Multianvil High-Pressure Synthesis of Dy4B6O15: The First Oxoborate with Edge-Sharing BO4 Tetrahedra
Hubert Huppertz; Benjamin von der Eltz; Journal of the American Chemical Society 124 (2002) 9376–9377; doi:10.1021/ja017691z

data_4115016
_publ_section_title
;
 Multianvil High-Pressure Synthesis of Dy4B6O15: The First Oxoborate with
 Edge-Sharing BO4 Tetrahedra
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9376
_journal_page_last               9377
_journal_paper_doi               10.1021/ja017691z
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'B6 Dy4 O15'
_chemical_formula_sum            'B6 Dy4 O15'
_chemical_formula_weight         954.86
_chemical_name_common            Dysprosiumborate
_chemical_name_systematic
; 
 Dysprosiumborate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Dr. H. Huppertz'
_audit_contact_author_address
;
  'Department Chemie
   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 7806'
_audit_contact_author_phone      '+49 (0)89 2180 7442'
_audit_creation_date             02-05-12
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.657(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6938(10)
_cell_length_b                   4.3777(10)
_cell_length_c                   18.9304(10)
_cell_measurement_reflns_used    11099
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.154
_cell_measurement_theta_min      2.910
_cell_volume                     962.6(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0841503
_diffrn_orient_matrix_UB_12      -0.0376740
_diffrn_orient_matrix_UB_13      0.0130112
_diffrn_orient_matrix_UB_21      0.0111277
_diffrn_orient_matrix_UB_22      -0.0065661
_diffrn_orient_matrix_UB_23      -0.0515631
_diffrn_orient_matrix_UB_31      0.0144016
_diffrn_orient_matrix_UB_32      0.2252066
_diffrn_orient_matrix_UB_33      0.0006732
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  'vertically mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11351
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         3.51
_diffrn_source_current           75.00
_diffrn_source_power             4.125
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    30.804
_exptl_absorpt_correction_T_max  0.4496
_exptl_absorpt_correction_T_min  0.2000
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.589
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.240
_refine_ls_extinction_coef       0.00107(3)
_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   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0155
_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^)+(0.0000P)^2^+7.9982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0349
_refine_ls_wR_factor_ref         0.0356
_reflns_number_gt                1319
_reflns_number_total             1405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017691z_s1.cif
_cod_data_source_block           c:\dy4b6o15
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4115016
_kl_diffrn_measurement_scan_angle phi/omega-scan
_kl_diffrn_measurement_scan_step_degree 1.3
_kl_diffrn_measurement_scan_time_per_degree 30.0
_kl_diffrn_measurement_detector_distance 30.0