Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Kumagai, Hitoshi' ; Groupe des Materiaux Inorganiques Institut de Physique et Chimie des Materiaux de Strasbourg 23 rue du Loess 67037 Strasbourg Cedex France Present Address: Applied Molecular Science Institute of Molecular Science Nishigounaka 38, Myoudaiji, Okazaki 444-8585 Japan ; 'Oka, Yoshimi' ; Applied Molecular Science Institute of Molecular Science Nishigounaka 38, Myoudaiji, Okazaki 444-8585 Japan ; 'Inoue, Katsuya' ; Applied Molecular Science Institute of Molecular Science Nishigounaka 38, Myoudaiji, Okazaki 444-8585 Japan ; 'Kurmoo, Mohamedally' ; Groupe des Materiaux Inorganiques Institut de Physique et Chimie des Materiaux de Strasbourg 23 rue du Loess 67037 Strasbourg Cedex France ; _publ_contact_author_name 'Dr MOHAMEDALLY KURMOO' _publ_contact_author_address ; GMI IPCMS 23 rue du Loess Strasbourg 67037 FRANCE ; _publ_contact_author_phone '+33 3 88 10 71 33' _publ_contact_author_fax '+33 3 88 10 72 47' _publ_contact_author_email kurmoo@ipcms.u-strasbg.fr _publ_requested_journal J. C. S. Dalton.' _publ_section_title ; Hydrothermal synthesis, structure, and magnetism of square grid cobaltII-carboxylate compounds with and without pillars ; _publ_requested_coeditor_name ; ? ; #============================================================================= _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; data_5/14B _database_code_CSD 182521 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H18 Co O6 ' _chemical_formula_moiety 'C18 H18 Co O6 ' _chemical_formula_weight 389.27 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 36.564(5) _cell_length_b 6.4037(9) _cell_length_c 7.327(1) _cell_angle_alpha 90 _cell_angle_beta 92.101(4) _cell_angle_gamma 90 _cell_volume 1714.5(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 288.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.005 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 3986 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 28.40 _diffrn_measured_fraction_theta_max 0.9098 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.9098 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1957 _reflns_number_gt 1394 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1272 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1957 _refine_ls_number_parameters 115 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.81 _refine_diff_density_min -0.67 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Co' 'Co' 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.5000 0.0236(2) Uani 1.00 d S . . O1 O 0.22071(6) 0.1641(4) 0.2604(3) 0.0314(6) Uani 1.00 d . . . O2 O 0.20911(6) 0.1635(4) 0.6719(3) 0.0325(6) Uani 1.00 d . . . O3 O 0.27708(7) -0.0374(4) 0.5150(3) 0.0342(7) Uani 1.00 d . . . C1 C 0.19931(9) 0.0081(5) 0.2374(4) 0.0266(8) Uani 1.00 d . . . C2 C 0.16081(10) 0.0247(6) 0.2874(5) 0.0347(10) Uani 1.00 d . . . C3 C 0.14653(10) 0.1980(6) 0.3525(5) 0.0352(10) Uani 1.00 d . . . C4 C 0.10858(10) 0.2252(6) 0.4036(5) 0.0368(10) Uani 1.00 d . . . C5 C 0.0815(1) 0.0806(7) 0.3624(6) 0.047(1) Uani 1.00 d . . . C6 C 0.0461(1) 0.1155(8) 0.4130(7) 0.056(1) Uani 1.00 d . . . C7 C 0.0371(1) 0.2915(8) 0.5052(7) 0.058(1) Uani 1.00 d . . . C8 C 0.0634(1) 0.4372(8) 0.5479(7) 0.059(1) Uani 1.00 d . . . C9 C 0.0989(1) 0.4065(7) 0.4955(6) 0.050(1) Uani 1.00 d . . . H1 H 0.1451 -0.0966 0.2573 0.0485 Uiso 1.00 calc . . . H2 H 0.1635 0.3122 0.3774 0.0485 Uiso 1.00 calc . . . H3 H 0.0851 -0.0473 0.2876 0.0485 Uiso 1.00 calc . . . H4 H 0.0261 0.0237 0.4060 0.0485 Uiso 1.00 calc . . . H5 H 0.0121 0.3092 0.5486 0.0485 Uiso 1.00 calc . . . H6 H 0.0592 0.5762 0.5915 0.0485 Uiso 1.00 calc . . . H7 H 0.1179 0.4785 0.5421 0.0485 Uiso 1.00 calc . . . H8 H 0.2678 -0.1468 0.5877 0.0410 Uiso 1.00 calc . . . H9 H 0.2987 -0.0586 0.4493 0.0410 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0298(3) 