Enantioselective synthesis of tungsten trimetallic cluster chalcogenides
Eva M. Guillamon; Marta Blasco; Rosa Llusar; Inorganica Chimica Acta 424 (2015) 248–253; doi:

data_1518919
_publ_section_title
;
 Enantioselective synthesis of tungsten trimetallic cluster chalcogenides
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              248
_journal_page_last               253
_journal_volume                  424
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C54 H84 Br3 P6 S4 W3, Br, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H88 Br4 Cl4 P6 S4 W3'
_chemical_formula_weight         2088.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.6703(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.02802(15)
_cell_length_b                   24.0309(3)
_cell_length_c                   12.3079(2)
_cell_measurement_reflns_used    17661
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.4320
_cell_measurement_theta_min      3.3700
_cell_volume                     3557.28(9)
_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(2)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
  1 omega  -82.30  -55.00   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  178.0000  150.0000 39

  2 omega  -68.00   12.50   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -37.0000    0.0000 115

  3 omega  -20.00    5.20   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   60.0000 36

  4 omega   -7.00   20.30   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   90.0000 39

  5 omega  -64.00   48.00   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -77.0000 -150.0000 160

  6 omega  -92.00   13.00   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -57.0000  -90.0000 150

  7 omega  -50.00   69.00   0.7000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877   77.0000    0.0000 170
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0034457000
_diffrn_orient_matrix_UB_12      -0.0014355000
_diffrn_orient_matrix_UB_13      0.0574384000
_diffrn_orient_matrix_UB_21      -0.0238353000
_diffrn_orient_matrix_UB_22      0.0269892000
_diffrn_orient_matrix_UB_23      0.0009250000
_diffrn_orient_matrix_UB_31      -0.0538208000
_diffrn_orient_matrix_UB_32      -0.0118574000
_diffrn_orient_matrix_UB_33      -0.0048360000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40359
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.195
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42117
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2016
_exptl_crystal_recrystallization_method
'slow vapour diffusion of diethyl ether into a sample solution in CH2Cl2'
_exptl_crystal_size_max          0.3772
_exptl_crystal_size_mid          0.2463
_exptl_crystal_size_min          0.0282
_refine_diff_density_max         2.104
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Flack x determined using 5588 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         16591
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+18.0366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.788
_reflns_number_gt                14211
_reflns_number_total             16591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2015-424-248-253-3.cif
_cod_data_source_block           str1465
_cod_database_code               1518919
_shelx_res_checksum              13957