Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Michael Guy Gardiner' 'Evan J. Peacock' 'Brian W. Skelton' 'Jun Wang' _publ_contact_author_name 'Dr Michael Guy Gardiner' _publ_contact_author_address ; Dr Michael Guy Gardiner School of Chemistry University of Tasmania GPO Box 252-75 Hobart TAS 7001 AUSTRALIA ; _publ_contact_author_email MICHAEL.GARDINER@UTAS.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Tailoring porphyrinogens for structural control of their metallo- derivatives: steric blocking of the macrocyclic cavity through trans-N,N'-dimethylation ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. 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. ; data_mgjw4 _database_code_CSD 196192 _audit_creation_method Xtal3.6 _audit_creation_date 01-11-11 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H80 K2 N6 O2' _chemical_formula_moiety ? _chemical_formula_weight 851.4 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 12.194(3) _cell_length_b 12.608(3) _cell_length_c 17.834(5) _cell_angle_alpha 80.359(4) _cell_angle_beta 80.055(4) _cell_angle_gamma 68.724(4) _cell_volume 2500.1(11) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5105 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 17.5 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .231 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .31 _exptl_crystal_size_min .27 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .58 _exptl_absorpt_correction_T_max .89 _diffrn_reflns_number 24183 _reflns_number_total 8738 _reflns_Friedel_coverage 0 _reflns_number_gt 6008 _reflns_threshold_expression 'F > 4.00 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 .053 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .086 _refine_ls_wR_factor_ref .114 _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_number_reflns 5825 _refine_ls_number_parameters 550 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .014 _refine_diff_density_min -.578 _refine_diff_density_max 1.153 _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 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _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 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' K ? 0 4 .179 .25 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 '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 K1 .30150(9) .85726(9) .29376(6) .0376(9) Uani ? ? 1.00000 ? ? K2 .12776(9) .70194(9) .21126(6) .0378(9) Uani ? ? 1.00000 ? ? O11 .1592(3) .9376(3) .1624(2) .046(3) Uani ? ? 1.00000 ? ? C12 .0402(5) .9671(4) .1719(3) .041(4) Uani ? ? 1.00000 ? ? C13 .0028(5) .9394(5) .1128(3) .048(5) Uani ? ? 1.00000 ? ? C14 .1065(5) .8860(5) .0632(3) .047(5) Uani ? ? 1.00000 ? ? C15 .1997(5) .8852(4) .0951(3) .042(4) Uani ? ? 1.00000 ? ? C1 .3299(5) .8516(5) .0682(3) .046(5) Uani ? ? 1.00000 ? ? C111 .3604(5) .9624(6) .0466(3) .062(6) Uani ? ? 1.00000 ? ? C112 .2921(6) 1.0484(7) -.0152(4) .076(7) Uani ? ? 1.00000 ? ? C121 .3597(6) .7827(7) -.0006(3) .069(6) Uani ? ? 1.00000 ? ? C122 .4896(7) .7411(9) -.0310(4) .101(9) Uani ? ? 1.00000 ? ? N21 .0372(3) .8613(3) .3296(2) .032(3) Uani ? ? 1.00000 ? ? C22 .0758(4) .8291(5) .4014(3) .042(5) Uani ? ? 1.00000 ? ? C23 .0888(5) .9192(5) .4266(3) .048(5) Uani ? ? 1.00000 ? ? C24 .0548(5) 1.0135(5) .3689(3) .049(5) Uani ? ? 1.00000 ? ? C25 .0244(4) .9744(4) .3110(3) .041(4) Uani ? ? 1.00000 ? ? C2 -.0264(4) 1.0349(4) .2384(3) .045(5) Uani ? ? 1.00000 ? ? C211 -.0143(5) 1.1551(5) .2219(4) .057(5) Uani ? ? 1.00000 ? ? C212 -.0527(6) 1.2207(5) .1453(4) .072(6) Uani ? ? 1.00000 ? ? C221 -.1582(5) 1.0441(5) .2471(3) .054(5) Uani ? ? 1.00000 ? ? C222 -.2336(6) 1.1034(7) .3153(5) .081(7) Uani ? ? 1.00000 ? ? O31 .2719(3) .6325(3) .3500(2) .047(3) Uani ? ? 1.00000 ? ? C32 .3268(4) .5412(4) .3085(3) .041(4) Uani ? ? 1.00000 ? ? C33 .2576(5) .4768(4) .3168(3) .047(5) Uani ? ? 1.00000 ? ? C34 .1549(5) .5283(5) .3656(3) .044(5) Uani ? ? 1.00000 ? ? C35 .1656(4) .6233(5) .3849(3) .040(4) Uani ? ? 1.00000 ? ? C3 .0903(4) .7090(5) .4378(3) .040(4) Uani ? ? 1.00000 ? ? C311 .1528(5) .6878(5) .5109(3) .051(5) Uani ? ? 1.00000 ? ? C312 .1701(7) .5725(7) .5549(3) .075(7) Uani ? ? 1.00000 ? ? C321 -.0329(5) .6965(5) .4582(3) .044(5) Uani ? ? 1.00000 ? ? C322 -.1172(6) .7733(6) .5161(4) .068(7) Uani ? ? 1.00000 ? ? N41 .3727(3) .6883(3) .1702(2) .034(3) Uani ? ? 1.00000 ? ? C42 .4006(4) .7796(5) .1316(3) .040(4) Uani ? ? 1.00000 ? ? C43 .4992(5) .7835(5) .1560(3) .046(5) Uani ? ? 1.00000 ? ? C44 .5326(4) .6905(5) .2132(3) .047(5) Uani ? ? 1.00000 ? ? C45 .4544(4) .6350(4) .2216(3) .039(4) Uani ? ? 1.00000 ? ? C4 .4506(4) .5258(4) .2700(3) .044(5) Uani ? ? 1.00000 ? ? C411 .5329(5) .4986(5) .3328(4) .057(5) Uani ? ? 1.00000 ? ? C412 .5332(6) .3945(6) .3886(4) .080(7) Uani ? ? 1.00000 ? ? C421 .4900(5) .4297(5) .2190(4) .060(6) Uani ? ? 1.00000 ? ? C422 .6149(6) .4044(7) .1771(5) .090(8) Uani ? ? 1.00000 ? ? N101 .4007(5) 1.0506(4) .2782(3) .060(5) Uani ? ? 1.00000 ? ? C1011 .4997(7) 1.0446(7) .2180(4) .080(8) Uani ? ? 1.00000 ? ? C1012 .3028(7) 1.1491(6) .2572(5) .084(8) Uani ? ? 1.00000 ? ? C101 .4334(6) 1.0535(6) .3524(4) .069(7) Uani ? ? 1.00000 ? ? C102 .5188(6) .9452(7) .3847(4) .066(7) Uani ? ? 1.00000 ? ? N102 .4714(5) .8537(5) .4042(3) .067(6) Uani ? ? 1.00000 ? ? C1021 .5694(9) .7479(7) .4203(4) .102(10) Uani ? ? 1.00000 ? ? C1022 .3894(7) .8697(7) .4743(4) .078(8) Uani ? ? 1.00000 ? ? N201 -.0848(5) .6523(6) .2017(3) .068(6) Uani ? ? 1.00000 ? ? C2011 -.1439(13) .6506(17) .2756(8) .070(15) Uani ? ? .50000 ? ? C2012 -.1650(12) .7440(13) .1537(8) .056(13) Uani ? ? .50000 ? ? C201 -.0595(14) .5470(12) .1677(11) .065(15) Uani ? ? .50000 ? ? C2011' -.1125(14) .5740(15) .2686(10) .070(16) Uani ? ? .50000 ? ? C2012' -.1746(17) .7607(17) .2050(13) .09(2) Uani ? ? .50000 ? ? C201' -.095(3) .612(3) .1349(13) .16(4) Uani ? ? .50000 ? ? C202 .0236(10) .5325(10) .0999(6) .123(14) Uani ? ? 1.00000 ? ? N202 .1392(6) .5320(6) .1024(4) .085(7) Uani ? ? 1.00000 ? ? C2021 .2006(10) .4111(9) .1334(6) .118(12) Uani ? ? 1.00000 ? ? C2022 .1987(15) .5568(13) .0292(6) .17(2) Uani ? ? 1.00000 ? ? H13 -.07766 .95062 .10718 .06200 Uiso ? ? 1.00000 ? ? H14 .11093 .85579 .01671 .06100 Uiso ? ? 1.00000 ? ? H111a .44275 .94275 .03113 .07400 Uiso ? ? 1.00000 ? ? H111b .34198 1.00037 .09258 .07400 Uiso ? ? 1.00000 ? ? H112a .31481 1.11368 -.02618 .12000 Uiso ? ? 1.00000 ? ? H112b .20965 1.06981 -.00058 .12000 Uiso ? ? 1.00000 ? ? H112c .31042 1.01218 -.06203 .12000 Uiso ? ? 1.00000 ? ? H121a .31459 .82961 -.04023 .09600 Uiso ? ? 1.00000 ? ? H121b .33278 .71871 .01558 .09600 Uiso ? ? 1.00000 ? ? H122a .50319 .69687 -.07439 .15900 Uiso ? ? 1.00000 ? ? H122b .53638 .69086 .00647 .15900 Uiso ? ? 1.00000 ? ? H122c .51819 .80176 -.04934 .15900 Uiso ? ? 1.00000 ? ? H23 .11442 .92014 .47385 .06500 Uiso ? ? 1.00000 ? ? H24 .05156 1.09077 .37051 .06100 Uiso ? ? 1.00000 ? ? H211a .06647 1.14648 .22173 .07900 Uiso ? ? 1.00000 ? ? H211b -.06073 1.19969 .26171 .07900 Uiso ? ? 1.00000 ? ? H212a -.04293 1.29320 .13918 .10300 Uiso ? ? 1.00000 ? ? H212b -.13387 1.23225 .14478 .10300 Uiso ? ? 1.00000 ? ? H212c -.00665 1.17904 .10479 .10300 Uiso ? ? 1.00000 ? ? H221a -.16110 .96795 .24921 .07700 Uiso ? ? 