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_7715513
_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_absolute_configuration rm
_chemical_formula_moiety
'C108 H140 B2 Co2 Fe2 N26, 2(C31 H58 N O8 S), 6(O) [+ solvent]'
_chemical_formula_sum            'C170 H256 B2 Co2 Fe2 N28 O22 S2'
_chemical_formula_weight         3359.31
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-02-16 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                75.8920(10)
_cell_angle_beta                 79.5850(10)
_cell_angle_gamma                71.7930(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8879(8)
_cell_length_b                   17.7778(12)
_cell_length_c                   22.5479(15)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.24
_cell_volume                     4728.7(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56005
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.390
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2064
_refine_ls_number_reflns         41960
_refine_ls_number_restraints     1262
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1398P)^2^+4.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2508
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                26851
_reflns_number_total             41960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00482e2.cif
_cod_data_source_block           1X2-A
_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_database_code               7715513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.887
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.68922
 0.31078
2. Restrained distances
 C44-C45
 1.51 with sigma of 0.02
 C44-C46
 1.51 with sigma of 0.02
 C44-C47
 1.51 with sigma of 0.02
 N27-C110
 1.34 with sigma of 0.02
 C112-O12
 1.21 with sigma of 0.02
 S1-C109
 1.82 with sigma of 0.02
 C110-C109
 1.51 with sigma of 0.02
 C110-O11
 1.21 with sigma of 0.02
 O13-C113
 1.43 with sigma of 0.02
 C113-C114
 1.51 with sigma of 0.02
 C114-C115
 1.51 with sigma of 0.02
 C116-C115
 1.51 with sigma of 0.02
 C116-C117
 1.51 with sigma of 0.02
 C118-C117
 1.51 with sigma of 0.02
 C118-C119
 1.51 with sigma of 0.02
 C120-C119
 1.51 with sigma of 0.02
 C120-C121
 1.51 with sigma of 0.02
 C121-C122
 1.51 with sigma of 0.02
 C122-C123
 1.51 with sigma of 0.02
 C123-C124
 1.51 with sigma of 0.02
 C111-C125
 1.51 with sigma of 0.02
 O15-C127
 1.38 with sigma of 0.02
 O15-C128
 1.43 with sigma of 0.02
 C128-C129
 1.51 with sigma of 0.02
 C130-C129
 1.51 with sigma of 0.02
 C130-C131
 1.51 with sigma of 0.02
 C132-C131
 1.51 with sigma of 0.02
 C132-C133
 1.51 with sigma of 0.02
 C133-C134
 1.51 with sigma of 0.02
 C134-C135
 1.51 with sigma of 0.02
 C135-C136
 1.51 with sigma of 0.02
 C136-C137
 1.51 with sigma of 0.02
 C138-C137
 1.51 with sigma of 0.02
 C138-C139
 1.51 with sigma of 0.02
 O21-C144
 1.43 with sigma of 0.02
 C144-C145
 1.51 with sigma of 0.02
 C146-C145
 1.51 with sigma of 0.02
 C146-C147
 1.51 with sigma of 0.02
 C147-C148
 1.51 with sigma of 0.02
 C149-C148
 1.51 with sigma of 0.02
 C149-C150
 1.51 with sigma of 0.02
 C150-C151
 1.51 with sigma of 0.02
 C151-C152
 1.51 with sigma of 0.02
 C152-C153
 1.51 with sigma of 0.02
 C153-C154
 1.51 with sigma of 0.02
 C154-C155
 1.51 with sigma of 0.02
 C162-C163
 1.51 with sigma of 0.02
 C163-C164
 1.51 with sigma of 0.02
 C164-C165
 1.51 with sigma of 0.02
 C165-C166
 1.51 with sigma of 0.02
 C166-C167
 1.51 with sigma of 0.02
 C167-C168
 1.51 with sigma of 0.02
 C169-C170
 1.51 with sigma of 0.02
 C45-C47
 2.55 with sigma of 0.02
 C45-C46
 2.55 with sigma of 0.02
 S1-C110
 2.65 with sigma of 0.02
 C110-C111
 2.55 with sigma of 0.02
 C113-C115
 2.55 with sigma of 0.02
 C114-C116
 2.55 with sigma of 0.02
 C115-C117
 2.55 with sigma of 0.02
 C116-C118
 2.55 with sigma of 0.02
 C117-C119
 2.55 with sigma of 0.02
 C118-C120
 2.55 with sigma of 0.02
 C119-C121
 2.55 with sigma of 0.02
 C120-C122
 2.55 with sigma of 0.02
 C121-C123
 2.55 with sigma of 0.02
 C122-C124
 2.55 with sigma of 0.02
 C128-C130
 2.55 with sigma of 0.02
 C129-C131
 2.55 with sigma of 0.02
 C130-C132
 2.55 with sigma of 0.02
 C131-C133
 2.55 with sigma of 0.02
 C132-C134
 2.55 with sigma of 0.02
 C133-C135
 2.55 with sigma of 0.02
 C134-C136
 2.55 with sigma of 0.02
 C135-C137
 2.55 with sigma of 0.02
 C136-C138
 2.55 with sigma of 0.02
 C137-C139
 2.55 with sigma of 0.02
 O21-C145
 2.55 with sigma of 0.02
 C143-C144
 2.45 with sigma of 0.02
 C144-C146
 2.55 with sigma of 0.02
 C145-C147
 2.55 with sigma of 0.02
 C147-C149
 2.55 with sigma of 0.02
 C148-C150
 2.55 with sigma of 0.02
 C149-C151
 2.55 with sigma of 0.02
 C150-C152
 2.55 with sigma of 0.02
 C151-C153
 2.55 with sigma of 0.02
 C152-C154
 2.55 with sigma of 0.02
 C153-C155
 2.55 with sigma of 0.02
 C168-C170
 2.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C11: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C26 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
N19 \\sim N20 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
N21 \\sim N22 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C105 \\sim C106 \\sim C107 \\sim C108: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
S1 \\sim O9 \\sim O8 \\sim C10: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
C111 \\sim N27 \\sim C110 \\sim O11 \\sim C109: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C111 \\sim C112 \\sim C125: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
