Assessing the Donor Ability of Boratabenzene and 9-Borataphenanthrene Anions through Metal Complexes with Carbonyl Ligands
Rojales, Katherine; Masilamani, Tamizmani; Bartholome, Tyler A.; Martin, Caleb Daniel; Dalton Transactions  (2022) –; doi:10.1039/D2DT02795J

data_7711577
_publ_section_title
;
 Assessing the Donor Ability of Boratabenzene and 9-Borataphenanthrene
 Anions through Metal Complexes with Carbonyl Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02795J
_journal_year                    2022
_chemical_formula_moiety         'C66 H100 B2 K2 O18 Si2 W2'
_chemical_formula_sum            'C66 H100 B2 K2 O18 Si2 W2'
_chemical_formula_weight         1705.14
_chemical_name_common            'TMB-boratabenzene W(CO)3 complex'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2022-08-26 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1180(10)
_cell_length_b                   11.7793(3)
_cell_length_c                   20.0868(6)
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.99
_cell_measurement_theta_min      2.57
_cell_volume                     7445.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            93320
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    3.295
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9237
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.413
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+13.7187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8234
_reflns_number_total             9237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02795j2.cif
_cod_data_source_block           CDM429_1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7711577
_shelx_estimated_absorpt_t_min   0.510
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2013-3
_shelx_res_checksum              56275
_shelx_hkl_checksum              40091