Isolating the ring-redox states of boron sub-phthalocyanines.
Zhou, Wen; McKearney, Declan; Okada, Yusuke; Kobayashi, Nagao; Leznoff, Daniel B.; Chemical communications (Cambridge, England) 61 (2025) 3832–3835; doi:10.1039/d4cc06727d

data_7134251
_publ_section_title
;
 Isolating the ring-redox states of boron sub-phthalocyanines.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3832
_journal_page_last               3835
_journal_paper_doi               10.1039/d4cc06727d
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'8(C24 H12 B F N6), 8(C H1.25 Ag0.288 O0.5), 4(C1.75 H1.75), 8(C H2.5 O0.5), 1.694(Ag), 8(C6 H14 O3), 12(F6 Sb)'
_chemical_formula_sum            'C263 H255 Ag4 B8 F80 N48 O32 Sb12'
_chemical_formula_weight         8099.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2024-07-06 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.704(7)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   23.995(2)
_cell_length_b                   15.5710(12)
_cell_length_c                   26.2282(18)
_cell_measurement_reflns_used    8581
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.912
_cell_measurement_theta_min      2.75
_cell_volume                     9335.4(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            126909
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.912
_diffrn_reflns_theta_min         3.344
_exptl_absorpt_coefficient_mu    9.264
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.8571.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       Block
_exptl_crystal_F_000             3985
_exptl_crystal_size_max          0.827
_exptl_crystal_size_mid          0.397
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.286
_refine_diff_density_min         -2.259
_refine_diff_density_rms         0.312
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         8581
_refine_ls_number_restraints     574
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1779P)^2^+96.0626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2540
_refine_ls_wR_factor_ref         0.2577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8146
_reflns_number_total             8581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06727d2.cif
_cod_data_source_block           SubPcBFSbF6AgSbF6_0m_a_pl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134249--7134252.cif.
;
_cod_database_code               7134251
_shelx_shelxl_version_number     2018/3
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O5-C58 = O5-C55 = C55-C56 = C56-O4 = O4-C57
 1.5 with sigma of 0.02
 C66-O7 = O7-C65 = C65-C64 = C64-O6 = O6-C63
 1.4 with sigma of 0.02
 C59-C60 = C60-C61 = C61-C62
 1.4 with sigma of 0.01
 C58-C55 = O5-C56 = F10-F15 = F12-F11
 2 with sigma of 0.01
 C60_$1-C60
 1.4 with sigma of 0.01
 C62_$1-C62
 1.4 with sigma of 0.01
 C61_$1-C61
 2.8 with sigma of 0.01
 O3-N1
 2.88 with sigma of 0.01
3. Restrained planarity
 C59, C60, C61, C62
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O7 \\sim O6 \\sim C65 \\sim C64 \\sim C63 \\sim C66: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O4 \\sim O5 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Ag2 \\sim Ag1 \\sim Sb1 \\sim Sb2 \\sim Sb3 \\sim F19 \\sim F1 \\sim F2 \\sim
F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11
\\sim F12 \\sim F13 \\sim F14 \\sim F15: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag2) \\sim Ueq, Uanis(Ag1) \\sim Ueq, Uanis(Sb1) \\sim Ueq, Uanis(Sb2)
\\sim Ueq, Uanis(Sb3) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Ag2)=0.5*(1-FVAR(2))
 Sof(Ag1)=0.5*FVAR(2)
 Sof(Sb3)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=1-FVAR(2)
 Sof(Sb1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Fixed Sof: C55(0.25) H55A(0.25) H55B(0.25) C56(0.25) H56A(0.25) H56B(0.25)
 C57(0.25) H57A(0.25) H57B(0.25) H57C(0.25) C58(0.25) H58A(0.25) H58B(0.25)
 H58C(0.25) O4(0.25) O5(0.25) C59(0.125) H59A(0.125) H59B(0.125) H59C(0.125)
 C60(0.25) C61(0.25) H61(0.25) C62(0.25) H62(0.25) O6(0.25) O7(0.25) C63(0.25)
 H63A(0.125) H63B(0.125) H63C(0.125) H63D(0.125) H63E(0.125) H63F(0.125)
 C64(0.25) H64A(0.25) H64B(0.25) C65(0.25) H65A(0.25) H65B(0.25) C66(0.25)
 H66A(0.125) H66B(0.125) H66C(0.125) H66D(0.125) H66E(0.125) H66F(0.125)
6.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C64(H64A,H64B), C65(H65A,H65B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C19(H19), C20(H20), C21(H21), C22(H22), C61(H61), C62(H62)
6.c Disordered Me refined with riding coordinates:
 C63(H63A,H63B,H63C,H63D,H63E,H63F), C66(H66A,H66B,H66C,H66D,H66E,H66F)
6.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C49(H49A,H49B,H49C), C54(H54A,H54B,
 H54C)
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_shelx_res_checksum              81664
_shelx_hkl_checksum              33081
_olex2_submission_special_instructions 'No special instructions were received'