Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #=========================================================================== # (Publishing Staff Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof J Harrowfield' _publ_contact_author_address ; Prof J Harrowfield Research Centre for Advanced Minerals University of Western Australia Nedlands WA 6907 AUSTRALIA ; _publ_contact_author_email JMH@CHEM.UWA.EDU.AU _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_section_title ; Chirality in Coordination Polymers: Homo- vs Hetero- chiral Strand Construction ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_address 'Donnelly,Paul S.' ; ? ; 'Harrowfield, J.' ; Research Centre for Advanced Minerals University of Western Australia Nedlands WA 6907 AUSTRALIA ; '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 ; _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_pdgn _database_code_CSD 169054 _audit_creation_method Xtal3.6 _audit_creation_date 00-01-04 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H43 Cl3 Co1 N8 O7.5 Zn1' _chemical_formula_moiety ? _chemical_formula_weight 722.27 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.9590(10) _cell_length_b 14.7310(10) _cell_length_c 17.536(2) _cell_angle_alpha 90.00000 _cell_angle_beta 115.269(2) _cell_angle_gamma 90.00000 _cell_volume 2793.7(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.72 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6800 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.795 _exptl_crystal_description cuboid _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.885 _diffrn_reflns_number 27761 _reflns_number_total 7086 _reflns_Friedel_coverage 0 _reflns_number_gt 5374 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.28 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _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 .045 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_number_reflns 5374 _refine_ls_number_parameters 495 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .03 _refine_diff_density_min -1.511 _refine_diff_density_max 1.843 _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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 176 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 0 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 30 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' Zn ? 0 4 .222 1.431 '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 Zn .73925(4) .28211(3) .59762(3) .02597(19) Uani ? ? 1.00000 ? ? Co .25376(4) .26671(3) .62040(3) .01900(19) Uani ? ? 1.00000 ? ? N0 .5827(3) .1858(2) .5673(2) .0244(13) Uani ? ? 1.00000 ? ? C01 .6402(3) .0954(3) .5892(3) .0312(17) Uani ? ? 1.00000 ? ? C02 .7643(3) .0935(3) .5847(3) .0368(18) Uani ? ? 1.00000 ? ? O1 .8094(2) .16895(17) .57483(17) .0348(12) Uani ? ? 1.00000 ? ? O2 .8158(3) .0193(2) .5909(3) .0614(18) Uani ? ? 1.00000 ? ? C1 .4742(3) .2058(2) .5858(2) .0241(14) Uani ? ? 1.00000 ? ? C2a .3741(3) .1336(3) .5474(2) .0276(16) Uani ? ? 1.00000 ? ? N3a .2542(2) .1606(2) .54945(18) .0238(12) Uani ? ? 1.00000 ? ? C4a .1561(3) .1796(2) .4630(2) .0280(15) Uani ? ? 1.00000 ? ? C4a' .0459(3) .2147(2) .4731(2) .0295(16) Uani ? ? 1.00000 ? ? N3a' .0886(2) .2943(2) .53163(17) .0215(12) Uani ? ? 1.00000 ? ? C2a' -.0090(3) .3245(3) .5576(2) .0320(18) Uani ? ? 1.00000 ? ? C2b .4285(3) .2977(2) .5430(2) .0248(15) Uani ? ? 1.00000 ? ? N3b .3368(2) .34219(19) .56703(18) .0226(12) Uani ? ? 1.00000 ? ? C4b .3915(4) .4221(3) .6243(3) .0303(17) Uani ? ? 1.00000 ? ? C4b' .2904(4) .4564(2) .6461(3) .0281(16) Uani ? ? 1.00000 ? ? N3b' .2490(3) .3789(2) .68173(19) .0245(13) Uani ? ? 1.00000 ? ? C2b' .1335(3) .4020(3) .6914(3) .0326(18) Uani ? ? 1.00000 ? ? C2c .5188(3) .2116(2) .6814(2) .0258(15) Uani ? ? 1.00000 ? ? N3c .4161(3) .2270(2) .70787(18) .0281(14) Uani ? ? 1.00000 ? ? C4c .3911(4) .1450(3) .7491(3) .043(2) Uani ? ? 1.00000 ? ? C4c' .2796(4) .1680(4) .7650(3) .047(2) Uani ? ? 1.00000 ? ? N3c' .1787(3) .1982(2) .6833(2) .0266(13) Uani ? ? 1.00000 ? ? C2c' .0744(3) .2392(3) .6960(3) .0297(17) Uani ? ? 1.00000 ? ? C1' .0320(3) .3303(2) .6520(2) .0236(14) Uani ? ? 1.00000 ? ? N0' -.0829(3) .3590(2) .65940(18) .0243(13) Uani ? ? 1.00000 ? ? C01' -.0702(4) .3810(3) .7445(2) .0325(18) Uani ? ? 1.00000 ? ? C02' -.1949(4) .3844(3) .7470(3) .044(2) Uani ? ? 1.00000 ? ? O1' -.2886(2) .35428(18) .68468(17) .0345(13) Uani ? ? 1.00000 ? ? O2' -.1997(3) .4162(3) .8111(2) .088(3) Uani ? ? 1.00000 ? ? Cl1 .65524(9) .36858(7) .47689(6) .0371(4) Uani ? ? 1.00000 ? ? Cl2 .46728(14) .37016(11) .86269(7) .0758(7) Uani ? ? 1.00000 ? ? Cl3 .11269(8) .42120(6) .39467(6) .0322(4) Uani ? ? 1.00000 ? ? O01 .0520(3) .04537(18) .5938(2) .0455(14) Uani ? ? 1.00000 ? ? O02 .7377(3) .2493(3) .8625(2) .076(2) Uani ? ? 1.00000 ? ? O03 .8430(3) .1669(2) .7648(2) .0627(19) Uani ? ? 1.00000 ? ? O04 .311(2) -.0260(13) .6209(13) .094(6) Uiso ? ? .25000 ? ? O04' .3782(14) -.0242(10) .6656(10) .060(4) Uiso ? ? .25000 ? ? H01A .589(4) .049(3) .554(2) .033(10) Uiso ? ? 1.00000 ? ? H01B .655(3) .082(2) .645(2) .014(8) Uiso ? ? 1.00000 ? ? H0 .554(4) .189(3) .511(3) .031(11) Uiso ? ? 1.00000 ? ? H2aA .401(3) .076(2) .577(2) .016(8) Uiso ? ? 1.00000 ? ? H2aB .361(4) .122(3) .493(3) .031(10) Uiso ? ? 1.00000 ? ? H3a .228(4) .111(3) .568(2) .032(11) Uiso ? ? 1.00000 ? ? H4aA .135(4) .124(3) .431(3) .041(11) Uiso ? ? 1.00000 ? ? H4aB .193(3) .225(2) .439(2) .014(8) Uiso ? ? 1.00000 ? ? H4a'A .009(4) .173(3) .502(3) .037(11) Uiso ? ? 1.00000 ? ? H4a'B -.017(4) .233(3) .423(3) .031(10) Uiso ? ? 1.00000 ? ? H3a' .094(4) .339(3) .499(3) .034(11) Uiso ? ? 1.00000 ? ? H2a'A -.061(4) .283(3) .537(3) .037(12) Uiso ? ? 1.00000 ? ? H2a'B -.031(4) .388(3) .536(3) .040(12) Uiso ? ? 1.00000 ? ? H2bA .389(3) .289(2) .480(2) .019(9) Uiso ? ? 1.00000 ? ? H2bB .498(3) .336(2) .556(2) .023(9) Uiso ? ? 1.00000 ? ? H3b .278(3) .363(2) .519(2) .026(10) Uiso ? ? 1.00000 ? ? H4bA .414(4) .465(3) .593(2) .036(11) Uiso ? ? 1.00000 ? ? H4bB .455(3) .399(2) .675(2) .021(9) Uiso ? ? 1.00000 ? ? H4b'A .226(4) .478(3) .596(2) .028(10) Uiso ? ? 1.00000 ? ? H4b'B .316(3) .506(3) .683(2) .027(10) Uiso ? ? 1.00000 ? ? H2b'A .100(4) .455(3) .661(3) .039(11) Uiso ? ? 1.00000 ? ? H2b'B .158(4) .411(3) .754(3) .038(11) Uiso ? ? 1.00000 ? ? H3b' .315(4) .370(3) .732(3) .039(12) Uiso ? ? 1.00000 ? ? H2cA .575(3) .265(2) .703(2) .025(9) Uiso ? ? 1.00000 ? ? H2cB .563(4) .155(3) .708(2) .035(11) Uiso ? ? 1.00000 ? ? H3c .442(4) .277(3) .745(3) .057(14) Uiso ? ? 1.00000 ? ? H4cA .460(5) .135(3) .803(3) .059(14) Uiso ? ? 1.00000 ? ? H4cB .371(4) .097(3) .710(3) .051(15) Uiso ? ? 1.00000 ? ? H4c'A .293(5) .221(3) .804(3) .060(16) Uiso ? ? 1.00000 ? ? H4c'B .257(4) .117(3) .784(3) .053(14) Uiso ? ? 1.00000 ? ? H3c' .148(4) .151(3) .656(2) .029(11) Uiso ? ? 1.00000 ? ? H2c'A .093(5) .238(3) .752(4) .070(17) Uiso ? ? 1.00000 ? ? H2c'B .006(4) .196(3) .675(3) .039(11) Uiso ? ? 1.00000 ? ? H0' -.114(4) .408(3) .627(3) .036(11) Uiso ? ? 1.00000 ? ? H01'A -.028(3) .436(3) .766(2) .030(10) Uiso ? ? 1.00000 ? ? H01'B -.025(3) .332(3) .780(2) .026(10) Uiso ? ? 1.00000 ? ? H01a .08605 -.00301 .62289 .06700 Uiso ? ? 1.00000 ? ? H01b -.03966 .03599 .57838 .06700 Uiso ? ? 1.00000 ? ? H02a .71377 .21602 .89845 .11300 Uiso ? ? 1.00000 ? ? H02b .78108 .20372 .86060 .11300 Uiso ? ? 1.00000 ? ? H03a .80263 .15824 .79969 .09400 Uiso ? ? 