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_7716278
_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 Se2'
_chemical_formula_sum            'C23 H26 Fe N6 O Se2'
_chemical_formula_weight         616.27
_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             2023-05-17
_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                 97.447(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0416(18)
_cell_length_b                   14.803(3)
_cell_length_c                   10.017(2)
_cell_measurement_reflns_used    761
_cell_measurement_temperature    400.6(8)
_cell_measurement_theta_max      16.0530
_cell_measurement_theta_min      3.1500
_cell_volume                     1329.4(5)
_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      400.6(8)
_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 0.892
_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  17.00   1.00   15.00    --   23.49  77.00  90.00   25
;
_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      0.0217309000
_diffrn_orient_matrix_UB_12      0.0435776000
_diffrn_orient_matrix_UB_13      -0.0188824000
_diffrn_orient_matrix_UB_21      -0.0521783000
_diffrn_orient_matrix_UB_22      0.0196652000
_diffrn_orient_matrix_UB_23      0.0385138000
_diffrn_orient_matrix_UB_31      0.0553156000
_diffrn_orient_matrix_UB_32      0.0012116000
_diffrn_orient_matrix_UB_33      0.0573389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1739
_diffrn_reflns_av_unetI/netI     0.5612
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10855
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.638
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20697
_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    1.540
_exptl_crystal_description       needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6842
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.4421
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.3070
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.777
_reflns_number_gt                1033
_reflns_number_total             6842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmos1_8a_vt_4_400_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716278
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.515
_reflns_odcompleteness_completeness 89.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.57
_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.a Ternary CH refined with riding coordinates:
 N008(H008), C00B(H00B), C00I(H00I), C00N(H00N)
2.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00C), C00K(H00D,H00F), C00M(H00G,H00H), C00P(H00J,H00K), C00R(H00M,
 H00P)
2.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00L(H00L), C00O(H00O), C1(H1), C3(H3), C6(H6), C19(H19),
 C1AA(H1AA), C0AA(H0AA)
2.d Idealised Me refined as rotating group:
 C00S(H00Q,H00R,H00S)
;
_shelx_res_checksum              69229
_shelx_hkl_checksum              44025
_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 3.938
_oxdiff_exptl_absorpt_empirical_full_min 0.375