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_7706325
_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(Cl O4), C2 H3 N'
_chemical_formula_sum            'C38 H33 Cl2 N13 Ni O8'
_chemical_formula_weight         929.38
_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             2020-12-04
_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                 96.5810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.51580(10)
_cell_length_b                   22.5839(2)
_cell_length_c                   19.1174(2)
_cell_measurement_reflns_used    20416
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      68.9230
_cell_measurement_theta_min      2.2720
_cell_volume                     4081.33(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -86.00  -2.00   1.00    1.00    --  -38.13 125.00   0.00   84
  2  \w    -10.00  41.00   1.00    1.00    --  -38.13  38.00 120.00   51
  3  \w   -123.00 -80.00   1.00    1.00    --  -38.13 -84.00  48.00   43
  4  \w     11.00 105.00   1.00    1.00    --   38.13  57.00-120.00   94
  5  \w     32.00  58.00   1.00    1.00    --   38.13-125.00-180.00   26
  6  \w      1.00  49.00   1.00    1.00    --   38.13 -99.00 -30.00   48
  7  \w      3.00  71.00   1.00    1.00    --   38.13 -99.00-120.00   68
  8  \w     79.00 108.00   1.00    4.00    --  100.00-111.00 -60.00   29
  9  \w     81.00 151.00   1.00    4.00    --  100.00 178.00 120.00   70
 10  \w     24.00 112.00   1.00    4.00    --  100.00 -61.00 150.00   88
 11  \w     42.00 117.00   1.00    4.00    --  100.00 -77.00  90.00   75
 12  \w     85.00 112.00   1.00    4.00    --  100.00-111.00  90.00   27
 13  \w     21.00 121.00   1.00    4.00    --  100.00 -30.00 150.00  100
 14  \w     67.00 118.00   1.00    4.00    --  100.00  77.00 -90.00   51
 15  \w    101.00 178.00   1.00    4.00    --  100.00 111.00-180.00   77
 16  \w     88.00 113.00   1.00    4.00    --  100.00-111.00-180.00   25
 17  \w     91.00 178.00   1.00    4.00    --  100.00  77.00-120.00   87
 18  \w     58.00  83.00   1.00    4.00    --  100.00 178.00   0.00   25
 19  \w     99.00 142.00   1.00    4.00    --  100.00 178.00   0.00   43
 20  \w     88.00 113.00   1.00    4.00    --  100.00-111.00  30.00   25
 21  \w    100.00 144.00   1.00    4.00    --  100.00 111.00  60.00   44
 22  \w     37.00  64.00   1.00    4.00    --  100.00-111.00-180.00   27
 23  \w     97.00 149.00   1.00    4.00    --  100.00  45.00-120.00   52
 24  \w    144.00 169.00   1.00    4.00    --  100.00  77.00 -90.00   25
 25  \w     24.00  58.00   1.00    4.00    --  100.00 -94.00  90.00   34
 26  \w     12.00 175.00   1.00    4.00    --  100.00   0.00  60.00  163
;
_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      0.1544003000
_diffrn_orient_matrix_UB_12      -0.0191123000
_diffrn_orient_matrix_UB_13      0.0212247000
_diffrn_orient_matrix_UB_21      0.0263445000
_diffrn_orient_matrix_UB_22      0.0570868000
_diffrn_orient_matrix_UB_23      0.0437239000
_diffrn_orient_matrix_UB_31      -0.0449415000
_diffrn_orient_matrix_UB_32      -0.0320821000
_diffrn_orient_matrix_UB_33      0.0649507000
_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  0.0197
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.897
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.638
_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    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0715P)^2^+3.9109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7166
_reflns_number_total             7537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           4_NiL6ClO4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_database_code               7706325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H33 Cl2 N13 Ni O8'
_reflns_odcompleteness_completeness 99.99
_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
 Cl2A-O5A \\sim Cl2B-O5B
 with sigma of 0.02
 Cl2B-O7B \\sim Cl2A-O7A
 with sigma of 0.02
 Cl2A-O8A \\sim Cl2B-O8B
 with sigma of 0.02
 Cl2B-O6B \\sim Cl2A-O6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Rigid body (RIGU) restrains
 Cl2A, O6A, O5A, O8A, O7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2B, O8B, O7B, O5B, O6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl2B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(O8B)=1-FVAR(1)
 Sof(Cl2A)=Sof(O8A)=Sof(O7A)=Sof(O5A)=Sof(O6A)=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), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              9663
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.876