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_7717404
_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
'C50 H78 Fe N6, 2(B F4), 0.5(H2 O), 0.5(C H4 O)'
_chemical_formula_sum            'C50.5 H81 B2 F8 Fe N6 O'
_chemical_formula_weight         1017.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-02
_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                88.8600(10)
_cell_angle_beta                 86.8620(10)
_cell_angle_gamma                89.547(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5737(2)
_cell_length_b                   17.0941(3)
_cell_length_c                   29.4514(4)
_cell_measurement_reflns_used    43689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8400
_cell_measurement_theta_min      2.3040
_cell_volume                     5314.12(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -35.00  73.00   1.00   40.00    --  -17.00  72.00-150.00  108
  2  \w    -69.00  22.00   1.00   40.00    --  -17.00 -72.00  90.00   91
  3  \w    -69.00  22.00   1.00   40.00    --  -17.00 -72.00 -90.00   91
  4  \w    -85.00 -21.00   1.00   40.00    --  -17.00   0.00  90.00   64
  5  \w    -31.00 -13.00   1.00   40.00    --  -17.00  54.00  60.00   18
  6  \w    -78.00  73.00   1.00   40.00    --  -17.00  18.00-180.00  151
  7  \w    -31.00  73.00   1.00   40.00    --  -17.00  54.00-120.00  104
  8  \w    -62.00  22.00   1.00   40.00    --  -17.00 -72.00 -60.00   84
  9  \w    -76.00  20.00   1.00   40.00    --  -17.00 -72.00 120.00   96
 10  \w    -85.00 -24.00   1.00   40.00    --  -17.00 -72.00  60.00   61
 11  \w   -107.00  22.00   1.00   40.00    --  -17.00 -72.00-120.00  129
;
_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      0.0086449000
_diffrn_orient_matrix_UB_12      -0.0196990000
_diffrn_orient_matrix_UB_13      0.0210396000
_diffrn_orient_matrix_UB_21      0.0281339000
_diffrn_orient_matrix_UB_22      -0.0320912000
_diffrn_orient_matrix_UB_23      -0.0117592000
_diffrn_orient_matrix_UB_31      0.0603937000
_diffrn_orient_matrix_UB_32      0.0174554000
_diffrn_orient_matrix_UB_33      0.0010009000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            121955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63093
_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_density_diffrn    1.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.189
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         24353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0715
_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^)+(0.0565P)^2^+11.9097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19406
_reflns_number_total             24353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02667e2.cif
_cod_data_source_block           1c14
_cod_depositor_comments
'Adding full bibliography for 7717398--7717404.cif.'
_cod_original_formula_sum        'C50.50 H81 B2 F8 Fe N6 O'
_cod_database_code               7717404
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.658
_oxdiff_exptl_absorpt_empirical_full_max 1.716
_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, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: F13(0.4) F13'(0.6) F14(0.4) F14'(0.6)
3.a Free rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 N3(H3), N6(H6), N9(H9A), N12(H12), C6(H6A), C31(H31), C56(H56), C81(H81)
3.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C37(H37A,H37B),
  C38(H38A,H38B), 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), C62(H62A,H62B), C63(H63A,H63B),
  C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,
 H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
 C73(H73A,H73B), C74(H74A,H74B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B),
  C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,
 H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
 C99(H99A,H99B)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C26(H26),
  C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36),
 C51(H51), C52(H52), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60), C61(H61),
  C76(H76), C77(H77), C78(H78), C79(H79), C83(H83), C84(H84), C85(H85), C86(H86)
3.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C75(H75A,H75B,H75C), C100(H10A,H10B,
 H10C), C101(H10D,H10E,H10F)
3.f Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'