The number and shape of lattice solvent molecules controls spin-crossover in an isomorphous series of crystalline solvate salts.
Berdiell, Izar Capel; Kulmaczewski, Rafal; Shahid, Namrah; Cespedes, Oscar; Halcrow, Malcolm A.; Chemical communications (Cambridge, England) 57 (2021) 6566–6569; doi:10.1039/d1cc02624k

data_7128429
_publ_section_title
;
 The number and shape of lattice solvent molecules controls spin-crossover
 in an isomorphous series of crystalline solvate salts.
;
_journal_issue                   53
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6566
_journal_page_last               6569
_journal_paper_doi               10.1039/d1cc02624k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), 0.5(C2 H6 O)'
_chemical_formula_sum            'C27 H27 Cl2 Fe N12 O10.5'
_chemical_formula_weight         814.35
_chemical_name_systematic
; 
Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)
diperchlorate hemi-ethanol solvate
;
_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
_audit_creation_date             2020-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                79.143(9)
_cell_angle_beta                 78.844(9)
_cell_angle_gamma                75.480(8)
_cell_formula_units_Z            2
_cell_length_a                   8.2123(7)
_cell_length_b                   10.9318(10)
_cell_length_c                   20.008(2)
_cell_measurement_reflns_used    6098
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.41
_cell_measurement_theta_min      4.47
_cell_volume                     1687.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13392
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.845
_diffrn_reflns_theta_min         4.224
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6407
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.9623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5519
_reflns_number_total             6407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02624k13.cif
_cod_data_source_block           80-etoh
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_original_formula_sum        'C27 H27 Cl2 Fe N12 O10.50'
_cod_database_code               7128429
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4A-O48A = Cl4A-O49A = Cl4A-O50A = Cl4A-O51A
 1.43461 with sigma of 0.02
 Cl4B-O48B = Cl4B-O49B = Cl4B-O50B = Cl4B-O51B
 1.43461 with sigma of 0.02
 O48A-O49A = O48A-O50A = O48A-O51A = O49A-O50A = O49A-O51A = O50A-O51A
 2.342718 with sigma of 0.02
 O48B-O49B = O48B-O50B = O48B-O51B = O49B-O50B = O49B-O51B = O50B-O51B
 2.342718 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl4A(0.5) O48A(0.5) O49A(0.5) O50A(0.5) O51A(0.5) Cl4B(0.5)
 O48B(0.5) O49B(0.5) O50B(0.5) O51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) O54(0.5) H54(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
4.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
4.e Idealised tetrahedral OH refined as rotating group:
 O54(H54)
;
_shelx_res_checksum              24271
_shelx_hkl_checksum              34170
_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 1.452
_oxdiff_exptl_absorpt_empirical_full_min 0.802