A synchrotron study of μ~3~-chloro-tri-μ-chloro-μ~3~-sulfido-hexakis(triphenylphospine)triruthenium(II)‒tetrahydrofuran‒water (1/1.25/0.75)
Vicki-Anne Tolhurst; David Cookson; Peter Turner; Acta Crystallographica Section E 59 (2003) m218–m219; doi:10.1107/S1600536803006573

data_2202186
_publ_section_title
;A synchrotron study of
 \m~3~-chloro-tri-\m-chloro-\m~3~-sulfido-hexakis(triphenylphospine)triruthenium(II)--tetrahydrofuran--water
 (1/1.25/0.75)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m218
_journal_page_last               m219
_journal_paper_doi               10.1107/S1600536803006573
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Ru3 Cl4 S (C18 H15 P1)6], 1.25C4 H8 O, 0.75 H2 O'
_chemical_formula_moiety         'C108H90Cl4P6Ru3S, 1.25C4H8O, 0.75H2O'
_chemical_formula_sum            'C113 H100 Cl4 O2 P6 Ru3 S'
_chemical_formula_weight         2152.82
_chemical_name_common
;
'\m~3~-Chloro-tri-\m-chloro-\m~3~-
sulfidohexakis (triphenylphospine)triruthenium(II)
;
_chemical_name_systematic
;
\m~3~-Chloro-tri-\m-chloro- 1\k^2^Cl,2\k^2^Cl,3\k^2^Cl-triangulo-\m~3~
-sulfidohexakis(triphenylphosphine)triruthenium(II)--tetrahydrofuran--water
(1/1.25/0.75)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.904(11)
_cell_angle_beta                 92.328(11)
_cell_angle_gamma                102.784(11)
_cell_formula_units_Z            2
_cell_length_a                   14.183(4)
_cell_length_b                   14.699(5)
_cell_length_c                   25.814(9)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      19.4
_cell_measurement_theta_min      2.3
_cell_volume                     5239(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART--KAPPA (Bruker, 2001)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2001)'
_computing_molecular_graphics
;
TEXSAN for Windows (Molecular Structure Corporation, 1997),
Xtal3.6 (Hall et al., 1999),
ORTEPII (Johnson, 1976) and WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type
;
SMART 6000 detector mounted on a Bruker Kappa Platform
;
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  'Double Diamond 111'
_diffrn_radiation_source         'ChemMatCARS, APS, Argonne National Lab, USA'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.55940
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            109758
_diffrn_reflns_theta_full        19.0
_diffrn_reflns_theta_max         19.0
_diffrn_reflns_theta_min         1.3
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessings, 1995; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.42
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         15139
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.42
_refine_ls_R_factor_all          0.116
_refine_ls_R_factor_gt           0.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.06P)^2^+6P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.223
_refine_ls_wR_factor_ref         0.243
_reflns_number_gt                12160
_reflns_number_total             15139
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6099.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Replacing the "\K" substring with the "\k" substring in the
 _chemical_name_systematic data item value.

 Antanas Vaitkus,
 2017-03-29
;
_cod_database_code               2202186
_cod_database_fobs_code          2202186