'Twisted' scorpionates: synthesis of a tris(2-pyridonyl)borate (Thp) ligand; lessons in the requirements for successful B(L2D)3 type ligands
Philip J. Bailey; Nicola L. Bell; Lim Li Gim; Tai Yucheng; Nicholas Funnell; Fraser White; Simon Parsons; Chem.Commun. 47 (2011) 11659–; doi:10.1039/c1cc14473a

data_7106973
_publ_section_title
;
 'Twisted' scorpionates: synthesis of a tris(2-pyridonyl)borate (Thp)
 ligand; lessons in the requirements for successful B(L2D)3 type ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              11659
_journal_paper_doi               10.1039/c1cc14473a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'Lim Li Gim'
_chemical_formula_moiety         'C22 H22 B N5 O3'
_chemical_formula_sum            'C22 H22 B N5 O3'
_chemical_formula_weight         415.26
_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                 93.5990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5746(2)
_cell_length_b                   10.6207(2)
_cell_length_c                   16.5475(3)
_cell_measurement_reflns_used    16956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.214
_cell_volume                     2030.18(6)
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'Phi and Omega 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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38547
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9849
_exptl_absorpt_correction_T_min  0.8857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_recrystallization_method
'slow diffusion of diethyl ether into dichloromethane solution'
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.6633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                4101
_reflns_number_total             5167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14473a.txt
_cod_data_source_block           pb9009
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7106973