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_4326331
_publ_section_title
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 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            'C33 H32 B4 Fe6 Mo2 O13 Se2'
_chemical_formula_weight         1364.73
_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                 92.191(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6872(4)
_cell_length_b                   18.8944(5)
_cell_length_c                   16.9128(5)
_cell_measurement_reflns_used    23661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7605
_cell_measurement_theta_min      2.9714
_cell_volume                     4370.6(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.211
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
There were two peaks in the difference Fourier map which
could not be modelled as meaningful solvents. Platon 
squeeze was applied to produce intensity data devoid of the
scattering contribution from solvents.The squeeze results
are as listed above.
;
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                4805
_reflns_number_total             7680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201046g_si_002_3.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4326331