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_7716279
_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
_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                 97.425(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9654(5)
_cell_length_b                   14.6855(7)
_cell_length_c                   9.9205(6)
_cell_measurement_reflns_used    3161
_cell_measurement_temperature    299.95(10)
_cell_measurement_theta_max      19.2750
_cell_measurement_theta_min      3.1850
_cell_volume                     1295.19(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      299.95(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 0.940
_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    -37.00   6.00   1.00   15.00    --  -22.71 -77.00 -60.00   43
  2  \w      4.00  42.00   1.00   15.00    --  -22.71  77.00  30.00   38
  3  \w      3.00  33.00   1.00   15.00    --  -22.71  77.00-180.00   30
  4  \w    -91.00  -8.00   1.00   15.00    --  -22.71 -38.00 120.00   83
  5  \w    -44.00  46.00   1.00   15.00    --  -22.71  57.00 150.00   90
  6  \w    -34.00   9.00   1.00   15.00    --  -22.71 -77.00  60.00   43
  7  \w    -41.00   9.00   1.00   15.00    --  -22.71 -77.00-180.00   50
  8  \w     17.00  67.00   1.00   15.00    --   23.49 -99.00-150.00   50
  9  \w      2.00  90.00   1.00   15.00    --   23.49  57.00 -60.00   88
 10  \w    -15.00  67.00   1.00   15.00    --   23.49 -99.00  30.00   82
 11  \w    -45.00  37.00   1.00   15.00    --   23.49 -57.00 -90.00   82
 12  \w      2.00  93.00   1.00   15.00    --   23.49  57.00  60.00   91
;
_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      -0.0639440000
_diffrn_orient_matrix_UB_12      -0.0140381000
_diffrn_orient_matrix_UB_13      -0.0447269000
_diffrn_orient_matrix_UB_21      0.0465485000
_diffrn_orient_matrix_UB_22      -0.0272810000
_diffrn_orient_matrix_UB_23      -0.0363147000
_diffrn_orient_matrix_UB_31      -0.0100042000
_diffrn_orient_matrix_UB_32      -0.0373110000
_diffrn_orient_matrix_UB_33      0.0434099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_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       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21667
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.531
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74845
_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    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.870
_reflns_number_gt                3080
_reflns_number_total             7197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00924j2.cif
_cod_data_source_block           agrmor01_1a_vt_5_300_00_auto
_cod_depositor_comments
'Adding full bibliography for 7716275--7716292.cif.'
_cod_database_code               7716279
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.563
_reflns_odcompleteness_completeness 93.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.46
_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
 N006-C1 = N006-C00S
 1.29 with sigma of 0.02
 N1-C7 = N007-C00J = N007-C00P = N1-C4
 1.34 with sigma of 0.02
 N006-C00S = N006-C1
 1.29 with sigma of 0.02
3. Others
 Fixed Sof: N007(0.5) C00J(0.5) C00L(0.5) H00L(0.5) C00P(0.5) H00P(0.5)
 C00S(0.5) H00S(0.5) C00W(0.5) H00X(0.5) C00X(0.5) H00Y(0.5) N1(0.5) C4(0.5)
 H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C1(0.5) H1(0.5)
4.a Ternary CH refined with riding coordinates:
 N005(H005), C00D(H00D), C00F(H00F), C00M(H00M)
4.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00K(H00C,H00E), C00N(H00H,H00J), C00O(H00K,H00N), C00V(H00V,
 H00W)
4.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00L(H00L), C00P(H00P), C00R(H00R), C00S(H00S),
 C00T(H00T), C00W(H00X), C00X(H00Y), C4(H4), C5(H5), C6(H6), C8(H8), C1(H1)
4.d Idealised Me refined as rotating group:
 C00U(H00O,H00Q,H00U)
;
_shelx_res_checksum              33082
_shelx_hkl_checksum              32244
_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 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.808