#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/35/2013524.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_2013524
loop_
_publ_author_name
'Deluzet, André'
'Guillou, Olivier'
_publ_section_title
;
 catena-Poly[[bis[pentaaquaerbium(III)]-μ-benzenehexacarboxylato]
 tetrahydrate]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m277
_journal_page_last               m279
_journal_paper_doi               10.1107/S010827010300341X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Er2 (C12 O12) (H2 O)10] , 4H2 O'
_chemical_formula_moiety         'C12 H20 Er2 O22 , 4H2 O'
_chemical_formula_sum            'C12 H28 Er2 O26'
_chemical_formula_weight         922.86
_chemical_name_common            'erbium mellitate'
_chemical_name_systematic
;catena-Poly[[bis[pentaaquaerbium(III)]-μ-benzenehexacarboxylato]
 tetrahydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 100.3390(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.44990(10)
_cell_length_b                   9.2595(2)
_cell_length_c                   16.2911(4)
_cell_measurement_reflns_used    8641
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     1253.95(4)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'DIAMOND (Brandeburg, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17561
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.760
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Alcock, 1970)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.48
_refine_diff_density_min         -2.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.037
_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)+(0.0438P)²+4.4981P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.085
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                2884
_reflns_number_total             3648
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ta1398.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013524
_cod_database_fobs_code          2013524
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Er 0.44714(2) 0.09373(2) 0.166967(13) 0.01942(9) Uani d . 1 . . Er
O1 0.3852(5) -0.1071(4) 0.0788(3) 0.0305(9) Uani d . 1 . . O
O2 0.2436(4) -0.0332(5) 0.2225(3) 0.0327(9) Uani d . 1 . . O
O3 0.5629(5) 0.3262(5) 0.1793(3) 0.0432(11) Uani d . 1 . . O
O4 0.5821(6) -0.1022(6) 0.2418(4) 0.0666(19) Uani d . 1 . . O
O5 0.4831(6) 0.1657(8) 0.3068(3) 0.0645(17) Uani d . 1 . . O
O11 0.2213(4) 0.2442(4) 0.1606(2) 0.0251(8) Uani d . 1 . . O
O12 -0.0095(5) 0.3468(5) 0.1020(3) 0.0378(10) Uani d . 1 . . O
C12 0.0892(5) 0.2457(5) 0.1092(3) 0.0190(10) Uani d . 1 . . C
C11 0.0474(5) 0.1155(5) 0.0537(3) 0.0162(9) Uani d . 1 . . C
O21 0.3902(4) 0.1855(4) 0.0308(2) 0.0224(8) Uani d . 1 . . O
O22 0.2539(4) 0.2518(4) -0.0932(2) 0.0297(9) Uani d . 1 . . O
C22 0.2662(5) 0.1823(5) -0.0270(3) 0.0184(9) Uani d . 1 . . C
C21 0.1282(5) 0.0886(5) -0.0130(3) 0.0154(9) Uani d . 1 . . C
O31 0.3177(4) -0.0687(4) -0.1181(2) 0.0274(8) Uani d . 1 . . O
O32 0.0834(5) -0.0705(5) -0.2082(2) 0.0356(10) Uani d . 1 . . O
C32 0.1670(5) -0.0595(5) -0.1375(3) 0.0191(9) Uani d . 1 . . C
C31 0.0804(5) -0.0276(5) -0.0658(3) 0.0156(9) Uani d . 1 . . C
O1W 0.1943(11) -0.3524(13) 0.0654(7) 0.037(2) Uani d P 0.50 . . O
O2W 0.291(4) -0.3798(18) 0.110(2) 0.193(16) Uani d P 0.50 . . O
O3W 0.671(6) -0.531(4) 0.0462(10) 0.433(7) Uani d P 0.50 . . O
O4W 0.5025(13) -0.4638(13) 0.0816(10) 0.073(4) Uani d P 0.50 . . O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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
O31 Er O5 3_655 . 113.56(16) n
O31 Er O21 3_655 . 75.54(13) n
O5 Er O21 . . 141.9(2) n
O31 Er O11 3_655 . 142.76(14) n
O5 Er O11 . . 80.61(18) n
O21 Er O11 . . 73.49(13) n
O31 Er O1 3_655 . 79.55(14) n
O5 Er O1 . . 142.7(2) n
O21 Er O1 . . 73.94(14) n
O11 Er O1 . . 110.62(13) n
O31 Er O3 3_655 . 75.44(14) n
O5 Er O3 . . 71.2(2) n
O21 Er O3 . . 76.19(15) n
O11 Er O3 . . 77.50(14) n
O1 Er O3 . . 144.88(15) n
O31 Er O4 3_655 . 74.43(17) n
O5 Er O4 . . 75.5(3) n
O21 Er O4 . . 139.9(2) n
O11 Er O4 . . 142.33(17) n
O1 Er O4 . . 75.0(2) n
O3 Er O4 . . 120.19(19) n
O31 Er O2 3_655 . 144.37(14) n
O5 Er O2 . . 75.40(17) n
O21 Er O2 . . 119.80(12) n
O11 Er O2 . . 71.02(13) n
O1 Er O2 . . 75.27(15) n
O3 Er O2 . . 137.06(16) n
O4 Er O2 . . 74.97(16) n
C12 O11 Er . . 130.3(3) n
O12 C12 O11 . . 124.4(5) n
O12 C12 C11 . . 117.6(4) n
O11 C12 C11 . . 118.0(4) n
C31 C11 C21 3 . 120.1(4) n
C31 C11 C12 3 . 119.0(4) n
C21 C11 C12 . . 120.7(4) n
C22 O21 Er . . 133.8(3) n
O22 C22 O21 . . 123.9(4) n
O22 C22 C21 . . 118.9(4) n
O21 C22 C21 . . 117.2(4) n
C31 C21 C11 . . 119.2(4) n
C31 C21 C22 . . 119.9(4) n
C11 C21 C22 . . 120.9(4) n
C32 O31 Er . 3_655 145.6(3) n
O32 C32 O31 . . 127.4(5) n
O32 C32 C31 . . 117.3(4) n
O31 C32 C31 . . 115.3(4) n
C21 C31 C11 . 3 120.6(4) n
C21 C31 C32 . . 120.1(4) n
C11 C31 C32 3 . 119.3(4) 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
Er O31 3_655 2.281(3) y
Er O5 . 2.341(5) y
Er O21 . 2.343(3) y
Er O11 . 2.350(3) y
Er O1 . 2.351(4) y
Er O3 . 2.358(4) y
Er O4 . 2.362(5) y
Er O2 . 2.391(4) y
O11 C12 . 1.269(5) n
O12 C12 . 1.246(6) n
C12 C11 . 1.510(6) n
C11 C31 3 1.394(6) n
C11 C21 . 1.405(6) n
O21 C22 . 1.277(5) n
O22 C22 . 1.244(6) n
C22 C21 . 1.504(6) n
C21 C31 . 1.392(6) n
O31 C32 . 1.259(6) n
O31 Er 3_655 2.281(3) n
O32 C32 . 1.243(6) n
C32 C31 . 1.514(6) n
C31 C11 3 1.394(6) n
O1W O2W . 1.03(4) n
O3W O4W . 1.74(6) n