0.0179(3) 0.0234(3) -0.0007(3) 0.0031(2) -0.0011(3) O1 0.038(1) 0.028(1) 0.028(1) -0.006(1) -0.0002(10) -0.003(1) O2 0.036(1) 0.026(1) 0.036(1) 0.000(1) 0.007(1) 0.005(1) O3 0.047(1) 0.022(1) 0.034(1) 0.003(1) 0.010(1) 0.004(1) C1 0.034(2) 0.025(2) 0.020(2) -0.001(1) 0.000(1) 0.001(1) C2 0.035(2) 0.031(2) 0.038(2) -0.002(2) 0.003(2) -0.004(2) C3 0.034(2) 0.038(2) 0.034(2) 0.002(2) 0.000(1) -0.006(2) C4 0.036(2) 0.040(2) 0.034(2) 0.010(2) 0.003(1) -0.001(2) C5 0.042(2) 0.048(2) 0.050(2) 0.003(2) 0.006(2) -0.010(2) C6 0.038(2) 0.066(3) 0.065(3) -0.003(2) 0.010(2) 0.001(3) C7 0.038(2) 0.072(4) 0.066(3) 0.015(2) 0.013(2) 0.004(3) C8 0.060(3) 0.057(3) 0.061(3) 0.025(2) 0.010(2) -0.013(2) C9 0.044(2) 0.054(3) 0.053(3) 0.009(2) -0.001(2) -0.016(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 CO1 CO1 4.866 . 4_555 yes CO1 CO1 4.866 . 4_554 yes CO1 CO1 4.866 . 4_564 yes CO1 CO1 4.866 . 4_565 yes CO1 O1 2.096(2) . . yes CO1 O1 3.460(2) . 4_555 yes CO1 O1 3.460(2) . 6_555 yes CO1 O1 5.739(2) . 7_555 yes CO1 O1 4.360(2) . 6_545 yes CO1 O1 5.739(2) . 1_556 yes CO1 O1 2.096(2) . 7_556 yes CO1 O1 4.360(2) . 4_565 yes CO1 O2 2.066(2) . . yes CO1 O2 5.833(2) . 4_555 yes CO1 O2 5.833(2) . 6_555 yes CO1 O2 4.675(2) . 6_546 yes CO1 O2 3.842(2) . 4_554 yes CO1 O2 3.842(2) . 6_556 yes CO1 O2 2.066(2) . 7_556 yes CO1 O2 4.675(2) . 4_564 yes CO1 O3 2.091(2) . . yes CO1 O3 4.099(2) . 4_555 yes CO1 O3 4.099(2) . 6_555 yes CO1 O3 4.670(2) . 7_546 yes CO1 O3 3.965(2) . 4_554 yes CO1 O3 3.965(2) . 6_556 yes CO1 O3 2.091(2) . 7_556 yes CO1 O3 4.670(2) . 1_565 yes CO1 C1 3.046(3) . . yes CO1 C1 3.071(3) . 4_555 yes CO1 C1 3.071(3) . 6_555 yes CO1 C1 5.981(3) . 7_555 yes CO1 C1 5.410(3) . 6_545 yes CO1 C1 5.517(3) . 7_546 yes CO1 C1 5.981(3) . 1_556 yes CO1 C1 3.046(3) . 7_556 yes CO1 C1 5.517(3) . 1_565 yes CO1 C1 5.410(3) . 4_565 yes CO1 C2 3.843(4) . . yes CO1 C2 4.321(4) . 4_555 yes CO1 C2 4.321(4) . 6_555 yes CO1 C2 3.843(4) . 7_556 yes CO1 C3 3.911(4) . . yes CO1 C3 5.471(4) . 4_555 yes CO1 C3 5.471(4) . 6_555 yes CO1 C3 5.848(4) . 6_545 yes CO1 C3 3.911(4) . 7_556 yes CO1 C3 5.848(4) . 4_565 yes CO1 C4 5.196(4) . . yes CO1 C4 5.196(4) . 7_556 yes CO1 C9 5.613(4) . . yes CO1 C9 5.613(4) . 7_556 yes CO1 H1 4.724 . . no CO1 H1 4.447 . 4_555 no CO1 H1 4.447 . 6_555 no CO1 H1 5.907 . 7_546 no CO1 H1 4.724 . 7_556 no CO1 H1 5.907 . 1_565 no CO1 H2 3.279 . . no CO1 H2 5.590 . 4_555 no CO1 H2 5.590 . 6_555 no CO1 H2 5.113 . 6_545 no CO1 H2 3.279 . 7_556 no CO1 H2 5.113 . 4_565 no CO1 H7 5.068 . . no CO1 H7 5.068 . 7_556 no CO1 H8 2.694 . . no CO1 H8 4.381 . 4_555 no CO1 H8 4.381 . 6_555 no CO1 H8 3.966 . 7_546 no CO1 H8 3.183 . 4_554 no CO1 H8 3.183 . 6_556 no CO1 H8 2.694 . 7_556 no CO1 H8 3.966 . 1_565 no CO1 H9 2.694 . . no CO1 H9 3.883 . 4_555 no CO1 H9 3.883 . 6_555 no CO1 H9 4.792 . 7_546 no CO1 H9 4.635 . 4_554 no CO1 H9 4.635 . 6_556 no CO1 H9 2.694 . 7_556 no CO1 H9 4.792 . 1_565 no O1 O1 4.224(2) . 4_555 yes O1 O1 3.859(3) . 6_555 yes O1 O1 4.579(5) . 7_555 yes O1 O1 3.859(3) . 6_545 yes O1 O1 4.224(2) . 4_554 yes O1 O1 4.192(4) . 7_556 yes O1 O1 5.650(4) . 4_564 yes O1 O1 5.650(4) . 4_565 yes O1 O2 3.060(3) . . yes O1 O2 5.238(3) . 6_555 yes O1 O2 5.244(3) . 6_545 yes O1 O2 5.778(3) . 6_546 yes O1 O2 5.901(3) . 7_546 yes O1 O2 4.318(3) . 1_554 yes O1 O2 2.232(3) . 4_554 yes O1 O2 5.773(3) . 6_556 yes O1 O2 2.821(3) . 7_556 yes O1 O2 4.373(3) . 4_564 yes O1 O3 3.019(3) . . yes O1 O3 5.886(3) . 4_555 yes O1 O3 2.783(3) . 6_555 yes O1 O3 4.927(3) . 6_545 yes O1 O3 4.337(3) . 7_546 yes O1 O3 2.900(3) . 4_554 yes O1 O3 5.640(3) . 6_556 yes O1 O3 2.901(3) . 7_556 yes O1 O3 5.796(3) . 1_565 yes O1 C1 1.276(4) . . yes O1 C1 3.774(4) . 4_555 yes O1 C1 3.661(4) . 6_555 yes O1 C1 5.201(4) . 7_555 yes O1 C1 5.119(4) . 6_545 yes O1 C1 4.037(4) . 4_554 yes O1 C1 5.070(4) . 7_556 yes O1 C1 5.462(4) . 