Synthesis, Structures and Chemistry of the Metallaboranes of Group 4-9 with M2B5 Core Having a Cross Cluster M-M Bond
Bag, R.; Saha, S.; Borthakur, R.; Mondal, B.; Roisnel, T.; Dorcet, V.; Halet, J.-F.; Ghosh, S.; Inorganics 7 (2019) 27–; doi:10.3390/inorganics7030027

data_1556666
_publ_section_title
;
 Synthesis, Structures and Chemistry of the Metallaboranes of Group 4-9
 with M2B5 Core Having a Cross Cluster M-M Bond
;
_journal_name_full               Inorganics
_journal_page_first              27
_journal_paper_doi               10.3390/inorganics7030027
_journal_volume                  7
_journal_year                    2019
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H38 B4 Fe O3 W2'
_chemical_formula_sum            'C23 H38 B4 Fe O3 W2'
_chemical_formula_weight         829.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 110.538(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6885(13)
_cell_length_b                   16.2795(16)
_cell_length_c                   15.0773(17)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5267
_cell_measurement_theta_min      2.5022
_cell_measurement_wavelength     0.71073
_cell_volume                     2686.6(5)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42572
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.999
_exptl_absorpt_coefficient_mu    9.097
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.496
_refine_diff_density_min         -2.129
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+10.0436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5606
_reflns_number_total             6147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Compound_4.cif
_cod_data_source_block           SGGRB4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1556666
_shelx_res_checksum              45915
_shelx_hkl_checksum              92241