A mixed-spin spin-crossover thiozolylimine [Fe<sub>4</sub>L<sub>6</sub>]<sup>8+</sup> cage.
Li, Li; Craze, Alexander R.; Mustonen, Outi; Zenno, Hikaru; Whittaker, Jacob J.; Hayami, Shinya; Lindoy, Leonard F.; Marjo, Christopher E.; Clegg, Jack K.; Aldrich-Wright, Janice R; Li, Feng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9935–9938; doi:10.1039/c9dt01947b

data_7700224
_publ_section_title
;
 A mixed-spin spin-crossover thiozolylimine
 [Fe<sub>4</sub>L<sub>6</sub>]<sup>8+</sup> cage.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9935
_journal_page_last               9938
_journal_paper_doi               10.1039/c9dt01947b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C120 H84 Fe4 N24 S12, 8(B F4), 9/25(C2 H3 N)'
_chemical_formula_sum            'C138.5 H111.75 B8 F32 Fe4 N32 S12'
_chemical_formula_weight         3526.94
_chemical_name_systematic        P21onc
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-05-30
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-30 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.200(7)
_cell_length_b                   29.750(6)
_cell_length_c                   30.060(6)
_cell_measurement_reflns_used    135734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.227
_cell_measurement_theta_min      0.597
_cell_volume                     30490(11)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.2661
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            135734
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        17.227
_diffrn_reflns_theta_max         17.227
_diffrn_reflns_theta_min         0.597
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             14326
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1867
_refine_ls_number_reflns         18459
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_gt           0.1110
_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^)+(0.1603P)^2^+288.7571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2711
_refine_ls_wR_factor_ref         0.3242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9939
_reflns_number_total             18459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01947b2.cif
_cod_data_source_block           p21onc_a
_cod_depositor_comments          'Adding full bibliography for 7700224.cif.'
_cod_original_formula_sum        'C138.50 H111.75 B8 F32 Fe4 N32 S12'
_cod_database_code               7700224
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.663
_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
2. Restrained distances
 B86-F03W
 1.39 with sigma of 0.02
 B86-F07M
 1.39 with sigma of 0.02
 F045-B86
 1.39 with sigma of 0.02
 F0AG-B86
 1.39 with sigma of 0.02
 F14-B1
 1.39 with sigma of 0.02
 B1-F17
 1.39 with sigma of 0.02
 B1-F16
 1.39 with sigma of 0.02
 F15-B1
 1.39 with sigma of 0.02
 B127-F3AA
 1.4 with sigma of 0.02
 B127-F3
 1.4 with sigma of 0.02
 B127-F1AA
 1.4 with sigma of 0.02
 F2AA-B127
 1.4 with sigma of 0.02
 B60-F03B
 1.4 with sigma of 0.02
 B60-F0AH
 1.4 with sigma of 0.02
 B60-F040
 1.4 with sigma of 0.02
 B60-F02H
 1.4 with sigma of 0.02
 B4-F5
 1.4 with sigma of 0.02
 B4-F1
 1.4 with sigma of 0.02
 B4-F6
 1.4 with sigma of 0.02
 B4-F2
 1.4 with sigma of 0.02
 B6-F1F
 1.4 with sigma of 0.02
 B6-F6AA
 1.4 with sigma of 0.02
 B6-F1D
 1.4 with sigma of 0.02
 F012-B83
 1.4 with sigma of 0.02
 F7AA-B6
 1.4 with sigma of 0.02
 C7-N0B0
 1.26 with sigma of 0.02
 C0BM-S00W
 1.78 with sigma of 0.02
 C7-C0BM
 1.412 with sigma of 0.02
 B2-F7 \\sim B2-F8 \\sim B2-F9 \\sim B2-F12
