# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _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 B100495F: " Polycatenane systems from Co(II) and trans-1,2-bis(4-pyridyl)ethene [bpe]. Synthesis and structure of [Co(bpe)2(NCS)2].CH3OH, [Co(bpe)2(H2O)2](ClO4)2.2CH3OH and [Co(bpe)2(H2O)2(CH3OH)2](ClO4)2.bpe.H2O " The compounds have been identified in the paper with number 1, 2, and 3. (in this cif file they have been called data_(1), data_(2), and data_(3). 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_coden_ASTM ? _journal_name_full 'New Journal of Chemistry' _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 ; Polycatenane systems from Co(II) and trans-1,2-bis(4-pyridyl)ethene [bpe]. Synthesis and structure of [Co(bpe)2(NCS)2].CH3OH, [Co(bpe)2(H2O)2](ClO4)2.2CH3OH and [Co(bpe)2(H2O)2(CH3OH)2](ClO4)2.bpe.H2O ; loop_ _publ_author_name _publ_author_address 'De Munno, Giovanni ' ; Dipartimento di Chimica Universit\'a degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Francesca Cipriani' ; 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 ; 'Miguel Julve' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; 'Jose Antonio Real' ; Departament de Quimica Inorganica Facultat de Quimica Dr. Moliner 50 E-46100 Burjassot, Valencia Spain ; #=========================================================================== # 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) _database_code_CSD 164616 #============================================================================ _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(bpe)2(NCS)2].CH3OH' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H24 S2 Co N6 O' _chemical_formula_weight 571.54 _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 0 108 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 96 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 24 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 4 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 S Sulphur 0 8 0.1100 0.1240 Internat_Tables_Vol_IV_Table_2.3.1 Co Cobalt 0 4 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 'P4/ncc' _symmetry_cell_setting 13 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x+1/2,-y+1/2,z' '-y+1/2,x,z' 'y,-x+1/2,z' '-x,y+1/2,-z+1/2' 'x+1/2,-y,-z+1/2' 'y+1/2,x+1/2,-z+1/2' '-y,-x,-z+1/2' '-x,-y,-z' 'x+1/2,y+1/2,-z' 'y+1/2,-x,-z' '-y,x+1/2,-z' 'x,-y+1/2,z+1/2' '-x+1/2,y,z+1/2' '-y+1/2,-x+1/2,z+1/2' 'y,x,z+1/2' _cell_length_a 15.798(5) _cell_length_b 15.798(5) _cell_length_c 15.674(7) _cell_length_alpha 90. _cell_length_beta 90. _cell_length_gamma 90. _cell_volume 3912(2) _cell_formula_units_Z 4 _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 orange _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn . _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 5.67 _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 'Bruker 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 24.