Bottom-up synthesis of functionalized {Ce4(SiW9O34)2(l)2} polyoxometalates
Dufaye, Maxime; Duval, Sylvain; Nursiah, Kelvinraj; Stoclet, Gregory; Trivelli, Xavier; Loiseau, Thierry; CrystEngComm 20 (2018) 7144–; doi:10.1039/C8CE01447G

data_7231649
_publ_section_title
;
 Bottom-up synthesis of functionalized {Ce4(SiW9O34)2(l)2}
 polyoxometalates
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7144
_journal_paper_doi               10.1039/C8CE01447G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'Ce9 Cs3.25 Na6 O166.25 Si4 W36, 15.5(O), Na O0.5'
_chemical_formula_sum            'Ce9 Cs3.25 Na7 O182.25 Si4 W36'
_chemical_formula_weight         11500.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                70.021(3)
_cell_angle_beta                 86.051(3)
_cell_angle_gamma                66.330(3)
_cell_formula_units_Z            2
_cell_length_a                   18.7410(11)
_cell_length_b                   21.5447(12)
_cell_length_c                   30.6060(16)
_cell_measurement_reflns_used    9350
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.24
_cell_volume                     10603.4(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            308589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         0.710
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.005
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1571 before and 0.0636 after correction. The Ratio of minimum to maximum transmission is 0.5409. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.602
_exptl_crystal_description       block
_exptl_crystal_F_000             9912
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.083
_refine_diff_density_min         -4.205
_refine_diff_density_rms         0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         43321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+900.6484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29938
_reflns_number_total             43321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01447g2.cif
_cod_data_source_block           kn013tp_sq
_cod_depositor_comments
'Adding full bibliography for 7231646--7231650.cif.'
_cod_original_cell_volume        10603.5(11)
_cod_database_code               7231649
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Sof(W1B)=Sof(W3B)=Sof(W2B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O1B)=Sof(O6B)=
 Sof(O5B)=1-FVAR(1)
 Sof(W3A)=Sof(W1A)=Sof(W2A)=Sof(O3A)=Sof(O1A)=Sof(O2A)=Sof(O4A)=Sof(O5A)=
 Sof(O6A)=FVAR(1)
 Sof(W11B)=Sof(W12B)=Sof(W10B)=Sof(O38B)=Sof(O40B)=Sof(O39B)=Sof(O37B)=
 Sof(O36B)=Sof(O35B)=1-FVAR(2)
 Sof(W12A)=Sof(W11A)=Sof(W10A)=Sof(O40A)=Sof(O39A)=Sof(O38A)=Sof(O36A)=
 Sof(O37A)=Sof(O35A)=FVAR(2)
 Sof(Cs2B)=1-FVAR(3)
 Sof(Cs2A)=FVAR(3)
 Fixed Sof: Cs3(0.75) O12W(0.25) O38W(0.5) O2W(0.5) Cs1(0.5) O45W(0.5)
 O2IA(0.5) O43W(0.5) O42W(0.5) O49W(0.5) O26W(0.5) O16W(0.5) O51W(0.5)
 O39W(0.5) O34W(0.5) O23W(0.5) O37W(0.5) O11W(0.5) O32W(0.5) O53W(0.25)
 O41W(0.5) O52W(0.25) O54W(0.25) O29W(0.5) O14W(0.5) O4W(0.5) O28W(0.5)
 O27W(0.5) O24W(0.5) O17W(0.25) O1W(0.25) O8W(0.25) O3W(0.25) O6W(0.25)
 O7W(0.25) O18W(0.25)
;
_shelx_res_checksum              83323
_shelx_fab_checksum              83215
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'