Molybdenum-Phosphorus Triple Bond Stabilization by Ancillary Alkoxide Ligation: Synthesis and Structure of a Terminal Phosphide Tris-1-methylcyclohexanoxide Complex
Frances H. Stephens; Joshua S. Figueroa; Paula L. Diaconescu; Christopher C. Cummins; Journal of the American Chemical Society 125 (2003) 9264–9265; doi:10.1021/ja0354317

data_4114034
_publ_section_title
;
 Molybdenum-Phosphorus Triple Bond Stabilization by Ancillary Alkoxide
 Ligation: Synthesis and Structure of a Terminal Phosphide
 Tris-1-methylcyclohexanoxide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9264
_journal_page_last               9265
_journal_paper_doi               10.1021/ja0354317
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C59 H75 Mo2 N2 O4 P2'
_chemical_formula_weight         1130.03
_chemical_name_common            (mu-P2)[Mo(N[i-Pr]Ar)(O-2,6-Me2C6H3)2]2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7073(8)
_cell_length_b                   16.8765(7)
_cell_length_c                   18.0139(7)
_cell_measurement_temperature    183(2)
_cell_volume                     5687.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22054
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.9734
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00006(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          1.714
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+14.7314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                3324
_reflns_number_total             4095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0354317si20030616_025104_2.cif
_cod_data_source_block           01033m
_cod_original_sg_symbol_H-M      'P 21 21 21'
_cod_database_code               4114034