Experimental and Theoretical Investigations of Catalytic Alkyne Cross-Metathesis with Imidazolin-2-iminato Tungsten Alkylidyne Complexes
Beer, Stephan; Brandhorst, Kai; Hrib, Cristian G.; Wu, Xian; Haberlag, Birte; Grunenberg, Jörg; Jones, Peter G.; Tamm, Matthias; Organometallics 28 (2009) 1534–; doi:10.1021/om801119t

data_4068826
_publ_section_title
;
 Experimental and Theoretical Investigations of Catalytic Alkyne
 Cross-Metathesis with Imidazolin-2-iminato Tungsten Alkylidyne Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1534
_journal_paper_doi               10.1021/om801119t
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C40 H63 N3 O2 W'
_chemical_formula_weight         801.78
_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                108.379(10)
_cell_angle_beta                 95.936(10)
_cell_angle_gamma                99.252(10)
_cell_formula_units_Z            4
_cell_length_a                   11.2439(14)
_cell_length_b                   18.7446(18)
_cell_length_c                   20.785(3)
_cell_measurement_reflns_used    28126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5727
_cell_measurement_theta_min      2.5483
_cell_volume                     4047.2(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1057
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67698
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.668
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         16480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                11273
_reflns_number_total             16480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801119t_si_006.cif
_cod_data_source_block           4b
_cod_original_cell_volume        4047.3(8)
_cod_database_code               4068826