Anthryl-Functionalized Cyanide-Bridged Fe/Co Cubes
Liu, Qi; Cheng, Yue; Liu, Shihao; Chen, Zi-Yi; Zhang, Yuan-Zhu; Dalton Transactions  (2023) –; doi:10.1039/D3DT01630G

data_7713746
_publ_section_title
;
 Anthryl-Functionalized Cyanide-Bridged Fe/Co Cubes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01630G
_journal_year                    2023
_chemical_formula_moiety
'C164 H136 B4 Co4 Fe4 N68 O4, 3.5(C F3 O3 S), 2(C2 H3 N), 0.5(O3 S), C4 H10 O, 0.5(C F3), 6[C2H3N], 6[C4H10O]'
_chemical_formula_sum            'C212 H230 B4 Co4 F12 Fe4 N76 O23 S4'
_chemical_formula_weight         5069.31
_chemical_name_systematic        '[(pzTp)Fe(CN)3Co(TpEtOAn)]4[OTf]4.8MeCN.7Et2O'
_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     iterative
_audit_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-06 deposited with the CCDC.	2023-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                93.235(2)
_cell_angle_beta                 92.907(2)
_cell_angle_gamma                108.862(2)
_cell_formula_units_Z            2
_cell_length_a                   19.4205(9)
_cell_length_b                   20.0866(11)
_cell_length_c                   34.3463(17)
_cell_measurement_reflns_used    9684
_cell_measurement_temperature    99.91
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.34
_cell_volume                     12624.8(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.91
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            120789
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.818
_diffrn_reflns_theta_max         24.818
_diffrn_reflns_theta_min         2.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             5244
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.888
_exptl_transmission_factor_min   0.807
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3037
_refine_ls_number_reflns         43028
_refine_ls_number_restraints     1400
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1403P)^2^+42.7825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.3098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24399
_reflns_number_total             43028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01630g2.cif
_cod_data_source_block           1
_cod_database_code               7713746
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
;
1. Shared sites
{S5, C195}
{O20, F9}
{O21, F17}
{O22, F19}
2. Restrained distances
 O23-C49
 1.42 with sigma of 0.01
 O23-C199
 1.42 with sigma of 0.02
 C99-C49
 1.54 with sigma of 0.02
 C49-C199
 2.4 with sigma of 0.02
 C193-F12 = C97-F10 = C97-F8 = F13-C191 = F11-C191 = F20-C191 = F2-C95 = F15-C95
 1.35 with sigma of 0.02
 O13-S6
 1.4 with sigma of 0.02
 C25-C199
 1.54 with sigma of 0.02
 N62-C183
 2.5 with sigma of 0.02
 C183-N62
 2.25 with sigma of 0.02
 C81-C133 = C81-C183 = N62-C133 = N62-N70 = N70-C183
 1.4 with sigma of 0.02
 C95-S2
 1.8 with sigma of 0.02
 O19-C95
 2.6 with sigma of 0.02
 S2-O19
 1.42 with sigma of 0.02
 S3-O14
 1.4 with sigma of 0.02
 F3-C14
 1.35 with sigma of 0.02
 O14-C14
 2.2 with sigma of 0.02
 F20-F13
 2.2 with sigma of 0.02
 F13-C14
 1.37 with sigma of 0.02
 O24-C203
 1.42 with sigma of 0.02
 O24-C101
 1.42 with sigma of 0.02
 O6-O14
 2.4 with sigma of 0.02
 S3-O6
 1.42 with sigma of 0.02
 S3-C14
 1.75 with sigma of 0.02
 C188-C108
 1.5 with sigma of 0.02
 O3-C200 = O3-C188
 1.42 with sigma of 0.02
 S2-C95
 1.82 with sigma of 0.02
