Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name _publ_author_address 'Stephen Ralph ' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Alexia M T Bygott ' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Rodney J. Geue ' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'A. M. Sargeson ' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C Willis ' '' _publ_contact_author ;Dr Stephen Ralph Department of Chemistry University of Wollongong Northfields Avenue Wollongong New South Wales 2522 AUSTRALIA ; _publ_contact_author_email SRALPH@UOW.EDU.AU _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? _publ_contact_author_address ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_fax ? #ActaC _publ_contact_author_phone ? #ActaC #_publ_requested_category 'FM ' _publ_contact_author_name 'Anthony C. Willis' _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_section_title #ActaC ; ? ; data_sr1 _database_code_depnum_ccdc_archive 'CCDC 656300' _audit_creation_date 2007-07-24 _audit_creation_method manually_edited_in _audit_update_record ; 1990 - data collected 1990-12 - report written 2007-07-31 - construct cif ; _chemical_compound_source local #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ; C22 H50 N6 2+, (C F3 S O3 -)2 ; _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C24 H50 F6 N6 O6 S2' #ActaC _chemical_formula_weight 696.81 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Philips PW1100/20 software' _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_ADDREF_ABSORB_SORTRF #ActaC _computing_structure_solution shelxs-86 #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 10.713(1) #ActaC _cell_length_b 13.768(1) #ActaC _cell_length_c 23.554(1) #ActaC _cell_angle_alpha 90.0 #ActaC _cell_angle_beta 91.05(1) #ActaC _cell_angle_gamma 90.0 #ActaC _cell_volume 3473.4(4) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 30 #ActaC _cell_measurement_theta_max 36 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M P21/n #ActaC _symmetry_space_group_name_Hall '-P 2yn' #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description block #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max .24 #ActaC _exptl_crystal_size_mid .21 #ActaC _exptl_crystal_size_min .20 #ActaC _exptl_crystal_density_diffrn 1.332 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1480 #ActaC _exptl_absorpt_process_details xtal_ABSORB _exptl_absorpt_coefficient_mu 2.04 #ActaC _exptl_absorpt_correction_type analytical #ActaC _exptl_absorpt_correction_T_min .683 #ActaC _exptl_absorpt_correction_T_max .739 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 1.5418 #ActaC _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'scintillation counter' #ActaC _diffrn_measurement_device_type 'Philips PW1100/20' #ActaC _diffrn_measurement_method ' \w-2\q scans ' #ActaC _diffrn_standards_number 3 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 120 #ActaC _diffrn_standards_decay_% 11 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? ? ? ? ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 5165 #ActaC _diffrn_reflns_av_R_equivalents 0 #ActaC _diffrn_reflns_av_sigmaI/netI ? #ActaC _diffrn_reflns_limit_h_min -12 #ActaC _diffrn_reflns_limit_h_max 12 #ActaC _diffrn_reflns_limit_k_min -15 #ActaC _diffrn_reflns_limit_k_max 15 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 26 #ActaC _diffrn_reflns_theta_min 2 #ActaC _diffrn_reflns_theta_max 60 #ActaC _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 60 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 96 .017 .009 International_Tables_Vol_IV_Table_2.2B H ? 0 200 0 0 International_Tables_Vol_IV_Table_2.2B F ? 0 24 .069 .053 International_Tables_Vol_IV_Table_2.2B N ? 0 24 .029 .018 International_Tables_Vol_IV_Table_2.2B O ? 0 24 .047 .032 International_Tables_Vol_IV_Table_2.2B S ? 0 8 .319 .557 International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC _atom_site_occupancy C1 0.4908(7) 0.3006(6) 0.2010(3) 0.071(5) Uani ? ? 1.0 C2 0.4344(6) 0.2833(4) 0.2594(3) 0.050(4) Uani ? ? 1.0 C3 0.1901(6) 0.1749(5) 0.5036(3) 0.055(4) Uani ? ? 1.0 C4 0.1674(7) 0.1497(6) 0.5661(3) 0.082(5) Uani ? ? 1.0 C11 0.5425(6) 0.2510(5) 0.2991(3) 0.060(4) Uani ? ? 1.0 N12 0.5075(4) 0.2279(4) 0.3578(2) 0.052(3) Uani ? ? 1.0 C13 0.6213(6) 0.2179(5) 0.3936(3) 0.061(4) Uani ? ? 1.0 C14 0.5955(6) 0.1887(5) 0.4540(3) 0.058(4) Uani ? ? 1.0 C141 0.7193(7) 0.1689(7) 0.4860(3) 0.083(5) Uani ? ? 1.0 C15 0.5177(6) 0.2655(5) 0.4836(3) 0.061(4) Uani ? ? 1.0 N16 0.4167(5) 0.2245(4) 0.5185(2) 0.067(4) Uani ? ? 1.0 C17 0.3271(6) 0.1607(5) 0.4880(3) 0.056(4) Uani ? ? 1.0 C21 0.3294(6) 0.2092(5) 0.2525(3) 0.055(4) Uani ? ? 1.0 N22 0.2372(4) 0.2076(3) 0.2986(2) 0.050(3) Uani ? ? 1.0 C23 0.1209(6) 0.1604(5) 0.2791(3) 0.062(4) Uani ? ? 1.0 C24 0.0139(6) 0.1639(6) 0.3180(3) 0.072(5) Uani ? ? 1.0 C241 -0.1062(8) 0.137(1) 0.2859(4) 0.121(8) Uani ? ? 1.0 C25 0.0232(7) 0.0994(6) 0.3685(4) 0.084(6) Uani ? ? 1.0 N26 0.1323(5) 0.1174(5) 0.4056(2) 0.069(4) Uani ? ? 1.0 C27 0.1156(6) 0.1026(5) 0.4663(3) 0.062(4) Uani ? ? 1.0 C31 0.3811(6) 0.3833(4) 0.2764(3) 0.054(4) Uani ? ? 1.0 N32 0.3297(5) 0.3841(3) 0.3345(2) 0.047(3) Uani ? ? 1.0 C33 0.2688(6) 0.4784(5) 0.3484(3) 0.057(4) Uani ? ? 1.0 C34 0.2373(6) 0.4913(4) 0.4099(3) 0.057(4) Uani ? ? 1.0 C341 0.1906(9) 0.5960(5) 0.4172(4) 0.087(6) Uani ? ? 1.0 C35 0.1416(7) 0.4223(6) 0.4329(4) 0.081(5) Uani ? ? 1.0 N36 0.1895(5) 0.3218(4) 0.4410(2) 0.062(3) Uani ? ? 1.0 C37 0.1455(6) 0.2782(5) 0.4929(3) 0.063(4) Uani ? ? 1.0 S5 0.4217(2) -0.0690(1) 0.35974(8) 0.066(1) Uani ? ? 1.0 C5 0.5359(9) -0.0785(8) 0.3056(4) 0.094(7) Uani ? ? 1.0 O51 0.3623(6) 0.0194(4) 0.3484(3) 0.115(5) Uani ? ? 1.0 O52 0.4935(6) -0.0683(5) 0.4114(2) 0.112(5) Uani ? ? 1.0 O53 0.3466(7) -0.1503(5) 0.3539(3) 0.143(6) Uani ? ? 1.0 F51 0.6075(6) -0.1526(5) 0.3112(3) 0.151(6) Uani ? ? 1.0 F52 0.4832(7) -0.0858(6) 0.2554(2) 0.169(6) Uani ? ? 1.0 F53 0.6095(6) -0.0032(5) 0.3062(3) 0.170(6) Uani ? ? 1.0 S6 0.6344(2) 0.5288(2) 0.4003(1) 0.098(2) Uani ? ? 1.0 C6 0.778(1) 0.5144(7) 0.3625(5) 0.108(8) Uani ? ? 1.0 O61A 0.558(1) 0.4691(9) 0.3719(5) 0.109(3) Uiso ? ? 0.59(1) O62A 0.627(1) 0.6233(9) 0.4085(5) 0.109(3) Uiso ? ? 0.59(1) O63A 0.687(1) 0.4780(8) 0.4541(5) 0.109(3) Uiso ? ? 0.59(1) O61B 0.556(1) 0.444(1) 0.3995(6) 0.091(4) Uiso ? ? 0.41(1) O62B 0.645(1) 0.576(1) 0.4504(6) 0.091(4) Uiso ? ? 0.41(1) O63B 0.551(1) 0.608(1) 0.3582(6) 0.091(4) Uiso ? ? 0.41(1) F61A 0.879(1) 0.5606(9) 0.3879(6) 0.121(4) Uiso ? ? 0.52(1) F62A 0.821(1) 0.4278(9) 0.3492(6) 0.121(4) Uiso ? ? 0.52(1) F63A 0.775(1) 0.559(1) 0.3128(6) 0.121(4) Uiso ? ? 0.52(1) F61B 0.831(1) 0.594(1) 0.3549(7) 0.133(5) Uiso ? ? 0.48(1) F62B 0.826(1) 0.444(1) 0.3930(7) 0.133(5) Uiso ? ? 0.48(1) F63B 0.744(1) 0.479(1) 0.3103(6) 0.133(5) Uiso ? ? 0.48(1) H12 0.4641 0.1662 0.3603 0.08 Uiso ? ? 1.0 H16 0.3746 0.2846 0.5383 0.08 Uiso ? ? 1.0 H22 0.2781 0.1792 0.3321 0.08 Uiso ? ? 1.0 H26 0.2104 0.0652 0.3854 0.08 Uiso ? ? 1.0 H32A 0.2681 0.3263 0.3365 0.08 Uiso ? ? 1.0 H32B 0.3865 0.3705 0.3628 0.08 Uiso ? ? 1.0 H36 0.1661 0.2699 0.4047 0.08 Uiso ? ? 