1.00000 ? ? H221b -.19111 1.08562 .20031 .07700 Uiso ? ? 1.00000 ? ? H222a -.31401 1.10514 .31984 .13600 Uiso ? ? 1.00000 ? ? H222b -.23312 1.17705 .31355 .13600 Uiso ? ? 1.00000 ? ? H222c -.20311 1.05938 .36245 .13600 Uiso ? ? 1.00000 ? ? H33 .27636 .40726 .29195 .06200 Uiso ? ? 1.00000 ? ? H34 .08858 .50181 .37984 .06000 Uiso ? ? 1.00000 ? ? H311a .10327 .74353 .54436 .06900 Uiso ? ? 1.00000 ? ? H311b .22576 .69997 .49620 .06900 Uiso ? ? 1.00000 ? ? H312a .21042 .56224 .59770 .11800 Uiso ? ? 1.00000 ? ? H312b .22213 .51424 .52120 .11800 Uiso ? ? 1.00000 ? ? H312c .09964 .55780 .56936 .11800 Uiso ? ? 1.00000 ? ? H321a -.02256 .61813 .47868 .05900 Uiso ? ? 1.00000 ? ? H321b -.06820 .71029 .41170 .05900 Uiso ? ? 1.00000 ? ? H322a -.19268 .76219 .52532 .10100 Uiso ? ? 1.00000 ? ? H322b -.13195 .85199 .49548 .10100 Uiso ? ? 1.00000 ? ? H322c -.08631 .75984 .56245 .10100 Uiso ? ? 1.00000 ? ? H43 .53643 .84150 .13743 .05800 Uiso ? ? 1.00000 ? ? H44 .60020 .66909 .24028 .06100 Uiso ? ? 1.00000 ? ? H411a .50830 .56249 .36163 .07000 Uiso ? ? 1.00000 ? ? H411b .61214 .48739 .30926 .07000 Uiso ? ? 1.00000 ? ? H412a .58406 .38101 .42556 .12100 Uiso ? ? 1.00000 ? ? H412b .55874 .32891 .36069 .12100 Uiso ? ? 1.00000 ? ? H412c .45491 .40401 .41305 .12100 Uiso ? ? 1.00000 ? ? H421a .43627 .44726 .18247 .07800 Uiso ? ? 1.00000 ? ? H421b .48754 .36048 .25053 .07800 Uiso ? ? 1.00000 ? ? H422a .63436 .34516 .14633 .13400 Uiso ? ? 1.00000 ? ? H422b .66986 .38575 .21269 .13400 Uiso ? ? 1.00000 ? ? H422c .61859 .47252 .14463 .13400 Uiso ? ? 1.00000 ? ? H1011a .56932 .97924 .22993 .13700 Uiso ? ? 1.00000 ? ? H1011b .52338 1.11091 .21322 .13700 Uiso ? ? 1.00000 ? ? H1011c .48353 1.03838 .16910 .13700 Uiso ? ? 1.00000 ? ? H1012a .23579 1.15258 .29626 .13700 Uiso ? ? 1.00000 ? ? H1012b .28026 1.14341 .21005 .13700 Uiso ? ? 1.00000 ? ? H1012c .32011 1.21594 .25416 .13700 Uiso ? ? 1.00000 ? ? H101a .36467 1.07291 .38920 .09500 Uiso ? ? 1.00000 ? ? H101b .46770 1.11308 .34828 .09500 Uiso ? ? 1.00000 ? ? H102a .54593 .95659 .42926 .08500 Uiso ? ? 1.00000 ? ? H102b .58863 .92230 .34698 .08500 Uiso ? ? 1.00000 ? ? H1021a .54087 .68448 .43315 .15500 Uiso ? ? 1.00000 ? ? H1021b .60548 .75225 .46177 .15500 Uiso ? ? 1.00000 ? ? H1021c .62704 .73261 .37626 .15500 Uiso ? ? 1.00000 ? ? H1022a .35537 .81215 .48622 .12300 Uiso ? ? 1.00000 ? ? H1022b .32495 .94244 .46519 .12300 Uiso ? ? 1.00000 ? ? H1022c .42543 .87458 .51492 .12300 Uiso ? ? 1.00000 ? ? H2011a -.21117 .62784 .27571 .09200 Uiso ? ? .50000 ? ? H2011b -.16457 .71826 .29485 .09200 Uiso ? ? .50000 ? ? H2011c -.09047 .58889 .30778 .09200 Uiso ? ? .50000 ? ? H2012a -.22944 .72311 .14719 .07400 Uiso ? ? .50000 ? ? H2012b -.12227 .75606 .10437 .07400 Uiso ? ? .50000 ? ? H2012c -.19314 .81305 .17681 .07400 Uiso ? ? .50000 ? ? H201a -.13182 .54799 .15414 .08400 Uiso ? ? .50000 ? ? H201b -.02829 .48498 .20307 .08400 Uiso ? ? .50000 ? ? H202a -.01244 .59125 .06069 .15200 Uiso ? ? .50000 ? ? H202b .03049 .45994 .08441 .15200 Uiso ? ? .50000 ? ? H201'a -.13133 .67862 .09681 .07100 Uiso ? ? .50000 ? ? H201'b -.15673 .57463 .14630 .22100 Uiso ? ? .50000 ? ? H202'a .01710 .53854 .04635 .15200 Uiso ? ? .50000 ? ? H202'b .02470 .45751 .12250 .15200 Uiso ? ? .50000 ? ? H2011'a -.18367 .56176 .26589 .10100 Uiso ? ? .50000 ? ? H2011'b -.11646 .60175 .31546 .10100 Uiso ? ? .50000 ? ? H2011'c -.04872 .49895 .26864 .10100 Uiso ? ? .50000 ? ? H2012'a -.25230 .75911 .20529 .07400 Uiso ? ? .50000 ? ? H2012'b -.16248 .81539 .16087 .07400 Uiso ? ? .50000 ? ? H2012'c -.17568 .79581 .24971 .07400 Uiso ? ? .50000 ? ? H2021a .28383 .39520 .13678 .18700 Uiso ? ? 1.00000 ? ? H2021b .20291 .35883 .09641 .18700 Uiso ? ? 1.00000 ? ? H2021c .16532 .38735 .18022 .18700 Uiso ? ? 1.00000 ? ? H2022a .27755 .55348 .03120 .24600 Uiso ? ? 1.00000 ? ? H2022b .15731 .62523 .00219 .24600 Uiso ? ? 1.00000 ? ? H2022c .20911 .49515 -.00316 .24600 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 K1 .0433(6) .0448(6) .0256(6) -.0163(5) -.0014(4) -.0065(4) K2 .0422(6) .0462(6) .0269(6) -.0175(5) -.0069(5) -.0017(5) O11 .045(2) .055(2) .037(2) -.0170(17) .0012(16) -.0066(17) C12 .044(3) .047(3) .035(3) -.023(2) -.004(2) .006(2) C13 .045(3) .059(3) .039(3) -.020(3) -.013(2) .007(3) C14 .058(3) .064(4) .024(3) -.026(3) -.011(2) .001(2) C15 .052(3) .052(3) .022(2) -.020(2) -.003(2) -.002(2) C1 .049(3) .069(4) .021(2) -.022(3) -.004(2) -.000(2) C111 .056(4) .079(4) .046(3) -.031(3) -.003(3) .018(3) C112 .068(4) .100(5) .047(4) -.030(4) -.007(3) .028(4) C121 .070(4) .109(5) .022(3) -.022(4) .001(3) -.023(3) C122 .081(5) .160(8) .043(4) -.013(5) .013(4) -.047(5) N21 .039(2) .041(2) .0197(19) -.0183(17) -.0027(16) -.0051(16) C22 .040(3) .058(3) .031(3) -.020(2) -.006(2) -.005(2) C23 .058(3) .060(3) .030(3) -.026(3) .000(2) -.014(3) C24 .059(3) .048(3) .048(3) -.024(3) .005(3) -.021(3) C25 .039(3) .045(3) .034(3) -.012(2) .003(2) -.009(2) C2 .038(3) .043(3) .048(3) -.010(2) -.001(2) -.006(2) C211 .058(4) .040(3) .066(4) -.011(3) -.008(3) .000(3) C212 .080(5) .043(3) .074(5) -.008(3) -.011(4) .015(3) C221 .041(3) .061(4) .049(3) -.008(3) .001(3) -.002(3) C222 .047(4) .090(5) .093(6) -.008(3) .016(4) -.035(4) O31 .047(2) .056(2) .037(2) -.0178(18) -.0079(16) -.0009(17) C32 .042(3) .038(3) .037(3) -.004(2) -.010(2) .001(2) C33 .052(3) .040(3) .051(3) -.018(3) -.009(3) -.001(2) C34 .045(3) .049(3) .042(3) -.026(2) -.006(2) .005(2) C35 .042(3) .056(3) .025(2) -.023(2) -.004(2) -.000(2) C3 .049(3) .057(3) .021(2) -.028(2) -.006(2) -.000(2) C311 .066(4) .074(4) .026(3) -.036(3) -.014(3) -.005(3) C312 .100(5) .106(5) .037(3) -.060(4) -.034(3) .025(3) C321 .047(3) .064(3) .025(3) -.023(3) -.001(2) -.009(2) C322 .065(4) .102(5) .049(4) -.042(4) .015(3) -.035(4) N41 .040(2) .043(2) .020(2) -.0163(18) -.0017(16) -.0051(17) C42 .041(3) .057(3) .017(2) -.012(2) .005(2) -.013(2) C43 .041(3) .062(3) .033(3) -.023(3) .006(2) -.004(2) C44 .036(3) .061(3) .037(3) -.012(2) -.004(2) .001(3) C45 .035(3) .050(3) .027(3) -.011(2) -.002(2) -.006(2) C4 .040(3) .043(3) .045(3) -.011(2) -.004(2) -.001(2) C411 .045(3) .064(4) .055(4) -.016(3) -.018(3) .018(3) C412 .070(4) .080(5) .076(5) -.017(4) -.032(4) .034(4) C421 .051(3) .052(3) .066(4) -.005(3) .002(3) -.022(3) C422 .063(4) .091(5) .105(6) -.013(4) .026(4) -.051(5) N101 .069(3) .061(3) .057(3) -.031(3) -.005(3) -.009(2) C1011 .092(5) .107(6) .047(4) -.049(5) .009(4) -.014(4) C1012 .076(5) .063(4) .112(7) -.021(4) -.022(4) -.007(4) C101 .083(5) .080(5) .060(4) -.041(4) .002(4) -.028(4) C102 .075(4) .092(5) .043(3) -.044(4) -.005(3) -.009(3) N102 .092(4) .074(4) .046(3) -.036(3) -.015(3) -.011(3) C1021 .153(8) .086(6) .052(4) -.015(5) -.022(5) -.017(4) C1022 .084(5) .097(5) .064(5) -.049(4) -.014(4) .007(4) N201 .063(3) .106(5) .044(3) -.043(3) -.014(3) .006(3) C2011 .057(9) .097(12) .042(8) -.008(9) -.015(6) -.003(9) C2012 .055(8) .071(9) .049(8) -.028(6) -.009(7) -.005(7) C201 .057(8) .054(8) .095(14) -.021(7) -.014(8) -.023(8) C2011' .057(9) .083(11) .072(10) -.031(9) -.022(8) .014(9) C2012' .084(12) .094(13) .103(15) -.044(11) -.027(12) .041(12) C201' .17(3) .22(3) .065(14) -.03(2) .006(14) -.093(18) C202 .123(8) .155(10) .126(9) -.067(7) -.008(7) -.074(8) N202 .093(5) .104(5) .061(4) -.034(4) -.002(3) -.030(4) C2021 .139(9) .112(8) .092(7) -.020(6) -.017(6) -.032(6) C2022 .291(18) .219(14) .073(7) -.185(14) .038(9) -.019(8) # 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 K1 O11 . . 