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_7706112
_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
_chemical_formula_moiety         'C29 H41 N2 P'
_chemical_formula_sum            'C29 H41 N2 P'
_chemical_formula_weight         448.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.4446(12)
_cell_length_b                   10.7492(3)
_cell_length_c                   12.5916(3)
_cell_measurement_reflns_used    6627
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      66.619
_cell_measurement_theta_min      2.185
_cell_volume                     5474.2(3)
_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_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22897
_diffrn_reflns_point_group_measured_fraction_full 0.806
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        66.619
_diffrn_reflns_theta_max         66.619
_diffrn_reflns_theta_min         2.185
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.8642
_exptl_absorpt_correction_T_min  0.7731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2043 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     1085
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0505P)^2^+1.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.628
_reflns_Friedel_fraction_max     0.628
_reflns_number_gt                6627
_reflns_number_total             7792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03633a2.cif
_cod_data_source_block           g535_mn
_cod_database_code               7706112
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.884
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              21709