# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1904 data_global #=============================================================================== # 1. SUBMISSION DETAILS #=============================================================================== _publ_contact_author ; Prof. G. De Munno Dipartimento di Chimica Universit\'a della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; _publ_contact_author_phone '39 984 492068' _publ_contact_author_fax '39 984 492044' _publ_contact_author_email demunno@unical.it _publ_contact_letter ; Dear Sir I am sending the cif file of the paper 9/08901B: "New supramolecular complexes of manganese(II) and cobalt(II) with nucleic bases. Crystal structure of [M(H2O)6(1-Mecyt)6](ClO4)2.H2O, [Co(1-Mecyt)4](ClO4)2 and [M(cyt)2(H2O)4](ClO4)2.2cyt.2H2O [M = CoII, MnII; cyt = cytosine; 1-Mecyt = 1-methylcytosine]" The compounds have been identified in the paper with number 1, 2, 3, 4 and 5. (in this cif file they have been called data_(1), data_(2), data_(3), data_(4) and data_(5)). For further comunications or informations contact me at this E-mail address: demunno@unical.it Yours sincerely Giovanni De Munno ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Dalton Transactions' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST #=============================================================================== _publ_section_title ; New supramolecular complexes of manganese(II) and cobalt(II) with nucleic bases. Crystal structure of [M(H2O)6(1-Mecyt)6](ClO4)2.H2O, [Co(1-Mecyt)4](ClO4)2 and [M(cyt)2(H2O)4](ClO4)2.2cyt.2H2O [M = CoII, MnII; cyt = cytosine; 1-Mecyt = 1-methylcytosine] ; loop_ _publ_author_name _publ_author_address 'Giovanni De Munno' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Marcella Medaglia ' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Donatella Armentano' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Jane Anastassopoulou' ; National Techincal University of Athens, Chemical, Enineering, Radiation Chemistry and Biochemistry 15780 Athens Greece ; 'Theophilos Theophanides' ; National Techincal University of Athens, Chemical, Enineering, Radiation Chemistry and Biochemistry 15780 Athens Greece ; #=============================================================================== # 4. TEXT #=============================================================================== _publ_section_abstract ; ? ; _publ_section_experimental ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #============================================================================== # 5. CHEMICAL DATA #============================================================================== #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, put the structure code in the "data_?" # line below, using a unique identifier. data_(1) #=============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Mn(H2O)6(1-Mecyt)6](ClO4)2.H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H56 Cl2 Mn N18 O21' _chemical_formula_weight 1130.8 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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 Carbon 0 60 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 112 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 36 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 42 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 4 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Mn Manganese 0 2 0.2950 0.7290 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/m 1' 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 7.511(2) _cell_length_b 32.346(6) _cell_length_c 10.526(3) _cell_length_alpha 90. _cell_length_beta 104.78(2) _cell_length_gamma 90. _cell_volume 2472.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour colorless _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_F_000 1178 _exptl_absorpt_coefficient_mu 4.68 _exptl_absorpt_correction_type ? #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_number 5622 _reflns_number_total 4886 _reflns_number_observed 2234 _reflns_observed_criterion >2\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0008*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2234 _refine_ls_number_parameters 346 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 11.58 _refine_ls_R_factor_obs 5.53 _refine_ls_wR_factor_all 7.37 _refine_ls_wR_factor_obs 6.33 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.40 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -0.32 _refine_diff_density_max 0.37 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Mn1 1.00 0. 0. 0. 0.0821(7) Uani Mn ? ? ? O3 1.00 0.1144(7) -0.0452(1) 0.1526(3) 0.069(2) Uani O ? ? ? O4 1.00 0.2357(9) 0.0409(1) 0.0778(6) 0.129(3) Uani O ? ? ? O5 1.00 -0.1504(8) 0.0276(1) 0.1241(4) 0.103(2) Uani O ? ? ? N1 1.00 0.2539(6) 0.0316(1) 0.5657(4) 0.049(2) Uani N ? ? ? C1 1.00 0.2156(9) 0.0742(2) 0.5982(6) 0.070(3) Uani C ? ? ? C2 1.00 0.1642(8) 0.0160(2) 0.4444(5) 0.046(2) Uani C ? ? ? O2 1.00 0.0527(5) 0.0388(1) 0.3675(3) 0.057(1) Uani O ? ? ? N3 1.00 0.2003(6) -0.0228(1) 0.4119(4) 0.044(2) Uani N ? ? ? C4 1.00 0.3185(8) -0.0468(2) 0.4981(5) 0.046(2) Uani C ? ? ? N4 1.00 0.3473(7) -0.0849(1) 0.4625(5) 0.062(2) Uani N ? ? ? C5 1.00 0.4118(8) -0.0314(2) 0.6241(5) 0.054(2) Uani C ? ? ? C6 1.00 0.3735(8) 0.0072(2) 0.6520(5) 0.058(2) Uani C ? ? ? N11 1.00 0.2631(7) 0.1839(1) 0.2530(5) 0.063(2) Uani N ? ? ? C11 1.00 0.333(1) 0.2025(2) 0.3807(7) 0.096(3) Uani C ? ? ? C21 1.00 0.2900(9) 0.1416(2) 0.2385(6) 0.058(2) Uani C ? ? ? O21 1.00 0.3717(7) 0.1211(1) 0.3345(4) 0.080(2) Uani O ? ? ? N31 1.00 0.2210(7) 0.1242(1) 0.1180(5) 0.062(2) Uani N ? ? ? C41 1.00 0.1366(9) 0.1477(2) 0.0169(6) 0.065(3) Uani C ? ? ? N41 1.00 0.0693(8) 0.1290(2) -0.0982(5) 0.092(3) Uani N ? ? ? C51 1.00 0.1139(9) 0.1906(2) 0.0282(7) 0.072(3) Uani C ? ? ? C61 1.00 0.1792(9) 0.2070(2) 0.1468(8) 0.074(3) Uani C ? ? ? N12 1.00 0.4317(6) -0.1591(1) 0.0553(5) 0.057(2) Uani N ? ? ? C12 1.00 0.5334(9) -0.1713(2) 0.1890(6) 0.079(3) Uani C ? ? ? C22 1.00 0.3644(9) -0.1194(2) 0.0334(6) 0.067(3) Uani C ? ? ? O22 1.00 0.3938(7) -0.0947(1) 0.1285(4) 0.095(2) Uani O ? ? ? N32 1.00 0.2644(7) -0.1080(1) -0.0876(5) 0.063(2) Uani N ? ? ? C42 1.00 0.2303(8) -0.1356(2) -0.1851(6) 0.054(2) Uani C ? ? ? N42 1.00 0.1270(7) -0.1233(1) -0.3015(4) 0.064(2) Uani N ? ? ? C52 1.00 0.3060(8) -0.1759(2) -0.1668(6) 0.058(2) Uani C ? ? ? C62 1.00 0.4001(8) -0.1863(2) -0.0456(6) 0.060(3) Uani C ? ? ? Cl1 1.00 0.0659(3) -0.19630(4) -0.6021(1) 0.0607(6) Uani Cl ? ? ? O6 1.00 0.1459(9) -0.2147(2) -0.4821(5) 0.125(3) Uani O ? ? ? O7 1.00 0.200(1) -0.1867(2) -0.6676(9) 0.210(5) Uani O ? ? ? O8 1.00 -0.0507(9) -0.2241(1) -0.6826(5) 0.127(3) Uani O ? ? ? O9 1.00 -0.0236(8) -0.1598(1) -0.5874(6) 0.128(3) Uani O ? ? ? O10 1.00 0.5 0. 