Protonation of Rhenium Alkyne Complexes Produces η3-Allyl Rhenium Complexes via Observable 1-Metallacyclopropene Intermediates
Charles P. Casey; John T. Brady; Timothy M. Boller; Frank Weinhold; Randy K. Hayashi; Journal of the American Chemical Society 120 (1998) 12500–12511; doi:10.1021/ja9815374

data_4116900
_publ_contact_author
; 
    Prof. Charles P. Casey 
    Department of Chemistry 
    University of Wisconsin 
    Madison, WI  53706-1396  USA 
;
_publ_contact_author_email       casey@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2620584
_publ_section_title
;
 Protonation of Rhenium Alkyne Complexes Produces \h3-Allyl Rhenium
 Complexes via Observable 1-Metallacyclopropene Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12500
_journal_page_last               12511
_journal_paper_doi               10.1021/ja9815374
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C26 H26 B F4 O2 Re'
_chemical_formula_weight         643.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.055(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1677(3)
_cell_length_b                   11.5677(3)
_cell_length_c                   14.4477(3)
_cell_measurement_reflns_used    5050
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     2487.89(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi 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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5261
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0.01
_diffrn_standards_number         174
_exptl_absorpt_coefficient_mu    4.935
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.887
_refine_diff_density_min         -3.030
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.051(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_obs          0.0287
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0712
_refine_ls_wR_factor_obs         0.0705
_reflns_number_observed          4217
_reflns_number_total             4544
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9815374.cif
_cod_data_source_block           compound_12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116900