Photochemically Generated Transients from κ2- and κ3-Triphos Derivatives of Group 6 Metal Carbonyls and Their Reactivity with Olefins
Kyran, Samuel J.; Muhammad, Sohail; Knestrick, Matthew; Bengali, Ashfaq A.; Darensbourg, Donald J.; Organometallics 31 (2012) 3163–; doi:10.1021/om300044k

data_4078032
_publ_section_title
;
 Photochemically Generated Transients from \k2- and \k3-Triphos
 Derivatives of Group 6 Metal Carbonyls and Their Reactivity with Olefins
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3163
_journal_paper_doi               10.1021/om300044k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C45 H39 Mo O5 P3'
_chemical_formula_sum            'C45 H39 Mo O5 P3'
_chemical_formula_weight         848.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.990(7)
_cell_angle_beta                 76.863(7)
_cell_angle_gamma                83.283(7)
_cell_formula_units_Z            2
_cell_length_a                   9.735(6)
_cell_length_b                   9.906(6)
_cell_length_c                   21.266(13)
_cell_measurement_reflns_used    6158
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      1.98
_cell_volume                     1974(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24184
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pale-brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             866
_exptl_crystal_recrystallization_method
'hexane vapor diffusion into a THF solution'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0409P)^2^+0.3480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                7744
_reflns_number_total             9733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300044k_si_001.cif
_cod_data_source_block           triphosmoco4
_cod_database_code               4078032