Synthesis of Heterocyclic Ligands by Diheterocyclization at the Rhenium(I) Allenylidene [(triphos)(CO)2Re{C=C=CPh2}](OSO2CF3). 1. Reactivity with Dipolar N,N-Heterocycles
Nicoletta Mantovani; Paola Bergamini; Andrea Marchi; Lorenza Marvelli; Roberto Rossi; Valerio Bertolasi; Valeria Ferretti; Isaac de los Rios; Maurizio Peruzzini; Organometallics 25 (2006) 416–426; doi:10.1021/om050663v

data_4063317
_publ_section_title
;
 Synthesis of Heterocyclic Ligands by Diheterocyclization at the
 Rhenium(I) Allenylidene [(triphos)(CO)2Re{C\\db C\\db CPh2}](OSO2CF3).
 1. Reactivity with Dipolar N,N-Heterocycles
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              416
_journal_page_last               426
_journal_paper_doi               10.1021/om050663v
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C61 H52 N2 O2 P3 Re S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C61.5 H53 Cl N2 O2 P3 Re S'
_chemical_formula_weight         1198.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.0420(6)
_cell_angle_beta                 76.4760(7)
_cell_angle_gamma                61.3240(6)
_cell_formula_units_Z            2
_cell_length_a                   13.7255(2)
_cell_length_b                   14.2675(2)
_cell_length_c                   17.4984(3)
_cell_measurement_reflns_used    43543
_cell_measurement_temperature    295
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.13
_cell_volume                     2830.74(8)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD server software (Nonius, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III(Burnett & Johnson, 1996)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43543
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.706
_refine_diff_density_min         -2.183
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0135(6)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         16126
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+2.9303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                13966
_reflns_number_total             16126
_reflns_threshold_expression     I>2sigma(I)
_cod_original_formula_sum        'C61.50 H53 Cl N2 O2 P3 Re S'
_cod_database_code               4063317