Strong upconverted circularly polarized emission from a chiral tetrahedral Yb/Eu cage.
Yao, Zhiwei; Gao, Ting; Yan, Pengfei; Zhou, Yanyan; Li, Hongfeng; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5731–5738; doi:10.1039/d5dt00219b

data_7718277
_publ_section_title
;
 Strong upconverted circularly polarized emission from a chiral
 tetrahedral Yb/Eu cage.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5731
_journal_page_last               5738
_journal_paper_doi               10.1039/d5dt00219b
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C296 H188 F36 N4 O32 P8 Yb4, 26(C4 H8 O), 2(C6 H14), 1.2[C4H8O]'
_chemical_formula_sum            'C412 H424 F36 N4 O58 P8 Yb4'
_chemical_formula_weight         7983.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-14 deposited with the CCDC.	2025-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.292(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   43.1068(13)
_cell_length_b                   21.1124(5)
_cell_length_c                   29.4778(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.518
_cell_measurement_theta_min      2.557
_cell_volume                     20762.5(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            626320
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8224
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 19783 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0105(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3076
_refine_ls_number_reflns         47768
_refine_ls_number_restraints     2362
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+13.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                43524
_reflns_number_total             47768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00219b2.cif
_cod_data_source_block           yzw_0110
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

 Adding full bibliography for 7718277.cif.
;
_cod_original_cell_volume        20762.5(11)
_cod_database_code               7718277
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C157-C156 = C158-C157 = C159-C158 = C159-C156
 1.54 with sigma of 0.01
 C217-C216 = C218-C217 = C219-C218 = C220-C219 = C221-C220
 1.54 with sigma of 0.01
 C233-C232 = C234-C233 = C235-C234
 1.54 with sigma of 0.01
 O28-C235 = O28-C232
 1.43 with sigma of 0.01
 O31-C259 = O31-C256
 1.43 with sigma of 0.01
 C259-C258 = C258-C257 = C257-C256
 1.54 with sigma of 0.01
 C203-C202 = C202-C201 = C201-C200
 1.54 with sigma of 0.01
 O25-C203 = O25-C200
 1.43 with sigma of 0.01
 C251-C250 = C250-C249 = C249-C248
 1.54 with sigma of 0.01
 O30-C248 = O30-C251
 1.43 with sigma of 0.01
 C185-C184 = C186-C185 = C187-C186
 1.54 with sigma of 0.01
 O23-C187 = O23-C184
 1.43 with sigma of 0.01
 C211-C210 = C210-C209 = C209-C208
 1.54 with sigma of 0.01
 O26-C208 = O26-C211
 1.43 with sigma of 0.01
 C229-C228 = C230-C229 = C231-C230
 1.51 with sigma of 0.01
 O27-C231 = O27-C228
 1.43 with sigma of 0.01
 O29-C243 = O29-C240
 1.43 with sigma of 0.01
 C243-C242 = C242-C241 = C241-C240
 1.54 with sigma of 0.01
 C237-C236 = C238-C237 = C239-C238
 1.54 with sigma of 0.01
 C219-C221 = C220-C218 = C216-C218 = C217-C219
 2.515 with sigma of 0.02
 C235-C232
 2.336 with sigma of 0.02
