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_1549574
_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 F3 N7 O3 S Sb, 2(C F3 O3 S), 2.55(C2 H3 N)'
_chemical_formula_sum            'C38 H40.5 F9 N9.5 O9 S3 Sb'
_chemical_formula_weight         1163.24
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                102.659(14)
_cell_angle_beta                 97.475(14)
_cell_angle_gamma                99.315(14)
_cell_formula_units_Z            4
_cell_length_a                   12.726(5)
_cell_length_b                   18.899(8)
_cell_length_c                   20.823(8)
_cell_measurement_reflns_used    8322
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.018
_cell_measurement_theta_min      2.829
_cell_volume                     4750(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.9776
_diffrn_measured_fraction_theta_max 0.9776
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            133890
_diffrn_reflns_theta_full        27.5000
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1068 before and 0.0599 after correction. The Ratio of minimum to maximum transmission is 0.9185. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6264
_exptl_crystal_description       block
_exptl_crystal_F_000             2348.5265
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.1889
_refine_diff_density_min         -1.2450
_refine_diff_density_rms         0.1616
_refine_ls_d_res_high            0.7696
_refine_ls_d_res_low             7.4778
_refine_ls_goodness_of_fit_ref   1.0632
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    128
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         21371
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0631
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+6.1174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              23
_reflns_limit_k_min              -24
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                16665
_reflns_number_total             21371
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8sc01682h2.cif
_cod_data_source_block           ASRS11050_P-1
_cod_depositor_comments
;

2019-01-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549568--1549574.cif.
;
_cod_original_formula_moiety
'2(C31 H33 F3 N7 O3 S Sb), 4(C F3 O3 S), 5(C2 H3 N)'
_cod_original_formula_sum        'C76 H81 F18 N19 O18 S6 Sb2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2326.49
_cod_database_code               1549574
_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. Restrained distances
 F2-C40 \\sim F3-F1
 with sigma of 0.02
 F5-C41 \\sim F4-F6
 with sigma of 0.02
 F2-F3 \\sim F3-F1
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C1'(H1'a,H1'b), C24(H24a,H24b), C29'(H29d,H29e),
 C3'(H3'a,H3'b), C28(H28a,H28b), C5'(H5'a,H5'b), C1(H1a,H1b), C25'(H25d,H25e),
 C27'(H27d,H27e), C26(H26a,H26b)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C17'(H17'), C22(H22), C8'(H8'), C11'(H11'), C20'(H20'),
 C0aa(H0aa), C16'(H16'), C23'(H23'), C10(H10), C22'(H22'), C16(H16), C7(H7),
 C9'(H9'), C14'(H14'), C21'(H21'), C15(H15), C20(H20), C15'(H15'), C10'(H10'),
 C9(H9), C8(H8), C21(H21)
3.c Idealised Me refined as rotating group:
 C28'(H28c,H28d,H28e), C30'(H30a,H30b,H30c), C25(H25a,H25b,H25c), C29(H29a,
 H29b,H29c), C27(H27a,H27b,H27c), C35(H35a,H35b,H35c), C39(H39a,H39b,H39c),
 C31(H31a,H31b,H31c), C26'(H26c,H26d,H26e), C33(H33a,H33b,H33c), C37(H37a,H37b,
 H37c)
;
_olex2_submission_special_instructions 'No special instructions were received'