Reactions of ((i)PrO)3M≡M(O(i)Pr)3 (M = Mo, W) with low-coordinate phosphorus compounds. Formation of the first four-membered planar metallacycles, containing an M≡M triple bond.
Kovalenko, Oleksandr O.; Brusylovets, Oleksii A.; Kinzhybalo, Vasyl; Lis, Tadeusz; Brusilovets, Anatolii I.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 4814–4817; doi:10.1039/c1dt10099h

data_7015784
_publ_section_title
;
 Reactions of ((i)PrO)3M\\tb M(O(i)Pr)3 (M = Mo, W) with low-coordinate
 phosphorus compounds. Formation of the first four-membered planar
 metallacycles, containing an M\\tb M triple bond.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4814
_journal_page_last               4817
_journal_paper_doi               10.1039/c1dt10099h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C27 H69 Mo2 N2 O6 P Si3'
_chemical_formula_sum            'C27 H69 Mo2 N2 O6 P Si3'
_chemical_formula_weight         824.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.643(3)
_cell_length_b                   16.741(4)
_cell_length_c                   21.756(6)
_cell_measurement_reflns_used    17496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      4.28
_cell_volume                     4176.7(19)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
'Oxford Xcalibur PX \k-geometry diffractometer with CCD area detector'
;
_diffrn_measurement_method       '\w and \f'
_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  0.1081
_diffrn_reflns_av_sigmaI/netI    0.1163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51763
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 1995-2003)
;
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.038P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                6314
_reflns_number_total             8632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10099h.txt
_cod_data_source_block           anat3abs
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7015784