2.976(4) ? K1 N21 . . 3.159(4) ? K1 C22 . . 3.169(5) ? K1 C23 . . 3.159(5) ? K1 C24 . . 3.149(5) ? K1 C25 . . 3.141(5) ? K1 O31 . . 2.972(4) ? K1 N41 . . 3.118(4) ? K1 C42 . . 3.108(5) ? K1 C43 . . 3.131(5) ? K1 C44 . . 3.121(5) ? K1 C45 . . 3.094(5) ? K1 N101 . . 3.046(7) ? K1 N102 . . 3.080(7) ? K2 O11 . . 3.095(4) ? K2 C12 . . 3.113(5) ? K2 C13 . . 3.197(5) ? K2 C14 . . 3.190(5) ? K2 C15 . . 3.105(6) ? K2 N21 . . 2.952(4) ? K2 O31 . . 3.105(4) ? K2 C32 . . 3.117(5) ? K2 C33 . . 3.175(5) ? K2 C35 . . 3.149(5) ? K2 N41 . . 2.898(4) ? K2 N201 . . 2.916(7) ? K2 N202 . . 3.076(8) ? O11 C12 . . 1.349(6) ? O11 C15 . . 1.394(6) ? C12 C13 . . 1.358(9) ? C12 C2 . . 1.516(7) ? C13 C14 . . 1.426(7) ? C13 H13 . . .959 ? C14 C15 . . 1.353(9) ? C14 H14 . . .954 ? C15 C1 . . 1.500(7) ? C1 C111 . . 1.545(10) ? C1 C121 . . 1.538(9) ? C1 C42 . . 1.507(7) ? C111 C112 . . 1.531(9) ? C111 H111a . . .945 ? C111 H111b . . .971 ? C112 H112a . . .941 ? C112 H112b . . .942 ? C112 H112c . . .973 ? C121 C122 . . 1.508(10) ? C121 H121a . . .953 ? C121 H121b . . .961 ? C122 H122a . . .985 ? C122 H122b . . .949 ? C122 H122c . . .940 ? N21 C22 . . 1.387(6) ? N21 C25 . . 1.366(7) ? C22 C23 . . 1.358(10) ? C22 C3 . . 1.504(8) ? C23 C24 . . 1.424(7) ? C23 H23 . . .951 ? C24 C25 . . 1.372(9) ? C24 H24 . . .965 ? C25 C2 . . 1.500(7) ? C2 C211 . . 1.550(9) ? C2 C221 . . 1.551(8) ? C211 C212 . . 1.528(9) ? C211 H211a . . .951 ? C211 H211b . . .951 ? C212 H212a . . .950 ? C212 H212b . . .948 ? C212 H212c . . .941 ? C221 C222 . . 1.518(9) ? C221 H221a . . .968 ? C221 H221b . . .974 ? C222 H222a . . .962 ? C222 H222b . . .926 ? C222 H222c . . .977 ? O31 C32 . . 1.371(6) ? O31 C35 . . 1.373(7) ? C32 C33 . . 1.344(9) ? C32 C4 . . 1.504(7) ? C33 C34 . . 1.404(7) ? C33 H33 . . .984 ? C34 C35 . . 1.355(9) ? C34 H34 . . .963 ? C35 C3 . . 1.492(7) ? C3 C311 . . 1.559(8) ? C3 C321 . . 1.542(8) ? C311 C312 . . 1.492(10) ? C311 H311a . . .960 ? C311 H311b . . .943 ? C312 H312a . . .943 ? C312 H312b . . .991 ? C312 H312c . . .929 ? C321 C322 . . 1.519(8) ? C321 H321a . . .965 ? C321 H321b . . .960 ? C322 H322a . . .963 ? C322 H322b . . .961 ? C322 H322c . . .931 ? N41 C42 . . 1.361(7) ? N41 C45 . . 1.382(6) ? C42 C43 . . 1.367(9) ? C43 C44 . . 1.406(7) ? C43 H43 . . .979 ? C44 C45 . . 1.350(9) ? C44 H44 . . .957 ? C45 C4 . . 1.509(7) ? C4 C411 . . 1.544(9) ? C4 C421 . . 1.525(9) ? C411 C412 . . 1.508(10) ? C411 H411a . . .956 ? C411 H411b . . .954 ? C412 H412a . . .936 ? C412 H412b . . .962 ? C412 H412c . . .953 ? C421 C422 . . 1.521(9) ? C421 H421a . . .947 ? C421 H421b . . .963 ? C422 H422a . . .937 ? C422 H422b . . .944 ? C422 H422c . . .962 ? N101 C1011 . . 1.460(9) ? N101 C1012 . . 1.425(8) ? N101 C101 . . 1.456(10) ? C1011 H1011a . . .970 ? C1011 H1011b . . .965 ? C1011 H1011c . . .948 ? C1012 H1012a . . .971 ? C1012 H1012b . . .949 ? C1012 H1012c . . .932 ? C101 C102 . . 1.481(9) ? C101 H101a . . .953 ? C101 H101b . . .971 ? C102 N102 . . 1.437(11) ? C102 H102a . . .963 ? C102 H102b . . .974 ? N102 C1021 . . 1.457(10) ? N102 C1022 . . 1.452(9) ? C1021 H1021a . . .962 ? C1021 H1021b . . .942 ? C1021 H1021c . . .954 ? C1022 H1022a . . .938 ? C1022 H1022b . . .977 ? C1022 H1022c . . .931 ? N201 C2011 . . 1.390(15) ? N201 C2012 . . 1.470(14) ? N201 C201 . . 1.46(2) ? N201 C2011' . . 1.491(18) ? N201 C2012' . . 1.410(18) ? N201 C201' . . 1.41(3) ? C2011 H2011a . . .96 ? C2011 H2011b . . .91 ? C2011 H2011c . . .986 ? C2012 H2012a . . .944 ? C2012 H2012b . . .960 ? C2012 H2012c . . .949 ? C201 C202 . . 1.43(2) ? C201 H201a . . .949 ? C201 H201b . . .926 ? C2011' H2011'a . . .95 ? C2011' H2011'b . . .95 ? C2011' H2011'c . . .983 ? C2012' H2012'a . . .95 ? C2012' H2012'b . . .98 ? C2012' H2012'c . . .97 ? C201' C202 . . 1.53(3) ? C201' H201'a . . 1.00 ? C201' H201'b . . 1.00 ? C202 N202 . . 1.416(16) ? C202 H202a . . .963 ? C202 H202b . . .969 ? C202 H202'a . . .960 ? C202 H202'b . . .959 ? N202 C2021 . . 1.490(12) ? N202 C2022 . . 1.424(14) ? C2021 H2021a . . .971 ? C2021 H2021b . . .998 ? C2021 H2021c . . .926 ? C2022 H2022a . . .95 ? C2022 H2022b . . .927 ? C2022 H2022c . . 1.004 ? 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 O11 K1 N21 . . . 63.93(10) ? O11 K1 C22 . . . 89.19(12) ? O11 K1 C23 . . . 97.77(13) ? O11 K1 C24 . . . 77.68(13) ? O11 K1 C25 . . . 56.11(12) ? O11 K1 O31 . . . 101.85(12) ? O11 K1 N41 . . . 64.95(10) ? O11 K1 C42 . . . 57.15(11) ? O11 K1 C43 . . . 78.81(12) ? O11 K1 C44 . . . 98.82(12) ? O11 K1 C45 . . . 90.61(12) ? O11 K1 N101 . . . 99.38(13) ? O11 K1 N102 . . . 158.71(15) ? N21 K1 C22 . . . 25.32(12) ? N21 K1 C23 . . . 41.71(15) ? N21 K1 C24 . . . 41.63(15) ? N21 K1 C25 . . . 25.04(13) ? N21 K1 O31 . . . 64.27(10) ? N21 K1 N41 . . . 94.25(12) ? N21 K1 C42 . . . 107.84(14) ? N21 K1 C43 . . . 132.97(15) ? N21 K1 C44 . . . 133.00(15) ? N21 K1 C45 . . . 108.19(14) ? N21 K1 N101 . . . 130.38(12) ? N21 K1 N102 . . . 129.49(13) ? C22 K1 C23 . . . 24.79(17) ? C22 K1 C24 . . . 41.35(15) ? C22 K1 C25 . . . 40.95(12) ? C22 K1 O31 . . . 56.22(12) ? C22 K1 N41 . . . 108.08(15) ? C22 K1 C42 . . . 128.06(17) ? C22 K1 C43 . . . 149.95(18) ? C22 K1 C44 . . . 135.10(16) ? C22 K1 C45 . . . 111.82(15) ? C22 K1 N101 . . . 128.31(15) ? C22 K1 N102 . . . 104.89(15) ? C23 K1 C24 . . . 26.09(13) ? C23 K1 C25 . . . 41.73(14) ? C23 K1 O31 . . . 77.22(13) ? C23 K1 N41 . . . 132.69(16) ? C23 K1 C42 . . . 149.53(17) ? C23 K1 C43 . . . 174.5(2) ? C23 K1 C44 . . . 153.25(14) ? C23 K1 C45 . . . 134.49(16) ? C23 K1 N101 . . . 103.78(16) ? C23 K1 N102 . . . 89.45(16) ? C24 K1 C25 . . . 25.19(17) ? C24 K1 O31 . . . 97.53(13) ? C24 K1 N41 . . . 132.83(16) ? C24 K1 C42 . . . 134.79(15) ? C24 K1 C43 . . . 153.48(14) ? C24 K1 C44 . . . 174.5(2) ? C24 K1 C45 . . . 149.75(18) ? C24 K1 N101 . . . 90.74(16) ? C24 K1 N102 . . . 102.24(16) ? C25 K1 O31 . . . 89.24(13) ? C25 K1 N41 . . . 107.86(14) ? C25 K1 C42 . . . 111.54(14) ? C25 K1 C43 . . . 134.88(15) ? C25 K1 C44 . . . 149.65(17) ? C25 K1 C45 . . . 128.23(16) ? C25 K1 N101 . . . 105.95(14) ? C25 K1 N102 . . . 127.21(15) ? O31 K1 N41 . . . 65.28(10) ? O31 K1 C42 . . . 90.50(13) ? O31 K1 C43 . . . 99.13(13) ? O31 K1 C44 . . . 78.93(13) ? O31 K1 C45 . . . 57.29(12) ? O31 K1 N101 . . . 158.41(13) ? O31 K1 N102 . . . 99.27(14) ? N41 K1 C42 . . . 25.26(13) ? N41 K1 C43 . . . 41.91(15) ? N41 K1 C44 . . . 41.83(15) ? N41 K1 C45 . . . 25.70(11) ? N41 K1 N101 . . . 121.79(13) ? N41 K1 N102 . . . 123.08(13) ? C42 K1 C43 . . . 25.32(16) ? C42 K1 C44 . . . 41.73(13) ? C42 K1 C45 . . . 41.57(12) ? C42 K1 N101 . . . 97.78(15) ? C42 K1 N102 . . . 120.29(15) ? C43 K1 C44 . . . 25.99(13) ? C43 K1 C45 . . . 41.91(15) ? C43 K1 N101 . . . 81.16(16) ? C43 K1 N102 . . . 95.27(16) ? C44 K1 C45 . . . 25.09(17) ? C44 K1 N101 . . . 94.05(16) ? C44 K1 N102 . . . 82.58(15) ? C45 K1 N101 . . . 118.89(14) ? C45 K1 N102 . . . 98.58(14) ? N101 K1 N102 . . . 59.37(15) ? O11 K2 C12 . . . 25.09(12) ? O11 K2 C13 . . . 41.46(15) ? O11 K2 C14 . . . 41.88(15) ? O11 K2 C15 . . . 25.99(12) ? O11 K2 N21 . . . 