The Metal or the Ligand? The Preferred Locus for Redox Changes in Oxygen Atom Transfer Reactions of Rhenium Amidodiphenoxides.
Hoffman, Justin M.; Oliver, Allen G.; Brown, Seth N.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b00985

data_4125869
_publ_section_title
;
 The Metal or the Ligand? The Preferred Locus for Redox Changes in Oxygen
 Atom Transfer Reactions of Rhenium Amidodiphenoxides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b00985
_journal_year                    2017
_chemical_formula_moiety         'C56 H80 N2 O8 Re2'
_chemical_formula_sum            'C56 H80 N2 O8 Re2'
_chemical_formula_weight         1281.62
_chemical_name_common            (ONO^Cat^)ReO(\m-O)2ReO(ONO^Cat^)
_chemical_name_systematic
;
 Di-\m-oxo-bis(bis(3,5-di-tert-butyl-2-phenoxo)amido)-
dioxodirhenium(VII)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                76.2764(13)
_cell_angle_beta                 83.2527(13)
_cell_angle_gamma                69.4931(13)
_cell_formula_units_Z            1
_cell_length_a                   10.1539(10)
_cell_length_b                   11.2274(11)
_cell_length_c                   13.3373(13)
_cell_measurement_reflns_used    7435
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      2.46
_cell_volume                     1382.5(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004; Sheldrick, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT/XPREP
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.580
_diffrn_reflns_theta_min         2.459
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.487
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6234
_exptl_absorpt_correction_type   multi-scan
_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            'dark purple'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method
;
Crystals were grown by vapor diffusion of hexane into a
dichloromethane solution of the complex. 
;
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.7466
_exptl_transmission_factor_min   0.6234
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         8179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7207
_reflns_number_total             8179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00985_si_002.cif
_cod_data_source_block           repurple
_cod_database_code               4125869
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2013-4
_shelx_res_checksum              65806
_shelx_hkl_checksum              9970