Quantitative Determination of the Regioselectivity of Nucleophilic Addition to η-Propargyl Rhenium Complexes and Direct Observation of an Equilibrium Between η-Propargyl Rhenium Complexes and Rhenacyclobutenes.
Casey, Charles P.; Boller, Timothy M.; Samec, Joseph S. M.; Reinert-Nash, John R; Organometallics 28 (2009) 123–131; doi:10.1021/om800739j

data_4068348
_publ_section_title
;
 Quantitative Determination of the Regioselectivity of Nucleophilic
 Addition to \h-Propargyl Rhenium Complexes and Direct Observation of an
 Equilibrium Between \h-Propargyl Rhenium Complexes and Rhenacyclobutenes.
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              123
_journal_page_last               131
_journal_paper_doi               10.1021/om800739j
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         '(C49 H46 F12 O2 P2 Re)+ (B F4)- 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H50 B Cl4 F16 O2 P2 Re'
_chemical_formula_weight         1399.66
_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                 91.723(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.907(2)
_cell_length_b                   15.589(3)
_cell_length_c                   24.225(5)
_cell_measurement_reflns_used    3279
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.61
_cell_volume                     5627.0(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device       'Bruker SMART/P4'
_diffrn_measurement_method       '\f scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1882
_diffrn_reflns_av_sigmaI/netI    0.3767
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21340
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        -0.08
_diffrn_standards_number         130
_exptl_absorpt_coefficient_mu    2.498
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.00447(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         8864
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.2227
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                3312
_reflns_number_total             8864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800739j_si_001.cif
_cod_data_source_block           99186
_cod_database_code               4068348