Stereocontrolled Formation of Ketomethylene Isosteres through Tandem Chain Extension Reactions
Weimin Lin; Nancy Tryder; Fan Su; Charles K. Zercher; Jerry P. Jasinski; Ray J. Butcher; Journal of Organic Chemistry 71 (2006) 8140–8145; doi:10.1021/jo061184o

data_4022010
_publ_contact_author_address
;
Department of Chemistry
Keene State College
229 Main Street
Keene, New Hampshirte 03435-2001 USA
;
_publ_contact_author_email       jjasinski@keene.edu
_publ_contact_author_fax         '603 358-2897'
_publ_contact_author_name        'Jerry P. Jasinski'
_publ_contact_author_phone       '603 358-2563'
_publ_section_title
;
 Stereocontrolled Formation of Ketomethylene Isosteres through
 Tandem Chain Extension Reactions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8140
_journal_page_last               8145
_journal_paper_doi               10.1021/jo061184o
_journal_volume                  71
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H22 N5 O7 '
_chemical_formula_sum            'C18 H22 N5 O7'
_chemical_formula_weight         420.40
_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'
_audit_creation_date             2006-07-02
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.29(2)
_cell_angle_beta                 112.06(3)
_cell_angle_gamma                89.876(9)
_cell_formula_units_Z            2
_cell_length_a                   8.384(4)
_cell_length_b                   20.291(5)
_cell_length_c                   6.443(4)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    295.1
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.0
_cell_volume                     1015.8(8)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'CrystalStructure 3.7.0'
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14789
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             442.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1982 Friedel Pairs'
_refine_ls_abs_structure_Flack   1(3)
_refine_ls_extinction_coef       251(10)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     295
_refine_ls_number_reflns         2196
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    8767.1400    12276.1000    3857.8000
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                2196
_reflns_number_total             4127
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo061184osi20060706_041400.cif
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C18 H22 N5 O7 '
_cod_database_code               4022010