High Yield Synthesis and Reactivity of a Phosphinidene Bridged Dimolybdenum Complex
M. Esther García; Víctor Riera; Miguel A. Ruiz; David Sáez; Jacqueline Vaissermann; John C. Jeffery; Journal of the American Chemical Society 124 (2002) 14304–14305; doi:10.1021/ja021072o

data_4115345
_publ_contact_author             'Ruiz, Miguel A.'
_publ_contact_author_email       ' mara@sauron.quimica.uniovi.es '
_publ_contact_author_fax         ' 34 985 103446 '
_publ_section_title
;
 High Yield Synthesis and Reactivity of a Phosphinidene Bridged
 Dimolybdenum Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14304
_journal_page_last               14305
_journal_paper_doi               10.1021/ja021072o
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C44 H47 Mo2 O4 P'
_chemical_formula_weight         862.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.244(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1070(12)
_cell_length_b                   24.320(3)
_cell_length_c                   16.839(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4096.3(9)
_computing_data_collection       SMART/SAINT
_computing_molecular_graphics    XSHELL
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD '
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26584
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         9307
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                7054
_reflns_number_total             9307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja021072o_s1_3.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        4096.3(8)
_cod_database_code               4115345