Pentacyclic fused diborepinium ions with carbene- and carbone-mediated deep-blue to red emission.
Hollister, Kimberly K.; Molino, Andrew; Le, VuongVy V; Jones, Nula; Smith, Wyatt J.; Müller, Peter; Dickie, Diane A.; Wilson, David J. D.; Gilliard, Jr, Robert J; Chemical science 15 (2024) 14358–14370; doi:10.1039/d4sc03835e

data_1572280
_publ_section_title
;
 Pentacyclic fused diborepinium ions with carbene- and carbone-mediated
 deep-blue to red emission.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14358
_journal_page_last               14370
_journal_paper_doi               10.1039/d4sc03835e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C76 H86 B2 Cl2 N4), C7 H8'
_chemical_formula_sum            'C159 H180 B4 Cl4 N8'
_chemical_formula_weight         2388.14
_chemical_name_common            WJS-5
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-28 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                95.587(4)
_cell_angle_beta                 96.221(4)
_cell_angle_gamma                90.244(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1202(5)
_cell_length_b                   17.0454(8)
_cell_length_c                   19.6957(11)
_cell_measurement_reflns_used    6605
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      68.2820
_cell_measurement_theta_min      2.6049
_cell_volume                     3361.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_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 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49634
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.602
_diffrn_reflns_theta_min         2.267
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         12273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0625P)^2^+1.5372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8498
_reflns_number_total             12273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03835e2.cif
_cod_data_source_block           3Cl
_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 1572276--1572287.cif.
;
_cod_database_code               1572280
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C76A) = Uanis(C75A) = Uanis(C74A)
Uanis(C66A) = Uanis(C67A) = Uanis(C68A) = Uanis(C69A) = Uanis(C70A) =
Uanis(C71A)
Uanis(B2) = Uanis(B2A)
Uanis(C76A) = Uanis(C75A) = Uanis(C74A) = Uanis(C73A) = Uanis(C72A) =
Uanis(C66A) = Uanis(C70A) = Uanis(C69A) = Uanis(C68A) = Uanis(C67A) =
Uanis(C71A)
3. Others
 Sof(Cl2A)=Sof(C66A)=Sof(C71A)=Sof(C70A)=Sof(H70A)=Sof(C69A)=Sof(H69A)=
 Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=
 Sof(H73A)=Sof(C74A)=Sof(C75A)=Sof(H75A)=Sof(C76A)=Sof(B2A)=1-FVAR(1)
 Sof(Cl2)=Sof(C66)=Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=
 Sof(C70)=Sof(H70)=Sof(C71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=Sof(C74)=
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(B2)=FVAR(1)
 Fixed Sof: C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C78(0.5) C79(0.5) H79(0.5)
 C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82(0.5) C83(0.5) H83(0.5)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C27(H27), C34(H34), C38(H38), C48(H48), C51(H51), C60(H60), C63(H63)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19),
 C20(H20), C23(H23), C24(H24), C30(H30), C31(H31), C32(H32), C40(H40), C41(H41),
  C44(H44), C45(H45), C46(H46), C56(H56), C57(H57), C58(H58), C67(H67),
 C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C75(H75), C70A(H70A),
 C69A(H69A), C68A(H68A), C67A(H67A), C72A(H72A), C73A(H73A), C75A(H75A),
 C79(H79), C80(H80), C81(H81), C82(H82), C83(H83)
4.c Fitted hexagon refined as free rotating group:
 C66A(C71A,C70A,C69A,C68A,C67A)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              37159
_shelx_hkl_checksum              1494
_olex2_submission_special_instructions 'No special instructions were received'