The structural parameter of spin states of <i>C</i> <sub>1</sub>-symmetric four-coordinate cobalt complexes: <i>D</i> <sub>4</sub>.
Zheng, Chenggong; Liu, Jiyong; Wang, Yongtao; Li, Haoran; Wang, Yuwen; Lu, Zhan; Chemical science 17 (2026) 492–499; doi:10.1039/d5sc06683b

data_1576169
_publ_section_title
;
 The structural parameter of spin states of <i>C</i>
 <sub>1</sub>-symmetric four-coordinate cobalt complexes: <i>D</i>
 <sub>4</sub>.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              492
_journal_page_last               499
_journal_paper_doi               10.1039/d5sc06683b
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         '2(C18 H28 Fe N O4 Si2), C H Cl3, 2(C F3 O3 S)'
_chemical_formula_sum            'C39 H57 Cl3 F6 Fe2 N2 O14 S2 Si4'
_chemical_formula_weight         1286.39
_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     dual
_audit_creation_date             2022-12-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-31 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3643(2)
_cell_length_b                   21.3942(2)
_cell_length_c                   15.4590(2)
_cell_measurement_reflns_used    22607
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      79.3630
_cell_measurement_theta_min      4.1090
_cell_volume                     5730.52(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -122.00 -73.00   0.50    0.50    --  -49.37-125.00 -90.00   98
  2  \w   -122.00 -33.00   0.50    0.50    --  -49.37 -57.00  90.00  178
  3  \w    -65.00  24.00   0.50    0.50    --  -49.37  57.00 -90.00  178
  4  \w    -48.00 -12.00   0.50    1.20    --  -88.50  45.00-150.00   72
  5  \w     -9.00  30.00   0.50    0.50    --  -49.37  19.00-150.00   78
  6  \w     -9.00  30.00   0.50    0.50    --  -49.37  19.00  60.00   78
  7  \w     94.00 170.00   0.50    1.20    --  110.00  15.00 150.00  152
  8  \w     94.00 160.00   0.50    1.20    --  110.00  15.00  90.00  132
  9  \w     98.00 178.00   0.50    1.20    --  110.00  30.00  30.00  160
 10  \w    140.00 173.00   0.50    1.20    --  110.00  61.00 -30.00   66
 11  \w     94.00 119.00   0.50    1.20    --  110.00  61.00 -30.00   50
 12  \w     40.00 103.00   0.50    1.20    --  110.00 -95.00-150.00  126
 13  \w     45.00 107.00   0.50    1.20    --  110.00-111.00-180.00  124
 14  \w     37.00  71.00   0.50    1.20    --  110.00-111.00-120.00   68
 15  \w     37.00  72.00   0.50    1.20    --  110.00-111.00-150.00   70
 16  \w     80.00 107.00   0.50    1.20    --  110.00-111.00-150.00   54
 17  \w     39.00  95.00   0.50    1.20    --  110.00-111.00 -90.00  112
 18  \w     39.00  64.00   0.50    1.20    --  110.00-111.00 -60.00   50
 19  \w     34.00  97.00   0.50    1.20    --  110.00 -95.00 -90.00  126
 20  \w     34.00  96.00   0.50    0.50    --   49.37-125.00 -90.00  124
 21  \w     50.00 100.00   0.50    1.20    --  110.00-111.00  90.00  100
 22  \w     53.00  95.00   0.50    1.20    --  110.00 -95.00 120.00   84
 23  \w    -30.00   9.00   0.50    0.50    --   49.37 -19.00-120.00   78
 24  \w     47.00  73.00   0.50    1.20    --  110.00 -61.00-180.00   52
 25  \w     39.00  66.00   0.50    1.20    --  110.00 -61.00 -30.00   54
 26  \w    102.00 178.00   0.50    1.20    --  110.00 111.00-150.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0123513000
_diffrn_orient_matrix_UB_12      -0.0708114000
_diffrn_orient_matrix_UB_13      -0.0106162000
_diffrn_orient_matrix_UB_21      0.0441678000
_diffrn_orient_matrix_UB_22      -0.0022940000
_diffrn_orient_matrix_UB_23      0.0896831000
_diffrn_orient_matrix_UB_31      -0.0762074000
_diffrn_orient_matrix_UB_32      -0.0127486000
_diffrn_orient_matrix_UB_33      0.0426293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.784
_diffrn_reflns_theta_min         3.532
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.516
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.69a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_recrystallization_method 'Slow evaporation from CHCl3 solution'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         12232
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+3.2433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10484
_reflns_number_total             12232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06683b2.cif
_cod_data_source_block           c201222_1_2
_cod_depositor_comments
'Adding full bibliography for 1576157--1576173.cif.'
_cod_database_code               1576169
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C41H58Cl3F6Fe2O14S2Si4
_shelx_estimated_absorpt_t_max   0.419
_shelx_estimated_absorpt_t_min   0.245
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1E-Cl2E \\sim Cl2E-Cl3E \\sim Cl3E-Cl1E \\sim Cl1F-Cl2F \\sim Cl2F-Cl3F
\\sim Cl3F-Cl1F
 with sigma of 0.02
 Cl2E-C1E \\sim Cl2F-C1F \\sim Cl1E-C1E \\sim Cl1F-C1F \\sim Cl3E-C1E \\sim
Cl3F-C1F
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2F \\sim C1F \\sim Cl1F \\sim Cl3F \\sim Cl2E \\sim Cl1E \\sim C1E \\sim
Cl3E: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(Cl2E) = Uanis(Cl2F)
Uanis(C1E) = Uanis(C1F)
Uanis(Cl1E) = Uanis(Cl1F)
Uanis(Cl3E) = Uanis(Cl3F)
4. Rigid body (RIGU) restrains
 C1E, Cl1E, Cl2E, Cl3E, C1F, Cl2F, Cl1F, Cl3F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl2F)=Sof(Cl1F)=Sof(Cl3F)=Sof(C1F)=Sof(H1F)=1-FVAR(1)
 Sof(Cl1E)=Sof(Cl2E)=Sof(Cl3E)=Sof(C1E)=Sof(H1E)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1E(H1E), C1F(H1F)
6.b Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C12A(H12A,H12B), C9B(H9BA,H9BB), C12B(H12C,H12D)
6.c Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C),
 C18A(H18A,H18B,H18C), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F), C13B(H13D,
 H13E,H13F), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F),
 C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              17228
_olex2_submission_original_sample_id c201222_1_2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.101
_oxdiff_exptl_absorpt_empirical_full_min 0.526