Altering the solubility of metal-organic polyhedra <i>via</i> pendant functionalization of Cp<sub>3</sub>Zr<sub>3</sub>O(OH)<sub>3</sub> nodes.
Sullivan, Meghan G.; Sokolow, Gregory E.; Jensen, Eric T.; Crawley, Matthew R.; MacMillan, Samantha N.; Cook, Timothy R.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 338–346; doi:10.1039/d2dt03401h

data_7711919
_publ_section_title
;
 Altering the solubility of metal-organic polyhedra <i>via</i> pendant
 functionalization of Cp<sub>3</sub>Zr<sub>3</sub>O(OH)<sub>3</sub> nodes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              338
_journal_page_last               346
_journal_paper_doi               10.1039/d2dt03401h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C182.69 H146.688 O40 Zr12, 5(Cl), 0.5(C3 N O), C2.74 H7.043 N0.452 O0.97, O, C3 H7 N O, [+ solvents]'
_chemical_formula_sum            'C192 H155 Cl4 O41 Zr12'
_chemical_formula_weight         4354.59
_chemical_name_common            ZrMOP-ben-tetrahedron
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2022-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.4705(2)
_cell_length_b                   42.42650(10)
_cell_length_c                   31.99240(10)
_cell_measurement_reflns_used    168927
_cell_measurement_temperature    103(1)
_cell_measurement_theta_max      77.7810
_cell_measurement_theta_min      2.2920
_cell_volume                     52217.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -66.00   8.00   0.50    7.69    --  -48.30  69.00  76.00  148
  2  \w     47.00  78.00   0.50    7.69    --   48.30-125.00-122.00   62
  3  \w   -106.00 -80.00   0.50   30.75    --  -86.25 -69.00 -56.00   52
  4  \w    -59.00 -34.00   0.50   30.75    --  -86.25  52.00-105.00   50
  5  \w     71.00  96.00   0.50   30.75    --  107.75-125.00-122.00   50
  6  \w     57.00  82.00   0.50   30.75    --  107.75 -69.00 -56.00   50
  7  \w    112.00 137.00   0.50   30.75    --  107.75  52.00-105.00   50
  8  \w     81.00 114.00   0.50   30.75    --  107.75 145.00 122.00   66
  9  \w   -108.00 -61.00   0.50    7.69    --  -48.30-145.00  70.00   94
 10  \w    -26.00  24.00   0.50    7.69    --  -48.30  19.00-180.00  100
 11  \w     83.00 108.00   0.50   30.75    --  107.75-125.00 -90.00   50
 12  \w     40.00  78.00   0.50   30.75    --  107.75-125.00 -90.00   76
 13  \w     63.00 103.00   0.50   30.75    --  107.75 -77.00-180.00   80
 14  \w     37.00  71.00   0.50   30.75    --  107.75 -61.00-180.00   68
 15  \w    148.00 175.00   0.50   30.75    --  107.75 111.00  70.91   54
 16  \w     39.00  65.00   0.50   30.75    --  107.75 -61.00 -30.00   52
 17  \w    104.00 143.00   0.50   30.75    --  107.75  30.00 150.00   78
 18  \w    150.00 178.00   0.50   30.75    --  107.75  30.00 150.00   56
 19  \w    148.00 174.00   0.50   30.75    --  107.75  61.00-150.00   52
 20  \w     99.00 167.00   0.50   30.75    --  107.75  30.00  90.00  136
 21  \w    103.00 137.00   0.50   30.75    --  107.75 111.00  70.91   68
