#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/53/2005340.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_2005340
loop_
_publ_author_name
'Chevrier, G.'
'Goukassov, A.'
_publ_section_title
;
 The Hydrogen-Bonding System in Deuterated Copper Fluorosilicate
 Tetrahydrate: a Neutron Diffraction Study
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2121
_journal_page_last               2123
_journal_paper_doi               10.1107/S0108270196003927
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'Cu Si F6 , 4D2 O'
_chemical_formula_moiety         'Cu F6 Si , 4D2 O '
_chemical_formula_sum            'Cu D8 F6 O4 Si'
_chemical_formula_weight         285.7
_chemical_name_systematic
' Deuterated copper flurosilicate tetrahydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 105.16(1)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   5.33(2)
_cell_length_b                   9.60(5)
_cell_length_c                   7.18(5)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    296
_cell_measurement_theta_max      36.5
_cell_measurement_theta_min      12.5
_cell_volume                     355(3)
_diffrn_measurement_device       '4-circle 6T2 at Orphee reactor'
_diffrn_measurement_method
; unique set between 45 and 120°. ω scans between 2θ = 2 and 45°, ω--θ
scans between 2θ = 45 and 60° and ω--2θ scans between 2θ = 60 and 120°
;
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.520(2)
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            759
_diffrn_reflns_theta_max         60.0
_diffrn_standards_decay_%        <0.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.0683(estimated)
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.679
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             10.891
_exptl_crystal_size_max          4.00
_exptl_crystal_size_mid          3.50
_exptl_crystal_size_min          3.00
_refine_diff_density_max         '0.65 fm \%A^-3^'
_refine_diff_density_min         '-0.75 fm \%A^-3^'
_refine_ls_extinction_coef       ' G~eq~ = 0.113(5)'
_refine_ls_extinction_method
' type 2 anisotropic extinction (Coppens & Hamilton, 1970)'
_refine_ls_goodness_of_fit_obs   5.713
_refine_ls_hydrogen_treatment    'D-atoms refined'
_refine_ls_number_parameters     101
_refine_ls_number_reflns         433
_refine_ls_R_factor_obs          0.0647
_refine_ls_shift/esd_max         0.00007
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details     'w = 1/σ²(F²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0465
_reflns_number_observed          433
_reflns_number_total             571
_reflns_observed_criterion       F^2^>2.5\s(F^2^)
_cod_data_source_file            br1141.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F^2^)' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/\s^2^(F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        354.(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'Cu D8 F6 Si O4'
_cod_database_code               2005340
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,1/2+y,1/2-z
x,1/2-y,1/2+z
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
_atom_site_aniso_type_symbol
Cu .020(2) .017(2) .020(2) .0003(17) .0134(17) .0013(16) Cu
Si .004(3) .011(3) .010(3) -.001(3) .003(2) -.000(3) Si
F1 .029(2) .022(2) .037(3) -.0100(19) .018(2) .0025(18) F
F2 .037(3) .023(2) .024(2) -.0002(18) .0193(19) -.0053(18) F
F3 .030(3) .038(3) .021(3) .0033(17) .0008(18) .0012(17) F
O1 .028(3) .022(3) .030(3) -.005(2) .013(2) .002(2) O
O2 .024(2) .029(3) .023(3) .008(2) .0145(19) -.002(2) O
D11 .043(4) .035(3) .040(4) -.004(3) .029(3) -.003(3) D
D12 .051(4) .036(4) .043(5) -.021(3) .023(3) -.012(3) D
D21 .050(3) .034(3) .034(4) .013(3) .027(3) -.000(3) D
D22 .042(3) .020(3) .042(4) .012(3) .018(3) .007(3) D
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_type_symbol
Cu 0.0000 0.0000 0.0000 0.0176(9) Uani Cu
Si 0.5000 0.0000 0.5000 0.0083(13) Uani Si
F1 0.7311(7) 0.1050(4) 0.4529(6) 0.0274(11) Uani F
F2 0.3893(8) 0.1334(4) 0.6110(5) 0.0255(10) Uani F
F3 0.2981(7) 0.0471(4) 0.2921(5) 0.0305(11) Uani F
O1 0.1260(8) 0.1582(5) -0.1203(7) 0.0257(12) Uani O
O2 -0.2393(7) 0.1269(5) 0.0790(7) 0.0236(12) Uani O
D11 0.2204(10) 0.1406(5) -0.2153(8) 0.0361(15) Uani D
D12 0.2198(11) 0.2301(6) -0.0398(8) 0.0414(17) Uani D
D21 -0.2500(10) 0.1226(5) 0.2092(10) 0.0364(15) Uani D
D22 -0.2427(10) 0.2232(5) 0.0437(7) 0.0336(16) Uani D
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu 0.7689 0.0000 ' Delapalme (1985)'
Si 0.4150 0.0000 ' Delapalme (1985)'
F 0.5650 0.0000 ' Delapalme (1985)'
D 0.6670 0.0000 ' Delapalme (1985)'
O 0.5805 0.0000 ' Delapalme (1985)'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu O1 1_555 180.0 no
O2 Cu O2 1_555 180.0 no
F3 Cu F3 1_555 180.0 no
O1 Cu O2 1_555 88.3(5) yes
O1 Cu O2 2_555 91.7(7) yes
O1 Cu F3 1_555 90.8(8) yes
O1 Cu F3 2_555 89.2(6) yes
O2 Cu F3 1_555 87.8(6) yes
O2 Cu F3 2_555 92.2(8) yes
F1 Si F1 1_555 180.0 no
F2 Si F2 1_555 180.0 no
F3 Si F3 1_555 180.0 no
F1 Si F2 1_555 90.3(6) yes
F1 Si F2 2_656 89.7(7) yes
F1 Si F3 1_555 89.6(6) yes
F1 Si F3 2_656 90.4(7) yes
F2 Si F3 1_555 89.6(8) yes
F2 Si F3 2_656 90.4(6) yes
D11 O1 D12 1_555 105.5(13) yes
D21 O2 D22 1_555 107.4(15) yes
Cu O1 D11 1_555 118.8(12) no
Cu O1 D12 1_555 118.8(13) no
Cu O2 D21 1_555 118.0(12) no
Cu O2 D22 1_555 119.6(13) no
Cu F3 Si 1_555 153(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O1 1_555 1_555 1.951(8) yes
Cu O2 1_555 1_555 1.952(7) yes
Cu F3 1_555 1_555 2.320(13) yes
O1 O2 1_555 1_555 2.718(11) no
O1 O2 1_555 2_555 2.800(15) no
O1 F3 1_555 1_555 3.05(2) no
O2 F3 1_555 1_555 2.974(12) no
O1 F3 1_555 2_555 3.009(11) no
O2 F3 1_555 2_555 3.089(17) no
Si F1 1_555 1_555 1.693(6) yes
Si F2 1_555 1_555 1.693(7) yes
Si F3 1_555 1_555 1.658(10) yes
F1 F2 1_555 1_555 2.401(9) no
F1 F2 1_555 2_656 2.388(12) no
F1 F3 1_555 1_555 2.361(10) no
F2 F3 1_555 1_555 2.362(15) no
F1 F3 1_555 2_656 2.378(12) no
F2 F3 1_555 2_656 2.378(9) no
O1 D11 1_555 1_555 0.962(8) yes
O1 D12 1_555 1_555 0.953(8) yes
O1 D22 1_555 1_555 2.617(10) no
O2 D21 1_555 1_555 0.952(10) yes
O2 D22 1_555 1_555 0.957(8) yes
O2 D12 1_555 1_555 2.965(12) no
