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_7027408
_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            'C16 H24 B N6 Tl'
_chemical_formula_weight         515.59
_chemical_melting_point          232
_chemical_name_systematic
; 
 [methyltris(3,5-dimethylpyrazol-1-yl)boratothallium(I)] 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.1250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.46560(10)
_cell_length_b                   9.96760(10)
_cell_length_c                   17.0414(3)
_cell_measurement_reflns_used    7222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.04
_cell_volume                     1936.45(4)
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14261
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    8.350
_exptl_absorpt_correction_T_max  0.2528
_exptl_absorpt_correction_T_min  0.1229
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_crystal_colour            'colourless, transparent'
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.651
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.00185(10)
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                3304
_reflns_number_total             4432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902264csup1.cif
_cod_data_source_block           LB59
_cod_database_code               7027408