Spin-crossover iron (II) complex showing thermal hysteresis around room temperature with symmetry breaking and an unusually high T(LIESST) of 120 K.
Clemente Leon, Miguel; García-López, Víctor; Palacios-Corella, Mario; Cardona-Serra, Salvador; Coronado, Eugenio; Chemical Communications  (2019) –; doi:10.1039/C9CC05988A

data_7124158
_publ_section_title
;
 Spin-crossover iron (II) complex showing thermal hysteresis around room
 temperature with symmetry breaking and an unusually high T(LIESST) of 120
 K.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05988A
_journal_year                    2019
_chemical_formula_moiety         '2(C26 H18 Fe N10 O8), 4(Cl O4), 7(C3 H6 O)'
_chemical_formula_sum            'C73 H78 Cl4 Fe2 N20 O39'
_chemical_formula_weight         2113.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.    2019-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.715(2)
_cell_angle_beta                 88.876(2)
_cell_angle_gamma                89.761(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8517(4)
_cell_length_b                   18.4107(4)
_cell_length_c                   19.5908(4)
_cell_measurement_reflns_used    8663
_cell_measurement_temperature    300.05(10)
_cell_measurement_theta_max      21.5510
_cell_measurement_theta_min      3.4950
_cell_volume                     4633.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_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    -66.00 -12.00   1.00   15.00    --  -15.04 -57.00  60.00   54
  2  \w    -74.00   5.00   1.00   15.00    --  -15.04 -67.00 146.34   79
  3  \w    -81.00   6.00   1.00   15.00    --  -15.04 -57.00-120.00   87
  4  \w    -83.00  -3.00   1.00   15.00    --  -15.04 -67.00  12.67   80
  5  \w    -53.00  40.00   1.00   15.00    --   15.83 -69.00  39.19   93
  6  \w    -52.00  39.00   1.00   15.00    --   15.83 -64.00 150.13   91
  7  \w    -52.00  39.00   1.00   15.00    --   15.83 -64.00 -41.43   91
  8  \w    -22.00  37.00   1.00   15.00    --   15.83 -57.00  90.00   59
  9  \w    -36.00  40.00   1.00   15.00    --   15.83 -68.00-123.46   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0546443000
_diffrn_orient_matrix_UB_12      0.0051198000
_diffrn_orient_matrix_UB_13      -0.0015262000
_diffrn_orient_matrix_UB_21      -0.0026956000
_diffrn_orient_matrix_UB_22      0.0029942000
_diffrn_orient_matrix_UB_23      0.0360251000
_diffrn_orient_matrix_UB_31      0.0073505000
_diffrn_orient_matrix_UB_32      0.0380774000
_diffrn_orient_matrix_UB_33      -0.0034467000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.1387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64980
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1260
_refine_ls_number_reflns         19501
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.0817
_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^)+(0.0978P)^2^+1.2690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8691
_reflns_number_total             19501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05988a3.cif
_cod_data_source_block           vg1801c77
_cod_original_cell_volume        4633.2(2)
_cod_database_code               7124158
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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, All O(H) groups
2. Restrained distances
 O31B-Cl4
 1.35 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O30A \\sim O30B \\sim O31A \\sim O31B \\sim O32A \\sim O32B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(O31A)=1-FVAR(1)
 Sof(O30B)=FVAR(1)
 Fixed Sof: O30A(0.5) O31B(0.5) O32A(0.5) O32B(0.5) C56A(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C56B(0.5) H56D(0.5) H56E(0.5) H56F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C3(H3A), C5(H5A), C6(H6), C7(H7A), C9(H9), C11(H11), C14(H14),
 C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C27(H27), C29(H29),
  C31(H31), C32(H32), C33(H33), C35(H35), C37(H37), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C48(H48), C50(H50)
5.b Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56A(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C56B(H56D,H56E,H56F)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O5(H5), O7(H7), O9(H9A), O11(H11A), O13(H13), O15(H15)
;
_shelx_res_checksum              6533
_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 1.686
_oxdiff_exptl_absorpt_empirical_full_min 0.577