Kinetic stabilization of low-oxidation state and terminal hydrido main group metal complexes by a sterically demanding N,N'-bis(2,6-terphenyl)triazenide.
Leverett, Anthony R.; Diachenko, Vera; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13197–13204; doi:10.1039/c9dt02562f

data_7700757
_publ_section_title
;
 Kinetic stabilization of low-oxidation state and terminal hydrido main
 group metal complexes by a sterically demanding
 N,N'-bis(2,6-terphenyl)triazenide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13197
_journal_page_last               13204
_journal_paper_doi               10.1039/c9dt02562f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H50 N3 Tl, 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H54 N3 Tl'
_chemical_formula_weight         919.34
_chemical_name_common            '[Tl(N3Dmp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                102.694(7)
_cell_angle_beta                 95.730(7)
_cell_angle_gamma                110.677(8)
_cell_formula_units_Z            2
_cell_length_a                   10.558(2)
_cell_length_b                   11.470(2)
_cell_length_c                   20.162(3)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.703
_cell_measurement_theta_min      2.480
_cell_volume                     2186.0(7)
_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      183.01
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30536
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.260
_exptl_absorpt_coefficient_mu    3.732
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0746 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.8082. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9447
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0542P)^2^+1.0170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7038
_reflns_number_total             9447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_cell_volume        2185.9(7)
_cod_original_formula_sum        'C51.50 H54 N3 Tl'
_cod_database_code               7700757
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.604
_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
 C50-C55 = C55-C54 = C54-C53 = C53-C52 = C52-C51 = C51-C50
 1.4 with sigma of 0.01
 Tl-N1 \\sim Tl1A-N1 \\sim Tl-N3 \\sim Tl1A-N3
 with sigma of 0.02
 C50-C52 \\sim C50-C54 \\sim C51-C53 \\sim C55-C51 \\sim C54-C52 \\sim C55-C53
 with sigma of 0.04
 C49-C51 \\sim C49-C55
 with sigma of 0.04
3. Restrained planarity
 C49, C50, C55, C54, C53, C52, C51
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C55 \\sim C54 \\sim C53 \\sim C52 \\sim C51: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C49, C50, C55, C54, C53, C52, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Tl)=1-FVAR(1)
 Sof(Tl1A)=FVAR(1)
 Fixed Sof: C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) C55(0.5) H55(0.5)
 C54(0.5) H54(0.5) C53(0.5) H53(0.5) C52(0.5) H52(0.5) C51(0.5) H51(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C5(H5), C28(H28), C29(H29), C42(H42), C35(H35), C18(H18), C44(H44),
 C33(H33), C20(H20), C3(H3), C4(H4), C11(H11), C9(H9), C55(H55), C54(H54),
 C53(H53), C52(H52), C51(H51)
7.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C46(H46A,H46B,
 H46C), C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C13(H13A,
 H13B,H13C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C),
 C38(H38A,H38B,H38C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              90019
_olex2_submission_special_instructions 'No special instructions were received'