Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1218 data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-12-10 _audit_update_record ? #=========================================================================== #== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Crawley, Western Australia 6009, Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_address 'Ogden, Mark I.' ? 'Skelton, Brian W.' ; Department of Chemistry, University of Western Australia, Crawley, WA 6009, Australia. ; 'White, Allan H.' ? _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram 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. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_mofe _database_code_CSD 165283 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C62 H90 Cl8 Fe3 N3 O8' _chemical_formula_moiety ? _chemical_formula_weight 1456.58 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.8800(10) _cell_length_b 14.7650(10) _cell_length_c 25.914(2) _cell_angle_alpha 90.00000 _cell_angle_beta 100.6810(10) _cell_angle_gamma 90.00000 _cell_volume 7474.7(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 23.1 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .909 _exptl_crystal_description rhomboid _exptl_crystal_size_max .45 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .45 _exptl_crystal_size_rad ? _exptl_crystal_colour dark _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 .665 _exptl_absorpt_correction_T_max .831 _diffrn_reflns_number 70920 _reflns_number_total 18533 _reflns_Friedel_coverage 0 _reflns_number_gt 13314 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.04 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _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 .043 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_number_reflns 13314 _refine_ls_number_parameters 1154 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .056 _refine_diff_density_min -.603 _refine_diff_density_max .594 _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 ? 0 248 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 360 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 32 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 12 .301 .845 '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' O ? 0 32 .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 Fe1 .436687(16) .23533(2) .757697(13) .02204(15) Uani ? ? 1.00000 ? ? O11 .40900(8) .34712(10) .69559(6) .0224(7) Uani ? ? 1.00000 ? ? C101 .35184(13) .40242(17) .70213(11) .0272(12) Uani ? ? 1.00000 ? ? C102 .31505(12) .35262(16) .73974(9) .0256(11) Uani ? ? 1.00000 ? ? O102 .33725(8) .27651(11) .75671(6) .0275(8) Uani ? ? 1.00000 ? ? N10 .26030(11) .38857(14) .75318(9) .0343(11) Uani ? ? 1.00000 ? ? C1011 .22375(17) .3383(2) .78870(15) .0500(18) Uani ? ? 1.00000 ? ? C1012 .1674(2) .2812(3) .7588(2) .075(3) Uani ? ? 1.00000 ? ? C1021 .23181(17) .4765(2) .73432(16) .0502(18) Uani ? ? 1.00000 ? ? C1022 .2516(2) .5514(2) .7735(2) .067(2) Uani ? ? 1.00000 ? ? C11 .41941(11) .34248(15) .64302(9) .0219(10) Uani ? ? 1.00000 ? ? C12 .47336(11) .39133(15) .62982(9) .0218(10) Uani ? ? 1.00000 ? ? C13 .48376(12) .38639(16) .57804(9) .0250(11) Uani ? ? 1.00000 ? ? C14 .44270(12) .33452(16) .54016(9) .0254(11) Uani ? ? 1.00000 ? ? C141 .45478(13) .32697(18) .48361(9) .0312(12) Uani ? ? 1.00000 ? ? C142 .52370(16) .3679(2) .47714(12) .0397(16) Uani ? ? 1.00000 ? ? C143 .4549(2) .2271(2) .46806(14) .0484(18) Uani ? ? 1.00000 ? ? C144 .39715(18) .3772(3) .44692(12) .0481(18) Uani ? ? 1.00000 ? ? C15 .38901(13) .28701(16) .55553(10) .0263(11) Uani ? ? 1.00000 ? ? C16 .37657(11) .28864(15) .60653(9) .0236(10) Uani ? ? 1.00000 ? ? C1 .32072(12) .22788(16) .61986(10) .0251(11) Uani ? ? 1.00000 ? ? O21 .54588(8) .31819(11) .75685(6) .0224(7) Uani ? ? 1.00000 ? ? C201 .56479(13) .37765(18) .80120(10) .0273(12) Uani ? ? 1.00000 ? ? C202 .50857(14) .37533(19) .83201(10) .0349(13) Uani ? ? 1.00000 ? ? O202 .45731(10) .32532(15) .81613(7) .0465(11) Uani ? ? 1.00000 ? ? N20 .51298(14) .4233(2) .87531(10) .0553(15) Uani ? ? 1.00000 ? ? C2011 .4584(3) .4136(5) .9064(2) .127(4) Uani ? ? 1.00000 ? ? C2012 .3975(4) .4587(6) .8882(3) .174(7) Uani ? ? 1.00000 ? ? C2021 .5740(2) .4774(3) .89802(16) .060(2) Uani ? ? 1.00000 ? ? C2022 .5564(3) .5729(3) .9103(2) .078(3) Uani ? ? 1.00000 ? ? C21 .59643(11) .32505(15) .72471(9) .0222(10) Uani ? ? 1.00000 ? ? C22 .65425(11) .26951(16) .73578(9) .0236(10) Uani ? ? 