Trapping of Hemiquinone Radicals at Mo and P Sites by Phosphide-Bridged Dimolybdenum Species: Chemistry of Complexes [Mo2(η5-C5H5)2(OC6H4OH)(μ-PR2)(CO)4] and [Mo2(η5-C5H5)2{μ-PR(OC6H4OH)}(CO)4]-(R = Cy, Ph)
Alvarez, Celedonio M.; Alvarez, M. Angeles; Alonso, María; García, M. Esther; Rueda, M. Teresa; Ruiz, Miguel A.; Herson, Patrick; Inorganic Chemistry 45 (2006) 9593–9606; doi:10.1021/ic061344e

data_4333056
_publ_section_title
;
 Trapping of Hemiquinone Radicals at Mo and P Sites by Phosphide-Bridged
 Dimolybdenum Species:&#x00A0; Chemistry of Complexes
 [Mo2(\h5-C5H5)2(OC6H4OH)(\m-PR2)(CO)4] and
 [Mo2(\h5-C5H5)2{\m-PR(OC6H4OH)}(CO)4]-(R = Cy, Ph)
;
_journal_issue                   23
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9593
_journal_page_last               9606
_journal_paper_doi               10.1021/ic061344e
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H31 Mo2 O6 P1'
_chemical_formula_sum            'C24 H31 Mo2 O6 P'
_chemical_formula_weight         638.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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      2.2
_audit_creation_date             2006-03-10T10:02:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.517(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.252(3)
_cell_length_b                   8.8714(15)
_cell_length_c                   18.616(3)
_cell_measurement_reflns_used    1435
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.655
_cell_measurement_wavelength     0.71073
_cell_volume                     2518.8(8)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker Smart'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega 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  0.0460
_diffrn_reflns_av_unetI/netI     0.041
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21567
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.035
_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^)+(0.0345P)^2^+0.9836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3765
_reflns_number_total             5503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061344esup2.cif
_cod_data_source_block           compound8a
_cod_depositor_comments
;
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_original_formula_sum        'C24 H31 Mo2 O6 P1'
_cod_database_code               4333056