Deoxygenation of Nitroxyl Radicals by Oxorhenium(V) Complexes with Redox-Active Ligands
Cameron A. Lippert; Jake D. Soper; Inorganic Chemistry 49 (2010) 3682–3684; doi:10.1021/ic9024684

data_4315376
_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
;
 Deoxygenation of Nitroxyl Radicals by Oxorhenium(V) Complexes with
 Redox-Active Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3682
_journal_page_last               3684
_journal_paper_doi               10.1021/ic9024684
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H60 N O5 Re'
_chemical_formula_sum            'C36 H60 N O5 Re'
_chemical_formula_weight         773.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   11.6064(8)
_cell_length_b                   30.002(2)
_cell_length_c                   10.6924(7)
_cell_measurement_reflns_used    6310
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.27
_cell_measurement_theta_min      2.59
_cell_volume                     3723.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34143
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.27
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.302
_exptl_absorpt_correction_T_max  0.9074
_exptl_absorpt_correction_T_min  0.2639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.241
_refine_diff_density_min         -2.651
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0389P)^2^+18.6619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                2885
_reflns_number_total             3835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9024684_si_002.cif
_cod_data_source_block           '[ReV(O)(3,5-tBu2cat)2]-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3723.2(4)
_cod_database_code               4315376