New insights into addition reactions of dialkylzinc reagents to trifluoromethyl ketones: structural authentication of a beta-hydride elimination product containing a tetranuclear zinc chain.
Hevia, Eva; Kennedy, Alan R.; Klett, Jan; Livingstone, Zoe; McCall, Matthew D.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 520–526; doi:10.1039/b911818g

data_7024169
_publ_section_title
;
 New insights into addition reactions of dialkylzinc reagents to
 trifluoromethyl ketones: structural authentication of a beta-hydride
 elimination product containing a tetranuclear zinc chain.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              520
_journal_page_last               526
_journal_paper_doi               10.1039/b911818g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C56 H54 F18 O6 Zn4'
_chemical_formula_weight         1426.47
_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                96.141(2)
_cell_angle_beta                 113.380(3)
_cell_angle_gamma                98.272(3)
_cell_formula_units_Z            1
_cell_length_a                   10.7331(4)
_cell_length_b                   12.0496(4)
_cell_length_c                   12.6837(3)
_cell_measurement_reflns_used    16163
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.66
_cell_volume                     1465.52(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       '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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34585
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.741
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8333
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1246P)^2^+0.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                5873
_reflns_number_total             8333
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b911818g.txt
_cod_data_source_block           jkmat3
_cod_original_cell_volume        1465.52(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024169