Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Dr Phil Andrews' _publ_contact_author_address ; Dr Phil Andrews Department of Chemistry Monash University Clayton Melbourne Victoria 3800 AUSTRALIA ; _publ_contact_author_email p.andrews@sci.monash.edu.au _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Andrews, Phil' 'Armstrong, David R.' 'Raston, Colin' 'Roberts, Brett A.' 'Skelton, Brian W.' 'White, Allan' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; data_r'lipmdeta _database_code_CSD 154200 #------------------------------------------------------------------------------ _audit_creation_date '19100-11-22' ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 7.6805(2) _cell_length_b 16.0419(2) _cell_length_c 18.9022(4) _cell_angle_alpha 90 _cell_angle_beta 100.5403(8) _cell_angle_gamma 90 _cell_volume 2289.64(7) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'unknown' _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 429.74 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H46 Li N4 Si2 ' _chemical_formula_moiety 'C22 H46 Li N4 Si2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 948.00 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 12605 _reflns_number_total 6575 _reflns_number_gt 4188 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03221 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si 0 8 0.072 0.071 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Li 0 4 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 88 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 184 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Si(2) 0.91087(7) 0.13177(3) 0.87821(3) 0.0242(1) 1.000 . Uani d ? N(1) 0.8635(2) 0.12063(8) 0.65679(7) 0.0203(4) 1.000 . Uani d ? N(01) 1.2851(2) 0.13806(8) 0.65260(8) 0.0259(4) 1.000 . Uani d ? N(04) 1.2772(2) 0.28416(8) 0.74349(8) 0.0249(4) 1.000 . Uani d ? N(07) 0.9821(2) 0.32320(8) 0.62560(8) 0.0239(4) 1.000 . Uani d ? C(2) 0.8662(2) 0.0941(1) 0.72719(9) 0.0182(5) 1.000 . Uani d ? C(02) 1.4390(2) 0.1941(1) 0.6710(1) 0.0318(6) 1.000 . Uani d ? C(3) 0.8296(2) 0.0073(1) 0.73801(9) 0.0209(5) 1.000 . Uani d ? C(03) 1.4429(2) 0.2385(1) 0.7413(1) 0.0328(6) 1.000 . Uani d ? C(4) 0.7792(2) -0.0441(1) 0.6811(1) 0.0256(5) 1.000 . Uani d ? C(5) 0.7642(3) -0.0143(1) 0.6105(1) 0.0289(5) 1.000 . Uani d ? C(05) 1.2676(2) 0.3614(1) 0.7010(1) 0.0293(5) 1.000 . Uani d ? C(6) 0.8096(2) 0.0677(1) 0.60157(9) 0.0239(5) 1.000 . Uani d ? C(06) 1.0777(2) 0.3867(1) 0.6747(1) 0.0300(5) 1.000 . Uani d ? C(7) 0.7946(3) 0.1044(1) 0.5277(1) 0.0362(6) 1.000 . Uani d ? C(011) 1.3002(3) 0.0661(1) 0.7014(1) 0.0413(7) 1.000 . Uani d ? C(012) 1.2781(3) 0.1074(1) 0.5793(1) 0.0400(6) 1.000 . Uani d ? C(21) 0.9045(2) 0.1515(1) 0.78323(9) 0.0213(5) 1.000 . Uani d ? C(22) 0.9446(3) 0.2315(1) 0.9303(1) 0.0440(7) 1.000 . Uani d ? C(23) 1.0932(3) 0.0583(1) 0.9180(1) 0.0427(7) 1.000 . Uani d ? C(24) 0.6991(3) 0.0873(1) 0.8978(1) 0.0316(6) 1.000 . Uani d ? C(041) 1.2670(3) 0.3037(1) 0.8183(1) 0.0402(6) 1.000 . Uani d ? C(071) 0.7901(2) 0.3319(1) 0.6215(1) 0.0313(6) 1.000 . Uani d ? C(072) 1.0229(3) 0.3322(1) 0.5535(1) 0.0405(6) 1.000 . Uani d ? Li 1.0653(4) 0.2058(2) 0.6762(2) 0.0253(8) 1.000 . Uani d ? H(1) 0.8409 -0.0141 0.7855 0.025 1.000 . Uiso c ? H(2) 0.7538 -0.1009 0.6891 0.031 1.000 . Uiso c ? H(3) 0.7241 -0.0493 0.5703 0.035 1.000 . Uiso c ? H(4) 0.9066 0.1254 0.5217 0.043 1.000 . Uiso c ? H(5) 0.7569 0.0626 0.4927 0.043 1.000 . Uiso c ? H(6) 0.7107 0.1486 0.5221 0.043 1.000 . Uiso c ? H(7) 1.3270 0.4047 0.7302 0.035 1.000 . Uiso c ? H(8) 1.3236 0.3527 0.6608 0.035 1.000 . Uiso c ? H(9) 1.0754 0.4382 0.6498 0.036 1.000 . Uiso c ? H(10) 1.0205 0.3930 0.7149 0.036 1.000 . Uiso c ? H(11) 1.5442 0.1621 0.6742 0.038 1.000 . Uiso c ? H(12) 1.4343 0.2345 0.6340 0.038 1.000 . Uiso c ? H(13) 1.5384 0.2770 0.7482 0.039 1.000 . Uiso c ? H(14) 1.4608 0.1986 0.7790 0.039 1.000 . Uiso c ? H(15) 1.2005 0.0307 0.6879 0.050 1.000 . Uiso c ? H(16) 1.4054 0.0361 0.6986 0.050 1.000 . Uiso c ? H(17) 1.3046 0.0850 0.7493 0.050 1.000 . Uiso c ? H(18) 1.1785 0.0718 0.5664 0.048 1.000 . Uiso c ? H(19) 1.2679 0.1533 0.5470 0.048 1.000 . Uiso c ? H(20) 1.3832 0.0773 0.5768 0.048 1.000 . Uiso c ? H(21) 1.3646 0.3378 0.8385 0.048 1.000 . Uiso c ? H(22) 1.1597 0.3325 0.8198 0.048 1.000 . Uiso c ? H(23) 1.2700 0.2535 0.8451 0.048 1.000 . Uiso c ? H(24) 0.7532 0.3852 0.6025 0.038 1.000 . Uiso c ? H(25) 0.7304 0.2898 0.5909 0.038 1.000 . Uiso c ? H(26) 0.7626 0.3263 0.6682 0.038 1.000 . Uiso c ? H(27) 1.1468 0.3259 0.5557 0.049 1.000 . Uiso c ? H(28) 0.9615 0.2907 0.5228 0.049 1.000 . Uiso c ? H(29) 0.9871 0.3858 0.5351 0.049 1.000 . Uiso c ? H(32) 0.9533 0.2200 0.9801 0.053 1.000 . Uiso c ? H(33) 1.0506 0.2575 0.9225 0.053 1.000 . Uiso c ? H(34) 0.8471 0.2676 0.9148 0.053 1.000 . Uiso c ? H(35) 1.0975 0.0540 0.9684 0.051 1.000 . Uiso c ? H(36) 1.0711 0.0049 0.8965 0.051 1.000 . Uiso c ? H(37) 1.2032 0.0789 0.9091 0.051 1.000 . Uiso c ? H(38) 0.6050 0.1253 0.8824 0.038 1.000 . Uiso c ? H(39) 0.6745 0.0359 0.8729 0.038 1.000 . Uiso c ? H(40) 0.7105 0.0780 0.9481 0.038 1.000 . Uiso c ? H(41) 0.9300 0.2068 0.7704 0.026 1.000 . Uiso c ? 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 Si(2) 0.0258(3) 0.0261(3) 0.0204(3) -0.0025(2) 0.0030(2) -0.0035(2) N(1) 0.0192(8) 0.0227(7) 0.0191(8) 0.0026(6) 0.0042(6) -0.0002(6) N(01) 0.0235(9) 0.0228(8) 0.0323(9) 0.0028(7) 0.0070(7) -0.0001(7) N(04) 0.0207(9) 0.0278(8) 0.0267(9) -0.0008(6) 0.0055(7) 0.0004(6) N(07) 0.0197(9) 0.0237(8) 0.0288(9) 0.0009(6) 0.0057(7) 0.0015(6) C(2) 0.0101(9) 0.0222(9) 0.022(1) 0.0025(7) 0.0033(7) 0.0022(7) C(02) 0.018(1) 0.033(1) 0.045(1) 0.0056(8) 0.0064(9) 0.0004(9) C(3) 0.020(1) 0.0214(9) 0.021(1) 0.0025(7) 0.0038(8) 0.0032(7) C(03) 0.021(1) 0.035(1) 0.040(1) 0.0011(8) 0.0013(9) 0.0018(9) C(4) 0.030(1) 0.0169(9) 0.029(1) 0.0005(7) 0.0039(9) -0.0004(8) C(5) 0.035(1) 0.025(1) 0.024(1) 0.0013(8) -0.0008(9) -0.0072(8) C(05) 0.026(1) 0.0233(9) 0.040(1) -0.0047(8) 0.0080(9) -0.0014(8) C(6) 0.024(1) 0.026(1) 0.021(1) 0.0068(8) 0.0022(8) 0.0001(8) C(06) 0.027(1) 0.0198(9) 0.043(1) -0.0014(8) 0.0054(9) -0.0016(8) C(7) 0.050(1) 0.033(1) 0.025(1) 0.0036(9) 0.006(1) 0.0002(8) C(011) 0.037(1) 0.030(1) 0.060(2) 0.0114(9) 0.015(1) 0.012(1) C(012) 0.038(1) 0.039(1) 0.046(1) 0.0055(9) 0.013(1) -0.010(1) C(21) 0.021(1) 0.0197(9) 0.024(1) -0.0039(7) 0.0049(8) -0.0014(7) C(22) 0.062(2) 0.042(1) 0.030(1) -0.018(1) 0.014(1) -0.011(1) C(23) 0.039(1) 0.056(1) 0.029(1) 0.007(1) -0.003(1) 0.001(1) C(24) 0.039(1) 0.030(1) 0.027(1) -0.0009(9) 0.0087(9) -0.0002(8) C(041) 0.037(1) 0.050(1) 0.033(1) -0.008(1) 0.006(1) -0.009(1) C(071) 0.024(1) 0.028(1) 0.040(1) 0.0015(8) 0.0024(9) 0.0019(9) C(072) 0.039(1) 0.047(1) 0.036(1) 0.008(1) 0.010(1) 0.009(1) Li 0.021(2) 0.025(1) 0.031(2) 0.002(1) 0.007(1) 0.001(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4188 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_all 0.0483 _refine_ls_wR_factor_ref 0.0483 _refine_ls_goodness_of_fit_all 2.325 _refine_ls_goodness_of_fit_ref 2.325 _refine_ls_shift/su_max 0.0056 _refine_ls_shift/su_mean 0.0017 _refine_diff_density_min -0.38 _refine_diff_density_max 0.29 #------------------------------------------------------------------------------ _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 Si(2) C(21) 1.815(2) . . yes Si(2) C(22) 1.871(2) . . yes Si(2) C(23) 1.879(2) . . yes Si(2) C(24) 1.874(2) . . yes N(1) C(2) 1.393(2) . . yes N(1) C(6) 1.351(2) . . yes N(1) Li 2.048(3) . . yes N(01) C(02) 1.475(2) . . yes N(01) C(011) 1.469(2) . . yes N(01) C(012) 1.462(2) . . yes N(01) Li 2.123(3) . . yes N(04) C(03) 1.475(2) . . yes N(04) C(05) 1.471(2) . . yes N(04) C(041) 1.465(2) . . yes N(04) Li 2.257(3) . . yes N(07) C(06) 1.479(2) . . yes N(07) C(071) 1.469(2) . . yes N(07) C(072) 1.461(2) . . yes N(07) Li 2.156(3) . . yes C(2) C(3) 1.443(2) . . yes C(2) C(21) 1.393(2) . . yes C(02) C(03) 1.502(3) . . yes C(02) H(11) 0.95 . . no C(02) H(12) 0.95 . . no C(3) C(4) 1.354(2) . . yes C(3) H(1) 0.95 . . no C(03) H(13) 0.95 . . no C(03) H(14) 0.95 . . no C(4) C(5) 1.402(2) . . yes C(4) H(2) 0.95 . . no C(5) C(6) 1.378(2) . . yes C(5) H(3) 0.95 . . no C(05) C(06) 1.508(2) . . yes C(05) H(7) 0.95 . . no C(05) H(8) 0.95 . . no C(6) C(7) 1.500(2) . . yes C(06) H(9) 0.95 . . no C(06) H(10) 0.95 . . no C(7) H(4) 0.95 . . no C(7) H(5) 0.95 . . no C(7) H(6) 0.95 . . no C(011) H(15) 0.95 . . no C(011) H(16) 0.95 . . no C(011) H(17) 0.95 . . no C(012) H(18) 0.95 . . no C(012) H(19) 0.95 . . no C(012) H(20) 0.95 . . no C(21) H(41) 0.95 . . no C(22) H(32) 0.95 . . no C(22) H(33) 0.95 . . no C(22) H(34) 0.95 . . no C(23) H(35) 0.95 . . no C(23) H(36) 0.95 . . no C(23) H(37) 0.95 . . no C(24) H(38) 0.95 . . no C(24) H(39) 0.95 . . no C(24) H(40) 0.95 . . no C(041) H(21) 0.95 . . no C(041) H(22) 0.95 . . no C(041) H(23) 0.95 . . no C(071) H(24) 0.95 . . no C(071) H(25) 0.95 . . no C(071) H(26) 0.95 . . no C(072) H(27) 0.95 . . no C(072) H(28) 0.95 . . no C(072) H(29) 0.95 . . no #------------------------------------------------------------------------------ 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 C(21) Si(2) C(22) 110.36(8) . . . yes C(21) Si(2) C(23) 112.85(9) . . . yes C(21) Si(2) C(24) 113.25(8) . . . yes C(22) Si(2) C(23) 107.7(1) . . . yes C(22) Si(2) C(24) 105.26(9) . . . yes C(23) Si(2) C(24) 106.97(9) . . . yes C(2) N(1) C(6) 119.7(1) . . . yes C(2) N(1) Li 98.8(1) . . . yes C(6) N(1) Li 132.3(1) . . . yes C(02) N(01) C(011) 111.3(1) . . . yes C(02) N(01) C(012) 108.5(1) . . . yes C(02) N(01) Li 105.8(1) . . . yes C(011) N(01) C(012) 108.5(1) . . . yes C(011) N(01) Li 104.2(1) . . . yes C(012) N(01) Li 118.6(1) . . . yes C(03) N(04) C(05) 111.1(1) . . . yes C(03) N(04) C(041) 109.4(1) . . . yes C(03) N(04) Li 104.1(1) . . . yes C(05) N(04) C(041) 109.9(1) . . . yes C(05) N(04) Li 101.7(1) . . . yes C(041) N(04) Li 120.2(1) . . . yes C(06) N(07) C(071) 110.3(1) . . . yes C(06) N(07) C(072) 110.6(1) . . . yes C(06) N(07) Li 104.5(1) . . . yes C(071) N(07) C(072) 109.0(1) . . . yes C(071) N(07) Li 108.6(1) . . . yes C(072) N(07) Li 113.8(1) . . . yes N(1) C(2) C(3) 117.4(1) . . . yes N(1) C(2) C(21) 119.3(1) . . . yes C(3) C(2) C(21) 123.3(2) . . . yes N(01) C(02) C(03) 112.5(2) . . . yes N(01) C(02) H(11) 108.7 . . . no N(01) C(02) H(12) 108.7 . . . no C(03) C(02) H(11) 108.7 . . . no C(03) C(02) H(12) 108.7 . . . no H(11) C(02) H(12) 109.5 . . . no C(2) C(3) C(4) 120.6(2) . . . yes C(2) C(3) H(1) 119.7 . . . no C(4) C(3) H(1) 119.7 . . . no N(04) C(03) C(02) 112.5(1) . . . yes N(04) C(03) H(13) 108.7 . . . no N(04) C(03) H(14) 108.7 . . . no C(02) C(03) H(13) 108.7 . . . no C(02) C(03) H(14) 108.7 . . . no H(13) C(03) H(14) 109.5 . . . no C(3) C(4) C(5) 120.7(2) . . . yes C(3) C(4) H(2) 119.7 . . . no C(5) C(4) H(2) 119.7 . . . no C(4) C(5) C(6) 117.6(2) . . . yes C(4) C(5) H(3) 121.2 . . . no C(6) C(5) H(3) 121.2 . . . no N(04) C(05) C(06) 110.8(1) . . . yes N(04) C(05) H(7) 109.1 . . . no N(04) C(05) H(8) 109.1 . . . no C(06) C(05) H(7) 109.1 . . . no C(06) C(05) H(8) 109.1 . . . no H(7) C(05) H(8) 109.5 . . . no N(1) C(6) C(5) 123.6(2) . . . yes N(1) C(6) C(7) 115.6(1) . . . yes C(5) C(6) C(7) 120.7(2) . . . yes N(07) C(06) C(05) 111.2(1) . . . yes N(07) C(06) H(9) 109.0 . . . no N(07) C(06) H(10) 109.0 . . . no C(05) C(06) H(9) 109.0 . . . no C(05) C(06) H(10) 109.0 . . . no H(9) C(06) H(10) 109.5 . . . no C(6) C(7) H(4) 109.5 . . . no C(6) C(7) H(5) 109.5 . . . no C(6) C(7) H(6) 109.5 . . . no H(4) C(7) H(5) 109.5 . . . no H(4) C(7) H(6) 109.5 . . . no H(5) C(7) H(6) 109.5 . . . no N(01) C(011) H(15) 109.5 . . . no N(01) C(011) H(16) 109.5 . . . no N(01) C(011) H(17) 109.5 . . . no H(15) C(011) H(16) 109.5 . . . no H(15) C(011) H(17) 109.5 . . . no H(16) C(011) H(17) 109.5 . . . no N(01) C(012) H(18) 109.5 . . . no N(01) C(012) H(19) 109.5 . . . no N(01) C(012) H(20) 109.5 . . . no H(18) C(012) H(19) 109.5 . . . no H(18) C(012) H(20) 109.5 . . . no H(19) C(012) H(20) 109.5 . . . no Si(2) C(21) C(2) 127.0(1) . . . yes Si(2) C(21) H(41) 116.5 . . . no C(2) C(21) H(41) 116.5 . . . no Si(2) C(22) H(32) 109.5 . . . no Si(2) C(22) H(33) 109.5 . . . no Si(2) C(22) H(34) 109.5 . . . no H(32) C(22) H(33) 109.5 . . . no H(32) C(22) H(34) 109.5 . . . no H(33) C(22) H(34) 109.5 . . . no Si(2) C(23) H(35) 109.5 . . . no Si(2) C(23) H(36) 109.5 . . . no Si(2) C(23) H(37) 109.5 . . . no H(35) C(23) H(36) 109.5 . . . no H(35) C(23) H(37) 109.5 . . . no H(36) C(23) H(37) 109.5 . . . no Si(2) C(24) H(38) 109.5 . . . no Si(2) C(24) H(39) 109.5 . . . no Si(2) C(24) H(40) 109.5 . . . no H(38) C(24) H(39) 109.5 . . . no H(38) C(24) H(40) 109.5 . . . no H(39) C(24) H(40) 109.5 . . . no N(04) C(041) H(21) 109.5 . . . no N(04) C(041) H(22) 109.5 . . . no N(04) C(041) H(23) 109.5 . . . no H(21) C(041) H(22) 109.5 . . . no H(21) C(041) H(23) 109.5 . . . no H(22) C(041) H(23) 109.5 . . . no N(07) C(071) H(24) 109.5 . . . no N(07) C(071) H(25) 109.5 . . . no N(07) C(071) H(26) 109.5 . . . no H(24) C(071) H(25) 109.5 . . . no H(24) C(071) H(26) 109.5 . . . no H(25) C(071) H(26) 109.5 . . . no N(07) C(072) H(27) 109.5 . . . no N(07) C(072) H(28) 109.5 . . . no N(07) C(072) H(29) 109.5 . . . no H(27) C(072) H(28) 109.5 . . . no H(27) C(072) H(29) 109.5 . . . no H(28) C(072) H(29) 109.5 . . . no N(1) Li N(01) 103.1(1) . . . yes N(1) Li N(04) 156.5(2) . . . yes N(1) Li N(07) 110.5(1) . . . yes N(01) Li N(04) 83.3(1) . . . yes N(01) Li N(07) 122.5(2) . . . yes N(04) Li N(07) 83.6(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(1) C(02) 3.523(2) . 