Ternary lanthanide complexes of hydrotris[3-(2-pyridyl)pyrazol-1-yl]borate (Tp^py^) and anionic <i>O</i>,<i>O</i>-bidentate chelates: [Tb(Tp^py^)(dbm)~2~] and [Eu(Tp^py^)(trop)(NO~3~)] (Hdbm is dibenzoylmethane and Htrop is tropolone)
Ward, Michael D.; McCleverty, Jon A.; Mann, Karen L. V.; Jeffery, John C.; Motson, Graham R.; Hurst, Joanne; Acta Crystallographica Section C 55 (1999) 2055–2058; doi:10.1107/S0108270199011051

data_2009235
_publ_section_title
;
 Ternary lanthanide complexes of
 hydrotris[3-(2-pyridyl)pyrazol-1-yl]borate (Tp^py^) and anionic
 <i>O</i>,<i>O</i>-bidentate chelates: [Tb(Tp^py^)(dbm)~2~] and
 [Eu(Tp^py^)(trop)(NO~3~)] (Hdbm is dibenzoylmethane and Htrop is
 tropolone)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2055
_journal_page_last               2058
_journal_paper_doi               10.1107/S0108270199011051
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Tb(C15 H11 O2 )2 (C24 H19 B N9)]'
_chemical_formula_moiety         'C54 H41 B N9 O4 Tb'
_chemical_formula_sum            'C54 H41 B N9 O4 Tb'
_chemical_formula_weight         1049.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.284(9)
_cell_angle_beta                 92.329(13)
_cell_angle_gamma                110.712(11)
_cell_formula_units_Z            2
_cell_length_a                   11.4944(17)
_cell_length_b                   14.1547(18)
_cell_length_c                   16.292(2)
_cell_measurement_reflns_used    210
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3
_cell_volume                     2319.7(6)
_computing_cell_refinement       'SAINT (Siemens, 1995a)'
_computing_data_collection       'SMART (Siemens, 1995a)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Siemens, 1995b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'Siemens Smart area detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21541
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.597
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                7337
_reflns_number_total             10457
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf1328.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2009235