 22  \w     39.00  69.00   0.50   30.75    --  107.75 -61.00 -60.00   60
 23  \w     44.00  69.00   0.50   30.75    --  107.75-125.00 150.00   50
 24  \w     36.00 104.00   0.50   30.75    --  107.75 -94.00 -90.00  136
 25  \w     39.00  66.00   0.50   30.75    --  107.75-102.00 115.26   54
 26  \w     67.00  93.00   0.50   30.75    --  107.75-102.00 115.26   52
 27  \w    100.00 129.00   0.50   30.75    --  107.75 125.00 -60.00   58
 28  \w     65.00 107.00   0.50   30.75    --  107.75-125.00  30.00   84
 29  \w     48.00  73.00   0.50   30.75    --  107.75 -63.00 152.23   50
 30  \w    109.00 135.00   0.50   30.75    --  107.75  61.00-150.00   52
 31  \w     38.00  66.00   0.50   30.75    --  107.75 -61.00 -90.00   56
 32  \w     37.00  63.00   0.50   30.75    --  107.75 -77.00  30.00   52
 33  \w    109.00 135.00   0.50   30.75    --  107.75  61.00   0.00   52
 34  \w     52.00 102.00   0.50   30.75    --  107.75 -77.00-120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0044506000
_diffrn_orient_matrix_UB_12      -0.0279032000
_diffrn_orient_matrix_UB_13      -0.0303508000
_diffrn_orient_matrix_UB_21      -0.0397058000
_diffrn_orient_matrix_UB_22      -0.0047501000
_diffrn_orient_matrix_UB_23      -0.0007856000
_diffrn_orient_matrix_UB_31      -0.0028170000
_diffrn_orient_matrix_UB_32      0.0227588000
_diffrn_orient_matrix_UB_33      -0.0373504000
_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  0.0693
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            437426
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.166
_diffrn_reflns_theta_min         2.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.571
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.69a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             17464
_exptl_crystal_recrystallization_method 'Grown from reaction mixture'
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2422
_refine_ls_number_reflns         55533
_refine_ls_number_restraints     743
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0487P)^2^+424.7133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                48684
_reflns_number_total             55533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03401h2.cif
_cod_data_source_block           rmc29_abs
_cod_depositor_comments
'Adding full bibliography for 7711919--7711923.cif.'
_cod_database_code               7711919
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C163H100O45Zr12
_chemical_oxdiff_usercomment     'Crystallized from DMA.'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.404
_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
2. Restrained distances
 C11B-C166 = C168-C163 = C163-C12B
 1.37 with sigma of 0.02
 C11B-C12B
 1.38 with sigma of 0.02
 C166-C167 = C167-C168
 1.36 with sigma of 0.02
 C107-C106 = C106-C105
 1.36 with sigma of 0.02
 C108-C107 = C105-C104 = C104-C103
 1.37 with sigma of 0.02
