#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/95/2239529.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_2239529
loop_
_publ_author_name
'Tambornino, Frank'
'Bielec, Philipp'
'Hoch, Constantin'
_publ_section_title
;
 Redetermination of [EuCl₂(H₂O)₆]Cl
;
_journal_coeditor_code           WM5012
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i27
_journal_paper_doi               10.1107/S1600536814010307
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Eu Cl2 (H2 O)6] Cl'
_chemical_formula_moiety         'H12 Cl2 Eu O6 +, Cl -'
_chemical_formula_sum            'Cl3 Eu H12 O6'
_chemical_formula_weight         366.41
_chemical_name_common
;
Europium(III) chloride hexahydrate
;
_chemical_name_systematic
;
Hexaaquadichloridoeuropium(III) chloride
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.653(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6438(12)
_cell_length_b                   6.5322(10)
_cell_length_c                   7.929(3)
_cell_measurement_reflns_used    13548
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5
_cell_volume                     498.5(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe IPDS I'
_diffrn_measurement_method       'φ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13401
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    3.743
_exptl_absorpt_correction_T_max  0.5095
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MulScanAbs in PLATON; Spek, 2009)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'stretched cuboid'
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.773
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0150
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0323
_reflns_number_gt                1653
_reflns_number_total             1762
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL [EuCl2(H2O)6]Cl - IPDSAg - 06.03.2014
TITL P2/n AbsCorr, Tidy - fertig
CELL   0.56083    9.6438    6.5322    7.9286    90.000    93.653    90.000
ZERR 2           0.0012    0.0010    0.0030     0.000     0.013     0.000
LATT 1
SYMM -x+1/2,y,-z+1/2
SFAC   Eu  Cl   O   H
UNIT 2 6 12 24
ACTA
OMIT 0 51
FMAP 2
MERG 4
PLAN 50
L.S. 10
BOND
BOND $H
BIND O1 H1
BIND O1 H2
BIND O1 H3
BIND O1 H4
BIND O1 H5
BIND O1 H6
BIND O2 H1
BIND O2 H2
BIND O2 H3
BIND O2 H4
BIND O2 H5
BIND O2 H6
BIND O3 H1
BIND O3 H2
BIND O3 H3
BIND O3 H4
BIND O3 H5
BIND O3 H6
HTAB
WGHT    0.0172
FVAR       0.72976   1.20850
EU    1    0.750000    0.150918    0.250000    10.50000    0.01398    0.01346 =
         0.01244    0.00000   -0.00293    0.00000
CL1   2    0.441556    0.165321    0.760100    11.00000    0.02417    0.02396 =
         0.02861    0.00198   -0.00541   -0.00652
CL2   2    0.750000    0.623870    0.750000    10.50000    0.02974    0.03053 =
         0.02350    0.00000   -0.00328    0.00000
O1    3    0.854270    0.425553    0.087245    11.00000    0.03678    0.02290 =
         0.02143    0.00384   -0.00845   -0.00999
O2    3    0.781641    0.048385    0.956146    11.00000    0.03361    0.02769 =
         0.01748   -0.00389   -0.00012   -0.00470
O3    3    0.560545    0.300161    0.106035    11.00000    0.02496    0.03170 =
         0.02497   -0.00276   -0.01132    0.00670
H1    4    0.827114    0.453503    0.001378    11.00000   20.04195
H2    4    0.845833    0.084227    0.902419    11.00000   20.02866
H3    4    0.766364   -0.062923    0.932574    11.00000   20.04778
H4    4    0.551193    0.265246    0.020129    11.00000   20.04268
H5    4    0.880620    0.520143    0.128913    11.00000   20.03313
H6    4    0.491286    0.318732    0.151702    11.00000   20.03679
HKLF 4
REM  P2/n AbsCorr, Tidy - fertig
REM R1 =  0.0150 for   1653 Fo > 4sig(Fo)  and  0.0180 for all   1762 data
REM     66 parameters refined using      0 restraints
END
WGHT      0.0172      0.0000
REM Highest difference peak  0.633,  deepest hole -0.773,  1-sigma level  0.103
Q1    1   0.8029  0.0979  0.2000  11.00000  0.05    0.63