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F12 \\sim F12-F7 \\sim F8-F12 \\sim F7-F9
 with sigma of 0.04
 B1-F14 \\sim B1-F15 \\sim B1-F16 \\sim B1-F17
 with sigma of 0.02
 F14-F15 \\sim F15-F16 \\sim F16-F17 \\sim F17-F14 \\sim F15-F17 \\sim F14-F16
 with sigma of 0.04
 B4-F1 \\sim B4-F2 \\sim B4-F5 \\sim B4-F6
 with sigma of 0.02
 F1-F2 \\sim F2-F5 \\sim F5-F6 \\sim F6-F1 \\sim F2-F6 \\sim F1-F5
 with sigma of 0.04
 B6-F1D \\sim B6-F1F
 with sigma of 0.02
 F13-F18 \\sim F18-F19 \\sim F19-F1A \\sim F1A-F13 \\sim F18-F1A \\sim F13-F19
 with sigma of 0.04
 F8AA-B3B \\sim F19-B3A \\sim F0BA-B3B \\sim F18-B3A \\sim F18-B3B \\sim
F1A-B3A \\sim F9AA-B3B \\sim F13-
 B3A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
B2 \\sim F7 \\sim F8 \\sim F9 \\sim F12: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
B1 \\sim F14 \\sim F15 \\sim F16 \\sim F17: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
B4 \\sim F1 \\sim F2 \\sim F5 \\sim F6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
B6 \\sim F1D \\sim F1F: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uiso(B3A) = Uiso(B3B)
4. Others
 Fixed Sof: F19(0.5) B3A(0.5) F1A(0.5) F13(0.5) F0BA(0.5) F8AA(0.5) F9AA(0.5)
 B3B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C028(H028), C02A(H02A), C02R(H02R), C032(H032), C033(H033), C038(H038),
 C03H(H03H), C03I(H03I), C03K(H03K), C03L(H03L), C03R(H03R), C03S(H03S),
 C03T(H03T), C03U(H03U), C03V(H03V), C03Y(H03Y), C03Z(H03Z), C042(H042),
 C043(H043), C046(H046), C047(H047), C04B(H04B), C04C(H04C), C04E(H04E),
 C04G(H04G), C04H(H04H), C04J(H04J), C04K(H04K), C04N(H04N), C04P(H04P),
 C04S(H04S), C04T(H04T), C04U(H04U), C04V(H04V), C04W(H04W), C04Y(H04Y),
 C050(H050), C057(H057), C05B(H05B), C05D(H05D), C05H(H05H), C05I(H05I),
 C05J(H05J), C05M(H05M), C05N(H05N), C05Q(H05Q), C05S(H05S), C05T(H05T),
 C05U(H05U), C05V(H05V), C05W(H05W), C05Y(H05Y), C05Z(H05Z), C060(H060),
 C063(H063), C064(H064), C065(H065), C066(H066), C068(H068), C06A(H06A),
 C06C(H06C), C06D(H06D), C06E(H06E), C06F(H06F), C06K(H06K), C06L(H06L),
 C06M(H06M), C06N(H06N), C06O(H06O), C06P(H06P), C06Q(H06Q), C06R(H06R),
 C06T(H06T), C06V(H06V), C06W(H06W), C06X(H06X), C06Y(H06Y), C06Z(H06Z),
 C070(H070), C071(H071), C073(H073), C074(H074), C076(H076), C077(H077),
 C078(H078), C079(H079), C07A(H07A), C07D(H07D), C07H(H07H), C07I(H07I),
 C07J(H07J), C07K(H07K), C07N(H07N), C07O(H07O), C07S(H07S), C07U(H07U),
 C07V(H07V), C07W(H07W), C07X(H07X), C07Y(H07Y), C07Z(H07Z), C083(H083),
 C085(H085), C086(H086), C087(H087), C088(H088), C089(H089), C08A(H08A),
 C08G(H08G), C08H(H08H), C08J(H08J), C08K(H08K), C08L(H08L), C08M(H08M),
 C08N(H08N), C08P(H08P), C08Q(H08Q), C08R(H08R), C08T(H08T), C08W(H08W),
 C08X(H08X), C08Y(H08Y), C093(H093), C094(H094), C095(H095), C097(H097),
 C098(H098), C09A(H09A), C09B(H09B), C09C(H09C), C09D(H09D), C09E(H09E),
 C09F(H09F), C09G(H09G), C09H(H09H), C09I(H09I), C09L(H09L), C09M(H09M),
 C09N(H09N), C09P(H09P), C09Q(H09Q), C09S(H09S), C09X(H09X), C09Y(H09Y),
 C0A4(H0A4), C0A8(H0A8), C0A9(H0A9), C0AB(H0AB), C0AD(H0AD), C0AE(H0AE),
 C0AJ(H0AJ), C0AK(H0AK), C0AM(H0AM), C0AN(H0AN), C0AQ(H0AQ), C0AR(H0AR),
 C0AS(H0AS), C0AU(H0AU), C0B2(H0B2), C0B5(H0B5), C0B6(H0B6), C0BA(H0BA),
 C0BB(H0BB), C0BG(H0BG), C0BM(H0BM), C0BO(H0BO), C0BV(H0BV)
5.b Idealised Me refined as rotating group:
 C0AI(H0AC,H0AF,H0AG), C0B3(H0BC,H0BD,H0BE), C0B7(H0BN,H0BP,H0BQ), C0BD(H0BF,
 H0BH,H0BI), C0BR(H0BJ,H0BK,H0BL), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              64846
_shelx_fab_checksum              6420
_olex2_submission_special_instructions 'No special instructions were received'