Cluster Expansion Reactions of Group 6 and 8 Metallaboranes Using Transition Metal Carbonyl Compounds of Groups 7-9
K. Geetharani; Shubhankar Kumar Bose; Satyanarayan Sahoo; Babu Varghese; Shaikh M. Mobin; Sundargopal Ghosh; Inorganic Chemistry 50 (2011) 5824–5832; doi:10.1021/ic200802c

data_4325456
_publ_section_title
;
 Cluster Expansion Reactions of Group 6 and 8 Metallaboranes Using
 Transition Metal Carbonyl Compounds of Groups 7-9
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5824
_journal_page_last               5832
_journal_paper_doi               10.1021/ic200802c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C31.5 H38 B4 Fe2 Mo2 O5.5 Se2'
_chemical_formula_weight         1009.36
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.939(3)
_cell_angle_beta                 97.194(2)
_cell_angle_gamma                119.025(2)
_cell_formula_units_Z            12
_cell_length_a                   18.0715(9)
_cell_length_b                   18.3109(9)
_cell_length_c                   41.907(2)
_cell_measurement_reflns_used    8221
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.6
_cell_volume                     11929.4(10)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1452
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            135275
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.99
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       needle
_exptl_crystal_F_000             5940
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.193
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.422
_refine_ls_extinction_coef       0.00098(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2560
_refine_ls_number_reflns         135275
_refine_ls_number_restraints     2328
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1839
_refine_ls_R_factor_gt           0.1280
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+1157.0714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3117
_refine_ls_wR_factor_ref         0.3417
_reflns_number_gt                85007
_reflns_number_total             135275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200802c_si_001_4.cif
_cod_data_source_block           new2
_cod_original_cell_volume        11929.4(11)
_cod_database_code               4325456