New Dicarboxylic Acid Bipyridine Ligand for Ruthenium Polypyridyl Sensitization of TiO2
William B. Heuer; Hai-Long Xia; William Ward; Zhen Zhou; Wayne H. Pearson; Maxime A. Siegler; Amy A. Narducci Sarjeant; Maria Abrahamsson; Gerald J. Meyer; Inorganic Chemistry 51 (2012) 3981–3988; doi:10.1021/ic201395q

data_4328729
_publ_section_title
;
 New Dicarboxylic Acid Bipyridine Ligand for Ruthenium Polypyridyl
 Sensitization of TiO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3981
_journal_page_last               3988
_journal_paper_doi               10.1021/ic201395q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C34 H24 N6 O4 Ru, 3(C H4 O), 2(Cl)'
_chemical_formula_sum            'C37 H36 Cl2 N6 O7 Ru'
_chemical_formula_weight         848.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5838(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.82563(16)
_cell_length_b                   18.6217(4)
_cell_length_c                   25.0098(4)
_cell_measurement_reflns_used    20892
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      1.96
_cell_volume                     4090.81(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54048
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.29
_platon_squeeze_details
;
A first refinement against F2 was not completely satisfactory because
some residual electron density was found in two voids located at 
(0  0  0.5) and (0  0.5  0), which include 67 electrons in a volume
of 238 \%A3. Such voids contains some amount of disordered solvent
molecules (probably methanol). Their contribution was then taken
out for the subsequent stages of the refinement 
using the program SQUEEZE. 
;
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8032
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+7.4444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                7177
_reflns_number_total             8032
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201395q_si_001_1.cif
_cod_data_source_block           Ru(bpy)2(dfm)(Cl)2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328729