Construction of Bowl-Shaped Copper Clusters and Nitrate-Selective Sensing
Huo, Nannan; Zhang, De-Ke; Wei, Yu-Zhen; Luo, Peng; Li, Si; Dalton Transactions  (2026) –; doi:10.1039/D6DT00475J

data_7720731
_publ_section_title
;
 Construction of bowl-shaped copper clusters and nitrate-selective
 sensing.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6015
_journal_page_last               6023
_journal_paper_doi               10.1039/d6dt00475j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'2(C105 H93 Cu4 N6 O3 P4), 3(C H4 O), 2(C H O2), 1(H2 O), 3[CH3OH]'
_chemical_formula_sum            'C218 H214 Cu8 N12 O17 P8'
_chemical_formula_weight         4030.08
_chemical_name_systematic        Cu4-HCOO
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-03-13 deposited with the CCDC.	2026-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.7990(10)
_cell_angle_beta                 90.0840(10)
_cell_angle_gamma                94.3670(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8024(2)
_cell_length_b                   20.9403(3)
_cell_length_c                   31.9803(4)
_cell_measurement_reflns_used    61634
_cell_measurement_temperature    200
_cell_measurement_theta_max      77.2260
_cell_measurement_theta_min      2.1650
_cell_volume                     9879.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  22.00   0.50    0.29    --  -45.07  70.00 -75.00  170
  2  \w    -67.00 -24.00   0.50    0.80    --  -97.00  57.00-150.00   86
  3  \w    -76.00 -50.00   0.50    0.80    --  -97.00  70.00 -75.00   52
  4  \w    -69.00 -24.00   0.50    0.80    --  -97.00  57.00  30.00   90
  5  \w    -51.00 -24.00   0.50    0.80    --  -97.00  57.00  90.00   54
  6  \w    -69.00 -24.00   0.50    0.80    --  -97.00  57.00 120.00   90
  7  \w   -108.00 -81.00   0.50    0.80    --  -97.00 109.00  53.09   54
  8  \w    -67.00 -27.00   0.50    0.80    --  -97.00 109.00  53.09   80
  9  \w    -90.00 -23.00   0.50    0.29    --  -45.07 125.00  60.00  134
 10  \w   -150.00 -91.00   0.50    0.80    --  -97.00 -99.00  90.00  118
 11  \w   -137.00-111.00   0.50    0.80    --  -97.00 -99.00 -60.00   52
 12  \w   -137.00 -83.00   0.50    0.80    --  -97.00-125.00-120.00  108
 13  \w   -168.00 -92.00   0.50    0.80    --  -97.00 -99.00-150.00  152
 14  \w   -170.00 -84.00   0.50    0.80    --  -97.00 -38.00-120.00  172
 15  \w   -109.00 -26.00   0.50    0.29    --  -45.07 -70.00 152.00  166
 16  \w   -150.00 -77.00   0.50    0.80    --  -97.00 -70.00 152.00  146
 17  \w    -14.00  17.00   0.50    0.29    --   45.07 -19.00 -90.00   62
 18  \w      2.00  28.00   0.50    0.29    --   45.07 -70.00 152.00   52
 19  \w    -25.00  20.00   0.50    0.29    --   45.07 -19.00-150.00   90
 20  \w     41.00  82.00   0.50    0.80    --  106.74 -70.00 152.00   82
 21  \w    -28.00  40.00   0.50    0.29    --   45.07 -38.00 150.00  136
 22  \w     88.00 128.00   0.50    0.80    --  106.74 125.00  30.00   80
 23  \w     81.00 106.00   0.50    0.80    --  106.74 -99.00 150.00   50
 24  \w     37.00  63.00   0.50    0.80    --  106.74-125.00  90.00   52
 25  \w     61.00  94.00   0.50    0.80    --  106.74-125.00  30.00   66
 26  \w     38.00 112.00   0.50    0.80    --  106.74-125.00 -30.00  148
 27  \w     48.00 112.00   0.50    0.80    --  106.74-125.00 -60.00  128
 28  \w     39.00 112.00   0.50    0.80    --  106.74-125.00-120.00  146
 29  \w     46.00  72.00   0.50    0.80    --  106.74-125.00-180.00   52
 30  \w     77.00 110.00   0.50    0.80    --  106.74-125.00-180.00   66
 31  \w     39.00 112.00   0.50    0.80    --  106.74-125.00   0.00  146
 32  \w     49.00 112.00   0.50    0.80    --  106.74-125.00  60.00  126
 33  \w     40.00 103.00   0.50    0.80    --  106.74-125.00 150.00  126
 34  \w     44.00  69.00   0.50    0.80    --  106.74 -99.00 150.00   50
