Mild P-P Bond Cleavage in the Methyldiphosphenyl Complex [Mo2Cp2(μ-PCy2)(μ-κ(2):κ(2)-P2Me)(CO)2] To Give Novel Phosphide-Bridged Trinuclear Derivatives.
Alvarez, M. Angeles; García, M Esther; García-Vivó, Daniel; Lozano, Raquel; Ramos, Alberto; Ruiz, Miguel A.; Inorganic chemistry 53 (2014) 11261–11273; doi:10.1021/ic501857f

data_4341286
_publ_section_title
;
 Mild P-P Bond Cleavage in the Methyldiphosphenyl Complex
 [Mo2Cp2(\m-PCy2)(\m-\k(2):\k(2)-P2Me)(CO)2] To Give Novel
 Phosphide-Bridged Trinuclear Derivatives.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11261
_journal_page_last               11273
_journal_paper_doi               10.1021/ic501857f
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H35 Fe Mo2 O5 P3'
_chemical_formula_sum            'C28 H35 Fe Mo2 O5 P3'
_chemical_formula_weight         792.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.591(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9099(2)
_cell_length_b                   23.5511(5)
_cell_length_c                   15.7915(4)
_cell_measurement_reflns_used    9131
_cell_measurement_temperature    100.2(2)
_cell_measurement_theta_max      69.4748
_cell_measurement_theta_min      8.7995
_cell_measurement_wavelength     1.54184
_cell_volume                     3295.72(14)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17884
_diffrn_reflns_theta_full        69.6
_diffrn_reflns_theta_max         69.6
_diffrn_reflns_theta_min         8.81
_exptl_absorpt_coefficient_mu    11.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+2.6898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                5408
_reflns_number_total             6059
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501857f_si_002.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
'Adding full bibliography for 4341286--4341289.cif.'
_cod_original_cell_volume        3295.72(13)
_cod_database_code               4341286