data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Merged_cif_files_deposit_reviewed.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-11-10 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Cheetham, Anthony K.' # Name of author for correspondence _publ_contact_author_address ;Department of Materials Science and Metallurgy University of Cambridge Cambridge CB2 3QZ, UK ; # Address of author for correspondence _publ_contact_author_email akc30@cam.ac.uk _publ_contact_author_fax +44(0)1223767061 _publ_contact_author_phone +44(0)1223334567 _publ_contact_letter ; Submission dated :2010-11-10 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as part of a journal submission Dalton Transactions Cheetham, Anthony K. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; Detailed Investigations of Phase Transitions and Magnetic Structure in Fe(III), Co(II), Mn(II) and Ni(II) 3,4,5-trihydroxybenzoate (gallate) dihydrates by Neutron and X-ray diffraction ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' P.J.Saines ; ? ; ;Department of Materials Science and Metallurgy University of Cambridge Cambridge CB2 3QZ, UK ; H.H.-M.Yeung ; ? ; ;Department of Materials Science and Metallurgy University of Cambridge Cambridge CB2 3QZ, UK ; J.R.Hester ; ? ; ;Bragg Institute, ANSTO Locked bag 2001 Kirrawee DC NSW 2232 Australia ; A.R.Lennie ; ? ; ;Diamond Light Source Ltd. Harwell Science and Innovation Campus Didcot OX11 ODE, U.K. ; A.K.Cheetham ; ? ; ;Department of Materials Science and Metallurgy University of Cambridge Cambridge CB2 3QZ, UK ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_nigallate_p1 _database_code_depnum_ccdc_archive 'CCDC 803624' #TrackingRef '- Merged_cif_files_deposit.cif' _audit_creation_date 2010-11-10T10:01:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C7 H4 Ni O5, 2(H2 O)' _chemical_formula_sum 'C7 H8 Ni O7' _chemical_formula_weight 262.84 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2"' _symmetry_Int_Tables_number 152 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 8.8079(3) _cell_length_b 8.8079(3) _cell_length_c 21.1663(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1422.06(7) _cell_formula_units_Z 6 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6087 _cell_measurement_theta_min 2.8319 _cell_measurement_theta_max 29.1629 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rhombohedral _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.0831 _exptl_crystal_size_min 0.0561 _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_number 16110 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 29.23 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 2410 _reflns_number_gt 2204 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0310P)^2^+1.2462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 2410 _refine_ls_number_parameters 161 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(15) _refine_diff_density_max 0.399 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ni1 Ni 0.03473(3) 0.98102(3) 0.082815(12) 0.00732(8) Uani 1 1 d . . . O6 O 0.0986(2) 1.0986(2) 0 0.0116(4) Uani 