1.0 H1A 0.5527 0.3499 0.2031 0.08 Uiso ? ? 1.0 H1B 0.5270 0.2423 0.1871 0.08 Uiso ? ? 1.0 H1C 0.4240 0.3204 0.1765 0.08 Uiso ? ? 1.0 H4A 0.1900 0.0836 0.5725 0.08 Uiso ? ? 1.0 H4B 0.2180 0.1903 0.5896 0.08 Uiso ? ? 1.0 H4C 0.0825 0.1583 0.5757 0.08 Uiso ? ? 1.0 H11A 0.5791 0.1948 0.2830 0.08 Uiso ? ? 1.0 H11B 0.6023 0.3020 0.3004 0.08 Uiso ? ? 1.0 H13A 0.6729 0.1696 0.3770 0.08 Uiso ? ? 1.0 H13B 0.6641 0.2783 0.3939 0.08 Uiso ? ? 1.0 H14 0.5477 0.1306 0.4544 0.08 Uiso ? ? 1.0 H141A 0.7625 0.1178 0.4677 0.08 Uiso ? ? 1.0 H141B 0.7694 0.2259 0.4859 0.08 Uiso ? ? 1.0 H141C 0.7033 0.1507 0.5241 0.08 Uiso ? ? 1.0 H15A 0.5717 0.3028 0.5075 0.08 Uiso ? ? 1.0 H15B 0.4812 0.3061 0.4554 0.08 Uiso ? ? 1.0 H17A 0.3348 0.1726 0.4486 0.08 Uiso ? ? 1.0 H17B 0.3494 0.0954 0.4962 0.08 Uiso ? ? 1.0 H21A 0.2859 0.2230 0.2180 0.08 Uiso ? ? 1.0 H21B 0.3662 0.1465 0.2505 0.08 Uiso ? ? 1.0 H23A 0.0950 0.1906 0.2445 0.08 Uiso ? ? 1.0 H23B 0.1387 0.0938 0.2721 0.08 Uiso ? ? 1.0 H24 0.0138 0.2286 0.3325 0.08 Uiso ? ? 1.0 H241A -0.1191 0.1826 0.2555 0.08 Uiso ? ? 1.0 H241B -0.0986 0.0740 0.2706 0.08 Uiso ? ? 1.0 H241C -0.1741 0.1402 0.3108 0.08 Uiso ? ? 1.0 H25A -0.0495 0.1072 0.3901 0.08 Uiso ? ? 1.0 H25B 0.0281 0.0340 0.3552 0.08 Uiso ? ? 1.0 H27A 0.0292 0.1089 0.4741 0.08 Uiso ? ? 1.0 H27B 0.1420 0.0382 0.4756 0.08 Uiso ? ? 1.0 H31A 0.4462 0.4301 0.2748 0.08 Uiso ? ? 1.0 H31B 0.3165 0.4004 0.2503 0.08 Uiso ? ? 1.0 H33A 0.3236 0.5293 0.3379 0.08 Uiso ? ? 1.0 H33B 0.1935 0.4830 0.3264 0.08 Uiso ? ? 1.0 H34 0.3117 0.4774 0.4307 0.08 Uiso ? ? 1.0 H341A 0.2543 0.6408 0.4072 0.08 Uiso ? ? 1.0 H341B 0.1186 0.6070 0.3942 0.08 Uiso ? ? 1.0 H341C 0.1708 0.6045 0.4562 0.08 Uiso ? ? 1.0 H35A 0.1156 0.4459 0.4688 0.08 Uiso ? ? 1.0 H35B 0.0720 0.4201 0.4075 0.08 Uiso ? ? 1.0 H37A 0.1737 0.3176 0.5238 0.08 Uiso ? ? 1.0 H37B 0.0569 0.2781 0.4915 0.08 Uiso ? ? 1.0 loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC C1 .080(5) .079(5) .056(4) -.003(4) .019(4) .006(4) C2 .055(4) .048(4) .048(4) -.000(3) .004(3) .001(3) C3 .047(4) .072(5) .046(4) -.007(3) .006(3) .005(3) C4 .078(5) .106(6) .062(5) -.004(5) .008(4) .009(4) C11 .053(4) .067(4) .061(4) -.001(3) .001(3) .001(3) N12 .045(3) .055(3) .055(3) -.005(2) -.003(2) -.002(3) C13 .048(4) .072(5) .062(4) .007(3) .003(3) -.003(4) C14 .050(4) .061(4) .063(4) .005(3) .001(3) .001(3) C141 .061(5) .121(7) .067(5) .010(5) -.001(4) .011(5) C15 .054(4) .061(4) .069(5) -.007(3) .014(3) -.004(4) N16 .053(3) .076(4) .071(4) -.008(3) .006(3) -.021(3) C17 .051(4) .057(4) .059(4) .001(3) -.002(3) .007(3) C21 .057(4) .058(4) .049(4) .003(3) -.001(3) -.009(3) N22 .049(3) .051(3) .049(3) -.005(2) -.000(2) -.003(2) C23 .057(4) .068(5) .061(4) -.007(4) -.005(3) -.006(3) C24 .048(4) .093(6) .076(5) -.005(4) -.004(4) -.017(4) C241 .053(5) .21(1) .096(7) -.001(6) -.004(5) -.027(7) C25 .070(5) .099(6) .082(6) -.038(5) .005(4) -.013(5) N26 .066(4) .087(4) .055(4) -.023(3) .008(3) -.006(3) C27 .051(4) .069(5) .065(5) -.010(3) .007(3) .011(4) C31 .065(4) .048(4) .049(4) -.005(3) .002(3) .005(3) N32 .055(3) .040(3) .047(3) .002(2) .001(2) .003(2) C33 .061(4) .049(4) .061(4) .010(3) -.007(3) -.003(3) C34 .063(4) .040(4) .068(5) .007(3) -.006(4) -.005(3) C341 .123(7) .052(5) .086(6) .013(4) .015(5) -.014(4) C35 .071(5) .066(5) .108(7) .015(4) .020(5) .014(4) N36 .066(3) .046(3) .075(4) .005(3) .020(3) .009(3) C37 .047(4) .075(5) .067(5) -.000(3) .000(3) -.008(4) S5 .077(1) .058(1) .062(1) -.004(1) -.0098(9) .0077(9) C5 .088(7) .102(7) .093(7) .011(6) -.002(5) -.005(6) O51 .117(5) .102(5) .126(5) .054(4) .029(4) .045(4) O52 .123(5) .136(6) .075(4) .013(4) -.032(4) .009(4) O53 .158(7) .099(5) .173(8) -.065(5) .031(6) -.022(5) F51 .139(5) .147(6) .168(6) .070(5) -.003(4) -.037(5) F52 .163(6) .28(1) .062(4) .017(6) -.004(4) -.013(5) F53 .145(6) .148(6) .220(8) -.052(5) .097(6) -.039(5) S6 .117(2) .092(2) .086(2) -.051(1) .026(1) -.035(1) C6 .16(1) .069(6) .099(8) -.021(6) .005(7) .003(6) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; The structure was solved with use of direct methods, leading to location of most of the non-hydrogen atoms. One anion appeared to be disordered rotationally about the C---S bond so that there were two orientations of the O and F atoms. Therefore there are two sites for each of these atoms. Relative occupancies were refined and restraints were placed on bonding distances and angles. Isotropic displacement parameters were used for these sites with appropriate constraints on their values. Anisotropic displacement factors were used for other non-H atoms. Hydrogen atoms attached to carbon atoms were included at geometrically determined positions which were periodically recalculated but were not refined. 7 of the 8 hydrogen atoms attached to nitrogen were observed in difference electron density maps and were included at these positions and not refined. Examination of the hydrogen-bonding network suggests that the missing amine H atom is bonded to N16 and its position is calculated to be (0.4512, 0.1803, 0.5455); it is not included in the structure. The largest peaks in a final difference electron density map are located near atoms of the disordered triflate anion. ; _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]' _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC #_refine_ls_abs_structure_Flack . #ActaC _refine_ls_number_reflns 2592 #ActaC _refine_ls_number_parameters 212 #ActaC _refine_ls_number_restraints ? #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all ? #ActaC _refine_ls_R_factor_gt .092 #ActaC _reflns_threshold_expression I>3\s(I) _refine_ls_wR_factor_all ? #ActaC _refine_ls_wR_factor_gt .131 #ActaC _refine_ls_wR_factor_ref .131 #ActaC _refine_ls_goodness_of_fit_all ? #ActaC _refine_ls_goodness_of_fit_ref 3.23 #ActaC _refine_ls_shift/su_max .07 #ActaC _refine_ls_shift/su_mean ? #ActaC _refine_diff_density_min -.69 #ActaC _refine_diff_density_max 0.68 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC C1 C2 1.531(9) . . ? C2 C11 1.542(9) . . ? C2 C21 1.525(9) . . ? C2 C31 1.547(9) . . ? C3 C4 1.53(1) . . ? C3 C17 1.532(9) . . ? C3 C27 1.541(9) . . ? C3 C37 1.52(1) . . ? C11 N12 1.473(9) . . ? N12 C13 1.476(8) . . ? C13 C14 1.51(1) . . ? C14 C141 1.54(1) . . ? C14 C15 1.523(9) . . ? C15 N16 1.483(9) . . ? N16 C17 1.478(8) . . ? C21 N22 1.480(8) . . ? N22 C23 1.470(8) . . ? C23 C24 1.48(1) . . ? C24 C241 1.53(1) . . ? C24 C25 1.49(1) . . ? C25 N26 1.47(1) . . ? N26 C27 1.459(9) . . ? C31 N32 1.486(8) . . ? N32 C33 1.493(8) . . ? C33 C34 1.50(1) . . ? C34 C341 1.54(1) . . ? C34 C35 1.51(1) . . ? C35 N36 1.487(9) . . ? N36 C37 1.448(9) . . ? S5 C5 1.79(1) . . ? S5 O51 1.396(6) . . ? S5 O52 1.427(6) . . ? S5 O53 1.385(7) . . ? C5 F51 1.28(1) . . ? C5 F52 1.30(1) . . ? C5 F53 1.30(1) . . ? S6 C6 1.80(1) . . ? S6 O61A 1.33(1) . . ? S6 O62A 1.32(1) . . ? S6 O63A 1.55(1) . . ? S6 O61B 1.43(2) . . ? S6 O62B 1.35(2) . . ? S6 O63B 1.72(1) . . ? C6 F61A 1.38(2) . . ? C6 F62A 1.32(2) . . ? C6 F63A 1.32(2) . . ? C6 F61B 1.25(2) . . ? C6 F62B 1.31(2) . . ? C6 F63B 1.37(2) . . ? C1 H1A .949 . . ? C1 H1B .953 . . ? C1 H1C .952 . . ? C4 H4A .953 . . ? C4 H4B .950 . . ? C4 H4C .949 . . ? C11 H11A .951 . . ? C11 H11B .950 . . ? N12 H12 .971 . . ? C13 H13A .953 . . ? C13 H13B .949 . . ? C14 H14 .951 . . ? C141 H141A .951 . . ? C141 H141B .951 . . ? C141 H141C .950 . . ? C15 H15A .950 . . ? C15 H15B .947 . . ? N16 H16 1.055 . . ? C17 H17A .948 . . ? C17 H17B .949 . . ? C21 H21A .949 . . ? C21 H21B .951 . . ? N22 H22 .977 . . ? C23 H23A .951 . . ? C23 H23B .952 . . ? C24 H24 .955 . . ? C241 H241A .96 . . ? C241 H241B .94 . . ? C241 H241C .943 . . ? C25 H25A .945 . . ? C25 H25B .954 . . ? N26 H26 1.207 . . ? C27 H27A .950 . . ? C27 H27B .955 . . ? C31 H31A .951 . . ? C31 H31B .947 . . ? N32 H32A 1.035 . . ? N32 H32B .912 . . ? C33 H33A .950 . . ? C33 H33B .952 . . ? C34 H34 .947 . . ? C341 H341A .953 . . ? C341 H341B .948 . . ? C341 H341C .953 . . ? C35 H35A .952 . . ? C35 H35B .948 . . ? N36 H36 1.139 . . ? C37 H37A .953 . . ? C37 H37B .949 . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC C1 C2 C11 106.6(5) . . . ? C1 C2 C21 108.2(5) . . . ? C1 C2 C31 104.3(5) . . . ? C11 C2 C21 114.6(5) . . . ? C11 C2 C31 112.1(5) . . . ? C21 C2 C31 110.4(5) . . . ? C4 C3 C17 111.7(5) . . . ? C4 C3 C27 108.1(6) . . . ? C4 C3 C37 108.5(6) . . . ? C17 C3 C27 105.6(5) . . . ? C17 C3 C37 112.3(5) . . . ? C27 C3 C37 110.6(5) . . . ? C2 C11 N12 115.5(5) . . . ? C11 N12 C13 109.5(5) . . . ? N12 C13 C14 113.6(5) . . . ? C13 C14 C141 109.8(5) . . . ? C13 C14 C15 111.0(6) . . . ? C141 C14 C15 111.9(6) . . . ? C14 C15 N16 113.6(5) . . . ? C15 N16 C17 115.6(5) . . . ? C3 C17 N16 115.1(5) . . . ? C2 C21 N22 115.7(5) . . . ? C21 N22 C23 110.5(5) . . . ? N22 C23 C24 116.9(6) . . . ? C23 C24 C241 109.9(7) . . . ? C23 C24 C25 115.8(6) . . . ? C241 C24 C25 107.2(7) . . . ? C24 C25 N26 114.6(7) . . . ? C25 N26 C27 116.7(6) . . . ? C3 C27 N26 113.4(5) . . . ? C2 C31 N32 112.9(5) . . . ? C31 N32 C33 112.2(5) . . . ? N32 C33 C34 114.8(5) . . . ? C33 C34 C341 107.4(6) . . . ? C33 C34 C35 116.0(6) . . . ? C341 C34 C35 109.0(6) . . . ? C34 C35 N36 113.4(6) . . . ? C35 N36 C37 112.1(6) . . . ? C3 C37 N36 115.0(5) . . . ? C5 S5 O51 104.1(4) . . . ? C5 S5 O52 104.1(4) . . . ? C5 S5 O53 105.9(5) . . . ? O51 S5 O52 113.2(4) . . . ? O51 S5 O53 115.1(4) . . . ? O52 S5 O53 113.2(4) . . . ? S5 C5 F51 113.6(7) . . . ? S5 C5 F52 111.2(7) . . . ? S5 C5 F53 110.8(7) . . . ? F51 C5 F52 106.3(9) . . . ? F51 C5 F53 105.8(8) . . . ? F52 C5 F53 108.8(9) . . . ? C6 S6 O61A 101.8(7) . . . ? C6 S6 O62A 103.7(6) . . . ? C6 S6 O63A 92.9(6) . . . ? C6 S6 O61B 114.1(7) . . . ? C6 S6 O62B 115.4(7) . . . ? C6 S6 O63B 103.1(6) . . . ? O61A S6 O62A 130.2(8) . . . ? O61A S6 O63A 110.2(7) . . . ? O62A S6 O63A 110.4(7) . . . ? O61B S6 O62B 116.0(9) . . . ? O61B S6 O63B 102.1(8) . . . ? O62B S6 O63B 103.6(8) . . . ? S6 C6 F61A 113.9(9) . . . ? S6 C6 F62A 121.3(9) . . . ? S6 C6 F63A 112.5(9) . . . ? S6 C6 F61B 112(1) . . . ? S6 C6 F62B 98.3(9) . . . ? S6 C6 F63B 105.5(9) . . . ? F61A C6 F62A 104(1) . . . ? F61A C6 F63A 100(1) . . . ? F62A C6 F63A 102(1) . . . ? F61B C6 F62B 124(1) . . . ? F61B C6 F63B 107(1) . . . ? F62B C6 F63B 109(1) . . . ? C2 C1 H1A 110.6 . . . ? C2 C1 H1B 110.3 . . . ? C2 C1 H1C 106.6 . . . ? H1A C1 H1B 109.4 . . . ? H1A C1 H1C 110.2 . . . ? H1B C1 H1C 109.8 . . . ? C3 C4 H4A 109.0 . . . ? C3 C4 H4B 109.1 . . . ? C3 C4 H4C 111.8 . . . ? H4A C4 H4B 109.2 . . . ? H4A C4 H4C 108.8 . . . ? H4B C4 H4C 109.0 . . . ? C2 C11 H11A 107.6 . . . ? C2 C11 H11B 107.7 . . . ? N12 C11 H11A 108.2 . . . ? N12 C11 H11B 108.2 . . . ? H11A C11 H11B 109.4 . . . ? C11 N12 H12 112.1 . . . ? C13 N12 H12 105.9 . . . ? N12 C13 H13A 108.1 . . . ? N12 C13 H13B 108.4 . . . ? C14 C13 H13A 108.5 . . . ? C14 C13 H13B 108.9 . . . ? H13A C13 H13B 109.3 . . . ? C13 C14 H14 109.9 . . . ? C141 C14 H14 107.8 . . . ? C15 C14 H14 106.3 . . . ? C14 C141 H141A 109.4 . . . ? C14 C141 H141B 109.5 . . . ? C14 C141 H141C 109.9 . . . ? H141A C141 H141B 109.3 . . . ? H141A C141 H141C 109.4 . . . ? H141B C141 H141C 109.4 . . . ? C14 C15 H15A 108.3 . . . ? C14 C15 H15B 108.1 . . . ? N16 C15 H15A 108.6 . . . ? N16 C15 H15B 108.5 . . . ? H15A C15 H15B 109.7 . . . ? C15 N16 H16 105.6 . . . ? C17 N16 H16 113.7 . . . ? C3 C17 H17A 108.3 . . . ? C3 C17 H17B 108.2 . . . ? N16 C17 H17A 107.7 . . . ? N16 C17 H17B 107.8 . . . ? H17A C17 H17B 109.7 . . . ? C2 C21 H21A 107.9 . . . ? C2 C21 H21B 107.9 . . . ? N22 C21 H21A 107.9 . . . ? N22 C21 H21B 107.9 . . . ? H21A C21 H21B 109.5 . . . ? C21 N22 H22 107.6 . . . ? C23 N22 H22 116.1 . . . ? N22 C23 H23A 107.9 . . . ? N22 C23 H23B 108.0 . . . ? C24 C23 H23A 107.4 . . . ? C24 C23 H23B 107.3 . . . ? H23A C23 H23B 109.2 . . . ? C23 C24 H24 104.9 . . . ? C241 C24 H24 113.3 . . . ? C25 C24 H24 105.8 . . . ? C24 C241 H241A 108.7 . . . ? C24 C241 H241B 109.5 . . . ? C24 C241 H241C 109.5 . . . ? H241A C241 H241B 109 . . . ? H241A C241 H241C 109 . . . ? H241B C241 H241C 111 . . . ? C24 C25 H25A 108.7 . . . ? C24 C25 H25B 107.7 . . . ? N26 C25 H25A 108.3 . . . ? N26 C25 H25B 107.9 . . . ? H25A C25 H25B 109.6 . . . ? C25 N26 H26 102.4 . . . ? C27 N26 H26 113.6 . . . ? C3 C27 H27A 109.1 . . . ? C3 C27 H27B 108.7 . . . ? N26 C27 H27A 108.3 . . . ? N26 C27 H27B 108.2 . . . ? H27A C27 H27B 109.0 . . . ? C2 C31 H31A 108.6 . . . ? C2 C31 H31B 108.7 . . . ? N32 C31 H31A 108.3 . . . ? N32 C31 H31B 108.6 . . . ? H31A C31 H31B 109.7 . . . ? C31 N32 H32A 106.4 . . . ? C31 N32 H32B 114.7 . . . ? C33 N32 H32A 112.1 . . . ? C33 N32 H32B 107.9 . . . ? H32A N32 H32B 103.2 . . . ? N32 C33 H33A 108.1 . . . ? N32 C33 H33B 108.0 . . . ? C34 C33 H33A 108.3 . . . ? C34 C33 H33B 108.2 . . . ? H33A C33 H33B 109.3 . . . ? C33 C34 H34 105.9 . . . ? C341 C34 H34 113.8 . . . ? C35 C34 H34 104.9 . . . ? C34 C341 H341A 110.1 . . . ? C34 C341 H341B 110.5 . . . ? C34 C341 H341C 107.6 . . . ? H341A C341 H341B 109.4 . . . ? H341A C341 H341C 109.4 . . . ? H341B C341 H341C 109.8 . . . ? C34 C35 H35A 108.5 . . . ? C34 C35 H35B 108.9 . . . ? N36 C35 H35A 108.1 . . . ? N36 C35 H35B 108.5 . . . ? H35A C35 H35B 109.4 . . . ? C35 N36 H36 114.6 . . . ? C37 N36 H36 107.6 . . . ? C3 C37 H37A 108.1 . . . ? C3 C37 H37B 108.4 . . . ? N36 C37 H37A 107.8 . . . ? N36 C37 H37B 108.2 . . . ? H37A C37 H37B 109.2 . . . ? #loop_ #_geom_torsion_atom_site_label_1 #ActaC #_geom_torsion_atom_site_label_2 #ActaC #_geom_torsion_atom_site_label_3 #ActaC #_geom_torsion_atom_site_label_4 #ActaC #_geom_torsion #ActaC #_geom_torsion_site_symmetry_1 #ActaC #_geom_torsion_site_symmetry_2 #ActaC #_geom_torsion_site_symmetry_3 #ActaC #_geom_torsion_site_symmetry_4 #ActaC #_geom_torsion_publ_flag #ActaC # ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_number_total 5165 #ActaC _reflns_number_gt 3448 #ActaC #_reflns_observed_criterion refl_observed_if_F>_6.00_sigma(F) _reflns_d_resolution_high 0.890 # ?? 