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_4114033
_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            'C21 H39 Mo O3 P'
_chemical_formula_weight         466.43
_chemical_name_common            PMo(O(1-MeCy))3
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   10.8130(4)
_cell_length_b                   10.8130(4)
_cell_length_c                   69.271(3)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    183(2)
_cell_volume                     7014.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD Area-detector'
_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  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            8573
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.646
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+12.6036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                1016
_reflns_number_total             1127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0354317si20030616_025104_1.cif
_cod_data_source_block           002174m
_cod_original_cell_volume        7014.2(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4114033