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_7231650
_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         'C8 H10 Ce4 Na10 O104 Si2 W18, 2(O)'
_chemical_formula_sum            'C8 H10 Ce4 Na10 O106 Si2 W18'
_chemical_formula_weight         5958.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2429(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5499(3)
_cell_length_b                   12.9776(3)
_cell_length_c                   26.9266(6)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      36.16
_cell_measurement_theta_min      2.24
_cell_volume                     4686.00(18)
_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      100.02
_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 0.996
_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  0.0550
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            223683
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.280
_diffrn_reflns_theta_min         1.528
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.094
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.3479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1367 before and 0.0586 after correction. The Ratio of minimum to maximum transmission is 0.4657. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.926
_refine_diff_density_min         -2.952
_refine_diff_density_rms         0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         22562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+48.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18961
_reflns_number_total             22562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01447g2.cif
_cod_data_source_block           sd149
_cod_depositor_comments
;
Adding full bibliography for 7231646--7231650.cif.

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H5 Ce2 Na5 O53 Si W9'
_cod_original_formula_weight         2979.01
_cod_original_formula_moiety         'C4 H5 Ce2 Na5 O52 Si W9, O'
_cod_original_formula_units_Z            4
_cod_database_code               7231650
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Sof(W1B)=Sof(W3B)=Sof(O6B)=Sof(O1B)=Sof(O5B)=Sof(W2B)=Sof(O4B)=Sof(O2B)=
 Sof(O3B)=1-FVAR(1)
 Sof(W1A)=Sof(W2A)=Sof(W3A)=Sof(O5A)=Sof(O4A)=Sof(O3A)=Sof(O6A)=Sof(O1A)=
 Sof(O2A)=FVAR(1)
 Fixed Sof: OW15(0.8) Na1(0.75) OW12(0.2) Na6(0.25)
3.a Free rotating group:
 W1B(W3B,O6B,O1B,O5B,W2B,O4B,O2B,O3B)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
3.c Tetrahedral OH refined with riding coordinates:
 O39(H39)
;
_shelx_res_checksum              68737
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'