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

data_1518918
_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 Se4 W3, F6 P1'
_chemical_formula_sum            'C42 H84 Br3 F6 P7 Se4 W3'
_chemical_formula_weight         2027.00
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.6097(11)
_cell_length_b                   15.6097(11)
_cell_length_c                   23.225(3)
_cell_measurement_reflns_used    5236
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.956
_cell_measurement_theta_min      2.312
_cell_volume                     4900.9(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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9032
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         2.312
_exptl_absorpt_coefficient_mu    9.547
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.853828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.1084 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.8538.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2874
_exptl_crystal_recrystallization_method
'slow vapour diffusion of diethyl ether into a sample solution in CH2Cl2'
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 1044 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.032(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_full    0.599
_reflns_Friedel_fraction_max     0.614
_reflns_number_gt                2890
_reflns_number_total             3092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2015-424-248-253-2.cif
_cod_data_source_block           str649
_cod_original_cell_volume        4900.9(10)
_cod_database_code               1518918
_shelx_res_checksum              96844