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_7711574
_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         'C45 H46 B K Mo O9 Si, C H2 Cl2'
_chemical_formula_sum            'C46 H48 B Cl2 K Mo O9 Si'
_chemical_formula_weight         989.68
_chemical_name_common            'borataphenanthrene Mo(CO)3 complex'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-26 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3096(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3574(3)
_cell_length_b                   32.3930(7)
_cell_length_c                   9.8045(2)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.59
_cell_measurement_theta_min      2.98
_cell_volume                     4455.04(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            42894
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         2.380
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 5259 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.021(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10932
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.989
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                10780
_reflns_number_total             10932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02795j2.cif
_cod_data_source_block           CDM407_1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7711574
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H3), C7(H4), C8(H5), C9(H6), C10(H9), C11(H10), C12(H11), C13(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28), C29(H29),
  C30(H30), C37(H37), C38(H38), C39(H39), C40(H40)
1.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              11270
_shelx_hkl_checksum              58828