Synthesis and Structure of Trinuclear W3S4 Clusters Bearing Aminophosphine Ligands and Their Reactivity toward Halides and Pseudohalides.
Beltrán, Tomás F; Pino-Chamorro, Jose Ángel; Fernández-Trujillo, M Jesús; Safont, Vicent S.; Basallote, Manuel G.; Llusar, Rosa; Inorganic chemistry 54 (2015) 607–618; doi:10.1021/ic5025313

data_4342053
_publ_section_title
;
 Synthesis and Structure of Trinuclear W3S4 Clusters Bearing
 Aminophosphine Ligands and Their Reactivity toward Halides and
 Pseudohalides.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              607
_journal_page_last               618
_journal_paper_doi               10.1021/ic5025313
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C42 H48 Br3 N3 P3 S4 W3, C24 H20 B, C2 H3 N, C4 O'
_chemical_formula_sum            'C72 H71 B Br3 N4 O P3 S4 W3'
_chemical_formula_weight         2031.57
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-05-07
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                101.274(3)
_cell_angle_beta                 105.565(3)
_cell_angle_gamma                105.842(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1815(5)
_cell_length_b                   14.9361(5)
_cell_length_c                   20.2894(7)
_cell_measurement_reflns_used    21128
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      29.3857
_cell_measurement_theta_min      2.8328
_cell_volume                     3811.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -100.00  -58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4378  178.0000   60.0000 42

  2 omega    1.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4378  -99.0000   90.0000 27

  3 omega  -19.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4378  -99.0000    0.0000 50

  4 omega  -11.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4378  -99.0000  -60.0000 42

  5 omega  -77.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9066    0.0000  -90.0000 176

  6 omega    9.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9066  -99.0000   30.0000 27

  7 omega    0.00   27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9066  -57.0000   30.0000 27

  8 omega   14.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9066  -99.0000  120.0000 27

  9 omega   35.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9066  178.0000    0.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0193865000
_diffrn_orient_matrix_UB_12      -0.0319746000
_diffrn_orient_matrix_UB_13      -0.0186088000
_diffrn_orient_matrix_UB_21      -0.0266357000
_diffrn_orient_matrix_UB_22      0.0064684000
_diffrn_orient_matrix_UB_23      -0.0327175000
_diffrn_orient_matrix_UB_31      0.0444221000
_diffrn_orient_matrix_UB_32      0.0399540000
_diffrn_orient_matrix_UB_33      0.0046011000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.1760
_exptl_crystal_size_mid          0.1280
_exptl_crystal_size_min          0.0637
_refine_diff_density_max         2.725
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13412
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+10.6808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                11547
_reflns_number_total             13412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5025313_si_002.cif
_cod_data_source_block           str1359
_cod_depositor_comments
'Adding full bibliography for 4342053--4342056.cif.'
_cod_original_cell_volume        3811.6(2)
_cod_database_code               4342053
_chemical_oxdiff_formula         'C66 H68 B Br3 P3 N3 S4 W3'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32