Q2    1   0.8269  0.1808  0.2219  11.00000  0.05    0.63
Q3    1   0.3968  0.1576  0.8115  11.00000  0.05    0.42
Q4    1   0.4214  0.1126  0.8544  11.00000  0.05    0.41
Q5    1   0.8038  0.3227  0.1448  11.00000  0.05    0.38
Q6    1   0.2500  0.2564  0.7500  10.50000  0.05    0.36
Q7    1   0.3420  0.2066  0.8535  11.00000  0.05    0.35
Q8    1   0.6714  0.0202  0.2085  11.00000  0.05    0.35
Q9    1   0.4790  0.2522  0.6634  11.00000  0.05    0.34
Q10   1   0.4371  0.1574  0.6981  11.00000  0.05    0.34
;
_cod_data_source_file            wm5012sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        498.4(2)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2239529
_cod_database_fobs_code          2239529
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
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
Eu Eu1 0.7500 0.150918(18) 0.2500 0.01345(3) Uani d S 1 2
Cl Cl1 0.44156(5) 0.16532(7) 0.76010(6) 0.02588(9) Uani d . 1 1
Cl Cl2 0.7500 0.62387(11) 0.7500 0.02813(13) Uani d S 1 2
O O1 0.85427(18) 0.4256(2) 0.0872(2) 0.0275(3) Uani d . 1 1
O O2 0.78164(18) 0.0484(2) 0.9561(2) 0.0263(3) Uani d . 1 1
O O3 0.56055(17) 0.3002(2) 0.1060(2) 0.0278(3) Uani d . 1 1
H H1 0.827(4) 0.454(6) 0.001(5) 0.051(4) Uiso d . 1 1
H H2 0.846(3) 0.084(5) 0.902(4) 0.035(3) Uiso d . 1 1
H H3 0.766(4) -0.063(7) 0.933(5) 0.058(5) Uiso d . 1 1
H H4 0.551(4) 0.265(6) 0.020(5) 0.052(5) Uiso d . 1 1
H H5 0.881(4) 0.520(5) 0.129(5) 0.040(3) Uiso d . 1 1
H H6 0.491(4) 0.319(6) 0.152(5) 0.044(4) Uiso 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
Eu1 0.01398(5) 0.01346(5) 0.01244(6) 0.000 -0.00293(3) 0.000
Cl1 0.02417(18) 0.02396(18) 0.0286(2) -0.00652(16) -0.00541(16) 0.00198(17)
Cl2 0.0297(3) 0.0305(3) 0.0235(3) 0.000 -0.0033(2) 0.000
O1 0.0368(8) 0.0229(6) 0.0214(8) -0.0100(6) -0.0085(6) 0.0038(5)
O2 0.0336(7) 0.0277(7) 0.0175(7) -0.0047(6) -0.0001(6) -0.0039(5)
O3 0.0250(6) 0.0317(7) 0.0250(8) 0.0067(5) -0.0113(6) -0.0028(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Eu Eu -0.3977 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0000 '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'
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Eu1 O1 H1 . . . 122(3) n
Eu1 O1 H1 . 6_555 6_555 122(3) n
Eu1 O1 H5 . . . 121(3) n
Eu1 O1 H5 . 6_555 6_555 121(3) n
Eu1 O2 H2 1_556 . . 124(3) n
Eu1 O2 H2 1_556 6_555 6_655 124(3) n
Eu1 O2 H3 1_556 . . 117(3) n
Eu1 O2 H3 1_556 6_555 6_655 117(3) n
Eu1 O3 H4 . . . 112(3) n
Eu1 O3 H4 . 6_555 6_555 112(3) n
Eu1 O3 H6 . . . 120(3) n
Eu1 O3 H6 . 6_555 6_655 120(3) n
O1 Eu1 O1 2_655 . . 86.43(9) n
O1 Eu1 O2 2_655 . 1_554 140.68(5) n
O1 Eu1 O2 . . 1_554 67.83(6) n
O1 Eu1 Cl1 2_655 . 3_656 105.35(5) n
O1 Eu1 Cl1 . . 3_656 145.35(4) n
O2 Eu1 O2 1_554 . 2_656 148.45(8) n
O2 Eu1 Cl1 1_554 . 3_656 83.83(4) n
O2 Eu1 Cl1 2_656 . 3_656 72.65(4) n
O3 Eu1 O1 2_655 . 2_655 76.70(6) n
O3 Eu1 O1 . . 2_655 67.31(6) n
O3 Eu1 O2 2_655 . 1_554 116.15(7) n
O3 Eu1 O2 . . 1_554 77.82(6) n
O3 Eu1 O3 2_655 . . 130.01(8) n
O3 Eu1 Cl1 2_655 . 3_656 146.64(4) n
O3 Eu1 Cl1 . . 3_656 78.18(5) n
Cl1 Eu1 Cl1 3_656 . 4_655 83.51(2) n
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
Eu1 O1 . 2.4618(15) yes
Eu1 O1 2_655 2.4618(16) no
Eu1 O2 1_554 2.4620(18) yes
Eu1 O2 2_656 2.4620(18) no
Eu1 O3 . 2.3078(16) yes
Eu1 O3 2_655 2.3078(15) no
Eu1 Cl1 3_656 2.7690(12) yes
Eu1 Cl1 4_655 2.7690(12) no
O1 H1 . 0.74(4) no
O1 H5 . 0.74(4) no
O2 H3 . 0.76(4) n
O2 H2 . 0.81(3) n
O3 H4 . 0.72(4) n
O3 H6 . 0.79(4) n
Cl1 H2 6_555 2.535(4) n
Cl1 H4 5_455 2.3535(4) n
Cl1 H5 4_566 2.36(3) no
Cl2 H1 2_655 2.36(4) no
Cl2 H3 1_565 2.5071(4) no
Cl2 H6 3_666 2.53(4) n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 Cl2 . . 1_554 0.74(4) 2.36(4) 3.081(2) 166.08 y
O2 H2 Cl1 . . 2_656 0.81(3) 2.54(3) 3.351(2) 174.97 y
O2 H3 Cl2 . . 1_545 0.76(4) 2.51(4) 3.2234(19) 157.37 y
O3 H4 Cl1 . . 1_554 0.72(4) 2.35(4) 3.036(2) 160.44 y
O1 H5 Cl1 6_556 4_566 . 0.74(2) 2.36(3) 3.095(2) 173.89 y
O3 H6 Cl2 . . 3_666 0.79(4) 2.53(4) 3.310(2) 170.66 y
