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_1549571
_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         'C30 H33 F2 N7 P, 3(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C37 H39 F11 N9 O9 P S3'
_chemical_formula_weight         1089.92
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-01-27 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                109.504(13)
_cell_angle_beta                 98.444(13)
_cell_angle_gamma                111.998(9)
_cell_formula_units_Z            2
_cell_length_a                   13.753(7)
_cell_length_b                   14.060(7)
_cell_length_c                   14.321(7)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.436
_cell_measurement_theta_min      2.901
_cell_volume                     2300(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.02
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55372
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.8652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.8666.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       plate
_exptl_crystal_F_000             1116
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN Et2O'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.2467
_refine_ls_R_factor_gt           0.1889
_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^)+(0.1970P)^2^+134.4340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5278
_refine_ls_wR_factor_ref         0.5690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5160
_reflns_number_total             7797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01682h2.cif
_cod_data_source_block           asrs11029_1
_cod_depositor_comments
'Adding full bibliography for 1549568--1549574.cif.'
_cod_original_cell_volume        2300.1(19)
_cod_database_code               1549571
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00U(H00C,H00D), C014(H01A,H01B), C017(H01C,H01D), C01D(H01F,
 H01G), C01N(H01Q,H01R)
2.b Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C013(H013), C019(H019), C01B(H01E), C01E(H01H), C01J(H01O),
 C01L(H01P), C01O(H01S), C01Q(H01T), C01R(H01U), C01S(H01V), C01V(H01Z)
2.c Idealised Me refined as rotating group:
 C01G(H01I,H01J,H01K), C01I(H01L,H01M,H01N), C01U(H01W,H01X,H01Y), C01W(H0AA,H,
 HA), C01Y(H01,HB,HC)
;
_olex2_submission_special_instructions 'No special instructions were received'