 35  \w     38.00 103.00   0.50    0.80    --  106.74 -99.00  60.00  130
 36  \w     37.00  77.00   0.50    0.80    --  106.74 -99.00-120.00   80
 37  \w    100.00 160.00   0.50    0.80    --  106.74  19.00 -90.00  120
 38  \w     91.00 169.00   0.50    0.80    --  106.74  70.00 -75.00  156
 39  \w    129.00 154.00   0.50    0.80    --  106.74  57.00   0.00   50
 40  \w    141.00 167.00   0.50    0.80    --  106.74  19.00   0.00   52
 41  \w    110.00 135.00   0.50    0.80    --  106.74  19.00   0.00   50
 42  \w     27.00  91.00   0.50    0.29    --   45.07  70.00 -75.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0209598000
_diffrn_orient_matrix_UB_12      0.0533030000
_diffrn_orient_matrix_UB_13      -0.0298667000
_diffrn_orient_matrix_UB_21      0.0894067000
_diffrn_orient_matrix_UB_22      -0.0088475000
_diffrn_orient_matrix_UB_23      -0.0233157000
_diffrn_orient_matrix_UB_31      -0.0496214000
_diffrn_orient_matrix_UB_32      -0.0502980000
_diffrn_orient_matrix_UB_33      -0.0297865000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            136916
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.384
_diffrn_reflns_theta_min         2.117
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             4188
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.963
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2774
_refine_ls_number_reflns         40190
_refine_ls_number_restraints     1739
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0617P)^2^+17.9839P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34289
_reflns_number_total             40190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00475j2.cif
_cod_data_source_block           Cu4-HCOO
_cod_depositor_comments
'Adding full bibliography for 7720727--7720731.cif.'
_cod_database_code               7720731
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.747
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 C251-C252
 1.5 with sigma of 0.01
 C119-C118
 1.5 with sigma of 0.01
 C243-C240
 1.53 with sigma of 0.01
 C261-C260
 1.5 with sigma of 0.01
 C263-O6
 1.25 with sigma of 0.01
 O8-C238 \\sim O15-C259
 with sigma of 0.01
 N14-C126 \\sim N8-C83 \\sim N8-C85 \\sim N14-C120 \\sim N13-C120 \\sim N12-C85
\\sim N12-C98 \\sim N13-C119
 with sigma of 0.01
 N11-C241 \\sim N16-C251 \\sim N11-C239 \\sim N16-C250 \\sim N15-C250 \\sim
N7-C239 \\sim N15-C171 ~
 N7-C171
 with sigma of 0.01
 N11-C242 \\sim N16-C252
 with sigma of 0.01
 N5-C259 \\sim N5-C238 \\sim N10-C238 \\sim N17-C259 \\sim N17-C260 \\sim
N10-C240
 with sigma of 0.01
 O11-C265 \\sim O16-C265
 with sigma of 0.01
 O17-C266 \\sim C266-O12
 with sigma of 0.01
 O6-C263 \\sim C263-O7
 with sigma of 0.01
3. Rigid bond restraints
 O7, C263
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C263
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C237 \\sim C244 \\sim
C245 \\sim C246 \\sim C247 \\sim C248 \\sim C249: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C106 \\sim C107
\\sim C108 \\sim C109 \\sim C110 \\sim C111: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C133 \\sim
C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C98 \\sim C99 \\sim C118 \\sim C119: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C80 \\sim C83 \\sim C87 \\sim C89 \\sim C90 \\sim C91 \\sim C121 \\sim C122
\\sim C123 \\sim C124 \\sim C125 \\sim C126: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N8 \\sim N12 \\sim N13 \\sim N14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C241 \\sim C242 \\sim C251 \\sim C252: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
N7 \\sim N11 \\sim N15 \\sim N16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C226 \\sim C227 \\sim C228 \\sim C229 \\sim C230 \\sim C231 \\sim C253 \\sim
