Solid-State Changes in Ligand-to-Metal Charge-Transfer Spectra of (NH3)5RuIII(2,4-dihydroxybenzoate) and (NH3)5RuIII(xanthine) Chromophores
Karsten Krogh-Jespersen; Robert T. Stibrany; Elizabeth John; John D. Westbrook; Thomas J. Emge; Michael J. Clarke; Joseph A. Potenza; Harvey J. Schugar; Inorganic Chemistry 47 (2008) 9813–9827; doi:10.1021/ic800511g

data_4305515
_publ_contact_author
;
  Joseph A. Potenza
  Department of Chemistry and Chemical Biology
  Rutgers, The State University of New Jersey
  610 Taylor Road
  Piscataway, New Jersey 08801 USA
;
_publ_contact_author_email       potenza@rutchem.com
_publ_section_title
;
Solid-State Changes in Ligand-to-Metal Charge-Transfer Spectra of
(NH3)5RuIII(2,4-dihydroxybenzoate) and (NH3)5RuIII(xanthine) Chromophores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9813
_journal_page_last               9827
_journal_paper_doi               10.1021/ic800511g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '2(C7 H20 N5 O4 Ru),C3 H7 N O, 2(O4 S)'
_chemical_formula_sum            'C17 H47 N11 O17 Ru2 S2'
_chemical_formula_weight         943.94
_chemical_name_common            2
_chemical_name_systematic
; 
 [(NH~3~)~5~Ru(III)(2,4-dihydroxybenzoate)]^.^SO~4~^.^0.5(CH~3~)~2~NCHO 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.970(10)
_cell_angle_beta                 93.920(10)
_cell_angle_gamma                80.923(8)
_cell_formula_units_Z            1
_cell_length_a                   9.6174(8)
_cell_length_b                   12.864(2)
_cell_length_c                   7.3320(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      18.7
_cell_measurement_theta_min      12.1
_cell_volume                     893.6(2)
_computing_cell_refinement       'Enraf-Nonius SDP (1985)'
_computing_data_collection       'Enraf-Nonius SDP (1985)'
_computing_data_reduction        'CAD-4-PC (Enraf-Nonius, 1993)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996), ORTEP32 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(1)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'scintillation counter'
_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  0.6316
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2302
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      1.75(1)
_exptl_crystal_density_method
'floatation in mixture of 1,2-dibromoethane/heptane'
_exptl_crystal_description       plate
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         2301
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.2455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                2231
_reflns_number_total             2301
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800511g_si_001_5.cif
_cod_data_source_block           ruyel
_cod_database_code               4305515