1_455 no #------------------------------------------------------------------------------ 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 Si(2) C(21) C(2) N(1) . . . . 178.6(1) no Si(2) C(21) C(2) C(3) . . . . -1.8(2) no N(1) C(2) C(3) C(4) . . . . -5.7(2) no N(1) C(6) C(5) C(4) . . . . -1.6(3) no N(1) Li N(01) C(02) . . . . -175.7(1) no N(1) Li N(01) C(011) . . . . -58.3(2) no N(1) Li N(01) C(012) . . . . 62.3(2) no N(1) Li N(04) C(03) . . . . 100.2(4) no N(1) Li N(04) C(05) . . . . -144.3(4) no N(1) Li N(04) C(041) . . . . -22.8(4) no N(1) Li N(07) C(06) . . . . 146.5(1) no N(1) Li N(07) C(071) . . . . 28.8(2) no N(1) Li N(07) C(072) . . . . -92.8(2) no N(01) C(02) C(03) N(04) . . . . -54.5(2) no N(01) Li N(1) C(2) . . . . 98.1(1) no N(01) Li N(1) C(6) . . . . -46.8(2) no N(01) Li N(04) C(03) . . . . -7.4(1) no N(01) Li N(04) C(05) . . . . 108.1(1) no N(01) Li N(04) C(041) . . . . -130.4(1) no N(01) Li N(07) C(06) . . . . -91.9(2) no N(01) Li N(07) C(071) . . . . 150.4(2) no N(01) Li N(07) C(072) . . . . 28.8(2) no N(04) C(05) C(06) N(07) . . . . -63.0(2) no N(04) Li N(1) C(2) . . . . -5.5(4) no N(04) Li N(1) C(6) . . . . -150.4(3) no N(04) Li N(01) C(02) . . . . -18.7(1) no N(04) Li N(01) C(011) . . . . 98.7(1) no N(04) Li N(01) C(012) . . . . -140.7(1) no N(04) Li N(07) C(06) . . . . -14.0(1) no N(04) Li N(07) C(071) . . . . -131.7(1) no N(04) Li N(07) C(072) . . . . 106.6(1) no N(07) Li N(1) C(2) . . . . -129.4(1) no N(07) Li N(1) C(6) . . . . 85.6(2) no N(07) Li N(01) C(02) . . . . 59.3(2) no N(07) Li N(01) C(011) . . . . 176.7(2) no N(07) Li N(01) C(012) . . . . -62.7(2) no N(07) Li N(04) C(03) . . . . -131.3(1) no N(07) Li N(04) C(05) . . . . -15.7(1) no N(07) Li N(04) C(041) . . . . 105.8(2) no C(2) N(1) C(6) C(5) . . . . -3.3(3) no C(2) N(1) C(6) C(7) . . . . 174.3(1) no C(2) C(3) C(4) C(5) . . . . 1.0(3) no C(2) C(21) Si(2) C(22) . . . . -173.9(2) no C(2) C(21) Si(2) C(23) . . . . 65.5(2) no C(2) C(21) Si(2) C(24) . . . . -56.2(2) no C(02) C(03) N(04) C(05) . . . . -75.8(2) no C(02) C(03) N(04) C(041) . . . . 162.7(1) no C(02) C(03) N(04) Li . . . . 33.0(2) no C(3) C(2) N(1) C(6) . . . . 6.8(2) no C(3) C(2) N(1) Li . . . . -143.9(1) no C(3) C(4) C(5) C(6) . . . . 2.7(3) no C(03) N(04) C(05) C(06) . . . . 153.9(1) no C(03) C(02) N(01) C(011) . . . . -69.0(2) no C(03) C(02) N(01) C(012) . . . . 171.7(2) no C(03) C(02) N(01) Li . . . . 43.5(2) no C(4) C(3) C(2) C(21) . . . . 174.6(2) no C(4) C(5) C(6) C(7) . . . . -179.1(2) no C(5) C(6) N(1) Li . . . . 135.8(2) no C(05) C(06) N(07) C(071) . . . . 159.5(1) no C(05) C(06) N(07) C(072) . . . . -79.9(2) no C(05) C(06) N(07) Li . . . . 42.9(2) no C(6) N(1) C(2) C(21) . . . . -173.5(2) no C(06) C(05) N(04) C(041) . . . . -84.8(2) no C(06) C(05) N(04) Li . . . . 43.6(2) no C(7) C(6) N(1) Li . . . . -46.5(2) no C(21) C(2) N(1) Li . . . . 35.8(2) no #------------------------------------------------------------------------------ data_pca17 _database_code_CSD 154201 _audit_creation_method Xtal3.6 _audit_creation_date 00-05-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C36 H74 K2 N8 Si2' _chemical_formula_moiety ? _chemical_formula_weight 753.41 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.274(3) _cell_length_b 19.453(11) _cell_length_c 12.098(16) _cell_angle_alpha 90.00000 _cell_angle_beta 99.89(8) _cell_angle_gamma 90.00000 _cell_volume 2382(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.05 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 14.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .28 _exptl_crystal_description block _exptl_crystal_size_max .38 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.95 _diffrn_reflns_number 6327 _reflns_number_total 3289 _reflns_Friedel_coverage ? _reflns_number_gt 1077 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 22.96 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .049 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .038 _refine_ls_goodness_of_fit_ref 1.775 _refine_ls_number_reflns 1077 _refine_ls_number_parameters 237 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .032 _refine_diff_density_min -.18 _refine_diff_density_max .29 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 72 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 4 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' K ? 0 4 .179016 .25 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 148 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K .37232(17) .51574(8) .10372(13) .0821(12) Uani ? ? 1.00000 ? ? N1 .6520(6) .5096(4) .1287(5) .074(5) Uani ? ? 1.00000 ? ? C2 .6723(8) .5777(5) .1519(7) .060(7) Uani ? ? 1.00000 ? ? C21 .6100(9) .6290(4) .0838(8) .068(6) Uani ? ? 1.00000 ? ? Si2 .6232(2) .72193(13) .0968(2) .0900(18) Uani ? ? 1.00000 ? ? C22 .7909(7) .7566(4) .0867(8) .128(8) Uani ? ? 1.00000 ? ? C23 .5036(8) .7629(4) -.0188(7) .128(7) Uani ? ? 1.00000 ? ? C24 .5823(9) .7570(4) .2320(8) .144(8) Uani ? ? 1.00000 ? ? C3 .7627(11) .5947(6) .2527(10) .085(8) Uani ? ? 1.00000 ? ? C4 .8260(10) .5470(8) .3216(8) .089(8) Uani ? ? 1.00000 ? ? C5 .8062(12) .4774(8) .2952(10) .100(9) Uani ? ? 1.00000 ? ? C6 .7186(11) .4626(5) .2009(10) .083(8) Uani ? ? 1.00000 ? ? N01 .3068(10) .4122(4) .2568(8) .117(7) Uani ? ? 1.00000 ? ? C011 .4151(13) .3667(6) .2748(9) .182(12) Uani ? ? 1.00000 ? ? C012 .1960(14) .3714(8) .1996(11) .258(16) Uani ? ? 1.00000 ? ? C02 .3030(17) .4997(9) .3926(10) .178(12) Uani ? ? 1.00000 ? ? C03 .280(2) .4392(8) .3590(14) .219(16) Uani ? ? 1.00000 ? ? N04 .3135(9) .5572(4) .3179(6) .092(6) Uani ? ? 1.00000 ? ? C041 .4336(11) .5949(5) .3558(7) .132(9) Uani ? ? 1.00000 ? ? C05 .2037(12) .6010(8) .3105(9) .181(12) Uani ? ? 1.00000 ? ? C06 .1633(11) .6438(5) .2172(11) .144(9) Uani ? ? 1.00000 ? ? N07 .1630(7) .6162(4) .1065(7) .089(6) Uani ? ? 1.00000 ? ? C071 .0474(13) .5789(5) .0732(9) .170(11) Uani ? ? 1.00000 ? ? C072 .1724(10) .6705(5) .0280(9) .164(9) Uani ? ? 1.00000 ? ? H21 .546(5) .607(3) .019(4) .05(2) Uiso ? ? 1.00000 ? ? H22a .79951 .80524 .09590 .18600 Uiso ? ? 1.00000 ? ? H22b .81440 .74767 .01022 .18600 Uiso ? ? 1.00000 ? ? H22c .86202 .73527 .13741 .18600 Uiso ? ? 1.00000 ? ? H23a .51802 .74789 -.09252 .18700 Uiso ? ? 1.00000 ? ? H23b .51028 .81229 -.01827 .18700 Uiso ? ? 1.00000 ? ? H23c .41278 .75173 -.01485 .18700 Uiso ? ? 1.00000 ? ? H24a .63861 .74185 .29816 .20500 Uiso ? ? 1.00000 ? ? H24b .49084 .74458 .24280 .20500 Uiso ? ? 1.00000 ? ? H24c .58162 .80744 .23464 .20500 Uiso ? ? 1.00000 ? ? H3 .797(6) .637(3) .264(5) .05(2) Uiso ? ? 1.00000 ? ? H4 .890(6) .561(3) .392(5) .08(3) Uiso ? ? 1.00000 ? ? H5 .854(8) .441(4) .342(6) .16(5) Uiso ? ? 1.00000 ? ? H6 .705(6) .413(3) .174(5) .07(2) Uiso ? ? 1.00000 ? ? H011a .40551 .32875 .32070 .24300 Uiso ? ? 1.00000 ? ? H011b .49721 .39058 .30812 .24300 Uiso ? ? 1.00000 ? ? H011c .43336 .34924 .20304 .24300 Uiso ? ? 1.00000 ? ? H012a .11873 .40269 .18860 .36000 Uiso ? ? 1.00000 ? ? H012b .17638 .33555 .24664 .36000 Uiso ? ? 1.00000 ? ? H012c .21178 .35684 .13183 .36000 Uiso ? ? 1.00000 ? ? H02a .38611 .49957 .44534 .22500 Uiso ? ? 1.00000 ? ? H02b .23674 .51526 .43735 .22500 Uiso ? ? 1.00000 ? ? H03a .31814 .41160 .42184 .25000 Uiso ? ? 1.00000 ? ? H03b .18272 .43629 .35700 .25000 Uiso ? ? 1.00000 ? ? H041a .44539 .61051 .43225 .16000 Uiso ? ? 1.00000 ? ? H041b .44547 .63524 .31035 .16000 Uiso ? ? 1.00000 ? ? H041c .51278 .56629 .35147 .16000 Uiso ? ? 1.00000 ? ? H05a .20119 .62293 .38022 .20000 Uiso ? ? 1.00000 ? ? H05b .12559 .56586 .30579 .20000 Uiso ? ? 1.00000 ? ? H06a .22962 .68160 .23131 .18000 Uiso ? ? 1.00000 ? ? H06b .08051 .66569 .22464 .18000 Uiso ? ? 1.00000 ? ? H071a -.02974 .60901 .06771 .24000 Uiso ? ? 1.00000 ? ? H071b .03743 .54320 .12318 .24000 Uiso ? ? 1.00000 ? ? H071c .04402 .55969 -.00119 .24000 Uiso ? ? 1.00000 ? ? H072a .10694 .70524 .02888 .22600 Uiso ? ? 1.00000 ? ? H072b .16497 .65401 -.04809 .22600 Uiso ? ? 1.00000 ? ? H072c .25818 .69261 .04618 .22600 Uiso ? ? 1.00000 ? ? 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 .0943(14) .0958(14) .0616(10) .0231(12) .0290(9) .0073(11) N1 .096(5) .051(5) .073(5) .013(5) .011(4) -.006(4) C2 .053(6) .080(9) .049(6) -.004(6) .012(5) -.002(6) C21 .076(7) .056(7) .071(6) -.008(5) .006(5) .006(5) Si2 .089(2) .0692(18) .115(2) -.0030(16) .0251(16) .0054(16) C22 .088(7) .082(7) .215(10) -.014(6) .024(6) .018(6) C23 .101(7) .109(8) .167(9) .015(6) .001(6) .046(6) C24 .192(9) .081(7) .169(9) -.005(6) .062(8) -.035(6) C3 .089(9) .070(9) .096(9) -.007(7) .011(7) .017(8) C4 .081(8) .126(11) .060(8) -.018(8) .013(7) -.017(8) C5 .098(9) .125(12) .073(8) .016(9) .004(7) .018(9) C6 .093(9) .061(9) .097(8) .017(7) .022(7) -.001(7) N01 .155(9) .095(8) .100(7) .002(6) .022(7) .019(6) C011 .232(14) .148(12) .168(11) .019(10) .037(10) .040(9) C012 .247(16) .267(18) .233(16) -.124(14) -.036(13) .031(12) C02 .272(14) .201(17) .076(8) -.043(17) .072(8) .007(12) C03 .42(3) .138(13) .135(15) .043(17) .144(17) .056(12) N04 .096(7) .108(7) .071(5) .026(6) .009(5) -.013(5) C041 .137(10) .156(10) .099(8) -.011(8) .004(7) -.004(7) C05 .170(12) .281(17) .082(9) .112(12) -.001(8) -.056(9) C06 .189(12) .117(9) .123(10) .061(8) .022(9) -.019(8) N07 .101(7) .083(6) .086(6) .023(5) .018(5) .000(5) C071 .205(13) .121(10) .172(11) -.045(9) .002(9) -.041(8) C072 .182(10) .157(10) .164(10) .034(8) .061(8) .077(9) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published K N1 . . 2.839(7) ? K N01 . . 2.894(10) ? K N04 . . 2.876(8) ? K N07 . . 2.910(8) ? K H21 . . 2.83(5) ? K K . '3 665' 3.977(4) ? K N1 . '3 665' 2.824(7) ? N1 C2 . . 1.363(13) ? N1 C6 . . 1.365(13) ? C2 C21 . . 1.379(12) ? C2 C3 . . 1.438(13) ? C21 Si2 . . 1.819(8) ? C21 H21 . . 1.03(5) ? Si2 C22 . . 1.874(8) ? Si2 C23 . . 1.874(8) ? Si2 C24 . . 1.885(10) ? C22 H22a . . .955(8) ? C22 H22b . . 1.011(9) ? C22 H22c . . .963(7) ? C23 H23a . . .974(9) ? C23 H23b . . .964(8) ? C23 H23c . . .967(8) ? C24 H24a . . .950(9) ? C24 H24b . . 1.000(9) ? C24 H24c . . .982(8) ? C3 C4 . . 1.339(17) ? C3 H3 . . .90(6) ? C4 C5 . . 1.40(2) ? C4 H4 . . 1.02(6) ? C5 C6 . . 1.357(16) ? C5 H5 . . .99(8) ? C6 H6 . . 1.02(6) ? N01 C011 . . 1.409(16) ? N01 C012 . . 1.460(16) ? N01 C03 . . 1.41(2) ? C011 H011a . . .938(12) ? C011 H011b . . .987(12) ? C011 H011c . . .980(12) ? C012 H012a . . .991(14) ? C012 H012b . . .944(15) ? C012 H012c . . .908(14) ? C02 C03 . . 1.25(2) ? C02 N04 . . 1.455(18) ? C02 H02a . . .974(15) ? C02 H02b . . .988(17) ? C03 H03a . . .957(16) ? C03 H03b . . 1.00(2) ? N04 C041 . . 1.441(13) ? N04 C05 . . 1.403(16) ? C041 H041a . . .961(9) ? C041 H041b . . .977(10) ? C041 H041c . . .994(11) ? C05 C06 . . 1.407(17) ? C05 H05a . . .950(12) ? C05 H05b . . 1.048(14) ? C06 N07 . . 1.443(15) ? C06 H06a . . .997(11) ? C06 H06b . . .969(12) ? N07 C071 . . 1.392(14) ? N07 C072 . . 1.434(13) ? C071 H071a . . .979(12) ? C071 H071b . . .937(11) ? C071 H071c . . .970(11) ? C072 H072a . . .955(10) ? C072 H072b . . .965(11) ? C072 H072c . . .972(10) ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N1 K N01 . . . 104.2(3) ? N1 K N04 . . . 106.3(2) ? N1 K N07 . . . 139.7(2) ? N1 K H21 . . . 51.4(10) ? N1 K K . . '3 665' 45.22(13) ? N1 K N1 . . '3 665' 90.77(19) ? N01 K N04 . . . 60.7(3) ? N01 K N07 . . . 101.9(3) ? N01 K H21 . . . 154.1(10) ? N01 K K . . '3 665' 123.2(2) ? N01 K N1 . . '3 665' 121.7(3) ? N04 K N07 . . . 62.0(2) ? N04 K H21 . . . 113.3(10) ? N04 K K . . '3 665' 151.08(18) ? N04 K N1 . . '3 665' 161.8(2) ? N07 K H21 . . . 95.6(10) ? N07 K K . . '3 665' 132.81(17) ? N07 K N1 . . '3 665' 100.9(2) ? H21 K K . . '3 665' 48.8(11) ? H21 K N1 . . '3 665' 72.6(10) ? K K N1 '3 665' . '3 665' 45.55(14) ? K N1 C2 . . . 95.6(5) ? K N1 C6 . . . 118.9(6) ? K N1 K . . '3 665' 89.23(17) ? C2 N1 C6 . . . 118.5(7) ? C2 N1 K . . '3 665' 111.0(5) ? C6 N1 K . . '3 665' 118.0(7) ? N1 C2 C21 . . . 122.7(7) ? N1 C2 C3 . . . 116.8(8) ? C21 C2 C3 . . . 120.4(9) ? C2 C21 Si2 . . . 130.4(7) ? C2 C21 H21 . . . 109(3) ? Si2 C21 H21 . . . 121(3) ? C21 Si2 C22 . . . 114.1(4) ? C21 Si2 C23 . . . 