#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/04/2210442.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_2210442
loop_
_publ_author_name
'Rahahlia, N.'
'Benmerad, B.'
'Guehria-Laidoudi, A.'
'Dahaoui, S.'
'Lecomte, C.'
_publ_section_title
;
 Poly[[tetraaqua-μ₄-glutarato-cerium(III)] chloride dihydrate]
;
_journal_coeditor_code           XU2099
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2145
_journal_page_last               m2147
_journal_paper_doi               10.1107/S1600536806030741
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ce (C5 H6 O4) (H2 O)4] Cl , 2H2 O'
_chemical_formula_moiety         'C5 H14 Ce O8 + , Cl - , 2H2 O'
_chemical_formula_sum            'C5 H18 Ce Cl O10'
_chemical_formula_weight         413.76
_chemical_name_common
;
Polymeric tetraaquacerium(III)-μ₄-glutarato chloride dihydrate
;
_chemical_name_systematic
;
Poly[[tetraaqua-μ₄-glutarato-cerium(III)] chloride dihydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                110.500(5)
_cell_angle_beta                 95.531(5)
_cell_angle_gamma                103.439(5)
_cell_formula_units_Z            2
_cell_length_a                   7.932(5)
_cell_length_b                   8.803(5)
_cell_length_c                   10.509(5)
_cell_measurement_reflns_used    21564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.5
_cell_volume                     655.7(6)
_computing_cell_refinement       DENZO
_computing_data_collection       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       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  0.031
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21564
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         3.5
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.713
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.83
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.020
_refine_ls_R_factor_gt           0.017
_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)+(0.0151P)²+0.3197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.033
_refine_ls_wR_factor_ref         0.034
_reflns_number_gt                3561
_reflns_number_total             3827
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2099.cif
_cod_data_source_block           I
_cod_database_code               2210442
_cod_database_fobs_code          2210442
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
O O1 0.68431(16) 0.59638(15) 0.50985(12) 0.0098(2) Uani d . 1
O O2 0.37375(17) 0.68194(15) 0.40535(12) 0.0109(2) Uani d . 1
O O3 0.17130(16) 0.22319(16) 0.28234(12) 0.0116(2) Uani d . 1
O O4 0.56069(16) 0.21155(15) 0.36169(12) 0.0099(2) Uani d . 1
O O1W 0.76092(17) 0.39701(16) 0.20186(14) 0.0150(3) Uani d . 1
H H11 0.7891 0.3149 0.1684 0.022 Uiso d R 1
H H12 0.8291 0.4676 0.1901 0.022 Uiso d R 1
O O2W 0.61657(17) 0.66570(16) 0.21681(14) 0.0142(3) Uani d . 1
H H21 0.5405 0.6784 0.1630 0.021 Uiso d R 1
H H22 0.7056 0.6945 0.2041 0.021 Uiso d R 1
O O3W 0.23648(18) 0.46833(16) 0.13784(13) 0.0158(3) Uani d . 1
H H31 0.1828 0.4173 0.0593 0.024 Uiso d R 1
H H32 0.1990 0.5492 0.1675 0.024 Uiso d R 1
O O4W 0.39806(17) 0.18317(16) 0.05783(12) 0.0130(3) Uani d . 1
H H41 0.4589 0.1753 0.0051 0.020 Uiso d R 1
H H42 0.3078 0.0931 0.0210 0.020 Uiso d R 1
O O5W 0.56947(17) 0.12130(15) 0.83394(13) 0.0119(2) Uani d . 1
H H51 0.6690 0.1516 0.8332 0.018 Uiso d R 1
H H52 0.5322 0.0250 0.7829 0.018 Uiso d R 1
O O6W 0.12111(17) 0.88340(16) 0.93030(13) 0.0123(2) Uani d . 1
H H61 0.0865 0.8535 0.9850 0.018 Uiso d R 1
H H62 0.0439 0.8644 0.8729 0.018 Uiso d R 1
C C5 0.3719(2) 0.7876(2) 0.52214(17) 0.0083(3) Uani d . 1
C C4 0.2811(2) 0.9241(2) 0.52772(17) 0.0082(3) Uani d . 1
H H4A 0.2369 0.9121 0.4323 0.010 Uiso calc R 1
H H4B 0.3676 1.0371 0.5759 0.010 Uiso calc R 1
C C3 0.1259(2) 0.9098(2) 0.60438(17) 0.0089(3) Uani d . 1
H H3A 0.1695 0.9195 0.6992 0.011 Uiso calc R 1
H H3B 0.0732 1.0033 0.6120 0.011 Uiso calc R 1
C C2 0.9857(2) 0.7403(2) 0.52639(18) 0.0125(3) Uani d . 1
H H2A 0.9451 0.7329 0.4317 0.015 Uiso calc R 1
H H2B 1.0423 0.6489 0.5172 0.015 Uiso calc R 1
C C1 0.8255(2) 0.7069(2) 0.59004(17) 0.0089(3) Uani d . 1
Cl Cl1 0.99395(5) 0.27253(5) 0.84452(4) 0.01088(8) Uani d . 1
Ce Ce1 0.474519(13) 0.428248(12) 0.289380(10) 0.00656(3) Uani d . 1
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'
H H 0.0000 0.0000 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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
C1 O1 Ce1 . . 156.05(11) ?
