Supramolecular Iron Metallocubanes Exhibiting Site-Selective Thermal and Light-Induced Spin-Crossover.
Berdiell, Izar Capel; Hochdörffer, Tim; Desplanches, Cédric; Kulmaczewski, Rafal; Shahid, Namrah; Wolny, Juliusz A.; Warriner, Stuart L.; Cespedes, Oscar; Schünemann, Volker; Chastanet, Guillaume; Halcrow, Malcolm A.; Journal of the American Chemical Society 141 (2019) 18759–18770; doi:10.1021/jacs.9b08862

data_4129159
_publ_section_title
;
 Supramolecular Iron Metallocubanes Exhibiting Site-Selective Thermal and
 Light-Induced Spin-Crossover.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18759
_journal_page_last               18770
_journal_paper_doi               10.1021/jacs.9b08862
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C12 H17 Fe N7 O4, 2(B F4)'
_chemical_formula_sum            'C12 H17 B2 F8 Fe N7 O4'
_chemical_formula_weight         552.80
_chemical_name_systematic
;
[4,6-Di(pyrazol-1-yl)pyrimid-2-one]triaqua[acetonitrile]
iron(II) di[tetrafluoroborate] (compound 4)
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                109.358(9)
_cell_angle_beta                 94.272(7)
_cell_angle_gamma                91.322(8)
_cell_formula_units_Z            2
_cell_length_a                   10.0049(9)
_cell_length_b                   10.1934(11)
_cell_length_c                   11.1633(11)
_cell_measurement_reflns_used    3813
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      73.35
_cell_measurement_theta_min      4.28
_cell_volume                     1069.75(19)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8475
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.45
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.653
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_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    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4018
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.8837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                3639
_reflns_number_total             4018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b08862_si_012.cif
_cod_data_source_block           ic130bf4
_cod_depositor_comments
'Adding full bibliography for 4129157--4129168.cif.'
_cod_original_cell_volume        1069.75(18)
_cod_database_code               4129159
_olex2_refinement_description
;
1. 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, All O(H,H) groups
2. Restrained distances
 B25A-F26A = B25A-F27A = B25A-F28A = B25A-F29A
 1.38998 with sigma of 0.02
 B25B-F26B = B25B-F27B = B25B-F28B = B25B-F29B
 1.38998 with sigma of 0.02
 F26A-F27A = F26A-F28A = F26A-F29A = F27A-F28A = F27A-F29A = F28A-F29A
 2.269837 with sigma of 0.02
 F26B-F27B = F26B-F28B = F26B-F29B = F27B-F28B = F27B-F29B = F28B-F29B
 2.269837 with sigma of 0.02
 O19-H19A = O19-H19B = O20-H20A = O20-H20B = O21-H21A = O21-H21B
 0.9 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B25A(0.5) F26A(0.5) F27A(0.5) F28A(0.5) F29A(0.5) B25B(0.5)
 F26B(0.5) F27B(0.5) F28B(0.5) F29B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;