Lattice solvent- and substituent-dependent spin-crossover in isomeric iron(II) complexes.
Kuppusamy, Senthil Kumar; Mizuno, Asato; Kämmerer, Lea; Salamon, Soma; Heinrich, Benoît; Bailly, Corinne; Šalitroš, Ivan; Wende, Heiko; Ruben, Mario; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10851–10865; doi:10.1039/d4dt00429a

data_7716142
_publ_section_title
;
 Lattice solvent- and substituent-dependent spin-crossover in isomeric
 iron(II) complexes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10851
_journal_page_last               10865
_journal_paper_doi               10.1039/d4dt00429a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H26 Fe N10 O4, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C30 H29 Cl2 Fe N11 O12'
_chemical_formula_weight         862.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-08-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.291(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0964(11)
_cell_length_b                   33.9875(14)
_cell_length_c                   8.3387(5)
_cell_measurement_reflns_used    2366
_cell_measurement_temperature    300
_cell_measurement_theta_max      23.0090
_cell_measurement_theta_min      2.7320
_cell_volume                     3930.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'imaging plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -41.00  90.00   1.00  600.60    --    0.00 180.00 278.00  131
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0510453000
_diffrn_orient_matrix_UB_12      0.0002564000
_diffrn_orient_matrix_UB_13      -0.0151037000
_diffrn_orient_matrix_UB_21      0.0005084000
_diffrn_orient_matrix_UB_22      0.0208796000
_diffrn_orient_matrix_UB_23      -0.0020079000
_diffrn_orient_matrix_UB_31      -0.0001259000
_diffrn_orient_matrix_UB_32      -0.0005299000
_diffrn_orient_matrix_UB_33      -0.0851501000
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1308
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14651
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        23.255
_diffrn_reflns_theta_max         23.255
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       needle
_exptl_crystal_F_000             1768
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0874
_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^)+(0.1232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2570
_reflns_number_total             5599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00429a2.cif
_cod_data_source_block           skr405
_cod_depositor_comments
'Adding full bibliography for 7716135--7716142.cif.'
_cod_database_code               7716142
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Fe Cl'
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C26B, C26A, C26C}
3. Restrained distances
 C27B-C28B = C27A-C28A = C27C-C28C
 1.52 with sigma of 0.01
 C26A-O3A = C26B-O3B = C26C-O3C
 1.43 with sigma of 0.01
 O4B-C27B = O4A-C27A = O4C-C27C
 1.23 with sigma of 0.01
 O3A-C27A = O3B-C27B = O3C-C27C
 1.32 with sigma of 0.01
 C20-C26B \\sim C20-C26A \\sim C20-C26C
 with sigma of 0.02
 C28A-O4A \\sim C28B-O4B \\sim C28C-O4C
 with sigma of 0.02
 O3A-O4A \\sim O3B-O4B \\sim O3C-O4C
 with sigma of 0.02
 Cl2-O11 \\sim Cl2-O12 \\sim Cl2-O10 \\sim Cl2-O9
 with sigma of 0.02
 O9-O10 \\sim O10-O11 \\sim O11-O12
 with sigma of 0.02
 Cl2-O13 \\sim Cl2-O15 \\sim Cl2-O14 \\sim Cl2-O21
 with sigma of 0.02
 O13-O14 \\sim O14-O15 \\sim O15-O21 \\sim O21-O13
 with sigma of 0.02
4. Restrained planarity
 O3A, C27A, C28A, O4A
 with sigma of 0.1
 O3B, O4B, C27B, C28B
 with sigma of 0.1
 O3C, C27C, O4C, C28C
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O11 \\sim O15: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O12 \\sim O21: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O10 \\sim O14: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O9 \\sim O13: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(C28B) = Uanis(C28A) = Uanis(C28C)
Uanis(C26B) = Uanis(C26A) = Uanis(C26C)
Uanis(O4B) = Uanis(O4A) = Uanis(O4C)
Uanis(C27B) = Uanis(C27A) = Uanis(C27C)
Uanis(O3B) = Uanis(O3A) = Uanis(O3C)
6. Rigid body (RIGU) restrains
 C27B, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3A, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4B, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3C, C27C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27C, C28C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27C, O4C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 1*[Sof(O3A)+Sof(C27A)+Sof(C28A)+Sof(H28D)+Sof(H28E)+Sof(H28F)+Sof(O4A)+
 Sof(C26A)+Sof(H26C)+Sof(H26D)]+1*[Sof(O3B)+Sof(C26B)+Sof(H26A)+Sof(H26B)+
 Sof(O4B)+Sof(C27B)+Sof(C28B)+Sof(H28A)+Sof(H28B)+Sof(H28C)]+1*[Sof(C26C)+
 Sof(H26E)+Sof(H26F)+Sof(O3C)+Sof(C27C)+Sof(O4C)+Sof(C28C)+Sof(H28G)+Sof(H28H)+
 Sof(H28I)]=1 with esd of 0.001
 Sof(O13)=Sof(O15)=Sof(O14)=Sof(O21)=1-FVAR(1)
 Sof(O11)=Sof(O12)=Sof(O10)=Sof(O9)=FVAR(1)
 Sof(O3A)=Sof(C27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(O4A)=Sof(C26A)=
 Sof(H26C)=Sof(H26D)=FVAR(2)
 Sof(O3B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(O4B)=Sof(C27B)=Sof(C28B)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(3)
 Sof(C26C)=Sof(H26E)=Sof(H26F)=Sof(O3C)=Sof(C27C)=Sof(O4C)=Sof(C28C)=Sof(H28G)=
 Sof(H28H)=Sof(H28I)=FVAR(4)
8.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C26B(H26A,H26B), C26A(H26C,H26D), C26C(H26E,H26F)
8.b Me refined with riding coordinates:
 C28B(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C28C(H28G,H28H,H28I)
8.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C7(H7), C2(H2), C21(H21), C3(H3), C19(H19), C9(H9), C25(H25),
 C10(H10), C15(H15), C11(H11), C23(H23), C17(H17), C24(H24), C16(H16)
8.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C01I(H01A,H01B,H01C)
;
_shelx_res_checksum              73966
_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 2.087
_oxdiff_exptl_absorpt_empirical_full_min 0.558