Mixed Ligated Tris(amidinate)dimolybdenum Complexes as Catalysts for Radical Addition of CCl4 to 1-Hexene: Leaving Ligand Lability Controls Catalyst Activity.
Rej, Supriya; Majumdar, Moumita; Kando, Shun; Sugino, Yoshitaka; Tsurugi, Hayato; Mashima, Kazushi; Inorganic chemistry 56 (2017) 634–644; doi:10.1021/acs.inorgchem.6b02525

data_4345145
_publ_section_title
;
 Mixed Ligated Tris(amidinate)dimolybdenum Complexes as Catalysts for
 Radical Addition of CCl4 to 1-Hexene: Leaving Ligand Lability Controls
 Catalyst Activity.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              634
_journal_page_last               644
_journal_paper_doi               10.1021/acs.inorgchem.6b02525
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C64 H59 Mo2 N6 O8 P (C4 H8 O)'
_chemical_formula_sum            'C68 H67 Mo2 N6 O9 P'
_chemical_formula_weight         1335.13
_chemical_name_common            Mo2-1b
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                102.092(5)
_cell_angle_beta                 109.366(5)
_cell_angle_gamma                109.082(5)
_cell_formula_units_Z            2
_cell_length_a                   15.094(5)
_cell_length_b                   15.389(5)
_cell_length_c                   15.719(5)
_cell_measurement_reflns_used    8262
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.24
_cell_volume                     3041.4(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2020
_diffrn_reflns_av_sigmaI/netI    0.3677
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29919
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_correction_T_min  0.9421
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         13573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.2900
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.2490
_reflns_number_gt                4147
_reflns_number_total             13573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02525_si_002.cif
_cod_data_source_block           Mo2-1b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4345145