Tris(3,5-di-tert-butylcatecholato)molybdenum(VI): Lewis Acidity and Nonclassical Oxygen Atom Transfer Reactions
Amanda H. Randolph; Nicholas J. Seewald; Karl Rickert; and Seth N. Brown; Inorganic Chemistry 52 (2013) 12587–12598; doi:10.1021/ic401736f

data_4336586
_publ_section_title
;
 Tris(3,5-di-tert-butylcatecholato)molybdenum(VI): Lewis Acidity and
 Nonclassical Oxygen Atom Transfer Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12587
_journal_page_last               12598
_journal_paper_doi               10.1021/ic401736f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C47 H65 Mo N O6, C2 H3 N'
_chemical_formula_sum            'C49 H68 Mo N2 O6'
_chemical_formula_weight         876.99
_chemical_name_common            (3,5-tBu2Cat)3Mo(py)
_chemical_name_systematic
;
 Tris(3,5-di-tert-butylcatecholato)(pyridine)molybdenum(VI) 
acetonitrile solvate
;
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.913(4)
_cell_angle_beta                 95.778(4)
_cell_angle_gamma                101.514(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5873(17)
_cell_length_b                   12.436(2)
_cell_length_c                   18.282(3)
_cell_measurement_reflns_used    4260
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.16
_cell_volume                     2343.1(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27516
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.8773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       rod
_exptl_crystal_F_000             932
_exptl_crystal_recrystallization_method
;
 Crystals were grown by diffusion of acetonitrile into a
solution of the complex in benzene.
;
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                7159
_reflns_number_total             9535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401736f_si_002_2.cif
_cod_data_source_block           mopy
_cod_database_code               4336586