Reaction of N[triple bond, length as m-dash]W(O(t)Bu)(3) with σ(3)λ(5)-phosphoranes. The [2 + 2] cycloaddition across the W[triple bond, length as m-dash]N triple bond results in the first representative of an inorganic four-membered metallacycle with conjugated endo- and exocyclic double bonds.
Kovalenko, Oleksandr O.; Kinzhybalo, Vasyl; Lis, Tadeusz; Khavryuchenko, Oleksiy V.; Rusanov, Eduard B.; Brusilovets, Anatolii I.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 5132–5136; doi:10.1039/c2dt12492k

data_7018928
_publ_section_title
;
 Reaction of N[triple bond, length as m-dash]W(O(t)Bu)(3) with
 \s(3)\l(5)-phosphoranes. The [2 + 2] cycloaddition across the W[triple
 bond, length as m-dash]N triple bond results in the first representative
 of an inorganic four-membered metallacycle with conjugated endo- and
 exocyclic double bonds.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5132
_journal_page_last               5136
_journal_paper_doi               10.1039/c2dt12492k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C22 H54 N3 O3 P S Si2 W'
_chemical_formula_weight         711.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.321(6)
_cell_length_b                   10.967(3)
_cell_length_c                   32.293(10)
_cell_measurement_reflns_used    11387
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      1.07
_cell_volume                     6740(4)
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT v7.34a (Bruker, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            43909
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    3.633
_exptl_absorpt_correction_T_max  0.6118
_exptl_absorpt_correction_T_min  0.4189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker-Nonius, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         14645
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+9.9928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                11387
_reflns_number_total             14645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12492k.txt
_cod_data_source_block           b2
_cod_original_cell_volume        6740(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7018928