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_1556668
_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_moiety         'C24 H30 B4 O4 W3'
_chemical_formula_sum            'C24 H30 B4 O4 W3'
_chemical_formula_weight         977.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                85.443(4)
_cell_angle_beta                 79.671(3)
_cell_angle_gamma                70.858(3)
_cell_formula_units_Z            8
_cell_length_a                   16.8420(15)
_cell_length_b                   19.051(2)
_cell_length_c                   19.390(2)
_cell_measurement_reflns_used    9464
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.26
_cell_volume                     5780.8(10)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            172558
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.948
_exptl_absorpt_coefficient_mu    11.937
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_refine_diff_density_max         13.677
_refine_diff_density_min         -12.441
_refine_diff_density_rms         0.479
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         20278
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+895.0753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17986
_reflns_number_total             20278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Compound_3.cif
_cod_data_source_block           SGGR2
_cod_original_cell_volume        5780.6(10)
_cod_database_code               1556668
_shelx_estimated_absorpt_t_min   0.154
_shelx_estimated_absorpt_t_max   0.489
_shelx_res_checksum              95427
_shelx_hkl_checksum              93166