#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:17:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178944 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/73/4117303.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4117303
loop_
_publ_author_name
'Christophe Volkringer'
'Natacha Henry'
'Stéphane Grandjean'
'Thierry Loiseau'
_publ_section_title
;
 Uranyl and/or Rare-Earth Mellitates in Extended Organic-Inorganic
 Networks: A Unique Case of Heterometallic Cation-Cation Interaction with
 UVI=O-LnIII Bonding (Ln = Ce, Nd)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1275
_journal_page_last               1283
_journal_paper_doi               10.1021/ja209915n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '2(Ce 3+).  1(C12 O12). 6(O1 H2)'
_chemical_formula_sum            'C12 H12 Ce2 O18'
_chemical_formula_weight         724.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5874(3)
_cell_length_b                   6.73900(10)
_cell_length_c                   10.2833(2)
_cell_measurement_reflns_used    7523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.469
_cell_measurement_theta_min      2.484
_cell_volume                     941.60(3)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART/SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14626
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.76
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    4.871
_exptl_absorpt_correction_T_max  0.7061
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.555
_exptl_crystal_description       Block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1515
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0227P)²+0.5243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                1409
_reflns_number_total             1515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209915n_si_001.cif
_cod_data_source_block           cv48bcor
_cod_database_code               4117303
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ce1 Ce 0.200168(10) 0.13326(2) 0.0000 0.01068(6) Uani 1 2 d S
C1 C 0.09977(14) 0.0731(3) 0.25541(17) 0.0132(3) Uani 1 1 d .
O11 O 0.13515(13) 0.2404(2) 0.23107(14) 0.0263(4) Uani 1 1 d .
O12 O 0.10679(11) -0.0691(2) 0.17536(13) 0.0179(3) Uani 1 1 d .
C3 C 0.29423(19) 0.6257(4) 0.0000 0.0114(5) Uani 1 2 d S
C4 C 0.04799(13) 0.0378(3) 0.38280(16) 0.0116(3) Uani 1 1 d .
O2W O 0.02258(18) 0.2771(4) 0.0000 0.0301(5) Uani 1 2 d SD
O31 O 0.23679(16) 0.4805(3) 0.0000 0.0269(5) Uani 1 2 d S
C5 C 0.09669(19) 0.0739(4) 0.5000 0.0112(5) Uani 1 2 d S
O32 O 0.26861(16) 0.8017(3) 0.0000 0.0212(4) Uani 1 2 d S
O1W O 0.33806(15) 0.1111(2) 0.16074(18) 0.0285(4) Uani 1 1 d D
H11 H 0.353(2) -0.007(3) 0.187(3) 0.045(7) Uiso 1 1 d DU
H12 H 0.349(2) 0.194(4) 0.225(2) 0.035(7) Uiso 1 1 d DU
H21 H -0.023(4) 0.251(14) -0.060(6) 0.09(2) Uiso 0.50 1 d PDU
H22 H 0.055(4) 0.388(6) 0.0000 0.11(2) Uiso 1 2 d SDU
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O31 Ce1 O32 145.39(8) . 1_545
O31 Ce1 O1W 84.42(5) . .
O32 Ce1 O1W 69.95(5) 1_545 .
O31 Ce1 O1W 84.42(5) . 6
O32 Ce1 O1W 69.95(5) 1_545 6
O1W Ce1 O1W 82.66(10) . 6
O31 Ce1 O12 128.04(4) . 6
O32 Ce1 O12 72.70(5) 1_545 6
O1W Ce1 O12 142.59(5) . 6
O1W Ce1 O12 82.85(6) 6 6
O31 Ce1 O12 128.04(4) . .
O32 Ce1 O12 72.70(5) 1_545 .
O1W Ce1 O12 82.85(6) . .
O1W Ce1 O12 142.59(5) 6 .
O12 Ce1 O12 88.15(6) 6 .
O31 Ce1 O2W 80.12(8) . .
O32 Ce1 O2W 134.49(8) 1_545 .
O1W Ce1 O2W 135.80(5) . .
O1W Ce1 O2W 135.80(5) 6 .
O12 Ce1 O2W 75.04(5) 6 .
O12 Ce1 O2W 75.04(5) . .
O31 Ce1 O11 78.56(4) . .
O32 Ce1 O11 112.44(4) 1_545 .
O1W Ce1 O11 70.85(6) . .
O1W Ce1 O11 149.60(6) 6 .
O12 Ce1 O11 127.38(5) 6 .