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_number 2385 _reflns_number_total 1549 _reflns_number_observed 651 _reflns_observed_criterion >s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Bruker P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement 'Bruker P3/V' _computing_data_reduction 'Bruker SHELXTL-PLUS,(VMS vers 4.21/V, 1990)' _computing_structure_solution 'Bruker SHELXTL-PLUS' _computing_structure_refinement 'Bruker SHELXTL-PLUS' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker 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)+ 0.0100*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 651 _refine_ls_number_parameters 82 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 18.35 _refine_ls_R_factor_obs 8.48 _refine_ls_wR_factor_all 18.85 _refine_ls_wR_factor_obs 13.17 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.03 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.001 _refine_diff_density_min -0.52 _refine_diff_density_max 0.53 #=========================================================================== # 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 0.25 0.25(4) 0.75 0.25 0.043 Uani Co . . . N1 1.00 0.1849(8) 0.6787(8) 0.1532(7) 0.053(5) Uani N . . . C1 1.00 0.140(1) 0.715(1) 0.093(1) 0.070(6) Uani C . . . C2 1.00 0.077(1) 0.674(1) 0.040(1) 0.077(7) Uani C . . . C3 1.00 0.072(1) 0.586(1) 0.0474(9) 0.064(6) Uani C . . . C4 1.00 0.125(1) 0.545(1) 0.107(1) 0.064(6) Uani C . . . C5 1.00 0.179(1) 0.593(1) 0.1588(9) 0.057(5) Uani C . . . C6 1.00 0.011(1) 0.5395(9) -0.007(1) 0.080(6) Uani C . . . N2 0.50 0.3410(8) 0.6590(8) 0.25 0.059(4) Uani N . . . C7 0.50 0.391(1) 0.609(1) 0.25 0.084(7) Uani C . . . S1 0.50 0.4630(5) 0.5370(5) 0.25 0.35(1) Uani S . . . H5 1.00 0.214(1) 0.565(1) 0.2000(9) 0.06 iso H . C5 . H1 1.00 0.147(1) 0.775(1) 0.086(1) 0.06 iso H . C1 . H6 1.00 -0.017(1) 0.5805(9) -0.042(1) 0.06 iso H . C6 . H4 1.00 0.123(1) 0.485(1) 0.113(1) 0.06 iso H . C4 . H2 1.00 0.042(1) 0.704(1) -0.001(1) 0.06 iso H . C2 . 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 0.043(1) 0.043(1) 0.044(2) -0.022(2) 0.0 0.0 Co N1 0.06(1) 0.051(9) 0.050(6) 0.001(7) -0.008(7) -0.010(5) N C1 0.11(1) 0.036(8) 0.07(1) 0.002(8) -0.00(1) -0.028(9) C C2 0.10(1) 0.05(1) 0.08(1) 0.01(1) -0.05(1) -0.01(1) C C3 0.07(1) 0.07(1) 0.059(8) -0.015(9) -0.007(9) -0.033(9) C C4 0.07(1) 0.05(1) 0.08(1) -0.010(9) -0.014(9) -0.019(9) C C5 0.06(1) 0.049(9) 0.061(9) -0.003(8) -0.010(9) -0.011(8) C C6 0.09(1) 0.08(1) 0.065(9) -0.00(1) -0.02(1) -0.05(1) C N2 0.056(6) 0.056(6) 0.07(1) 0.002(9) 0.002(9) -0.017(8) N C7 0.10(1) 0.10(1) 0.05(1) 0.00(1) 0.00(1) 0.01(2) C S1 0.46(2) 0.46(2) 0.139(9) -0.07(1) -0.07(1) 0.40(2) S #=========================================================================== # 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 # #Complete list of bond lengths for non-H atoms. # N1 C1 1.31(2) . . N1 C5 1.37(2) . . N1 Co1 2.15(1) . . C1 C2 1.45(2) . . C2 C3 1.40(2) . . C3 C4 1.41(2) . . C3 C6 1.48(2) . . C4 C5 1.39(2) . . N2 C7 1.11(2) . . C7 S1 1.62(2) . . C6 C6 1.39(2) . 