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_7120550
_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                78.012(9)
_cell_angle_beta                 68.748(10)
_cell_angle_gamma                68.609(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4339(13)
_cell_length_b                   12.7007(13)
_cell_length_c                   12.9423(13)
_cell_measurement_reflns_used    4641
_cell_measurement_temperature    245.00(10)
_cell_measurement_theta_max      67.7020
_cell_measurement_theta_min      3.6690
_cell_volume                     1766.9(4)
_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      N~2~
_diffrn_ambient_temperature      245.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9656
_diffrn_measured_fraction_theta_max 0.9656
_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    -31.00  16.00   0.50    2.00    --    0.00 -77.00 120.00   94
  2  \w    -68.00  -7.00   0.50    2.00    --    0.00 -19.00-120.00  122
  3  \w    -70.00  -1.00   0.50    2.00    --    0.00 -37.00-180.00  138
  4  \w      7.00  51.00   0.50    2.00    --    0.00  19.00  30.00   88
  5  \w     -1.00  56.00   0.50    2.00    --    0.00  37.00 -60.00  114
  6  \w    -21.00  21.00   0.50    2.00    --    0.00 -87.00  72.00   84
  7  \w    -86.00 -16.00   0.50   10.00    --  -80.49  57.00   0.00  140
  8  \w    -95.00 -59.00   0.50   10.00    --  -80.49 125.00   0.00   72
  9  \w   -149.00 -81.00   0.50   10.00    --  -80.49 -19.00-180.00  136
 10  \w   -151.00 -81.00   0.50   10.00    --  -80.49 -19.00 -90.00  140
 11  \w   -152.00-127.00   0.50   10.00    --  -80.49 -57.00 150.00   50
 12  \w   -115.00 -81.00   0.50   10.00    --  -80.49 -57.00 150.00   68
 13  \w    -27.00   0.00   0.50    2.00    --    0.57 -19.00 -60.00   54
 14  \w     33.00  59.00   0.50   10.00    --  104.00 -37.00 -30.00   52
 15  \w     35.00 105.00   0.50   10.00    --  104.00 -99.00 150.00  140
 16  \w     35.00  60.00   0.50   10.00    --  104.00 -37.00-180.00   50
 17  \w     33.00  91.00   0.50   10.00    --  104.00 -97.00 -67.00  116
 18  \w    118.00 175.00   0.50   10.00    --  104.00  37.00 150.00  114
 19  \w     40.00  98.00   0.50   10.00    --  104.00 -19.00 -30.00  116
 20  \w     67.00 102.00   0.50   10.00    --  104.00 -99.00-180.00   70
 21  \w     34.00  63.00   0.50   10.00    --  104.00-125.00 -60.00   58
 22  \w     75.00 120.00   0.50   10.00    --  104.00-125.00 -60.00   90
 23  \w     33.00  71.00   0.50   10.00    --  104.00 -37.00 -90.00   76
 24  \w     33.00  58.00   0.50   10.00    --  104.00 -37.00  60.00   50
 25  \w     68.00 103.00   0.50   10.00    --  104.00 -99.00   0.00   70
 26  \w     35.00  71.00   0.50   10.00    --  104.00 -37.00   0.00   72
 27  \w     44.00  82.00   0.50   10.00    --  104.00 -57.00  60.00   76
 28  \w     39.00  71.00   0.50   10.00    --  104.00 -37.00-150.00   64
 29  \w     39.00  70.00   0.50   10.00    --  104.00 -37.00 150.00   62
 30  \w    103.00 130.00   0.50   10.00    --  104.00  37.00  90.00   54
 31  \w    150.00 175.00   0.50   10.00    --  104.00  37.00  90.00   50
 32  \w     37.00  64.00   0.50   10.00    --  104.00 -37.00 120.00   54
 33  \w     35.00  61.00   0.50   10.00    --  104.00 -99.00  30.00   52
 34  \w     71.00 107.00   0.50   10.00    --  104.00 -99.00  30.00   72
 35  \w     39.00  74.00   0.50   10.00    --  104.00 -57.00-150.00   70
 36  \w     39.00  80.00   0.50   10.00    --  104.00 -57.00 -60.00   82
 37  \w     38.00  96.00   0.50   10.00    --  104.00 -57.00 150.00  116
 38  \w     58.00  87.00   0.50   10.00    --  104.00 -99.00-150.00   58
 39  \w    111.00 136.00   0.50   10.00    --  104.00 125.00-120.00   50
 40  \w    139.00 174.00   0.50   10.00    --  104.00 125.00-120.00   70
 41  \w     80.00 110.00   0.50   10.00    --  104.00 -99.00 -90.00   60
 42  \w     43.00  69.00   0.50   10.00    --  104.00 -57.00   0.00   52
 43  \w     60.00 109.00   0.50   10.00    --  104.00 -99.00  60.00   98
;
_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      -0.0248341000
_diffrn_orient_matrix_UB_12      -0.0595032000
_diffrn_orient_matrix_UB_13      0.1187840000
_diffrn_orient_matrix_UB_21      -0.0800706000
_diffrn_orient_matrix_UB_22      -0.0537874000
_diffrn_orient_matrix_UB_23      -0.0244967000
_diffrn_orient_matrix_UB_31      0.1123670000
_diffrn_orient_matrix_UB_32      -0.1032783000
_diffrn_orient_matrix_UB_33      -0.0415551000
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15217
_diffrn_reflns_theta_full        67.0767
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.028
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.139
_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    2.0342
_exptl_crystal_description       needle
_exptl_crystal_F_000             1051.9848
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.3481
_refine_diff_density_min         -1.2525
_refine_diff_density_rms         0.1885
_refine_ls_d_res_high            0.8370
_refine_ls_d_res_low             12.0164
_refine_ls_goodness_of_fit_ref   1.0129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0129
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+6.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4432
_reflns_number_total             6074
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc05998a2.cif
_cod_data_source_block           NP08_245K_2h
_cod_database_code               7120550
_chemical_oxdiff_formula         'C34 H20 Co1 F6 I2 N3 O8 S2'
_diffrn_oxdiff_ac3_digest_frames
;
0120a8f2ebcbd982b3146109c1690a6bd603514d14f
;
_diffrn_oxdiff_ac3_digest_hkl
;
016231464df24776ee3899c33ce90fd2427a10
;
_reflns_odcompleteness_completeness 96.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C28(H28), C26(H26), C1(H1), C22(H22), C7(H7), C3(H3), C5(H5),
 C6(H6), C15(H15), C12(H12), C14(H14), C17(H17), C30(H30), C23(H23), C21(H21),
 C31(H31), C19(H19), C2(H2), 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 2.092
_oxdiff_exptl_absorpt_empirical_full_min 0.445