O12 Ce1 O11 49.68(4) . .
O2W Ce1 O11 65.60(4) . .
O31 Ce1 O11 78.56(4) . 6
O32 Ce1 O11 112.44(4) 1_545 6
O1W Ce1 O11 149.60(6) . 6
O1W Ce1 O11 70.85(6) 6 6
O12 Ce1 O11 49.68(4) 6 6
O12 Ce1 O11 127.38(5) . 6
O2W Ce1 O11 65.60(4) . 6
O11 Ce1 O11 128.70(8) . 6
O31 Ce1 C1 103.17(4) . 6
O32 Ce1 C1 92.88(5) 1_545 6
O1W Ce1 C1 156.12(6) . 6
O1W Ce1 C1 75.71(6) 6 6
O12 Ce1 C1 24.97(5) 6 6
O12 Ce1 C1 108.46(5) . 6
O2W Ce1 C1 68.09(4) . 6
O11 Ce1 C1 132.59(5) . 6
O11 Ce1 C1 24.71(5) 6 6
O31 Ce1 C1 103.17(4) . .
O32 Ce1 C1 92.88(5) 1_545 .
O1W Ce1 C1 75.71(6) . .
O1W Ce1 C1 156.12(6) 6 .
O12 Ce1 C1 108.46(5) 6 .
O12 Ce1 C1 24.98(5) . .
O2W Ce1 C1 68.09(4) . .
O11 Ce1 C1 24.71(5) . .
O11 Ce1 C1 132.59(5) 6 .
C1 Ce1 C1 123.10(7) 6 .
O31 Ce1 H22 60.9(5) . .
O32 Ce1 H22 153.8(5) 1_545 .
O1W Ce1 H22 127.1(3) . .
O1W Ce1 H22 127.1(3) 6 .
O12 Ce1 H22 88.7(4) 6 .
O12 Ce1 H22 88.7(4) . .
O2W Ce1 H22 19.3(5) . .
O11 Ce1 H22 64.36(4) . .
O11 Ce1 H22 64.36(4) 6 .
C1 Ce1 H22 75.3(2) 6 .
C1 Ce1 H22 75.3(2) . .
O11 C1 O12 121.51(17) . .
O11 C1 C4 119.71(16) . .
O12 C1 C4 118.77(16) . .
O11 C1 Ce1 61.73(10) . .
O12 C1 Ce1 59.79(9) . .
C4 C1 Ce1 178.51(13) . .
C1 O11 Ce1 93.56(11) . .
C1 O12 Ce1 95.23(11) . .
O32 C3 O31 125.1(3) . .
O32 C3 C5 119.6(2) . 3
O31 C3 C5 115.3(2) . 3
C5 C4 C4 120.32(12) . 2
C5 C4 C1 120.14(16) . .
C4 C4 C1 119.51(10) 2 .
Ce1 O2W H21 125(5) . .
Ce1 O2W H22 81(4) . .
H21 O2W H22 122(6) . .
C3 O31 Ce1 153.43(19) . .
C4 C5 C4 119.4(2) . 6_556
C4 C5 C3 120.08(12) . 3_545
C4 C5 C3 120.08(12) 6_556 3_545
C3 O32 Ce1 173.7(2) . 1_565
Ce1 O1W H11 116(2) . .
Ce1 O1W H12 126(2) . .
H11 O1W H12 108(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O31 2.392(2) .
Ce1 O32 2.420(2) 1_545
Ce1 O1W 2.5030(17) .
Ce1 O1W 2.5030(17) 6
Ce1 O12 2.5923(14) 6
Ce1 O12 2.5923(14) .
Ce1 O2W 2.600(2) .
Ce1 O11 2.6360(15) .
Ce1 O11 2.6360(15) 6
Ce1 C1 2.9872(18) 6
Ce1 C1 2.9872(18) .
Ce1 H22 2.61(7) .
C1 O11 1.251(2) .
C1 O12 1.267(2) .
C1 C4 1.506(2) .
C3 O32 1.236(3) .
C3 O31 1.252(3) .
C3 C5 1.523(4) 3
C4 C5 1.396(2) .
C4 C4 1.400(3) 2
O2W H21 0.90(2) .
O2W H22 0.87(2) .
C5 C4 1.396(2) 6_556
C5 C3 1.523(4) 3_545
O32 Ce1 2.420(2) 1_565
O1W H11 0.863(18) .
O1W H12 0.883(17) .
