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_1549570
_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         'C24 H18 N7 P, 0.5(C2 H3 N)'
_chemical_formula_sum            'C25 H19.5 N7.5 P'
_chemical_formula_weight         455.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-04
_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                90
_cell_angle_beta                 114.6194(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0553(5)
_cell_length_b                   25.1646(12)
_cell_length_c                   14.6359(6)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.06
_cell_volume                     4371.2(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            206509
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         2.871
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0604 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.9529. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0377P)^2^+2.6112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9215
_reflns_number_total             10847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01682h2.cif
_cod_data_source_block           as606_p21n
_cod_depositor_comments
;

2019-01-20
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(C24 H18 N7 P), C2 H3 N'
_cod_original_formula_sum        'C50 H39 N15 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     911.90
_cod_database_code               1549570
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.956
_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:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C1'(H1'A,H1'B), C3'(H3'A,H3'B),
 C2'(H2'A,H2'B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C23(H23), C14(H14), C8(H8), C16(H16), C20(H20), C9(H9), C15(H15),
 C22(H22), C11(H11), C21(H21), C10(H10), C11'(H11'), C10'(H10'), C9'(H9'),
 C8'(H8'), C20'(H20'), C21'(H21'), C23'(H23'), C22'(H22'), C17'(H17'),
 C14'(H14'), C15'(H15'), C16'(H16')
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              23941
_olex2_submission_special_instructions 'No special instructions were received'