Hexakis(antipyrine-<i>O</i>)terbium(III) triiodide at 160K: confirmation of a centrosymmetric structure for a brilliantly triboluminescent complex
Clegg, William; Bourhill, Grant; Sage, Ian; Acta Crystallographica Section E 58 (2002) m159–m161; doi:10.1107/S1600536802005093

data_2201141
_publ_section_title
;
 Hexakis(antipyrine-<i>O</i>)terbium(III) triiodide at 160K:
 confirmation of a centrosymmetric structure for a brilliantly
 triboluminescent complex
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m159
_journal_page_last               m161
_journal_paper_doi               10.1107/S1600536802005093
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Tb (C11 H12 N2 O)6] I3'
_chemical_formula_moiety         'C66 H72 N12 O6 Tb1 3+, 3 I 1-'
_chemical_formula_sum            'C66 H72 I3 N12 O6 Tb'
_chemical_formula_weight         1668.98
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_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            3
_cell_length_a                   13.7474(3)
_cell_length_b                   13.7474(3)
_cell_length_c                   31.9658(14)
_cell_measurement_reflns_used    12573
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      3.0
_cell_volume                     5231.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997b)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            15672
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         28.9
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.766
_refine_ls_extinction_coef       0.00009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0204P)^2^+8.1659P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0474
_reflns_number_gt                2692
_reflns_number_total             2945
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6149.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2201141
_cod_database_fobs_code          2201141