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_7015783
_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_sum            'C27 H69 N2 O6 P Si3 W2'
_chemical_formula_weight         1000.78
_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                 99.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.679(3)
_cell_length_b                   16.861(4)
_cell_length_c                   21.651(6)
_cell_measurement_reflns_used    31714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      3
_cell_volume                     4200.3(19)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2003)'
_computing_data_reduction        CrysAlisRED
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64307
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    5.631
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction,
2003), analytical numeric
absorption using a multifaceted
crystal model
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.87
_refine_diff_density_min         -0.78
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         15009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                12588
_reflns_number_total             15009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10099h.txt
_cod_data_source_block           anat11pa
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7015783