1.00000 ? ? C23 .70393(12) .27955(16) .70448(9) .0246(11) Uani ? ? 1.00000 ? ? C24 .69799(11) .34207(16) .66374(9) .0251(11) Uani ? ? 1.00000 ? ? C241 .75348(12) .35246(18) .62990(10) .0301(12) Uani ? ? 1.00000 ? ? C242 .7230(2) .3858(4) .57498(15) .067(2) Uani ? ? 1.00000 ? ? C243 .78838(18) .2618(2) .62415(14) .0449(17) Uani ? ? 1.00000 ? ? C244 .80647(18) .4206(3) .65646(17) .053(2) Uani ? ? 1.00000 ? ? C25 .64006(12) .39714(16) .65559(9) .0247(11) Uani ? ? 1.00000 ? ? C26 .58838(11) .38901(15) .68490(9) .0223(10) Uani ? ? 1.00000 ? ? C2 .52343(11) .44411(16) .67001(9) .0224(11) Uani ? ? 1.00000 ? ? O31 .52606(8) .13083(11) .78597(6) .0245(8) Uani ? ? 1.00000 ? ? C301 .52058(13) .0815(2) .83302(10) .0311(13) Uani ? ? 1.00000 ? ? C302 .44858(13) .09778(17) .84269(10) .0302(12) Uani ? ? 1.00000 ? ? O302 .41084(9) .15248(12) .81419(7) .0337(9) Uani ? ? 1.00000 ? ? N30 .42683(12) .05374(16) .88092(9) .0398(12) Uani ? ? 1.00000 ? ? C3011 .4668(2) -.0170(3) .91313(15) .067(2) Uani ? ? 1.00000 ? ? C3012 .4472(4) -.1106(3) .8938(2) .102(4) Uani ? ? 1.00000 ? ? C3021 .35778(16) .0725(2) .89187(13) .0464(17) Uani ? ? 1.00000 ? ? C3022 .3590(3) .1384(4) .9350(2) .080(3) Uani ? ? 1.00000 ? ? C31 .56283(11) .08247(15) .75273(9) .0228(10) Uani ? ? 1.00000 ? ? C32 .53187(11) .00953(15) .72325(9) .0236(11) Uani ? ? 1.00000 ? ? C33 .57072(12) -.03756(16) .69265(10) .0255(11) Uani ? ? 1.00000 ? ? C34 .63854(11) -.01527(16) .69101(9) .0243(11) Uani ? ? 1.00000 ? ? C341 .67775(12) -.06900(17) .65571(10) .0287(12) Uani ? ? 1.00000 ? ? C342 .67026(15) -.17096(19) .66414(12) .0350(14) Uani ? ? 1.00000 ? ? C343 .75434(15) -.0465(2) .66682(15) .0460(17) Uani ? ? 1.00000 ? ? C344 .64816(17) -.0439(2) .59885(11) .0403(16) Uani ? ? 1.00000 ? ? C35 .66627(12) .05893(16) .72038(9) .0245(11) Uani ? ? 1.00000 ? ? C36 .62933(11) .10960(15) .75090(9) .0225(10) Uani ? ? 1.00000 ? ? C3 .66083(12) .19552(16) .77693(9) .0241(11) Uani ? ? 1.00000 ? ? O41 .42028(8) .16057(11) .70230(6) .0247(8) Uani ? ? 1.00000 ? ? C41 .39205(11) .10119(15) .66579(9) .0220(10) Uani ? ? 1.00000 ? ? C42 .34275(11) .12983(16) .62308(9) .0241(11) Uani ? ? 1.00000 ? ? C43 .31514(12) .06657(17) .58529(10) .0270(11) Uani ? ? 1.00000 ? ? C44 .33538(12) -.02431(17) .58864(10) .0285(12) Uani ? ? 1.00000 ? ? C441 .30810(15) -.09327(18) .54528(11) .0378(14) Uani ? ? 1.00000 ? ? C442 .3684(2) -.1206(3) .51864(15) .055(2) Uani ? ? 1.00000 ? ? C443 .2806(3) -.1773(3) .56857(16) .063(2) Uani ? ? 1.00000 ? ? C444 .25141(17) -.0546(2) .50340(13) .0464(17) Uani ? ? 1.00000 ? ? C45 .38306(12) -.05088(17) .63280(10) .0271(12) Uani ? ? 1.00000 ? ? C46 .41086(11) .00952(15) .67177(9) .0228(10) Uani ? ? 1.00000 ? ? C4 .45845(11) -.02006(17) .72120(10) .0247(11) Uani ? ? 1.00000 ? ? Fe2 .524458(18) .67685(2) .745542(14) .02932(17) Uani ? ? 1.00000 ? ? Cl21 .62420(3) .61182(5) .74861(3) .0438(4) Uani ? ? 1.00000 ? ? Cl22 .45344(4) .58054(5) .77284(3) .0452(4) Uani ? ? 1.00000 ? ? Cl23 .53560(4) .79346(5) .79777(3) .0419(3) Uani ? ? 1.00000 ? ? Cl24 .47960(4) .71796(5) .66516(3) .0416(3) Uani ? ? 1.00000 ? ? Fe3 .64320(2) .22531(3) .988836(17) .0463(2) Uani ? ? 1.00000 ? ? Cl31 .70806(11) .11469(15) 1.03212(8) .0485(9) Uani ? ? .50000 ? ? Cl32 .53917(10) .16605(16) .96557(7) .0641(11) Uani ? ? .50000 ? ? Cl33 .68111(13) .25733(16) .91822(8) .0694(12) Uani ? ? .50000 ? ? Cl34 .6372(3) .3386(2) 1.03745(14) .0596(14) Uani ? ? .50000 ? ? Cl31' .6725(2) .0933(2) 1.00732(19) .158(3) Uani ? ? .50000 ? ? Cl32' .54422(15) .2340(3) .93836(16) .145(3) Uani ? ? .50000 ? ? Cl33' .71972(16) .29114(18) .94837(12) .0942(17) Uani ? ? .50000 ? ? Cl34' .6360(3) .3156(4) 1.05610(17) .098(3) Uani ? ? .50000 ? ? O01 .3164(4) .6009(5) .6452(3) .118(5) Uani ? ? .50000 ? ? O02 .3202(5) .5057(7) .5562(4) .167(8) Uani ? ? .50000 ? ? H101a .3220(14) .4101(18) .6685(11) .036(8) Uiso ? ? 1.00000 ? ? H101b .3649(15) .463(2) .7159(11) .041(8) Uiso ? ? 1.00000 ? ? H1011a .2084(17) .384(2) .8109(13) .056(9) Uiso ? ? 1.00000 ? ? H1011b .2596(18) .303(2) .8114(13) .060(10) Uiso ? ? 1.00000 ? ? H1012a .147(2) .251(3) .7829(17) .088(14) Uiso ? ? 1.00000 ? ? H1012b .184(2) .240(3) .7381(17) .090(15) Uiso ? ? 1.00000 ? ? H1012c .128(2) .314(3) .7335(15) .078(13) Uiso ? ? 1.00000 ? ? H1021a .1870(16) .470(2) .7274(11) .039(8) Uiso ? ? 1.00000 ? ? H1021b .2442(17) .489(2) .7025(13) .057(10) Uiso ? ? 1.00000 ? ? H1022a .233(2) .609(3) .7641(14) .076(12) Uiso ? ? 1.00000 ? ? H1022b .300(2) .557(3) .7766(14) .074(12) Uiso ? ? 