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_7706330
_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(Cl O4)'
_chemical_formula_sum            'C36 H30 Cl2 Fe N12 O8'
_chemical_formula_weight         885.47
_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             2020-12-03
_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                90.483(3)
_cell_angle_beta                 94.246(3)
_cell_angle_gamma                89.407(4)
_cell_formula_units_Z            4
_cell_length_a                   14.8446(7)
_cell_length_b                   14.4714(7)
_cell_length_c                   17.0415(6)
_cell_measurement_reflns_used    10228
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      68.4140
_cell_measurement_theta_min      2.5180
_cell_volume                     3650.5(3)
_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      180.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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   -119.00   9.00   1.00    1.50    --  -37.94 -19.00-180.00  128
  2  \w    -38.00  -2.00   1.00    1.50    --  -37.94 125.00 -90.00   36
  3  \w   -116.00  -6.00   1.00    1.50    --  -37.94 -57.00 150.00  110
  4  \w    -87.00 -50.00   1.00    1.50    --  -37.94 125.00 -90.00   37
  5  \w     28.00  66.00   1.00    1.50    --   37.94-125.00  30.00   38
  6  \w      2.00  75.00   1.00    1.50    --   37.94 -99.00  90.00   73
  7  \w     20.00  78.00   1.00    6.00    --  100.00-111.00  30.00   58
  8  \w     72.00 145.00   1.00    6.00    --  100.00  45.00-120.00   73
  9  \w     68.00 110.00   1.00    6.00    --  100.00 -94.00  90.00   42
 10  \w     28.00 131.00   1.00    6.00    --  100.00 -61.00  30.00  103
 11  \w    102.00 129.00   1.00    6.00    --  100.00 111.00   0.00   27
 12  \w    140.00 173.00   1.00    6.00    --  100.00 111.00   0.00   33
 13  \w    100.00 174.00   1.00    6.00    --  100.00 111.00  60.00   74
 14  \w    120.00 177.00   1.00    6.00    --  100.00 111.00  30.00   57
 15  \w     70.00 158.00   1.00    6.00    --  100.00  45.00 120.00   88
 16  \w    125.00 151.00   1.00    6.00    --  100.00 178.00  60.00   26
 17  \w     36.00  98.00   1.00    6.00    --  100.00-111.00-150.00   62
 18  \w     21.00  47.00   1.00    6.00    --  100.00-111.00-120.00   26
 19  \w     60.00 110.00   1.00    6.00    --  100.00-111.00-120.00   50
 20  \w     57.00  84.00   1.00    6.00    --  100.00 178.00-180.00   27
 21  \w     27.00  70.00   1.00    6.00    --  100.00 -30.00 -90.00   43
 22  \w     87.00 131.00   1.00    6.00    --  100.00 -30.00 -90.00   44
 23  \w     50.00  77.00   1.00    6.00    --  100.00-111.00-180.00   27
 24  \w     52.00 112.00   1.00    6.00    --  100.00-111.00   0.00   60
 25  \w     77.00 165.00   1.00    6.00    --  100.00  30.00-180.00   88
 26  \w     54.00 113.00   1.00    6.00    --  100.00-111.00  60.00   59
 27  \w     13.00  40.00   1.00    6.00    --  100.00 -94.00  90.00   27
;
_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      0.0812007158
_diffrn_orient_matrix_UB_12      -0.0647292233
_diffrn_orient_matrix_UB_13      -0.0110714351
_diffrn_orient_matrix_UB_21      0.0582282953
_diffrn_orient_matrix_UB_22      0.0840824075
_diffrn_orient_matrix_UB_23      -0.0167474836
_diffrn_orient_matrix_UB_31      0.0290939115
_diffrn_orient_matrix_UB_32      0.0086618653
_diffrn_orient_matrix_UB_33      0.0884011319
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         69.000
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.286
_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_correction_T_min  0.339
_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            'dark red'
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.194
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         13344
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1512P)^2^+2.6579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10797
_reflns_number_total             13344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           6_FeL6_180K
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_database_code               7706330
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H30 Cl2 Fe N12 O8'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.870(2)
 0.130(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uiso(O3B) = Uiso(O3A)
Uiso(O2B) = Uiso(O2A)
Uiso(O1B) = Uiso(O1A)
Uiso(O4B) = Uiso(O4A)
Uanis(O15A) = Uanis(O15B)
Uanis(O14B) = Uanis(O14A)
Uanis(O16B) = Uanis(O16A)
4. Same fragment restrains
{O1B, O2B, O3B, O4B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1A, O2A, O3A, O4A}
5. Others
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=FVAR(1)
 Sof(O14B)=Sof(O15B)=Sof(O16B)=1-FVAR(2)
 Sof(O14A)=Sof(O15A)=Sof(O16A)=FVAR(2)
6.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), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C10B(H10B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B),
  C16B(H16B), C17B(H17B), C22B(H22B), C23B(H23B), C24B(H24B), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C34B(H34B), C35B(H35B), C36B(H36B)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C8B(H8BA,H8BB,
 H8BC), C20B(H20D,H20E,H20F), C32B(H32D,H32E,H32F)
;
_shelx_res_checksum              57063
_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 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.773