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_4088497
_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 H93 Cl2 Mo2 N5 O2'
_chemical_formula_sum            'C69 H93 Cl2 Mo2 N5 O2'
_chemical_formula_weight         1287.26
_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                 99.784(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0752(6)
_cell_length_b                   24.9881(12)
_cell_length_c                   22.0685(11)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.23
_cell_volume                     6562.0(6)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44083
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown(dark)
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         11604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1085P)^2^+1.5617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1829
_reflns_number_gt                8566
_reflns_number_total             11604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00132_si_003.cif
_cod_data_source_block           compound_17
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088497