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_7124159
_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         'C26 H18 Fe N10 O8), 2(Cl O4), 3.5(C3 H6 O)'
_chemical_formula_sum            'C36.5 H39 Cl2 Fe N10 O19.5'
_chemical_formula_weight         1056.53
_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             2019-07-29
_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                90
_cell_angle_beta                 91.571(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2527(3)
_cell_length_b                   17.9600(3)
_cell_length_c                   12.8378(2)
_cell_measurement_reflns_used    8938
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.9390
_cell_measurement_theta_min      3.5490
_cell_volume                     4437.37(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
  1 omega  -84.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -57.0000   60.0000 89

  2 omega  -66.00    6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -57.0000  -60.0000 72

  3 omega  -36.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442   57.0000 -150.0000 90

  4 omega  -64.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -57.0000  150.0000 51

  5 omega   12.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -57.0000 -150.0000 25

  6 omega  -25.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -57.0000  -90.0000 49
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0493327000
_diffrn_orient_matrix_UB_12      0.0168342000
_diffrn_orient_matrix_UB_13      -0.0063113000
_diffrn_orient_matrix_UB_21      0.0106074000
_diffrn_orient_matrix_UB_22      0.0025364000
_diffrn_orient_matrix_UB_23      -0.0358987000
_diffrn_orient_matrix_UB_31      -0.0225367000
_diffrn_orient_matrix_UB_32      -0.0356258000
_diffrn_orient_matrix_UB_33      -0.0055446000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32411
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9404
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0434P)^2^+6.0488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6897
_reflns_number_total             9404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05988a3.cif
_cod_data_source_block           vg1801a77
_cod_original_formula_sum        'C36.5 H39 Cl2 Fe1 N10 O19.5'
_cod_database_code               7124159
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.809
_reflns_odcompleteness_completeness 99.72
_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. Uiso/Uaniso restraints and constraints
O20 \\sim C36 \\sim C37: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Rigid body (RIGU) restrains
 O20, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O20(0.5) C36(0.5) H36a(0.5) H36b(0.5) H36c(0.5) C37(0.5) C38(0.5)
 H38a(0.5) H38b(0.5) H38c(0.5)
5.a Me refined with riding coordinates:
 C36(H36a,H36b,H36c)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9a), C11(H11a), C14(H14),
 C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24)
5.c Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c), C32(H32a,H32b,
 H32c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C38(H38a,H38b,H38c)
5.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O11(H11), O13(H13), O15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'