 C235-C233 = C232-C234
 2.515 with sigma of 0.02
 C256-C258 = C259-C257
 2.515 with sigma of 0.02
 C256-C259
 2.336 with sigma of 0.02
 C200-C202 = C201-C203
 2.515 with sigma of 0.02
 O31-C258 = O31-C257
 2.426 with sigma of 0.02
 C200-C203
 2.336 with sigma of 0.02
 O30-C249 = O30-C250
 2.426 with sigma of 0.02
 C248-C250 = C251-C249
 2.515 with sigma of 0.02
 C248-C251
 2.336 with sigma of 0.02
 C187-C184
 2.336 with sigma of 0.02
 C187-C185 = C184-C186
 2.515 with sigma of 0.02
 C211-C209 = C210-C208
 2.515 with sigma of 0.02
 C208-C211
 2.336 with sigma of 0.02
 O27-C229 = O27-C230
 2.426 with sigma of 0.02
 C231-C228
 2.336 with sigma of 0.02
 C231-C229 = C230-C228
 2.515 with sigma of 0.02
 C243-C241 = C242-C240
 2.515 with sigma of 0.02
 C240-C243
 2.336 with sigma of 0.02
 C239-C237 = C236-C238
 2.515 with sigma of 0.02
 C239-C236
 2.336 with sigma of 0.02
 O28A-C237 = O28A-C238
 2.426 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C216 \\sim C217 \\sim C218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim
C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C232 \\sim C233 \\sim C234 \\sim C235 \\sim O28 \\sim C236 \\sim C237 \\sim
C238 \\sim C239 \\sim O28A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C200 \\sim C201 \\sim C202 \\sim C203 \\sim O25 \\sim C204 \\sim C205 \\sim
C206 \\sim C207 \\sim O25A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C252 \\sim C253 \\sim C254 \\sim C255 \\sim O30A \\sim C248 \\sim C249 \\sim
C250 \\sim C251 \\sim O30: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C260 \\sim C261 \\sim C262 \\sim C263 \\sim O31A \\sim C256 \\sim C257 \\sim
C258 \\sim C259 \\sim O31: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C240 \\sim C241 \\sim C242 \\sim C243 \\sim O29 \\sim C244 \\sim C245 \\sim
C246 \\sim C247 \\sim O29A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C228 \\sim C229 \\sim C230 \\sim C231 \\sim O27: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C208 \\sim C209 \\sim C210 \\sim C211 \\sim O26 \\sim C212 \\sim C213 \\sim
C214 \\sim C215 \\sim O26A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C192 \\sim C193 \\sim C194 \\sim C195 \\sim O24 \\sim C196 \\sim C197 \\sim
C198 \\sim C199 \\sim O24A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C137 \\sim C138 \\sim F13 \\sim F14 \\sim F15 \\sim C150 \\sim F13A \\sim F14A
\\sim F15A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O21 \\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim
C174 \\sim C175: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C117 \\sim C118 \\sim F7 \\sim F8 \\sim F9 \\sim C149 \\sim F7A \\sim F8A \\sim
F9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C184 \\sim C185 \\sim C186 \\sim C187 \\sim O23 \\sim C188 \\sim C189 \\sim
C190 \\sim C191 \\sim O23A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C128 \\sim F10 \\sim F11 \\sim F12 \\sim F10A \\sim F11A \\sim F12A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C155 \\sim C156 \\sim C158 \\sim O18 \\sim C157 \\sim C159: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C108 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O22 \\sim C176 \\sim C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181 \\sim