1_565 yes O1 C2 2.380(4) . . yes O1 C2 4.668(4) . 4_555 yes O1 C2 4.933(4) . 6_555 yes O1 C2 5.981(4) . 6_545 yes O1 C2 4.209(4) . 4_554 yes O1 C2 5.715(4) . 7_556 yes O1 C2 5.936(4) . 1_565 yes O1 C3 2.827(4) . . yes O1 C3 5.694(4) . 4_555 yes O1 C3 5.784(4) . 6_545 yes O1 C3 4.591(4) . 4_554 yes O1 C3 5.602(4) . 7_556 yes O1 C3 5.690(4) . 4_564 yes O1 C4 4.287(4) . . yes O1 C4 5.392(4) . 4_554 yes O1 C5 5.200(5) . . yes O1 C5 5.983(5) . 4_554 yes O1 C9 5.076(5) . . yes O1 C9 5.524(5) . 4_564 yes O1 H1 3.230 . . no O1 H1 4.673 . 4_555 no O1 H1 5.148 . 6_555 no O1 H1 4.548 . 4_554 no O1 H1 5.482 . 1_565 no O1 H2 2.477 . . no O1 H2 5.900 . 4_555 no O1 H2 5.916 . 1_545 no O1 H2 4.932 . 6_545 no O1 H2 4.596 . 4_554 no O1 H2 4.915 . 7_556 no O1 H2 4.802 . 4_564 no O1 H3 5.150 . . no O1 H3 5.990 . 4_554 no O1 H7 4.798 . . no O1 H7 5.761 . 4_554 no O1 H7 4.636 . 4_564 no O1 H8 3.518 . . no O1 H8 2.868 . 6_555 no O1 H8 5.807 . 6_545 no O1 H8 3.516 . 7_546 no O1 H8 5.644 . 1_554 no O1 H8 2.177 . 4_554 no O1 H8 4.931 . 6_556 no O1 H8 3.306 . 7_556 no O1 H8 5.280 . 1_565 no O1 H9 3.433 . . no O1 H9 5.745 . 4_555 no O1 H9 2.436 . 6_555 no O1 H9 5.801 . 7_555 no O1 H9 4.920 . 6_545 no O1 H9 4.492 . 7_546 no O1 H9 3.776 . 4_554 no O1 H9 3.394 . 7_556 no O1 H9 5.876 . 1_565 no O2 O2 4.220(2) . 4_555 yes O2 O2 4.500(3) . 6_546 yes O2 O2 4.220(2) . 4_554 yes O2 O2 4.500(3) . 6_556 yes O2 O2 4.131(5) . 7_556 yes O2 O2 5.678(5) . 7_557 yes O2 O2 5.657(4) . 4_564 yes O2 O2 5.657(4) . 4_565 yes O2 O3 3.060(3) . . yes O2 O3 3.563(3) . 4_555 yes O2 O3 5.426(3) . 6_555 yes O2 O3 5.057(3) . 6_546 yes O2 O3 4.273(3) . 7_546 yes O2 O3 5.556(4) . 4_554 yes O2 O3 3.017(3) . 6_556 yes O2 O3 2.813(3) . 7_556 yes O2 O3 5.822(3) . 1_565 yes O2 C1 3.342(4) . . yes O2 C1 1.256(4) . 4_555 yes O2 C1 5.081(4) . 6_555 yes O2 C1 5.476(4) . 7_546 yes O2 C1 4.290(4) . 1_556 yes O2 C1 5.810(4) . 6_556 yes O2 C1 3.989(4) . 7_556 yes O2 C1 5.340(4) . 4_565 yes O2 C2 3.388(4) . . yes O2 C2 2.323(4) . 4_555 yes O2 C2 4.983(4) . 1_556 yes O2 C2 5.157(4) . 7_556 yes O2 C2 5.565(4) . 4_565 yes O2 C3 3.220(4) . . yes O2 C3 3.545(4) . 4_555 yes O2 C3 5.567(4) . 1_556 yes O2 C3 5.362(4) . 7_556 yes O2 C3 4.892(4) . 4_565 yes O2 C4 4.123(4) . . yes O2 C4 4.801(4) . 4_555 yes O2 C4 5.673(4) . 4_565 yes O2 C5 5.141(5) . . yes O2 C5 5.162(5) . 4_555 yes O2 C8 5.650(5) . . yes O2 C9 4.466(5) . . yes O2 C9 5.990(5) . 4_555 yes O2 C9 5.490(5) . 4_565 yes O2 H1 4.119 . . no O2 H1 2.484 . 4_555 no O2 H1 5.234 . 1_556 no O2 H2 2.842 . . no O2 H2 3.809 . 4_555 no O2 H2 5.572 . 1_556 no O2 H2 4.686 . 7_556 no O2 H2 4.062 . 4_565 no O2 H3 5.419 . . no O2 H3 4.702 . 4_555 no O2 H7 3.984 . . no O2 H7 5.571 . 1_545 no O2 H7 4.940 . 4_565 no O2 H8 3.004 . . no O2 H8 3.663 . 4_555 no O2 H8 5.789 . 6_555 no O2 H8 5.534 . 6_546 no O2 H8 3.924 . 7_546 no O2 H8 4.859 . 4_554 no O2 H8 2.277 . 6_556 no O2 H8 3.745 . 7_556 no O2 H8 4.959 . 1_565 no O2 H9 3.975 . . no O2 H9 3.850 . 4_555 no O2 H9 4.886 . 6_555 no O2 H9 5.406 . 6_546 no O2 H9 3.982 . 7_546 no O2 H9 3.319 . 6_556 no O2 H9 2.693 . 7_556 no O3 O3 3.6949(6) . 4_555 yes O3 O3 5.357(4) . 6_555 yes O3 O3 5.357(4) . 6_545 yes O3 O3 5.151(4) . 6_546 yes O3 O3 3.369(5) . 7_546 yes O3 O3 3.6949(6) . 4_554 yes O3 O3 5.151(4) . 6_556 yes O3 O3 4.182(5) . 7_556 yes O3 C1 3.447(4) . . yes O3 C1 3.334(4) . 4_555 yes O3 C1 4.060(4) . 6_555 yes O3 C1 3.572(4) . 6_545 yes O3 C1 3.606(4) . 7_546 yes O3 C1 3.925(4) . 7_556 yes O3 C2 4.527(4) . . yes O3 C2 4.763(4) . 4_555 yes O3 C2 4.837(4) . 6_555 yes O3 C2 4.278(4) . 6_545 yes O3 C2 4.093(4) . 7_546 yes O3 C2 4.218(4) . 7_556 yes O3 C3 5.105(4) . . yes O3 C3 5.552(4) . 4_555 yes O3 C3 4.299(4) . 6_545 yes O3 C3 5.586(4) . 6_546 yes O3 C3 5.142(4) . 7_546 yes O3 C3 3.643(4) . 7_556 yes O3 C4 5.490(4) . 6_545 yes O3 C4 4.653(4) . 7_556 yes O3 C5 5.981(5) . 