1 2 d S . . O8 O -0.2142(2) 0.8113(2) 0.05265(7) 0.0111(3) Uani 1 1 d . . . O1 O 0 0.8714(2) 0.1667 0.0104(4) Uani 1 2 d S . . O7 O 0.3035(2) 1.1736(2) 0.09919(7) 0.0149(4) Uani 1 1 d D . . O3 O -0.0393(2) 1.1520(2) 0.11524(7) 0.0121(3) Uani 1 1 d . . . O2 O 0.1021(2) 0.7829(2) 0.06322(7) 0.0140(3) Uani 1 1 d D . . C1 C 0 0.7205(4) 0.1667 0.0099(7) Uani 1 2 d S . . C3 C 0 1.2366(4) 0.1667 0.0117(7) Uani 1 2 d S . . C8 C -0.2670(4) 0.7330(4) 0 0.0118(7) Uani 1 2 d S . . C6 C 0.2492(4) 1.2492(4) 0 0.0104(6) Uani 1 2 d S . . C9 C -0.4354(4) 0.5646(4) 0 0.0124(6) Uani 1 2 d S . . C7 C 0.3624(3) 1.2977(3) 0.05180(10) 0.0121(5) Uani 1 1 d D . . O9 O 0.6816(3) 0.1339(3) 0.04806(8) 0.0261(4) Uani 1 1 d D . . O10 O 0.5288(2) 0.8070(3) 0.12579(8) 0.0264(4) Uani 1 1 d D . . C5 C 0.0477(3) 1.5071(3) 0.11181(11) 0.0130(5) Uani 1 1 d . . . H5 H 0.0779 1.4679 0.0746 0.016 Uiso 1 1 calc R . . C10 C -0.4817(3) 0.4553(3) 0.05286(11) 0.0131(5) Uani 1 1 d . . . H10 H -0.4074 0.4888 0.0888 0.016 Uiso 1 1 calc R . . C2 C 0.0504(3) 0.6661(3) 0.11235(10) 0.0119(5) Uani 1 1 d D . . C4 C 0 1.4056(4) 0.1667 0.0136(7) Uani 1 2 d S . . H10A H 0.424(2) 0.718(4) 0.1187(18) 0.094(8) Uiso 1 1 d D . . H10B H 0.602(4) 0.801(5) 0.0992(16) 0.094(8) Uiso 1 1 d D . . H9B H 0.776(3) 0.158(5) 0.0693(17) 0.094(8) Uiso 1 1 d D . . H9A H 0.590(3) 0.045(4) 0.0658(17) 0.094(8) Uiso 1 1 d D . . H7 H 0.364(3) 1.214(3) 0.1331(7) 0.032(8) Uiso 1 1 d D . . H2 H 0.116(4) 0.746(3) 0.0276(6) 0.034(9) Uiso 1 1 d D . . 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 Ni1 0.00854(14) 0.00619(14) 0.00654(12) 0.00023(10) -0.00026(10) 0.00316(12) O6 0.0105(7) 0.0105(7) 0.0093(9) 0.0016(4) -0.0016(4) 0.0020(10) O8 0.0095(8) 0.0096(8) 0.0096(8) -0.0015(6) 0.0002(6) 0.0013(6) O1 0.0167(13) 0.0092(8) 0.0077(10) 0.0003(4) 0.0006(9) 0.0084(7) O7 0.0138(8) 0.0151(9) 0.0094(8) 0.0037(7) -0.0036(6) 0.0023(7) O3 0.0180(9) 0.0127(8) 0.0090(8) -0.0036(6) -0.0038(6) 0.0101(7) O2 0.0228(10) 0.0144(9) 0.0092(8) 0.0030(7) 0.0046(7) 0.0125(8) C1 0.0126(17) 0.0085(11) 0.0100(15) 0.0001(6) 0.0001(12) 0.0063(8) C3 0.0111(17) 0.0093(12) 0.0153(17) -0.0011(7) -0.0022(13) 0.0055(9) C8 0.0102(12) 0.0102(12) 0.0130(17) 0.0000(6) 0.0000(6) 0.0036(14) C6 0.0079(11) 0.0079(11) 0.0116(15) -0.0001(6) 0.0001(6) 0.0012(14) C9 0.0112(12) 0.0112(12) 0.0123(16) -0.0004(6) 0.0004(6) 0.0039(14) C7 0.0135(12) 0.0120(12) 0.0092(11) 0.0032(9) 0.0014(8) 0.0052(10) O9 0.0280(11) 0.0412(13) 0.0170(9) -0.0034(8) -0.0024(8) 0.0232(10) O10 0.0186(10) 0.0396(12) 0.0201(9) -0.0076(8) -0.0022(7) 0.0138(10) C5 0.0194(12) 0.0147(13) 0.0083(10) -0.0015(9) 0.0009(8) 0.0112(11) C10 0.0107(12) 0.0120(12) 0.0123(11) -0.0003(9) -0.0006(9) 0.0024(10) C2 0.0153(12) 0.0117(11) 0.0102(11) 0.0010(9) 0.0006(9) 0.0078(10) C4 0.0214(18) 0.0096(11) 0.0137(16) -0.0023(7) -0.0045(14) 0.0107(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ni1 O6 1.9695(9) . ? Ni1 O1 1.9701(9) . ? Ni1 O3 2.0359(15) . ? Ni1 O8 2.0424(16) . ? Ni1 O7 2.1412(16) . ? Ni1 O2 2.1463(16) . ? O6 C6 1.326(4) . ? O6 Ni1 1.9696(9) 6_465 ? O8 C8 1.270(2) . ? O1 C1 1.328(4) . ? O1 Ni1 