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_4328147
_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         'C54 H78 Mo N2 O4, 2 (C2 H3 N)'
_chemical_formula_sum            'C58 H84 Mo N4 O4'
_chemical_formula_weight         997.23
_chemical_name_common            '(tBuClip)Mo(OiPr)2 . 2 CH3CN'
_chemical_name_systematic
; 
 (4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy-
 3,5-di-tert-butylphenyl)amido)-diisopropoxymolybdenum(VI) bisacetonitrile
 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   'difmap or geom'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.332(3)
_cell_angle_beta                 78.155(3)
_cell_angle_gamma                88.443(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8491(17)
_cell_length_b                   14.7791(18)
_cell_length_c                   14.9039(18)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.31
_cell_volume                     2842.7(6)
_computing_cell_refinement
'APEX2/SAINT (Bruker, 2004)(Bruker, 2004; Sheldrick, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT/XPREP
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57132
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9392
_exptl_absorpt_correction_T_min  0.8904
_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            brownish-purple
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_recrystallization_method
;
Crystals were grown from benzene layered with acetonitrile 
;
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         9609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+4.1315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                8706
_reflns_number_total             9609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201736h_si_002_3.cif
_cod_data_source_block           ss145_0m
_cod_database_code               4328147