#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:25:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179245 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/65/4316535.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_4316535
loop_
_publ_author_name
'Jennifer L. Nicholls'
'Sarah E. Hulse'
'Samantha K. Callear'
'Graham J. Tizzard'
'Richard A. Stephenson'
'Michael B. Hursthouse'
'William Clegg'
'Ross W. Harrington'
'Andrew M. Fogg'
_publ_section_title
;
 Synthesis and Structure of Pillared Molybdates and Tungstates with
 Framework Layers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8545
_journal_page_last               8551
_journal_paper_doi               10.1021/ic101145p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'Ce2 (Mo O4)2 (H2 O)2 (C4 H2 O4)'
_chemical_formula_sum            'C4 H6 Ce2 Mo2 O14'
_chemical_formula_weight         750.21
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.671(6)
_cell_angle_beta                 85.649(7)
_cell_angle_gamma                87.288(11)
_cell_formula_units_Z            2
_cell_length_a                   7.2307(9)
_cell_length_b                   7.4798(9)
_cell_length_c                   13.5668(7)
_cell_measurement_reflns_used    10001
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      1.45
_cell_volume                     716.98(13)
_computing_cell_refinement       'Rigaku TwinSolve'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku TwinSolve'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.794
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device_type
'Rigaku Saturn 724 on Crystal Logic goniometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4475
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.007
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku TwinSolve'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.023
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.572
_refine_ls_extinction_coef       0.0032(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1073P)²+38.4881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2096
_reflns_number_gt                4125
_reflns_number_total             4475
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic101145p_si_002_6.cif
_cod_data_source_block           ssi0053
_cod_database_code               4316535
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.09514(10) 0.67063(11) 0.20010(5) 0.0091(2) Uani 1 1 d . . .
Ce2 Ce 0.37279(10) 0.16882(11) 0.20574(5) 0.0086(2) Uani 1 1 d . . .
O1 O 0.3076(15) 0.6222(15) 0.3477(7) 0.0142(19) Uani 1 1 d U . .
O2 O 0.3467(16) 0.3217(15) 0.3512(6) 0.0151(19) Uani 1 1 d U . .
C1 C 0.3735(19) 0.465(2) 0.3817(9) 0.0112(19) Uani 1 1 d U . .
C2 C 0.4940(18) 0.4386(19) 0.4709(9) 0.011(2) Uani 1 1 d U . .
H2 H 0.5650 0.3277 0.4861 0.013 Uiso 1 1 calc R . .
O3 O -0.0914(14) 0.8055(16) 0.3400(7) 0.0138(18) Uani 1 1 d U . .
O4 O 0.1434(14) 0.9948(16) 0.3235(7) 0.0147(19) Uani 1 1 d U . .
C3 C 0.0047(18) 0.919(2) 0.3715(9) 0.0113(19) Uani 1 1 d U . .
C4 C -0.054(2) 0.957(2) 0.4760(10) 0.015(2) Uani 1 1 d U . .
H4 H -0.1706 0.9177 0.5073 0.017 Uiso 1 1 calc R . .
Mo1 Mo -0.07818(15) 0.21461(17) 0.11014(8) 0.0092(3) Uani 1 1 d . . .
O5 O 0.0683(14) 0.3479(15) 0.1682(7) 0.014(2) Uani 1 1 d . . .
O6 O -0.1125(15) 0.3119(15) -0.0180(7) 0.015(2) Uani 1 1 d . . .
O7 O -0.2933(15) 0.1931(16) 0.1804(8) 0.017(2) Uani 1 1 d . . .
O8 O 0.0350(15) -0.0018(15) 0.1191(7) 0.014(2) Uani 1 1 d . . .
Mo2 Mo 0.55742(15) 0.70199(16) 0.10918(7) 0.0087(3) Uani 1 1 d . . .
O9 O 0.4185(14) 0.5084(15) 0.1434(8) 0.014(2) Uani 1 1 d . . .
O10 O 0.3998(15) 0.8677(15) 0.1528(7) 0.015(2) Uani 1 1 d . . .
O11 O 0.7635(15) 0.6712(15) 0.1729(8) 0.015(2) Uani 1 1 d . . .
O12 O 0.6108(15) 0.7625(17) -0.0220(7) 0.019(2) Uani 1 1 d . . .
