Iron(II)‒alkoxide and ‒aryloxide complexes of a tris(thioether)borate ligand: synthesis, molecular structures, and implications on the origin of instability of their iron(II)‒catecholate counterpart
Wang, Peng; Yap, Glenn P. A.; Riordan, Charles G.; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621008500

data_2022423
_publ_section_title
;
 Iron(II)--alkoxide and --aryloxide complexes of a tris(thioether)borate
 ligand: synthesis, molecular structures, and implications on the origin
 of instability of their iron(II)--catecholate counterpart
;
_journal_coeditor_code           YO3080
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621008500
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Fe (C21 H38 B S3) (C8 H9 O)]'
_chemical_formula_moiety         'C29 H47 B Fe O S3'
_chemical_formula_sum            'C29 H47 B Fe O S3'
_chemical_formula_weight         574.50
_chemical_name_systematic
(2,6-Dimethylphenolato){tris[(<i>tert</i>-butylsulfanyl)methyl]phenylborato-\k^3^<i>S</i>,<i>S</i>',<i>S</i>''}iron(II)
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.664(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4960(19)
_cell_length_b                   15.036(2)
_cell_length_c                   36.375(6)
_cell_measurement_reflns_used    1011
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.24
_cell_volume                     6284.9(17)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS1997 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            42065
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         2.231
_diffrn_source                   'fine focus sealed tube'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_correction_T_min  0.896586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7796
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+6.6546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                7494
_reflns_number_total             7796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yo3080sup1.cif
_cod_data_source_block           3
_cod_original_cell_volume        6285.0(18)
_cod_database_code               2022423
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.904
_shelx_hkl_checksum              97707
_shelx_res_checksum              46406
_cod_database_fobs_code 2022423