1.9701(9) 5 ? O7 C7 1.380(3) . ? O3 C3 1.266(2) . ? O2 C2 1.370(3) . ? C1 C2 1.401(3) 5 ? C1 C2 1.401(3) . ? C3 O3 1.266(2) 5 ? C3 C4 1.489(5) . ? C8 O8 1.270(2) 6_465 ? C8 C9 1.483(5) . ? C6 C7 1.397(3) . ? C6 C7 1.397(3) 6_465 ? C9 C10 1.397(3) 6_465 ? C9 C10 1.397(3) . ? C7 C10 1.381(3) 1_665 ? C5 C2 1.389(3) 1_565 ? C5 C4 1.396(3) . ? C10 C7 1.381(3) 1_445 ? C2 C5 1.389(3) 1_545 ? C4 C5 1.396(3) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ni1 O1 173.28(5) . . ? O6 Ni1 O3 91.37(5) . . ? O1 Ni1 O3 91.74(7) . . ? O6 Ni1 O8 91.51(7) . . ? O1 Ni1 O8 94.37(4) . . ? O3 Ni1 O8 91.33(7) . . ? O6 Ni1 O7 79.37(7) . . ? O1 Ni1 O7 94.68(4) . . ? O3 Ni1 O7 89.74(6) . . ? O8 Ni1 O7 170.85(6) . . ? O6 Ni1 O2 97.65(4) . . ? O1 Ni1 O2 79.26(7) . . ? O3 Ni1 O2 170.97(6) . . ? O8 Ni1 O2 88.67(6) . . ? O7 Ni1 O2 91.70(7) . . ? C6 O6 Ni1 113.94(6) . . ? C6 O6 Ni1 113.94(6) . 6_465 ? Ni1 O6 Ni1 132.13(11) . 6_465 ? C8 O8 Ni1 129.74(16) . . ? C1 O1 Ni1 114.37(5) . 5 ? C1 O1 Ni1 114.37(5) . . ? Ni1 O1 Ni1 131.25(11) 5 . ? C7 O7 Ni1 109.80(13) . . ? C3 O3 Ni1 129.12(16) . . ? C2 O2 Ni1 109.89(13) . . ? O1 C1 C2 120.05(15) . 5 ? O1 C1 C2 120.05(15) . . ? C2 C1 C2 119.9(3) 5 . ? O3 C3 O3 126.3(3) 5 . ? O3 C3 C4 116.86(15) 5 . ? O3 C3 C4 116.86(15) . . ? O8 C8 O8 125.9(3) 6_465 . ? O8 C8 C9 117.05(15) 6_465 . ? O8 C8 C9 117.05(15) . . ? O6 C6 C7 120.64(15) . . ? O6 C6 C7 120.64(15) . 6_465 ? C7 C6 C7 118.7(3) . 6_465 ? C10 C9 C10 121.2(3) 6_465 . ? C10 C9 C8 119.38(16) 6_465 . ? C10 C9 C8 119.38(16) . . ? O7 C7 C10 125.2(2) . 1_665 ? O7 C7 C6 113.6(2) . . ? C10 C7 C6 121.3(2) 1_665 . ? C2 C5 C4 119.2(2) 1_565 . ? C7 C10 C9 118.7(2) 1_445 . ? O2 C2 C5 125.6(2) . 1_545 ? O2 C2 C1 114.2(2) . . ? C5 C2 C1 120.2(2) 1_545 . ? C5 C4 C5 121.3(3) . 5 ? C5 C4 C3 119.36(15) . . ? C5 C4 C3 119.36(15) 5 . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_fegall _database_code_depnum_ccdc_archive 'CCDC 803625' #TrackingRef '- Merged_cif_files_deposit.cif' _audit_creation_date 2010-11-10T11:14:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'fe gallate dihydrate' _chemical_formula_moiety 'C7 H3 Fe O5, 2(H2 O)' _chemical_formula_sum 'C7 H7 Fe1 O7' _chemical_formula_weight 258.98 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2"' _symmetry_Int_Tables_number 152 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 8.6716(4) _cell_length_b 8.6716(4) _cell_length_c 10.8650(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 707.55(6) _cell_formula_units_Z 3 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2114 _cell_measurement_theta_min 3.291 _cell_measurement_theta_max 29.1876 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.2393 _exptl_crystal_size_mid 0.0488 _exptl_crystal_size_min 0.0295 _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 393 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.604 _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_number 3367 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.918 _reflns_number_total 1114 _reflns_number_gt 1036 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0500P)^2^+0.9388P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1114 