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

data_1518917
_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
'C42 H84 Br3 P6 S4 W3, Br, 2(C H2 Cl2), C7 H8'
_chemical_formula_sum            'C51 H96 Br4 Cl4 P6 S4 W3'
_chemical_formula_weight         2036.32
_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     iterative
_cell_angle_alpha                90
_cell_angle_beta                 98.1070(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.97738(16)
_cell_length_b                   19.6767(3)
_cell_length_c                   14.88601(19)
_cell_measurement_temperature    293(2)
_cell_volume                     3473.20(8)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.940
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            76264
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.402
_diffrn_reflns_theta_min         2.912
_exptl_absorpt_coefficient_mu    7.702
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       prism
_exptl_crystal_F_000             1972
_exptl_crystal_recrystallization_method
'slow vapour diffusion of toluene into a sample solution in CH2Cl2'
_exptl_crystal_size_max          0.1924
_exptl_crystal_size_mid          0.1594
_exptl_crystal_size_min          0.1197
_refine_diff_density_max         5.319
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details
;
 Flack x determined using 7481 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         17297
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0411P)^2^+16.4900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                16603
_reflns_number_total             17297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2015-424-248-253-1.cif
_cod_data_source_block           str1621_superflip
_cod_original_cell_volume        3473.21(8)
_cod_database_code               1518917
_shelx_res_checksum              55463