'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_7106974
_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_formula_moiety         'C24 H24 B1 Cl7 Cu1 N5 O3'
_chemical_formula_sum            'C24 H24 B Cl7 Cu N5 O3'
_chemical_formula_weight         753.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-03-28
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 91.247(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5238(2)
_cell_length_b                   16.9403(5)
_cell_length_c                   21.7245(6)
_cell_measurement_reflns_used    17681
_cell_measurement_temperature    100
_cell_measurement_theta_max      73
_cell_measurement_theta_min      2
_cell_volume                     3136.18(15)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29658
_diffrn_reflns_theta_full        71.390
_diffrn_reflns_theta_max         72.847
_diffrn_reflns_theta_min         3.309
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.778
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.20
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0016
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.0002370
_refine_ls_shift/su_mean         0.0000225
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 8.21P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1444
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1444
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5739
_reflns_number_total             6197
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.49
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0604
_oxford_refine_ls_scale          3.60(5)
_oxford_reflns_number_all        6197
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'pb1003 in P2(1)/c'
_cod_data_source_file            c1cc14473a.txt
_cod_data_source_block           pb1003
_cod_original_cell_volume        3136.17(16)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C24 H24 B1 Cl7 Cu1 N5 O3'
_cod_database_code               7106974