Remarkable carbene-induced transformation of 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene, P3C3But3, to the 1,2,4-triphosphole, P3C2But2CBut(carbene). Crystal and molecular structure of the planar triphosphole complex [Mo(CO)3(η5-P3C2But2CBut(carbene))] [carbene = C(N(Me)C(Me)=C(Me)N(Me))]
Clendenning, Scott B.; Hitchcock, Peter B.; Nixon, John F.; Nyulászi, László; Chemical Communications  (2000) 1305–; doi:10.1039/b001285h

data_7110901
_publ_section_title
;
 Remarkable carbene-induced transformation of
 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene, P3C3But3, to the
 1,2,4-triphosphole, P3C2But2CBut(carbene). Crystal and molecular
 structure of the planar triphosphole complex
 [Mo(CO)3(\h5-P3C2But2CBut(carbene))] [carbene = C(N(Me)C(Me)=C(Me)N(Me))]
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1305
_journal_paper_doi               10.1039/b001285h
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H39 Mo1 N2 O3 P3'
_chemical_formula_structural     'C25 H39 N2 MO O3 P3'
_chemical_formula_sum            'C25 H39 Mo N2 O3 P3'
_chemical_formula_weight         604.43
_chemical_name_common            '[Mo(CO)3{P3C2tBu2C(tBu)(C3N2Me4)}]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-02-02T10:40:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.436(2)
_cell_angle_beta                 96.562(2)
_cell_angle_gamma                114.401(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5667(3)
_cell_length_b                   10.9262(3)
_cell_length_c                   13.8900(4)
_cell_measurement_reflns_used    10211
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     1448.18(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS_97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13414
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         4.62
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+0.9906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                4645
_reflns_number_total             5046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001285hsup1.cif
_cod_data_source_block           feb400
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110901