1.0 _reflns_d_resolution_low 22.1 # 9.882 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.7338 _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; Hall, S. R.; Stewart, J. M., Eds. XTAL3.0 Reference Manual. Universities of Western Australia and Maryland. Lamb: Perth, 1990. Olthof -Hazekamp, R., CRYLSQ, in reference 1 (1990). Waser, J., Acta Crystallogr., 16, 1091-1094 (1963). International Tables for X-ray Crystallography; Kynoch Press: Birmingham, England, 1974; Vol. IV, pp 99-101, 149-150. (Present distributor Kluwer Academic Publishers, Dordrecht, The Netherlands.) Sheldrick, G. M. SHELXS-86. In Crystallographic Computing 3, Sheldrick, G. M.; Krueger, C.; Goddard, R., Eds. Oxford University Press: Oxford, England, 1985; pp. 175-189. ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; # start Validation Reply Form _vrf_PLAT027_sr1 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 60.00 Deg. RESPONSE: ... The PW1100/20 could not collect data beyond 2theta 128 deg without risking collisions. 120 deg was used here as it was felt that there was barely any significant data beyond that value. ; _vrf_PLAT353_sr1 ; PROBLEM: Long N-H Bond (0.87A) N26 - H26 ... 1.21 Ang. RESPONSE: ... Hydrogen atoms attached to nitrogen come from a difference electron density map and are not refined. ; # end Validation Reply Form #===END # Attachment 'sr2.cif.txt' data_sr2 _database_code_depnum_ccdc_archive 'CCDC 656301' _audit_creation_date 2007-07-24 _audit_creation_method manually_edited_in _audit_update_record ; 1991 - data collected 1997-07 - refinement completed and report written 2007-07-24 - construct cif ; _chemical_compound_source local #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ; C22 H48 Cd N6 2+, 2(P F6 -), 3(H2 O) ; _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C22 H54 Cd F12 N6 O3 P2' #ActaC _chemical_formula_weight 853.05 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Philips PW1100/20 software' _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_ADDREF_ABSORB_SORTRF #ActaC _computing_structure_solution shelxs-86 #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 19.692(2) #ActaC _cell_length_b 16.616(2) #ActaC _cell_length_c 11.137(1) #ActaC _cell_angle_alpha 90.0 #ActaC _cell_angle_beta 90.0 #ActaC _cell_angle_gamma 90.0 #ActaC _cell_volume 3644.1(7) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 38 #ActaC _cell_measurement_theta_max 42 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M Pnma #ActaC _symmetry_space_group_name_Hall -P_2ac_2n #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +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 _exptl_crystal_description block #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max .26 #ActaC _exptl_crystal_size_mid .18 #ActaC _exptl_crystal_size_min .17 #ActaC _exptl_crystal_density_diffrn 1.555 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1752 #ActaC _exptl_absorpt_process_details xtal_ABSORB _exptl_absorpt_coefficient_mu 6.65 #ActaC _exptl_absorpt_correction_type analytical #ActaC _exptl_absorpt_correction_T_min .352 #ActaC _exptl_absorpt_correction_T_max .449 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 1.5418 #ActaC _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'scintillation counter' #ActaC _diffrn_measurement_device_type 'Philips PW1100/20' #ActaC _diffrn_measurement_method ' \w-2\q scans ' #ActaC _diffrn_standards_number 3 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 90 #ActaC _diffrn_standards_decay_% 18 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? ? ? ? ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 3135 #ActaC _diffrn_reflns_av_R_equivalents 0 #ActaC _diffrn_reflns_av_sigmaI/netI ? #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 22 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 19 #ActaC _diffrn_reflns_limit_l_min -12 #ActaC _diffrn_reflns_limit_l_max 10 #ActaC _diffrn_reflns_theta_min 2 #ActaC _diffrn_reflns_theta_max 64 #ActaC _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 64 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 88 .017 .009 International_Tables_Vol_IV_Table_2.2B H ? 0 216 0 0 International_Tables_Vol_IV_Table_2.2B Cd ? 0 4 -.079 4.653 International_Tables_Vol_IV_Table_2.2B F ? 0 48 .069 .053 International_Tables_Vol_IV_Table_2.2B N ? 0 24 .029 .018 International_Tables_Vol_IV_Table_2.2B O ? 0 12 .047 .032 International_Tables_Vol_IV_Table_2.2B P ? 0 8 .283 .434 International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC _atom_site_occupancy Cd 0.33313(4) .25 0.15136(6) 0.0453(3) Uani ? ? 1.0 C1 0.3331(8) 0.5476(7) 0.1484(11) 0.114(7) Uani ? ? 1.0 C2 0.3346(5) 0.4541(5) 0.1511(8) 0.067(3) Uani ? ? 1.0 C11 0.4062(6) 0.4268(5) 0.1218(9) 0.069(4) Uani ? ? 1.0 N12 0.4124(4) 0.3450(4) 0.0729(6) 0.061(3) Uani ? ? 1.0 C13 0.4842(5) 0.3255(7) 0.0628(10) 0.081(4) Uani ? ? 1.0 C14 0.5006(8) .25 -0.0080(14) 0.078(5) Uani ? ? 1.0 C14A 0.5781(11) .25 -0.0289(23) 0.14(1) Uani ? ? 1.0 C21 0.3114(6) 0.4294(5) 0.2777(9) 0.075(4) Uani ? ? 1.0 N22 0.3265(4) 0.3444(4) 0.3140(6) 0.054(2) Uani ? ? 1.0 C23 0.2871(5) 0.3260(5) 0.4238(7) 0.061(3) Uani ? ? 1.0 C24 0.3082(7) .25 0.4884(9) 0.053(4) Uani ? ? 1.0 C24A 0.2770(8) .25 0.6145(12) 0.073(5) Uani ? ? 1.0 C31 0.2832(6) 0.4286(6) 0.0547(8) 0.078(4) Uani ? ? 1.0 N32 0.2549(4) 0.3453(5) 0.0681(6) 0.061(3) Uani ? ? 1.0 C33 0.2149(6) 0.3260(8) -0.0398(8) 0.089(5) Uani ? ? 1.0 C34 0.1727(8) .25 -0.0313(13) 0.086(7) Uani ? ? 1.0 C34A 0.1205(9) .25 -0.1339(16) 0.12(1) Uani ? ? 1.0 P1 0.4025(5) 0.4790(7) 0.7130(7) 0.100(4) Uani ? ? 0.50(1) F11 0.469(1) 0.510(2) 0.677(2) 0.216(6) Uiso ? ? 0.50(1) F12 0.432(1) 0.460(2) 0.841(2) 0.216(6) Uiso ? ? 0.50(1) F13 0.386(1) 0.563(1) 0.754(2) 0.216(6) Uiso ? ? 0.50(1) F14 0.334(1) 0.455(1) 0.746(2) 0.216(6) Uiso ? ? 0.50(1) F15 0.383(1) 0.506(2) 0.591(2) 0.216(6) Uiso ? ? 0.50(1) F16 0.413(1) 0.397(2) 0.645(2) 0.216(6) Uiso ? ? 0.50(1) P2 0.4277(5) 0.4275(7) 0.7183(7) 0.106(4) Uani ? ? 0.50(1) F21 0.479(1) 0.474(1) 0.653(2) 0.190(5) Uiso ? ? 0.50(1) F22 0.418(1) 0.503(1) 0.817(2) 0.190(5) Uiso ? ? 0.50(1) F23 0.372(1) 0.447(2) 0.627(2) 0.190(5) Uiso ? ? 0.50(1) F24 0.380(1) 0.373(1) 0.792(2) 0.190(5) Uiso ? ? 0.50(1) F25 0.442(1) 0.355(1) 0.641(2) 0.190(5) Uiso ? ? 0.50(1) F26 0.481(1) 0.401(1) 0.804(2) 0.190(5) Uiso ? ? 0.50(1) O1 0.4823(6) 0.3362(10) 0.4131(12) 0.203(8) Uani ? ? 1.0 O2 0.371(1) 0.664(1) 0.728(2) 0.155(9) Uiso ? ? 0.50(1) H1A 0.3639 0.5684 0.2063 0.140 Uiso ? ? 1.0 H1B 0.3456 0.5662 0.0708 0.140 Uiso ? ? 1.0 H1C 0.2883 0.5647 0.1667 0.140 Uiso ? ? 1.0 H11A 0.4246 0.4632 0.0646 0.090 Uiso ? ? 1.0 H11B 0.4322 0.4292 0.1936 0.090 Uiso ? ? 1.0 H12 0.3999 0.3505 0.0000 0.070 Uiso ? ? 1.0 H13A 0.5063 0.3696 0.0249 0.090 Uiso ? ? 1.0 H13B 0.5017 0.3190 0.1417 0.090 Uiso ? ? 1.0 H14 0.4771 .25 -0.0824 0.090 Uiso ? ? 1.0 H14AA 0.5909 0.2964 -0.0735 0.140 Uiso ? ? 1.0 H14AB 0.6014 .25 0.0455 0.140 Uiso ? ? 1.0 H21A 0.3330 0.4641 0.3336 0.090 Uiso ? ? 1.0 H21B 0.2636 0.4366 0.2819 0.090 Uiso ? ? 1.0 H22 0.3674 0.3469 0.3393 0.070 Uiso ? ? 1.0 H23A 0.2920 0.3699 0.4778 0.090 Uiso ? ? 1.0 H23B 0.2407 0.3208 0.4016 0.090 Uiso ? ? 1.0 H24 0.3563 .25 0.4962 0.090 Uiso ? ? 1.0 H24AA 0.2925 0.2956 0.6578 0.140 Uiso ? ? 1.0 H24AB 0.2288 .25 0.6084 0.140 Uiso ? ? 1.0 H31A 0.2463 0.4655 0.0571 0.090 Uiso ? ? 