65.01(10) ? O11 K2 O31 . . . 96.27(11) ? O11 K2 C32 . . . 110.38(14) ? O11 K2 C33 . . . 134.72(15) ? O11 K2 C35 . . . 109.69(14) ? O11 K2 N41 . . . 66.12(10) ? O11 K2 N201 . . . 125.20(14) ? O11 K2 N202 . . . 125.84(15) ? C12 K2 C13 . . . 24.81(17) ? C12 K2 C14 . . . 41.45(14) ? C12 K2 C15 . . . 41.34(12) ? C12 K2 N21 . . . 57.15(12) ? C12 K2 O31 . . . 109.66(14) ? C12 K2 C32 . . . 130.20(17) ? C12 K2 C33 . . . 150.84(17) ? C12 K2 C35 . . . 112.91(15) ? C12 K2 N41 . . . 91.14(13) ? C12 K2 N201 . . . 101.32(16) ? C12 K2 N202 . . . 124.64(16) ? C13 K2 C14 . . . 25.80(13) ? C13 K2 C15 . . . 41.33(14) ? C13 K2 N21 . . . 78.21(13) ? C13 K2 O31 . . . 134.34(15) ? C13 K2 C32 . . . 151.81(18) ? C13 K2 C33 . . . 175.63(18) ? C13 K2 C35 . . . 135.41(14) ? C13 K2 N41 . . . 99.14(13) ? C13 K2 N201 . . . 84.85(17) ? C13 K2 N202 . . . 100.29(17) ? C14 K2 C15 . . . 24.78(17) ? C14 K2 N21 . . . 98.57(13) ? C14 K2 O31 . . . 135.18(16) ? C14 K2 C32 . . . 137.18(15) ? C14 K2 C33 . . . 155.09(14) ? C14 K2 C35 . . . 151.45(18) ? C14 K2 N41 . . . 79.06(13) ? C14 K2 N201 . . . 96.50(16) ? C14 K2 N202 . . . 86.18(17) ? C15 K2 N21 . . . 90.93(13) ? C15 K2 O31 . . . 110.67(14) ? C15 K2 C32 . . . 114.33(15) ? C15 K2 C33 . . . 137.01(15) ? C15 K2 C35 . . . 130.74(17) ? C15 K2 N41 . . . 57.87(12) ? C15 K2 N201 . . . 121.17(15) ? C15 K2 N202 . . . 100.42(17) ? N21 K2 O31 . . . 65.19(10) ? N21 K2 C32 . . . 90.57(12) ? N21 K2 C33 . . . 98.21(13) ? N21 K2 C35 . . . 57.21(12) ? N21 K2 N41 . . . 103.69(13) ? N21 K2 N201 . . . 100.60(14) ? N21 K2 N202 . . . 160.97(17) ? O31 K2 C32 . . . 25.45(12) ? O31 K2 C33 . . . 41.29(15) ? O31 K2 C35 . . . 25.35(12) ? O31 K2 N41 . . . 66.29(10) ? O31 K2 N201 . . . 126.61(13) ? O31 K2 N202 . . . 123.18(14) ? C32 K2 C33 . . . 24.64(17) ? C32 K2 C35 . . . 41.20(12) ? C32 K2 N41 . . . 58.15(12) ? C32 K2 N201 . . . 122.89(16) ? C32 K2 N202 . . . 98.45(16) ? C33 K2 C35 . . . 41.06(14) ? C33 K2 N41 . . . 79.17(13) ? C33 K2 N201 . . . 98.35(17) ? C33 K2 N202 . . . 83.91(17) ? C35 K2 N41 . . . 91.57(13) ? C35 K2 N201 . . . 102.41(15) ? C35 K2 N202 . . . 121.76(16) ? N41 K2 N201 . . . 155.69(15) ? N41 K2 N202 . . . 95.30(16) ? N201 K2 N202 . . . 60.44(18) ? K1 O11 K2 . . . 80.96(9) ? K1 O11 C12 . . . 122.4(3) ? K1 O11 C15 . . . 120.4(3) ? K2 O11 C12 . . . 78.2(3) ? K2 O11 C15 . . . 77.4(3) ? C12 O11 C15 . . . 106.3(5) ? K2 C12 O11 . . . 76.7(3) ? K2 C12 C13 . . . 81.1(3) ? K2 C12 C2 . . . 115.3(3) ? O11 C12 C13 . . . 110.9(4) ? O11 C12 C2 . . . 116.5(5) ? C13 C12 C2 . . . 132.1(5) ? K2 C13 C12 . . . 74.1(3) ? K2 C13 C14 . . . 76.8(3) ? K2 C13 H13 . . . 112.7 ? C12 C13 C14 . . . 106.5(5) ? C12 C13 H13 . . . 126.3 ? C14 C13 H13 . . . 127.1 ? K2 C14 C13 . . . 77.4(3) ? K2 C14 C15 . . . 74.1(3) ? K2 C14 H14 . . . 113.9 ? C13 C14 C15 . . . 106.4(5) ? C13 C14 H14 . . . 127.6 ? C15 C14 H14 . . . 125.9 ? K2 C15 O11 . . . 76.6(3) ? K2 C15 C14 . . . 81.1(3) ? K2 C15 C1 . . . 114.4(3) ? O11 C15 C14 . . . 109.8(4) ? O11 C15 C1 . . . 117.1(5) ? C14 C15 C1 . . . 132.7(5) ? C15 C1 C111 . . . 107.8(4) ? C15 C1 C121 . . . 109.5(6) ? C15 C1 C42 . . . 110.3(4) ? C111 C1 C121 . . . 111.6(5) ? C111 C1 C42 . . . 108.3(5) ? C121 C1 C42 . . . 109.4(4) ? C1 C111 C112 . . . 115.3(6) ? C1 C111 H111a . . . 109.0 ? C1 C111 H111b . . . 107.4 ? C112 C111 H111a . . . 109.7 ? C112 C111 H111b . . . 107.5 ? H111a C111 H111b . . . 107.7 ? C111 C112 H112a . . . 111.4 ? C111 C112 H112b . . . 111.0 ? C111 C112 H112c . . . 108.6 ? H112a C112 H112b . . . 110.3 ? H112a C112 H112c . . . 107.6 ? H112b C112 H112c . . . 107.8 ? C1 C121 C122 . . . 114.0(7) ? C1 C121 H121a . . . 108.2 ? C1 C121 H121b . . . 107.1 ? C122 C121 H121a . . . 109.8 ? C122 C121 H121b . . . 110.0 ? H121a C121 H121b . . . 107.4 ? C121 C122 H122a . . . 110.2 ? C121 C122 H122b . . . 111.7 ? C121 C122 H122c . . . 112.3 ? H122a C122 H122b . . . 106.2 ? H122a C122 H122c . . . 106.6 ? H122b C122 H122c . . . 109.5 ? K1 N21 K2 . . . 80.27(9) ? K1 N21 C22 . . . 77.7(3) ? K1 N21 C25 . . . 76.7(3) ? K2 N21 C22 . . . 120.7(3) ? K2 N21 C25 . . . 120.6(3) ? C22 N21 C25 . . . 106.6(5) ? K1 C22 N21 . . . 77.0(3) ? K1 C22 C23 . . . 77.2(3) ? K1 C22 C3 . . . 115.0(3) ? N21 C22 C23 . . . 110.1(5) ? N21 C22 C3 . . . 117.7(5) ? C23 C22 C3 . . . 132.2(5) ? K1 C23 C22 . . . 78.0(3) ? K1 C23 C24 . . . 76.6(3) ? K1 C23 H23 . . . 112.3 ? C22 C23 C24 . . . 106.6(5) ? C22 C23 H23 . . . 127.2 ? C24 C23 H23 . . . 126.2 ? K1 C24 C23 . . . 77.3(3) ? K1 C24 C25 . . . 77.1(3) ? K1 C24 H24 . . . 113.0 ? C23 C24 C25 . . . 106.7(5) ? C23 C24 H24 . . . 126.9 ? C25 C24 H24 . . . 126.4 ? K1 C25 N21 . . . 78.3(2) ? K1 C25 C24 . . . 77.7(3) ? K1 C25 C2 . . . 115.1(3) ? N21 C25 C24 . . . 110.0(4) ? N21 C25 C2 . . . 118.2(5) ? C24 C25 C2 . . . 131.7(5) ? C12 C2 C25 . . . 110.0(4) ? C12 C2 C211 . . . 108.8(4) ? C12 C2 C221 . . . 108.6(5) ? C25 C2 C211 . . . 109.5(5) ? C25 C2 C221 . . . 108.8(4) ? C211 C2 C221 . . . 111.1(4) ? C2 C211 C212 . . . 114.3(6) ? C2 C211 H211a . . . 108.7 ? C2 C211 H211b . . . 109.0 ? C212 C211 H211a . . . 107.6 ? C212 C211 H211b . . . 108.4 ? H211a C211 H211b . . . 108.7 ? C211 C212 H212a . . . 109.6 ? C211 C212 H212b . . . 109.1 ? C211 C212 H212c . . . 110.0 ? H212a C212 H212b . . . 108.9 ? H212a C212 H212c . . . 109.5 ? H212b C212 H212c . . . 109.8 ? C2 C221 C222 . . . 114.1(6) ? C2 C221 H221a . . . 108.4 ? C2 C221 H221b . . . 108.2 ? C222 C221 H221a . . . 111.3 ? C222 C221 H221b . . . 109.3 ? H221a C221 H221b . . . 105.1 ? C221 C222 H222a . . . 111.6 ? C221 C222 H222b . . . 112.3 ? C221 C222 H222c . . . 109.2 ? H222a C222 H222b . . . 109.7 ? H222a C222 H222c . . . 105.4 ? H222b C222 H222c . . . 108.2 ? K1 O31 K2 . . . 80.86(9) ? K1 O31 C32 . . . 120.4(3) ? K1 O31 C35 . . . 122.5(3) ? K2 O31 C32 . . . 77.8(3) ? K2 O31 C35 . . . 79.1(3) ? C32 O31 C35 . . . 107.0(5) ? K2 C32 O31 . . . 76.8(2) ? K2 C32 C33 . . . 80.1(3) ? K2 C32 C4 . . . 114.3(3) ? O31 C32 C33 . . . 109.4(4) ? O31 C32 C4 . . . 117.4(5) ? C33 C32 C4 . . . 133.0(5) ? K2 C33 C32 . . . 75.2(3) ? K2 C33 C34 . . . 78.3(3) ? K2 C33 H33 . . . 111.9 ? C32 C33 C34 . . . 107.5(5) ? C32 C33 H33 . . . 125.2 ? C34 C33 H33 . . . 127.2 ? C33 C34 C35 . . . 107.0(5) ? C33 C34 H34 . . . 125.3 ? C35 C34 H34 . . . 127.7 ? K2 C35 O31 . . . 75.5(2) ? K2 C35 C34 . . . 79.9(3) ? K2 C35 C3 . . . 114.2(3) ? O31 C35 C34 . . . 109.1(4) ? O31 C35 C3 . . . 118.2(5) ? C34 C35 C3 . . . 132.6(5) ? C22 C3 C35 . . . 111.0(4) ? C22 C3 C311 . . . 107.8(5) ? C22 C3 C321 . . . 109.1(4) ? C35 C3 C311 . . . 108.6(4) ? C35 C3 C321 . . . 109.1(5) ? C311 C3 C321 . . . 111.2(4) ? C3 C311 C312 . . . 114.1(6) ? C3 C311 H311a . . . 107.5 ? C3 C311 H311b . . . 108.3 ? C312 C311 H311a . . . 107.1 ? C312 C311 H311b . . . 111.0 ? H311a C311 H311b . . . 108.6 ? C311 C312 H312a . . . 111.4 ? C311 C312 H312b . . . 107.8 ? C311 C312 H312c . . . 112.7 ? H312a C312 H312b . . . 106.2 ? H312a C312 H312c . . . 111.1 ? H312b C312 H312c . . . 107.2 ? C3 C321 C322 . . . 115.2(6) ? C3 C321 H321a . . . 108.5 ? C3 C321 H321b . . . 108.5 ? C322 C321 H321a . . . 107.8 ? C322 C321 H321b . . . 109.9 ? H321a C321 H321b . . . 106.6 ? C321 C322 H322a . . . 110.7 ? C321 C322 H322b . . . 109.0 ? C321 C322 H322c . . . 111.7 ? H322a C322 H322b . . . 106.7 ? H322a C322 H322c . . . 