109.2(4) ? C21 Si2 C24 . . . 114.2(4) ? C22 Si2 C23 . . . 106.9(4) ? C22 Si2 C24 . . . 105.7(4) ? C23 Si2 C24 . . . 106.2(4) ? Si2 C22 H22a . . . 114.6(6) ? Si2 C22 H22b . . . 111.4(6) ? Si2 C22 H22c . . . 114.1(7) ? H22a C22 H22b . . . 104.2(8) ? H22a C22 H22c . . . 107.9(7) ? H22b C22 H22c . . . 103.6(7) ? Si2 C23 H23a . . . 111.9(6) ? Si2 C23 H23b . . . 112.5(6) ? Si2 C23 H23c . . . 112.5(6) ? H23a C23 H23b . . . 106.4(8) ? H23a C23 H23c . . . 106.1(7) ? H23b C23 H23c . . . 107.0(8) ? Si2 C24 H24a . . . 115.1(7) ? Si2 C24 H24b . . . 112.4(6) ? Si2 C24 H24c . . . 113.2(7) ? H24a C24 H24b . . . 105.4(9) ? H24a C24 H24c . . . 106.8(8) ? H24b C24 H24c . . . 103.0(8) ? C2 C3 C4 . . . 122.9(11) ? C2 C3 H3 . . . 121(4) ? C4 C3 H3 . . . 114(4) ? C3 C4 C5 . . . 119.5(10) ? C3 C4 H4 . . . 121(4) ? C5 C4 H4 . . . 119(4) ? C4 C5 C6 . . . 116.6(11) ? C4 C5 H5 . . . 122(5) ? C6 C5 H5 . . . 121(5) ? N1 C6 C5 . . . 125.6(10) ? N1 C6 H6 . . . 114(3) ? C5 C6 H6 . . . 120(3) ? K N01 C011 . . . 105.8(7) ? K N01 C012 . . . 108.8(7) ? K N01 C03 . . . 113.7(8) ? C011 N01 C012 . . . 105.3(9) ? C011 N01 C03 . . . 111.3(10) ? C012 N01 C03 . . . 111.5(12) ? N01 C011 H011a . . . 115.1(12) ? N01 C011 H011b . . . 111.4(10) ? N01 C011 H011c . . . 110.3(10) ? H011a C011 H011b . . . 107.4(11) ? H011a C011 H011c . . . 107.9(12) ? H011b C011 H011c . . . 104.2(12) ? N01 C012 H012a . . . 105.7(12) ? N01 C012 H012b . . . 110.2(11) ? N01 C012 H012c . . . 110.6(13) ? H012a C012 H012b . . . 106.6(14) ? H012a C012 H012c . . . 109.5(13) ? H012b C012 H012c . . . 113.8(15) ? C03 C02 N04 . . . 123.4(12) ? C03 C02 H02a . . . 107.7(16) ? C03 C02 H02b . . . 111.1(18) ? N04 C02 H02a . . . 105.0(14) ? N04 C02 H02b . . . 103.6(13) ? H02a C02 H02b . . . 104.5(12) ? N01 C03 C02 . . . 125.5(16) ? N01 C03 H03a . . . 112.0(15) ? N01 C03 H03b . . . 107.5(14) ? C02 C03 H03a . . . 103.9(15) ? C02 C03 H03b . . . 100.9(17) ? H03a C03 H03b . . . 104.8(18) ? K N04 C02 . . . 113.1(7) ? K N04 C041 . . . 97.4(6) ? K N04 C05 . . . 113.8(6) ? C02 N04 C041 . . . 110.2(8) ? C02 N04 C05 . . . 111.2(11) ? C041 N04 C05 . . . 110.3(9) ? N04 C041 H041a . . . 115.2(10) ? N04 C041 H041b . . . 114.3(8) ? N04 C041 H041c . . . 111.2(9) ? H041a C041 H041b . . . 106.3(9) ? H041a C041 H041c . . . 105.0(8) ? H041b C041 H041c . . . 103.8(10) ? N04 C05 C06 . . . 122.3(11) ? N04 C05 H05a . . . 111.1(10) ? N04 C05 H05b . . . 102.0(13) ? C06 C05 H05a . . . 113.3(14) ? C06 C05 H05b . . . 103.0(9) ? H05a C05 H05b . . . 101.8(11) ? C05 C06 N07 . . . 118.5(10) ? C05 C06 H06a . . . 101.6(10) ? C05 C06 H06b . . . 109.2(12) ? N07 C06 H06a . . . 109.0(11) ? N07 C06 H06b . . . 112.8(10) ? H06a C06 H06b . . . 104.2(9) ? K N07 C06 . . . 112.1(6) ? K N07 C071 . . . 104.0(6) ? K N07 C072 . . . 110.7(6) ? C06 N07 C071 . . . 109.2(9) ? C06 N07 C072 . . . 110.6(8) ? C071 N07 C072 . . . 110.1(8) ? N07 C071 H071a . . . 110.4(9) ? N07 C071 H071b . . . 112.5(10) ? N07 C071 H071c . . . 111.2(12) ? H071a C071 H071b . . . 108.1(13) ? H071a C071 H071c . . . 105.5(10) ? H071b C071 H071c . . . 108.9(10) ? N07 C072 H072a . . . 112.7(10) ? N07 C072 H072b . . . 112.6(9) ? N07 C072 H072c . . . 109.7(8) ? H072a C072 H072b . . . 107.8(9) ? H072a C072 H072c . . . 107.2(10) ? H072b C072 H072c . . . 106.4(11) ? K H21 C21 . . . 110(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag K C2 3.548(10) . '3 665' ? K C2 3.268(9) . . ? K C21 3.328(9) . . ? K C21 3.639(9) . '3 665' ? K C6 3.697(11) . . ? K C6 3.667(13) . '3 665' ? K C011 3.546(12) . . ? K C012 3.638(15) . . ? K C02 3.698(15) . . ? K C03 3.695(18) . . ? K C041 3.378(10) . . ? K C05 3.673(14) . . ? K C06 3.704(12) . . ? K C071 3.517(13) . . ? K C072 3.671(10) . . ? K H21 3.00(5) . '3 665' ? K H6 3.59(5) . '3 665' ? K H011b 3.550(3) . . ? K H011c 3.474(2) . . ? K H012a 3.688(2) . . ? K H012c 3.547(2) . . ? K H041b 3.402(3) . . ? K H041c 3.248(4) . . ? K H071b 3.529(2) . . ? K H071c 3.500(2) . . ? K H072b 3.715(2) . . ? K H072c 3.663(2) . . ? N1 C21 2.407(11) . . ? N1 C3 2.387(13) . . ? N1 C4 2.781(12) . . ? N1 C5 2.422(13) . . ? N1 H21 2.46(5) . . ? N1 H6 2.01(6) . . ? C2 Si2 2.908(11) . . ? C2 C4 2.439(13) . . ? C2 C5 2.808(16) . . ? C2 C6 2.344(14) . . ? C2 H21 1.97(5) . . ? C2 H3 2.05(6) . . ? C21 C3 2.445(14) . . ? C21 H3 2.65(5) . . ? Si2 H21 2.51(5) . . ? Si2 H22a 2.432(3) . . ? Si2 H22b 2.432(3) . . ? Si2 H22c 2.432(3) . . ? Si2 H23a 2.413(4) . . ? Si2 H23b 2.412(3) . . ? Si2 H23c 2.415(2) . . ? Si2 H24a 2.444(4) . . ? Si2 H24b 2.447(3) . . ? Si2 H24c 2.444(3) . . ? C22 C24 2.997(14) . . ? C3 C5 2.364(19) . . ? C3 C6 2.665(15) . . ? C3 H4 2.06(6) . . ? C4 C6 2.343(16) . . ? C4 H3 1.89(6) . . ? C4 H5 2.09(8) . . ? C5 H4 2.09(6) . . ? C5 H6 2.07(6) . . ? C6 H5 2.05(7) . . ? N01 C02 2.371(18) . . ? N01 N04 2.915(12) . . ? N01 H011a 1.997(9) . . ? N01 H011b 1.993(10) . . ? N01 H011c 1.976(10) . . ? N01 H012a 1.975(10) . . ? N01 H012b 1.993(9) . . ? N01 H012c 1.972(9) . . ? N01 H03a 1.980(10) . . ? N01 H03b 1.961(10) . . ? C011 C012 2.281(18) . . ? C011 C03 2.33(2) . . ? C011 H012b 2.492(13) . . ? C011 H012c 2.480(11) . . ? C011 H03a 2.351(13) . . ? C012 C03 2.37(2) . . ? C012 H011a 2.527(13) . . ? C012 H011c 2.470(14) . . ? C012 H03b 2.308(14) . . ? C02 C041 2.37(2) . . ? C02 C05 2.36(2) . . ? C02 H03a 1.751(17) . . ? C02 H03b 1.746(17) . . ? C02 H041a 2.603(17) . . ? C02 H041c 2.634(17) . . ? C02 H05a 2.610(17) . . ? C02 H05b 2.330(16) . . ? C03 N04 2.387(18) . . ? C03 H011a 2.585(18) . . ? C03 H011b 2.59(2) . . ? C03 H012a 2.517(17) . . ? C03 H012b 2.560(16) . . ? C03 H02a 1.807(17) . . ? C03 H02b 1.854(17) . . ? N04 C06 2.461(13) . . ? N04 N07 2.982(11) . . ? N04 H02a 1.948(7) . . ? N04 H02b 1.941(8) . . ? N04 H041a 2.044(8) . . ? N04 H041b 2.048(9) . . ? N04 H041c 2.025(9) . . ? N04 H05a 1.957(9) . . ? N04 H05b 1.918(9) . . ? C041 C05 2.334(16) . . ? C041 H02a 2.244(10) . . ? C041 H05a 2.516(11) . . ? C05 N07 2.449(14) . . ? C05 H02b 2.252(14) . . ? C05 H041a 2.667(11) . . ? C05 H041b 2.572(13) . . ? C05 H06a 1.881(15) . . ? C05 H06b 1.953(13) . . ? C06 C071 2.310(16) . . ? C06 C072 2.365(17) . . ? C06 H05a 1.985(13) . . ? C06 H05b 1.934(12) . . ? C06 H071a 2.536(11) . . ? C06 H071b 2.509(10) . . ? C06 H072a 2.550(12) . . ? C06 H072c 2.613(13) . . ? N07 H05b 2.690(9) . . ? N07 H06a 2.003(8) . . ? N07 H06b 2.026(8) . . ? N07 H071a 1.960(7) . . ? N07 H071b 1.953(8) . . ? N07 H071c 1.963(7) . . ? N07 H072a 2.007(8) . . ? N07 H072b 2.013(8) . . ? N07 H072c 1.985(8) . . ? C071 C072 2.316(16) . . ? C071 H06b 2.472(11) . . ? C071 H072a 2.611(11) . . ? C071 H072b 2.522(12) . . ? C072 H06a 2.439(11) . . ? C072 H071a 2.513(11) . . ? C072 H071c 2.519(10) . . ? H22a H22b 1.5513(10) . . ? H22a H22c 1.5513(7) . . ? H22b H22c 1.551(2) . . ? H23a H23b 1.5515(9) . . ? H23a H23c 1.5513(9) . . ? H23b H23c 1.5515(5) . . ? H23c H072c 2.1894(7) . . ? H24a H24b 1.5514(5) . . ? H24a H24c 1.5514(7) . . ? H24b H24c 1.5513(6) . . ? H24b H041b 2.3537(12) . . ? H3 H4 2.24(8) . . ? H5 H6 2.39(9) . . ? H011a H011b 1.5514(6) . . ? H011a H011c 1.5514(18) . . ? H011a H012b 2.3743(7) . . ? H011a H03a 2.2973(12) . . ? H011b H011c 1.5513(13) . . ? H011c H012c 2.2963(7) . . ? H012a H012b 1.5514(7) . . ? H012a H012c 1.5514(6) . . ? H012a H03b 2.133(2) . . ? H012b H012c 1.5513(17) . . ? H012b H03b 2.3659(13) . . ? H02a H02b 1.5513(4) . . ? H02a H03a 1.8517(9) . . ? H02a H041a 2.2554(12) . . ? H02a H041c 2.2750(10) . . ? H02b H03a 2.2034(10) . . ? H02b H03b 1.8514(9) . . ? H02b H05a 2.2162(11) . . ? H02b H05b 2.0450(15) . . ? H03a H03b 1.5514(5) . . ? H041a H041b 1.5514(19) . . ? H041a H041c 1.5514(10) . . ? H041b H041c 1.5513(7) . . ? H05a H05b 1.5512(8) . . ? H05a H06a 2.194(2) . . ? H05a H06b 2.2294(19) . . ? H05b H06b 2.1894(11) . . ? H05b H071b 2.282(3) . . ? H06a H06b 1.5514(4) . . ? H06a H072c 2.318(3) . . ? H06b H071a 2.3161(19) . . ? H071a H071b 1.5513(7) . . ? H071a H071c 1.5513(8) . . ? H071b H071c 1.551(2) . . ? H071c H072b 2.3398(9) . . ? H072a H072b 1.5513(9) . . ? H072a H072c 1.5514(4) . . ? H072b H072c 1.5513(10) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 824 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 7 4 -3 -7 -4 3 -7 4 -3 7 -4 4 9 5 4 -9 5 -4 -9 -5 -4 9 -5 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -13 _reflns_limit_l_max 13 _reflns_number_observed ? _reflns_d_resolution_high .911 _reflns_d_resolution_low 10.163 _diffrn_reflns_av_sigmaI/netI .069 _diffrn_reflns_theta_min 2. _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atom-block _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .152 _refine_ls_wR_factor_all .054 _refine_ls_goodness_of_fit_all 1.324 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_pca23m _database_code_CSD 154202 _audit_creation_method Xtal3.6 _audit_creation_date 00-05-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30 H64 Mg1 N8 O2 P2 Si2' _chemical_formula_moiety ? _chemical_formula_weight 711.32 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 13.489(4) _cell_length_b 19.258(5) _cell_length_c 17.536(4) _cell_angle_alpha 90.00000 _cell_angle_beta 108.74(2) _cell_angle_gamma 90.00000 _cell_volume 4314(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 9.8 _cell_measurement_theta_max 14.7 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .205 _exptl_crystal_description needle _exptl_crystal_size_max .65 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .90 _exptl_absorpt_correction_T_max .96 _diffrn_reflns_number 15731 _reflns_number_total 7628 _reflns_Friedel_coverage ? _reflns_number_gt 2075 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 10 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .053 _refine_ls_wR_factor_ref .057 _refine_ls_goodness_of_fit_ref 1.54 _refine_ls_number_reflns 2075 _refine_ls_number_parameters 434 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .059 _refine_diff_density_min -.20 _refine_diff_density_max .21 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 120 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 8 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Mg ? 0 4 .041992 .036011 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 8 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .090027 .094971 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 256 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mg .81543(18) .89160(12) .61225(14) .0653(15) Uani ? ? 1.00000 ? ? O1 .8507(3) .9808(2) .5759(3) .072(3) Uani ? ? 1.00000 ? ? P1 .83966(16) 1.05532(11) .55529(13) .0782(14) Uani ? ? 1.00000 ? ? N11 .8121(5) 1.0659(3) .4587(4) .097(4) Uani ? ? 1.00000 ? ? C111 .8705(7) 1.0269(6) .4160(5) .144(8) Uani ? ? 1.00000 ? ? C112 .7529(8) 1.1235(6) .4145(6) .165(9) Uani ? ? 1.00000 ? ? N12 .7448(4) 1.0892(3) .5808(4) .086(4) Uani ? ? 1.00000 ? ? C121 .7476(8) 1.1591(5) .6114(7) .151(8) Uani ? ? 1.00000 ? ? C122 .6442(6) 1.0554(4) .5612(5) .105(6) Uani ? ? 1.00000 ? ? N13 .9469(5) 1.0971(3) .6007(4) .106(5) Uani ? ? 1.00000 ? ? C131 .9971(7) 1.0877(5) .6856(5) .127(7) Uani ? ? 1.00000 ? ? C132 .9886(8) 1.1523(6) .5646(7) .186(10) Uani ? ? 1.00000 ? ? O2 .7664(3) .9128(2) .7010(2) .078(3) Uani ? ? 1.00000 ? ? P2 .72766(18) .91226(11) .77059(12) .0785(14) Uani ? ? 1.00000 ? ? N21 .6055(6) .9104(6) .7423(4) .184(8) Uani ? ? 1.00000 ? ? C211 .5362(7) .9022(6) .6678(6) .155(9) Uani ? ? 1.00000 ? ? C212 .544(2) .8451(16) .7788(15) .23(3) Uani ? ? .50000 ? ? N22 .7674(10) .9795(4) .8240(5) .228(10) Uani ? ? 1.00000 ? ? C221 .8057(10) 1.0374(6) .8136(8) .195(11) Uani ? ? 1.00000 ? ? C222 .639(2) 1.0135(14) .8352(15) .22(2) Uani ? ? .50000 ? ? N23 .7672(6) .8490(4) .8292(4) .128(6) Uani ? ? 1.00000 ? ? C231 .8384(9) .8006(5) .8266(6) .158(9) Uani ? ? 1.00000 ? ? C232 .815(3) .8700(17) .9235(12) .28(3) Uani ? ? .50000 ? ? N31 .9400(4) .8239(3) .6413(3) .071(4) Uani ? ? 1.00000 ? ? C32 1.0324(5) .8347(3) .7068(4) .067(5) Uani ? ? 1.00000 ? ? C321 1.0431(6) .8903(4) .7562(5) .085(5) Uani ? ? 1.00000 ? ? Si3 1.1527(2) .91128(14) .84559(15) .1054(18) Uani ? ? 1.00000 ? ? C322 1.1688(9) .8491(6) .9312(5) .155(8) Uani ? ? 1.00000 ? ? C323 1.2825(7) .9190(7) .8298(6) .174(10) Uani ? ? 1.00000 ? ? C324 1.1253(9) .9979(5) .8833(6) .157(9) Uani ? ? 1.00000 ? ? C33 1.1105(6) .7826(4) .7150(5) .098(6) Uani ? ? 1.00000 ? ? C34 1.0966(7) .7277(4) .6661(5) .111(6) Uani ? ? 1.00000 ? ? C35 1.0029(7) .7178(4) .6027(5) .105(6) Uani ? ? 1.00000 ? ? C36 .9295(6) .7681(4) .5945(4) .083(5) Uani ? ? 1.00000 ? ? N41 .6952(4) .8550(3) .5143(3) .071(4) Uani ? ? 1.00000 ? ? C42 .6343(5) .7970(4) .5159(4) .071(5) Uani ? ? 1.00000 ? ? Si4 .5982(2) .67586(13) .60083(16) .0976(18) Uani ? ? 1.00000 ? ? C421 .6595(6) .7558(4) .5829(4) .083(5) Uani ? ? 1.00000 ? ? C422 .4667(8) .6899(6) .6120(8) .175(10) Uani ? ? 1.00000 ? ? C423 .6846(8) .6361(5) .6957(5) .132(7) Uani ? ? 1.00000 ? ? C424 .5797(8) .6084(5) .5201(6) .143(8) Uani ? ? 