Modulating the Frontier Orbitals of L(X)Ga-Substituted Diphosphenes [L(X)GaP]2 (X = Cl, Br) and their Facile Oxidation to Radical Cations
Sharma, Mahendra K.; Chabbra, Sonia; Wölper, Christoph; Weinert, Hanns Micha; Reijerse, Edward; Schnegg, Alexander; Schulz, Stephan; Chemical Science  (2022) –; doi:10.1039/D2SC04207J

data_1567773
_publ_section_title
;
 Modulating the Frontier Orbitals of L(X)Ga-Substituted Diphosphenes
 [L(X)GaP]2 (X = Cl, Br) and their Facile Oxidation to Radical Cations
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04207J
_journal_year                    2022
_chemical_formula_sum            'C89 H95 B Br2 F20 Ga2 N6 P2'
_chemical_formula_weight         2000.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                77.921(2)
_cell_angle_beta                 77.403(2)
_cell_angle_gamma                87.595(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5498(4)
_cell_length_b                   16.6890(7)
_cell_length_c                   23.2672(9)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.40
_cell_measurement_theta_min      2.71
_cell_volume                     4650.5(3)
_computing_cell_refinement       'Bruker APEX3(v2017.3-0)'
_computing_data_collection       'Bruker APEX3(v2017.3-0)'
_computing_data_reduction        'Bruker APEX3(v2017.3-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker APEX3(v2017.3-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture (Photon II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/Queen'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1279
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            234649
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.216
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 

 Crystal faces:

     H       K       L      d(mm)

   0.000   0.000  -1.000   0.00700
   0.000   0.000   1.000   0.00700
   0.000   1.000  -1.000   0.03900
  -1.000   1.000   1.000   0.05600
   1.000  -1.000  -1.000   0.06500
  -1.000  -1.000   1.000   0.03800
   0.000  -1.000   0.000   0.05900
   0.000   1.000   0.000   0.05200
  -1.000  -1.000   0.000   0.04600
   1.000   1.000   0.000   0.04600
  -1.000   0.000   0.000   0.05500
   1.000  -1.000   0.000   0.07000
  -1.000   1.000   0.000   0.06000

  13 Faces  +  22 Corners  =  33 Edges  +  2

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         19037
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+30.0612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14631
_reflns_number_total             19037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04207j2.cif
_cod_data_source_block           mks_077m_sq
_cod_database_code               1567773
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              79250
_shelx_fab_checksum              66665