C254 \\sim C255 \\sim C256 \\sim C257 \\sim C258: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C238 \\sim C240 \\sim C243 \\sim C259 \\sim C260 \\sim C261: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N5 \\sim N10 \\sim N17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C79 \\sim C81 \\sim C82 \\sim C84 \\sim C86 \\sim C88 \\sim C127 \\sim C128
\\sim C129 \\sim C130 \\sim C131 \\sim C132: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C20 \\sim C50 \\sim C55 \\sim C56 \\sim C61 \\sim C63: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C4 \\sim C25 \\sim C26 \\sim C29 \\sim C53 \\sim C54: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C165 \\sim C170 \\sim C208 \\sim C213 \\sim C221 \\sim C223: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O12 \\sim O17 \\sim O18 \\sim O19: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C268 \\sim C269
\\sim C270 \\sim C271 \\sim C272 \\sim C273: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O6 \\sim O7 \\sim C263: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O20 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O14) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C120) \\sim Ueq, Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C238) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C267) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C240) \\sim Ueq, Uanis(C260) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(C100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=
 Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=1-FVAR(1)
 Sof(C92)=Sof(H92)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94)=Sof(C95)=Sof(C96)=
 Sof(H96)=Sof(C97)=Sof(H97)=FVAR(1)
 Sof(C244)=Sof(C245)=Sof(H245)=Sof(C246)=Sof(H246)=Sof(C247)=Sof(H247)=
 Sof(C248)=Sof(H248)=Sof(C249)=Sof(H249)=1-FVAR(2)
 Sof(C232)=Sof(C233)=Sof(H233)=Sof(C234)=Sof(H234)=Sof(C235)=Sof(H235)=
 Sof(C236)=Sof(H236)=Sof(C237)=Sof(H237)=FVAR(2)
 Sof(C106)=Sof(C107)=Sof(H107)=Sof(C108)=Sof(H108)=Sof(C109)=Sof(H109)=
 Sof(C110)=Sof(H110)=Sof(C111)=Sof(H111)=1-FVAR(3)
 Sof(C73)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(H78)=FVAR(3)
 Sof(C133)=Sof(H133)=Sof(C134)=Sof(H134)=Sof(C135)=Sof(H135)=Sof(C136)=
 Sof(H136)=Sof(C137)=Sof(C138)=Sof(H138)=1-FVAR(4)
 Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=Sof(C114)=Sof(H114)=Sof(C115)=
 Sof(H115)=Sof(C116)=Sof(C117)=Sof(H117)=FVAR(4)
 Sof(O14)=Sof(N13)=Sof(H13)=Sof(N14)=Sof(H14)=Sof(C118)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C119)=Sof(H11D)=Sof(H11E)=Sof(C120)=Sof(C121)=Sof(C122)=
 Sof(H122)=Sof(C123)=Sof(H123)=Sof(C124)=Sof(H124)=Sof(C125)=Sof(H125)=
 Sof(C126)=1-FVAR(5)
 Sof(O9)=Sof(N8)=Sof(H8)=Sof(N12)=Sof(H12A)=Sof(C80)=Sof(C83)=Sof(C85)=
 Sof(C87)=Sof(H87)=Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90)=Sof(C91)=Sof(H91)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=FVAR(5)
 Sof(N15)=Sof(H15)=Sof(N16)=Sof(H16)=Sof(C250)=Sof(C251)=Sof(H25A)=Sof(H25B)=
 Sof(C252)=Sof(H25C)=Sof(H25D)=Sof(H25E)=1-FVAR(6)
 Sof(N7)=Sof(H7)=Sof(N11)=Sof(H11)=Sof(C239)=Sof(C241)=Sof(H24C)=Sof(H24D)=
 Sof(C242)=Sof(H24E)=Sof(H24F)=Sof(H24G)=FVAR(6)
 Sof(C253)=Sof(C254)=Sof(H254)=Sof(C255)=Sof(H255)=Sof(C256)=Sof(H256)=
 Sof(C257)=Sof(H257)=Sof(C258)=Sof(H258)=1-FVAR(7)
 Sof(C226)=Sof(C227)=Sof(H227)=Sof(C228)=Sof(H228)=Sof(C229)=Sof(H229)=
 Sof(C230)=Sof(H230)=Sof(C231)=Sof(H231)=FVAR(7)
 Sof(H5B)=Sof(O15)=Sof(N17)=Sof(H17)=Sof(C259)=Sof(C260)=Sof(H26A)=Sof(H26B)=
 Sof(C261)=Sof(H26C)=Sof(H26D)=Sof(H26E)=1-FVAR(8)
 Sof(H5A)=Sof(O8)=Sof(N10)=Sof(H10)=Sof(C238)=Sof(C240)=Sof(H24A)=Sof(H24B)=
 Sof(C243)=Sof(H24H)=Sof(H24I)=Sof(H24J)=FVAR(8)
 Sof(C127)=Sof(C128)=Sof(H128)=Sof(C129)=Sof(H129)=Sof(C130)=Sof(H130)=
 Sof(C131)=Sof(H131)=Sof(C132)=Sof(H132)=1-FVAR(9)
 Sof(C79)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82)=Sof(C84)=Sof(H84)=Sof(C86)=
 Sof(H86)=Sof(C88)=Sof(H88)=FVAR(9)
 Sof(H26I)=Sof(H26J)=Sof(H26K)=Sof(O11)=Sof(H11F)=1-FVAR(10)