1.00000 ? ? C43 .5454(6) .7821(4) .4455(4) .088(5) Uani ? ? 1.00000 ? ? C44 .5278(6) .8215(4) .3801(4) .101(6) Uani ? ? 1.00000 ? ? C45 .5924(6) .8787(4) .3775(4) .096(6) Uani ? ? 1.00000 ? ? C46 .6726(6) .8924(4) .4464(4) .087(5) Uani ? ? 1.00000 ? ? C212' .5580(14) .9624(12) .7958(11) .151(17) Uani ? ? .50000 ? ? C222' .834(2) .9686(11) .9194(10) .170(18) Uani ? ? .50000 ? ? C232' .6961(15) .8015(10) .8558(11) .138(15) Uani ? ? .50000 ? ? H111a .81693 1.00607 .36898 .20000 Uiso ? ? 1.00000 ? ? H111b .90239 .98912 .45013 .20000 Uiso ? ? 1.00000 ? ? H111c .91576 1.05419 .39497 .20000 Uiso ? ? 1.00000 ? ? H112a .71307 1.14435 .44469 .22000 Uiso ? ? 1.00000 ? ? H112b .79995 1.15972 .40670 .22000 Uiso ? ? 1.00000 ? ? H112c .70475 1.11127 .36191 .22000 Uiso ? ? 1.00000 ? ? H121a .72797 1.15993 .66120 .21000 Uiso ? ? 1.00000 ? ? H121b .69716 1.18899 .57419 .21000 Uiso ? ? 1.00000 ? ? H121c .82452 1.17817 .62395 .21000 Uiso ? ? 1.00000 ? ? H122a .64568 1.00789 .54258 .15000 Uiso ? ? 1.00000 ? ? H122b .61700 1.05207 .60646 .15000 Uiso ? ? 1.00000 ? ? H122c .59148 1.07800 .51871 .15000 Uiso ? ? 1.00000 ? ? H131a 1.06280 1.05905 .70031 .18600 Uiso ? ? 1.00000 ? ? H131b .95515 1.06238 .71449 .18600 Uiso ? ? 1.00000 ? ? H131c 1.02023 1.12942 .71847 .18600 Uiso ? ? 1.00000 ? ? H132a 1.05518 1.14574 .55412 .25000 Uiso ? ? 1.00000 ? ? H132b .98846 1.20034 .58086 .25000 Uiso ? ? 1.00000 ? ? H132c .95045 1.15320 .50679 .25000 Uiso ? ? 1.00000 ? ? H211a .54776 .93981 .63212 .22000 Uiso ? ? 1.00000 ? ? H211b .55256 .85970 .64181 .22000 Uiso ? ? 1.00000 ? ? H211c .45733 .89978 .64212 .22000 Uiso ? ? 1.00000 ? ? H212a .56829 .80315 .76854 .32000 Uiso ? ? .50000 ? ? H212b .56515 .85420 .83616 .32000 Uiso ? ? .50000 ? ? H212c .46902 .84492 .76119 .32000 Uiso ? ? .50000 ? ? H221a .86560 1.02701 .79477 .25000 Uiso ? ? 1.00000 ? ? H221b .75358 1.05808 .76546 .25000 Uiso ? ? 1.00000 ? ? H221c .83223 1.08090 .84236 .25000 Uiso ? ? 1.00000 ? ? H222a .58557 1.02060 .78335 .27000 Uiso ? ? .50000 ? ? H222b .60745 .97672 .86121 .27000 Uiso ? ? .50000 ? ? H222c .66042 1.05048 .86567 .27000 Uiso ? ? .50000 ? ? H231a .81809 .77911 .77506 .22000 Uiso ? ? 1.00000 ? ? H231b .90501 .82566 .83124 .22000 Uiso ? ? 1.00000 ? ? H231c .86919 .76069 .86235 .22000 Uiso ? ? 1.00000 ? ? H232a .86798 .90714 .93255 .36000 Uiso ? ? .50000 ? ? H232b .75696 .89662 .93905 .36000 Uiso ? ? .50000 ? ? H232c .83759 .83649 .96119 .36000 Uiso ? ? .50000 ? ? H321 .98532 .92418 .74373 .10500 Uiso ? ? 1.00000 ? ? H322a 1.22840 .85801 .97531 .22000 Uiso ? ? 1.00000 ? ? H322b 1.17325 .80131 .91336 .22000 Uiso ? ? 1.00000 ? ? H322c 1.10769 .84983 .94918 .22000 Uiso ? ? 1.00000 ? ? H323a 1.33738 .92995 .87688 .27000 Uiso ? ? 1.00000 ? ? H323b 1.28123 .95371 .78902 .27000 Uiso ? ? 1.00000 ? ? H323c 1.30104 .87535 .80848 .27000 Uiso ? ? 1.00000 ? ? H324a 1.18246 1.01175 .93079 .21000 Uiso ? ? 1.00000 ? ? H324b 1.06333 .99617 .89947 .21000 Uiso ? ? 1.00000 ? ? H324c 1.11623 1.03329 .84414 .21000 Uiso ? ? 1.00000 ? ? H33 1.17915 .78736 .75985 .12400 Uiso ? ? 1.00000 ? ? H34 1.15598 .69390 .67418 .13400 Uiso ? ? 1.00000 ? ? H35 .99042 .67499 .56875 .13500 Uiso ? ? 1.00000 ? ? H36 .86344 .76295 .54784 .11000 Uiso ? ? 1.00000 ? ? H421 .72190 .76964 .62909 .10500 Uiso ? ? 1.00000 ? ? H422a .43474 .64834 .62018 .24000 Uiso ? ? 1.00000 ? ? H422b .42084 .71505 .56820 .24000 Uiso ? ? 1.00000 ? ? H422c .47409 .71919 .66074 .24000 Uiso ? ? 1.00000 ? ? H423a .70060 .66725 .74133 .18000 Uiso ? ? 1.00000 ? ? H423b .75475 .62406 .69130 .18000 Uiso ? ? 1.00000 ? ? H423c .65853 .59406 .71028 .18000 Uiso ? ? 1.00000 ? ? H424a .55094 .56570 .53267 .21000 Uiso ? ? 1.00000 ? ? H424b .64822 .59480 .51449 .21000 Uiso ? ? 1.00000 ? ? H424c .53767 .62349 .46852 .21000 Uiso ? ? 1.00000 ? ? H43 .50019 .74267 .44622 .11200 Uiso ? ? 1.00000 ? ? H44 .46768 .81041 .33160 .13800 Uiso ? ? 1.00000 ? ? H45 .57927 .90791 .32877 .12500 Uiso ? ? 1.00000 ? ? H46 .71697 .93314 .44453 .12500 Uiso ? ? 1.00000 ? ? H212'a .58277 .94991 .85208 .18000 Uiso ? ? .50000 ? ? H212'b .57923 1.00995 .79227 .18000 Uiso ? ? .50000 ? ? H212'c .48237 .96197 .77889 .18000 Uiso ? ? .50000 ? ? H222'a .79003 .94096 .94238 .24000 Uiso ? ? .50000 ? ? H222'b .89338 .93734 .92162 .24000 Uiso ? ? .50000 ? ? H222'c .85956 1.00587 .95126 .24000 Uiso ? ? .50000 ? ? H232'a .65866 .82985 .87998 .20000 Uiso ? ? .50000 ? ? H232'b .64866 .78248 .80633 .20000 Uiso ? ? .50000 ? ? H232'c .72074 .76261 .88970 .20000 Uiso ? ? .50000 ? ? 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 Mg .0701(18) .0652(17) .0626(16) -.0024(15) .0240(14) .0014(14) O1 .067(3) .066(3) .088(4) -.003(3) .030(3) .017(3) P1 .0669(15) .0755(15) .0960(17) .0001(14) .0315(13) .0183(14) N11 .072(4) .120(6) .099(5) .013(4) .028(4) .052(4) C111 .115(8) .232(12) .112(8) .030(8) .074(7) .048(8) C112 .118(8) .212(12) .166(10) .051(8) .045(8) .112(9) N12 .077(4) .064(4) .121(5) .004(4) .040(4) -.004(4) C121 .126(9) .095(8) .236(12) .006(6) .064(8) -.038(8) C122 .079(6) .112(7) .141(7) -.018(6) .057(6) -.020(6) N13 .068(5) .096(5) .144(6) -.023(4) .017(4) .030(5) C131 .119(8) .127(8) .121(8) -.015(7) .017(6) -.014(7) C132 .138(10) .140(10) .258(13) -.062(8) .033(9) .085(9) O2 .091(4) .090(4) .063(3) -.010(3) .040(3) -.007(3) P2 .0996(18) .0762(16) .0660(14) .0009(14) .0353(13) .0005(13) N21 .093(6) .374(14) .102(6) .071(8) .057(5) .070(8) C211 .083(7) .215(12) .172(10) -.030(8) .046(7) -.018(9) C212 .20(3) .29(4) .21(3) -.10(2) .10(2) .01(2) N22 .484(18) .110(7) .179(8) -.123(9) .229(11) -.081(6) C221 .249(14) .113(10) .249(13) -.072(9) .115(11) -.087(9) C222 .25(3) .22(3) .20(3) .09(2) .10(2) -.04(2) N23 .138(7) .139(7) .125(6) .059(5) .068(5) .079(5) C231 .237(13) .104(8) .124(8) .035(8) .046(8) .047(7) C232 .39(4) .33(4) .067(15) .19(3) .01(2) .03(2) N31 .079(4) .061(4) .075(4) .002(3) .027(3) -.002(3) C32 .063(5) .064(5) .073(5) .003(4) .020(4) .021(4) C321 .081(6) .069(6) .095(6) -.005(5) .015(5) -.023(5) Si3 .097(2) .111(2) .0913(19) -.0076(18) .0073(16) -.0010(17) C322 .193(11) .145(10) .093(7) -.006(8) -.001(7) .032(7) C323 .081(7) .291(16) .135(9) -.033(9) .014(6) -.038(9) C324 .182(11) .126(9) .130(9) -.012(8) .002(8) -.046(7) C33 .099(7) .081(6) .102(7) .019(5) .015(5) .013(5) C34 .115(7) .069(6) .145(8) .025(5) .038(6) .013(6) C35 .124(8) .067(6) .112(7) .011(5) .018(6) -.009(5) C36 .103(6) .068(6) .085(6) .010(5) .040(5) .002(5) N41 .078(4) .087(5) .053(4) -.001(4) .028(3) .005(3) C42 .070(5) .081(6) .068(5) .004(5) .031(4) .000(4) Si4 .104(2) .088(2) .111(2) -.0194(16) .0478(17) -.0113(16) C421 .072(6) .093(6) .082(6) -.023(5) .020(5) -.009(5) C422 .131(9) .157(10) .280(14) -.007(8) .128(10) .029(10) C423 .191(10) .099(8) .105(7) -.007(7) .048(7) .013(6) C424 .180(10) .107(8) .133(8) -.038(7) .037(8) -.031(7) C43 .066(6) .102(7) .086(6) .005(5) .009(5) -.014(5) C44 .088(7) .130(8) .076(6) .036(6) .012(5) -.016(5) C45 .120(7) .109(7) .060(5) .028(6) .029(5) .004(5) C46 .104(6) .101(7) .061(5) .007(6) .032(5) -.005(5) C212' .104(15) .23(2) .139(17) .062(16) .066(14) .014(17) C222' .28(3) .16(2) .060(13) -.02(2) .038(16) -.048(13) C232' .142(17) .127(16) .155(17) -.035(14) .061(14) .076(14) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Mg O1 . . 1.943(5) ? Mg O2 . . 1.919(6) ? Mg N31 . . 2.057(6) ? Mg N41 . . 2.071(5) ? O1 P1 . . 1.476(5) ? P1 N11 . . 1.625(7) ? P1 N12 . . 1.621(7) ? P1 N13 . . 1.623(6) ? N11 C111 . . 1.457(13) ? N11 C112 . . 1.440(12) ? C111 H111a . . .990(8) ? C111 H111b . . .952(10) ? C111 H111c . . .964(11) ? C112 H112a . . .955(12) ? C112 H112b . . .982(12) ? C112 H112c . . .971(9) ? N12 C121 . . 1.447(11) ? N12 C122 . . 1.443(10) ? C121 H121a . . .991(13) ? C121 H121b . . .967(9) ? C121 H121c . . 1.055(10) ? C122 H122a . . .974(9) ? C122 H122b . . .978(10) ? C122 H122c . . .954(7) ? N13 C131 . . 1.435(11) ? N13 C132 . . 1.441(14) ? C131 H131a . . 1.005(9) ? C131 H131b . . 1.000(11) ? C131 H131c . . .980(9) ? C132 H132a . . .980(12) ? C132 H132b . . .968(11) ? C132 H132c . . .978(11) ? O2 P2 . . 1.475(6) ? P2 N21 . . 1.561(7) ? P2 N22 . . 1.588(9) ? P2 N23 . . 1.573(7) ? N21 C211 . . 1.351(11) ? N21 C212 . . 1.74(3) ? N21 C212' . . 1.64(2) ? C211 H211a . . 1.002(12) ? C211 H211b . . .995(12) ? C211 H211c . . 1.014(9) ? C212 H212a . . .91(3) ? C212 H212b . . .97(3) ? C212 H212c . . .95(3) ? N22 C221 . . 1.266(15) ? N22 C222 . . 1.92(3) ? N22 C222' . . 1.637(18) ? C221 H221a . . .987(15) ? C221 H221b . . .992(11) ? C221 H221c . . .984(11) ? C222 C212' . . 1.47(3) ? C222 H222a . . .97(2) ? C222 H222b . . 1.01(3) ? C222 H222c . . .88(3) ? C222 H212'b . . .91(2) ? N23 C231 . . 1.349(14) ? N23 C232 . . 1.62(2) ? N23 C232' . . 1.50(2) ? C231 H231a . . .950(9) ? C231 H231b . . 1.000(12) ? C231 H231c . . .995(9) ? C232 C222' . . 1.92(4) ? C232 H232a . . .99(3) ? C232 H232b . . 1.04(4) ? C232 H232c . . .90(3) ? C232 H222'a . . 1.47(3) ? N31 C32 . . 1.413(7) ? N31 C36 . . 1.333(9) ? C32 C321 . . 1.355(10) ? C32 C33 . . 1.429(11) ? C321 Si3 . . 1.821(7) ? C321 H321 . . .986(7) ? Si3 C322 . . 1.877(10) ? Si3 C323 . . 1.864(11) ? Si3 C324 . . 1.875(11) ? C322 H322a . . .935(9) ? C322 H322b . . .980(11) ? C322 H322c . . .973(13) ? C323 H323a . . .939(9) ? C323 H323b . . .976(12) ? C323 H323c . . .984(13) ? C324 H324a . . .973(9) ? C324 H324b . . .966(13) ? C324 H324c . . .946(10) ? C33 C34 . . 1.336(11) ? C33 H33 . . 1.008(7) ? C34 C35 . . 1.403(11) ? C34 H34 . . 1.006(9) ? C35 C36 . . 1.360(11) ? C35 H35 . . .998(8) ? C36 H36 . . 1.002(7) ? N41 C42 . . 1.393(9) ? N41 C46 . . 1.339(9) ? C42 C421 . . 1.366(10) ? C42 C43 . . 1.446(9) ? Si4 C421 . . 1.822(8) ? Si4 C422 . . 1.866(12) ? Si4 C423 . . 1.862(9) ? Si4 C424 . . 1.877(10) ? C421 H421 . . .999(6) ? C422 H422a . . .942(12) ? C422 H422b . . .950(11) ? C422 H422c . . 1.001(13) ? C423 H423a . . .967(9) ? C423 H423b . . 1.001(11) ? C423 H423c . . .951(10) ? C424 H424a . . .965(10) ? C424 H424b . . .995(12) ? C424 H424c . . .946(9) ? C43 C44 . . 1.332(11) ? C43 H43 . . .977(8) ? C44 C45 . . 1.414(12) ? C44 H44 . . .991(7) ? C45 C46 . . 1.363(9) ? C45 H45 . . .990(8) ? C46 H46 . . .995(8) ? C212' H222a . . 1.22(2) ? C212' H222b . . 1.159(18) ? C212' H212'a . . .96(2) ? C212' H212'b . . .97(2) ? C212' H212'c . . .967(18) ? C222' H232a . . 1.26(2) ? C222' H222'a . . .97(2) ? C222' H222'b . . 1.00(2) ? C222' H222'c . . .91(2) ? C232' H232'a . . .93(2) ? C232' H232'b . . .969(17) ? C232' H232'c . . .948(18) ? H222a H212'b . . .28713(5) ? H222b H212'a . . .60728(12) ? H232a H222'b . . .73114(13) ? H232b H222'a . . .9565(2) ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O1 Mg O2 . . . 105.2(2) ? O1 Mg N31 . . . 112.0(2) ? O1 Mg N41 . . . 103.7(2) ? O2 Mg N31 . . . 113.6(2) ? O2 Mg N41 . . . 111.3(2) ? N31 Mg N41 . . . 110.4(2) ? Mg O1 P1 . . . 157.4(4) ? O1 P1 N11 . . . 110.3(3) ? O1 P1 N12 . . . 110.5(3) ? O1 P1 N13 . . . 111.0(3) ? N11 P1 N12 . . . 107.5(3) ? N11 P1 N13 . . . 108.6(4) ? N12 P1 N13 . . . 108.8(3) ? P1 N11 C111 . . . 119.4(5) ? P1 N11 C112 . . . 124.0(6) ? C111 N11 C112 . . . 114.7(8) ? N11 C111 H111a . . . 105.4(8) ? N11 C111 H111b . . . 106.2(8) ? N11 C111 H111c . . . 115.4(10) ? H111a C111 H111b . . . 106.0(11) ? H111a C111 H111c . . . 106.5(9) ? H111b C111 H111c . . . 116.3(9) ? N11 C112 H112a . . . 109.8(10) ? N11 C112 H112b . . . 110.5(8) ? N11 C112 H112c . . . 114.3(10) ? H112a C112 H112b . . . 106.4(11) ? H112a C112 H112c . . . 107.8(9) ? H112b C112 H112c . . . 107.7(11) ? P1 N12 C121 . . . 123.2(6) ? P1 N12 C122 . . . 121.2(5) ? C121 N12 C122 . . . 114.7(7) ? N12 C121 H121a . . . 111.0(9) ? N12 C121 H121b . . . 112.0(8) ? N12 C121 H121c . . . 107.9(9) ? H121a C121 H121b . . . 104.8(10) ? H121a C121 H121c . . . 109.6(9) ? H121b C121 H121c . . . 111.5(10) ? N12 C122 H122a . . . 112.6(7) ? N12 C122 H122b . . . 113.9(7) ? N12 C122 H122c . . . 112.9(8) ? H122a C122 H122b . . . 105.3(8) ? H122a C122 H122c . . . 104.9(7) ? H122b C122 H122c . . . 106.5(8) ? P1 N13 C131 . . . 119.7(6) ? P1 N13 C132 . . . 124.3(6) ? C131 N13 C132 . . . 115.3(7) ? N13 C131 H131a . . . 114.8(9) ? N13 C131 H131b . . . 115.6(7) ? N13 C131 H131c . . . 117.5(8) ? H131a C131 H131b . . . 101.4(8) ? H131a C131 H131c . . . 102.2(7) ? H131b C131 H131c . . . 103.1(9) ? N13 C132 H132a . . . 119.8(9) ? N13 C132 H132b . . . 122.5(12) ? N13 C132 H132c . . . 108.5(9) ? H132a C132 H132b . . . 105.5(10) ? H132a C132 H132c . . . 91.0(12) ? H132b C132 H132c . . . 103.8(10) ? Mg O2 P2 . . . 167.4(3) ? O2 P2 N21 . . . 110.9(3) ? O2 P2 N22 . . . 109.9(5) ? O2 P2 N23 . . . 114.2(4) ? N21 P2 N22 . . . 109.1(6) ? N21 P2 N23 . . . 106.9(5) ? N22 P2 N23 . . . 105.5(4) ? P2 N21 C211 . . . 130.0(8) ? P2 N21 C212 . . . 118.8(10) ? P2 N21 C212' . . . 111.8(8) ? C211 N21 C212 . . . 90.3(10) ? C211 N21 C212' . . . 