7_556 yes O3 C8 5.902(5) . 7_556 yes O3 C9 5.994(5) . 6_545 yes O3 C9 5.688(5) . 6_546 yes O3 C9 4.614(5) . 7_556 yes O3 H1 5.133 . . no O3 H1 5.275 . 4_555 no O3 H1 4.524 . 6_555 no O3 H1 5.033 . 6_545 no O3 H1 4.004 . 7_546 no O3 H1 5.199 . 7_556 no O3 H2 4.791 . . no O3 H2 5.310 . 4_555 no O3 H2 5.941 . 1_545 no O3 H2 3.791 . 6_545 no O3 H2 4.975 . 6_546 no O3 H2 5.462 . 7_546 no O3 H2 2.700 . 7_556 no O3 H3 5.832 . 7_546 no O3 H7 5.707 . 6_545 no O3 H7 4.937 . 6_546 no O3 H7 3.897 . 7_556 no O3 H8 0.950 . . no O3 H8 4.384 . 4_555 no O3 H8 5.284 . 6_555 no O3 H8 5.171 . 6_546 no O3 H8 2.694 . 7_546 no O3 H8 3.352 . 4_554 no O3 H8 4.216 . 6_556 no O3 H8 4.729 . 7_556 no O3 H8 5.739 . 1_565 no O3 H9 0.950 . . no O3 H9 3.308 . 4_555 no O3 H9 5.288 . 6_555 no O3 H9 5.450 . 6_545 no O3 H9 5.918 . 6_546 no O3 H9 3.806 . 7_546 no O3 H9 4.293 . 4_554 no O3 H9 5.769 . 6_556 no O3 H9 4.729 . 7_556 no C1 C1 3.6652(2) . 4_555 yes C1 C1 4.896(5) . 6_555 yes C1 C1 4.896(5) . 6_545 yes C1 C1 3.6652(2) . 4_554 yes C1 C2 1.471(5) . . yes C1 C2 4.322(5) . 4_555 yes C1 C2 5.987(5) . 6_545 yes C1 C2 3.544(5) . 4_554 yes C1 C3 2.456(5) . . yes C1 C3 5.140(5) . 4_555 yes C1 C3 5.609(5) . 1_545 yes C1 C3 3.609(5) . 4_554 yes C1 C4 3.836(5) . . yes C1 C4 4.316(5) . 4_554 yes C1 C5 4.462(5) . . yes C1 C5 5.057(5) . 4_554 yes C1 C6 5.835(5) . . yes C1 C8 5.851(6) . 4_554 yes C1 C9 4.906(5) . . yes C1 C9 5.692(5) . 1_545 yes C1 C9 4.815(5) . 4_554 yes C1 C9 5.495(5) . 4_564 yes C1 H1 2.104 . . no C1 H1 4.396 . 4_555 no C1 H1 4.015 . 4_554 no C1 H2 2.580 . . no C1 H2 5.326 . 4_555 no C1 H2 4.766 . 1_545 no C1 H2 5.267 . 6_545 no C1 H2 3.553 . 4_554 no C1 H2 5.779 . 7_556 no C1 H2 5.231 . 4_564 no C1 H3 4.220 . . no C1 H3 5.915 . 4_555 no C1 H3 5.230 . 4_554 no C1 H6 5.836 . 4_564 no C1 H7 4.838 . . no C1 H7 5.083 . 1_545 no C1 H7 4.507 . 4_554 no C1 H7 4.627 . 4_564 no C1 H8 3.656 . . no C1 H8 3.495 . 6_555 no C1 H8 4.992 . 6_545 no C1 H8 2.886 . 7_546 no C1 H8 5.549 . 1_554 no C1 H8 2.909 . 4_554 no C1 H8 5.509 . 6_556 no C1 H8 4.439 . 7_556 no C1 H9 3.922 . . no C1 H9 3.096 . 6_555 no C1 H9 3.880 . 6_545 no C1 H9 5.800 . 7_545 no C1 H9 3.681 . 7_546 no C1 H9 4.281 . 4_554 no C1 H9 4.206 . 7_556 no C2 C2 3.6774(6) . 4_555 yes C2 C2 3.6774(6) . 4_554 yes C2 C3 1.323(5) . . yes C2 C3 4.428(5) . 4_555 yes C2 C3 5.343(5) . 1_545 yes C2 C3 3.513(5) . 4_554 yes C2 C3 5.923(5) . 4_564 yes C2 C4 2.478(5) . . yes C2 C4 5.218(5) . 4_555 yes C2 C4 5.542(5) . 1_545 yes C2 C4 3.705(5) . 4_554 yes C2 C4 5.851(5) . 4_564 yes C2 C5 2.994(5) . . yes C2 C5 5.246(6) . 4_555 yes C2 C5 4.232(5) . 4_554 yes C2 C6 4.367(6) . . yes C2 C6 5.009(6) . 4_554 yes C2 C7 5.143(6) . . yes C2 C7 5.306(6) . 4_554 yes C2 C8 4.878(6) . . yes C2 C8 5.566(6) . 1_545 yes C2 C8 4.904(6) . 4_554 yes C2 C8 5.213(6) . 4_564 yes C2 C9 3.698(6) . . yes C2 C9 4.834(6) . 1_545 yes C2 C9 4.119(6) . 4_554 yes C2 C9 4.754(6) . 4_564 yes C2 H1 0.988 . . no C2 H1 3.542 . 4_555 no C2 H1 3.933 . 4_554 no C2 H1 5.659 . 1_565 no C2 H2 1.957 . . no C2 H2 4.830 . 4_555 no C2 H2 4.610 . 1_545 no C2 H2 3.703 . 4_554 no C2 H2 5.204 . 4_564 no C2 H3 2.806 . . no C2 H3 4.676 . 4_555 no C2 H3 4.511 . 4_554 no C2 H4 5.034 . . no C2 H4 5.583 . 4_554 no C2 H6 5.642 . . no C2 H6 5.255 . 1_545 no C2 H6 5.502 . 4_554 no C2 H6 4.689 . 4_564 no C2 H7 3.822 . . no C2 H7 4.289 . 1_545 no C2 H7 3.984 . 4_554 no C2 H7 3.951 . 4_564 no C2 H8 4.551 . . no C2 H8 4.396 . 6_555 no C2 H8 5.778 . 6_545 no C2 H8 3.652 . 7_546 no C2 H8 4.298 . 4_554 no C2 H8 5.598 . 6_556 no C2 H8 4.832 . 7_556 no C2 H9 5.164 . . no C2 H9 3.537 . 6_555 no C2 H9 4.398 . 6_545 no C2 H9 3.823 . 7_546 no C2 H9 5.702 . 4_554 no C2 H9 4.171 . 7_556 no C3 C3 4.456(4) . 4_555 yes C3 C3 4.456(4) . 4_554 yes C3 C3 5.328(5) . 4_564 yes C3 C3 5.328(5) . 4_565 yes C3 C4 1.461(5) . . yes C3 C4 5.097(5) . 4_555 yes C3 C4 4.444(5) . 