Crystal structure of tris-{<i>N</i>,<i>N</i>-diethyl-<i>N</i>'-[(4-nitro-phen-yl)(oxo)meth-yl]carbamimido-thio-ato}cobalt(III).
Roecker, Lee; Parkin, Sean; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 713–716; doi:10.1107/S2056989024005449

data_2023159
_publ_section_title
;
 Crystal structure of
 tris-{<i>N</i>,<i>N</i>-diethyl-<i>N</i>'-[(4-nitro-phen-yl)(oxo)meth-yl]carbamimido-thio-ato}cobalt(III).
;
_journal_coeditor_code           NX2011
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              713
_journal_page_last               716
_journal_paper_doi               10.1107/S2056989024005449
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Co (C12 H14 N3 O3 S1)3]'
_chemical_formula_moiety         'C36 H42 Co N9 O9 S3'
_chemical_formula_sum            'C36 H42 Co N9 O9 S3'
_chemical_formula_weight         899.89
_chemical_name_systematic
Tris{<i>N</i>,<i>N</i>-diethyl-<i>N</i>'-[(4-nitrophenyl)(oxo)methyl]carbamimidothioato}cobalt(III)
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.6906(3)
_cell_length_b                   16.6906(3)
_cell_length_c                   9.1346(2)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      3.06
_cell_volume                     2203.76(7)
_computing_cell_refinement
;
<i>APEX2</i> (Bruker, 2006)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2006)
;
_computing_data_reduction
;
<i>APEX2</i> (Bruker, 2006)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            30546
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.137
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[<i>SADABS</i> (Krause <i>et al</i>., 2015),
<i>XABS2</i> (Parkin <i>et al</i>., 1995)]
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       shard
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.251
_refine_ls_extinction_coef       0.00080(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0455P)^2^+0.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                2571
_reflns_number_total             2682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2011.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023159.cif.'
_cod_original_cell_volume        2203.76(9)
_cod_database_code               2023159
_shelx_estimated_absorpt_t_min   0.592
_shelx_estimated_absorpt_t_max   0.828
_shelx_hkl_checksum              74443
_shelx_res_checksum              7588
_shelx_fab_checksum              12903