1.00000 ? ? H1022c .243(2) .537(3) .8092(17) .087(14) Uiso ? ? 1.00000 ? ? H13 .5227(14) .4188(18) .5704(10) .031(7) Uiso ? ? 1.00000 ? ? H142a .5299(15) .360(2) .4427(12) .045(8) Uiso ? ? 1.00000 ? ? H142b .5652(18) .337(2) .5013(14) .063(10) Uiso ? ? 1.00000 ? ? H142c .5275(14) .430(2) .4854(11) .038(8) Uiso ? ? 1.00000 ? ? H143a .4641(17) .221(2) .4308(14) .058(10) Uiso ? ? 1.00000 ? ? H143b .412(2) .204(2) .4671(14) .067(11) Uiso ? ? 1.00000 ? ? H143c .4915(18) .192(2) .4936(14) .058(10) Uiso ? ? 1.00000 ? ? H144a .4046(16) .370(2) .4122(13) .054(9) Uiso ? ? 1.00000 ? ? H144b .3942(16) .445(2) .4572(12) .054(9) Uiso ? ? 1.00000 ? ? H144c .3519(17) .353(2) .4485(12) .049(9) Uiso ? ? 1.00000 ? ? H15 .3600(13) .2525(17) .5320(10) .023(6) Uiso ? ? 1.00000 ? ? H1a .2793(12) .2357(15) .5938(9) .017(6) Uiso ? ? 1.00000 ? ? H1b .3081(13) .2451(16) .6526(10) .024(6) Uiso ? ? 1.00000 ? ? H201a .5686(13) .437(2) .7886(10) .032(7) Uiso ? ? 1.00000 ? ? H201b .6035(14) .3576(18) .8220(11) .031(7) Uiso ? ? 1.00000 ? ? H2011a .4748(10) .431(2) .9456(11) .059(10) Uiso ? ? 1.00000 ? ? H2011b .4440(16) .353(3) .9050(11) .22(4) Uiso ? ? 1.00000 ? ? H2012a .363(2) .444(4) .912(2) .23(3) Uiso ? ? 1.00000 ? ? H2012b .376(2) .434(4) .8522(19) .18(3) Uiso ? ? 1.00000 ? ? H2012c .4080(12) .524(3) .888(2) .16(3) Uiso ? ? 1.00000 ? ? H2021a .600(2) .484(3) .8737(19) .110(17) Uiso ? ? 1.00000 ? ? H2021b .597(2) .467(3) .9346(16) .081(13) Uiso ? ? 1.00000 ? ? H2022a .605(3) .604(3) .9248(18) .110(16) Uiso ? ? 1.00000 ? ? H2022b .520(3) .571(4) .944(2) .14(2) Uiso ? ? 1.00000 ? ? H2022c .528(4) .588(5) .873(3) .19(3) Uiso ? ? 1.00000 ? ? H23 .7398(13) .2435(16) .7126(9) .019(6) Uiso ? ? 1.00000 ? ? H242a .7585(18) .385(2) .5558(13) .063(10) Uiso ? ? 1.00000 ? ? H242b .704(2) .451(3) .5754(14) .072(12) Uiso ? ? 1.00000 ? ? H242c .688(2) .346(3) .5616(16) .087(16) Uiso ? ? 1.00000 ? ? H243a .8221(16) .268(2) .5994(12) .048(9) Uiso ? ? 1.00000 ? ? H243b .758(2) .221(2) .6109(14) .063(11) Uiso ? ? 1.00000 ? ? H243c .8107(17) .241(2) .6564(13) .049(9) Uiso ? ? 1.00000 ? ? H244a .8435(17) .429(2) .6365(13) .057(9) Uiso ? ? 1.00000 ? ? H244b .8268(16) .400(2) .6911(13) .046(9) Uiso ? ? 1.00000 ? ? H244c .785(2) .481(3) .6571(15) .082(13) Uiso ? ? 1.00000 ? ? H25 .6340(14) .4385(19) .6314(11) .034(7) Uiso ? ? 1.00000 ? ? H2a .5056(12) .4578(16) .7020(9) .020(6) Uiso ? ? 1.00000 ? ? H2b .5360(11) .5031(16) .6566(9) .014(5) Uiso ? ? 1.00000 ? ? H301a .5530(15) .1046(19) .8613(11) .038(8) Uiso ? ? 1.00000 ? ? H301b .5281(13) .014(2) .8291(10) .033(7) Uiso ? ? 1.00000 ? ? H3011a .4595(15) -.004(2) .9516(12) .044(8) Uiso ? ? 1.00000 ? ? H3011b .512(2) -.002(2) .9150(14) .063(11) Uiso ? ? 1.00000 ? ? H3012a .472(2) -.149(3) .9169(19) .103(16) Uiso ? ? 1.00000 ? ? H3012b .457(2) -.118(3) .8563(19) .106(15) Uiso ? ? 1.00000 ? ? H3012c .400(3) -.119(3) .8964(19) .106(17) Uiso ? ? 1.00000 ? ? H3021a .3402(15) .012(2) .9024(12) .048(9) Uiso ? ? 1.00000 ? ? H3021b .3310(17) .094(2) .8606(13) .058(10) Uiso ? ? 1.00000 ? ? H3022a .312(2) .146(3) .9425(15) .079(12) Uiso ? ? 1.00000 ? ? H3022b .380(2) .196(3) .9292(18) .098(17) Uiso ? ? 1.00000 ? ? H3022c .391(2) .122(3) .9668(18) .091(16) Uiso ? ? 1.00000 ? ? H33 .5485(13) -.0842(17) .6723(10) .025(7) Uiso ? ? 1.00000 ? ? H342a .6978(15) -.204(2) .6415(12) .046(8) Uiso ? ? 1.00000 ? ? H342b .6208(16) -.191(2) .6553(11) .041(8) Uiso ? ? 1.00000 ? ? H342c .6881(16) -.186(2) .6993(13) .052(9) Uiso ? ? 1.00000 ? ? H343a .7749(18) -.084(2) .6414(13) .064(10) Uiso ? ? 1.00000 ? ? H343b .7729(16) -.057(2) .7046(13) .051(9) Uiso ? ? 1.00000 ? ? H343c .7608(14) .013(2) .6557(11) .038(8) Uiso ? ? 1.00000 ? ? H344a .6689(15) -.077(2) .5739(11) .041(8) Uiso ? ? 1.00000 ? ? H344b .6525(16) .022(2) .5939(12) .053(9) Uiso ? ? 1.00000 ? ? H344c .5973(16) -.054(2) .5894(11) .042(8) Uiso ? ? 1.00000 ? ? H35 .7119(12) .0744(14) .7211(8) .012(5) Uiso ? ? 1.00000 ? ? H3a .6401(13) .2152(17) .8041(10) .029(7) Uiso ? ? 1.00000 ? ? H3b .7104(13) .1845(17) .7921(9) .025(6) Uiso ? ? 1.00000 ? ? H43 .2814(13) .0866(16) .5566(10) .023(6) Uiso ? ? 1.00000 ? ? H442a .354(2) -.168(3) .4901(16) .085(13) Uiso ? ? 1.00000 ? ? H442b .403(2) -.149(3) .5464(15) .075(12) Uiso ? ? 1.00000 ? ? H442c .3848(19) -.064(3) .5029(14) .070(12) Uiso ? ? 1.00000 ? ? H443a .266(2) -.222(3) .5393(16) .086(13) Uiso ? ? 1.00000 ? ? H443b .238(2) -.159(3) .5838(19) .110(17) Uiso ? ? 