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_4088488
_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         'C57 H75 Br Mo2 N4 O'
_chemical_formula_sum            'C57 H75 Br Mo2 N4 O'
_chemical_formula_weight         1104.00
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/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                 109.111(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.855(3)
_cell_length_b                   18.257(3)
_cell_length_c                   21.137(3)
_cell_measurement_reflns_used    7869
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.86
_cell_volume                     5416.6(16)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34677
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.9072
_exptl_absorpt_correction_T_min  0.6431
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0479P)^2^+2.2803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                7080
_reflns_number_total             9509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00132_si_003.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        5416.6(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088488