Activation of the CP bond in phosphanylphosphaalkenes (CP–P bond system) in the reaction with nucleophilic reagents: MeLi, nBuLi and tBuLi
Ziółkowska, Aleksandra; Szynkiewicz, Natalia; Ponikiewski, Łukasz; RSC Advances 12 (2022) 10989–10996; doi:10.1039/D1RA09215D

data_7244745
_publ_section_title
;
 Activation of the C&#xE001;P bond in phosphanylphosphaalkenes
 (C&#xE001;P--P bond system) in the reaction with nucleophilic reagents:
 MeLi, nBuLi and tBuLi
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10989
_journal_page_last               10996
_journal_paper_doi               10.1039/D1RA09215D
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C72 H88 Li1 P6, C12 H30 Li1 O6'
_chemical_formula_sum            'C84 H118 Li2 O6 P6'
_chemical_formula_weight         1423.48
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2021-07-01T15:04:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2021-10-06 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                115.094(3)
_cell_angle_beta                 100.381(3)
_cell_angle_gamma                98.093(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1986(5)
_cell_length_b                   19.2100(8)
_cell_length_c                   20.5903(9)
_cell_measurement_reflns_used    20560
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     4168.4(3)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area X-Red32 1.65.0.0 (STOE, 2018) 
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      ' 210 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.1161
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36927
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.231
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     905
_refine_ls_number_reflns         19849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1257P)^2^+2.5439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2091
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0
_reflns_number_gt                10756
_reflns_number_total             19849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra09215d2.cif
_cod_data_source_block           3a'
_cod_database_code               7244745
_shelx_estimated_absorpt_t_min   0.96
_shelx_estimated_absorpt_t_max   0.965