Synthesis of NiII porphyrin—NiII 5,15-diazaporphyrin hybrid tapes
Wang, Lina; Liao, Zian; Lin, Peng; Jia, Yingying; Liu, Le; Xu, Ling; Zhou, Mingbo; Yin, Bangshao; Rao, Yutao; Nakai, Akito; Tanaka, Takayuki; Shimizu, Daiki; Osuka, Atsuhiro; Song, Jianxin; Chemical Science 15 (2024) 10207–10213; doi:10.1039/D4SC01450B

data_1571717
_publ_section_title
;
 Synthesis of NiII porphyrin---NiII 5,15-diazaporphyrin hybrid tapes
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              10207
_journal_page_last               10213
_journal_paper_doi               10.1039/D4SC01450B
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C480 H487 Cl3 N42 Ni9'
_chemical_formula_sum            'C480 H487 Cl3 N42 Ni9'
_chemical_formula_weight         7478.83
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-08 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                104.2487(11)
_cell_angle_beta                 96.2653(12)
_cell_angle_gamma                105.3083(13)
_cell_formula_units_Z            1
_cell_length_a                   19.8298(3)
_cell_length_b                   27.6668(4)
_cell_length_c                   28.8267(4)
_cell_measurement_reflns_used    42880
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.0770
_cell_measurement_theta_min      3.9490
_cell_volume                     14526.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     21.00  91.00   1.00    3.00    --   36.54  57.00  60.00   70
  2  \w     76.00 105.00   1.00    3.00    --   36.54  38.00  60.00   29
  3  \w     75.00 105.00   1.00    3.00    --   36.54  38.00  30.00   30
  4  \w     71.00 104.00   1.00    3.00    --   36.54  77.00  60.00   33
  5  \w     63.00  90.00   1.00    3.00    --   36.54  57.00 -30.00   27
  6  \w     72.00 104.00   1.00    3.00    --   36.54  57.00 -60.00   32
  7  \w     73.00 100.00   1.00    3.00    --   36.54  57.00-120.00   27
  8  \w     72.00 104.00   1.00    3.00    --   36.54  38.00-120.00   32
  9  \w     66.00 100.00   1.00    3.00    --   36.54  77.00-120.00   34
 10  \w     55.00 104.00   1.00    3.00    --   36.54  77.00 -60.00   49
 11  \w     66.00 103.00   1.00    3.00    --   36.54  19.00 -60.00   37
 12  \w     56.00  93.00   1.00    3.00    --   36.54  38.00 -60.00   37
 13  \w     39.00 106.00   1.00    3.00    --   36.54  19.00-120.00   67
 14  \w     30.00  55.00   1.00    3.00    --   36.54 -38.00-120.00   25
 15  \w     19.00  54.00   1.00    3.00    --   36.54 -77.00 -60.00   35
 16  \w     65.00  90.00   1.00    3.00    --   36.54-125.00   0.00   25
 17  \w     57.00  88.00   1.00    3.00    --   36.54-125.00  60.00   31
 18  \w     49.00  86.00   1.00    3.00    --   36.54-125.00 120.00   37
 19  \w     35.00  60.00   1.00    3.00    --   36.54 -77.00 150.00   25
 20  \w     16.00  54.00   1.00    3.00    --   36.54 -38.00  90.00   38
 21  \w     24.00  57.00   1.00    3.00    --   36.54 -77.00  30.00   33
 22  \w     24.00  51.00   1.00    3.00    --   36.54-125.00   0.00   27
 23  \w     24.00  56.00   1.00    3.00    --   36.54-125.00  60.00   32
 24  \w     20.00  51.00   1.00    3.00    --   36.54 -57.00 -30.00   31
 25  \w      9.00  38.00   1.00    3.00    --   36.54 -57.00-120.00   29
