Synthesis of Im3[Re3(μ3-S)(μ-S)3Br9]Br (Im = 1-Ethyl-3-methylimidazolium) by Means of an Ionic Liquid
Sakamoto, Hideshi; Watanabe, Yusuke; Saito, Taro; Inorganic Chemistry 45 (2006) 4578–4579; doi:10.1021/ic060428k

data_4332475
_publ_section_title
;
 Synthesis of Im3[Re3(\m3-S)(\m-S)3Br9]Br (Im =
 1-Ethyl-3-methylimidazolium) by Means of an Ionic Liquid
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4578
_journal_page_last               4579
_journal_paper_doi               10.1021/ic060428k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C18 H33 Br10 N6 Re3 S4'
_chemical_formula_weight         1819.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.691(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1806(6)
_cell_length_b                   19.2756(11)
_cell_length_c                   18.5823(12)
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.53
_cell_volume                     3977.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.366[pixels/mm]
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29879
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.387
_exptl_absorpt_correction_T_max  0.2473
_exptl_absorpt_correction_T_min  0.0478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.135
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         9867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                8175
_reflns_number_total             9867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060428ksup1.cif
_cod_data_source_block           imre3s4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332475