#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100722.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_1100722 loop_ _publ_author_name 'andrea c. sudik' 'adrien p. cote' _publ_section_title ; tba ; _chemical_formula_moiety '(C33 H15 Fe3 N3 O16), (Cl4 Fe), O' _chemical_formula_sum 'C33 H15 Cl4 Fe4 N3 O17' _chemical_formula_weight 1090.61 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P-62c _symmetry_space_group_name_Hall P-6c-2c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z+1/2' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 12.531(3) _cell_length_b 12.531(3) _cell_length_c 18.476(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2512.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 715 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 25.14 _exptl_crystal_description octahedral _exptl_crystal_colour orange _exptl_crystal_size_max 0.042 _exptl_crystal_size_mid 0.041 _exptl_crystal_size_min 0.037 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9433 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _diffrn_ambient_temperature 153(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 '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_% ? _diffrn_reflns_number 11323 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.15 _reflns_number_total 1543 _reflns_number_gt 1292 _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^)+(0.1172P)^2^+5.2365P] 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 0.015(3) _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 -0.01(10) _refine_ls_number_reflns 1543 _refine_ls_number_parameters 116 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.1044 _refine_ls_wR_factor_ref 0.2550 _refine_ls_wR_factor_gt 0.2454 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_restrained_S_all 1.260 _refine_ls_shift/su_max 0.002 _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 0.7270(2) 1.2195(2) 0.7500 0.0233(6) Uani 1 2 d S . . O1 O 0.6667 1.3333 0.7500 0.018(4) Uani 1 6 d S . . O2 O 0.8499(8) 1.3019(7) 0.6692(4) 0.034(2) Uani 1 1 d . . . O3 O 0.7800(11) 1.0882(12) 0.7500 0.047(3) Uani 1 2 d S . . O4 O 0.6106(8) 1.1159(8) 0.6719(5) 0.042(2) Uani 1 1 d . . . C1 C 0.716(3) 0.982(3) 0.7500 0.21(3) Uani 1 2 d S . . H1 H 0.6321 0.9569 0.7500 0.255 Uiso 1 2 calc SR . . N1 N 0.738(2) 0.893(2) 0.7500 0.119(10) Uani 1 2 d SD . . C3 C 0.5160(11) 1.1110(13) 0.6423(8) 0.046(3) Uani 1 1 d . . . C4 C 0.5680(13) 1.0240(18) 0.5353(7) 0.064(5) Uani 1 1 d . . . H4 H 0.6384 1.0371 0.5598 0.03(3) Uiso 1 1 calc R . . C5 C 0.4835(12) 1.0521(13) 0.5685(7) 0.047(4) Uani 1 1 d . . . C6 C 0.3754(11) 1.0259(11) 0.5325(6) 0.041(3) Uani 1 1 d . . . H6 H 0.3204 1.0452 0.5545 0.050 Uiso 1 1 calc R . . C7 C 0.805(6) 0.896(5) 0.692(3) 0.16(3) Uani 0.50 1 d P . . C8 C 0.643(5) 0.767(3) 0.7500 0.30(4) Uani 1 2 d SD . . O1W O 0.3333 0.6667 0.594(6) 0.22(4) Uani 0.50 3 d SP . . Fe2 Fe 0.0000 1.0000 0.5000 0.099(3) Uani 1 6 d S . . Cl1 Cl -0.1618(12) 1.0000 0.5000 0.051(4) Uani 0.333 2 d SP . . Cl2 Cl -0.1453(17) 0.9805(19) 0.574(2) 0.31(2) 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 0.0169(11) 0.0207(12) 0.0349(10) 0.000 0.000 0.0114(10) O1 0.001(5) 0.001(5) 0.053(11) 0.000 0.000 0.000(2) O2 0.040(5) 0.030(5) 0.041(5) 0.012(4) 0.018(4) 0.024(4) O3 0.041(8) 0.033(8) 0.069(9) 0.000 0.000 0.019(6) O4 0.041(6) 0.037(5) 0.054(5) -0.017(4) -0.010(4) 0.024(4) C1 0.042(16) 0.032(17) 0.56(10) 0.000 0.000 0.018(14) N1 0.11(2) 0.053(14) 0.23(3) 0.000 0.000 0.069(15) C3 0.037(8) 0.032(8) 0.072(9) -0.017(7) -0.018(6) 0.018(7) C4 0.051(9) 0.116(14) 0.038(7) -0.038(9) -0.021(7) 0.052(10) C5 0.037(9) 0.042(8) 0.052(7) -0.011(6) 0.000(6) 0.014(7) C6 0.022(6) 0.054(8) 0.047(6) 0.000(6) -0.003(6) 0.019(6) C7 0.31(8) 0.17(5) 0.15(4) 0.06(4) 0.13(5) 0.21(7) C8 0.21(6) 0.06(3) 0.63(14) 0.000 0.000 0.07(4) O1W 0.13(4) 0.13(4) 0.39(12) 0.000 0.000 0.065(18) Fe2 0.097(4) 0.097(4) 0.105(5) 0.000 0.000 0.0483(19) Cl1 0.020(5) 0.050(9) 0.095(12) -0.004(9) -0.002(5) 0.025(4) Cl2 0.105(12) 0.118(16) 0.65(5) -0.14(3) 0.12(2) 0.004(11)