1.00000 ? ? H03b .92739 .13245 .80556 .09400 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 Zn .0196(2) .0272(2) .0309(2) -.00041(16) .01047(17) -.00346(16) Co .0135(2) .0217(2) .0184(2) -.00064(17) .00352(16) .00303(17) N0 .0182(14) .0262(15) .0265(16) .0017(11) .0072(12) -.0012(12) C01 .0208(18) .0279(18) .039(2) .0006(15) .0073(16) -.0027(16) C02 .0194(18) .032(2) .052(2) .0005(15) .0080(17) -.0106(18) O1 .0243(13) .0307(14) .0500(17) -.0024(11) .0162(12) -.0105(12) O2 .0305(16) .0296(15) .123(3) .0035(13) .0316(19) -.0131(17) C1 .0170(16) .0271(17) .0251(17) .0017(13) .0061(13) -.0011(13) C2a .0174(16) .0301(19) .031(2) .0015(14) .0064(14) -.0035(15) N3a .0168(13) .0211(14) .0276(15) -.0008(11) .0039(11) .0021(11) C4a .0242(17) .0248(17) .0233(18) .0027(14) -.0013(14) -.0051(14) C4a' .0220(17) .0266(18) .028(2) -.0001(14) -.0002(15) .0017(15) N3a' .0167(13) .0258(14) .0208(14) .0006(11) .0068(11) .0033(11) C2a' .0189(17) .050(2) .027(2) .0038(17) .0092(15) .0035(18) C2b .0160(16) .0302(18) .028(2) .0012(14) .0085(14) .0015(14) N3b .0163(13) .0254(14) .0231(15) .0011(11) .0055(12) .0027(12) C4b .030(2) .0277(18) .035(2) -.0098(15) .0158(17) -.0047(16) C4b' .032(2) .0208(16) .034(2) -.0083(15) .0172(17) -.0041(15) N3b' .0177(14) .0277(15) .0265(16) -.0029(12) .0078(12) .0016(12) C2b' .0218(18) .031(2) .047(2) -.0027(15) .0165(17) -.0039(17) C2c .0163(15) .0293(18) .0261(18) .0018(14) .0035(13) .0037(14) N3c .0208(14) .0372(17) .0220(15) .0027(13) .0051(12) .0053(13) C4c .023(2) .061(3) .042(3) .013(2) .0111(19) .032(2) C4c' .023(2) .080(4) .034(2) .009(2) .0084(17) .034(2) N3c' .0191(14) .0298(16) .0268(16) .0012(12) .0059(12) .0071(13) C2c' .0249(18) .035(2) .032(2) .0019(16) .0146(15) .0077(16) C1' .0164(15) .0277(17) .0264(17) .0007(13) .0088(13) .0037(14) N0' .0177(14) .0299(15) .0254(15) .0001(12) .0094(12) .0025(12) C01' .030(2) .039(2) .028(2) -.0088(17) .0127(16) -.0060(17) C02' .046(2) .055(3) .040(2) -.028(2) .027(2) -.018(2) O1' .0291(14) .0404(15) .0399(15) -.0094(11) .0205(12) -.0124(12) O2' .068(2) .152(4) .069(2) -.072(3) .053(2) -.072(3) Cl1 .0286(5) .0401(5) .0378(5) .0013(4) .0095(4) .0097(4) Cl2 .0769(9) .0978(10) .0258(5) .0520(8) -.0037(5) -.0132(6) Cl3 .0340(5) .0315(4) .0296(5) .0019(4) .0122(4) .0085(4) O01 .0421(17) .0301(14) .0569(19) .0016(12) .0140(14) .0086(13) O02 .044(2) .147(4) .0367(19) .014(2) .0178(16) .018(2) O03 .053(2) .073(2) .050(2) .0013(18) .0103(17) -.0126(18) # 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 Zn N0 . . 2.225(3) ? Zn O1 . . 1.982(3) ? Zn Cl1 . . 2.3018(11) ? Zn N0' . '1 655' 2.239(3) ? Zn O1' . '1 655' 2.002(3) ? Co N3a . . 2.000(3) ? Co N3a' . . 1.966(2) ? Co N3b . . 1.973(3) ? Co N3b' . . 1.985(3) ? Co N3c . . 1.981(3) ? Co N3c' . . 1.973(4) ? N0 C01 . . 1.473(5) ? N0 C1 . . 1.496(5) ? N0 H0 . . .89(4) ? C01 C02 . . 1.519(6) ? C01 H01A . . .95(4) ? C01 H01B . . .94(4) ? C02 O1 . . 1.279(5) ? C02 O2 . . 1.237(5) ? C1 C2a . . 1.526(5) ? C1 C2b . . 1.531(5) ? C1 C2c . . 1.529(5) ? C2a N3a . . 1.503(5) ? C2a H2aA . . .98(3) ? C2a H2aB . . .92(5) ? N3a C4a . . 1.494(4) ? N3a H3a . . .90(4) ? C4a C4a' . . 1.494(6) ? C4a H4aA . . .96(4) ? C4a H4aB . . .99(4) ? C4a' N3a' . . 1.497(5) ? C4a' H4a'A . . 1.01(5) ? C4a' H4a'B . . .93(3) ? N3a' C2a' . . 1.490(6) ? N3a' H3a' . . .89(4) ? C2a' C1' . . 1.514(5) ? C2a' H2a'A . . .83(4) ? C2a' H2a'B . . 1.00(4) ? C2b N3b . . 1.484(5) ? C2b H2bA . . 1.00(4) ? C2b H2bB . . .95(4) ? N3b C4b . . 1.503(5) ? N3b H3b . . .89(3) ? C4b C4b' . . 1.503(7) ? C4b H4bA . . .95(5) ? C4b H4bB . . .95(3) ? C4b' N3b' . . 1.486(5) ? C4b' H4b'A . . .94(3) ? C4b' H4b'B . . .94(4) ? N3b' C2b' . . 1.500(6) ? N3b' H3b' . . .91(4) ? C2b' C1' . . 1.533(5) ? C2b' H2b'A . . .93(4) ? C2b' H2b'B . . 1.02(5) ? C2c N3c . . 1.504(6) ? C2c H2cA . . .99(4) ? C2c H2cB . . .99(4) ? N3c C4c . . 1.502(6) ? N3c H3c . . .95(5) ? C4c C4c' . . 1.512(8) ? C4c H4cA . . .96(4) ? C4c H4cB . . .95(5) ? C4c' N3c' . . 1.493(5) ? C4c' H4c'A . . 1.00(5) ? C4c' H4c'B . . .91(5) ? N3c' C2c' . . 1.485(6) ? N3c' H3c' . . .84(4) ? C2c' C1' . . 1.522(5) ? C2c' H2c'A . . .91(6) ? C2c' H2c'B . . .98(4) ? C1' N0' . . 1.495(5) ? N0' C01' . . 1.472(6) ? N0' H0' . . .89(4) ? C01' C02' . . 1.511(7) ? C01' H01'A . . .94(4) ? C01' H01'B . . .95(4) ? C02' O1' . . 1.266(4) ? C02' O2' . . 1.240(7) ? O01 H01a . . .870 ? O01 H01b . . 1.020 ? O02 H02a . . .935 ? O02 H02b . . .858 ? O03 H03a . . .936 ? O03 H03b . . 1.082 ? 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 N0 Zn O1 . . . 78.52(11) ? N0 Zn Cl1 . . . 98.07(8) ? N0 Zn N0' . . '1 655' 165.20(11) ? N0 Zn O1' . . '1 655' 97.13(13) ? O1 Zn Cl1 . . . 109.64(9) ? O1 Zn N0' . . '1 655' 97.26(11) ? O1 Zn O1' . . '1 655' 145.39(11) ? Cl1 Zn N0' . . '1 655' 96.70(8) ? Cl1 Zn O1' . . '1 655' 104.96(8) ? N0' Zn O1' '1 655' . '1 655' 78.20(12) ? N3a Co N3a' . . . 86.42(11) ? N3a Co N3b . . . 90.58(13) ? N3a Co N3b' . . . 174.91(13) ? N3a Co N3c . . . 89.36(12) ? N3a Co N3c' . . . 94.05(14) ? N3a' Co N3b . . . 92.70(12) ? N3a' Co N3b' . . . 90.30(12) ? N3a' Co N3c . . . 174.75(13) ? N3a' Co N3c' . . . 90.30(12) ? N3b Co N3b' . . . 85.68(14) ? N3b Co N3c . . . 90.47(13) ? N3b Co N3c' . . . 174.64(12) ? N3b' Co N3c . . . 94.12(12) ? N3b' Co N3c' . . . 89.86(14) ? N3c Co N3c' . . . 86.88(13) ? Zn N0 C01 . . . 105.2(2) ? Zn N0 C1 . . . 122.8(2) ? Zn N0 H0 . . . 97(3) ? C01 N0 C1 . . . 118.2(3) ? C01 N0 H0 . . . 104(3) ? C1 N0 H0 . . . 106(3) ? N0 C01 C02 . . . 111.1(3) ? N0 C01 H01A . . . 113(2) ? N0 C01 H01B . . . 109(2) ? C02 C01 H01A . . . 109(3) ? C02 C01 H01B . . . 107(2) ? H01A C01 H01B . . . 108(3) ? C01 C02 O1 . . . 118.0(3) ? C01 C02 O2 . . . 118.2(4) ? O1 C02 O2 . . . 123.8(4) ? Zn O1 C02 . . . 117.6(3) ? N0 C1 C2a . . . 110.9(3) ? N0 C1 C2b . . . 103.2(3) ? N0 C1 C2c . . . 108.6(2) ? C2a C1 C2b . . . 110.6(2) ? C2a C1 C2c . . . 111.3(3) ? C2b C1 C2c . . . 111.9(3) ? C1 C2a N3a . . . 112.5(3) ? C1 C2a H2aA . . . 110.9(17) ? C1 C2a H2aB . . . 109(3) ? N3a C2a H2aA . . . 108(2) ? N3a C2a H2aB . . . 110(2) ? H2aA C2a H2aB . . . 106(3) ? Co N3a C2a . . . 118.5(2) ? Co N3a C4a . . . 105.9(2) ? Co N3a H3a . . . 108(3) ? C2a N3a C4a . . . 111.7(3) ? C2a N3a H3a . . . 106(3) ? C4a N3a H3a . . . 106(2) ? N3a C4a C4a' . . . 107.2(3) ? N3a C4a H4aA . . . 109(2) ? N3a C4a H4aB . . . 104.9(16) ? C4a' C4a H4aA . . . 110(3) ? C4a' C4a H4aB . . . 113(2) ? H4aA C4a H4aB . . . 113(4) ? C4a C4a' N3a' . . . 107.0(3) ? C4a C4a' H4a'A . . . 116(3) ? C4a C4a' H4a'B . . . 113(3) ? N3a' C4a' H4a'A . . . 104(2) ? N3a' C4a' H4a'B . . . 109(2) ? H4a'A C4a' H4a'B . . . 108(4) ? Co N3a' C4a' . . . 108.3(2) ? Co N3a' C2a' . . . 118.2(2) ? Co N3a' H3a' . . . 110(2) ? C4a' N3a' C2a' . . . 111.2(3) ? C4a' N3a' H3a' . . . 103(3) ? C2a' N3a' H3a' . . . 105(3) ? N3a' C2a' C1' . . . 114.8(3) ? N3a' C2a' H2a'A . . . 100(4) ? N3a' C2a' H2a'B . . . 106(3) ? C1' C2a' H2a'A . . . 111(3) ? C1' C2a' H2a'B . . . 106(3) ? H2a'A C2a' H2a'B . . . 119(3) ? C1 C2b N3b . . . 113.8(3) ? C1 C2b H2bA . . . 108.8(19) ? C1 C2b H2bB . . . 109(2) ? N3b C2b H2bA . . . 108(2) ? N3b C2b H2bB . . . 111(3) ? H2bA C2b H2bB . . . 107(3) ? Co N3b C2b . . . 117.9(2) ? Co N3b C4b . . . 106.8(3) ? Co N3b H3b . . . 107(3) ? C2b N3b C4b . . . 111.8(3) ? C2b N3b H3b . . . 105(3) ? C4b N3b H3b . . . 108(2) ? N3b C4b C4b' . . . 105.4(3) ? N3b C4b H4bA . . . 107(2) ? N3b C4b H4bB . . . 107(2) ? C4b' C4b H4bA . . . 112(3) ? C4b' C4b H4bB . . . 107(3) ? H4bA C4b H4bB . . . 118(3) ? C4b C4b' N3b' . . . 107.3(3) ? C4b C4b' H4b'A . . . 108(3) ? C4b C4b' H4b'B . . . 112(3) ? N3b' C4b' H4b'A . . . 112(3) ? N3b' C4b' H4b'B . . . 113(3) ? H4b'A C4b' H4b'B . . . 105(3) ? Co N3b' C4b' . . . 108.7(3) ? Co N3b' C2b' . . . 119.4(2) ? Co N3b' H3b' . . . 101(3) ? C4b' N3b' C2b' . . . 111.2(3) ? C4b' N3b' H3b' . . . 102(3) ? C2b' N3b' H3b' . . . 113(4) ? N3b' C2b' C1' . . . 112.5(3) ? N3b' C2b' H2b'A . . . 108(3) ? N3b' C2b' H2b'B . . . 107(3) ? C1' C2b' H2b'A . . . 105(2) ? C1' C2b' H2b'B . . . 112(3) ? H2b'A C2b' H2b'B . . . 112(4) ? C1 C2c N3c . . . 113.4(3) ? C1 C2c H2cA . . . 109(2) ? C1 C2c H2cB . . . 110(3) ? N3c C2c H2cA . . . 106(3) ? N3c C2c H2cB . . . 108(3) ? H2cA C2c H2cB . . . 111(3) ? Co N3c C2c . . . 117.7(2) ? Co N3c C4c . . . 106.2(2) ? Co N3c H3c . . . 103(3) ? C2c N3c C4c . . . 112.6(3) ? C2c N3c H3c . . . 105(4) ? C4c N3c H3c . . . 112(3) ? N3c C4c C4c' . . . 106.4(4) ? N3c C4c H4cA . . . 109(3) ? N3c C4c H4cB . . . 107(3) ? C4c' C4c H4cA . . . 108(4) ? C4c' C4c H4cB . . . 110(3) ? H4cA C4c H4cB . . . 116(4) ? C4c C4c' N3c' . . . 107.7(4) ? C4c C4c' H4c'A . . . 114(3) ? C4c C4c' H4c'B . . . 108(3) ? N3c' C4c' H4c'A . . . 105(3) ? N3c' C4c' H4c'B . . . 111(2) ? H4c'A C4c' H4c'B . . . 112(5) ? Co N3c' C4c' . . . 108.3(3) ? Co N3c' C2c' . . . 119.1(2) ? Co N3c' H3c' . . . 107(3) ? C4c' N3c' C2c' . . . 111.4(4) ? C4c' N3c' H3c' . . . 106(2) ? C2c' N3c' H3c' . . . 104(3) ? N3c' C2c' C1' . . . 113.7(4) ? N3c' C2c' H2c'A . . . 109(4) ? N3c' C2c' H2c'B . . . 107(3) ? C1' C2c' H2c'A . . . 116(3) ? C1' C2c' H2c'B . . . 110(2) ? H2c'A C2c' H2c'B . . . 100(4) ? C2a' C1' C2b' . . . 110.8(4) ? C2a' C1' C2c' . . . 112.8(3) ? C2a' C1' N0' . . . 103.3(3) ? C2b' C1' C2c' . . . 110.5(3) ? C2b' C1' N0' . . . 110.3(3) ? C2c' C1' N0' . . . 108.9(3) ? C1' N0' C01' . . . 116.8(3) ? C1' N0' H0' . . . 108(3) ? C1' N0' Zn . . '1 455' 122.2(2) ? C01' N0' H0' . . . 108(3) ? C01' N0' Zn . . '1 455' 105.5(2) ? H0' N0' Zn . . '1 455' 93(2) ? N0' C01' C02' . . . 