A bifunctional molecular catalyst built up of l-proline grafted polyoxometalate for one-pot three-component green synthesis of heterocycles
Dai, Guoyong; Li, Qi; Zang, Dejin; Wei, Yongge; Green Chemistry 25 (2023) 6263–6269; doi:10.1039/D3GC00951C

data_7246941
_publ_section_title
;
 A bifunctional molecular catalyst built up of l-proline grafted
 polyoxometalate for one-pot three-component green synthesis of
 heterocycles
;
_journal_issue                   16
_journal_name_full               'Green Chemistry'
_journal_page_first              6263
_journal_page_last               6269
_journal_paper_doi               10.1039/D3GC00951C
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C28 H46 Mn Mo6 N4 O30, 2.5(C2 H3 N), 3(C16 H36 N)'
_chemical_formula_sum            'C81 H161.5 Mn Mo6 N9.5 O30'
_chemical_formula_weight         2379.27
_chemical_name_systematic        Boc-L-Pro-Mn-Anderson
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc26sc4j
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-09 deposited with the CCDC.	2023-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.708(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1600(5)
_cell_length_b                   14.7868(3)
_cell_length_c                   33.2539(11)
_cell_measurement_reflns_used    13983
_cell_measurement_temperature    109.3(8)
_cell_measurement_theta_max      70.7380
_cell_measurement_theta_min      3.6520
_cell_volume                     11541.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.3(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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   -111.00 -19.00   1.00    5.00    --  -40.81 -57.00  60.00   92
  2  \w    -69.00  30.00   1.00    5.00    --  -40.81  57.00-150.00   99
  3  \w    -85.00 -30.00   1.00    5.00    --  -40.81 125.00 -90.00   55
  4  \w    -64.00  33.00   1.00    5.00    --  -40.81  38.00   0.00   97
  5  \w    -64.00 -37.00   1.00    5.00    --  -40.81  77.00  30.00   27
  6  \w     85.00 173.00   1.00   15.00    --  100.91  45.00-180.00   88
  7  \w     29.00 130.00   1.00   15.00    --  100.91 -61.00  30.00  101
  8  \w     32.00 117.00   1.00   15.00    --  100.91 -77.00-180.00   85
  9  \w     30.00 107.00   1.00   15.00    --  100.91 -61.00 -90.00   77
 10  \w     74.00 109.00   1.00   15.00    --  100.91 -95.00 120.00   35
 11  \w     48.00 127.00   1.00   15.00    --  100.91 -45.00 150.00   79
 12  \w     25.00  51.00   1.00   15.00    --  100.91 -95.00 120.00   26
 13  \w     87.00 131.00   1.00   15.00    --  100.91  61.00 -30.00   44
 14  \w     86.00 117.00   1.00   15.00    --  100.91-125.00 -30.00   31
 15  \w     22.00 110.00   1.00   15.00    --  100.91 -95.00  30.00   88
 16  \w     35.00 156.00   1.00   15.00    --  100.91   0.00 -30.00  121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0339663000
_diffrn_orient_matrix_UB_12      0.0643172000
_diffrn_orient_matrix_UB_13      0.0216164000
_diffrn_orient_matrix_UB_21      -0.0439188000
_diffrn_orient_matrix_UB_22      -0.0754487000
_diffrn_orient_matrix_UB_23      0.0002919000
_diffrn_orient_matrix_UB_31      0.0349818000
_diffrn_orient_matrix_UB_32      -0.0322100000
_diffrn_orient_matrix_UB_33      0.0424730000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            81684
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.486
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             4924
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

;
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 8142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.070(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2338
_refine_ls_number_reflns         40519
_refine_ls_number_restraints     1245
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+54.4544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2342
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.851
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                28480
_reflns_number_total             40519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc00951c2.cif
_cod_data_source_block           exp_3691
_cod_depositor_comments
'Adding full bibliography for 7246941--7246942.cif.'
