Nucleophilic addition of phosphines to rhenium allenylidenes. Unprecedented double P‒H bond activation to give an η1-P-phospha-1-butadienyl ligand
Maurizio Peruzzini; Pierluigi Barbaro; Valerio Bertolasi; Claudio Bianchini; Isaac de los Rios; Nicoletta Mantovani; Lorenza Marvelli; Roberto Rossi; Dalton Trans.  (2003) 4121–4131; doi:10.1039/b303216g

data_7012982
_publ_section_title
;
 Nucleophilic addition of phosphines to rhenium allenylidenes.
 Unprecedented double P--H bond activation to give an
 \h1-P-phospha-1-butadienyl ligand
;
_journal_issue                   21
_journal_name_full               'Dalton Trans.'
_journal_page_first              4121
_journal_page_last               4131
_journal_paper_doi               10.1039/b303216g
_journal_year                    2003
_chemical_formula_moiety         'C58 H49 O2 P3 Re, C24 H20 B'
_chemical_formula_sum            'C82 H69 B O2 P3 Re'
_chemical_formula_weight         1376.29
_chemical_name_systematic
;
?
;
_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                113.430(1)
_cell_angle_beta                 105.697(1)
_cell_angle_gamma                93.961(1)
_cell_formula_units_Z            2
_cell_length_a                   12.2030(2)
_cell_length_b                   16.7569(3)
_cell_length_c                   19.3716(5)
_cell_measurement_reflns_used    52404
_cell_measurement_temperature    295
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3428.34(13)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD server software'
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.062
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52404
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV: R.H. Blessing, Acta Crystallogr. Sect A, 1995, 51, 33
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.965
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         19771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+2.1037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                15139
_reflns_number_total             19771
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b303216g.txt
_cod_data_source_block           (I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3428.3(1)
_cod_database_code               7012982