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_7239599
_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         'C3 H3 As3 Ce6 Na15 O155 W27, O'
_chemical_formula_sum            'C3 H3 As3 Ce6 Na15 O156 W27'
_chemical_formula_weight         8909.33
_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             2019-09-23
_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                105.118(3)
_cell_angle_beta                 98.139(3)
_cell_angle_gamma                112.226(2)
_cell_formula_units_Z            2
_cell_length_a                   18.4264(12)
_cell_length_b                   19.3634(12)
_cell_length_c                   26.7239(15)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.34
_cell_volume                     8207.4(9)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f 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  0.0626
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            110252
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_min         1.289
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.208
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1735 before and 0.0644 after correction. The Ratio of minimum to maximum transmission is 0.5523. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.605
_exptl_crystal_description       block
_exptl_crystal_F_000             7758
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.748
_refine_diff_density_min         -3.501
_refine_diff_density_rms         0.486
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         32729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0629P)^2^+583.8150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22284
_reflns_number_total             32729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01663e2.cif
_cod_data_source_block           md07g_sq
_cod_depositor_comments
;Adding full bibliography for 7239596--7239599.cif.

 Adding full bibliography for 7239596--7239599.cif.
;
_cod_database_code               7239599
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.282
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Na3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C3(H3)
;
_shelx_res_checksum              38880
_shelx_fab_checksum              74576
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'