 26  \w     13.00  49.00   1.00    3.00    --   36.54 -57.00-150.00   36
 27  \w     15.00  60.00   1.00    3.00    --   36.54 -77.00-180.00   45
 28  \w     21.00  71.00   1.00    3.00    --   36.54 -99.00-120.00   50
 29  \w     14.00  43.00   1.00    3.00    --   36.54 -38.00-180.00   29
 30  \w      8.00  35.00   1.00    3.00    --   36.54  19.00-120.00   27
 31  \w     18.00  65.00   1.00    3.00    --   36.54  38.00-120.00   47
 32  \w     26.00  71.00   1.00    3.00    --   36.54  57.00-120.00   45
 33  \w     19.00  47.00   1.00    3.00    --   36.54  38.00 -60.00   28
 34  \w     20.00  52.00   1.00    3.00    --   36.54  57.00 -30.00   32
 35  \w     19.00  67.00   1.00    3.00    --   36.54  38.00  30.00   48
 36  \w     60.00 104.00   1.00    3.00    --   36.54  57.00 120.00   44
 37  \w     61.00  87.00   1.00    3.00    --   36.54  77.00 150.00   26
 38  \w     40.00  67.00   1.00    3.00    --   36.54  77.00 120.00   27
 39  \w     27.00  80.00   1.00    3.00    --   36.54  57.00 150.00   53
 40  \w     23.00  66.00   1.00    3.00    --   36.54  38.00  60.00   43
 41  \w     22.00  57.00   1.00    3.00    --   36.54  57.00 120.00   35
 42  \w     12.00  48.00   1.00    3.00    --   36.54  77.00 150.00   36
 43  \w     22.00  68.00   1.00    3.00    --   36.54  57.00 -60.00   46
 44  \w     10.00  40.00   1.00    3.00    --   36.54  77.00 -60.00   30
 45  \w     12.00  39.00   1.00    3.00    --   36.54  77.00   0.00   27
 46  \w     11.00  63.00   1.00    3.00    --   36.54  77.00  60.00   52
 47  \w     11.00  36.00   1.00    3.00    --   36.54  77.00 120.00   25
 48  \w      1.00  26.00   1.00    3.00    --   36.54  92.00 168.99   25
 49  \w     92.00 127.00   1.00   16.00    --  111.00  63.00 150.00   35
 50  \w    128.00 178.00   1.00   16.00    --  111.00  50.00 150.00   50
 51  \w    141.00 175.00   1.00   16.00    --  111.00  50.00 120.00   34
 52  \w    152.00 177.00   1.00   16.00    --  111.00  38.00  30.00   25
 53  \w    152.00 177.00   1.00   16.00    --  111.00  38.00   0.00   25
 54  \w    144.00 175.00   1.00   16.00    --  111.00  77.00 -30.00   31
 55  \w    139.00 166.00   1.00   16.00    --  111.00  77.00  30.00   27
 56  \w    131.00 177.00   1.00   16.00    --  111.00  77.00   0.00   46
 57  \w    131.00 169.00   1.00   16.00    --  111.00  25.00   0.00   38
 58  \w    130.00 178.00   1.00   16.00    --  111.00  25.00  60.00   48
 59  \w    126.00 176.00   1.00   16.00    --  111.00  77.00 -60.00   50
 60  \w    126.00 153.00   1.00   16.00    --  111.00  50.00-150.00   27
 61  \w    122.00 178.00   1.00   16.00    --  111.00  77.00-150.00   56
 62  \w    122.00 176.00   1.00   16.00    --  111.00  77.00-120.00   54
 63  \w    122.00 177.00   1.00   16.00    --  111.00  77.00-180.00   55
 64  \w    118.00 178.00   1.00   16.00    --  111.00  77.00 -90.00   60
 65  \w    117.00 175.00   1.00   16.00    --  111.00  77.00  60.00   58
 66  \w    120.00 177.00   1.00   16.00    --  111.00  77.00  90.00   57
 67  \w     92.00 130.00   1.00   16.00    --  111.00  63.00 -30.00   38
 68  \w     95.00 122.00   1.00   16.00    --  111.00  50.00 -90.00   27
 69  \w     94.00 121.00   1.00   16.00    --  111.00  50.00 -60.00   27
