A new route to tris(pyrazolyl)borate ligands and new structural variations in TlTp complexes †
Janiak, Christoph; Braun, Lothar; Girgsdies, Frank; Journal of the Chemical Society, Dalton Transactions  (1999) 3133–; doi:10.1039/a902264c

data_7027410
_publ_section_title
;
 A new route to tris(pyrazolyl)borate ligands and new structural
 variations in TlTp complexes&#x200A;&#x2020;
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3133
_journal_paper_doi               10.1039/a902264c
_journal_year                    1999
_chemical_formula_sum            'C15 H22 B N6 Tl'
_chemical_formula_weight         501.57
_chemical_name_systematic
; 
 [hydrotris(3,5-dimethylpyrazol-1-yl)boratothallium(I)] 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.8120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.6275(5)
_cell_length_b                   8.61680(10)
_cell_length_c                   15.6585(2)
_cell_measurement_reflns_used    6521
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.53
_cell_volume                     3585.57(9)
_computing_cell_refinement       'SMART (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13372
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    9.016
_exptl_absorpt_correction_T_max  0.8000
_exptl_absorpt_correction_T_min  0.4236
_exptl_crystal_colour            'colourless, transparent'
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.862
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                2909
_reflns_number_total             4110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902264csup1.cif
_cod_data_source_block           LB95
_cod_database_code               7027410