Reactions of the Carbyne-Bridged Radical Complex [Mo2(η5-C5H5)2(μ-CPh)(μ-PCy2)(μ-CO)]+with Bidentate Ligands Having E‒H Bonds (E = O, S, N)
Alvarez, M. Angeles; García, M. Esther; Menéndez, Sonia; Ruiz, Miguel A.; Organometallics 33 (2014) 1181–; doi:10.1021/om401192m

data_4082695
_publ_section_title
;
 Reactions of the Carbyne-Bridged Radical Complex
 [Mo2(\h5-C5H5)2(\m-CPh)(\m-PCy2)(\m-CO)]+with Bidentate Ligands Having
 E--H Bonds (E = O, S, N)
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1181
_journal_paper_doi               10.1021/om401192m
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H41 Mo2 O3 P, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C37.5 H44 Cl3 Mo2 O3 P'
_chemical_formula_weight         871.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.629(3)
_cell_angle_beta                 70.066(3)
_cell_angle_gamma                64.625(3)
_cell_formula_units_Z            4
_cell_length_a                   14.9549(5)
_cell_length_b                   16.6837(5)
_cell_length_c                   18.6223(7)
_cell_measurement_reflns_used    20671
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      73.2874
_cell_measurement_theta_min      3.0310
_cell_measurement_wavelength     1.54184
_cell_volume                     3814.0(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33745
_diffrn_reflns_theta_full        73.45
_diffrn_reflns_theta_max         73.45
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    7.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.467
_refine_diff_density_min         -1.64
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         14720
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+9.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                12492
_reflns_number_total             14720
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om401192m_si_002.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C75 H88 Cl6 Mo4 O6 P2'
_cod_original_formula_weight         1743.85
_cod_original_formula_moiety         '2(C36 H41 Mo2 O3 P), 3(C H2 Cl2)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3814.0(2)
_cod_database_code               4082695