9_565 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. # C5 N1 Co1 121(1) . . . C1 N1 Co1 123(1) . . . C7 N2 Co1 180(2) . . . C1 N1 C5 116(1) . . . N1 C1 C2 127(1) . . . N1 Co1 N2 88.1(5) . . . N1 Co1 N1 90.4(6) . . 2_565 N1 Co1 N1 89.8(6) . . 7_655 N1 Co1 N1d 176.3(7) . . 8_665 N1 Co1 N2 91.9(5) . . 2_565 C1 C2 C3 115(1) . . . C2 C3 C6 119(1) . . . C2 C3 C4 118(1) . . . C4 C3 C6 123(1) . . . C3 C4 C5 120(1) . . . C3 C6 C6 120(1) . . 9_565 N1 C5 C4 123(1) . . . N2 C7 S1 180(2) . . . #=========================================================================== #=========================================================================== data_(2) _database_code_CSD 164617 #============================================================================ _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(bpe)2(NCS)2].CH3OH' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H32 Cl2 Co N4 O12' _chemical_formula_weight 722.4 _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 0 208 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 256 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 32 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 96 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1 Cl Chlorine 0 16 0.1320 0.1590 Internat_Tables_Vol_IV_Table_2.3.1 Co Cobalt 0 8 0.2990 0.9730 Internat_Tables_Vol_IV_Table_2.3.1 #=========================================================================== # 11. CRYSTAL DATA #=========================================================================== _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4(1)cd' _symmetry_cell_setting 110 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x+1/2,-y+1/2,z+1/2' '-y,x+1/2,z+1/4' 'y+1/2,-x,z+3/4' 'x,-y,z+1/2' '-x+1/2,y+1/2,z' '-y,-x+1/2,z+3/4' 'y+1/2,x,z+1/4' 'x+1/2,y+1/2,z+1/2' '-x+1,-y+1,z+1' '-y+1/2,x+1,z+3/4' 'y+1,-x+1/2,z+5/4' 'x+1/2,-y+1/2,z+1' '-x+1,y+1,z+1/2' '-y+1/2,-x+1,z+5/4' 'y+1,x+1/2,z+3/4' _cell_length_a 19.490(5) _cell_length_b 19.490(5) _cell_length_c 16.508(7) _cell_length_alpha 90. _cell_length_beta 90. _cell_length_gamma 90. _cell_volume 6271(3) _cell_formula_units_Z 8 _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 parallelepiped _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.530 _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 7.85 _exptl_absorpt_correction_type ? #=========================================================================== # 12. 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 'Bruker 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 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_number 4672 _reflns_number_total 1443 _reflns_number_observed 823 _reflns_observed_criterion >2\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Bruker P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement ' Bruker P3/V' _computing_data_reduction ' Bruker SHELXTL-PLUS,(VMS vers 4.21/V, 1990)' _computing_structure_solution ' Bruker SHELXTL-PLUS' _computing_structure_refinement ' Bruker SHELXTL-PLUS' _computing_molecular_graphics ' Bruker XP' _computing_publication_material ' Bruker SHELXTL-PLUS and PARST' #=========================================================================== # 13. 