Tuning spin-crossover transition temperatures in non-symmetrical homoleptic meridional/facial [Fe(didentate)<sub>3</sub>]<sup>2+</sup> complexes: what for and who cares about it?
Deorukhkar, Neel; Besnard, Céline; Guénée, Laure; Piguet, Claude; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1206–1223; doi:10.1039/d0dt03828h

data_7706338
_publ_section_title
;
 Tuning spin-crossover transition temperatures in non-symmetrical
 homoleptic meridional/facial [Fe(didentate)<sub>3</sub>]<sup>2+</sup>
 complexes: what for and who cares about it?
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1206
_journal_page_last               1223
_journal_paper_doi               10.1039/d0dt03828h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C36 H30 N12 Ni, 2(B F4), C H4 O, 0.5(C2 H3 N)'
_chemical_formula_sum            'C38 H35.5 B2 F8 N12.5 Ni O'
_chemical_formula_weight         915.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                94.6407(12)
_cell_angle_beta                 100.7070(12)
_cell_angle_gamma                113.7978(17)
_cell_formula_units_Z            2
_cell_length_a                   11.6311(2)
_cell_length_b                   12.8430(2)
_cell_length_c                   14.99232(18)
_cell_measurement_reflns_used    24192
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.1760
_cell_measurement_theta_min      3.0250
_cell_volume                     1982.94(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.972
_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    -49.00 -13.00   0.50    0.50    --  -52.43 125.00 -30.00   72
  2  \w    -44.00 -18.00   0.50    0.50    --  -52.43 125.00-120.00   52
  3  \w     34.00  59.00   0.50    0.50    --   28.00  78.00   0.34   50
  4  \w     44.00  69.00   0.50    0.50    --   36.00  74.00 175.48   50
  5  \w    -93.00 -24.00   0.50    0.50    --  -52.43 -15.00  60.00  138
  6  \w    -65.00 -40.00   0.50    0.50    --  -28.00 -66.00 -34.87   50
  7  \w     37.00  62.00   0.50    0.50    --   75.25 -60.00 -75.17   50
  8  \w     44.00  99.00   0.50    0.50    --   69.88  15.00 -90.00  110
  9  \w     92.00 118.00   0.50    0.50    --   75.25  37.00 -49.50   52
 10  \w     83.00 109.00   0.50    0.50    --   75.25   6.00 -85.55   52
 11  \w     48.00  73.00   0.50    0.50    --   75.25  11.00-166.65   50
 12  \w     51.00  81.00   0.50    0.50    --   75.25   6.00 -85.55   60
 13  \w     64.00 117.00   0.50    0.50    --   75.25  21.00 -58.77  106
 14  \w     78.00 110.00   0.50    0.50    --   75.25   2.00  38.12   64
 15  \w     43.00  72.00   0.50    0.50    --   75.25   2.00  38.12   58
 16  \w     52.00  83.00   0.50    0.50    --   69.88   0.00  60.00   62
 17  \w     90.00 115.00   0.50    0.50    --   75.25  47.00  47.61   50
 18  \w     90.00 115.00   0.50    0.50    --   75.25  47.00 122.13   50
 19  \w     45.00  91.00   0.50    0.50    --   75.25   3.00 133.90   92
 20  \w     37.00 100.00   0.50    0.50    --   69.88   0.00 150.00  126
 21  \w     67.00 116.00   0.50    0.50    --   75.25  22.00 164.73   98
 22  \w     82.00 112.00   0.50    0.50    --   75.25  21.00  81.34   60
 23  \w     53.00  89.00   0.50    0.50    --   75.25  13.00  90.76   72
 24  \w     51.00  99.00   0.50    0.50    --   75.25   8.00  14.55   96
 25  \w     89.00 114.00   0.50    0.50    --   75.25  23.00-154.95   50
 26  \w     41.00  94.00   0.50    0.50    --   68.73-125.00 150.00  106
 27  \w     41.00  92.00   0.50    0.50    --   68.73-125.00  90.00  102
 28  \w     37.00  95.00   0.50    0.50    --   69.88-125.00  30.00  116
