An Experimental and Theoretical Investigation of the Carbon Dioxide Insertion Process into the Tungsten-Nitrogen Bond of an Anionic W(0) Complex
Donald J. Darensbourg; Brian J. Frost; David L. Larkins; Inorganic Chemistry 40 (2001) 1993–1999; doi:10.1021/ic001006s

data_4319548
_publ_section_title
;
 An Experimental and Theoretical Investigation of the Carbon Dioxide
 Insertion Process into the Tungsten-Nitrogen Bond of an Anionic W(0)
 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1993
_journal_page_last               1999
_journal_paper_doi               10.1021/ic001006s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C16 H18 N2 Na O8 W'
_chemical_formula_weight         573.16
_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                73.9650(10)
_cell_angle_beta                 86.4450(10)
_cell_angle_gamma                79.7780(10)
_cell_formula_units_Z            2
_cell_length_a                   7.2771(5)
_cell_length_b                   10.9638(7)
_cell_length_c                   13.1279(8)
_cell_measurement_temperature    163(2)
_cell_volume                     990.58(11)
_computing_cell_refinement       'Bruker SMART'
_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      163(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11727
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    5.898
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.5139
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             554
_refine_diff_density_max         0.906
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0016(3)
_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   1.214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+2.7400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                4130
_reflns_number_total             4498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001006s.cif
_cod_data_source_block           dd391
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319548