Acylimido Complexes of Tungsten(IV) Formed by Oxygen Atom Transfer to Nitrile-κ2N,C Complexes
Simon Thomas; Patrick J. Lim; Robert W. Gable; Charles G. Young; Inorganic Chemistry 37 (1998) 590–593; doi:10.1021/ic9709178

data_4322632
_publ_section_title
;
 Acylimido Complexes of Tungsten(IV) Formed by Oxygen Atom Transfer to
 Nitrile-\k2N,C Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              590
_journal_page_last               593
_journal_paper_doi               10.1021/ic9709178
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C27 H37 B N7 O2 S W'
_chemical_formula_weight         718.36
_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   'not located'
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.83(7)
_cell_angle_beta                 89.50(6)
_cell_angle_gamma                67.35(3)
_cell_formula_units_Z            2
_cell_length_a                   9.640(3)
_cell_length_b                   12.344(6)
_cell_length_c                   14.471(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      9.7
_cell_volume                     1566.3(17)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4-MachS diffractometer'
_diffrn_measurement_method       \w:2\q
_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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6903
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.7289
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   'Gaussian integration (Sheldrick, 1976)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.517
_refine_diff_density_min         -2.700
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.0014(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_ref   1.287
_refine_ls_hydrogen_treatment    'not located'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+20.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                5874
_reflns_number_total             6139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9709178.cif
_cod_data_source_block           '[LW{NC(O)Me}(SPh)(CO).0.5(hexane)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+20.1610P] 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^)+(0.0578P)^2^+20.1610P] 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        1566.3(16)
_cod_database_code               4322632