Synthons for Coordinatively Unsaturated Complexes of Tungsten, and Their Use for the Synthesis of High Oxidation-State Silylene Complexes
Benjamin V. Mork; T. Don Tilley; Journal of the American Chemical Society 126 (2004) 4375–4385; doi:10.1021/ja030548g

data_4112381
_publ_section_title
;
 Synthons for Coordinatively Unsaturated Complexes of Tungsten, and Their
 Use for the Synthesis of High Oxidation-State Silylene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4375
_journal_page_last               4385
_journal_paper_doi               10.1021/ja030548g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C46 H31 B F21 N P2 W'
_chemical_formula_weight         1258.36
_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
_cell_angle_alpha                114.902(1)
_cell_angle_beta                 110.473(1)
_cell_angle_gamma                94.868(1)
_cell_formula_units_Z            2
_cell_length_a                   12.822(1)
_cell_length_b                   14.878(1)
_cell_length_c                   15.005(1)
_cell_measurement_reflns_used    4907
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      4.0
_cell_volume                     2339.8(3)
_computing_cell_refinement       'SAINT (Siemens)'
_computing_data_collection       'SMART (Siemens)'
_computing_data_reduction        'SAINT (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(1)
_diffrn_measurement_device       'Siemens SMART diffractometer'
_diffrn_measurement_method       'omega scans, 0.3 deg'
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11764
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.456
_refine_diff_density_min         -2.366
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         7425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1171
_refine_ls_wR_factor_obs         0.1096
_reflns_number_observed          6125
_reflns_number_total             7425
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030548g_c2_1.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0619P)^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^)+(0.0619P)^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        2340.1(4)
_cod_database_code               4112381