Chiral spin-crossover complexes based on an enantiopure Schiff base ligand with three chiral carbon centers.
Regueiro, Alejandro; García-López, Víctor; Forment-Aliaga, Alicia; Clemente-León, Miguel; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10637–10643; doi:10.1039/d4dt00924j

data_7716287
_publ_section_title
;
 Chiral spin-crossover complexes based on an enantiopure Schiff base
 ligand with three chiral carbon centers.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10637
_journal_page_last               10643
_journal_paper_doi               10.1039/d4dt00924j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C23 H25 Fe N6 O S2'
_chemical_formula_sum            'C23 H25 Fe N6 O S2'
_chemical_formula_weight         521.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-02
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.383(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9161(4)
_cell_length_b                   14.5306(6)
_cell_length_c                   9.6438(4)
_cell_measurement_reflns_used    3657
_cell_measurement_temperature    149.8(4)
_cell_measurement_theta_max      24.0450
_cell_measurement_theta_min      3.2560
_cell_volume                     1241.67(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_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    -95.00  28.00   1.00    5.00    --  -21.11 -19.00 -60.00  123
  2  \w    -53.00  21.00   1.00    5.00    --  -21.11  77.00 -30.00   74
  3  \w    -24.00  46.00   1.00    5.00    --  -21.11  57.00 120.00   70
  4  \w    -10.00  42.00   1.00    5.00    --   21.90  77.00-150.00   52
  5  \w     14.00  79.00   1.00    5.00    --   21.90  57.00 120.00   65
  6  \w    -10.00  42.00   1.00    5.00    --   21.90  77.00 -30.00   52
  7  \w    -10.00  16.00   1.00    5.00    --   21.90  77.00 150.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0795628000
_diffrn_orient_matrix_UB_12      0.0038524000
_diffrn_orient_matrix_UB_13      -0.0029478000
_diffrn_orient_matrix_UB_21      0.0066296000
_diffrn_orient_matrix_UB_22      0.0486285000
_diffrn_orient_matrix_UB_23      0.0032401000
_diffrn_orient_matrix_UB_31      -0.0053921000
_diffrn_orient_matrix_UB_32      0.0019642000
_diffrn_orient_matrix_UB_33      -0.0738904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12097
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.832
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6271
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0456P)^2^+0.2115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.850
_reflns_number_gt                4521
_reflns_number_total             6271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos_01sa_vt_2_150_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716287
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.570
_reflns_odcompleteness_completeness 90.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.77
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N008-C00O = N7-C8 = N008-C00U = N7-C11
 1.34 with sigma of 0.02
3. Rigid bond restraints
 C00T, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C00T \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: N008(0.5) C00K(0.5) H00K(0.5) C00O(0.5) C00T(0.5) H00T(0.5)
 C00U(0.5) H00U(0.5) C00W(0.5) H00W(0.5) C00X(0.5) H00X(0.5) C5(0.5) H5(0.5)
 C6(0.5) H6(0.5) N7(0.5) C8(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C20(0.5)
 H20(0.5)
6.a Ternary CH refined with riding coordinates:
 N005(H005), C00E(H00E), C00I(H00I)
6.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00J(H00C,H00D), C00L(H00F,H00G), C00M(H00J,H00L), C00P(H00M,
 H00N)
6.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00W(H00W), C00X(H00X), C5(H5), C6(H6), C11(H11), C12(H12),
 C20(H20)
6.d Idealised Me refined as rotating group:
 C00V(H00O,H00P,H00V)
;
_shelx_res_checksum              89259
_shelx_hkl_checksum              44591
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.544