Tris(dibenzoylmethanido-κ^2^<i>O</i>,<i>O</i>')[(6<i>R</i>,8<i>R</i>)-({-})-7,7-dimethyl-3-(2-pyridyl)-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-κ^2^<i>N</i>,<i>N</i>']terbium(III)
Chen, Lei-Qi; Guo, Jian-Nan; Xuan, Wei-Min; Lin, Yi-Ji; Zhang, Hui; Acta Crystallographica Section E 65 (2009) m705–; doi:10.1107/S1600536809019783

data_2222404
_publ_section_title
Tris(dibenzoylmethanido-\k^2^<i>O</i>,<i>O</i>')[(6<i>R</i>,8<i>R</i>)-({-})-7,7-dimethyl-3-(2-pyridyl)-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-\k^2^<i>N</i>,<i>N</i>']terbium(III)
_journal_coeditor_code           NG2576
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m705
_journal_paper_doi               10.1107/S1600536809019783
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Tb (C15 H11 O2)3 (C17 H18 N2)]'
_chemical_formula_moiety         'C62 H51 N2 O6 Tb'
_chemical_formula_sum            'C62 H51 N2 O6 Tb'
_chemical_formula_weight         1078.97
_chemical_name_systematic
;
Tris(dibenzoylmethanido-\k^2^<i>O</i>,<i>O</i>')[(6<i>R</i>,8<i>R</i>)-(-)-
7,7-dimethyl-3-(2-pyridyl)-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-
\k^2^<i>N</i>,<i>N</i>']terbium(III)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 92.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5158(19)
_cell_length_b                   20.790(4)
_cell_length_c                   12.769(3)
_cell_measurement_reflns_used    11553
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.20
_cell_volume                     2523.8(9)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       \w
_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  0.0897
_diffrn_reflns_av_sigmaI/netI    0.1255
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19632
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_T_max  0.6372
_exptl_absorpt_correction_T_min  0.5237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.221
_refine_ls_abs_structure_details 'Flack (1983), 3779 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.008(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8346
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+1.367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                5624
_reflns_number_total             8346
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2576.cif
_cod_data_source_block           I
_cod_original_cell_volume        2523.7(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2222404
_cod_database_fobs_code          2222404