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_4082696
_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         'C32 H12 B F24, C36 H42 Mo2 O2 P'
_chemical_formula_sum            'C68 H54 B F24 Mo2 O2 P'
_chemical_formula_weight         1592.77
_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_date             2014-01-27T17:01:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.047(5)
_cell_angle_beta                 90.120(5)
_cell_angle_gamma                91.407(5)
_cell_formula_units_Z            2
_cell_length_a                   14.051(5)
_cell_length_b                   14.551(5)
_cell_length_c                   15.927(5)
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      19.826
_cell_measurement_theta_min      2.365
_cell_measurement_wavelength     0.71073
_cell_volume                     3255.4(19)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            48834
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         12179
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+10.9903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                9373
_reflns_number_total             12179
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om401192m_si_002.cif
_cod_data_source_block           compound8p
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-10

The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_database_code               4082696