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_7716140
_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                 99.3980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7191(2)
_cell_length_b                   24.0393(3)
_cell_length_c                   14.5992(2)
_cell_measurement_reflns_used    27707
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.0560
_cell_measurement_theta_min      1.7670
_cell_volume                     3711.42(10)
_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      300
_diffrn_detector                 'imaging plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    --    0.00 180.00 120.00  180
  2  \w    -90.00  90.00   1.00  300.60    --    0.00 180.00 298.00  180
;
_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      -0.0324150000
_diffrn_orient_matrix_UB_12      0.0205631000
_diffrn_orient_matrix_UB_13      0.0218397000
_diffrn_orient_matrix_UB_21      0.0341093000
_diffrn_orient_matrix_UB_22      0.0211343000
_diffrn_orient_matrix_UB_23      -0.0191638000
_diffrn_orient_matrix_UB_31      -0.0477864000
_diffrn_orient_matrix_UB_32      0.0011196000
_diffrn_orient_matrix_UB_33      -0.0397580000
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58355
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_min         2.104
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91310
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_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         0.374
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         8179
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+1.5487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6534
_reflns_number_total             8179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00429a2.cif
_cod_data_source_block           skr369
_cod_depositor_comments
'Adding full bibliography for 7716135--7716142.cif.'
_cod_database_code               7716140
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O B F'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.811
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2G-B2B
 1.44 with sigma of 0.02
 C27-C28A = C27-C28B
 1.54 with sigma of 0.02
 B2B-F2G \\sim B2B-F2F \\sim B2B-F2H \\sim B2B-F2E
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1J \\sim F1E \\sim F1B \\sim F1F \\sim F1K \\sim F1D \\sim F1H \\sim F1I \\sim
F1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F2C \\sim F2G: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F2H \\sim F2D: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C28A) = Uanis(C28B)
Uanis(F2B) = Uanis(F2F)
Uanis(F2A) = Uanis(F2E)
Uanis(B2B) = Uanis(B2A)
Uanis(F2C) = Uanis(F2G)
4. Others
 1*[Sof(F1D)+Sof(F1A)+Sof(F1B)]+1*[Sof(F1H)+Sof(F1E)+Sof(F1F)]+1*[Sof(F1I)+
 Sof(F1J)+Sof(F1K)]=1 with esd of 0.0001
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(F1D)=Sof(F1A)=Sof(F1B)=FVAR(2)
 Sof(F2G)=Sof(F2F)=Sof(F2H)=Sof(F2E)=Sof(B2B)=1-FVAR(3)
 Sof(F2D)=Sof(F2A)=Sof(F2C)=Sof(F2B)=Sof(B2A)=FVAR(3)
 Sof(F1H)=Sof(F1E)=Sof(F1F)=FVAR(4)
 Sof(F1I)=Sof(F1J)=Sof(F1K)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C13(H13A,H13B)
5.b Me refined with riding coordinates:
 C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F)
5.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C5(H5), C7(H7), C25(H25), C9(H9), C15(H15), C11(H11),
 C23(H23), C10(H10), C1(H1), C24(H24), C16(H16), C2(H2), C3(H3), C17(H17)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              48456
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.817