Synthesis and reactivity of [(silox)2Mo=NR]2Hg (R=tBu, tAmyl; silox=OSitBu3): unusual thermal stability and ready nucleophilic cleavage rationalized by electronic factors.
Rosenfeld, Devon C.; Wolczanski, Peter T.; Barakat, Khaldoon A.; Buda, Corneliu; Cundari, Thomas R.; Schroeder, Frank C.; Lobkovsky, Emil B.; Inorganic chemistry 46 (2007) 9715–9735; doi:10.1021/ic7010953

data_4339650
_publ_section_title
;
 Synthesis and reactivity of [(silox)2Mo=NR]2Hg (R=tBu, tAmyl;
 silox=OSitBu3): unusual thermal stability and ready nucleophilic cleavage
 rationalized by electronic factors.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9715
_journal_page_last               9735
_journal_paper_doi               10.1021/ic7010953
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C28 H63 Cl Mo N O2 Si2'
_chemical_formula_weight         633.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.231(2)
_cell_angle_beta                 99.950(2)
_cell_angle_gamma                97.400(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6651(7)
_cell_length_b                   12.4896(9)
_cell_length_c                   17.2926(13)
_cell_measurement_temperature    173(2)
_cell_volume                     1801.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21809
_diffrn_reflns_theta_full        31.55
_diffrn_reflns_theta_max         31.55
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.8170
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.211
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                8979
_reflns_number_total             10875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7010953_si1.cif
_cod_data_source_block           dcr600
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339650