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_7713747
_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, 7(C F3 O3 S), C4 H10 O, 4(C2 H3 N), 2.5(C8 H20 N), 0.5(C8 N), [C2H3N], [C4H10O]'
_chemical_formula_sum            'C213 H221 B4 Co4 F21 Fe4 N76 O27 S7'
_chemical_formula_weight         5403.42
_chemical_name_systematic
'[NEt4]3[(pzTp)Fe(CN)3Co(TpEtOAn)]4[OTf]7.5MeCN.2Et2O'
_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                96.0810(10)
_cell_angle_beta                 91.5700(10)
_cell_angle_gamma                100.7960(10)
_cell_formula_units_Z            2
_cell_length_a                   18.6217(8)
_cell_length_b                   20.0661(7)
_cell_length_c                   36.4748(14)
_cell_measurement_reflns_used    9618
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.25
_cell_volume                     13297.2(9)
_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 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      109.89
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0873
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            153765
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.804
_diffrn_reflns_theta_max         24.803
_diffrn_reflns_theta_min         2.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.761
_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    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3916
_refine_ls_number_reflns         45483
_refine_ls_number_restraints     2393
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1747P)^2^+27.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2513
_refine_ls_wR_factor_ref         0.2950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30546
_reflns_number_total             45483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01630g2.cif
_cod_data_source_block           2
_cod_database_code               7713747
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Shared sites
{F99, O32}
2. Restrained distances
 F13-C240
 1.3 with sigma of 0.02
 C235-N37
 1.47 with sigma of 0.02
 N57-C191 = N37-C115 = N37-C117 = N37-C115
 1.47 with sigma of 0.02
 O4-C82 = S5-O17 = S10-O11 = C189-N57 = S2-O25
 1.42 with sigma of 0.02
 N37-C130
 1.47 with sigma of 0.01
 C229-C115 = C189-C195 = C119-C235 = C231-C130 = C185-C85 = C117-C233
 1.5 with sigma of 0.02
 F3-C240
 1.32 with sigma of 0.02
 C97-C193 = C144-C191
 1.5 with sigma of 0.02
 C227-F19 = F25-C240 = F7-C239 = F15-C239 = C239-F29 = C125-F26 = F27-C237
 1.35 with sigma of 0.02
 C125-F17 = C223-F23 = F11-C223 = F30-C150 = F28-C150 = F2-C150
 1.35 with sigma of 0.02
 S11-O31
 1.37 with sigma of 0.02
 C133-C171 = N72-C133 = S5-O33
 1.4 with sigma of 0.02
 O4-C91 = N57-C97 = S11-O8 = N57-C95 = S9-O29 = S9-O7 = S9-O19 = S11-O19
 1.42 with sigma of 0.02
 C91-C143 = C193-C97
 1.54 with sigma of 0.02
 S5-C239
 1.75 with sigma of 0.02
 S9-C227 = S10-C125 = S2-C125 = C237-S2
 1.8 with sigma of 0.02
 N54-C155
 1.47 with sigma of 0.01
 O2-C128
 1.42 with sigma of 0.001
 O26-C183
 1.42 with sigma of 0.001
 C187-C183 = C161-C151
 1.54 with sigma of 0.01
 O26-C161
 1.42 with sigma of 0.001
 N37-C235
 1.45 with sigma of 0.01
 C231-C130
 1.54 with sigma of 0.01
 C229-C115
 1.54 with sigma of 0.01
 C79A-C1B = C266-C1D
 1.53 with sigma of 0.02