0. 0.258(9) Uani O ? ? ? H41B 1.00 0.0793(8) 0.1011(2) -0.1057(5) 0.06 iso H ? N41 ? H4A 1.00 0.4239(7) -0.1014(1) 0.5201(5) 0.06 iso H ? N4 ? H51 1.00 0.0597(9) 0.2080(2) -0.0463(7) 0.06 iso H ? C51 ? H4B 1.00 0.2925(7) -0.0946(1) 0.3814(5) 0.06 iso H ? N4 ? H61 1.00 0.1652(9) 0.2364(2) 0.1606(8) 0.06 iso H ? C61 ? H3W 1.00 0.272(6) 0.0692(5) 0.075(5) 0.06 iso H ? O4 ? H5 1.00 0.4943(8) -0.0492(2) 0.6841(5) 0.06 iso H ? C5 ? H12A 1.00 0.5410(9) -0.1480(2) 0.2486(6) 0.06 iso H ? C12 ? H12B 1.00 0.4781(9) -0.1946(2) 0.2223(6) 0.06 iso H ? C12 ? H12C 1.00 0.6519(9) -0.1791(2) 0.1825(6) 0.06 iso H ? C12 ? H1A 1.00 0.2861(9) 0.0805(2) 0.6859(6) 0.06 iso H ? C1 ? H6 1.00 0.4351(8) 0.0184(2) 0.7368(5) 0.06 iso H ? C6 ? H1B 1.00 0.2408(9) 0.0944(2) 0.5365(6) 0.06 iso H ? C1 ? H1C 1.00 0.0904(9) 0.0753(2) 0.5976(6) 0.06 iso H ? C1 ? H11A 1.00 0.308(1) 0.2320(2) 0.3780(7) 0.06 iso H ? C11 ? H42A 1.00 0.1046(7) -0.1412(1) -0.3707(4) 0.06 iso H ? N42 ? H42B 1.00 0.0792(7) -0.0974(1) -0.3110(4) 0.06 iso H ? N42 ? H11B 1.00 0.281(1) 0.1893(2) 0.4453(7) 0.06 iso H ? C11 ? H52 1.00 0.2885(8) -0.1953(2) -0.2395(6) 0.06 iso H ? C52 ? H11C 1.00 0.461(1) 0.1984(2) 0.4049(7) 0.06 iso H ? C11 ? H62 1.00 0.4500(8) -0.2139(2) -0.0297(6) 0.06 iso H ? C62 ? H4W 1.00 0.349(4) 0.028(1) 0.078(6) 0.06 iso H ? O4 ? H2W 1.00 0.147(6) -0.039(1) 0.244(1) 0.06 iso H ? O3 ? H5W 1.00 -0.207(6) 0.0543(7) 0.110(4) 0.06 iso H ? O5 ? H6W 1.00 -0.075(6) 0.031(1) 0.212(2) 0.06 iso H ? O5 ? H1W 1.00 0.223(4) -0.059(1) 0.144(4) 0.06 iso H ? O3 ? H41A 1.00 0.0154(8) 0.1444(2) -0.1696(5) 0.06 iso H ? N41 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Mn1 0.162(2) 0.0412(7) 0.0297(6) -0.0051(6) -0.0031(8) 0.0293(9) Mn O3 0.114(4) 0.050(2) 0.032(2) -0.001(2) 0.003(2) 0.026(2) O O4 0.178(6) 0.049(3) 0.129(4) -0.017(3) -0.063(5) 0.029(3) O O5 0.195(6) 0.056(3) 0.043(2) -0.008(2) 0.005(3) 0.045(3) O N1 0.047(3) 0.052(3) 0.042(3) -0.011(2) 0.006(2) -0.005(2) N C1 0.068(5) 0.066(4) 0.067(4) -0.025(3) 0.012(4) -0.010(4) C C2 0.045(4) 0.054(3) 0.034(3) -0.000(3) 0.012(3) -0.004(3) C O2 0.063(3) 0.054(2) 0.045(2) 0.004(2) 0.001(2) 0.012(2) O N3 0.049(3) 0.045(3) 0.034(2) -0.001(2) 0.008(2) 0.002(2) N C4 0.044(4) 0.047(3) 0.044(3) -0.000(3) 0.013(3) 0.002(3) C N4 0.069(4) 0.057(3) 0.052(3) -0.003(2) -0.000(3) 0.014(3) N C5 0.048(4) 0.069(4) 0.037(3) -0.002(3) -0.000(3) 0.009(3) C C6 0.054(4) 0.079(5) 0.034(3) -0.008(3) -0.000(3) -0.002(4) C N11 0.068(4) 0.041(3) 0.073(3) -0.007(3) 0.017(3) -0.007(3) N C11 0.106(6) 0.071(5) 0.100(6) -0.018(4) 0.027(5) -0.016(4) C C21 0.051(4) 0.049(3) 0.066(4) -0.002(3) 0.016(3) -0.005(3) C O21 0.087(4) 0.072(3) 0.070(3) 0.015(2) -0.004(3) 0.010(3) O N31 0.077(4) 0.040(3) 0.060(3) 0.005(2) 0.015(3) -0.007(3) N C41 0.069(5) 0.054(4) 0.064(4) 0.010(3) 0.011(4) -0.012(4) C N41 0.136(6) 0.070(4) 0.057(3) 0.008(3) -0.001(4) -0.019(4) N C51 0.073(5) 0.050(4) 0.082(5) 0.018(3) 0.002(4) -0.006(4) C C61 0.070(5) 0.036(3) 0.108(6) 0.008(4) 0.025(5) 0.001(3) C N12 0.053(3) 0.053(3) 0.057(3) -0.004(2) 0.002(3) 0.016(3) N C12 0.074(5) 0.086(5) 0.065(4) 0.007(4) -0.006(4) 0.025(4) C C22 0.066(5) 0.066(4) 0.058(4) -0.020(3) -0.006(4) 0.018(4) C O22 0.114(4) 0.086(3) 0.068(3) -0.038(3) -0.031(3) 0.045(3) O N32 0.078(4) 0.048(3) 0.053(3) -0.014(2) -0.006(3) 0.012(3) N C42 0.046(4) 0.057(4) 0.052(4) -0.009(3) 0.007(3) 0.002(3) C N42 0.080(4) 0.060(3) 0.045(3) -0.011(2) 0.005(3) 0.010(3) N C52 0.064(4) 0.046(3) 0.058(4) -0.014(3) 0.011(4) 0.004(3) C C62 0.054(4) 0.047(3) 0.072(4) -0.001(3) 0.018(4) 0.003(3) C Cl1 0.078(1) 0.0463(8) 0.0494(9) -0.0026(7) 0.0040(9) 0.0069(9) Cl O6 0.187(6) 0.109(4) 0.058(3) 0.012(3) -0.030(4) 0.021(4) O O7 0.190(7) 0.191(7) 0.240(9) 0.033(6) 0.145(8) -0.010(6) O O8 0.178(6) 0.068(3) 0.107(4) -0.019(3) -0.057(4) -0.004(3) O O9 0.153(5) 0.075(3) 0.134(5) -0.037(3) -0.016(4) 0.055(3) O O10 0.19(1) 0.34(2) 0.23(1) -0.10(1) 0.09(1) -0.02(1) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Mn1 O3 2.180(3) . . . Mn1 O4 2.195(6) . . . Mn1 O5 2.129(6) . . . N1 C1 1.465(7) . . . N1 C2 1.379(6) . . . N1 C6 1.357(7) . . . C2 O2 1.248(6) . . . C2 N3 1.346(7) . . . N3 C4 1.342(6) . . . C4 N4 1.322(7) . . . C4 C5 1.422(7) . . . C5 C6 1.330(9) . . . N11 C11 1.445(8) . . . N11 C21 1.397(7) . . . N11 C61 1.358(8) . . . C21 O21 1.235(7) . . . C21 N31 1.363(8) . . . N31 C41 1.328(7) . . . C41 N41 1.332(8) . . . C41 C51 1.409(9) . . . C51 C61 1.33(1) . . . N12 C12 1.474(7) . . . N12 C22 1.377(8) . . . N12 C62 1.352(8) . . . C22 O22 1.257(8) . . . C22 N32 1.355(7) . . . N32 C42 1.334(7) . . . C42 N42 1.332(7) . . . C42 C52 1.416(8) . . . C52 C62 1.334(8) . . . Cl1 O6 1.387(5) . . . Cl1 O7 1.39(1) . . . Cl1 O8 1.384(5) . . . Cl1 O9 1.388(5) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # O3 Mn1 O4 90.0(2) . . . O3 Mn1 O5 90.0(1) . . . O4 Mn1 O5 91.2(2) . . . O3 Mn1 O4 90.0(2) . . 3_555. O3 Mn1 O5 90.0(1) . . 3_555 O4 Mn1 O5 88.8(2) . . 