Synthesis and Decomposition of Alkyl Complexes of Molybdenum(IV) That Contain a [(Me3SiNCH2CH2)3N]3- Ligand. Direct Detection of α-Elimination Processes That Are More than Six Orders of Magnitude Faster than β-Elimination Processes
Richard R. Schrock; Scott W. Seidel; Nadia C. Mösch-Zanetti; Keng-Yu Shih; Myra B. O'Donoghue; William M. Davis; William M. Reiff; Journal of the American Chemical Society 119 (1997) 11876–11893; doi:10.1021/ja970697x

data_4117077
_publ_section_title
;
 Synthesis and Decomposition of Alkyl Complexes of Molybdenum(IV) That
 Contain a [(Me3SiNCH2CH2)3N]3- Ligand. Direct Detection of \a-Elimination
 Processes That Are More than Six Orders of Magnitude Faster than
 \b-Elimination Processes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11876
_journal_page_last               11893
_journal_paper_doi               10.1021/ja970697x
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C16 H39 F3 Mo N4 O3 S Si3'
_chemical_formula_weight         604.78
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.951(4)
_cell_length_b                   10.999(2)
_cell_length_c                   12.050(2)
_cell_measurement_temperature    188(2)
_cell_volume                     2776.8(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\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  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7745
_diffrn_reflns_theta_max         19.99
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.61(10)
_refine_ls_extinction_coef       0.0034(5)
_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_all   0.996
_refine_ls_goodness_of_fit_obs   1.016
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2559
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.361
_refine_ls_restrained_S_obs      1.016
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_obs          0.0486
_refine_ls_shift/esd_max         -0.041
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+12.7601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1542
_refine_ls_wR_factor_obs         0.1068
_reflns_number_observed          2268
_reflns_number_total             2595
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970697x_4.cif
_cod_data_source_block           95066
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+12.7601P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+12.7601P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2776.7(10)
_cod_database_code               4117077