Development of sterically hindered siloxide-functionalized polyoxotungstates for the complexation of 5d-metals.
Auvray, Thomas; Nachtigall, Olaf; Brennessel, William W.; Jones, William D.; Matson, Ellen M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4300–4310; doi:10.1039/d1dt00256b

data_7706757
_publ_section_title
;
 Development of sterically hindered siloxide-functionalized
 polyoxotungstates for the complexation of 5d-metals.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4300
_journal_page_last               4310
_journal_paper_doi               10.1039/d1dt00256b
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         '1(C36 H30 O37 P Si3 W9), 3(C24 H52 N)'
_chemical_formula_sum            'C108 H186 N3 O37 P Si3 W9'
_chemical_formula_weight         3888.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-01-25 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.2815(2)
_cell_length_b                   31.4764(2)
_cell_length_c                   28.51028(19)
_cell_measurement_reflns_used    151374
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.2600
_cell_measurement_theta_min      2.5250
_cell_volume                     27174.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.931
_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    -23.00  12.00   0.50    1.73    --  -49.75  32.00  67.00   70
  2  \w     -5.00  23.00   0.50    1.73    --  -49.75  19.00  90.00   56
  3  \w    -30.00  13.00   0.50    1.73    --  -49.75  57.00 -60.00   86
  4  \w     -4.00  24.00   0.50    1.73    --  -49.75  19.00 -90.00   56
  5  \w     -4.00  23.00   0.50    1.73    --  -49.75  19.00-150.00   54
  6  \w     -5.00  21.00   0.50    1.73    --  -49.75  19.00-180.00   52
  7  \w    -44.00 -19.00   0.50    6.93    --  -84.25  45.00-120.00   50
  8  \w    -38.00 -13.00   0.50    6.93    --  -84.25  45.00 -60.00   50
  9  \w    -62.00 -34.00   0.50    1.73    --  -49.75  57.00 -60.00   56
 10  \w    -80.00 -45.00   0.50    1.73    --  -49.75 125.00 -60.00   70
 11  \w     61.00 118.00   0.50    1.73    --   49.75  32.00  67.00  114
 12  \w    117.00 178.00   0.50    6.93    --  105.75  32.00  67.00  122
 13  \w    128.00 155.00   0.50    6.93    --  105.75  77.00  90.00   54
 14  \w     98.00 178.00   0.50    6.93    --  105.75  30.00   0.00  160
 15  \w    126.00 172.00   0.50    6.93    --  105.75  15.00 -60.00   92
 16  \w    135.00 178.00   0.50    6.93    --  105.75  77.00-150.00   86
 17  \w    116.00 178.00   0.50    6.93    --  105.75  30.00-180.00  124
 18  \w    117.00 162.00   0.50    6.93    --  105.75 125.00-180.00   90
 19  \w     96.00 160.00   0.50    6.93    --  105.75 125.00-150.00  128
 20  \w     87.00 177.00   0.50    6.93    --  105.75  77.00 -90.00  180
 21  \w     98.00 164.00   0.50    6.93    --  105.75  30.00  30.00  132
 22  \w    107.00 174.00   0.50    6.93    --  105.75  15.00 150.00  134
 23  \w    103.00 162.00   0.50    6.93    --  105.75 125.00   0.00  118
 24  \w     85.00 116.00   0.50    6.93    --  105.75  77.00-150.00   62
 25  \w     35.00  75.00   0.50    6.93    --  105.75 -61.00 -30.00   80
 26  \w     78.00 104.00   0.50    6.93    --  105.75 -94.00 -90.00   52
 27  \w     66.00  92.00   0.50    6.93    --  105.75-125.00-180.00   52
 28  \w     62.00 105.00   0.50    6.93    --  105.75 -94.00-180.00   86
 29  \w     44.00  69.00   0.50    6.93    --  105.75-125.00 -60.00   50
