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_4065143
_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         'C24 H26 O2 Zn'
_chemical_formula_sum            'C24 H26 O2 Zn'
_chemical_formula_weight         411.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.058(3)
_cell_length_b                   45.201(7)
_cell_length_c                   5.7359(9)
_cell_measurement_reflns_used    3440
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.69
_cell_volume                     4163.3(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11383
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.7379
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                2271
_reflns_number_total             2615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200581f_si_002.cif
_cod_data_source_block           nd1107
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4065143