Associating Borate and Silicate Chemistry by Extreme Conditions: High-Pressure Synthesis, Crystal Structure, and Properties of the New Borates RE~3~B~5~O~12~ (RE = Er–Lu)
Emme, Holger; Valldor, Martin; Pöttgen, Rainer; Huppertz, Hubert; Chemistry of Materials 17 (2005) 2707–2715; doi:10.1021/cm047741+

data_1100926
_publ_section_title
;
 Associating Borate and Silicate Chemistry by Extreme Conditions:
 High-Pressure Synthesis, Crystal Structure, and Properties of
 the New Borates RE~3~B~5~O~12~ (RE = Er--Lu)
;
_journal_coden_ASTM              CMATEX
_journal_issue                   10
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2707
_journal_page_last               2715
_journal_paper_doi               10.1021/cm047741+
_journal_volume                  17
_journal_year                    2005
_chemical_formula_moiety         'B5 O12 Tm3'
_chemical_formula_sum            'B5 O12 Tm3'
_chemical_formula_weight         752.84
_chemical_name_common            Trituliumpentaborate
_chemical_name_systematic        Trituliumpentaborate
_space_group_IT_number           53
_space_group_name_Hall           '-P 2ac 2'
_space_group_name_H-M_alt        'P m n a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_contact_author_address
; 
  'Department Chemie und Biochemie
   Ludwig-Maximilians-Universitaet Muenchen
   Butenandtstrasse 5-13 (Haus D)
   81377 Muenchen
   Germany' 
;
_audit_contact_author_email      huh@cup.uni-muenchen.de
_audit_contact_author_fax        '+49 (0)89 2180 77440'
_audit_contact_author_phone      '+49 (0)89 2180 77442'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.820(3)
_cell_length_b                   4.6019(9)
_cell_length_c                   12.477(3)
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.85
_cell_measurement_theta_min      4.40
_cell_volume                     736.1(3)
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'profile data from \f/\w-scans'
_diffrn_radiation_collimation    0.5
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8905
_diffrn_reflns_theta_full        32.92
_diffrn_reflns_theta_max         32.92
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    35.932
_exptl_absorpt_correction_T_max  0.2821
_exptl_absorpt_correction_T_min  0.1628
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Herrendorf,B\"arnighausen,HABITUS, 1993/1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.793
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.171
_refine_diff_density_min         -5.779
_refine_diff_density_rms         0.805
_refine_ls_extinction_coef       0.0043(2)
_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   0.814
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                751
_reflns_number_total             1412
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4000576
_cod_data_source_file            cm047741+si20041223_064526.cif
_cod_data_source_block           Tm3B5O12
_cod_original_sg_symbol_H-M      Pmna
_cod_database_code               1100926