Reaction of 2H-Azirine-Phosphine Oxides and -Phosphonates with Enolates Derived from β-Keto Esters.
Vélez Del Burgo, Ander; Ochoa de Retana, Ana M.; de Los Santos, Jesús M; Palacios, Francisco; The Journal of organic chemistry 81 (2016) 100–108; doi:10.1021/acs.joc.5b02347

data_4036512
_publ_section_title
;
 Reaction of 2H-Azirine-Phosphine Oxides and -Phosphonates with Enolates
 Derived from \b-Keto Esters.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              100
_journal_page_last               108
_journal_paper_doi               10.1021/acs.joc.5b02347
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C23 H24 N O3 P'
_chemical_formula_sum            'C23 H24 N O3 P'
_chemical_formula_weight         393.40
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                102.196(5)
_cell_angle_beta                 101.982(5)
_cell_angle_gamma                99.839(7)
_cell_formula_units_Z            2
_cell_length_a                   8.587(3)
_cell_length_b                   10.068(4)
_cell_length_c                   13.250(5)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.64
_cell_measurement_theta_min      2.32
_cell_volume                     1067.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
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_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_av_R_equivalents  0.0795
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10482
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.10
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_refine_ls_number_reflns         3752
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_refine_ls_R_factor_all          0.1557
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_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^)+(0.1386P)^2^+4.4342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3372
_refine_ls_wR_factor_ref         0.3576
_reflns_number_gt                2567
_reflns_number_total             3752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            DATOSm.cif
_cod_data_source_block           datosm
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1067.2(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4036512