Crystalline bilayer formation in homoleptic low-spin Fe(II) compounds with alkyl chain substituents.
Geoghegan, Blaise L.; Koutsoukos, Spyridon; Phonsri, Wasinee; Murray, Keith S.; Cragg, Peter J.; Dymond, Marcus K.; Gass, Ian A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18698–18710; doi:10.1039/d4dt02667e

data_7717398
_publ_section_title
;
 Crystalline bilayer formation in homoleptic low-spin Fe(II) compounds
 with alkyl chain substituents.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18698
_journal_page_last               18710
_journal_paper_doi               10.1039/d4dt02667e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H38 Fe N6, 2(B F4)'
_chemical_formula_sum            'C30 H38 B2 F8 Fe N6'
_chemical_formula_weight         712.16
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2017-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2024-09-09 deposited with the CCDC.	2024-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.377(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6481(3)
_cell_length_b                   18.3359(4)
_cell_length_c                   18.2408(5)
_cell_measurement_reflns_used    23099
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5480
_cell_measurement_theta_min      2.2300
_cell_volume                     3212.72(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9923
_diffrn_measured_fraction_theta_max 0.9923
_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    -79.00  23.00   1.00    8.00    --  -13.00 -72.00 -90.00  102
  2  \w    -29.00  69.00   1.00    8.00    --  -13.00  72.00  30.00   98
  3  \w    -63.00  23.00   1.00    8.00    --  -13.00 -72.00  90.00   86
  4  \w    -80.00  -8.00   1.00    8.00    --  -13.00   0.00 -90.00   72
  5  \w    -35.00 -15.00   1.00    8.00    --  -13.00 -72.00-180.00   20
  6  \w    -49.00  77.00   1.00    8.00    --  -13.00  72.00 -90.00  126
  7  \w    -86.00 -23.00   1.00    8.00    --  -13.00 -54.00 150.00   63
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0497805000
_diffrn_orient_matrix_UB_12      -0.0285968000
_diffrn_orient_matrix_UB_13      0.0037152000
_diffrn_orient_matrix_UB_21      0.0502329000
_diffrn_orient_matrix_UB_22      0.0232631000
_diffrn_orient_matrix_UB_23      -0.0137861000
_diffrn_orient_matrix_UB_31      0.0214326000
_diffrn_orient_matrix_UB_32      0.0117389000
_diffrn_orient_matrix_UB_33      0.0363190000
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37793
_diffrn_reflns_theta_full        27.5000
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.4722
_exptl_crystal_description       block
_exptl_crystal_F_000             1474.2917
_exptl_crystal_recrystallization_method 'Slow evaporation of the solvent'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.9091
_refine_diff_density_min         -0.5715
_refine_diff_density_rms         0.1105
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             8.5088
_refine_ls_goodness_of_fit_ref   1.0449
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0449
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.8891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -9
_reflns_number_gt                5769
_reflns_number_total             7315
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1C4
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_database_code               7717398
_oxdiff_exptl_absorpt_empirical_full_min 0.348
_oxdiff_exptl_absorpt_empirical_full_max 3.425
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F4(0.72) F4'(0.28) B1(0.72) B1'(0.28)
3.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6), C6(H6a), C21(H21)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C27(H27a,H27b), C28(H28a,
 H28b), C29(H29a,H29b)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3a), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C16(H16),
  C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26)
3.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C30(H30a,H30b,H30c)
;
_olex2_submission_special_instructions 'No special instructions were received'