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_1567774
_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 H94 B Br2 F20 Ga2 N6 P2'
_chemical_formula_weight         1999.71
_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'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 99.720(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.557(2)
_cell_length_b                   20.432(2)
_cell_length_c                   20.684(2)
_cell_measurement_reflns_used    9278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      80.66
_cell_measurement_theta_min      3.00
_cell_volume                     8979.5(15)
_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 0.993
_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  0.0949
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            405733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         81.277
_diffrn_reflns_theta_min         2.079
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             4068
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         19684
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0307P)^2^+6.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16685
_reflns_number_total             19684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04207j2.cif
_cod_data_source_block           mks_056m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        8979.6(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567774
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              45675