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_7024168
_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            'C16 H27 F3 N2 O Zn'
_chemical_formula_weight         385.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 109.426(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2967(4)
_cell_length_b                   12.6431(4)
_cell_length_c                   9.5096(4)
_cell_measurement_reflns_used    3127
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.00
_cell_measurement_theta_min      3.48
_cell_volume                     940.73(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.965
_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           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4909
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         68.69
_diffrn_reflns_theta_min         4.93
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                3892
_reflns_number_total             4909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b911818g.txt
_cod_data_source_block           jkzoe2t
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7024168