# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1349 data_global #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Prof. Dr. Hans H. Karsch Technische Universit\"at M\"unchen Anorganisch-chemisches Institut Lichtenbergstrasse 4 D-85747 Garching Bundesrepublik Deutschland ; _publ_contact_author_phone '049 89 2891 3132' _publ_contact_author_fax '049 89 2891 4421' _publ_contact_author_email 'Hans.H.Karsch@lrz.tu-muenchen.de' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; For deposition only. Please supply CSD-number. ; #============================================================================ # 2. PROCESSING SUMMARY (IUCr Office 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_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Phosphorus Containing Alkaline Earth Metal ate-Complexes: Synthesis and Characterization of [Mg(CH2PMe2)4][Li(TMEDA)]2, [Mg(CH2PPh2)4][Li(TMEDA)]2 and [Be2(CH2PMe2)6][Li(TMEDA)]2; ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Hans H. Karsch' ; Technische Universit\"at M\"unchen Anorganisch-chemisches Institut Lichtenbergstrasse 4 D-85747 Garching Bundesrepublik Deutschland ; 'Volker Graf' ; Technische Universit\"at M\unchen Anorganisch-chemisches Institut Lichtenbergstrasse 4 D-85747 Garching Bundesrepublik Deutschland ; 'Manfred Reisky' ; Technische Universit\"at M\"unchen Anorganisch-chemisches Institut Lichtenbergstrasse 4 D-85747 Garching Bundesrepublik Deutschland ; #============================================================================ # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_experimental ; ? ; _publ_section_references ; Kopf, J. @ R\"ubcke, H.-C. (1993). Program CADSHEL. Version 3.1. University of Hamburg, Germany. Sheldrick, G. M. (1993). Programm SHELXS-86. University of G/"ottingen, Germany Sheldrick, G. M. (1985). Crystallographic Computing 3, edited by G.M. Sheldrick, C. Kr\"uger, @ R. Goddard, pp.175-189. Oxford: Oxford University Press. Sheldrick, G. M. Program SHELXL-93. University of G\"ottingen, Germany. Sheldrick, G. M. J. Appl. Cryst. (in press). Siemens Inc. (1990). Program Package SHELXTL-PLUS. Release 4.1. Siemens Analytical X-Ray Instruments Inc. Madison (WI 53719), USA. Walker, N. @ Stuart, D. (1983). Acta Cryst. A39, 158-166. Walker, N. (1993). Program DIFABS. Version 9.0. BASF AG, Germany. ; _publ_section_figure_captions ; Fig.1 : Structure of (1). ; _publ_section_acknowledgements ; ; data_iogra1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C23 H26 K O P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H26 K O P' _chemical_formula_weight 388.51 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.432(1) _cell_length_b 19.929(1) _cell_length_c 10.026(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.56(1) _cell_angle_gamma 90.00 _cell_volume 2084.