Hydrothermal Synthesis and Crystal Structure of Two New Hydrated Alkaline Earth Metal Borates Sr3B6O11(OH)2 and Ba3B6O11(OH)2
Carla Heyward; Colin McMillen; Joseph Kolis; Inorganic Chemistry 51 (2012) 3956–3962; doi:10.1021/ic202316t

data_4328763
_publ_section_title
;
 Hydrothermal Synthesis and Crystal Structure of Two New Hydrated Alkaline
 Earth Metal Borates Sr3B6O11(OH)2 and Ba3B6O11(OH)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3956
_journal_page_last               3962
_journal_paper_doi               10.1021/ic202316t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'B6 Ba3 H2 O13'
_chemical_formula_weight         686.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_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                 90.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9580(14)
_cell_length_b                   7.0240(14)
_cell_length_c                   11.346(2)
_cell_measurement_reflns_used    4589
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.90
_cell_volume                     554.51(18)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 1999)'
_computing_publication_material  'SHELXTL (Bruker-AXS, 1999)'
_computing_structure_refinement  'SHELXTL (Bruker-AXS, 1999)'
_computing_structure_solution    'SHELXTL (Bruker-AXS, 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC8S'
_diffrn_measurement_method       '\w 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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4558
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.609
_exptl_absorpt_correction_T_max  0.4841
_exptl_absorpt_correction_T_min  0.2991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.114
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0161(7)
_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   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1940
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.6759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                1919
_reflns_number_total             1940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202316t_si_001_2.cif
_cod_data_source_block           cdm1335pc
_cod_original_cell_volume        554.51(19)
_cod_database_code               4328763