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_7233592
_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            'C48 H48 N3 O3 P3'
_chemical_formula_weight         807.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc229sck
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.640(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8088(8)
_cell_length_b                   8.9035(5)
_cell_length_c                   33.3890(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4200.7(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            50858
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.174
_diffrn_reflns_theta_max         67.174
_diffrn_reflns_theta_min         2.961
_exptl_absorpt_coefficient_mu    1.659
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.401
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.1413
_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^)+(0.1993P)^2^+31.8784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3985
_refine_ls_wR_factor_ref         0.4363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4205
_reflns_number_total             7357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04896k2.cif
_cod_data_source_block           shelx
_cod_database_code               7233592
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              29592