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_7231647
_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         'C10 H13 Ce4 Cs2.5 Na7.5 O97 Si2 W18, 4(O)'
_chemical_formula_sum            'C10 H13 Ce4 Cs2.5 Na7.5 O101 Si2 W18'
_chemical_formula_weight         6179.86
_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             2017-05-11
_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                 98.754(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2090(7)
_cell_length_b                   12.8421(6)
_cell_length_c                   28.4056(14)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.22
_cell_volume                     4762.3(4)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            106571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         1.451
_exptl_absorpt_coefficient_mu    24.633
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3307
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 'numerical''
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.310
_exptl_crystal_description       prism
_exptl_crystal_F_000             5386
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.704
_refine_diff_density_min         -3.392
_refine_diff_density_rms         0.541
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0925P)^2^+1049.7632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.1963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9561
_reflns_number_total             9773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01447g2.cif
_cod_data_source_block           kn033monop_hklf5
_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_weight         3089.93
_cod_original_formula_moiety      'C5 H6.5 Ce2 Cs1.25 Na3.75 O48.5 Si W9, 2(O)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C5 H6.50 Ce2 Cs1.25 Na3.75 O50.50 Si W9'
_cod_database_code               7231647
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8969(9)
 0.1031(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Others
 Fixed Sof: Cs1(0.75) OW3(0.7) Na3(0.75) H10B(0.5) OW2(0.3) OW11(0.5)
 OW12(0.5) OW9(0.33333) OW8(0.33333) Cs2(0.25) Cs3(0.25) OW10(0.33333) OW14(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C10(H10A,H10B), C0AA(H0AA,H0AB)
4.b Tetrahedral OH refined with riding coordinates:
 O39(H39)
;
_shelx_res_checksum              7835
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'