#------------------------------------------------------------------------------ #$Date: 2023-12-22 15:07:40 +0000 (Fri, 22 Dec 2023) $ #$Revision: 288505 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105090.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_2105090 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_paper_doi 10.1107/S0108768112009263 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety 'C30 H24 N6 Ru Cl2, 6(H2O)' _chemical_formula_sum 'C30 H36 Cl2 N6 O6 Ru' _chemical_formula_weight 748.62 _chemical_name_systematic ; Tris(2,2?-bipyridyl)dichlororuthenium(II) hexahydrate ; _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 13.1383(12) _cell_length_b 13.1383(12) _cell_length_c 20.995(3) _cell_measurement_reflns_used 3247 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 54.971 _cell_measurement_theta_min 5.280 _cell_volume 3138.5(6) _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 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _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 0.71073 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 11174 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.66 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6762 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.5842 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Chip _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _platon_squeeze_details ; The unit cell contains 6 water molecules and 2 chlorine ions 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 0.977 _refine_diff_density_min -0.561 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1220 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0614 _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^)+(0.0767P)^2^+5.4397P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1439 _refine_ls_wR_factor_ref 0.1529 _reflns_number_gt 994 _reflns_number_total 1220 _reflns_threshold_expression >2\s(I) _iucr_refine_instructions_details ; TITL Ru-hexahy4-17-5-10-150k-Dstar2 in P 6/m c c CELL 0.71073 13.1383 13.1383 20.9955 90.000 90.000 120.000 ZERR 4.00 0.0012 0.0012 0.0028 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, Z SYMM - Y, - X, 1/2 - Z SYMM Y, X, 1/2 - Z SYMM X - Y, - Y, 1/2 - Z SYMM - X + Y, Y, 1/2 - Z SYMM X, X - Y, 1/2 - Z SYMM - X, - X + Y, 1/2 - Z SYMM - Y, X - Y, Z SYMM Y, - X + Y, Z SYMM X - Y, X, Z SYMM - X + Y, - X, Z SFAC C H N RU Cl O UNIT 120 144 24 4 8 24 MERG 2 OMIT 0 1 2 OMIT 0 1 0 OMIT -1 8 1 OMIT 0 0 4 OMIT 0 0 6 OMIT -1 2 0 OMIT 0 2 0 OMIT -2 10 1 OMIT -3 9 1 OMIT -1 10 2 OMIT 0 1 10 OMIT -2 10 3 OMIT -1 11 5 OMIT -1 3 7 OMIT 0 0 8 OMIT -1 3 0 OMIT 0 0 10 OMIT 0 2 6 OMIT 0 1 4 OMIT -1 3 2 OMIT -1 3 5 OMIT -1 3 4 OMIT 0 4 4 OMIT 0 4 2 OMIT 0 5 6 OMIT -1 3 11 OMIT -2 5 9 OMIT -2 