diffrn_orient_matrix_UB_21 -0.08201 _diffrn_orient_matrix_UB_22 -0.01224 _diffrn_orient_matrix_UB_23 -0.07701 _diffrn_orient_matrix_UB_31 0.01455 _diffrn_orient_matrix_UB_32 0.07936 _diffrn_orient_matrix_UB_33 0.00704 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' N 0 4 0.006 0.003 'International Tables' O 0 2 0.011 0.006 'International Tables' Si 0 8 0.082 0.070 'International Tables' Mg 0 2 0.049 0.036 'International Tables' K 0 2 0.200 0.250 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom K(1) 0.75156(2) 0.06981(2) 0.09777(3) 0.0238 Uij ? ? Si(1) 0.78031(3) -0.16728(3) -0.22311(4) 0.0170 Uij ? ? Si(2) 0.74718(3) -0.21270(3) 0.08091(4) 0.0189 Uij ? ? Si(3) 0.30013(3) -0.34999(3) -0.19270(4) 0.0184 Uij ? ? Si(4) 0.32571(3) -0.25161(2) -0.45162(4) 0.0175 Uij ? ? Mg(1) 0.52054(3) -0.14054(3) -0.11291(4) 0.0143 Uij ? ? O(1) 0.50542(7) 0.01897(6) -0.07545(9) 0.0163 Uij ? ? N(1) 0.70186(8) -0.16204(8) -0.0736(1) 0.0166 Uij ? ? N(2) 0.36004(8) -0.24426(7) -0.2525(1) 0.0163 Uij ? ? C(1) 0.7700(1) -0.0420(1) -0.2887(2) 0.0262 Uij ? ? C(2) 0.9535(1) -0.1626(1) -0.1601(2) 0.0277 Uij ? ? C(3) 0.7230(1) -0.2947(1) -0.4033(2) 0.0293 Uij ? ? C(4) 0.7967(2) -0.3511(1) 0.0163(2) 0.0347 Uij ? ? C(5) 0.6174(1) -0.2248(1) 0.1864(2) 0.0274 Uij ? ? C(6) 0.8804(1) -0.1167(1) 0.2446(2) 0.0355 Uij ? ? C(7) 0.2674(1) -0.2914(1) 0.0143(2) 0.0283 Uij ? ? C(8) 0.4088(1) -0.4511(1) -0.1877(2) 0.0297 Uij ? ? C(9) 0.1457(1) -0.4334(1) -0.3223(2) 0.0318 Uij ? ? C(10) 0.1623(1) -0.2304(1) -0.5230(2) 0.0306 Uij ? ? C(11) 0.3451(2) -0.3856(1) -0.5956(2) 0.0300 Uij ? ? C(12) 0.4294(1) -0.1374(1) -0.4808(2) 0.0263 Uij ? ? H(1) 0.689(2) -0.020(2) -0.295(2) 0.047(5) Uij ? ? H(2) 0.788(2) -0.052(2) -0.390(2) 0.050(5) Uij ? ? H(3) 0.823(2) 0.019(1) -0.212(2) 0.034(4) Uij ? ? H(4) 0.987(2) -0.160(2) -0.252(2) 0.042(5) Uij ? ? H(5) 0.992(2) -0.097(2) -0.059(3) 0.061(6) Uij ? ? H(6) 0.977(2) -0.228(2) -0.136(2) 0.053(5) Uij ? ? H(7) 0.730(2) -0.352(2) -0.373(2) 0.048(5) Uij ? ? H(8) 0.638(2) -0.297(2) -0.449(2) 0.048(5) Uij ? ? H(9) 0.770(2) -0.295(2) -0.484(2) 0.047(5) Uij ? ? H(10) 0.869(2) -0.347(2) -0.020(3) 0.054(5) Uij ? ? H(11) 0.818(2) -0.373(2) 0.115(2) 0.053(5) Uij ? ? H(12) 0.730(2) -0.407(2) -0.081(3) 0.068(6) Uij ? ? H(13) 0.646(2) -0.240(2) 0.277(2) 0.044(5) Uij ? ? H(14) 0.548(2) -0.277(2) 0.118(3) 0.056(6) Uij ? ? H(15) 0.586(2) -0.156(1) 0.230(2) 0.037(4) Uij ? ? H(16) 0.908(2) -0.150(2) 0.319(2) 0.044(5) Uij ? ? H(17) 0.947(2) -0.101(2) 0.202(3) 0.061(6) Uij ? ? H(18) 0.854(2) -0.052(2) 0.303(2) 0.050(5) Uij ? ? H(19) 0.333(2) -0.236(2) 0.089(2) 0.042(5) Uij ? ? H(20) 0.260(2) -0.347(2) 0.062(3) 0.057(6) Uij ? ? H(21) 0.194(2) -0.260(1) 0.005(2) 0.037(4) Uij ? ? H(22) 0.402(2) -0.498(2) -0.301(3) 0.080(7) Uij ? ? H(23) 