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_1575492
_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         'C38 H37 Br P2'
_chemical_formula_sum            'C38 H37 Br P2'
_chemical_formula_weight         635.568
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_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                 92.113(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1559(4)
_cell_length_b                   19.8934(10)
_cell_length_c                   19.7435(8)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      55.64
_cell_measurement_theta_min      3.15
_cell_volume                     3201.2(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)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.9858
_diffrn_measured_fraction_theta_max 0.9858
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2868
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.9858
_diffrn_reflns_Laue_measured_fraction_max 0.9858
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89523
_diffrn_reflns_point_group_measured_fraction_full 0.9858
_diffrn_reflns_point_group_measured_fraction_max 0.9858
_diffrn_reflns_theta_full        66.4018
_diffrn_reflns_theta_max         66.40
_diffrn_reflns_theta_min         3.15
_diffrn_source_current           0.64
_diffrn_source_power             0.028652800000000003
_diffrn_source_voltage           44.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3458
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1429 before and 0.0994 after correction.
The Ratio of minimum to maximum transmission is 0.4594.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       Shard
_exptl_crystal_F_000             1322.803
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.7150
_refine_diff_density_min         -0.6020
_refine_diff_density_rms         0.1479
_refine_ls_d_res_high            0.8412
_refine_ls_d_res_low             14.0087
_refine_ls_extinction_coef       0.0071(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0291
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0291
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                3406
_reflns_number_total             5556
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc03456f2.cif
_cod_data_source_block           1_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1575490--1575492.cif.'
_cod_database_code               1575492
_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), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15), C20(H20),
 C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C30(H30), C32(H32), C33(H33),
  C34(H34), C36(H36), C37(H37)
2.b Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C29(H29a,H29b,H29c), C31(H31a,H31b,
 H31c), C35(H35a,H35b,H35c), C38(H38a,H38b,H38c)
;
_olex2_submission_special_instructions 'No special instructions were received'