Ketone Deprotonation Mediated by Mono- and Heterobimetallic Alkali and Alkaline Earth Metal Amide Bases: Structural Characterization of Potassium, Calcium, and Mixed Potassium-Calcium Enolates
Xuyang He; Bruce C. Noll; Alicia Beatty; Robert E. Mulvey; Kenneth W. Henderson; Journal of the American Chemical Society 126 (2004) 7444–7445; doi:10.1021/ja048750m

data_4112690
_publ_contact_author_address
; 
 Department of Chemistry and Biochemistry
 University of Notre Dame
 Notre Dame, IN 46556
;
_publ_contact_author_email       Kenneth.W.Henderson.43@nd.edu
_publ_contact_author_fax         574.631.6652
_publ_contact_author_name        'Professor Kenneth W. Henderson'
_publ_contact_author_phone       574.631.8025
_publ_section_title
;
 Ketone Deprotonation Mediated by Mono- and Heterobimetallic Alkali and
 Alkaline Earth Metal Amide Bases: Structural Characterization of
 Potassium, Calcium, and Mixed Potassium-Calcium Enolates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7444
_journal_page_last               7445
_journal_paper_doi               10.1021/ja048750m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C60 H84 Ca K2 O8'
_chemical_formula_sum            'C60 H84 Ca K2 O8'
_chemical_formula_weight         1051.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 115.091(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.746(5)
_cell_length_b                   12.270(2)
_cell_length_c                   19.878(4)
_cell_measurement_reflns_used    8759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.26
_cell_volume                     5907.9(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\w 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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23731
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. Acta Cryst. (1995) A51, 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+10.9297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                3720
_reflns_number_total             5343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048750msi20040304_085120.cif
_cod_data_source_block           kwh1003bcn
_cod_original_cell_volume        5907.8(19)
_cod_database_code               4112690