C182 \\sim C183: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O25A) \\sim Ueq, Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq,
Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq, Uanis(C203) \\sim Ueq,
Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(C202)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(C128)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F10A) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12A) \\sim Ueq,
Uanis(C138) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(C150) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14A) \\sim Ueq,
Uanis(F15A) \\sim Ueq, Uanis(C255) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(F10A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C262) \\sim Ueq, Uanis(C263) \\sim Ueq, Uanis(O31A) \\sim Ueq,
Uanis(C260) \\sim Ueq, Uanis(C261) \\sim Ueq, Uanis(C258) \\sim Ueq,
Uanis(C259) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(C256) \\sim Ueq, Uanis(C257)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{C108, F4A, F5A, F6A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C108, F4, F5, F6}
{C117, C149, F7A, F8A, F9A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C117, C118, F7, F8, F9}
{C128, F10A, F11A, F12A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C128, F10, F11, F12}
{C137, C150, F13A, F14A, F15A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C137, C138, F13, F14, F15}
{O21, C172, C173, C174, C175} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O21, C168, C169, C170, C171}
{O22, C180, C181, C182, C183} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O22, C176, C177, C178, C179}
{C188, C189, C190, C191, O23A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C184, C185, C186, C187, O23}
{C196, C197, C198, C199, O24A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C192, C193, C194, C195, O24}
{C204, C205, C206, C207, O25A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C200, C201, C202, C203, O25}
{C212, C213, C214, C215, O26A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C208, C209, C210, C211, O26}
{C222, C223, C224, C225, C226, C227} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C216, C217, C218, C219, C220, C221}
{C236, C237, C238, C239, O28A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C232, C233, C234, C235, O28}
{C244, C245, C246, C247, O29A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C240, C241, C242, C243, O29}
{C252, C253, C254, C255, O30A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C248, C249, C250, C251, O30}
{C260, C261, C262, C263, O31A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C256, C257, C258, C259, O31}
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(C149)=Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(C118)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(C150)=Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(C138)=Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(4)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(4)
 Sof(H15E)=Sof(H15F)=Sof(H15I)=Sof(H15J)=Sof(C159)=Sof(H15M)=Sof(H15N)=1-FVAR(5)
 Sof(H15C)=Sof(H15D)=Sof(H15G)=Sof(H15H)=Sof(C157)=Sof(H15K)=Sof(H15L)=FVAR(5)
 Sof(C172)=Sof(H17E)=Sof(H17F)=Sof(C173)=Sof(H17G)=Sof(H17H)=Sof(C174)=
