C–H Bond Activation at Antimony(III): Synthesis and Reactivity of Sb(III)-Oxyaryl Species
Dunes, Gabriel; Cordier, Marie; Kahlal, Samia; Pollnitz, Alpar; Saillard, Jean-Yves; Silvestru, Cristian; Sarazin, Yann; Dalton Transactions  (2024) –; doi:10.1039/D4DT01400F

data_7716309
_publ_section_title
;
 C--H Bond Activation at Antimony(III): Synthesis and Reactivity of
 Sb(III)-Oxyaryl Species
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D4DT01400F
_journal_year                    2024
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H40 N2 O Sb, C D2 Cl2, Cl'
_chemical_formula_sum            'C27 H40 Cl3 D2 N2 O Sb'
_chemical_formula_weight         640.74
_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   mixed
_atom_sites_solution_primary     dual
_audit_update_record
;
2024-02-28 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.303(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7009(8)
_cell_length_b                   17.2182(17)
_cell_length_c                   18.3636(18)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4363
_cell_measurement_theta_min      2.3657
_cell_measurement_wavelength     0.710730
_cell_volume                     2996.9(5)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2023)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0497011
_diffrn_orient_matrix_UB_12      -0.0453640
_diffrn_orient_matrix_UB_13      0.0279145
_diffrn_orient_matrix_UB_21      -0.0102147
_diffrn_orient_matrix_UB_22      0.0241642
_diffrn_orient_matrix_UB_23      0.0480871
_diffrn_orient_matrix_UB_31      -0.0925046
_diffrn_orient_matrix_UB_32      -0.0270416
_diffrn_orient_matrix_UB_33      -0.0038580
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            36748
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.366
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6833
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+4.5420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                6762
_reflns_number_total             6833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt01400f3.cif
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C27 H40 D2 Cl3 N2 O Sb'
_cod_database_code               7716309
_shelx_res_checksum              43541