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_7249333
_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         'C28 H36 N2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C28 H37 N2 O2.5'
_chemical_formula_weight         441.59
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-21 deposited with the CCDC.	2024-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                87.836(2)
_cell_angle_beta                 79.244(2)
_cell_angle_gamma                74.869(3)
_cell_formula_units_Z            4
_cell_length_a                   11.2840(4)
_cell_length_b                   12.1389(4)
_cell_length_c                   19.1724(5)
_cell_measurement_reflns_used    10861
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.4340
_cell_measurement_theta_min      2.0260
_cell_volume                     2490.40(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_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    -58.00  66.00   1.00   30.00    --  -22.90  57.00  90.00  124
  2  \w    -58.00  66.00   1.00   30.00    --  -22.90  57.00   0.00  124
  3  \w   -112.00  15.00   1.00   30.00    --  -22.90 -72.00  60.00  127
  4  \w   -112.00  15.00   1.00   30.00    --  -22.90 -72.00-120.00  127
  5  \w   -112.00  15.00   1.00   30.00    --  -22.90 -72.00 120.00  127
  6  \w    -61.00  66.00   1.00   30.00    --  -22.90  72.00  30.00  127
  7  \w   -112.00  15.00   1.00   30.00    --  -22.90 -72.00-180.00  127
  8  \w    -61.00 -36.00   1.00   30.00    --  -22.90  72.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0418750000
_diffrn_orient_matrix_UB_12      0.0512882000
_diffrn_orient_matrix_UB_13      -0.0082886000
_diffrn_orient_matrix_UB_21      -0.0140913000
_diffrn_orient_matrix_UB_22      0.0169342000
_diffrn_orient_matrix_UB_23      0.0362525000
_diffrn_orient_matrix_UB_31      0.0493494000
_diffrn_orient_matrix_UB_32      0.0273349000
_diffrn_orient_matrix_UB_33      -0.0059440000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0495
_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       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45828
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83518
_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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         10166
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.3709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6046
_reflns_number_total             10166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra06111j2.cif
_cod_data_source_block           njz_pe_longchain
_cod_original_formula_sum        'C28 H37 N2 O2.50'
_cod_database_code               7249333
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H N O '
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.996
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C131-C130
 1.55 with sigma of 0.01
 C128-C127
 1.55 with sigma of 0.01
3. Others
 Fixed Sof: H12K(0.65) H12L(0.65) H12M(0.35) H12N(0.35) C126(0.65) H12O(0.65)
 H12P(0.65) C127(0.65) H12Q(0.65) H12R(0.65) C128(0.65) H12S(0.65) H12T(0.65)
 H12U(0.65) C129(0.35) H12V(0.35) H12W(0.35) C130(0.35) H13A(0.35) H13B(0.35)
 C131(0.35) H13C(0.35) H13D(0.35) H13E(0.35) O200(0.5) H20C(0.5) H20D(0.5)
 O201(0.5) H20E(0.5) H20F(0.5)
4.a Free rotating group:
 O200(H20C,H20D), O201(H20E,H20F)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C117(H11A,H11B), C118(H11C,H11D), C119(H11E,
 H11F), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H),
 C124(H12I,H12J), C125(H12K,H12L), C125(H12M,H12N), C126(H12O,H12P), C127(H12Q,
 H12R), C129(H12V,H12W), C130(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C15(H15),
  C16(H16), C101(H101), C102(H10A), C103(H103), C105(H105), C106(H106),
 C107(H107), C110(H110), C113(H113), C115(H115), C116(H116)
4.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C128(H12S,H12T,H12U), C131(H13C,H13D,H13E)
;
_shelx_res_checksum              26438
_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.681