Synthesis and chemical reactivity of methoxycarbonyl-1,3-dioxinyl(pivaloyl)ketene—a persistent α-oxoketene
Wallfisch, Bianca C.; Belaj, Ferdinand; Wentrup, Curt; Kappe, C. Oliver; Kollenz, Gert; Journal of the Chemical Society, Perkin Transactions 1  (2002) 599–; doi:10.1039/b111143d

data_7204333
_publ_section_title
;
 Synthesis and chemical reactivity of
 methoxycarbonyl-1,3-dioxinyl(pivaloyl)ketene---a persistent
 \a-oxoketene
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              599
_journal_paper_doi               10.1039/b111143d
_journal_year                    2002
_chemical_formula_sum            'C28 H44 N2 O7'
_chemical_formula_weight         520.65
_chemical_melting_point          394
_chemical_name_systematic
; 
R,R-2-(1-Isopropyl-4-(isopropylimino)-2-oxo-3-pivaloylazetidin
-3-yl)-2,6-di-tert-butyl-5-methoxycarbonyl-1,3-dioxin-4(2H)-one
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.885(3)
_cell_length_b                   16.338(5)
_cell_length_c                   17.537(5)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      18.78
_cell_measurement_theta_min      3.71
_cell_volume                     2832.2(15)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe 4-circle'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3991
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        3.9
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2.5(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0223P)^2^+1.0042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3296
_reflns_number_total             3660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111143d.txt
_cod_data_source_block           7b_B(BCW410c)
_cod_database_code               7204333