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_7231646
_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_sum            'C10 H22 Ce4 K4 N2 Na4 O98 Si2 W18'
_chemical_formula_weight         5912.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                79.826(2)
_cell_angle_beta                 74.283(2)
_cell_angle_gamma                65.695(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8048(9)
_cell_length_b                   13.6116(9)
_cell_length_c                   15.3227(11)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.49
_cell_volume                     2336.5(3)
_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      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41566
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.303
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1161 before and 0.0682 after correction. The Ratio of minimum to maximum transmission is 0.5522. The \l/2 correction factor is Not present.'
_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    4.202
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.850
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         9482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0515P)^2^+5.5997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8361
_reflns_number_total             9482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01447g2.cif
_cod_data_source_block           test
_cod_depositor_comments
;
Adding full bibliography for 7231646--7231650.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C5 H11 Ce2 K2 N Na2 O49 Si W9'
_cod_original_formula_weight         2956.31
_cod_original_formula_moiety         'C5 H11 Ce2 K2 N Na2 O48 Si W9, O'
_cod_original_formula_units_Z            2
_cod_database_code               7231646
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              76727
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'