 Sof(H17I)=Sof(H17J)=Sof(C175)=Sof(H17K)=Sof(H17L)=1-FVAR(6)
 Sof(C168)=Sof(H16A)=Sof(H16B)=Sof(C169)=Sof(H16C)=Sof(H16D)=Sof(C170)=
 Sof(H17A)=Sof(H17B)=Sof(C171)=Sof(H17C)=Sof(H17D)=FVAR(6)
 Sof(C180)=Sof(H18A)=Sof(H18B)=Sof(C181)=Sof(H18C)=Sof(H18D)=Sof(C182)=
 Sof(H18E)=Sof(H18F)=Sof(C183)=Sof(H18G)=Sof(H18H)=1-FVAR(7)
 Sof(C176)=Sof(H17M)=Sof(H17N)=Sof(C177)=Sof(H17O)=Sof(H17P)=Sof(C178)=
 Sof(H17Q)=Sof(H17R)=Sof(C179)=Sof(H17S)=Sof(H17T)=FVAR(7)
 Sof(C188)=Sof(H18Q)=Sof(H18R)=Sof(C189)=Sof(H18S)=Sof(H18T)=Sof(C190)=
 Sof(H19I)=Sof(H19J)=Sof(C191)=Sof(H19K)=Sof(H19L)=Sof(O23A)=1-FVAR(8)
 Sof(C184)=Sof(H18I)=Sof(H18J)=Sof(C185)=Sof(H18K)=Sof(H18L)=Sof(C186)=
 Sof(H18M)=Sof(H18N)=Sof(C187)=Sof(H18O)=Sof(H18P)=Sof(O23)=FVAR(8)
 Sof(C196)=Sof(H19M)=Sof(H19N)=Sof(C197)=Sof(H19O)=Sof(H19P)=Sof(C198)=
 Sof(H19Q)=Sof(H19R)=Sof(C199)=Sof(H19S)=Sof(H19T)=Sof(O24A)=1-FVAR(9)
 Sof(C192)=Sof(H19A)=Sof(H19B)=Sof(C193)=Sof(H19C)=Sof(H19D)=Sof(C194)=
 Sof(H19E)=Sof(H19F)=Sof(C195)=Sof(H19G)=Sof(H19H)=Sof(O24)=FVAR(9)
 Sof(C204)=Sof(H20M)=Sof(H20N)=Sof(C205)=Sof(H20O)=Sof(H20P)=Sof(C206)=
 Sof(H20Q)=Sof(H20R)=Sof(C207)=Sof(H20S)=Sof(H20T)=Sof(O25A)=1-FVAR(10)
 Sof(C200)=Sof(H20A)=Sof(H20B)=Sof(C201)=Sof(H20C)=Sof(H20D)=Sof(C202)=
 Sof(H20E)=Sof(H20F)=Sof(C203)=Sof(H20G)=Sof(H20H)=Sof(O25)=FVAR(10)
 Sof(C212)=Sof(H21N)=Sof(H21O)=Sof(C213)=Sof(H21P)=Sof(H21Q)=Sof(C214)=
 Sof(H21R)=Sof(H21S)=Sof(C215)=Sof(H21T)=Sof(H21U)=Sof(O26A)=1-FVAR(11)
 Sof(C208)=Sof(H20I)=Sof(H20J)=Sof(C209)=Sof(H20K)=Sof(H20L)=Sof(C210)=
 Sof(H21J)=Sof(H21K)=Sof(C211)=Sof(H21L)=Sof(H21M)=Sof(O26)=FVAR(11)
 Sof(C222)=Sof(H22F)=Sof(H22G)=Sof(H22H)=Sof(C223)=Sof(H22I)=Sof(H22J)=
 Sof(C224)=Sof(H22K)=Sof(H22L)=Sof(C225)=Sof(H22M)=Sof(H22N)=Sof(C226)=
 Sof(H22O)=Sof(H22P)=Sof(C227)=Sof(H22Q)=Sof(H22R)=Sof(H22S)=1-FVAR(12)
 Sof(C216)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C217)=Sof(H21D)=Sof(H21E)=
 Sof(C218)=Sof(H21F)=Sof(H21G)=Sof(C219)=Sof(H21H)=Sof(H21I)=Sof(C220)=
 Sof(H22A)=Sof(H22B)=Sof(C221)=Sof(H22C)=Sof(H22D)=Sof(H22E)=FVAR(12)
 Sof(C236)=Sof(H23I)=Sof(H23J)=Sof(C237)=Sof(H23K)=Sof(H23L)=Sof(C238)=
 Sof(H23M)=Sof(H23N)=Sof(C239)=Sof(H23O)=Sof(H23P)=Sof(O28A)=0.5*(1-FVAR(14))
 Sof(C232)=Sof(H23A)=Sof(H23B)=Sof(C233)=Sof(H23C)=Sof(H23D)=Sof(C234)=
 Sof(H23E)=Sof(H23F)=Sof(C235)=Sof(H23G)=Sof(H23H)=Sof(O28)=0.5*FVAR(14)
 Sof(C244)=Sof(H24I)=Sof(H24J)=Sof(C245)=Sof(H24K)=Sof(H24L)=Sof(C246)=
 Sof(H24M)=Sof(H24N)=Sof(C247)=Sof(H24O)=Sof(H24P)=Sof(O29A)=1-FVAR(14)
 Sof(C240)=Sof(H24A)=Sof(H24B)=Sof(C241)=Sof(H24C)=Sof(H24D)=Sof(C242)=
 Sof(H24E)=Sof(H24F)=Sof(C243)=Sof(H24G)=Sof(H24H)=Sof(O29)=FVAR(14)
 Sof(C252)=Sof(H25A)=Sof(H25B)=Sof(C253)=Sof(H25C)=Sof(H25D)=Sof(C254)=
 Sof(H25E)=Sof(H25F)=Sof(C255)=Sof(H25G)=Sof(H25H)=Sof(O30A)=0.5*(1-FVAR(16))
 Sof(C248)=Sof(H24Q)=Sof(H24R)=Sof(C249)=Sof(H24S)=Sof(H24T)=Sof(C250)=
 Sof(H25I)=Sof(H25J)=Sof(C251)=Sof(H25K)=Sof(H25L)=Sof(O30)=0.5*FVAR(16)
 Sof(C260)=Sof(H26A)=Sof(H26B)=Sof(C261)=Sof(H26C)=Sof(H26D)=Sof(C262)=
 Sof(H26E)=Sof(H26F)=Sof(C263)=Sof(H26G)=Sof(H26H)=Sof(O31A)=0.5*(1-FVAR(17))
 Sof(C256)=Sof(H25M)=Sof(H25N)=Sof(C257)=Sof(H25O)=Sof(H25P)=Sof(C258)=
 Sof(H25Q)=Sof(H25R)=Sof(C259)=Sof(H25S)=Sof(H25T)=Sof(O31)=0.5*FVAR(17)