110.5(9) ? C212 N21 C212' . . . 84.8(13) ? N21 C211 H211a . . . 108.7(9) ? N21 C211 H211b . . . 110.7(9) ? N21 C211 H211c . . . 137.4(12) ? H211a C211 H211b . . . 101.9(11) ? H211a C211 H211c . . . 96.2(8) ? H211b C211 H211c . . . 96.6(8) ? N21 C212 H212a . . . 109(2) ? N21 C212 H212b . . . 103(2) ? N21 C212 H212c . . . 118(2) ? H212a C212 H212b . . . 111(3) ? H212a C212 H212c . . . 110(3) ? H212b C212 H212c . . . 106(3) ? P2 N22 C221 . . . 135.2(10) ? P2 N22 C222 . . . 101.2(10) ? P2 N22 C222' . . . 117.9(9) ? C221 N22 C222 . . . 97.9(12) ? C221 N22 C222' . . . 98.4(11) ? C222 N22 C222' . . . 98.8(13) ? N22 C221 H221a . . . 106.5(11) ? N22 C221 H221b . . . 105.4(10) ? N22 C221 H221c . . . 140.7(14) ? H221a C221 H221b . . . 103.3(13) ? H221a C221 H221c . . . 98.2(11) ? H221b C221 H221c . . . 97.9(9) ? N22 C222 C212' . . . 106.4(18) ? N22 C222 H222a . . . 112(2) ? N22 C222 H222b . . . 109(2) ? N22 C222 H222c . . . 102(2) ? N22 C222 H212'b . . . 119(2) ? C212' C222 H222a . . . 55.8(15) ? C212' C222 H222b . . . 51.9(14) ? C212' C222 H222c . . . 151(3) ? C212' C222 H212'b . . . 40.0(14) ? H222a C222 H222b . . . 103(2) ? H222a C222 H222c . . . 117(3) ? H222a C222 H212'b . . . 17.1(4) ? H222b C222 H222c . . . 113(3) ? H222b C222 H212'b . . . 86(2) ? H222c C222 H212'b . . . 126(3) ? P2 N23 C231 . . . 127.5(8) ? P2 N23 C232 . . . 114.4(12) ? P2 N23 C232' . . . 123.9(8) ? C231 N23 C232 . . . 98.8(13) ? C231 N23 C232' . . . 97.1(10) ? C232 N23 C232' . . . 85.4(14) ? N23 C231 H231a . . . 110.0(9) ? N23 C231 H231b . . . 107.2(9) ? N23 C231 H231c . . . 132.0(12) ? H231a C231 H231b . . . 105.3(12) ? H231a C231 H231c . . . 101.4(9) ? H231b C231 H231c . . . 97.9(9) ? N23 C232 C222' . . . 102.9(14) ? N23 C232 H232a . . . 112(2) ? N23 C232 H232b . . . 108(2) ? N23 C232 H232c . . . 120(3) ? N23 C232 H222'a . . . 114.7(16) ? C222' C232 H232a . . . 36.1(14) ? C222' C232 H232b . . . 69.1(19) ? C222' C232 H232c . . . 136(2) ? C222' C232 H222'a . . . 29.8(10) ? H232a C232 H232b . . . 100(3) ? H232a C232 H232c . . . 110(3) ? H232a C232 H222'a . . . 59.8(16) ? H232b C232 H232c . . . 105(3) ? H232b C232 H222'a . . . 40.4(11) ? H232c C232 H222'a . . . 123(2) ? Mg N31 C32 . . . 123.1(4) ? Mg N31 C36 . . . 116.2(4) ? C32 N31 C36 . . . 120.7(6) ? N31 C32 C321 . . . 121.4(6) ? N31 C32 C33 . . . 114.1(6) ? C321 C32 C33 . . . 124.5(6) ? C32 C321 Si3 . . . 128.0(5) ? C32 C321 H321 . . . 117.8(6) ? Si3 C321 H321 . . . 114.2(6) ? C321 Si3 C322 . . . 113.6(4) ? C321 Si3 C323 . . . 115.5(4) ? C321 Si3 C324 . . . 107.7(4) ? C322 Si3 C323 . . . 107.2(5) ? C322 Si3 C324 . . . 105.8(5) ? C323 Si3 C324 . . . 106.4(6) ? Si3 C322 H322a . . . 113.1(9) ? Si3 C322 H322b . . . 110.3(8) ? Si3 C322 H322c . . . 110.9(8) ? H322a C322 H322b . . . 108.2(10) ? H322a C322 H322c . . . 108.8(10) ? H322b C322 H322c . . . 105.2(11) ? Si3 C323 H323a . . . 113.6(9) ? Si3 C323 H323b . . . 111.6(7) ? Si3 C323 H323c . . . 110.8(9) ? H323a C323 H323b . . . 108.2(12) ? H323a C323 H323c . . . 107.5(10) ? H323b C323 H323c . . . 104.7(10) ? Si3 C324 H324a . . . 110.7(8) ? Si3 C324 H324b . . . 111.1(8) ? Si3 C324 H324c . . . 112.3(9) ? H324a C324 H324b . . . 106.3(11) ? H324a C324 H324c . . . 107.8(10) ? H324b C324 H324c . . . 108.5(10) ? C32 C33 C34 . . . 123.0(7) ? C32 C33 H33 . . . 118.5(7) ? C34 C33 H33 . . . 118.5(8) ? C33 C34 C35 . . . 121.4(8) ? C33 C34 H34 . . . 118.7(7) ? C35 C34 H34 . . . 119.8(8) ? C34 C35 C36 . . . 115.3(7) ? C34 C35 H35 . . . 121.4(8) ? C36 C35 H35 . . . 123.2(7) ? N31 C36 C35 . . . 125.5(6) ? N31 C36 H36 . . . 118.2(7) ? C35 C36 H36 . . . 116.2(7) ? Mg N41 C42 . . . 124.5(4) ? Mg N41 C46 . . . 116.6(5) ? C42 N41 C46 . . . 118.8(5) ? N41 C42 C421 . . . 119.8(5) ? N41 C42 C43 . . . 118.3(6) ? C421 C42 C43 . . . 121.9(7) ? C421 Si4 C422 . . . 113.2(4) ? C421 Si4 C423 . . . 108.3(4) ? C421 Si4 C424 . . . 114.3(4) ? C422 Si4 C423 . . . 108.0(5) ? C422 Si4 C424 . . . 106.2(5) ? C423 Si4 C424 . . . 106.4(4) ? C42 C421 Si4 . . . 129.6(5) ? C42 C421 H421 . . . 117.1(7) ? Si4 C421 H421 . . . 113.3(5) ? Si4 C422 H422a . . . 112.9(9) ? Si4 C422 H422b . . . 112.5(11) ? Si4 C422 H422c . . . 109.6(7) ? H422a C422 H422b . . . 110.1(10) ? H422a C422 H422c . . . 105.9(13) ? H422b C422 H422c . . . 105.3(11) ? Si4 C423 H423a . . . 113.2(7) ? Si4 C423 H423b . . . 111.3(8) ? Si4 C423 H423c . . . 114.3(7) ? H423a C423 H423b . . . 104.1(9) ? H423a C423 H423c . . . 108.0(10) ? H423b C423 H423c . . . 105.3(9) ? Si4 C424 H424a . . . 112.6(9) ? Si4 C424 H424b . . . 110.8(7) ? Si4 C424 H424c . . . 113.7(7) ? H424a C424 H424b . . . 104.6(9) ? H424a C424 H424c . . . 108.5(9) ? H424b C424 H424c . . . 106.0(11) ? C42 C43 C44 . . . 119.5(7) ? C42 C43 H43 . . . 119.5(7) ? C44 C43 H43 . . . 121.0(6) ? C43 C44 C45 . . . 122.0(6) ? C43 C44 H44 . . . 119.1(8) ? C45 C44 H44 . . . 118.9(7) ? C44 C45 C46 . . . 116.3(7) ? C44 C45 H45 . . . 121.9(6) ? C46 C45 H45 . . . 121.8(8) ? N41 C46 C45 . . . 125.0(7) ? N41 C46 H46 . . . 119.1(6) ? C45 C46 H46 . . . 115.9(7) ? N21 C212' C222 . . . 108.1(18) ? N21 C212' H222a . . . 105.1(15) ? N21 C212' H222b . . . 120.4(14) ? N21 C212' H212'a . . . 111.4(17) ? N21 C212' H212'b . . . 111.3(18) ? N21 C212' H212'c . . . 112.9(16) ? C222 C212' H222a . . . 41.1(12) ? C222 C212' H222b . . . 43.1(12) ? C222 C212' H212'a . . . 74.0(15) ? C222 C212' H212'b . . . 37.3(12) ? C222 C212' H212'c . . . 135(2) ? H222a C212' H222b . . . 81.2(13) ? H222a C212' H212'a . . . 112.7(18) ? H222a C212' H212'b . . . 6.9(3) ? H222a C212' H212'c . . . 107.6(18) ? H222b C212' H212'a . . . 31.6(6) ? H222b C212' H212'b . . . 75.5(13) ? H222b C212' H212'c . . . 121(2) ? H212'a C212' H212'b . . . 106.8(18) ? H212'a C212' H212'c . . . 107(2) ? H212'b C212' H212'c . . . 107(2) ? N22 C222' C232 . . . 97.5(11) ? N22 C222' H232a . . . 110.8(13) ? N22 C222' H222'a . . . 106.8(17) ? N22 C222' H222'b . . . 106.7(15) ? N22 C222' H222'c . . . 120.2(17) ? C232 C222' H232a . . . 27.4(11) ? C232 C222' H222'a . . . 48.6(14) ? C232 C222' H222'b . . . 61.0(15) ? C232 C222' H222'c . . . 142.0(16) ? H232a C222' H222'a . . . 69.3(13) ? H232a C222' H222'b . . . 35.3(7) ? H232a C222' H222'c . . . 125.6(18) ? H222'a C222' H222'b . . . 104.1(19) ? H222'a C222' H222'c . . . 110(2) ? H222'b C222' H222'c . . . 108(2) ? N23 C232' H232'a . . . 106.1(15) ? N23 C232' H232'b . . . 104.8(17) ? N23 C232' H232'c . . . 123.0(17) ? H232'a C232' H232'b . . . 109.3(18) ? H232'a C232' H232'c . . . 108(2) ? H232'b C232' H232'c . . . 105.1(18) ? C222 H222a C212' . . . 83.1(18) ? C222 H222a H212'b . . . 69.6(18) ? C212' H222a H212'b . . . 24.0(10) ? C222 H222b C212' . . . 85.0(17) ? C222 H222b H212'a . . . 138.9(14) ? C212' H222b H212'a . . . 56.2(12) ? C232 H232a C222' . . . 116(2) ? C232 H232a H222'b . . . 155.5(12) ? C222' H232a H222'b . . . 51.8(12) ? C232 H232b H222'a . . . 94.6(18) ? C212' H212'a H222b . . . 92.2(13) ? C222 H212'b C212' . . . 103(2) ? C222 H212'b H222a . . . 93.3(18) ? C212' H212'b H222a . . . 149.0(13) ? C232 H222'a C222' . . . 101.6(19) ? C232 H222'a H232b . . . 45.0(14) ? C222' H222'a H232b . . . 142.7(12) ? C222' H222'b H232a . . . 92.9(14) ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Mg P1 3.355(3) . . ? Mg P2 3.374(4) . . ? Mg C32 3.066(6) . . ? Mg C321 3.290(7) . . ? Mg C36 2.903(8) . . ? Mg C42 3.081(7) . . ? Mg C421 3.291(8) . . ? Mg C46 2.928(7) . . ? Mg H122a 3.155(2) . . ? Mg H321 2.751(2) . . ? Mg H36 2.882(3) . . ? Mg H421 2.727(2) . . ? Mg H46 2.923(2) . . ? O1 N11 2.547(8) . . ? O1 C111 3.033(11) . . ? O1 N12 2.546(7) . . ? O1 C122 3.071(9) . . ? O1 N13 2.556(8) . . ? O1 C131 3.066(9) . . ? O1 O2 3.069(7) . . ? O1 P2 4.449(6) . . ? O1 N31 3.317(7) . . ? O1 N41 3.159(7) . . ? O1 C46 3.213(8) . . ? O1 H111b 2.522(5) . . ? O1 H111c 3.099(5) . '3 776' ? O1 H122a 2.688(5) . . ? O1 H131a 3.348(4) . . ? O1 H131b 2.857(4) . . ? O1 H321 3.117(4) . . ? O1 H46 2.594(4) . . ? P1 C111 2.663(10) . . ? P1 C112 2.708(10) . . ? P1 C121 2.700(11) . . ? P1 C122 2.672(9) . . ? P1 C131 2.646(8) . . ? P1 C132 2.710(11) . . ? P1 O2 4.082(5) . . ? P1 C46 3.976(8) . . ? P1 H111a 3.320(2) . . ? P1 H111b 2.597(2) . . ? P1 H111b 3.614(2) . '3 776' ? P1 H111c 3.288(3) . . ? P1 H112a 2.737(2) . . ? P1 H112b 3.197(2) . . ? P1 H112c 3.465(2) . . ? P1 H121a 3.402(2) . . ? P1 H121b 3.293(2) . . ? P1 H121c 2.692(2) . . ? P1 H122a 2.712(2) . . ? P1 H122b 3.400(3) . . ? P1 H122c 3.229(2) . . ? P1 H131a 3.258(2) . . ? P1 H131b 2.728(2) . . ? P1 H131c 3.417(2) . . ? P1 H132a 3.394(2) . . ? P1 H132b 3.384(2) . . ? P1 H132c 2.707(2) . . ? P1 H46 3.159(2) . . ? N11 N12 2.618(10) . . ? N11 N13 2.637(8) . . ? N11 H111a 1.968(7) . . ? N11 H111b 1.951(6) . . ? N11 H111c 2.064(7) . . ? N11 H112a 1.980(6) . . ? N11 H112b 2.008(6) . . ? N11 H112c 2.041(5) . . ? N11 H132c 2.452(6) . . ? C111 C112 2.440(16) . . ? C111 H112c 2.679(10) . . ? C112 H111a 2.634(12) . . ? C112 H111c 2.685(11) . . ? C112 H132c 2.698(9) . . ? N12 N13 2.639(9) . . ? N12 H112a 2.521(6) . . ? N12 H121a 2.026(6) . . ? N12 H121b 2.019(6) . . ? N12 H121c 2.036(5) . . ? N12 H122a 2.027(5) . . ? N12 H122b 2.045(7) . . ? N12 H122c 2.016(5) . . ? C121 C122 2.434(12) . . ? C121 H122b 2.695(10) . . ? C122 H121a 2.671(8) . . ? C122 H121b 2.660(8) . . ? N13 H121c 2.400(7) . . ? N13 H131a 2.069(6) . . ? N13 H131b 2.074(7) . . ? N13 H131c 2.078(6) . . ? N13 H132a 2.108(7) . . ? N13 H132b 2.124(7) . . ? N13 H132c 1.982(7) . . ? C131 C132 2.431(16) . . ? C132 H131c 2.630(13) . . ? O2 N21 2.500(10) . . ? O2 C211 2.978(10) . . ? O2 N22 2.508(11) . . ? O2 C221 3.045(12) . . ? O2 N23 2.560(9) . . ? O2 C231 3.014(10) . . ? O2 N31 3.328(8) . . ? O2 C321 3.568(9) . . ? O2 N41 3.295(7) . . ? O2 C421 3.685(8) . . ? O2 H122a 3.289(4) . . ? O2 H211a 2.853(4) . . ? O2 H211b 2.919(5) . . ? O2 H221a 2.815(4) . . ? O2 H221b 3.044(5) . . ? O2 H231a 2.866(5) . . ? O2 H231b 2.964(4) . . ? O2 H321 2.812(5) . . ? O2 H421 3.010(5) . . ? P2 C211 2.640(8) . . ? P2 C212 2.85(3) . . ? P2 C221 2.641(11) . . ? P2 C222 2.72(3) . . ? P2 C231 2.622(10) . . ? P2 C232 2.68(2) . . ? P2 C212' 2.65(2) . . ? P2 C222' 2.762(17) . . ? P2 C232' 2.71(2) . . ? P2 H211a 2.878(2) . . ? P2 H211b 2.877(2) . . ? P2 H211c 3.626(2) . . ? P2 H212a 2.998(2) . . ? P2 H212b 3.000(3) . . ? P2 H212c 3.676(3) . . ? P2 H221a 2.832(2) . . ? P2 H221b 2.835(2) . . ? P2 H221c 3.603(2) . . ? P2 H222a 2.890(2) . . ? P2 H222b 2.890(3) . . ? P2 H222c 3.415(2) . . ? P2 H231a 2.830(2) . . ? P2 H231b 2.829(2) . . ? P2 H231c 3.575(2) . . ? P2 H232a 2.864(2) . . ? P2 H232b 2.868(2) . . ? P2 H232c 3.509(2) . . ? P2 H321 3.661(3) . . ? P2 H421 3.685(2) . . ? P2 H212'a 2.860(3) . . ? P2 H212'b 2.860(2) . . ? P2 H212'c 3.492(3) . . ? P2 H222'a 2.909(2) . . ? P2 H222'b 2.905(2) . . ? P2 H222'c 3.582(2) . . ? P2 H232'a 2.866(2) . . ? P2 H232'b 2.864(2) . . ? P2 H232'c 3.578(2) . . ? N21 N22 2.565(13) . . ? N21 C222 2.51(3) . . ? N21 N23 2.519(10) . . ? N21 C232' 2.88(2) . . ? N21 H211a 1.922(7) . . ? N21 H211b 1.940(8) . . ? N21 H211c 2.207(6) . . ? N21 H212a 2.209(11) . . ? N21 H212b 2.180(9) . . ? N21 H212c 2.342(9) . . ? N21 H222a 2.284(11) . . ? N21 H222b 2.437(9) . . ? N21 H212'a 2.181(9) . . ? N21 H212'b 2.183(10) . . ? N21 H212'c 2.200(9) . . ? N21 H232'b 2.693(10) . . ? C211 C212 2.21(3) . . ? C211 C212' 2.46(2) . . ? C211 H212a 2.541(11) . . ? C211 H212c 2.382(12) . . ? C211 H212'c 2.561(12) . . ? C212 N23 2.86(3) . . ? C212 C212' 2.28(4) . . ? C212 C232' 2.23(3) . . ? C212 H211b 2.46(3) . . ? C212 H211c 2.53(2) . . ? C212 H212'a 2.36(3) . . ? C212 H212'c 2.40(3) . . ? C212 H232'a 1.97(2) . . ? C212 H232'b 1.80(3) . . ? N22 N23 2.516(11) . . ? N22 C232 2.68(3) . . ? N22 C212' 2.73(2) . . ? N22 H221a 1.813(13) . . ? N22 H221b 1.804(9) . . ? N22 H221c 2.121(9) . . ? N22 H222a 2.455(12) . . ? N22 H222b 2.448(14) . . ? N22 H222c 2.272(12) . . ? N22 H232a 2.397(8) . . ? N22 H232b 2.612(10) . . ? N22 H212'b 2.488(13) . . ? N22 H222'a 2.132(9) . . ? N22 H222'b 2.147(9) . . ? N22 H222'c 2.236(8) . . ? C221 C222 2.44(3) . . ? C221 C222' 2.21(2) . . ? C221 H222c 2.426(15) . . ? C221 H222'b 2.695(11) . . ? C221 H222'c 2.366(12) . . ? C222 C222' 2.71(3) . . ? C222 H221b 2.42(3) . . ? C222 H212'a 1.52(3) . . ? C222 H212'c 2.26(3) . . ? C222 H222'a 2.68(2) . . ? N23 C222' 2.78(2) . . ? N23 H212a 2.697(7) . . ? N23 H231a 1.898(8) . . ? N23 H231b 1.902(8) . . ? N23 H231c 2.146(7) . . ? N23 H232a 2.192(7) . . ? N23 H232b 2.178(8) . . ? N23 H232c 2.215(7) . . ? N23 H222'a 2.604(7) . . ? N23 H222'b 2.579(7) . . ? N23 H232'a 1.977(8) . . ? N23 H232'b 1.986(7) . . ? N23 H232'c 2.170(8) . . ? C231 C232 2.26(3) . . ? C231 C232' 2.14(3) . . ? C231 H232c 2.463(10) . . ? C231 H232'b 2.492(13) . . ? C231 H232'c 2.325(13) . . ? C232 C232' 2.12(3) . . ? C232 H231b 2.47(3) . . ? C232 H231c 2.57(3) . . ? C232 H222'b 1.68(3) . . ? C232 H222'c 2.69(3) . . ? C232 H232'a 2.14(3) . . ? C232 