Tris(pyronato)- and Tris(pyridonato)-ruthenium(III) Complexes and Solution NMR Studies
David C. Kennedy; Adam Wu; Brian O. Patrick; Brian R. James; Inorganic Chemistry 44 (2005) 6529–6535; doi:10.1021/ic050034d

data_4309555
_publ_section_title
;
Tris(pyronato)- and Tris(pyridonato)-ruthenium(III) Complexes and Solution
NMR Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6529
_journal_page_last               6535
_journal_paper_doi               10.1021/ic050034d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C18 H15 O9 Ru'
_chemical_formula_weight         476.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.017(3)
_cell_length_b                   11.6860(8)
_cell_length_c                   18.6414(14)
_cell_measurement_reflns_used    10999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      3.04
_cell_volume                     3707.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3820
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3820
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                1991
_reflns_number_total             3820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050034dsi20050110_071317.cif
_cod_data_source_block           bj297
_cod_original_cell_volume        3707.0(7)
_cod_database_code               4309555