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_1560374
_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
'C36 H48 Ag4 N24, 3(B F4), B F3.99, 3(C2 H3 N)'
_chemical_formula_sum            'C42 H57 Ag4 B4 F15.987 N27'
_chemical_formula_weight         1718.59
_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             2020-04-23
_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                85.032(7)
_cell_angle_beta                 81.796(8)
_cell_angle_gamma                77.855(7)
_cell_formula_units_Z            2
_cell_length_a                   11.052(3)
_cell_length_b                   14.637(4)
_cell_length_c                   21.244(5)
_cell_measurement_reflns_used    11831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.240
_cell_volume                     3319.6(15)
_computing_cell_refinement       'APEX3 (Bruker,2015)'
_computing_data_collection       'APEX3 (Bruker,2015)'
_computing_data_reduction        'SAINT+ (Bruker,2009)'
_computing_molecular_graphics    '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
'Olex2 (Dolomanov et al., 2009),intrinsic phasing'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9956
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64288
_diffrn_reflns_theta_full        27.9263
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.261
_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            yellow
_exptl_crystal_density_diffrn    1.7192
_exptl_crystal_description       block
_exptl_crystal_F_000             1693.5905
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.0808
_refine_diff_density_min         -1.7892
_refine_diff_density_rms         0.2481
_refine_ls_d_res_high            0.7588
_refine_ls_d_res_low             9.0852
_refine_ls_goodness_of_fit_ref   1.0461
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     897
_refine_ls_number_reflns         15858
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.0432
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.0017
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+18.0746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                11831
_reflns_number_total             15858
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06957d2.cif
_cod_data_source_block           bip523_a
_cod_depositor_comments
'Adding full bibliography for 1560371--1560374.cif.'
_cod_original_cell_volume        3319.5(14)
_cod_database_code               1560374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F5) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(C41) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2A) \\sim Ueq, Uanis(F2B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F1A) \\sim Ueq, Uanis(F1B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F15A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F2B) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: F1A(0.5) F2A(0.4) F5(0.66) F7(0.66) F1aa(0.33333) F0aa(0.33333)
 F1B(0.5) F2B(0.6) F15A(0.5) F15B(0.5)
4.a Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C11(H11a,
 H11b,H11c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c),
 C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C26(H26a,H26b,H26c), C25(H25a,H25b,
 H25c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c), C35(H35a,H35b,H35c), C34(H34a,
 H34b,H34c), C41(H41a,H41b,H41c), C71(H71a,H71b,H71c), C51(H51a,H51b,H51c)
;
_olex2_submission_special_instructions 'No special instructions were received'