4_554 yes C3 C4 5.105(5) . 4_564 yes C3 C4 5.682(5) . 4_565 yes C3 C5 2.498(5) . . yes C3 C5 4.843(6) . 4_555 yes C3 C5 4.595(6) . 4_554 yes C3 C6 3.753(6) . . yes C3 C6 5.957(6) . 4_555 yes C3 C6 5.199(6) . 4_554 yes C3 C7 4.236(6) . . yes C3 C7 5.618(6) . 4_554 yes C3 C7 5.694(6) . 4_564 yes C3 C8 3.735(6) . . yes C3 C8 5.945(6) . 1_545 yes C3 C8 5.501(6) . 4_554 yes C3 C8 4.379(6) . 4_564 yes C3 C9 2.459(6) . . yes C3 C9 5.473(6) . 1_545 yes C3 C9 4.952(6) . 4_554 yes C3 C9 3.994(6) . 4_564 yes C3 C9 5.679(6) . 4_565 yes C3 H1 2.011 . . no C3 H1 3.039 . 4_555 no C3 H1 4.407 . 4_554 no C3 H1 4.570 . 1_565 no C3 H2 0.973 . . no C3 H2 5.068 . 4_555 no C3 H2 5.708 . 1_545 no C3 H2 4.831 . 4_554 no C3 H2 4.743 . 4_564 no C3 H2 4.984 . 4_565 no C3 H3 2.767 . . no C3 H3 4.082 . 4_555 no C3 H3 4.735 . 4_554 no C3 H3 5.343 . 1_565 no C3 H4 4.575 . . no C3 H4 5.574 . 4_554 no C3 H5 5.222 . . no C3 H6 4.419 . . no C3 H6 5.433 . 1_545 no C3 H6 3.935 . 4_564 no C3 H7 2.522 . . no C3 H7 4.936 . 1_545 no C3 H7 4.986 . 4_554 no C3 H7 3.223 . 4_564 no C3 H7 5.596 . 4_565 no C3 H8 5.190 . . no C3 H8 4.685 . 6_555 no C3 H8 4.729 . 7_546 no C3 H8 4.915 . 4_554 no C3 H8 5.166 . 6_556 no C3 H8 4.262 . 7_556 no C3 H9 5.819 . . no C3 H9 3.414 . 6_555 no C3 H9 5.718 . 6_545 no C3 H9 4.762 . 7_546 no C3 H9 5.645 . 6_556 no C3 H9 3.353 . 7_556 no C4 C4 4.662(5) . 4_555 yes C4 C4 4.662(5) . 4_554 yes C4 C4 5.081(5) . 4_564 yes C4 C4 5.081(5) . 4_565 yes C4 C5 1.382(6) . . yes C4 C5 4.045(6) . 4_555 yes C4 C5 4.501(6) . 4_554 yes C4 C5 5.573(6) . 1_565 yes C4 C5 5.683(6) . 4_565 yes C4 C6 2.394(6) . . yes C4 C6 4.953(6) . 4_555 yes C4 C6 4.723(6) . 4_554 yes C4 C6 5.948(6) . 4_564 yes C4 C7 2.776(6) . . yes C4 C7 5.073(6) . 4_554 yes C4 C7 4.937(6) . 4_564 yes C4 C8 2.411(6) . . yes C4 C8 5.425(6) . 1_545 yes C4 C8 5.215(6) . 4_554 yes C4 C8 3.726(6) . 4_564 yes C4 C8 5.501(6) . 4_565 yes C4 C9 1.395(6) . . yes C4 C9 5.951(6) . 4_555 yes C4 C9 5.299(6) . 1_545 yes C4 C9 5.035(6) . 4_554 yes C4 C9 3.814(6) . 4_564 yes C4 C9 4.961(6) . 4_565 yes C4 H1 2.698 . . no C4 H1 2.987 . 4_555 no C4 H1 5.034 . 4_554 no C4 H1 4.679 . 1_565 no C4 H2 2.101 . . no C4 H2 5.237 . 4_555 no C4 H2 5.596 . 4_554 no C4 H2 5.315 . 4_564 no C4 H2 4.936 . 4_565 no C4 H3 2.109 . . no C4 H3 3.183 . 4_555 no C4 H3 4.703 . 4_554 no C4 H3 4.807 . 1_565 no C4 H4 3.282 . . no C4 H4 5.498 . 2_555 no C4 H4 5.100 . 4_555 no C4 H4 4.912 . 4_554 no C4 H4 5.406 . 3_556 no C4 H4 5.938 . 1_565 no C4 H5 3.762 . . no C4 H5 5.445 . 2_555 no C4 H5 5.501 . 4_554 no C4 H5 5.603 . 3_556 no C4 H5 5.238 . 4_564 no C4 H5 5.346 . 3_566 no C4 H6 3.223 . . no C4 H6 4.754 . 1_545 no C4 H6 5.875 . 4_554 no C4 H6 3.130 . 4_564 no C4 H6 5.563 . 4_565 no C4 H7 1.937 . . no C4 H7 4.897 . 1_545 no C4 H7 5.244 . 4_554 no C4 H7 3.286 . 4_564 no C4 H7 5.049 . 4_565 no C4 H8 5.938 . 6_555 no C4 H8 5.843 . 7_546 no C4 H8 5.811 . 6_556 no C4 H8 5.264 . 7_556 no C4 H9 4.555 . 6_555 no C4 H9 5.533 . 7_546 no C4 H9 5.893 . 6_556 no C4 H9 4.117 . 7_556 no C5 C5 3.806(2) . 4_555 yes C5 C5 3.806(2) . 4_554 yes C5 C6 1.378(6) . . yes C5 C6 5.017(6) . 2_555 yes C5 C6 4.462(7) . 4_555 yes C5 C6 3.713(6) . 4_554 yes C5 C6 5.157(6) . 3_556 yes C5 C7 2.382(6) . . yes C5 C7 5.198(6) . 2_555 yes C5 C7 5.573(7) . 4_555 yes C5 C7 5.421(7) . 1_545 yes C5 C7 3.853(6) . 4_554 yes C5 C7 5.072(6) . 3_556 yes C5 C7 5.034(7) . 4_564 yes C5 C8 2.750(7) . . yes C5 C8 4.396(7) . 1_545 yes C5 C8 4.078(7) . 4_554 yes C5 C8 3.895(7) . 4_564 yes C5 C8 5.954(7) . 4_565 yes C5 C9 2.381(6) . . yes C5 C9 5.608(6) . 4_555 yes C5 C9 4.466(6) . 1_545 yes C5 C9 4.182(6) . 4_554 yes C5 C9 4.306(6) . 4_564 yes C5 C9 5.701(6) . 4_565 yes C5 H1 2.724 . . no C5 H1 3.647 . 4_555 no C5 H1 5.082 . 4_554 no C5 H1 5.821 . 1_565 no C5 H2 3.346 . . no C5 H2 5.362 . 4_555 no C5 H2 5.762 . 1_545 no C5 H2 5.361 . 