Deprotonation Induced Ligand-to-Metal Electron Transfer: Synthesis of a Mixed-Valence Rh(-I,I) Dinuclear Compound and Its Reaction with Dioxygen
Cristina Tejel; Miguel A. Ciriano; M. Pilar del Río; Fieke van den Bruele; Dennis G. H. Hetterscheid; Nearchos Tsichlis i Spithas; Bas de Bruin; Journal of the American Chemical Society 130 (2008) 5844–5845; doi:10.1021/ja711495v

data_4107738
_publ_contact_author_address
;
 Dr. Cristina Tejel
 Departamento de Qu\'imica Inorg\'anica
 Instituto de Ciencia de Materiales de Arag\'on
 C.S.I.C.-Universidad de Zaragoza
 50009 Zaragoza, Spain
;
_publ_contact_author_email       ctejel@unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Cristina Tejel'
_publ_contact_author_phone       '+34 976 762285'
_publ_section_title
;
 Deprotonation Induced Ligand-to-Metal Electron Transfer: Synthesis of a
 Mixed-Valence Rh(-I,I) Dinuclear Compound and Its Reaction with Dioxygen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5844
_journal_page_last               5845
_journal_paper_doi               10.1021/ja711495v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '(C26 H28 N3 Rh2 Cl);1.5(H2 O)'
_chemical_formula_sum            'C26 H31 Cl N3 O1.5 Rh2'
_chemical_formula_weight         650.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                68.666(2)
_cell_angle_beta                 80.702(2)
_cell_angle_gamma                84.965(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8928(9)
_cell_length_b                   11.4651(12)
_cell_length_c                   13.0649(13)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.418
_cell_measurement_theta_min      2.322
_cell_volume                     1223.9(2)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v. 6.10 Bruker 2000'
_computing_publication_material  'XCIF program, SHELTXL v. 6.10, Bruker 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\W rotations with narrow frames'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10426
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.8585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction (1996)
Bruker-AXS Nithin SAINT+ package v. 6.01  
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.8459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                3863
_reflns_number_total             5299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711495v-file001.cif
_cod_data_source_block           cta79ac
_cod_original_formula_sum        'C26 H31 Cl N3 O1.50 Rh2'
_cod_database_code               4107738