1.0 H31B 0.3050 0.4317 -0.0211 0.090 Uiso ? ? 1.0 H32 0.2249 0.3505 0.1228 0.070 Uiso ? ? 1.0 H33A 0.1851 0.3698 -0.0553 0.090 Uiso ? ? 1.0 H33B 0.2456 0.3201 -0.1052 0.090 Uiso ? ? 1.0 H34 0.1491 .25 0.0431 0.090 Uiso ? ? 1.0 H34AA 0.0920 0.2958 -0.1269 0.140 Uiso ? ? 1.0 H34AB 0.1435 .25 -0.2089 0.140 Uiso ? ? 1.0 loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Cd .0563(5) .0400(4) .0396(4) 0 .0020(4) 0 C1 .19(2) .038(5) .11(1) .010(7) .013(9) .008(6) C2 .101(8) .037(4) .063(5) .013(5) .002(6) .004(4) C11 .101(8) .037(4) .069(6) -.013(5) -.003(5) .006(4) N12 .072(5) .048(4) .062(4) -.004(3) .010(4) -.003(3) C13 .068(7) .076(7) .099(8) -.010(5) .021(6) -.007(6) C14 .074(9) .073(9) .09(1) 0 .026(8) 0 C14A .11(2) .12(2) .19(2) 0 .09(2) 0 C21 .116(8) .043(5) .066(6) .023(5) .008(6) .003(4) N22 .073(5) .045(4) .044(3) .009(3) .005(3) -.001(3) C23 .072(6) .064(5) .046(5) .008(5) .011(4) .000(4) C24 .062(7) .065(7) .032(5) 0 -.001(5) 0 C24A .08(1) .09(1) .051(7) 0 .015(7) 0 C31 .116(9) .061(6) .057(5) .031(6) .007(6) .018(5) N32 .070(5) .071(5) .042(4) .017(4) -.002(3) .005(3) C33 .090(8) .13(1) .047(5) .016(8) -.018(5) .017(6) C34 .059(9) .14(2) .053(8) 0 -.010(7) 0 C34A .06(1) .21(2) .09(1) 0 -.020(9) 0 P1 .096(6) .133(8) .071(4) -.030(6) -.010(4) .002(5) P2 .100(7) .141(9) .077(5) -.034(6) -.017(4) -.005(5) O1 .132(9) .29(2) .19(1) -.05(1) -.036(9) .11(1) _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; The structure was solved with use of heavy atom methods, leading to location of all non-hydrogen atoms of the cation. The anion, however, appeared to be disordered over two sites. Two perchlorate units of occupancy 0.5 were fitted to the peaks in the electron density map and their relative occupancies were varied in subsequent least-squares refinement, with bond lengths and angles being restrained and with F displacement factors being constrained to be equal. In addition one water molecule was identified in a general crystallographic position, plus another of partial occupancy which was mutually exclusive with one position of the disordered perchlorate. The disordered F and O atoms were refined with isotropic displacement factors, and the remaining non-H atoms with anisotropic factors. Hydrogen atoms were included at geometrically determined positions which were periodically recalculated but were not refined. The water H atoms were not located. ; _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0004|Fo|^2^]' _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC #_refine_ls_abs_structure_Flack . #ActaC _refine_ls_number_reflns 2592 #ActaC _refine_ls_number_parameters 212 #ActaC _refine_ls_number_restraints ? #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all ? #ActaC _refine_ls_R_factor_gt .071 #ActaC _reflns_threshold_expression I>3\s(I) _refine_ls_wR_factor_all ? #ActaC _refine_ls_wR_factor_gt .101 #ActaC _refine_ls_wR_factor_ref .101 #ActaC _refine_ls_goodness_of_fit_all ? #ActaC _refine_ls_goodness_of_fit_ref 3.64 #ActaC _refine_ls_shift/su_max .08 #ActaC _refine_ls_shift/su_mean ? #ActaC _refine_diff_density_min -.8 #ActaC _refine_diff_density_max 0.8 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Cd N12 2.386(7) . . ? Cd N22 2.400(7) . . ? Cd N32 2.397(7) . . ? C1 C2 1.55(1) . . ? C2 C11 1.52(2) . . ? C2 C21 1.54(1) . . ? C2 C31 1.53(1) . . ? C11 N12 1.47(1) . . ? C21 N22 1.50(1) . . ? C31 N32 1.50(1) . . ? N12 C13 1.46(1) . . ? N22 C23 1.48(1) . . ? N32 C33 1.47(1) . . ? C13 C14 1.52(1) . . ? C23 C24 1.51(1) . . ? C33 C34 1.52(2) . . ? C14 C14A 1.54(3) . . ? C24 C24A 1.53(2) . . ? C34 C34A 1.54(2) . . ? P1 F11 1.46(3) . . ? P2 F21 1.46(3) . . ? P1 F12 1.57(2) . . ? P2 F22 1.68(3) . . ? P1 F13 1.51(3) . . ? P2 F23 1.52(3) . . ? P1 F14 1.45(2) . . ? P2 F24 1.54(2) . . ? P1 F15 1.48(2) . . ? P2 F25 1.51(2) . . ? P1 F16 1.58(3) . . ? P2 F26 1.49(2) . . ? C1 H1A .95 . . ? C1 H1B .95 . . ? C1 H1C .95 . . ? C11 H11A .95 . . ? C21 H21A .95 . . ? C31 H31A .95 . . ? C11 H11B .95 . . ? C21 H21B .95 . . ? C31 H31B .95 . . ? N12 H12 .85 . . ? N22 H22 .85 . . ? N32 H32 .85 . . ? C13 H13A .95 . . ? C23 H23A .95 . . ? C33 H33A .95 . . ? C13 H13B .95 . . ? C23 H23B .95 . . ? C33 H33B .95 . . ? C14 H14 .95 . . ? C24 H24 .95 . . ? C34 H34 .95 . . ? C14A H14AA .95 . . ? C24A H24AA .95 . . ? C34A H34AA .95 . . ? C14A H14AB .95 . . ? C24A H24AB .95 . . ? C34A H34AB .95 . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N12 Cd N12 82.8(2) . . 8 ? N22 Cd N22 81.6(2) . . 8 ? N32 Cd N32 82.8(3) . . 8 ? N12 Cd N22 83.1(2) . . . ? N12 Cd N32 80.9(3) . . . ? N22 Cd N32 79.9(2) . . . ? N12 Cd N22 138.1(3) . . 8 ? N12 Cd N32 135.7(2) . . 8 ? N22 Cd N32 133.6(2) . . 8 ? C1 C2 C11 108.2(9) . . . ? C1 C2 C21 106.2(8) . . . ? C1 C2 C31 104.5(9) . . . ? C11 C2 C21 113.2(8) . . . ? C11 C2 C31 112.4(8) . . . ? C21 C2 C31 111.8(9) . . . ? C2 C11 N12 115.6(8) . . . ? C2 C21 N22 116.1(8) . . . ? C2 C31 N32 115.5(8) . . . ? Cd N12 C11 115.0(6) . . . ? Cd N22 C21 115.0(5) . . . ? Cd N32 C31 114.2(6) . . . ? Cd N12 C13 121.2(6) . . . ? Cd N22 C23 121.1(5) . . . ? Cd N32 C33 121.0(6) . . . ? C11 N12 C13 108.3(8) . . . ? C21 N22 C23 108.2(7) . . . ? C31 N32 C33 108.6(8) . . . ? N12 C13 C14 115.5(10) . . . ? N22 C23 C24 114.9(8) . . . ? N32 C33 C34 115.1(9) . . . ? C13 C14 C14A 106.8(9) . . . ? C23 C24 C24A 109.0(7) . . . ? C33 C34 C34A 108.7(8) . . . ? C13 C14 C13 111.7(12) . . 8 ? C23 C24 C23 113.3(9) . . 8 ? C33 C34 C33 112.9(11) . . 8 ? C2 C1 H1A 110 . . . ? C2 C1 H1B 110 . . . ? C2 C1 H1C 108 . . . ? H1A C1 H1B 109 . . . ? H1A C1 H1C 110 . . . ? H1B C1 H1C 110 . . . ? C2 C11 H11A 107 . . . ? C2 C21 H21A 107.8 . . . ? C2 C31 H31A 107.9 . . . ? C2 C11 H11B 107.9 . . . ? C2 C21 H21B 107.8 . . . ? C2 C31 H31B 108 . . . ? N12 C11 H11A 108.0 . . . ? N22 C21 H21A 107.9 . . . ? N32 C31 H31A 108 . . . ? N12 C11 H11B 107.8 . . . ? N22 C21 H21B 107.7 . . . ? N32 C31 H31B 107.8 . . . ? H11A C11 H11B 110 . . . ? H21A C21 H21B 110 . . . ? H31A C31 H31B 110 . . . ? Cd N12 H12 103.4 . . . ? Cd N22 H22 103.3 . . . ? Cd N32 H32 103.6 . . . ? C11 N12 H12 103.3 . . . ? C21 N22 H22 103.4 . . . ? C31 N32 H32 103.6 . . . ? C13 N12 H12 103.3 . . . ? C23 N22 H22 103.4 . . . ? C33 N32 H32 103.6 . . . ? N12 C13 H13A 107.9 . . . ? N22 C23 H23A 108.1 . . . ? N32 C33 H33A 108 . . . ? N12 C13 H13B 107.8 . . . ? N22 C23 H23B 108.0 . . . ? N32 C33 H33B 108 . . . ? C14 C13 H13A 108 . . . ? C24 C23 H23A 108.2 . . . ? C34 C33 H33A 108 . . . ? C14 C13 H13B 108 . . . ? C24 C23 H23B 108.2 . . . ? C34 C33 H33B 108 . . . ? H13A C13 H13B 109 . . . ? H23A C23 H23B 109.4 . . . ? H33A C33 H33B 109 . . . ? C13 C14 H14 110.4 . . . ? C23 C24 H24 108.5 . . . ? C33 C34 H34 108.8 . . . ? C14A C14 H14 111 . . . ? C24A C24 H24 108 . . . ? C34A C34 H34 109 . . . ? H14 C14 C13 110.4 . . 8 ? H24 C24 C23 108.5 . . 8 ? H34 C34 C33 108.8 . . 8 ? C14 C14A H14AA 110 . . . ? C24 C24A H24AA 110 . . . ? C34 C34A H34AA 110 . . . ? C14 C14A H14AB 110 . . . ? C24 C24A H24AB 110 . . . ? C34 C34A H34AB 110 . . . ? H14AA C14A H14AB 109 . . . ? H24AA C24A H24AB 111 . . . ? H34AA C34A H34AB 111 . . . ? H14AA C14A H14AA 108 . . 