Phenyl tris(3-tert-butylpyrazolyl)borato complexes of lithium and thallium, [PhTpBut]M (M = Li, Tl): a novel structure for a monomeric tris(pyrazolyl)boratothallium complex and a study of its stereochemical nonrigidity by 1H and 205Tl NMR spectroscopy
Kisko, Jennifer L.; Hascall, Tony; Kimblin, Clare; Parkin, Gerard; Journal of the Chemical Society, Dalton Transactions  (1999) 1929–; doi:10.1039/a901875a

data_7027371
_publ_section_title
;
 Phenyl tris(3-tert-butylpyrazolyl)borato complexes of lithium and
 thallium, [PhTpBut]M (M&#x2005;=&#x2005;Li, Tl): a novel structure for a
 monomeric tris(pyrazolyl)boratothallium complex and a study of its
 stereochemical nonrigidity by 1H and 205Tl NMR spectroscopy
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1929
_journal_paper_doi               10.1039/a901875a
_journal_year                    1999
_chemical_formula_sum            'C27 H39 B N6'
_chemical_formula_weight         458.45
_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
_cell_angle_alpha                114.0030(10)
_cell_angle_beta                 101.4090(10)
_cell_angle_gamma                109.4400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6639(8)
_cell_length_b                   12.1658(8)
_cell_length_c                   12.2480(8)
_cell_measurement_temperature    173(2)
_cell_volume                     1380.66(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9658
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0059(19)
_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_all   1.070
_refine_ls_goodness_of_fit_obs   1.180
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.180
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_obs          0.0740
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.0735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1842
_refine_ls_wR_factor_obs         0.1610
_reflns_number_observed          3788
_reflns_number_total             5729
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901875asup1.cif
_cod_data_source_block           tphs10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.0735P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.0735P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1380.7(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027371