3_555 C2 N1 C6 119.3(4) . . . C1 N1 C6 121.8(5) . . . C1 N1 C2 118.9(4) . . . N1 C2 N3 119.7(5) . . . N1 C2 O2 118.1(5) . . . O2 C2 N3 122.2(5) . . . C2 N3 C4 120.5(5) . . . N3 C4 C5 120.8(5) . . . N3 C4 N4 118.4(5) . . . N4 C4 C5 120.9(5) . . . C4 C5 C6 116.9(5) . . . N1 C6 C5 122.8(5) . . . C21 N11 C61 119.8(5) . . . C11 N11 C61 121.3(6) . . . C11 N11 C21 118.8(5) . . . N11 C21 N31 118.3(5) . . . N11 C21 O21 119.6(5) . . . O21 C21 N31 122.1(6) . . . C21 N31 C41 120.0(5) . . . N31 C41 C51 122.6(5) . . . N31 C41 N41 117.6(6) . . . N41 C41 C51 119.8(6) . . . C41 C51 C61 116.6(6) . . . N11 C61 C51 122.5(7) . . . C22 N12 C62 119.4(5) . . . C12 N12 C62 121.4(5) . . . C12 N12 C22 119.2(5) . . . N12 C22 N32 120.2(5) . . . N12 C22 O22 118.5(5) . . . O22 C22 N32 121.2(5) . . . C22 N32 C42 119.5(5) . . . N32 C42 C52 121.3(5) . . . N32 C42 N42 117.4(5) . . . N42 C42 C52 121.3(5) . . . C42 C52 C62 117.3(5) . . . N12 C62 C52 122.1(6) . . . O8 Cl1 O9 111.9(3) . . . O7 Cl1 O9 107.3(4) . . . O7 Cl1 O8 105.4(4) . . . O6 Cl1 O9 112.0(3) . . . O6 Cl1 O8 109.7(3) . . . O6 Cl1 O7 110.3(4) . . . #=============================================================================== #=============================================================================== data_(2) #============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(H2O)6(1-Mecyt)6](ClO4)2.H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H56 Cl2 Co N18 O21' _chemical_formula_weight 1134.8 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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 Carbon 0 60 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 112 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 36 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 42 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 4 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Co Cobalt 0 2 0.2990 0.9730 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/m 1' 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 7.674(3) _cell_length_b 31.939(6) _cell_length_c 10.363(2) _cell_length_alpha 90. _cell_length_beta 103.96(2) _cell_length_gamma 90. _cell_volume 2464.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour 'pale pink' _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 5.50 _exptl_absorpt_correction_type ? #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_number 5662 _reflns_number_total 4872 _reflns_number_observed 2718 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0010*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2718 _refine_ls_number_parameters 346 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 9.32 _refine_ls_R_factor_obs 4.92 _refine_ls_wR_factor_all 7.75 _refine_ls_wR_factor_obs 6.41 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.41 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -0.36 _refine_diff_density_max 0.43 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Co1 1.00 0. 0. 0. 0.0451(3) Uani Co ? ? ? O3 1.00 0.1114(4) -0.04465(9) 0.1446(3) 0.053(1) Uani O ? ? ? O4 1.00 0.2186(5) 0.0388(1) 0.0788(4) 0.074(1) Uani O ? ? ? O5 1.00 -0.1411(5) 0.0258(1) 0.1276(3) 0.059(1) Uani O ? ? ? N1 1.00 0.2509(5) 0.0311(1) 0.5688(3) 0.047(1) Uani N ? ? ? C1 1.00 0.2091(7) 0.0735(1) 0.6072(5) 0.063(2) Uani C ? ? ? C2 1.00 0.1633(6) 0.0161(1) 0.4449(4) 0.045(1) Uani C ? ? ? O2 1.00 0.0492(4) 0.0390(1) 0.3721(3) 0.056(1) Uani O ? ? ? N3 1.00 0.2025(5) -0.0227(1) 0.4082(3) 0.042(1) Uani N ? ? ? C4 1.00 0.3208(6) -0.0465(1) 0.4921(4) 0.044(2) Uani C ? ? ? N4 1.00 0.3536(6) -0.0844(1) 0.4522(4) 0.059(1) Uani N ? ? ? C5 1.00 0.4103(6) -0.0321(2) 0.6197(4) 0.050(2) Uani C ? ? ? C6 1.00 0.3715(6) 0.0063(2) 0.6530(4) 0.054(2) Uani C ? ? ? N11 1.00 0.2596(5) 0.1831(1) 0.2682(4) 0.058(1) Uani N ? ? ? C11 1.00 0.3347(8) 0.2016(2) 0.3977(6) 0.088(3) Uani C ? ? ? C21 1.00 0.2834(6) 0.1403(2) 0.2512(5) 0.057(2) Uani C ? ? ? O21 1.00 0.3643(5) 0.1194(1) 0.3464(3) 0.075(1) Uani O ? ? ? N31 1.00 0.2127(5) 0.1232(1) 0.1304(4) 0.056(1) Uani N ? ? ? C41 1.00 0.1273(7) 0.1475(2) 0.0295(5) 0.060(2) Uani C ? ? ? N41 1.00 0.0603(6) 0.1289(2) -0.0869(4) 0.082(2) Uani N ? ? ? C51 1.00 0.1101(8) 0.1905(2) 0.0439(6) 0.072(2) Uani C ? ? ? C61 1.00 0.1759(7) 0.2071(2) 0.1642(6) 0.074(2) Uani C ? ? ? N12 1.00 0.4398(5) -0.1570(1) 0.0484(4) 0.052(1) Uani N ? ? ? C12 1.00 0.5452(7) -0.1689(2) 0.1803(5) 0.072(2) Uani C ? ? ? C22 1.00 0.3684(7) -0.1175(2) 0.0282(5) 0.057(2) Uani C ? ? ? O22 1.00 0.3968(5) -0.0923(1) 0.1224(3) 0.081(2) Uani O ? ? ? N32 1.00 0.2667(5) -0.1066(1) -0.0933(4) 0.056(1) Uani N ? ? ? C42 1.00 0.2371(6) -0.1343(1) -0.1922(4) 0.049(2) Uani C ? ? ? N42 1.00 0.1318(6) -0.1230(1) -0.3088(4) 0.064(2) Uani N ? ? ? C52 1.00 0.3124(7) -0.1748(1) -0.1750(5) 0.056(2) Uani C ? ? ? C62 1.00 0.4114(7) -0.1849(1) -0.0546(5) 0.059(2) Uani C ? ? ? Cl1 1.00 0.0720(2) -0.19652(4) -0.6127(1) 0.0578(5) Uani Cl ? ? ? O6 1.00 0.1502(8) -0.2150(1) -0.4917(4) 0.121(2) Uani O ? ? ? O7 1.00 0.2003(8) -0.1868(2) -0.6823(7) 0.185(3) Uani O ? ? ? O8 1.00 -0.0441(7) -0.2249(1) -0.6926(5) 0.119(2) Uani O ? ? ? O9 1.00 -0.0165(7) -0.1593(1) -0.5961(5) 0.115(2) Uani O ? ? ? O10 1.00 0.5 0. 0. 