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_7015785
_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_absolute_configuration ad
_chemical_formula_sum            'C28 H69 Mo2 N2 O6 P S Si2'
_chemical_formula_weight         840.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.439(3)
_cell_length_b                   17.008(5)
_cell_length_c                   25.776(7)
_cell_measurement_reflns_used    4
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10655
_cell_measurement_theta_min      55
_cell_volume                     4138(2)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'KUMA KM4 CCD kappa-geometry diffractometer'
_diffrn_measurement_method       /w
_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  0.1102
_diffrn_reflns_av_sigmaI/netI    0.1334
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53107
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.63
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         10070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0451
_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^)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                7195
_reflns_number_total             10070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10099h.txt
_cod_data_source_block           anat6abs
_cod_database_code               7015785