 30  \w     39.00  64.00   0.50    6.93    --  105.75-125.00 -30.00   50
 31  \w     46.00  72.00   0.50    6.93    --  105.75-125.00 -90.00   52
 32  \w     39.00 105.00   0.50    6.93    --  105.75 -94.00-150.00  132
 33  \w     36.00  70.00   0.50    6.93    --  105.75 -94.00 -90.00   68
 34  \w     39.00  87.00   0.50    6.93    --  105.75-125.00-150.00   96
 35  \w     34.00  63.00   0.50    6.93    --  105.75-125.00-120.00   58
 36  \w     37.00 106.00   0.50    6.93    --  105.75 -94.00 -60.00  138
 37  \w     36.00  97.00   0.50    6.93    --  105.75 -94.00   0.00  122
 38  \w     68.00 106.00   0.50    6.93    --  105.75 -94.00  90.00   76
 39  \w     75.00 106.00   0.50    6.93    --  105.75 -94.00 120.00   62
 40  \w     40.00 104.00   0.50    6.93    --  105.75 -94.00 150.00  128
 41  \w     48.00  74.00   0.50    6.93    --  105.75 -61.00 150.00   52
 42  \w     48.00  73.00   0.50    6.93    --  105.75 -61.00 120.00   50
 43  \w     35.00 105.00   0.50    6.93    --  105.75 -94.00  60.00  140
 44  \w     36.00 106.00   0.50    6.93    --  105.75 -94.00 -30.00  140
 45  \w     47.00  75.00   0.50    6.93    --  105.75 -61.00-120.00   56
 46  \w     34.00 105.00   0.50    6.93    --  105.75 -94.00-120.00  142
 47  \w     38.00  68.00   0.50    6.93    --  105.75 -61.00   0.00   60
 48  \w     34.00  59.00   0.50    6.93    --  105.75 -61.00  30.00   50
 49  \w     -1.00  24.00   0.50    1.73    --   49.75 -32.00 -91.00   50
 50  \w    -19.00   8.00   0.50    1.73    --   49.75 -19.00-120.00   54
 51  \w     21.00  81.00   0.50    1.73    --   49.75 -99.00-150.00  120
 52  \w     86.00 126.00   0.50    6.93    --  105.75  77.00  90.00   80
 53  \w     43.00  83.00   0.50    6.93    --  105.75-125.00 150.00   80
 54  \w    -81.00 -41.00   0.50    1.73    --  -49.75 -32.00 -91.00   80
 55  \w   -106.00 -74.00   0.50    1.73    --  -49.75-125.00-150.00   64
 56  \w   -115.00 -63.00   0.50    6.93    --  -84.25 -77.00-150.00  104
 57  \w   -120.00 -86.00   0.50    1.73    --  -49.75 -32.00 -91.00   68
 58  \w   -140.00-115.00   0.50    6.93    --  -84.25 -32.00 -91.00   50
;
_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      0.0212499000
_diffrn_orient_matrix_UB_12      0.0244850000
_diffrn_orient_matrix_UB_13      -0.0409312000
_diffrn_orient_matrix_UB_21      -0.0043660000
_diffrn_orient_matrix_UB_22      -0.0396240000
_diffrn_orient_matrix_UB_23      -0.0314140000
_diffrn_orient_matrix_UB_31      -0.0460361000
_diffrn_orient_matrix_UB_32      0.0150582000
_diffrn_orient_matrix_UB_33      -0.0159451000
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            504469
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         89.915
_diffrn_reflns_theta_min         2.550
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             14992
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.015
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.028(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3009
_refine_ls_number_reflns         57366
_refine_ls_number_restraints     2656
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+147.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                51756
_reflns_number_total             57366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00256b2.cif
_cod_data_source_block           jonon28
_cod_depositor_comments
'Adding full bibliography for 7706755--7706757.cif.'
