Preparation and Characterization of 1,3-Butadiene and Isoprene Complexes, W~2~(OCH~2~^t^Bu)~6~(diene)(py), and Studies of the Selective Hydrogenation of 1,3-Dienes
Barry, Jane T.; Bollinger, John C.; Chisholm, Malcolm H.; Glasgow, Katherine C.; Huffman, John C.; Lucas, Eric A.; Lubkovsky, Emil B.; Streib, William E.; Organometallics 18 (1999) 2300–2308; doi:10.1021/om990059i

data_5000314
_publ_section_title
;
 Preparation and Characterization of 1,3-Butadiene and Isoprene Complexes,
 W~2~(OCH~2~^t^Bu)~6~(diene)(py), and Studies of the Selective Hydrogenation
 of 1,3-Dienes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2300
_journal_page_last               2308
_journal_paper_doi               10.1021/om990059i
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C47 H87 N O6 W2'
_chemical_formula_weight         1129.88
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.130(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.520(3)
_cell_length_b                   18.475(5)
_cell_length_c                   26.692(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5135.5(24)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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    0.1185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6685
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.518
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             2288
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.173
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6681
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.135
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_obs          0.0471
_refine_ls_shift/esd_max         0.032
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l]
 where P = 1.00000Fo^2^ + 0.00000Fc^2^
;
_refine_ls_wR_factor_all         0.1145
_refine_ls_wR_factor_obs         0.0945
_reflns_number_observed          4474
_reflns_number_total             6685
_reflns_observed_criterion       >2sigma(I)
_cod_database_code               5000314