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_7128430
_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(B F4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B2 F8 Fe N13 O2'
_chemical_formula_weight         821.12
_chemical_name_systematic
;
Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)
ditetrafluoroborate 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             2020-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                83.832(5)
_cell_angle_beta                 79.727(4)
_cell_angle_gamma                82.425(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2464(3)
_cell_length_b                   12.5340(9)
_cell_length_c                   17.7464(9)
_cell_measurement_reflns_used    5844
_cell_measurement_temperature    187(2)
_cell_measurement_theta_max      72.43
_cell_measurement_theta_min      4.21
_cell_volume                     1782.48(17)
_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      187(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.919
_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     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11206
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.788
_diffrn_reflns_theta_min         3.571
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.213
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.493
_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    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         11206
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1058P)^2^+0.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8519
_reflns_number_total             11206
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9227\% 
 around [0.00 0.71 0.71] (reciprocal) or [-0.33 0.85 0.40] (direct)
;
_cod_data_source_file            d1cc02624k6.cif
_cod_data_source_block           80etcnmt
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_database_code               7128430
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4795(12)
 0.5205(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
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39558 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39558 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.278982 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.278982 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.51 with sigma of 0.02
 C53A-C54A = C53B-C54B
 1.48 with sigma of 0.02
 C54A-N55A = C54B-N55B
 1.15 with sigma of 0.02
 C52A-C54A = C52B-C54B
 2.44 with sigma of 0.02
 C53A-N55A = C53B-N55B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5)
 F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5) C52A(0.6) H52A(0.6) H52B(0.6)
 H52C(0.6) C53A(0.6) H53A(0.6) H53B(0.6) C54A(0.6) N55A(0.6) C52B(0.4)
 H52D(0.4) H52E(0.4) H52F(0.4) C53B(0.4) H53C(0.4) H53D(0.4) C54B(0.4) N55B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.b Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
5.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)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              81595
_shelx_hkl_checksum              49658
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous