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_4316530
_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         'C5 H3 Mo Nd O8 S'
_chemical_formula_sum            'C5 H3 Mo Nd O8 S'
_chemical_formula_weight         463.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 93.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.6918(18)
_cell_length_b                   7.2951(4)
_cell_length_c                   7.4407(4)
_cell_measurement_reflns_used    4091
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1933.27(18)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics
'OLEX2 (Dolomanov, Bourhis, Gildea, Howard & Puschmann, 2009)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 66.065
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1351
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15260
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.849
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_correction_T_min  0.4473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2220
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+213.8900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                1896
_reflns_number_total             2220
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic101145p_si_002_1.cif
_cod_data_source_block           2008src0992
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4316530