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 199(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 13 _exptl_crystal_description ? _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method ? _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 199(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4' _diffrn_measurement_method 'omega/theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 6.13 _diffrn_reflns_number 4763 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.0 _reflns_number_total 4529 _reflns_number_observed 3285 _reflns_observed_criterion >4sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'CADSHEL V3.10 (Kopf, R\"ubcke, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL(TM) PC' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.9816P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4528 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_obs 0.0363 _refine_ls_wR_factor_all 0.0993 _refine_ls_wR_factor_obs 0.0853 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.046 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K1 K 0.06358(4) 0.31278(2) 0.17934(4) 0.03256(12) Uani 1 d . . P1 P 0.29907(5) 0.40823(3) 0.29848(5) 0.03122(13) Uani 1 d . . O1 O -0.0812(2) 0.42465(8) 0.1494(2) 0.0533(4) Uani 1 d . . C11 C -0.1666(3) 0.44390(13) 0.0430(2) 0.0524(6) Uani 1 d . . H11A H -0.2476(3) 0.41821(13) 0.0479(2) 0.063 Uiso 1 calc R . H11B H -0.1267(3) 0.43521(13) -0.0445(2) 0.063 Uiso 1 calc R . C12 C -0.1916(3) 0.51719(13) 0.0602(2) 0.0530(6) Uani 1 d . . H12A H -0.2782(3) 0.52952(13) 0.0271(2) 0.064 Uiso 1 calc R . H12B H -0.1269(3) 0.54462(13) 0.0136(2) 0.064 Uiso 1 calc R . C13 C -0.1809(3) 0.52539(14) 0.2097(3) 0.0654(7) Uani 1 d . . H13A H -0.1561(3) 0.57178(14) 0.2340(3) 0.079 Uiso 1 calc R . H13B H -0.2626(3) 0.51402(14) 0.2537(3) 0.079 Uiso 1 calc R . C14 C -0.0787(3) 0.47696(14) 0.2459(3) 0.0610(7) Uani 1 d . . H14A H 0.0059(3) 0.49948(14) 0.2462(3) 0.073 Uiso 1 calc R . H14B H -0.0939(3) 0.45843(14) 0.3360(3) 0.073 Uiso 1 calc R . C21 C 0.3433(2) 0.49688(10) 0.2789(2) 0.0326(4) Uani 1 d . . C22 C 0.2665(2) 0.54706(11) 0.3333(2) 0.0428(5) Uani 1 d . . H22 H 0.1962(2) 0.53491(11) 0.3879(2) 0.051 Uiso 1 calc R . C23 C 0.2909(3) 0.61403(11) 0.3093(2) 0.0504(6) Uani 1 d . . H23 H 0.2374(3) 0.64746(11) 0.3470(2) 0.061 Uiso 1 calc R . C24 C 0.3922(3) 0.63250(12) 0.2308(2) 0.0523(6) Uani 1 d . . H24 H 0.4091(3) 0.67861(12) 0.2145(2) 0.063 Uiso 1 calc R . C25 C 0.4688(2) 0.58416(11) 0.1762(3) 0.0527(6) Uani 1 d . . H25 H 0.5389(2) 0.59681(11) 0.1219(3) 0.063 Uiso 1 calc R . C26 C 0.4444(2) 0.51683(11) 0.1997(2) 0.0440(5) Uani 1 d . . H26 H 0.4981(2) 0.48379(11) 0.1609(2) 0.053 Uiso 1 calc R . C31 C 0.4525(2) 0.36710(9) 0.2671(2) 0.0323(4) Uani 1 d . . C32 C 0.5612(2) 0.37550(11) 0.3478(2) 0.0425(5) Uani 1 d . . H32 H 0.5566(2) 0.40298(11) 0.4250(2) 0.051 Uiso 1 calc R . C33 C 0.6751(2) 0.34443(12) 0.3167(2) 0.0477(5) Uani 1 d . . H33 H 0.7482(2) 0.35043(12) 0.3726(2) 0.057 Uiso 1 calc R . C34 C 0.6830(2) 0.30480(11) 0.2050(3) 0.0498(6) Uani 1 d . . H34 H 0.7618(2) 0.28370(11) 0.1836(3) 0.060 Uiso 1 calc R . C35 C 0.5769(2) 0.29548(11) 0.1237(2) 0.0475(5) Uani 1 d . . H35 H 0.5826(2) 0.26807(11) 0.0465(2) 0.057 Uiso 1 calc R . C36 C 0.4619(2) 0.32643(10) 0.1555(2) 0.0384(5) Uani 1 d . . H36 H 0.3887(2) 0.31962(10) 0.1000(2) 0.046 Uiso 1 calc R . C1 C 0.2842(2) 0.40154(11) 0.4813(2) 0.0390(5) Uani 1 d . . H1A H 0.3594(2) 0.42308(11) 0.5245(2) 0.047 Uiso 1 calc R . H1B H 0.2066(2) 0.42603(11) 0.5099(2) 0.047 Uiso 1 calc R . C2 C 0.2754(2) 0.32866(11) 0.5279(2) 0.0396(5) Uani 1 d . . H2A H 0.3552(2) 0.30527(11) 0.5023(2) 0.048 Uiso 1 calc R . H2B H 0.2713(2) 0.32830(11) 0.6265(2) 0.048 Uiso 1 calc R . C41 C 0.1630(2) 0.28935(10) 0.4738(2) 0.0323(4) Uani 1 d . . C42 C 0.1697(2) 0.22719(10) 0.4074(2) 0.0362(4) Uani 1 d . . H42 H 0.2463(2) 0.20442(10) 0.3839(2) 0.043 Uiso 1 calc R . C43 C 0.0444(2) 0.20445(11) 0.3816(2) 0.0404(5) Uani 1 d . . H43 H 0.0214(2) 0.16387(11) 0.3378(2) 0.049 Uiso 1 calc R . C44 C -0.0398(2) 0.25212(12) 0.4318(2) 0.0409(5) Uani 1 d . . H44 H -0.1307(2) 0.24955(12) 0.4284(2) 0.049 Uiso 1 calc R . C45 C 0.0322(2) 0.30471(10) 0.4884(2) 0.0357(4) Uani 1 d . . H45 H -0.0015(2) 0.34381(10) 0.5293(2) 0.043 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0398(2) 0.0361(2) 0.0217(2) -0.0006(2) -0.0033(2) 0.0004(2) P1 0.0360(3) 0.0328(3) 0.0248(2) 0.0006(2) -0.0030(2) -0.0033(2) O1 0.0561(10) 0.0517(10) 0.0518(10) -0.0009(8) -0.0114(8) 0.0127(8) C11 0.0598(15) 0.0555(15) 0.0416(13) -0.0005(11) -0.0117(11) 0.0013(12) C12 0.063(2) 0.0546(15) 0.0418(13) 0.0059(11) 0.0018(11) 0.0086(12) C13 0.094(2) 0.058(2) 0.0440(14) -0.0060(12) 0.0046(14) 0.0099(15) C14 0.066(2) 0.067(2) 0.0496(15) -0.0048(13) -0.0168(13) 0.0012(14) C21 0.0383(10) 0.0332(10) 0.0262(9) 0.0006(8) -0.0073(8) -0.0005(8) C22 0.0489(13) 0.0415(12) 0.0379(11) -0.0026(9) 0.0000(9) 0.0028(10) C23 0.067(2) 0.0359(11) 0.0480(13) -0.0048(10) 0.0000(12) 0.0091(11) C24 0.073(2) 0.0326(12) 0.0512(14) 0.0041(10) -0.0025(12) -0.0027(11) C25 0.0575(15) 0.0385(12) 0.062(2) 0.0098(11) 0.0127(12) -0.0026(11) C26 0.0504(13) 0.0346(11) 0.0473(13) 0.0039(10) 0.0081(10) 0.0038(10) C31 0.0395(10) 0.0272(9) 0.0300(9) 0.0056(8) -0.0018(8) -0.0032(8) C32 0.0452(12) 0.0415(12) 0.0407(12) 0.0004(9) -0.0077(9) -0.0026(10) C33 0.0399(12) 0.0433(12) 0.0597(15) 0.0065(11) -0.0081(11) -0.0002(10) C34 0.0434(12) 0.0386(12) 0.067(2) 0.0083(11) 