 F2-C95 = F15-C95
 1.35 with sigma of 0.02
 S2-O19 = S2-O25 = S2-O18
 1.42 with sigma of 0.02
 S1-O9 = S1-O8 = S1-O7
 1.42 with sigma of 0.02
 F1-C189 = F4-C189 = F6-C189
 1.35 with sigma of 0.02
 S1-C189
 1.82 with sigma of 0.02
 C14-F5
 1.35 with sigma of 0.02
 N43-C27 = C27-C155 = N71-C83
 1.35 with sigma of 0.02
 C83-C155
 1.4 with sigma of 0.02
 C131-C169
 1.4 with sigma of 0.02
 N58-B2
 1.45 with sigma of 0.02
 N69-N58
 1.32 with sigma of 0.02
 N41-C159 = C159-C115 = N76-C129
 1.35 with sigma of 0.02
 C129-C115
 1.43 with sigma of 0.02
 N41-B3
 1.45 with sigma of 0.02
 C184-N54
 1.35 with sigma of 0.02
 N72-N54
 1.32 with sigma of 0.02
 N54-C184 = N72-C87
 1.35 with sigma of 0.02
 N54-C184
 1.35 with sigma of 0.02
 N58-C39 = C169-C39 = N69-C131
 1.35 with sigma of 0.02
 N62-C133 = N70-C183 = C183-C81
 1.35 with sigma of 0.02
 C133-C81
 1.4 with sigma of 0.02
 C183-C81 = N70-C183 = N62-C133
 1.35 with sigma of 0.02
 C116-C114
 1.39 with sigma of 0.02
 C116-C120 = C114-C112 = C110-C112 = C122-C110
 1.39 with sigma of 0.02
 C90-C94 = C88-C108 = C102-C108 = C100-C94
 1.39 with sigma of 0.02
 C90-C94 = C100-C94
 1.39 with sigma of 0.01
 C179-C121
 1.5 with sigma of 0.02
 C137-N33
 1.35 with sigma of 0.02
 N68-N33 = N68-C210
 1.35 with sigma of 0.01
 C210-C143
 1.4 with sigma of 0.01
 F7-C95
 1.35 with sigma of 0.02
 O4-C43
 1.42 with sigma of 0.02
 S3-C191
 1.82 with sigma of 0.01
 C197-C199 = C25-C101
 1.54 with sigma of 0.02
 C43-C118
 1.5 with sigma of 0.02
 C184-C119
 1.35 with sigma of 0.01
 N41-N76
 1.32 with sigma of 0.02
 N70-N61
 1.32 with sigma of 0.02
 N70-N62 = N70-N61
 1.32 with sigma of 0.01
 N70-N62
 1.32 with sigma of 0.001
 N62-C133
 1.35 with sigma of 0.01
 N70-C183
 1.35 with sigma of 0.02
 O5-C17 = O5-C180
 1.42 with sigma of 0.01
 O5-C180
 1.42 with sigma of 0.001
 S3-O16 = S3-O14 = S3-O6 = S3-O17 = S3-O15
 1.42 with sigma of 0.02
 C201-C203
 1.54 with sigma of 0.01
 C25-C101
 1.54 with sigma of 0.01
 O24-C101 = O24-C203
 1.42 with sigma of 0.01
 C141-C35
 1.45 with sigma of 0.01
 S4-O10 = S6-O10 = S6-O12 = S4-O12
 1.42 with sigma of 0.01
 C75-C29
 1.4 with sigma of 0.01
 O4-C121
 1.42 with sigma of 0.01
 F10-S4
 2.4 with sigma of 0.04
 S4-F10
 2.6 with sigma of 0.04
 N61-C29
 2.3 with sigma of 0.04
 C165-C75
 2.3 with sigma of 0.04
 N70-C75
 2.3 with sigma of 0.04
 C169-N58
 2.25 with sigma of 0.04
 C39-C131
 2.25 with sigma of 0.04
 N69-C39
 2.25 with sigma of 0.04
 C27-N71
 2.25 with sigma of 0.04
 C159-C129
 2.25 with sigma of 0.04
 N54-C119
 2.25 with sigma of 0.04
 N54-C87
 2.25 with sigma of 0.04
 C184-C87
 2.3 with sigma of 0.04
 C184-N72
 2.3 with sigma of 0.04
 C155-N71
 2.25 with sigma of 0.04
 N58-C169
 2.25 with sigma of 0.04
 C131-N58
 2.25 with sigma of 0.04
 C39-N69
 2.25 with sigma of 0.04
 N62-C81
 2.25 with sigma of 0.04
 C183-C133
 2.25 with sigma of 0.04
 C81-N70
 2.25 with sigma of 0.04
 N70-C133
 2.25 with sigma of 0.04
 C112-C120
 2.78 with sigma of 0.04
 C122-C114
 2.78 with sigma of 0.04
 C110-C116
 2.78 with sigma of 0.04
 C116-C112
 2.408 with sigma of 0.04
 C122-C116
 2.408 with sigma of 0.04
 C122-C112
 2.408 with sigma of 0.04
 C110-C124
 2.408 with sigma of 0.04
 C112-C122
 2.408 with sigma of 0.04
 C94-C108
 2.78 with sigma of 0.04
 C100-C88
 2.78 with sigma of 0.04
 C100-C90
 2.408 with sigma of 0.04
 C100-C108
 2.408 with sigma of 0.04
 C116-C43
 2.8 with sigma of 0.04
 C201-O24
 2.45 with sigma of 0.04
 F13-F5
