# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Tanaka, Saya' 'Masaoka, Shigeyuki' 'Yamauchi, Kosei' 'Sakai, Ken' _publ_contact_author_name 'Sakai, Ken' _publ_contact_author_email ksakai@chem.kyushu-univ.jp _publ_section_title ; Photochemical and Thermal Hydrogen Production from Water Catalyzed by Carboxylate-Bridged Dirhodium(II) Complexes ; # Attachment '- Crystal data for 2.cif' #===================================================================== data_070402Rh2gly4 _database_code_depnum_ccdc_archive 'CCDC 783174' #TrackingRef '- Crystal data for 2.cif' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; NONE ; _chemical_name_common ? _chemical_formula_iupac ? _chemical_formula_moiety 'C8 H16 O14 Rh2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H16 O14 Rh2' _chemical_formula_weight 542.03 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.755(2) _cell_length_b 12.509(3) _cell_length_c 7.990(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.707(3) _cell_angle_gamma 90.00 _cell_volume 734.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 2395 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.56 _cell_special_details ; ? # Insert any comments here. ; _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.452 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 2.326 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.977 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART APEX CCD-detector diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3770 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 1498 _reflns_number_gt 1369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976) ; #========================================================================= # 8. Refinement Data _refine_special_details ; 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^ > 2sigma(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_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^)+(0.0259P)^2^+1.1689P] 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_extinction_expression not_refined _refine_ls_number_reflns 1498 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0451 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.678 _refine_diff_density_min -0.524 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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 Rh1 Rh 0.98745(3) 1.040082(15) 0.86019(2) 0.00730(8) Uani 1 1 d . . . O6 O 1.1573(3) 0.62732(14) 0.9339(2) 0.0149(4) Uani 1 1 d . . . H6 H 1.1000 0.6251 1.0070 0.022 Uiso 1 1 calc R . . O3 O 0.3922(2) 0.90980(14) 0.6167(2) 0.0123(4) Uani 1 1 d . . . H3 H 0.3826 0.9762 0.6010 0.018 Uiso 1 1 calc R . . O7 O 0.9689(3) 1.12323(16) 0.5984(3) 0.0120(4) Uani 1 1 d . . . O1 O 1.2540(2) 1.08330(15) 0.9639(2) 0.0114(4) Uani 1 1 d . . . O4 O 0.9243(2) 1.18115(14) 0.9553(2) 0.0117(4) Uani 1 1 d . . . O5 O 1.0480(2) 0.89445(14) 0.7802(2) 0.0110(4) Uani 1 1 d . . . O2 O 0.7218(2) 0.99241(14) 0.7723(2) 0.0107(4) Uani 1 1 d . . . C4 C 1.0801(4) 0.7070(2) 0.8049(3) 0.0126(5) Uani 1 1 d . . . H4A H 0.9561 0.6844 0.7331 0.015 Uiso 1 1 calc R . . H4B H 1.1542 0.7131 0.7250 0.015 Uiso 1 1 calc R . . C2 C 0.4761(3) 0.8878(2) 0.8006(3) 0.0117(5) Uani 1 1 d . . . H2A H 0.4860 0.8094 0.8182 0.014 Uiso 1 1 calc R . . H2B H 0.3975 0.9156 0.8668 0.014 Uiso 1 1 calc R . . C3 C 1.0690(3) 0.8159(2) 0.8847(3) 0.0108(5) Uani 1 1 d . . . C1 C 0.6633(4) 0.93678(19) 0.8748(3) 0.0100(5) Uani 1 1 d . . . H7 H 0.878(4) 1.124(2) 0.529(4) 0.007(8) Uiso 1 1 d . . . H8 H 1.035(5) 1.117(3) 0.564(5) 0.023(12) Uiso 1 1 d . . . 