Hydrothermal Crystal Growth and Structure Determination of Double Hydroxides LiSb(OH)6, BaSn(OH)6, and SrSn(OH)6.
Mizoguchi, Hiroshi; Bhuvanesh, Nattamai S. P.; Kim, Young-Il; Ohara, Satoshi; Woodward, Patrick M.; Inorganic chemistry 53 (2014) 10570–10577; doi:10.1021/ic5016252

data_4341553
_publ_section_title
;
 Hydrothermal Crystal Growth and Structure Determination of Double
 Hydroxides LiSb(OH)6, BaSn(OH)6, and SrSn(OH)6.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10570
_journal_page_last               10577
_journal_paper_doi               10.1021/ic5016252
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'H6 O6 Sn, Ba'
_chemical_formula_sum            'Ba H6 O6 Sn'
_chemical_formula_weight         358.08
_chemical_name_common            BaSn(OH)6
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-23T15:23:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.205(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3928(2)
_cell_length_b                   6.3440(1)
_cell_length_c                   10.5679(2)
_cell_measurement_reflns_used    1454
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     578.776(19)
_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_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.492386E-1
_diffrn_orient_matrix_UB_12      -0.104825
_diffrn_orient_matrix_UB_13      0.22475E-2
_diffrn_orient_matrix_UB_21      0.244609E-1
_diffrn_orient_matrix_UB_22      0.148133E-1
_diffrn_orient_matrix_UB_23      0.155014
_diffrn_orient_matrix_UB_31      -0.671398E-1
_diffrn_orient_matrix_UB_32      -0.759815E-1
_diffrn_orient_matrix_UB_33      0.178554E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            17297
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.46
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    11.029
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.383
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00479(12)
_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   1.158
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.9485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0329
_reflns_number_gt                1099
_reflns_number_total             1329
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5016252_si_002.cif
_cod_data_source_block           Woodward1097
_cod_original_cell_volume        578.775(19)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4341553