Low Coordinate, Monomeric Molybdenum and Tungsten(III) Complexes: Structure, Reactivity and Calculational Studies of (silox)3Mo and (silox)3ML (M = Mo, W; L = PMe3, CO; silox =tBu3SiO)
David S. Kuiper; Peter T. Wolczanski; Emil B. Lobkovsky; Thomas R. Cundari; Journal of the American Chemical Society 130 (2008) 12931–12943; doi:10.1021/ja802706u

data_4108391
_publ_section_title
;
 Low Coordinate, Monomeric Molybdenum and Tungsten(III) Complexes:
 Structure, Reactivity and Calculational Studies of (silox)3Mo and
 (silox)3ML (M = Mo, W; L = PMe3, CO; silox =tBu3SiO)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12931
_journal_page_last               12943
_journal_paper_doi               10.1021/ja802706u
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C37 H81 O4 Si3 W'
_chemical_formula_weight         858.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.684(2)
_cell_length_b                   21.091(4)
_cell_length_c                   24.354(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4449.0(16)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       CCD
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27578
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    2.709
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       needle
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.805
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         10175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_obs          0.0368
_refine_ls_shift/esd_max         2.838
_refine_ls_shift/esd_mean        0.157
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0912
_refine_ls_wR_factor_obs         0.0865
_reflns_number_observed          8656
_reflns_number_total             10176
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja802706u_si_001_3.cif
_cod_data_source_block           asv228
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] 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^)+(0.0529P)^2^+0.0000P] 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        4449.0(15)
_cod_database_code               4108391