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_7717400
_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         'C34 H46 Fe N6, 2(C F3 O3 S)'
_chemical_formula_sum            'C36 H46 F6 Fe N6 O6 S2'
_chemical_formula_weight         892.76
_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'
_atom_sites_solution_hydrogens   geom
_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                 108.114(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8837(3)
_cell_length_b                   10.45420(10)
_cell_length_c                   19.3400(3)
_cell_measurement_reflns_used    18104
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3040
_cell_measurement_theta_min      2.8170
_cell_volume                     4013.09(10)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -75.00  73.00   1.00    4.00    --  -16.70  19.00-120.00  148
  2  \w   -106.00  19.00   1.00    4.00    --  -16.70 -57.00  60.00  125
  3  \w    -50.00  73.00   1.00    4.00    --  -16.70  38.00 -90.00  123
  4  \w   -106.00  10.00   1.00    4.00    --  -16.70 -57.00-180.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0273469000
_diffrn_orient_matrix_UB_12      0.0427294000
_diffrn_orient_matrix_UB_13      0.0139802000
_diffrn_orient_matrix_UB_21      0.0229660000
_diffrn_orient_matrix_UB_22      -0.0510378000
_diffrn_orient_matrix_UB_23      0.0023726000
_diffrn_orient_matrix_UB_31      0.0002518000
_diffrn_orient_matrix_UB_32      0.0132475000
_diffrn_orient_matrix_UB_33      -0.0358945000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.483
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66364
_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    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method 'slow evaporation of the solvent'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_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     516
_refine_ls_number_reflns         9179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0431P)^2^+4.9038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7983
_reflns_number_total             9179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1c6
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_database_code               7717400
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.693
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_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.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6), C6(H6A), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18),
  C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'