#------------------------------------------------------------------------------ #$Date: 2014-10-25 18:23:10 +0100 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105091.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2105091 loop_ _publ_author_name 'Low, Kian Sing' 'Cole, Jacqueline M.' 'Zhou, Xiaolan' 'Yufa, Nataliya' _publ_section_title ; Rationalizing the molecular origins of Ru- and Fe-based dyes for dye-sensitized solar cells ; _journal_coeditor_code ZB5022 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 137 _journal_page_last 149 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety 'C30 H24 Fe N6, 2(NCS)' _chemical_formula_sum 'C32 H24 Fe N8 S2' _chemical_formula_weight 642.28 _chemical_name_systematic ; tris(2,2'-bipyridyl) iron(II) dithiocyanate ; _space_group_IT_number 192 _space_group_name_Hall '-P 6 2c' _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6 2c' _symmetry_space_group_name_H-M 'P 6/m c c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 4 _cell_length_a 13.1837(9) _cell_length_b 13.1837(9) _cell_length_c 21.2735(14) _cell_measurement_reflns_used 3247 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 54.971 _cell_measurement_theta_min 5.280 _cell_volume 3202.2(4) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution ; SIR92 (Altomare et al., J. Appl. Cryst. (1994). 27, 435) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'phi or omega oscillation scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 26491 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.57 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8573 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Chip _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _platon_squeeze_details ; The unit cell contains 2 NCS counterions and 3 acetonitirile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 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^ > 2\s(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_diff_density_max 0.323 _refine_diff_density_min -0.270 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1259 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.134 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0487 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+3.3496P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.1145 _reflns_number_gt 1165 _reflns_number_total 1259 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file zb5022.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M P6/mcc _cod_database_code 2105091 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' '-y, -x, -z+1/2' 'x-y, -y, -z+1/2' 'x, x-y, -z+1/2' 'y, x, -z+1/2' '-x+y, y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' 'y, x, z-1/2' '-x+y, y, z-1/2' '-x, -x+y, z-1/2' '-y, -x, z-1/2' 'x-y, -y, z-1/2' 'x, x-y, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity N N1 0.67794(13) 0.21313(14) 0.19921(8) 0.0230(4) Uani d . 1 1 C C4 0.78247(19) 0.10828(18) 0.18768(11) 0.0320(5) Uani d . 1 1 H H4A 0.8363 0.0889 0.2035 0.038 Uiso calc R 1 1 C C5 0.75801(15) 0.18462(15) 0.22066(10) 0.0235(4) Uani d . 1 1 C C1 0.62321(18) 0.16518(17) 0.14468(10) 0.0282(4) Uani d . 1 1 H H1A 0.5676 0.1831 0.1300 0.034 Uiso calc R 1 1 C C3 0.7263(2) 0.06123(18) 0.13113(11) 0.0351(5) Uani d . 1 1 H H3A 0.7426 0.0109 0.1083 0.042 Uiso calc R 1 1 C C2 0.64568(19) 0.09035(18) 0.10931(11) 0.0330(5) Uani d . 1 1 H H2A 0.6070 0.0602 0.0714 0.040 Uiso calc R 1 1 Fe Fe 0.6667 0.3333 0.2500 0.0189(2) Uani d S 1 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0212(8) 0.0185(7) 0.0269(8) 0.0080(6) 0.0015(6) 0.0005(6) C4 0.0328(11) 0.0257(10) 0.0409(12) 0.0172(9) 0.0057(9) 0.0022(9) C5 0.0208(8) 0.0183(8) 0.0317(10) 0.0101(7) 0.0039(7) 0.0028(7) C1 0.0277(10) 0.0244(9) 0.0301(11) 0.0112(8) -0.0026(8) -0.0038(8) C3 0.0434(12) 0.0234(10) 0.0391(12) 0.0170(10) 0.0108(10) -0.0029(8) C2 0.0338(11) 0.0256(10) 0.0332(11) 0.0101(9) 0.0010(9) -0.0061(8) Fe 0.0170(2) 0.0170(2) 0.0229(3) 0.00848(12) 0.000 0.000 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' S S 0.1246 0.1234 '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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C1 N1 C5 . . 117.79(17) C1 N1 Fe . . 127.46(13) C5 N1 Fe . . 114.53(13) C3 C4 C5 . . 119.7(2) C3 C4 H4A . . 120.1 C5 C4 H4A . . 120.1 N1 C5 C4 . . 121.47(19) N1 C5 C5 . 7_665 114.54(11) C4 C5 C5 . 7_665 123.98(13) N1 C1 C2 . . 123.20(19) N1 C1 H1A . . 118.4 C2 C1 H1A . . 118.4 C2 C3 C4 . . 118.81(19) C2 C3 H3A . . 120.6 C4 C3 H3A . . 120.6 C3 C2 C1 . . 119.0(2) C3 C2 H2A . . 120.5 C1 C2 H2A . . 120.5 N1 Fe N1 7_665 . 81.67(9) N1 Fe N1 7_665 11_655 93.16(6) N1 Fe N1 . 11_655 92.47(9) N1 Fe N1 7_665 3_655 92.47(9) N1 Fe N1 . 3_655 93.16(6) N1 Fe N1 11_655 3_655 172.56(9) N1 Fe N1 7_665 9 93.16(6) N1 Fe N1 . 9 172.56(9) N1 Fe N1 11_655 9 93.16(6) N1 Fe N1 3_655 9 81.67(9) N1 Fe N1 7_665 5_665 172.56(9) N1 Fe N1 . 5_665 93.16(6) N1 Fe N1 11_655 5_665 81.67(9) N1 Fe N1 3_655 5_665 93.16(6) N1 Fe N1 9 5_665 92.47(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C1 . 1.345(3) N1 C5 . 1.364(2) N1 Fe . 1.9841(16) C4 C3 . 1.386(3) C4 C5 . 1.391(3) C4 H4A . 0.9300 C5 C5 7_665 1.460(4) C1 C2 . 1.386(3) C1 H1A . 0.9300 C3 C2 . 1.378(3) C3 H3A . 0.9300 C2 H2A . 0.9300 Fe N1 7_665 1.9841(16) Fe N1 11_655 1.9841(16) Fe N1 3_655 1.9841(16) Fe N1 9 1.9841(16) Fe N1 5_665 1.9841(16) 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 _platon_squeeze_void_content 1 -0.009 -0.008 -0.072 1005 285 ' ' 2 0.000 0.500 0.250 7 1 ' ' 3 0.000 0.500 0.750 7 1 ' ' 4 0.500 0.000 0.250 7 1 ' ' 5 0.500 0.000 0.750 7 1 ' ' 6 0.500 0.500 0.250 7 1 ' ' 7 0.500 0.500 0.750 7 1 ' ' _journal_paper_doi 10.1107/S0108768112009263