0.133(4) Uani O ? ? ? H41B 1.00 0.0703(6) 0.1010(2) -0.0944(4) 0.06 Uiso H ? N41 ? H4A 1.00 0.4302(6) -0.1009(1) 0.5097(4) 0.06 Uiso H ? N4 ? H51 1.00 0.0559(8) 0.2079(2) -0.0306(6) 0.06 Uiso H ? C51 ? H4B 1.00 0.2987(6) -0.0941(1) 0.3711(4) 0.06 Uiso H ? N4 ? H61 1.00 0.1619(7) 0.2365(2) 0.1780(6) 0.06 Uiso H ? C61 ? H3W 1.00 0.230(5) 0.0666(6) 0.112(4) 0.06 Uiso H ? O4 ? H5 1.00 0.4928(6) -0.0500(2) 0.6798(4) 0.06 Uiso H ? C5 ? H12A 1.00 0.5528(7) -0.1456(2) 0.2399(5) 0.06 Uiso H ? C12 ? H12B 1.00 0.4899(7) -0.1921(2) 0.2136(5) 0.06 Uiso H ? C12 ? H12C 1.00 0.6636(7) -0.1766(2) 0.1739(5) 0.06 Uiso H ? C12 ? H1A 1.00 0.2796(7) 0.0798(1) 0.6949(5) 0.06 Uiso H ? C1 ? H6 1.00 0.4332(6) 0.0175(2) 0.7377(4) 0.06 Uiso H ? C6 ? H1B 1.00 0.2343(7) 0.0937(1) 0.5454(5) 0.06 Uiso H ? C1 ? H1C 1.00 0.0839(7) 0.0746(1) 0.6066(5) 0.06 Uiso H ? C1 ? H11A 1.00 0.3088(8) 0.2310(2) 0.3950(6) 0.06 Uiso H ? C11 ? H42A 1.00 0.1093(6) -0.1408(1) -0.3780(4) 0.06 Uiso H ? N42 ? H42B 1.00 0.0840(6) -0.0971(1) -0.3183(4) 0.06 Uiso H ? N42 ? H11B 1.00 0.2818(8) 0.1883(2) 0.4622(6) 0.06 Uiso H ? C11 ? H52 1.00 0.2950(7) -0.1942(1) -0.2477(5) 0.06 Uiso H ? C52 ? H11C 1.00 0.4624(8) 0.1974(2) 0.4219(6) 0.06 Uiso H ? C11 ? H62 1.00 0.4613(7) -0.2125(1) -0.0388(5) 0.06 Uiso H ? C62 ? H4W 1.00 0.326(3) 0.031(1) 0.054(4) 0.06 Uiso H ? O4 ? H2W 1.00 0.157(5) -0.033(1) 0.232(2) 0.06 Uiso H ? O3 ? H5W 1.00 -0.183(5) 0.0539(5) 0.111(4) 0.06 Uiso H ? O5 ? H6W 1.00 -0.058(5) 0.028(1) 0.212(2) 0.06 Uiso H ? O5 ? H1W 1.00 0.214(3) -0.060(1) 0.134(4) 0.06 Uiso H ? O3 ? H41A 1.00 0.0064(6) 0.1442(2) -0.1583(4) 0.06 Uiso H ? N41 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Co1 0.0600(6) 0.0384(5) 0.0316(4) -0.0056(4) 0.0029(4) 0.0106(4) Co O3 0.072(2) 0.048(2) 0.034(2) -0.003(1) 0.003(2) 0.018(2) O O4 0.068(3) 0.046(2) 0.097(3) -0.018(2) -0.005(2) 0.006(2) O O5 0.083(2) 0.050(2) 0.038(2) -0.007(1) 0.008(2) 0.022(2) O N1 0.047(2) 0.048(2) 0.040(2) -0.010(2) 0.006(2) -0.002(2) N C1 0.060(3) 0.057(3) 0.064(3) -0.019(3) 0.008(3) -0.001(3) C C2 0.043(3) 0.053(3) 0.036(2) 0.002(2) 0.013(2) -0.001(2) C O2 0.063(2) 0.058(2) 0.041(2) 0.001(1) 0.003(2) 0.012(2) O N3 0.045(2) 0.045(2) 0.033(2) -0.003(2) 0.007(2) 0.004(2) N C4 0.041(3) 0.051(3) 0.038(2) 0.003(2) 0.012(2) 0.002(2) C N4 0.067(3) 0.055(3) 0.048(2) -0.005(2) -0.002(2) 0.008(2) N C5 0.051(3) 0.056(3) 0.038(2) 0.002(2) -0.000(2) 0.003(2) C C6 0.049(3) 0.068(3) 0.040(2) -0.008(2) 0.000(2) -0.000(3) C N11 0.060(3) 0.042(2) 0.066(3) -0.005(2) 0.012(2) -0.006(2) N C11 0.101(5) 0.069(4) 0.086(4) -0.020(3) 0.024(4) -0.017(4) C C21 0.050(3) 0.051(3) 0.063(3) 0.003(3) 0.015(3) -0.003(2) C O21 0.083(3) 0.069(2) 0.065(2) 0.012(2) -0.000(2) 0.013(2) O N31 0.064(3) 0.042(2) 0.055(2) 0.004(2) 0.012(2) -0.000(2) N C41 0.058(3) 0.054(3) 0.061(3) 0.008(3) 0.008(3) -0.011(3) C N41 0.115(4) 0.068(3) 0.054(3) 0.010(2) 0.000(3) -0.021(3) N C51 0.077(4) 0.045(3) 0.084(4) 0.015(3) 0.003(3) -0.002(3) C C61 0.068(4) 0.037(3) 0.108(5) 0.005(3) 0.023(3) 0.006(3) C N12 0.052(2) 0.045(2) 0.052(2) -0.004(2) 0.005(2) 0.013(2) N C12 0.073(4) 0.072(4) 0.064(3) 0.006(3) 0.006(3) 0.024(3) C C22 0.054(3) 0.059(3) 0.051(3) -0.013(2) 0.001(2) 0.017(2) C O22 0.093(3) 0.076(3) 0.062(2) -0.030(2) -0.019(2) 0.041(2) O N32 0.066(3) 0.045(2) 0.050(2) -0.011(2) 0.003(2) 0.012(2) N C42 0.052(3) 0.045(3) 0.046(3) -0.005(2) 0.009(2) 0.003(2) C N42 0.078(3) 0.063(3) 0.043(2) -0.013(2) 0.006(2) 0.013(2) N C52 0.065(3) 0.045(3) 0.052(3) -0.015(2) 0.012(2) 0.004(2) C C62 0.057(3) 0.040(3) 0.074(3) -0.007(2) 0.022(3) 0.004(2) C Cl1 0.0749(9) 0.0432(7) 0.0486(7) -0.0025(5) 0.0071(6) 0.0062(6) Cl O6 0.186(5) 0.097(3) 0.060(3) 0.009(2) -0.027(3) 0.027(3) O O7 0.166(6) 0.169(6) 0.212(6) 0.030(5) 0.129(5) 0.004(5) O O8 0.165(5) 0.071(3) 0.098(3) -0.012(2) -0.039(3) -0.013(3) O O9 0.141(4) 0.069(3) 0.120(4) -0.027(3) -0.005(3) 0.040(3) O O10 0.069(4) 0.222(8) 0.102(5) -0.064(5) 0.026(4) -0.018(5) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Co1 O3 2.096(3) . . . Co1 O4 2.088(3) . . . Co1 O5 2.071(4) . . . N1 C1 1.469(6) . . . N1 C2 1.383(5) . . . N1 C6 1.363(5) . . . C2 O2 1.246(5) . . . C2 N3 1.350(6) . . . N3 C4 1.334(5) . . . C4 N4 1.322(6) . . . C4 C5 1.412(6) . . . N4 H4A 0.900(5) . . . N4 H4B 0.900(5) . . . C5 C6 1.328(7) . . . N11 C11 1.452(7) . . . N11 C21 1.395(6) . . . N11 C61 1.353(7) . . . C21 O21 1.229(6) . . . C21 N31 1.354(6) . . . N31 C41 1.340(6) . . . C41 N41 1.332(6) . . . C41 C51 1.393(7) . . . C51 C61 1.336(8) . . . N12 C12 1.461(6) . . . N12 C22 1.371(6) . . . N12 C62 1.368(6) . . . C22 O22 1.243(6) . . . C22 N32 1.357(6) . . . N32 C42 1.331(6) . . . C42 N42 1.332(5) . . . C42 C52 1.409(6) . . . C52 C62 1.334(6) . . . Cl1 O6 1.385(4) . . . Cl1 O7 1.389(7) . . . Cl1 O8 1.395(4) . . . Cl1 O9 1.399(5) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # O3 Co1 O4 88.5(1) . . . O3 Co1 O5 90.0(1) . . . O4 Co1 O5 90.5(1) . . . O3 Co1 O4 91.5(1) . . 3_555 O3 Co1 O5 90.0(1) . . 3_555 O4 Co1 O5 89.5(1) . . 3_555 C2 N1 C6 119.7(4) . . . C1 N1 C6 121.4(4) . . . C1 N1 C2 118.9(4) . . . N1 C2 N3 119.2(4) . . . N1 C2 O2 118.1(4) . . . O2 C2 N3 122.7(4) . . . C2 N3 C4 120.2(4) . . . N3 C4 C5 121.7(4) . . . N3 C4 N4 118.0(4) . . . N4 C4 C5 120.3(4) . . . C4 C5 C6 117.1(4) . . . N1 C6 C5 122.1(4) . . . C21 N11 C61 120.5(4) . . . C11 N11 C61 120.8(4) . . . C11 N11 C21 118.7(4) . . . N11 C21 N31 118.5(4) . . . N11 C21 O21 119.2(4) . . . O21 C21 N31 122.4(5) . . . C21 N31 C41 120.0(4) . . . N31 C41 C51 121.9(4) . . . N31 C41 N41 117.3(4) . . . N41 C41 C51 120.8(5) . . . C41 C51 C61 117.9(5) . . . N11 C61 C51 121.2(6) . . . C22 N12 C62 119.9(4) . . . C12 N12 C62 120.6(4) . . . C12 N12 C22 119.5(4) . . . N12 C22 N32 119.7(4) . . . N12 C22 O22 119.2(4) . . . O22 C22 N32 121.1(4) . . . C22 N32 C42 119.9(4) . . . N32 C42 C52 121.5(4) . . . N32 C42 N42 118.1(4) . . . N42 C42 C52 120.4(4) . . . C42 C52 C62 117.7(4) . . . N12 C62 C52 121.3(5) . . . O8 Cl1 O9 111.5(2) . . . O7 Cl1 O9 107.5(4) . . . O7 Cl1 O8 105.6(4) . . . O6 Cl1 O9 111.6(3) . . . O6 Cl1 O8 109.6(3) . . . O6 Cl1 O7 111.1(3) . . . #=============================================================================== #=============================================================================== #=============================================================================== data_(3) #============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(1-Mecyt)4](ClO4)2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H28 Cl2 Co N12 O12' _chemical_formula_weight 758.4 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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 Carbon 0 20 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 28 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 12 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 12 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 2 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Co Cobalt 0 1 0.2990 0.9730 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I4/m' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2-x,-y,1/2+z' '3/4-y,1/4+x,1/4+z' '3/4+y,3/4-x,3/4+z' '-x,-y,-z' '1/2+x,+y,1/2-z' '1/4+y,3/4-x,3/4-z' '1/4-y,1/4+x,1/4-z' '1/2+x,1/2+y,1/2+z' '1-x,1/2-y,1+z' '5/4-y,3/4+x,3/4+z' '5/4+y,5/4-x,5/4+z' '1/2-x,1/2-y,1/2-z' '1+x,1/2+y,1-z' '3/4+y,5/4-x,5/4-z' '3/4-y,3/4+x,3/4-z' _cell_length_a 13.737(2) _cell_length_b 13.737(2) _cell_length_c 16.131(3) _cell_length_alpha 90. _cell_length_beta 90. _cell_length_gamma 90. _cell_volume 3044.