The Electronic Nature of Terminal Oxo Ligands in Transition-Metal Complexes: Ambiphilic Reactivity of Oxorhenium Species
Jessica L. Smeltz; Cassandra P. Lilly; Paul D. Boyle; Elon A. Ison; Journal of the American Chemical Society 135 (2013) 9433–9441; doi:10.1021/ja401390v

data_4119969
_publ_section_title
;
 The Electronic Nature of Terminal Oxo Ligands in Transition-Metal
 Complexes: Ambiphilic Reactivity of Oxorhenium Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9433
_journal_page_last               9441
_journal_paper_doi               10.1021/ja401390v
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C45 H32 B F15 N3 O2 Re'
_chemical_formula_weight         1128.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.018(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.405(3)
_cell_length_b                   13.412(3)
_cell_length_c                   28.537(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.92
_cell_measurement_theta_min      2.78
_cell_volume                     4879.0(18)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi 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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            147027
_diffrn_reflns_theta_full        36.67
_diffrn_reflns_theta_max         38.16
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_T_max  0.7282
_exptl_absorpt_correction_T_min  0.5889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Acta Cryst. (1990), A46, 194 as the 'BYPASS procedure'
P. v.d. Sluis & A.L. Spek
;
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         25465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                17634
_reflns_number_total             25465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401390v_si_001_6.cif
_cod_data_source_block           x12089
_cod_original_cell_volume        4879.1(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4119969