Redox-Active Ligands Facilitate Bimetallic O2 Homolysis at Five-Coordinate Oxorhenium(V) Centers
Cameron A. Lippert; Stephen A. Arnstein; C. David Sherrill; Jake D. Soper; Journal of the American Chemical Society 132 (2010) 3879–3892; doi:10.1021/ja910500a

data_4102131
_publ_contact_author_address
;School of Chemistry and Biochemistry
Georgia Institute of Technology
Atlanta, GA  30332-0400
;
_publ_contact_author_email       jake.soper@chemistry.gatech.edu
_publ_contact_author_name        'Jake D. Soper'
_publ_contact_author_phone       404-894-4022
_publ_section_title
;
 Redox-Active Ligands Facilitate Bimetallic O2 Homolysis at
 Five-Coordinate Oxorhenium(V) Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3879
_journal_page_last               3892
_journal_paper_doi               10.1021/ja910500a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C31 H40 N O10.5 P Re'
_chemical_formula_weight         811.81
_chemical_name_common            (Et3NH)[ReV(O)(PPh3)(ox)2]1.5EtOH
_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                90.283(8)
_cell_angle_beta                 97.568(7)
_cell_angle_gamma                99.833(8)
_cell_formula_units_Z            2
_cell_length_a                   9.694(5)
_cell_length_b                   13.247(6)
_cell_length_c                   13.861(7)
_cell_measurement_reflns_used    6871
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.43
_cell_volume                     1737.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23686
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_T_max  0.5969
_exptl_absorpt_correction_T_min  0.3006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue/purple
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0410P)^2^+1.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                7893
_reflns_number_total             8461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910500a_si_001.cif
_cod_data_source_block           '[ReV(O)(PPh3)(ox)2]-'
_cod_original_cell_volume        1737.8(14)
_cod_original_formula_sum        'C31 H40 N O10.50 P Re'
_cod_database_code               4102131