111.2(3) ? N0' C01' H01'A . . . 114(3) ? N0' C01' H01'B . . . 107(3) ? C02' C01' H01'A . . . 109(3) ? C02' C01' H01'B . . . 107(3) ? H01'A C01' H01'B . . . 109(3) ? C01' C02' O1' . . . 119.0(4) ? C01' C02' O2' . . . 117.8(4) ? O1' C02' O2' . . . 123.3(5) ? C02' O1' Zn . . '1 455' 118.1(3) ? H01a O01 H01b . . . 103.0 ? H02a O02 H02b . . . 88.8 ? H03a O03 H03b . . . 95.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1500 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 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -23 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 10.791 _diffrn_reflns_av_sigmaI/netI .072 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_shift/su_mean .001 #========================================================================== # 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 #===END #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_pd59el _database_code_CSD 169055 _audit_creation_method Xtal3.6 _audit_creation_date 00-01-10 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H53 Cl3 Co2 N8 O12.5' _chemical_formula_moiety ? _chemical_formula_weight 805.89 _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 11.9830(10) _cell_length_b 9.3804(8) _cell_length_c 14.7200(10) _cell_angle_alpha 90.00000 _cell_angle_beta 100.577(2) _cell_angle_gamma 90.00000 _cell_volume 1626.5(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7071 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.335 _exptl_crystal_description needle _exptl_crystal_size_max .15 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _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 .783 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 18154 _reflns_number_total 4119 _reflns_Friedel_coverage 0 _reflns_number_gt 3293 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .022 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _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 .048 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.497 _refine_ls_number_reflns 3293 _refine_ls_number_parameters 256 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .04 _refine_diff_density_min -.895 _refine_diff_density_max .839 _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 36 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 25 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 106 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 6 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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 Co1 .00000 1.00000 1.00000 .0182(2) Uani ? ? 1.00000 ? ? Co2 .50000 1.00000 1.00000 .0208(3) Uani ? ? 1.00000 ? ? N0 .3462(2) .8771(3) .93513(18) .0227(12) Uani ? ? 1.00000 ? ? C01 .3840(3) .7260(4) .9439(2) .0261(15) Uani ? ? 1.00000 ? ? C02 .5080(3) .7150(4) .9312(2) .0262(15) Uani ? ? 1.00000 ? ? O1 .5684(2) .8266(3) .94447(16) .0262(11) Uani ? ? 1.00000 ? ? O2 .5416(2) .5972(3) .9091(2) .0395(14) Uani ? ? 1.00000 ? ? C1 .2321(3) .9091(4) .9564(2) .0211(14) Uani ? ? 1.00000 ? ? C2a .2427(3) .9129(4) 1.0620(2) .0251(15) Uani ? ? 1.00000 ? ? N3a .1365(2) .9577(3) 1.09333(18) .0230(12) Uani ? ? 1.00000 ? ? C4a .0975(6) .8355(8) 1.1551(5) .028(3) Uani ? ? .50000 ? ? C4a' -.0193(6) .8739(8) 1.1713(4) .029(3) Uani ? ? .50000 ? ? N3a' -.0918(2) .8855(3) 1.07149(19) .0238(13) Uani ? ? 1.00000 ? ? C2a' -.2028(3) .9428(4) 1.0877(2) .0280(16) Uani ? ? 1.00000 ? ? C2b .1441(3) .7986(4) .9127(2) .0262(15) Uani ? ? 1.00000 ? ? N3b .0269(2) .8281(3) .92940(18) .0225(12) Uani ? ? 1.00000 ? ? C4b -.0565(6) .8451(9) .8369(5) .032(3) Uani ? ? .50000 ? ? C4b' -.1680(6) .9007(8) .8548(5) .030(3) Uani ? ? .50000 ? ? C4d -.1152(5) .7440(7) 1.0116(4) .023(3) Uani ? ? .50000 ? ? C4d' -.0069(6) .7010(7) .9831(4) .024(3) Uani ? ? .50000 ? ? Cl1 .34743(9) .95034(12) .71037(7) .0403(5) Uani ? ? 1.00000 ? ? Cl2 -.1763(2) .7842(3) .76718(17) .0634(14) Uani ? ? .50000 ? ? O01 .5088(2) .8881(3) 1.12446(16) .0277(11) Uani ? ? 1.00000 ? ? O02 .4122(2) 1.3733(3) .8379(2) .0393(14) Uani ? ? 1.00000 ? ? O03 .0639(6) .7702(9) 1.2237(5) .067(4) Uani ? ? .50000 ? ? O04 .2545(4) .5038(8) 1.1181(4) .128(5) Uani ? ? .90000 ? ? O05 .4128(14) .9964(14) 1.2955(8) .100(9) Uani ? ? .35000 ? ? O06 -.0937(7) .6067(8) 1.0144(5) .015(3) Uani ? ? .25000 ? ? O07 -.0505(10) .5387(13) .9910(8) .011(2) Uiso ? ? .15000 ? ? O08 -.177(3) .599(4) .986(2) .050(8) Uiso ? ? .10000 ? ? H0 .33973 .88894 .86970 .02900 Uiso ? ? 1.00000 ? ? H01A .33669 .66921 .89822 .03400 Uiso ? ? 1.00000 ? ? H01B .37710 .69098 1.00362 .03400 Uiso ? ? 1.00000 ? ? H2aA .30215 .97757 1.08693 .03200 Uiso ? ? 1.00000 ? ? H2aB .26320 .81967 1.08585 .03200 Uiso ? ? 1.00000 ? ? H3aA .15398 1.04148 1.12978 .02900 Uiso ? ? .50000 ? ? H3aB .11673 .88317 1.13156 .02900 Uiso ? ? .50000 ? ? H4aA .14974 .82827 1.21125 .03500 Uiso ? ? .50000 ? ? H4aB .09622 .74703 1.12204 .03500 Uiso ? ? .50000 ? ? H4a'A -.01939 .96197 1.20265 .03500 Uiso ? ? .50000 ? ? H4a'B -.04910 .80114 1.20530 .03500 Uiso ? ? .50000 ? ? H3a'A -.04686 .87025 1.13112 .03600 Uiso ? ? .50000 ? ? H3a'B -.10610 .79602 1.04087 .03600 Uiso ? ? .50000 ? ? H2a'A -.20214 .94767 1.05061 .03200 Uiso ? ? 1.00000 ? ? H2a'B -.26097 .87738 1.05883 .03200 Uiso ? ? 1.00000 ? ? H2bA .16742 .70668 .93718 .03400 Uiso ? ? 1.00000 ? ? H2bB .14227 .79691 .84739 .03400 Uiso ? ? 1.00000 ? ? H3bA -.02128 .83482 .87046 .02900 Uiso ? ? .50000 ? ? H3bB .00450 .74790 .96161 .02900 Uiso ? ? .50000 ? ? H4bA -.06766 .75462 .80714 .03900 Uiso ? ? .50000 ? ? H4bB -.02488 .90937 .79864 .03900 Uiso ? ? .50000 ? ? H4b'A -.19957 .83689 .89297 .07800 Uiso ? ? .50000 ? ? H4b'B -.21844 .91673 .79906 .07800 Uiso ? ? .50000 ? ? H4dA -.14030 .67169 1.04835 .02900 Uiso ? ? .50000 ? ? H4dB -.17277 .76307 .95956 .02900 Uiso ? ? .50000 ? ? H4d'A .05130 .68277 1.03461 .03000 Uiso ? ? .50000 ? ? H4d'B -.01754 .61989 .94390 .03000 Uiso ? ? .50000 ? ? H01a .53282 .80272 1.13646 .04100 Uiso ? ? 1.00000 ? ? H01b .53880 .92720 1.17265 .04100 Uiso ? ? 1.00000 ? ? H02a .38145 1.37369 .88745 .05900 Uiso ? ? 1.00000 ? ? H02b .44696 1.45394 .86276 .05900 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 Co1 .0169(3) .0202(3) .0165(3) -.0021(2) .0005(2) -.0005(2) Co2 .0184(3) .0205(3) .0231(3) -.0013(2) .0026(2) -.0029(3) N0 .0191(13) .0257(14) .0234(13) -.0015(11) .0040(10) -.0047(11) C01 .0223(16) .0221(16) .0343(17) -.0038(13) .0057(13) -.0068(14) C02 .0251(16) .0252(16) .0283(16) -.0005(13) .0052(13) -.0054(14) O1 .0244(12) .0243(12) .0304(12) -.0020(10) .0065(9) -.0046(10) O2 .0303(14) .0284(14) .0627(19) -.0021(11) .0158(13) -.0159(13) C1 .0179(14) .0232(15) .0220(14) -.0020(12) .0033(11) -.0032(12) C2a .0174(15) .0350(19) .0219(15) -.0009(13) .0011(12) -.0008(14) N3a .0208(13) .0282(14) .0190(12) .0028(11) .0014(10) -.0015(11) C4a .025(3) .033(4) .027(3) .000(3) .004(3) .007(3) C4a' .027(3) .039(4) .021(3) .001(3) .004(3) .010(3) N3a' .0182(13) .0253(14) .0269(13) -.0010(11) .0015(10) .0047(11) C2a' .0308(18) .0279(17) .0275(16) .0025(14) .0112(14) .0038(14) C2b .0186(15) .0253(17) .0340(17) -.0008(13) .0023(13) -.0078(14) N3b .0206(13) .0243(14) .0227(13) -.0034(11) .0040(10) -.0035(11) C4b .020(3) .045(4) .028(3) .001(3) -.006(3) -.016(3) C4b' .023(3) .037(4) .028(3) .001(3) -.001(3) -.010(3) C4d .022(3) .021(3) .026(3) -.005(2) .005(2) -.000(3) C4d' .025(3) .021(3) .028(3) -.001(3) .005(3) -.001(3) Cl1 .0415(5) .0454(5) .0324(4) -.0026(4) .0029(4) -.0087(4) Cl2 .0605(15) .0795(19) .0435(12) .0196(14) -.0081(11) -.0209(13) O01 .0299(13) .0237(12) .0274(12) -.0004(10) .0001(10) .0001(10) O02 .0424(16) .0273(14) .0475(16) .0011(12) .0067(13) -.0042(12) O03 .068(5) .091(6) .044(4) .024(4) .018(3) .037(4) O04 .045(3) .222(8) .114(4) .017(4) .008(3) -.089(5) O05 .167(14) .058(7) .063(7) .018(9) -.009(8) -.001(6) O06 .017(4) .012(4) .018(4) -.005(3) .007(3) -.002(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Co1 N3a . . 1.974(2) ? Co1 N3a' . . 1.973(3) ? Co1 N3b . . 1.977(3) ? Co1 N3a . '3 577' 1.974(2) ? Co1 N3a' . '3 577' 1.973(3) ? Co1 N3b . '3 577' 1.977(3) ? Co2 N0 . . 2.234(3) ? Co2 O1 . . 2.057(2) ? Co2 O01 . . 2.097(2) ? Co2 N0 . '3 677' 2.234(3) ? Co2 O1 . '3 677' 2.057(2) ? Co2 O01 . '3 677' 2.097(2) ? N0 C01 . . 1.487(4) ? N0 C1 . . 1.488(4) ? N0 H0 . . .958 ? C01 C02 . . 1.534(5) ? C01 H01A . . .958 ? C01 H01B . . .956 ? C02 O1 . . 1.268(4) ? C02 O2 . . 1.241(5) ? C1 C2a . . 1.537(5) ? C1 C2b . . 