 Sof(H26F)=Sof(H26G)=Sof(H26H)=Sof(O16)=Sof(H16A)=FVAR(10)
 Sof(O13)=Sof(H13A)=Sof(H13B)=1-FVAR(11)
 Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(11)
 Sof(C268)=Sof(H268)=Sof(C269)=Sof(H269)=Sof(C270)=Sof(H270)=Sof(C271)=
 Sof(C272)=Sof(H272)=Sof(C273)=Sof(H273)=1-FVAR(12)
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=
 Sof(H69)=Sof(C70)=Sof(H70)=FVAR(12)
 Fixed Sof: O12(0.7) O17(0.7) C266(0.7) H266(0.7) O18(0.3) O19(0.3) C267(0.3)
 H267(0.3)
6.a Everything fixed:
 H10A, H16A, O20, H20A, H20B, O13, H13A, H13B
6.b Riding coordinates:
 C265(H26I,H26J,H26K), C265(H26F,H26G,H26H)
6.c Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C71(H71A,H71B), C98(H98A,H98B), C119(H11D,H11E), C224(H22A,
 H22B), C240(H24A,H24B), C241(H24C,H24D), C251(H25A,H25B), C260(H26A,H26B)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N6(H6), C5(H5), C6(H6A), C12(H12), C18(H18), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61),
 C63(H63), N8(H8), N12(H12A), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82), C84(H84),
  C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92),
 C93(H93), C94(H94), C96(H96), C97(H97), N13(H13), N14(H14), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C107(H107), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C115(H115), C117(H117), C122(H122), C123(H123), C124(H124), C125(H125),
 C128(H128), C129(H129), C130(H130), C131(H131), C132(H132), C268(H268),
 C269(H269), C270(H270), C272(H272), C273(H273), C133(H133), C134(H134),
 C135(H135), C136(H136), C138(H138), N1(H1), N5(H5A), N5(H5B), N9(H9),
 C156(H156), C157(H157), C158(H158), C160(H160), C161(H161), C162(H162),
 C163(H163), C165(H165), C166(H166), C168(H168), C169(H169), C172(H172),
 C173(H173), C174(H174), C175(H175), C176(H176), C177(H177), C178(H178),
 C180(H180), C181(H181), C182(H182), C183(H183), C184(H184), C185(H185),
 C186(H186), C187(H187), C188(H188), C189(H189), C190(H190), C191(H191),
 C192(H192), C193(H193), C194(H194), C195(H195), C196(H196), C197(H197),
 C198(H198), C199(H199), C200(H200), C201(H201), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C207(H207), C208(H208), C209(H209),
 C210(H210), C211(H211), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C217(H217), C218(H218), C219(H219), C220(H220), C221(H221),
 C222(H222), C223(H223), N7(H7), N10(H10), N11(H11), C227(H227), C228(H228),
 C229(H229), C230(H230), C231(H231), C233(H233), C234(H234), C235(H235),
 C236(H236), C237(H237), N15(H15), N16(H16), N17(H17), C245(H245), C246(H246),
 C247(H247), C248(H248), C249(H249), C254(H254), C255(H255), C256(H256),
 C257(H257), C258(H258), C263(H263), C266(H266), C267(H267)
6.e Fitted hexagon refined as free rotating group:
 C65(C66,C67,C68,C69,C70), C73(C74,C75,C76,C77,C78), C92(C93,C94,C95,C96,C97),
 C100(C101,C102,C103,C104,C105), C106(C107,C108,C109,C110,C111), C112(C113,C114,
 C115,C116,C117), C121(C122,C123,C124,C125,C126), C127(C128,C129,C130,C131,
 C132), C268(C269,C270,C271,C272,C273), C133(C134,C135,C136,C137,C138),
 C226(C227,C228,C229,C230,C231), C232(C233,C234,C235,C236,C237), C244(C245,C246,
 C247,C248,C249), C253(C254,C255,C256,C257,C258)
6.f Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C72(H72A,H72B,H72C), C99(H99A,H99B,H99C), C118(H11A,H11B,
 H11C), C225(H22C,H22D,H22E), C242(H24E,H24F,H24G), C243(H24H,H24I,H24J),
 C252(H25C,H25D,H25E), C261(H26C,H26D,H26E), C262(H26L,H26M,H26N), C264(H26O,
 H26P,H26Q)
6.g Idealised tetrahedral OH refined as rotating group:
 O5(H5C), O11(H11F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 466\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[CH3OH] per Asymmetric Unit 
which account for 108 electrons 
per unit cell.
;
_shelx_res_checksum              23622
_shelx_fab_checksum              89408
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.702
_oxdiff_exptl_absorpt_empirical_full_min 0.352