 C108-C103
 1.38 with sigma of 0.02
 C119-C120 = C116-C117 = C117-C118
 1.37 with sigma of 0.02
 C120-C115 = C115-C116
 1.36 with sigma of 0.02
 C119-C118
 1.38 with sigma of 0.02
 C114-C115
 1.521 with sigma of 0.02
 C11B-C163
 2.38 with sigma of 0.04
 C166-C168
 2.36 with sigma of 0.04
 C11B-C167 = C167-C163 = C168-C12B
 2.37 with sigma of 0.04
 C108-C106 = C106-C104 = C105-C103
 2.37 with sigma of 0.04
 C108-C104
 2.38 with sigma of 0.04
 C107-C105
 2.36 with sigma of 0.04
 C119-C115 = C115-C117 = C116-C118
 2.37 with sigma of 0.04
 C120-C116
 2.36 with sigma of 0.04
 C119-C117
 2.38 with sigma of 0.04
 C144-C139 \\sim C30B-C25B
 with sigma of 0.02
 C139-C143 \\sim C25B-C29B
 with sigma of 0.04
 C144-C143 \\sim C30B-C29B
 with sigma of 0.02
 C140-C142 \\sim C26B-C28B
 with sigma of 0.04
 C139-C140 \\sim C25B-C26B
 with sigma of 0.02
 C140-C141 \\sim C26B-C27B
 with sigma of 0.02
 C141-C142 \\sim C27B-C28B
 with sigma of 0.02
 C139-C141 \\sim C25B-C27B
 with sigma of 0.04
 C142-C143 \\sim C28B-C29B
 with sigma of 0.02
 C141-C143 \\sim C27B-C29B
 with sigma of 0.04
 C136-C139 \\sim C136-C25B
 with sigma of 0.04
 C144-C140 \\sim C30B-C26B
 with sigma of 0.04
 C144-C142 \\sim C30B-C28B
 with sigma of 0.04
 C11B-C163 \\sim C11B-C167 \\sim C163-C167 \\sim C168-C166 \\sim C168-C12B
\\sim C12B-C166
 with sigma of 0.04
 C11B-C166 \\sim C166-C167 \\sim C167-C168 \\sim C168-C163 \\sim C163-C12B
\\sim C12B-C11B
 with sigma of 0.02
 C160-C159 \\sim C195-C198
 with sigma of 0.02
 C157-C159 \\sim C197-C198
 with sigma of 0.04
 C161-C157 \\sim C201-C197
 with sigma of 0.02
 C161-C194 \\sim C201-C194
 with sigma of 0.02
 C161-C158 \\sim C201-C196
 with sigma of 0.04
 C161-C162 \\sim C201-C162
 with sigma of 0.02
 C157-C158 \\sim C197-C196
 with sigma of 0.02
 C157-C194 \\sim C197-C194
 with sigma of 0.04
 C160-C161 \\sim C195-C201
 with sigma of 0.02
 C158-C159 \\sim C196-C198
 with sigma of 0.02
 C161-C159 \\sim C201-C198
 with sigma of 0.04
 C157-C162 \\sim C197-C162
 with sigma of 0.04
 Zr4-C161 \\sim Zr4-C201
 with sigma of 0.04
 Zr4-C157 \\sim Zr4-C197
 with sigma of 0.04
 C160-C157 \\sim C195-C197
 with sigma of 0.04
 C160-C158 \\sim C195-C196
 with sigma of 0.04
 C160-C162 \\sim C195-C162
 with sigma of 0.04
 C160-C194 \\sim C195-C194
 with sigma of 0.04
 Zr4-C160 \\sim Zr4-C195
 with sigma of 0.02
 Zr4-C158 \\sim Zr4-C196
 with sigma of 0.02
 Zr4-C159 \\sim Zr4-C198
 with sigma of 0.02
 C93-C94 \\sim C21B-C94
 with sigma of 0.02
 C92-C94 \\sim C20B-C94
 with sigma of 0.04
 C19B-C95 \\sim C19B-C23B
 with sigma of 0.04
 C94-C95 \\sim C94-C23B
 with sigma of 0.02
 C96-C94 \\sim C24B-C94
 with sigma of 0.04
 C19B-C93 \\sim C19B-C21B
 with sigma of 0.04
 C92-C93 \\sim C20B-C21B
 with sigma of 0.02
 C19B-C92 \\sim C19B-C20B
 with sigma of 0.02
 C96-C19B \\sim C24B-C19B
 with sigma of 0.02
 C96-C95 \\sim C24B-C23B
 with sigma of 0.02
 C108-C104 \\sim C108-C106 \\sim C104-C106 \\sim C105-C107 \\sim C105-C103