1.533(4) ? C1 C2a' . '3 577' 1.547(5) ? C2a N3a . . 1.491(4) ? C2a H2aA . . .956 ? C2a H2aB . . .958 ? N3a C4a . . 1.586(8) ? N3a H3aA . . .953 ? N3a H3aB . . .954 ? N3a C4b' . '3 577' 1.544(8) ? C4a C4a' . . 1.505(10) ? C4a H4aA . . .944 ? C4a H4aB . . .961 ? C4a' N3a' . . 1.567(7) ? C4a' H4a'A . . .946 ? C4a' H4a'B . . .954 ? N3a' C2a' . . 1.494(5) ? N3a' H3a'A . . .953 ? N3a' H3a'B . . .954 ? C2a' H2a'A . . .550 ? C2a' H2a'B . . .966 ? C2b N3b . . 1.495(4) ? C2b H2bA . . .957 ? C2b H2bB . . .958 ? N3b C4b . . 1.543(7) ? N3b C4d' . . 1.526(7) ? N3b H3bA . . .952 ? N3b H3bB . . .954 ? C4b C4b' . . 1.502(10) ? C4b H3bA . . .596 ? C4b H4bA . . .953 ? C4b H4bB . . .949 ? C4b' H4b'A . . .946 ? C4b' H4b'B . . .938 ? C4d C4d' . . 1.491(10) ? C4d H4dA . . .950 ? C4d H4dB . . .949 ? C4d' H4d'A . . .947 ? C4d' H4d'B . . .949 ? O01 H01a . . .859 ? O01 H01b . . .820 ? O02 H02a . . .876 ? O02 H02b . . .907 ? 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 N3a Co1 N3a' . . . 89.50(11) ? N3a Co1 N3b . . . 90.42(11) ? N3a Co1 N3a . . '3 577' 180.0000 ? N3a Co1 N3a' . . '3 577' 90.50(11) ? N3a Co1 N3b . . '3 577' 89.58(11) ? N3a' Co1 N3b . . . 89.85(12) ? N3a' Co1 N3a . . '3 577' 90.50(11) ? N3a' Co1 N3a' . . '3 577' 180.0000 ? N3a' Co1 N3b . . '3 577' 90.15(12) ? N3b Co1 N3a . . '3 577' 89.58(11) ? N3b Co1 N3a' . . '3 577' 90.15(12) ? N3b Co1 N3b . . '3 577' 180.0000 ? N3a Co1 N3a' '3 577' . '3 577' 89.50(11) ? N3a Co1 N3b '3 577' . '3 577' 90.42(11) ? N3a' Co1 N3b '3 577' . '3 577' 89.85(12) ? N0 Co2 O1 . . . 77.29(10) ? N0 Co2 O01 . . . 91.18(9) ? N0 Co2 N0 . . '3 677' 180.0000 ? N0 Co2 O1 . . '3 677' 102.71(10) ? N0 Co2 O01 . . '3 677' 88.82(10) ? O1 Co2 O01 . . . 89.53(10) ? O1 Co2 N0 . . '3 677' 102.71(10) ? O1 Co2 O1 . . '3 677' 180.0000 ? O1 Co2 O01 . . '3 677' 90.47(10) ? O01 Co2 N0 . . '3 677' 88.82(9) ? O01 Co2 O1 . . '3 677' 90.47(10) ? O01 Co2 O01 . . '3 677' 180.0000 ? N0 Co2 O1 '3 677' . '3 677' 77.29(10) ? N0 Co2 O01 '3 677' . '3 677' 91.18(9) ? O1 Co2 O01 '3 677' . '3 677' 89.53(10) ? Co2 N0 C01 . . . 103.93(18) ? Co2 N0 C1 . . . 121.6(2) ? Co2 N0 H0 . . . 106.1(2) ? C01 N0 C1 . . . 116.8(3) ? C01 N0 H0 . . . 99.5(3) ? C1 N0 H0 . . . 106.3 ? N0 C01 C02 . . . 109.9(3) ? N0 C01 H01A . . . 109.8 ? N0 C01 H01B . . . 109.3 ? C02 C01 H01A . . . 109.8 ? C02 C01 H01B . . . 109.7 ? H01A C01 H01B . . . 108.3 ? C01 C02 O1 . . . 117.7(3) ? C01 C02 O2 . . . 117.4(3) ? O1 C02 O2 . . . 124.9(3) ? Co2 O1 C02 . . . 117.1(2) ? N0 C1 C2a . . . 108.0(2) ? N0 C1 C2b . . . 111.3(3) ? N0 C1 C2a' . . '3 577' 103.8(3) ? C2a C1 C2b . . . 111.3(3) ? C2a C1 C2a' . . '3 577' 112.0(3) ? C2b C1 C2a' . . '3 577' 110.2(2) ? C1 C2a N3a . . . 113.7(2) ? C1 C2a H2aA . . . 108.7 ? C1 C2a H2aB . . . 108.5 ? N3a C2a H2aA . . . 108.7 ? N3a C2a H2aB . . . 108.7 ? H2aA C2a H2aB . . . 108.4 ? Co1 N3a C2a . . . 119.1(2) ? Co1 N3a C4a . . . 104.5(3) ? Co1 N3a H3aA . . . 107.1 ? Co1 N3a H3aB . . . 107.1 ? Co1 N3a C4b' . . '3 577' 105.5(3) ? C2a N3a C4a . . . 109.4(3) ? C2a N3a H3aA . . . 107.2 ? C2a N3a H3aB . . . 107.1 ? C2a N3a C4b' . . '3 577' 104.5(3) ? C4a N3a H3aA . . . 109.3 ? C4a N3a C4b' . . '3 577' 114.2(4) ? H3aA N3a H3aB . . . 108.9 ? H3aB N3a C4b' . . '3 577' 113.8(4) ? N3a C4a C4a' . . . 107.4(5) ? N3a C4a H4aA . . . 109.6 ? N3a C4a H4aB . . . 108.2 ? C4a' C4a H4aA . . . 111.4 ? C4a' C4a H4aB . . . 111.0 ? H4aA C4a H4aB . . . 109.1 ? C4a C4a' N3a' . . . 103.8(5) ? C4a C4a' H4a'A . . . 111.8 ? C4a C4a' H4a'B . . . 111.1 ? N3a' C4a' H4a'A . . . 110.3 ? N3a' C4a' H4a'B . . . 110.2 ? H4a'A C4a' H4a'B . . . 109.6 ? H4a'A C4a' H3a'A . . . 117.6 ? Co1 N3a' C4a' . . . 105.7(3) ? Co1 N3a' C2a' . . . 119.3(2) ? Co1 N3a' C4d . . . 102.6(3) ? Co1 N3a' H3a'A . . . 107.3 ? Co1 N3a' H3a'B . . . 107.3 ? C4a' N3a' C2a' . . . 103.4(4) ? C4a' N3a' C4d . . . 118.2(4) ? C4a' N3a' H3a'B . . . 113.7 ? C2a' N3a' C4d . . . 108.5(3) ? C2a' N3a' H3a'A . . . 106.0 ? C2a' N3a' H3a'B . . . 107.7 ? C4d N3a' H3a'A . . . 113.4 ? H3a'A N3a' H3a'B . . . 109.0 ? N3a' C2a' H2a'A . . . 72.3 ? N3a' C2a' H2a'B . . . 107.0 ? N3a' C2a' C1 . . '3 577' 113.3(3) ? H2a'A C2a' H2a'B . . . 75.9 ? H2a'B C2a' C1 . . '3 577' 107.2 ? C1 C2b N3b . . . 113.6(3) ? C1 C2b H2bA . . . 108.7 ? C1 C2b H2bB . . . 108.6 ? N3b C2b H2bA . . . 108.9 ? N3b C2b H2bB . . . 108.6 ? H2bA C2b H2bB . . . 108.3 ? Co1 N3b C2b . . . 119.1(2) ? Co1 N3b C4b . . . 103.8(3) ? Co1 N3b C4d' . . . 106.3(3) ? Co1 N3b H3bA . . . 107.1 ? Co1 N3b H3bB . . . 107.1 ? C2b N3b C4b . . . 110.5(4) ? C2b N3b C4d' . . . 106.7(3) ? C2b N3b H3bA . . . 107.1 ? C2b N3b H3bB . . . 107.1 ? C4b N3b C4d' . . . 110.3(4) ? C4b N3b H3bB . . . 108.9 ? C4d' N3b H3bA . . . 110.4 ? H3bA N3b H3bB . . . 109.0 ? N3b C4b C4b' . . . 109.5(5) ? N3b C4b H4bA . . . 109.1 ? N3b C4b H4bB . . . 109.0 ? C4b' C4b H4bA . . . 109.5 ? C4b' C4b H4bB . . . 110.4 ? H3bA C4b H4bA . . . 104.8 ? H3bA C4b H4bB . . . 107.3 ? H4bA C4b H4bB . . . 109.3 ? C4b C4b' H4b'A . . . 110.6 ? C4b C4b' H4b'B . . . 110.7 ? C4b C4b' N3a . . '3 577' 103.9(5) ? C4b C4b' H3aA . . '3 577' 100.6 ? H4b'A C4b' H4b'B . . . 110.9 ? H4b'A C4b' N3a . . '3 577' 109.8 ? H4b'A C4b' H3aA . . '3 577' 117.5 ? H4b'B C4b' N3a . . '3 577' 110.7 ? H4b'B C4b' H3aA . . '3 577' 106.0 ? N3a' C4d C4d' . . . 107.9(5) ? N3a' C4d H4dA . . . 108.8 ? N3a' C4d H4dB . . . 108.5 ? C4d' C4d H3a'B . . . 110.0 ? C4d' C4d H4dA . . . 110.5 ? C4d' C4d H4dB . . . 111.4 ? H3a'B C4d H4dA . . . 101.1 ? H3a'B C4d H4dB . . . 113.8 ? H4dA C4d H4dB . . . 109.6 ? N3b C4d' C4d . . . 105.2(5) ? N3b C4d' H4d'A . . . 109.2 ? N3b C4d' H4d'B . . . 109.2 ? C4d C4d' H3bB . . . 104.9 ? C4d C4d' H4d'A . . . 112.1 ? C4d C4d' H4d'B . . . 111.2 ? H3bB C4d' H4d'A . . . 111.4 ? H3bB C4d' H4d'B . . . 107.3 ? H4d'A C4d' H4d'B . . . 109.8 ? Co2 O01 H01a . . . 127.4 ? Co2 O01 H01b . . . 118.4 ? H01a O01 H01b . . . 99.3 ? H02a O02 H02b . . . 83.9 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # 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_000 844 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 16 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 10.066 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_theta_min 2.02 _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 atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .06 _refine_ls_wR_factor_all .055 _refine_ls_goodness_of_fit_all 1.505 _refine_ls_shift/su_mean .005 #========================================================================== # 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 #===END #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_pdmnx _database_code_CSD 169056 _audit_creation_method Xtal3.6 _audit_creation_date 01-05-10 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H57.35 Cl3.65 Co1 Mn1.325 N8 O15.675' _chemical_formula_moiety ? _chemical_formula_weight 897.976 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.495(2) _cell_length_b 15.356(2) _cell_length_c 20.682(3) _cell_angle_alpha 90.00000 _cell_angle_beta 106.232(2) _cell_angle_gamma 90.00000 _cell_volume 3810.1(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7144 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 21.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.196 _exptl_crystal_description plate _exptl_crystal_size_max .45 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _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 .62 _exptl_absorpt_correction_T_max .89 _diffrn_reflns_number 37058 _reflns_number_total 9580 _reflns_Friedel_coverage 0 _reflns_number_gt 7808 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _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 .064 _refine_ls_wR_factor_ref .077 _refine_ls_goodness_of_fit_ref 1.346 _refine_ls_number_reflns 7808 _refine_ls_number_parameters 490 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .026 _refine_diff_density_min -.803 _refine_diff_density_max .929 _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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 229.4 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 14.6 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' Mn ? 0 5.3 .295 .729 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 62.7 .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 Co .78596(4) 1.16199(3) .83345(3) .0184(2) Uani ? ? 1.00000 ? ? Mn1 .72546(5) .75965(4) .82468(3) .0263(3) Uani ? ? 1.00000 ? ? Mn2 .85099(16) .56049(12) .83205(12) .0296(9) Uani ? ? .3249(16) ? ? N0 .8635(3) .8712(2) .83248(18) .0226(14) Uani ? ? 