0.0102(11) 0.0026(10) C35 0.0570(14) 0.0396(12) 0.0461(13) -0.0036(10) 0.0097(11) 0.0005(10) C36 0.0470(12) 0.0345(11) 0.0336(10) 0.0007(8) -0.0012(9) -0.0030(9) C1 0.0481(12) 0.0436(12) 0.0253(9) -0.0002(9) -0.0003(8) -0.0076(10) C2 0.0456(12) 0.0470(12) 0.0261(9) 0.0079(9) -0.0042(8) -0.0041(10) C41 0.0384(10) 0.0370(10) 0.0214(9) 0.0060(8) 0.0006(8) 0.0009(8) C42 0.0466(11) 0.0393(11) 0.0227(9) 0.0046(8) 0.0023(8) 0.0093(9) C43 0.0571(13) 0.0377(11) 0.0263(10) 0.0038(8) -0.0075(9) -0.0046(10) C44 0.0373(11) 0.0536(13) 0.0318(10) 0.0145(10) -0.0054(8) -0.0023(10) C45 0.0425(11) 0.0371(11) 0.0275(9) 0.0062(8) 0.0034(8) 0.0092(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.708(2) . ? K1 C43 2.970(2) . ? K1 C44 2.991(2) 4_565 ? K1 C43 3.010(2) 4_565 ? K1 C44 3.014(2) . ? K1 C45 3.040(2) 4_565 ? K1 C42 3.052(2) . ? K1 C42 3.059(2) 4_565 ? K1 C41 3.083(2) 4_565 ? K1 C45 3.123(2) . ? K1 C41 3.155(2) . ? K1 P1 3.3200(7) . ? P1 C31 1.828(2) . ? P1 C21 1.837(2) . ? P1 C1 1.846(2) . ? O1 C14 1.422(3) . ? O1 C11 1.435(3) . ? C11 C12 1.494(4) . ? C12 C13 1.510(3) . ? C13 C14 1.481(4) . ? C21 C26 1.385(3) . ? C21 C22 1.396(3) . ? C22 C23 1.380(3) . ? C23 C24 1.375(3) . ? C24 C25 1.369(3) . ? C25 C26 1.386(3) . ? C31 C36 1.386(3) . ? C31 C32 1.397(3) . ? C32 C33 1.378(3) . ? C33 C34 1.374(3) . ? C34 C35 1.381(3) . ? C35 C36 1.389(3) . ? C1 C2 1.529(3) . ? C2 C41 1.506(3) . ? C41 C45 1.408(3) . ? C41 C42 1.409(3) . ? C41 K1 3.083(2) 4_566 ? C42 C43 1.405(3) . ? C42 K1 3.059(2) 4_566 ? C43 C44 1.391(3) . ? C43 K1 3.010(2) 4_566 ? C44 C45 1.406(3) . ? C44 K1 2.991(2) 4_566 ? C45 K1 3.040(2) 4_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 C43 129.27(6) . . ? O1 K1 C44 93.89(6) . 4_565 ? C43 K1 C44 103.07(6) . 4_565 ? O1 K1 C43 87.27(6) . 4_565 ? C43 K1 C43 126.16(3) . 4_565 ? C44 K1 C43 26.81(6) 4_565 4_565 ? O1 K1 C44 102.69(6) . . ? C43 K1 C44 26.88(6) . . ? C44 K1 C44 113.23(5) 4_565 . ? C43 K1 C44 140.03(6) 4_565 . ? O1 K1 C45 120.52(6) . 4_565 ? C43 K1 C45 82.10(6) . 4_565 ? C44 K1 C45 26.94(6) 4_565 4_565 ? C43 K1 C45 44.09(6) 4_565 4_565 ? C44 K1 C45 100.53(6) . 4_565 ? O1 K1 C42 137.83(5) . . ? C43 K1 C42 26.95(6) . . ? C44 K1 C42 120.35(6) 4_565 . ? C43 K1 C42 134.38(6) 4_565 . ? C44 K1 C42 43.68(6) . . ? C45 K1 C42 94.44(6) 4_565 . ? O1 K1 C42 108.79(6) . 4_565 ? C43 K1 C42 116.53(6) . 4_565 ? C44 K1 C42 43.80(6) 4_565 4_565 ? C43 K1 C42 26.77(6) 4_565 4_565 ? C44 K1 C42 141.24(6) . 4_565 ? C45 K1 C42 43.58(5) 4_565 4_565 ? C42 K1 C42 112.98(5) . 4_565 ? O1 K1 C41 131.33(5) . 4_565 ? C43 K1 C41 90.09(6) . 4_565 ? C44 K1 C41 44.01(5) 4_565 4_565 ? C43 K1 C41 44.06(5) 4_565 4_565 ? C44 K1 C41 114.95(6) . 4_565 ? C45 K1 C41 26.57(5) 4_565 4_565 ? C42 K1 C41 90.55(5) . 