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_7706329
_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 Ni, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C38 H33 B2 F8 N13 Ni'
_chemical_formula_weight         904.10
_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             2020-12-03
_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
_cell_angle_beta                 94.9100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.42950(10)
_cell_length_b                   22.5937(3)
_cell_length_c                   18.8708(2)
_cell_measurement_reflns_used    10349
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      68.8710
_cell_measurement_theta_min      2.3350
_cell_volume                     4005.62(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.988
_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 -11.00   1.00    1.00    --  -38.13 -57.00 -30.00  105
  2  \w    -43.00  -8.00   1.00    1.00    --  -38.13 -38.00-150.00   35
  3  \w     35.00  95.00   1.00    1.00    --   38.13-125.00-120.00   60
  4  \w     38.00  66.00   1.00    1.00    --   38.13-125.00 150.00   28
  5  \w     77.00 103.00   1.00    4.00    --  100.00 178.00  90.00   26
  6  \w    108.00 175.00   1.00    4.00    --  100.00 111.00  60.00   67
  7  \w     29.00  62.00   1.00    4.00    --  100.00 -30.00-150.00   33
  8  \w     27.00  83.00   1.00    4.00    --  100.00 -94.00-150.00   56
  9  \w     85.00 151.00   1.00    4.00    --  100.00 178.00-120.00   66
 10  \w    107.00 178.00   1.00    4.00    --  100.00 111.00-180.00   71
 11  \w    111.00 170.00   1.00    4.00    --  100.00 111.00 150.00   59
 12  \w     73.00 131.00   1.00    4.00    --  100.00 -30.00-150.00   58
 13  \w     68.00 112.00   1.00    4.00    --  100.00-111.00 -90.00   44
 14  \w    101.00 139.00   1.00    4.00    --  100.00 111.00 -60.00   38
 15  \w     74.00 128.00   1.00    4.00    --  100.00 -45.00   0.00   54
;
_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      -0.1623316000
_diffrn_orient_matrix_UB_12      -0.0085088000
_diffrn_orient_matrix_UB_13      -0.0015524000
_diffrn_orient_matrix_UB_21      0.0229445000
_diffrn_orient_matrix_UB_22      -0.0598687000
_diffrn_orient_matrix_UB_23      0.0385071000
_diffrn_orient_matrix_UB_31      0.0002051000
_diffrn_orient_matrix_UB_32      0.0316817000
_diffrn_orient_matrix_UB_33      0.0722184000
_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  0.0170
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.802
_diffrn_reflns_theta_min         3.058
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.746
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0535P)^2^+2.5689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6669
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           5_NiL6BF4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_database_code               7706329
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H34 B2 F8 N12 Ni'
_reflns_odcompleteness_completeness 99.92
_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. Uiso/Uaniso restraints and constraints
F5A \\sim F5B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
F6A \\sim F6B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
F2B \\sim F2A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F1A \\sim F1B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F4A \\sim F4B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F3A \\sim F3B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
3. Rigid body (RIGU) restrains
 F5A, B2, F8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7B, B2, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5B, B2, F8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7A, B2, F8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6A, B2, F7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
 Sof(F2A)=Sof(F1B)=Sof(F3B)=Sof(F4B)=1-FVAR(2)
 Sof(F1A)=Sof(F3A)=Sof(F4A)=Sof(F2B)=FVAR(2)
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), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C35(H35), C36(H36)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              40387
_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 1.108
_oxdiff_exptl_absorpt_empirical_full_min 0.868