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_7706334
_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(B F4), 2[C2H3N]'
_chemical_formula_sum            'C40 H36 B2 F8 N14 Zn'
_chemical_formula_weight         951.82
_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             2020-10-25
_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                77.910(3)
_cell_angle_beta                 83.652(3)
_cell_angle_gamma                73.048(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8497(5)
_cell_length_b                   13.0576(5)
_cell_length_c                   14.6652(5)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      68.7510
_cell_measurement_theta_min      4.5260
_cell_volume                     2119.41(15)
_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    'SHELXL 2018/3 (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   -110.00 -12.00   1.00    1.00    --  -38.13 -38.00 -60.00   98
  2  \w    -53.00  44.00   1.00    1.00    --  -38.13  19.00 120.00   97
  3  \w     51.00  77.00   1.00    1.00    --   38.13-125.00  30.00   26
  4  \w    -32.00  71.00   1.00    1.00    --   38.13 -57.00-180.00  103
  5  \w     24.00  88.00   1.00    1.00    --   38.13-125.00-180.00   64
  6  \w     19.00 121.00   1.00    4.00    --  100.00 -30.00  60.00  102
  7  \w     19.00 105.00   1.00    4.00    --  100.00-111.00 -90.00   86
  8  \w     19.00  87.00   1.00    4.00    --  100.00 -77.00  90.00   68
  9  \w     64.00 132.00   1.00    4.00    --  100.00  30.00  90.00   68
 10  \w     88.00 113.00   1.00    4.00    --  100.00-111.00-180.00   25
 11  \w    144.00 174.00   1.00    4.00    --  100.00  30.00  90.00   30
 12  \w     73.00 132.00   1.00    4.00    --  100.00 178.00 -60.00   59
 13  \w     22.00  85.00   1.00    4.00    --  100.00 -61.00 -60.00   63
 14  \w     19.00  46.00   1.00    4.00    --  100.00 -94.00   0.00   27
 15  \w     42.00  74.00   1.00    4.00    --  100.00 -61.00  30.00   32
 16  \w     20.00 109.00   1.00    4.00    --  100.00 -94.00  30.00   89
 17  \w     69.00 129.00   1.00    4.00    --  100.00  45.00 -90.00   60
 18  \w    108.00 133.00   1.00    4.00    --  100.00 -61.00  30.00   25
 19  \w     99.00 151.00   1.00    4.00    --  100.00 178.00 -90.00   52
 20  \w     14.00  91.00   1.00    4.00    --  100.00 -94.00 -60.00   77
 21  \w     76.00 113.00   1.00    4.00    --  100.00-111.00   0.00   37
 22  \w     40.00 159.00   1.00    4.00    --  100.00   0.00-120.00  119
;
_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      -0.0787111000
_diffrn_orient_matrix_UB_12      0.0346797000
_diffrn_orient_matrix_UB_13      -0.0841841000
_diffrn_orient_matrix_UB_21      -0.0688238000
_diffrn_orient_matrix_UB_22      -0.0825277000
_diffrn_orient_matrix_UB_23      0.0465262000
_diffrn_orient_matrix_UB_31      -0.0871350000
_diffrn_orient_matrix_UB_32      0.0880178000
_diffrn_orient_matrix_UB_33      0.0481911000
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16019
_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         68.837
_diffrn_reflns_theta_min         3.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
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    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0857P)^2^+1.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6327
_reflns_number_total             7730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           2_ZnL6BF4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_original_cell_volume        2119.42(15)
_cod_database_code               7706334
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H30 B2 F8 N12 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.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)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16902
_shelx_fab_checksum              67581
_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 1.429
_oxdiff_exptl_absorpt_empirical_full_min 0.556