Reversible structural change of [Co<sub>2</sub>Fe<sub>2</sub>] complexes between diamagnetic hydrogen-bonded 1D chains and paramagnetic complexes within a layered structure of amphiphilic anions.
Mihara, Nozomi; Iitsuka, Soyoka; Shiga, Takuya; Nihei, Masayuki; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7190–7196; doi:10.1039/d4dt00482e

data_7715514
_publ_section_title
;
 Reversible structural change of [Co<sub>2</sub>Fe<sub>2</sub>] complexes
 between diamagnetic hydrogen-bonded 1D chains and paramagnetic complexes
 within a layered structure of amphiphilic anions.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7190
_journal_page_last               7196
_journal_paper_doi               10.1039/d4dt00482e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C108 H140 B2 Co2 Fe2 N26, 2(C18 H22 B Fe N9), 4(C3 H7 N O),H1'
_chemical_formula_sum            'C156 H248 B4 Co2 Fe4 N48 O22'
_chemical_formula_weight         3532.51
_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   mixed
_audit_creation_date             2024-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-16 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                95.341(4)
_cell_angle_beta                 92.874(3)
_cell_angle_gamma                94.153(4)
_cell_formula_units_Z            1
_cell_length_a                   12.484(3)
_cell_length_b                   16.445(4)
_cell_length_c                   22.402(5)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.24
_cell_volume                     4559.6(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27629
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.473
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1874
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         20042
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+5.7470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14149
_reflns_number_total             20042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00482e2.cif
_cod_data_source_block           1T2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7715513--7715515.cif.
;
_cod_original_cell_volume        4559.6(17)
_cod_database_code               7715514
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Restrained distances
 H79-O3
 0.84 with sigma of 0.02
 H3-O3
 0.84 with sigma of 0.02
 H4-O4
 0.84 with sigma of 0.02
 H89-O4
 0.84 with sigma of 0.02
 H81-O5
 0.84 with sigma of 0.02
 H84-O5
 0.84 with sigma of 0.02
 H6-O6
 0.84 with sigma of 0.02
 H85-O6
 0.84 with sigma of 0.02
 H83-O7A
 0.84 with sigma of 0.02
 H88-O7A
 0.84 with sigma of 0.02
 H105-O7B
 0.84 with sigma of 0.02
 H102-O7B
 0.84 with sigma of 0.02
 O8A-H82
 0.84 with sigma of 0.02
 O8A-H80
 0.84 with sigma of 0.02
 H87-O9B
 0.84 with sigma of 0.02
 H86-O9B
 0.84 with sigma of 0.02
 H97-O12A
 0.84 with sigma of 0.02
 H95-O12A
 0.84 with sigma of 0.02
 H14-O14B
 0.84 with sigma of 0.02
 H100-O14B
 0.84 with sigma of 0.02
 H101-O11
 0.84 with sigma of 0.02
 H94-O11
 0.84 with sigma of 0.02
 H103-O9A
 0.84 with sigma of 0.02
 H104-O9A
 0.84 with sigma of 0.02
 H114-O15A
 0.84 with sigma of 0.02
 H115-O15A
 0.84 with sigma of 0.02
 H79-H3
 1.33 with sigma of 0.04
 H89-H4
 1.33 with sigma of 0.04
 H81-H84
 1.33 with sigma of 0.04
 H6-H85
 1.33 with sigma of 0.04
 H83-H88
 1.33 with sigma of 0.04
 H105-H102
 1.33 with sigma of 0.04
 H82-H80
 1.33 with sigma of 0.04
 H87-H86
 1.33 with sigma of 0.04
 H97-H95
 1.33 with sigma of 0.04
 H14-H100
 1.33 with sigma of 0.04
 H101-H94
 1.33 with sigma of 0.04
 H103-H104
 1.33 with sigma of 0.04
 H114-H115
 1.33 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C42 \\sim C44 \\sim C43 \\sim C45: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C51 \\sim C53 \\sim C52 \\sim C54: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C26B \\sim C24 \\sim C27B \\sim C25B: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C24 \\sim C27A \\sim C26A \\sim C25A: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
3. Rigid body (RIGU) restrains
 C42, C44, C43, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C51, C53, C52, C54
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C26B, C24, C27B, C25B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C24, C27A, C26A, C25A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O2B)=Sof(C74B)=Sof(H106)=Sof(C76B)=Sof(H107)=Sof(H108)=Sof(H109)=Sof(O7B)=
 Sof(H105)=Sof(H102)=Sof(O7A)=Sof(H88)=Sof(H83)=Sof(O9B)=Sof(H87)=Sof(H86)=
 Sof(O14B)=Sof(H14)=Sof(H100)=1-FVAR(1)
 Sof(O2A)=Sof(C76A)=Sof(H110)=Sof(C74A)=Sof(H111)=Sof(H112)=Sof(H113)=Sof(O8A)=
 Sof(H80)=Sof(H82)=Sof(O9A)=Sof(H103)=Sof(H104)=Sof(O12A)=Sof(H97)=Sof(H95)=
 Sof(O15A)=Sof(H114)=Sof(H115)=FVAR(1)
 Sof(C25B)=Sof(H116)=Sof(H117)=Sof(H118)=Sof(C26B)=Sof(H119)=Sof(H120)=
 Sof(H121)=Sof(C27B)=Sof(H122)=Sof(H123)=Sof(H124)=1-FVAR(2)
 Sof(C25A)=Sof(H25)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26)=Sof(H26A)=Sof(H26B)=
 Sof(C27A)=Sof(H27)=Sof(H27A)=Sof(H27B)=FVAR(2)
5.a Fixed occupancy and ADP/Uiso:
 H79(H3), H4(H89), H81(H84), H6(H85), H105(H102), H88(H83), H80(H82),
 H103(H104), H87(H86), H101(H94), H97(H95), H14(H100), H114(H115)
5.b Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15), C19(H19), C20(H20), C22(H22), C28(H28), C29(H29),
 C31(H31), C37(H37), C38(H38), C40(H40), C47(H47), C49(H49), C50(H50), C59(H59),
  C64(H64), C69(H69), C74B(H106), C76A(H110), C77(H77)
5.d Idealised Me refined as rotating group:
 C7(H7,H7A,H7B), C8(H8,H8A,H8B), C12(H12,H12A,H12B), C13(H13,H13A,H13B),
 C17(H17,H17A,H17B), C18(H18,H18A,H18B), C25A(H25,H25A,H25B), C26A(H26,H26A,
 H26B), C27A(H27,H27A,H27B), C25B(H116,H117,H118), C26B(H119,H120,H121),
 C27B(H122,H123,H124), C34(H34,H34A,H34B), C35(H35,H35A,H35B), C36(H36,H36A,
 H36B), C43(H43,H43A,H43B), C44(H44,H44A,H44B), C45(H45,H45A,H45B), C52(H52,
 H52A,H52B), C53(H53,H53A,H53B), C54(H54,H54A,H54B), C61(H61,H61A,H61B),
 C62(H62,H62A,H62B), C66(H66,H66A,H66B), C67(H67,H67A,H67B), C71(H71,H71A,H71B),
  C72(H72,H72A,H72B), C73(H73,H73A,H73B), C76B(H107,H108,H109), C75(H75,H75A,
 H75B), C74A(H111,H112,H113), C78(H78,H78A,H78B)
;
_shelx_res_checksum              24639
_olex2_submission_special_instructions 'No special instructions were received'