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_7706326
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
;
2020-12-05 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4286(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8236(2)
_cell_length_b                   14.3119(2)
_cell_length_c                   16.9607(3)
_cell_measurement_reflns_used    8536
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.0030
_cell_measurement_theta_min      2.9440
_cell_volume                     3587.54(9)
_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      100.01(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 0.987
_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    -68.00  40.00   1.00    1.50    --  -38.13  38.00-150.00  108
  2  \w     40.00  67.00   1.00    1.50    --   38.13 -99.00-180.00   27
  3  \w    -37.00  74.00   1.00    1.50    --   38.13 -77.00   0.00  111
  4  \w    102.00 138.00   1.00    6.00    --  100.00 -30.00 -60.00   36
  5  \w    153.00 178.00   1.00    6.00    --  100.00 111.00 -60.00   25
  6  \w     83.00 178.00   1.00    6.00    --  100.00  77.00  90.00   95
  7  \w     66.00 150.00   1.00    6.00    --  100.00  30.00 -90.00   84
  8  \w     97.00 146.00   1.00    6.00    --  100.00 178.00-150.00   49
  9  \w    103.00 178.00   1.00    6.00    --  100.00 111.00 -30.00   75
 10  \w    107.00 141.00   1.00    6.00    --  100.00 111.00 -60.00   34
 11  \w     99.00 150.00   1.00    6.00    --  100.00 178.00 120.00   51
 12  \w     99.00 132.00   1.00    6.00    --  100.00 178.00  90.00   33
 13  \w     95.00 136.00   1.00    6.00    --  100.00 -77.00 -30.00   41
 14  \w     19.00  84.00   1.00    6.00    --  100.00 -30.00 -60.00   65
;
_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      0.0512977000
_diffrn_orient_matrix_UB_12      -0.0875816000
_diffrn_orient_matrix_UB_13      0.0315186000
_diffrn_orient_matrix_UB_21      -0.0469952000
_diffrn_orient_matrix_UB_22      -0.0584146000
_diffrn_orient_matrix_UB_23      -0.0676183000
_diffrn_orient_matrix_UB_31      0.0776062000
_diffrn_orient_matrix_UB_32      0.0227896000
_diffrn_orient_matrix_UB_33      -0.0522161000
_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  0.0190
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.807
_diffrn_reflns_theta_min         2.990
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.379
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.392
_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    1.639
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0544P)^2^+3.0331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6023
_reflns_number_total             6553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           6_FeL6_100K
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_original_cell_volume        3587.54(10)
_cod_database_code               7706326
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H30 Cl2 Fe N12 O8'
_reflns_odcompleteness_completeness 99.93
_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
 Cl1-O1 \\sim Cl1A-O1A
 with sigma of 0.02
 Cl1-O2 \\sim Cl1A-O2A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1A-O3A
 with sigma of 0.02
 O2-O4 \\sim O2A-O4A
 with sigma of 0.04
 Cl1-O4 \\sim Cl1A-O4A
 with sigma of 0.02
 O1-O4 \\sim O1A-O4A
 with sigma of 0.04
 O1-O3 \\sim O1A-O3A
 with sigma of 0.04
 O2-O3 \\sim O2A-O3A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O3 \\sim O3A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 O1A, O3A, Cl1A, O2A, O4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3A, Cl1A, O1A, O2A, O4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O3A)=Sof(Cl1A)=Sof(O1A)=Sof(O2A)=Sof(O4A)=1-FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
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)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              89658
_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 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.723