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_4112687
_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         'C72 H84 K4 O4'
_chemical_formula_sum            'C72 H84 K4 O4'
_chemical_formula_weight         1169.79
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.937(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.868(4)
_cell_length_b                   14.045(3)
_cell_length_c                   21.610(4)
_cell_measurement_reflns_used    6282
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.547
_cell_measurement_theta_min      2.345
_cell_volume                     6674(2)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.2443
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33067
_diffrn_reflns_theta_full        22.04
_diffrn_reflns_theta_max         22.04
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.9402
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         8033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0000P)^2^+45.8549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2145
_reflns_number_gt                5653
_reflns_number_total             8033
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           bcn07m
_cod_database_code               4112687