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_7706328
_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 Fe N12, 2(B F4), 0.5(C5 H12 O), 0.2(C2 H3 N), 0.3(C2 N)'
_chemical_formula_sum            'C39.5 H36.6 B2 F8 Fe N12.5 O0.5'
_chemical_formula_weight         923.88
_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             2020-12-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-05 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.760(4)
_cell_angle_beta                 83.510(4)
_cell_angle_gamma                74.276(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8247(6)
_cell_length_b                   12.9758(6)
_cell_length_c                   14.7202(6)
_cell_measurement_reflns_used    5439
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      68.7860
_cell_measurement_theta_min      3.0490
_cell_volume                     2120.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_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    -64.00  -5.00   1.00    5.00    --  -38.19 125.00 120.00   59
  2  \w   -114.00  -8.00   1.00    5.00    --  -38.19 -38.00-120.00  106
  3  \w   -110.00 -10.00   1.00    5.00    --  -38.19 -57.00   0.00  100
  4  \w      1.00  36.00   1.00    5.00    --   38.19 -99.00 120.00   35
  5  \w     51.00  97.00   1.00    5.00    --   38.19-125.00-120.00   46
  6  \w     72.00 176.00   1.00   20.00    --  100.00  45.00 150.00  104
  7  \w     67.00 172.00   1.00   20.00    --  100.00  30.00 -90.00  105
  8  \w     99.00 129.00   1.00   20.00    --  100.00 -45.00  60.00   30
  9  \w    148.00 177.00   1.00   20.00    --  100.00 111.00  90.00   29
 10  \w    106.00 142.00   1.00   20.00    --  100.00 111.00  90.00   36
 11  \w    102.00 160.00   1.00   20.00    --  100.00 111.00 -30.00   58
 12  \w     60.00 141.00   1.00   20.00    --  100.00 178.00 150.00   81
 13  \w    112.00 138.00   1.00   20.00    --  100.00 178.00 120.00   26
 14  \w     19.00 113.00   1.00   20.00    --  100.00-111.00 120.00   94
 15  \w     58.00  84.00   1.00   20.00    --  100.00 178.00 120.00   26
 16  \w     21.00 112.00   1.00   20.00    --  100.00-111.00 -30.00   91
 17  \w     83.00 137.00   1.00   20.00    --  100.00 178.00 -90.00   54
 18  \w     76.00 131.00   1.00   20.00    --  100.00 -45.00 -90.00   55
 19  \w     99.00 151.00   1.00   20.00    --  100.00 178.00 -30.00   52
 20  \w     60.00 133.00   1.00   20.00    --  100.00 -61.00  30.00   73
 21  \w     17.00  44.00   1.00   20.00    --  100.00 -94.00   0.00   27
 22  \w     83.00 139.00   1.00   20.00    --  100.00 178.00   0.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0212084000
_diffrn_orient_matrix_UB_12      0.0608976000
_diffrn_orient_matrix_UB_13      -0.0996912000
_diffrn_orient_matrix_UB_21      -0.0957208000
_diffrn_orient_matrix_UB_22      -0.0409809000
_diffrn_orient_matrix_UB_23      -0.0336239000
_diffrn_orient_matrix_UB_31      -0.0936546000
_diffrn_orient_matrix_UB_32      0.1019442000
_diffrn_orient_matrix_UB_33      0.0209668000
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16085
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         69.825
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.579
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         7746
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1144P)^2^+0.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6203
_reflns_number_total             7746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           7_FeL6BF4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_original_cell_volume        2120.94(17)
_cod_original_formula_sum        'C39.50 H36.60 B2 F8 Fe N12.50 O0.50'
_cod_database_code               7706328
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38.5 H36 B2 F8 Fe N12 O0.5'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Shared sites
{C5S, C38}
3. Restrained distances
 C1A-C1B
 1.456 with sigma of 0.01
 C1A-N1
 1.137 with sigma of 0.01
 N1-C1A
 1.14 with sigma of 0.02
 C1C-N13
 1.137 with sigma of 0.01
 C1B-N1
 2.593 with sigma of 0.02
 C1C-C1D
 1.456 with sigma of 0.01
 C1D-N13
 2.593 with sigma of 0.02
 N13-C1C
 1.14 with sigma of 0.02
 N13-C1D
 2.59 with sigma of 0.04
 N1-C1B
 2.59 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N13 \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(F7B) = Uanis(F7A)
Uanis(F8B) = Uanis(F8A)
Uanis(F6B) = Uanis(F6A)
Uiso(C5S) = Uiso(C38)
Uiso(N37) = Uiso(C39) = Uiso(C38)
Uiso(N1) = Uiso(C1A) = Uiso(C1B) = Uiso(C1D) = Uiso(C1C) = Uiso(N13)
5. Rigid body (RIGU) restrains
 N13, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
 Fixed Sof: O2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C3S(0.5) C4S(0.5)
 H4SA(0.5) H4SB(0.5) H4SC(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5) C6S(0.5)
 H6SA(0.5) H6SB(0.5) H6SC(0.5) N37(0.2) C38(0.2) C39(0.2) H39A(0.2) H39B(0.2)
 H39C(0.2) N1(0.15) C1A(0.15) C1B(0.15) N13(0.15) C1C(0.15) C1D(0.15)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C14(H14),
 C1(H1), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C34(H34), C35(H35), C36(H36)
7.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C1S(H1SA,H1SB,
 H1SC), C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C39(H39A,
 H39B,H39C)
;
_shelx_res_checksum              3448
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.761