Coordinative Unsaturation in an Antimony(III)-Complex with the 2-Salicylidenaminophenolato Ligand: Synthesis, Crystal Structure, Spectroscopic Analysis, and DFT Studies
Knerr, Steven; Böhme, Uwe; Herbig, Marcus; Crystals 13 (2023) 1300–; doi:10.3390/cryst13091300

data_1569818
_publ_contact_author
;Uwe B\"ohme 
 Institut f\"ur Anorganische Chemie  
 Technische Universit\"at Bergakademie Freiberg
 Leipziger Str. 29 
 09599 Freiberg 
 Germany
;
_publ_section_title
;
 Coordinative Unsaturation in an Antimony(III)-Complex with the
 2-Salicylidenaminophenolato Ligand: Synthesis, Crystal Structure,
 Spectroscopic Analysis, and DFT Studies
;
_journal_issue                   9
_journal_name_full               Crystals
_journal_page_first              1300
_journal_paper_doi               10.3390/cryst13091300
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C15 H14 N O3 Sb'
_chemical_formula_sum            'C15 H14 N O3 Sb'
_chemical_formula_weight         378.02
_chemical_melting_point          429
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 104.932(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8915(6)
_cell_length_b                   16.5156(6)
_cell_length_c                   7.7866(4)
_cell_measurement_reflns_used    46353
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      56.05
_cell_measurement_theta_min      3.87
_cell_volume                     1353.35(12)
_computing_cell_refinement       'STOE X-AREA (STOE, 2009)'
_computing_data_collection       'STOE X-AREA (STOE, 2009)'
_computing_data_reduction        'STOE X-RED (STOE, 2009)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2018 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      ' 386 frames, detector distance = 114 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.647
_diffrn_reflns_theta_min         2.295
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  0.8002
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       Prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0221P)^2^+2.1892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2948
_reflns_number_total             3130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            SK5_3.cif
_cod_data_source_block           SK5_3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569818
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.749
_shelx_res_checksum              58108
_shelx_hkl_checksum              1885