Addition of Ynamines to the Tungsten η1-Vinylidene Complexes (η5-C5H5)(NO)(CO)WCC(H)R
Ipaktschi, Junes; Mohseni-Ala, Javad; Dülmer, Ansgar; Steffens, Stefan; Wittenburg, Christian; Heck, Jürgen; Organometallics 23 (2004) 4902–; doi:10.1021/om049554r

data_4076295
_publ_section_title
;
 Addition of Ynamines to the Tungsten \h1-Vinylidene Complexes
 (\h5-C5H5)(NO)(CO)WCC(H)R
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4902
_journal_paper_doi               10.1021/om049554r
_journal_volume                  23
_journal_year                    2004
_chemical_formula_moiety         'C19 H28 N2 O2 W'
_chemical_formula_sum            'C19 H28 N2 O2 W'
_chemical_formula_weight         500.28
_chemical_name_systematic
;(2-(Diethylamino)-3-methyl-5-tert.-butyl)-1-(carbonyl-nitrosyl-

cyclopentadienyltungsta)-1,3,4-pentatrien 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.593(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8384(8)
_cell_length_b                   14.0307(17)
_cell_length_c                   18.567(2)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      1.91
_cell_volume                     2019.0(4)
_computing_cell_refinement       'STOE IPDS CONTROL Software'
_computing_data_collection       'STOE IPDS CONTROL Software'
_computing_data_reduction        'STOE IPDS CONTROL Software'
_computing_molecular_graphics
'ORTEP-3 for Windows (C.K. Johnson, M.N. Burnett, L.J. Farrugia 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'STOE Image Plate Diffractometer System'
_diffrn_measurement_method       phi-rotation
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14442
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    5.733
_exptl_absorpt_correction_T_max  0.7758
_exptl_absorpt_correction_T_min  0.4287
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'crystal fragment'
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+3.8854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                3103
_reflns_number_total             3625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049554rsi20040730_054746.cif
_cod_data_source_block           ipak069j
_cod_depositor_comments
;
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        2019.1(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4076295