Novel Mixed-Valent (V/VI) Triple Perovskite Ruthenates: Observation of a Complex Low-Temperature Structural and Magnetic Transition
Katharine E. Stitzer; Mark D. Smith; William R. Gemmill; Hans-Conrad zur Loye; Journal of the American Chemical Society 124 (2002) 13877–13885; doi:10.1021/ja0271781

data_4115315
_publ_section_title
;
 Novel Mixed-Valent (V/VI) Triple Perovskite Ruthenates: Observation of a
 Complex Low-Temperature Structural and Magnetic Transition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13877
_journal_page_last               13885
_journal_paper_doi               10.1021/ja0271781
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'Ba3 Li O9 Ru2'
_chemical_formula_weight         765.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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            2
_cell_length_a                   5.7820(2)
_cell_length_b                   5.7820(2)
_cell_length_c                   14.1490(8)
_cell_measurement_reflns_used    2926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.071
_cell_measurement_theta_min      2.880
_cell_volume                     409.65(3)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.624 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5488
_diffrn_reflns_theta_full        40.07
_diffrn_reflns_theta_max         40.07
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    17.832
_exptl_absorpt_correction_T_max  0.6976
_exptl_absorpt_correction_T_min  0.4239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.203
_exptl_crystal_description       needle
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.567
_refine_diff_density_min         -3.103
_refine_diff_density_rms         0.422
_refine_ls_extinction_coef       0.0139(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                468
_reflns_number_total             542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0271781_s1_1.cif
_cod_data_source_block           ks3002bs
_cod_database_code               4115315