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_7717399
_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         'C38 H54 Fe N6, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H54 F6 Fe N6 O6 S2'
_chemical_formula_weight         948.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2017-08-01
_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                 110.978(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8910(6)
_cell_length_b                   10.3579(2)
_cell_length_c                   19.4682(5)
_cell_measurement_reflns_used    14845
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.6180
_cell_measurement_theta_min      4.6830
_cell_volume                     4498.3(2)
_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  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9933
_diffrn_measured_fraction_theta_max 0.9933
_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    -87.00  77.00   1.00   12.00    --  -13.00  45.00 -90.00  164
  2  \w   -179.00   0.00   1.00   60.00    --  -90.00  60.00-120.00  179
  3  \w   -133.00  -2.00   1.00   60.00    --  -90.00  22.00-150.00  131
  4  \w   -164.00   0.00   1.00   60.00    --  -90.00  60.00 -90.00  164
  5  \w   -153.00  -4.00   1.00   60.00    --  -90.00  60.00  60.00  149
  6  \w   -169.00-105.00   1.00   60.00    --  -90.00  60.00   0.00   64
  7  \w    -96.00 -41.00   1.00   60.00    --  -90.00  45.00  30.00   55
  8  \w   -114.00 -30.00   1.00   60.00    --  -90.00  45.00-150.00   84
  9  \w   -156.00 -57.00   1.00   60.00    --  -90.00  60.00  90.00   99
 10  \w   -162.00-141.00   1.00   60.00    --  -90.00  60.00 -60.00   21
 11  \w   -164.00-143.00   1.00   60.00    --  -90.00  60.00-150.00   21
 12  \w   -179.00-159.00   1.00   60.00    --  -90.00  60.00 -30.00   20
;
_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      0.0061573000
_diffrn_orient_matrix_UB_12      0.1478371000
_diffrn_orient_matrix_UB_13      -0.0024075000
_diffrn_orient_matrix_UB_21      -0.0386904000
_diffrn_orient_matrix_UB_22      -0.0005052000
_diffrn_orient_matrix_UB_23      -0.0825657000
_diffrn_orient_matrix_UB_31      -0.0568646000
_diffrn_orient_matrix_UB_32      0.0163802000
_diffrn_orient_matrix_UB_33      0.0190316000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38312
_diffrn_reflns_theta_full        68.2397
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.96
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.217
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50120
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.4010
_exptl_crystal_description       plate
_exptl_crystal_F_000             1988.7654
_exptl_crystal_recrystallization_method 'Slow evaporation of the solvent'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.8888
_refine_diff_density_min         -0.7713
_refine_diff_density_rms         0.0974
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.1537
_refine_ls_goodness_of_fit_ref   1.0393
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     552
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0393
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1274P)^2^+2.1597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -28
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6741
_reflns_number_total             8188
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1C8
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_database_code               7717399
_oxdiff_exptl_absorpt_empirical_full_min 0.536
_oxdiff_exptl_absorpt_empirical_full_max 2.723
_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.a Ternary CH refined with riding coordinates:
 N6(H6), N3(H3), C6(H6a), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b), C32(H32a,H32b), C35(H35a,H35b), C33(H33a,H33b), C12(H12a,
 H12b), C37(H37a,H37b), C34(H34a,H34b), C13(H13a,H13b), C15(H15a,H15b),
 C18(H18a,H18b), C14(H14a,H14b), C16(H16a,H16b), C36(H36a,H36b), C17(H17a,H17b)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C30(H30), C23(H23), C21(H21), C22(H22), C9(H9), C4(H4), C29(H29),
 C28(H28), C10(H10), C3(H3a), C8(H8), C1(H1), C27(H27), C11(H11), C2(H2)
2.d Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C19(H19a,H19b,H19c)
;
_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
;