 N54A-C79A = N54A-C266 = N54A-C85A = N54A-C1A
 1.45 with sigma of 0.02
 O21-S7
 1.42 with sigma of 0.02
 O93-S12
 1.42 with sigma of 0.02
 S12-O9
 1.42 with sigma of 0.02
 F76-C250
 1.35 with sigma of 0.02
 F32-C250
 1.35 with sigma of 0.02
 F99-C250
 1.35 with sigma of 0.02
 S13-O27
 1.42 with sigma of 0.02
 O18-S13
 1.42 with sigma of 0.02
 N60-C101 = N78-C241 = N60-C99 = N60-C80 = N78-C201 = N60-C69 = N78-C247 = N78-
 C243
 1.45 with sigma of 0.02
 C255-C241 = C141-C101 = C80-C123 = C99-C180 = C245-C243 = C259-C247 = C201-
 C199 = C69-C121
 1.53 with sigma of 0.02
 O35-O17
 2.4 with sigma of 0.02
 C95-C222
 1.53 with sigma of 0.01
 S5-O35 = S5-O33
 1.42 with sigma of 0.01
 O1-C232
 1.44 with sigma of 0.01
 O1-C212
 1.42 with sigma of 0.01
 O3-C82 = O3-C105
 1.42 with sigma of 0.01
 S11-O19 = S9-O19
 1.42 with sigma of 0.02
 S8-O9 = S12-O9 = S8-O16 = S12-O16
 1.42 with sigma of 0.02
 N35-C213 = N72-N35 = N58-N35 = N46-N34 = N71-N34 = N34-C192
 1.37 with sigma of 0.02
 C235-C115 = C97-C191 = C117-C130
 2.2 with sigma of 0.04
 O29-O19 = O33-O35 = F15-F29 = F29-F7
 2.3 with sigma of 0.04
 O7-O29 = C125-O25 = O17-C239 = F15-S5 = F29-S5
 2.4 with sigma of 0.04
 C230-C133 = C221-C158 = F5-F19 = F3-C193
 2.2 with sigma of 0.04
 N57-C193 = C239-O35 = O33-C239 = F7-S5
 2.5 with sigma of 0.04
 C119-N37
 2.68 with sigma of 0.01
 C231-N37
 2.7 with sigma of 0.01
 N37-C229
 2.7 with sigma of 0.01
 C115-C235
 2.4 with sigma of 0.04
 C266-C79A
 2.4 with sigma of 0.04
 O21-C150
 2.6 with sigma of 0.04
 O93-O9
 2.45 with sigma of 0.04
 O93-C250
 2.6 with sigma of 0.04
 F76-S12
 2.6 with sigma of 0.04
 C250-O9
 2.5 with sigma of 0.04
 F76-O32
 2.4 with sigma of 0.04
 F99-F76
 2.4 with sigma of 0.04
 F32-S12
 2.6 with sigma of 0.04
 F99-F32
 2.4 with sigma of 0.04
 F23-F11
 2.45 with sigma of 0.04
 O27-C223
 2.6 with sigma of 0.04
 O18-C223
 2.5 with sigma of 0.04
 F25-S11
 2.5 with sigma of 0.04
 S11-F25
 2.7 with sigma of 0.04
 O33-O35
 2.5 with sigma of 0.04
 O17-O35
 2.5 with sigma of 0.04
 C85-C155 \\sim C85A-C266
 with sigma of 0.04
 C164-C210 \\sim C1A-C1E
 with sigma of 0.02
 C85-C164 \\sim C85A-C1A
 with sigma of 0.04
 C155-C173 \\sim C266-C1D
 with sigma of 0.02
 N54-C155 \\sim N54A-C266
 with sigma of 0.02
 N54-C79 \\sim N54A-C79A
 with sigma of 0.02
 N54-C85 \\sim N54A-C85A
 with sigma of 0.02
 N54-C164 \\sim N54A-C1A
 with sigma of 0.02
 C155-C164 \\sim C266-C1A
 with sigma of 0.04
 N54-C169 \\sim N54A-C1B
 with sigma of 0.04
 N54-C173 \\sim N54A-C1D
 with sigma of 0.04
 N54-C185 \\sim N54A-C1C
 with sigma of 0.04
 N54-C210 \\sim N54A-C1E
 with sigma of 0.04
 C79-C169 \\sim C79A-C1B
 with sigma of 0.02
 C79-C85 \\sim C79A-C85A
 with sigma of 0.04
 C79-C155 \\sim C79A-C266
 with sigma of 0.04
 C85-C185 \\sim C85A-C1C
 with sigma of 0.02
 C79-C164 \\sim C79A-C1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N37 \\sim C115 \\sim C117 \\sim C130 \\sim C229 \\sim C231 \\sim C233 \\sim
C235: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
F26 \\sim F31 \\sim O11 \\sim O24 \\sim S2 \\sim F27 \\sim O25 \\sim C237 \\sim
S10 \\sim F17 \\sim O36 \\sim C125: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
S7 \\sim F2 \\sim F28 \\sim F30 \\sim O15 \\sim O21 \\sim O23 \\sim C150:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F26 \\sim F31 \\sim O11 \\sim O24 \\sim S2 \\sim O25 \\sim S10 \\sim F17 \\sim