 2.45 with sigma of 0.04
 F5-F3
 2.4 with sigma of 0.04
 F13-F3
 2.4 with sigma of 0.04
 C119-N72
 2.25 with sigma of 0.01
 C29-N61
 2.25 with sigma of 0.01
 C133-N70
 2.25 with sigma of 0.01
 N70-C81
 2.25 with sigma of 0.01
 F5-S3
 2.5 with sigma of 0.04
 O6-C191
 2.5 with sigma of 0.04
 O17-C14
 2.5 with sigma of 0.04
 O16-C191
 2.5 with sigma of 0.04
 O14-C14
 2.5 with sigma of 0.04
 O17-O14
 2.4 with sigma of 0.04
 C101-C203
 2.4 with sigma of 0.04
 O24-C25
 2.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O23 \\sim C49 \\sim C99 \\sim C197 \\sim C199 \\sim O24 \\sim C25 \\sim C101
\\sim C201 \\sim C203: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
S1 \\sim F1 \\sim F4 \\sim F6 \\sim O7 \\sim O8 \\sim O9 \\sim C189: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N41 \\sim N76 \\sim C115 \\sim C129 \\sim C159: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N58 \\sim N69 \\sim C39 \\sim C131 \\sim C169: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N70 \\sim N62 \\sim C81 \\sim C133 \\sim C183: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C126 \\sim C128 \\sim C130 \\sim C132 \\sim C134 \\sim C136: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O10 \\sim O12 \\sim S4 \\sim F8 \\sim F10 \\sim F14 \\sim O11 \\sim C97 \\sim
S6 \\sim F12 \\sim F16 \\sim F18 \\sim O13 \\sim C193: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C82 \\sim C90 \\sim C92 \\sim C94 \\sim C96 \\sim C98 \\sim C100 \\sim C102
\\sim C104 \\sim C106 \\sim C108 \\sim C188 \\sim C43 \\sim C110 \\sim C112
\\sim C114 \\sim C116 \\sim C118 \\sim C120 \\sim C122 \\sim C124 \\sim C126
\\sim C128 \\sim C130 \\sim C132 \\sim C134 \\sim C136: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
N58 \\sim N69 \\sim C39 \\sim C131 \\sim C169 \\sim N43 \\sim N71 \\sim C27
\\sim C83 \\sim C155: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N54 \\sim N72 \\sim C87 \\sim C119 \\sim C184: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N33 \\sim N68 \\sim C137 \\sim C143 \\sim C210 \\sim B3 \\sim N41 \\sim N76
\\sim C115 \\sim C129 \\sim C159: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
S3 \\sim F13 \\sim O15 \\sim F3 \\sim F5 \\sim O14 \\sim C14 \\sim F11 \\sim
F20 \\sim O6 \\sim C191: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
S3 \\sim F13 \\sim O15 \\sim F3 \\sim F5 \\sim O14 \\sim O17 \\sim C14 \\sim
F11 \\sim F20 \\sim O6 \\sim O16 \\sim C191: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C121) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C116) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N72) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(B3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C143) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S5) = Uanis(C195)
Uanis(O22) = Uanis(F19)
Uanis(O21) = Uanis(F17)
Uanis(O20) = Uanis(F9)
4. Others
 Fixed Sof: O3(0.7) N41(0.6) N58(0.4) N61(0.6) N69(0.4) N76(0.6) C29(0.6)
 H29(0.6) C39(0.4) H39(0.4) C75(0.6) H75(0.6) C82(0.7) H82(0.7) C84(0.7)
 H84(0.7) C86(0.7) H86(0.7) C88(0.7) C90(0.7) C92(0.7) H92(0.7) C94(0.7)
 H94(0.7) C96(0.7) H96(0.7) C98(0.7) H98(0.7) C100(0.7) C102(0.7) C104(0.7)
 H104(0.7) C106(0.7) H106(0.7) C108(0.7) C115(0.6) H115(0.6) C129(0.6)
 H129(0.6) C131(0.4) H131(0.4) C159(0.6) H159(0.6) C165(0.6) H165(0.6)
 C169(0.4) H169(0.4) C188(0.7) H18C(0.7) H18D(0.7) C200(0.7) H20A(0.7)
 H20B(0.7) O4(0.3) N43(0.6) N54(0.4) N62(0.4) N71(0.6) N72(0.4) C27(0.6)
