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_7128426
_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, 0.9(B F4), 1.1(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B0.9 Cl1.1 F3.6 Fe N13 O6.4'
_chemical_formula_weight         835.02
_chemical_name_systematic
;
Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)
tetrafluoroborate(2/0.9) perchlorate(2/1.1) 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             2020-07-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                82.678(3)
_cell_angle_beta                 78.686(4)
_cell_angle_gamma                85.091(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3123(5)
_cell_length_b                   12.3617(5)
_cell_length_c                   17.5779(6)
_cell_measurement_reflns_used    5626
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      73.39
_cell_measurement_theta_min      4.15
_cell_volume                     1753.25(14)
_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      125(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.927
_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_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13546
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.588
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.964
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_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            brown
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0598P)^2^+0.8511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5375
_reflns_number_total             6565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02624k11.cif
_cod_data_source_block           etcnmalt
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_original_cell_volume        1753.24(14)
_cod_original_formula_sum        'C29 H29 B0.90 Cl1.10 F3.60 Fe N13 O6.40'
_cod_database_code               7128426
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43 = B42-F44 = B42-F45 = B42-F46
 1.37 with sigma of 0.02
 B47-F48 = B47-F49 = B47-F50 = B47-F51
 1.37 with sigma of 0.02
 F43-F44 = F43-F45 = F43-F46 = F44-F45 = F44-F46 = F45-F46
 2.24 with sigma of 0.02
 F48-F49 = F48-F50 = F48-F51 = F49-F50 = F49-F51 = F50-F51
 2.24 with sigma of 0.02
 Cl42-O43 = Cl42-O44 = Cl42-O45 = Cl42-O46
 1.45 with sigma of 0.02
 Cl47-O48 = Cl47-O49 = Cl47-O50 = Cl47-O51
 1.45 with sigma of 0.02
 O43-O44 = O43-O45 = O43-O46 = O44-O45 = O44-O46 = O45-O46
 2.37 with sigma of 0.02
 O48-O49 = O48-O50 = O48-O51 = O49-O50 = O49-O51 = O50-O51
 2.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B42 \\sim F43 \\sim F44 \\sim F45 \\sim F46: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
B47 \\sim F48 \\sim F49 \\sim F50 \\sim F51: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
4. Others
 Fixed Sof: B42(0.49) F43(0.49) F44(0.49) F45(0.49) F46(0.49) Cl42(0.51)
 O43(0.51) O44(0.51) O45(0.51) O46(0.51) B47(0.41) F48(0.41) F49(0.41)
 F50(0.41) F51(0.41) Cl47(0.59) O48(0.59) O49(0.59) O50(0.59) O51(0.59)
5.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
5.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
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              65368
_shelx_hkl_checksum              21248
_olex2_submission_special_instructions 'No special instructions were received'