 29  \w     67.00  94.00   0.50    0.50    --   75.25-131.00  88.28   54
 30  \w     38.00  63.00   0.50    0.50    --   75.25-104.00  84.80   50
 31  \w     57.00 116.00   0.50    0.50    --   75.25-162.00 153.09  118
 32  \w     53.00  88.00   0.50    0.50    --   69.88-125.00 -30.00   70
 33  \w     68.00  97.00   0.50    0.50    --   75.25-118.00 -15.73   58
 34  \w     36.00  68.00   0.50    0.50    --   68.73-125.00 -60.00   64
 35  \w     36.00  95.00   0.50    0.50    --   69.88-125.00 -90.00  118
 36  \w     70.00  98.00   0.50    0.50    --   75.25-161.00-168.36   56
 37  \w     51.00 109.00   0.50    0.50    --   75.25-140.00-156.63  116
 38  \w     35.00  96.00   0.50    0.50    --   75.25-117.00-161.61  122
 39  \w     41.00  67.00   0.50    0.50    --   75.25 -92.00-160.72   52
 40  \w     41.00  67.00   0.50    0.50    --   75.25-115.00-122.99   52
 41  \w     45.00  96.00   0.50    0.50    --   75.25-116.00-110.54  102
 42  \w     41.00  92.00   0.50    0.50    --   75.25-111.00 -64.22  102
 43  \w     47.00  96.00   0.50    0.50    --   75.25-116.00-142.08   98
 44  \w     52.00  87.00   0.50    0.50    --   75.25-119.00  38.17   70
 45  \w     48.00 103.00   0.50    0.50    --   75.25-129.00  29.01  110
 46  \w     69.00  94.00   0.50    0.50    --   75.25-114.00 115.26   50
 47  \w     73.00 101.00   0.50    0.50    --   75.25-127.00 149.63   56
 48  \w     62.00 103.00   0.50    0.50    --   75.25-150.00  31.88   82
 49  \w     67.00 101.00   0.50    0.50    --   75.25-127.00  57.76   68
 50  \w     39.00  64.00   0.50    0.50    --   75.25-118.00 -15.73   50
 51  \w     62.00  96.00   0.50    0.50    --   75.25-116.00  86.16   68
 52  \w     60.00 104.00   0.50    0.50    --   75.25-131.00 -76.26   88
 53  \w     48.00  73.00   0.50    0.50    --   75.25-106.00-132.40   50
 54  \w     51.00  76.00   0.50    0.50    --   75.25-110.00-178.39   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1208950000
_diffrn_orient_matrix_UB_12      -0.0037097000
_diffrn_orient_matrix_UB_13      0.0303324000
_diffrn_orient_matrix_UB_21      -0.0731347000
_diffrn_orient_matrix_UB_22      -0.1295698000
_diffrn_orient_matrix_UB_23      -0.0415071000
_diffrn_orient_matrix_UB_31      0.0476104000
_diffrn_orient_matrix_UB_32      -0.0302961000
_diffrn_orient_matrix_UB_33      0.0929111000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34638
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.466
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       plate
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0803P)^2^+1.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6951
_reflns_number_total             7887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           11_NiL7BF4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_original_cell_volume        1982.93(6)
_cod_original_formula_sum        'C38 H35.50 B2 F8 N12.50 Ni O'
_cod_database_code               7706338
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37.5 H34 B2 F8 N12 Ni O1.5'
_reflns_odcompleteness_completeness 97.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
Uiso(N37) = Uiso(C37)
3. Others
 Fixed Sof: C2S(0.5) N37(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C35(H35), C36(H36)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C1S(H1SA,H1SB,
 H1SC), C37(H37A,H37B,H37C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              58101
_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 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.778