O36 \\sim C125: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O19 \\sim S9 \\sim F5 \\sim F9 \\sim F19 \\sim O7 \\sim O29 \\sim C227 \\sim
S11 \\sim F3 \\sim F13 \\sim F25 \\sim O8 \\sim O31 \\sim C240: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N41 \\sim N80 \\sim C87 \\sim C94 \\sim C175 \\sim N40 \\sim N84 \\sim C160
\\sim C215 \\sim C217: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N57 \\sim C95 \\sim C97 \\sim C144 \\sim C189 \\sim C191 \\sim C193 \\sim C195
\\sim C222: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C158 \\sim C73 \\sim C135 \\sim C111 \\sim C221: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O3 \\sim N46 \\sim N58 \\sim N81 \\sim C103 \\sim C105 \\sim C107 \\sim C118
\\sim C134 \\sim C205 \\sim C207 \\sim C209 \\sim C211 \\sim C213 \\sim C244
\\sim O4 \\sim N71 \\sim N72 \\sim N77 \\sim C71 \\sim C91 \\sim C93 \\sim C129
\\sim C133 \\sim C143 \\sim C171 \\sim C179 \\sim C192 \\sim C230 \\sim C236:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N39 \\sim N75 \\sim C81 \\sim C110 \\sim C181 \\sim N59 \\sim N38 \\sim C109
\\sim C196 \\sim C219: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N54A \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C79A \\sim C85A
\\sim C266: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
N54 \\sim C79 \\sim C85 \\sim C155 \\sim C164 \\sim C169 \\sim C173 \\sim C185
\\sim C210 \\sim N54A \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim
C79A \\sim C85A \\sim C266: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O9 \\sim O16 \\sim S8 \\sim F14 \\sim F20 \\sim F24 \\sim O32 \\sim C188 \\sim
S12 \\sim F76 \\sim F99 \\sim O93 \\sim C250: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O9 \\sim O16 \\sim S8 \\sim F14 \\sim F20 \\sim F24 \\sim O32 \\sim C188 \\sim
S12 \\sim F32 \\sim F76 \\sim F99 \\sim O93 \\sim C250: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
S13 \\sim F11 \\sim F23 \\sim F266 \\sim O18 \\sim O27 \\sim O37 \\sim C223:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N60 \\sim C69 \\sim C80 \\sim C99 \\sim C101 \\sim C121 \\sim C123 \\sim C141
\\sim C180 \\sim N78 \\sim C201 \\sim C241 \\sim C243 \\sim C245 \\sim C247
\\sim C255 \\sim C259: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N37 \\sim C115 \\sim C117 \\sim C119 \\sim C130 \\sim C229 \\sim C231 \\sim
C233 \\sim C235: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
S5 \\sim F7 \\sim F15 \\sim F29 \\sim O17 \\sim O33 \\sim O35 \\sim C239:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(N56) \\sim Ueq, Uanis(S11) \\sim Ueq, Uanis(S9) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C240) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C169)
\\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(N54) \\sim Ueq, Uanis(F7) \\sim Ueq,
Uanis(F29) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(C239) \\sim Ueq, Uanis(S5)
\\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(F23) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C119) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C231) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(F19) \\sim Ueq,
Uanis(F9) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(C227) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C217) \\sim Ueq, Uanis(N80) \\sim Ueq, Uanis(S9) \\sim Ueq, Uanis(F19)
