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_1549572
_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
'C31 H33 F4 N7 O3 S Sb, C F3 O3 S, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H39 F7 N9 O6 S2 Sb'
_chemical_formula_weight         1012.63
_chemical_name_systematic
'tris((1-ethyl-1H-benzo[d]imidazol-2-yl)methyl)amino antimony fluoride bis triflate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-26
_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                79.6653(7)
_cell_angle_beta                 63.0215(6)
_cell_angle_gamma                84.7868(7)
_cell_formula_units_Z            2
_cell_length_a                   13.1877(6)
_cell_length_b                   13.3482(7)
_cell_length_c                   13.4824(7)
_cell_measurement_reflns_used    5455
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.19
_cell_volume                     2080.63(18)
_computing_data_collection       'Bruker APEX2'
_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      193.15
_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 0.997
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18546
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8607
_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    1.616
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN Et2O'
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0510P)^2^+0.9045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7725
_reflns_number_total             9603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01682h2.cif
_cod_data_source_block           vic17b0
_cod_depositor_comments
'Adding full bibliography for 1549568--1549574.cif.'
_cod_database_code               1549572
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10A(0.034) H10B(0.034) H13(0.036) H14(0.043) H15(0.044)
 H16(0.039) H18A(0.04) H18B(0.04) H19A(0.061) H19B(0.061) H19C(0.061)
 H20A(0.03) H20B(0.03) H23(0.034) H24(0.042) H25(0.041) H26(0.038) H28A(0.044)
 H28B(0.044) H29A(0.066) H29B(0.066) H29C(0.066) H30A(0.032) H30B(0.032)
 H33(0.036) H34(0.039) H35(0.041) H36(0.037) H38A(0.039) H38B(0.039)
 H39A(0.061) H39B(0.061) H39C(0.061) H2SA(0.12) H2SB(0.12) H2SC(0.12)
 H4SA(0.173) H4SB(0.173) H4SC(0.173)
 Fixed X: H10A(0.6011) H10B(0.7345) H13(0.6327) H14(0.6405) H15(0.6501)
 H16(0.6492) H18A(0.6024) H18B(0.6043) H19A(0.7577) H19B(0.8023) H19C(0.8042)
 H20A(0.768) H20B(0.7123) H23(0.8905) H24(1.0814) H25(1.215) H26(1.1641)
 H28A(0.9331) H28B(1.0514) H29A(1.0765) H29B(0.9835) H29C(1.1018) H30A(0.5343)
 H30B(0.4701) H33(0.5969) H34(0.477) H35(0.3192) H36(0.2751) H38A(0.3041)
 H38B(0.3538) H39A(0.1605) H39B(0.1854) H39C(0.2351) H2SA(1.0327) H2SB(0.9229)
 H2SC(0.9109) H4SA(0.1034) H4SB(0.2172) H4SC(0.1709)
 Fixed Y: H10A(0.0872) H10B(0.1053) H13(0.2444) H14(0.1256) H15(-0.0482) H16(-
 0.1113) H18A(-0.1308) H18B(-0.0728) H19A(-0.1868) H19B(-0.1309) H19C(-0.0729)
 H20A(0.2163) H20B(0.3284) H23(0.4414) H24(0.4856) H25(0.4521) H26(0.3735)
 H28A(0.2852) H28B(0.333) H29A(0.1617) H29B(0.1309) H29C(0.1787) H30A(0.2147)
 H30B(0.2194) H33(0.6473) H34(0.7668) H35(0.7168) H36(0.5447) H38A(0.3502)
 H38B(0.2547) H39A(0.279) H39B(0.3922) H39C(0.2967) H2SA(0.1194) H2SB(0.1915)
 H2SC(0.0706) H4SA(0.6026) H4SB(0.5833) H4SC(0.697)
 Fixed Z: H10A(0.8062) H10B(0.7277) H13(0.3489) H14(0.2367) H15(0.2939)
 H16(0.4677) H18A(0.6695) H18B(0.7627) H19A(0.7047) H19B(0.5771) H19C(0.6703)
 H20A(0.7988) H20B(0.8067) H23(0.3303) H24(0.2178) H25(0.287) H26(0.4713)
 H28A(0.7771) H28B(0.6818) H29A(0.7404) H29B(0.7061) H29C(0.6108) H30A(0.9171)
 H30B(0.8401) H33(0.7189) H34(0.8289) H35(0.9972) H36(1.0664) H38A(1.1133)
 H38B(1.0479) H39A(1.0917) H39B(1.0232) H39C(0.9578) H2SA(0.2697) H2SB(0.2941)
 H2SC(0.3111) H4SA(0.8272) H4SB(0.8428) H4SC(0.826)
;
_olex2_submission_special_instructions 'No special instructions were received'