Tris(1,4,7,10-tetraoxa-13,16-dithiacyclooctadecane-<i>S</i>,<i>S</i>')ruthenium(II) Bis(hexafluorophosphate)‒Water‒Methanol (1/2/1)
Blake, A. J.; Radek, C.; Schröder, M.; Acta Crystallographica Section C 52 (1996) 1401–1403; doi:10.1107/S0108270196001497

data_2004943
_publ_section_title
;Tris(1,4,7,10-tetraoxa-13,16-dithiacyclooctadecane-<i>S</i>,<i>S</i>')ruthenium(II)
 Bis(hexafluorophosphate)--Water--Methanol (1/2/1)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1401
_journal_page_last               1403
_journal_paper_doi               10.1107/S0108270196001497
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac
'[Ru (C12 H24 O4 S2)3](P F6)2, 2H2 O1, C1 H4 O1'
_chemical_formula_moiety
'C36 H72 O12 S6 Ru 2+,2(P F6 -),2(H2 O),C H3 O H'
_chemical_formula_sum            'C37 H80 F12 O15 P2 Ru S6'
_chemical_formula_weight         1348.19
_chemical_name_systematic
;
Tris(1,4,7,10-tetraoxa-13,16-dithiacyclooctadecane)ruthenium(II)
bis(hexafluorophosphate) dihydrate methanol solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.629(2)
_cell_length_b                   18.629(2)
_cell_length_c                   29.863(5)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     8975(2)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       'learnt-profile (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3380
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      1.49
_exptl_crystal_density_method    flotation
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment
;
H atoms riding with U~iso~(H) = 1.2U~eq~(C); water and methanol
H atoms not located
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.251
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_obs          0.0361
_refine_ls_shift/esd_max         0.30
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.060P)^2^ + 42.41P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1275
_refine_ls_wR_factor_obs         0.1002
_reflns_number_observed          2270
_reflns_number_total             2608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1354.cif
_cod_data_source_block           rusoox
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-01-27
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               2004943