5 13 OMIT -2 8 9 OMIT -2 8 1 FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 REM WGHT 0.200000 REM WGHT 0.084400 5.034300 WGHT 0.076700 5.439700 FVAR 17.17370 N1 3 0.681084 0.207661 0.198021 11.00000 0.02762 0.02392 = 0.03553 -0.00011 0.00383 0.01242 C1 1 0.761816 0.179982 0.220536 11.00000 0.02836 0.02303 = 0.03543 0.00370 0.00486 0.01339 C2 1 0.786076 0.102876 0.187185 11.00000 0.03681 0.02956 = 0.04920 -0.00107 0.00221 0.01951 AFIX 43 H2 2 0.840926 0.084298 0.202990 11.00000 -1.20000 AFIX 0 C5 1 0.627147 0.159671 0.142553 11.00000 0.03035 0.03023 = 0.03244 -0.00138 0.00091 0.01301 AFIX 43 H5 2 0.572167 0.178335 0.127057 11.00000 -1.20000 AFIX 0 C3 1 0.728782 0.054223 0.130820 11.00000 0.04242 0.02706 = 0.04461 0.00016 0.00992 0.01958 AFIX 43 H3 2 0.743601 0.001656 0.108708 11.00000 -1.20000 AFIX 0 C4 1 0.649447 0.084124 0.107553 11.00000 0.03589 0.02529 = 0.04559 -0.00210 0.00126 0.01217 AFIX 43 H4 2 0.611525 0.053986 0.068942 11.00000 -1.20000 AFIX 0 RU1 4 0.666667 0.333333 0.250000 10.16667 0.02115 0.02115 = 0.03069 0.00000 0.00000 0.01058 HKLF 4 REM Ru-hexahy4-17-5-10-150k-Dstar2 in P 6/m c c REM R1 = 0.0614 for 994 Fo > 4sig(Fo) and 0.0769 for all 1220 data REM 57 parameters refined using 0 restraints END WGHT 0.0756 5.6218 REM Highest difference peak 0.977, deepest hole -0.561, 1-sigma level 0.108 Q1 1 0.6667 0.3333 0.2024 10.33333 0.05 0.98 Q2 1 1.0000 0.0000 0.2500 10.08333 0.05 0.77 Q3 1 0.6667 0.3333 0.1557 10.33333 0.05 0.54 Q4 1 0.5413 -0.0994 0.0000 10.50000 0.05 0.48 Q5 1 0.8472 -0.0169 0.0000 10.50000 0.05 0.46 Q6 1 0.5184 0.1414 0.0000 10.50000 0.05 0.41 Q7 1 1.0000 0.0000 0.0000 10.08333 0.05 0.33 Q8 1 0.8733 0.0177 0.2012 11.00000 0.05 0.32 Q9 1 0.6667 0.3333 0.0000 10.16667 0.05 0.32 Q10 1 0.7696 0.1381 0.1885 11.00000 0.05 0.32 Q11 1 0.7420 0.0624 0.1704 11.00000 0.05 0.31 Q12 1 0.6345 0.2690 0.2500 10.50000 0.05 0.31 Q13 1 0.7002 0.4005 0.2500 10.50000 0.05 0.31 Q14 1 0.6537 0.1859 0.1962 11.00000 0.05 0.31 Q15 1 0.5975 -0.0256 0.0614 11.00000 0.05 0.31 Q16 1 0.7771 0.0942 0.2486 11.00000 0.05 0.30 Q17 1 0.6694 0.1866 0.1696 11.00000 0.05 0.29 Q18 1 0.7222 0.1911 0.1812 11.00000 0.05 0.29 Q19 1 0.9555 0.0382 0.0444 11.00000 0.05 0.29 Q20 1 0.6596 0.0565 0.1455 11.00000 0.05 0.28 ; _cod_data_source_file zb5022.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: data name '_iucr_refine_instruction_details' was replaced with '_iucr_refine_instructions_details' as specified in the replacement file 'data/replacement-values/replacement_tags.lst'. Automatic conversion script Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas ; _cod_original_cell_volume 3138.6(6) _cod_original_sg_symbol_H-M P6/mcc _cod_database_code 2105090 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, -x, -z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z+1/2' '-y, x-y, z' 'y, -x+y, z' 'x-y, x, z' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z' 'y, x, z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z-1/2' 'y, -x+y, -z' '-y, x-y, -z' '-x+y, -x, -z' 'x-y, x, -z' 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 0.6811(3) 0.2077(3) 0.19802(16) 0.0292(8) Uani d . 