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 823 _refine_ls_number_parameters 133 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 12.37 _refine_ls_R_factor_obs 7.18 _refine_ls_wR_factor_all 9.38 _refine_ls_wR_factor_obs 7.66 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.49 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.001 _refine_diff_density_min -0.61 _refine_diff_density_max 0.69 #=============================================================================== # 14. 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 0.50 0. 0. 0. 0.0273(7) Uani Co . . . O1 0.50 0. 0. -0.128(2) 0.053(8) Uani O . . . Cl1 1.00 0.0379(3) 0.1785(2) 0.2464(8) 0.062(2) Uani Cl . . . O3 1.00 0.1031(8) 0.1487(8) 0.256(2) 0.109(7) Uani O . . . O4 1.00 0.020(1) 0.2139(9) 0.315(1) 0.101(8) Uani O . . . O5 1.00 0.039(1) 0.223(1) 0.179(1) 0.101(8) Uani O . . . O6 1.00 -0.0092(9) 0.1261(8) 0.240(2) 0.126(9) Uani O . . . C13 1.00 -0.1619(9) -0.033(1) -0.239(2) 0.09(1) Uani C . . . O7 1.00 -0.1137(8) 0.0095(8) -0.216(1) 0.094(8) Uani O . . . N2 1.00 -0.4226(7) 0.4198(7) 0.001(1) 0.035(3) iso N . . . C3 1.00 -0.1776(9) 0.1872(8) 0.014(1) 0.041(4) iso C . . . C4 1.00 -0.191(1) 0.1227(9) -0.019(1) 0.053(6) iso C . . . C11 1.00 -0.4256(9) 0.3731(9) -0.062(1) 0.037(4) iso C . . . C5 1.00 -0.1423(8) 0.0705(8) -0.022(1) 0.037(5) iso C . . . C2 1.00 -0.1130(9) 0.1945(9) 0.041(1) 0.043(5) iso C . . . C6 1.00 -0.2272(9) 0.243(1) 0.020(1) 0.051(6) iso C . . . C12 1.00 -0.3816(9) 0.3176(9) -0.068(1) 0.046(5) iso C . . . C7 1.00 -0.2862(8) 0.2482(8) -0.015(1) 0.038(4) iso C . . . N1 1.00 -0.0799(7) 0.0791(7) 0.0129(9) 0.029(3) iso N . . . C8 1.00 -0.3330(8) 0.3074(8) -0.010(1) 0.038(5) iso C . . . C9 1.00 -0.330(1) 0.3541(9) 0.054(1) 0.050(5) iso C . . . C1 1.00 -0.065(1) 0.142(1) 0.038(1) 0.050(6) iso C . . . C10 1.00 -0.3765(9) 0.4118(8) 0.057(1) 0.037(4) iso C . . . O2 0.50 0. 0. 0.128(2) 0.040(8) iso O . . . H2 1.00 -0.0982(9) 0.2383(9) 0.061(1) 0.06 iso H . C2 . H4 1.00 -0.236(1) 0.1153(9) -0.042(1) 0.06 iso H . C4 . H5 1.00 -0.1527(8) 0.0275(8) -0.048(1) 0.06 iso H . C5 . H6 1.00 -0.2141(9) 0.283(1) 0.051(1) 0.06 iso H . C6 . H7 1.00 -0.3004(8) 0.2096(8) -0.047(1) 0.06 iso H . C7 . H9 1.00 -0.296(1) 0.3482(9) 0.095(1) 0.06 iso H . C9 . H10 1.00 -0.3735(9) 0.4442(8) 0.100(1) 0.06 iso H . C10 . H11 1.00 -0.4592(9) 0.3802(9) -0.103(1) 0.06 iso H . C11 . H12 1.00 -0.3852(9) 0.2856(9) -0.112(1) 0.06 iso H . C12 . H1W 1.00 -0.040(2) -0.003(9) -0.161(1) 0.06 iso H . O1 . H2W 1.00 -0.022(7) 0.033(5) 0.1630(9) 0.06 iso H . O2 . H1 1.00 -0.019(1) 0.149(1) 0.059(1) 0.06 iso H . C1 . H13A 1.00 -0.1452(9) -0.055(1) -0.287(2) 0.06 iso H . C13 . H13B 1.00 -0.2011(9) -0.006(1) -0.252(2) 0.06 iso H . C13 . H13C 1.00 -0.1748(9) -0.068(1) -0.200(2) 0.06 iso H . C13 . H7A 1.00 -0.1352(8) 0.0422(8) -0.194(1) 0.06 iso H . O7 . 