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_7716282
_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 H0.5 Fe N6 O S2'
_chemical_formula_weight         496.76
_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                 96.242(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9004(4)
_cell_length_b                   14.5127(8)
_cell_length_c                   9.6200(4)
_cell_measurement_reflns_used    2389
_cell_measurement_temperature    132(4)
_cell_measurement_theta_max      21.9970
_cell_measurement_theta_min      3.2650
_cell_volume                     1235.24(10)
_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      132(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 0.896
_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    -29.00  48.00   1.00   25.00    --  -21.11  57.00 -60.00   77
  2  \w    -10.00  42.00   1.00   25.00    --   21.90  77.00  30.00   52
  3  \w      0.00  81.00   1.00   25.00    --   21.90  57.00  90.00   81
  4  \w     -9.00  65.00   1.00   25.00    --   21.90 -99.00-120.00   74
  5  \w      1.00  91.00   1.00   25.00    --   21.90  57.00-180.00   90
  6  \w      7.00  53.00   1.00   25.00    --   21.90 -77.00 -30.00   46
;
_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      0.0329224000
_diffrn_orient_matrix_UB_12      -0.0432425000
_diffrn_orient_matrix_UB_13      0.0194331000
_diffrn_orient_matrix_UB_21      -0.0599834000
_diffrn_orient_matrix_UB_22      -0.0093120000
_diffrn_orient_matrix_UB_23      0.0408471000
_diffrn_orient_matrix_UB_31      -0.0418231000
_diffrn_orient_matrix_UB_32      -0.0207459000
_diffrn_orient_matrix_UB_33      -0.0587880000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10926
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.864
_diffrn_reflns_theta_min         2.807
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86040
_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    1.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             493
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 1153 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(15)
_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     312
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0339P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.827
_reflns_number_gt                3786
_reflns_number_total             6147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos01sc_vt_1_130_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_original_formula_sum        'C23 H0.50 Fe N6 O S2'
_cod_database_code               7716282
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.837
_reflns_odcompleteness_completeness 89.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.80
_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
 C00N-N006 = N006-C19
 1.29 with sigma of 0.02
 N009-C00M = N5-C6 = N009-C00U = N5-C10
 1.24 with sigma of 0.02
 N006-C19 = N006-C00N
 1.29 with sigma of 0.02
3. Others
 Fixed Sof: N009(0.5) C00M(0.5) C00N(0.5) H00N(0.5) C00T(0.5) H00T(0.5)
 C00U(0.5) H00U(0.5) C00W(0.5) H00X(0.5) C00X(0.5) H00Y(0.5) C3(0.5) H3(0.5)
 C4(0.5) H4(0.5) N5(0.5) C6(0.5) C10(0.5) H10(0.5) C13(0.5) H13(0.5) C19(0.5)
 H19(0.5)
4.a Ternary CH refined with riding coordinates:
 N007(H007), C00D(H00D), C00H(H00H), C00J(H00J)
4.b Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00I(H00C,H00E), C00L(H00G,H00I), C00P(H00L,H00M), C00R(H00P,
 H00Q)
4.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00K(H00K), C00N(H00N), C00O(H00O), C00S(H00S), C00T(H00T),
 C00U(H00U), C00W(H00X), C00X(H00Y), C3(H3), C4(H4), C10(H10), C13(H13),
 C19(H19)
4.d Idealised Me refined as rotating group:
 C00V(H00R,H00V,H00W)
;
_shelx_res_checksum              2089
_shelx_hkl_checksum              93453
_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 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.772