\\sim C103-C107
 with sigma of 0.04
 C108-C107 \\sim C107-C106 \\sim C106-C105 \\sim C105-C104 \\sim C104-C103
\\sim C103-C108
 with sigma of 0.02
 C175-C177 \\sim C13B-C15B
 with sigma of 0.04
 C177-C179 \\sim C15B-C17B
 with sigma of 0.04
 C176-C178 \\sim C14B-C16B
 with sigma of 0.04
 C176-C180 \\sim C14B-C18B
 with sigma of 0.04
 C178-C179 \\sim C16B-C17B
 with sigma of 0.02
 C175-C180 \\sim C13B-C18B
 with sigma of 0.02
 C174-C180 \\sim C174-C18B
 with sigma of 0.04
 C177-C178 \\sim C15B-C16B
 with sigma of 0.02
 C174-C175 \\sim C174-C13B
 with sigma of 0.02
 C175-C179 \\sim C13B-C17B
 with sigma of 0.04
 C180-C179 \\sim C18B-C17B
 with sigma of 0.02
 C174-C176 \\sim C174-C14B
 with sigma of 0.04
 C175-C176 \\sim C13B-C14B
 with sigma of 0.02
 C178-C180 \\sim C16B-C18B
 with sigma of 0.04
 C177-C176 \\sim C15B-C14B
 with sigma of 0.02
 C127-C131 \\sim C1B-C5B
 with sigma of 0.04
 C132-C130 \\sim C6B-C4B
 with sigma of 0.04
 C129-C128 \\sim C3B-C2B
 with sigma of 0.02
 C132-C128 \\sim C6B-C2B
 with sigma of 0.04
 C127-C132 \\sim C1B-C6B
 with sigma of 0.02
 C126-C127 \\sim C126-C1B
 with sigma of 0.02
 C131-C130 \\sim C5B-C4B
 with sigma of 0.02
 C131-C129 \\sim C5B-C3B
 with sigma of 0.04
 C126-C132 \\sim C126-C6B
 with sigma of 0.04
 C127-C126 \\sim C1B-C126
 with sigma of 0.02
 C127-C128 \\sim C1B-C2B
 with sigma of 0.02
 C130-C128 \\sim C4B-C2B
 with sigma of 0.04
 C132-C131 \\sim C6B-C5B
 with sigma of 0.02
 C130-C129 \\sim C4B-C3B
 with sigma of 0.02
 C126-C128 \\sim C126-C2B
 with sigma of 0.04
 C127-C129 \\sim C1B-C3B
 with sigma of 0.04
 C119-C117 \\sim C119-C115 \\sim C117-C115 \\sim C116-C120 \\sim C116-C118
\\sim C118-C120
 with sigma of 0.04
 C119-C120 \\sim C120-C115 \\sim C115-C116 \\sim C116-C117 \\sim C117-C118
\\sim C118-C119
 with sigma of 0.02
 C154-C152 \\sim C153-C155 \\sim C156-C151
 with sigma of 0.02
 C154-C155 \\sim C156-C151 \\sim C152-C153
 with sigma of 0.02
3. Restrained planarity
 C11B, C166, C167, C168, C163, C12B
 with sigma of 0.1
 C20B, C91, C24B, C23B, C22B, C21B
 with sigma of 0.1
 C7B, C8B, C9B, C10B, C194
 with sigma of 0.1
 C162, C163, C168, C167, C166
 with sigma of 0.1
 C108, C107, C106, C105, C104, C103
 with sigma of 0.1
 C14B, C15B, C16B, C17B, C18B, C13B
 with sigma of 0.1
 C176, C175, C180, C179, C178, C177
 with sigma of 0.1
 C78, C79, C84, C83, C82, C81, C80
 with sigma of 0.1
 C102, C103, C108, C107, C106, C105, C104
 with sigma of 0.1
 C119, C120, C115, C116, C117, C118
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C11B \\sim C166 \\sim C167 \\sim C168 \\sim C163 \\sim C12B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C108 \\sim C107 \\sim C106 \\sim C105 \\sim C104 \\sim C103: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C119 \\sim C120 \\sim C115 \\sim C116 \\sim C117 \\sim C118: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C155 \\sim C156 \\sim C151 \\sim C152 \\sim C153 \\sim