Reactions of [Ru(NO)Cl<sub>5</sub>]<sup>2-</sup> with pseudotrilacunary {XW<sub>9</sub>O<sub>33</sub>}<sup>9-</sup> (X = As<sup>III</sup>, Sb<sup>III</sup>) anions.
Mukhacheva, Anna A.; Shmakova, Alexandra A.; Volchek, Victoria V.; Romanova, Tamara E.; Benassi, Enrico; Gushchin, Artem L.; Yanshole, Vadim; Sheven, Dmitri G.; Kompankov, Nikolay B.; Abramov, Pavel A.; Sokolov, Maxim N.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15989–15999; doi:10.1039/c9dt03328a

data_7701659
_publ_section_title
;
 Reactions of [Ru(NO)Cl<sub>5</sub>]<sup>2-</sup> with pseudotrilacunary
 {XW<sub>9</sub>O<sub>33</sub>}<sup>9-</sup> (X = As<sup>III</sup>,
 Sb<sup>III</sup>) anions.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15989
_journal_page_last               15999
_journal_paper_doi               10.1039/c9dt03328a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C8 H24 N4 O62 Ru1.02 Sb W16.98'
_chemical_formula_weight         4514.94
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-09-05 deposited with the CCDC.	2019-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.1706(14)
_cell_length_b                   21.1706(14)
_cell_length_c                   15.680(2)
_cell_measurement_reflns_used    2159
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.2410
_cell_measurement_theta_min      2.5390
_cell_volume                     6086.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5031
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.670
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    24.556
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.696
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             5845
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.157
_refine_diff_density_max         1.675
_refine_diff_density_min         -2.406
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+364.2240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1079
_reflns_number_total             1353
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c9dt03328a2.cif
_cod_data_source_block           DMA2
_cod_original_cell_volume        6086.0(11)
_cod_original_sg_symbol_Hall     '-R 3 2'
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7701659
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.057
_shelx_estimated_absorpt_t_max   0.113
_shelx_res_checksum              67638