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour 'dark pink' _exptl_crystal_description polyhedral _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.655 _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 8.2000 _exptl_absorpt_correction_type ? #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_number 1967 _reflns_number_total 1676 _reflns_number_observed 1312 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0018*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 1312 _refine_ls_number_parameters 107 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 5.98 _refine_ls_R_factor_obs 4.69 _refine_ls_wR_factor_all 7.96 _refine_ls_wR_factor_obs 6.80 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.29 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.001 _refine_diff_density_min -0.58 _refine_diff_density_max 0.44 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Co1 1.00 0.5 0.25 0.375 0.0232(2) Uani Co ? ? ? N1 1.00 0.7047(2) 0.2449(2) 0.5635(2) 0.0463(9) Uani N ? ? ? C1 1.00 0.7492(4) 0.3258(3) 0.6082(3) 0.073(2) Uani C ? ? ? C2 1.00 0.6400(2) 0.2654(2) 0.5011(2) 0.0300(8) Uani C ? ? ? O2 1.00 0.6188(2) 0.3500(1) 0.4820(1) 0.0375(7) Uani O ? ? ? N3 1.00 0.6004(2) 0.1903(2) 0.4567(1) 0.0264(6) Uani N ? ? ? C4 1.00 0.6204(2) 0.0974(2) 0.4773(2) 0.0321(8) Uani C ? ? ? N4 1.00 0.5802(2) 0.0261(2) 0.4342(2) 0.0459(9) Uani N ? ? ? C5 1.00 0.6842(3) 0.0765(3) 0.5441(2) 0.052(1) Uani C ? ? ? C6 1.00 0.7235(3) 0.1515(3) 0.5844(3) 0.061(2) Uani C ? ? ? Cl1 1.00 0.5 0.25 0.7132(1) 0.0984(9) Uani Cl ? ? ? O3 1.00 0.5830(5) 0.2424(7) 0.7585(3) 0.194(4) Uani O ? ? ? O4 1.00 0.5070(5) 0.3234(7) 0.6548(5) 0.216(4) Uani O ? ? ? H1C 1.00 0.6999(4) 0.3653(3) 0.6337(3) 0.06 Uiso H ? C1 ? H5 1.00 0.6980(3) 0.0105(3) 0.5597(2) 0.06 Uiso H ? C5 ? H1A 1.00 0.7921(4) 0.3009(3) 0.6501(3) 0.06 Uiso H ? C1 ? H6 1.00 0.7666(3) 0.1391(3) 0.6300(3) 0.06 Uiso H ? C6 ? H1B 1.00 0.7857(4) 0.3645(3) 0.5696(3) 0.06 Uiso H ? C1 ? H4B 1.00 0.5925(2) -0.0364(2) 0.4472(2) 0.06 Uiso H ? N4 ? H4A 1.00 0.5403(2) 0.0404(2) 0.3916(2) 0.06 Uiso H ? N4 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Co1 0.0222(3) 0.0222(3) 0.0252(4) 0. 0. 0. Co N1 0.048(2) 0.036(1) 0.056(2) -0.005(1) -0.026(1) 0.003(1) N C1 0.083(3) 0.057(3) 0.080(3) -0.010(2) -0.049(3) -0.013(2) C C2 0.033(1) 0.027(1) 0.031(1) -0.000(1) -0.005(1) 0.001(1) C O2 0.052(1) 0.022(1) 0.038(1) -0.0018(8) -0.008(1) 0.0015(9) O N3 0.033(1) 0.019(1) 0.027(1) -0.0004(8) -0.0021(9) 0.0016(9) N C4 0.037(2) 0.025(1) 0.035(1) 0.004(1) 0.003(1) 0.004(1) C N4 0.075(2) 0.019(1) 0.044(2) 0.003(1) -0.009(1) -0.001(1) N C5 0.062(2) 0.033(2) 0.061(2) 0.008(2) -0.022(2) 0.015(2) C C6 0.065(2) 0.045(2) 0.073(3) 0.001(2) -0.039(2) 0.014(2) C Cl1 0.080(1) 0.164(2) 0.051(1) 0. 0. 0.033(1) Cl O3 0.131(4) 0.35(1) 0.097(4) 0.012(4) -0.049(3) 0.063(6) O O4 0.136(5) 0.31(1) 0.201(6) 0.133(6) -0.012(5) 0.026(7) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_site_symmetry_3 # # Complete list of bond lengths for non-H atoms. # Co1 N3 2.076(2) . . . N1 C1 1.459(5) . . . N1 C2 1.372(4) . . . N1 C6 1.352(5) . . . C2 O2 1.237(3) . . . C2 N3 1.369(3) . . . N3 C4 1.347(3) . . . C4 N4 1.322(4) . . . C4 C5 1.418(5) . . . C5 C6 1.332(5) . . . Cl1 O3 1.359(6) . . . Cl1 O4 1.384(9) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 # # Complete list of bond angles for non-H atoms. # N3 Co1 N3 101.2(1) . . 10_554 N3 Co1 N3 113.7(1) . . 7_555 C1 N1 C2 118.6(3) . . . C1 N1 C6 121.3(3) . . . C2 N1 C6 120.1(3) . . . N1 C2 O2 121.9(3) . . . N1 C2 N3 119.1(2) . . . O2 C2 N3 119.0(3) . . . Co N3 C2 107.3(2) . . . Co N3 C4 131.8(2) . . . C2 N3 C4 120.2(2) . . . N3 C4 N4 119.1(3) . . . N3 C4 C5 120.4(3) . . . N4 C4 C5 120.6(3) . . . C4 C5 C6 117.7(3) . . . N1 C6 C5 122.3(4) . . . O3 Cl1 O4 111.4(4) . . . O3 Cl1 O3 114.9(5) . . . O3 Cl1 O4 111.6(5) . . . O4 Cl1 O4 94.1(7) . . . #=============================================================================== #=============================================================================== data_(4) #============================================================================= _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Mn(cyt)2(H2O)4](ClO4)2.2cyt.2H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H32 Cl2 Mn N12 O18' _chemical_formula_weight 806.4 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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 Carbon 0 16 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 32 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 12 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 18 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 2 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Mn Manganese 0 1 0.2950 0.7290 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 6.829(5) _cell_length_b 9.997(4) _cell_length_c 12.911(5) _cell_length_alpha 71.65(3) _cell_length_beta 87.33(5) _cell_length_gamma 72.19(5) _cell_volume 795.