Synthesis and activation potential of an open shell diphosphine.
Helmdach, Kai; Ludwig, Stephan; Villinger, Alexander; Hollmann, Dirk; Kösters, Jutta; Seidel, Wolfram W.; Chemical communications (Cambridge, England)  (2017) –; doi:10.1039/c7cc02114c

data_7120121
_publ_section_title
;
 Synthesis and activation potential of an open shell diphosphine.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/c7cc02114c
_journal_year                    2017
_chemical_formula_moiety         'C26 H24 B F4 N P2'
_chemical_formula_sum            'C26 H24 B F4 N P2'
_chemical_formula_weight         499.21
_chemical_name_systematic
Ethanebis(diphenylphosphoranylidene)ammonium-tetrafluoroborate
_chemical_properties_physical    ', Moisture-sensitive'
_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'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-03-17 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0029(15)
_cell_length_b                   13.0353(13)
_cell_length_c                   10.6338(8)
_cell_measurement_reflns_used    3152
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      2.40
_cell_volume                     2356.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016 '
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19858
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.396
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethylether'
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1344 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5164
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0767P)^2^+3.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                3695
_reflns_number_total             5164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           kh463
_cod_database_code               7120121
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2014-3
_shelx_res_checksum              62554
_shelx_hkl_checksum              78383