1.00000 ? ? C01 .9298(3) .8414(3) .7872(2) .0270(17) Uani ? ? 1.00000 ? ? C02 .9424(3) .7429(3) .7901(3) .032(2) Uani ? ? 1.00000 ? ? O1 .8828(3) .69937(18) .8187(2) .0393(16) Uani ? ? 1.00000 ? ? O2 1.0119(3) .7115(2) .7636(2) .0469(18) Uani ? ? 1.00000 ? ? C1 .8423(3) .9664(2) .8315(2) .0206(15) Uani ? ? 1.00000 ? ? C2a .9458(3) 1.0181(2) .8284(2) .0254(17) Uani ? ? 1.00000 ? ? N3a .9344(3) 1.1147(2) .83620(18) .0236(14) Uani ? ? 1.00000 ? ? C4a 1.0157(3) 1.1484(3) .8981(3) .035(2) Uani ? ? 1.00000 ? ? C4a' .9869(4) 1.2433(3) .9034(3) .035(2) Uani ? ? 1.00000 ? ? N3a' .8670(3) 1.2465(2) .90273(17) .0251(14) Uani ? ? 1.00000 ? ? C2a' .8242(3) 1.3381(2) .8988(2) .0271(17) Uani ? ? 1.00000 ? ? C2b .8133(3) .9853(2) .8974(2) .0230(16) Uani ? ? 1.00000 ? ? N3b .7708(3) 1.0757(2) .90126(16) .0217(14) Uani ? ? 1.00000 ? ? C4b .6521(4) 1.0772(3) .9032(2) .0279(18) Uani ? ? 1.00000 ? ? C4b' .6180(4) 1.1717(3) .9003(2) .0294(19) Uani ? ? 1.00000 ? ? N3b' .6413(3) 1.2095(2) .83913(17) .0209(13) Uani ? ? 1.00000 ? ? C2b' .6246(3) 1.3060(2) .8355(2) .0264(17) Uani ? ? 1.00000 ? ? C2c .7436(3) .9854(2) .7709(2) .0220(16) Uani ? ? 1.00000 ? ? N3c .7152(3) 1.0796(2) .76073(16) .0199(13) Uani ? ? 1.00000 ? ? C4c .7310(4) 1.1154(2) .6971(2) .0249(17) Uani ? ? 1.00000 ? ? C4c' .7111(4) 1.2116(2) .6972(2) .0266(17) Uani ? ? 1.00000 ? ? N3c' .7870(3) 1.2459(2) .76132(17) .0219(13) Uani ? ? 1.00000 ? ? C2c' .7661(3) 1.3400(2) .7722(2) .0268(17) Uani ? ? 1.00000 ? ? C1' .7309(3) 1.3565(2) .8355(2) .0245(16) Uani ? ? 1.00000 ? ? N0' .7088(3) 1.4525(2) .83822(19) .0278(15) Uani ? ? 1.00000 ? ? C01' .6046(4) 1.4856(3) .7902(3) .033(2) Uani ? ? 1.00000 ? ? C02' .5987(3) 1.5840(2) .7927(2) .0263(17) Uani ? ? 1.00000 ? ? O1' .6846(2) 1.62377(17) .82451(17) .0299(13) Uani ? ? 1.00000 ? ? O2' .5075(2) 1.61668(19) .7621(2) .0374(15) Uani ? ? 1.00000 ? ? Cl0 1.09958(11) .85319(8) .95433(6) .0451(6) Uani ? ? 1.00000 ? ? Cl11 .56523(9) .84102(7) .83867(6) .0347(5) Uani ? ? 1.00000 ? ? Cl12 .6713(3) .7570(2) .69525(18) .0359(15) Uani ? ? .3249(16) ? ? Cl13 1.1332(4) .4495(3) .8855(2) .118(3) Uani ? ? .6751(16) ? ? Cl23 1.0205(3) .4794(2) .8382(2) .0378(16) Uani ? ? .3249(16) ? ? Cl24 .4704(7) .3287(6) 1.0648(4) .108(5) Uani ? ? .3249(16) ? ? O10 .8953(6) .5244(4) .8035(5) .088(5) Uani ? ? .6751(16) ? ? O11 .7985(3) .7501(2) .9363(2) .055(2) Uani ? ? 1.00000 ? ? O12 .6725(5) .7657(4) .7147(3) .048(3) Uani ? ? .6751(16) ? ? O21 .7856(7) .5635(5) .7101(5) .026(4) Uani ? ? .3249(16) ? ? O22 .9109(4) .5759(3) .9618(2) .073(3) Uani ? ? 1.00000 ? ? O01 .6143(7) .9058(5) .6158(3) .134(5) Uani ? ? 1.00000 ? ? O02 .6319(10) .3530(5) 1.0130(4) .171(7) Uani ? ? 1.00000 ? ? O03 .8530(10) .3467(6) 1.0716(4) .178(8) Uani ? ? 1.00000 ? ? O04 .7132(7) .4182(8) .6075(4) .168(8) Uani ? ? 1.00000 ? ? O05 .6990(8) .7684(9) 1.0335(4) .198(9) Uani ? ? 1.00000 ? ? O06 .3912(14) 1.0033(5) .5563(5) .239(10) Uani ? ? 1.00000 ? ? O07 .5062(10) .9142(8) .9809(7) .136(9) Uani ? ? .6751(16) ? ? O08 .736(2) .5924(15) .6588(12) .35(2) Uani ? ? .6751(16) ? ? O09 .4720(18) .837(2) .9597(10) .15(2) Uani ? ? .3249(16) ? ? O010 .6759(7) .6004(5) .6260(5) .028(4) Uani ? ? .3249(16) ? ? H0 .90022 .86048 .86323 .02100 Uiso ? ? 1.00000 ? ? H01A .88951 .86052 .73406 .03300 Uiso ? ? 1.00000 ? ? H01B 1.00093 .86415 .80407 .03800 Uiso ? ? 1.00000 ? ? H2aA 1.00679 .99701 .85992 .02500 Uiso ? ? 1.00000 ? ? H2aB .95770 1.01937 .78534 .03700 Uiso ? ? 1.00000 ? ? H3a .95009 1.13890 .80377 .02000 Uiso ? ? 1.00000 ? ? H4aA 1.01133 1.11786 .93864 .01600 Uiso ? ? 1.00000 ? ? H4aB 1.08848 1.14222 .89481 .01700 Uiso ? ? 1.00000 ? ? H4a'A 1.02742 1.27271 .94313 .02500 Uiso ? ? 1.00000 ? ? H4a'B .99708 1.28108 .86549 .05400 Uiso ? ? 1.00000 ? ? H3a' .86207 1.22899 .94540 .03100 Uiso ? ? 1.00000 ? ? H2a'A .80417 1.35411 .94043 .02900 Uiso ? ? 1.00000 ? ? H2a'B .88220 1.36973 .90611 .03700 Uiso ? ? 1.00000 ? ? H2bA .75522 .94944 .89696 .01200 Uiso ? ? 1.00000 ? ? H2bB .87992 .98478 .93396 .03200 Uiso ? ? 1.00000 ? ? H3b .80314 1.10061 .93695 .03100 Uiso ? ? 1.00000 ? ? H4bA .61284 1.04630 .86604 .03000 Uiso ? ? 1.00000 ? ? H4bB .64875 1.05371 .94038 .02300 Uiso ? ? 1.00000 ? ? H4b'A .53220 1.17591 .89011 .02700 Uiso ? ? 1.00000 ? ? H4b'B .65897 1.20385 .93764 .04000 Uiso ? ? 1.00000 ? ? H3b' .58654 1.19306 .80065 .02200 Uiso ? ? 1.00000 ? ? H2b'A .56670 1.32015 .79630 .03100 Uiso ? ? 1.00000 ? ? H2b'B .59911 1.33084 .87286 .04500 Uiso ? ? 1.00000 ? ? H2cA .75512 .96569 .72919 .02400 Uiso ? ? 1.00000 ? ? H2cB .68100 .95498 .77567 .01800 Uiso ? ? 1.00000 ? ? H3c .64724 1.08254 .75371 .00900 Uiso ? ? 1.00000 ? ? H4cA .79902 1.11132 .69270 .03100 Uiso ? ? 1.00000 ? ? H4cB .67978 1.07737 .65635 .05500 Uiso ? ? 1.00000 ? ? H4c'A .72616 1.23742 .65997 .03200 Uiso ? ? 1.00000 ? ? H4c'B .63561 1.22190 .69610 .02400 Uiso ? ? 1.00000 ? ? H3c' .85006 1.24421 .75748 .05300 Uiso ? ? 1.00000 ? ? H2c'A .83799 1.37027 .77503 .02800 Uiso ? ? 1.00000 ? ? H2c'B .70990 1.35900 .73438 .01600 Uiso ? ? 1.00000 ? ? H0'A .70629 1.46494 .87785 .05000 Uiso ? ? 1.00000 ? ? H01'A .60079 1.47286 .74090 .03000 Uiso ? ? 1.00000 ? ? H01'B .54979 1.46475 .80732 .04100 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 Co .0174(2) .0100(2) .0254(3) -.00048(18) .00191(19) .00025(19) Mn1 .0212(3) .0155(3) .0409(4) -.0014(2) .0063(3) .0012(2) Mn2 .0240(10) .0158(8) .0481(13) .0005(7) .0087(9) -.0007(8) N0 .0229(16) .0109(13) .0334(18) .0016(12) .0067(14) .0014(12) C01 .0214(18) .0174(17) .044(2) -.0015(14) .0115(17) -.0052(17) C02 .0195(18) .0210(19) .053(3) .0004(15) .0068(18) -.0083(19) O1 .0252(15) .0137(13) .083(3) -.0005(11) .0221(16) -.0031(15) O2 .0357(18) .0226(15) .091(3) -.0034(13) .031(2) -.0183(17) C1 .0199(17) .0113(15) .030(2) .0003(13) .0065(15) -.0001(14) C2a .0200(17) .0127(16) .042(2) -.0005(14) .0069(17) -.0012(16) N3a .0180(15) .0137(14) .0366(19) -.0010(12) .0034(14) .0022(13) C4a .022(2) .0155(18) .056(3) .0036(15) -.007(2) -.0032(18) C4a' .024(2) .0204(19) .051(3) -.0014(16) -.0064(19) -.0083(19) N3a' .0261(16) .0153(14) .0279(17) .0031(13) -.0026(13) -.0004(13) C2a' .028(2) .0132(16) .033(2) .0037(15) -.0034(17) -.0040(15) C2b .027(2) .0127(15) .028(2) .0033(14) .0053(16) .0028(14) N3b .0259(16) .0134(14) .0243(16) .0015(12) .0042(13) -.0025(12) C4b .035(2) .0170(17) .035(2) .0037(16) .0167(18) .0046(16) C4b' .038(2) .0185(18) .034(2) .0067(16) .0147(19) .0017(16) N3b' .0217(15) .0105(13) .0288(17) -.0007(11) .0044(13) -.0010(12) C2b' .0241(19) .0122(16) .040(2) .0011(14) .0035(17) .0011(15) C2c .0229(18) .0116(15) .030(2) -.0008(13) .0041(15) .0009(14) N3c .0188(15) .0130(13) .0257(16) -.0006(11) .0030(12) -.0002(12) C4c .034(2) .0162(17) .025(2) -.0028(15) .0077(17) -.0011(14) C4c' .035(2) .0144(16) .027(2) -.0013(15) .0035(17) .0009(15) N3c' .0199(15) .0131(14) .0311(17) -.0015(12) .0046(13) -.0001(12) C2c' .030(2) .0119(16) .036(2) .0008(15) .0050(17) .0031(15) C1' .027(2) .0078(14) .033(2) .0021(13) -.0012(16) .0008(14) N0' .0279(17) .0096(13) .040(2) .0046(12) .0000(15) -.0011(13) C01' .024(2) .0164(17) .052(3) .0004(15) -.0002(19) .0010(18) C02' .0192(18) .0146(16) .046(2) .0022(14) .0108(17) .0034(16) O1' .0211(13) .0133(12) .053(2) -.0000(10) .0058(13) .0018(12) O2' .0206(14) .0179(13) .069(2) .0016(11) .0050(15) .0110(14) Cl0 .0493(7) .0425(6) .0323(6) .0023(5) -.0070(5) -.0015(5) Cl11 .0269(5) .0236(5) .0557(7) -.0001(4) .0151(5) -.0050(5) Cl12 .0359(17) .0299(16) .0386(18) -.0045(13) .0048(14) -.0056(14) Cl13 .141(3) .108(3) .120(3) -.027(3) .061(3) .021(2) Cl23 .0298(16) .0214(14) .064(2) .0025(12) .0160(16) .0018(15) Cl24 .097(5) .117(6) .113(6) -.014(5) .033(4) .033(5) O10 .076(5) .025(3) .186(9) -.009(3) .073(6) -.011(4) O11 .047(2) .040(2) .061(2) -.0115(17) -.0156(18) .0130(18) O12 .061(3) .041(3) .046(3) -.014(3) .022(3) -.020(2) O21 .019(4) .012(4) .048(5) .000(3) .010(4) -.003(4) O22 .093(4) .053(3) .067(3) .029(3) .012(3) .015(2) O01 .167(7) .117(6) .085(4) -.069(5) -.020(4) .001(4) O02 .334(14) .106(6) .076(5) .025(7) .062(6) -.013(4) O03 .321(13) .120(6) .107(6) .063(8) .082(7) -.020(5) O04 .136(7) .253(12) .146(7) .044(7) .088(6) .071(8) O05 .178(9) .346(16) .077(5) -.108(10) .047(5) -.017(7) O06 .56(2) .083(5) .143(7) -.033(9) .215(12) -.018(5) O07 .132(9) .120(9) .199(12) .001(7) .116(9) .020(8) O08 .39(3) .36(3) .43(3) -.30(2) .35(3) -.32(3) O09 .103(15) .27(3) .091(14) -.050(18) .062(13) .027(17) O010 .027(4) .020(4) .044(5) -.010(3) .020(4) -.028(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Co N3a . . 