Synthesis of Phosphine-Ligated Zinc Acetylide Dimers: Enhanced Reactivity in Carbonyl Additions
Wilson, Erin E.; Oliver, Allen G.; Hughes, Russell P.; Ashfeld, Brandon L.; Organometallics 30 (2011) 5214–; doi:10.1021/om200581f

data_4065142
_publ_section_title
;
 Synthesis of Phosphine-Ligated Zinc Acetylide Dimers: Enhanced Reactivity
 in Carbonyl Additions
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5214
_journal_paper_doi               10.1021/om200581f
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C56 H50 P2 Zn2'
_chemical_formula_sum            'C56 H50 P2 Zn2'
_chemical_formula_weight         915.64
_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                100.399(4)
_cell_angle_beta                 93.380(4)
_cell_angle_gamma                91.285(4)
_cell_formula_units_Z            1
_cell_length_a                   8.3380(11)
_cell_length_b                   11.6200(17)
_cell_length_c                   12.1537(18)
_cell_measurement_reflns_used    2772
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.23
_cell_volume                     1155.5(3)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX-II v2010-7'
_computing_data_reduction        'Bruker SAINT v7.68A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16148
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.9074
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.1473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                3540
_reflns_number_total             4703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200581f_si_002.cif
_cod_data_source_block           nd1110a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065142