109.2 ? H322b C322 H322c . . . 109.3 ? K1 N41 K2 . . . 81.80(9) ? K1 N41 C42 . . . 77.0(3) ? K1 N41 C45 . . . 76.2(3) ? K2 N41 C42 . . . 120.9(3) ? K2 N41 C45 . . . 120.5(3) ? C42 N41 C45 . . . 106.7(5) ? K1 C42 C1 . . . 115.1(3) ? K1 C42 N41 . . . 77.8(2) ? K1 C42 C43 . . . 78.3(3) ? C1 C42 N41 . . . 119.0(5) ? C1 C42 C43 . . . 130.8(5) ? N41 C42 C43 . . . 110.0(4) ? K1 C43 C42 . . . 76.4(3) ? K1 C43 C44 . . . 76.6(3) ? K1 C43 H43 . . . 111.7 ? C42 C43 C44 . . . 106.2(5) ? C42 C43 H43 . . . 125.7 ? C44 C43 H43 . . . 128.1 ? K1 C44 C43 . . . 77.4(3) ? K1 C44 C45 . . . 76.4(3) ? K1 C44 H44 . . . 114.1 ? C43 C44 C45 . . . 107.8(5) ? C43 C44 H44 . . . 126.1 ? C45 C44 H44 . . . 126.1 ? K1 C45 N41 . . . 78.1(3) ? K1 C45 C44 . . . 78.6(3) ? K1 C45 C4 . . . 114.7(3) ? N41 C45 C44 . . . 109.2(4) ? N41 C45 C4 . . . 119.2(5) ? C44 C45 C4 . . . 131.4(5) ? C32 C4 C45 . . . 110.3(4) ? C32 C4 C411 . . . 108.4(4) ? C32 C4 C421 . . . 109.4(5) ? C45 C4 C411 . . . 108.2(5) ? C45 C4 C421 . . . 109.1(4) ? C411 C4 C421 . . . 111.5(4) ? C4 C411 C412 . . . 114.3(6) ? C4 C411 H411a . . . 109.1 ? C4 C411 H411b . . . 109.4 ? C412 C411 H411a . . . 107.4 ? C412 C411 H411b . . . 108.4 ? H411a C411 H411b . . . 108.1 ? C411 C412 H412a . . . 111.7 ? C411 C412 H412b . . . 108.8 ? C411 C412 H412c . . . 109.9 ? H412a C412 H412b . . . 109.1 ? H412a C412 H412c . . . 109.6 ? H412b C412 H412c . . . 107.6 ? C4 C421 C422 . . . 114.8(7) ? C4 C421 H421a . . . 109.5 ? C4 C421 H421b . . . 108.3 ? C422 C421 H421a . . . 108.8 ? C422 C421 H421b . . . 107.4 ? H421a C421 H421b . . . 107.8 ? C421 C422 H422a . . . 111.2 ? C421 C422 H422b . . . 109.9 ? C421 C422 H422c . . . 108.4 ? H422a C422 H422b . . . 110.5 ? H422a C422 H422c . . . 108.5 ? H422b C422 H422c . . . 108.1 ? K1 N101 C1011 . . . 115.2(5) ? K1 N101 C1012 . . . 102.6(5) ? K1 N101 C101 . . . 108.0(4) ? C1011 N101 C1012 . . . 107.6(5) ? C1011 N101 C101 . . . 110.9(6) ? C1012 N101 C101 . . . 112.3(6) ? N101 C1011 H1011a . . . 110.9 ? N101 C1011 H1011b . . . 111.4 ? N101 C1011 H1011c . . . 113.6 ? H1011a C1011 H1011b . . . 105.6 ? H1011a C1011 H1011c . . . 107.2 ? H1011b C1011 H1011c . . . 107.7 ? N101 C1012 H1012a . . . 108.2 ? N101 C1012 H1012b . . . 110.9 ? N101 C1012 H1012c . . . 111.1 ? H1012a C1012 H1012b . . . 107.5 ? H1012a C1012 H1012c . . . 108.6 ? H1012b C1012 H1012c . . . 110.4 ? N101 C101 C102 . . . 115.3(6) ? N101 C101 H101a . . . 110.2 ? N101 C101 H101b . . . 109.4 ? C102 C101 H101a . . . 107.0 ? C102 C101 H101b . . . 107.7 ? H101a C101 H101b . . . 106.9 ? C101 C102 N102 . . . 113.2(7) ? C101 C102 H102a . . . 110.7 ? C101 C102 H102b . . . 108.3 ? N102 C102 H102a . . . 109.1 ? N102 C102 H102b . . . 109.1 ? H102a C102 H102b . . . 106.1 ? K1 N102 C102 . . . 113.6(4) ? K1 N102 C1021 . . . 118.5(6) ? K1 N102 C1022 . . . 99.1(5) ? C102 N102 C1021 . . . 107.8(7) ? C102 N102 C1022 . . . 110.8(6) ? C1021 N102 C1022 . . . 106.4(5) ? N102 C1021 H1021a . . . 110.0 ? N102 C1021 H1021b . . . 110.8 ? N102 C1021 H1021c . . . 110.5 ? H1021a C1021 H1021b . . . 108.4 ? H1021a C1021 H1021c . . . 107.6 ? H1021b C1021 H1021c . . . 109.5 ? N102 C1022 H1022a . . . 111.4 ? N102 C1022 H1022b . . . 107.4 ? N102 C1022 H1022c . . . 111.5 ? H1022a C1022 H1022b . . . 107.1 ? H1022a C1022 H1022c . . . 111.4 ? H1022b C1022 H1022c . . . 107.9 ? K2 N201 C2011 . . . 106.2(9) ? K2 N201 C2012 . . . 111.3(8) ? K2 N201 C201 . . . 113.2(7) ? K2 N201 C2011' . . . 112.6(8) ? K2 N201 C2012' . . . 102.6(11) ? K2 N201 C201' . . . 119.5(13) ? C2011 N201 C2012 . . . 107.1(9) ? C2011 N201 C201 . . . 113.0(12) ? C2012 N201 C201 . . . 105.8(10) ? C2011' N201 C2012' . . . 108.0(11) ? C2011' N201 C201' . . . 107.6(17) ? C2012' N201 C201' . . . 105.7(15) ? N201 C2011 H2011a . . . 108.8 ? N201 C2011 H2011b . . . 112.5 ? N201 C2011 H2011c . . . 107.2 ? H2011a C2011 H2011b . . . 112.3 ? H2011a C2011 H2011c . . . 105.6 ? H2011b C2011 H2011c . . . 110.1 ? N201 C2012 H2012a . . . 110.1 ? N201 C2012 H2012b . . . 109.2 ? N201 C2012 H2012c . . . 109.8 ? H2012a C2012 H2012b . . . 109.1 ? H2012a C2012 H2012c . . . 110.0 ? H2012b C2012 H2012c . . . 108.7 ? N201 C201 C202 . . . 115.5(13) ? N201 C201 H201a . . . 107.5 ? N201 C201 H201b . . . 108.7 ? C202 C201 H201a . . . 106.9 ? C202 C201 H201b . . . 106.5 ? H201a C201 H201b . . . 111.7 ? N201 C2011' H2011'a . . . 111.6 ? N201 C2011' H2011'b . . . 111.5 ? N201 C2011' H2011'c . . . 109.1 ? H2011'a C2011' H2011'b . . . 110.3 ? H2011'a C2011' H2011'c . . . 107 ? H2011'b C2011' H2011'c . . . 107.1 ? N201 C2012' H2012'a . . . 114 ? N201 C2012' H2012'b . . . 111.6 ? N201 C2012' H2012'c . . . 112.4 ? H2012'a C2012' H2012'b . . . 106 ? H2012'a C2012' H2012'c . . . 107.4 ? H2012'b C2012' H2012'c . . . 105 ? N201 C201' C202 . . . 112(2) ? N201 C201' H201'a . . . 110 ? N201 C201' H201'b . . . 109.8 ? C202 C201' H201'a . . . 111.1 ? C202 C201' H201'b . . . 112 ? H201'a C201' H201'b . . . 102 ? C201 C202 N202 . . . 119.4(13) ? C201 C202 H202a . . . 107.2 ? C201 C202 H202b . . . 105.7 ? C201' C202 N202 . . . 128.7(18) ? C201' C202 H202'a . . . 105.7 ? C201' C202 H202'b . . . 103.7 ? N202 C202 H202a . . . 108.9 ? N202 C202 H202b . . . 108.2 ? N202 C202 H202'a . . . 104.8 ? N202 C202 H202'b . . . 104.9 ? H202a C202 H202b . . . 106.8 ? H202'a C202 H202'b . . . 107.9 ? K2 N202 C202 . . . 109.6(6) ? K2 N202 C2021 . . . 111.7(6) ? K2 N202 C2022 . . . 110.1(9) ? C202 N202 C2021 . . . 101.9(9) ? C202 N202 C2022 . . . 113.7(10) ? C2021 N202 C2022 . . . 109.5(8) ? N202 C2021 H2021a . . . 112.5 ? N202 C2021 H2021b . . . 109.3 ? N202 C2021 H2021c . . . 114.8 ? H2021a C2021 H2021b . . . 103.3 ? H2021a C2021 H2021c . . . 109.1 ? H2021b C2021 H2021c . . . 107.1 ? N202 C2022 H2022a . . . 113.2 ? N202 C2022 H2022b . . . 114.3 ? N202 C2022 H2022c . . . 108.4 ? H2022a C2022 H2022b . . . 110.1 ? H2022a C2022 H2022c . . . 104.1 ? H2022b C2022 H2022c . . . 105.9 ? 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 ? ? ? ? ? ? ? ? ? ? ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 928 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min -20 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 17.39 _diffrn_reflns_av_sigmaI/netI .096 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .129 _refine_ls_wR_factor_all .153 _refine_ls_goodness_of_fit_all 1.406 _refine_ls_shift/su_mean .0003 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_mgjwx _database_code_CSD 196193 _audit_creation_method Xtal3.6 _audit_creation_date 01-11-12 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C46 H70 K2 N4 O2' _chemical_formula_moiety ? _chemical_formula_weight 789.29 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_n_m_a _symmetry_space_group_name_Hall -p_2ac_2n loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,1/2+z +x,1/2-y,+z _cell_length_a 23.941(3) _cell_length_b 17.131(2) _cell_length_c 10.8320(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4442.6(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.18 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5646 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 21.1 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .254 _exptl_crystal_description prism _exptl_crystal_size_max .25 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .86 _exptl_absorpt_correction_T_max .96 _diffrn_reflns_number 43940 _reflns_number_total 5966 _reflns_Friedel_coverage 0 _reflns_number_gt 4509 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.02 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .034 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .04 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.489 _refine_ls_number_reflns 4509 _refine_ls_number_parameters 391 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .009 _refine_diff_density_min -.29 _refine_diff_density_max .367 _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 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _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 ? 