_cod_original_cell_volume        27174.7(4)
_cod_database_code               7706757
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.326
_shelx_estimated_absorpt_t_min   0.229
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.972(12)
 0.028(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C73-C74 = C74-C75 = C75-C76 = C76-C77 = C77-C78 = C79-C80 = C80-C81 = C81-C82
 = C82-C83 = C83-C84 = C85-C86 = C86-C87 = C87-C88 = C88-C89 = C89-C90 = C91-
 C92 = C92-C93 = C93-C94 = C94-C95 = C95-C96
 1.52 with sigma of 0.03
 C97-C98 = C98-C99 = C99-C100 = C100-C101 = C101-C102 = C103-C104 = C104-C105 =
  C105-C106 = C106-C107 = C107-C108 = C109-C110 = C110-C111 = C111-C112 = C112-
 C113 = C113-C114 = C115-C116 = C116-C117 = C117-C118 = C118-C119 = C119-C120
 1.52 with sigma of 0.03
 C121-C122 = C122-C123 = C123-C124 = C124-C125 = C125-C126 = C127-C128 = C128-
 C129 = C129-C130 = C130-C131 = C131-C132 = C133-C134 = C134-C135 = C135-C136 =
 C136-C137 = C137-C138 = C139-C140 = C140-C141 = C141-C142 = C142-C143 = C143-
 C144
 1.52 with sigma of 0.03
 C145-C146 = C146-C147 = C147-C148 = C148-C149 = C149-C150 = C151-C152 = C152-
 C153 = C153-C154 = C154-C155 = C155-C156 = C157-C158 = C158-C159 = C159-C160 =
 C160-C161 = C161-C162 = C163-C164 = C164-C165 = C165-C166 = C166-C167 = C167-
 C168
 1.52 with sigma of 0.03
 C169-C170 = C170-C171 = C171-C172 = C172-C173 = C173-C174 = C175-C176 = C176-
 C177 = C177-C178 = C178-C179 = C179-C180 = C181-C182 = C182-C183 = C183-C184 =
 C184-C185 = C185-C186 = C187-C188 = C188-C189 = C189-C190 = C190-C191 = C191-
 C192
 1.52 with sigma of 0.03
 C193-C194 = C194-C195 = C195-C196 = C196-C197 = C197-C198 = C199-C200 = C200-
 C201 = C201-C202 = C202-C203 = C203-C204 = C205-C206 = C206-C207 = C207-C208 =
 C208-C209 = C209-C210 = C211-C212 = C212-C213 = C213-C214 = C214-C215 = C215-
 C216
 1.52 with sigma of 0.03
 C42-C43 \\sim C42-C43'
 with sigma of 0.01
 C66-C67 \\sim C66'-C67'
 with sigma of 0.01
 C73-C79 \\sim C73-C85 \\sim C73-C91 \\sim C79-C85 \\sim C79-C91 \\sim C85-C91
 with sigma of 0.06
 C97-C103 \\sim C97-C109 \\sim C97-C115 \\sim C103-C109 \\sim C103-C115 \\sim
C109-C115
 with sigma of 0.06
 C121-C127 \\sim C121-C133 \\sim C121-C139 \\sim C127-C133 \\sim C127-C139
\\sim C133-C139
 with sigma of 0.06
 C145-C151 \\sim C145-C157 \\sim C145-C163 \\sim C151-C157 \\sim C151-C163
\\sim C157-C163
 with sigma of 0.06
 C169-C175 \\sim C169-C181 \\sim C169-C187 \\sim C175-C181 \\sim C175-C187
\\sim C181-C187
 with sigma of 0.06
 C193-C199 \\sim C193-C205 \\sim C193-C211 \\sim C199-C205 \\sim C199-C211
\\sim C205-C211
 with sigma of 0.06
4. Restrained planarity
 C43, C45, C47, C44, C46, C48
 with sigma of 0.02
 C43', C45', C47', C44', C46', C48'
 with sigma of 0.02
 C61, C63, C65, C62, C64, C66
 with sigma of 0.02
 C61', C63', C65', C62', C64', C66'
 with sigma of 0.02
 C67, C69, C71, C68, C70, C72
 with sigma of 0.02
 C67', C69', C71', C68', C70', C72'
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
C72 \\sim C72': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C102) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C144) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(N1) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq,
Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96)
\\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C145) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C150) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq,
Uanis(C157) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq,
Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(C175) \\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(C178) \\sim Ueq, Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq,
Uanis(C181) \\sim Ueq, Uanis(C182) \\sim Ueq, Uanis(C183) \\sim Ueq,
Uanis(C184) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq,
Uanis(C187) \\sim Ueq, Uanis(C188) \\sim Ueq, Uanis(C189) \\sim Ueq,
Uanis(C190) \\sim Ueq, Uanis(C191) \\sim Ueq, Uanis(C192) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C193) \\sim Ueq, Uanis(C194) \\sim Ueq, Uanis(C195) \\sim Ueq,
Uanis(C196) \\sim Ueq, Uanis(C197) \\sim Ueq, Uanis(C198) \\sim Ueq,
Uanis(C199) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq,
Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq,
Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(C208) \\sim Ueq, Uanis(C209) \\sim Ueq, Uanis(C210) \\sim Ueq,
Uanis(C211) \\sim Ueq, Uanis(C212) \\sim Ueq, Uanis(C213) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq: with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C43) = Uanis(C43') = Uanis(C46) = Uanis(C46')
Uanis(C44) = Uanis(C44') = Uanis(C47) = Uanis(C47')
Uanis(C45) = Uanis(C45') = Uanis(C48) = Uanis(C48')
6. Rigid body (RIGU) restrains
 C61, C62, C63, C64, C65, C66, C67, C68, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61', C62', C63', C64', C65', C66', C67', C68', C69', C70', C71', C72'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82, C83, C84, C85, C86, C87,
  C88, C89, C90, C91, C92, C93, C94, C95, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108, C109,
  C110, C111, C112, C113, C114, C115, C116, C117, C118, C119, C120
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C121, C122, C123, C124, C125, C126, C127, C128, C129, C130, C131, C132,
 C133, C134, C135, C136, C137, C138, C139, C140, C141, C142, C143, C144
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C145, C146, C147, C148, C149, C150, C151, C152, C153, C154, C155, C156,
 C157, C158, C159, C160, C161, C162, C163, C164, C165, C166, C167, C168
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C169, C170, C171, C172, C173, C174, C175, C176, C177, C178, C179, C180,
 C181, C182, C183, C184, C185, C186, C187, C188, C189, C190, C191, C192
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C193, C194, C195, C196, C197, C198, C199, C200, C201, C202, C203, C204,
 C205, C206, C207, C208, C209, C210, C211, C212, C213, C214, C215, C216
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{C43, C48, C47, C46, C45, C44} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C43, C44, C45, C46, C47, C48}
{C43, C44, C45, C46, C47, C48} sigma for 1-2: 0.02, 1-3: 0.04
{C43', C48', C47', C46', C45', C44'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C43', C44', C45', C46', C47', C48'}