H232'c 2.40(3) . . ? N31 C321 2.414(8) . . ? N31 C33 2.385(9) . . ? N31 C34 2.738(10) . . ? N31 C35 2.394(10) . . ? N31 H321 2.573(5) . . ? N31 H36 2.011(5) . . ? C32 Si3 2.862(7) . . ? C32 C34 2.430(11) . . ? C32 C35 2.846(10) . . ? C32 C36 2.387(9) . . ? C32 H321 2.014(7) . . ? C32 H33 2.105(6) . . ? C321 C324 2.984(12) . . ? C321 C33 2.464(11) . . ? C321 H33 2.688(8) . . ? Si3 H321 2.399(2) . . ? Si3 H322a 2.404(2) . . ? Si3 H322b 2.401(3) . . ? Si3 H322c 2.403(3) . . ? Si3 H323a 2.400(3) . . ? Si3 H323b 2.401(3) . . ? Si3 H323c 2.397(3) . . ? Si3 H324a 2.398(3) . . ? Si3 H324b 2.398(3) . . ? Si3 H324c 2.399(3) . . ? C322 C324 2.992(14) . . ? C323 C324 2.994(17) . . ? C33 C35 2.389(10) . . ? C33 C36 2.682(10) . . ? C33 H34 2.022(8) . . ? C34 C36 2.334(11) . . ? C34 H33 2.022(8) . . ? C34 H35 2.104(8) . . ? C35 H34 2.094(8) . . ? C35 H36 2.015(8) . . ? C36 H35 2.081(8) . . ? N41 C421 2.387(10) . . ? N41 C43 2.437(9) . . ? N41 C44 2.763(8) . . ? N41 C45 2.397(8) . . ? N41 H421 2.534(5) . . ? N41 H46 2.019(6) . . ? C42 Si4 2.891(8) . . ? C42 C44 2.400(9) . . ? C42 C45 2.794(10) . . ? C42 C46 2.352(11) . . ? C42 H421 2.027(6) . . ? C42 H43 2.106(6) . . ? Si4 H421 2.400(3) . . ? Si4 H422a 2.396(3) . . ? Si4 H422b 2.396(3) . . ? Si4 H422c 2.395(3) . . ? Si4 H423a 2.412(3) . . ? Si4 H423b 2.412(2) . . ? Si4 H423c 2.413(3) . . ? Si4 H424a 2.418(3) . . ? Si4 H424b 2.417(3) . . ? Si4 H424c 2.419(3) . . ? C421 C423 2.985(12) . . ? C421 C43 2.459(9) . . ? C421 H43 2.668(6) . . ? C422 C424 2.994(17) . . ? C423 C424 2.994(12) . . ? C43 C45 2.403(12) . . ? C43 C46 2.727(11) . . ? C43 H44 2.010(7) . . ? C44 C46 2.360(10) . . ? C44 H43 2.017(9) . . ? C44 H45 2.112(9) . . ? C45 H44 2.083(8) . . ? C45 H46 2.009(7) . . ? C46 H45 2.064(6) . . ? C212' H212b 2.19(2) . . ? C212' H212c 2.54(2) . . ? C212' H222c 2.28(2) . . ? C222' H221a 2.61(2) . . ? C222' H221c 2.55(2) . . ? C222' H232b 1.83(2) . . ? C222' H232c 2.64(2) . . ? C232' H212a 1.902(16) . . ? C232' H212b 1.97(2) . . ? C232' H231a 2.53(2) . . ? C232' H231c 2.43(2) . . ? C232' H232b 2.322(18) . . ? C232' H232c 2.291(17) . . ? H111a H111b 1.5513(3) . . ? H111a H111c 1.5663(3) . . ? H111b H111c 1.6281(3) . . ? H112a H112b 1.5513(3) . . ? H112a H112c 1.5560(3) . . ? H112b H112c 1.5775(3) . . ? H112b H132c 2.2200(5) . . ? H112c H211c 2.1751(6) . '3 676' ? H121a H121b 1.5513(3) . . ? H121a H121c 1.6712(4) . . ? H121b H121c 1.6712(4) . . ? H122a H122b 1.5514(2) . . ? H122a H122c 1.5284(3) . . ? H122b H122c 1.5477(3) . . ? H131a H131b 1.5513(4) . . ? H131a H131c 1.5444(3) . . ? H131b H131c 1.5502(3) . . ? H131b H221a 2.2355(4) . . ? H132a H132b 1.5513(3) . . ? H132a H132c 1.3971(4) . . ? H132b H132c 1.5317(3) . . ? H132b H231c 2.1911(5) . '2 756' ? H211a H211b 1.5512(4) . . ? H211a H211c 1.5001(3) . . ? H211b H211c 1.5001(3) . . ? H211c H212c 2.2998(4) . . ? H212a H212b 1.5513(3) . . ? H212a H212c 1.5316(4) . . ? H212a H232'a 2.0096(4) . . ? H212a H232'b 1.1451(3) . . ? H212b H212c 1.5318(3) . . ? H212b H212'a 1.8679(5) . . ? H212b H232'a 1.3336(3) . . ? H212b H232'b 1.9567(3) . . ? H212c H212'c 2.2747(6) . . ? H221a H221b 1.5513(4) . . ? H221a H221c 1.4891(2) . . ? H221b H221c 1.4893(3) . . ? H221c H34 2.2079(6) . '2 756' ? H221c H222'c 2.3277(4) . . ? H222a H222b 1.5513(3) . . ? H222a H222c 1.5805(3) . . ? H222a H212'a 1.8266(3) . . ? H222a H212'c 1.7745(4) . . ? H222b H222c 1.5807(3) . . ? H222b H212'b 1.3116(2) . . ? H222b H212'c 1.8564(4) . . ? H222c H422a 2.3379(5) . '2 656' ? H222c H212'a 2.1782(5) . . ? H222c H212'b 1.5999(3) . . ? H231a H231b 1.5513(3) . . ? H231a H231c 1.5054(3) . . ? H231b H231c 1.5053(3) . . ? H231c H232'c 2.2041(6) . . ? H232a H232b 1.5512(4) . . ? H232a H232c 1.5504(3) . . ? H232a H222'a 1.2946(3) . . ? H232a H222'c 1.9390(5) . . ? H232b H232c 1.5502(3) . . ? H232b H424b 2.2750(4) . '4 565' ? H232b H222'b 2.1109(5) . . ? H232b H232'a 1.8979(3) . . ? H232c H35 2.3147(5) . '4 565' ? H232c H36 2.3994(4) . '4 565' ? H232c H222'a 2.1052(5) . . ? H232c H222'b 2.2705(4) . . ? H232c H232'a 2.3793(6) . . ? H232c H232'c 2.1933(4) . . ? H322a H322b 1.5513(3) . . ? H322a H322c 1.5513(5) . . ? H322b H322c 1.5513(3) . . ? H323a H323b 1.5515(3) . . ? H323a H323c 1.5514(3) . . ? H323b H323c 1.5513(4) . . ? H323c H33 2.3240(4) . . ? H324a H324b 1.5514(4) . . ? H324a H324c 1.5514(3) . . ? H324a H222'a 2.3202(5) . '3 777' ? H324a H222'c 2.3383(5) . '3 777' ? H324b H324c 1.5513(2) . . ? H33 H34 2.3005(4) . . ? H35 H36 2.3525(5) . . ? H422a H422b 1.5513(3) . . ? H422a H422c 1.5514(3) . . ? H422b H422c 1.5514(3) . . ? H423a H423b 1.5514(2) . . ? H423a H423c 1.5513(3) . . ? H423b H423c 1.5514(4) . . ? H424a H424b 1.5513(4) . . ? H424a H424c 1.5514(3) . . ? H424b H424c 1.5513(4) . . ? H424c H43 2.3557(6) . . ? H43 H44 2.3168(4) . . ? H45 H46 2.3204(4) . . ? H212'a H212'b 1.5515(3) . . ? H212'a H212'c 1.5551(3) . . ? H212'b H212'c 1.5553(3) . . ? H222'a H222'b 1.5514(4) . . ? H222'a H222'c 1.5403(3) . . ? H222'b H222'c 1.5403(3) . . ? H232'a H232'b 1.5513(3) . . ? H232'a H232'c 1.5216(3) . . ? H232'b H232'c 1.5218(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1544 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 0 0 -9 0 0 0 12 0 0 -12 0 0 0 8 0 0 -8 5 7 -6 -5 -7 6 5 7 6 -5 -7 -6 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -20 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .839 _reflns_d_resolution_low 12.774 _diffrn_reflns_av_sigmaI/netI .071 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atom-block _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .23 _refine_ls_wR_factor_all .095 _refine_ls_goodness_of_fit_all 1.25 _refine_ls_shift/su_mean .01 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_pca21 _database_code_CSD 154203 _audit_creation_method Xtal3.6 _audit_creation_date 00-05-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C36 H74 N8 Na2 Si2' _chemical_formula_moiety ? _chemical_formula_weight 721.2 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 10.221(5) _cell_length_b 21.645(10) _cell_length_c 11.430(2) _cell_angle_alpha 90.00000 _cell_angle_beta 115.10(3) _cell_angle_gamma 90.00000 _cell_volume 2289.9(17) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.046 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 18.4 _cell_measurement_theta_max 22.2 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .128 _exptl_crystal_description block _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid .6 _exptl_crystal_size_min .32 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .93 _exptl_absorpt_correction_T_max .97 _diffrn_reflns_number 5200 _reflns_number_total 4015 _reflns_Friedel_coverage ? _reflns_number_gt 2324 _reflns_threshold_expression 'I > 3.00 sig(F )' _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .027 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 2.34 _refine_ls_number_reflns 2324 _refine_ls_number_parameters 366 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .099 _refine_diff_density_min -.18 _refine_diff_density_max .24 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 72 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Na ? 0 4 .030029 .025024 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 4 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 148 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na .38490(13) .54742(5) .87127(10) .0542(6) Uani ? ? 1.00000 ? ? N1 .4846(3) .55702(11) 1.1092(2) .0537(13) Uani ? ? 1.00000 ? ? C2 .5919(4) .60126(13) 1.1632(3) .0497(15) Uani ? ? 1.00000 ? ? Si2 .83121(11) .66967(4) 1.16204(9) .0683(5) Uani ? ? 1.00000 ? ? C21 .6965(4) .60887(15) 1.1200(3) .0570(17) Uani ? ? 1.00000 ? ? C22 .9708(7) .6659(4) 1.3343(5) .117(3) Uani ? ? 1.00000 ? ? C23 .9289(8) .6640(3) 1.0572(7) .105(4) Uani ? ? 1.00000 ? ? C24 .7510(7) .7486(2) 1.1387(8) .111(4) Uani ? ? 1.00000 ? ? C3 .5821(5) .63922(16) 1.2640(3) .069(2) Uani ? ? 1.00000 ? ? C4 .4701(6) .6364(2) 1.2935(4) .081(2) Uani ? ? 1.00000 ? ? C5 .3580(5) .5953(2) 1.2294(4) .081(2) Uani ? ? 1.00000 ? ? C6 .3738(5) .55682(18) 1.1416(3) .068(2) Uani ? ? 1.00000 ? ? N01 .0981(3) .55181(12) .7853(3) .0657(16) Uani ? ? 1.00000 ? ? C011 .0301(6) .5174(2) .8535(6) .089(3) Uani ? ? 1.00000 ? ? C012 .0526(9) .5272(4) .6566(6) .123(4) Uani ? ? 1.00000 ? ? C02 .0590(6) .6179(2) .7854(6) .093(3) Uani ? ? 1.00000 ? ? C03 .1369(5) .66132(19) .7398(5) .085(2) Uani ? ? 1.00000 ? ? N04 .2924(3) .66017(11) .8118(2) .0589(14) Uani ? ? 1.00000 ? ? C041 .3376(6) .69530(19) .9322(4) .082(2) Uani ? ? 1.00000 ? ? C05 .3651(7) .68615(18) .7343(5) .091(3) Uani ? ? 1.00000 ? ? C06 .3679(6) .6442(2) .6334(5) .102(3) Uani ? ? 1.00000 ? ? N07 .4458(4) .58749(14) .6839(3) .0725(16) Uani ? ? 1.00000 ? ? C071 .3954(9) .5406(3) .5782(5) .123(4) Uani ? ? 1.00000 ? ? C072 .5988(6) .5943(3) .7282(7) .111(4) Uani ? ? 1.00000 ? ? H21 .694(3) .5827(13) 1.061(3) .057(9) Uiso ? ? 1.00000 ? ? H22a .891(7) .666(3) 1.396(6) .23(3) Uiso ? ? 1.00000 ? ? H22b 1.022(6) .634(3) 1.354(6) .16(3) Uiso ? ? 1.00000 ? ? H22c 1.035(5) .691(2) 1.350(4) .118(19) Uiso ? ? 1.00000 ? ? H23a .989(7) .625(3) 1.068(6) .22(3) Uiso ? ? 1.00000 ? ? H23b .865(7) .670(3) .982(6) .20(4) Uiso ? ? 1.00000 ? ? H23c 1.004(5) .691(2) 1.076(4) .131(19) Uiso ? ? 1.00000 ? ? H24a .695(6) .756(2) 1.051(5) .15(3) Uiso ? ? 1.00000 ? ? H24b .667(6) .754(2) 1.153(5) .14(2) Uiso ? ? 1.00000 ? ? H24c .814(5) .775(2) 1.160(4) .13(2) Uiso ? ? 1.00000 ? ? H3 .660(4) .6662(15) 1.300(3) .076(11) Uiso ? ? 1.00000 ? ? H4 .463(4) .6645(18) 1.360(4) .125(15) Uiso ? ? 1.00000 ? ? H5 .278(4) .5923(17) 1.246(3) .098(14) Uiso ? ? 1.00000 ? ? H6 .300(4) .5259(14) 1.095(3) .078(11) Uiso ? ? 1.00000 ? ? H011a .066(4) .5311(18) .941(4) .109(17) Uiso ? ? 1.00000 ? ? H011b -.076(5) .5203(19) .810(4) .127(17) Uiso ? ? 1.00000 ? ? H011c .070(4) .470(2) .867(3) .112(14) Uiso ? ? 1.00000 ? ? H012a -.062(7) .534(3) .619(5) .18(3) Uiso ? ? 1.00000 ? ? H012b .111(5) .553(2) .611(4) .130(18) Uiso ? ? 1.00000 ? ? H012c .068(4) .4821(18) .667(3) .081(13) Uiso ? ? 1.00000 ? ? H02a .083(6) .633(3) .874(6) .21(3) Uiso ? ? 1.00000 ? ? H02b -.046(4) .6231(17) .737(4) .105(14) Uiso ? ? 1.00000 ? ? H03a .097(4) .7050(16) .738(3) .086(11) Uiso ? ? 1.00000 ? ? H03b .108(5) .645(2) .648(5) .16(2) Uiso ? ? 1.00000 ? ? H041a .441(4) .6910(16) .973(3) .089(14) Uiso ? ? 1.00000 ? ? H041b .305(3) .7394(16) .915(3) .085(11) Uiso ? ? 1.00000 ? ? H041c .280(4) .6773(17) .992(3) .106(13) Uiso ? ? 1.00000 ? ? H05a .477(5) .6831(19) .774(4) .118(17) Uiso ? ? 1.00000 ? ? H05b .312(4) .7243(17) .693(3) .091(12) Uiso ? ? 1.00000 ? ? H06a .415(4) .6672(16) .586(3) .096(12) Uiso ? ? 1.00000 ? ? H06b .241(7) .627(3) .565(6) .20(2) Uiso ? ? 1.00000 ? ? H071a .279(7) .542(3) .549(5) .17(3) Uiso ? ? 1.00000 ? ? H071b .427(5) .558(2) .516(5) .16(2) Uiso ? ? 1.00000 ? ? H071c .472(7) .501(3) .618(6) .20(3) Uiso ? ? 1.00000 ? ? H072a .635(4) .6102(18) .673(4) .097(15) Uiso ? ? 1.00000 ? ? H072b .635(6) .630(3) .793(5) .15(2) Uiso ? ? 1.00000 ? ? H072c .647(5) .555(2) .751(4) .128(17) Uiso ? ? 1.00000 ? ? 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 Na .0661(8) .0519(7) .0412(6) .0103(6) .0194(6) .0061(5) N1 .0678(19) .0471(15) .0421(13) -.0014(14) .0194(14) -.0012(12) C2 .062(2) .0417(17) .0364(16) .0079(16) .0122(15) .0005(14) Si2 .0623(6) .0636(6) .0658(6) -.0018(5) .0145(5) -.0039(5) C21 .061(2) .055(2) .051(2) .0042(17) .0199(17) -.0120(16) C22 .099(4) .119(5) .081(3) -.039(4) -.012(3) -.001(3) C23 .093(4) .112(4) .123(5) -.023(4) .058(4) -.005(4) C24 .085(4) .062(3) .163(6) -.007(3) .031(4) -.010(3) C3 .093(3) .059(2) .057(2) -.011(2) .035(2) -.0138(18) C4 .127(4) .065(3) .066(2) .011(3) .056(3) .000(2) C5 .088(3) .091(3) .080(3) .015(3) .051(3) .020(3) C6 .078(3) .068(2) .056(2) -.006(2) .026(2) .0060(19) N01 .0651(19) .0577(17) .0718(19) -.0003(15) .0267(15) .0038(14) C011 .073(3) .087(3) .112(4) -.003(3) .045(3) .017(3) C012 .143(6) .127(5) .095(4) -.034(5) .047(4) -.029(4) C02 .071(3) .078(3) .134(4) .026(2) .048(3) .031(3) C03 .082(3) .052(2) .099(3) .016(2) .017(3) .010(2) N04 .0664(19) .0443(16) .0559(15) .0059(13) .0163(14) .0031(13) C041 .103(4) .054(2) .075(3) .007(3) .024(3) -.008(2) C05 .144(5) .047(2) .087(3) .001(3) .053(3) .020(2) C06 .139(5) .095(3) .094(3) .033(3) .072(3) .044(3) N07 .085(2) .074(2) .0689(18) .0183(18) .0426(17) .0229(16) C071 .159(6) .143(5) .069(3) .013(5) .050(4) -.008(3) C072 .097(4) .104(4) .142(5) .012(4) .059(4) .043(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Na N1 . . 2.475(2) ? Na N01 . . 2.669(3) ? Na N04 . . 2.601(3) ? Na N07 . . 2.619(4) ? Na N1 . '3 667' 2.586(3) ? N1 C2 . . 1.388(4) ? N1 C6 . . 1.332(6) ? C2 C21 . . 1.364(6) ? C2 C3 . . 1.453(5) ? Si2 C21 . . 1.816(4) ? Si2 C22 . . 1.880(5) ? Si2 C23 . . 1.861(10) ? Si2 C24 . . 1.865(5) ? C21 H21 . . .87(3) ? C22 H22a . . 