Synthesis of triarylborane-centered N-heterocyclic carbene cages with tunable photophysical properties
Zhang, Yi-Fan; Zhang, Ya-Wen; Li, Xin; Sun, Li-Ying; Han, Ying-Feng; Chemical Communications 59 (2023) 2291–2294; doi:10.1039/D2CC06584C

data_7131320
_publ_section_title
;
 Synthesis of triarylborane-centered N-heterocyclic carbene cages with
 tunable photophysical properties
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              2291
_journal_page_last               2294
_journal_paper_doi               10.1039/D2CC06584C
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'C144 H138 Ag3 B2 N12, 3(F6 P), 4[C2H3N], 2[C4H10O]'
_chemical_formula_sum            'C160 H170 Ag3 B2 F18 N16 O2 P3'
_chemical_formula_weight         3129.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.09.28 svn.r5c12d49f for OlexSys, GUI svn.r6264)
;
_audit_update_record
;
2023-01-13 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.276(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.755(2)
_cell_length_b                   19.4743(14)
_cell_length_c                   29.186(2)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    201.0
_cell_measurement_theta_max      24.84
_cell_measurement_theta_min      2.20
_cell_volume                     15775.1(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (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      201.00
_diffrn_measured_fraction_theta_full 0.996
_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  0.0943
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            86867
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.999
_diffrn_reflns_theta_max         19.999
_diffrn_reflns_theta_min         1.895
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0932 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.9116.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             6464
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         7346
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0973P)^2^+116.7666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4733
_reflns_number_total             7346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06584c2.cif
_cod_data_source_block           c144h138ag3b2f18n12p3
_cod_original_cell_volume        15776(2)
_cod_database_code               7131320
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.898
_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. Restrained distances
 P2-F18 = P2-F12 = P2-F16 = P2-F17 = P2-F10 = P2-F19 = P2-F7 = P2-F8 = P2-F15 =
  P2-F11 = P2-F9
 1.6 with sigma of 0.01
 C67-C18 = C66-C22 = C65-C20 = C64-C61 = C70-C59 = C68-C51 = C72-C49
 1.5 with sigma of 0.01
 C69-C47 = C71-C57
 1.54 with sigma of 0.01
 F3-F5 \\sim F3-F4 \\sim F3-F6 \\sim F3-F2 \\sim F1-F5 \\sim F1-F4 \\sim F1-F6
\\sim F1-F2 \\sim F5-F4 \\sim F5-F2
 \\sim F4-F6 \\sim F6-F2
 with sigma of 0.02
 F12-F10 \\sim F12-F9 \\sim F12-F7 \\sim F12-F8 \\sim F11-F10 \\sim F11-F9
\\sim F11-F7 \\sim F11-F8 \\sim F10-
 F9 \\sim F10-F8 \\sim F9-F7 \\sim F7-F8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Ag2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C66, C21, C65, C20, C19, C67, C18, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P1, F1, F2, F3, F4, F5, F6, F13, F14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F7, F12, F8, F19, F15, F18, F16, F17, F9, F11, F10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C40, C37, C55, C63, C53, N4, C38, C54, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C71, C58, C59, C70, C60, C61, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C47, C51, C68, C69, C48, C49, C50, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: F4(0.7) F5(0.6) F6(0.7) P2(0.5) F7(0.5) F8(0.3) F9(0.3) F10(0.3)
 F11(0.3) F12(0.25) F13(0.5) F14(0.5) F15(0.25) F16(0.25) F17(0.15) F18(0.2)
 F19(0.2)
6.a Me refined with riding coordinates:
 C71(H71A,H71B,H71C)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C13(H13), C14(H14), C15(H15), C19(H19), C21(H21), C26(H26),
 C27(H27), C31(H31), C32(H32), C34(H34), C36(H36), C40(H40), C43(H43), C48(H48),
  C50(H50), C52(H52), C54(H54), C55(H55), C56(H56), C58(H58), C60(H60), C63(H63)
6.c Fitted hexagon refined as free rotating group:
 C17(C18,C19,C20,C21,C22), C46(C47,C48,C49,C50,C51), C57(C58,C59,C60,C61,C62)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C41(H41A,H41B,
 H41C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22840
_shelx_hkl_checksum              90086
_shelx_fab_checksum              14362
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'