An OCO3-Trianionic Pincer Tungsten(VI) Alkylidyne: Rational Design of a Highly Active Alkyne Polymerization Catalyst
Soumya Sarkar; Kevin P. McGowan; Subramaniam Kuppuswamy; Ion Ghiviriga; Khalil A. Abboud; Adam S. Veige; Journal of the American Chemical Society 134 (2012) 4509–4512; doi:10.1021/ja2117975

data_4117656
_publ_section_title
;
 An OCO3-Trianionic Pincer Tungsten(VI) Alkylidyne: Rational Design of a
 Highly Active Alkyne Polymerization Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4509
_journal_page_last               4512
_journal_paper_doi               10.1021/ja2117975
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C39 H54 O4 W'
_chemical_formula_weight         770.67
_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
_audit_update_record
;

2011-09-13 # Formatted by publCIF

;
_cell_angle_alpha                79.010(1)
_cell_angle_beta                 84.608(1)
_cell_angle_gamma                63.709(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2871(2)
_cell_length_b                   11.2440(2)
_cell_length_c                   17.2488(3)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.73
_cell_volume                     1755.84(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29784
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    3.327
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_correction_T_min  0.4485
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       plates
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0193P)^2^+0.8546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                7347
_reflns_number_total             8054
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja2117975_si_002_1.cif
_cod_data_source_block           ss72
_cod_database_code               4117656