Catalyst-free hydrophosphination of alkenes in presence of 2-methyltetrahydrofuran: a green and easy access to a wide range of tertiary phosphines
Bissessar, Damien; Egly, Julien; Achard, Thierry; Steffanut, Pascal; Bellemin-Laponnaz, Stéphane; RSC Advances 9 (2019) 27250–; doi:10.1039/C9RA04896K

data_7233593
_publ_section_title
;
 Catalyst-free hydrophosphination of alkenes in presence of
 2-methyltetrahydrofuran: a green and easy access to a wide range of
 tertiary phosphines
;
_journal_issue                   47
_journal_name_full               'RSC Advances'
_journal_page_first              27250
_journal_paper_doi               10.1039/C9RA04896K
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C36 H40 O6 P2'
_chemical_formula_weight         630.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc229sdl
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.613(4)
_cell_angle_beta                 92.777(3)
_cell_angle_gamma                103.471(3)
_cell_formula_units_Z            1
_cell_length_a                   5.6788(4)
_cell_length_b                   8.9086(4)
_cell_length_c                   16.4624(11)
_cell_measurement_temperature    173(2)
_cell_volume                     808.76(9)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.003
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1913
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_Laue_measured_fraction_full 1.003
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16776
_diffrn_reflns_point_group_measured_fraction_full 1.003
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.349
_diffrn_reflns_theta_min         1.239
_exptl_absorpt_coefficient_mu    0.180
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.08(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.847
_refine_ls_R_factor_all          0.2133
_refine_ls_R_factor_gt           0.1689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4599
_refine_ls_wR_factor_ref         0.4923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2433
_reflns_number_total             3594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04896k2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7233593
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4
_shelx_res_checksum              30766