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_4129168
_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         'C14 H18 Fe N6 O2, 2(B F4), H2 O'
_chemical_formula_sum            'C14 H20 B2 F8 Fe N6 O3'
_chemical_formula_weight         549.83
_chemical_name_systematic
;
Catena-[2-methyl-4,6-(pyrazol-1-yl)pyrimidine]-aqua-acetone-iron(II) 
ditetrafluoroborate monohydrate (compound 5.H2O)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.628(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1084(2)
_cell_length_b                   9.56750(10)
_cell_length_c                   21.0007(4)
_cell_measurement_reflns_used    4223
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.32
_cell_measurement_theta_min      4.17
_cell_volume                     2177.96(6)
_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      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu 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  0.0210
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8404
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.62
_diffrn_reflns_theta_min         4.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.481
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.751
_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    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4261
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+1.6258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                3835
_reflns_number_total             4261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b08862_si_013.cif
_cod_data_source_block           89-b-cu
_cod_depositor_comments
'Adding full bibliography for 4129157--4129168.cif.'
_cod_database_code               4129168
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 B29A-F30A = B29A-F31A = B29A-F32A = B29A-F33A
 1.37156 with sigma of 0.02
 B29B-F30B = B29B-F31B = B29B-F32B = B29B-F33B
 1.37156 with sigma of 0.02
 F30A-F31A = F30A-F32A = F30A-F32A = F31A-F32A = F31A-F33A = F32A-F33A
 2.239757 with sigma of 0.02
 F30B-F31B = F30B-F32B = F30B-F32B = F31B-F32B = F31B-F33B = F32B-F33B
 2.239757 with sigma of 0.02
 O23-H23A = O23-H23B = O34-H34A = O34-H34B
 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: B29A(0.71) F30A(0.71) F31A(0.71) F32A(0.71) F33A(0.71) B29B(0.29)
 F30B(0.29) F31B(0.29) F32B(0.29) F33B(0.29)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17)
4.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;