Nonclassical Oxygen Atom Transfer as a Synthetic Strategy: Preparation of an Oxorhenium(V) Complex of the Bis(3,5-di-tert-butyl-2-phenoxo)amide Ligand
Daniel D. Wright; Seth N. Brown; Inorganic Chemistry 52 (2013) 7831–7833; doi:10.1021/ic4010592

data_4335492
_publ_section_title
;
 Nonclassical Oxygen Atom Transfer as a Synthetic Strategy: Preparation of
 an Oxorhenium(V) Complex of the Bis(3,5-di-tert-butyl-2-phenoxo)amide
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7831
_journal_page_last               7833
_journal_paper_doi               10.1021/ic4010592
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H55 N O3 P Re'
_chemical_formula_sum            'C46 H55 N O3 P Re'
_chemical_formula_weight         887.08
_chemical_name_common            (ONO)ReO(PPh3)
_chemical_name_systematic
;
 Oxo(triphenylphosphine)(bis(3,5-di-tert-butyl-2-phenoxo)amido)rhenium(V)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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                   10.1620(6)
_cell_length_b                   14.7652(9)
_cell_length_c                   28.6116(18)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.46
_cell_volume                     4293.0(5)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            68460
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.7218
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method
;
 Crystals were grown from a methanol solution of the complex
after filtration through silica gel.
;
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         12039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0387
_reflns_number_gt                11313
_reflns_number_total             12039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010592_si_002.cif
_cod_data_source_block           reop
_cod_database_code               4335492