Reverse micelle synthesis and downsizing effects in iron(iii) spin crossover materials.
Lazaro, Sharon E.; Harding, Phimphaka; Boonyang, Upsorn; Telfer, Shane G.; Phonsri, Wasinee; Murray, Keith S.; Harding, David J.; RSC advances 16 (2026) 5707–5715; doi:10.1039/d5ra07308a

data_7251741
_publ_section_title
;
 Reverse micelle synthesis and downsizing effects in iron(iii) spin
 crossover materials.
;
_journal_issue                   7
_journal_name_full               'RSC advances'
_journal_page_first              5707
_journal_page_last               5715
_journal_paper_doi               10.1039/d5ra07308a
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C32 H22 Fe N4 O2, N O3, C2 H6 O'
_chemical_formula_sum            'C34 H28 Fe N5 O6'
_chemical_formula_weight         658.46
_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             2025-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-26 deposited with the CCDC.	2026-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.389(6)
_cell_angle_beta                 78.976(6)
_cell_angle_gamma                67.687(5)
_cell_formula_units_Z            2
_cell_length_a                   10.2636(11)
_cell_length_b                   11.9494(11)
_cell_length_c                   12.8936(12)
_cell_measurement_reflns_used    4291
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      3.5
_cell_volume                     1435.9(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
scan:
	Number of images: 36
	           Slice: 20.0000 - 200.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 36
	           Slice: 20.0000 - 200.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 36
	           Slice: 20.0000 - 200.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 36
	           Slice: 20.0000 - 200.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 35
	           Slice: 22.0000 - 197.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 31
	           Slice: 44.0000 - 199.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1482
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5398
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.056
_diffrn_reflns_theta_min         3.492
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0014(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.1059
_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^)+(0.1829P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2785
_refine_ls_wR_factor_ref         0.3282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2978
_reflns_number_total             5398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra07308a2.cif
_cod_data_source_block           sel13
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7251741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.453
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.919(5)
 0.081(5)
2. 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, All O(H,H) groups
3. Restrained distances
 O6-C33 \\sim O6-C33A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 O6-C34 \\sim O6-C34A
 with sigma of 0.04
4. Rigid bond restraints
 C33A, C34A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C34A \\sim C33A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
6. Rigid body (RIGU) restrains
 C34, C33, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H6A(0.65) H6B(0.35) C33(0.65) H33A(0.65) H33B(0.65) C34(0.65)
 H34A(0.65) H34B(0.65) H34C(0.65) C33A(0.35) H33C(0.35) H33D(0.35) C34A(0.35)
 H34D(0.35) H34E(0.35) H34F(0.35)
8.a Free rotating group:
 O6(C33,C34)
8.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C33A(H33C,H33D)
8.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C13(H13), C24(H24), C31(H31), C12(H12), C29(H29), C6(H6), C10(H10),
 C17(H17), C18(H18), C15(H15), C1(H1), C2(H2), C14(H14), C8(H8), C30(H30),
 C7(H7), C3(H3), C28(H28), C19(H19), C23(H23), C22(H22)
8.d Tetrahedral OH refined with riding coordinates:
 O6(H6A), O6(H6B)
8.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              43538
_olex2_submission_special_instructions 'No special instructions were received'