O13 O -0.0625(18) 0.4346(18) 0.3544(9) 0.024(3) Uani 1 1 d . . .
O14 O 0.5285(14) -0.0694(15) 0.3410(7) 0.016(2) Uani 1 1 d . . .
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'
Mo Mo -1.6832 0.6857 '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
_geom_angle_publ_flag
O1 Ce1 O3 74.9(3) . . ?
O1 Ce1 O5 102.9(3) . . ?
O1 Ce1 O6 140.3(4) . 2_565 ?
O1 Ce1 O8 114.9(3) . 1_565 ?
O1 Ce1 O9 71.6(3) . . ?
O1 Ce1 O10 68.5(3) . . ?
O1 Ce1 O11 138.9(3) . 1_455 ?
O1 Ce1 O13 71.4(4) . . ?
O3 Ce1 O5 125.4(3) . . ?
O3 Ce1 O6 140.9(3) . 2_565 ?
O3 Ce1 O8 76.3(3) . 1_565 ?
O3 Ce1 O9 146.4(3) . . ?
O3 Ce1 O10 105.8(3) . . ?
O3 Ce1 O11 71.2(3) . 1_455 ?
O3 Ce1 O13 62.8(4) . . ?
O5 Ce1 O6 72.2(3) . 2_565 ?
O5 Ce1 O8 141.0(3) . 1_565 ?
O5 Ce1 O9 64.7(3) . . ?
O5 Ce1 O10 124.4(3) . . ?
O5 Ce1 O11 79.4(4) . 1_455 ?
O5 Ce1 O13 65.0(4) . . ?
O6 Ce1 O8 72.5(4) 2_565 1_565 ?
O6 Ce1 O9 70.9(3) 2_565 . ?
O6 Ce1 O10 81.9(4) 2_565 . ?
O6 Ce1 O11 80.1(4) 2_565 1_455 ?
O6 Ce1 O13 132.5(4) 2_565 . ?
O8 Ce1 O9 117.3(3) 1_565 . ?
O8 Ce1 O10 65.4(3) 1_565 . ?
O8 Ce1 O11 78.6(4) 1_565 1_455 ?
O8 Ce1 O13 135.6(4) 1_565 . ?
O9 Ce1 O10 60.4(3) . . ?
O9 Ce1 O11 139.1(3) . 1_455 ?
O9 Ce1 O13 106.4(4) . . ?
O10 Ce1 O11 143.2(3) . 1_455 ?
O10 Ce1 O13 139.9(4) . . ?
O11 Ce1 O13 72.9(4) 1_455 . ?
O2 Ce2 O4 75.7(4) . 1_545 ?
O2 Ce2 O5 81.8(4) . . ?
O2 Ce2 O7 94.2(4) . 1_655 ?
O2 Ce2 O9 71.1(3) . . ?
O2 Ce2 O10 144.7(3) . 1_545 ?
O2 Ce2 O12 141.0(4) . 2_665 ?
O2 Ce2 O14 78.1(4) . . ?
O4 Ce2 O5 76.4(3) 1_545 . ?
O4 Ce2 O7 139.0(3) 1_545 1_655 ?
O4 Ce2 O9 133.3(4) 1_545 . ?
O4 Ce2 O10 78.5(4) 1_545 1_545 ?
O4 Ce2 O12 129.2(4) 1_545 2_665 ?
O4 Ce2 O14 68.3(3) 1_545 . ?
O5 Ce2 O7 142.4(3) . 1_655 ?
O5 Ce2 O9 67.2(3) . . ?
O5 Ce2 O10 115.0(4) . 1_545 ?
O5 Ce2 O12 77.4(3) . 2_665 ?
O5 Ce2 O14 142.6(3) . . ?
O7 Ce2 O9 76.1(3) 1_655 . ?
O7 Ce2 O10 89.6(4) 1_655 1_545 ?
O7 Ce2 O12 83.1(4) 1_655 2_665 ?
O7 Ce2 O14 70.7(3) 1_655 . ?
O9 Ce2 O10 143.3(3) . 1_545 ?
O9 Ce2 O12 70.5(4) . 2_665 ?
O9 Ce2 O14 132.3(3) . . ?
O10 Ce2 O12 74.4(4) 1_545 2_665 ?