4_554 no C5 H3 0.997 . . no C5 H3 3.122 . 4_555 no C5 H3 4.223 . 4_554 no C5 H3 5.614 . 1_565 no C5 H4 2.095 . . no C5 H4 4.346 . 2_555 no C5 H4 4.584 . 4_555 no C5 H4 3.903 . 4_554 no C5 H4 4.390 . 3_556 no C5 H5 3.271 . . no C5 H5 4.706 . 2_555 no C5 H5 5.741 . 1_545 no C5 H5 4.187 . 4_554 no C5 H5 5.792 . 2_556 no C5 H5 4.303 . 3_556 no C5 H5 5.154 . 4_564 no C5 H5 5.249 . 3_566 no C5 H6 3.695 . . no C5 H6 3.743 . 1_545 no C5 H6 4.709 . 4_554 no C5 H6 3.051 . 4_564 no C5 H6 5.861 . 4_565 no C5 H6 5.616 . 3_566 no C5 H7 3.142 . . no C5 H7 4.272 . 1_545 no C5 H7 4.509 . 4_554 no C5 H7 3.935 . 4_564 no C5 H7 5.837 . 4_565 no C5 H9 5.522 . 6_555 no C5 H9 5.643 . 7_546 no C5 H9 5.480 . 7_556 no C6 C6 4.057(9) . 2_555 yes C6 C6 3.951(4) . 4_555 yes C6 C6 3.951(4) . 4_554 yes C6 C6 3.934(9) . 3_556 yes C6 C7 1.361(7) . . yes C6 C7 4.384(6) . 2_555 yes C6 C7 5.083(7) . 4_555 yes C6 C7 5.331(7) . 1_545 yes C6 C7 3.969(7) . 4_554 yes C6 C7 5.445(7) . 2_556 yes C6 C7 4.066(7) . 3_556 yes C6 C7 4.836(7) . 4_564 yes C6 C7 5.785(7) . 4_565 yes C6 C7 4.916(7) . 3_566 yes C6 C8 2.362(7) . . yes C6 C8 5.539(7) . 2_555 yes C6 C8 5.861(7) . 4_555 yes C6 C8 4.495(7) . 1_545 yes C6 C8 4.495(7) . 4_554 yes C6 C8 5.359(7) . 3_556 yes C6 C8 3.986(7) . 4_564 yes C6 C8 5.481(7) . 4_565 yes C6 C8 4.940(7) . 3_566 yes C6 C9 2.737(6) . . yes C6 C9 5.703(7) . 4_555 yes C6 C9 4.962(7) . 1_545 yes C6 C9 4.970(7) . 4_554 yes C6 C9 4.785(7) . 4_564 yes C6 C9 5.543(7) . 4_565 yes C6 H1 4.068 . . no C6 H1 4.337 . 4_555 no C6 H2 4.493 . . no C6 H3 2.016 . . no C6 H3 5.073 . 2_555 no C6 H3 3.079 . 4_555 no C6 H3 4.869 . 4_554 no C6 H3 5.365 . 3_556 no C6 H3 5.632 . 1_565 no C6 H4 0.938 . . no C6 H4 3.509 . 2_555 no C6 H4 3.818 . 4_555 no C6 H4 3.864 . 4_554 no C6 H4 5.759 . 2_556 no C6 H4 3.125 . 3_556 no C6 H4 5.862 . 1_565 no C6 H5 2.041 . . no C6 H5 4.119 . 2_555 no C6 H5 5.573 . 4_555 no C6 H5 5.411 . 1_545 no C6 H5 3.978 . 4_554 no C6 H5 4.716 . 2_556 no C6 H5 3.469 . 3_556 no C6 H5 4.691 . 4_564 no C6 H5 4.268 . 3_566 no C6 H6 3.257 . . no C6 H6 3.718 . 1_545 no C6 H6 5.048 . 4_554 no C6 H6 5.868 . 3_556 no C6 H6 3.124 . 4_564 no C6 H6 5.355 . 4_565 no C6 H6 4.326 . 3_566 no C6 H7 3.607 . . no C6 H7 4.924 . 1_545 no C6 H7 5.410 . 4_554 no C6 H7 4.644 . 4_564 no C6 H7 5.833 . 4_565 no C7 C7 4.539(9) . 2_555 yes C7 C7 5.231(7) . 4_555 yes C7 C7 5.231(7) . 4_554 yes C7 C7 4.577(10) . 2_556 yes C7 C7 4.614(10) . 3_556 yes C7 C7 4.534(6) . 4_564 yes C7 C7 4.534(6) . 4_565 yes C7 C7 3.805(9) . 3_566 yes C7 C8 1.368(7) . . yes C7 C8 5.451(7) . 2_555 yes C7 C8 5.562(7) . 1_545 yes C7 C8 5.845(7) . 4_554 yes C7 C8 5.098(7) . 2_556 yes C7 C8 5.944(7) . 3_556 yes C7 C8 3.926(7) . 4_564 yes C7 C8 4.413(7) . 4_565 yes C7 C8 4.071(7) . 3_566 yes C7 C9 2.381(6) . . yes C7 C9 4.839(7) . 4_564 yes C7 C9 4.601(6) . 4_565 yes C7 C9 5.336(6) . 3_566 yes C7 H1 5.058 . . no C7 H1 4.474 . 4_555 no C7 H1 5.896 . 1_565 no C7 H2 4.752 . . no C7 H2 5.859 . 4_565 no C7 H3 3.246 . . no C7 H3 5.346 . 2_555 no C7 H3 3.089 . 4_555 no C7 H3 5.818 . 4_554 no C7 H3 5.021 . 3_556 no C7 H3 4.874 . 1_565 no C7 H3 5.525 . 4_565 no C7 H4 1.900 . . no C7 H4 4.104 . 2_555 no C7 H4 3.599 . 4_555 no C7 H4 4.835 . 4_554 no C7 H4 5.255 . 2_556 no C7 H4 3.153 . 3_556 no C7 H4 4.760 . 1_565 no C7 H4 5.991 . 2_565 no C7 H4 5.302 . 4_565 no C7 H4 5.010 . 3_566 no C7 H5 0.987 . . no C7 H5 4.379 . 2_555 no C7 H5 5.635 . 4_555 no C7 H5 5.158 . 4_554 no C7 H5 3.790 . 2_556 no C7 H5 4.258 . 3_556 no C7 H5 4.283 . 4_564 no C7 H5 4.847 . 4_565 no C7 H5 3.142 . 3_566 no C7 H6 2.084 . . no C7 H6 5.807 . 2_555 no C7 H6 4.690 . 1_545 no C7 H6 5.023 . 2_556 no C7 H6 3.277 . 4_564 no C7 H6 4.425 . 4_565 no C7 H6 3.667 . 3_566 no C7 H7 3.189 . . no C7 H7 5.987 . 1_545 no C7 H7 4.811 . 4_564 no C7 H7 5.052 . 4_565 no C7 H7 5.853 . 3_566 no C8 C8 5.594(10) . 2_556 yes C8 C8 3.751(2) . 