_cod_original_cell_volume        11541.6(5)
_cod_original_formula_sum        'C81 H161.50 Mn Mo6 N9.50 O30'
_cod_database_code               7246941
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Mn Mo C N O '
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.178
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C47-C48 = C48-C49 = C50-C49 = C50-C51
 1.54 with sigma of 0.02
 N8-C51 = N8-C48
 1.45 with sigma of 0.02
 C24-O29
 1.38 with sigma of 0.02
 N4-C24
 1.42 with sigma of 0.02
 C38-N7
 1.42 with sigma of 0.02
 O58-C38
 1.16 with sigma of 0.02
 O57-C38
 1.38 with sigma of 0.02
 C39-O57
 1.42 with sigma of 0.02
 O29-C25
 1.42 with sigma of 0.02
 C25-C27 = C25-C28
 1.54 with sigma of 0.02
 O59-C53
 1.42 with sigma of 0.02
 C53-C56 = C53-C54 = C53-C55
 1.54 with sigma of 0.02
 C24-O30
 1.16 with sigma of 0.02
 C40-C39 = C41-C39
 1.54 with sigma of 0.02
 C42-C39
 1.54 with sigma of 0.02
 N19-C161
 1.13 with sigma of 0.02
 C161-C162
 1.44 with sigma of 0.02
 C140-C139 = C138-C139
 1.54 with sigma of 0.02
 C95-C96 = C94-C95
 1.54 with sigma of 0.02
 C147-C148 = C146-C147
 1.54 with sigma of 0.02
 C71B-C72B = C71B-C70B = C70B-C69 = C69-C70A = C70A-C71A = C72A-C71A
 1.54 with sigma of 0.02
 C135-C134 = C1a-C134 = C136-C1a = C135-C1b
 1.54 with sigma of 0.02
 C63-C64A = C64B-C63
 1.54 with sigma of 0.02
 C99-C100 = C99-C98 = C97-C98
 1.54 with sigma of 0.02
 C144-C143 = C143-C142 = C142-C141
 1.54 with sigma of 0.02
 C91-C90 = C92-C91
 1.54 with sigma of 0.02
 C67-C68 = C67-C66
 1.54 with sigma of 0.02
 C103-C102
 1.54 with sigma of 0.02
 C103-C104
 1.54 with sigma of 0.02
 C83-C84 = C83-C82 = C81-C82
 1.54 with sigma of 0.02
 C88-C87 = C86-C87
 1.54 with sigma of 0.02
 C25-C26
 1.54 with sigma of 0.001
 N8-C52
 1.41 with sigma of 0.02
 C52-O59
 1.38 with sigma of 0.02
 C52-O60
 1.23 with sigma of 0.02
 C55-C56
 2.54 with sigma of 0.04
 O29-C28
 2.44 with sigma of 0.04
 C41-O57
 2.44 with sigma of 0.04
 C27-C28
 2.54 with sigma of 0.04
 O29-C27
 2.44 with sigma of 0.04
 O59-C55
 2.44 with sigma of 0.04
 O59-C56
 2.44 with sigma of 0.04
 C56-C54
 2.54 with sigma of 0.04
 C55-C54
 2.54 with sigma of 0.04
 O59-C54
 2.44 with sigma of 0.04
 C40-O57
 2.44 with sigma of 0.04
 C40-C41
 2.54 with sigma of 0.04
 C42-O57
 2.44 with sigma of 0.04
 C42-C41
 2.54 with sigma of 0.04
 C40-C42
 2.54 with sigma of 0.04
 C49-C51 = C50-C48
 2.54 with sigma of 0.04
 C47-N8
 2.45 with sigma of 0.04
 C49-C47
 2.55 with sigma of 0.04
 C48-C51
 2.4 with sigma of 0.04
 C26-C28
 2.54 with sigma of 0.04
 O29-C26
 2.44 with sigma of 0.04
 C27-C26
 2.54 with sigma of 0.04
 C48-C52
 2.58 with sigma of 0.04
 C52-C51
 2.52 with sigma of 0.04
 N8-O60
 2.3 with sigma of 0.04
 O60-O59
 2.28 with sigma of 0.04
3. Restrained planarity
 C34, N7, C37, C38, O57, O58
 with sigma of 0.1
 C48, N8, C52, O60, O59, C51
 with sigma of 0.1
4. Rigid bond restraints
 C33, O58, C34, N7, C35, O57, C37, C41, C38, C36, C39, C42, C40, O55, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11, C93, C94, C95, C96
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N14, C145, C146, C147, C148
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N14, C137, C138, C139, C140