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.71073 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour colorless _exptl_crystal_description needles _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_F_000 415 _exptl_absorpt_coefficient_mu 6.7900 _exptl_absorpt_correction_type ? #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_number 2487 _reflns_number_total 2265 _reflns_number_observed 2258 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0013*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2258 _refine_ls_number_parameters 238 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 6.87 _refine_ls_R_factor_obs 6.86 _refine_ls_wR_factor_all 9.18 _refine_ls_wR_factor_obs 9.17 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.91 _refine_ls_shift/esd_mean 0.003 _refine_ls_shift/esd_max 0.000 _refine_diff_density_min -0.79 _refine_diff_density_max 0.95 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Mn1 1.00 0. 0. 0. 0.0208(4) Uani Mn ? ? ? O3 1.00 0.2485(6) 0.0576(4) -0.0944(3) 0.033(1) Uani O ? ? ? O4 1.00 0.2227(6) -0.1557(4) 0.1367(3) 0.030(1) Uani O ? ? ? N1 1.00 -0.0704(7) -0.0713(5) -0.2451(4) 0.030(2) Uani N ? ? ? C2 1.00 0.0329(8) -0.1908(5) -0.1596(4) 0.025(2) Uani C ? ? ? O2 1.00 0.0345(6) -0.1792(4) -0.0655(3) 0.030(1) Uani O ? ? ? N3 1.00 0.1283(7) -0.3202(5) -0.1769(3) 0.027(2) Uani N ? ? ? C4 1.00 0.1268(9) -0.3301(6) -0.2785(5) 0.036(2) Uani C ? ? ? N4 1.00 0.2251(9) -0.4613(6) -0.2897(5) 0.053(2) Uani N ? ? ? C5 1.00 0.024(1) -0.2060(7) -0.3690(5) 0.040(2) Uani C ? ? ? C6 1.00 -0.074(1) -0.0803(7) -0.3477(5) 0.036(2) Uani C ? ? ? N11 1.00 0.2804(7) -0.5530(5) 0.0171(4) 0.029(2) Uani N ? ? ? C21 1.00 0.3790(8) -0.6920(5) 0.0126(5) 0.025(2) Uani C ? ? ? O21 1.00 0.3909(6) -0.7125(4) -0.0792(3) 0.032(1) Uani O ? ? ? N31 1.00 0.4615(7) -0.8013(5) 0.1055(4) 0.027(2) Uani N ? ? ? C41 1.00 0.4483(8) -0.7708(6) 0.1989(5) 0.031(2) Uani C ? ? ? N41 1.00 0.5362(8) -0.8831(5) 0.2895(4) 0.038(2) Uani N ? ? ? C51 1.00 0.3450(9) -0.6282(6) 0.2072(5) 0.038(2) Uani C ? ? ? C61 1.00 0.2644(9) -0.5227(6) 0.1140(5) 0.033(2) Uani C ? ? ? Cl1 1.00 0.4058(3) -0.7262(2) 0.5531(1) 0.0441(7) Uani Cl ? ? ? O9 1.00 0.103(1) -0.3319(8) 0.3084(6) 0.104(3) Uani O ? ? ? O8 1.00 0.601(2) -0.697(2) 0.524(1) 0.135(5) Uiso O ? ? ? O51 1.00 0.305(3) -0.574(2) 0.509(1) 0.056(5) Uiso O ? ? ? O61 1.00 0.522(3) -0.802(2) 0.492(2) 0.076(5) Uiso O ? ? ? O71 1.00 0.497(3) -0.762(2) 0.659(1) 0.051(4) Uiso O ? ? ? O81 1.00 0.256(5) -0.818(3) 0.582(2) 0.133(9) Uiso O ? ? ? O5 1.00 0.231(2) -0.602(1) 0.5139(9) 0.080(3) Uiso O ? ? ? O6 1.00 0.410(2) -0.838(1) 0.5097(8) 0.069(2) Uiso O ? ? ? O7 1.00 0.395(2) -0.776(1) 0.6669(8) 0.073(3) Uiso O ? ? ? H11 1.00 0.2250(7) -0.4795(5) -0.0449(4) 0.06 Uiso H ? ? ? H2W 1.00 0.380(4) -0.014(5) -0.092(6) 0.06 Uiso H ? ? ? H11 1.00 0.2250(7) -0.4795(5) -0.0449(4) 0.06 Uiso H ? N11 ? H2W 1.00 0.380(4) -0.014(5) -0.092(6) 0.06 Uiso H ? O3 ? H1 1.00 -0.1360(7) 0.0152(5) -0.2330(4) 0.06 Uiso H ? N1 ? H4A 1.00 0.2838(9) -0.5304(6) -0.2252(5) 0.06 Uiso H ? N4 ? H4B 1.00 0.2207(9) -0.4638(6) -0.3504(5) 0.06 Uiso H ? N4 ? H1W 1.00 0.286(9) 0.141(4) -0.092(6) 0.06 Uiso H ? O3 ? H41A 1.00 0.6023(8) -0.9730(5) 0.2836(4) 0.06 Uiso H ? N41 ? H41B 1.00 0.5293(8) -0.8675(5) 0.3549(4) 0.06 Uiso H ? N41 ? H5 1.00 0.026(1) -0.2140(7) -0.4417(5) 0.06 Uiso H ? C5 ? H51 1.00 0.3326(9) -0.6087(6) 0.2763(5) 0.06 Uiso H ? C51 ? H3W 1.00 0.349(6) -0.207(6) 0.111(5) 0.06 Uiso H ? O4 ? H61 1.00 0.1936(9) -0.4240(6) 0.1152(5) 0.06 Uiso H ? C61 ? H6 1.00 -0.148(1) 0.0052(7) -0.4064(5) 0.06 Uiso H ? C6 ? H4W 1.00 0.20(1) -0.236(4) 0.194(4) 0.06 Uiso H ? O4 ? H5W 1.00 0.09(1) -0.251(4) 0.336(5) 0.06 Uiso H ? O9 ? H6W 1.00 0.16(1) -0.412(4) 0.374(3) 0.06 Uiso H ? O9 ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Mn1 0.0211(6) 0.0134(6) 0.0185(6) -0.0081(5) 0.0035(5) -0.0003(5) Mn O3 0.028(2) 0.019(2) 0.036(2) -0.011(2) 0.013(2) -0.005(2) O O4 0.023(2) 0.027(2) 0.026(2) -0.006(2) 0.003(2) 0.002(2) O N1 0.031(3) 0.018(2) 0.029(3) -0.009(2) -0.000(2) 0.005(2) N C2 0.025(3) 0.015(2) 0.024(3) -0.008(2) 0.004(2) -0.004(2) C O2 0.036(2) 0.016(2) 0.024(2) -0.011(2) 0.001(2) -0.003(2) O N3 0.031(3) 0.016(2) 0.021(2) -0.010(2) 0.002(2) -0.005(2) N C4 0.033(3) 0.027(3) 0.028(3) -0.016(2) 0.010(2) -0.008(2) C N4 0.061(4) 0.038(3) 0.034(3) -0.027(3) 0.008(3) -0.004(3) N C5 0.038(3) 0.039(3) 0.024(3) -0.012(3) 0.000(3) -0.005(3) C C6 0.036(3) 0.032(3) 0.025(3) -0.005(2) -0.001(3) 0.000(3) C N11 0.032(3) 0.017(2) 0.026(2) -0.007(2) 0.005(2) -0.002(2) N C21 0.018(3) 0.014(2) 0.033(3) -0.009(2) 0.008(2) -0.003(2) C O21 0.034(2) 0.020(2) 0.027(2) -0.011(2) 0.008(2) -0.003(2) O N31 0.023(2) 0.015(2) 0.031(3) -0.008(2) 0.007(2) 0.000(2) N C41 0.020(3) 0.024(3) 0.034(3) -0.010(2) 0.006(2) -0.007(2) C N41 0.040(3) 0.030(3) 0.028(3) -0.004(2) -0.001(2) -0.001(2) N C51 0.030(3) 0.031(3) 0.034(3) -0.016(3) 0.005(3) -0.006(3) C C61 0.029(3) 0.019(3) 0.036(3) -0.016(2) 0.005(3) -0.001(2) C Cl1 0.056(1) 0.0284(8) 0.0298(8) -0.0118(7) 0.0052(7) 0.0004(7) Cl O9 0.105(6) 0.081(5) 0.085(5) 0.025(4) 0.026(4) -0.029(5) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Mn1 O3 2.158(4) . . . Mn1 O4 2.219(4) . . . Mn1 O2 2.158(4) . . . N1 C2 1.367(6) . . . N1 C6 1.358(9) . . . C2 O2 1.258(7) . . . C2 N3 1.342(7) . . . N3 C4 1.346(8) . . . C4 N4 1.329(8) . . . C4 C5 1.424(7) . . . C5 C6 1.337(9) . . . N11 C21 1.364(7) . . . N11 C61 1.369(8) . . . C21 O21 1.260(8) . . . C21 N31 1.346(6) . . . N31 C41 1.326(8) . . . C41 N41 1.347(6) . . . C41 C51 1.419(8) . . . C51 C61 1.331(7) . . . Cl1 O8 1.46(2) . . . Cl1 O51 1.40(2) . . . Cl1 O61 1.33(2) . . . Cl1 O71 1.42(2) . . . Cl1 O81 1.54(4) . . . Cl1 O5 1.41(1) . . . Cl1 O6 1.40(1) . . . Cl1 O7 1.40(1) . . . O8 O61 1.49(3) . . . O8 O71 1.84(2) . . . O51 O5 0.64(3) . . . O61 O6 0.93(3) . . . O71 O7 0.75(2) . . . O81 O6 1.39(3) . . . O81 O7 1.71(4) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 # # Complete list of bond angles for non-H atoms. # O2 Mn1 O3 90.4(2) . . . O2 Mn1 O4 88.9(2) . . . O3 Mn1 O4 90.4(1) . . . O2 Mn1 O3 89.6(2) . . 2_555 O2 Mn1 O4 91.1(2) . . 2_555 O3 Mn1 O4 89.6(1) . . 