 70  \w     94.00 139.00   1.00   16.00    --  111.00  50.00   0.00   45
 71  \w     95.00 126.00   1.00   16.00    --  111.00  50.00  60.00   31
 72  \w     92.00 118.00   1.00   16.00    --  111.00  63.00 120.00   26
 73  \w     95.00 122.00   1.00   16.00    --  111.00  50.00 150.00   27
 74  \w     94.00 120.00   1.00   16.00    --  111.00  50.00 120.00   26
 75  \w     95.00 120.00   1.00   16.00    --  111.00  50.00  90.00   25
 76  \w     92.00 118.00   1.00   16.00    --  111.00  63.00  90.00   26
 77  \w     92.00 118.00   1.00   16.00    --  111.00  38.00  90.00   26
 78  \w     92.00 120.00   1.00   16.00    --  111.00  38.00 120.00   28
 79  \w     92.00 118.00   1.00   16.00    --  111.00  38.00 150.00   26
 80  \w     84.00 110.00   1.00   16.00    --  111.00  77.00 120.00   26
 81  \w     84.00 110.00   1.00   16.00    --  111.00  77.00  90.00   26
 82  \w     92.00 118.00   1.00   16.00    --  111.00  63.00  60.00   26
 83  \w     92.00 133.00   1.00   16.00    --  111.00  38.00  30.00   41
 84  \w     92.00 125.00   1.00   16.00    --  111.00  38.00   0.00   33
 85  \w     92.00 119.00   1.00   16.00    --  111.00  63.00   0.00   27
 86  \w     92.00 138.00   1.00   16.00    --  111.00  63.00  30.00   46
 87  \w     92.00 118.00   1.00   16.00    --  111.00  63.00 -60.00   26
 88  \w     92.00 123.00   1.00   16.00    --  111.00  38.00 -30.00   31
 89  \w     92.00 126.00   1.00   16.00    --  111.00  63.00 -90.00   34
 90  \w     94.00 122.00   1.00   16.00    --  111.00  50.00-120.00   28
 91  \w     95.00 120.00   1.00   16.00    --  111.00  50.00-150.00   25
 92  \w     92.00 118.00   1.00   16.00    --  111.00  63.00-180.00   26
 93  \w     92.00 119.00   1.00   16.00    --  111.00  38.00-180.00   27
 94  \w     92.00 118.00   1.00   16.00    --  111.00  38.00-150.00   26
 95  \w     92.00 118.00   1.00   16.00    --  111.00  63.00-120.00   26
 96  \w     92.00 118.00   1.00   16.00    --  111.00  63.00-150.00   26
 97  \w     84.00 110.00   1.00   16.00    --  111.00  77.00-180.00   26
 98  \w     84.00 110.00   1.00   16.00    --  111.00  77.00-150.00   26
 99  \w     84.00 110.00   1.00   16.00    --  111.00  77.00-120.00   26
100  \w     84.00 110.00   1.00   16.00    --  111.00  77.00 -90.00   26
101  \w     84.00 110.00   1.00   16.00    --  111.00  77.00 -60.00   26
102  \w     84.00 110.00   1.00   16.00    --  111.00  77.00 -30.00   26
103  \w     84.00 110.00   1.00   16.00    --  111.00  77.00  30.00   26
104  \w     84.00 110.00   1.00   16.00    --  111.00  77.00   0.00   26
105  \w     93.00 120.00   1.00   16.00    --  111.00  38.00  60.00   27
106  \w     87.00 114.00   1.00   16.00    --  111.00  25.00   0.00   27
107  \w     86.00 113.00   1.00   16.00    --  111.00  25.00 -60.00   27
108  \w     89.00 116.00   1.00   16.00    --  111.00  25.00-120.00   27
109  \w     87.00 112.00   1.00   16.00    --  111.00  25.00-150.00   25
110  \w     88.00 115.00   1.00   16.00    --  111.00  25.00-180.00   27
111  \w     94.00 122.00   1.00   16.00    --  111.00 -50.00-120.00   28
112  \w    111.00 137.00   1.00   16.00    --  111.00 -77.00-150.00   26
113  \w     74.00 116.00   1.00   16.00    --  111.00-111.00-120.00   42
