Proton transfer vs. oligophosphine formation by P-C/P-H σ-bond metathesis: decoding the competing Brønsted and Lewis type reactivities of imidazolio-phosphines.
Cicač-Hudi, Mario; Feil, Christoph M.; Birchall, Nicholas; Nieger, Martin; Gudat, Dietrich; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17401–17413; doi:10.1039/d0dt03633a

data_7706119
_publ_section_title
;
 Proton transfer vs. oligophosphine formation by P-C/P-H \s-bond
 metathesis: decoding the competing Br\/onsted and Lewis type reactivities
 of imidazolio-phosphines.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17401
_journal_page_last               17413
_journal_paper_doi               10.1039/d0dt03633a
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
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_chemical_formula_sum            'C28 H40.5 I N2.5 O0.5 P'
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_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   12.8127(8)
_cell_measurement_reflns_used    7381
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.308
_cell_measurement_theta_min      1.834
_cell_volume                     12745.3(14)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
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_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63973
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.074
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_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.821
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_refine_ls_abs_structure_details
;
 Flack x determined using 3308 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1376P)^2^+31.7700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7380
_reflns_number_total             7918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03633a2.cif
_cod_data_source_block           g481_mn_sq
_cod_original_cell_volume        12745.1(14)
_cod_original_formula_sum        'C28 H40.50 I N2.50 O0.50 P'
_cod_database_code               7706119
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.688
_shelx_estimated_absorpt_t_max   0.873
_shelx_res_checksum              11670
_shelx_fab_checksum              79749
_platon_squeeze_void_probe_radius 1.20