4_564 yes C8 C8 3.751(2) . 4_565 yes C8 C8 4.734(10) . 3_566 yes C8 C9 1.381(6) . . yes C8 C9 4.411(7) . 4_564 yes C8 C9 3.624(6) . 4_565 yes C8 H1 5.059 . . no C8 H1 3.960 . 4_555 no C8 H1 4.777 . 1_565 no C8 H1 5.363 . 4_565 no C8 H2 3.992 . . no C8 H2 4.600 . 4_565 no C8 H3 3.742 . . no C8 H3 3.138 . 4_555 no C8 H3 3.908 . 1_565 no C8 H3 4.345 . 4_565 no C8 H4 3.139 . . no C8 H4 5.290 . 2_555 no C8 H4 4.210 . 4_555 no C8 H4 5.677 . 4_554 no C8 H4 5.890 . 2_556 no C8 H4 4.428 . 3_556 no C8 H4 5.953 . 4_564 no C8 H4 4.117 . 1_565 no C8 H4 5.923 . 2_565 no C8 H4 4.576 . 4_565 no C8 H4 4.777 . 3_566 no C8 H5 2.049 . . no C8 H5 5.148 . 2_555 no C8 H5 4.199 . 2_556 no C8 H5 5.551 . 3_556 no C8 H5 4.364 . 4_564 no C8 H5 5.892 . 1_565 no C8 H5 4.487 . 4_565 no C8 H5 3.257 . 3_566 no C8 H6 0.960 . . no C8 H6 5.525 . 1_545 no C8 H6 5.363 . 2_556 no C8 H6 3.343 . 4_564 no C8 H6 3.993 . 4_565 no C8 H6 4.564 . 3_566 no C8 H7 2.011 . . no C8 H7 4.305 . 4_564 no C8 H7 4.104 . 4_565 no C8 H9 5.101 . 7_556 no C9 C9 3.854(3) . 4_564 yes C9 C9 3.854(3) . 4_565 yes C9 H1 4.061 . . no C9 H1 3.198 . 4_555 no C9 H1 4.029 . 1_565 no C9 H1 5.081 . 4_565 no C9 H2 2.616 . . no C9 H2 5.841 . 4_555 no C9 H2 5.488 . 4_564 no C9 H2 4.021 . 4_565 no C9 H3 3.311 . . no C9 H3 3.195 . 4_555 no C9 H3 5.680 . 4_554 no C9 H3 3.841 . 1_565 no C9 H3 4.664 . 4_565 no C9 H4 3.662 . . no C9 H4 5.879 . 2_555 no C9 H4 4.932 . 4_555 no C9 H4 5.701 . 4_554 no C9 H4 5.407 . 3_556 no C9 H4 4.798 . 1_565 no C9 H4 5.481 . 4_565 no C9 H4 5.912 . 3_566 no C9 H5 3.274 . . no C9 H5 5.618 . 2_555 no C9 H5 5.386 . 2_556 no C9 H5 4.834 . 4_564 no C9 H5 5.547 . 4_565 no C9 H5 4.448 . 3_566 no C9 H6 1.963 . . no C9 H6 5.563 . 1_545 no C9 H6 3.250 . 4_564 no C9 H6 4.653 . 4_565 no C9 H6 5.796 . 3_566 no C9 H7 0.890 . . no C9 H7 5.991 . 1_545 no C9 H7 3.497 . 4_564 no C9 H7 4.106 . 4_565 no C9 H8 5.666 . 6_556 no C9 H8 5.168 . 7_556 no C9 H9 5.058 . 6_555 no C9 H9 5.431 . 6_556 no C9 H9 3.875 . 7_556 no #------------------------------------------------------------------------------ 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 CO1 CO1 CO1 97.7 4_555 . 4_554 yes CO1 CO1 CO1 180.0 4_555 . 4_564 yes CO1 CO1 CO1 82.3 4_555 . 4_565 yes CO1 CO1 O1 116.35(7) 4_555 . . yes CO1 CO1 O1 21.84(4) 4_555 . 4_555 yes CO1 CO1 O1 158.16(4) 4_555 . 6_555 yes CO1 CO1 O1 143.06(2) 4_555 . 7_555 yes CO1 CO1 O1 76.71(3) 4_555 . 6_545 yes CO1 CO1 O1 36.94(2) 4_555 . 1_556 yes CO1 CO1 O1 63.65(7) 4_555 . 7_556 yes CO1 CO1 O1 103.29(3) 4_555 . 4_565 yes CO1 CO1 O2 49.03(7) 4_555 . . yes CO1 CO1 O2 19.73(2) 4_555 . 4_555 yes CO1 CO1 O2 160.27(2) 4_555 . 6_555 yes CO1 CO1 O2 24.90(3) 4_555 . 6_546 yes CO1 CO1 O2 90.40(4) 4_555 . 4_554 yes CO1 CO1 O2 89.60(4) 4_555 . 6_556 yes CO1 CO1 O2 130.97(7) 4_555 . 7_556 yes CO1 CO1 O2 155.10(3) 4_555 . 4_564 yes CO1 CO1 O3 52.71(7) 4_555 . . yes CO1 CO1 O3 25.16(3) 4_555 . 4_555 yes CO1 CO1 O3 154.84(3) 4_555 . 6_555 yes CO1 CO1 O3 50.87(3) 4_555 . 7_546 yes CO1 CO1 O3 117.12(3) 4_555 . 4_554 yes CO1 CO1 O3 62.88(3) 4_555 . 6_556 yes CO1 CO1 O3 127.29(7) 4_555 . 7_556 yes CO1 CO1 O3 129.13(3) 4_555 . 1_565 yes CO1 CO1 C1 97.13(6) 4_555 . . yes CO1 CO1 C1 37.12(6) 4_555 . 4_555 yes CO1 CO1 C1 142.88(6) 4_555 . 6_555 yes CO1 CO1 C1 149.24(3) 4_555 . 7_555 yes CO1 CO1 C1 70.96(3) 4_555 . 6_545 yes CO1 CO1 C1 33.66(3) 4_555 . 7_546 yes CO1 CO1 C1 30.76(3) 4_555 . 