Nucleophilic conjugate 1,3-addition of phosphines to oligoynoates
Jie-Cheng Deng; Chih-Wei Kuo; Shih-Ching Chuang; Chem.Commun. 50 (2014) 10580–; doi:10.1039/C4cc02870H

data_7115567
_publ_section_title
;
 Nucleophilic conjugate 1,3-addition of phosphines to oligoynoates
;
_journal_name_full               Chem.Commun.
_journal_page_first              10580
_journal_paper_doi               10.1039/C4cc02870H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C40 H24 N O4 P'
_chemical_formula_sum            'C40 H24 N O4 P'
_chemical_formula_weight         613.57
_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                79.783(7)
_cell_angle_beta                 89.864(6)
_cell_angle_gamma                66.349(6)
_cell_formula_units_Z            2
_cell_length_a                   9.9693(10)
_cell_length_b                   10.0382(10)
_cell_length_c                   17.310(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1557.1(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12000
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.9127
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red(dark)
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.8133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1871
_reflns_number_gt                3786
_reflns_number_total             5216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02870h2.cif
_cod_data_source_block           a12537a
_cod_original_cell_volume        1557.0(3)
_cod_database_code               7115567