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_diff_density_max 0.99 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.05818(8) 0.05818(8) 0.5 0.00802(19) Uani 1 2 d S . . O1 O 0.1126(4) 0 0.3333 0.0099(6) Uani 1 2 d S . . O2 O 0.1204(4) 0.3129(3) 0.4703(2) 0.0156(6) Uani 1 1 d . . . O3 O -0.1891(4) -0.0227(4) 0.4353(2) 0.0168(6) Uani 1 1 d . . . C1 C 0.2694(6) 0 0.3333 0.0125(11) Uani 1 2 d S . . C2 C 0.3754(5) 0.0606(6) 0.4375(3) 0.0159(8) Uani 1 1 d . . . C5 C 0.5349(5) 0.0592(6) 0.4391(3) 0.0163(8) Uani 1 1 d . . . H5 H 0.6092 0.0974 0.5098 0.02 Uiso 1 1 calc R . . C4 C 0.5836(7) 0 0.3333 0.0172(12) Uani 1 2 d S . . C3 C -0.2453(6) 0 0.3333 0.0134(11) Uani 1 2 d S . . O4A O 0.1616(12) 0.4529(11) 0.2593(7) 0.0434(15) Uiso 0.47 1 d P . . O4B O 0.289(3) 0.541(2) 0.3035(16) 0.0434(15) Uiso 0.21 1 d P . . O4C O 0.4254(17) 0.5778(17) 0.4407(11) 0.0434(15) Uiso 0.32 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 0.0091(3) 0.0091(3) 0.0068(3) -0.00046(14) 0.00046(14) 0.0052(3) O1 0.0073(11) 0.0154(19) 0.0096(14) -0.0009(15) -0.0004(8) 0.0077(10) O2 0.0308(17) 0.0136(12) 0.0091(12) 0.0033(10) 0.0068(11) 0.0162(12) O3 0.0118(13) 0.0311(17) 0.0105(12) 0.0000(11) -0.0013(10) 0.0130(12) C1 0.0086(17) 0.018(3) 0.014(2) 0.000(2) 0.0000(11) 0.0088(14) C2 0.0144(18) 0.026(2) 0.0114(17) -0.0062(16) -0.0038(14) 0.0128(17) C5 0.0104(18) 0.031(2) 0.0119(15) -0.0035(15) -0.0025(14) 0.0134(17) C4 0.0151(18) 0.030(3) 0.012(2) -0.002(2) -0.0009(11) 0.0150(17) C3 0.0122(19) 0.020(3) 0.010(2) -0.002(2) -0.0010(11) 0.0102(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.9985(12) . ? Fe1 O1 1.9985(12) 2 ? Fe1 O3 2.020(3) . ? Fe1 O3 2.020(3) 4_556 ? Fe1 O2 2.020(3) . ? Fe1 O2 2.020(3) 4_556 ? O1 C1 1.360(6) . ? O1 Fe1 1.9984(12) 3_554 ? O2 C2 1.360(5) 4_556 ? O3 C3 1.264(4) . ? C1 C2 1.385(4) 5 ? C1 C2 1.385(4) . ? C2 O2 1.360(5) 4_556 ? C2 C5 1.388(5) . ? C5 C4 1.407(4) . ? C4 C5 1.407(4) 5 ? C4 C3 1.485(7) 1_655 ? C3 O3 1.264(4) 5 ? C3 C4 1.485(7) 1_455 ? O4A O4B 1.09(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_3 _geom_angle_publ_flag O1 Fe1 O1 179.05(10) . 2 ? O1 Fe1 O3 86.58(11) . . ? O1 Fe1 O3 92.76(8) 2 . ? O1 Fe1 O3 92.76(8) . 4_556 ? O1 Fe1 O3 86.58(11) 2 4_556 ? O3 Fe1 O3 90.45(17) . 4_556 ? O1 Fe1 O2 99.40(8) . . ? O1 Fe1 O2 81.25(11) 2 . ? O3 Fe1 O2 88.89(12) . . ? O3 Fe1 O2 167.76(10) 4_556 . ? O1 Fe1 O2 81.25(11) . 4_556 ? O1 Fe1 O2 99.40(8) 2 4_556 ? O3 Fe1 O2 167.76(10) . 4_556 ? O3 Fe1 O2 88.89(12) 4_556 4_556 ? O2 Fe1 O2 94.32(18) . 4_556 ? C1 O1 Fe1 111.23(9) . 3_554 ? C1 O1 Fe1 111.23(9) . . ? Fe1 O1 Fe1 137.53(17) 3_554 . ? C2 O2 Fe1 111.8(2) 4_556 . ? C3 O3 Fe1 132.5(3) . . ? O1 C1 C2 118.3(2) . 5 ? O1 C1 C2 118.3(2) . . ? C2 C1 C2 123.4(5) 5 . ? O2 C2 C1 115.5(4) 4_556 . ? O2 C2 C5 125.7(4) 4_556 . ? C1 C2 C5 118.8(4) . . ? C2 C5 C4 118.4(4) . . ? C5 C4 C5 122.3(5) . 5 ? C5 C4 C3 118.9(3) . 1_655 ? C5 C4 C3 118.9(3) 5 1_655 ? O3 C3 O3 124.8(5) 5 . ? O3 C3 C4 117.6(2) 5 1_455 ? O3 C3 C4 117.6(2) . 