Synthesis of P,P-bidentate caged phosphines via tungsten pentacarbonyl-promoted cycloaddition reactions of 1-alkyl-1,2-diphospholes
Zagidullin, Almaz A.; Ganushevich, Yulia S.; Korchagin, Denis V.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Miluykov, Vasili A.; New Journal of Chemistry 48 (2024) 6848–6856; doi:10.1039/D3NJ05665A

data_7063093
_publ_section_title
;
 Synthesis of P,P-bidentate caged phosphines via tungsten
 pentacarbonyl-promoted cycloaddition reactions of
 1-alkyl-1,2-diphospholes
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6848
_journal_page_last               6856
_journal_paper_doi               10.1039/D3NJ05665A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C43 H37 O4 P3 W,1.5(C7 H8)'
_chemical_formula_sum            'C53.5 H49 O4 P3 W'
_chemical_formula_weight         1032.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-11-28 deposited with the CCDC.	2024-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.002(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.7665(11)
_cell_length_b                   9.3053(2)
_cell_length_c                   28.2716(7)
_cell_measurement_reflns_used    8556
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.5780
_cell_measurement_theta_min      2.1200
_cell_volume                     9297.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_molecular_graphics
;
 DIAMOND Version 4.6.8
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39224
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.499
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       needle
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9519
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+2.1292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7177
_reflns_number_total             9519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj05665a2.cif
_cod_data_source_block           comp3b_x1177fin
_cod_depositor_comments
'Adding full bibliography for 7063092--7063094.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C53.50 H49 O4 P3 W'
_cod_database_code               7063093
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              32343
_shelx_hkl_checksum              85174