2_555 C2 N1 C6 121.1(5) . . . N1 C2 N3 119.4(5) . . . N1 C2 O2 119.8(5) . . . O2 C2 N3 120.7(5) . . . Mn1 O2 C2 135.5(4) . . . C2 N3 C4 119.9(5) . . . N3 C4 C5 121.5(5) . . . N3 C4 N4 116.6(5) . . . N4 C4 C5 121.9(6) . . . C4 C5 C6 116.7(6) . . . N1 C6 C5 121.3(6) . . . C21 N11 C61 121.3(5) . . . N11 C21 N31 119.2(5) . . . N11 C21 O21 118.3(5) . . . O21 C21 N31 122.5(5) . . . C21 N31 C41 119.3(5) . . . N31 C41 C51 123.3(5) . . . N31 C41 N41 117.1(5) . . . N41 C41 C51 119.6(5) . . . C41 C51 C61 116.0(6) . . . N11 C61 C51 121.0(5) . . . O6 Cl1 O7 110.3(6) . . . O5 Cl1 O7 106.1(6) . . . O5 Cl1 O6 112.0(7) . . . O81 Cl1 O7 71(1) . . . O81 Cl1 O6 56(1) . . . O81 Cl1 O5 86(1) . . . O71 Cl1 O7 30.6(8) . . . O71 Cl1 O6 120.3(8) . . . O71 Cl1 O5 120.3(9) . . . O71 Cl1 O81 99(1) . . . O61 Cl1 O7 127(1) . . . O61 Cl1 O6 40(1) . . . O61 Cl1 O5 125(1) . . . O61 Cl1 O81 96(2) . . . O61 Cl1 O71 114(1) . . . O51 Cl1 O7 111.8(8) . . . O51 Cl1 O6 127.9(9) . . . O51 Cl1 O5 26.3(9) . . . O51 Cl1 O81 113(1) . . . O51 Cl1 O71 112(1) . . . O51 Cl1 O61 121(1) . . . O8 Cl1 O7 110.2(8) . . . O8 Cl1 O6 104.0(8) . . . O8 Cl1 O5 114.3(9) . . . O8 Cl1 O81 157(1) . . . O8 Cl1 O71 80(1) . . . O8 Cl1 O61 64(1) . . . O8 Cl1 O51 89(1) . . . Cl1 O8 O71 49.3(7) . . . Cl1 O8 O61 54(1) . . . O61 O8 O71 87(1) . . . Cl1 O51 O5 77(2) . . . Cl1 O61 O8 62(1) . . . O8 O61 O6 135(2) . . . Cl1 O61 O6 74(2) . . . Cl1 O71 O8 51.1(7) . . . O8 O71 O7 124(2) . . . Cl1 O71 O7 73(1) . . . Cl1 O81 O7 51(1) . . . Cl1 O81 O6 57(1) . . . O6 O81 O7 95(2) . . . Cl1 O5 O51 76(2) . . . O61 O6 O81 133(2) . . . Cl1 O6 O81 67(1) . . . Cl1 O6 O61 66(1) . . . O71 O7 O81 129(2) . . . Cl1 O7 O81 58(1) . . . Cl1 O7 O71 76(1) . . . #============================================================================ #=============================================================================== data_(5) #============================================================================= _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(cyt)2(H2O)4](ClO4)2.2cyt.2H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H32 Cl2 Co N12 O18' _chemical_formula_weight 810.4 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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 Carbon 0 16 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 32 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 12 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 18 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 2 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Co Cobalt 0 1 0.2990 0.9730 Internat_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 6.756(2) _cell_length_b 9.985(2) _cell_length_c 12.837(3) _cell_length_alpha 72.16(2) _cell_length_beta 87.78(2) _cell_length_gamma 72.19(2) _cell_volume 783.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.710730 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_colour 'pale pink' _exptl_crystal_description needles _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_F_000 417 _exptl_absorpt_coefficient_mu 8.1600 _exptl_absorpt_correction_type ? #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; ? ; _diffrn_special_details ;? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus xray_tube' _diffrn_radiation_monochromator 'highly-oriented graphite crystal' _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_number 3963 _reflns_number_total 3449 _reflns_number_observed 2155 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Siemens P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Siemens P3/V' _computing_data_reduction 'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)' _computing_structure_solution 'Siemens SHELXTL-PLUS' _computing_structure_refinement 'Siemens SHELXTL-PLUS' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens SHELXTL-PLUS and PARST' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0020*F^2^))' _refine_ls_hydrogen_treatment '"riding model" with fixed isotropic U' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_number_reflns 2155 _refine_ls_number_parameters 239 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 9.78 _refine_ls_R_factor_obs 6.09 _refine_ls_wR_factor_all 12.46 _refine_ls_wR_factor_obs 9.55 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.69 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.002 _refine_diff_density_min -1.03 _refine_diff_density_max 0.91 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_disorder_group # #label occ x/a y/b z/c Ueq the typ cal att dis # Co1 1.00 0. 0. 0. 0.0271(4) Uani Co ? ? ? O3 1.00 0.2361(7) 0.0566(5) -0.0936(4) 0.040(2) Uani O ? ? ? O4 1.00 0.2186(7) -0.1486(5) 0.1303(3) 0.035(2) Uani O ? ? ? N1 1.00 -0.0658(8) -0.0694(6) -0.2416(4) 0.036(2) Uani N ? ? ? C2 1.00 0.0358(9) -0.1888(6) -0.1557(5) 0.031(2) Uani C ? ? ? O2 1.00 0.0385(7) -0.1783(4) -0.0608(3) 0.038(2) Uani O ? ? ? N3 1.00 0.1307(8) -0.3187(5) -0.1739(4) 0.035(2) Uani N ? ? ? C4 1.00 0.128(1) -0.3280(7) -0.2756(5) 0.042(2) Uani C ? ? ? N4 1.00 0.224(1) -0.4597(7) -0.2888(5) 0.059(2) Uani N ? ? ? C5 1.00 0.025(1) -0.2046(8) -0.3664(5) 0.048(3) Uani C ? ? ? C6 1.00 -0.071(1) -0.0774(8) -0.3455(5) 0.043(2) Uani C ? ? ? N11 1.00 0.2805(8) -0.5552(6) 0.0189(4) 0.037(2) Uani N ? ? ? C21 1.00 0.3796(9) -0.6949(6) 0.0133(5) 0.035(2) Uani C ? ? ? O21 1.00 0.3918(7) -0.7152(5) -0.0784(4) 0.041(2) Uani O ? ? ? N31 1.00 0.4610(8) -0.8047(5) 0.1064(4) 0.036(2) Uani N ? ? ? C41 1.00 0.4485(9) -0.7756(7) 0.2023(5) 0.036(2) Uani C ? ? ? N41 1.00 0.5353(9) -0.8872(7) 0.2905(5) 0.049(2) Uani N ? ? ? C51 1.00 0.343(1) -0.6321(7) 0.2094(5) 0.046(3) Uani C ? ? ? C61 1.00 0.263(1) -0.5256(7) 0.1164(6) 0.047(2) Uani C ? ? ? Cl1 1.00 0.4068(3) -0.7247(2) 0.5541(1) 0.0529(7) Uani Cl ? ? ? O5 1.00 0.252(1) -0.5889(9) 0.5105(7) 0.108(4) Uani O ? ? ? O9 1.00 0.100(1) -0.3295(9) 0.3003(6) 0.100(3) Uani O ? ? ? O81 1.00 0.245(6) -0.799(4) 0.593(3) 0.11(1) Uiso