Molybdenum(VI) Complexes of a 2,2'-Biphenyl-bridged Bis(amidophenoxide): Competition between Metal-Ligand and Metal-Amidophenoxide π Bonding
Jason A. Kopec; Sukesh Shekar; Seth N. Brown; Inorganic Chemistry 51 (2012) 1239–1250; doi:10.1021/ic201736h

data_4328146
_publ_section_title
;
 Molybdenum(VI) Complexes of a 2,2'-Biphenyl-bridged Bis(amidophenoxide):
 Competition between Metal-Ligand and Metal-Amidophenoxide \p Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1239
_journal_page_last               1250
_journal_paper_doi               10.1021/ic201736h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C55 H73 Mo N3 O3, C2 H3 N'
_chemical_formula_sum            'C57 H76 Mo N4 O3'
_chemical_formula_weight         961.16
_chemical_name_common            '(tBuClip)Mo(O)(Lut) . CH3CN'
_chemical_name_systematic
;
 Oxo(3,5-lutidine)(4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy-3,5-di-tert-
butylphenyl)amido)molybdenum(VI) acetonitrile solvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5173(7)
_cell_length_b                   12.1833(4)
_cell_length_c                   19.6759(6)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.61
_cell_measurement_theta_min      3.93
_cell_volume                     5397.8(3)
_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  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50292
_diffrn_reflns_theta_full        69.74
_diffrn_reflns_theta_max         69.74
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    2.325
_exptl_absorpt_correction_T_max  0.7087
_exptl_absorpt_correction_T_min  0.6251
_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            'dark green'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method
;
 Crystals were grown from benzene/acetonitrile.
;
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9975
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0377P)^2^+4.1367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                9566
_reflns_number_total             9975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201736h_si_002_2.cif
_cod_data_source_block           moolut
_cod_database_code               4328146