Mixed amidophenolate-catecholates of molybdenum(vi).
Shekar, Sukesh; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 3601–3611; doi:10.1039/c3dt53496k

data_7029151
_publ_section_title
;
 Mixed amidophenolate-catecholates of molybdenum(vi).
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3601
_journal_page_last               3611
_journal_paper_doi               10.1039/c3dt53496k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C56 H80 Mo2 O10, 2(C6 H6)'
_chemical_formula_sum            'C68 H92 Mo2 O10'
_chemical_formula_weight         1261.30
_chemical_name_common            '(3,5tBuCat)4Mo2O2 . 2 C6H6'
_chemical_name_systematic
; 
 Tetrakis(3,5-di-tert-butylcatecholato)dioxodimolybedenum(VI)
di-benzene solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.3779(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7617(3)
_cell_length_b                   16.6561(4)
_cell_length_c                   16.5304(4)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    119(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.45
_cell_volume                     3238.30(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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      119(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37715
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.7990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

 Sheldrick, G. M. (2004) SADABS, University of Gottingen, Germany.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
;
 Crystals were grown from C6H6/CH3CN in a recrystallization attempt of 
 (tBuClip)Mo(\m-3,5-tBu2Cat)2Mo(O)(3,5-tBu2Cat) that was exposed to air.
;
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0275P)^2^+2.0577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                6694
_reflns_number_total             7332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53496k.txt
_cod_data_source_block           ss1140m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7029151