C1 O1 Ce1 . 2_666 94.85(10) ?
Ce1 O1 Ce1 . 2_666 108.33(6) ?
C5 O2 Ce1 . . 142.98(11) ?
C1 O3 Ce1 2_666 . 94.48(10) ?
C5 O4 Ce1 2_666 . 133.80(11) ?
Ce1 O1W H11 . . 128.8 ?
Ce1 O1W H12 . . 124.9 ?
H11 O1W H12 . . 105.3 ?
Ce1 O2W H21 . . 109.5 ?
Ce1 O2W H22 . . 132.2 ?
H21 O2W H22 . . 110.8 ?
Ce1 O3W H31 . . 134.9 ?
Ce1 O3W H32 . . 120.1 ?
H31 O3W H32 . . 105.0 ?
Ce1 O4W H41 . . 122.6 ?
Ce1 O4W H42 . . 131.5 ?
H41 O4W H42 . . 105.9 ?
H51 O5W H52 . . 108.3 ?
H61 O6W H62 . . 108.9 ?
C5 C4 H4A . . 109.5 ?
C3 C4 H4A . . 109.5 ?
C5 C4 H4B . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 108.1 ?
C2 C3 H3A 1_455 . 109.6 ?
C4 C3 H3A . . 109.6 ?
C2 C3 H3B 1_455 . 109.6 ?
C4 C3 H3B . . 109.6 ?
H3A C3 H3B . . 108.1 ?
C1 C2 H2A . . 108.2 ?
C3 C2 H2A 1_655 . 108.2 ?
C1 C2 H2B . . 108.2 ?
C3 C2 H2B 1_655 . 108.2 ?
H2A C2 H2B . . 107.3 ?
O1 Ce1 O3W . . 137.71(5) ?
O4 Ce1 O3W . . 142.53(4) ?
O2 Ce1 O3W . . 65.61(5) ?
O1 Ce1 O4W . . 147.98(4) ?
O4 Ce1 O4W . . 80.12(6) ?
O2 Ce1 O4W . . 137.96(5) ?
O3W Ce1 O4W . . 72.40(5) ?
O1 Ce1 O2W . . 84.69(5) ?
O4 Ce1 O2W . . 138.56(5) ?
O2 Ce1 O2W . . 70.05(6) ?
O3W Ce1 O2W . . 72.26(5) ?
O4W Ce1 O2W . . 99.48(6) ?
O1 Ce1 O1W . . 81.73(6) ?
O4 Ce1 O1W . . 73.83(4) ?
O2 Ce1 O1W . . 131.93(4) ?
O3W Ce1 O1W . . 118.49(6) ?
O4W Ce1 O1W . . 71.07(5) ?
O2W Ce1 O1W . . 67.18(5) ?
O3W Ce1 O1 . 2_666 100.89(6) ?
O4W Ce1 O1 . 2_666 120.38(5) ?
O2W Ce1 O1 . 2_666 135.90(4) ?
O1W Ce1 O1 . 2_666 140.28(4) ?
O3W Ce1 O3 . . 71.99(6) ?
