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_7716283
_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             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                 96.324(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8517(3)
_cell_length_b                   14.4554(5)
_cell_length_c                   9.5844(3)
_cell_measurement_reflns_used    2368
_cell_measurement_temperature    92(3)
_cell_measurement_theta_max      22.0790
_cell_measurement_theta_min      3.2790
_cell_volume                     1218.91(7)
_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      92(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_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    -42.00   7.00   1.00   20.00    --  -15.98 -77.00-120.00   49
  2  \w    -90.00 -33.00   1.00   20.00    --  -15.98 -19.00   0.00   57
  3  \w    -37.00  64.00   1.00   20.00    --   16.91 -19.00  30.00  101
  4  \w     -2.00  86.00   1.00   20.00    --   16.91  57.00-150.00   88
  5  \w    -13.00  42.00   1.00   20.00    --   16.91  77.00  90.00   55
  6  \w    -42.00 -11.00   1.00   20.00    --   16.91 -77.00  60.00   31
;
_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      0.0343434000
_diffrn_orient_matrix_UB_12      -0.0432748000
_diffrn_orient_matrix_UB_13      0.0184434000
_diffrn_orient_matrix_UB_21      -0.0594582000
_diffrn_orient_matrix_UB_22      -0.0103572000
_diffrn_orient_matrix_UB_23      0.0414549000
_diffrn_orient_matrix_UB_31      -0.0421963000
_diffrn_orient_matrix_UB_32      -0.0207256000
_diffrn_orient_matrix_UB_33      -0.0590329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8677
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.734
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92539
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4813
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0284P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                3446
_reflns_number_total             4813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos01sc_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716283
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.834
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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: N00A(0.5) C00M(0.5) H00M(0.5) C00R(0.5) H00R(0.5) C00S(0.5)
 C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C0AA(0.5) H0AA(0.5) C2AA(0.5)
 H2AA(0.5) C1AA(0.5) H1AA(0.5) N5(0.5) C6(0.5) C9(0.5) H9(0.5) C18(0.5) H18(0.5)
3.a Ternary CH refined with riding coordinates:
 N008(H008), C00B(H00B), C00F(H00F), C00N(H00N)
3.b Secondary CH2 refined with riding coordinates:
 C00E(H00A,H00C), C00G(H00D,H00E), C00J(H00G,H00H), C00K(H00J,H00K), C00O(H00L,
 H00O)
3.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00M(H00M), C00P(H00P), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C1(H1), C2(H2), C3(H3), C0AA(H0AA), C2AA(H2AA), C1AA(H1AA), C9(H9), C18(H18)
3.d Idealised Me refined as rotating group:
 C00V(H00S,H00U,H00V)
;
_shelx_res_checksum              92825
_shelx_hkl_checksum              45660
_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.790