 Fixed Sof: C228(0.5) H22T(0.5) H22U(0.5) C229(0.5) H22V(0.5) H22W(0.5)
 C230(0.5) H23Q(0.5) H23R(0.5) C231(0.5) H23S(0.5) H23T(0.5) O27(0.5)
 Fixed Y: Yb1(0.629221)
6.a Riding coordinates:
 C216(H21A,H21B,H21C), C221(H22C,H22D,H22E), C222(H22F,H22G,H22H), C227(H22Q,
 H22R,H22S)
6.b Secondary CH2 refined with riding coordinates:
 C151(H15O,H15P), C152(H15Q,H15R), C153(H15S,H15T), C154(H15U,H15V), C155(H15A,
 H15B), C156(H15C,H15D), C156(H15E,H15F), C158(H15G,H15H), C158(H15I,H15J),
 C157(H15K,H15L), C159(H15M,H15N), C160(H16E,H16F), C161(H16G,H16H), C162(H16I,
 H16J), C163(H16K,H16L), C164(H16M,H16N), C165(H16O,H16P), C166(H16Q,H16R),
 C167(H16S,H16T), C168(H16A,H16B), C169(H16C,H16D), C170(H17A,H17B), C171(H17C,
 H17D), C176(H17M,H17N), C177(H17O,H17P), C178(H17Q,H17R), C179(H17S,H17T),
 C184(H18I,H18J), C185(H18K,H18L), C186(H18M,H18N), C187(H18O,H18P), C192(H19A,
 H19B), C193(H19C,H19D), C194(H19E,H19F), C195(H19G,H19H), C200(H20A,H20B),
 C201(H20C,H20D), C202(H20E,H20F), C203(H20G,H20H), C208(H20I,H20J), C209(H20K,
 H20L), C210(H21J,H21K), C211(H21L,H21M), C217(H21D,H21E), C218(H21F,H21G),
 C219(H21H,H21I), C220(H22A,H22B), C232(H23A,H23B), C233(H23C,H23D), C234(H23E,
 H23F), C235(H23G,H23H), C240(H24A,H24B), C241(H24C,H24D), C242(H24E,H24F),
 C243(H24G,H24H), C188(H18Q,H18R), C189(H18S,H18T), C190(H19I,H19J), C191(H19K,
 H19L), C196(H19M,H19N), C197(H19O,H19P), C198(H19Q,H19R), C199(H19S,H19T),
 C204(H20M,H20N), C205(H20O,H20P), C206(H20Q,H20R), C207(H20S,H20T), C212(H21N,
 H21O), C213(H21P,H21Q), C214(H21R,H21S), C215(H21T,H21U), C223(H22I,H22J),
 C224(H22K,H22L), C225(H22M,H22N), C226(H22O,H22P), C236(H23I,H23J), C237(H23K,
 H23L), C238(H23M,H23N), C239(H23O,H23P), C244(H24I,H24J), C245(H24K,H24L),
 C246(H24M,H24N), C247(H24O,H24P), C252(H25A,H25B), C253(H25C,H25D), C254(H25E,
 H25F), C255(H25G,H25H), C260(H26A,H26B), C261(H26C,H26D), C262(H26E,H26F),
 C263(H26G,H26H), C228(H22T,H22U), C229(H22V,H22W), C230(H23Q,H23R), C231(H23S,
 H23T), C248(H24Q,H24R), C249(H24S,H24T), C250(H25I,H25J), C251(H25K,H25L),
 C256(H25M,H25N), C257(H25O,H25P), C258(H25Q,H25R), C259(H25S,H25T), C172(H17E,
 H17F), C173(H17G,H17H), C174(H17I,H17J), C175(H17K,H17L), C180(H18A,H18B),
 C181(H18C,H18D), C182(H18E,H18F), C183(H18G,H18H)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C57(H57),
 C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68),
  C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
 C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86),
  C87(H87), C88(H88), C90(H90), C91(H91), C93(H93), C94(H94), C96(H96),
 C100(H100), C101(H101), C103(H103), C104(H104), C106(H106), C110(H110),
 C111(H111), C113(H113), C114(H114), C116(H116), C120(H120), C121(H121),
 C123(H123), C124(H124), C126(H126), C130(H130), C131(H131), C133(H133),
 C134(H134), C136(H136), C140(H140), C141(H141), C143(H143), C144(H144),
 C146(H146)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 1930\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.2[C4H8O] per Asymmetric Unit 
which account for 96 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58053
_shelx_hkl_checksum              65206
_shelx_fab_checksum              91216
_olex2_submission_special_instructions 'No special instructions were received'