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 Rh1 0.00861(12) 0.00636(11) 0.00706(12) 0.00009(7) 0.00269(8) -0.00069(7) O6 0.0216(10) 0.0088(9) 0.0141(9) 0.0014(7) 0.0057(8) 0.0024(8) O3 0.0133(9) 0.0080(9) 0.0127(9) 0.0023(7) 0.0002(8) -0.0011(7) O7 0.0110(10) 0.0160(10) 0.0086(10) 0.0010(8) 0.0026(10) -0.0016(9) O1 0.0113(9) 0.0130(9) 0.0094(9) 0.0012(7) 0.0026(8) -0.0021(7) O4 0.0156(10) 0.0087(9) 0.0111(9) 0.0005(7) 0.0050(8) 0.0004(7) O5 0.0129(9) 0.0098(9) 0.0111(9) 0.0004(7) 0.0052(7) 0.0009(7) O2 0.0094(9) 0.0108(9) 0.0111(9) 0.0018(7) 0.0022(7) -0.0013(7) C4 0.0169(14) 0.0092(12) 0.0114(12) -0.0003(10) 0.0043(11) 0.0006(10) C2 0.0116(13) 0.0121(13) 0.0113(12) 0.0009(10) 0.0034(10) -0.0022(10) C3 0.0074(12) 0.0117(12) 0.0140(13) -0.0010(10) 0.0043(10) -0.0014(10) C1 0.0116(13) 0.0067(11) 0.0126(13) -0.0026(9) 0.0050(11) 0.0005(9) #========================================================================= # 10. Molecular Geometry loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O5 2.0346(18) . ? Rh1 O1 2.0379(18) . ? Rh1 O2 2.0409(19) . ? Rh1 O4 2.0419(18) . ? Rh1 O7 2.299(2) . ? Rh1 Rh1 2.3992(7) 3_777 ? O6 C4 1.421(3) . ? O6 H6 0.8400 . ? O3 C2 1.430(3) . ? O3 H3 0.8400 . ? O7 H7 0.74(3) . ? O7 H8 0.66(4) . ? O1 C1 1.267(3) 3_777 ? O4 C3 1.263(3) 3_777 ? O5 C3 1.266(3) . ? O2 C1 1.264(3) . ? C4 C3 1.518(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C2 C1 1.511(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.263(3) 3_777 ? C1 O1 1.267(3) 3_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Rh1 O1 93.38(7) . . ? O5 Rh1 O2 86.53(7) . . ? O1 Rh1 O2 176.17(7) . . ? O5 Rh1 O4 176.04(7) . . ? O1 Rh1 O4 87.29(7) . . ? O2 Rh1 O4 92.53(7) . . ? O5 Rh1 O7 94.18(7) . . ? O1 Rh1 O7 90.53(8) . . ? O2 Rh1 O7 93.30(8) . . ? O4 Rh1 O7 89.71(7) . . ? O5 Rh1 Rh1 87.72(5) . 3_777 ? O1 Rh1 Rh1 87.91(5) . 3_777 ? O2 Rh1 Rh1 88.26(5) . 3_777 ? O4 Rh1 Rh1 88.41(5) . 3_777 ? O7 Rh1 Rh1 177.61(5) . 3_777 ? C4 O6 H6 109.5 . . ? C2 O3 H3 109.5 . . ? Rh1 O7 H7 117(2) . . ? Rh1 O7 H8 120(3) . . ? H7 O7 H8 111(4) . . ? C1 O1 Rh1 118.51(17) 3_777 . ? C3 O4 Rh1 117.70(16) 3_777 . ? C3 O5 Rh1 118.80(16) . . ? C1 O2 Rh1 118.06(16) . . ? O6 C4 C3 113.1(2) . . ? O6 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? O6 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O3 C2 C1 112.9(2) . . ? O3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? O3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O4 C3 O5 126.9(2) 3_777 . ? O4 C3 C4 117.5(2) 3_777 . ? O5 C3 C4 115.6(2) . . ? O2 C1 O1 126.7(2) . 3_777 ? O2 C1 C2 117.9(2) . . ? O1 C1 C2 115.3(2) 3_777 . ? _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) ; #====================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #========================================================================= # END of CIF #=========================================================================