0 184 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 280 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' K ? 0 8 .179 .25 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 8 .008 .006 '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 K1 .121226(18) .25000 .54163(4) .0248(2) Uani ? ? 1.00000 ? ? K2 -.088314(19) .25000 .71344(5) .0332(3) Uani ? ? 1.00000 ? ? N11 .23362(7) .25000 .61949(16) .0225(8) Uani ? ? 1.00000 ? ? C12 .25429(5) .18637(8) .68065(13) .0225(7) Uani ? ? 1.00000 ? ? C13 .28721(6) .20841(9) .78017(14) .0249(7) Uani ? ? 1.00000 ? ? N21 .13751(5) .11076(7) .70721(11) .0213(6) Uani ? ? 1.00000 ? ? C21 .14986(6) .13647(10) .83307(14) .0265(8) Uani ? ? 1.00000 ? ? C22 .08405(5) .09683(8) .66166(14) .0229(7) Uani ? ? 1.00000 ? ? C23 .09021(6) .07430(9) .54070(14) .0271(8) Uani ? ? 1.00000 ? ? C24 .14790(6) .07412(9) .51190(14) .0263(8) Uani ? ? 1.00000 ? ? C25 .17689(6) .09668(8) .61522(13) .0225(7) Uani ? ? 1.00000 ? ? C2 .23986(6) .10540(8) .63276(13) .0226(7) Uani ? ? 1.00000 ? ? C211 .26700(6) .09615(10) .50308(14) .0271(8) Uani ? ? 1.00000 ? ? C212 .33055(7) .10124(14) .50248(19) .0400(10) Uani ? ? 1.00000 ? ? C221 .26126(6) .04078(9) .72075(14) .0270(8) Uani ? ? 1.00000 ? ? C222 .24934(9) -.04225(10) .6771(2) .0400(10) Uani ? ? 1.00000 ? ? N31 .03471(6) .25000 .71755(15) .0214(8) Uani ? ? 1.00000 ? ? C34 .00247(6) .20851(8) .90409(14) .0254(7) Uani ? ? 1.00000 ? ? C35 .02272(5) .18592(8) .78931(13) .0215(7) Uani ? ? 1.00000 ? ? C3 .03096(6) .10322(8) .73844(14) .0240(7) Uani ? ? 1.00000 ? ? C311 -.01876(6) .08327(10) .65079(17) .0312(8) Uani ? ? 1.00000 ? ? C312 -.07459(7) .06751(11) .7144(2) .0387(10) Uani ? ? 1.00000 ? ? C321 .03239(7) .04292(9) .84521(16) .0301(8) Uani ? ? 1.00000 ? ? C322 .04216(8) -.04084(10) .8042(2) .0410(10) Uani ? ? 1.00000 ? ? O101 .08881(15) .27115(17) .2997(3) .064(2) Uani ? ? .50000 ? ? C102 .1256(6) .3060(7) .2158(8) .162(10) Uani ? ? .50000 ? ? C103 .1522(2) .25000 .1442(5) .119(4) Uani ? ? 1.00000 ? ? C104 .1156(3) .1731(5) .1652(7) .073(4) Uani ? ? .50000 ? ? C105 .0697(2) .2037(3) .2393(4) .059(3) Uani ? ? .50000 ? ? O201 -.10885(9) .25000 .47039(18) .0596(13) Uani ? ? 1.00000 ? ? C202 -.0682(2) .2722(3) .3801(4) .079(4) Uani ? ? .50000 ? ? C203 -.09213(15) .25000 .2558(3) .0589(19) Uani ? ? 1.00000 ? ? C204 -.15428(16) .25000 .2790(3) .078(2) Uani ? ? 1.00000 ? ? C205 -.1587(2) .2736(4) .4080(4) .092(5) Uani ? ? .50000 ? ? H13 .3043(7) .1748(9) .8388(15) .030(4) Uiso ? ? 1.00000 ? ? H21a .1820(7) .1672(10) .8338(16) .036(5) Uiso ? ? 1.00000 ? ? H21b .1551(7) .0919(10) .8892(16) .031(4) Uiso ? ? 1.00000 ? ? H21c .1179(7) .1672(9) .8641(15) .029(4) Uiso ? ? 1.00000 ? ? H23 .0607(7) .0613(11) .4855(15) .033(4) Uiso ? ? 1.00000 ? ? H24 .1645(7) .0609(10) .4308(16) .033(4) Uiso ? ? 1.00000 ? ? H211a .2555(7) .0452(10) .4664(15) .027(4) Uiso ? ? 1.00000 ? ? H211b .2522(6) .1386(9) .4500(14) .025(4) Uiso ? ? 1.00000 ? ? H212a .3441(8) .0994(11) .421(2) .047(5) Uiso ? ? 1.00000 ? ? H212b .3469(8) .0570(13) .5451(19) .052(6) Uiso ? ? 1.00000 ? ? H212c .3435(9) .1481(13) .538(2) .060(7) Uiso ? ? 1.00000 ? ? H221a .3001(7) .0485(10) .7308(15) .030(4) Uiso ? ? 1.00000 ? ? H221b .2441(7) .0463(10) .8042(16) .031(4) Uiso ? ? 1.00000 ? ? H222a .2628(8) -.0791(12) .7365(18) .045(5) Uiso ? ? 1.00000 ? ? H222b .2683(9) -.0544(13) .602(2) .062(6) Uiso ? ? 1.00000 ? ? H222c .2099(9) -.0482(12) .660(2) .058(6) Uiso ? ? 1.00000 ? ? H34 -.0089(7) .1760(10) .9740(15) .032(4) Uiso ? ? 1.00000 ? ? H311a -.0225(7) .1250(11) .5910(16) .034(5) Uiso ? ? 1.00000 ? ? H311b -.0082(7) .0373(11) .6039(16) .036(5) Uiso ? ? 1.00000 ? ? H312a -.0758(8) .0145(12) .7488(18) .048(5) Uiso ? ? 1.00000 ? ? H312b -.1051(9) .0712(11) .6565(18) .049(6) Uiso ? ? 1.00000 ? ? H312c -.0816(7) .1004(11) .7885(17) .038(5) Uiso ? ? 1.00000 ? ? H321a .0600(7) .0570(10) .9043(16) .033(5) Uiso ? ? 1.00000 ? ? H321b -.0029(7) .0457(10) .8906(15) .033(4) Uiso ? ? 1.00000 ? ? H322a .0446(8) -.0725(12) .8726(19) .049(6) Uiso ? ? 1.00000 ? ? H322b .0771(8) -.0477(11) .7625(17) .040(5) Uiso ? ? 1.00000 ? ? H322c .0130(9) -.0602(13) .752(2) .060(6) Uiso ? ? 1.00000 ? ? H102a .17235 .30704 .24378 .25000 Uiso ? ? .50000 ? ? H102b .12850 .33658 .14924 .25000 Uiso ? ? .50000 ? ? H103a .19099 .23889 .14473 .08000 Uiso ? ? .50000 ? ? H103b .14476 .26528 .05348 .08000 Uiso ? ? .50000 ? ? H104a .13559 .13977 .22562 .08600 Uiso ? ? .50000 ? ? H104b .10296 .14663 .10237 .08600 Uiso ? ? .50000 ? ? H105a .05749 .16470 .29375 .08500 Uiso ? ? .50000 ? ? H105b .04113 .21404 .17922 .08500 Uiso ? ? .50000 ? ? H202a -.03329 .24319 .39567 .09900 Uiso ? ? .50000 ? ? H202b -.05927 .32591 .38578 .09900 Uiso ? ? .50000 ? ? H203a -.07755 .20048 .23283 .07300 Uiso ? ? .50000 ? ? H203b -.08210 .28764 .19431 .07300 Uiso ? ? .50000 ? ? H204a -.16868 .19918 .26466 .09900 Uiso ? ? .50000 ? ? H204b -.17292 .28708 .22524 .10100 Uiso ? ? .50000 ? ? H205a -.16542 .32746 .41940 .12800 Uiso ? ? .50000 ? ? H205b -.19074 .24620 .44874 .12800 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 K1 .0213(2) .0291(2) .0240(2) .00000 -.00027(17) .00000 K2 .0205(2) .0355(3) .0437(3) .00000 -.0033(2) .00000 N11 .0188(8) .0254(9) .0233(9) .00000 -.0010(7) .00000 C12 .0160(6) .0257(7) .0257(7) .0004(5) .0006(5) .0003(6) C13 .0190(6) .0291(8) .0267(8) .0012(6) -.0034(6) .0022(6) N21 .0190(5) .0224(6) .0226(6) -.0007(5) .0010(5) -.0026(5) C21 .0225(7) .0356(9) .0215(7) -.0004(7) -.0003(6) -.0044(6) C22 .0189(7) .0205(7) .0294(8) -.0022(5) .0010(6) -.0030(6) C23 .0217(7) .0291(8) .0304(8) -.0037(6) -.0016(6) -.0085(7) C24 .0238(7) .0276(8) .0273(8) -.0013(6) .0021(6) -.0080(6) C25 .0211(7) .0219(7) .0245(7) .0006(5) .0018(5) -.0023(6) C2 .0189(6) .0253(7) .0235(7) .0011(5) .0002(5) -.0004(6) C211 .0238(7) .0323(8) .0251(8) .0025(6) .0031(6) -.0011(7) C212 .0248(8) .0588(13) .0363(10) .0033(8) .0079(7) -.0012(9) C221 .0256(7) .0272(8) .0281(8) .0041(6) .0009(6) .0013(6) C222 .0521(12) .0275(9) .0405(10) .0058(8) -.0041(9) .0016(8) N31 .0172(8) .0229(8) .0242(9) .00000 .0014(7) .00000 C34 .0244(7) .0253(7) .0264(8) -.0004(6) .0043(6) .0021(6) C35 .0165(6) .0211(7) .0269(7) -.0003(5) .0002(5) -.0005(6) C3 .0201(6) .0204(7) .0316(8) -.0022(5) .0031(6) -.0029(6) C311 .0206(7) .0309(8) .0421(9) -.0050(6) .0013(7) -.0109(8) C312 .0239(8) .0353(10) .0570(12) -.0057(7) .0067(8) -.0100(9) C321 .0274(8) .0239(7) .0391(9) -.0018(6) .0080(7) .0028(7) C322 .0395(10) .0239(8) .0595(12) .0018(7) .0100(9) .0042(9) O101 .097(2) .066(4) .0296(13) -.0253(19) .0044(14) -.0053(14) C102 .279(15) .132(8) .074(6) -.146(9) .073(7) -.033(5) C103 .096(3) .167(5) .093(4) .00000 .046(3) .00000 C104 .064(3) .078(4) .076(5) .003(3) .020(3) -.007(4) C105 .078(3) .066(3) .034(2) -.022(3) -.001(2) -.009(2) O201 .0638(13) .0779(15) .0371(11) .00000 .0027(10) .00000 C202 .077(3) .103(7) .056(2) -.026(3) .004(2) .020(3) C203 .085(2) .0436(16) .0486(17) .00000 .0130(16) .00000 C204 .078(2) .115(3) .0415(18) .00000 .0044(17) .00000 C205 .078(3) .151(10) .046(2) .056(4) .000(2) .003(3) # 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 K1 N11 . . 