Synthesis and Structure of Pillared Molybdates and Tungstates with Framework Layers
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; Inorganic Chemistry 49 (2010) 8545–8551; doi:10.1021/ic101145p

data_4316535
_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 \w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1073P)^2^+38.4881P] where P=(Fo^2^+2Fc^2^)/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>2\s(I)
_cod_data_source_file            ic101145p_si_002_6.cif
_cod_data_source_block           ssi0053
_cod_database_code               4316535