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 0.019(1) 0.015(1) 0.047(1) 0. 0. 0.001(1) Co O1 0.04(1) 0.06(2) 0.06(1) 0. 0. -0.00(1) O Cl1 0.067(3) 0.036(2) 0.084(4) -0.002(4) 0.012(4) -0.000(2) Cl O3 0.08(1) 0.09(1) 0.16(2) 0.00(1) -0.02(1) -0.004(9) O O4 0.13(2) 0.09(1) 0.09(1) -0.02(1) 0.05(1) -0.04(1) O O5 0.12(2) 0.09(1) 0.09(1) 0.01(1) 0.03(1) -0.01(1) O O6 0.13(1) 0.07(1) 0.18(2) 0.02(2) 0.06(2) -0.04(1) O C13 0.04(1) 0.13(2) 0.11(2) 0.06(2) 0.01(1) -0.04(1) Cl O7 0.08(1) 0.07(1) 0.13(2) -0.02(1) -0.06(1) -0.004(9) O #=========================================================================== # 15. 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 # # # Complete list of bond lengths for non-H atoms. # Co1 O1 2.12(3) . . Co1 N1 2.20(1) . . Co1 N2 2.17(1) . 13_554 Cl1 O3 1.41(2) . . Cl1 O4 1.37(2) . . Cl1 O5 1.41(2) . . Cl1 O6 1.38(2) . . C13 O7 1.31(3) . . N2 C11 1.39(3) . . N2 C10 1.29(2) . . C3 C4 1.40(2) . . C3 C2 1.34(3) . . C3 C6 1.45(2) . . C4 C5 1.40(2) . . C11 C12 1.39(2) . . C5 N1 1.36(2) . . C2 C1 1.39(3) . . C6 C7 1.29(3) . . C12 C8 1.37(3) . . C7 C8 1.47(2) . . N1 C1 1.33(2) . . C8 C9 1.39(3) . . C9 C10 1.44(2) . . 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. # O1 Co1 N1 95.6(4) . . . O1 Co1 O2 180.0(1) . . . O2 Co1 N1 84.4(4) . . . O1 Co1 N2 90.6(5) . . 13_554 N1 Co1 N1 168.9(8) . . 10_444 O2 Co1 N2 89.4(5) . . 13_554 N1 Co1 N2 89.2(5) . . 13_554 N1 Co1 N2 90.7(5) . . 6_445 N2 Co1 N2 179(1) 13_554 . 6_445 O5 Cl1 O6 114(1) . . . O4 Cl1 O6 105(1) . . . O4 Cl1 O5 110(1) . . . O3 Cl1 O6 108(1) . . . O3 Cl1 O5 110(1) . . . O3 Cl1 O4 110(1) . . . C11 N2 C10 119(2) . . . C2 C3 C6 122(2) . . . C4 C3 C6 125(2) . . . C4 C3 C2 114(2) . . . C3 C4 C5 123(2) . . . N2 C11 C12 123(2) . . . C4 C5 N1 120(2) . . . C3 C2 C1 123(2) . . . C3 C6 C7 129(2) . . . C11 C12 C8 119(2) . . . C6 C7 C8 126(2) . . . Co1 N1 C5 120(1) . . . C5 N1 C1 117(1) . . . C11 N2 Co1 116(1) . . 13_454 C11 N2 Co1 125(1) . . 13_454 Co1 N1 C1 121(1) . . . C12 C8 C7 120(1) . . . C7 C8 C9 122(1) . . . C12 C8 C9 118(2) . . . C8 C9 C10 121(2) . . . C2 C1 N1 123(2) . . . N2 C10 C9 120(2) . . . #=========================================================================== #=========================================================================== data_(3) _database_code_CSD 164618 #=========================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety '[Co(bpe)2(H2O)2(CH3OH)2](ClO4)2.bpe.H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H44 Cl2 Co N6 O13' _chemical_formula_weight 920.6 _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 38 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1 H Hydrogen 0 44 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1 N Nitrogen 0 6 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1 O Oxygen 0 13 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 #=========================================================================== # 16. CRYSTAL DATA #=========================================================================== _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_cell_setting 2 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 8.958(4) _cell_length_b 11.093(7) _cell_length_c 12.994(5) _cell_length_alpha 105.73(5) _cell_length_beta 94.55(3) _cell_length_gamma 113.60 _cell_volume 1112.8(9) _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 orange _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.29 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_F_000 477 _exptl_absorpt_coefficient_mu 5.72 _exptl_absorpt_correction_type ? #=========================================================================== #=== # 17. 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 'Bruker 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 24.0 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_number 3887 _reflns_number_total 3493 _reflns_number_observed 2305 _reflns_observed_criterion >3\s(I) _diffrn_reflns_reduction_process ? _computing_data_collection 'Bruker P3/V,(VMS vers 4.21/V, 1990)' _computing_cell_refinement ' Bruker P3/V' _computing_data_reduction ' Bruker SHELXTL-PLUS,(VMS vers 4.21/V, 1990)' _computing_structure_solution ' Bruker SHELXTL-PLUS' _computing_structure_refinement ' Bruker SHELXTL-PLUS' _computing_molecular_graphics ' Bruker XP' _computing_publication_material ' Bruker SHELXTL-PLUS and PARST' #=========================================================================== # 18. REFINEMENT DATA #=========================================================================== _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/(\s^2^(F)+ 0.0118*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 2305 _refine_ls_number_parameters 272 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 9.93 _refine_ls_R_factor_obs 7.22 _refine_ls_wR_factor_all 16.13 _refine_ls_wR_factor_obs 11.98 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.04 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/esd_max 0.001 _refine_diff_density_min -0.41 _refine_diff_density_max 1.02 #=========================================================================== # 19. 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 0.50 0. 0. 0. 0.0362(6) Uanu Co . . . N1 1.00 0.0869(7) -0.1050(6) -0.1322(4) 0.043(2) Uani N . . . C1 1.00 0.120(1) -0.2120(9) -0.1302(6) 0.062(3) Uani C . . . C2 1.00 0.159(1) -0.2880(9) -0.2186(6) 0.066(4) Uani C . . . C3 1.00 0.168(1) -0.2545(8) -0.3118(6) 0.051(3) Uani C . . . C4 1.00 0.139(1) -0.1428(8) -0.3133(6) 0.059(4) Uani C . . . C5 1.00 0.0997(9) -0.0719(7) -0.2234(6) 0.051(3) Uani C . . . C6 1.00 0.207(1) -0.3328(9) -0.4090(6) 0.057(3) Uani C . . . C7 1.00 0.239(1) -0.4385(8) -0.4181(6) 0.054(3) Uani C . . . C8 1.00 0.2665(9) -0.5243(8) -0.5160(6) 0.052(4) Uani C . . . C9 1.00 0.286(1) -0.6416(9) -0.5153(7) 0.066(4) Uani C . . . C10 1.00 0.304(1) -0.7231(9) -0.6105(7) 0.071(4) Uani C . . . N2 1.00 0.3016(9) -0.6979(7) -0.7041(6) 0.062(3) Uani N . . . C11 1.00 