Nonclassical oxygen atom transfer reactions of oxomolybdenum(VI) bis(catecholate)
Travis Marshall-Roth; Sean C. Liebscher; Karl Rickert; Nicholas J. Seewald; Allen G. Oliver; Seth N. Brown; Chem.Commun. 48 (2012) 7826–; doi:10.1039/c2cc33523a

data_7108098
_publ_section_title
;
 Nonclassical oxygen atom transfer reactions of oxomolybdenum(VI)
 bis(catecholate)
;
_journal_name_full               Chem.Commun.
_journal_page_first              7826
_journal_paper_doi               10.1039/c2cc33523a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C34 H47 Mo N O6, 1.5 (C6 H12)'
_chemical_formula_sum            'C43 H65 Mo N O6'
_chemical_formula_weight         787.90
_chemical_name_common            'Mo(O)(DBCat)2(ONC5H4CH3) . 1.5 C6H12'
_chemical_name_systematic
;
Oxobis(3,5-di-tert-butylcatecholato)(4-picoline-N-oxide)molybdenum(VI)
sesquicyclohexane 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                 90.045(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.4007(9)
_cell_length_b                   35.850(2)
_cell_length_c                   16.3779(11)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.68
_cell_measurement_theta_min      2.20
_cell_volume                     8455.3(9)
_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      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            98563
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.8426
_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 purple'
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method
;
Crystals were grown from benzene/cyclohexane.
;
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.009
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         17287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0614P)^2^+11.9426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                11780
_reflns_number_total             17287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33523a.txt
_cod_data_source_block           moop21c2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108098