C124 \\sim C123 \\sim C122 \\sim C121 \\sim C120: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 1.7A
C124 \\sim C123 \\sim C122 \\sim C121 \\sim C120 \\sim C119 \\sim C118: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C119 \\sim C118 \\sim C117 \\sim C116 \\sim C115 \\sim C114 \\sim C113: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C111 \\sim C112 \\sim O12 \\sim O13 \\sim C113: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C128 \\sim O15 \\sim C127 \\sim O14 \\sim C126 \\sim C125: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C134 \\sim C133 \\sim C132 \\sim C131 \\sim C130 \\sim C129 \\sim C128: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C139 \\sim C138 \\sim C137 \\sim C136 \\sim C135 \\sim C134: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C155 \\sim C154 \\sim C153 \\sim C152 \\sim C151 \\sim C150 \\sim C149 \\sim
C148 \\sim C147 \\sim C146: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
C152 \\sim C151 \\sim C150 \\sim C149 \\sim C148: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 1.7A
C148 \\sim C147 \\sim C146 \\sim C145: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
C145 \\sim C144 \\sim O21 \\sim C143 \\sim O20: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C142 \\sim N28 \\sim C143 \\sim C156: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C160 \\sim C159 \\sim O22 \\sim O23 \\sim C158: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C170 \\sim C169 \\sim C168 \\sim C167 \\sim C166 \\sim C165 \\sim C164 \\sim
C163 \\sim C162 \\sim C161: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
Uanis(C47) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C15, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C26, C27, C28, C29
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C53, C54, C55, C56
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N19, N20, C63, C64, C65, C66, C67
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N21, N22, C68, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C105, C106, C107, C108
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S1, O9, O8, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C111, N27, C110, O11, C109
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C111, C112, C125
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C124, C123, C122, C121, C120
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C124, C123, C122, C121, C120, C119, C118
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C119, C118, C117, C116, C115, C114, C113
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C111, C112, O12, O13, C113
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C128, O15, C127, O14, C126, C125
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C134, C133, C132, C131, C130, C129, C128
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C139, C138, C137, C136, C135, C134
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C155, C154, C153, C152, C151, C150, C149, C148, C147, C146
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C152, C151, C150, C149, C148
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C148, C147, C146, C145
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C145, C144, O21, C143, O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C142, N28, C143, C156
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C160, C159, O22, O23, C158
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C170, C169, C168, C167, C166, C165, C164, C163, C162, C161
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O2A(0.5) O2B(0.5)
6.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), C111(H111), C142(H142)
6.b Secondary CH2 refined with riding coordinates:
 C109(H10M,H10N), C113(H11A,H11B), C114(H11C,H11D), C115(H11E,H11F), C116(H11G,
 H11H), C117(H11I,H11J), C118(H143,H144), C119(H11K,H11L), C120(H12A,H12B),
 C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H), C125(H12L,H12M), C126(H12N,
 H12O), C128(H12P,H12Q), C129(H12R,H12S), C130(H13A,H13B), C131(H13C,H13D),
 C132(H13E,H13F), C133(H13G,H13H), C134(H13I,H13J), C135(H13K,H13L), C136(H13M,
 H13N), C137(H13O,H13P), C138(H13Q,H13R), C140(H14D,H14E), C144(H14F,H14G),
 C145(H14H,H14I), C146(H14J,H14K), C147(H14L,H14M), C148(H14N,H14O), C149(H14P,
 H14Q), C150(H15D,H15E), C151(H15F,H15G), C152(H15H,H15I), C153(H15J,H15K),
 C154(H15L,H15M), C156(H15Q,H15R), C157(H15S,H15T), C159(H15U,H15V), C160(H16A,
 H16B), C161(H16C,H16D), C162(H16E,H16F), C163(H16G,H16H), C164(H16I,H16J),
 C165(H16K,H16L), C166(H16M,H16N), C167(H16O,H16P), C168(H16Q,H16R), C169(H16S,
 H16T)
6.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C72(H72A,H72B,H72C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C97(H97A,
 H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C106(H10D,H10E,H10F),
 C107(H10G,H10H,H10I), C108(H10J,H10K,H10L), C124(H12I,H12J,H12K), C139(H13S,
 H13T,H13U), C155(H15N,H15O,H15P), C170(H17A,H17B,H17C)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C17(H17), C22(H22), C24(H24), C25(H25), C30(H30), C31(H31),
 C33(H33), C39(H39), C40(H40), C42(H42), C49(H49), C51(H51), C52(H52), C59(H59),
  C64(H64), C69(H69), C73(H73), C74(H74), C76(H76), C83(H83), C85(H85),
 C86(H86), C91(H91), C92(H92), C94(H94), C100(H100), C101(H101), C103(H103),
 N27(H27), N28(H28)
6.e Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              31712
_shelx_fab_checksum              29573
_platon_squeeze_void_probe_radius 1.20