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_7716286
_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 H26 Fe N6 O S2'
_chemical_formula_sum            'C23 H26 Fe N6 O S2'
_chemical_formula_weight         522.47
_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             2022-09-16
_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                 96.509(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9762(8)
_cell_length_b                   14.6245(11)
_cell_length_c                   9.7166(6)
_cell_measurement_reflns_used    2997
_cell_measurement_temperature    249.90(14)
_cell_measurement_theta_max      21.8160
_cell_measurement_theta_min      3.2250
_cell_volume                     1267.30(17)
_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      249.90(14)
_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      -0.0783390000
_diffrn_orient_matrix_UB_12      0.0080562000
_diffrn_orient_matrix_UB_13      -0.0037198000
_diffrn_orient_matrix_UB_21      0.0134097000
_diffrn_orient_matrix_UB_22      0.0477212000
_diffrn_orient_matrix_UB_23      0.0039386000
_diffrn_orient_matrix_UB_31      -0.0043090000
_diffrn_orient_matrix_UB_32      0.0022122000
_diffrn_orient_matrix_UB_33      -0.0732922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0798
_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       -13
_diffrn_reflns_number            12380
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.859
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71115
_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    1.369
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6386
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.843
_reflns_number_gt                3661
_reflns_number_total             6386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos_01sa_vt_4_250_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716286
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.575
_reflns_odcompleteness_completeness 90.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.79
_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. Others
 Fixed Sof: N007(0.5) O009(0.5) C00N(0.5) C00O(0.5) H00O(0.5) C00S(0.5)
 H00S(0.5) C00U(0.5) H00U(0.5) C00V(0.5) H00Q(0.5) H00V(0.5) H00W(0.5)
 C00W(0.5) H00X(0.5) C00X(0.5) H00Y(0.5) C1(0.5) H1(0.5) C2(0.5) N3(0.5)
 C4(0.5) H4(0.5) C7(0.5) H7(0.5) C9(0.5) H9(0.5) C12(0.5) H12(0.5) O0AA(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
3.a Ternary CH refined with riding coordinates:
 N005(H005), C00B(H00B), C00G(H00G), C00H(H00H)
3.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00C), C00I(H00D,H00E), C00L(H00F,H00I), C00M(H00K,H00L), C00Q(H00M,
 H00N)
3.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00O(H00O), C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00W(H00X), C00X(H00Y), C1(H1), C4(H4), C7(H7), C9(H9), C12(H12)
3.d Idealised Me refined as rotating group:
 C00V(H00Q,H00V,H00W), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              56114
_shelx_hkl_checksum              5547
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.573