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_4328145
_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         'C96 H130 Mo2 N6 O4, 0.5 (C4 H10 O)'
_chemical_formula_sum            'C98 H135 Mo2 N6 O4.5'
_chemical_formula_weight         1661.00
_chemical_name_common
'(tBuClip)Mo(\m-N)(\m-NH2)Mo(tBuClip) . 0.5 Et2O'
_chemical_name_systematic
; 
 (\m-Nitrido)(\m-amido)bis(4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy-
3,5-di-tert-butylphenyl)amido)dimolybdenum(VI) hemidiethylether 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   'geom or difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.7516(8)
_cell_angle_beta                 84.1354(8)
_cell_angle_gamma                75.3810(7)
_cell_formula_units_Z            2
_cell_length_a                   14.7223(2)
_cell_length_b                   15.4117(3)
_cell_length_c                   21.2348(4)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.93
_cell_measurement_theta_min      3.12
_cell_volume                     4637.66(14)
_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 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44466
_diffrn_reflns_theta_full        67.16
_diffrn_reflns_theta_max         67.16
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_T_max  0.7623
_exptl_absorpt_correction_T_min  0.4707
_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            violet
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       'thin tablet'
_exptl_crystal_F_000             1770
_exptl_crystal_recrystallization_method
;
 Crystals were grown by slow cooling of a diethyl ether solution.
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         15691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+4.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                13443
_reflns_number_total             15691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201736h_si_002_1.cif
_cod_data_source_block           ss20
_cod_original_formula_sum        'C98 H135 Mo2 N6 O4.50'
_cod_database_code               4328145