The Trigonal Prismatic Cluster Compound W6CCl15 and a Carambolage of Tungsten Clusters in the Structure of the Heteroleptic Cluster Compound W30C2(Cl,Br)68
Markus Ströbele; H.-Jürgen Meyer; Inorganic Chemistry 49 (2010) 5986–5991; doi:10.1021/ic100516t

data_4315923
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie
Ob dem Himmelreich 7
72074 T\"ubingen
Bundesrepublik Deutschland
;
_publ_contact_author_email       juergen.meyer@uni-tuebingen.de
_publ_contact_author_fax         '07071 29-5702'
_publ_contact_author_name        'H.-J\"urgen Meyer'
_publ_contact_author_phone       '07071 29-76226'
_publ_section_title
;
 The Trigonal Prismatic Cluster Compound W6CCl15 and a Carambolage of
 Tungsten Clusters in the Structure of the Heteroleptic Cluster Compound
 W30C2(Cl,Br)68
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5986
_journal_page_last               5991
_journal_paper_doi               10.1021/ic100516t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         W30C2Cl36.8Br31.182
_chemical_formula_sum            'C2 Br31.182 Cl36.8 W30'
_chemical_formula_weight         9337.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.75(2)
_cell_angle_beta                 68.85(2)
_cell_angle_gamma                71.19(2)
_cell_formula_units_Z            1
_cell_length_a                   12.003(2)
_cell_length_b                   14.862(3)
_cell_length_c                   15.792(3)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.12
_cell_volume                     2472.7(9)
_computing_cell_refinement       'STOE IPDS I SOFTWARE'
_computing_data_collection       'STOE IPDS I SOFTWARE'
_computing_data_reduction        'STOE IPDS I SOFTWARE'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  'Word XP'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       Oscillation
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28335
_diffrn_reflns_theta_full        24.90
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0.0001
_exptl_absorpt_coefficient_mu    48.324
_exptl_absorpt_correction_T_max  0.1041
_exptl_absorpt_correction_T_min  0.0118
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'HABITUS, STOE X-Shape/X-Red'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3949.6
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.408
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                6509
_reflns_number_total             8077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100516t_si_001_2.cif
_cod_data_source_block           W30C2(Cl,Br)68
_cod_original_cell_volume        2472.9(8)
_cod_original_formula_sum        'C2 Br31.182 Cl36.80 W30'
_cod_database_code               4315923