O ? ? ? O6 1.00 0.403(2) -0.836(1) 0.5105(8) 0.079(3) Uiso O ? ? ? O7 1.00 0.400(2) -0.773(1) 0.6679(8) 0.076(3) Uiso O ? ? ? O8 1.00 0.600(2) -0.693(2) 0.528(1) 0.123(4) Uiso O ? ? ? O61 1.00 0.524(4) -0.803(3) 0.493(2) 0.071(7) Uiso O ? ? ? O71 1.00 0.500(4) -0.755(2) 0.659(2) 0.050(5) Uiso O ? ? ? H2W 1.00 0.374(4) -0.007(6) -0.096(7) 0.06 Uiso H ? ? ? H1 1.00 -0.1315(8) 0.0171(6) -0.2295(4) 0.06 Uiso H ? O3 ? H4A 1.00 0.283(1) -0.5288(7) -0.2242(5) 0.06 Uiso H ? N4 ? H4B 1.00 0.220(1) -0.4622(7) -0.3494(5) 0.06 Uiso H ? N4 ? H1W 1.00 0.26(1) 0.142(5) -0.087(7) 0.06 Uiso H ? O3 ? H41A 1.00 0.6015(9) -0.9771(7) 0.2846(5) 0.06 Uiso H ? N41 ? H41B 1.00 0.5285(9) -0.8716(7) 0.3560(5) 0.06 Uiso H ? N41 ? H5 1.00 0.026(1) -0.2127(8) -0.4391(5) 0.06 Uiso H ? C5 ? H51 1.00 0.331(1) -0.6125(7) 0.2785(5) 0.06 Uiso H ? C51 ? H3W 1.00 0.356(5) -0.183(7) 0.106(6) 0.06 Uiso H ? O4 ? H61 1.00 0.192(1) -0.4268(7) 0.1176(6) 0.06 Uiso H ? C61 ? H6 1.00 -0.146(1) 0.0081(8) -0.4041(5) 0.06 Uiso H ? C6 ? H4W 1.00 0.22(1) -0.231(5) 0.194(4) 0.06 Uiso H ? O4 ? H11 1.00 0.2251(8) -0.4817(6) -0.0431(4) 0.06 Uiso H ? N11 ? H5W 1.00 0.07(1) -0.250(5) 0.332(5) 0.06 Uiso H ? O9 ? H6W 1.00 0.14(1) -0.409(5) 0.368(3) 0.06 Uiso H ? O9 ? loop_ _atom_site_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 _atom_site_aniso_type_symbol # #label U11 U22 U33 U23 U13 U12 typ # Co1 0.0278(6) 0.0190(6) 0.0218(6) -0.0087(4) 0.0029(5) -0.0062(5) Co O3 0.034(2) 0.031(2) 0.036(2) -0.013(2) 0.008(2) -0.016(2) O O4 0.033(2) 0.029(2) 0.029(2) -0.004(2) -0.001(2) -0.006(2) O N1 0.037(3) 0.024(2) 0.032(3) -0.010(2) 0.003(2) -0.004(2) N C2 0.028(3) 0.023(3) 0.026(3) -0.009(2) 0.006(2) -0.012(2) C O2 0.045(3) 0.025(2) 0.026(2) -0.014(2) 0.007(2) -0.011(2) O N3 0.036(3) 0.022(2) 0.029(3) -0.013(2) 0.002(2) -0.008(2) N C4 0.036(3) 0.035(3) 0.032(3) -0.015(3) 0.007(3) -0.016(3) C N4 0.072(4) 0.037(3) 0.038(3) -0.025(3) 0.007(3) -0.011(3) N C5 0.051(4) 0.045(4) 0.024(3) -0.011(3) 0.001(3) -0.017(3) C C6 0.043(4) 0.041(4) 0.026(3) -0.010(3) 0.002(3) -0.009(3) C N11 0.038(3) 0.024(3) 0.034(3) -0.008(2) 0.001(2) -0.006(2) N C21 0.024(3) 0.024(3) 0.038(3) -0.013(3) 0.007(3) -0.010(2) C O21 0.041(3) 0.027(2) 0.036(2) -0.014(2) 0.006(2) -0.010(2) O N31 0.030(3) 0.025(2) 0.036(3) -0.012(2) 0.008(2) -0.010(2) N C41 0.023(3) 0.032(3) 0.036(3) -0.010(3) 0.003(3) -0.010(3) C N41 0.049(4) 0.040(3) 0.037(3) -0.006(3) -0.000(3) -0.012(3) N C51 0.037(4) 0.041(4) 0.035(3) -0.021(3) 0.007(3) -0.016(3) C C61 0.040(4) 0.031(3) 0.046(4) -0.022(3) 0.013(3) -0.012(3) C Cl1 0.065(1) 0.0354(9) 0.0351(9) -0.0136(7) 0.0055(9) -0.0095(9) Cl O5 0.136(8) 0.060(4) 0.093(6) -0.009(4) -0.014(6) 0.025(5) O O9 0.113(6) 0.075(5) 0.070(5) 0.008(4) 0.024(5) -0.034(5) O #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; The geometric calculation (and the starting release of this CIF file) has been made by a locally modified release of the program PARST of prof. M. Nardelli (we have already adviced prof. Nardelli about it). This release is interactive and has included into one body : I/O interface to other programs, no formated line, logical commands, better output listing and now we are developping a graphical interface PLUTO-like. All computational routines are the original ones. However this release is reserved for internal use of our laboratory only (it is neither public neither commercial release!). ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag # # Complete list of bond lengths for non-H atoms. # Co1 O3 2.073(5) . . . Co1 O4 2.124(4) . . . Co1 O2 2.097(5) . . . N1 C2 1.364(6) . . . N1 C6 1.362(9) . . . C2 O2 1.256(8) . . . C2 N3 1.348(8) . . . N3 C4 1.337(9) . . . C4 N4 1.336(9) . . . C4 C5 1.421(8) . . . C5 C6 1.34(1) . . . N11 C21 1.373(8) . . . N11 C61 1.36(1) . . . C21 O21 1.251(9) . . . C21 N31 1.346(7) . . . N31 C41 1.343(9) . . . C41 N41 1.322(7) . . . C41 C51 1.42(1) C51 C61 1.331(8) . . . Cl1 O5 1.399(7) . . . Cl1 O81 1.49(4) . . . Cl1 O6 1.40(1) . . . Cl1 O7 1.40(1) . . . Cl1 O8 1.44(2) . . . Cl1 O61 1.34(3) . . . Cl1 O71 1.42(2) . . . O81 O6 1.52(4) . . . O81 O7 1.57(5) . . . O6 O61 0.97(3) . . . O7 O71 0.75(3) . . . O8 O61 1.52(4) . . . O8 O71 1.79(3) . . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # # Complete list of bond angles for non-H atoms. # O2 Co1 O3 90.2(2) . . . O2 Co1 O4 87.3(2) . . . O3 Co1 O4 91.2(2) . . . O2 Co1 O3 89.8(2) . . 2_555 O2 Co1 O4 92.7(2) . . 2_555 O3 Co1 O4 88.8(2) . . 2_555 C2 N1 C6 121.9(5) . . . N1 C2 N3 118.9(6) . . . N1 C2 O2 120.6(5) . . . O2 C2 N3 120.5(5) . . . Co1 O2 C2 133.5(4) . . . C2 N3 C4 119.8(5) . . . N3 C4 C5 122.1(6) . . . N3 C4 N4 117.2(6) . . . N4 C4 C5 120.7(7) . . . C4 C5 C6 116.8(7) . . . N1 C6 C5 120.4(6) . . . C21 N11 C61 121.5(6) . . . N11 C21 N31 119.0(6) . . . N11 C21 O21 118.7(6) . . . O21 C21 N31 122.3(6) . . . C21 N31 C41 119.8(5) . . . N31 C41 C51 121.8(6) . . . N31 C41 N41 117.0(6) . . . N41 C41 C51 121.2(6) . . . C41 C51 C61 117.3(6) . . . N11 C61 C51 120.6(6) . . . O61 Cl1 O71 114(2) . . . O8 Cl1 O71 78(1) . . . O8 Cl1 O61 66(1) . . . O7 Cl1 O71 31(1) . . . O7 Cl1 O61 126(1) . . . O7 Cl1 O8 108.5(8) . . . O6 Cl1 O71 123(1) . . . O6 Cl1 O61 42(1) . . . O6 Cl1 O8 107.8(8) . . . O6 Cl1 O7 110.2(6) . . . O81 Cl1 O71 96(2) . . . O81 Cl1 O61 104(2) . . . O81 Cl1 O8 165(2) . . . O81 Cl1 O7 66(2) . . . O81 Cl1 O6 63(2) . . . O5 Cl1 O71 118(1) . . . O5 Cl1 O61 124(1) . . . O5 Cl1 O8 104.9(8) . . . O5 Cl1 O7 109.6(6) . . . O5 Cl1 O6 115.4(6) . . . O5 Cl1 O81 90(2) . . . Cl1 O81 O7 54(1) . . . Cl1 O81 O6 55(1) . . . O6 O81 O7 95(2) . . . Cl1 O6 O81 61(2) . . . O81 O6 O61 126(2) . . . Cl1 O6 O61 66(2) . . . Cl1 O7 O81 60(1) . . . O81 O7 O71 135(3) . . . Cl1 O7 O71 76(2) . . . Cl1 O8 O71 50.7(9) . . . Cl1 O8 O61 54(1) . . . O61 O8 O71 88(1) . . . O6 O61 O8 132(3) . . . Cl1 O61 O8 60(1) . . . Cl1 O61 O6 73(2) . . . O7 O71 O8 124(3) . . . Cl1 O71 O8 51.5(9) . . . Cl1 O71 O7 73(2) . . .