The Synthesis and Reactivity of a Molybdenum (IV) Stretched-Dihydrogen Complex
Thomas M. Cameron; Carlos G. Ortiz; Ion Ghiviriga; Khalil A. Abboud; James M. Boncella; Journal of the American Chemical Society 124 (2002) 922–923; doi:10.1021/ja0169365

data_4114610
_publ_section_title
;
 The Synthesis and Reactivity of a Molybdenum (IV) Stretched-Dihydrogen
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              922
_journal_page_last               923
_journal_paper_doi               10.1021/ja0169365
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C27 H54 Mo N3 P3 Si2'
_chemical_formula_weight         665.76
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.721(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4675(6)
_cell_length_b                   31.094(2)
_cell_length_c                   11.3851(6)
_cell_measurement_temperature    173(2)
_cell_volume                     3442.5(3)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23094
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00073(11)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.2999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                6606
_reflns_number_total             7865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0169365_s2.cif
_cod_data_source_block           1
_cod_database_code               4114610