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_4304928
_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 K N3'
_chemical_formula_weight         639.98
_chemical_melting_point          '326-332 deg.C (dec.)'
_chemical_name_systematic
;
((1,3-bis-(2',4',6'-triisopropylbiphenyl-2))(triazenido-N,N'))potassium
;
_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                101.089(16)
_cell_angle_beta                 104.113(13)
_cell_angle_gamma                91.023(14)
_cell_formula_units_Z            2
_cell_length_a                   9.4209(14)
_cell_length_b                   14.406(3)
_cell_length_c                   14.624(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1884.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9154
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        <0.5%
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep yellow'
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0029(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8625
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.8660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                7499
_reflns_number_total             8625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800029z-file003_1.cif
_cod_data_source_block           2a
_cod_database_code               4304928