1.978(3) ? Co N3a' . . 1.988(3) ? Co N3b . . 1.977(3) ? Co N3b' . . 1.982(3) ? Co N3c . . 1.975(3) ? Co N3c' . . 1.974(3) ? Mn1 N0 . . 2.404(3) ? Mn1 O1 . . 2.208(3) ? Mn1 Cl11 . . 2.4448(14) ? Mn1 Cl12 . . 2.571(4) ? Mn1 O11 . . 2.238(4) ? Mn1 O12 . . 2.185(6) ? Mn1 O1' . '1 545' 2.148(3) ? Mn2 O1 . . 2.201(3) ? Mn2 Cl23 . . 2.429(4) ? Mn2 O21 . . 2.424(10) ? Mn2 O22 . . 2.588(5) ? Mn2 N0' . '1 545' 2.459(4) ? Mn2 O1' . '1 545' 2.261(4) ? N0 C01 . . 1.486(6) ? N0 C1 . . 1.484(5) ? N0 H0 . . .692 ? C01 C02 . . 1.520(6) ? C01 H01A . . 1.113 ? C01 H01B . . .927 ? C02 O1 . . 1.264(6) ? C02 O2 . . 1.247(7) ? C1 C2a . . 1.534(6) ? C1 C2b . . 1.533(6) ? C1 C2c . . 1.520(5) ? C2a N3a . . 1.502(5) ? C2a H2aA . . .913 ? C2a H2aB . . .944 ? N3a C4a . . 1.487(5) ? N3a H3a . . .837 ? C4a C4a' . . 1.513(6) ? C4a H4aA . . .975 ? C4a H4aB . . .936 ? C4a' N3a' . . 1.496(6) ? C4a' H4a'A . . .950 ? C4a' H4a'B . . 1.011 ? N3a' C2a' . . 1.499(5) ? N3a' H3a' . . .941 ? C2a' C1' . . 1.516(5) ? C2a' H2a'A . . .993 ? C2a' H2a'B . . .850 ? C2b N3b . . 1.496(5) ? C2b H2bA . . .909 ? C2b H2bB . . .956 ? N3b C4b . . 1.495(6) ? N3b H3b . . .829 ? C4b C4b' . . 1.509(6) ? C4b H4bA . . .919 ? C4b H4bB . . .861 ? C4b' N3b' . . 1.493(6) ? C4b' H4b'A . . 1.035 ? C4b' H4b'B . . .939 ? N3b' C2b' . . 1.496(5) ? N3b' H3b' . . .928 ? C2b' C1' . . 1.537(6) ? C2b' H2b'A . . .950 ? C2b' H2b'B . . .990 ? C2c N3c . . 1.490(5) ? C2c H2cA . . .962 ? C2c H2cB . . .940 ? N3c C4c . . 1.489(6) ? N3c H3c . . .822 ? C4c C4c' . . 1.498(5) ? C4c H4cA . . .882 ? C4c H4cB . . 1.077 ? C4c' N3c' . . 1.494(5) ? C4c' H4c'A . . .931 ? C4c' H4c'B . . .950 ? N3c' C2c' . . 1.496(5) ? N3c' H3c' . . .815 ? C2c' C1' . . 1.515(7) ? C2c' H2c'A . . .999 ? C2c' H2c'B . . .939 ? C1' N0' . . 1.505(5) ? N0' C01' . . 1.489(5) ? N0' H0'A . . .851 ? C01' C02' . . 1.514(5) ? C01' H01'A . . 1.027 ? C01' H01'B . . .912 ? C02' O1' . . 1.250(4) ? C02' O2' . . 1.245(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 N3a Co N3a' . . . 86.25(14) ? N3a Co N3b . . . 90.48(15) ? N3a Co N3b' . . . 175.16(15) ? N3a Co N3c . . . 90.16(13) ? N3a Co N3c' . . . 93.30(14) ? N3a' Co N3b . . . 93.25(14) ? N3a' Co N3b' . . . 90.35(14) ? N3a' Co N3c . . . 175.20(16) ? N3a' Co N3c' . . . 90.52(13) ? N3b Co N3b' . . . 86.27(14) ? N3b Co N3c . . . 89.97(13) ? N3b Co N3c' . . . 174.83(13) ? N3b' Co N3c . . . 93.42(13) ? N3b' Co N3c' . . . 90.17(14) ? N3c Co N3c' . . . 86.50(13) ? N0 Mn1 O1 . . . 70.68(11) ? N0 Mn1 Cl11 . . . 102.92(9) ? N0 Mn1 Cl12 . . . 93.22(12) ? N0 Mn1 O11 . . . 84.22(13) ? N0 Mn1 O12 . . . 92.42(18) ? N0 Mn1 O1' . . '1 545' 149.11(11) ? O1 Mn1 Cl11 . . . 172.98(8) ? O1 Mn1 Cl12 . . . 85.11(13) ? O1 Mn1 O11 . . . 85.27(15) ? O1 Mn1 O12 . . . 88.6(2) ? O1 Mn1 O1' . . '1 545' 78.91(11) ? Cl11 Mn1 Cl12 . . . 98.36(9) ? Cl11 Mn1 O11 . . . 91.29(12) ? Cl11 Mn1 O12 . . . 94.69(17) ? Cl11 Mn1 O1' . . '1 545' 107.13(9) ? Cl12 Mn1 O11 . . . 170.35(14) ? Cl12 Mn1 O1' . . '1 545' 89.42(12) ? O11 Mn1 O12 . . . 173.7(2) ? O11 Mn1 O1' . . '1 545' 88.08(13) ? O12 Mn1 O1' . . '1 545' 92.12(17) ? O1 Mn2 Cl23 . . . 108.52(15) ? O1 Mn2 O21 . . . 82.6(2) ? O1 Mn2 O22 . . . 91.78(16) ? O1 Mn2 N0' . . '1 545' 144.91(15) ? O1 Mn2 O1' . . '1 545' 76.69(13) ? Cl23 Mn2 O21 . . . 95.7(2) ? Cl23 Mn2 O22 . . . 89.86(17) ? Cl23 Mn2 N0' . . '1 545' 106.49(13) ? Cl23 Mn2 O1' . . '1 545' 174.58(14) ? O21 Mn2 O22 . . . 173.1(2) ? O21 Mn2 N0' . . '1 545' 91.6(2) ? O21 Mn2 O1' . . '1 545' 83.3(2) ? O22 Mn2 N0' . . '1 545' 90.67(17) ? O22 Mn2 O1' . . '1 545' 91.49(17) ? N0' Mn2 O1' '1 545' . '1 545' 68.25(12) ? Mn1 N0 C01 . . . 104.7(2) ? Mn1 N0 C1 . . . 125.4(2) ? Mn1 N0 H0 . . . 99.8 ? C01 N0 C1 . . . 115.1(3) ? C01 N0 H0 . . . 99.3 ? C1 N0 H0 . . . 108.5 ? N0 C01 C02 . . . 110.6(4) ? N0 C01 H01A . . . 111.3 ? N0 C01 H01B . . . 107.0 ? C02 C01 H01A . . . 108.3 ? C02 C01 H01B . . . 106.4 ? H01A C01 H01B . . . 113.2 ? C01 C02 O1 . . . 118.5(4) ? C01 C02 O2 . . . 116.4(4) ? O1 C02 O2 . . . 125.1(4) ? Mn1 O1 Mn2 . . . 101.80(15) ? Mn1 O1 C02 . . . 117.0(3) ? Mn2 O1 C02 . . . 136.2(3) ? N0 C1 C2a . . . 111.1(3) ? N0 C1 C2b . . . 105.1(3) ? N0 C1 C2c . . . 107.5(3) ? C2a C1 C2b . . . 110.5(3) ? C2a C1 C2c . . . 111.4(3) ? C2b C1 C2c . . . 111.0(3) ? C1 C2a N3a . . . 113.6(3) ? C1 C2a H2aA . . . 109.4 ? C1 C2a H2aB . . . 114.0 ? N3a C2a H2aA . . . 111.0 ? N3a C2a H2aB . . . 97.2 ? H2aA C2a H2aB . . . 111.1 ? Co N3a C2a . . . 118.4(2) ? Co N3a C4a . . . 107.8(3) ? Co N3a H3a . . . 104.0 ? C2a N3a C4a . . . 112.0(3) ? C2a N3a H3a . . . 107.6 ? C4a N3a H3a . . . 106.2 ? N3a C4a C4a' . . . 106.2(3) ? N3a C4a H4aA . . . 112.6 ? N3a C4a H4aB . . . 110.2 ? C4a' C4a H4aA . . . 109.3 ? C4a' C4a H4aB . . . 111.0 ? H4aA C4a H4aB . . . 107.6 ? C4a C4a' N3a' . . . 106.7(3) ? C4a C4a' H4a'A . . . 116.1 ? C4a C4a' H4a'B . . . 114.4 ? N3a' C4a' H4a'A . . . 106.4 ? N3a' C4a' H4a'B . . . 108.5 ? H4a'A C4a' H4a'B . . . 104.3 ? Co N3a' C4a' . . . 107.0(3) ? Co N3a' C2a' . . . 118.1(2) ? Co N3a' H3a' . . . 109.6 ? C4a' N3a' C2a' . . . 111.8(3) ? C4a' N3a' H3a' . . . 108.1 ? C2a' N3a' H3a' . . . 101.8 ? N3a' C2a' C1' . . . 113.5(3) ? N3a' C2a' H2a'A . . . 110.9 ? N3a' C2a' H2a'B . . . 104.7 ? C1' C2a' H2a'A . . . 112.5 ? C1' C2a' H2a'B . . . 117.4 ? H2a'A C2a' H2a'B . . . 96.4 ? C1 C2b N3b . . . 113.5(3) ? C1 C2b H2bA . . . 105.2 ? C1 C2b H2bB . . . 109.4 ? N3b C2b H2bA . . . 105.6 ? N3b C2b H2bB . . . 102.1 ? H2bA C2b H2bB . . . 121.3 ? Co N3b C2b . . . 118.6(3) ? Co N3b C4b . . . 107.5(2) ? Co N3b H3b . . . 101.7 ? C2b N3b C4b . . . 112.6(3) ? C2b N3b H3b . . . 112.5 ? C4b N3b H3b . . . 102.1 ? N3b C4b C4b' . . . 106.6(3) ? N3b C4b H4bA . . . 105.8 ? N3b C4b H4bB . . . 108.3 ? C4b' C4b H4bA . . . 112.6 ? C4b' C4b H4bB . . . 110.7 ? H4bA C4b H4bB . . . 112.5 ? C4b C4b' N3b' . . . 106.7(4) ? C4b C4b' H4b'A . . . 109.5 ? C4b C4b' H4b'B . . . 112.9 ? N3b' C4b' H4b'A . . . 103.9 ? N3b' C4b' H4b'B . . . 107.5 ? H4b'A C4b' H4b'B . . . 115.5 ? Co N3b' C4b' . . . 107.7(2) ? Co N3b' C2b' . . . 118.6(3) ? Co N3b' H3b' . . . 108.4 ? C4b' N3b' C2b' . . . 111.7(3) ? C4b' N3b' H3b' . . . 110.4 ? C2b' N3b' H3b' . . . 99.7 ? N3b' C2b' C1' . . . 113.0(3) ? N3b' C2b' H2b'A . . . 109.3 ? N3b' C2b' H2b'B . . . 114.4 ? C1' C2b' H2b'A . . . 109.7 ? C1' C2b' H2b'B . . . 105.9 ? H2b'A C2b' H2b'B . . . 104.1 ? C1 C2c N3c . . . 114.1(3) ? C1 C2c H2cA . . . 112.9(4) ? C1 C2c H2cB . . . 109.0 ? N3c C2c H2cA . . . 105.5 ? N3c C2c H2cB . . . 109.0 ? H2cA C2c H2cB . . . 106.0 ? Co N3c C2c . . . 118.4(2) ? Co N3c C4c . . . 107.1(2) ? Co N3c H3c . . . 108.6 ? C2c N3c C4c . . . 113.5(3) ? C2c N3c H3c . . . 105.8 ? C4c N3c H3c . . . 102.0 ? N3c C4c C4c' . . . 107.5(3) ? N3c C4c H4cA . . . 115.7 ? N3c C4c H4cB . . . 107.2 ? C4c' C4c H4cA . . . 103.6 ? C4c' C4c H4cB . . . 118.2 ? H4cA C4c H4cB . . . 105.1 ? C4c C4c' N3c' . . . 106.5(3) ? C4c C4c' H4c'A . . . 110.3 ? C4c C4c' H4c'B . . . 109.2 ? N3c' C4c' H4c'A . . . 111.0 ? N3c' C4c' H4c'B . . . 110.0 ? H4c'A C4c' H4c'B . . . 109.8 ? Co N3c' C4c' . . . 107.7(2) ? Co N3c' C2c' . . . 118.6(3) ? Co N3c' H3c' . . . 105.3 ? C4c' N3c' C2c' . . . 112.3(3) ? C4c' N3c' H3c' . . . 107.1 ? C2c' N3c' H3c' . . . 105.1 ? N3c' C2c' C1' . . . 113.3(3) ? N3c' C2c' H2c'A . . . 105.5 ? N3c' C2c' H2c'B . . . 107.2 ? C1' C2c' H2c'A . . . 110.2 ? C1' C2c' H2c'B . . . 109.7 ? H2c'A C2c' H2c'B . . . 110.8 ? C2a' C1' C2b' . . . 111.2(3) ? C2a' C1' C2c' . . . 112.1(4) ? C2a' C1' N0' . . . 104.8(3) ? C2b' C1' C2c' . . . 112.1(3) ? C2b' C1' N0' . . . 109.1(3) ? C2c' C1' N0' . . . 107.3(3) ? C1' N0' C01' . . . 116.4(3) ? C1' N0' H0'A . . . 108.2 ? C1' N0' Mn2 . . '1 565' 121.1(3) ? C01' N0' H0'A . . . 107.7 ? C01' N0' Mn2 . . '1 565' 104.2(2) ? H0'A N0' Mn2 . . '1 565' 96.9(2) ? N0' C01' C02' . . . 111.1(3) ? N0' C01' H01'A . . . 112.7 ? N0' C01' H01'B . . . 103.5 ? C02' C01' H01'A . . . 103.6 ? C02' C01' H01'B . . . 106.7 ? H01'A C01' H01'B . . . 119.1 ? C01' C02' O1' . . . 117.6(3) ? C01' C02' O2' . . . 115.6(3) ? O1' C02' O2' . . . 126.9(4) ? C02' O1' Mn1 . . '1 565' 130.1(2) ? C02' O1' Mn2 . . '1 565' 117.6(3) ? Mn1 O1' Mn2 '1 565' . '1 565' 101.76(13) ? 