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_7715327
_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      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 106.339(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9243(7)
_cell_length_b                   24.8378(10)
_cell_length_c                   16.4756(5)
_cell_measurement_reflns_used    12053
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      30.1410
_cell_measurement_theta_min      1.7180
_cell_volume                     5860.6(4)
_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      340(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.896
_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   25.00   0.00  20.00   0.00    --   360
  2  \w    -19.50  27.50   0.50   25.00    --   20.00  90.00   0.00   94
  3  \w    -19.50  27.50   0.50   25.00    --   20.00  90.00  90.00   94
  4  \w    -19.50  27.50   0.50   25.00    --   20.00  90.00 180.00   94
  5  \w    -19.50  27.50   0.50   25.00    --   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      -0.0193262000
_diffrn_orient_matrix_UB_12      -0.0256279000
_diffrn_orient_matrix_UB_13      -0.0137340000
_diffrn_orient_matrix_UB_21      0.0434615000
_diffrn_orient_matrix_UB_22      -0.0122829000
_diffrn_orient_matrix_UB_23      0.0202040000
_diffrn_orient_matrix_UB_31      -0.0137862000
_diffrn_orient_matrix_UB_32      -0.0027696000
_diffrn_orient_matrix_UB_33      0.0376363000
_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  0.0172
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25526
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.591
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97545
_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    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             2212
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.615
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.247
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0849P)^2^+1.1297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5748
_reflns_number_total             8084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00425f2.cif
_cod_data_source_block           1_340K
_cod_depositor_comments
'Adding full bibliography for 7715321--7715329.cif.'
_cod_database_code               7715327
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C1A-C2A
 1.53 with sigma of 0.02
 C1B-C2B
 1.53 with sigma of 0.02
 C2A-C3A
 1.53 with sigma of 0.02
 C2B-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
2. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
3. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=Sof(H4BC)=Sof(H4BD)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B)
4.b Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32)
;
_shelx_res_checksum              1651
_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 1.144
_oxdiff_exptl_absorpt_empirical_full_min 0.873