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_4339651
_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            'C31 H72 Mo N O2 P Si2'
_chemical_formula_weight         673.99
_chemical_name_systematic
;
  ?
;
_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                 99.4590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3696(5)
_cell_length_b                   17.9130(10)
_cell_length_c                   23.8114(13)
_cell_measurement_temperature    173(2)
_cell_volume                     3942.1(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52242
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.8379
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.204
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         12000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+6.4878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                9825
_reflns_number_total             12000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7010953_si2.cif
_cod_data_source_block           dcr700
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               4339651