Synthesis and crystal structure of nonacarbonyltris[(2-thia-1,3,5-triaza-7-phosphatricylco[3.3.1.1]decane-κ1 P)-2,2-dioxide]triruthenium(0) – acetonitrile (7/6), C25.71H32.57N9.86O15P3S3Ru3
Ebong, Wisdom; Muniz, Alexandra E.; Khan, David R.; Unruh, Daniel K.; Yarbrough, Jason C.; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 17–21; doi:10.1515/ncrs-2021-0359

data_8104950
_publ_section_title
;
 Synthesis and crystal structure of
 nonacarbonyltris[(2-thia-1,3,5-triaza-7-phosphatricylco[3.3.1.1]decane-\k1
 P)-2,2-dioxide]triruthenium(0)&#x00A0;-- acetonitrile (7/6),
 C25.71H32.57N9.86O15P3S3Ru3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              17
_journal_page_last               21
_journal_paper_doi               10.1515/ncrs-2021-0359
_journal_volume                  237
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_sum            'C25.71 H32.57 N9.86 O15 P3 Ru3 S3'
_chemical_formula_weight         1212.06
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            14
_cell_length_a                   37.24213(9)
_cell_length_b                   37.24213(9)
_cell_length_c                   11.64828(3)
_cell_measurement_reflns_used    128816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.314
_cell_measurement_theta_min      3.604
_cell_volume                     13991.41(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0228736
_diffrn_orient_matrix_UB_12      0.0207807
_diffrn_orient_matrix_UB_13      -0.0535091
_diffrn_orient_matrix_UB_21      0.03927
_diffrn_orient_matrix_UB_22      0.0293866
_diffrn_orient_matrix_UB_23      -0.0684288
_diffrn_orient_matrix_UB_31      -0.014668
_diffrn_orient_matrix_UB_32      -0.031366
_diffrn_orient_matrix_UB_33      -0.099796
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            180987
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.364
_diffrn_reflns_theta_min         2.373
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.372
_exptl_absorpt_correction_T_max  0.09638
_exptl_absorpt_correction_T_min  0.01549
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
        Spherical absorption correction
        using equivalent radius and absorption coefficient.
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       column
_exptl_crystal_F_000             8412
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.054
_exptl_crystal_size_rad          0.045
_refine_diff_density_max         1.56
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details
;
 Flack x determined using 8783 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         19572
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                19241
_reflns_number_total             19572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0359_suppl.cif
_cod_data_source_block           yar20_01
_cod_original_cell_volume        13991.40(8)
_cod_database_code               8104950
_shelx_estimated_absorpt_t_min   0.21
_shelx_estimated_absorpt_t_max   0.555