Kinetic Studies on the Oxidation of η5-Cyclopentadienyl Methyl Tricarbonyl Molybdenum(II) and the Use of Its Oxidation Products as Olefin Epoxidation Catalysts
Al-Ajlouni, Ahmad M.; Veljanovski, Draganco; Capapé, Alejandro; Zhao, Jin; Herdtweck, Eberhardt; Calhorda, Maria José; Kühn, Fritz E.; Organometallics 28 (2009) 639–; doi:10.1021/om8009206

data_4068538
_publ_section_title
;
 Kinetic Studies on the Oxidation of \h5-Cyclopentadienyl Methyl
 Tricarbonyl Molybdenum(II) and the Use of Its Oxidation Products as
 Olefin Epoxidation Catalysts
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              639
_journal_paper_doi               10.1021/om8009206
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H8 Mo O3'
_chemical_formula_sum            'C6 H8 Mo O3'
_chemical_formula_weight         224.06
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5225(5)
_cell_length_b                   7.9532(5)
_cell_length_c                   13.9632(7)
_cell_measurement_reflns_used    8146
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      3.45
_cell_volume                     724.34(8)
_computing_cell_refinement       'CrysAlis (Oxford, 2005)'
_computing_data_collection       'CrysAlis (Oxford, 2005)'
_computing_data_reduction        'CrysAlis (Oxford, 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2005)'
_computing_publication_material  'PLATON (Spek, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Oxford \k-CCD diffractometer '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5660
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_max  0.8388
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical absorption correction after crystal shape optimization.
 The crystal faces were determined optical with the program
 CrysAlis RED (Oxford, 2005) and refined with the program
 X-Shape (STOE, 2004). The final absorption correction was applied
 using the program X-Red32 (STOE, 2004).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.230
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(15)
_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+2.1247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                1662
_reflns_number_total             1711
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8009206_si_002.cif
_cod_data_source_block           ZHAP-1041-173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4068538