1.28(8) ? C22 H22b . . .84(6) ? C22 H22c . . .81(5) ? C23 H23a . . 1.02(7) ? C23 H23b . . .84(5) ? C23 H23c . . .91(5) ? C24 H24a . . .93(5) ? C24 H24b . . .95(7) ? C24 H24c . . .82(5) ? C3 C4 . . 1.325(9) ? C3 H3 . . .93(3) ? C4 C5 . . 1.389(6) ? C4 H4 . . 1.00(5) ? C5 C6 . . 1.365(7) ? C5 H5 . . .92(5) ? C6 H6 . . .98(3) ? N01 C011 . . 1.451(8) ? N01 C012 . . 1.443(8) ? N01 C02 . . 1.485(5) ? C011 H011a . . .95(4) ? C011 H011b . . .98(5) ? C011 H011c . . 1.09(4) ? C012 H012a . . 1.07(7) ? C012 H012b . . 1.10(6) ? C012 H012c . . .99(4) ? C02 C03 . . 1.463(9) ? C02 H02a . . .99(7) ? C02 H02b . . .98(4) ? C03 N04 . . 1.447(5) ? C03 H03a . . 1.03(4) ? C03 H03b . . 1.02(5) ? N04 C041 . . 1.465(5) ? N04 C05 . . 1.487(8) ? C041 H041a . . .96(4) ? C041 H041b . . 1.00(3) ? C041 H041c . . 1.14(4) ? C05 C06 . . 1.478(8) ? C05 H05a . . 1.04(5) ? C05 H05b . . .99(4) ? C06 N07 . . 1.444(5) ? C06 H06a . . 1.00(4) ? C06 H06b . . 1.25(6) ? N07 C071 . . 1.492(7) ? N07 C072 . . 1.432(7) ? C071 H071a . . 1.09(7) ? C071 H071b . . .97(6) ? C071 H071c . . 1.12(6) ? C072 H072a . . .92(5) ? C072 H072b . . 1.02(6) ? C072 H072c . . .96(4) ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N1 Na N01 . . . 106.11(12) ? N1 Na N04 . . . 98.22(8) ? N1 Na N07 . . . 137.81(11) ? N1 Na N1 . . '3 667' 91.24(8) ? N01 Na N04 . . . 69.50(9) ? N01 Na N07 . . . 106.98(11) ? N01 Na N1 . . '3 667' 120.57(9) ? N04 Na N07 . . . 70.23(10) ? N04 Na N1 . . '3 667' 163.68(12) ? N07 Na N1 . . '3 667' 93.86(11) ? Na N1 C2 . . . 115.2(2) ? Na N1 C6 . . . 107.62(18) ? Na N1 Na . . '3 667' 88.76(9) ? C2 N1 C6 . . . 118.9(3) ? C2 N1 Na . . '3 667' 106.5(2) ? C6 N1 Na . . '3 667' 116.2(2) ? N1 C2 C21 . . . 121.0(3) ? N1 C2 C3 . . . 115.8(4) ? C21 C2 C3 . . . 123.2(3) ? C21 Si2 C22 . . . 113.5(3) ? C21 Si2 C23 . . . 109.6(2) ? C21 Si2 C24 . . . 112.8(2) ? C22 Si2 C23 . . . 107.2(3) ? C22 Si2 C24 . . . 106.4(3) ? C23 Si2 C24 . . . 107.0(4) ? C2 C21 Si2 . . . 127.9(3) ? C2 C21 H21 . . . 116(2) ? Si2 C21 H21 . . . 116(2) ? Si2 C22 H22a . . . 101(2) ? Si2 C22 H22b . . . 115(4) ? Si2 C22 H22c . . . 113(3) ? H22a C22 H22b . . . 109(6) ? H22a C22 H22c . . . 121(5) ? H22b C22 H22c . . . 98(5) ? Si2 C23 H23a . . . 116(5) ? Si2 C23 H23b . . . 105(6) ? Si2 C23 H23c . . . 116(3) ? H23a C23 H23b . . . 115(6) ? H23a C23 H23c . . . 96(5) ? H23b C23 H23c . . . 111(6) ? Si2 C24 H24a . . . 110(3) ? Si2 C24 H24b . . . 118(3) ? Si2 C24 H24c . . . 111(3) ? H24a C24 H24b . . . 89(5) ? H24a C24 H24c . . . 104(4) ? H24b C24 H24c . . . 121(5) ? C2 C3 C4 . . . 122.2(4) ? C2 C3 H3 . . . 112(3) ? C4 C3 H3 . . . 126(3) ? C3 C4 C5 . . . 120.3(5) ? C3 C4 H4 . . . 121(2) ? C5 C4 H4 . . . 119(2) ? C4 C5 C6 . . . 116.8(5) ? C4 C5 H5 . . . 123(2) ? C6 C5 H5 . . . 120(2) ? N1 C6 C5 . . . 125.6(4) ? N1 C6 H6 . . . 114(3) ? C5 C6 H6 . . . 121(3) ? Na N01 C011 . . . 119.0(2) ? Na N01 C012 . . . 101.0(4) ? Na N01 C02 . . . 106.7(3) ? C011 N01 C012 . . . 109.7(5) ? C011 N01 C02 . . . 107.7(4) ? C012 N01 C02 . . . 112.7(4) ? N01 C011 H011a . . . 110(3) ? N01 C011 H011b . . . 112(3) ? N01 C011 H011c . . . 109(2) ? H011a C011 H011b . . . 111(4) ? H011a C011 H011c . . . 101(3) ? H011b C011 H011c . . . 113(3) ? N01 C012 H012a . . . 101(3) ? N01 C012 H012b . . . 107(2) ? N01 C012 H012c . . . 106(2) ? H012a C012 H012b . . . 117(4) ? H012a C012 H012c . . . 106(4) ? H012b C012 H012c . . . 118(4) ? N01 C02 C03 . . . 115.5(5) ? N01 C02 H02a . . . 112(4) ? N01 C02 H02b . . . 110(2) ? C03 C02 H02a . . . 102(4) ? C03 C02 H02b . . . 111(3) ? H02a C02 H02b . . . 106(5) ? C02 C03 N04 . . . 114.8(4) ? C02 C03 H03a . . . 109(3) ? C02 C03 H03b . . . 100(3) ? N04 C03 H03a . . . 111(2) ? N04 C03 H03b . . . 110(3) ? H03a C03 H03b . . . 111(3) ? Na N04 C03 . . . 110.8(2) ? Na N04 C041 . . . 107.9(2) ? Na N04 C05 . . . 107.0(2) ? C03 N04 C041 . . . 111.0(4) ? C03 N04 C05 . . . 111.1(3) ? C041 N04 C05 . . . 109.0(3) ? N04 C041 H041a . . . 104(2) ? N04 C041 H041b . . . 111.3(18) ? N04 C041 H041c . . . 110.3(17) ? H041a C041 H041b . . . 113(3) ? H041a C041 H041c . . . 115(3) ? H041b C041 H041c . . . 103(3) ? N04 C05 C06 . . . 114.4(4) ? N04 C05 H05a . . . 117(3) ? N04 C05 H05b . . . 107(3) ? C06 C05 H05a . . . 85(3) ? C06 C05 H05b . . . 109(2) ? H05a C05 H05b . . . 123(3) ? C05 C06 N07 . . . 113.6(4) ? C05 C06 H06a . . . 107(2) ? C05 C06 H06b . . . 108(4) ? N07 C06 H06a . . . 109(2) ? N07 C06 H06b . . . 104(3) ? H06a C06 H06b . . . 115(4) ? Na N07 C06 . . . 109.1(4) ? Na N07 C071 . . . 108.5(4) ? Na N07 C072 . . . 110.3(4) ? C06 N07 C071 . . . 108.2(4) ? C06 N07 C072 . . . 112.8(4) ? C071 N07 C072 . . . 107.8(5) ? N07 C071 H071a . . . 101(3) ? N07 C071 H071b . . . 103(3) ? N07 C071 H071c . . . 104(3) ? H071a C071 H071b . . . 115(4) ? H071a C071 H071c . . . 129(5) ? H071b C071 H071c . . . 102(5) ? N07 C072 H072a . . . 119(2) ? N07 C072 H072b . . . 110(4) ? N07 C072 H072c . . . 111(3) ? H072a C072 H072b . . . 95(5) ? H072a C072 H072c . . . 102(4) ? H072b C072 H072c . . . 119(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Na Na 3.5406(16) . '3 667' ? Na C2 3.313(3) . . ? Na C2 3.263(3) . '3 667' ? Na C21 3.509(3) . . ? Na C21 3.495(4) . '3 667' ? Na C6 3.392(5) . '3 667' ? Na C6 3.146(4) . . ? Na C011 3.604(7) . . ? Na C012 3.268(7) . . ? Na C02 3.408(6) . . ? Na C03 3.396(4) . . ? Na C041 3.354(5) . . ? Na C05 3.353(5) . . ? Na C06 3.378(6) . . ? Na C071 3.400(7) . . ? Na C072 3.394(8) . . ? Na H21 3.12(3) . '3 667' ? Na H21 3.07(3) . . ? Na H6 3.06(4) . . ? Na H012b 3.10(4) . . ? Na H012c 3.39(3) . . ? Na H041a 3.28(3) . . ? Na H071a 3.37(6) . . ? N1 C21 2.396(5) . . ? N1 C3 2.407(4) . . ? N1 C4 2.771(6) . . ? N1 C5 2.399(6) . . ? N1 H21 2.49(4) . . ? N1 H6 1.94(4) . . ? C2 Si2 2.864(4) . . ? C2 C4 2.433(8) . . ? C2 C5 2.800(7) . . ? C2 C6 2.343(6) . . ? C2 H21 1.91(4) . . ? C2 H3 2.00(3) . . ? Si2 H21 2.34(3) . . ? Si2 H22a 2.48(7) . . ? Si2 H22b 2.36(5) . . ? Si2 H22c 2.32(4) . . ? Si2 H23a 2.48(8) . . ? Si2 H23b 2.23(8) . . ? Si2 H23c 2.40(6) . . ? Si2 H24a 2.35(4) . . ? Si2 H24b 2.45(5) . . ? Si2 H24c 2.29(4) . . ? C21 C3 2.478(7) . . ? C21 H3 2.56(4) . . ? C22 C24 2.998(9) . . ? C23 C24 2.994(12) . . ? C3 C5 2.353(7) . . ? C3 C6 2.673(6) . . ? C3 H4 2.03(5) . . ? C4 C6 2.345(5) . . ? C4 H3 2.02(4) . . ? C4 H5 2.04(4) . . ? C5 H4 2.07(4) . . ? C5 H6 2.05(3) . . ? C6 H5 1.99(4) . . ? N01 C03 2.494(5) . . ? N01 H011a 1.99(5) . . ? N01 H011b 2.03(5) . . ? N01 H011c 2.08(4) . . ? N01 H012a 1.95(5) . . ? N01 H012b 2.05(5) . . ? N01 H012c 1.96(4) . . ? N01 H02a 2.07(7) . . ? N01 H02b 2.04(4) . . ? N01 H03b 2.58(5) . . ? C011 C012 2.367(11) . . ? C011 C02 2.371(7) . . ? C011 H012a 2.46(5) . . ? C011 H012c 2.45(4) . . ? C011 H02a 2.55(6) . . ? C011 H02b 2.59(4) . . ? C012 C02 2.438(10) . . ? C012 H011b 2.60(6) . . ? C012 H011c 2.64(4) . . ? C012 H02b 2.64(4) . . ? C012 H03b 2.62(5) . . ? C02 N04 2.451(7) . . ? C02 H011a 2.57(4) . . ? C02 H011b 2.60(5) . . ? C02 H012a 2.54(6) . . ? C02 H012b 2.67(5) . . ? C02 H03a 2.04(4) . . ? C02 H03b 1.93(6) . . ? C03 C041 2.400(6) . . ? C03 C05 2.420(9) . . ? C03 H02a 1.94(8) . . ? C03 H02b 2.03(4) . . ? C03 H041b 2.63(3) . . ? C03 H041c 2.64(3) . . ? C03 H05b 2.48(4) . . ? N04 C06 2.492(7) . . ? N04 H02a 2.59(7) . . ? N04 H03a 2.05(4) . . ? N04 H03b 2.04(4) . . ? N04 H041a 1.94(3) . . ? N04 H041b 2.05(4) . . ? N04 H041c 2.15(4) . . ? N04 H05a 2.16(6) . . ? N04 H05b 2.01(4) . . ? C041 C05 2.403(9) . . ? C041 H03a 2.53(3) . . ? C05 N07 2.445(6) . . ? C05 H03b 2.54(5) . . ? C05 H041a 2.50(3) . . ? C05 H041b 2.65(4) . . ? C05 H06a 2.01(4) . . ? C05 H06b 2.22(6) . . ? C06 C071 2.378(8) . . ? C06 C072 2.396(8) . . ? C06 H05a 1.74(4) . . ? C06 H05b 2.03(4) . . ? C06 H071a 2.43(6) . . ? C06 H071b 2.52(5) . . ? C06 H072a 2.67(4) . . ? C06 H072b 2.58(5) . . ? N07 H05a 2.27(4) . . ? N07 H06a 2.01(3) . . ? N07 H06b 2.13(6) . . ? N07 H071a 2.01(5) . . ? N07 H071b 1.95(6) . . ? N07 H071c 2.08(7) . . ? N07 H072a 2.05(5) . . ? N07 H072b 2.02(5) . . ? N07 H072c 1.99(5) . . ? C071 C072 2.364(9) . . ? C071 H06b 2.41(7) . . ? C071 H072a 2.68(4) . . ? C071 H072c 2.51(4) . . ? C072 H05a 2.46(5) . . ? C072 H06a 2.46(3) . . ? C072 H071b 2.44(4) . . ? C072 H071c 2.44(6) . . ? H22a H22b 1.75(11) . . ? H22a H22c 1.84(10) . . ? H22a H3 2.14(7) . . ? H22b H22c 1.24(8) . . ? H23a H23b 1.57(8) . . ? H23a H23c 1.44(8) . . ? H23a H011c 2.35(8) . '3 667' ? H23b H23c 1.44(7) . . ? H24a H24b 1.31(9) . . ? H24a H24c 1.38(6) . . ? H24b H24c 1.54(8) . . ? H3 H4 2.39(7) . . ? H4 H5 2.37(5) . . ? H5 H6 2.33(5) . . ? H6 H011a 2.29(5) . . ? H6 H072c 2.38(5) . '3 667' ? H011a H011b 1.60(5) . . ? H011a H011c 1.58(6) . . ? H011a H02a 2.37(8) . . ? H011b H011c 1.74(6) . . ? H011b H012a 2.27(8) . . ? H011c H012c 2.29(5) . . ? H012a H012b 1.86(9) . . ? H012a H012c 1.65(8) . . ? H012a H02b 2.32(8) . . ? H012b H012c 1.79(6) . . ? H012b H03b 2.04(6) . . ? H012b H06b 2.28(9) . . ? H012b H071a 2.13(10) . . ? H02a H02b 1.58(6) . . ? H02a H03a 2.25(8) . . ? H02a H041c 2.12(6) . . ? H02b H03a 2.29(6) . . ? H02b H03b 2.26(8) . . ? H03a H03b 1.69(6) . . ? H03a H041b 2.35(4) . . ? H03b H06b 2.00(10) . . ? H041a H041b 1.64(5) . . ? H041a H041c 1.77(6) . . ? H041b H041c 1.68(5) . . ? H05a H05b 1.78(6) . . ? H05a H06a 2.00(6) . . ? H05a H072b 1.92(8) . . ? H05b H06a 2.29(6) . . ? H06a H06b 1.90(8) . . ? H06a H072a 2.38(5) . . ? H06b H071a 1.91(9) . . ? H071a H071b 1.74(10) . . ? H071a H071c 2.00(9) . . ? H071b H071c 1.62(8) . . ? H071c H072c 2.14(7) . . ? H072a H072b 1.44(8) . . ? H072a H072c 1.46(6) . . ? H072b H072c 1.71(8) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 792 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 10 -5 -6 10 5 6 -10 -5 -6 -10 5 5 11 -8 -5 11 8 -5 -11 8 5 -11 -8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -12 _reflns_limit_l_max 11 _reflns_number_observed 2324 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .033 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atom-block _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .091 _refine_ls_wR_factor_all .052 _refine_ls_goodness_of_fit_all 1.92 _refine_ls_shift/su_mean .0071 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_pca7 _database_code_CSD 154204 _audit_creation_method Xtal3.6 _audit_creation_date 00-05-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30 H60 N6 Na2 Si2' _chemical_formula_moiety ? _chemical_formula_weight 607.00 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C_2_2_21 _symmetry_space_group_name_Hall c_2c_2 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z +x,-y,-z -x,+y,1/2-z 1/2+x,1/2+y,+z 1/2-x,1/2-y,1/2+z 1/2+x,1/2-y,-z 1/2-x,1/2+y,1/2-z _cell_length_a 13.671(10) _cell_length_b 15.719(13) _cell_length_c 18.497(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3975(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .136 _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .95 _exptl_absorpt_correction_T_max .96 _diffrn_reflns_number 1560 _reflns_number_total 1560 _reflns_Friedel_coverage ? _reflns_number_gt 642 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .054 _refine_ls_wR_factor_ref .052 _refine_ls_goodness_of_fit_ref 2.11 _refine_ls_number_reflns 642 _refine_ls_number_parameters 187 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .017 _refine_diff_density_min -.16 _refine_diff_density_max .13 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 120 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Na ? 0 8 .030029 .025024 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 8 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 240 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na1 .50000 .8589(4) .75000 .104(7) Uani ? ? 1.00000 ? ? Na2 .50000 .6548(4) .75000 .105(7) Uani ? ? 1.00000 ? ? N1 .6354(6) .7623(7) .7497(7) .078(7) Uani ? ? 1.00000 ? ? C2 .6637(10) .7484(10) .8203(7) .065(10) Uani ? ? 1.00000 ? ? C21 .5961(11) .7468(12) .8751(7) .079(10) Uani ? ? 1.00000 ? ? Si2 .6160(3) .7331(3) .9717(2) .086(3) Uani ? ? 1.00000 ? ? C22 .4948(9) .7438(12) 1.0185(6) .143(12) Uani ? ? 1.00000 ? ? C23 .6965(11) .8244(11) 1.0077(8) .129(14) Uani ? ? 1.00000 ? ? C24 .6735(13) .6362(11) 1.0001(8) .159(17) Uani ? ? 1.00000 ? ? C3 .7653(11) .7436(9) .8326(6) .066(10) Uani ? ? 1.00000 ? ? C4 .8321(9) .7513(12) .7815(9) .083(11) Uani ? ? 1.00000 ? ? C5 .8043(13) .7679(12) .7099(9) .098(14) Uani ? ? 1.00000 ? ? C6 .7051(15) .7653(12) .6986(7) .099(12) Uani ? ? 1.00000 ? ? N01 .5122(12) .9819(8) .6691(8) .106(12) Uani ? ? 1.00000 ? ? C011 .4269(17) .9820(13) .6263(12) .20(2) Uani ? ? 1.00000 ? ? C012 .592(2) .9775(18) .6186(15) .24(3) Uani ? ? 1.00000 ? ? C01 .517(3) 1.0530(10) .7158(9) .19(2) Uani ? ? 1.00000 ? ? N02 .5814(12) .5348(11) .6965(11) .141(16) Uani ? ? 1.00000 ? ? C021 .6715(12) .5287(10) .7395(15) .173(18) Uani ? ? 1.00000 ? ? C022 .605(2) .5351(15) .6212(15) .24(3) Uani ? ? 