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_7128425
_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             2020-07-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                107.978(3)
_cell_angle_beta                 99.002(3)
_cell_angle_gamma                95.195(3)
_cell_formula_units_Z            4
_cell_length_a                   8.3169(3)
_cell_length_b                   20.4484(7)
_cell_length_c                   22.6673(8)
_cell_measurement_reflns_used    10156
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      73.29
_cell_measurement_theta_min      3.57
_cell_volume                     3581.8(2)
_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      180(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.946
_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_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28990
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.529
_diffrn_reflns_theta_min         3.578
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.860
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       lath
_exptl_crystal_F_000             1707
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         13444
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      12.195
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0965P)^2^+4.9720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10282
_reflns_number_total             13444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02624k12.cif
_cod_data_source_block           etcnmamt
_cod_depositor_comments
'Adding full bibliography for 7128414--7128431.cif.'
_cod_original_formula_sum        'C29 H29 B0.90 Cl1.10 F3.60 Fe N13 O6.40'
_cod_database_code               7128425
_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
 B52-F53 = B52-F54 = B52-F55 = B52-F56
 1.37 with sigma of 0.02
 B57-F58 = B57-F59 = B57-F60 = B57-F61
 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
 F53-F54 = F53-F55 = F53-F56 = F54-F55 = F54-F56 = F55-F56
 2.24 with sigma of 0.02
 F58-F59 = F58-F60 = F58-F61 = F59-F60 = F59-F61 = F60-F61
 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
 Cl52-O53 = Cl52-O54 = Cl52-O55 = Cl52-O56
 1.45 with sigma of 0.02
 Cl57-O48 = Cl57-O49 = Cl57-O50 = Cl57-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
 O53-O54 = O53-O55 = O53-O56 = O54-O55 = O54-O56 = O55-O56
 2.37 with sigma of 0.02
 O58-O59 = O58-O60 = O58-O61 = O59-O60 = O59-O61 = O60-O61
 2.37 with sigma of 0.02
 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
3. Uiso/Uaniso restraints and constraints
B57 \\sim Cl57: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
B42 \\sim Cl42: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Others
 Fixed Sof: B42(0.41) F43(0.41) F44(0.41) F45(0.41) F46(0.41) Cl42(0.59)
 O43(0.59) O44(0.59) O45(0.59) O46(0.59) B47(0.49) F48(0.49) F49(0.49)
 F50(0.49) F51(0.49) Cl47(0.51) O48(0.51) O49(0.51) O50(0.51) O51(0.51)
 B52(0.41) F53(0.41) F54(0.41) F55(0.41) F56(0.41) Cl52(0.59) O53(0.59)
 O54(0.59) O55(0.59) O56(0.59) B57(0.49) F58(0.49) F59(0.49) F60(0.49)
 F61(0.49) Cl57(0.51) O58(0.51) O59(0.51) O60(0.51) O61(0.51) C66A(0.74)
 H66A(0.74) H66B(0.74) H66C(0.74) C67A(0.74) H67A(0.74) H67B(0.74) C68A(0.74)
 N69A(0.74) C66B(0.26) H66D(0.26) H66E(0.26) H66F(0.26) C67B(0.26) H67C(0.26)
 H67D(0.26) C68B(0.26) N69B(0.26)
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              3488
_shelx_hkl_checksum              5263
_olex2_submission_special_instructions 'No special instructions were received'