1.00000 ? ? H443c .3187(19) -.206(2) .5922(14) .061(11) Uiso ? ? 1.00000 ? ? H444a .2349(17) -.100(2) .4765(13) .063(10) Uiso ? ? 1.00000 ? ? H444b .2681(17) -.004(2) .4840(13) .061(10) Uiso ? ? 1.00000 ? ? H444c .2108(16) -.039(2) .5209(12) .049(9) Uiso ? ? 1.00000 ? ? H45 .3988(12) -.1114(17) .6360(9) .023(6) Uiso ? ? 1.00000 ? ? H4a .4403(13) .0038(17) .7522(10) .031(7) Uiso ? ? 1.00000 ? ? H4b .4559(12) -.0812(17) .7232(9) .018(6) 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 Fe1 .02025(16) .02457(17) .02260(16) .00070(13) .00731(13) .00167(13) O11 .0206(8) .0242(8) .0249(8) .0039(6) .0104(6) .0019(6) C101 .0234(12) .0255(13) .0363(14) .0057(10) .0147(11) .0050(10) C102 .0220(11) .0267(12) .0298(12) .0009(9) .0090(10) -.0010(10) O102 .0250(8) .0274(9) .0329(9) .0045(7) .0130(7) .0061(7) N10 .0276(11) .0304(11) .0507(14) .0075(9) .0224(10) .0059(10) C1011 .0466(18) .0425(18) .074(2) .0113(15) .0438(18) .0124(16) C1012 .049(2) .050(2) .139(5) -.0075(19) .053(3) -.002(3) C1021 .0351(17) .0389(17) .085(3) .0176(14) .0346(17) .0168(16) C1022 .051(2) .0335(18) .129(4) .0057(16) .049(2) -.004(2) C11 .0212(11) .0222(11) .0240(11) .0036(9) .0088(9) .0028(9) C12 .0204(11) .0204(11) .0253(11) .0024(9) .0063(9) .0018(9) C13 .0239(12) .0250(12) .0273(12) -.0002(10) .0080(10) .0052(10) C14 .0269(12) .0243(12) .0254(12) .0007(10) .0055(10) .0030(9) C141 .0380(14) .0330(14) .0236(12) -.0057(11) .0077(11) -.0016(10) C142 .0476(18) .0474(18) .0281(15) -.0134(14) .0171(13) -.0078(13) C143 .067(2) .0416(18) .0424(18) -.0128(17) .0263(17) -.0119(14) C144 .048(2) .067(2) .0283(16) -.0005(17) .0050(14) .0107(15) C15 .0269(12) .0241(12) .0264(12) -.0010(10) .0010(10) .0002(10) C16 .0193(11) .0233(11) .0284(12) .0018(9) .0047(9) .0045(9) C1 .0188(11) .0261(12) .0301(13) -.0011(9) .0037(10) .0022(10) O21 .0195(8) .0266(8) .0226(8) .0003(6) .0080(6) -.0018(6) C201 .0266(12) .0291(13) .0271(13) -.0019(11) .0072(10) -.0031(10) C202 .0381(15) .0403(15) .0296(13) -.0104(12) .0152(11) -.0062(11) O202 .0423(11) .0648(14) .0391(11) -.0269(10) .0248(9) -.0237(10) N20 .0580(17) .075(2) .0416(14) -.0335(15) .0315(13) -.0301(13) C2011 .123(5) .190(6) .094(4) -.101(5) .090(4) -.103(4) C2012 .132(6) .184(7) .249(9) -.084(5) .150(7) -.148(7) C2021 .059(2) .070(2) .053(2) -.026(2) .0198(19) -.0263(19) C2022 .076(3) .074(3) .081(3) -.016(2) .005(3) -.032(2) C21 .0182(10) .0254(11) .0247(11) -.0027(9) .0085(9) -.0025(9) C22 .0210(11) .0258(12) .0236(11) -.0032(9) .0032(9) -.0034(9) C23 .0176(11) .0280(12) .0281(12) .0021(10) .0036(9) -.0015(10) C24 .0202(11) .0305(13) .0255(12) -.0030(10) .0067(9) -.0033(10) C241 .0219(12) .0408(14) .0298(13) .0005(11) .0110(10) .0007(11) C242 .044(2) .119(4) .044(2) .028(2) .0266(17) .026(2) C243 .0414(17) .053(2) .0469(19) .0045(15) .0244(15) -.0051(16) C244 .0404(18) .056(2) .072(3) -.0170(16) .0324(18) -.0156(19) C25 .0230(12) .0259(12) .0257(12) -.0016(9) .0062(10) .0025(10) C26 .0200(11) .0227(11) .0241(11) -.0009(9) .0040(9) -.0027(9) C2 .0214(11) .0218(12) .0249(12) .0007(9) .0070(9) .0007(9) O31 .0230(8) .0286(9) .0242(8) .0037(7) .0097(7) .0045(7) C301 .0271(13) .0426(16) .0249(13) .0035(12) .0087(10) .0109(11) C302 .0292(13) .0362(14) .0277(13) .0038(11) .0121(10) .0072(11) O302 .0279(9) .0416(10) .0355(10) .0090(8) .0162(8) .0139(8) N30 .0369(12) .0494(14) .0389(13) .0132(11) .0220(10) .0207(11) C3011 .064(2) .092(3) .055(2) .038(2) .038(2) .046(2) C3012 .156(6) .071(3) .104(4) .062(3) .092(4) .047(3) C3021 .0385(16) .056(2) .052(2) .0093(14) .0290(15) .0203(16) C3022 .059(3) .103(4) .089(4) .013(3) .039(3) -.021(3) C31 .0206(11) .0247(11) .0249(12) .0049(9) .0085(9) .0050(9) C32 .0198(11) .0224(11) .0287(12) -.0007(9) .0051(9) .0065(9) C33 .0218(11) .0237(12) .0306(13) .0016(9) .0039(10) .0011(10) C34 .0201(11) .0258(12) .0279(12) .0028(9) .0071(9) .0033(9) C341 .0217(11) .0315(13) .0349(13) -.0007(10) .0103(10) -.0051(10) C342 .0322(14) .0329(14) .0413(16) .0063(12) .0102(13) -.0032(12) C343 .0265(14) .050(2) .065(2) -.0032(13) .0193(15) -.0226(17) C344 .0481(18) .0410(17) .0356(15) -.0014(14) .0177(14) -.0044(13) C35 .0166(11) .0286(12) .0289(12) .0007(9) .0062(9) .0028(10) C36 .0204(11) .0255(12) .0214(11) .0020(9) .0034(9) .0038(9) C3 .0195(11) .0287(13) .0243(12) .0016(9) .0049(10) .0005(9) O41 .0225(8) .0235(8) .0280(9) .0011(6) .0038(7) -.0001(7) C41 .0170(10) .0248(12) .0258(12) -.0029(9) .0080(9) -.0003(9) C42 .0181(10) .0267(12) .0292(12) -.0028(9) .0091(9) .0026(9) C43 .0228(11) .0309(13) .0280(12) -.0041(10) .0063(10) .0026(10) C44 .0243(12) .0303(13) .0339(13) -.0064(10) .0128(10) -.0030(10) C441 .0430(16) .0338(14) .0374(15) -.0072(12) .0098(12) -.0075(12) C442 .060(2) .060(2) .047(2) .0106(19) .0122(17) -.0159(18) C443 .093(3) .044(2) .049(2) -.031(2) .003(2) -.0060(17) C444 .0461(18) .052(2) .0406(17) -.0095(15) .0059(14) -.0141(15) C45 .0238(12) .0226(12) .0380(14) -.0008(10) .0141(10) -.0016(10) C46 .0161(10) .0243(11) .0304(12) -.0003(9) .0104(9) .0028(9) C4 .0180(11) .0227(12) .0348(14) -.0001(9) .0086(10) .0050(10) Fe2 .02513(18) .02833(19) .0345(2) .00132(15) .00565(15) -.00261(15) Cl21 .0272(3) .0363(4) .0664(5) .0049(3) .0049(3) -.0066(3) Cl22 .0411(4) .0404(4) .0588(5) -.0074(3) .0217(3) -.0048(3) Cl23 .0427(4) .0362(4) .0433(4) .0048(3) -.0008(3) -.0096(3) Cl24 .0427(4) .0491(4) .0327(3) .0069(3) .0063(3) -.0021(3) Fe3 .0419(2) .0565(3) .0408(2) -.0051(2) .00837(19) .0058(2) Cl31 .0519(10) .0424(9) .0484(9) -.0118(8) .0026(8) .0072(7) Cl32 .0504(10) .0828(14) .0521(10) -.0248(10) -.0088(8) -.0036(10) Cl33 .0924(16) .0796(14) .0441(10) .0044(12) .0333(10) .0237(9) Cl34 .0573(14) .0537(12) .065(2) -.0018(10) .0032(15) -.0193(12) Cl31' .198(4) .091(2) .236(5) .083(3) .171(4) .105(3) Cl32' .0813(19) .144(3) .178(3) .019(2) -.059(2) -.081(3) Cl33' .110(2) .0801(16) .109(2) -.0066(14) .0653(18) .0251(15) Cl34' .0464(14) .157(4) .091(3) -.006(2) .014(2) -.050(3) O01 .088(5) .095(5) .165(7) -.002(4) .012(5) .056(5) O02 .185(9) .142(8) .159(8) .067(7) -.006(7) -.003(7) # 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 Fe1 O11 . . 2.2999(15) ? Fe1 O102 . . 2.0639(17) ? Fe1 O21 . . 2.4955(16) ? Fe1 O202 . . 1.999(2) ? Fe1 O31 . . 2.3647(16) ? Fe1 O302 . . 2.0451(19) ? Fe1 O41 . . 1.7921(16) ? O11 C101 . . 1.435(3) ? O11 C11 . . 1.417(3) ? C101 C102 . . 1.513(4) ? C101 H101a . . .97(3) ? C101 H101b . . .98(3) ? C102 O102 . . 1.257(3) ? C102 N10 . . 1.315(3) ? N10 C1011 . . 1.474(4) ? N10 C1021 . . 1.464(4) ? C1011 C1012 . . 1.498(5) ? C1011 H1011a . . .97(3) ? C1011 H1011b . . .99(3) ? C1012 H1012a . . .92(5) ? C1012 H1012b . . .92(5) ? C1012 H1012c . . 1.04(4) ? C1021 C1022 . . 1.503(6) ? C1021 H1021a . . .88(3) ? C1021 H1021b . . .92(4) ? C1022 H1022a . . .95(4) ? C1022 H1022b . . .95(4) ? C1022 H1022c . . 1.00(5) ? C11 C12 . . 1.387(3) ? C11 C16 . . 1.397(3) ? C12 C13 . . 1.397(3) ? C12 C2 . . 1.516(3) ? C13 C14 . . 1.385(3) ? C13 H13 . . .96(3) ? C14 C141 . . 1.532(4) ? C14 C15 . . 1.396(4) ? C141 C142 . . 1.535(4) ? C141 C143 . . 1.529(4) ? C141 C144 . . 1.537(4) ? C142 H142a . . .93(3) ? C142 H142b . . 1.05(3) ? C142 H142c . . .94(3) ? C143 H143a . . 1.02(4) ? C143 H143b . . .92(4) ? C143 H143c . . 1.03(3) ? C144 H144a . . .94(4) ? C144 H144b . . 1.04(3) ? C144 H144c . . .97(3) ? C15 C16 . . 1.389(4) ? C15 H15 . . .91(2) ? C16 C1 . . 1.516(3) ? C1 C42 . . 1.510(3) ? C1 H1a . . .97(2) ? C1 H1b . . .96(3) ? O21 C201 . . 1.440(3) ? O21 C21 . . 1.423(3) ? C201 C202 . . 1.490(4) ? C201 H201a . . .94(3) ? C201 H201b . . .90(3) ? C202 O202 . . 1.264(3) ? C202 N20 . . 1.316(4) ? N20 C2011 . . 1.473(7) ? N20 C2021 . . 1.480(5) ? C2011 C2012 . . 1.386(9) ? C2011 H2011a . . 1.04(3) ? C2011 H2011b . . .93(4) ? C2012 H2012a . . 1.03(5) ? C2012 H2012b . . 1.02(5) ? C2012 H2012c . . .99(4) ? C2021 C2022 . . 1.501(6) ? C2021 H2021a . . .89(5) ? C2021 H2021b . . .99(4) ? C2022 H2022a . . 1.08(5) ? C2022 H2022b . . 1.24(6) ? C2022 H2022c . . 1.05(7) ? C21 C22 . . 1.398(3) ? C21 C26 . . 1.386(3) ? C22 C23 . . 1.397(4) ? C22 C3 . . 1.515(3) ? C23 C24 . . 1.391(3) ? C23 H23 . . .88(2) ? C24 C241 . . 1.539(4) ? C24 C25 . . 1.393(3) ? C241 C242 . . 1.521(5) ? C241 C243 . . 1.528(4) ? C241 C244 . . 1.525(4) ? C242 H242a . . .93(4) ? C242 H242b . . 1.04(4) ? C242 H242c . . .93(4) ? C243 H243a . . 1.01(3) ? C243 H243b . . .88(4) ? C243 H243c . . .92(3) ? C244 H244a . . .98(4) ? C244 H244b . . .96(3) ? C244 H244c . . .99(4) ? C25 C26 . . 1.392(4) ? C25 H25 . . .87(3) ? C26 C2 . . 1.514(3) ? C2 H2a . . .98(3) ? C2 H2b . . .99(2) ? O31 C301 . . 1.442(3) ? O31 C31 . . 1.421(3) ? C301 C302 . . 1.518(4) ? C301 H301a . . .95(3) ? C301 H301b . . 1.01(3) ? C302 O302 . . 1.247(3) ? C302 N30 . . 1.323(4) ? N30 C3011 . . 1.474(5) ? N30 C3021 . . 1.479(4) ? C3011 C3012 . . 1.498(7) ? C3011 H3011a . . 1.05(3) ? C3011 H3011b . . .92(4) ? C3012 H3012a . . .91(5) ? C3012 H3012b . . 1.03(5) ? C3012 H3012c . . .96(5) ? C3021 C3022 . . 