# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof M Julve' _publ_contact_author_address ; Departament de Quimica Inorganica, Facultat de Quimica de la Universitat de Valencia Dr.Moliner, 50 Valencia Burjassot 46100 SPAIN ; _publ_contact_author_phone '34 963864856' _publ_contact_author_fax '34 963864322' _publ_contact_author_email miguel.julve@uv.es _publ_contact_letter ; Dear Sir I am sending the cif file of the paper XXXXXXXX: Oxalate and 2,2'-bipyrimidine as bischelating ligands in the honeycomb layered compound {[Fe2(bpym)(ox)2] . 5H2O}n The compound has been identified in the paper with number 1. For further comunications or informations contact me at this E-mail address: miguel.julve@uv.es Yours sincerely Miguel Julve ; _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _publ_section_title ; Oxalate and 2,2'-bipyrimidine as bischelating ligands in the honeycomb layered compound {[Fe2(bpym)(ox)2] . 5H2O}n ; loop_ _publ_author_name _publ_author_address 'Donatella Armentano' ; Dipartimento di Chimica Università degli Studi della Calabria, P. Bucci 15/c I-87030 Arcavacata di Rende, Cosenza Italy ; 'Giovanni De Munno' ; Dipartimento di Chimica Università degli Studi della Calabria, P. Bucci 15/c I-87030 Arcavacata di Rende, Cosenza Italy ; 'Francesc Lloret' ; Departament de Química Inorgànica/Instituto de Ciencia Molecular Facultat de Química de la Universitat de València, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Miguel Julve' ; Departament de Química Inorgànica/Instituto de Ciencia Molecular Facultat de Química de la Universitat de València, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Jacques Curely' ; Centre de Physique Molécularie Optique et Hertzienne, Université Bordeaux I, 351 Cours de la Libération, 33405- Talence Cédex, France ; 'Amy M. Babb' ; Department of Chemistry, University of Houston-Clear Lake, Houston TX 77058, USA ; ; J.Y.Lu ; ; Department of Chemistry, University of Houston-Clear Lake, Houston TX 77058, USA ; #=============================================================================== # 5. CHEMICAL DATA #=============================================================================== data_1 _database_code_CSD 189567 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Fe2 N4 O13' _chemical_formula_weight 544.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.674(3) _cell_length_b 16.940(4) _cell_length_c 6.1570(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.60(2) _cell_angle_gamma 90.00 _cell_volume 988.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7277 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1256 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.06 _reflns_number_total 1123 _reflns_number_gt 876 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+3.0615P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1123 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.67191(4) 0.0000 0.0343(3) Uani 1 2 d S . . O1 O 0.3396(3) 0.68065(16) 0.1837(4) 0.0447(7) Uani 1 1 d . . . O2 O 0.3613(3) 0.75500(16) -0.1902(4) 0.0429(7) Uani 1 1 d . . . N1 N 0.4165(3) 0.57003(16) -0.2039(5) 0.0317(7) Uani 1 1 d . . . C1 C 0.4542(5) 0.5000 -0.1122(8) 0.0289(10) Uani 1 2 d S . . C2 C 0.2437(4) 0.7283(2) 0.1087(6) 0.0339(8) Uani 1 1 d . . . C3 C 0.3360(4) 0.5695(2) -0.4090(6) 0.0409(9) Uani 1 1 d . . . H3A H 0.3079 0.6173 -0.4787 0.049 Uiso 1 1 calc R . . C4 C 0.2943(6) 0.5000 -0.5184(10) 0.0477(14) Uani 1 2 d S . . H4A H 0.2399 0.5000 -0.6613 0.057 Uiso 1 2 calc SR . . O3 O 1.0000 0.3388(7) 0.5000 0.079(4) Uani 0.50 2 d SP . . O4 O 0.9153(15) 0.4530(10) 0.149(2) 0.171(7) Uani 0.50 1 d P . . O5 O 0.9586(14) 0.6199(10) 0.284(3) 0.208(9) Uani 0.50 1 d P . . 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 Fe1 0.0360(4) 0.0250(4) 0.0425(5) 0.000 0.0091(3) 0.000 O1 0.0461(15) 0.0435(15) 0.0477(16) 0.0224(14) 0.0169(12) 0.0147(13) O2 0.0441(15) 0.0447(15) 0.0441(15) 0.0136(13) 0.0187(13) 0.0089(13) N1 0.0320(15) 0.0298(15) 0.0325(15) 0.0038(13) 0.0044(12) -0.0005(12) C1 0.029(2) 0.029(2) 0.028(2) 0.000 0.006(2) 0.000 C2 0.0382(19) 0.0295(17) 0.0345(19) 0.0063(16) 0.0082(16) -0.0028(16) C3 0.044(2) 0.039(2) 0.038(2) 0.0099(18) 0.0020(17) 0.0016(17) C4 0.044(3) 0.065(4) 0.031(3) 0.000 0.001(3) 0.000 O3 0.119(10) 0.065(7) 0.064(7) 0.000 0.048(7) 0.000 O4 0.129(10) 0.25(2) 0.147(10) 0.001(11) 0.058(8) 0.030(10) O5 0.118(11) 0.183(16) 0.34(3) 0.168(17) 0.093(16) 0.019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.101(3) . ? Fe1 O1 2.101(3) 2_655 ? Fe1 O2 2.126(3) 2_655 ? Fe1 O2 2.126(3) . ? Fe1 N1 2.191(3) . ? Fe1 N1 2.191(3) 2_655 ? O1 C2 1.246(4) . ? O2 C2 1.253(4) 7_565 ? N1 C1 1.333(4) . ? N1 C3 1.344(5) . ? C1 N1 1.333(3) 6_565 ? C1 C1 1.484(9) 5_665 ? C2 O2 1.253(4) 7_565 ? C2 C2 1.553(7) 7_565 ? C3 C4 1.376(5) . ? C4 C3 1.376(5) 6_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_3 _geom_angle_publ_flag O1 Fe1 O1 171.91(15) . 2_655 ? O1 Fe1 O2 96.28(11) . 2_655 ? O1 Fe1 O2 78.31(10) 2_655 2_655 ? O1 Fe1 O2 78.31(10) . . ? O1 Fe1 O2 96.28(11) 2_655 . ? O2 Fe1 O2 97.10(16) 2_655 . ? O1 Fe1 N1 97.86(11) . . ? O1 Fe1 N1 88.53(10) 2_655 . ? O2 Fe1 N1 163.00(10) 2_655 . ? O2 Fe1 N1 94.97(11) . . ? O1 Fe1 N1 88.53(10) . 2_655 ? O1 Fe1 N1 97.86(11) 2_655 2_655 ? O2 Fe1 N1 94.97(11) 2_655 2_655 ? O2 Fe1 N1 163.00(10) . 2_655 ? N1 Fe1 N1 76.05(15) . 2_655 ? C2 O1 Fe1 114.9(2) . . ? C2 O2 Fe1 113.7(2) 7_565 . ? C1 N1 C3 116.7(3) . . ? C1 N1 Fe1 114.9(2) . . ? C3 N1 Fe1 128.4(2) . . ? N1 C1 N1 125.8(4) 6_565 . ? N1 C1 C1 117.1(2) 6_565 5_665 ? N1 C1 C1 117.1(2) . 5_665 ? O1 C2 O2 126.9(3) . 7_565 ? O1 C2 C2 116.4(4) . 7_565 ? O2 C2 C2 116.7(4) 7_565 7_565 ? N1 C3 C4 121.5(4) . . ? C3 C4 C3 117.7(5) . 6_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.437 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.084