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_1567772
_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            'C65 H94 Cl2 Ga2 N6 P2'
_chemical_formula_weight         1231.74
_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   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                83.603(4)
_cell_angle_beta                 75.258(6)
_cell_angle_gamma                72.565(4)
_cell_formula_units_Z            4
_cell_length_a                   14.863(2)
_cell_length_b                   20.330(5)
_cell_length_c                   25.712(6)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      2.20
_cell_volume                     7163(3)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_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(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/QUEEN'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            264320
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         1.639
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_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    1.142
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.550
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1435
_refine_ls_number_reflns         43665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30501
_reflns_number_total             43665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04207j2.cif
_cod_data_source_block           mks_037am_sq
_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_database_code               1567772
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              86663
_shelx_fab_checksum              49399