2.8199(17) ? K1 N21 . . 3.0098(12) ? K1 C22 . . 3.0607(14) ? K1 C23 . . 3.1002(16) ? K1 C24 . . 3.0968(16) ? K1 C25 . . 3.0512(14) ? K1 N31 . . 2.8145(17) ? K1 O101 . . 2.757(3) ? K1 N21 . 8 3.0098(12) ? K1 C22 . 8 3.0607(14) ? K1 C23 . 8 3.1002(16) ? K1 C24 . 8 3.0968(16) ? K1 C25 . 8 3.0512(14) ? K1 O101 . 8 2.757(3) ? K2 N31 . . 2.9457(16) ? K2 C34 . . 3.0811(16) ? K2 C35 . . 2.9911(14) ? K2 C312 . . 3.143(2) ? K2 O201 . . 2.678(2) ? K2 C13 . '3 456' 3.0649(15) ? K2 C13 . '6 456' 3.0649(15) ? K2 C34 . 8 3.0811(16) ? K2 C35 . 8 2.9911(14) ? K2 C312 . 8 3.143(2) ? N11 C12 . . 1.3682(17) ? N11 C12 . 8 1.3682(17) ? C12 C13 . . 1.388(2) ? C12 C2 . . 1.521(2) ? C13 H13 . . .950(16) ? C13 C13 . 8 1.425(2) ? N21 C21 . . 1.463(2) ? N21 C22 . . 1.3923(17) ? N21 C25 . . 1.3927(18) ? C21 H21a . . .933(18) ? C21 H21b . . .983(17) ? C21 H21c . . .988(16) ? C22 C23 . . 1.374(2) ? C22 C3 . . 1.523(2) ? C23 C24 . . 1.416(2) ? C23 H23 . . .951(17) ? C24 C25 . . 1.373(2) ? C24 H24 . . .990(17) ? C25 C2 . . 1.527(2) ? C2 C211 . . 1.556(2) ? C2 C221 . . 1.548(2) ? C211 C212 . . 1.524(2) ? C211 H211a . . .998(17) ? C211 H211b . . .993(16) ? C212 H212a . . .95(2) ? C212 H212b . . .97(2) ? C212 H212c . . .94(2) ? C221 C222 . . 1.526(2) ? C221 H221a . . .945(17) ? C221 H221b . . .997(17) ? C222 H222a . . .96(2) ? C222 H222b . . .96(2) ? C222 H222c . . .97(2) ? N31 C35 . . 1.3754(17) ? N31 C35 . 8 1.3754(17) ? C34 C35 . . 1.389(2) ? C34 H34 . . .979(17) ? C34 C34 . 8 1.421(2) ? C35 C3 . . 1.533(2) ? C3 C311 . . 1.561(2) ? C3 C321 . . 1.551(2) ? C311 C312 . . 1.528(2) ? C311 H311a . . .969(18) ? C311 H311b . . .972(18) ? C312 H312a . . .98(2) ? C312 H312b . . .96(2) ? C312 H312c . . .995(19) ? C321 C322 . . 1.520(2) ? C321 H321a . . .952(17) ? C321 H321b . . .979(17) ? C322 H322a . . .92(2) ? C322 H322b . . .957(19) ? C322 H322c . . .96(2) ? O101 C102 . . 1.400(12) ? O101 C105 . . 1.405(6) ? C102 C103 . . 1.388(12) ? C102 H102a . . 1.159 ? C102 H102b . . .893 ? C103 C104 . . 1.599(8) ? C103 H103a . . .947 ? C103 H103b . . 1.033 ? C104 C105 . . 1.459(9) ? C104 H104a . . .991 ? C104 H104b . . .872 ? C105 H105a . . .938 ? C105 H105b . . .960 ? O201 C202 . . 1.432(5) ? O201 C205 . . 1.430(6) ? O201 C202 . 8 1.432(5) ? O201 C205 . 8 1.430(6) ? C202 C203 . . 1.512(6) ? C202 H202a . . .987 ? C202 H202b . . .946 ? C203 C204 . . 1.509(5) ? C203 H203a . . .9506 ? C203 H203b . . .958 ? C203 H203a . 8 .9506 ? C203 H203b . 8 .958 ? C204 C205 . . 1.458(6) ? C204 H204a . . .9493 ? C204 H204b . . .971 ? C204 C205 . 8 1.458(6) ? C204 H204a . 8 .9493 ? C204 H204b . 8 .971 ? C205 H205a . . .945 ? C205 H205b . . 1.001 ? C205 C205 . 8 .808(10) ? C205 H205b . 8 .947 ? 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 N11 K1 N21 . . . 72.43(3) ? N11 K1 C22 . . . 98.65(3) ? N11 K1 C23 . . . 103.27(3) ? N11 K1 C24 . . . 80.47(3) ? N11 K1 C25 . . . 60.34(3) ? N11 K1 N31 . . . 119.98(5) ? N11 K1 O101 . . . 123.57(8) ? N11 K1 N21 . . 8 72.43(3) ? N11 K1 C22 . . 8 98.65(3) ? N11 K1 C23 . . 8 103.27(3) ? N11 K1 C24 . . 8 80.47(3) ? N11 K1 C25 . . 8 60.34(3) ? N11 K1 O101 . . 8 123.57(8) ? N21 K1 C22 . . . 26.50(3) ? N21 K1 C23 . . . 42.57(4) ? N21 K1 C24 . . . 42.62(4) ? N21 K1 C25 . . . 26.56(3) ? N21 K1 N31 . . . 72.05(3) ? N21 K1 O101 . . . 134.99(7) ? N21 K1 N21 . . 8 104.85(3) ? N21 K1 C22 . . 8 117.64(4) ? N21 K1 C23 . . 8 143.36(4) ? N21 K1 C24 . . 8 143.74(4) ? N21 K1 C25 . . 8 118.03(4) ? N21 K1 O101 . . 8 119.92(6) ? C22 K1 C23 . . . 25.76(4) ? C22 K1 C24 . . . 43.12(4) ? C22 K1 C25 . . . 43.79(4) ? C22 K1 N31 . . . 59.89(3) ? C22 K1 O101 . . . 115.76(7) ? C22 K1 N21 . . 8 117.64(4) ? C22 K1 C22 . . 8 118.03(4) ? C22 K1 C23 . . 8 139.82(4) ? C22 K1 C24 . . 8 159.76(4) ? C22 K1 C25 . . 8 138.94(4) ? C22 K1 O101 . . 8 102.08(7) ? C23 K1 C24 . . . 26.42(4) ? C23 K1 C25 . . . 43.09(4) ? C23 K1 N31 . . . 79.98(3) ? C23 K1 O101 . . . 93.27(7) ? C23 K1 N21 . . 8 143.36(4) ? C23 K1 C22 . . 8 139.82(4) ? C23 K1 C23 . . 8 152.28(4) ? C23 K1 C24 . . 8 173.56(5) ? C23 K1 C25 . . 8 160.26(4) ? C23 K1 O101 . . 8 78.57(7) ? C24 K1 C25 . . . 25.79(4) ? C24 K1 N31 . . . 102.84(3) ? C24 K1 O101 . . . 95.00(7) ? C24 K1 N21 . . 8 143.74(4) ? C24 K1 C22 . . 8 159.76(4) ? C24 K1 C23 . . 8 173.56(4) ? C24 K1 C24 . . 8 153.30(4) ? C24 K1 C25 . . 8 140.77(4) ? C24 K1 O101 . . 8 80.29(7) ? C25 K1 N31 . . . 98.31(3) ? C25 K1 O101 . . . 118.98(7) ? C25 K1 N21 . . 8 118.03(4) ? C25 K1 C22 . . 8 138.94(4) ? C25 K1 C23 . . 8 160.26(4) ? C25 K1 C24 . . 8 140.77(4) ? C25 K1 C25 . . 8 118.81(4) ? C25 K1 O101 . . 8 104.96(7) ? N31 K1 O101 . . . 115.87(8) ? N31 K1 N21 . . 8 72.05(3) ? N31 K1 C22 . . 8 59.89(3) ? N31 K1 C23 . . 8 79.98(3) ? N31 K1 C24 . . 8 102.84(3) ? N31 K1 C25 . . 8 98.31(3) ? N31 K1 O101 . . 8 115.87(8) ? O101 K1 N21 . . 8 119.92(7) ? O101 K1 C22 . . 8 102.08(7) ? O101 K1 C23 . . 8 78.57(7) ? O101 K1 C24 . . 8 80.29(7) ? O101 K1 C25 . . 8 104.96(7) ? O101 K1 O101 . . 8 15.10(9) ? N21 K1 C22 8 . 8 26.50(3) ? N21 K1 C23 8 . 8 42.57(4) ? N21 K1 C24 8 . 8 42.62(4) ? N21 K1 C25 8 . 8 26.56(3) ? N21 K1 O101 8 . 8 134.99(6) ? C22 K1 C23 8 . 8 25.76(4) ? C22 K1 C24 8 . 8 43.12(4) ? C22 K1 C25 8 . 8 43.79(4) ? C22 K1 O101 8 . 8 115.76(7) ? C23 K1 C24 8 . 8 26.42(4) ? C23 K1 C25 8 . 8 43.09(4) ? C23 K1 O101 8 . 8 93.27(7) ? C24 K1 C25 8 . 8 25.79(4) ? C24 K1 O101 8 . 8 95.00(7) ? C25 K1 O101 8 . 8 118.98(7) ? N31 K2 C34 . . . 44.32(4) ? N31 K2 C35 . . . 26.78(3) ? N31 K2 C312 . . . 84.00(3) ? N31 K2 O201 . . . 101.44(6) ? N31 K2 C13 . . '3 456' 166.38(3) ? N31 K2 C13 . . '6 456' 166.38(3) ? N31 K2 C34 . . 8 44.32(4) ? N31 K2 C35 . . 8 26.78(3) ? N31 K2 C312 . . 8 84.00(3) ? C34 K2 C35 . . . 26.40(4) ? C34 K2 C312 . . . 72.22(5) ? C34 K2 O201 . . . 142.03(5) ? C34 K2 C13 . . '3 456' 136.42(4) ? C34 K2 C13 . . '6 456' 128.11(4) ? C34 K2 C34 . . 8 26.67(4) ? C34 K2 C35 . . 8 43.41(4) ? C34 K2 C312 . . 8 98.83(5) ? C35 K2 C312 . . . 62.69(4) ? C35 K2 O201 . . . 115.67(5) ? C35 K2 C13 . . '3 456' 160.60(4) ? C35 K2 C13 . . '6 456' 140.59(4) ? C35 K2 C34 . . 8 43.41(4) ? C35 K2 C35 . . 8 43.06(4) ? C35 K2 C312 . . 8 105.74(4) ? C312 K2 O201 . . . 91.29(4) ? C312 K2 C13 . . '3 456' 109.43(4) ? C312 K2 C13 . . '6 456' 82.55(4) ? C312 K2 C34 . . 8 98.83(5) ? C312 K2 C35 . . 8 105.74(4) ? C312 K2 C312 . . 8 168.00(5) ? O201 K2 C13 . . '3 456' 81.01(5) ? O201 K2 C13 . . '6 456' 81.01(5) ? O201 K2 C34 . . 8 142.03(5) ? O201 K2 C35 . . 8 115.67(5) ? O201 K2 C312 . . 8 91.29(4) ? C13 K2 C13 '3 456' . '6 456' 26.88(4) ? C13 K2 C34 '3 456' . 8 128.11(4) ? C13 K2 C35 '3 456' . 8 140.59(4) ? C13 K2 C312 '3 456' . 8 82.55(4) ? C13 K2 C34 '6 456' . 