0.386(2) -0.497(2) -0.124(3) 0.074(7) Uij ? ? H(24) 0.482(2) -0.419(2) -0.151(3) 0.057(6) Uij ? ? H(25) 0.115(2) -0.487(2) -0.279(2) 0.045(5) Uij ? ? H(26) 0.080(2) -0.388(2) -0.326(2) 0.051(5) Uij ? ? H(27) 0.151(2) -0.468(2) -0.436(3) 0.053(5) Uij ? ? H(28) 0.101(2) -0.283(2) -0.514(3) 0.069(7) Uij ? ? H(29) 0.150(2) -0.240(2) -0.639(2) 0.051(5) Uij ? ? H(30) 0.151(2) -0.163(2) -0.466(3) 0.053(5) Uij ? ? H(31) 0.283(2) -0.435(2) -0.606(3) 0.076(7) Uij ? ? H(32) 0.414(2) -0.416(2) -0.548(3) 0.059(6) Uij ? ? H(33) 0.360(2) -0.373(2) -0.686(3) 0.087(8) Uij ? ? H(34) 0.399(2) -0.139(2) -0.580(3) 0.057(6) Uij ? ? H(35) 0.430(2) -0.070(2) -0.411(2) 0.041(5) Uij ? ? H(36) 0.514(2) -0.151(1) -0.467(2) 0.045(5) Uij ? ? 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 K(1) 0.0147(1) 0.0190(1) 0.0317(1) 0.00340(9) 0.0039(1) 0.0002(1) Si(1) 0.0148(1) 0.0183(2) 0.0181(2) 0.0052(1) 0.0050(1) 0.0049(1) Si(2) 0.0163(2) 0.0209(2) 0.0214(2) 0.0055(1) 0.0033(1) 0.0096(1) Si(3) 0.0175(2) 0.0163(2) 0.0198(2) 0.0004(1) 0.0012(1) 0.0066(1) Si(4) 0.0189(2) 0.0166(2) 0.0149(1) 0.0029(1) 0.0015(1) 0.0038(1) Mg(1) 0.0123(2) 0.0133(2) 0.0159(2) 0.0026(1) 0.0026(1) 0.0029(1) O(1) 0.0197(4) 0.0167(4) 0.0140(3) 0.0045(3) 0.0050(3) 0.0063(3) N(1) 0.0141(4) 0.0181(4) 0.0185(4) 0.0052(3) 0.0037(3) 0.0063(3) N(2) 0.0162(4) 0.0154(4) 0.0155(4) 0.0015(3) 0.0024(3) 0.0039(3) C(1) 0.0264(6) 0.0271(6) 0.0288(6) 0.0049(5) 0.0087(5) 0.0130(5) C(2) 0.0182(5) 0.0364(7) 0.0311(6) 0.0097(5) 0.0093(5) 0.0111(6) C(3) 0.0356(7) 0.0258(7) 0.0230(6) 0.0074(5) 0.0060(5) 0.0027(5) C(4) 0.0386(8) 0.0312(7) 0.0464(8) 0.0188(6) 0.0172(7) 0.0216(6) C(5) 0.0264(6) 0.0355(7) 0.0254(6) 0.0071(5) 0.0089(5) 0.0154(5) C(6) 0.0289(7) 0.0447(9) 0.0290(7) -0.0026(6) -0.0055(5) 0.0168(6) C(7) 0.0288(7) 0.0346(7) 0.0261(6) 0.0064(6) 0.0095(5) 0.0144(5) C(8) 0.0307(7) 0.0227(6) 0.0353(7) 0.0068(5) 0.0020(6) 0.0113(5) C(9) 0.0251(6) 0.0285(7) 0.0361(7) -0.0074(5) -0.0026(5) 0.0119(6) C(10) 0.0260(6) 0.0374(8) 0.0275(6) 0.0089(6) -0.0013(5) 0.0127(6) C(11) 0.0418(8) 0.0221(6) 0.0216(6) 0.0064(6) 0.0063(5) 0.0009(5) C(12) 0.0329(7) 0.0256(6) 0.0211(6) 0.0015(5) 0.0066(5) 0.0095(5) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/\s^2^(F)' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5156 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_obs 0.0229 _refine_ls_wR_factor_all 0.0410 _refine_ls_wR_factor_obs 0.0404 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.558 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.17 _refine_diff_density_max 0.32 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag K(1) O(1) 2.782(1) ? ? yes K(1) O(1) 2.903(1) ? ? yes K(1) N(1) 2.8551(9) ? ? yes K(1) N(2) 2.804(1) ? ? yes Si(1) N(1) 1.707(1) ? ? yes Si(1) C(1) 