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_4129158
_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 N8 O3, 2(Cl O4)'
_chemical_formula_sum            'C14 H18 Cl2 Fe N8 O11'
_chemical_formula_weight         601.11
_chemical_name_systematic
;
[4,6-Di(pyrazol-1-yl)pyrimid-2-one]diaqua-bis[acetonitrile]
iron(II) diperchlorate (compound 3)
;
_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             2018-06-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                86.767(2)
_cell_angle_beta                 77.965(3)
_cell_angle_gamma                76.781(2)
_cell_formula_units_Z            4
_cell_length_a                   10.4570(3)
_cell_length_b                   15.2881(4)
_cell_length_c                   15.3002(4)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.44
_cell_measurement_theta_min      4.40
_cell_volume                     2328.76(11)
_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 0.983
_diffrn_measured_fraction_theta_max 0.972
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15126
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.73
_diffrn_reflns_theta_min         4.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.983
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.670
_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            orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         15126
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1118P)^2^+0.8218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                12359
_reflns_number_total             15126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b08862_si_011.cif
_cod_data_source_block           130-clo4
_cod_depositor_comments
'Adding full bibliography for 4129157--4129168.cif.'
_cod_database_code               4129158
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_twin_special_details
;
Component 2 rotated by -179.9936\% 
 around [0.00 0.71 0.71] (reciprocal) or [-0.41 0.65 0.64] (direct)
;
_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
 Cl5A-O59A = Cl5A-O60A = Cl5A-O61A = Cl5A-O62A
 1.433 with sigma of 0.02
 Cl5B-O59B = Cl5B-O60B = Cl5B-O61B = Cl5B-O62B
 1.433 with sigma of 0.02
 O59A-O60A = O59A-O61A = O59A-O62A = O60A-O61A = O60A-O62A = O61A-O62A
 2.340089 with sigma of 0.02
 O59B-O60B = O59B-O61B = O59B-O62B = O60B-O61B = O60B-O62B = O61B-O62B
 2.340089 with sigma of 0.02
 O19-H19A = O19-H19B = O20-H20A = O20-H20B
 0.9 with sigma of 0.02
 O45-H45A = O45-H45B = O46-H46A = O46-H46B
 0.9 with sigma of 0.02
 H19A-H19B = H20A-H20B = H45A-H45B = H46A-H46B
 1.47 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl5A(0.61) O59A(0.61) O60A(0.61) O61A(0.61) O62A(0.61) Cl5B(0.39)
 O59B(0.39) O60B(0.39) O61B(0.39) O62B(0.39)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), N7(H7), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18),
 C31(H31), N33(H33), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44)
4.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C49(H49A,H49B,H49C), C52(H52A,H52B,
 H52C)
;