Isostructural Potassium and Thallium Salts of Sterically Crowded Triazenes: A Structural and Computational Study
Hyui Sul Lee; Sven-Oliver Hauber; Denis Vinduš; Mark Niemeyer; Inorganic Chemistry 47 (2008) 4401–4412; doi:10.1021/ic800029z

data_4304933
_publ_contact_author_address
;
Institut f\"ur Anorganische und Analytische Chemie
Johannes Gutenberg-Universit\"at Mainz
Duesbergweg 10-14
D-55099 Mainz
Germany
;
_publ_contact_author_email       niemeyer@uni-mainz.de
_publ_contact_author_name        'Mark Niemeyer'
_publ_section_title
;
Isostructural Potassium and Thallium Salts of Sterically Crowded Triazenes:
A Structural and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4401
_journal_page_last               4412
_journal_paper_doi               10.1021/ic800029z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C42 H54 N3 Tl'
_chemical_formula_weight         805.25
_chemical_melting_point          '289-293 deg.C (dec.)'
_chemical_name_systematic
;
((1,3-bis-(2',4',6'-triisopropylbiphenyl-2))(triazenido-N,N'))thallium
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.603(8)
_cell_angle_beta                 104.350(10)
_cell_angle_gamma                90.816(11)
_cell_formula_units_Z            2
_cell_length_a                   9.4318(14)
_cell_length_b                   14.4350(16)
_cell_length_c                   14.8042(15)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      6.0
_cell_volume                     1908.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9757
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.4827
_exptl_absorpt_correction_T_min  0.2244
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                8042
_reflns_number_total             9211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800029z-file003_6.cif
_cod_data_source_block           3a
_cod_database_code               4304933