Two isostructural triboluminescent lanthanide complexes
Clegg, William; Sage, Ian; Oswald, Iain; Brough, Peter; Bourhill, Grant; e-mail: bgourhill@dera.gov.uk; Acta Crystallographica Section C 56 (2000) 1323–1325; doi:10.1107/S0108270100011641

data_2011577
_publ_section_title
;
 Two isostructural triboluminescent lanthanide complexes
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1323
_journal_page_last               1325
_journal_paper_doi               10.1107/S0108270100011641
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Tb (C11 H19 O2)3 (C7 H10 N2)]'
_chemical_formula_sum            'C40 H67 N2 O6 Tb'
_chemical_formula_weight         830.88
_chemical_name_systematic
;
Tris(1,3-di-t-butyl-propane-1,3-dionato)(4-dimethylaminopyridine)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'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.643(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9465(11)
_cell_length_b                   18.972(2)
_cell_length_c                   11.0469(12)
_cell_measurement_reflns_used    5819
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.50
_cell_volume                     2146.9(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .927
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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     .71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_sigmaI/netI    .0419
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18460
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  .751
_exptl_absorpt_correction_T_min  .551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .18
_refine_diff_density_max         1.238
_refine_diff_density_min         -2.538
_refine_ls_abs_structure_details 'Flack (1983), 4588 Friedel pairs'
_refine_ls_abs_structure_Flack   .019(7)
_refine_ls_extinction_coef       .00062(18)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          .031
_refine_ls_R_factor_gt           .029
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0140P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .054
_reflns_number_gt                9418
_reflns_number_total             9868
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1415.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2011577
_cod_database_fobs_code          2011577