8 ? H24AA C24A H24AA 106 . . 8 ? H34AA C34A H34AA 107 . . 8 ? F11 P1 F12 90(1) . . . ? F21 P2 F22 90(1) . . . ? F11 P1 F13 87(2) . . . ? F21 P2 F23 93(1) . . . ? F11 P1 F14 175(2) . . . ? F21 P2 F24 174(1) . . . ? F11 P1 F15 83(1) . . . ? F21 P2 F25 91(1) . . . ? F11 P1 F16 93(2) . . . ? F21 P2 F26 89(1) . . . ? F12 P1 F13 90(1) . . . ? F22 P2 F23 101(1) . . . ? F12 P1 F14 93(1) . . . ? F22 P2 F24 91(1) . . . ? F12 P1 F15 172(2) . . . ? F22 P2 F25 173(1) . . . ? F12 P1 F16 102(2) . . . ? F22 P2 F26 84(1) . . . ? F13 P1 F14 89(1) . . . ? F23 P2 F24 92(1) . . . ? F13 P1 F15 87(1) . . . ? F23 P2 F25 85(1) . . . ? F13 P1 F16 168(1) . . . ? F23 P2 F26 175(2) . . . ? F14 P1 F15 94(1) . . . ? F24 P2 F25 87(1) . . . ? F14 P1 F16 90(2) . . . ? F24 P2 F26 85(1) . . . ? F15 P1 F16 82(1) . . . ? F25 P2 F26 90(1) . . . ? #loop #_geom_torsion_atom_site_label_1 \ #ActaC #_geom_torsion_atom_site_label_2 #ActaC #_geom_torsion_atom_site_label_3 #ActaC #_geom_torsion_atom_site_label_4 #ActaC #_geom_torsion #ActaC #_geom_torsion_site_symmetry_1 #ActaC #_geom_torsion_site_symmetry_2 #ActaC #_geom_torsion_site_symmetry_3 #ActaC #_geom_torsion_site_symmetry_4 #ActaC #_geom_torsion_publ_flag #ActaC # ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_total 3135 #ActaC _reflns_number_gt 2592 #ActaC #_reflns_observed_criterion refl_observed_if_F>_6.00_sigma(F) _reflns_d_resolution_high 0.858 # ?? 1.0 _reflns_d_resolution_low 22.1 # 9.882 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.7338 _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; Hall, S. R.; Stewart, J. M., Eds. XTAL3.0 Reference Manual. Universities of Western Australia and Maryland. Lamb: Perth, 1990. Olthof -Hazekamp, R., CRYLSQ, in reference 1 (1990). Waser, J., Acta Crystallogr., 16, 1091-1094 (1963). International Tables for X-ray Crystallography; Kynoch Press: Birmingham, England, 1974; Vol. IV, pp 99-101, 149-150. (Present distributor Kluwer Academic Publishers, Dordrecht, The Netherlands.) Sheldrick, G. M. SHELXS-86. In Crystallographic Computing 3, Sheldrick, G. M.; Krueger, C.; Goddard, R., Eds. Oxford University Press: Oxford, England, 1985; pp. 175-189. ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; # start Validation Reply Form _vrf_PLAT027_sr2 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 64.00 Deg. RESPONSE: ... The PW1100/20 could not collect data above 2theta 128 deg without risk of collisions. ; _vrf_PLAT241_sr2 ; PROBLEM: Check High Ueq as Compared to Neighbors for F11 RESPONSE: ... Only one isotropic displacement is used for all F atoms and so it's not surprising that it's large in comparison to the Ueq of the anisotropic P atom sites at the centre. ; _vrf_PLAT242_sr2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for P1 RESPONSE: ... Only one isotropic displacement is used for all F atoms and so it's not surprising that it's large in comparison to the Ueq of the anisotropic P atom sites at the centre. ; _vrf_PLAT306_sr2 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 RESPONSE: ... Yes, H atoms missing on water molecules. ; _vrf_PLAT431_sr2 ; PROBLEM: Short Inter HL..A Contact F13 .. O2 .. 1.73 Ang. RESPONSE: ... Disorder - they are not present simultaneously. ; # end Validation Reply Form #===END # Attachment 'sr3a.cif.txt' data_sr3a _database_code_depnum_ccdc_archive 'CCDC 656302' _audit_update_record ; 1991 - data collected 1997-09 - refinement completed and report written 2007-07-24 - default cif edited ; _audit_creation_date 97-00-24 _audit_creation_method from_xtal_archive_file_using_CIFIO _chemical_compound_source local #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ; C22 H48 Hg N6 2+, 2(P F6 -), 2.82(H2 O) ; _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C22 H53.64 F12 Hg N6 O2.82 P2' #ActaC _chemical_formula_weight 937.62 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Philips PW1100/20 software' _computing_cell_refinement 'Philips PW1100/20 software' _computing_data_reduction xtal_ADDREF_ABSORB_SORTRF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 19.76(5) #ActaC _cell_length_b 16.49(3) #ActaC _cell_length_c 11.03(2) #ActaC _cell_angle_alpha 90.0 #ActaC _cell_angle_beta 90.0 #ActaC _cell_angle_gamma 90.0 #ActaC _cell_volume 3595(13) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 29.4 #ActaC _cell_measurement_theta_max 37.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M Pnma #ActaC _symmetry_space_group_name_Hall -P_2ac_2n #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +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 _exptl_crystal_description prism #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max .30 #ActaC _exptl_crystal_size_mid .22 #ActaC _exptl_crystal_size_min .13 #ActaC _exptl_crystal_density_diffrn 1.732 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1872.8 #1887.57 #ActaC _exptl_absorpt_process_details xtal_ABSORB _exptl_absorpt_coefficient_mu 8.93 #ActaC _exptl_absorpt_correction_type analytical #ActaC _exptl_absorpt_correction_T_min .228 #ActaC _exptl_absorpt_correction_T_max .471 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; Previous experience had shown that the crystal lattice parameters changed systematically on exposure to X-rays, with a major phase change occurring after about 10 hours. Consequently data were collected very rapidly and only to 2-theta 100 deg so that measurements would be completed before this time. ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 1.5418 #ActaC _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'scintillation counter' #ActaC _diffrn_measurement_device_type 'Philips PW1100/20' #ActaC _diffrn_measurement_method ' \w-2\q scans ' #ActaC _diffrn_standards_number 3 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 45 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? ? ? ? ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 1925 #ActaC _diffrn_reflns_av_R_equivalents 0 #ActaC _diffrn_reflns_av_sigmaI/netI .025 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 19 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 16 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 10 #ActaC _diffrn_reflns_theta_min 4.47 #ActaC _diffrn_reflns_theta_max 50.09 #ActaC _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 50 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 88 .017 .009 International_Tables_Vol_IV_Table_2.2B H ? 0 214.56 0 0 International_Tables_Vol_IV_Table_2.2B Hg ? 0 4 -4.99 7.686 International_Tables_Vol_IV_Table_2.2B F ? 0 48 .069 .053 International_Tables_Vol_IV_Table_2.2B N ? 0 24 .029 .018 International_Tables_Vol_IV_Table_2.2B O ? 0 11.28 .047 .032 International_Tables_Vol_IV_Table_2.2B P ? 0 8 .283 .434 International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC _atom_site_occupancy Hg .33424(5) .25000 .15482(9) .0504(7) Uani ? ? 1.0 C1 .3354(13) .5502(13) .153(2) .11(2) Uani ? ? 1.0 C2 .3361(9) .4554(12) .1581(15) .061(5) Uiso ? ? 1.0 C11 .4075(10) .4281(14) .1275(17) .076(6) Uiso ? ? 1.0 N12 .4118(7) .3467(9) .0728(15) .075(12) Uani ? ? 