[4 + 2] Cycloadditions of 1-Phosphono-1,3-butadienes with Nitroso Heterodienophiles: A Versatile Synthetic Route for Polyfunctionalized Aminophosphonic Derivatives
Jean-Christophe Monbaliu; Bernard Tinant; Jacqueline Marchand-Brynaert; Journal of Organic Chemistry 75 (2010) 5478–5486; doi:10.1021/jo100230r

data_4025584
_publ_section_title
;
 [4 + 2] Cycloadditions of 1-Phosphono-1,3-butadienes with Nitroso
 Heterodienophiles: A Versatile Synthetic Route for Polyfunctionalized
 Aminophosphonic Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5478
_journal_page_last               5486
_journal_paper_doi               10.1021/jo100230r
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C22 H40 N O8 P S Si'
_chemical_formula_weight         537.67
_space_group_IT_number           2
_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                101.319(5)
_cell_angle_beta                 105.017(6)
_cell_angle_gamma                113.361(7)
_cell_formula_units_Z            2
_cell_length_a                   10.985(5)
_cell_length_b                   11.889(8)
_cell_length_c                   12.965(6)
_cell_measurement_temperature    146(2)
_cell_volume                     1413.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      146(2)
_diffrn_measured_fraction_theta_full 0.771
_diffrn_measured_fraction_theta_max 0.771
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9768
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.9045
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0460P)^2^+0.5047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                3814
_reflns_number_total             5399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo100230r_si_003.cif
_cod_data_source_block           jcmon9
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4025584