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_7717401
_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         'C46 H70 Fe N6, 2(C F3 O3 S)'
_chemical_formula_sum            'C48 H70 F6 Fe N6 O6 S2'
_chemical_formula_weight         1061.10
_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                 104.208(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5740(7)
_cell_length_b                   10.1229(2)
_cell_length_c                   19.4863(3)
_cell_measurement_reflns_used    18505
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      69.7730
_cell_measurement_theta_min      3.3410
_cell_volume                     5272.81(19)
_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 0.9869
_diffrn_measured_fraction_theta_max 0.9869
_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    -89.00  89.00   0.50    4.00    --    0.00  60.00-180.00  356
  2  \w    -13.00  57.00   0.50    4.00    --    0.00  60.00-150.00  140
  3  \w    -89.00  89.00   0.50    4.00    --    0.00  14.00 120.00  356
  4  \w   -168.00-142.00   0.50   20.00    --  -90.00  60.00  30.00   52
  5  \w   -136.00 -97.00   0.50   20.00    --  -90.00  60.00  30.00   78
  6  \w   -177.00 -77.00   0.50   20.00    --  -90.00  60.00-180.00  200
  7  \w    -45.00  -3.00   0.50   20.00    --  -90.00  60.00-180.00   84
  8  \w    -34.00  -6.00   0.50   20.00    --  -90.00  60.00  30.00   56
  9  \w   -178.00-114.00   0.50   20.00    --  -90.00  60.00 -60.00  128
 10  \w    -78.00  -1.00   0.50   20.00    --  -90.00  60.00 -60.00  154
 11  \w   -127.00 -81.00   0.50   20.00    --  -90.00  60.00-120.00   92
 12  \w    -28.00  -2.00   0.50   20.00    --  -90.00  60.00-120.00   52
 13  \w   -174.00-148.00   0.50   20.00    --  -90.00  60.00  60.00   52
 14  \w   -178.00 -74.00   0.50   20.00    --  -90.00  57.00 120.00  208
 15  \w   -179.00 -99.00   0.50   20.00    --  -90.00  57.00 -30.00  160
 16  \w    -94.00  -2.00   0.50   20.00    --  -90.00  57.00 -30.00  184
 17  \w   -178.00-132.00   0.50   20.00    --  -90.00  57.00  90.00   92
 18  \w    -62.00 -23.00   0.50   20.00    --  -90.00  57.00  90.00   78
 19  \w   -128.00-102.00   0.50   20.00    --  -90.00  43.00  90.00   52
 20  \w    -27.00  -1.00   0.50   20.00    --  -90.00  43.00  90.00   52
 21  \w   -170.00 -85.00   0.50   20.00    --  -90.00  43.00-120.00  170
 22  \w    -37.00 -11.00   0.50   20.00    --  -90.00  43.00-120.00   52
 23  \w    -65.00 -37.00   0.50   20.00    --  -90.00  43.00  90.00   56
 24  \w   -115.00  -1.00   0.50   20.00    --  -90.00  14.00  90.00  228
 25  \w    -89.00 -63.00   0.50   20.00    --  -90.00  14.00 120.00   52
 26  \w   -140.00-100.00   0.50   20.00    --  -90.00  14.00 120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0055650000
_diffrn_orient_matrix_UB_12      -0.1460214000
_diffrn_orient_matrix_UB_13      -0.0189148000
_diffrn_orient_matrix_UB_21      -0.0573090000
_diffrn_orient_matrix_UB_22      -0.0123408000
_diffrn_orient_matrix_UB_23      -0.0253449000
_diffrn_orient_matrix_UB_31      0.0025803000
_diffrn_orient_matrix_UB_32      0.0409222000
_diffrn_orient_matrix_UB_33      -0.0751857000
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52976
_diffrn_reflns_theta_full        70.0543
_diffrn_reflns_theta_max         70.05
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71869
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.3366
_exptl_crystal_description       plate
_exptl_crystal_F_000             2245.3411
_exptl_crystal_recrystallization_method 'Slow evaporation of the solvent'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.5981
_refine_diff_density_min         -0.5394
_refine_diff_density_rms         0.0860
_refine_ls_d_res_high            0.8201
_refine_ls_d_res_low             13.3653
_refine_ls_goodness_of_fit_ref   1.0043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    114
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0043
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0764P)^2^+4.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              32
_reflns_limit_h_min              -33
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7089
_reflns_number_total             9879
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1C12
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_database_code               7717401
_oxdiff_exptl_absorpt_empirical_full_min 0.649
_oxdiff_exptl_absorpt_empirical_full_max 1.451
_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: F2'(0.5) F3'(0.5) O2(0.65) S1'(0.35) S1(0.65) O3'(0.35) O2'(0.35)
 O3(0.65) F3(0.5) F2(0.5)
3.a Ternary CH refined with riding coordinates:
 N6(H6), N3(H3), C6(H6a), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C35(H35a,H35b), C18(H18a,H18b), C37(H37a,H37b), C12(H12a,H12b), C38(H38a,
 H38b), C39(H39a,H39b), C16(H16a,H16b), C41(H41a,H41b), C42(H42a,H42b),
 C15(H15a,H15b), C13(H13a,H13b), C19(H19a,H19b), C44(H44a,H44b), C17(H17a,H17b),
  C40(H40a,H40b), C36(H36a,H36b), C20(H20a,H20b), C14(H14a,H14b), C43(H43a,
 H43b), C45(H45a,H45b), C21(H21a,H21b), C22(H22a,H22b)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C11(H11), C25(H25), C34(H34), C26(H26), C1(H1), C3(H3a),
 C9(H9), C8(H8), C4(H4), C10(H10), C32(H32), C33(H33), C2(H2), C31(H31)
3.d Idealised Me refined as rotating group:
 C46(H46a,H46b,H46c), C23(H23a,H23b,H23c)
;
_olex2_submission_special_instructions 'No special instructions were received'