Methine (CH) Transfer via a Chlorine Atom Abstraction/Benzene-Elimination Strategy: Molybdenum Methylidyne Synthesis and Elaboration to a Phosphaisocyanide Complex
Theodor Agapie; Paula L. Diaconescu; Christopher C. Cummins; Journal of the American Chemical Society 124 (2002) 2412–2413; doi:10.1021/ja017278r

data_4114678
_publ_section_title
;
 Methine (CH) Transfer via a Chlorine Atom Abstraction/Benzene-Elimination
 Strategy: Molybdenum Methylidyne Synthesis and Elaboration to a
 Phosphaisocyanide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2412
_journal_page_last               2413
_journal_paper_doi               10.1021/ja017278r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C106 H154 Mo2 N6 Na2 O5 P2'
_chemical_formula_weight         1892.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.7850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0270(19)
_cell_length_b                   11.0543(7)
_cell_length_c                   38.510(3)
_cell_measurement_temperature    183(2)
_cell_volume                     11536.1(14)
_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 0.995
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            22720
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.9536
_exptl_absorpt_correction_T_min  0.9128
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         8301
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.316
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+53.3129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                7727
_reflns_number_total             8301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017278r_s2.cif
_cod_data_source_block           01148m
_cod_original_cell_volume        11536.2(13)
_cod_database_code               4114678