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C72A, C71A, C70A, C69, C70B, C71B, C72B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C104, C103, C102, C101, N11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C84, C83, C82, C81, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88, C87, C86, C85, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C19, O26, C20, C21, C22, N4, C23, C24, O30, O29, C26, C27, C25, C28
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C56, C54, C55, C53, O59, O60, C52, N8, C50, C51, C49, C48, C47, O56, N6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
Uanis(O58) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(O55) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O58) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C145) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C149)
\\sim Ueq, Uanis(C141) \\sim Ueq, Uanis(C138) \\sim Ueq, Uanis(C146) \\sim Ueq,
Uanis(C150) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C139) \\sim Ueq,
Uanis(C147) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C143) \\sim Ueq,
Uanis(C152) \\sim Ueq, Uanis(C144) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C66) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C70B) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C71A) \\sim Ueq,
Uanis(C71B) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C64B)
\\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C112) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C105)
\\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C116) \\sim Ueq,
Uanis(C120) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C128) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C122)
\\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C125) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C134) \\sim Ueq,
Uanis(C126) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C131) \\sim Ueq,
Uanis(C135) \\sim Ueq, Uanis(C1a) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C132)
\\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C1b) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N19) \\sim Ueq, Uanis(C162) \\sim Ueq, Uanis(C161) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O47)
\\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C148) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C138) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C71B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C72B) \\sim Ueq, Uanis(C72A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C160) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C91)
\\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C104) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C86) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C88) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O29)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O30) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O30) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C24) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O56) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(O60) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(O59) \\sim Ueq,
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C70A) = Uanis(C70B)
Uanis(C71A) = Uanis(C71B)
6. Others
 Fixed Sof: C136(0.5) H13g(0.5) H13h(0.5) H13i(0.5) C71A(0.5) H71a(0.5)
 H71b(0.5) C70A(0.5) H70a(0.5) H70b(0.5) H69a(0.5) H69b(0.5) H69c(0.5)
