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_7231648
_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            'C12 H42 Ce4 N6 Na4 O94.7 Si2 W18'
_chemical_formula_weight         5803.64
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-12
_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                79.2760(19)
_cell_angle_beta                 75.0343(17)
_cell_angle_gamma                65.2698(15)
_cell_formula_units_Z            1
_cell_length_a                   12.7662(4)
_cell_length_b                   13.7583(5)
_cell_length_c                   15.2105(6)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.24
_cell_volume                     2334.97(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.526
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.139
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1234 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.5581. 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    4.127
_exptl_crystal_description       block
_exptl_crystal_F_000             2550
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.773
_refine_diff_density_min         -2.123
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0244P)^2^+14.1615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12288
_reflns_number_total             14135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01447g2.cif
_cod_data_source_block           kns02
_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            'C6 H21 Ce2 N3 Na2 O47.35 Si W9'
_cod_original_formula_weight         2901.82
_cod_original_formula_moiety
'C6 H13 Ce2 N Na2 O45.35 Si W9, 2(O), 2(H4 N)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2334.98(15)
_cod_database_code               7231648
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 N2-H2D = N2-H2C = N2-H2E = N2-H2F
 0.91 with sigma of 0.02
 N3-H3E = N3-H3D = N3-H3C
 0.91 with sigma of 0.02
 H2F-H2D
 1.486 with sigma of 0.04
 H2D-H2C
 1.486 with sigma of 0.04
 H2D-H2E
 1.486 with sigma of 0.04
 H2E-H2F
 1.486 with sigma of 0.04
 H2E-H2C
 1.486 with sigma of 0.04
 H2C-H2F
 1.486 with sigma of 0.04
 H3E-H3D
 1.486 with sigma of 0.04
 H3E-H3C
 1.486 with sigma of 0.04
 H3E-H3F
 1.486 with sigma of 0.04
 H3D-H3C
 1.486 with sigma of 0.04
 H3D-H3F
 1.486 with sigma of 0.04
 H3F-H3C
 1.486 with sigma of 0.04
3. Others
 Fixed Sof: Na2(0.5) OW11(0.5) OW4(0.5) OW3(0.35)
 Fixed Uiso: H2F(0.02) H3F(0.04)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B), C6(H6A,H6B), C5(H5A,H5B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              95162
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'