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 1875.7 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 16 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -28 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 9.909 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .08 _refine_ls_wR_factor_all .081 _refine_ls_goodness_of_fit_all 1.262 _refine_ls_shift/su_mean .003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_p147 _database_code_CSD 169057 _audit_creation_method Xtal3.6 _audit_creation_date 00-11-15 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H55 Cl5 Co1 Mn2 N8 O13.5' _chemical_formula_moiety ? _chemical_formula_weight 945.75 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.303(2) _cell_length_b 15.336(2) _cell_length_c 20.730(3) _cell_angle_alpha 90.00000 _cell_angle_beta 106.226(3) _cell_angle_gamma 90.00000 _cell_volume 3755.5(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.673 _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 2.5 _cell_measurement_theta_max 22.5 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.521 _exptl_crystal_description plate _exptl_crystal_size_max .3 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _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 .65 _exptl_absorpt_correction_T_max .91 _diffrn_reflns_number 36797 _reflns_number_total 6588 _reflns_Friedel_coverage 0 _reflns_number_gt 4829 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 24.96 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .054 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _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 .084 _refine_ls_wR_factor_ref .101 _refine_ls_goodness_of_fit_ref 1.931 _refine_ls_number_reflns 4829 _refine_ls_number_parameters 263 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .036 _refine_diff_density_min -1.932 _refine_diff_density_max 2.495 _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 _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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 220 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 20 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' Mn ? 0 8 .295 .729 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 54 .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 Co .78830(9) 1.16175(7) .83360(6) .0127(5) Uani ? ? 1.00000 ? ? Mn1 .72262(11) .76347(8) .82840(8) .0215(7) Uani ? ? 1.00000 ? ? Mn2 .85516(12) .55908(9) .83258(8) .0264(7) Uani ? ? 1.00000 ? ? Cl0 1.1055(3) .84607(19) .95513(13) .0414(14) Uani ? ? 1.00000 ? ? Cl11 .5588(2) .84489(15) .83752(13) .0284(11) Uani ? ? 1.00000 ? ? Cl12 .6756(3) .7579(2) .7018(2) .077(2) Uani ? ? 1.00000 ? ? Cl21 .7847(5) .5629(3) .7051(3) .037(3) Uani ? ? .50000 ? ? Cl22 .9103(5) .5705(4) .9622(3) .036(3) Uani ? ? .50000 ? ? Cl23 1.0282(2) .47647(16) .84017(15) .0361(13) Uani ? ? 1.00000 ? ? O11 .7925(6) .7567(5) .9439(4) .0347(17) Uiso ? ? 1.00000 ? ? O21 .7899(17) .5622(14) .7244(10) .067(5) Uiso ? ? .50000 ? ? O22 .8988(14) .5683(11) .9422(8) .044(4) Uiso ? ? .50000 ? ? N0 .8646(6) .8700(4) .8358(3) .0140(14) Uiso ? ? 1.00000 ? ? C01 .9325(8) .8379(6) .7922(4) .023(2) Uiso ? ? 1.00000 ? ? C02 .9441(8) .7407(6) .7961(4) .0208(19) Uiso ? ? 1.00000 ? ? O1 .8863(5) .6987(4) .8278(3) .0217(14) Uiso ? ? 1.00000 ? ? O2 1.0115(5) .7057(4) .7687(3) .0264(15) Uiso ? ? 1.00000 ? ? C1 .8432(7) .9663(5) .8332(4) .0146(17) Uiso ? ? 1.00000 ? ? C2a .9495(7) 1.0159(5) .8315(4) .0146(17) Uiso ? ? 1.00000 ? ? N3a .9393(6) 1.1129(5) .8365(4) .0177(15) Uiso ? ? 1.00000 ? ? C4a 1.0216(8) 1.1489(6) .8975(5) .027(2) Uiso ? ? 1.00000 ? ? C4a' .9918(8) 1.2441(6) .9013(5) .024(2) Uiso ? ? 1.00000 ? ? N3a' .8708(6) 1.2457(5) .9019(4) .0183(15) Uiso ? ? 1.00000 ? ? C2a' .8275(7) 1.3375(6) .8996(4) .0197(19) Uiso ? ? 1.00000 ? ? C2b .8129(7) .9855(6) .8976(4) .0180(18) Uiso ? ? 1.00000 ? ? N3b .7710(6) 1.0764(5) .9011(3) .0166(15) Uiso ? ? 1.00000 ? ? C4b .6490(8) 1.0780(6) .9013(5) .022(2) Uiso ? ? 1.00000 ? ? C4b' .6149(8) 1.1720(6) .8974(4) .021(2) Uiso ? ? 1.00000 ? ? N3b' .6397(6) 1.2102(5) .8368(3) .0157(15) Uiso ? ? 1.00000 ? ? C2b' .6244(8) 1.3075(6) .8347(4) .0194(19) Uiso ? ? 1.00000 ? ? C2c .7463(7) .9843(6) .7715(4) .0171(18) Uiso ? ? 1.00000 ? ? N3c .7173(6) 1.0796(4) .7610(3) .0132(14) Uiso ? ? 1.00000 ? ? C4c .7343(7) 1.1144(6) .6970(4) .0198(19) Uiso ? ? 1.00000 ? ? C4c' .7143(8) 1.2114(6) .6991(4) .021(2) Uiso ? ? 1.00000 ? ? N3c' .7918(6) 1.2453(5) .7625(3) .0153(15) Uiso ? ? 1.00000 ? ? C2c' .7714(7) 1.3398(6) .7729(4) .0187(18) Uiso ? ? 1.00000 ? ? C1' .7341(7) 1.3578(5) .8353(4) .0155(17) Uiso ? ? 1.00000 ? ? N0' .7148(6) 1.4529(5) .8397(4) .0187(16) Uiso ? ? 1.00000 ? ? C01' .6071(8) 1.4866(6) .7943(5) .023(2) Uiso ? ? 1.00000 ? ? C02' .6005(8) 1.5855(6) .7970(4) .021(2) Uiso ? ? 1.00000 ? ? O1' .6900(5) 1.6250(4) .8291(3) .0211(14) Uiso ? ? 1.00000 ? ? O2' .5100(5) 1.6190(4) .7687(3) .0251(14) Uiso ? ? 1.00000 ? ? O01 .7231(17) 1.4393(14) .6110(10) .163(7) Uiso ? ? 1.00000 ? ? O02 .3124(15) 1.2810(12) .4658(9) .143(6) Uiso ? ? 1.00000 ? ? O03 .5681(16) .9885(13) .4366(9) .156(7) Uiso ? ? 1.00000 ? ? O04 .8372(13) 1.1467(10) .5690(8) .042(4) Uiso ? ? .50000 ? ? O05 .6065(12) .8940(9) .6073(7) .034(3) Uiso ? ? .50000 ? ? O06 .486(2) 1.1818(16) .5620(12) .086(7) Uiso ? ? .50000 ? ? O07 .662(3) .900(2) .6055(16) .129(11) Uiso ? ? .50000 ? ? O08 .600(2) 1.1617(18) .5186(14) .105(8) Uiso ? ? .50000 ? ? O09 .7755(18) .9937(15) .5432(11) .076(6) Uiso ? ? .50000 ? ? O010 .534(3) 1.358(2) .5434(15) .119(10) Uiso ? ? .50000 ? ? O011 .720(5) 1.146(3) .537(3) .22(2) Uiso ? ? .50000 ? ? O012 .431(4) 1.432(3) .481(2) .202(18) Uiso ? ? .50000 ? ? H0 .91800 .85952 .87700 .02200 Uiso ? ? 1.00000 ? ? H01A .89360 .85393 .74624 .03000 Uiso ? ? 1.00000 ? ? H01B 1.00447 .86487 .80394 .03000 Uiso ? ? 1.00000 ? ? H2aA 1.01153 .99553 .86670 .02300 Uiso ? ? 1.00000 ? ? H2aB .96489 1.00248 .78920 .02300 Uiso ? ? 1.00000 ? ? H3a .96208 1.13816 .80191 .02300 Uiso ? ? 1.00000 ? ? H4aA 1.01599 1.11901 .93675 .03700 Uiso ? ? 1.00000 ? ? H4aB 1.09773 1.14273 .89443 .03700 Uiso ? ? 1.00000 ? ? H3a' .87197 1.22336 .94335 .02400 Uiso ? ? 1.00000 ? ? H4a'A 1.03937 1.27161 .94030 .03200 Uiso ? ? 1.00000 ? ? H4a'B 1.00064 1.27530 .86242 .03200 Uiso ? ? 1.00000 ? ? H2a'A .80085 1.34731 .93798 .02800 Uiso ? ? 1.00000 ? ? H2a'B .89045 1.37674 .90265 .02800 Uiso ? ? 1.00000 ? ? H2bA .75640 .94583 .90155 .02200 Uiso ? ? 1.00000 ? ? H2bB .87923 .97730 .93447 .02200 Uiso ? ? 1.00000 ? ? H3b .80850 1.09858 .94320 .02200 Uiso ? ? 1.00000 ? ? H4bA .60378 1.04709 .86289 .02900 Uiso ? ? 1.00000 ? ? H4bB .63939 1.05136 .94075 .02900 Uiso ? ? 1.00000 ? ? H4b'A .53591 1.17858 .89389 .02900 Uiso ? ? 1.00000 ? ? H4b'B .65678 1.20302 .93695 .02900 Uiso ? ? 1.00000 ? ? H3b' .58444 1.19448 .79882 .02000 Uiso ? ? 1.00000 ? ? H2b'A .56735 1.32192 .79467 .02600 Uiso ? ? 1.00000 ? ? H2b'B .60106 1.32476 .87255 .02600 Uiso ? ? 1.00000 ? ? H2cA .76632 .96338 .73358 .02300 Uiso ? ? 1.00000 ? ? H2cB .68148 .95476 .77629 .02300 Uiso ? ? 1.00000 ? ? H3c .63956 1.08463 .75235 .01700 Uiso ? ? 1.00000 ? ? H4cA .81009 1.10333 .69493 .02600 Uiso ? ? 1.00000 ? ? H4cB .68290 1.08859 .65876 .02600 Uiso ? ? 1.00000 ? ? H4c'A .72895 1.23886 .66117 .02600 Uiso ? ? 1.00000 ? ? H4c'B .63750 1.22181 .69824 .02600 Uiso ? ? 1.00000 ? ? H3c' .86267 1.24166 .75560 .02100 Uiso ? ? 1.00000 ? ? H2c'A .83969 1.37174 .77636 .02300 Uiso ? ? 1.00000 ? ? H2c'B .71448 1.36102 .73445 .02300 Uiso ? ? 1.00000 ? ? H01'A .60093 1.46857 .74874 .03000 Uiso ? ? 1.00000 ? ? H01'B .54454 1.46115 .80677 .03000 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 Co .0130(6) .0050(5) .0211(6) -.0005(4) .0066(4) .0002(4) Mn1 .0180(7) .0081(6) .0405(9) .0002(5) .0114(6) -.0005(6) Mn2 .0239(8) .0143(7) .0428(9) .0001(6) .0124(7) .0003(6) Cl0 .0502(17) .0419(16) .0269(13) -.0031(13) .0022(12) .0023(12) Cl11 .0207(12) .0175(11) .0487(15) .0023(9) .0125(10) -.0020(10) Cl12 .066(2) .044(2) .120(4) -.0033(18) .026(2) -.002(2) Cl21 .042(3) .024(3) .053(3) -.001(2) .026(3) .000(2) Cl22 .037(3) .034(3) .032(3) .008(2) -.000(2) .005(2) Cl23 .0359(14) .0232(12) .0551(17) -.0007(11) .0227(13) -.0017(11) # 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 Co N3a . . 1.988(8) ? Co N3a' . . 1.971(7) ? Co N3b . . 1.971(8) ? Co N3b' . . 1.992(8) ? Co N3c . . 1.970(6) ? Co N3c' . . 1.962(7) ? Mn1 Cl11 . . 2.422(3) ? Mn1 Cl12 . . 2.526(5) ? Mn1 O11 . . 2.310(7) ? Mn1 N0 . . 2.365(7) ? Mn1 O1 . . 2.249(7) ? Mn1 O1' . '1 545' 2.163(6) ? Mn2 Cl21 . . 2.542(6) ? Mn2 Cl22 . . 2.587(5) ? Mn2 Cl23 . . 