 H27(0.6) C43(0.3) H43A(0.3) H43B(0.3) C81(0.4) H81(0.4) C83(0.6) H83(0.6)
 C87(0.4) H87(0.4) C110(0.3) H110(0.3) C112(0.3) H112(0.3) C114(0.3) H114(0.3)
 C116(0.3) H116(0.3) C118(0.3) C120(0.3) C122(0.3) C124(0.3) H124(0.3)
 C126(0.3) C128(0.3) C130(0.3) H130(0.3) C132(0.3) H132(0.3) C134(0.3)
 H134(0.3) C136(0.3) H136(0.3) C119(0.4) H119(0.4) C121(0.3) H12A(0.3)
 H12B(0.3) C133(0.4) H133(0.4) C155(0.6) H155(0.6) C183(0.4) H183(0.4)
 C184(0.4) H184(0.4) S3(0.5) F13(0.5) O15(0.5) S4(0.5) S5(0.5) F3(0.2) F5(0.2)
 F8(0.5) F10(0.5) F14(0.5) O11(0.5) O14(0.2) O17(0.2) O20(0.5) O21(0.5)
 O22(0.5) O23(0.6) C14(0.2) C49(0.6) HF(0.6) HG(0.6) C97(0.5) C99(0.6) HH(0.6)
 HI(0.6) HJ(0.6) C197(0.6) HK(0.6) HL(0.6) HM(0.6) C199(0.6) HN(0.6) HO(0.6)
 S6(0.5) F9(0.5) F11(0.3) F12(0.5) F16(0.5) F17(0.5) F18(0.5) F19(0.5) F20(0.3)
 O6(0.3) O13(0.5) O16(0.3) O24(0.4) C25(0.4) HP(0.4) HQ(0.4) HR(0.4) C101(0.4)
 HS(0.4) HT(0.4) C191(0.3) C193(0.5) C195(0.5) C201(0.4) HU(0.4) HV(0.4)
 HW(0.4) C203(0.4) HX(0.4) HY(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C22(H22A,H22B), C47(H47A,H47B), C161(H16A,H16B), C180(H18A,
 H18B), C212(H21A,H21B), C188(H18C,H18D), C200(H20A,H20B), C43(H43A,H43B),
 C121(H12A,H12B), C49(HF,HG), C199(HN,HO), C101(HS,HT), C203(HX,HY)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C23(H23),
 C24(H24), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C37(H37), C38(H38), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
 C48(H48), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C69(H69),
 C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C79(H79),
  C85(H85), C89(H89), C93(H93), C107(H107), C109(H109), C111(H111), C113(H113),
 C117(H117), C125(H125), C127(H127), C135(H135), C137(H137), C139(H139),
 C140(H140), C141(H141), C142(H142), C143(H143), C144(H144), C145(H145),
 C146(H146), C147(H147), C149(H149), C150(H150), C151(H151), C153(H153),
 C154(H154), C156(H156), C157(H157), C158(H158), C160(H160), C163(H163),
 C166(H166), C167(H167), C168(H168), C170(H170), C171(H171), C172(H172),
 C173(H173), C174(H174), C175(H175), C176(H176), C177(H177), C178(H178),
 C181(H181), C182(H182), C186(H186), C187(H187), C190(H190), C192(H192),
 C194(H194), C196(H196), C198(H198), C202(H202), C204(H204), C206(H206),
 C208(H208), C210(H210), C29(H29), C39(H39), C75(H75), C82(H82), C84(H84),
 C86(H86), C92(H92), C94(H94), C96(H96), C98(H98), C104(H104), C106(H106),
 C115(H115), C129(H129), C131(H131), C159(H159), C165(H165), C169(H169),
 C27(H27), C81(H81), C83(H83), C87(H87), C110(H110), C112(H112), C114(H114),
 C116(H116), C124(H124), C130(H130), C132(H132), C134(H134), C136(H136),
 C119(H119), C133(H133), C155(H155), C183(H183), C184(H184)
5.c Fitted hexagon refined as free rotating group:
 C82(C84,C86,C88,C90,C92), C96(C98,C100,C102,C104,C106)
5.d Naphthalene refined as free rotating group:
 C118(C120,C122,C124,C126,C128,C130,C132,C134,C136)
5.e Idealised Me refined as rotating group:
 C19(H,HA,HB), C105(HC,HD,HE), C99(HH,HI,HJ), C197(HK,HL,HM), C25(HP,HQ,HR),
 C201(HU,HV,HW)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 809 electrons were 
found in a volume of 3631\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
6[C2H3N], 6[C4H10O] per Asymmetric Unit 
which account for 768 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76291
_shelx_fab_checksum              41848
_olex2_submission_special_instructions 'No special instructions were received'