1_455 ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_20101020mngall _database_code_depnum_ccdc_archive 'CCDC 803626' #TrackingRef '- Merged_cif_files_deposit_reviewed.cif' _audit_creation_date 2010-11-10T16:02:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C7 H4 Mn1 O5, 2(H2 O)' _chemical_formula_sum 'C7 H8 Mn O7' _chemical_formula_weight 259.07 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2"' _symmetry_Int_Tables_number 152 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 9.0659(2) _cell_length_b 9.0659(2) _cell_length_c 21.7273(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1546.53(6) _cell_formula_units_Z 6 _cell_measurement_temperature 102(2) _cell_measurement_reflns_used 3757 _cell_measurement_theta_min 3.1949 _cell_measurement_theta_max 29.1602 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour brown _exptl_crystal_size_max 0.475 _exptl_crystal_size_mid 0.0859 _exptl_crystal_size_min 0.0657 _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 102(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_number 7041 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.2 _diffrn_reflns_theta_max 29.22 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.882 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2447 _reflns_number_gt 2207 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. The bond distances and angles of the hydrogens on the water and hydroxide groups molecule are restrained to a distance of 0.87. Additionally the bond angle of the water molecule and C-O-H bonds are restrained to angles of 1.42 and 1.86 radians. Hydrogens bonded to carbons were restrained using AFIX setting 43 and displacement parameter were set to 1.2 times the carbon on which they ride. Similarly hydrogens attached to oxygens have their thermals restrained to 1.5 times that of the atoms on which they ride. ; _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^)+(0.0405P)^2^+1.3108P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2447 _refine_ls_number_parameters 158 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_diff_density_max 0.490 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.080 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mn1 Mn 0.97805(5) 0.01724(4) 0.082936(18) 0.01348(13) Uani 1 1 d . . . O1 O 0.8910(3) -0.1090(3) 0.0000 0.0174(6) Uani 1 2 d S . . O2 O 0.6984(3) -0.1920(3) 0.09976(9) 0.0255(5) Uani 1 1 d D . . H2 H 0.636(4) -0.232(4) 0.1324(8) 0.038 Uiso 1 1 d D . . O3 O 1.2290(3) 0.1882(3) 0.04952(9) 0.0203(5) Uani 1 1 d . . . O6 O 1.0000 0.1351(3) 0.1667 0.0169(6) Uani 1 2 d S . . O7 O 0.9168(3) 0.2314(3) 0.06368(10) 0.0261(6) Uani 1 1 d D . . H7 H 0.899(5) 0.273(4) 0.0305(8) 0.039 Uiso 1 1 d D . . O8 O 1.0519(3) -0.1562(3) 0.11859(9) 0.0230(5) Uani 1 1 d . . . C1 C 0.7443(4) -0.2557(4) 0.0000 0.0163(9) Uani 1 2 d S . . C2 C 0.6378(4) -0.3072(4) 0.05151(13) 0.0193(6) Uani 1 1 d D . . C3 C 1.2743(5) 0.2743(5) 0.0000 0.0164(9) Uani 1 2 d S . . C4 C 1.4370(5) 0.4370(5) 0.0000 0.0184(9) Uani 1 2 d S . . C5 C 0.4874(4) -0.4605(4) 0.05266(13) 0.0189(6) Uani 1 1 d . . . H5 H 0.4188 -0.4961 0.0887 0.023 Uiso 1 1 calc R . . C6 C 1.0000 0.2827(5) 0.1667 0.0176(9) Uani 1 2 d S . . C7 C 0.9584(4) 0.3397(4) 0.11332(13) 0.0221(7) Uani 1 1 d D . . C8 C 1.0000 -0.2473(5) 0.1667 0.0193(9) Uani 1 2 d S . . C9 C 1.0000 -0.4109(5) 0.1667 0.0229(10) Uani 1 2 d S . . C10 C 0.9620(4) 0.4939(4) 0.11260(15) 0.0236(7) Uani 1 1 d . . . H10 H 0.9388 0.5346 0.0757 0.028 Uiso 1 1 calc R . . O10 O 0.4713(3) 0.1927(4) 0.12755(12) 0.0381(6) Uani 1 1 d D . . H10A H 0.478(5) 0.101(3) 0.134(2) 0.057 Uiso 1 1 d D . . H10B H 0.569(3) 0.276(3) 0.1153(18) 0.057 Uiso 1 1 d D . . O9 O 1.3220(4) -0.1311(4) 0.04558(12) 0.0429(7) Uani 1 1 d D . . H9A H 1.238(4) -0.224(3) 0.0306(18) 0.064 Uiso 1 1 d D . . H9B H 1.356(5) -0.149(5) 0.0812(11) 0.064 Uiso 1 1 d D . . 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 Mn1 0.0148(2) 0.0099(2) 0.0120(2) -0.00076(15) 0.00022(16) 0.00336(18) O1 0.0138(9) 0.0138(9) 0.0151(13) -0.0019(6) 0.0019(6) -0.0003(11) O2 0.0208(11) 0.0232(12) 0.0153(10) -0.0068(10) 0.0052(8) -0.0019(10) O3 0.0128(10) 0.0200(11) 0.0191(11) 0.0034(9) -0.0016(9) 0.0014(9) O6 0.0280(17) 0.0154(10) 0.0116(13) -0.0013(6) -0.0025(12) 0.0140(8) O7 0.0459(16) 0.0264(13) 0.0156(11) -0.0049(9) -0.0064(10) 0.0254(12) O8 0.0361(14) 0.0217(12) 0.0184(11) 0.0044(9) 0.0074(10) 0.0199(11) C1 0.0106(13) 0.0106(13) 0.017(2) -0.0012(9) 0.0012(9) -0.0023(16) C2 0.0189(15) 0.0185(15) 0.0138(14) -0.0039(12) 0.0002(12) 0.0043(13) C3 0.0135(14) 0.0135(14) 0.018(2) 0.0012(9) -0.0012(9) 0.0038(17) C4 0.0161(14) 0.0161(14) 0.015(2) 0.0018(9) -0.0018(9) 0.0024(17) C5 0.0149(15) 0.0150(15) 0.0166(14) 0.0022(12) 0.0035(12) -0.0001(12) C6 0.027(2) 0.0145(14) 0.015(2) 0.0006(9) 0.0012(18) 0.0136(12) C7 0.0325(18) 0.0258(17) 0.0148(14) -0.0037(13) -0.0023(13) 0.0197(15) C8 0.026(2) 0.0173(15) 0.018(2) 0.0024(10) 0.0047(19) 0.0130(12) C9 0.034(3) 0.0180(15) 0.022(2) 0.0010(10) 0.002(2) 0.0171(13) C10 0.0410(18) 0.0226(17) 0.0152(14) 0.0013(12) 0.0003(13) 0.0218(15) O10 0.0273(13) 0.0478(17) 0.0303(13) 0.0147(13) 0.0023(11) 0.0121(13) O9 0.056(2) 0.067(2) 0.0269(14) 0.0117(14) 0.0036(13) 0.0460(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Mn1 O1 2.0675(13) . ? Mn1 O6 2.0688(13) . ? Mn1 O8 2.139(2) . ? Mn1 O3 2.140(2) . ? Mn1 O7 2.308(2) . ? Mn1 O2 2.315(2) . ? O6 C6 1.337(5) . ? O6 Mn1 2.0688(13) 6_765 ? O1 C1 1.331(5) . ? O1 Mn1 2.0674(13) 4_645 ? O3 C3 1.268(3) . ? C8 O8 1.268(3) 6_765 ? C8 O8 1.268(3) . ? C8 C9 1.481(6) . ? O7 C7 1.377(4) . ? O2 C2 1.381(3) . ? C3 O3 1.268(3) 4_645 ? C3 C4 1.480(6) . ? C2 C5 1.379(4) . ? C2 C1 1.397(4) . ? C6 C7 1.401(4) 6_765 ? C6 C7 1.401(4) . ? C1 C2 1.397(4) 4_645 ? C5 C4 1.399(4) 1_445 ? C4 C5 1.399(4) 4_755 ? C4 C5 1.399(4) 1_665 ? C7 C10 1.379(4) . ? C10 C9 1.399(4) 1_565 ? C9 C10 1.399(4) 1_545 ? C9 C10 1.399(4) 6_755 ? 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 Mn1 O6 164.56(5) . . ? O1 Mn1 O8 94.73(6) . . ? O6 Mn1 O8 94.39(9) . . ? O1 Mn1 O3 94.48(9) . . ? O6 Mn1 O3 97.54(6) . . ? O8 Mn1 O3 92.54(10) . . ? O1 Mn1 O7 96.99(6) . . ? O6 Mn1 O7 74.12(8) . . ? O8 Mn1 O7 168.28(8) . . ? O3 Mn1 O7 86.79(9) . . ? O1 Mn1 O2 74.07(8) . . ? O6 Mn1 O2 93.89(6) . . ? O8 Mn1 O2 87.62(9) . . ? O3 Mn1 O2 168.52(8) . . ? O7 Mn1 O2 95.35(10) . . ? C6 O6 Mn1 117.95(7) . 