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_7716288
_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 Se2'
_chemical_formula_sum            'C23 H25 Fe N6 O Se2'
_chemical_formula_weight         615.26
_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
_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                 97.401(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9670(5)
_cell_length_b                   14.6787(8)
_cell_length_c                   9.9286(5)
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      16.6350
_cell_measurement_theta_min      3.1840
_cell_volume                     1295.95(12)
_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      air
_diffrn_ambient_temperature      300.00(10)
_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 0.939
_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    -38.00  46.00   1.00   15.00    --  -22.71  57.00 120.00   84
  2  \w    -80.00  -9.00   1.00   15.00    --  -22.71 124.00-117.00   71
  3  \w      2.00  92.00   1.00   15.00    --   23.49  57.00   0.00   90
  4  \w     -4.00  96.00   1.00   15.00    --   23.49  38.00 -90.00  100
  5  \w     -8.00  39.00   1.00   15.00    --   23.49  77.00  90.00   47
  6  \w     38.00  79.00   1.00   15.00    --   23.49-124.00 163.00   41
  7  \w     -8.00  33.00   1.00   15.00    --   23.49  77.00 -30.00   41
  8  \w    -23.00  98.00   1.00   15.00    --   23.49  19.00-180.00  121
  9  \w     39.00  97.00   1.00   15.00    --   23.49 178.00 120.00   58
 10  \w     -8.00  41.00   1.00   15.00    --   23.49  77.00-180.00   49
 11  \w    -46.00  19.00   1.00   15.00    --   23.49 -57.00-150.00   65
;
_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      -0.0226214000
_diffrn_orient_matrix_UB_12      0.0436689000
_diffrn_orient_matrix_UB_13      0.0202430000
_diffrn_orient_matrix_UB_21      0.0585026000
_diffrn_orient_matrix_UB_22      0.0202619000
_diffrn_orient_matrix_UB_23      -0.0313988000
_diffrn_orient_matrix_UB_31      -0.0492345000
_diffrn_orient_matrix_UB_32      0.0040260000
_diffrn_orient_matrix_UB_33      -0.0616472000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1224
_diffrn_reflns_av_unetI/netI     0.2146
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21626
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71015
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       needle
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 660 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.2576
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0153P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                2279
_reflns_number_total             7211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos1_8a_vt_1_300_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716288
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.507
_reflns_odcompleteness_completeness 93.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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-C00G = N8-C7 = N8-C5 = N008-C00P
 1.34 with sigma of 0.02
 N11-C14 = N007-C00Q
 1.29 with sigma of 0.02
 N007-C00C = N11-C00C
 1.45 with sigma of 0.02
3. Others
 Fixed Sof: N007(0.5) N008(0.5) C00G(0.5) C00W(0.5) H00W(0.5) C00U(0.5)
 H00U(0.5) C00K(0.5) H00K(0.5) C00P(0.5) H00P(0.5) C00Q(0.5) H00Q(0.5) C7(0.5)
 C12(0.5) H12(0.5) C0AA(0.5) H0AA(0.5) C10(0.5) H10(0.5) C5(0.5) H5(0.5)
 N8(0.5) N11(0.5) C14(0.5) H14(0.5)
4.a Ternary CH refined with riding coordinates:
 N004(H004), C00E(H00E), C00L(H00L)
4.b Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), C00I(H00C,H00D), C00J(H00F,H00G), C00R(H00H,H00I), C00S(H00J,
 H00N)
4.c Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00U(H00U), C00K(H00K), C00P(H00P), C00M(H00M), C00O(H00O),
 C00Q(H00Q), C00T(H00T), C00V(H00V), C12(H12), C0AA(H0AA), C10(H10), C5(H5),
 C14(H14)
4.d Fitted hexagon refined as free rotating group:
 N008(C00G,C00W,C00U,C00K,C00P), C7(C12,C0AA,C10,C5,N8)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              75260
_shelx_hkl_checksum              8137
_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 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.780