1.00000 ? ? C02 .5212(17) .4603(12) .7122(12) .16(3) Uani ? ? 1.00000 ? ? H21 .533(5) .748(6) .862(4) .02(3) Uiso ? ? 1.00000 ? ? H22a .50030 .73518 1.06937 .22000 Uiso ? ? 1.00000 ? ? H22b .45034 .69697 1.00142 .22000 Uiso ? ? 1.00000 ? ? H22c .46346 .79467 1.00823 .22000 Uiso ? ? 1.00000 ? ? H23a .71146 .81920 1.05659 .19200 Uiso ? ? 1.00000 ? ? H23b .66497 .87907 .99946 .19200 Uiso ? ? 1.00000 ? ? H23c .75804 .82724 .98042 .19200 Uiso ? ? 1.00000 ? ? H24a .68581 .63406 1.05111 .16600 Uiso ? ? 1.00000 ? ? H24b .74268 .63320 .97853 .16600 Uiso ? ? 1.00000 ? ? H24c .64287 .58680 .98467 .16600 Uiso ? ? 1.00000 ? ? H3 .78956 .73150 .88153 .09600 Uiso ? ? 1.00000 ? ? H4 .90379 .74875 .79272 .12000 Uiso ? ? 1.00000 ? ? H5 .84892 .77679 .67023 .15300 Uiso ? ? 1.00000 ? ? H6 .68471 .76167 .64633 .12900 Uiso ? ? 1.00000 ? ? H01a .49704 1.10059 .68567 .13500 Uiso ? ? 1.00000 ? ? H01b .59227 1.06394 .71900 .13500 Uiso ? ? 1.00000 ? ? H011a .41515 1.02601 .59829 .33000 Uiso ? ? 1.00000 ? ? H011b .36685 .98109 .66389 .33000 Uiso ? ? 1.00000 ? ? H011c .41638 .92752 .60371 .33000 Uiso ? ? 1.00000 ? ? H012a .60181 1.02496 .59003 .34000 Uiso ? ? 1.00000 ? ? H012b .57676 .92908 .58279 .34000 Uiso ? ? 1.00000 ? ? H012c .65331 .95883 .63931 .34000 Uiso ? ? 1.00000 ? ? H021a .70324 .48105 .72480 .29000 Uiso ? ? 1.00000 ? ? H021b .65024 .52583 .78845 .29000 Uiso ? ? 1.00000 ? ? H021c .70382 .57953 .73028 .29000 Uiso ? ? 1.00000 ? ? H022a .63425 .48119 .61191 .42000 Uiso ? ? 1.00000 ? ? H022b .65249 .57844 .61672 .42000 Uiso ? ? 1.00000 ? ? H022c .54946 .54434 .59681 .42000 Uiso ? ? 1.00000 ? ? H02a .46879 .45707 .67784 .33000 Uiso ? ? 1.00000 ? ? H02b .56091 .40960 .70563 .33000 Uiso ? ? 1.00000 ? ? 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 Na1 .097(7) .078(5) .135(7) .00000 .026(9) .00000 Na2 .080(7) .076(5) .159(8) .00000 -.010(9) .00000 N1 .063(7) .107(8) .063(6) .009(9) -.001(7) .020(10) C2 .063(11) .067(10) .065(10) .028(10) -.007(8) .014(12) C21 .048(9) .118(12) .072(10) -.024(14) -.014(8) .036(11) Si2 .088(3) .106(4) .065(2) .005(3) -.000(2) .000(3) C22 .090(9) .251(17) .089(9) .012(19) .016(9) -.007(16) C23 .111(12) .214(17) .064(12) -.006(13) -.044(12) -.005(11) C24 .21(2) .165(15) .103(16) .018(16) -.058(16) .044(11) C3 .067(10) .073(10) .056(9) .000(12) -.004(8) .011(10) C4 .075(11) .087(12) .087(11) .004(11) -.004(9) .016(14) C5 .060(12) .107(15) .126(16) -.009(12) .020(10) -.041(14) C6 .091(12) .141(16) .065(9) .002(16) .011(10) -.014(13) N01 .114(12) .090(11) .113(12) -.011(12) -.010(12) .017(10) C011 .22(2) .119(18) .26(3) .004(17) -.15(2) .019(17) C012 .21(3) .31(3) .22(3) -.05(3) .06(3) .13(2) C01 .38(4) .066(11) .12(2) -.05(2) .01(3) .028(10) N02 .116(15) .114(14) .19(2) -.020(12) -.017(14) .028(14) C021 .089(12) .103(15) .33(3) -.006(12) -.01(2) -.01(2) C022 .27(3) .24(3) .20(3) -.08(3) .10(3) .00(2) C02 .09(2) .121(14) .28(4) .051(16) -.03(2) -.042(16) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Na1 Na2 . . 3.207(10) ? Na1 N1 . . 2.393(11) ? Na1 N01 . . 2.451(15) ? Na1 N1 . '4 656' 2.393(11) ? Na1 N01 . '4 656' 2.451(15) ? Na2 N1 . . 2.506(11) ? Na2 N02 . . 2.404(19) ? Na2 N1 . '4 656' 2.506(11) ? Na2 N02 . '4 656' 2.404(19) ? N1 C2 . . 1.379(18) ? N1 C6 . . 1.34(2) ? C2 C21 . . 1.372(19) ? C2 C3 . . 1.41(2) ? C21 Si2 . . 1.820(13) ? C21 H21 . . .89(6) ? Si2 C22 . . 1.878(13) ? Si2 C23 . . 1.927(17) ? Si2 C24 . . 1.793(18) ? C22 H22a . . .954(12) ? C22 H22b . . 1.005(16) ? C22 H22c . . .927(17) ? C23 H23a . . .931(14) ? C23 H23b . . .973(17) ? C23 H23c . . .982(15) ? C24 H24a . . .959(15) ? C24 H24b . . 1.028(17) ? C24 H24c . . .928(17) ? C3 C4 . . 1.32(2) ? C3 H3 . . .983(11) ? C4 C5 . . 1.40(2) ? C4 H4 . . 1.003(13) ? C5 C6 . . 1.37(3) ? C5 H5 . . .964(17) ? C6 H6 . . 1.007(13) ? N01 C011 . . 1.41(3) ? N01 C012 . . 1.44(3) ? N01 C01 . . 1.41(2) ? C011 H011a . . .88(2) ? C011 H011b . . 1.08(2) ? C011 H011c . . .96(2) ? C012 H012a . . .92(3) ? C012 H012b . . 1.03(3) ? C012 H012c . . .97(3) ? C01 H01a . . .971(19) ? C01 H01b . . 1.05(4) ? C01 C01 . '4 656' 1.34(3) ? N02 C021 . . 1.47(3) ? N02 C022 . . 1.43(3) ? N02 C02 . . 1.46(3) ? C021 H021a . . .907(17) ? C021 H021b . . .95(3) ? C021 H021c . . .930(16) ? C022 H022a . . .95(2) ? C022 H022b . . .94(3) ? C022 H022c . . .90(3) ? C02 H02a . . .96(2) ? C02 H02b . . .97(2) ? C02 C02 . '4 656' 1.51(3) ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Na2 Na1 N1 . . . 50.6(3) ? Na2 Na1 N01 . . . 142.1(3) ? Na2 Na1 N1 . . '4 656' 50.6(3) ? Na2 Na1 N01 . . '4 656' 142.1(3) ? N1 Na1 N01 . . . 116.5(5) ? N1 Na1 N1 . . '4 656' 101.3(4) ? N1 Na1 N01 . . '4 656' 123.7(5) ? N01 Na1 N1 . . '4 656' 123.7(5) ? N01 Na1 N01 . . '4 656' 75.8(5) ? N1 Na1 N01 '4 656' . '4 656' 116.5(5) ? Na1 Na2 N1 . . . 47.6(3) ? Na1 Na2 N02 . . . 141.7(4) ? Na1 Na2 N1 . . '4 656' 47.6(3) ? Na1 Na2 N02 . . '4 656' 141.7(4) ? N1 Na2 N02 . . . 100.7(5) ? N1 Na2 N1 . . '4 656' 95.2(4) ? N1 Na2 N02 . . '4 656' 150.7(5) ? N02 Na2 N1 . . '4 656' 150.7(5) ? N02 Na2 N02 . . '4 656' 76.6(6) ? N1 Na2 N02 '4 656' . '4 656' 100.7(5) ? Na1 N1 Na2 . . . 81.8(3) ? Na1 N1 C2 . . . 108.4(8) ? Na1 N1 C6 . . . 121.9(10) ? Na2 N1 C2 . . . 95.6(8) ? Na2 N1 C6 . . . 123.3(10) ? C2 N1 C6 . . . 118.2(11) ? N1 C2 C21 . . . 121.0(12) ? N1 C2 C3 . . . 115.9(11) ? C21 C2 C3 . . . 122.9(12) ? C2 C21 Si2 . . . 128.9(11) ? C2 C21 H21 . . . 116(4) ? Si2 C21 H21 . . . 115(4) ? C21 Si2 C22 . . . 108.0(6) ? C21 Si2 C23 . . . 109.6(7) ? C21 Si2 C24 . . . 117.0(8) ? C22 Si2 C23 . . . 106.2(7) ? C22 Si2 C24 . . . 109.1(8) ? C23 Si2 C24 . . . 106.4(7) ? Si2 C22 H22a . . . 111.8(10) ? Si2 C22 H22b . . . 108.9(11) ? Si2 C22 H22c . . . 113.0(11) ? H22a C22 H22b . . . 104.7(15) ? H22a C22 H22c . . . 111.2(15) ? H22b C22 H22c . . . 106.8(12) ? Si2 C23 H23a . . . 113.3(13) ? Si2 C23 H23b . . . 110.5(11) ? Si2 C23 H23c . . . 110.2(12) ? H23a C23 H23b . . . 109.1(15) ? H23a C23 H23c . . . 108.4(15) ? H23b C23 H23c . . . 105.0(15) ? Si2 C24 H24a . . . 113.3(13) ? Si2 C24 H24b . . . 109.2(12) ? Si2 C24 H24c . . . 115.1(13) ? H24a C24 H24b . . . 102.6(15) ? H24a C24 H24c . . . 110.6(16) ? H24b C24 H24c . . . 104.9(15) ? C2 C3 C4 . . . 124.2(12) ? C2 C3 H3 . . . 119.4(12) ? C4 C3 H3 . . . 116.3(14) ? C3 C4 C5 . . . 120.4(13) ? C3 C4 H4 . . . 121.7(16) ? C5 C4 H4 . . . 117.8(15) ? C4 C5 C6 . . . 113.9(14) ? C4 C5 H5 . . . 125.1(17) ? C6 C5 H5 . . . 120.9(16) ? N1 C6 C5 . . . 126.5(13) ? N1 C6 H6 . . . 118.5(18) ? C5 C6 H6 . . . 114.9(16) ? Na1 N01 C011 . . . 106.7(11) ? Na1 N01 C012 . . . 114.2(14) ? Na1 N01 C01 . . . 104.7(10) ? C011 N01 C012 . . . 105.2(17) ? C011 N01 C01 . . . 112(2) ? C012 N01 C01 . . . 114(2) ? N01 C011 H011a . . . 119(2) ? N01 C011 H011b . . . 105.5(18) ? N01 C011 H011c . . . 111.5(19) ? H011a C011 H011b . . . 105(2) ? H011a C011 H011c . . . 115(2) ? H011b C011 H011c . . . 98.9(19) ? N01 C012 H012a . . . 116(2) ? N01 C012 H012b . . . 107(2) ? N01 C012 H012c . . . 114(2) ? H012a C012 H012b . . . 105(3) ? H012a C012 H012c . . . 110(3) ? H012b C012 H012c . . . 102(3) ? N01 C01 H01a . . . 104.3(16) ? N01 C01 H01b . . . 102(2) ? N01 C01 C01 . . '4 656' 124.1(19) ? H01a C01 H01b . . . 100(2) ? H01a C01 C01 . . '4 656' 116(2) ? H01b C01 C01 . . '4 656' 106(2) ? Na2 N02 C021 . . . 102.5(12) ? Na2 N02 C022 . . . 120.3(14) ? Na2 N02 C02 . . . 106.6(13) ? C021 N02 C022 . . . 109.6(19) ? C021 N02 C02 . . . 108.1(16) ? C022 N02 C02 . . . 109.0(18) ? N02 C021 H021a . . . 107(2) ? N02 C021 H021b . . . 105.3(16) ? N02 C021 H021c . . . 104.0(19) ? H021a C021 H021b . . . 113(2) ? H021a C021 H021c . . . 115(2) ? H021b C021 H021c . . . 111(2) ? N02 C022 H022a . . . 106(2) ? N02 C022 H022b . . . 104(2) ? N02 C022 H022c . . . 107(2) ? H022a C022 H022b . . . 110(3) ? H022a C022 H022c . . . 114(3) ? H022b C022 H022c . . . 115(3) ? N02 C02 H02a . . . 109.3(18) ? N02 C02 H02b . . . 109(2) ? N02 C02 C02 . . '4 656' 113.5(17) ? H02a C02 H02b . . . 107(2) ? H02a C02 C02 . . '4 656' 109(2) ? H02b C02 C02 . . '4 656' 109.2(18) ? 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 #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Na1 C2 3.116(15) . . ? Na1 C2 3.116(15) . '4 656' ? Na1 C21 3.192(15) . . ? Na1 C21 3.192(15) . '4 656' ? Na1 C6 3.31(2) . . ? Na1 C6 3.31(2) . '4 656' ? Na1 C011 3.16(2) . . ? Na1 C011 3.16(2) . '4 656' ? Na1 C012 3.31(3) . '4 656' ? Na1 C012 3.31(3) . . ? Na1 C01 3.124(17) . '4 656' ? Na1 C01 3.124(17) . . ? Na1 H21 2.74(8) . '4 656' ? Na1 H21 2.74(8) . . ? Na1 H011b 3.089(4) . '4 656' ? Na1 H011b 3.089(4) . . ? Na1 H011c 3.129(3) . '4 656' ? Na1 H011c 3.129(3) . . ? Na2 C2 2.976(14) . . ? Na2 C2 2.976(14) . '4 656' ? Na2 C21 3.029(15) . '4 656' ? Na2 C21 3.029(15) . . ? Na2 C6 3.43(2) . '4 656' ? Na2 C6 3.43(2) . . ? Na2 C021 3.077(17) . '4 656' ? Na2 C021 3.077(17) . . ? Na2 C022 3.36(3) . '4 656' ? Na2 C022 3.36(3) . . ? Na2 C02 3.15(2) . . ? Na2 C02 3.15(2) . '4 656' ? Na2 H21 2.58(8) . . ? Na2 H21 2.58(8) . '4 656' ? Na2 H021b 2.973(5) . . ? Na2 H021b 2.973(5) . '4 656' ? Na2 H021c 3.049(3) . '4 656' ? Na2 H021c 3.049(3) . . ? N1 C21 2.394(17) . . ? N1 C3 2.364(17) . . ? N1 C4 2.758(16) . . ? N1 C5 2.43(2) . . ? N1 H21 2.51(7) . . ? N1 H6 2.028(12) . . ? C2 Si2 2.886(14) . . ? C2 C4 2.412(19) . . ? C2 C5 2.82(2) . . ? C2 C6 2.337(19) . . ? C2 H21 1.94(6) . . ? C2 H3 2.078(14) . . ? C21 C22 2.992(17) . . ? C21 C3 2.44(2) . . ? C21 H3 2.658(15) . . ? Si2 H21 2.34(6) . . ? Si2 H22a 2.401(4) . . ? Si2 H22b 2.399(4) . . ? Si2 H22c 2.396(4) . . ? Si2 H23a 2.449(4) . . ? Si2 H23b 2.444(5) . . ? Si2 H23c 2.446(4) . . ? Si2 H24a 2.343(4) . . ? Si2 H24b 2.341(4) . . ? Si2 H24c 2.342(5) . . ? C22 C24 2.99(2) . . ? C23 C24 2.98(2) . . ? C3 C5 2.36(2) . . ? C3 C6 2.634(18) . . ? C3 H4 2.034(14) . . ? C4 C6 2.33(2) . . ? C4 H3 1.963(17) . . ? C4 H5 2.110(17) . . ? C5 H4 2.071(17) . . ? C5 H6 2.016(17) . . ? C6 H5 2.04(2) . . ? N01 C01 2.44(2) . '4 656' ? N01 H01a 1.901(13) . . ? N01 H01b 1.926(15) . . ? N01 H011a 1.989(15) . . ? N01 H011b 1.990(16) . . ? N01 H011c 1.978(15) . . ? N01 H012a 2.024(15) . . ? N01 H012b 2.005(15) . . ? N01 H012c 2.039(16) . . ? C011 C012 2.26(4) . . ? C011 C01 2.34(3) . . ? C011 H01a 2.37(2) . . ? C011 H012a 2.57(2) . . ? C011 H012b 2.35(2) . . ? C012 C01 2.39(4) . . ? C012 H01a 2.64(3) . . ? C012 H01b 2.30(3) . . ? C012 H011a 2.56(3) . . ? C012 H011c 2.54(3) . . ? C01 H01a 1.979(17) . '4 656' ? C01 H01b 1.92(3) . '4 656' ? C01 H011a 2.61(3) . . ? C01 H011b 2.53(3) . . ? C01 H012a 2.64(2) . . ? N02 N02 2.98(3) . '4 656' ? N02 C02 2.49(3) . '4 656' ? N02 H021a 1.940(17) . . ? N02 H021b 1.95(2) . . ? N02 H021c 1.920(17) . . ? N02 H022a 1.92(2) . . ? N02 H022b 1.89(2) . . ? N02 H022c 1.90(2) . . ? N02 H02a 1.995(17) . . ? N02 H02b 1.995(18) . . ? C021 C022 2.37(4) . . ? C021 C02 2.98(3) . '4 656' ? C021 C02 2.37(3) . . ? C021 H022a 2.53(3) . . ? C021 H022b 2.42(3) . . ? C021 H02a 2.70(2) . '4 656' ? C021 H02b 2.486(17) . . ? C022 C02 2.35(3) . . ? C022 H021a 2.49(3) . . ? C022 H021c 2.52(3) . . ? C022 H02a 2.47(3) . . ? C022 H02b 2.59(3) . . ? C02 H021a 2.52(2) . . ? C02 H021b 2.56(2) . '4 656' ? C02 H021b 2.48(2) . . ? C02 H022a 2.44(2) . . ? C02 H022c 2.54(2) . . ? C02 H02a 2.04(2) . '4 656' ? C02 H02b 2.05(2) . '4 656' ? H22a H22b 1.5514(6) . . ? H22a H22c 1.5515(7) . . ? H22b H22c 1.5513(13) . . ? H23a H23b 1.5512(6) . . ? H23a H23c 1.5513(7) . . ? H23b H23c 1.5514(8) . . ? H23b H011c 2.3364(9) . '4 656' ? H24a H24b 1.5514(7) . . ? H24a H24c 1.5514(6) . . ? H24b H24c 1.5514(9) . . ? H3 H4 2.2827(10) . . ? H5 H6 2.3003(16) . . ? H01a H01a 2.3812(13) . '4 656' ? H01a H01b 2.2208(9) . '4 656' ? H01a H01b 1.5514(8) . . ? H01a H011a 2.2891(9) . . ? H01b H012c 2.3662(11) . . ? H011a H011b 1.5514(6) . . ? H011a H011c 1.5515(13) . . ? H011b H011c 1.5513(6) . . ? H011c H012b 2.2266(16) . . ? H012a H012b 1.5513(12) . . ? H012a H012c 1.5515(7) . . ? H012b H012c 1.5514(7) . . ? H021a H021b 1.5513(6) . . ? H021a H021c 1.5513(13) . . ? H021a H022a 2.2913(11) . . ? H021a H02b 2.2745(13) . . ? H021b H021c 1.5514(6) . . ? H021b H02a 2.0506(11) . '4 656' ? H021c H022b 2.2147(11) . . ? H022a H022b 1.5514(12) . . ? H022a H022c 1.5515(8) . . ? H022a H02b 2.2971(9) . . ? H022b H022c 1.5514(9) . . ? H022c H02a 2.3118(9) . . ? H02a H02b 1.5515(8) . . ? H02a H02b 2.3168(11) . '4 656' ? H02b H02b 2.3383(11) . '4 656' ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1328 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 6 7 -4 6 7 4 -6 7 4 6 -7 -4 -6 -7 4 -6 -7 -4 6 -7 -4 -6 7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .91 _reflns_d_resolution_low 10.315 _diffrn_reflns_av_sigmaI/netI .04 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .154 _refine_ls_wR_factor_all .066 _refine_ls_goodness_of_fit_all 1.58 _refine_ls_shift/su_mean .0013 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end