# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_r-3c _database_code_depnum_ccdc_archive 'CCDC 915782' #TrackingRef '16195_web_deposit_cif_file_0_AndresVega_1355489654.Fe_OHCO_3_HOHCO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe (C H O2)3 6 (C H2 O2)' _chemical_formula_sum 'C3 H3 Fe O6' _chemical_formula_weight 190.90 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 8.2420(10) _cell_length_b 8.2420(10) _cell_length_c 22.569(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1327.7(3) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2220 _cell_measurement_theta_min 3.376 _cell_measurement_theta_max 24.924 _exptl_crystal_description cube _exptl_crystal_colour Brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_process_details 'SADABS (BRUKER)' _exptl_special_details ; 20 sec frames separated by 0.3 deg each ; _diffrn_ambient_temperature 298(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 'Siemens SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 270 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0055 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 24.97 _reflns_number_total 270 _reflns_number_gt 264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 2001)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXTL-NT (Bruker, 1999)' _computing_structure_refinement 'SHELXTL-NT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL-NT (Bruker, 1999)' _computing_publication_material 'SHELXTL-NT (Bruker, 1999)' _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^)+(0.0383P)^2^+1.0101P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 270 _refine_ls_number_parameters 18 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0174 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0510 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.6667 0.3333 0.3333 0.0235(2) Uani 1 6 d S . . O1 O 0.65881(14) 0.11594(14) 0.38745(4) 0.0383(3) Uani 1 1 d . . . C1 C 0.7893(3) 0.1226(3) 0.4167 0.0325(4) Uani 1 2 d S . . H1 H 0.9021 0.2355 0.4167 0.039 Uiso 1 2 calc SR . . 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 0.0237(3) 0.0237(3) 0.0232(3) 0.000 0.000 0.01183(13) O1 0.0362(6) 0.0362(6) 0.0427(6) 0.0069(4) -0.0055(4) 0.0183(4) C1 0.0319(7) 0.0319(7) 0.0360(9) -0.0005(4) 0.0005(4) 0.0176(8) _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 2.1425(10) 2_655 ? Fe1 O1 2.1425(9) . Y Fe1 O1 2.1425(9) 31_655 ? Fe1 O1 2.1425(9) 3_665 ? Fe1 O1 2.1425(9) 32 ? Fe1 O1 2.1425(9) 33_545 ? O1 C1 1.239(3) . Y C1 O1 1.239(3) 10_545 ? 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 90.72(4) 2_655 . Y O1 Fe1 O1 89.28(4) 2_655 31_655 Y O1 Fe1 O1 180.0 . 31_655 Y O1 Fe1 O1 90.72(4) 2_655 3_665 ? O1 Fe1 O1 90.72(4) . 3_665 ? O1 Fe1 O1 89.28(4) 31_655 3_665 ? O1 Fe1 O1 180.0 2_655 32 ? O1 Fe1 O1 89.28(4) . 32 ? O1 Fe1 O1 90.72(4) 31_655 32 ? O1 Fe1 O1 89.28(4) 3_665 32 ? O1 Fe1 O1 89.28(4) 2_655 33_545 ? O1 Fe1 O1 89.28(4) . 33_545 ? O1 Fe1 O1 90.72(4) 31_655 33_545 ? O1 Fe1 O1 180.0 3_665 33_545 ? O1 Fe1 O1 90.72(4) 32 33_545 ? Fe1 Fe1 Fe1 132.797(5) 10_545 1_565 ? C1 O1 Fe1 127.12(11) . . Y O1 C1 O1 125.7(2) 10_545 . Y loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.001 0.000 0.250 75.2 25.3 2 -0.001 0.000 0.750 75.3 25.3 3 0.333 0.666 0.417 73.6 25.3 4 0.333 0.666 0.917 73.5 25.3 5 0.666 0.333 0.083 73.6 25.3 6 0.666 0.333 0.583 73.6 25.3 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.154 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.042