C154: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C79 \\sim C80: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C129 \\sim C130 \\sim C131 \\sim C132 \\sim C127 \\sim C128: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C6B \\sim C5B \\sim C4B \\sim C3B \\sim C2B \\sim C1B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C138) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C144) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C8B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C194) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C82) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C19B) \\sim Ueq: with sigma of 0.2 and sigma for terminal atoms of 0.4
Uanis(C14B) = Uanis(C176)
Uanis(C15B) = Uanis(C177)
5. Rigid body (RIGU) restrains
 C11B, C166, C167, C168, C163, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C108, C107, C106, C105, C104, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C175, C177, C176, C178, C180, C179, C15B, C16B, C17B, C18B, C14B, C13B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C162, C8B, C9B, C10B, C7B, C194, C11B, C166, C167, C168, C163, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C119, C120, C115, C116, C117, C118
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C30B)=Sof(H3A)=Sof(C25B)=Sof(C26B)=Sof(H06J)=Sof(C27B)=Sof(H05S)=
 Sof(C28B)=Sof(H2)=Sof(C29B)=Sof(H4)=Sof(H5BC)=Sof(H5BD)=1-FVAR(1)
 Sof(C144)=Sof(H3)=Sof(C139)=Sof(C140)=Sof(H06I)=Sof(C141)=Sof(H05R)=Sof(C142)=
 Sof(H055)=Sof(C143)=Sof(H060)=Sof(H5AA)=Sof(H5AB)=FVAR(1)
 Sof(C19B)=Sof(C24B)=Sof(H05Y)=Sof(C23B)=Sof(H20)=Sof(C22B)=Sof(H327)=
 Sof(C21B)=Sof(H15A)=Sof(C20B)=Sof(H1C)=1-FVAR(2)
 Sof(C96)=Sof(H05X)=Sof(C92)=Sof(H065)=Sof(C93)=Sof(H15)=Sof(C94)=Sof(H052)=
 Sof(C95)=Sof(H06S)=Sof(C91)=FVAR(2)
 Sof(H04J)=Sof(H04K)=Sof(C15B)=Sof(H05G)=Sof(C16B)=Sof(H26)=Sof(C17B)=Sof(H1V)=
 Sof(C18B)=Sof(H1W)=Sof(C14B)=Sof(H1X)=Sof(C13B)=1-FVAR(3)
 Sof(H04B)=Sof(H04I)=Sof(C175)=Sof(C177)=Sof(H05F)=Sof(C176)=Sof(H05H)=
 Sof(C178)=Sof(H05T)=Sof(C180)=Sof(H063)=Sof(C179)=Sof(H066)=FVAR(3)
 Sof(H06H)=Sof(H06K)=Sof(C1B)=Sof(C6B)=Sof(H87B)=Sof(C5B)=Sof(H65B)=Sof(C4B)=
 Sof(H43B)=Sof(C3B)=Sof(H06W)=Sof(C2B)=Sof(H53B)=1-FVAR(4)
 Sof(H06E)=Sof(H06G)=Sof(C127)=Sof(C132)=Sof(H87A)=Sof(C131)=Sof(H65A)=
 Sof(C130)=Sof(H43A)=Sof(C129)=Sof(H06V)=Sof(C128)=Sof(H53A)=FVAR(4)
 Sof(C160)=Sof(H04X)=Sof(C161)=Sof(C157)=Sof(H04W)=Sof(C158)=Sof(H04Y)=
 Sof(C159)=Sof(H059)=Sof(C162)=Sof(H07C)=Sof(H07D)=Sof(C166)=Sof(H8)=Sof(C167)=
 Sof(H9)=Sof(C168)=Sof(H10)=Sof(C163)=1-FVAR(5)
 Sof(C8B)=Sof(H07M)=Sof(C9B)=Sof(H34)=Sof(C10B)=Sof(H05J)=Sof(C7B)=Sof(C194)=
 Sof(H28A)=Sof(H28B)=Sof(C195)=Sof(H14)=Sof(C201)=Sof(C197)=Sof(H18)=Sof(C196)=
 Sof(H17)=Sof(C198)=Sof(H16)=FVAR(5)
 Fixed Sof: Cl1(0.5) H04R(0.5) H04S(0.5) H6B(0.75) H6A(0.25) H12A(0.75)
 H12(0.25) Cl4(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C66(H02B,H02C), C54(H03A,H03C), C186(H03G,H03J), C174(H04B,H04I), C174(H04J,
