data_4000228 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'C2 H10 F3 Fe N2 O4 S' _chemical_formula_weight 271.03 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.4111(6) _cell_length_b 9.5223(8) _cell_length_c 13.1307(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 801.61(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2607 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 23.00 _exptl_crystal_description Needle _exptl_crystal_colour Transparent _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 2.246 _exptl_crystal_density_method ? _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.762882 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3405 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 23.23 _reflns_number_total 1146 _reflns_number_observed 1057 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1146 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_obs 0.0315 _refine_ls_wR_factor_all 0.0825 _refine_ls_wR_factor_obs 0.0806 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.054 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.90646(10) 0.08673(6) 0.55878(4) 0.0147(2) Uani 1 d . . S1 S 1.4100(2) 0.08064(11) 0.49802(8) 0.0168(3) Uani 1 d . . F1 F 0.9010(5) 0.0838(3) 0.4163(2) 0.0236(6) Uani 1 d . . F2 F 0.9147(4) 0.0822(3) 0.7050(2) 0.0234(6) Uani 1 d . . F3 F 0.9074(5) -0.1162(2) 0.5620(2) 0.0228(6) Uani 1 d . . O1 O 0.5922(5) 0.0940(3) 0.5683(2) 0.0206(7) Uani 1 d . . O2 O 0.9109(7) 0.2991(3) 0.5734(2) 0.0218(7) Uani 1 d . . O3 O 1.2247(5) 0.0894(4) 0.5646(2) 0.0232(8) Uani 1 d . . O4 O 1.4137(7) -0.0494(3) 0.4432(3) 0.0308(8) Uani 1 d . . N1 N 1.7521(6) 0.2212(4) 0.8786(3) 0.0243(10) Uani 1 d . . H1 H 1.8587(6) 0.2787(4) 0.8907(3) 0.036 Uiso 1 calc R . H2 H 1.7980(6) 0.1449(4) 0.8465(3) 0.036 Uiso 1 calc R . H3 H 1.6932(6) 0.1964(4) 0.9372(3) 0.036 Uiso 1 calc R . C1 C 1.5960(9) 0.2940(4) 0.8137(4) 0.0238(11) Uani 1 d . . H4 H 1.6599(9) 0.3221(4) 0.7499(4) 0.029 Uiso 1 calc R . H5 H 1.5464(9) 0.3779(4) 0.8481(4) 0.029 Uiso 1 calc R . C2 C 1.4155(9) 0.1966(5) 0.7932(4) 0.0257(11) Uani 1 d . . H6 H 1.4601(9) 0.1215(5) 0.7483(4) 0.031 Uiso 1 calc R . H7 H 1.3683(9) 0.1550(5) 0.8565(4) 0.031 Uiso 1 calc R . N3 N 1.2418(6) 0.2756(4) 0.7452(3) 0.0262(10) Uani 1 d . . H8 H 1.1358(6) 0.2176(4) 0.7332(3) 0.039 Uiso 1 calc R . H9 H 1.2852(6) 0.3128(4) 0.6867(3) 0.039 Uiso 1 calc R . H10 H 1.2003(6) 0.3438(4) 0.7869(3) 0.039 Uiso 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 Fe1 0.0151(4) 0.0106(3) 0.0183(4) 0.0013(3) -0.0002(3) -0.0004(4) S1 0.0166(6) 0.0098(5) 0.0241(6) 0.0006(5) 0.0016(5) 0.0003(6) F1 0.0272(14) 0.0231(14) 0.0204(13) -0.0001(11) 0.0015(11) 0.005(2) F2 0.0294(14) 0.0216(13) 0.0191(13) 0.0041(11) -0.0032(12) 0.001(2) F3 0.029(2) 0.0087(12) 0.0311(14) 0.0017(10) 0.001(2) 0.0007(12) O1 0.014(2) 0.022(2) 0.025(2) 0.000(2) -0.001(2) 0.000(2) O2 0.028(2) 0.014(2) 0.024(2) 0.0064(13) -0.006(2) -0.003(2) O3 0.021(2) 0.025(2) 0.023(2) 0.001(2) -0.005(2) 0.004(2) O4 0.033(2) 0.018(2) 0.041(2) -0.0096(14) 0.001(2) -0.002(2) N1 0.023(2) 0.016(2) 0.034(3) 0.000(2) -0.005(2) -0.003(2) C1 0.024(3) 0.013(2) 0.035(3) 0.000(2) -0.007(3) 0.002(2) C2 0.027(3) 0.024(3) 0.026(3) 0.003(2) -0.003(3) -0.003(3) N3 0.024(2) 0.027(2) 0.027(2) -0.003(2) -0.002(2) -0.001(2)