4_565 ? C42 K1 C41 26.51(5) 4_565 4_565 ? O1 K1 C45 95.09(5) . . ? C43 K1 C45 43.68(6) . . ? C44 K1 C45 139.53(6) 4_565 . ? C43 K1 C45 166.32(6) 4_565 . ? C44 K1 C45 26.41(6) . . ? C45 K1 C45 124.99(3) 4_565 . ? C42 K1 C45 43.00(5) . . ? C42 K1 C45 155.98(6) 4_565 . ? C41 K1 C45 131.93(5) 4_565 . ? O1 K1 C41 113.81(5) . . ? C43 K1 C41 43.71(5) . . ? C44 K1 C41 145.62(6) 4_565 . ? C43 K1 C41 158.35(6) 4_565 . ? C44 K1 C41 43.26(5) . . ? C45 K1 C41 120.52(6) 4_565 . ? C42 K1 C41 26.17(5) . . ? C42 K1 C41 132.62(5) 4_565 . ? C41 K1 C41 114.70(4) 4_565 . ? C45 K1 C41 25.91(5) . . ? O1 K1 P1 88.75(4) . . ? C43 K1 P1 103.02(4) . . ? C44 K1 P1 143.70(5) 4_565 . ? C43 K1 P1 117.64(5) 4_565 . ? C44 K1 P1 101.37(4) . . ? C45 K1 P1 137.95(4) 4_565 . ? C42 K1 P1 77.81(4) . . ? C42 K1 P1 101.35(4) 4_565 . ? C41 K1 P1 111.47(4) 4_565 . ? C45 K1 P1 75.93(4) . . ? C41 K1 P1 60.83(4) . . ? C31 P1 C21 101.03(9) . . ? C31 P1 C1 102.76(10) . . ? C21 P1 C1 101.49(9) . . ? C31 P1 K1 109.10(6) . . ? C21 P1 K1 134.30(6) . . ? C1 P1 K1 104.29(7) . . ? C14 O1 C11 108.5(2) . . ? C14 O1 K1 121.44(14) . . ? C11 O1 K1 130.08(14) . . ? O1 C11 C12 106.5(2) . . ? C11 C12 C13 102.1(2) . . ? C14 C13 C12 102.6(2) . . ? O1 C14 C13 107.6(2) . . ? C26 C21 C22 117.5(2) . . ? C26 C21 P1 122.1(2) . . ? C22 C21 P1 120.1(2) . . ? C23 C22 C21 121.1(2) . . ? C24 C23 C22 120.2(2) . . ? C25 C24 C23 119.7(2) . . ? C24 C25 C26 120.3(2) . . ? C21 C26 C25 121.2(2) . . ? C36 C31 C32 118.3(2) . . ? C36 C31 P1 118.1(2) . . ? C32 C31 P1 123.6(2) . . ? C33 C32 C31 120.8(2) . . ? C34 C33 C32 120.1(2) . . ? C33 C34 C35 120.3(2) . . ? C34 C35 C36 119.6(2) . . ? C31 C36 C35 120.9(2) . . ? C2 C1 P1 112.19(14) . . ? C41 C2 C1 115.7(2) . . ? C45 C41 C42 107.0(2) . . ? C45 C41 C2 127.0(2) . . ? C42 C41 C2 125.8(2) . . ? C45 C41 K1 75.02(11) . 4_566 ? C42 C41 K1 75.77(11) . 4_566 ? C2 C41 K1 111.63(11) . 4_566 ? C45 C41 K1 75.77(11) . . ? C42 C41 K1 72.84(10) . . ? C2 C41 K1 120.49(12) . . ? K1 C41 K1 127.84(7) 4_566 . ? C43 C42 C41 108.7(2) . . ? C43 C42 K1 73.27(11) . . ? C41 C42 K1 80.99(11) . . ? C43 C42 K1 74.68(11) . 4_566 ? C41 C42 K1 77.72(10) . 4_566 ? K1 C42 K1 132.96(7) . 4_566 ? C44 C43 C42 107.6(2) . . ? C44 C43 K1 78.32(12) . . ? C42 C43 K1 79.78(11) . . ? C44 C43 K1 75.83(11) . 4_566 ? C42 C43 K1 78.55(11) . 4_566 ? K1 C43 K1 139.10(8) . 4_566 ? C43 C44 C45 108.6(2) . . ? C43 C44 K1 77.36(11) . 4_566 ? C45 C44 K1 78.50(11) . 4_566 ? C43 C44 K1 74.80(11) . . ? C45 C44 K1 81.12(12) . . ? K1 C44 K1 137.85(8) 4_566 . ? C44 C45 C41 108.1(2) . . ? C44 C45 K1 74.56(11) . 4_566 ? C41 C45 K1 78.42(11) . 4_566 ? C44 C45 K1 72.47(11) . . ? C41 C45 K1 78.32(11) . . ? K1 C45 K1 130.76(7) 4_566 . ? _refine_diff_density_max 0.345 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.048