Impact of flexible hexyl chain ordering in a mononuclear spin crossover iron(III) complex.
Hagiwara, Hiroaki; Sonoda, Kento; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5851–5860; doi:10.1039/d4dt00425f

data_7715324
_publ_section_title
;
 Impact of flexible hexyl chain ordering in a mononuclear spin crossover
 iron(III) complex.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5851
_journal_page_last               5860
_journal_paper_doi               10.1039/d4dt00425f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H46 Fe N8 O2, C24 H20 B'
_chemical_formula_sum            'C64 H66 B Fe N8 O2'
_chemical_formula_weight         1045.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-09 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                98.737(2)
_cell_angle_beta                 95.692(2)
_cell_angle_gamma                119.179(3)
_cell_formula_units_Z            2
_cell_length_a                   14.3314(4)
_cell_length_b                   14.6187(5)
_cell_length_c                   16.0247(3)
_cell_measurement_reflns_used    14841
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      30.5310
_cell_measurement_theta_min      2.3100
_cell_volume                     2838.25(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      250(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -80.00 100.00   0.50   20.00   0.00  20.00   0.00    --   360
  2  \w    -19.50  27.50   0.50   20.00    --   20.00  90.00   0.00   94
  3  \w    -19.50  27.50   0.50   20.00    --   20.00  90.00  90.00   94
  4  \w    -19.50  27.50   0.50   20.00    --   20.00  90.00 180.00   94
  5  \w    -19.50  27.50   0.50   20.00    --   20.00  90.00 270.00   94
;
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0570022000
_diffrn_orient_matrix_UB_12      0.0325269000
_diffrn_orient_matrix_UB_13      0.0027561000
_diffrn_orient_matrix_UB_21      -0.0042820000
_diffrn_orient_matrix_UB_22      0.0467800000
_diffrn_orient_matrix_UB_23      0.0071984000
_diffrn_orient_matrix_UB_31      0.0089826000
_diffrn_orient_matrix_UB_32      0.0038920000
_diffrn_orient_matrix_UB_33      0.0450589000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25421
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.886
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         15085
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.7837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11559
_reflns_number_total             15085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00425f2.cif
_cod_data_source_block           1_250K
_cod_depositor_comments
'Adding full bibliography for 7715321--7715329.cif.'
_cod_original_cell_volume        2838.25(16)
_cod_database_code               7715324
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C1-C2
 1.53 with sigma of 0.02
 C2-C3A
 1.53 with sigma of 0.02
 C2-C3B
 1.53 with sigma of 0.02
 C3A-C4
 1.53 with sigma of 0.02
 C3B-C4
 1.53 with sigma of 0.02
 C4-C5
 1.53 with sigma of 0.02
 C5-C6
 1.53 with sigma of 0.02
 C21A-C22A
 1.53 with sigma of 0.02
 C21B-C22B
 1.53 with sigma of 0.02
 C22A-C23
 1.53 with sigma of 0.02
 C22B-C23
 1.53 with sigma of 0.02
 C23-C24A
 1.53 with sigma of 0.02
 C23-C24B
 1.53 with sigma of 0.02
 C24A-C25A
 1.53 with sigma of 0.02
 C24B-C25B
 1.53 with sigma of 0.02
 C25A-C26
 1.53 with sigma of 0.02
 C25B-C26
 1.53 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C3A) = Uanis(C3B)
Uanis(C21A) = Uanis(C21B)
Uanis(C22A) = Uanis(C22B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C25B)
3. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H4BC)=Sof(H4BD)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=
 Sof(H25D)=Sof(H26C)=Sof(H26D)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H26A)=Sof(H26B)=FVAR(2)
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22C)=Sof(H22D)=1-FVAR(3)
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4(H4AA,H4AB),
 C4(H4BC,H4BD), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C22A(H22A,H22B),
 C22B(H22C,H22D), C23(H23A,H23B), C23(H23C,H23D), C24A(H24A,H24B), C24B(H24C,
 H24D), C25A(H25A,H25B), C25B(H25C,H25D), C26(H26A,H26B), C26(H26C,H26D),
 C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C27(H27), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F)
;
_shelx_res_checksum              21243
_olex2_exptl_crystal_mounting_method Fiber
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.071
_oxdiff_exptl_absorpt_empirical_full_min 0.903