2.444(3) ? Mn2 O21 . . 2.16(2) ? Mn2 O22 . . 2.189(16) ? Mn2 O1 . . 2.182(6) ? Mn2 N0' . '1 545' 2.408(8) ? Mn2 O1' . '1 545' 2.253(7) ? Cl21 O21 . . .39(2) ? Cl22 O22 . . .400(16) ? N0 C01 . . 1.476(13) ? N0 C1 . . 1.499(11) ? N0 H0 . . .934 ? C01 C02 . . 1.498(13) ? C01 H01A . . .971 ? C01 H01B . . .945 ? C02 O1 . . 1.271(12) ? C02 O2 . . 1.249(13) ? C1 C2a . . 1.522(12) ? C1 C2b . . 1.513(13) ? C1 C2c . . 1.510(10) ? C2a N3a . . 1.499(11) ? C2a H2aA . . .950 ? C2a H2aB . . .969 ? N3a C4a . . 1.488(11) ? N3a H3a . . .925 ? C4a C4a' . . 1.512(14) ? C4a H4aA . . .954 ? C4a H4aB . . .961 ? C4a' N3a' . . 1.492(13) ? C4a' H4a'A . . .954 ? C4a' H4a'B . . .970 ? N3a' C2a' . . 1.501(12) ? N3a' H3a' . . .922 ? C2a' C1' . . 1.530(11) ? C2a' H2a'A . . .953 ? C2a' H2a'B . . .969 ? C2b N3b . . 1.495(11) ? C2b H2bA . . .945 ? C2b H2bB . . .958 ? N3b C4b . . 1.503(12) ? N3b H3b . . .930 ? C4b C4b' . . 1.498(13) ? C4b H4bA . . .959 ? C4b H4bB . . .950 ? C4b' N3b' . . 1.493(12) ? C4b' H4b'A . . .959 ? C4b' H4b'B . . .963 ? N3b' C2b' . . 1.503(11) ? N3b' H3b' . . .917 ? C2b' C1' . . 1.552(13) ? C2b' H2b'A . . .952 ? C2b' H2b'B . . .945 ? C2c N3c . . 1.505(11) ? C2c H2cA . . .944 ? C2c H2cB . . .946 ? N3c C4c . . 1.498(12) ? N3c H3c . . .925 ? C4c C4c' . . 1.510(13) ? C4c H4cA . . .960 ? C4c H4cB . . .951 ? C4c' N3c' . . 1.486(10) ? C4c' H4c'A . . .953 ? C4c' H4c'B . . .954 ? N3c' C2c' . . 1.495(11) ? N3c' H3c' . . .925 ? C2c' C1' . . 1.514(13) ? C2c' H2c'A . . .957 ? C2c' H2c'B . . .959 ? C1' N0' . . 1.485(11) ? N0' C01' . . 1.487(11) ? C01' C02' . . 1.520(13) ? C01' H01'A . . .966 ? C01' H01'B . . .961 ? C02' O1' . . 1.270(10) ? C02' O2' . . 1.218(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N3a Co N3a' . . . 86.3(3) ? N3a Co N3b . . . 90.8(3) ? N3a Co N3b' . . . 176.5(3) ? N3a Co N3c . . . 89.6(3) ? N3a Co N3c' . . . 93.0(3) ? N3a' Co N3b . . . 93.4(3) ? N3a' Co N3b' . . . 91.5(3) ? N3a' Co N3c . . . 174.5(3) ? N3a' Co N3c' . . . 89.9(3) ? N3b Co N3b' . . . 86.7(3) ? N3b Co N3c . . . 90.3(3) ? N3b Co N3c' . . . 175.1(3) ? N3b' Co N3c . . . 92.8(3) ? N3b' Co N3c' . . . 89.7(3) ? N3c Co N3c' . . . 86.7(3) ? Cl11 Mn1 Cl12 . . . 98.32(12) ? Cl11 Mn1 O11 . . . 91.1(2) ? Cl11 Mn1 N0 . . . 104.74(19) ? Cl11 Mn1 O1 . . . 173.70(17) ? Cl11 Mn1 O1' . . '1 545' 110.2(2) ? Cl12 Mn1 O11 . . . 170.6(2) ? Cl12 Mn1 N0 . . . 92.4(2) ? Cl12 Mn1 O1 . . . 85.66(19) ? Cl12 Mn1 O1' . . '1 545' 89.14(19) ? O11 Mn1 N0 . . . 84.8(3) ? O11 Mn1 O1 . . . 84.9(2) ? O11 Mn1 O1' . . '1 545' 88.0(2) ? N0 Mn1 O1 . . . 70.1(2) ? N0 Mn1 O1' . . '1 545' 144.4(2) ? O1 Mn1 O1' . . '1 545' 74.6(2) ? Cl21 Mn2 Cl22 . . . 173.11(19) ? Cl21 Mn2 Cl23 . . . 96.71(16) ? Cl21 Mn2 O21 . . . 1.8(6) ? Cl21 Mn2 O22 . . . 172.6(5) ? Cl21 Mn2 O1 . . . 86.7(2) ? Cl21 Mn2 N0' . . '1 545' 92.1(2) ? Cl21 Mn2 O1' . . '1 545' 85.1(2) ? Cl22 Mn2 Cl23 . . . 89.85(15) ? Cl22 Mn2 O21 . . . 171.9(6) ? Cl22 Mn2 O22 . . . 1.0(5) ? Cl22 Mn2 O1 . . . 89.0(2) ? Cl22 Mn2 N0' . . '1 545' 88.1(2) ? Cl22 Mn2 O1' . . '1 545' 88.6(2) ? Cl23 Mn2 O21 . . . 98.2(6) ? Cl23 Mn2 O22 . . . 90.6(4) ? Cl23 Mn2 O1 . . . 110.5(2) ? Cl23 Mn2 N0' . . '1 545' 105.8(2) ? Cl23 Mn2 O1' . . '1 545' 175.0(2) ? O21 Mn2 O22 . . . 171.2(7) ? O21 Mn2 O1 . . . 87.1(6) ? O21 Mn2 N0' . . '1 545' 90.8(6) ? O21 Mn2 O1' . . '1 545' 83.5(6) ? O22 Mn2 O1 . . . 89.4(5) ? O22 Mn2 N0' . . '1 545' 87.3(5) ? O22 Mn2 O1' . . '1 545' 87.8(5) ? O1 Mn2 N0' . . '1 545' 143.5(3) ? O1 Mn2 O1' . . '1 545' 74.1(2) ? N0' Mn2 O1' '1 545' . '1 545' 69.5(2) ? Mn2 Cl21 O21 . . . 10(3) ? Mn2 Cl22 O22 . . . 5(3) ? Mn2 O21 Cl21 . . . 168(4) ? Mn2 O22 Cl22 . . . 174(3) ? Mn1 N0 C01 . . . 105.3(5) ? Mn1 N0 C1 . . . 124.0(5) ? Mn1 N0 H0 . . . 105.0 ? C01 N0 C1 . . . 115.4(7) ? C01 N0 H0 . . . 97.4(6) ? C1 N0 H0 . . . 105.9 ? N0 C01 C02 . . . 111.1(8) ? N0 C01 H01A . . . 108.0 ? N0 C01 H01B . . . 110.3 ? C02 C01 H01A . . . 108.5 ? C02 C01 H01B . . . 110.7 ? H01A C01 H01B . . . 108.2 ? C01 C02 O1 . . . 118.2(9) ? C01 C02 O2 . . . 117.9(9) ? O1 C02 O2 . . . 123.8(8) ? Mn1 O1 Mn2 . . . 105.3(3) ? Mn1 O1 C02 . . . 114.3(5) ? Mn2 O1 C02 . . . 130.7(6) ? N0 C1 C2a . . . 110.5(7) ? N0 C1 C2b . . . 104.1(7) ? N0 C1 C2c . . . 107.5(6) ? C2a C1 C2b . . . 110.4(7) ? C2a C1 C2c . . . 111.7(7) ? C2b C1 C2c . . . 112.4(7) ? C1 C2a N3a . . . 113.9(7) ? C1 C2a H2aA . . . 109.2 ? C1 C2a H2aB . . . 107.5 ? N3a C2a H2aA . . . 109.7 ? N3a C2a H2aB . . . 108.3 ? H2aA C2a H2aB . . . 107.9 ? Co N3a C2a . . . 117.9(5) ? Co N3a C4a . . . 107.1(6) ? Co N3a H3a . . . 107.6 ? C2a N3a C4a . . . 112.2(6) ? C2a N3a H3a . . . 108.2 ? C4a N3a H3a . . . 102.8 ? N3a C4a C4a' . . . 106.6(7) ? N3a C4a H4aA . . . 110.6 ? N3a C4a H4aB . . . 110.6 ? C4a' C4a H4aA . . . 110.1 ? C4a' C4a H4aB . . . 110.8 ? H4aA C4a H4aB . . . 108.2 ? C4a C4a' N3a' . . . 105.9(8) ? C4a C4a' H4a'A . . . 111.8 ? C4a C4a' H4a'B . . . 110.3 ? N3a' C4a' H4a'A . . . 111.3 ? N3a' C4a' H4a'B . . . 110.0 ? H4a'A C4a' H4a'B . . . 107.5 ? Co N3a' C4a' . . . 107.3(6) ? Co N3a' C2a' . . . 118.9(5) ? Co N3a' H3a' . . . 107.3(6) ? C4a' N3a' C2a' . . . 111.2(7) ? C4a' N3a' H3a' . . . 104.2 ? C2a' N3a' H3a' . . . 106.9 ? N3a' C2a' C1' . . . 113.0(7) ? N3a' C2a' H2a'A . . . 109.0 ? N3a' C2a' H2a'B . . . 108.1 ? C1' C2a' H2a'A . . . 110.2 ? C1' C2a' H2a'B . . . 108.8 ? H2a'A C2a' H2a'B . . . 107.6 ? C1 C2b N3b . . . 113.5(7) ? C1 C2b H2bA . . . 108.6 ? C1 C2b H2bB . . . 108.3 ? N3b C2b H2bA . . . 109.0 ? N3b C2b H2bB . . . 108.2 ? H2bA C2b H2bB . . . 109.2 ? Co N3b C2b . . . 118.5(6) ? Co N3b C4b . . . 107.3(5) ? Co N3b H3b . . . 107.5 ? C2b N3b C4b . . . 111.9(7) ? C2b N3b H3b . . . 107.4 ? C4b N3b H3b . . . 103.0 ? N3b C4b C4b' . . . 106.3(7) ? N3b C4b H4bA . . . 109.8 ? N3b C4b H4bB . . . 111.1 ? C4b' C4b H4bA . . . 110.0 ? C4b' C4b H4bB . . . 111.1 ? H4bA C4b H4bB . . . 108.7 ? C4b C4b' N3b' . . . 107.6(8) ? C4b C4b' H4b'A . . . 111.6 ? C4b C4b' H4b'B . . . 110.8 ? N3b' C4b' H4b'A . . . 109.6 ? N3b' C4b' H4b'B . . . 109.6 ? H4b'A C4b' H4b'B . . . 107.6 ? Co N3b' C4b' . . . 106.7(5) ? Co N3b' C2b' . . . 118.5(6) ? Co N3b' H3b' . . . 109.9 ? C4b' N3b' C2b' . . . 111.1(7) ? C4b' N3b' H3b' . . . 110.1 ? C2b' N3b' H3b' . . . 100.4 ? N3b' C2b' C1' . . . 113.1(7) ? N3b' C2b' H2b'A . . . 108.1 ? N3b' C2b' H2b'B . . . 108.6 ? C1' C2b' H2b'A . . . 108.6 ? C1' C2b' H2b'B . . . 108.7 ? H2b'A C2b' H2b'B . . . 109.7 ? C1 C2c N3c . . . 113.5(6) ? C1 C2c H2cA . . . 108.3 ? C1 C2c H2cB . . . 108.2 ? N3c C2c H2cA . . . 108.4 ? N3c C2c H2cB . . . 107.9 ? H2cA C2c H2cB . . . 110.4 ? Co N3c C2c . . . 118.3(5) ? Co N3c C4c . . . 107.9(5) ? Co N3c H3c . . . 107.9 ? C2c N3c C4c . . . 112.8(7) ? C2c N3c H3c . . . 107.4 ? C4c N3c H3c . . . 101.0 ? N3c C4c C4c' . . . 105.1(8) ? N3c C4c H4cA . . . 110.7 ? N3c C4c H4cB . . . 111.4 ? C4c' C4c H4cA . . . 110.1 ? C4c' C4c H4cB . . . 111.0 ? H4cA C4c H4cB . . . 108.5 ? C4c C4c' N3c' . . . 107.6(6) ? C4c C4c' H4c'A . . . 110.0 ? C4c C4c' H4c'B . . . 109.5 ? N3c' C4c' H4c'A . . . 110.7 ? N3c' C4c' H4c'B . . . 110.2 ? H4c'A C4c' H4c'B . . . 109.0 ? Co N3c' C4c' . . . 107.0(5) ? Co N3c' C2c' . . . 119.1(6) ? Co N3c' H3c' . . . 107.2 ? C4c' N3c' C2c' . . . 112.0(6) ? C4c' N3c' H3c' . . . 103.9 ? C2c' N3c' H3c' . . . 106.5 ? N3c' C2c' C1' . . . 113.7(7) ? N3c' C2c' H2c'A . . . 109.2 ? N3c' C2c' H2c'B . . . 108.9 ? C1' C2c' H2c'A . . . 108.1 ? C1' C2c' H2c'B . . . 108.8 ? H2c'A C2c' H2c'B . . . 108.1 ? C2a' C1' C2b' . . . 110.2(7) ? C2a' C1' C2c' . . . 112.0(7) ? C2a' C1' N0' . . . 103.9(6) ? C2b' C1' C2c' . . . 112.0(7) ? C2b' C1' N0' . . . 109.6(7) ? C2c' C1' N0' . . . 108.9(7) ? C1' N0' C01' . . . 115.6(6) ? C1' N0' Mn2 . . '1 565' 122.1(6) ? C01' N0' Mn2 . . '1 565' 104.7(5) ? N0' C01' C02' . . . 111.8(7) ? N0' C01' H01'A . . . 109.4 ? N0' C01' H01'B . . . 109.1 ? C02' C01' H01'A . . . 109.3 ? C02' C01' H01'B . . . 109.9 ? H01'A C01' H01'B . . . 107.2 ? C01' C02' O1' . . . 116.6(7) ? C01' C02' O2' . . . 117.0(8) ? O1' C02' O2' . . . 126.4(8) ? C02' O1' Mn1 . . '1 565' 126.9(5) ? C02' O1' Mn2 . . '1 565' 116.4(6) ? Mn1 O1' Mn2 '1 565' . '1 565' 105.8(3) ? 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 1956 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -24 _reflns_limit_l_max 23 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 12.119 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .127 _refine_ls_wR_factor_all .143 _refine_ls_goodness_of_fit_all 2.362 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END