 H04K), C90(H04R,H04S), C78(H06A,H06B), C102(H06C,H06D), C150(H07A,H07B),
 C162(H07C,H07D), C138(H5AA,H5AB), C138(H5BC,H5BD), C194(H28A,H28B), C126(H06E,
 H06G), C126(H06H,H06K), C114(H27A,H27B)
7.b Aromatic/amide H refined with riding coordinates:
 C37(H01M), C38(H01N), C11(H01T), C12(H01Y), C49(H025), C42(H028), C45(H02A),
 C137(H02G), C30(H02I), C31(H02J), C20(H02L), C61(H02M), C43(H02N), C27(H02P),
 C135(H02R), C50(H02S), C19(H02T), C184(H02U), C35(H02W), C60(H02X), C169(H02Y),
  C34(H030), C133(H031), C58(H033), C52(H034), C46(H035), C183(H037),
 C172(H03B), C23(H03D), C68(H03E), C56(H03F), C59(H03H), C64(H03I), C98(H03M),
 C124(H03N), C22(H03O), C28(H03Q), C99(H03S), C88(H03T), C87(H05U), C86(H06F),
 C85(H03K), C69(H03U), C51(H03V), C75(H03W), C14(H03X), C73(H03Z), C192(H040),
 C72(H041), C171(H043), C170(H044), C70(H045), C15(H046), C100(H047),
 C134(H048), C182(H049), C57(H04A), C112(H04C), C191(H04D), C4(H04E),
 C181(H04F), C3(H04G), C74(H04H), C7(H04L), C6(H04M), C97(H04N), C111(H04O),
 C122(H04P), C62(H04Q), C148(H04T), C109(H04U), C123(H04V), C160(H04X),
 C157(H04W), C158(H04Y), C159(H059), C76(H04Z), C110(H050), C121(H053),
 C71(H056), C147(H057), C145(H05A), C190(H05B), C177(H05F), C176(H05H),
 C63(H05I), C146(H05O), C178(H05T), C96(H05X), C92(H065), C93(H15), C94(H052),
 C95(H06S), C189(H05Z), C180(H063), C179(H066), C188(H067), C8B(H07M), C9B(H34),
  C10B(H05J), C81(H120), C80(H07E), C84(H21), C83(H229), C82(H99), C144(H3),
 C140(H06I), C141(H05R), C142(H055), C143(H060), C30B(H3A), C26B(H06J),
 C27B(H05S), C28B(H2), C29B(H4), C11B(H6B), C11B(H6A), C166(H8), C167(H9),
 C168(H10), C12B(H12A), C12B(H12), C195(H14), C197(H18), C196(H17), C198(H16),
 C24B(H05Y), C23B(H20), C22B(H327), C21B(H15A), C20B(H1C), C132(H87A),
 C131(H65A), C130(H43A), C129(H06V), C128(H53A), C152(H24), C153(H198),
 C154(H42), C155(H55), C156(H111), C108(H1G), C107(H1H), C106(H1I), C105(H1J),
 C104(H1K), C15B(H05G), C16B(H26), C17B(H1V), C18B(H1W), C14B(H1X), C6B(H87B),
 C5B(H65B), C4B(H43B), C3B(H06W), C2B(H53B), C119(H1M), C120(H1N), C116(H1P),
 C117(H1Q), C118(H1R)
7.c Fitted pentagon refined as free rotating group:
 C88(C87,C86,C85,C89), C160(C161,C157,C158,C159), C195(C201,C197,C196,C198)
7.d Fitted hexagon refined as free rotating group:
 C96(C19B,C92,C93,C94,C95), C81(C80,C79,C84,C83,C82), C144(C139,C140,C141,C142,
 C143), C30B(C25B,C26B,C27B,C28B,C29B), C91(C24B,C23B,C22B,C21B,C20B),
 C127(C132,C131,C130,C129,C128), C152(C153,C154,C155,C156,C151), C1B(C6B,C5B,
 C4B,C3B,C2B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 5912 electrons were 
found in a volume of 21416\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
16[C3H7NO], 10[H2O] per Asymmetric Unit 
which account for 5920 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46001
_shelx_hkl_checksum              86514
_shelx_fab_checksum              45476
_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 1.363
_oxdiff_exptl_absorpt_empirical_full_min 0.783