{C61, C66, C65, C64, C63, C62} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C61, C62, C63, C64, C65, C66}
{C67, C72, C71, C70, C69, C68} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C67, C68, C69, C70, C71, C72}
{C61, C62, C63, C64, C65, C66} sigma for 1-2: 0.02, 1-3: 0.04
{C61', C66', C65', C64', C63', C62'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C61', C62', C63', C64', C65', C66'}
{C67, C68, C69, C70, C71, C72} sigma for 1-2: 0.02, 1-3: 0.04
{C67', C72', C71', C70', C69', C68'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C67', C68', C69', C70', C71', C72'}
{N1, C79, C80, C81, C82, C83, C84} sigma for 1-2: 0.005, 1-3: 0.01
{N1, C85, C86, C87, C88, C89, C90} sigma for 1-2: 0.005, 1-3: 0.01
{N1, C91, C92, C93, C94, C95, C96} sigma for 1-2: 0.005, 1-3: 0.01
as in
{N1, C73, C74, C75, C76, C77, C78}
{N2, C103, C104, C105, C106, C107, C108} sigma for 1-2: 0.005, 1-3: 0.01
{N2, C109, C110, C111, C112, C113, C114} sigma for 1-2: 0.005, 1-3: 0.01
{N2, C115, C116, C117, C118, C119, C120} sigma for 1-2: 0.005, 1-3: 0.01
as in
{N2, C97, C98, C99, C100, C101, C102}
{N3, C127, C128, C129, C130, C131, C132} sigma for 1-2: 0.005, 1-3: 0.01
{N3, C133, C134, C135, C136, C137, C138} sigma for 1-2: 0.005, 1-3: 0.01
{N3, C139, C140, C141, C142, C143, C144} sigma for 1-2: 0.005, 1-3: 0.01
as in
{N3, C121, C122, C123, C124, C125, C126}
{N4, C151, C152, C153, C154, C155, C156} sigma for 1-2: 0.005, 1-3: 0.01
{N4, C157, C158, C159, C160, C161, C162} sigma for 1-2: 0.005, 1-3: 0.01
{N4, C163, C164, C165, C166, C167, C168} sigma for 1-2: 0.002, 1-3: 0.004
as in
{N4, C145, C146, C147, C148, C149, C150}
{N5, C175, C176, C177, C178, C179, C180} sigma for 1-2: 0.005, 1-3: 0.01
{N5, C181, C182, C183, C184, C185, C186} sigma for 1-2: 0.005, 1-3: 0.01
{N5, C187, C188, C189, C190, C191, C192} sigma for 1-2: 0.005, 1-3: 0.01
as in
{N5, C169, C170, C171, C172, C173, C174}
{N6, C199, C200, C201, C202, C203, C204} sigma for 1-2: 0.005, 1-3: 0.01
{N6, C205, C206, C207, C208, C209, C210} sigma for 1-2: 0.005, 1-3: 0.01
{N6, C211, C212, C213, C214, C215, C216} sigma for 1-2: 0.005, 1-3: 0.01
as in
{N6, C193, C194, C195, C196, C197, C198}
8. Others
 Sof(C43')=Sof(C44')=Sof(H44')=Sof(C45')=Sof(H45')=Sof(C46')=Sof(H46')=
 Sof(C47')=Sof(H47')=Sof(C48')=Sof(H48')=1-FVAR(1)
 Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(H47)=Sof(C48)=Sof(H48)=FVAR(1)
 Sof(C61')=Sof(C62')=Sof(H62')=Sof(C63')=Sof(H63')=Sof(C64')=Sof(H64')=
 Sof(C65')=Sof(H65')=Sof(C66')=Sof(C67')=Sof(C68')=Sof(H68')=Sof(C69')=
 Sof(H69')=Sof(C70')=Sof(H70')=Sof(C71')=Sof(H71')=Sof(C72')=Sof(H72')=1-FVAR(2)
 Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(C67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=
 Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72B)=FVAR(2)
 Fixed Sof: H35(0.5) H35A(0.5) H36(0.5) H36A(0.5) H37(0.5) H37A(0.5) H72(0.5)
 H72A(0.5) H73(0.5) H73A(0.5) H74(0.5) H74A(0.5)
 Fixed U11: C49(0.07914)
9.a Riding coordinates:
 O35(H35,H35A), O36(H36,H36A), O37(H37,H37A), O72(H72,H72A), O73(H73,H73A),
 O74(H74,H74A)
9.b Secondary CH2 refined with riding coordinates:
 C73(H73B,H73C), C74(H74B,H74C), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
