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_7015786
_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         'C30 H78 Mo2 N3 O6 P Si4'
_chemical_formula_sum            'C30 H78 Mo2 N3 O6 P Si4'
_chemical_formula_weight         912.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                88.52(3)
_cell_angle_beta                 86.50(3)
_cell_angle_gamma                64.50(3)
_cell_formula_units_Z            2
_cell_length_a                   11.760(3)
_cell_length_b                   13.424(4)
_cell_length_c                   16.339(5)
_cell_measurement_reflns_used    30064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      4
_cell_volume                     2323.8(13)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35863
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.68
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_correction_T_min  0.7632
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 1995-2003)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.810
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         13203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0688P)^2^+0.6707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                10678
_reflns_number_total             13203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10099h.txt
_cod_data_source_block           anat1abs
_cod_original_cell_volume        2323.8(12)
_cod_database_code               7015786