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_1556664
_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_formula_sum            'C24 H37 B4 Cr O4 W2'
_chemical_formula_weight         852.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.323(5)
_cell_length_b                   14.555(3)
_cell_length_c                   17.009(7)
_cell_measurement_reflns_used    4562
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.1
_cell_measurement_theta_min      3.2
_cell_volume                     5774(3)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker axs Kappa Apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2742
_diffrn_reflns_av_unetI/netI     0.2855
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37242
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.509
_diffrn_reflns_theta_max         24.509
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    8.346
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.296
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         8977
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.2386
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.2215
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3645
_reflns_number_total             8977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Compound_1.cif
_cod_data_source_block           wcrnew
_cod_database_code               1556664
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.555
_shelx_res_checksum              78216
_shelx_hkl_checksum              51614