Comparison of thallium(I) complexes with mesityl-substituted tris(pyrazolyl)hydroborate ligands, [Tl{HB(3-Ms-5-Mepz)~3~}] and [Tl{HB(3-Ms-5-Mepz)~2~(3-Me-5-Mspz)}]
Fujisawa, Kiyoshi; Shimizu, Masaya; Szilagyi, Robert K.; Acta Crystallographica Section C 72 (2016) 786–790; doi:10.1107/S2053229615023797

data_2020598
_publ_section_title
;
 Comparison of thallium(I) complexes with mesityl-substituted
 tris(pyrazolyl)hydroborate ligands, [Tl{HB(3-Ms-5-Mepz)~3~}] and
 [Tl{HB(3-Ms-5-Mepz)~2~(3-Me-5-Mspz)}]
;
_journal_coeditor_code           YP3109
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              786
_journal_page_last               790
_journal_paper_doi               10.1107/S2053229615023797
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Tl (C39 H46 B N6)]'
_chemical_formula_moiety         'C39 H46 B N6 Tl, H2 O1'
_chemical_formula_sum            'C39 H48 B N6 O Tl'
_chemical_formula_weight         832.03
_chemical_name_systematic
;
[Tris(3-mesityl-5-methyl-1<i>H</i>-pyrazol-1-yl-\
\k<i>N</i>^2^)hydroborato]thallium(I) monohydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   11.7826(11)
_cell_length_b                   11.7826(11)
_cell_length_c                   47.7550(4)
_cell_measurement_reflns_used    8683
_cell_measurement_temperature    182
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     5741.6(8)
_computing_cell_refinement       'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_data_collection       'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_molecular_graphics    'CrystalStructure (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2015)'
_computing_structure_solution    'Il Milione (Burla et al., 2007)'
_diffrn_ambient_temperature      182
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            20998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.458
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.25
_exptl_absorpt_correction_T_max  0.507
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Rigaku, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2922
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0396P)^2^+2.9797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                2759
_reflns_number_total             2922
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            yp3109sup1.cif
_cod_data_source_block           20140719_l65tl_73
_cod_depositor_comments
'Adding full bibliography for 2020598--2020599.cif.'
_cod_database_code               2020598
_cod_database_fobs_code          2020598