 H69d(0.5) C64A(0.5) H64a(0.5) H64b(0.5) H64c(0.5) H13n(0.5) H13o(0.5)
 H13p(0.5) H13q(0.5) C71B(0.5) H71c(0.5) H71d(0.5) H63a(0.5) H63b(0.5)
 H63c(0.5) H63d(0.5) C70B(0.5) H70c(0.5) H70d(0.5) C64B(0.5) H64d(0.5)
 H64e(0.5) H64f(0.5) C135(0.5) H13t(0.5) H13u(0.5) C1a(0.5) H13v(0.5) H13w(0.5)
 C1b(0.5) H13x(0.5) H13y(0.5) Hd(0.5) C72B(0.5) H72a(0.5) H72b(0.5) H72c(0.5)
 C72A(0.5) H72d(0.5) H72e(0.5) H72f(0.5)
7.a Ternary CH refined with riding coordinates:
 C20(H20), C6(H6), C34(H34), C48(H48)
7.b Secondary CH2 refined with riding coordinates:
 C44(H44a,H44b), C1(H1a,H1b), C3(H3a,H3b), C17(H17a,H17b), C2(H2a,H2b),
 C15(H15a,H15b), C31(H31a,H31b), C29(H29a,H29b), C30(H30a,H30b), C121(H12d,
 H12e), C62(H62a,H62b), C109(H10a,H10b), C105(H10c,H10d), C58(H58a,H58b),
 C113(H11a,H11b), C57(H57a,H57b), C110(H11c,H11d), C137(H13z,H), C114(H11e,
 H11f), C97(H97a,H97b), C45(H45a,H45b), C117(H11g,H11h), C61(H61a,H61b),
 C16(H16a,H16b), C73(H73a,H73b), C150(H15c,H15d), C21(H21a,H21b), C129(H12f,
 H12g), C106(H10e,H10f), C145(H14d,H14e), C149(H14f,H14g), C133(H13j,H13k),
 C141(H14h,H14i), C125(H12k,H12l), C118(H11l,H11m), C79(H79a,H79b), C127(H12m,
 H12n), C35(H35a,H35b), C43(H43a,H43b), C75(H75a,H75b), C66(H66a,H66b), C9(H9a,
 H9b), C7(H7a,H7b), C115(H11n,H11o), C142(H14j,H14k), C111(H11p,H11q),
 C71A(H71a,H71b), C119(H11r,H11s), C65(H65a,H65b), C70A(H70a,H70b), C69(H69a,
 H69b), C69(H69c,H69d), C126(H12o,H12p), C59(H59a,H59b), C138(H13,Ha),
 C123(H12q,H12r), C89(H89a,H89b), C146(H14l,H14m), C99(H99a,H99b), C101(H10l,
 H10m), C67(H67a,H67b), C130(H13l,H13m), C107(H10g,H10h), C77(H77a,H77b),
 C98(H98a,H98b), C37(H37a,H37b), C134(H13n,H13o), C134(H13p,H13q), C81(H81a,
 H81b), C85(H85a,H85b), C93(H93a,H93b), C131(H13r,H13s), C82(H82a,H82b),
 C143(H14n,H14o), C8(H8a,H8b), C147(H14p,H14q), C87(H87a,H87b), C90(H90a,H90b),
 C22(H22a,H22b), C86(H86a,H86b), C83(H83a,H83b), C74(H74a,H74b), C122(H12v,
 H12w), C91(H91a,H91b), C71B(H71c,H71d), C151(H15e,H15f), C78(H78a,H78b),
 C102(H10n,H10o), C139(H0aa,Hc), C23(H23a,H23b), C63(H63a,H63b), C63(H63c,H63d),
  C36(H36a,H36b), C70B(H70c,H70d), C49(H49a,H49b), C135(H13t,H13u), C1a(H13v,
 H13w), C94(H94a,H94b), C51(H51a,H51b), C50(H50a,H50b), C103(H10v,H10w),
 C95(H95a,H95b)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), N5(H5), N6(H6a)
7.d Idealised Me refined with riding coordinates:
 C158(H15m,H15n,H15o), C116(H11i,H11j,H11k), C156(H15j,H15k,H15l), C132(H13d,
 H13e,H13f), C136(H13g,H13h,H13i), C128(H12h,H12i,H12j), C13(H13a,H13b,H13c),
 C68(H68a,H68b,H68c), C64A(H64a,H64b,H64c), C76(H76a,H76b,H76c), C124(H12s,H12t,
 H12u), C14(H14a,H14b,H14c), C112(H11t,H11u,H11v), C40(H40a,H40b,H40c),
 C154(H15p,H15q,H15r), C108(H10i,H10j,H10k), C160(H16c,H16d,H16e), C88(H88a,
 H88b,H88c), C80(H80a,H80b,H80c), C144(H14r,H14s,H14t), C41(H41a,H41b,H41c),
 C162(H16f,H16g,H16h), C120(H12x,H12y,Hb), C60(H60a,H60b,H60c), C12(H12a,H12b,
 H12c), C26(H26a,H26b,H26c), C152(H15g,H15h,H15i), C27(H27a,H27b,H27c),
 C28(H28a,H28b,H28c), C64B(H64d,H64e,H64f), C42(H42a,H42b,H42c), C92(H92a,H92b,
 H92c), C84(H84a,H84b,H84c), C1b(H13x,H13y,Hd), C104(H10p,H10q,H10r), C100(H10s,
 H10t,H10u), C55(H55a,H55b,H55c), C54(H54a,H54b,H54c), C56(H56a,H56b,H56c),
 C148(H14u,H14v,H14w), C72B(H72a,H72b,H72c), C96(H96a,H96b,H96c), C72A(H72d,
 H72e,H72f), C140(H14x,H14y,He)
;