1.479(7) ? C3021 H3021a . . 1.02(3) ? C3021 H3021b . . .94(3) ? C3022 H3022a . . 1.00(4) ? C3022 H3022b . . .97(5) ? C3022 H3022c . . .98(4) ? C31 C32 . . 1.396(3) ? C31 C36 . . 1.390(3) ? C32 C33 . . 1.391(4) ? C32 C4 . . 1.515(3) ? C33 C34 . . 1.396(3) ? C33 H33 . . .93(2) ? C34 C341 . . 1.529(4) ? C34 C35 . . 1.389(3) ? C341 C342 . . 1.532(4) ? C341 C343 . . 1.533(4) ? C341 C344 . . 1.527(4) ? C342 H342a . . 1.00(3) ? C342 H342b . . 1.01(3) ? C342 H342c . . .94(3) ? C343 H343a . . 1.00(4) ? C343 H343b . . .99(3) ? C343 H343c . . .95(3) ? C344 H344a . . .96(3) ? C344 H344b . . .99(3) ? C344 H344c . . 1.01(3) ? C35 C36 . . 1.393(3) ? C35 H35 . . .93(2) ? C36 C3 . . 1.517(3) ? C3 H3a . . .93(3) ? C3 H3b . . 1.00(2) ? O41 C41 . . 1.335(3) ? C41 C42 . . 1.401(3) ? C41 C46 . . 1.405(3) ? C42 C43 . . 1.391(3) ? C43 C44 . . 1.399(3) ? C43 H43 . . .95(2) ? C44 C441 . . 1.539(4) ? C44 C45 . . 1.400(3) ? C441 C442 . . 1.544(5) ? C441 C443 . . 1.525(5) ? C441 C444 . . 1.523(4) ? C442 H442a . . 1.02(4) ? C442 H442b . . .98(4) ? C442 H442c . . 1.02(4) ? C443 H443a . . 1.01(4) ? C443 H443b . . 1.04(5) ? C443 H443c . . .98(3) ? C444 H444a . . .98(3) ? C444 H444b . . 1.00(4) ? C444 H444c . . 1.02(3) ? C45 C46 . . 1.383(3) ? C45 H45 . . .95(3) ? C46 C4 . . 1.509(3) ? C4 H4a . . 1.00(3) ? C4 H4b . . .91(3) ? Fe2 Cl21 . . 2.1912(8) ? Fe2 Cl22 . . 2.2105(9) ? Fe2 Cl23 . . 2.1759(8) ? Fe2 Cl24 . . 2.1942(8) ? Fe3 Cl31 . . 2.248(2) ? Fe3 Cl32 . . 2.224(2) ? Fe3 Cl33 . . 2.157(2) ? Fe3 Cl34 . . 2.110(4) ? Fe3 Cl31' . . 2.065(4) ? Fe3 Cl32' . . 2.155(3) ? Fe3 Cl33' . . 2.225(3) ? Fe3 Cl34' . . 2.220(5) ? 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 Fe1 O102 . . . 71.06(6) ? O11 Fe1 O21 . . . 74.79(5) ? O11 Fe1 O202 . . . 92.40(7) ? O11 Fe1 O31 . . . 138.91(6) ? O11 Fe1 O302 . . . 150.57(6) ? O11 Fe1 O41 . . . 84.09(6) ? O102 Fe1 O21 . . . 133.49(6) ? O102 Fe1 O202 . . . 82.82(7) ? O102 Fe1 O31 . . . 149.21(6) ? O102 Fe1 O302 . . . 79.51(7) ? O102 Fe1 O41 . . . 98.03(7) ? O21 Fe1 O202 . . . 67.93(7) ? O21 Fe1 O31 . . . 73.60(5) ? O21 Fe1 O302 . . . 129.34(6) ? O21 Fe1 O41 . . . 108.93(7) ? O202 Fe1 O31 . . . 99.33(7) ? O202 Fe1 O302 . . . 84.19(8) ? O202 Fe1 O41 . . . 175.88(8) ? O31 Fe1 O302 . . . 70.24(6) ? O31 Fe1 O41 . . . 82.02(6) ? O302 Fe1 O41 . . . 99.93(7) ? Fe1 O11 C101 . . . 114.69(14) ? Fe1 O11 C11 . . . 125.41(13) ? C101 O11 C11 . . . 113.65(17) ? O11 C101 C102 . . . 106.7(2) ? O11 C101 H101a . . . 109.2(18) ? O11 C101 H101b . . . 113.5(17) ? C102 C101 H101a . . . 110.4(18) ? C102 C101 H101b . . . 109.6(18) ? H101a C101 H101b . . . 107(2) ? C101 C102 O102 . . . 118.7(2) ? C101 C102 N10 . . . 119.8(2) ? O102 C102 N10 . . . 121.5(2) ? Fe1 O102 C102 . . . 122.77(16) ? C102 N10 C1011 . . . 119.4(2) ? C102 N10 C1021 . . . 123.9(3) ? C1011 N10 C1021 . . . 116.7(3) ? N10 C1011 C1012 . . . 111.6(3) ? N10 C1011 H1011a . . . 105(2) ? N10 C1011 H1011b . . . 105(2) ? C1012 C1011 H1011a . . . 114(2) ? C1012 C1011 H1011b . . . 113(2) ? H1011a C1011 H1011b . . . 107(3) ? C1011 C1012 H1012a . . . 108(3) ? C1011 C1012 H1012b . . . 111(3) ? C1011 C1012 H1012c . . . 117(2) ? H1012a C1012 H1012b . . . 109(4) ? H1012a C1012 H1012c . . . 107(4) ? H1012b C1012 H1012c . . . 105(3) ? N10 C1021 C1022 . . . 113.0(3) ? N10 C1021 H1021a . . . 106.3(19) ? N10 C1021 H1021b . . . 109(2) ? C1022 C1021 H1021a . . . 111(2) ? C1022 C1021 H1021b . . . 113(2) ? H1021a C1021 H1021b . . . 106(3) ? C1021 C1022 H1022a . . . 117(2) ? C1021 C1022 H1022b . . . 105(2) ? C1021 C1022 H1022c . . . 114(2) ? H1022a C1022 H1022b . . . 106(3) ? H1022a C1022 H1022c . . . 108(3) ? H1022b C1022 H1022c . . . 106(3) ? O11 C11 C12 . . . 117.99(18) ? O11 C11 C16 . . . 119.9(2) ? C12 C11 C16 . . . 122.1(2) ? C11 C12 C13 . . . 117.9(2) ? C11 C12 C2 . . . 122.5(2) ? C13 C12 C2 . . . 119.4(2) ? C12 C13 C14 . . . 122.5(2) ? C12 C13 H13 . . . 116.2(15) ? C14 C13 H13 . . . 121.3(15) ? C13 C14 C141 . . . 122.8(2) ? C13 C14 C15 . . . 117.2(2) ? C141 C14 C15 . . . 120.0(2) ? C14 C141 C142 . . . 112.2(2) ? C14 C141 C143 . . . 109.3(2) ? C14 C141 C144 . . . 109.0(2) ? C142 C141 C143 . . . 107.8(3) ? C142 C141 C144 . . . 108.7(2) ? C143 C141 C144 . . . 109.9(2) ? C141 C142 H142a . . . 109.7(18) ? C141 C142 H142b . . . 113(2) ? C141 C142 H142c . . . 113.2(19) ? H142a C142 H142b . . . 107(3) ? H142a C142 H142c . . . 109(3) ? H142b C142 H142c . . . 106(2) ? C141 C143 H143a . . . 109.8(18) ? C141 C143 H143b . . . 109(2) ? C141 C143 H143c . . . 