1 1 C C1 0.7618(3) 0.1800(3) 0.2205(2) 0.0287(8) Uani d . 1 1 C C2 0.7861(4) 0.1029(4) 0.1872(2) 0.0372(10) Uani d . 1 1 H H2 0.8409 0.0843 0.2030 0.045 Uiso calc R 1 1 C C5 0.6271(4) 0.1597(4) 0.1426(2) 0.0320(9) Uani d . 1 1 H H5 0.5722 0.1783 0.1271 0.038 Uiso calc R 1 1 C C3 0.7288(4) 0.0542(4) 0.1308(2) 0.0370(10) Uani d . 1 1 H H3 0.7436 0.0017 0.1087 0.044 Uiso calc R 1 1 C C4 0.6494(4) 0.0841(4) 0.1076(2) 0.0370(10) Uani d . 1 1 H H4 0.6115 0.0540 0.0689 0.044 Uiso calc R 1 1 Ru Ru1 0.6667 0.3333 0.2500 0.0243(3) 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 0.0276(17) 0.0239(16) 0.0355(19) 0.0124(14) 0.0038(14) -0.0001(14) C1 0.0284(19) 0.0230(17) 0.035(2) 0.0134(15) 0.0049(16) 0.0037(15) C2 0.037(2) 0.030(2) 0.049(3) 0.020(2) 0.002(2) -0.0011(19) C5 0.030(2) 0.030(2) 0.032(2) 0.0130(18) 0.0009(17) -0.0014(16) C3 0.042(2) 0.027(2) 0.045(2) 0.020(2) 0.010(2) 0.0002(19) C4 0.036(2) 0.0253(19) 0.046(3) 0.0122(17) 0.0013(19) -0.0021(18) Ru1 0.0212(3) 0.0212(3) 0.0307(5) 0.01058(15) 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' Ru Ru -1.2594 0.8363 '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' O O 0.0106 0.0060 '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 C5 N1 C1 . . 118.2(3) C5 N1 Ru1 . . 126.5(3) C1 N1 Ru1 . . 115.1(3) N1 C1 C2 . . 120.7(4) N1 C1 C1 . 3_665 115.4(2) C2 C1 C1 . 3_665 124.0(3) C3 C2 C1 . . 119.9(4) C3 C2 H2 . . 120.0 C1 C2 H2 . . 120.0 N1 C5 C4 . . 123.2(4) N1 C5 H5 . . 118.4 C4 C5 H5 . . 118.4 C4 C3 C2 . . 119.3(4) C4 C3 H3 . . 120.3 C2 C3 H3 . . 120.3 C3 C4 C5 . . 118.7(4) C3 C4 H4 . . 120.6 C5 C4 H4 . . 120.6 N1 Ru1 N1 . 3_665 78.98(19) N1 Ru1 N1 . 9_655 94.66(13) N1 Ru1 N1 3_665 9_655 92.37(18) N1 Ru1 N1 . 6_655 92.37(18) N1 Ru1 N1 3_665 6_655 94.66(13) N1 Ru1 N1 9_655 6_655 170.89(18) N1 Ru1 N1 . 12_665 94.66(13) N1 Ru1 N1 3_665 12_665 170.89(18) N1 Ru1 N1 9_655 12_665 94.66(13) N1 Ru1 N1 6_655 12_665 78.98(19) N1 Ru1 N1 . 7 170.89(18) N1 Ru1 N1 3_665 7 94.66(13) N1 Ru1 N1 9_655 7 78.98(19) N1 Ru1 N1 6_655 7 94.66(13) N1 Ru1 N1 12_665 7 92.37(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C5 . 1.345(5) N1 C1 . 1.366(5) N1 Ru1 . 2.065(3) C1 C2 . 1.393(6) C1 C1 3_665 1.454(9) C2 C3 . 1.376(7) C2 H2 . 0.9300 C5 C4 . 1.379(6) C5 H5 . 0.9300 C3 C4 . 1.374(6) C3 H3 . 0.9300 C4 H4 . 0.9300 Ru1 N1 3_665 2.065(3) Ru1 N1 9_655 2.065(3) Ru1 N1 6_655 2.065(3) Ru1 N1 12_665 2.065(3) Ru1 N1 7 2.065(3)