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_4342055
_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 H45 Cl3 N3 P3 S4 W3, C24 H20 B, C Cl2'
_chemical_formula_sum            'C67 H66 B Cl5 N3 P3 S4 W3'
_chemical_formula_weight         1873.98
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_cell_angle_alpha                100.7043(14)
_cell_angle_beta                 100.8016(14)
_cell_angle_gamma                108.1880(17)
_cell_formula_units_Z            2
_cell_length_a                   13.6639(3)
_cell_length_b                   15.5155(3)
_cell_length_c                   18.3338(3)
_cell_measurement_reflns_used    32319
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      29.0110
_cell_measurement_theta_min      3.1910
_cell_volume                     3500.76(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.00(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  -92.00  -64.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  178.0000    0.0000 40

  2 omega  -20.00   28.30   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000  -30.0000 69

  3 omega -103.00  -56.80   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  178.0000  120.0000 66

  4 omega  -12.00   14.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   60.0000 38

  5 omega  -62.00   21.30   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -57.0000  -60.0000 119

  6 omega  -34.00   93.40   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   19.0000  120.0000 182

  7 omega   33.00   72.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   39.0000 -128.0000 56

  8 omega   -5.00   26.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   39.0000 -128.0000 45

  9 omega -106.00  -57.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877 -178.0000 -120.0000 70

 10 omega  -20.00   59.10   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -99.0000  150.0000 113

 11 omega  -17.00   94.30   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   37.0000  120.0000 159

 12 omega  -65.00   44.90   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -37.0000  -30.0000 157
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0475149000
_diffrn_orient_matrix_UB_12      -0.0053460000
_diffrn_orient_matrix_UB_13      0.0182810000
_diffrn_orient_matrix_UB_21      -0.0272764000
_diffrn_orient_matrix_UB_22      -0.0492898000
_diffrn_orient_matrix_UB_23      -0.0090096000
_diffrn_orient_matrix_UB_31      0.0143366000
_diffrn_orient_matrix_UB_32      -0.0052651000
_diffrn_orient_matrix_UB_33      -0.0353549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58146
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.846
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         13744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+21.6530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12285
_reflns_number_total             13744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025313_si_003.cif
_cod_data_source_block           str1512
_cod_depositor_comments
'Adding full bibliography for 4342053--4342056.cif.'
_cod_original_cell_volume        3500.73(11)
_cod_database_code               4342055
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C H N3 P3 B Cl3 S4 W3'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: C42(0.67) C41(0.67) C41A(0.33) C42A(0.33) C67(0.73) C67A(0.27)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C16(H16A,H16B), C29(H29A,H29B), C30(H30A,H30B), C1(H1C,H1D),
 C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C14(H14), C8(H8), C53(H53), C54(H54), C50(H50), C48(H48),
 C60(H60), C66(H66), C56(H56), C62(H62), C4(H4), C59(H59), C21(H21), C22(H22),
 C13(H13), C10(H10), C57(H57), C64(H64), C63(H63), C12(H12), C65(H65), C44(H44),
  C46(H46), C45(H45), C47(H47), C32(H32), C58(H58), C33(H33), C34(H34),
 C11(H11), C7(H7), C6(H6), C20(H20), C38(H38), C39(H39), C5(H5), C18(H18),
 C28(H28), C27(H27), C36(H36), C19(H19), C24(H24), C35(H35), C26(H26), C25(H25)
;
_shelx_res_checksum              53083
_shelx_hkl_checksum              60275
_olex2_submission_special_instructions 'No special instructions were received'