6_765 ? C6 O6 Mn1 117.94(7) . . ? Mn1 O6 Mn1 124.11(14) 6_765 . ? C1 O1 Mn1 117.86(7) . 4_645 ? C1 O1 Mn1 117.86(7) . . ? Mn1 O1 Mn1 124.28(13) 4_645 . ? C3 O3 Mn1 129.2(2) . . ? O8 C8 O8 124.6(4) 6_765 . ? O8 C8 C9 117.7(2) 6_765 . ? O8 C8 C9 117.7(2) . . ? C7 O7 Mn1 111.45(18) . . ? C2 O2 Mn1 110.82(17) . . ? C8 O8 Mn1 128.6(2) . . ? O3 C3 O3 124.2(4) 4_645 . ? O3 C3 C4 117.89(19) 4_645 . ? O3 C3 C4 117.89(19) . . ? C5 C2 O2 124.4(3) . . ? C5 C2 C1 121.3(3) . . ? O2 C2 C1 114.3(3) . . ? O6 C6 C7 120.4(2) . 6_765 ? O6 C6 C7 120.4(2) . . ? C7 C6 C7 119.2(4) 6_765 . ? O1 C1 C2 120.70(19) . . ? O1 C1 C2 120.70(19) . 4_645 ? C2 C1 C2 118.6(4) . 4_645 ? C2 C5 C4 118.9(3) . 1_445 ? C5 C4 C5 120.9(4) 4_755 1_665 ? C5 C4 C3 119.6(2) 4_755 . ? C5 C4 C3 119.6(2) 1_665 . ? O7 C7 C10 125.1(3) . . ? O7 C7 C6 114.2(3) . . ? C10 C7 C6 120.6(3) . . ? C7 C10 C9 119.5(3) . 1_565 ? C10 C9 C10 120.5(4) 1_545 6_755 ? C10 C9 C8 119.7(2) 1_545 . ? C10 C9 C8 119.7(2) 6_755 . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- Mngallate_300K_reviewed.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_20101020mngall300k _database_code_depnum_ccdc_archive 'CCDC 803627' #TrackingRef '- Mngallate_300K_reviewed.cif' _audit_creation_date 2010-11-11T10:41:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C7 H4 Mn O5, 2(H2 O)' _chemical_formula_sum 'C7 H8 Mn O7' _chemical_formula_weight 259.07 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall 'P 32 2"' _symmetry_Int_Tables_number 154 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 9.0553(2) _cell_length_b 9.0553(2) _cell_length_c 10.8872(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 773.13(3) _cell_formula_units_Z 3 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 2409 _cell_measurement_theta_min 3.195 _cell_measurement_theta_max 29.1444 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour brown _exptl_crystal_size_max 0.4838 _exptl_crystal_size_mid 0.0994 _exptl_crystal_size_min 0.0574 _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 393 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0275 _diffrn_reflns_number 3485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.2 _diffrn_reflns_theta_max 29.144 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.87 _reflns_number_total 1213 _reflns_number_gt 1151 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. The bond distances and angles of the hydrogens on the water and hydroxide groups molecule are restrained to a distance of 0.87. Additionally the bond angle of the water molecule and C-O-H bonds are restrained to angles of 1.42 and 1.85 radians. Hydrogens bonded to carbons were restrained using AFIX setting 43 and displacement parameter were set to 1.2 times the carbon on which they ride. Similarly hydrogens attached to oxygens have their thermals restrained to 1.5 times that of the atoms on which they are bonded. ; _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^)+(0.0240P)^2^+0.0901P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1213 _refine_ls_number_parameters 