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_7128431
_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), C3 H5 N'
_chemical_formula_sum            'C29 H29 Cl2 Fe N13 O10'
_chemical_formula_weight         846.40
_chemical_name_systematic
;
Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)
diperchlorate propionitrile 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             2020-07-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                108.029(3)
_cell_angle_beta                 98.689(2)
_cell_angle_gamma                95.458(2)
_cell_formula_units_Z            4
_cell_length_a                   8.3390(2)
_cell_length_b                   20.3671(5)
_cell_length_c                   22.8144(7)
_cell_measurement_reflns_used    11254
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      73.69
_cell_measurement_theta_min      4.01
_cell_volume                     3600.56(18)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.929
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19056
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.871
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         19056
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1279P)^2^+5.4432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14582
_reflns_number_total             19056
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9209\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.42 0.31 0.85] (direct)
;
_cod_data_source_file            d1cc02624k17.cif
_cod_data_source_block           etcnclmt
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_database_code               7128431
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6094(12)
 0.3906(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C66A-C67A = C66B-C67B
 1.51 with sigma of 0.02
 C67A-C68A = C67B-C68B
 1.48 with sigma of 0.02
 C68A-N69A = C68B-N69B
 1.15 with sigma of 0.02
 C66A-C68A = C66B-C68B
 2.44 with sigma of 0.02
 C67A-N69A = C67B-N69B
 2.63 with sigma of 0.02
4. Others
 Fixed Sof: C66A(0.83) H66A(0.83) H66B(0.83) H66C(0.83) C67A(0.83) H67A(0.83)
 H67B(0.83) C68A(0.83) N69A(0.83) C66B(0.17) H66D(0.17) H66E(0.17) H66F(0.17)
 C67B(0.17) H67C(0.17) H67D(0.17) C68B(0.17) N69B(0.17)
5.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C67A(H67A,H67B), C67B(H67C,H67D)
5.b Me refined with riding coordinates:
 C66A(H66A,H66B,H66C), C66B(H66D,H66E,H66F)
5.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), N18A(H18A), C24A(H24A), C26A(H26A), C30A(H30A),
 C31A(H31A), C32A(H32A), C35A(H35A), C36A(H36A), C37A(H37A), N38A(H38A),
 C4B(H4B), C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
  C17B(H17B), N18B(H18B), C24B(H24B), C26B(H26B), C30B(H30B), C31B(H31B),
 C32B(H32B), C35B(H35B), C36B(H36B), C37B(H37B), N38B(H38B)
5.d Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C41A(H41A,H41B,H41C), C21B(H21D,H21E,H21F), C41B(H41D,
 H41E,H41F), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              72162
_shelx_hkl_checksum              32552
_olex2_submission_special_instructions 'No special instructions were received'