Tris(benzoimidazol)amine (L) complexes of pnictogen(iii) and pnictogen(v) cations and assessment of the [LP]<sup>3+</sup>/[LPF<sub>2</sub>]<sup>3+</sup> redox couple.
Swidan, Ala'aeddeen; Suter, Riccardo; Macdonald, Charles L. B.; Burford, Neil; Chemical science 9 (2018) 5837–5841; doi:10.1039/c8sc01682h

data_1549569
_publ_section_title
;
 Tris(benzoimidazol)amine (L) complexes of pnictogen(iii) and pnictogen(v)
 cations and assessment of the
 [LP]<sup>3+</sup>/[LPF<sub>2</sub>]<sup>3+</sup> redox couple.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              5837
_journal_page_last               5841
_journal_paper_doi               10.1039/c8sc01682h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'C32 H33 As F6 N7 O6 S2, C F3 O3 S, 2(C2 H3 N)'
_chemical_formula_sum            'C37 H39 As F9 N9 O9 S3'
_chemical_formula_weight         1095.87
_chemical_name_systematic
'tris((1-ethyl-1H-benzo[d]imidazol-2-yl)methyl)amino arsenic tristriflate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-10-19 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.9657(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0065(3)
_cell_length_b                   15.9167(3)
_cell_length_c                   21.8331(5)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.79
_cell_measurement_theta_min      3.50
_cell_volume                     4630.08(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25884
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         3.317
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.9527
_exptl_absorpt_correction_T_min  0.8327
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2232
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN diethylether'
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.223
_refine_diff_density_max         3.210
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1994P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2548
_refine_ls_wR_factor_ref         0.2635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6779
_reflns_number_total             8479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01682h2.cif
_cod_data_source_block           vic17e3
_cod_depositor_comments
'Adding full bibliography for 1549568--1549574.cif.'
_cod_database_code               1549569
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C18(H18A,H18B), C20(H20A,H20B), C28(H28A,H28B), C30(H30A,
 H30B), C38(H38A,H38B)
2.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C23(H23), C24(H24), C25(H25),
 C26(H26), C33(H33), C34(H34), C35(H35), C36(H36)
2.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_olex2_submission_special_instructions 'No special instructions were received'