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_4342056
_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_absolute_configuration ad
_chemical_formula_moiety
'C45 H42 N6 P3 S7 W3, C45 H24 N6 P3 S7 W3, 2(F6 P1)'
_chemical_formula_sum            'C90 H66 F12 N12 P8 S14 W6'
_chemical_formula_weight         3343.25
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-08
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.3126(3)
_cell_length_b                   16.3126(3)
_cell_length_c                   27.3343(4)
_cell_measurement_reflns_used    18145
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9010
_cell_measurement_theta_min      3.1180
_cell_volume                     6299.19(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 20.8101
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9818
_diffrn_measurement_details
;
  1 omega  -68.00  -40.70   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  178.0000  -90.0000 39

  2 omega -124.00  -91.80   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  178.0000  -90.0000 46

  3 omega  -49.00   42.00   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307   38.0000   60.0000 130

  4 omega   27.00   87.90   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000   30.0000 87

  5 omega   28.00   92.40   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000  -30.0000 92

  6 omega   65.00   92.30   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000 -180.0000 39

  7 omega   28.00  154.70   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   15.0000  -30.0000 181

  8 omega -121.00   -1.30   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -77.0000   60.0000 171

  9 omega -115.00   -5.10   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000  -90.0000 157

 10 omega  100.00  177.70   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000  -30.0000 111

 11 omega   76.00  178.20   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000   30.0000 146

 12 omega   25.00  116.00   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524 -111.0000  -30.0000 130

 13 omega   75.00  178.60   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000  120.0000 148

 14 omega -115.00   -5.10   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000  150.0000 157

 15 omega   57.00   94.80   0.7000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       37.7307  178.0000  -60.0000 54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0320597000
_diffrn_orient_matrix_UB_12      0.0230010000
_diffrn_orient_matrix_UB_13      -0.0485759000
_diffrn_orient_matrix_UB_21      0.0026260000
_diffrn_orient_matrix_UB_22      0.0867951000
_diffrn_orient_matrix_UB_23      0.0239366000
_diffrn_orient_matrix_UB_31      0.1041975000
_diffrn_orient_matrix_UB_32      0.0618170000
_diffrn_orient_matrix_UB_33      -0.0155460000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36371
_diffrn_reflns_theta_full        72.04
_diffrn_reflns_theta_max         72.04
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           n/a
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    13.481
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.1407
_exptl_crystal_size_mid          0.1166
_exptl_crystal_size_min          0.0657
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0706P)^2^+7.2753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                7546
_reflns_number_total             8136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5025313_si_005.cif
_cod_data_source_block           str1614
_cod_depositor_comments
'Adding full bibliography for 4342053--4342056.cif.'
_cod_original_cell_volume        6299.22(18)
_cod_database_code               4342056
_chemical_oxdiff_formula         'C45 H48 F6 N6 P4 S7 W3'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'