Synthesis, Characterization, and Electronic Structure of New Type of Heterometallic Boride Clusters
Shubhankar Kumar Bose; K. Geetharani; Satyanarayan Sahoo; K. Hari Krishna Reddy; Babu Varghese; Eluvathingal D. Jemmis; Sundargopal Ghosh; Inorganic Chemistry 50 (2011) 9414–9422; doi:10.1021/ic201046g

data_4326330
_publ_section_title
;
 Synthesis, Characterization, and Electronic Structure of New Type of
 Heterometallic Boride Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9414
_journal_page_last               9422
_journal_paper_doi               10.1021/ic201046g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C26 H37 B3 Fe2 O7 Ta2'
_chemical_formula_weight         967.59
_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                90.000(5)
_cell_angle_beta                 97.544(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   10.362(5)
_cell_length_b                   8.747(5)
_cell_length_c                   34.653(5)
_cell_measurement_reflns_used    7313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2.6
_cell_volume                     3114(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker axs Kappa apex 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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            40277
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.29
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.959
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.504
_refine_diff_density_min         -3.095
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.00030(4)
_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   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         10977
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+21.4936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                8894
_reflns_number_total             10977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201046g_si_002_2.cif
_cod_data_source_block           goshtab6fe
_cod_database_code               4326330