Reduction of π-Bound Nitriles to π-Bound Imines in a Tungsten(II) Bis(acetylacetonate) Coordination Sphere
Jackson, Andrew B.; Khosla, Chetna; Gaskins, Helen E.; White, Peter S.; Templeton, Joseph L.; Organometallics 27 (2008) 1322–; doi:10.1021/om7009039

data_4070645
_publ_section_title
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 Reduction of \p-Bound Nitriles to \p-Bound Imines in a Tungsten(II)
 Bis(acetylacetonate) Coordination Sphere
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_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1322
_journal_paper_doi               10.1021/om7009039
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C20 H25 N O5 W'
_chemical_formula_sum            'C20 H25 N O5 W'
_chemical_formula_weight         543.26
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.92
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3192(3)
_cell_length_b                   14.2955(4)
_cell_length_c                   17.0591(6)
_cell_measurement_reflns_used    6790
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.39
_cell_volume                     2026.16(12)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88084
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    5.731
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            lustrous
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.564
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.00007(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   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         88084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          2.527
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                71167
_reflns_number_total             88084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7009039_si.cif
_cod_data_source_block           c06034
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2026.15(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070645