0.285(1) -0.586(1) -0.7023(7) 0.070(4) Uani C . . . C12 1.00 0.274(1) -0.4931(9) -0.6129(7) 0.073(4) Uani C . . . N3 1.00 0.4130(9) 0.2843(8) -0.0537(7) 0.074(4) Uani N . . . C13 1.00 0.477(1) 0.253(1) -0.1400(9) 0.077(5) Uani C . . . C14 1.00 0.645(1) 0.310(1) -0.1395(8) 0.073(4) Uani C . . . C15 1.00 0.759(1) 0.4049(9) -0.0427(8) 0.066(4) Uani C . . . C16 1.00 0.699(1) 0.4437(9) 0.0457(8) 0.065(4) Uani C . . . C17 1.00 0.526(1) 0.379(1) 0.0383(9) 0.084(4) Uani C . . . C18 1.00 0.940(1) 0.4610(9) -0.0434(8) 0.065(4) Uani C . . . O1 1.00 0.2296(6) 0.0857(5) 0.1112(4) 0.046(2) Uani O . . . C19 1.00 0.369(1) 0.056(1) 0.1132(8) 0.070(4) Uani C . . . O2 1.00 0.0850(6) 0.1797(5) -0.0458(4) 0.049(2) Uani O . . . Cl1 1.00 0.9777(3) 0.2037(3) 0.6771(2) 0.080(1) Uani C . . . O3 1.00 0.948(2) 0.314(1) 0.671(1) 0.220(9) Uani O . . . O4 1.00 0.892(1) 0.1460(9) 0.7532(6) 0.114(4) Uani O . . . O5 1.00 1.147(1) 0.250(1) 0.7169(9) 0.177(8) Uani O . . . O6 1.00 0.927(2) 0.108(1) 0.5739(8) 0.184(8) Uani O . . . O7 1.00 0.533(5) -0.057(4) 0.466(3) 0.26(2) iso O . . . H2 1.00 0.183(1) -0.3629(9) -0.2126(6) 0.06 iso H . C2 . H10 1.00 0.319(1) -0.8033(9) -0.6079(7) 0.06 iso H . C10 . H16 1.00 0.772(1) 0.5117(9) 0.1130(8) 0.06 iso H . C16 . H6 1.00 0.206(1) -0.3043(9) -0.4724(6) 0.06 iso H . C6 . H17 1.00 0.483(1) 0.404(1) 0.1019(9) 0.06 iso H . C17 . H4 1.00 0.146(1) -0.1142(8) -0.3769(6) 0.06 iso H . C4 . H18 1.00 0.971(1) 0.4393(9) -0.1125(8) 0.06 iso H . C18 . H11 1.00 0.286(1) -0.564(1) -0.7689(7) 0.06 iso H . C11 . H1A 1.00 0.2722(6) 0.1714(5) 0.1166(4) 0.06 iso H . O1 . H7 1.00 0.248(1) -0.4628(8) -0.3531(6) 0.06 iso H . C7 . H19A 1.00 0.453(1) 0.119(1) 0.1779(8) 0.06 iso H . C19 . H19B 1.00 0.333(1) -0.038(1) 0.1132(8) 0.06 iso H . C19 . H19C 1.00 0.414(1) 0.065(1) 0.0497(8) 0.06 iso H . C19 . H12 1.00 0.264(1) -0.4112(9) -0.6167(7) 0.06 iso H . C12 . H1W 1.00 0.0636(6) 0.2408(5) -0.0030(4) 0.06 iso H . O2 . H2W 1.00 0.1897(6) 0.2114(5) -0.0414(4) 0.06 iso H . O2 . H1 1.00 0.113(1) -0.2376(9) -0.0652(6) 0.06 iso H . C1 . H5 1.00 0.0785(9) 0.0055(7) -0.2264(6) 0.06 iso H . C5 . H13 1.00 0.400(1) 0.189(1) -0.2071(9) 0.06 iso H . C13 . H9 1.00 0.286(1) -0.6650(9) -0.4494(7) 0.06 iso H . C9 . H14 1.00 0.684(1) 0.282(1) -0.2043(8) 0.06 iso H . C14 . 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 0.0348(8) 0.0325(8) 0.0282(7) 0.0104(5) 0.0099(5) 0.0162(6) Co N1 0.040(3) 0.042(3) 0.032(3) 0.011(3) 0.015(2) 0.023(3) N C1 0.068(5) 0.066(5) 0.034(4) 0.025(4) 0.023(3) 0.046(4) C C2 0.078(6) 0.058(5) 0.046(4) 0.022(4) 0.023(4) 0.050(5) C C3 0.055(5) 0.050(4) 0.029(4) 0.006(3) 0.008(3) 0.030(4) C C4 0.073(6) 0.050(5) 0.035(4) 0.017(3) 0.019(4) 0.035(4) C C5 0.053(5) 0.042(4) 0.043(4) 0.018(3) 0.025(3) 0.025(4) C C6 0.053(5) 0.059(5) 0.036(4) 0.012(4) 0.016(3) 0.025(4) C C7 0.050(5) 0.051(5) 0.041(4) 0.009(3) 0.018(3) 0.026(4) C C8 0.046(5) 0.046(4) 0.041(4) 0.004(3) 0.008(3) 0.017(4) C C9 0.061(5) 0.064(5) 0.047(5) 0.010(4) 0.012(4) 0.033(4) C C10 0.072(6) 0.056(5) 