The impact of whole-molecule disorder on spin-crossover in a family of isomorphous molecular crystals
Sephton, Holly E.; Watson, Rhiannon L.; Shahid, Namrah; Vasili, Hari Babu; Baker, Daniel L.; Saha, Dipankar; Capel Berdiell, Izar; Pask, Christopher M.; Cespedes, Oscar; Halcrow, Malcolm A.; Chemical Science 16 (2025) 9203–9212; doi:10.1039/D5SC00090D

data_1574390
_publ_section_title
;
 The impact of whole-molecule disorder on spin-crossover in a family of
 isomorphous molecular crystals
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              9203
_journal_page_last               9212
_journal_paper_doi               10.1039/D5SC00090D
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration ab
_chemical_formula_moiety         'C22 H16 Br2 Fe N10, 2(B F4)'
_chemical_formula_sum            'C22 H16 B2 Br2 F8 Fe N10'
_chemical_formula_weight         809.74
_chemical_name_systematic
Bis[2-{4-bromopyrazol-1-yl}-6-{pyrazol-1-yl}pyridine]iron(II)di(tetrafluoroborate)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2024-12-17 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.848(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5177(12)
_cell_length_b                   9.3657(13)
_cell_length_c                   16.524(3)
_cell_measurement_reflns_used    3435
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      1.21
_cell_volume                     1469.6(4)
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Diamond Light Source station I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.1718
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16061
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.820
_diffrn_reflns_theta_max         26.479
_diffrn_reflns_theta_min         1.197
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.dev.728-gc72b5fc4a
Scaling & analysis of unmerged intensities, absorption correction 
using spherical harmonics
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       fragment
_exptl_crystal_F_000             792
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.024(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.765
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                2873
_reflns_number_total             6420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00090d2.cif
_cod_data_source_block           HS13_lt
_cod_depositor_comments
'Adding full bibliography for 1574389--1574393.cif.'
_cod_original_cell_volume        1469.7(4)
_cod_database_code               1574390
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Br1A(0.72) Br3A(0.88) Br1B(0.28) Br3B(0.12)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C15(H15), C16(H16), C17(H17),
 C21(H21), C22(H22), C23(H23), C27(H27), C29(H29), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              688
_olex2_submission_special_instructions 'No special instructions were received'