Structure and Dynamics of α-Aryl Amide and Ketone Enolates: THF, PMDTA, TMTAN, HMPA, and Crypt-Solvated Lithium Enolates, and Comparison with Phosphazenium Analogues
Kristopher J. Kolonko; Ilia A. Guzei; Hans J. Reich; Journal of Organic Chemistry 75 (2010) 6163–6172; doi:10.1021/jo100970r

data_4025672
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Structure and Dynamics of \a-Aryl Amide and Ketone Enolates: THF, PMDTA,
 TMTAN, HMPA, and Crypt-Solvated Lithium Enolates, and Comparison with
 Phosphazenium Analogues
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6163
_journal_page_last               6172
_journal_paper_doi               10.1021/jo100970r
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C52 H68 F2 Li2 O8'
_chemical_formula_weight         872.94
_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                93.541(2)
_cell_angle_beta                 103.269(2)
_cell_angle_gamma                105.102(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0232(4)
_cell_length_b                   13.2311(5)
_cell_length_c                   19.1945(7)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.66
_cell_measurement_theta_min      2.39
_cell_volume                     2371.91(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36753
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.06
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.7800
_exptl_absorpt_correction_T_min  0.7517
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         8758
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0554P)^2^+1.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                8207
_reflns_number_total             8758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo100970r_si_006.cif
_cod_data_source_block           reich14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4025672