80 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_diff_density_max 0.181 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.03001(4) 0.0000 0.1667 0.02198(11) Uani 1 2 d S . . O1 O 0.1227(2) 0.1227(2) 0.0000 0.0296(5) Uani 1 2 d S . . O3 O -0.21734(18) -0.1723(2) 0.09718(13) 0.0384(4) Uani 1 1 d . . . O2 O 0.0984(3) -0.2113(2) 0.13183(12) 0.0455(5) Uani 1 1 d D . . H2 H 0.127(4) -0.247(3) 0.0697(14) 0.068 Uiso 1 1 d D . . C3 C -0.2598(3) -0.2598(3) 0.0000 0.0308(7) Uani 1 2 d S . . C1 C 0.2693(3) 0.2693(3) 0.0000 0.0268(6) Uani 1 2 d S . . C2 C 0.0493(3) -0.3235(3) 0.22913(17) 0.0328(5) Uani 1 1 d D . . C5 C 0.0461(3) -0.4772(3) 0.22732(18) 0.0350(5) Uani 1 1 d . . . H5 H 0.0743 -0.5145 0.1562 0.042 Uiso 1 1 calc R . . C4 C -0.4245(3) -0.4245(3) 0.0000 0.0325(7) Uani 1 2 d S . . O4 O 0.1671(5) -0.3010(4) -0.08070(19) 0.0942(9) Uani 1 1 d D . . H4A H 0.177(6) -0.218(4) -0.128(3) 0.141 Uiso 1 1 d D . . H4B H 0.200(6) -0.362(5) -0.121(3) 0.141 Uiso 1 1 d D . . 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 Mn1 0.02672(17) 0.01757(19) 0.01861(18) 0.00161(15) 0.00080(7) 0.00879(10) O1 0.0252(7) 0.0252(7) 0.0193(8) 0.0028(5) -0.0028(5) -0.0019(8) O3 0.0278(8) 0.0357(9) 0.0317(8) -0.0093(7) 0.0027(6) 0.0009(7) O2 0.0890(14) 0.0401(10) 0.0256(7) 0.0113(7) 0.0205(9) 0.0460(10) C3 0.0255(11) 0.0255(11) 0.0293(15) -0.0031(8) 0.0031(8) 0.0037(13) C1 0.0229(10) 0.0229(10) 0.0227(13) 0.0008(7) -0.0008(7) 0.0025(13) C2 0.0548(14) 0.0318(12) 0.0216(9) 0.0051(9) 0.0060(10) 0.0288(11) C5 0.0616(14) 0.0331(13) 0.0238(9) -0.0024(9) 0.0036(9) 0.0338(12) C4 0.0259(10) 0.0259(10) 0.0278(14) -0.0025(7) 0.0025(7) -0.0005(12) O4 0.164(3) 0.114(2) 0.0539(12) 0.0200(14) 0.0355(15) 0.107(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Mn1 O1 2.0736(9) 3 ? Mn1 O1 2.0736(9) . ? Mn1 O3 2.1281(14) . ? Mn1 O3 2.1281(14) 5 ? Mn1 O2 2.3187(15) 5 ? Mn1 O2 2.3187(15) . ? O1 C1 1.327(3) . ? O1 Mn1 2.0735(9) 2_554 ? O3 C3 1.2610(19) . ? O2 C2 1.379(2) . ? C3 O3 1.2610(19) 4 ? C3 C4 1.492(4) . ? C1 C2 1.395(2) 5 ? C1 C2 1.395(2) 2_554 ? C2 C5 1.377(3) . ? C2 C1 1.395(2) 3 ? C5 C4 1.388(2) 3_545 ? C4 C5 1.388(2) 2_444 ? C4 C5 1.388(2) 5_445 ? 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 Mn1 O1 164.26(5) 3 . ? O1 Mn1 O3 96.33(4) 3 . ? O1 Mn1 O3 94.45(6) . . ? O1 Mn1 O3 94.45(6) 3 5 ? O1 Mn1 O3 96.33(4) . 5 ? O3 Mn1 O3 93.40(9) . 5 ? O1 Mn1 O2 95.48(4) 3 5 ? O1 Mn1 O2 73.63(5) . 5 ? O3 Mn1 O2 168.07(5) . 5 ? O3 Mn1 O2 87.38(7) 5 5 ? O1 Mn1 O2 73.63(5) 3 . ? O1 Mn1 O2 95.48(4) . . ? O3 Mn1 O2 87.38(7) . . ? O3 Mn1 O2 168.07(5) 5 . ? O2 Mn1 O2 94.32(10) 5 . ? C1 O1 Mn1 118.07(4) . 2_554 ? C1 O1 Mn1 118.07(4) . . ? Mn1 O1 Mn1 123.87(9) 2_554 . ? C3 O3 Mn1 129.60(14) . . ? C2 O2 Mn1 111.20(12) . . ? O3 C3 O3 124.4(3) . 4 ? O3 C3 C4 117.81(14) . . ? O3 C3 C4 117.81(14) 4 . ? O1 C1 C2 120.80(13) . 5 ? O1 C1 C2 120.80(13) . 2_554 ? C2 C1 C2 118.4(3) 5 2_554 ? C5 C2 O2 124.72(18) . . ? C5 C2 C1 121.23(19) . 3 ? O2 C2 C1 114.05(18) . 3 ? C2 C5 C4 118.9(2) . 3_545 ? C5 C4 C5 121.2(3) 2_444 5_445 ? C5 C4 C3 119.41(13) 2_444 . ? C5 C4 C3 119.41(13) 5_445 . ?