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_7716139
_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(B F4), C2 H3 N'
_chemical_formula_sum            'C30 H29 B2 F8 Fe N11 O4'
_chemical_formula_weight         837.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.943(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7530(5)
_cell_length_b                   25.3452(12)
_cell_length_c                   15.2139(6)
_cell_measurement_reflns_used    6469
_cell_measurement_temperature    345
_cell_measurement_theta_max      24.3360
_cell_measurement_theta_min      2.1230
_cell_volume                     3733.2(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      345
_diffrn_detector                 'imaging plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -90.00  90.00   1.00  300.60    --    0.00 180.00 160.00  180
  2  \w      5.00  50.00   1.00  300.60    --    0.00 180.00  48.00   45
;
_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      0.0364768000
_diffrn_orient_matrix_UB_12      0.0197258000
_diffrn_orient_matrix_UB_13      -0.0207055000
_diffrn_orient_matrix_UB_21      -0.0394601000
_diffrn_orient_matrix_UB_22      0.0197977000
_diffrn_orient_matrix_UB_23      0.0182838000
_diffrn_orient_matrix_UB_31      0.0498465000
_diffrn_orient_matrix_UB_32      0.0012073000
_diffrn_orient_matrix_UB_33      0.0379848000
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29144
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30628
_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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1619P)^2^+1.0152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3580
_reflns_number_total             6589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00429a2.cif
_cod_data_source_block           skr369_345k
_cod_depositor_comments
'Adding full bibliography for 7716135--7716142.cif.'
_cod_database_code               7716139
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Fe B F'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.811
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Restrained distances
 B1-F1F = B1-F1E = B1-F1G = B1-F1H
 1.43 with sigma of 0.02
 C27B-C28A = C28C-C27C
 1.54 with sigma of 0.01
 F2E-B2B \\sim B2A-F2D
 with sigma of 0.02
 F1F-F1E \\sim F1F-F1G \\sim F1F-F1H \\sim F1E-F1G \\sim F1E-F1H \\sim F1G-F1H
 with sigma of 0.02
 B2B-F2E \\sim B2B-F2F \\sim B2B-F2G \\sim B2B-F2H
 with sigma of 0.02
 C27B-C28B \\sim C28C-C27C \\sim C28A-C27A
 with sigma of 0.02
 F2E-F2F \\sim F2E-F2G \\sim F2E-F2H \\sim F2F-F2G \\sim F2F-F2H \\sim F2G-F2H
 with sigma of 0.02
 O4A-C26 \\sim O4C-C26 \\sim O4B-C26
 with sigma of 0.02
 O4A-C27A \\sim C27B-O4B \\sim C27C-O4C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28C \\sim C28A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C28C \\sim C28B \\sim C28A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
F2F \\sim F2C \\sim F2B \\sim F2H \\sim F2D \\sim F2E \\sim F2G \\sim F2A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
B1 \\sim F1E \\sim F1F \\sim F1G \\sim F1H \\sim F1A \\sim F1B \\sim F1C \\sim
F1D: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(B2B) = Uanis(B2A)
Uanis(C28A) = Uanis(C28B) = Uanis(C28C)
Uanis(O4A) = Uanis(O4B) = Uanis(O4C)
Uanis(C27C) = Uanis(C27A) = Uanis(C27B)
4. Others
 1*[Sof(C28C)+Sof(H28A)+Sof(H28B)+Sof(H28C)+Sof(C27C)+Sof(H27D)+Sof(H27C)+
 Sof(O4C)]+1*[Sof(O4A)+Sof(C28A)+Sof(H28D)+Sof(H28E)+Sof(H28F)+Sof(C27A)+
 Sof(H27E)+Sof(H27F)]+1*[Sof(C27B)+Sof(H27A)+Sof(H27B)+Sof(C28B)+Sof(H28G)+
 Sof(H28H)+Sof(H28I)+Sof(O4B)]=1 with esd of 0.001
 Sof(C28C)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27C)=Sof(H27D)=Sof(H27C)=
 Sof(O4C)=FVAR(1)
 Sof(O4A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C27A)=Sof(H27E)=
 Sof(H27F)=FVAR(2)
 Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(C28B)=Sof(H28G)=Sof(H28H)=Sof(H28I)=
 Sof(O4B)=FVAR(3)
 Sof(F2E)=Sof(B2B)=Sof(F2F)=Sof(F2G)=Sof(F2H)=1-FVAR(4)
 Sof(F2A)=Sof(F2B)=Sof(F2C)=Sof(F2D)=Sof(B2A)=FVAR(4)
 Sof(F1A)=Sof(F1B)=Sof(F1C)=Sof(F1D)=1-FVAR(5)
 Sof(F1E)=Sof(F1F)=Sof(F1G)=Sof(F1H)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C27B(H27A,H27B), C27C(H27D,H27C), C27A(H27E,H27F)
5.b Me refined with riding coordinates:
 C28C(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C28B(H28G,H28H,H28I)
5.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C1(H1), C21(H21), C7(H7), C9(H9), C5(H5), C23(H23), C17(H17),
 C25(H25), C3(H3), C2(H2), C11(H11), C16(H16), C15(H15), C10(H10), C24(H24)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              29918
_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 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.523