UV Induced Hydrophosphination of Dimethyl-2-Vinylcyclopropane-1, 1-Dicarboxylate Towards Phosphine Chalcogenides
Adjei, Jeanette A.; Kerr, Michael A.; Ragogna, Paul J.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00791J

data_7712871
_publ_section_title
;
 UV Induced Hydrophosphination of Dimethyl-2-Vinylcyclopropane-1,
 1-Dicarboxylate Towards Phosphine Chalcogenides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00791J
_journal_year                    2023
_chemical_formula_sum            'C21 H23 O5 P'
_chemical_formula_weight         386.36
_chemical_melting_point          112.8
_chemical_name_systematic
'Dimethyl (E)-2-(4-(diphenylphosphoryl)but-2-en-1-yl) malonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2023-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                66.288(6)
_cell_angle_beta                 81.061(6)
_cell_angle_gamma                81.653(6)
_cell_formula_units_Z            4
_cell_length_a                   11.3445(14)
_cell_length_b                   13.716(3)
_cell_length_c                   14.665(2)
_cell_measurement_reflns_used    9271
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      2.50
_cell_volume                     2055.2(6)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex3
_computing_data_reduction        SAINT
_computing_molecular_graphics    Mercury
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_number            8643
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.776
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.745432
_exptl_absorpt_correction_T_min  0.634789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Cyclohexane/Benzene'
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6377
_reflns_number_total             8643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00791j2.cif
_cod_data_source_block           8
_cod_database_code               7712871
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              51480
_shelx_hkl_checksum              91604