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_7706333
_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 Zn, 2(Cl O4), 2.502(C2 H3 N)'
_chemical_formula_sum            'C41.01 H37.51 Cl2 N14.5 O8 Zn'
_chemical_formula_weight         997.69
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                62.805(4)
_cell_angle_beta                 69.432(4)
_cell_angle_gamma                70.165(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7622(7)
_cell_length_b                   14.6333(6)
_cell_length_c                   14.8701(5)
_cell_measurement_reflns_used    8280
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      68.6740
_cell_measurement_theta_min      3.8350
_cell_volume                     2258.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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    'ShelXS (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 0.983
_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   -116.00 -78.00   1.00    1.00    --  -38.13 -38.00  60.00   38
  2  \w   -104.00 -28.00   1.00    1.00    --  -38.13 -38.00 150.00   76
  3  \w    -58.00  -7.00   1.00    1.00    --  -38.13 -38.00  60.00   51
  4  \w    -88.00  -6.00   1.00    1.00    --  -38.13 125.00   0.00   82
  5  \w    -73.00  38.00   1.00    1.00    --  -38.13  77.00 -90.00  111
  6  \w      1.00  27.00   1.00    1.00    --   38.13 -99.00   0.00   26
  7  \w     88.00 149.00   1.00    4.00    --  100.00 178.00  90.00   61
  8  \w    115.00 145.00   1.00    4.00    --  100.00 178.00  30.00   30
  9  \w    101.00 173.00   1.00    4.00    --  100.00 111.00  30.00   72
 10  \w     76.00 117.00   1.00    4.00    --  100.00 178.00-150.00   41
 11  \w    100.00 131.00   1.00    4.00    --  100.00 111.00 -90.00   31
 12  \w     20.00 112.00   1.00    4.00    --  100.00-111.00-150.00   92
 13  \w    128.00 160.00   1.00    4.00    --  100.00 111.00 -30.00   32
 14  \w     58.00  84.00   1.00    4.00    --  100.00 178.00 150.00   26
 15  \w     25.00  84.00   1.00    4.00    --  100.00 -61.00 -90.00   59
 16  \w    100.00 172.00   1.00    4.00    --  100.00 111.00   0.00   72
 17  \w     66.00 146.00   1.00    4.00    --  100.00 178.00-120.00   80
 18  \w    103.00 133.00   1.00    4.00    --  100.00 -61.00 -90.00   30
 19  \w     92.00 148.00   1.00    4.00    --  100.00 178.00-180.00   56
 20  \w     73.00  98.00   1.00    4.00    --  100.00 178.00   0.00   25
 21  \w     20.00  51.00   1.00    4.00    --  100.00-111.00  60.00   31
 22  \w     71.00 109.00   1.00    4.00    --  100.00-111.00  60.00   38
 23  \w     69.00 159.00   1.00    4.00    --  100.00  45.00  90.00   90
 24  \w     65.00 176.00   1.00    4.00    --  100.00  30.00   0.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0778164000
_diffrn_orient_matrix_UB_12      0.1105938000
_diffrn_orient_matrix_UB_13      -0.0334363000
_diffrn_orient_matrix_UB_21      0.1042685000
_diffrn_orient_matrix_UB_22      0.0495486000
_diffrn_orient_matrix_UB_23      -0.0372104000
_diffrn_orient_matrix_UB_31      0.0223376000
_diffrn_orient_matrix_UB_32      0.0002573000
_diffrn_orient_matrix_UB_33      -0.1088771000
_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  0.0154
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17214
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.893
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.428
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         8245
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0946P)^2^+2.9823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7283
_reflns_number_total             8245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           1_ZnL6ClO4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_original_formula_sum        'C41.01 H37.51 Cl2 N14.50 O8 Zn'
_cod_database_code               7706333
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41.5 H38.25 Cl2 N14.5 O8 Zn'
_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. Restrained distances
 C42A-C41A
 1.54 with sigma of 0.02
 N43A-C41A
 1.16 with sigma of 0.02
 N43B-C42B
 1.16 with sigma of 0.02
 C42B-C41B
 1.54 with sigma of 0.02
 C42C-C41C
 1.54 with sigma of 0.02
 N44-C42C
 1.16 with sigma of 0.02
 C42A-N43A
 2.7 with sigma of 0.04
 C41B-N43B
 2.7 with sigma of 0.04
 C41C-N44
 2.7 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) = Uanis(C31B)
Uanis(C30B) = Uanis(C29B) = Uanis(C28B) = Uanis(C27B) = Uanis(C26B) =
Uanis(C25B) = Uanis(C30A) = Uanis(C29A) = Uanis(C28A) = Uanis(C27A) =
Uanis(C26A) = Uanis(C25A)
Uanis(N12A) = Uanis(N11A) = Uanis(N12B) = Uanis(N11B)
Uanis(N10A) = Uanis(N9A) = Uanis(N10B) = Uanis(N9B)
Uanis(C32B) = Uanis(C32A)
Uanis(N12A) = Uanis(C34A) = Uanis(C35A) = Uanis(C36A) = Uanis(N11A) =
Uanis(C33A) = Uanis(N12B) = Uanis(C36B) = Uanis(C35B) = Uanis(C34B) =
Uanis(N11B) = Uanis(C33B)
Uiso(C42A) = Uiso(C41A) = Uiso(C41B) = Uiso(C42B) = Uiso(C41C) = Uiso(C42C)
Uiso(N43A) = Uiso(N43B) = Uiso(N44)
Uanis(Zn1A) = Uanis(Zn1B)
4. Others
 1*[Sof(N43A)+Sof(C41A)+Sof(C42A)+Sof(H42A)+Sof(H42B)+Sof(H42C)]+1*[Sof(N43B)+
 Sof(C41B)+Sof(H41A)+Sof(H41B)+Sof(H41C)+Sof(C42B)]+1*[Sof(N44)+Sof(C41C)+
 Sof(H41D)+Sof(H41E)+Sof(H41F)+Sof(C42C)]=0.5 with esd of 0.001
 Sof(Zn1B)=Sof(N9B)=Sof(N10B)=Sof(N11B)=Sof(N12B)=Sof(C25B)=Sof(C26B)=
 Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=
 Sof(C30B)=Sof(C31B)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1)
 Sof(Zn1A)=Sof(N9A)=Sof(N10A)=Sof(N11A)=Sof(N12A)=Sof(C25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1)
 Sof(N43A)=Sof(C41A)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(2)
 Sof(N43B)=Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42B)=FVAR(3)
 Sof(N44)=Sof(C41C)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42C)=FVAR(4)
5.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), C26A(H26A),
 C27A(H27A), C28A(H28A), C29A(H29A), C34A(H34A), C35A(H35A), C36A(H36A),
 C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B), C34B(H34B), C35B(H35B),
 C36B(H36B)
5.b Idealised Me refined with everything fixed:
 C42A(H42A,H42B,H42C), C41B(H41A,H41B,H41C), C41C(H41D,H41E,H41F)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32A(H32A,H32B,H32C), C32B(H32D,H32E,
 H32F), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              33775
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.892