\\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C164) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C213) \\sim Ueq, Uanis(C230) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F99) = Uanis(O32)
4. Others
 Sof(N54A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=
 Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(H1EC)=Sof(C79A)=Sof(H79C)=Sof(H79D)=Sof(C85A)=
 Sof(H85C)=Sof(H85D)=Sof(C266)=Sof(H26A)=Sof(H26B)=1-FVAR(1)
 Sof(N54)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C155)=
 Sof(H15B)=Sof(H15C)=Sof(C164)=Sof(H16A)=Sof(H16B)=Sof(C169)=Sof(H16C)=
 Sof(H16D)=Sof(H16E)=Sof(C173)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C185)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C210)=Sof(H21C)=Sof(H21D)=Sof(H21E)=FVAR(1)
 Fixed Sof: H82C(0.5) H82D(0.5) H82A(0.5) H82B(0.5) H158(0.5) H15A(0.5)
 O3(0.5) N39(0.5) N41(0.5) N80(0.5) C87(0.5) H87(0.5) C175(0.5) H175(0.5)
 C94(0.5) H94(0.5) N46(0.5) N58(0.5) N75(0.5) N81(0.5) C73(0.5) H73(0.5)
 C81(0.5) H81(0.5) C103(0.5) H103(0.5) C105(0.5) H10A(0.5) H10B(0.5) C107(0.5)
 H107(0.5) C110(0.5) H110(0.5) C118(0.5) H118(0.5) C134(0.5) H134(0.5)
 C135(0.5) H135(0.5) C181(0.5) H181(0.5) C205(0.5) H205(0.5) C207(0.5)
 H207(0.5) C209(0.5) C211(0.5) H211(0.5) C213(0.5) H213(0.5) C244(0.5)
 H244(0.5) O4(0.5) N59(0.5) N71(0.5) N72(0.5) N77(0.5) N38(0.5) C71(0.5)
 H71(0.5) C91(0.5) H91A(0.5) H91B(0.5) C93(0.5) H93(0.5) C109(0.5) H109(0.5)
 C111(0.5) H111(0.5) C129(0.5) H129(0.5) C133(0.5) H133(0.5) C143(0.5)
 C171(0.5) H171(0.5) C179(0.5) H179(0.5) C192(0.5) H192(0.5) C196(0.5)
 H196(0.5) C215(0.5) H215(0.5) C160(0.5) H160(0.5) N40(0.5) N84(0.5) C217(0.5)
 H217(0.5) C219(0.5) H219(0.5) C221(0.5) H221(0.5) C230(0.5) H230(0.5)
 C236(0.5) H236(0.5) S2(0.3) F27(0.3) O25(0.3) C237(0.3) S10(0.7) F17(0.7)
 O36(0.7) C125(0.7) S8(0.8) F14(0.8) F20(0.8) F24(0.8) O32(0.8) C188(0.8)
 S12(0.2) F32(0.2) F76(0.2) F99(0.2) O93(0.2) C250(0.2) O19(0.5) S9(0.25)
 F5(0.25) F9(0.25) F19(0.25) O7(0.25) O29(0.25) C227(0.25) S11(0.25) F3(0.25)
 F13(0.25) F25(0.25) O8(0.25) O31(0.25) C240(0.25) S7(0.5) F2(0.5) F28(0.5)
 F30(0.5) O15(0.5) O21(0.5) O23(0.5) C150(0.5) N60(0.5) C69(0.5) H69A(0.5)
 H69B(0.5) C80(0.5) H80A(0.5) H80B(0.5) C99(0.5) H99A(0.5) H99B(0.5) C101(0.5)
 H10C(0.5) H10D(0.5) C121(0.5) H12C(0.5) H12D(0.5) H12E(0.5) C123(0.5)
 H12F(0.5) H12G(0.5) H12H(0.5) C141(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C180(0.5) H18D(0.5) H18E(0.5) H18F(0.5) S5(0.5) F7(0.5) F15(0.5) F29(0.5)
 O17(0.5) O33(0.5) O35(0.5) C239(0.5) S13(0.5) F11(0.5) F23(0.5) F266(0.5)
 O18(0.5) O27(0.5) O37(0.5) C223(0.5) N78(0.5) C199(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C201(0.5) H20A(0.5) H20B(0.5) C241(0.5) H24A(0.5) H24B(0.5)
 C243(0.5) H24C(0.5) H24D(0.5) C245(0.5) H24E(0.5) H24F(0.5) H24G(0.5)
 C247(0.5) H24H(0.5) H24I(0.5) C255(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 C259(0.5) H25D(0.5) H25E(0.5) H25F(0.5) N57(0.5) C95(0.5) H95A(0.5) H95B(0.5)
 C97(0.5) H97A(0.5) H97B(0.5) C144(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C189(0.5)
 H18G(0.5) H18H(0.5) C191(0.5) H19D(0.5) H19E(0.5) C193(0.5) H19F(0.5)
 H19G(0.5) H19H(0.5) C195(0.5) H19I(0.5) H19J(0.5) H19K(0.5) C222(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) N37(0.5) C115(0.5) C117(0.5) C119(0.5) C130(0.5)
