Influence of pH on CeIV-[AsIIIW9O33]9− association for the formation of hexanuclear cerium(iv) oxo-hydroxo-clusters stabilized by trivacant polyanions
Dufaye, Maxime; Duval, Sylvain; Stoclet, Gregory; Loiseau, Thierry; CrystEngComm 22 (2020) 371–380; doi:10.1039/C9CE01663E

data_7239598
_publ_section_title
;
 Influence of pH on CeIV-[AsIIIW9O33]9&#x2212; association for the
 formation of hexanuclear cerium(iv) oxo-hydroxo-clusters stabilized by
 trivacant polyanions
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              371
_journal_page_last               380
_journal_paper_doi               10.1039/C9CE01663E
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C9 H9 As Ce6 Na6 O81 W9, 2.38(O2)'
_chemical_formula_sum            'C9 H9 As Ce6 Na6 O85.75 W9'
_chemical_formula_weight         4197.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-26 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.152(3)
_cell_angle_beta                 101.470(3)
_cell_angle_gamma                101.060(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9097(7)
_cell_length_b                   15.2185(8)
_cell_length_c                   21.8082(13)
_cell_measurement_reflns_used    1288
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      13.52
_cell_measurement_theta_min      3.65
_cell_volume                     3798.4(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.985
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50492
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_min         0.954
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.682
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.4800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.2000 before and 0.1065 after correction. The Ratio of minimum to maximum transmission is 0.6454. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.670
_exptl_crystal_description       needle
_exptl_crystal_F_000             3724
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         15.620
_refine_diff_density_min         -3.334
_refine_diff_density_rms         0.679
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         15358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0845P)^2^+327.7084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10575
_reflns_number_total             15358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01663e2.cif
_cod_data_source_block           md07abis_sq
_cod_depositor_comments
;Adding full bibliography for 7239596--7239599.cif.

 Adding full bibliography for 7239596--7239599.cif.
;
_cod_database_code               7239598
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.417
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: OW3(0.5) OW8(0.5) OW18(0.75) OW11(0.5) OW17(0.5) OW29(0.75)
 OW21(0.75) OW4(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C3(H3), C1(H1), C4(H4), C6(H6), C7(H7), C9(H9), C8(H8)
;
_shelx_res_checksum              32435
_shelx_fab_checksum              27007
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'