O10 Ce2 O14 70.1(4) 1_545 . ?
O12 Ce2 O14 135.4(4) 2_665 . ?
Ce1 O1 C1 120.0(9) . . ?
Ce2 O2 C1 145.6(8) . . ?
O1 C1 O2 126.6(12) . . ?
O1 C1 C2 119.1(13) . . ?
O2 C1 C2 114.3(11) . . ?
C1 C2 C2 124.0(15) . 2_666 ?
Ce1 O3 C3 110.7(8) . . ?
Ce2 O4 C3 169.0(9) 1_565 . ?
O3 C3 O4 124.3(12) . . ?
O3 C3 C4 116.6(12) . . ?
O4 C3 C4 119.1(13) . . ?
C3 C4 C4 121.8(16) . 2_576 ?
O5 Mo1 O6 113.1(5) . . ?
O5 Mo1 O7 108.2(5) . . ?
O5 Mo1 O8 105.7(5) . . ?
O6 Mo1 O7 109.8(5) . . ?
O6 Mo1 O8 110.2(5) . . ?
O7 Mo1 O8 109.7(5) . . ?
Ce1 O5 Ce2 109.1(4) . . ?
Ce1 O5 Mo1 141.0(5) . . ?
Ce2 O5 Mo1 108.9(5) . . ?
Ce1 O6 Mo1 156.8(6) 2_565 . ?
Ce2 O7 Mo1 155.7(6) 1_455 . ?
Ce1 O8 Mo1 154.1(5) 1_545 . ?
O9 Mo2 O10 99.0(5) . . ?
O9 Mo2 O11 111.3(5) . . ?
O9 Mo2 O12 113.0(5) . . ?
O10 Mo2 O11 112.2(5) . . ?
O10 Mo2 O12 111.1(5) . . ?
O11 Mo2 O12 109.9(5) . . ?
Ce1 O9 Ce2 104.7(4) . . ?
Ce1 O9 Mo2 99.6(5) . . ?
Ce2 O9 Mo2 152.8(5) . . ?
Ce1 O10 Ce2 114.0(4) . 1_565 ?
Ce1 O10 Mo2 100.1(5) . . ?
Ce2 O10 Mo2 145.0(6) 1_565 . ?
Ce1 O11 Mo2 159.5(5) 1_655 . ?
Ce2 O12 Mo2 169.7(6) 2_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O1 2.575(10) . ?
Ce1 O3 2.583(10) . ?
Ce1 O5 2.553(12) . ?
Ce1 O6 2.442(9) 2_565 ?
Ce1 O8 2.513(10) 1_565 ?
Ce1 O9 2.712(10) . ?
Ce1 O10 2.675(11) . ?
Ce1 O11 2.454(11) 1_455 ?
Ce1 O13 2.679(12) . ?
Ce2 O2 2.459(10) . ?
Ce2 O4 2.446(10) 1_545 ?
Ce2 O5 2.554(10) . ?
Ce2 O7 2.423(11) 1_655 ?
Ce2 O9 2.543(11) . ?
Ce2 O10 2.490(12) 1_545 ?
Ce2 O12 2.439(10) 2_665 ?
Ce2 O14 2.579(8) . ?
O1 C1 1.259(17) . ?
O2 C1 1.25(2) . ?
C1 C2 1.520(18) . ?
C2 C2 1.33(3) 2_666 ?
O3 C3 1.275(18) . ?
O4 Ce2 2.446(10) 1_565 ?
O4 C3 1.250(16) . ?
C3 C4 1.526(18) . ?
C4 C4 1.31(3) 2_576 ?
Mo1 O5 1.809(12) . ?
Mo1 O6 1.779(9) . ?
Mo1 O7 1.759(10) . ?
Mo1 O8 1.766(11) . ?
O6 Ce1 2.442(9) 2_565 ?
O7 Ce2 2.423(11) 1_455 ?
O8 Ce1 2.513(10) 1_545 ?
Mo2 O9 1.767(11) . ?
Mo2 O10 1.799(11) . ?
Mo2 O11 1.762(11) . ?
Mo2 O12 1.766(9) . ?
O10 Ce2 2.490(12) 1_565 ?
O11 Ce1 2.454(11) 1_655 ?
O12 Ce2 2.439(10) 2_665 ?
