New Dinuclear Ruthenium Complexes: Structure and Oxidative Catalysis
Carlo Di Giovanni; Lydia Vaquer; Xavier Sala; Jordi Benet-Buchholz; Antoni Llobet; Inorganic Chemistry 52 (2013) 4335–4345; doi:10.1021/ic302481s

data_4334447
_publ_section_title
;
 New Dinuclear Ruthenium Complexes: Structure and Oxidative Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4335
_journal_page_last               4345
_journal_paper_doi               10.1021/ic302481s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C144 H100 F24 N32 O20 P4 Ru8'
_chemical_formula_weight         3987.00
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.256(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0198(19)
_cell_length_b                   34.255(5)
_cell_length_c                   30.625(4)
_cell_measurement_reflns_used    5482
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.08
_cell_measurement_theta_min      2.24
_cell_volume                     16671(4)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support whith MicroMount'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_sigmaI/netI    0.1864
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62722
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'rotating anode x-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate
_exptl_crystal_F_000             7904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
In order to avoid highly disordered water molecules the program Squeeze
was used. In total 32 diferent positions with disordered water molecules
were localized in the inital structure model.
Squeeze integrated on Platon: A.L.Speek (200)) Acta Cryst. D65, 148-155.
;
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2106
_refine_ls_number_reflns         26196
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                12196
_reflns_number_total             26196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302481s_si_002_2.cif
_cod_data_source_block           cdg268e_0m
_cod_database_code               4334447