8 136.42(4) ? C13 K2 C35 '6 456' . 8 160.60(4) ? C13 K2 C312 '6 456' . 8 109.43(4) ? C34 K2 C35 8 . 8 26.40(4) ? C34 K2 C312 8 . 8 72.22(4) ? C35 K2 C312 8 . 8 62.69(4) ? K1 N11 C12 . . . 119.34(8) ? K1 N11 C12 . . 8 119.34(8) ? C12 N11 C12 . . 8 105.64(14) ? N11 C12 C13 . . . 111.39(13) ? N11 C12 C2 . . . 118.65(12) ? C13 C12 C2 . . . 129.96(13) ? C12 C13 H13 . . . 126.8(10) ? C12 C13 K2 . . '3 556' 129.28(10) ? C12 C13 C13 . . 8 105.79(13) ? H13 C13 K2 . . '3 556' 72.9(10) ? H13 C13 C13 . . 8 127.3(10) ? K2 C13 C13 '3 556' . 8 76.56(8) ? K1 N21 C21 . . . 110.05(9) ? K1 N21 C22 . . . 78.79(7) ? K1 N21 C25 . . . 78.38(7) ? C21 N21 C22 . . . 124.58(12) ? C21 N21 C25 . . . 125.59(12) ? C22 N21 C25 . . . 109.82(11) ? N21 C21 H21a . . . 110.2(11) ? N21 C21 H21b . . . 111.6(10) ? N21 C21 H21c . . . 108.7(10) ? H21a C21 H21b . . . 109.2(14) ? H21a C21 H21c . . . 109.7(14) ? H21b C21 H21c . . . 107.5(14) ? K1 C22 N21 . . . 74.71(7) ? K1 C22 C23 . . . 78.73(9) ? K1 C22 C3 . . . 114.40(8) ? N21 C22 C23 . . . 106.70(12) ? N21 C22 C3 . . . 124.15(13) ? C23 C22 C3 . . . 129.10(13) ? K1 C23 C22 . . . 75.51(8) ? K1 C23 C24 . . . 76.66(9) ? K1 C23 H23 . . . 114.0(11) ? C22 C23 C24 . . . 108.39(13) ? C22 C23 H23 . . . 125.8(10) ? C24 C23 H23 . . . 125.8(10) ? K1 C24 C23 . . . 76.93(9) ? K1 C24 C25 . . . 75.25(8) ? K1 C24 H24 . . . 113.5(10) ? C23 C24 C25 . . . 108.24(13) ? C23 C24 H24 . . . 126.0(10) ? C25 C24 H24 . . . 125.8(10) ? K1 C25 N21 . . . 75.06(7) ? K1 C25 C24 . . . 78.96(9) ? K1 C25 C2 . . . 112.31(8) ? N21 C25 C24 . . . 106.85(12) ? N21 C25 C2 . . . 124.22(12) ? C24 C25 C2 . . . 128.93(13) ? C12 C2 C25 . . . 110.85(11) ? C12 C2 C211 . . . 107.83(12) ? C12 C2 C221 . . . 111.54(12) ? C25 C2 C211 . . . 106.85(11) ? C25 C2 C221 . . . 109.47(12) ? C211 C2 C221 . . . 110.17(12) ? C2 C211 C212 . . . 114.51(13) ? C2 C211 H211a . . . 109.5(9) ? C2 C211 H211b . . . 107.4(9) ? C212 C211 H211a . . . 108.8(9) ? C212 C211 H211b . . . 108.1(9) ? H211a C211 H211b . . . 108.2(13) ? C211 C212 H212a . . . 110.1(12) ? C211 C212 H212b . . . 110.8(12) ? C211 C212 H212c . . . 112.0(13) ? H212a C212 H212b . . . 106.5(17) ? H212a C212 H212c . . . 107.6(17) ? H212b C212 H212c . . . 109.6(18) ? C2 C221 C222 . . . 114.44(13) ? C2 C221 H221a . . . 107.3(10) ? C2 C221 H221b . . . 110.8(10) ? C222 C221 H221a . . . 110.5(10) ? C222 C221 H221b . . . 107.0(10) ? H221a C221 H221b . . . 106.6(14) ? C221 C222 H222a . . . 110.1(12) ? C221 C222 H222b . . . 112.2(13) ? C221 C222 H222c . . . 109.9(12) ? H222a C222 H222b . . . 105.7(18) ? H222a C222 H222c . . . 113.0(17) ? H222b C222 H222c . . . 105.8(18) ? K1 N31 K2 . . . 136.52(6) ? K1 N31 C35 . . . 122.43(8) ? K1 N31 C35 . . 8 122.43(8) ? K2 N31 C35 . . . 78.45(8) ? K2 N31 C35 . . 8 78.45(8) ? C35 N31 C35 . . 8 105.90(14) ? K2 C34 C35 . . . 73.18(8) ? K2 C34 H34 . . . 117.0(10) ? K2 C34 C34 . . 8 76.66(8) ? C35 C34 H34 . . . 129.1(10) ? C35 C34 C34 . . 8 106.18(13) ? H34 C34 C34 . . 8 124.7(10) ? K2 C35 N31 . . . 74.77(8) ? K2 C35 C34 . . . 80.42(8) ? K2 C35 C3 . . . 110.78(8) ? N31 C35 C34 . . . 110.87(12) ? N31 C35 C3 . . . 120.50(12) ? C34 C35 C3 . . . 128.62(13) ? C22 C3 C35 . . . 111.73(11) ? C22 C3 C311 . . . 106.77(12) ? C22 C3 C321 . . . 109.93(12) ? C35 C3 C311 . . . 108.84(11) ? C35 C3 C321 . . . 110.50(12) ? C311 C3 C321 . . . 108.94(12) ? C3 C311 C312 . . . 115.57(15) ? C3 C311 H311a . . . 108.4(10) ? C3 C311 H311b . . . 107.3(10) ? C312 C311 H311a . . . 110.5(10) ? C312 C311 H311b . . . 108.7(10) ? H311a C311 H311b . . . 105.8(15) ? K2 C312 C311 . . . 85.08(10) ? K2 C312 H312a . . . 156.6(12) ? K2 C312 H312b . . . 81.5(12) ? K2 C312 H312c . . . 54.7(11) ? C311 C312 H312a . . . 111.1(11) ? C311 C312 H312b . . . 110.9(12) ? C311 C312 H312c . . . 114.3(10) ? H312a C312 H312b . . . 106.6(16) ? H312a C312 H312c . . . 102.3(16) ? H312b C312 H312c . . . 111.0(16) ? C3 C321 C322 . . . 114.45(15) ? C3 C321 H321a . . . 110.3(10) ? C3 C321 H321b . . . 108.8(10) ? C322 C321 H321a . . . 109.2(10) ? C322 C321 H321b . . . 109.0(10) ? H321a C321 H321b . . . 104.5(14) ? C321 C322 H322a . . . 109.3(13) ? C321 C322 H322b . . . 112.8(11) ? C321 C322 H322c . . . 112.8(14) ? H322a C322 H322b . . . 104.5(17) ? H322a C322 H322c . . . 108.4(18) ? H322b C322 H322c . . . 108.5(17) ? K1 O101 C102 . . . 119.8(5) ? K1 O101 C105 . . . 115.3(3) ? C102 O101 C105 . . . 104.7(5) ? O101 C102 C103 . . . 110.9(8) ? O101 C102 H102a . . . 116.3 ? O101 C102 H102b . . . 145.3 ? C103 C102 H102a . . . 73.4 ? C103 C102 H102b . . . 85.4 ? H102a C102 H102b . . . 97.3 ? C102 C103 C104 . . . 103.8(7) ? C102 C103 H103a . . . 125.8 ? C102 C103 H103b . . . 106.1 ? C104 C103 H103a . . . 111.7 ? C104 C103 H103b . . . 104.4 ? H103a C103 H103b . . . 103.1 ? C103 C104 C105 . . . 101.2(5) ? C103 C104 H104a . . . 107.7 ? C103 C104 H104b . . . 120.6 ? C105 C104 H104a . . . 101.9 ? C105 C104 H104b . . . 110.7 ? H104a C104 H104b . . . 112.6 ? O101 C105 C104 . . . 107.9(5) ? O101 C105 H105a . . . 113.2 ? O101 C105 H105b . . . 113.3 ? C104 C105 H105a . . . 109.0 ? C104 C105 H105b . . . 103.3 ? H105a C105 H105b . . . 109.6 ? K2 O201 C202 . . . 123.2(2) ? K2 O201 C205 . . . 128.1(2) ? K2 O201 C202 . . 8 123.2(2) ? K2 O201 C205 . . 8 128.1(2) ? C202 O201 C205 . . . 99.8(3) ? C202 O201 C205 . . 8 108.7(3) ? C205 O201 C202 . . 8 108.7(3) ? C202 O201 C205 8 . 8 99.8(3) ? O201 C202 C203 . . . 106.5(4) ? O201 C202 H202a . . . 108.9 ? O201 C202 H202b . . . 111.5 ? O201 C202 H202a . . 8 115.4 ? C203 C202 H202a . . . 110.3 ? C203 C202 H202b . . . 112.9 ? C203 C202 H202a . . 8 116.7 ? H202a C202 H202b . . . 106.7 ? H202b C202 H202a . . 8 93.7 ? C202 C203 C204 . . . 103.1(3) ? C202 C203 H203a . . . 108.6 ? C202 C203 H203b . . . 110.8 ? C204 C203 H203a . . . 113.9 ? C204 C203 H203b . . . 111.3 ? C204 C203 C202 . . 8 103.1(3) ? C204 C203 H203a . . 8 113.9 ? C204 C203 H203b . . 8 111.3 ? H203a C203 H203b . . . 109.0 ? C202 C203 H203a 8 . 8 108.6 ? C202 C203 H203b 8 . 8 110.8 ? H203a C203 H203b 8 . 8 109.0 ? C203 C204 C205 . . . 103.4(3) ? C203 C204 H204a . . . 109.3 ? C203 C204 H204b . . . 110.7 ? C203 C204 C205 . . 8 103.4(3) ? C203 C204 H204a . . 8 109.3 ? C203 C204 H204b . . 8 110.7 ? C205 C204 H204a . . . 112.6 ? C205 C204 H204b . . . 111.1 ? H204a C204 H204b . . . 109.5 ? C205 C204 H204a 8 . 8 112.6 ? C205 C204 H204b 8 . 8 111.1 ? H204a C204 H204b 8 . 8 109.5 ? O201 C205 C204 . . . 108.3(4) ? O201 C205 H205a . . . 110.9 ? O201 C205 H205b . . . 107.4 ? O201 C205 H205b . . 8 110.8 ? C204 C205 H205a . . . 114.1 ? C204 C205 H205b . . . 110.4 ? C204 C205 H205b . . 8 113.9 ? H205a C205 H205b . . . 105.7 ? 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 #-------------------------------------------------------------------------- _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 1712 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 32 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _reflns_number_observed ? _reflns_d_resolution_high .732 _reflns_d_resolution_low 11.942 _diffrn_reflns_av_sigmaI/netI .06 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .061 _refine_ls_wR_factor_all .05 _refine_ls_goodness_of_fit_all 1.364 _refine_ls_shift/su_mean .001 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end