C-H Bond Activation in Aqueous Solution: Kinetics and Mechanism of H/D Exchange in Alcohols Catalyzed by Molybdocenes
Christoph Balzarek; Timothy J. R. Weakley; David R. Tyler; Journal of the American Chemical Society 122 (2000) 9427–9434; doi:10.1021/ja001535v

data_4116172
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 C-H Bond Activation in Aqueous Solution: Kinetics and Mechanism of H/D
 Exchange in Alcohols Catalyzed by Molybdocenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9427
_journal_page_last               9434
_journal_paper_doi               10.1021/ja001535v
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         'C13 H15 F3 Mo O3 S '
_chemical_formula_structural     '(C6 H7 )2 Mo H (O3 S C F3)'
_chemical_formula_sum            'C13 H15 F3 Mo O3 S'
_chemical_formula_weight         404.25
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0180(14)
_cell_length_b                   8.6571(6)
_cell_length_c                   13.973(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      13.8
_cell_volume                     1453.8(3)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01551
_diffrn_orient_matrix_UB_12      -0.11341
_diffrn_orient_matrix_UB_13      0.00252
_diffrn_orient_matrix_UB_21      0.08159
_diffrn_orient_matrix_UB_22      0.02121
_diffrn_orient_matrix_UB_23      -0.00493
_diffrn_orient_matrix_UB_31      0.00510
_diffrn_orient_matrix_UB_32      0.00548
_diffrn_orient_matrix_UB_33      0.07135
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_sigmaI/netI    0.04
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2983
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         32.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details   'North, Phillips & Matthews, 1968'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       'dark red block'
_exptl_crystal_F_000             808.00
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.81
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '6.7(5) \\times 10^-7^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.51
_refine_ls_goodness_of_fit_ref   1.59
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.020I)^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.034
_refine_ls_wR_factor_ref         0.033
_reflns_number_gt                2251
_reflns_number_total             2983
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            ja001535v_1.cif
_cod_data_source_block           7_C13H15F3MoO3S
_cod_original_cell_volume        1453.7(3)
_cod_original_sg_symbol_H-M      'P b c m '
_cod_original_formula_sum        'C13 H15 F3 Mo O3 S '
_cod_database_code               4116172