 C229(0.5) C231(0.5) C233(0.5) C235(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C82(H82C,H82D), C82(H82A,H82B), C88(H88A,H88B), C98(H98A,
 H98B), C128(H12A,H12B), C212(H21A,H21B), C232(H23A,H23B), C105(H10A,H10B),
 C91(H91A,H91B), C161(H16F,H16G), C183(H18I,H18J), C79(H79A,H79B), C85(H85A,
 H85B), C155(H15B,H15C), C164(H16A,H16B), C69(H69A,H69B), C80(H80A,H80B),
 C99(H99A,H99B), C101(H10C,H10D), C1A(H1AA,H1AB), C79A(H79C,H79D), C85A(H85C,
 H85D), C266(H26A,H26B), C201(H20A,H20B), C241(H24A,H24B), C243(H24C,H24D),
 C247(H24H,H24I), C95(H95A,H95B), C97(H97A,H97B), C189(H18G,H18H), C191(H19D,
 H19E)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C22(H22),
 C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C35(H35),
  C36(H36), C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C45(H45),
 C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C56(H56), C57(H57), C58(H58),
  C59(H59), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C70(H70),
 C72(H72), C76(H76), C77(H77), C78(H78), C83(H83), C84(H84), C86(H86), C90(H90),
  C92(H92), C96(H96), C100(H100), C102(H102), C104(H104), C106(H106),
 C108(H108), C112(H112), C114(H114), C116(H116), C120(H120), C122(H122),
 C124(H124), C126(H126), C127(H127), C131(H131), C132(H132), C138(H138),
 C140(H140), C142(H142), C145(H145), C146(H146), C147(H147), C148(H148),
 C149(H149), C152(H152), C154(H154), C156(H156), C157(H157), C158(H158),
 C158(H15A), C159(H159), C162(H162), C163(H163), C165(H165), C166(H166),
 C167(H167), C168(H168), C172(H172), C174(H174), C176(H176), C178(H178),
 C182(H182), C184(H184), C190(H190), C194(H194), C200(H200), C202(H202),
 C204(H204), C206(H206), C208(H208), C214(H214), C216(H216), C220(H220),
 C224(H224), C234(H234), C238(H238), C242(H242), C248(H248), C87(H87),
 C175(H175), C94(H94), C73(H73), C81(H81), C103(H103), C107(H107), C110(H110),
 C118(H118), C134(H134), C135(H135), C181(H181), C205(H205), C207(H207),
 C211(H211), C213(H213), C244(H244), C71(H71), C93(H93), C109(H109), C111(H111),
  C129(H129), C133(H133), C171(H171), C179(H179), C192(H192), C196(H196),
 C215(H215), C160(H160), C217(H217), C219(H219), C221(H221), C230(H230),
 C236(H236)
5.c Fitted pentagon refined as free rotating group:
 N41(N80,C87,C175,C94), C215(C160,N40,N84,C217)
5.d Idealised Me refined as rotating group:
 C151(H15D,H15E,H15F), C187(H18K,H18L,H18M), C137(H13A,H13B,H13C), C246(H24J,
 H24K,H24L), C228(H22D,H22E,H22F), C89(H89A,H89B,H89C), C169(H16C,H16D,H16E),
 C173(H17A,H17B,H17C), C185(H18A,H18B,H18C), C210(H21C,H21D,H21E), C121(H12C,
 H12D,H12E), C123(H12F,H12G,H12H), C141(H14A,H14B,H14C), C180(H18D,H18E,H18F),
 C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,
 H1EC), C199(H19A,H19B,H19C), C245(H24E,H24F,H24G), C255(H25A,H25B,H25C),
 C259(H25D,H25E,H25F), C144(H14D,H14E,H14F), C193(H19F,H19G,H19H), C195(H19I,
 H19J,H19K), C222(H22A,H22B,H22C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 141 electrons were 
found in a volume of 1127\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1[C2H3N], 1[C4H10O] per Asymmetric Unit 
which account for 128 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53212
_shelx_fab_checksum              61648
_olex2_submission_special_instructions 'No special instructions were received'