Double Spin Crossovers: A New Double Salt Strategy to Improve Magnetic and Memory Properties
Murray, Keith S.; Phonsri, Wasinee; Jameson, Guy N. L.; Lewis, Barnaby; Chemical Communications  (2019) –; doi:10.1039/C9CC07416C

data_7124389
_publ_section_title
;
 Double Spin Crossovers: A New Double Salt Strategy to Improve Magnetic
 and Memory Properties
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07416C
_journal_year                    2019
_chemical_formula_moiety
'C26 H32 Fe N12, C24 H16 Fe N4 O4, Cl O4, 2(C2 H3 N)'
_chemical_formula_sum            'C54 H54 Cl Fe2 N18 O8'
_chemical_formula_weight         1230.30
_chemical_name_common            '[Fe(3,5 Me2TPM)(TPM)][Fe(azp)2]ClO4 2MeCN'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-22 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.230(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2097(8)
_cell_length_b                   10.5679(3)
_cell_length_c                   32.232(2)
_cell_measurement_reflns_used    15134
_cell_measurement_temperature    299.99(11)
_cell_measurement_theta_max      28.6970
_cell_measurement_theta_min      2.9800
_cell_volume                     5749.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.849
_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     28.00  54.00   0.50   15.64    --  -12.80  38.00 -30.00   52
  2  \w    -26.00  59.00   0.50   15.64    --  -12.80  60.00 -89.00  170
  3  \w     50.00  77.00   0.50   15.64    --   11.70 178.00 120.00   54
  4  \w    -81.00   3.00   0.50   15.64    --  -12.80 -60.00 131.00  168
  5  \w    -11.00  15.00   0.50   15.64    --  -12.80 -99.00  90.00   52
  6  \w    -87.00 -30.00   0.50   15.64    --  -12.80 -19.00   0.00  114
  7  \w    -14.00  12.00   0.50   15.64    --  -12.80 -99.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315632000
_diffrn_orient_matrix_UB_12      -0.0441834000
_diffrn_orient_matrix_UB_13      0.0022028000
_diffrn_orient_matrix_UB_21      -0.0068569000
_diffrn_orient_matrix_UB_22      -0.0172764000
_diffrn_orient_matrix_UB_23      0.0202564000
_diffrn_orient_matrix_UB_31      -0.0268620000
_diffrn_orient_matrix_UB_32      -0.0474310000
_diffrn_orient_matrix_UB_33      -0.0094342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            66647
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         33.558
_diffrn_reflns_theta_min         2.298
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2548
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         19255
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8788
_reflns_number_total             19255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07416c2.cif
_cod_data_source_block           ws283_ht
_cod_database_code               7124389
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Fe3C20H40O2N4
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.970
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C19, C24, C19, C20
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Others
 Sof(N2')=Sof(N1')=1-FVAR(1)
 Sof(N2)=Sof(N1)=FVAR(1)
 Sof(N4')=Sof(N3')=1-FVAR(2)
 Sof(N3)=Sof(N4)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C40(H40), C50(H50)
4.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C49(H49), C42(H42), C43(H43), C41(H41), C47(H47), C32(H32), C2(H2),
 C14(H14), C48(H48), C44(H44), C37(H37), C45(H45), C46(H46), C11(H11), C15(H15),
  C10(H10), C5(H5), C23(H23), C16(H16), C22(H22), C17(H17), C8(H8), C3(H3),
 C9(H9), C4(H4), C21(H21), C20(H20)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C39(H39A,H39B,H39C), C30(H30A,H30B,
 H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C)
;
_shelx_res_checksum              69481
_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 2.566
_oxdiff_exptl_absorpt_empirical_full_min 0.492