Switchable on-off spin-crossover properties of iron(ii) compounds by trimming intermolecular hydrogen bonds.
Li, Na; Xue, Jin-Peng; Liu, Jing-Lin; Wang, Yao-Yao; Yao, Zi-Shuo; Tao, Jun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 998–1001; doi:10.1039/c9dt04685b

data_7703066
_publ_section_title
;
 Switchable on-off spin-crossover properties of iron(ii) compounds by
 trimming intermolecular hydrogen bonds.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              998
_journal_page_last               1001
_journal_paper_doi               10.1039/c9dt04685b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 3(C H4 O)'
_chemical_formula_sum            'C59 H44 Fe N10 O3 S2'
_chemical_formula_weight         1061.01
_chemical_name_systematic        C59H38FeN10O3S2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9880(3)
_cell_length_b                   24.7721(7)
_cell_length_c                   16.8246(5)
_cell_measurement_reflns_used    15987
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8950
_cell_measurement_theta_min      3.8990
_cell_volume                     4996.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     35.00  60.00   0.50   90.00    --    0.00  47.00  65.00   50
  2  \w    -50.00  -2.00   0.50   90.00    --    0.00 -82.00   0.00   96
  3  \w      3.00  28.00   0.50   90.00    --    0.00 -82.00   0.00   50
  4  \w    -60.00 -34.00   0.50   90.00    --    0.00 -82.00-150.00   52
  5  \w    -56.00 -28.00   0.50   90.00    --    0.00 -82.00 -30.00   56
  6  \w    -18.00  23.00   0.50   90.00    --    0.00 -77.00 -90.00   82
  7  \w    -50.00 -20.00   0.50   90.00    --    0.00 -82.00-120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0378370000
_diffrn_orient_matrix_UB_12      0.0145526000
_diffrn_orient_matrix_UB_13      0.0242888000
_diffrn_orient_matrix_UB_21      0.0339293000
_diffrn_orient_matrix_UB_22      0.0233662000
_diffrn_orient_matrix_UB_23      -0.0035026000
_diffrn_orient_matrix_UB_31      -0.0302331000
_diffrn_orient_matrix_UB_32      0.0079364000
_diffrn_orient_matrix_UB_33      -0.0342900000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.701
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull pinkish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             2200
_exptl_crystal_preparation
'FeCl2.6H2O (0.8 g, 0.003mol) and enough ascorbic acid was dissolved by MeOH(100 ml).Then the mixed solution was filtered. Pyridine (40 ml) was added when the filtrate was stirred. Yellow precipitate was collected.'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0395P)^2^+3.2344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4289
_reflns_number_total             4644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04685b2.cif
_cod_data_source_block           MeOH@150K
_cod_depositor_comments
'Adding full bibliography for 7703063--7703069.cif.'
_cod_database_code               7703066
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.690
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O2(0.5) H2A(0.5)
3.a Riding coordinates:
 O1(H1), C29(H29A,H29B,H29C), O2(H2A)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              79317
_olex2_exptl_crystal_mounting_method 'coordinate bond'
_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.621