0.059(6) -0.003(4) 0.009(4) 0.040(5) C N2 0.054(4) 0.059(4) 0.046(4) 0.000(3) 0.014(3) 0.025(3) N C11 0.072(6) 0.075(6) 0.039(4) 0.012(4) 0.020(4) 0.042(5) C C12 0.083(6) 0.060(5) 0.053(5) 0.017(4) 0.029(4) 0.042(5) C N3 0.043(4) 0.059(5) 0.091(6) 0.037(4) 0.011(4) 0.014(4) N C13 0.049(5) 0.066(6) 0.085(7) 0.025(5) 0.019(5) 0.016(4) C C14 0.045(5) 0.063(6) 0.083(7) 0.024(5) 0.019(5) 0.017(4) C C15 0.047(5) 0.052(5) 0.079(6) 0.034(5) 0.013(4) 0.025(4) C C16 0.043(5) 0.055(5) 0.076(6) 0.030(4) 0.006(4) 0.023(4) C C17 0.066(6) 0.080(7) 0.085(7) 0.047(6) 0.032(5) 0.045(5) C C18 0.038(4) 0.052(5) 0.084(6) 0.029(4) 0.014(4) 0.023(4) C O1 0.036(3) 0.046(3) 0.039(3) 0.007(2) 0.007(2) 0.020(2) O C19 0.055(5) 0.064(6) 0.066(6) 0.006(4) 0.006(4) 0.035(4) C O2 0.043(3) 0.042(3) 0.045(3) 0.013(2) 0.015(2) 0.022(2) O Cl1 0.086(2) 0.081(2) 0.046(1) 0.030(1) 0.015(1) 0.045(1) Cl O3 0.27(1) 0.19(1) 0.16(1) 0.136(9) 0.12(1) 0.18(1) O O4 0.101(6) 0.122(7) 0.081(5) 0.060(5) 0.026(4) 0.057(5) O O5 0.073(6) 0.26(1) 0.123(8) 0.111(8) 0.023(5) 0.057(7) O O6 0.21(1) 0.18(1) 0.061(6) -0.009(6) 0.018(7) 0.054(9) O #=========================================================================== # 20. 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 # # # Complete list of bond lengths for non-H atoms. # Co1 N1 2.183(6) . . Co1 O1 2.107(5) . . Co1 O2 2.100(6) . . N1 C1 1.34(1) . . N1 C5 1.33(1) . . C1 C2 1.39(1) . . C2 C3 1.36(1) . . C3 C4 1.37(1) . . C3 C6 1.48(1) . . C4 C5 1.38(1) . . C6 C7 1.29(1) . . C7 C8 1.47(1) . . C8 C9 1.38(1) . . C8 C12 1.39(1) . . C9 C10 1.39(1) . . C10 N2 1.32(1) . . N2 C11 1.31(2) . . C11 C12 1.37(1) . . N3 C13 1.33(1) . . N3 C17 1.35(1) . . C13 C14 1.38(1) . . C14 C15 1.40(1) . . C15 C16 1.35(1) . . C15 C18 1.48(1) . . C16 C17 1.40(1) . . C18 C18 1.31(1) . 2_745 O1 C19 1.41(1) . . Cl1 O3 1.37(2) . . Cl1 O4 1.429(9) . . Cl1 O5 1.39(1) . . Cl1 O6 1.37(1) . . 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. # O1 Co1 O2 89.3(2) . . . N1 Co1 O2 91.1(2) . . . N1 Co1 O1 92.9(2) . . . O1 Co1 N1 87.1(2) . . 2_555 O2 Co1 N1 88.9(2) . . 2_555 O1 Co1 O2 90.7(2) . . 2_555 Co1 N1 C5 121.5(5) . . . Co1 N1 C1 122.5(5) . . . C1 N1 C5 115.9(7) . . . N1 C1 C2 122.6(8) . . . C1 C2 C3 120.7(7) . . . C2 C3 C6 123.1(7) . . . C2 C3 C4 116.9(8) . . . C4 C3 C6 120.0(8) . . . C3 C4 C5 119.8(8) . . . N1 C5 C4 124.1(7) . . . C3 C6 C7 126.4(8) . . . C6 C7 C8 127.5(8) . . . C7 C8 C12 122.6(7) . . . C7 C8 C9 120.5(8) . . . C9 C8 C12 116.9(8) . . . C8 C9 C10 118.8(9) . . . C9 C10 N2 124.3(8) . . . C10 N2 C11 115.5(8) . . . N2 C11 C12 125.9(9) . . . C8 C12 C11 118.2(8) . . . C13 N3 C17 114.9(9) . . . N3 C13 C14 124(1) . . . C13 C14 C15 120(1) . . . C14 C15 C18 118.5(9) . . . C14 C15 C16 117.9(9) . . . C16 C15 C18 123.5(9) . . . C15 C16 C17 118.5(9) . . . C15 C18 C18 125(1) . . 2_745 N3 C17 C16 125(1) . . . Co1 O1 C19 133.8(5) . . . O5 Cl1 O6 110.7(7) . . . O4 Cl1 O6 112.0(6) . . . O4 Cl1 O5 106.5(7) . . . O3 Cl1 O6 107.9(8) . . . O3 Cl1 O5 109.5(9) . . . O3 Cl1 O4 110.2(7) . . .