The transformations of a methylene-bridged bis-triazolium salt: a mesoionic carbene based metallocage and analogues of TCNE and NacNac
Stubbe, Jessica; Suhr, Simon; Beerhues, Julia; Nößler, Maite; Sarkar, Biprajit; Chemical Science 12 (2021) 3170–3178; doi:10.1039/D0SC06957D

data_1560373
_publ_section_title
;
 The transformations of a methylene-bridged bis-triazolium salt: a
 mesoionic carbene based metallocage and analogues of TCNE and NacNac
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3170
_journal_page_last               3178
_journal_paper_doi               10.1039/D0SC06957D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         '4(B F4), 2(C9 H14 N6), 2(C2 H3 N)'
_chemical_formula_sum            'C22 H34 B4 F16 N14'
_chemical_formula_weight         841.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-24 deposited with the CCDC.	2021-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                97.92(9)
_cell_angle_beta                 92.65(7)
_cell_angle_gamma                102.91(7)
_cell_formula_units_Z            2
_cell_length_a                   10.15(2)
_cell_length_b                   11.83(3)
_cell_length_c                   15.93(4)
_cell_measurement_reflns_used    5771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.06
_cell_volume                     1841(8)
_computing_molecular_graphics
'Olex2 (Dolomanov et al., 2009), Diamond 3D, Version 4.0 (Brandenburg, 2014)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
'SHELXT 2014/5 (Sheldrick, 2014), intrinsic pahsing'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34133
_diffrn_reflns_theta_full        26.3859
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.9268.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.5186
_exptl_crystal_description       needle
_exptl_crystal_F_000             856.6978
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.7968
_refine_diff_density_min         -0.5748
_refine_diff_density_rms         0.0773
_refine_ls_d_res_high            0.7996
_refine_ls_d_res_low             9.8655
_refine_ls_goodness_of_fit_ref   1.1245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1245
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+1.5132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5771
_reflns_number_total             7514
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06957d2.cif
_cod_data_source_block           bip614_a
_cod_depositor_comments
'Adding full bibliography for 1560371--1560374.cif.'
_cod_database_code               1560373
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C10(H10), C18(H18)
2.b Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C12(H12a,H12b,H12c), C2(H2a,H2b,H2c), C7(H7a,H7b,H7c),
 C11(H11a,H11b,H11c), C8(H8a,H8b,H8c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c),
  C20(H20a,H20b,H20c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'