#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060217.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060217 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C2 H2 Mn O4' _chemical_formula_weight 144.97 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Pna2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.8962(14) _cell_length_b 8.3888(9) _cell_length_c 11.6442(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1259.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 3.024 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 223(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 7047 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2795 _reflns_number_gt 2606 _reflns_threshold_expression >2sigma(I) _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^)+(0.0706P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(3) _refine_ls_number_reflns 2795 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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 0.53471(5) 0.13727(7) 0.21804(6) 0.01174(17) Uani 1 1 d . . . Mn2 Mn 0.69702(5) -0.12624(7) 0.35106(6) 0.01230(17) Uani 1 1 d . . . Mn3 Mn 0.62330(5) 0.50183(7) 0.28016(8) 0.01411(16) Uani 1 1 d . . . O12 O 0.4762(3) 0.3693(3) 0.2713(4) 0.0195(7) Uani 1 1 d . . . O11 O 0.6569(3) 0.3573(4) 0.4308(4) 0.0226(8) Uani 1 1 d . . . O10 O 0.6238(3) 0.1072(4) 0.3778(3) 0.0170(7) Uani 1 1 d . . . O9 O 0.7645(3) -0.3598(3) 0.2991(3) 0.0190(7) Uani 1 1 d . . . O8 O 0.5860(3) 0.6563(4) 0.1345(4) 0.0239(8) Uani 1 1 d . . . O7 O 0.6116(3) -0.0919(4) 0.1891(3) 0.0178(8) Uani 1 1 d . . . O6 O 0.7529(3) -0.1127(4) 0.5227(4) 0.0264(9) Uani 1 1 d . . . O5 O 0.4880(3) 0.1730(4) 0.0437(3) 0.0223(8) Uani 1 1 d . . . C6 C 0.7845(3) -0.2212(5) 0.5834(4) 0.0169(10) Uani 1 1 d . . . H6 H 0.7713 -0.3260 0.5587 0.020 Uiso 1 1 calc R . . O4 O 0.8453(3) -0.0374(4) 0.2984(4) 0.0280(9) Uani 1 1 d . . . C5 C 0.8586(3) -0.3990(5) 0.2831(5) 0.0186(9) Uani 1 1 d . . . H5 H 0.9085 -0.3173 0.2856 0.022 Uiso 1 1 calc R . . O3 O 0.3897(3) 0.0350(4) 0.2646(4) 0.0238(8) Uani 1 1 d . . . O2 O 0.6665(2) 0.2957(4) 0.1770(3) 0.0158(7) Uani 1 1 d . . . C4 C 0.6585(4) 0.2123(6) 0.4463(5) 0.0201(10) Uani 1 1 d . . . H4 H 0.6881 0.1759 0.5152 0.024 Uiso 1 1 calc R . . O1 O 0.5784(2) -0.3027(4) 0.3952(3) 0.0155(7) Uani 1 1 d . . . C3 C 0.4743(4) 0.2959(6) -0.0122(4) 0.0178(10) Uani 1 1 d . . . H3 H 0.5044 0.3905 0.0151 0.021 Uiso 1 1 calc R . . C2 C 0.5833(4) 0.8004(6) 0.1175(4) 0.0195(10) Uani 1 1 d . . . H2 H 0.5584 0.8349 0.0459 0.023 Uiso 1 1 calc R . . C1 C 0.3816(4) 0.4025(5) 0.2897(5) 0.0215(11) Uani 1 1 d . . . H1 H 0.3353 0.3165 0.2972 0.026 Uiso 1 1 calc R . . 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 0.0117(3) 0.0079(3) 0.0156(4) 0.0014(3) -0.0015(3) 0.0001(2) Mn2 0.0117(3) 0.0087(3) 0.0166(4) 0.0016(3) -0.0018(3) -0.0001(2) Mn3 0.0156(3) 0.0087(3) 0.0180(3) -0.0020(2) 0.0010(3) -0.0012(2) O12 0.0139(16) 0.0124(14) 0.032(2) -0.0017(15) 0.0029(15) 0.0015(11) O11 0.034(2) 0.0123(15) 0.022(2) -0.0004(14) -0.0032(16) 0.0004(14) O10 0.0250(18) 0.0108(13) 0.0151(18) 0.0029(13) -0.0039(13) 0.0014(12) O9 0.0148(16) 0.0124(15) 0.030(2) -0.0035(14) 0.0011(15) 0.0008(11) O8 0.034(2) 0.0156(15) 0.0217(19) -0.0028(15) -0.0029(16) 0.0027(15) O7 0.0204(17) 0.0130(14) 0.0200(19) -0.0007(14) -0.0031(13) 0.0043(13) O6 0.033(2) 0.0221(17) 0.024(2) -0.0002(16) -0.0114(16) 0.0009(17) O5 0.029(2) 0.0184(15) 0.0195(19) 0.0037(15) -0.0111(16) -0.0022(15) C6 0.019(2) 0.014(2) 0.018(2) -0.0016(19) -0.0023(19) 0.0005(18) O4 0.0181(17) 0.0153(15) 0.050(3) 0.0040(18) 0.0040(17) -0.0049(13) C5 0.014(2) 0.0167(19) 0.025(3) -0.001(2) 0.001(2) -0.0032(17) O3 0.0195(17) 0.0145(15) 0.037(2) 0.0050(17) 0.0028(15) -0.0024(13) O2 0.0168(16) 0.0131(14) 0.0174(17) -0.0025(13) 0.0042(13) -0.0019(13) C4 0.025(3) 0.019(2) 0.017(3) -0.002(2) -0.0023(19) 0.007(2) O1 0.0167(17) 0.0126(14) 0.0171(17) -0.0022(13) 0.0022(13) -0.0001(13) C3 0.014(2) 0.019(2) 0.021(3) 0.000(2) -0.0063(18) -0.0011(18) C2 0.024(3) 0.019(2) 0.015(3) 0.002(2) -0.007(2) 0.003(2) C1 0.014(2) 0.0145(19) 0.036(3) -0.007(2) 0.000(2) -0.0021(17)