Reductive Cleavage of Acyl Halides to Carboxylato Alkylidyne Complexes from Their Reactions with the Quintuply Bonded Dimolybdenum Amidinate
Harisomayajula, N. V. Satyachand; Chen, Han-Gung; Kuo, Ting-Shen; Tsai, Yi-Chou; Organometallics 35 (2016) 1534–; doi:10.1021/acs.organomet.6b00132

data_4088500
_publ_section_title
;
 Reductive Cleavage of Acyl Halides to Carboxylato Alkylidyne Complexes
 from Their Reactions with the Quintuply Bonded Dimolybdenum Amidinate
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1534
_journal_paper_doi               10.1021/acs.organomet.6b00132
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C69 H92 Cl2 Mo2 N4 O3'
_chemical_formula_sum            'C69 H92 Cl2 Mo2 N4 O3'
_chemical_formula_weight         1288.25
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 121.509(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   59.79(4)
_cell_length_b                   11.819(8)
_cell_length_c                   45.08(3)
_cell_measurement_reflns_used    1199
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.09
_cell_measurement_theta_min      2.23
_cell_volume                     27159(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX2'
_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  0.2345
_diffrn_reflns_av_sigmaI/netI    0.4096
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            78865
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9951
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10816
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.561
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1311
_refine_ls_number_reflns         23706
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.2582
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2244
_reflns_number_gt                6903
_reflns_number_total             23706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00132_si_003.cif
_cod_data_source_block           compound_20
_cod_original_cell_volume        27156(33)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4088500