 C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,
 H94B), C95(H95A,H95B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B),
 C100(H10A,H10B), C101(H10C,H10D), C103(H10H,H10I), C104(H10J,H10K), C105(H10L,
 H10M), C106(H10N,H10O), C107(H10P,H10Q), C109(H10U,H10V), C110(H11A,H11B),
 C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C115(H11L,H11M), C116(H11N,
 H11O), C117(H11P,H11Q), C118(H11R,H11S), C119(H11T,H11U), C121(H12D,H12E),
 C122(H12F,H12G), C123(H12H,H12I), C124(H12J,H12K), C125(H12L,H12M), C127(H12Q,
 H12R), C128(H12S,H12T), C129(H12U,H12V), C130(H13A,H13B), C131(H13C,H13D),
 C133(H13H,H13I), C134(H13J,H13K), C135(H13L,H13M), C136(H13N,H13O), C137(H13P,
 H13Q), C139(H13U,H13V), C140(H14A,H14B), C141(H14C,H14D), C142(H14E,H14F),
 C143(H14G,H14H), C145(H14L,H14M), C146(H14N,H14O), C147(H14P,H14Q), C148(H14R,
 H14S), C149(H14T,H14U), C151(H15D,H15E), C152(H15F,H15G), C153(H15H,H15I),
 C154(H15J,H15K), C155(H15L,H15M), C157(H15Q,H15R), C158(H15S,H15T), C159(H15U,
 H15V), C160(H16A,H16B), C161(H16C,H16D), C163(H16H,H16I), C164(H16J,H16K),
 C165(H16L,H16M), C166(H16N,H16O), C167(H16P,H16Q), C169(H16U,H16V), C170(H17A,
 H17B), C171(H17C,H17D), C172(H17E,H17F), C173(H17G,H17H), C175(H17L,H17M),
 C176(H17N,H17O), C177(H17P,H17Q), C178(H17R,H17S), C179(H17T,H17U), C181(H18D,
 H18E), C182(H18F,H18G), C183(H18H,H18I), C184(H18J,H18K), C185(H18L,H18M),
 C187(H18Q,H18R), C188(H18S,H18T), C189(H18U,H18V), C190(H19A,H19B), C191(H19C,
 H19D), C193(H19H,H19I), C194(H19J,H19K), C195(H19L,H19M), C196(H19N,H19O),
 C197(H19P,H19Q), C199(H19U,H19V), C200(H20A,H20B), C201(H20C,H20D), C202(H20E,
 H20F), C203(H20G,H20H), C205(H20L,H20M), C206(H20N,H20O), C207(H20P,H20Q),
 C208(H20R,H20S), C209(H20T,H20U), C211(H21D,H21E), C212(H21F,H21G), C213(H21H,
 H21I), C214(H21J,H21K), C215(H21L,H21M)
9.c Me refined with riding coordinates:
 C78(H78A,H78B,H78C), C84(H84A,H84B,H84C), C90(H90A,H90B,H90C), C96(H96A,H96B,
 H96C), C102(H10E,H10F,H10G), C108(H10R,H10S,H10T), C114(H11I,H11J,H11K),
 C120(H12A,H12B,H12C), C126(H12N,H12O,H12P), C132(H13E,H13F,H13G), C138(H13R,
 H13S,H13T), C144(H14I,H14J,H14K), C150(H15A,H15B,H15C), C156(H15N,H15O,H15P),
 C162(H16E,H16F,H16G), C168(H16R,H16S,H16T), C174(H17I,H17J,H17K), C180(H18A,
 H18B,H18C), C186(H18N,H18O,H18P), C192(H19E,H19F,H19G), C198(H19R,H19S,H19T),
 C204(H20I,H20J,H20K), C210(H21A,H21B,H21C), C216(H21N,H21O,H21P)
9.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
 C34(H34), C35(H35B), C36(H36B), C38(H38), C39(H39), C40(H40), C41(H41),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C44'(H44'), C45'(H45'),
 C46'(H46'), C47'(H47'), C48'(H48'), C50(H50), C51(H51), C52(H52), C53(H53),
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64),
  C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72B), C62'(H62'),
 C63'(H63'), C64'(H64'), C65'(H65'), C68'(H68'), C69'(H69'), C70'(H70'),
 C71'(H71'), C72'(H72')
;
_shelx_res_checksum              7035
_shelx_hkl_checksum              42823
_olex2_submission_original_sample_id jonon28
_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 2.007
_oxdiff_exptl_absorpt_empirical_full_min 0.433