1_556 yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_690Cocarboxycinna _database_code_CSD 182522 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C10 H10 Co O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Co O6' _chemical_formula_weight 285.12 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #============================================================================ # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.3236(4) _cell_length_b 6.6084(4) _cell_length_c 7.2011(6) _cell_angle_alpha 90 _cell_angle_beta 101.948(5) _cell_angle_gamma 90 _cell_volume 527.2(1) _cell_formula_units_Z 2 _cell_measurement_temperature 294 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.81 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 294 _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K¥a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '¥p scans' _diffrn_measurement_details ; 2237 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 25. mm. Scan angle = 2.0 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 5.90 Omega = 0.00 Kappa = 0.00 90 frames Set 2 Theta = -4.70 Kappa = -169.50 Phi = 0.00 22 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2237 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1317 _reflns_number_gt 1061 _reflns_threshold_expression >3.0¥s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #============================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1061 _refine_ls_number_parameters 88 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_all 0.077 _refine_ls_wR_factor_ref 0.071 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.709 _refine_diff_density_min -0.647 #============================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CO 1.0000 0.0000 1.0000 0.0147(3) 0.500 Uani ? ? Co O1 0.9137(3) 0.0824(5) 1.2215(4) 0.017(1) 1.000 Uani ? ? O O2 1.0885(3) 0.2776(5) 1.0153(5) 0.021(1) 1.000 Uani ? ? O O3 1.1424(3) -0.1088(5) 1.2094(5) 0.020(1) 1.000 Uani ? ? O C1 1.1659(4) -0.2804(7) 1.2777(6) 0.016(2) 1.000 Uani ? ? C C2 1.2955(4) -0.3296(8) 1.3568(7) 0.023(2) 1.000 Uani ? ? C C3 1.3850(9) -0.195(2) 1.374(2) 0.027(5) 0.500 Uani ? ? C C4 0.5074(8) -0.249(2) 0.948(2) 0.022(4) 0.500 Uani ? ? C C5 0.5452(5) -0.070(1) 1.005(1) 0.039(3) 1.000 Uani ? ? C C6 0.6700(5) -0.019(1) 1.0777(9) 0.034(3) 1.000 Uani ? ? C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol CO 0.0136(3) 0.0139(4) 0.0167(3) 0.0019(3) -0.0000(3) 0.0002(3) Co O1 0.014(1) 0.021(1) 0.018(1) 0.004(1) 0.002(1) -0.002(1) O O2 0.022(1) 0.017(1) 0.025(1) -0.002(1) 0.003(1) 0.001(1) O O3 0.013(1) 0.020(2) 0.031(2) -0.000(1) -0.001(1) 0.008(1) O C1 0.013(2) 0.021(2) 0.015(2) 0.004(2) 0.001(1) 0.000(2) C C2 0.016(2) 0.030(3) 0.027(2) 0.002(2) 0.001(2) 0.003(2) C C3 0.021(4) 0.027(5) 0.034(5) 0.009(4) 0.002(4) 0.011(4) C C4 0.013(4) 0.023(4) 0.039(5) -0.000(4) 0.002(4) -0.007(4) C C5 0.032(3) 0.038(3) 0.049(3) -0.018(2) -0.013(3) 0.000(3) C C6 0.022(2) 0.042(3) 0.043(3) -0.012(2) -0.008(2) 0.001(3) C # 10. MOLECULAR GEOMETRY 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 CO O1 2.107(3) . . ? CO O1 2.107(3) . 3_757 ? CO O2 2.083(3) . . ? CO O2 2.083(3) . 3_757 ? CO O3 2.094(3) . . ? CO O3 2.094(3) . 3_757 ? O1 C1 1.280(6) . 2_757 ? O3 C1 1.243(6) . . ? C1 C2 1.496(6) . . ? C2 C3 1.33(1) . . ? C2 C6 1.366(8) . 2_747 ? C3 C4 1.43(1) . 4_645 ? C4 C5 1.29(1) . . ? C5 C5 1.37(1) . 3_657 ? C5 C6 1.443(7) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 O1 CO O1 180.00 . . 3_757 ? O1 CO O2 91.5(1) . . . ? O1 CO O2 88.5(1) . . 3_757 ? O1 CO O3 87.3(1) . . . ? O1 CO O3 92.7(1) . . 3_757 ? O1 CO O2 88.5(1) . 3_757 . ? O1 CO O2 91.5(1) . 3_757 3_757 ? O1 CO O3 92.7(1) . 3_757 . ? O1 CO O3 87.3(1) . 3_757 3_757 ? O2 CO O2 180.00 . . 3_757 ? O2 CO O3 88.5(1) . . . ? O2 CO O3 91.5(1) . . 3_757 ? O2 CO O3 91.5(1) . 3_757 . ? O2 CO O3 88.5(1) . 3_757 3_757 ? O3 CO O3 180.00 . . 3_757 ? CO O1 C1 128.6(3) . . 2_757 ? CO O3 C1 132.0(3) . . . ? O1 C1 O3 123.7(4) . 2_747 . ? O1 C1 C2 118.7(4) . 2_747 . ? O3 C1 C2 117.5(4) . . . ? C1 C2 C3 123.9(6) . . . ? C1 C2 C6 121.3(5) . . 2_747 ? C3 C2 C6 114.8(6) . . 2_747 ? C2 C3 C4 121.7(9) . . 4_645 ? C3 C4 C5 125.8(9) . 4_444 . ? C4 C5 C5 114.2(7) . . 3_657 ? C4 C5 C6 124.4(7) . . . ? C5 C5 C6 121.4(7) . 3_657 . ? C2 C6 C5 122.1(6) . 2_757 . ?