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_7717402
_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         'C54 H86 Fe N6, 2(C F3 O3 S)'
_chemical_formula_sum            'C56 H86 F6 Fe N6 O6 S2'
_chemical_formula_weight         1173.27
_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             2017-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2024-09-09 deposited with the CCDC.	2024-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.330(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   60.541(2)
_cell_length_b                   10.3428(5)
_cell_length_c                   19.2128(10)
_cell_measurement_reflns_used    18827
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      69.694
_cell_measurement_theta_min      2.9510
_cell_volume                     11903.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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   -103.00  77.00   1.00    8.00    --  -13.00  60.00-150.00  180
  2  \w     -7.00  25.00   1.00    8.00    --  -13.00  60.00 120.00   32
  3  \w   -179.00   0.00   1.00   40.00    --  -90.00  60.00 150.00  179
  4  \w   -179.00   0.00   1.00   40.00    --  -90.00  60.00  60.00  179
  5  \w   -173.00  -2.00   1.00   40.00    --  -90.00  60.00-150.00  171
  6  \w   -109.00   0.00   1.00   40.00    --  -90.00  40.00  90.00  109
  7  \w   -179.00 -29.00   1.00   40.00    --  -90.00  60.00 -30.00  150
  8  \w   -142.00  -6.00   1.00   40.00    --  -90.00  50.00  30.00  136
  9  \w   -108.00 -31.00   1.00   40.00    --  -90.00  40.00 120.00   77
 10  \w   -166.00 -17.00   1.00   40.00    --  -90.00  60.00-120.00  149
 11  \w   -162.00 -29.00   1.00   40.00    --  -90.00  50.00-180.00  133
 12  \w   -126.00 -27.00   1.00   40.00    --  -90.00  60.00 -90.00   99
 13  \w   -179.00 -48.00   1.00   40.00    --  -90.00  60.00   0.00  131
 14  \w   -176.00 -28.00   1.00   40.00    --  -90.00  60.00  90.00  148
 15  \w   -107.00 -53.00   1.00   40.00    --  -90.00  30.00 150.00   54
 16  \w   -156.00-130.00   1.00   40.00    --  -90.00  30.00-180.00   26
 17  \w   -100.00 -28.00   1.00   40.00    --  -90.00  50.00 -30.00   72
 18  \w   -179.00 -84.00   1.00   40.00    --  -90.00   0.00 -30.00   95
 19  \w   -133.00-113.00   1.00   40.00    --  -90.00  50.00 -90.00   20
 20  \w   -169.00-148.00   1.00   40.00    --  -90.00  60.00 -60.00   21
 21  \w   -162.00-141.00   1.00   40.00    --  -90.00  60.00  30.00   21
 22  \w   -164.00-143.00   1.00   40.00    --  -90.00  60.00-180.00   21
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       72
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70453
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         2.951
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (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    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             4992
_exptl_crystal_recrystallization_method 'Slow evaporation of the solvent'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         10876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1081P)^2^+58.2557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8122
_reflns_number_total             10876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1c16
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_original_cell_volume        11903.4(10)
_cod_database_code               7717402
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.616
_oxdiff_exptl_absorpt_empirical_full_max 1.761
_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 C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H12A(0.55) H12B(0.55) H12C(0.45) H12D(0.45) C13(0.55) H13A(0.55)
 H13B(0.55) C13'(0.45) H13C(0.45) H13D(0.45) C14(0.55) H14A(0.55) H14B(0.55)
 C14'(0.45) H14C(0.45) H14D(0.45) C15(0.55) H15A(0.55) H15B(0.55) C15'(0.45)
 H15C(0.45) H15D(0.45) H16A(0.55) H16B(0.55) H16C(0.45) H16D(0.45)
3.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6), C6(H6A), C33(H33)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12(H12C,H12D), C13(H13A,H13B), C13'(H13C,H13D), C14(H14A,
 H14B), C14'(H14C,H14D), C15(H15A,H15B), C15'(H15C,H15D), C16(H16A,H16B),
 C16(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B)
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), C28(H28),
  C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C54(H54A,H54B,H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'