#------------------------------------------------------------------------------
#$Date: 2023-04-10 20:11:16 +0300 (Mon, 10 Apr 2023) $
#$Revision: 282541 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/21/2212176.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212176
loop_
_publ_author_name
'Uchida, Hinako'
'Downs, Robert T.'
'Thompson, Richard M.'
_publ_section_title
;
 Reinvestigation of eakerite,
 Ca₂SnAl₂Si₆O₁₈(OH)₂·2H₂O: H-atom positions by
 single-crystal X-ray diffraction and correlation with Raman
 spectroscopic data
;
_journal_coeditor_code           HB2229
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i47
_journal_page_last               i49
_journal_paper_doi               10.1107/S1600536807002000
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Ca2 Sn Al2 Si6 O18 (O H)2, 2H2 O'
_chemical_formula_moiety         'Al2 H2 O20 Si6 Sn, 2(H2 O), 2(Ca)'
_chemical_formula_sum            'Al2 Ca2 H6 O22 Si6 Sn'
_chemical_formula_weight         779.40
_chemical_name_common            eakerite
_chemical_name_systematic
;
dicalcium tin dialuminosilicate dihydroxide dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 101.293(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.8202(5)
_cell_length_b                   7.6963(3)
_cell_length_c                   7.4449(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.8
_cell_measurement_theta_min      2.8
_cell_volume                     888.92(6)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'XTALDRAW (Downs & Hall-Wallace, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2 CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24042
_diffrn_reflns_theta_full        39.79
_diffrn_reflns_theta_max         39.79
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         5432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0267
_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/[σ²(Fo²)+(0.0266P)²+0.728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                4547
_reflns_number_total             5432
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2229.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2212176
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Sn Sn 0.0000 0.0000 0.0000 0.00651(3) Uani d S 1
Ca Ca 0.300365(19) 0.31104(4) 0.00225(4) 0.00876(5) Uani d . 1
Si Si1 0.45531(5) 0.16988(5) 0.71316(6) 0.00629(7) Uani d . 1
Si Si2 0.16629(3) 0.14507(3) 0.30892(6) 0.00636(7) Uani d . 1
Si Si3 0.49337(3) 0.21803(5) 0.33559(6) 0.00616(7) Uani d . 1
Al Al 0.27068(3) 0.02215(6) 0.68283(6) 0.00660(8) Uani d . 1
O O1 0.01960(7) 0.19958(15) -0.16104(16) 0.01086(19) Uani d . 1
O O2 0.50547(8) -0.01656(15) 0.72868(18) 0.0129(2) Uani d . 1
O O3 0.21455(7) 0.30912(14) 0.23632(15) 0.00992(18) Uani d . 1
O O4 0.12298(7) 0.02274(14) 0.14054(17) 0.00820(17) Uani d . 1
O O5 0.36271(7) 0.14553(15) -0.23084(15) 0.00947(18) Uani d . 1
O O6 0.44680(7) 0.33291(15) 0.16450(15) 0.00886(18) Uani d . 1
O O7 0.23642(7) 0.03515(16) 0.44934(15) 0.01008(19) Uani d . 1
O O8 0.31937(8) 0.00282(18) 0.1518(2) 0.0146(2) Uani d . 1
O O9 0.20206(7) 0.10401(16) -0.18049(16) 0.01123(19) Uani d . 1
O O10 0.43954(7) 0.22846(17) 0.49792(15) 0.0120(2) Uani d . 1
O O11 0.09213(7) 0.22090(16) 0.41285(15) 0.01080(19) Uani d . 1
H H81 0.316(3) 0.002(5) 0.239(6) 0.067(15) Uiso d . 1
H H82 0.363(2) -0.025(4) 0.140(4) 0.029(8) Uiso d . 1
H H9 0.150(2) 0.116(5) -0.204(5) 0.046(9) Uiso d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Sn O1 3 . 180.0 ?
O1 Sn O4 . . 89.85(5) ?
O1 Sn O4 3 . 90.15(5) ?
O1 Sn O4 . 3 90.15(5) ?
O1 Sn O4 3 3 89.85(5) ?
O4 Sn O4 . 3 180.0 ?
O1 Sn O6 . 4_545 89.64(5) ?
O1 Sn O6 3 4_545 90.36(5) ?
O4 Sn O6 3 2_455 84.18(4) ?
O4 Sn O6 . 2_455 95.83(4) ?
O1 Sn O6 . 2_455 90.36(5) ?
O1 Sn O6 3 2_455 89.64(5) ?
O4 Sn O6 3 4_545 95.82(4) ?
O4 Sn O6 . 4_545 84.17(4) ?
O6 Sn O6 . 3 180.0 ?
O6 Ca O4 . 4 69.73(4) ?
O6 Ca O3 . . 105.16(4) ?
O4 Ca O3 4 . 136.85(4) ?
O6 Ca O9 . . 140.52(4) ?
O4 Ca O9 4 . 121.16(4) ?
O3 Ca O9 . . 90.65(4) ?
O6 Ca O8 . 4 139.53(4) ?
O4 Ca O8 4 4 78.40(4) ?
O3 Ca O8 . 4 81.46(5) ?
O9 Ca O8 . 4 77.70(4) ?
O6 Ca O5 . . 84.96(4) ?
O4 Ca O5 4 . 74.74(4) ?
O3 Ca O5 . . 148.40(4) ?
O9 Ca O5 . . 64.98(4) ?
O8 Ca O5 4 . 110.41(4) ?
O6 Ca O8 . . 80.21(4) ?
O4 Ca O8 4 . 141.18(4) ?
O3 Ca O8 . . 73.77(4) ?
O9 Ca O8 . . 69.70(4) ?
