Kinetic Addition of Nucleophiles to η3-Propargyl Rhenium Complexes Occurs at the Central Carbon to Produce Rhenacyclobutenes
Charles P. Casey; John R. Nash; Chae S. Yi; Anthony D. Selmeczy; Steven Chung; Douglas R. Powell; Randy K. Hayashi; Journal of the American Chemical Society 120 (1998) 722–733; doi:10.1021/ja9729847

data_4116675
_publ_contact_author
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    Prof. Charles P. Casey 
    Department of Chemistry 
    University of Wisconsin 
    Madison, WI  53706-1396  USA 
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_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
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 Kinetic Addition of Nucleophiles to \h3-Propargyl Rhenium Complexes
 Occurs at the Central Carbon to Produce Rhenacyclobutenes
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              722
_journal_page_last               733
_journal_paper_doi               10.1021/ja9729847
_journal_volume                  120
_journal_year                    1998
_chemical_formula_moiety         '(C22 H35 O2 P Re)+ (B F4)-'
_chemical_formula_structural     '(C22 H35 O2 P Re)+ (B F4)-'
_chemical_formula_sum            'C22 H35 B F4 O2 P Re'
_chemical_formula_weight         635.48
_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                 101.218(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.6741(2)
_cell_length_b                   11.9960(3)
_cell_length_c                   16.6122(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     5018.58(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11098
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0.32
_diffrn_standards_number         367
_exptl_absorpt_coefficient_mu    4.952
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.979
_refine_diff_density_min         -2.033
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.030
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_obs          0.0316
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0785
_refine_ls_wR_factor_obs         0.0777
_reflns_number_observed          4889
_reflns_number_total             5029
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9729847.cif
_cod_data_source_block           compound_4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0408P)^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^)+(0.0408P)^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 
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_cod_original_cell_volume        5018.6(2)
_cod_database_code               4116675