O4W Ce1 O3 . . 73.26(5) ?
O2W Ce1 O3 . . 144.03(4) ?
O1W Ce1 O3 . . 136.38(5) ?
O1 Ce1 O3 2_666 . 49.75(4) yes
O3W Ce1 C1 . 2_666 84.13(6) ?
O4W Ce1 C1 . 2_666 97.39(5) ?
O2W Ce1 C1 . 2_666 145.03(4) ?
O1W Ce1 C1 . 2_666 147.73(5) ?
O3W Ce1 Ce1 . 2_666 124.24(4) ?
O4W Ce1 Ce1 . 2_666 145.94(3) ?
O2W Ce1 Ce1 . 2_666 113.60(4) ?
O1W Ce1 Ce1 . 2_666 113.72(4) ?
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
O1 C1 . 1.284(2) ?
O1 Ce1 . 2.4572(15) yes
O1 Ce1 2_666 2.6061(16) yes
O2 C5 . 1.258(2) ?
O2 Ce1 . 2.4945(16) yes
O3 C1 2_666 1.259(2) ?
O3 Ce1 . 2.6273(18) yes
O4 C5 2_666 1.282(2) ?
O4 Ce1 . 2.4910(16) yes
O1W Ce1 . 2.5687(18) yes
O1W H11 . 0.7803 ?
O1W H12 . 0.7779 ?
O2W Ce1 . 2.5314(16) yes
O2W H21 . 0.8400 ?
O2W H22 . 0.7346 ?
O3W Ce1 . 2.5198(16) yes
O3W H31 . 0.8051 ?
O3W H32 . 0.8078 ?
O4W Ce1 . 2.5246(15) yes
O4W H41 . 0.7647 ?
O4W H42 . 0.8714 ?
O5W H51 . 0.7736 ?
O5W H52 . 0.7925 ?
O6W H61 . 0.7604 ?
O6W H62 . 0.7601 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
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
_geom_hbond_publ_flag
O1W H11 O6W 2_666 0.78 2.02 2.797(3) 173 yes
O1W H12 Cl1 2_766 0.78 2.55 3.321(3) 169 yes
O2W H21 O5W 2_666 0.84 2.13 2.795(3) 135 yes
O2W H22 Cl1 2_766 0.74 2.46 3.179(2) 167 yes
O3W H31 Cl1 1_454 0.81 2.33 3.125(2) 172 yes
O3W H32 Cl1 2_666 0.81 2.46 3.207(3) 155 yes
O4W H41 O5W 1_554 0.77 2.03 2.783(3) 167 yes
O4W H42 O6W 1_544 0.87 1.93 2.801(3) 175 yes
O5W H51 Cl1 . 0.77 2.52 3.296(3) 176 yes
O5W H52 O4 2_656 0.79 2.01 2.801(3) 175 yes
O6W H61 Cl1 2_667 0.76 2.48 3.229(2) 171 yes
O6W H62 O3 2_566 0.76 2.04 2.788(3) 171 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ce1 O2 C5 O4 . 2_666 0.0(3) ?
Ce1 O2 C5 C4 . . -179.16(12) yes
O2 C5 C4 C3 . . 118.84(17) ?
O4 C5 C4 C3 2_666 . -60.4(2) ?
C5 C4 C3 C2 . 1_455 -62.67(18) yes
Ce1 O1 C1 O3 . 2_666 155.20(19) ?
Ce1 O1 C1 O3 2_666 2_666 -10.37(16) ?
Ce1 O1 C1 C2 . . -28.0(4) ?
Ce1 O1 C1 C2 2_666 . 166.40(13) ?
Ce1 O1 C1 Ce1 . 2_666 165.6(3) ?
C3 C2 C1 O3 1_655 2_666 -25.0(2) ?
C3 C2 C1 O1 1_655 . 158.32(15) ?
C3 C2 C1 Ce1 1_655 2_666 -127.5(5) ?
C1 O1 Ce1 O4 . . 120.3(3) ?
Ce1 O1 Ce1 O4 2_666 . -74.83(5) yes
C1 O1 Ce1 O2 . . -93.3(3) ?
Ce1 O1 Ce1 O2 2_666 . 71.50(6) yes