1.0 C13 .4834(11) .3256(14) .062(2) .093(7) Uiso ? ? 1.0 C14 .4998(15) .25000 -.011(2) .074(8) Uiso ? ? 1.0 C14A .578(2) .25000 -.032(5) .18(4) Uani ? ? 1.0 C21 .3123(9) .4301(12) .2832(17) .065(5) Uiso ? ? 1.0 N22 .3286(7) .3457(8) .3197(12) .059(9) Uani ? ? 1.0 C23 .2903(9) .3265(11) .4295(17) .060(5) Uiso ? ? 1.0 C24 .3103(11) .25000 .492(2) .046(6) Uiso ? ? 1.0 C24A .2779(16) .25000 .617(3) .08(2) Uani ? ? 1.0 C31 .2851(10) .4297(13) .0586(18) .074(6) Uiso ? ? 1.0 N32 .2528(7) .3462(9) .0736(12) .062(10) Uani ? ? 1.0 C33 .2132(10) .3260(13) -.038(2) .083(6) Uiso ? ? 1.0 C34 .1739(15) .25000 -.026(3) .085(9) Uiso ? ? 1.0 C34A .1185(18) .25000 -.125(3) .12(3) Uani ? ? 1.0 P1 .4001(8) .4820(10) .7216(14) .137(6) Uiso ? ? 0.59(2) F11 .4742(16) .499(2) .683(3) .285(8) Uiso ? ? 0.59(2) F12 .4139(19) .507(3) .850(3) .285(8) Uiso ? ? 0.59(2) F13 .383(2) .570(2) .692(4) .285(8) Uiso ? ? 0.59(2) F14 .3283(16) .465(2) .756(4) .285(8) Uiso ? ? 0.59(2) F15 .387(2) .455(3) .588(3) .285(8) Uiso ? ? 0.59(2) F16 .417(2) .392(2) .757(4) .285(8) Uiso ? ? 0.59(2) P2 .4259(10) .4351(14) .7139(18) .114(7) Uiso ? ? 0.41(2) F21 .481(2) .478(3) .639(5) .285(8) Uiso ? ? 0.41(2) F22 .439(3) .491(3) .823(4) .285(8) Uiso ? ? 0.41(2) F23 .372(2) .495(3) .664(5) .285(8) Uiso ? ? 0.41(2) F24 .371(2) .391(3) .790(5) .285(8) Uiso ? ? 0.41(2) F25 .414(3) .379(3) .606(4) .285(8) Uiso ? ? 0.41(2) F26 .481(2) .377(3) .762(5) .285(8) Uiso ? ? 0.41(2) O1 .4817(11) .3365(18) .418(2) .25(3) Uani ? ? 1.0 O2 .373(2) .662(3) .750(5) .144(19) Uiso ? ? 0.41(2) H1A .36649 .57164 .21060 .10000 Uiso ? ? 1.0 H1B .34737 .56828 .07423 .10000 Uiso ? ? 1.0 H1C .29076 .56734 .17236 .10000 Uiso ? ? 1.0 H11A .42637 .46591 .07195 .10000 Uiso ? ? 1.0 H11B .43338 .42802 .20010 .10000 Uiso ? ? 1.0 H12 .39879 .35339 .00006 .10000 Uiso ? ? 1.0 H13A .50598 .37010 .02531 .10000 Uiso ? ? 1.0 H13B .50062 .31778 .14183 .10000 Uiso ? ? 1.0 H14 .47615 .25000 -.08639 .10000 Uiso ? ? 1.0 H14AA .59169 .29718 -.07540 .10000 Uiso ? ? 1.0 H14AB .60142 .25000 .04365 .10000 Uiso ? ? 1.0 H21A .33249 .46561 .34061 .10000 Uiso ? ? 1.0 H21B .26454 .43613 .28571 .10000 Uiso ? ? 1.0 H22 .36931 .34868 .34446 .10000 Uiso ? ? 1.0 H23A .29597 .37003 .48499 .10000 Uiso ? ? 1.0 H23B .24390 .32217 .40781 .10000 Uiso ? ? 1.0 H24 .35803 .25000 .50211 .10000 Uiso ? ? 1.0 H24AA .29333 .29546 .66203 .10000 Uiso ? ? 1.0 H24AB .23008 .25000 .60926 .10000 Uiso ? ? 1.0 H31A .24976 .46873 .05708 .10000 Uiso ? ? 1.0 H31B .30826 .43026 -.01697 .10000 Uiso ? ? 1.0 H32 .22340 .35209 .12918 .10000 Uiso ? ? 1.0 H33A .18275 .36920 -.05371 .10000 Uiso ? ? 1.0 H33B .24381 .32042 -.10361 .10000 Uiso ? ? 1.0 H34 .15229 .25000 .05102 .10000 Uiso ? ? 1.0 H34AA .08946 .29536 -.11491 .10000 Uiso ? ? 1.0 H34AB .13892 .25000 -.20340 .10000 Uiso ? ? 1.0 loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Hg .0578(7) .0378(7) .0558(7) .00000 .0028(6) .00000 C1 .18(3) .044(13) .099(18) .013(15) -.028(17) .009(12) N12 .071(10) .055(11) .098(13) .007(8) .024(10) -.007(10) C14A .15(4) .07(3) .33(7) .00000 .18(4) .00000 N22 .085(11) .038(8) .054(9) .002(8) .015(8) .002(7) C24A .10(2) .08(2) .06(2) .00000 .006(18) .00000 N32 .065(9) .069(11) .054(10) .009(8) -.012(8) -.001(8) C34A .10(3) .18(4) .07(2) .00000 -.03(2) .00000 O1 .149(19) .34(4) .25(3) -.07(2) -.07(2) .15(3) _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; The structure was solved with use of heavy atom methods, leading to location of all non-hydrogen atoms of the cation. The anion, however, appeared to be disordered over two sites. Two perchlorate units of occupancy 0.5 were fitted to the peaks in the electron density map and their relative occupancies were varied in subsequent least-squares refinement, with bond lengths and angles being restrained and with F displacement factors being constrained to be equal. In addition one water molecule was identified in a general crystallographic position, plus another of partial occupancy which was mutually exclusive with one position of the disordered perchlorate. Mercury, nitrogen, terminal-carbon and the fully-occupied oxygen atom were refined with anisotropic displacement factors, and the remainder with isotropic factors. Hydrogen atoms were included at geometrically determined positions which were periodically recalculated but were not refined. ; _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]' _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC #_refine_ls_abs_structure_Flack . #ActaC _refine_ls_number_reflns 1492 #ActaC _refine_ls_number_parameters 157 #ActaC _refine_ls_number_restraints 42 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .088 #ActaC _refine_ls_R_factor_gt .067 #ActaC _reflns_threshold_expression I>3\s(I) _refine_ls_wR_factor_all .098 #ActaC _refine_ls_wR_factor_gt .09 #ActaC _refine_ls_wR_factor_ref .09 #ActaC _refine_ls_goodness_of_fit_all 1.955 #ActaC _refine_ls_goodness_of_fit_ref 2.061 #ActaC _refine_ls_shift/su_max .097 #ActaC _refine_ls_shift/su_mean .01 #ActaC _refine_diff_density_min -.881 #ActaC _refine_diff_density_max 1.815 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Hg N12 2.390(15) . . ? Hg N22 2.410(14) . . ? Hg N32 2.432(14) . . ? Hg N12 2.390(15) . 8 ? Hg N22 2.410(14) . 8 ? Hg N32 2.432(14) . 8 ? C1 C2 1.57(3) . . ? C1 H1A .95 . . ? C1 H1B .95 . . ? C1 H1C .95 . . ? C2 C11 1.52(3) . . ? C2 C21 1.52(3) . . ? C2 C31 1.55(3) . . ? C11 N12 1.47(3) . . ? C11 H11A .95 . . ? C11 H11B .95 . . ? N12 C13 1.46(3) . . ? N12 H12 .850 . . ? C13 C14 1.52(3) . . ? C13 H13A .95 . . ? C13 H13B .95 . . ? C14 C14A 1.57(5) . . ? C14 H14 .95 . . ? C14A H14AA .95 . . ? C14A H14AB .95 . . ? C14A H14AA .95 . 8 ? C21 N22 1.49(2) . . ? C21 H21A .95 . . ? C21 H21B .95 . . ? N22 C23 1.46(2) . . ? N22 H22 .850 . . ? C23 C24 1.49(2) . . ? C23 H23A .95 . . ? C23 H23B .95 . . ? C24 C24A 1.52(4) . . ? C24 H24 .95 . . ? C24A H24AA .95 . . ? C24A H24AB .95 . . ? C24A H24AA .95 . 8 ? C31 N32 1.53(3) . . ? C31 H31A .95 . . ? C31 H31B .95 . . ? N32 C33 1.49(3) . . ? N32 H32 .850 . . ? C33 C34 1.48(3) . . ? C33 H33A .95 . . ? C33 H33B .95 . . ? C34 C34A 1.55(5) . . ? C34 H34 .95 . . ? C34A H34AA .95 . . ? C34A H34AB .95 . . ? C34A H34AA .95 . 8 ? P1 F11 1.55(4) . . ? P1 F12 1.50(4) . . ? P1 F13 1.52(4) . . ? P1 F14 1.50(4) . . ? P1 F15 1.56(4) . . ? P1 F16 1.57(4) . . ? P2 F21 1.53(5) . . ? P2 F22 1.54(5) . . ? P2 F23 1.56(5) . . ? P2 F24 1.56(5) . . ? P2 F25 1.53(5) . . ? P2 F26 1.55(5) . . ? #loop_ #_geom_contact_atom_site_label_1 #ActaC #_geom_contact_atom_site_label_2 #ActaC #_geom_contact_distance #ActaC #_geom_contact_site_symmetry_1 #ActaC #_geom_contact_site_symmetry_2 #ActaC #_geom_contact_publ_flag #ActaC # O1 N22 3.22(3) . . ? # O1 F15 3.30(5) . . ? # O1 F21 3.37(6) . . ? # O1 F25 2.56(5) . . ? # O1 H11B 2.99(3) . . ? # O1 H13B 3.08(3) . . ? # O1 H22 2.37(2) . . ? # O1 H24 2.98(2) . . ? # O1 F11 3.07(5) . . ? # O1 F13 3.32(5) . . ? # O1 F21 3.21(6) . . ? # O1 O2 3.41(5) . . ? # O1 H34AA 3.12(2) . . ? # O1 O1 2.85(4) . . ? # O1 H24 2.98(2) . . ? # O2 P1 3.03(5) . . ? # O2 F11 3.43(6) . . ? # O2 F12 2.89(6) . . ? # O2 F13 1.66(6) . . ? # O2 F14 3.37(6) . . ? # O2 F22 3.20(7) . . ? # O2 F23 2.90(7) . . ? # O2 N32 3.17(5) . . ? # O2 H21B 3.19(5) . . ? # O2 H23B 2.91(5) . . ? # O2 H32 2.34(5) . . ? # O2 H34 2.68(5) . . ? # O2 H14AB 2.75(5) . . ? # O2 O1 3.41(5) . . ? # O2 H13A 3.48(5) . . ? # O2 H13B 2.78(5) . . ? # O2 H14AB 2.75(5) . . ? # O2 H34 2.68(5) . . ? # O2 O2 2.91(7) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC ########## ################# N12 Hg N22 83.0(5) . . . ? N12 Hg N32 81.4(5) . . . ? N12 Hg N12 83.7(5) . . 