110.8(19) ? H143a C143 H143b . . . 106(3) ? H143a C143 H143c . . . 110(3) ? H143b C143 H143c . . . 112(3) ? C141 C144 H144a . . . 107.6(19) ? C141 C144 H144b . . . 112.0(16) ? C141 C144 H144c . . . 112.9(18) ? H144a C144 H144b . . . 113(3) ? H144a C144 H144c . . . 108(3) ? H144b C144 H144c . . . 104(3) ? C14 C15 C16 . . . 122.9(2) ? C14 C15 H15 . . . 120.8(17) ? C16 C15 H15 . . . 116.3(17) ? C11 C16 C15 . . . 117.4(2) ? C11 C16 C1 . . . 124.2(2) ? C15 C16 C1 . . . 118.3(2) ? C16 C1 C42 . . . 111.3(2) ? C16 C1 H1a . . . 109.5(15) ? C16 C1 H1b . . . 111.5(15) ? C42 C1 H1a . . . 110.6(13) ? C42 C1 H1b . . . 108.9(14) ? H1a C1 H1b . . . 105(2) ? Fe1 O21 C201 . . . 113.00(14) ? Fe1 O21 C21 . . . 138.59(12) ? C201 O21 C21 . . . 108.40(17) ? O21 C201 C202 . . . 107.6(2) ? O21 C201 H201a . . . 108.4(16) ? O21 C201 H201b . . . 110.2(17) ? C202 C201 H201a . . . 108.9(18) ? C202 C201 H201b . . . 108(2) ? H201a C201 H201b . . . 113(2) ? C201 C202 O202 . . . 118.6(2) ? C201 C202 N20 . . . 120.4(2) ? O202 C202 N20 . . . 121.0(3) ? Fe1 O202 C202 . . . 132.4(2) ? C202 N20 C2011 . . . 118.3(3) ? C202 N20 C2021 . . . 123.3(3) ? C2011 N20 C2021 . . . 117.9(3) ? N20 C2011 C2012 . . . 116.9(5) ? N20 C2011 H2011a . . . 112.4(13) ? N20 C2011 H2011b . . . 109(2) ? C2012 C2011 H2011a . . . 108.1(15) ? C2012 C2011 H2011b . . . 102(2) ? H2011a C2011 H2011b . . . 108(2) ? C2011 C2012 H2012a . . . 109(3) ? C2011 C2012 H2012b . . . 109(3) ? C2011 C2012 H2012c . . . 107.4(16) ? H2012a C2012 H2012b . . . 106(4) ? H2012a C2012 H2012c . . . 112(5) ? H2012b C2012 H2012c . . . 113(4) ? N20 C2021 C2022 . . . 112.6(3) ? N20 C2021 H2021a . . . 109(3) ? N20 C2021 H2021b . . . 120(2) ? C2022 C2021 H2021a . . . 103(3) ? C2022 C2021 H2021b . . . 92(2) ? H2021a C2021 H2021b . . . 118(4) ? C2021 C2022 H2022a . . . 104(3) ? C2021 C2022 H2022b . . . 109(2) ? C2021 C2022 H2022c . . . 96(4) ? H2022a C2022 H2022b . . . 112(4) ? H2022a C2022 H2022c . . . 122(5) ? H2022b C2022 H2022c . . . 112(5) ? O21 C21 C22 . . . 118.8(2) ? O21 C21 C26 . . . 119.2(2) ? C22 C21 C26 . . . 122.0(2) ? C21 C22 C23 . . . 117.5(2) ? C21 C22 C3 . . . 121.9(2) ? C23 C22 C3 . . . 120.5(2) ? C22 C23 C24 . . . 122.8(2) ? C22 C23 H23 . . . 115.1(17) ? C24 C23 H23 . . . 122.1(17) ? C23 C24 C241 . . . 122.0(2) ? C23 C24 C25 . . . 117.0(2) ? C241 C24 C25 . . . 121.0(2) ? C24 C241 C242 . . . 111.2(2) ? C24 C241 C243 . . . 110.8(2) ? C24 C241 C244 . . . 108.5(2) ? C242 C241 C243 . . . 107.5(3) ? C242 C241 C244 . . . 109.3(3) ? C243 C241 C244 . . . 109.5(2) ? C241 C242 H242a . . . 107(2) ? C241 C242 H242b . . . 112(2) ? C241 C242 H242c . . . 107(3) ? H242a C242 H242b . . . 109(3) ? H242a C242 H242c . . . 112(4) ? H242b C242 H242c . . . 110(3) ? C241 C243 H243a . . . 110.7(17) ? C241 C243 H243b . . . 110(2) ? C241 C243 H243c . . . 111(2) ? H243a C243 H243b . . . 108(3) ? H243a C243 H243c . . . 110(3) ? H243b C243 H243c . . . 108(3) ? C241 C244 H244a . . . 111.9(18) ? C241 C244 H244b . . . 110.4(19) ? C241 C244 H244c . . . 110(2) ? H244a C244 H244b . . . 108(3) ? H244a C244 H244c . . . 105(3) ? H244b C244 H244c . . . 112(3) ? C24 C25 C26 . . . 122.7(2) ? C24 C25 H25 . . . 121(2) ? C26 C25 H25 . . . 116(2) ? C21 C26 C25 . . . 118.0(2) ? C21 C26 C2 . . . 122.1(2) ? C25 C26 C2 . . . 119.7(2) ? C12 C2 C26 . . . 108.61(19) ? C12 C2 H2a . . . 113.1(13) ? C12 C2 H2b . . . 112.9(12) ? C26 C2 H2a . . . 108.6(13) ? C26 C2 H2b . . . 107.7(13) ? H2a C2 H2b . . . 106(2) ? Fe1 O31 C301 . . . 114.94(14) ? Fe1 O31 C31 . . . 125.55(12) ? C301 O31 C31 . . . 112.74(18) ? O31 C301 C302 . . . 106.3(2) ? O31 C301 H301a . . . 109.0(18) ? O31 C301 H301b . . . 112.1(16) ? C302 C301 H301a . . . 110(2) ? C302 C301 H301b . . . 109.5(16) ? H301a C301 H301b . . . 110(2) ? C301 C302 O302 . . . 119.2(2) ? C301 C302 N30 . . . 119.7(2) ? O302 C302 N30 . . . 121.2(2) ? Fe1 O302 C302 . . . 127.45(17) ? C302 N30 C3011 . . . 123.7(3) ? C302 N30 C3021 . . . 119.7(2) ? C3011 N30 C3021 . . . 116.5(3) ? N30 C3011 C3012 . . . 112.6(3) ? N30 C3011 H3011a . . . 104.6(16) ? N30 C3011 H3011b . . . 106(2) ? C3012 C3011 H3011a . . . 114.4(17) ? C3012 C3011 H3011b . . . 116(2) ? H3011a C3011 H3011b . . . 102(3) ? C3011 C3012 H3012a . . . 106(3) ? C3011 C3012 H3012b . . . 109(3) ? C3011 C3012 H3012c . . . 107(3) ? H3012a C3012 H3012b . . . 113(4) ? H3012a C3012 H3012c . . . 108(4) ? H3012b C3012 H3012c . . . 114(4) ? N30 C3021 C3022 . . . 112.5(3) ? N30 C3021 H3021a . . . 105.3(18) ? N30 C3021 H3021b . . . 