Hysteretic spin crossover driven by anion conformational change
Phukkaphan, Natnaree; Cruickshank, Dyanne L.; Murray, Keith S.; Phonsri, Wasinee; Harding, Phimphaka; Harding, David J.; Chem. Commun.  (2017) –; doi:10.1039/C7CC05998A

data_7120548
_publ_section_title
;
 Hysteretic spin crossover driven by anion conformational change
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05998A
_journal_year                    2017
_chemical_formula_moiety         'C32 H20 Fe I2 N4 O2, C2 F6 N O4 S2'
_chemical_formula_sum            'C34 H20 F6 Fe I2 N5 O6 S2'
_chemical_formula_weight         1082.34
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-05-29 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                68.956(2)
_cell_angle_beta                 79.436(2)
_cell_angle_gamma                66.531(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3597(3)
_cell_length_b                   12.7897(3)
_cell_length_c                   13.7188(3)
_cell_measurement_reflns_used    12059
_cell_measurement_temperature    276(1)
_cell_measurement_theta_max      69.9160
_cell_measurement_theta_min      3.4060
_cell_volume                     1854.49(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      276(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9877
_diffrn_measured_fraction_theta_max 0.9882
_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    105.00 175.00   0.50    0.80    --  104.00  19.00 150.00  140
  2  \w    117.00 175.00   0.50    0.80    --  104.00 125.00 150.00  116
  3  \w    124.00 175.00   0.50    0.80    --  104.00  19.00 -90.00  102
  4  \w    105.00 132.00   0.50    0.80    --  104.00  19.00-180.00   54
  5  \w    138.00 172.00   0.50    0.80    --  104.00  19.00-180.00   68
  6  \w     -7.00  69.00   0.50    0.20    --    0.57  57.00-150.00  152
  7  \w      1.00  57.00   0.50    0.20    --   -0.57  37.00 -30.00  112
  8  \w     13.00  38.00   0.50    0.20    --   -0.57  19.00  60.00   50
  9  \w     39.00  65.00   0.50    0.20    --   -0.57  19.00  60.00   52
 10  \w     -2.00  70.00   0.50    0.20    --   -0.57  37.00 120.00  144
 11  \w    -30.00  -5.00   0.50    0.20    --   -0.57 -77.00  90.00   50
 12  \w   -153.00 -83.00   0.50    0.80    --  -82.50 -19.00-150.00  140
 13  \w     46.00 107.00   0.50    0.80    --  104.00-125.00-150.00  122
 14  \w     60.00  93.00   0.50    0.80    --  104.00 -99.00 -90.00   66
 15  \w     55.00 107.00   0.50    0.80    --  104.00 -99.00 -60.00  104
 16  \w     88.00 118.00   0.50    0.80    --  104.00-125.00 -30.00   60
 17  \w     87.00 119.00   0.50    0.80    --  104.00-125.00  90.00   64
 18  \w     33.00  58.00   0.50    0.80    --  104.00-125.00  90.00   50
 19  \w     35.00 107.00   0.50    0.80    --  104.00 -99.00  60.00  144
 20  \w     34.00 111.00   0.50    0.80    --  104.00-125.00-180.00  154
 21  \w     40.00  94.00   0.50    0.80    --  104.00 -99.00-120.00  108
 22  \w     37.00  93.00   0.50    0.80    --  104.00 -57.00 -60.00  112
 23  \w     34.00  61.00   0.50    0.80    --  104.00 -37.00-120.00   54
 24  \w     38.00  67.00   0.50    0.80    --  104.00 -37.00-150.00   58
 25  \w     76.00 102.00   0.50    0.80    --  104.00 -19.00 -30.00   52
 26  \w     68.00  96.00   0.50    0.80    --  104.00 -57.00 150.00   56
 27  \w    -80.00 -12.00   0.50    0.80    --  -82.50  19.00   0.00  136
 28  \w    -46.00 -16.00   0.50    0.80    --  -82.50  57.00-180.00   60
 29  \w    -89.00 -63.00   0.50    0.80    --  -82.50  57.00-180.00   52
 30  \w     35.00  69.00   0.50    0.80    --  104.00 -37.00 -90.00   68
 31  \w     46.00  71.00   0.50    0.80    --  104.00 -37.00 -60.00   50
 32  \w     33.00  71.00   0.50    0.80    --  104.00 -37.00  30.00   76
 33  \w     44.00  74.00   0.50    0.80    --  104.00 -57.00  60.00   60
 34  \w     63.00  89.00   0.50    0.80    --  104.00 -57.00  90.00   52
 35  \w     35.00  62.00   0.50    0.80    --  104.00 -37.00 150.00   54
 36  \w     37.00  71.00   0.50    0.80    --  104.00 -38.00 178.00   68
;
_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      -0.0763381000
_diffrn_orient_matrix_UB_12      -0.0636345000
_diffrn_orient_matrix_UB_13      -0.0136384000
_diffrn_orient_matrix_UB_21      -0.0914628000
_diffrn_orient_matrix_UB_22      0.1227878000
_diffrn_orient_matrix_UB_23      -0.0560896000
_diffrn_orient_matrix_UB_31      0.0656728000
_diffrn_orient_matrix_UB_32      -0.0068849000
_diffrn_orient_matrix_UB_33      -0.1057217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19930
_diffrn_reflns_theta_full        70.0394
_diffrn_reflns_theta_max         70.04
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.130
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.12b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168.000
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.1612
_refine_diff_density_min         -1.3966
_refine_diff_density_rms         0.1056
_refine_ls_d_res_high            0.8202
_refine_ls_d_res_low             12.7896
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0281
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+2.7085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                6046
_reflns_number_total             6966
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc05998a2.cif
_cod_data_source_block           NP08_275K
_cod_original_cell_volume        1854.50(9)
_cod_database_code               7120548
_chemical_oxdiff_formula         'C34 H20 Co1 F6 I2 N3 O8 S2'
_diffrn_oxdiff_ac3_digest_frames
;
014b1c36adc79efab1140c4ea95122bdf90306015e8
;
_diffrn_oxdiff_ac3_digest_hkl
;
01545b1cc1763d10277620ce34aabc01d41af3
;
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C26(H26), C7(H7), C5(H5), C1(H1), C6(H6), C23(H23), C31(H31),
 C28(H28), C17(H17), C12(H12), C30(H30), C15(H15), C2(H2), C22(H22), C14(H14),
 C3(H3), C21(H21), C19(H19), C18(H18)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.696
_oxdiff_exptl_absorpt_empirical_full_min 0.690