Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and spectroscopic study.
Gyton, Matthew R.; Leverett, Anthony R.; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5653–5661; doi:10.1039/d0dt00285b

data_7703901
_publ_section_title
;
 Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and
 spectroscopic study.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5653
_journal_page_last               5661
_journal_paper_doi               10.1039/d0dt00285b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H68 Br N6 Tl'
_chemical_formula_sum            'C48 H68 Br N6 Tl'
_chemical_formula_weight         1013.36
_chemical_name_systematic        '[TlBr(N3Dipp2)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.570(3)
_cell_length_b                   16.835(3)
_cell_length_c                   21.235(4)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.410
_cell_measurement_theta_min      2.354
_cell_volume                     4947.8(18)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33377
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.471
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.108
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0535 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8389. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       cube
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         10694
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0717P)^2^+1.7544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5942
_reflns_number_total             10694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           17
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_original_cell_volume        4947.6(19)
_cod_database_code               7703901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C8A \\sim C7-C9A \\sim C7-C9 \\sim C7-C8
 with sigma of 0.02
 C12A-C11A \\sim C12-C11
 with sigma of 0.04
 C10-C12A \\sim C10-C11A \\sim C10-C12 \\sim C10-C11
 with sigma of 0.02
 C34-C36A \\sim C34-C35A \\sim C34-C35 \\sim C34-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C8A \\sim C9A \\sim C9: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C10 \\sim C11A \\sim C11 \\sim C12A \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C34 \\sim C36A \\sim C36 \\sim C35A \\sim C35: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C7, C8A, C8, C9, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11A, C11, C12A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C36A, C36, C35A, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=1-FVAR(1)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(1)
 Sof(H10A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=1-FVAR(2)
 Sof(H10)=Sof(C12)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=FVAR(2)
 Sof(H34A)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35A)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=1-FVAR(3)
 Sof(H34)=Sof(C35)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C34(H34A), C34(H34), C31(H31), C46(H46), C10(H10A), C10(H10), C7(H7B),
 C7(H7A), C19(H19), C43(H43), C22(H22)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C28(H28), C27(H27), C41(H41), C29(H29), C16(H16), C5(H5), C17(H17),
 C3(H3), C15(H15), C39(H39), C40(H40)
6.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C44(H44A,H44B,
 H44C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C),
 C12A(H12A,H12B,H12C), C23(H23A,H23B,H23C), C8A(H8AA,H8AB,H8AC), C33(H33A,H33B,
 H33C), C11A(H11A,H11B,H11C), C20(H20A,H20B,H20C), C9A(H9AA,H9AB,H9AC),
 C36A(H36A,H36B,H36C), C35A(H35A,H35B,H35C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C12(H12D,H12E,H12F), C11(H11D,H11E,H11F), C35(H35D,H35E,H35F), C36(H36D,H36E,
 H36F)
;
_shelx_res_checksum              70806
_olex2_submission_special_instructions 'No special instructions were received'