107(2) ? C3022 C3021 H3021a . . . 109.6(18) ? C3022 C3021 H3021b . . . 111(2) ? H3021a C3021 H3021b . . . 111(3) ? C3021 C3022 H3022a . . . 110(2) ? C3021 C3022 H3022b . . . 114(3) ? C3021 C3022 H3022c . . . 113(3) ? H3022a C3022 H3022b . . . 113(4) ? H3022a C3022 H3022c . . . 111(4) ? H3022b C3022 H3022c . . . 97(4) ? O31 C31 C32 . . . 119.7(2) ? O31 C31 C36 . . . 118.35(19) ? C32 C31 C36 . . . 122.0(2) ? C31 C32 C33 . . . 117.5(2) ? C31 C32 C4 . . . 124.5(2) ? C33 C32 C4 . . . 118.0(2) ? C32 C33 C34 . . . 122.7(2) ? C32 C33 H33 . . . 116.0(17) ? C34 C33 H33 . . . 121.2(17) ? C33 C34 C341 . . . 119.9(2) ? C33 C34 C35 . . . 117.2(2) ? C341 C34 C35 . . . 122.9(2) ? C34 C341 C342 . . . 110.5(2) ? C34 C341 C343 . . . 112.0(2) ? C34 C341 C344 . . . 107.7(2) ? C342 C341 C343 . . . 107.8(2) ? C342 C341 C344 . . . 110.2(2) ? C343 C341 C344 . . . 108.7(3) ? C341 C342 H342a . . . 108.1(18) ? C341 C342 H342b . . . 111.6(16) ? C341 C342 H342c . . . 110(2) ? H342a C342 H342b . . . 110(2) ? H342a C342 H342c . . . 108(3) ? H342b C342 H342c . . . 109(3) ? C341 C343 H343a . . . 106(2) ? C341 C343 H343b . . . 109(2) ? C341 C343 H343c . . . 109.3(17) ? H343a C343 H343b . . . 116(3) ? H343a C343 H343c . . . 103(3) ? H343b C343 H343c . . . 114(2) ? C341 C344 H344a . . . 112.7(16) ? C341 C344 H344b . . . 109.8(17) ? C341 C344 H344c . . . 112.9(17) ? H344a C344 H344b . . . 111(3) ? H344a C344 H344c . . . 107(2) ? H344b C344 H344c . . . 103(2) ? C34 C35 C36 . . . 122.5(2) ? C34 C35 H35 . . . 119.3(14) ? C36 C35 H35 . . . 118.1(14) ? C31 C36 C35 . . . 118.0(2) ? C31 C36 C3 . . . 122.9(2) ? C35 C36 C3 . . . 119.0(2) ? C22 C3 C36 . . . 108.39(18) ? C22 C3 H3a . . . 108.5(16) ? C22 C3 H3b . . . 110.1(15) ? C36 C3 H3a . . . 113.3(16) ? C36 C3 H3b . . . 109.4(14) ? H3a C3 H3b . . . 107(2) ? Fe1 O41 C41 . . . 164.25(16) ? O41 C41 C42 . . . 120.2(2) ? O41 C41 C46 . . . 119.10(18) ? C42 C41 C46 . . . 120.7(2) ? C1 C42 C41 . . . 119.1(2) ? C1 C42 C43 . . . 122.2(2) ? C41 C42 C43 . . . 118.7(2) ? C42 C43 C44 . . . 121.9(2) ? C42 C43 H43 . . . 118.1(15) ? C44 C43 H43 . . . 120.0(15) ? C43 C44 C441 . . . 122.1(2) ? C43 C44 C45 . . . 117.6(2) ? C441 C44 C45 . . . 120.4(2) ? C44 C441 C442 . . . 107.6(2) ? C44 C441 C443 . . . 110.7(2) ? C44 C441 C444 . . . 112.8(2) ? C442 C441 C443 . . . 109.2(3) ? C442 C441 C444 . . . 108.2(3) ? C443 C441 C444 . . . 108.4(3) ? C441 C442 H442a . . . 111(2) ? C441 C442 H442b . . . 106(3) ? C441 C442 H442c . . . 107(2) ? H442a C442 H442b . . . 108(3) ? H442a C442 H442c . . . 110(3) ? H442b C442 H442c . . . 114(3) ? C441 C443 H443a . . . 108(2) ? C441 C443 H443b . . . 108(3) ? C441 C443 H443c . . . 108(2) ? H443a C443 H443b . . . 108(4) ? H443a C443 H443c . . . 106(3) ? H443b C443 H443c . . . 118(3) ? C441 C444 H444a . . . 111(2) ? C441 C444 H444b . . . 111.8(18) ? C441 C444 H444c . . . 108.1(16) ? H444a C444 H444b . . . 105(3) ? H444a C444 H444c . . . 106(3) ? H444b C444 H444c . . . 114(3) ? C44 C45 C46 . . . 122.3(2) ? C44 C45 H45 . . . 120.0(14) ? C46 C45 H45 . . . 117.6(14) ? C41 C46 C45 . . . 118.6(2) ? C41 C46 C4 . . . 119.0(2) ? C45 C46 C4 . . . 122.4(2) ? C32 C4 C46 . . . 113.2(2) ? C32 C4 H4a . . . 110.9(14) ? C32 C4 H4b . . . 110.4(15) ? C46 C4 H4a . . . 108.5(14) ? C46 C4 H4b . . . 107.7(14) ? H4a C4 H4b . . . 106(2) ? Cl21 Fe2 Cl22 . . . 109.51(3) ? Cl21 Fe2 Cl23 . . . 109.70(3) ? Cl21 Fe2 Cl24 . . . 111.19(3) ? Cl22 Fe2 Cl23 . . . 107.90(3) ? Cl22 Fe2 Cl24 . . . 108.09(3) ? Cl23 Fe2 Cl24 . . . 110.38(3) ? Cl31 Fe3 Cl32 . . . 105.55(8) ? Cl31 Fe3 Cl33 . . . 108.93(9) ? Cl31 Fe3 Cl34 . . . 111.63(12) ? Cl32 Fe3 Cl33 . . . 108.05(8) ? Cl32 Fe3 Cl34 . . . 108.72(15) ? Cl33 Fe3 Cl34 . . . 113.58(13) ? Cl31' Fe3 Cl32' . . . 112.53(16) ? Cl31' Fe3 Cl33' . . . 109.50(16) ? Cl31' Fe3 Cl34' . . . 116.18(19) ? Cl32' Fe3 Cl33' . . . 108.37(13) ? Cl32' Fe3 Cl34' . . . 104.84(17) ? Cl33' Fe3 Cl34' . . . 104.90(16) ? 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 3044 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 27 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -34 _reflns_limit_l_max 34 _reflns_number_observed ? _reflns_d_resolution_high .732 _reflns_d_resolution_low 14.234 _diffrn_reflns_av_sigmaI/netI .078 _diffrn_reflns_theta_min 1.43 _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 11 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .072 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.125 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end