8 ? N12 Hg N22 138.7(5) . . 8 ? N12 Hg N32 136.1(5) . . 8 ? N22 Hg N32 79.6(5) . . . ? N22 Hg N12 138.7(5) . . 8 ? N22 Hg N22 81.8(5) . . 8 ? N22 Hg N32 132.4(5) . . 8 ? N32 Hg N12 136.1(5) . . 8 ? N32 Hg N22 132.4(5) . . 8 ? N32 Hg N32 81.5(5) . . 8 ? N12 Hg N22 83.0(5) 8 . 8 ? N12 Hg N32 81.4(5) 8 . 8 ? N22 Hg N32 79.6(5) 8 . 8 ? C2 C1 H1A 110 . . . ? C2 C1 H1B 110 . . . ? C2 C1 H1C 107 . . . ? H1A C1 H1B 109 . . . ? H1A C1 H1C 110 . . . ? H1B C1 H1C 110 . . . ? C1 C2 C11 107.3(17) . . . ? C1 C2 C21 107.7(16) . . . ? C1 C2 C31 104.1(16) . . . ? C11 C2 C21 114.1(15) . . . ? C11 C2 C31 111.4(15) . . . ? C21 C2 C31 111.6(15) . . . ? C2 C11 N12 114.5(16) . . . ? C2 C11 H11A 108.2 . . . ? C2 C11 H11B 108.2 . . . ? N12 C11 H11A 108.2 . . . ? N12 C11 H11B 108.2 . . . ? H11A C11 H11B 109 . . . ? Hg N12 C11 114.6(11) . . . ? Hg N12 C13 119.5(12) . . . ? Hg N12 H12 104.4 . . . ? C11 N12 C13 107.8(15) . . . ? C11 N12 H12 104.4 . . . ? C13 N12 H12 104.4 . . . ? N12 C13 C14 116(2) . . . ? N12 C13 H13A 108 . . . ? N12 C13 H13B 107.7 . . . ? C14 C13 H13A 108 . . . ? C14 C13 H13B 108 . . . ? H13A C13 H13B 109 . . . ? C13 C14 C14A 106.7(19) . . . ? C13 C14 H14 111.1 . . . ? C13 C14 C13 110(2) . . 8 ? C14A C14 H14 111 . . . ? C14A C14 C13 106.7(19) . . 8 ? H14 C14 C13 111.1 . . 8 ? C14 C14A H14AA 110 . . . ? C14 C14A H14AB 110 . . . ? C14 C14A H14AA 110 . . 8 ? H14AA C14A H14AB 108 . . . ? H14AA C14A H14AA 110 . . 8 ? H14AB C14A H14AA 108 . . 8 ? C2 C21 N22 116.0(15) . . . ? C2 C21 H21A 107.8 . . . ? C2 C21 H21B 107.8 . . . ? N22 C21 H21A 107.9 . . . ? N22 C21 H21B 107.8 . . . ? H21A C21 H21B 109.5 . . . ? Hg N22 C21 114.8(10) . . . ? Hg N22 C23 120.4(10) . . . ? Hg N22 H22 103.7 . . . ? C21 N22 C23 108.3(13) . . . ? C21 N22 H22 103.7 . . . ? C23 N22 H22 103.7 . . . ? N22 C23 C24 115.4(15) . . . ? N22 C23 H23A 108.0 . . . ? N22 C23 H23B 108.0 . . . ? C24 C23 H23A 108.0 . . . ? C24 C23 H23B 108.0 . . . ? H23A C23 H23B 109.5 . . . ? C23 C24 C24A 108.0(13) . . . ? C23 C24 H24 108.4 . . . ? C23 C24 C23 115.4(18) . . 8 ? C24A C24 H24 108 . . . ? C24A C24 C23 108.0(13) . . 8 ? H24 C24 C23 108.4 . . 8 ? C24 C24A H24AA 110 . . . ? C24 C24A H24AB 110 . . . ? C24 C24A H24AA 110 . . 8 ? H24AA C24A H24AB 111 . . . ? H24AA C24A H24AA 104 . . 8 ? H24AB C24A H24AA 111 . . 8 ? C2 C31 N32 116.2(15) . . . ? C2 C31 H31A 107.8 . . . ? C2 C31 H31B 107.8 . . . ? N32 C31 H31A 107.7 . . . ? N32 C31 H31B 107.7 . . . ? H31A C31 H31B 109 . . . ? Hg N32 C31 110.6(10) . . . ? Hg N32 C33 120.3(11) . . . ? Hg N32 H32 105.1 . . . ? C31 N32 C33 109.4(14) . . . ? C31 N32 H32 105.1 . . . ? C33 N32 H32 105.1 . . . ? N32 C33 C34 113(2) . . . ? N32 C33 H33A 108.5 . . . ? N32 C33 H33B 108.5 . . . ? C34 C33 H33A 109 . . . ? C34 C33 H33B 109 . . . ? H33A C33 H33B 109 . . . ? C33 C34 C34A 108.0(17) . . . ? C33 C34 H34 108.3 . . . ? C33 C34 C33 116(2) . . 8 ? C34A C34 H34 108 . . . ? C34A C34 C33 108.0(17) . . 8 ? H34 C34 C33 108.3 . . 8 ? C34 C34A H34AA 110 . . . ? C34 C34A H34AB 110 . . . ? C34 C34A H34AA 110 . . 8 ? H34AA C34A H34AB 112 . . . ? H34AA C34A H34AA 104 . . 8 ? H34AB C34A H34AA 112 . . 8 ? F11 P1 F12 92(2) . . . ? F11 P1 F13 89(2) . . . ? F11 P1 F14 179(2) . . . ? F11 P1 F15 87(2) . . . ? F11 P1 F16 92(2) . . . ? F12 P1 F13 89(2) . . . ? F12 P1 F14 89(2) . . . ? F12 P1 F15 179(2) . . . ? F12 P1 F16 89(2) . . . ? F13 P1 F14 91(2) . . . ? F13 P1 F15 92(2) . . . ? F13 P1 F16 178(2) . . . ? F14 P1 F15 91(2) . . . ? F14 P1 F16 87(2) . . . ? F15 P1 F16 90(2) . . . ? P1 P2 F11 78(2) . . . ? F21 P2 F22 92(3) . . . ? F21 P2 F23 90(3) . . . ? F21 P2 F24 179(3) . . . ? F21 P2 F25 88(3) . . . ? F21 P2 F26 88(3) . . . ? F22 P2 F23 90(3) . . . ? F22 P2 F24 89(3) . . . ? F22 P2 F25 179(3) . . . ? F22 P2 F26 89(3) . . . ? F23 P2 F24 91(3) . . . ? F23 P2 F25 91(3) . . . ? F23 P2 F26 179(3) . . . ? F24 P2 F25 92(3) . . . ? F24 P2 F26 91(3) . . . ? F25 P2 F26 90(3) . . . ? #loop_ #_geom_torsion_atom_site_label_1 #ActaC #_geom_torsion_atom_site_label_2 #ActaC #_geom_torsion_atom_site_label_3 #ActaC #_geom_torsion_atom_site_label_4 #ActaC #_geom_torsion #ActaC #_geom_torsion_site_symmetry_1 #ActaC #_geom_torsion_site_symmetry_2 #ActaC #_geom_torsion_site_symmetry_3 #ActaC #_geom_torsion_site_symmetry_4 #ActaC #_geom_torsion_publ_flag #ActaC # ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _reflns_number_total 1925 #ActaC _reflns_number_gt 1474 #ActaC #_reflns_observed_criterion refl_observed_if_F>_6.00_sigma(F) _reflns_d_resolution_high 1.005 _reflns_d_resolution_low 9.882 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.7338 _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; Hall, S. R.; King, G. S. D.; Stewart, J. M., Eds. XTAL3.4 User's Manual. University of Western Australia. Lamb: Perth, 1995. Olthof -Hazekamp, R., CRYLSQ, in reference 1 (1995). Waser, J., Acta Crystallogr., 16, 1091-1094 (1963). International Tables for X-ray Crystallography; Kynoch Press: Birmingham, England, 1974; Vol. IV, pp 99-101, 149-150. (Present distributor Kluwer Academic Publishers, Dordrecht, The Netherlands.) ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; # start Validation Reply Form _vrf_THETM01_sr3a ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: ... Crystals of this compound decay when exposured to X-rays, with a major change occurring after about 10 hours. Consequently data were collected very rapidly and only to 2-theta 100 deg so that measurements would be completed before this happened. ; _vrf_PLAT023_sr3a ; PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]..... 50.09 Deg. RESPONSE: ... Crystals of this compound decay when exposured to X-rays, with a major change occurring after about 10 hours. Consequently data were collected very rapidly and only to 2-theta 100 deg so that measurements would be completed before this happened. ; _vrf_PLAT027_sr3a ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 50.00 Deg. RESPONSE: ... Crystals of this compound decay when exposured to X-rays, with a major change occurring after about 10 hours. Consequently data were collected very rapidly and only to 2-theta 100 deg so that measurements would be completed before this happened. ; _vrf_PLAT242_sr3a ; PROBLEM: Check Low Ueq as Compared to Neighbors for C14 RESPONSE: ... This is a low precision (but very interesting!) structure and C14's Uiso is only 2 or 3 su's different from it's neighbours' Ueq's. . ; _vrf_PLAT306_sr3a ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 RESPONSE: ... Yes, the H's are missing from the water molecules. ; # end Validation Reply Form #===END