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_7128423
_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), C2 H3 N'
_chemical_formula_sum            'C28 H27 B2 F8 Fe N13 O2'
_chemical_formula_weight         807.09
_chemical_name_systematic
;
Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)
ditetrafluoroborate acetonitrile 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                83.354(5)
_cell_angle_beta                 79.986(4)
_cell_angle_gamma                80.831(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2279(3)
_cell_length_b                   12.5396(6)
_cell_length_c                   17.5742(11)
_cell_measurement_reflns_used    6502
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      73.47
_cell_measurement_theta_min      4.19
_cell_volume                     1755.53(16)
_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      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.934
_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     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.934
_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       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6607
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.574
_diffrn_reflns_theta_min         3.585
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.837
_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            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6607
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0916P)^2^+2.4776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02624k7.cif
_cod_data_source_block           80-acnhs
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_original_cell_volume        1755.54(16)
_cod_database_code               7128423
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.603(4)
 0.397(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.39265 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.39265 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.274197 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.274197 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39265 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39265 with sigma of 0.02
 B47B-F48C = B47B-F49C = B47B-F50C = B47B-F51C
 1.39265 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.274197 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.274197 with sigma of 0.02
 F48C-F49C = F48C-F50C = F48C-F51C = F49C-F50C = F49C-F51C = F50C-F51C
 2.274197 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.48 with sigma of 0.02
 C53A-N54A = C53B-N54B
 1.15 with sigma of 0.02
 C52A-N54A = C52B-N54B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) F43A(0.67)
 F44A(0.67) F45A(0.67) F46A(0.67) F43B(0.33) F44B(0.33) F45B(0.33) F46B(0.33)
 B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.2)
 F49B(0.2) F50B(0.2) F51B(0.2) F48C(0.3) F49C(0.3) F50C(0.3) F51C(0.3)
 C52A(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53A(0.5) N54A(0.5) C52B(0.5)
 H52D(0.5) H52E(0.5) H52F(0.5) C53B(0.5) N54B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52A(H52A,H52B,H52C), C52B(H52D,
 H52E,H52F)
;
_shelx_res_checksum              20721
_shelx_hkl_checksum              49834
_olex2_submission_special_instructions 'No special instructions were received'