Activating a high-spin iron(II) complex to thermal spin-crossover with an inert non-isomorphous molecular dopant.
Halcrow, Malcolm A.; Vasili, Hari Babu; Pask, Christopher M.; Kulak, Alexander N.; Cespedes, Oscar; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6983–6992; doi:10.1039/d4dt00443d

data_7715538
_publ_section_title
;
 Activating a high-spin iron(II) complex to thermal spin-crossover with an
 inert non-isomorphous molecular dopant.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6983
_journal_page_last               6992
_journal_paper_doi               10.1039/d4dt00443d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H18 Fe N10, 2(F6 P)'
_chemical_formula_sum            'C22 H18 F12 Fe N10 P2'
_chemical_formula_weight         768.25
_chemical_name_systematic
;
Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) di(hexafluorophosphate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.792(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6500(5)
_cell_length_b                   9.4890(4)
_cell_length_c                   20.6037(5)
_cell_measurement_reflns_used    10906
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.81
_cell_volume                     2830.54(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Area detector scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10906
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0052(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0491P)^2^+1.7095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2670
_reflns_number_total             3234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00443d2.cif
_cod_data_source_block           mah35
_cod_depositor_comments
'Adding full bibliography for 7715536--7715541.cif.'
_cod_database_code               7715538
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P18-F19A
 1.58095 with sigma of 0.02
 P18-F20A
 1.58095 with sigma of 0.02
 P18-F21A
 1.58095 with sigma of 0.02
 P18-F22A
 1.58095 with sigma of 0.02
 P18-F23A
 1.58095 with sigma of 0.02
 P18-F24A
 1.58095 with sigma of 0.02
 P18-F19B
 1.58095 with sigma of 0.02
 P18-F20B
 1.58095 with sigma of 0.02
 P18-F21B
 1.58095 with sigma of 0.02
 P18-F22B
 1.58095 with sigma of 0.02
 P18-F23B
 1.58095 with sigma of 0.02
 P18-F24B
 1.58095 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 Fixed Sof: F19A(0.5) F20A(0.5) F21A(0.5) F22A(0.5) F23A(0.5) F24A(0.5)
 F19B(0.5) F20B(0.5) F21B(0.5) F22B(0.5) F23B(0.5) F24B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17)
;
_shelx_res_checksum              5411
_olex2_submission_special_instructions 'No special instructions were received'