A facile route to <i>cis</i>-olefin-linked phosphino-phosphonium salts of the form: [Ph<sub>2</sub>PC(R)C(H)P(R')<sub>2</sub>H][AlCl<sub>4</sub>].
Al-Zuhaika, Nahil; Severin, Simon; Schmuckler, Madeleine D.; Lough, Alan J.; Stephan, Douglas W.; Chemical communications (Cambridge, England) 61 (2025) 14967–14970; doi:10.1039/d5cc03456f

data_1575491
_publ_section_title
;
 A facile route to <i>cis</i>-olefin-linked phosphino-phosphonium salts of
 the form: [Ph<sub>2</sub>PC(R)C(H)P(R')<sub>2</sub>H][AlCl<sub>4</sub>].
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14967
_journal_page_last               14970
_journal_paper_doi               10.1039/d5cc03456f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C26 H39 P2, Al Cl4, C3 H3'
_chemical_formula_sum            'C29 H42 Al Cl4 P2'
_chemical_formula_weight         621.396
_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_Int_Tables_number      2
_audit_creation_date             2025-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-16 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.792(11)
_cell_angle_beta                 94.984(12)
_cell_angle_gamma                108.606(11)
_cell_formula_units_Z            2
_cell_length_a                   10.790(2)
_cell_length_b                   12.560(2)
_cell_length_c                   13.068(2)
_cell_measurement_reflns_used    3705
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.17
_cell_volume                     1666.6(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.9920
_diffrn_measured_fraction_theta_max 0.9920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.1483
_diffrn_reflns_Laue_measured_fraction_full 0.9920
_diffrn_reflns_Laue_measured_fraction_max 0.9920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25242
_diffrn_reflns_point_group_measured_fraction_full 0.9920
_diffrn_reflns_point_group_measured_fraction_max 0.9920
_diffrn_reflns_theta_full        24.9954
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.57
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             655.942
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.4620
_refine_diff_density_min         -0.9168
_refine_diff_density_rms         0.2247
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             12.9761
_refine_ls_extinction_coef       0.017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0781
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.1012
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1753P)^2^+0.6741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2621
_refine_ls_wR_factor_ref         0.3010
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3691
_reflns_number_total             5823
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc03456f2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1575490--1575492.cif.'
_cod_original_cell_volume        1666.5(5)
_cod_database_code               1575491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C16(H16), C17(H17),
 C20(H20), C21(H21), C24(H24), C29(H29), C28(H28), C27(H27)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C23(H23a,H23b,
 H23c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C18(H18a,H18b,H18c), C15(H15a,
 H15b,H15c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'