1.887(2) ? ? yes Si(1) C(2) 1.892(2) ? ? yes Si(1) C(3) 1.866(1) ? ? yes Si(2) N(1) 1.715(1) ? ? yes Si(2) C(4) 1.879(2) ? ? yes Si(2) C(5) 1.875(2) ? ? yes Si(2) C(6) 1.888(1) ? ? yes Si(3) N(2) 1.720(1) ? ? yes Si(3) C(7) 1.888(2) ? ? yes Si(3) C(8) 1.877(2) ? ? yes Si(3) C(9) 1.885(1) ? ? yes Si(4) N(2) 1.716(1) ? ? yes Si(4) C(10) 1.889(2) ? ? yes Si(4) C(11) 1.876(1) ? ? yes Si(4) C(12) 1.880(2) ? ? yes Mg(1) O(1) 2.0146(9) ? ? yes Mg(1) O(1) 2.0101(8) ? ? yes Mg(1) N(1) 2.044(1) ? ? yes Mg(1) N(2) 2.0428(9) ? ? yes O(1) O(1) 1.583(2) ? ? yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) K(1) O(1) 32.24(4) ? ? ? yes O(1) K(1) N(1) 73.39(2) ? ? ? yes O(1) K(1) N(2) 74.88(3) ? ? ? yes O(1) K(1) N(1) 70.45(2) ? ? ? yes O(1) K(1) N(2) 71.99(3) ? ? ? yes N(1) K(1) N(2) 142.44(3) ? ? ? yes N(1) Si(1) C(1) 110.29(6) ? ? ? yes N(1) Si(1) C(2) 114.59(6) ? ? ? yes N(1) Si(1) C(3) 113.13(6) ? ? ? yes C(1) Si(1) C(2) 103.63(7) ? ? ? yes C(1) Si(1) C(3) 109.27(6) ? ? ? yes C(2) Si(1) C(3) 105.37(6) ? ? ? yes N(1) Si(2) C(4) 114.51(7) ? ? ? yes N(1) Si(2) C(5) 110.04(6) ? ? ? yes N(1) Si(2) C(6) 112.65(7) ? ? ? yes C(4) Si(2) C(5) 108.04(8) ? ? ? yes C(4) Si(2) C(6) 106.51(7) ? ? ? yes C(5) Si(2) C(6) 104.50(7) ? ? ? yes N(2) Si(3) C(7) 109.61(6) ? ? ? yes N(2) Si(3) C(8) 111.91(7) ? ? ? yes N(2) Si(3) C(9) 115.22(6) ? ? ? yes C(7) Si(3) C(8) 109.47(7) ? ? ? yes C(7) Si(3) C(9) 103.91(7) ? ? ? yes C(8) Si(3) C(9) 106.33(6) ? ? ? yes N(2) Si(4) C(10) 113.37(6) ? ? ? yes N(2) Si(4) C(11) 113.83(6) ? ? ? yes N(2) Si(4) C(12) 109.82(5) ? ? ? yes C(10) Si(4) C(11) 106.84(6) ? ? ? yes C(10) Si(4) C(12) 104.80(7) ? ? ? yes C(11) Si(4) C(12) 107.65(7) ? ? ? yes O(1) Mg(1) O(1) 46.31(5) ? ? ? yes O(1) Mg(1) N(1) 112.20(4) ? ? ? yes O(1) Mg(1) N(2) 111.54(4) ? ? ? yes O(1) Mg(1) N(1) 110.02(3) ? ? ? yes O(1) Mg(1) N(2) 113.81(4) ? ? ? yes N(1) Mg(1) N(2) 132.16(4) ? ? ? yes K(1) O(1) K(1) 147.76(4) ? ? ? yes K(1) O(1) Mg(1) 86.43(3) ? ? ? yes K(1) O(1) Mg(1) 84.26(3) ? ? ? yes K(1) O(1) O(1) 78.11(5) ? ? ? yes K(1) O(1) Mg(1) 81.02(3) ? ? ? yes K(1) O(1) Mg(1) 83.26(3) ? ? ? yes K(1) O(1) O(1) 69.65(5) ? ? ? yes Mg(1) O(1) Mg(1) 133.69(5) ? ? ? yes Mg(1) O(1) O(1) 66.69(6) ? ? ? yes Mg(1) O(1) O(1) 67.00(5) ? ? ? yes K(1) N(1) Si(1) 100.74(4) ? ? ? yes K(1) N(1) Si(2) 100.91(4) ? ? ? yes K(1) N(1) Mg(1) 83.95(3) ? ? ? yes Si(1) N(1) Si(2) 123.46(6) ? ? ? yes Si(1) N(1) Mg(1) 118.68(6) ? ? ? yes Si(2) N(1) Mg(1) 115.08(6) ? ? ? yes K(1) N(2) Si(3) 102.50(5) ? ? ? yes K(1) N(2) Si(4) 103.94(5) ? ? ? yes K(1) N(2) Mg(1) 83.11(3) ? ? ? yes Si(3) N(2) Si(4) 121.03(5) ? ? ? yes Si(3) N(2) Mg(1) 119.09(5) ? ? ? yes Si(4) N(2) Mg(1) 115.72(6) ? ? ? yes #----------------------------------------------------------------------- #=END