The disentangling of hysteretic spin transition, polymorphism and metastability in bistable thin films formed by sublimation of bis(scorpionate) Fe(ii) molecules
Iasco, O.; Boillot, M.-L.; Bellec, A.; Guillot, R.; Rivière, E.; Mazerat, S.; Nowak, S.; Morineau, D.; Brosseau, A.; Miserque, F.; Repain, V.; Mallah, T.; Journal of Materials Chemistry C 5 (2017) 11067–; doi:10.1039/C7TC03276E

data_7236897
_publ_section_title
;
 The disentangling of hysteretic spin transition, polymorphism and
 metastability in bistable thin films formed by sublimation of
 bis(scorpionate) Fe(ii) molecules
;
_journal_issue                   42
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              11067
_journal_paper_doi               10.1039/C7TC03276E
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C60 H88 B4 Fe2 N24 O0'
_chemical_formula_weight         1300.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.669(5)
_cell_length_b                   20.669(5)
_cell_length_c                   8.603(3)
_cell_measurement_reflns_used    307
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      14.45
_cell_measurement_theta_min      2.75
_cell_volume                     3675.3(18)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  1.3178
_diffrn_reflns_av_unetI/netI     0.3063
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            42038
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.694
_diffrn_reflns_theta_max         20.694
_diffrn_reflns_theta_min         2.203
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.9912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.42(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1998
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.3011
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+20.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2503
_refine_ls_wR_factor_ref         0.3314
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                712
_reflns_number_total             1998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc03276e2.cif
_cod_data_source_block           Fe_T253k_tetragonal
_cod_original_cell_volume        3675(2)
_cod_database_code               7236897
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.996
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              15933
_shelx_hkl_checksum              82945
_shelx_fab_checksum              60450