A C3-symmetric chiral hexadentate podand ligand based on a tris(pyrazolyl)borate core
Motson, Graham R.; Mamula, Olimpia; Jeffery, John C.; McCleverty, Jon A.; Ward, Michael D.; von Zelewsky, Alex; Journal of the Chemical Society, Dalton Transactions  (2001) 1389–; doi:10.1039/b102295b

data_7010684
_publ_section_title
;
 A C3-symmetric chiral hexadentate podand ligand based on a
 tris(pyrazolyl)borate core
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1389
_journal_paper_doi               10.1039/b102295b
_journal_year                    2001
_chemical_formula_sum            'C45 H49 B N9 Tl'
_chemical_formula_weight         931.11
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.3970(18)
_cell_length_b                   20.3970(18)
_cell_length_c                   17.347(3)
_cell_measurement_temperature    173(2)
_cell_volume                     6250.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames (0.3 degrees)'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21871
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_correction_T_min  0.5078
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6361
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          1.143
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                5565
_reflns_number_total             6361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102295b.txt
_cod_data_source_block           1
_cod_original_cell_volume        6250.1(12)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7010684