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_1572277
_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(C32 H12 B F23.976), C44 H54 B2 N4, 2(C H2 Cl2)'
_chemical_formula_sum            'C110 H82 B4 Cl4 F47.95 N4'
_chemical_formula_weight         2555.88
_chemical_name_common            'FBP-sIPr cation BARF'
_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     dual
_audit_creation_date             2024-02-10
_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                79.135(2)
_cell_angle_beta                 72.923(2)
_cell_angle_gamma                89.308(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3947(8)
_cell_length_b                   12.5964(8)
_cell_length_c                   19.1553(12)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      29.1389
_cell_measurement_theta_min      2.3115
_cell_volume                     2804.6(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 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, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS double bounce multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85598
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.283
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.563
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         15059
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0682P)^2^+1.8178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12626
_reflns_number_total             15059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03835e2.cif
_cod_data_source_block           Gilliard_KKH_2_104_X2
_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               1572277
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
F19 \\sim F20 \\sim F21 \\sim F19A \\sim F20A \\sim F21A \\sim F19B \\sim F20B
\\sim F21B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(F19A) = Uanis(F19) = Uanis(F19B)
Uanis(F21A) = Uanis(F21) = Uanis(F21B)
Uanis(F4) = Uanis(F4A) = Uanis(F4B)
Uanis(F6) = Uanis(F6A) = Uanis(F6B)
Uanis(F5) = Uanis(F5B) = Uanis(F5A)
2. Others
 1*[Sof(F1)+Sof(F2)+Sof(F3)]+1*[Sof(F1A)+Sof(F2A)+Sof(F3A)]+1*[Sof(F1B)+
 Sof(F2B)+Sof(F3B)]=1 with esd of 0.02
 1*[Sof(F19)+Sof(F20)+Sof(F21)]+1*[Sof(F19A)+Sof(F20A)+Sof(F21A)]+1*[Sof(F19B)+
 Sof(F20B)+Sof(F21B)]=1 with esd of 0.02
 1*[Sof(F4)+Sof(F5)+Sof(F6)]+1*[Sof(F4A)+Sof(F5A)+Sof(F6A)]+1*[Sof(F4B)+
 Sof(F5B)+Sof(F6B)]=1 with esd of 0.02
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(5)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(5)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(6)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(7)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=0.35001*FVAR(9)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(9)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(9)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(10)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(11)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=FVAR(12)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C55A)=Sof(H55C)=Sof(H55D)=1-FVAR(13)
 Sof(Cl1)=Sof(Cl3)=Sof(C55)=Sof(H55A)=Sof(H55B)=FVAR(13)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C20(H20)
3.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C55A(H55C,H55D)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C30(H30), C32(H32), C35(H35), C38(H38), C40(H40),
 C43(H43), C46(H46), C48(H48), C51(H51), C54(H54), C2(H2), C4(H4), C5(H5),
 C7(H7), C8(H8), C9(H9), C10(H10)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              86348
_shelx_hkl_checksum              96565
_olex2_submission_special_instructions 'No special instructions were received'