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_7703893
_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 N6 Tl2'
_chemical_formula_sum            'C48 H68 N6 Tl2'
_chemical_formula_weight         1137.82
_chemical_name_systematic        '[Tl(N3Dipp2)]2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5767(5)
_cell_length_b                   20.2026(7)
_cell_length_c                   35.6666(11)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    180
_cell_measurement_theta_max      28.655
_cell_measurement_theta_min      2.490
_cell_volume                     9782.8(6)
_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      180.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            45357
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.158
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0667 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8008. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.454(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         21417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+2.7129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                15910
_reflns_number_total             21417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703893
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.437
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.546(7)
 0.454(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C19(H19), C82(H82), C70(H70), C91(H91), C7(H7), C58(H58), C94(H94), C43(H43),
 C46(H46), C22(H22), C79(H79), C67(H67), C10(H10), C34(H34), C31(H31), C55(H55)
3.b Aromatic/amide H refined with riding coordinates:
 C87(H87), C63(H63), C17(H17), C88(H88), C16(H16), C65(H65), C15(H15), C3(H3),
 C64(H64), C40(H40), C89(H89), C39(H39), C41(H41), C29(H29), C5(H5), C75(H75),
 C77(H77), C76(H76), C4(H4), C53(H53), C51(H51), C28(H28), C52(H52), C27(H27)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C20(H20A,H20B,H20C), C71(H71A,H71B,H71C), C72(H72A,H72B,
 H72C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C), C84(H84A,H84B,H84C), C96(H96A,
 H96B,H96C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C93(H93A,H93B,H93C),
 C47(H47A,H47B,H47C), C9(H9A,H9B,H9C), C83(H83A,H83B,H83C), C95(H95A,H95B,H95C),
  C35(H35A,H35B,H35C), C45(H45A,H45B,H45C), C81(H81A,H81B,H81C), C69(H69A,H69B,
 H69C), C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C80(H80A,
 H80B,H80C), C33(H33A,H33B,H33C), C68(H68A,H68B,H68C), C24(H24A,H24B,H24C),
 C92(H92A,H92B,H92C), C44(H44A,H44B,H44C), C23(H23A,H23B,H23C), C57(H57A,H57B,
 H57C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              51947
_olex2_submission_special_instructions 'No special instructions were received'