Synthesis, mixed-spin-state structure and Langmuir-Blodgett deposition of amphiphilic Fe(iii) quinolylsalicylaldiminate complexes.
Poungsripong, Peeranuch; Boonprab, Theerapoom; Harding, Phimphaka; Murray, Keith S.; Phonsri, Wasinee; Zhang, Ningjin; Kitchen, Jonathan A.; Harding, David J.; RSC advances 14 (2024) 28716–28723; doi:10.1039/d4ra06111j

data_7249332
_publ_section_title
;
 Synthesis, mixed-spin-state structure and Langmuir-Blodgett deposition of
 amphiphilic Fe(iii) quinolylsalicylaldiminate complexes.
;
_journal_issue                   39
_journal_name_full               'RSC advances'
_journal_page_first              28716
_journal_page_last               28723
_journal_paper_doi               10.1039/d4ra06111j
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C56 H70 Fe N4 O4, C H2 Cl2, N O3'
_chemical_formula_sum            'C57 H72 Cl2 Fe N5 O7'
_chemical_formula_weight         1065.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-21 deposited with the CCDC.	2024-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                87.532(3)
_cell_angle_beta                 83.977(3)
_cell_angle_gamma                72.535(3)
_cell_formula_units_Z            4
_cell_length_a                   10.1982(3)
_cell_length_b                   15.7867(6)
_cell_length_c                   35.2740(11)
_cell_measurement_reflns_used    10433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.4850
_cell_measurement_theta_min      2.1160
_cell_volume                     5386.9(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_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    -63.00  69.00   1.00   60.00    --  -20.00  72.00 -30.00  132
  2  \w   -109.00  23.00   1.00   60.00    --  -20.00 -72.00  90.00  132
  3  \w    -36.00  22.00   1.00   60.00    --  -20.00 -38.00 -60.00   58
  4  \w    -36.00  22.00   1.00   60.00    --  -20.00 -38.00 -60.00   58
  5  \w      7.00  56.00   1.00   60.00    --  -20.00  57.00-120.00   49
  6  \w   -103.00 -48.00   1.00   60.00    --  -20.00 -57.00 120.00   55
  7  \w    -62.00 -36.00   1.00   60.00    --  -20.00  72.00  90.00   26
  8  \w     14.00  40.00   1.00   60.00    --  -20.00  72.00  90.00   26
  9  \w    -54.00  19.00   1.00   60.00    --  -20.00 -57.00 150.00   73
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0508089000
_diffrn_orient_matrix_UB_12      0.0238161000
_diffrn_orient_matrix_UB_13      0.0141249000
_diffrn_orient_matrix_UB_21      -0.0478660000
_diffrn_orient_matrix_UB_22      0.0138942000
_diffrn_orient_matrix_UB_23      -0.0138895000
_diffrn_orient_matrix_UB_31      -0.0222166000
_diffrn_orient_matrix_UB_32      -0.0381919000
_diffrn_orient_matrix_UB_33      0.0040591000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            56242
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.764
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         20438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0769P)^2^+4.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12133
_reflns_number_total             20438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra06111j2.cif
_cod_data_source_block           njz_pe_41
_cod_database_code               7249332
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     'EV-BA6863-002 Block'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 95.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C118(H11A,H11B), C117(H11C,H11D), C120(H12A,
 H12B), C122(H12C,H12D), C119(H11E,H11F), C46(H46A,H46B), C121(H12E,H12F),
 C48(H48A,H48B), C123(H12G,H12H), C154(H15A,H15B), C148(H14A,H14B), C47(H47A,
 H47B), C126(H12I,H12J), C125(H12K,H12L), C127(H12M,H12N), C151(H15C,H15D),
 C45(H45A,H45B), C25(H25A,H25B), C24(H24A,H24B), C153(H15E,H15F), C149(H14C,
 H14D), C124(H12O,H12P), C152(H15G,H15H), C51(H51A,H51B), C53(H53A,H53B),
 C145(H14E,H14F), C147(H14G,H14H), C49(H49A,H49B), C19(H19A,H19B), C21(H21A,
 H21B), C22(H22A,H22B), C26(H26A,H26B), C146(H14I,H14J), C23(H23A,H23B),
 C155(H15I,H15J), C52(H52A,H52B), C50(H50A,H50B), C150(H15K,H15L), C55(H55A,
 H55B), C54(H54A,H54B), C20(H20A,H20B), C27(H27A,H27B), C400(H40C,H40D),
 C401(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C116(H116), C110(H110), C115(H115), C105(H105), C29(H29), C38(H38),
 C130(H130), C141(H141), C113(H113), C10(H10), C41(H41), C131(H131), C16(H16),
 C15(H15), C135(H135), C143(H143), C133(H133), C102(H102), C31(H31), C3(H3),
 C138(H138), C134(H134), C13(H13), C107(H107), C1(H1), C35(H35), C103(H103),
 C2(H2), C30(H30), C129(H129), C106(H106), C144(H144), C101(H101), C7(H7),
 C33(H33), C44(H44), C34(H34), C5(H5), C6(H6), C43(H43)
2.c Idealised Me refined as rotating group:
 C156(H15M,H15N,H15O), C128(H12Q,H12R,H12S), C28(H28A,H28B,H28C), C56(H56A,
 H56B,H56C)
;
_shelx_res_checksum              82448
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.711