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_7239596
_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_sum            'C13.68 H13.68 As4 Ce24 Na2 O214 W36'
_chemical_formula_weight         15209.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.7106(15)
_cell_length_b                   24.7106(15)
_cell_length_c                   23.2547(14)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.41
_cell_volume                     14199.6(15)
_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    'XT (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53274
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.360
_diffrn_reflns_theta_min         1.165
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.857
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1291 before and 0.0538 after correction. The Ratio of minimum to maximum transmission is 0.6313. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.557
_exptl_crystal_description       prism
_exptl_crystal_F_000             13316
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.466
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details
;
 Flack x determined using 5653 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         14485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+44.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12948
_reflns_number_total             14485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01663e2.cif
_cod_data_source_block           mc066bis
_cod_depositor_comments
;
 Adding full bibliography for 7239596--7239599.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         3802.32
_cod_original_formula_moiety         'C3.42 H3.42 As Ce6 Na0.5 O56 W9, 17.5(O)'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        14199.6(19)
_cod_original_formula_sum        'C3.42 H3.42 As Ce6 Na0.50 O73.50 W9'
_cod_database_code               7239596
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(O45B)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(O45A)=FVAR(1)
 Sof(O18W)=1-FVAR(2)
 Sof(O17W)=FVAR(2)
 Fixed Sof: O1W(0.75) Na1(0.5) O22W(0.25) O10W(0.5) O2W(0.5) O30W(0.5)
 O8W(0.4) O26W(0.3) O7W(0.3) O9W(0.3) O6W(0.3) O13W(0.2) O3W(0.3) O4W(0.2)
 O5W(0.2) O12W(0.2) O14W(0.2) O11W(0.1)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C1(H1)
;
_shelx_res_checksum              36238
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_original_sample_id 'compound 1'
_olex2_submission_special_instructions 'No special instructions were received'