#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/83/2238327.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_2238327
loop_
_publ_author_name
'Gieschen, Tobias'
'Reuter, Hans'
_publ_section_title
;
 Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H₂PO₂)₆],
 with some remarks on the so-called Ge₂(H₂PO₂)₆ structure type
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i44
_journal_paper_doi               10.1107/S1600536813018205
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Ca [Sn (H2 P O2)6]'
_chemical_formula_moiety         'Ca H12 O12 P6 Sn'
_chemical_formula_sum            'Ca H12 O12 P6 Sn'
_chemical_formula_weight         548.69
_chemical_name_systematic
;
Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H₂PO₂)₆], with
some remarks on the so-called Ge₂(H₂PO₂)₆ structure type
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.8619(4)
_cell_length_b                   11.8619(4)
_cell_length_c                   9.8668(4)
_cell_measurement_reflns_used    6570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.86
_cell_volume                     1202.31(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and Mercury
(Macrae et al., 2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω 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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18525
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.4593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0200
_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/[σ²(Fo²)+(0.0229P)²+3.9531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                731
_reflns_number_total             777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cq2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2238327
_cod_database_fobs_code          2238327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_symmetry_multiplicity
Sn Sn1 1.0000 1.0000 0.0000 0.01807(11) Uani d S 1 6
Ca Ca1 1.0000 1.0000 0.5000 0.0192(2) Uani d S 1 6
P P1 0.78540(5) 0.97330(6) 0.22095(6) 0.02205(14) Uani d . 1 1
H H1 0.7214 0.8488 0.1657 0.040(6) Uiso d R 1 1
H H2 0.7073 1.0296 0.2122 0.040(6) Uiso d R 1 1
O O1 0.89193(16) 1.05182(16) 0.11547(15) 0.0244(3) Uani d . 1 1
O O2 0.82943(19) 0.9728(2) 0.36084(18) 0.0408(5) Uani d . 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn1 0.02121(13) 0.02121(13) 0.01179(16) 0.01061(7) 0.000 0.000
Ca1 0.0229(3) 0.0229(3) 0.0117(4) 0.01146(15) 0.000 0.000
P1 0.0205(3) 0.0291(3) 0.0184(3) 0.0138(2) 0.00185(19) 0.0010(2)
O1 0.0300(8) 0.0253(8) 0.0196(7) 0.0150(7) 0.0060(6) 0.0019(6)
O2 0.0325(10) 0.0739(15) 0.0187(8) 0.0286(10) 0.0021(7) 0.0070(8)
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'
P P 0.1023 0.0942 '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
O1 Sn1 O1 11_565 2_765 180.0
O1 Sn1 O1 11_565 12_655 91.49(6)
O1 Sn1 O1 2_765 12_655 88.51(6)
O1 Sn1 O1 11_565 3_675 88.51(6)
O1 Sn1 O1 2_765 3_675 91.49(6)
O1 Sn1 O1 12_655 3_675 180.00(11)
O1 Sn1 O1 11_565 . 88.52(6)
O1 Sn1 O1 2_765 . 91.48(6)
O1 Sn1 O1 12_655 . 88.52(6)
O1 Sn1 O1 3_675 . 91.48(6)
O1 Sn1 O1 11_565 10_775 91.48(6)
O1 Sn1 O1 2_765 10_775 88.52(6)
O1 Sn1 O1 12_655 10_775 91.48(6)
O1 Sn1 O1 3_675 10_775 88.52(6)
O1 Sn1 O1 . 10_775 180.0
O2 Ca1 O2 10_776 11_566 88.81(7)
O2 Ca1 O2 10_776 2_765 91.19(7)
O2 Ca1 O2 11_566 2_765 180.0
O2 Ca1 O2 10_776 12_656 88.81(7)
O2 Ca1 O2 11_566 12_656 88.81(7)
O2 Ca1 O2 2_765 12_656 91.19(7)
O2 Ca1 O2 10_776 3_675 91.19(7)
O2 Ca1 O2 11_566 3_675 91.19(7)
O2 Ca1 O2 2_765 3_675 88.81(7)
O2 Ca1 O2 12_656 3_675 180.0
O2 Ca1 O2 10_776 . 180.0
O2 Ca1 O2 11_566 . 91.19(7)
O2 Ca1 O2 2_765 . 88.81(7)
O2 Ca1 O2 12_656 . 91.19(7)
O2 Ca1 O2 3_675 . 88.81(7)
O2 P1 O1 . . 116.70(11)
O2 P1 H1 . . 111.6
O1 P1 H1 . . 103.0
O2 P1 H2 . . 112.5
O1 P1 H2 . . 102.1
H1 P1 H2 . . 110.1
P1 O1 Sn1 . . 130.45(10)
P1 O2 Ca1 . . 146.56(12)
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
Sn1 O1 11_565 2.0265(15) ?
Sn1 O1 2_765 2.0265(15) ?
Sn1 O1 12_655 2.0266(16) ?
Sn1 O1 3_675 2.0266(16) ?
Sn1 O1 . 2.0266(15) yes
Sn1 O1 10_775 2.0266(16) ?
Ca1 O2 10_776 2.3302(19) ?
Ca1 O2 11_566 2.3302(19) ?
Ca1 O2 2_765 2.3302(19) ?
Ca1 O2 12_656 2.3302(19) ?
Ca1 O2 3_675 2.3302(19) ?
Ca1 O2 . 2.3303(19) yes
P1 O2 . 1.4768(18) yes
P1 O1 . 1.5397(16) yes
P1 H1 . 1.3900 ?
P1 H2 . 1.3900 ?