O8 Ca O8 . 4 138.27(3) ?
O5 Ca O8 . . 78.78(4) ?
O6 Ca O9 . 4 78.06(4) ?
O4 Ca O9 4 4 72.48(4) ?
O3 Ca O9 . 4 64.71(4) ?
O9 Ca O9 . 4 140.50(2) ?
O8 Ca O9 4 4 68.83(4) ?
O5 Ca O9 . 4 146.62(4) ?
O8 Ca O9 . 4 125.27(4) ?
O1 Si1 O5 2_556 1_556 115.38(6) ?
O1 Si1 O2 2_556 . 105.47(7) ?
O5 Si1 O2 1_556 . 109.48(7) ?
O1 Si1 O10 2_556 . 111.02(7) ?
O5 Si1 O10 1_556 . 108.28(6) ?
O2 Si1 O10 . . 106.88(7) ?
O7 Si2 O4 . . 109.44(6) ?
O7 Si2 O3 . . 108.44(6) ?
O4 Si2 O3 . . 110.62(6) ?
O7 Si2 O11 . . 110.36(6) ?
O4 Si2 O11 . . 110.00(6) ?
O3 Si2 O11 . . 107.95(6) ?
O6 Si3 O10 . . 109.86(6) ?
O6 Si3 O2 . 3_656 108.78(7) ?
O10 Si3 O2 . 3_656 107.86(7) ?
O6 Si3 O11 . 2 112.42(6) ?
O10 Si3 O11 . 2 109.44(6) ?
O2 Si3 O11 3_656 2 108.35(7) ?
O7 Al O9 . 1_556 117.37(6) ?
O7 Al O3 . 4_546 113.42(6) ?
O9 Al O3 1_556 4_546 101.22(6) ?
O7 Al O5 . 1_556 114.46(6) ?
O9 Al O5 1_556 1_556 99.07(6) ?
O3 Al O5 4_546 1_556 109.69(6) ?
Si1 O1 Sn 2_454 . 132.54(7) ?
Si3 O2 Si1 3_656 . 148.39(9) y
Si2 O3 Al . 4_556 130.99(7) y
Si2 O3 Ca . . 127.91(6) ?
Al O3 Ca 4_556 . 100.79(5) ?
Si2 O4 Sn . . 132.17(6) ?
Si2 O4 Ca . 4_545 124.55(6) ?
Sn O4 Ca . 4_545 103.28(4) ?
Si1 O5 Al 1_554 1_554 134.50(7) y
Si1 O5 Ca 1_554 . 128.43(6) ?
Al O5 Ca 1_554 . 96.78(5) ?
Si3 O6 Sn . 2 129.51(6) ?
Si3 O6 Ca . . 127.47(6) ?
Sn O6 Ca 2 . 102.15(4) ?
Si2 O7 Al . . 136.77(8) y
Ca O8 Ca . 4_545 109.11(5) ?
Ca O8 H81 4_545 . 104(4) ?
Ca O8 H81 . . 114(3) ?
Ca O8 H82 4_545 . 114(2) ?
Ca O8 H82 . . 104(2) ?
H81 O8 H82 . . 111(4) ?
Al O9 Ca 1_554 . 99.16(5) ?
Al O9 Ca 1_554 4_545 93.27(5) ?
Ca O9 Ca . 4_545 110.47(4) ?
Al O9 H9 1_554 . 129(2) ?
Ca O9 H9 . . 124(2) ?
Ca O9 H9 4_545 . 95(2) ?
Si3 O10 Si1 . . 136.01(8) y
Si3 O11 Si2 2_455 . 131.70(8) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn O1 3 2.0096(11) ?
Sn O1 . 2.0096(11) y
Sn O4 . 2.0281(11) y
Sn O4 3 2.0281(11) y
Sn O6 4_545 2.0653(11) ?
Sn O6 2_455 2.0653(11) ?
Ca O6 . 2.3997(11) y
Ca O4 4 2.4001(11) y
Ca O3 . 2.4097(11) y
Ca O9 . 2.4454(12) y
Ca O8 4 2.4962(14) y
Ca O5 . 2.5055(11) y
Ca O8 . 2.6126(14) y
Ca O9 4 2.6203(13) y
Si1 O1 2_556 1.5962(12) y
Si1 O5 1_556 1.6106(11) y
Si1 O2 . 1.6327(12) y
Si1 O10 . 1.6361(12) y
Si2 O7 . 1.6080(12) y
Si2 O4 . 1.6096(11) y
Si2 O3 . 1.6220(12) y
Si2 O11 . 1.6344(12) y
Si3 O6 . 1.6060(11) y
Si3 O10 . 1.6110(12) y
Si3 O2 3_656 1.6238(12) y
Si3 O11 2 1.6251(12) y
Al O7 . 1.7195(12) y
Al O9 1_556 1.7445(12) y
Al O3 4_546 1.7463(12) y
Al O5 1_556 1.7517(12) y
O2 Si3 3_656 1.6239(12) ?
O3 Al 4_556 1.7464(12) ?
O3 Ca . 2.4096(11) ?
O7 Al . 1.7194(12) ?
O8 Ca . 2.6126(14) ?
O8 H81 . 0.67(5) ?
O8 H82 . 0.74(3) ?
O9 Ca 4_545 2.6203(13) ?
O9 H9 . 0.81(3) ?
O10 Si1 . 1.6361(12) ?
O11 Si3 2_455 1.6251(12) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O8 H82 O2 3_656 0.74(3) 2.14(3) 2.7415(18) 138(3)
O8 H81 O7 . 0.66(4) 2.21(5) 2.7981(18) 150(5)
O9 H9 O1 . 0.81(3) 2.24(3) 3.0096(16) 157(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0010472
