A Rh-substituted polyoxometalate with an acetate-modified building block {As<sub>2</sub>W<sub>22</sub>O<sub>76</sub>(CH<sub>3</sub>COO)<sub>2</sub>}.
Liu, Zhen; Zhang, Xue; Wan, Rong; Li, Huafeng; Hong, Yumei; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Chemical communications (Cambridge, England) 57 (2021) 10250–10253; doi:10.1039/d1cc03646g

data_7128876
_publ_section_title
;
 A Rh-substituted polyoxometalate with an acetate-modified building block
 {As<sub>2</sub>W<sub>22</sub>O<sub>76</sub>(CH<sub>3</sub>COO)<sub>2</sub>}.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10250
_journal_page_last               10253
_journal_paper_doi               10.1039/d1cc03646g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'0.25(C32 H72 As8 N8 Na8 O336 Rh8 W88), 8(C2 H8 N), 7(O)'
_chemical_formula_sum            'C24 H82 As2 N10 Na2 O91 Rh2 W22'
_chemical_formula_weight         6413.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-19 deposited with the CCDC.	2021-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.0469(11)
_cell_length_b                   12.2563(4)
_cell_length_c                   23.2462(6)
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.268
_cell_measurement_theta_min      2.352
_cell_volume                     10847.8(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35713
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.295
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    24.238
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1049 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.5364. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.927
_exptl_crystal_description       needle
_exptl_crystal_F_000             11320
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.409
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         9618
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+291.2592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8520
_reflns_number_total             9618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03646g2.cif
_cod_data_source_block           m5014_0m
_cod_depositor_comments          'Adding full bibliography for 7128876.cif.'
_cod_database_code               7128876
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.324
_shelx_estimated_absorpt_t_min   0.113
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3W) \\sim Ueq, Uanis(O5W) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: Na2(0.5) O3W(0.5) O4W(0.5) O5W(0.5) O8W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N2(H2D,H2E), N3(H3D,H3E), N4(H4A,H4B), N5(H5D,H5E)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              48028
_olex2_submission_special_instructions 'No special instructions were received'