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_1575490
_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         'C28 H34 Br P2, Al Cl4'
_chemical_formula_sum            'C28 H34 Al Br Cl4 P2'
_chemical_formula_weight         681.225
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 109.043(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7254(7)
_cell_length_b                   19.8355(11)
_cell_length_c                   16.0902(10)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.26
_cell_volume                     3235.8(3)
_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 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7412
_diffrn_reflns_point_group_measured_fraction_full 0.9972
_diffrn_reflns_point_group_measured_fraction_max 0.9972
_diffrn_reflns_theta_full        24.9990
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.745552
_exptl_absorpt_correction_T_min  0.575104
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0612 before and 0.0405 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 
For component 2:
 wR2(int) was 0.1112 before and 0.0591 after correction.
 The Ratio of minimum to maximum transmission is 0.77.

Final HKLF 4 output contains 118753 reflections, Rint = 0.0650
 (49245 with I > 3sig(I), Rint = 0.0347)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       Shard
_exptl_crystal_F_000             1395.115
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.4117
_refine_diff_density_min         -0.4018
_refine_diff_density_rms         0.0737
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.0914
_refine_ls_goodness_of_fit_ref   1.0332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0332
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0245P)^2^+2.6036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -8
_reflns_number_gt                5100
_reflns_number_total             5692
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc03456f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1575490--1575492.cif.'
_cod_database_code               1575490
_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:
 C16(H16), C11(H11), C12(H12), C8(H8), C10(H10), C23(H23), C17(H17), C26(H26),
 C2(H2), C6(H6), C25(H25), C20(H20), C22(H22), C18(H18), C5(H5)
2.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C15(H15a,H15b,H15c), C21(H21a,H21b,H21c), C24(H24a,H24b,
 H24c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c)
;
_olex2_submission_special_instructions 'No special instructions were received'