114  \w     43.00  89.00   1.00   16.00    --  111.00 -77.00-150.00   46
115  \w     55.00 111.00   1.00   16.00    --  111.00-111.00-150.00   56
116  \w     45.00  82.00   1.00   16.00    --  111.00 -50.00-120.00   37
117  \w     42.00 118.00   1.00   16.00    --  111.00 -91.00 -90.00   76
118  \w    109.00 136.00   1.00   16.00    --  111.00 -77.00  30.00   27
119  \w     87.00 114.00   1.00   16.00    --  111.00  25.00  60.00   27
120  \w     84.00 110.00   1.00   16.00    --  111.00  77.00  60.00   26
121  \w     84.00 178.00   1.00   16.00    --  111.00  77.00 150.00   94
122  \w     42.00 116.00   1.00   16.00    --  111.00-111.00  30.00   74
123  \w     56.00 116.00   1.00   16.00    --  111.00-111.00 120.00   60
124  \w     46.00  93.00   1.00   16.00    --  111.00 -77.00  30.00   47
125  \w     13.00  38.00   1.00    3.00    --   36.54  19.00 -60.00   25
126  \w     15.00  52.00   1.00    3.00    --   36.54  77.00-120.00   37
127  \w     10.00  75.00   1.00    3.00    --   36.54  77.00-180.00   65
128  \w     84.00 120.00   1.00   16.00    --  111.00 178.00-150.00   36
129  \w    -32.00  -5.00   1.00    3.00    --   36.54 -38.00-180.00   27
130  \w    -23.00   3.00   1.00    3.00    --   36.54 -77.00-180.00   26
131  \w    -31.00  -3.00   1.00    3.00    --   36.54 -57.00-120.00   28
132  \w    -29.00  -2.00   1.00    3.00    --   36.54 -57.00-150.00   27
133  \w    -32.00  16.00   1.00    3.00    --   36.54 -38.00-120.00   48
134  \w    -17.00  11.00   1.00    3.00    --   36.54 -77.00 -60.00   28
135  \w    -26.00  14.00   1.00    3.00    --   36.54 -57.00 -30.00   40
136  \w     -7.00  38.00   1.00    3.00    --   36.54 -57.00  30.00   45
137  \w      1.00  73.00   1.00    3.00    --   36.54 -99.00 120.00   72
138  \w    -31.00  16.00   1.00    3.00    --   36.54 -77.00 150.00   47
139  \w    -20.00   9.00   1.00    3.00    --   36.54 -38.00  90.00   29
140  \w    -27.00  20.00   1.00    3.00    --   36.54 -77.00  30.00   47
141  \w    -30.00  30.00   1.00    3.00    --   36.54 -57.00 150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0646928000
_diffrn_orient_matrix_UB_12      -0.0480441000
_diffrn_orient_matrix_UB_13      -0.0064299000
_diffrn_orient_matrix_UB_21      0.0069314000
_diffrn_orient_matrix_UB_22      -0.0213650000
_diffrn_orient_matrix_UB_23      -0.0533296000
_diffrn_orient_matrix_UB_31      0.0498773000
_diffrn_orient_matrix_UB_32      -0.0294418000
_diffrn_orient_matrix_UB_33      0.0162514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            302803
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         4.101
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.855
_exptl_crystal_description       block
_exptl_crystal_F_000             3964
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2621
_refine_ls_number_reflns         51221
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1912P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2645
_refine_ls_wR_factor_ref         0.2935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27353
_reflns_number_total             51221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01450b2.cif
_cod_data_source_block           6-Cl
_cod_depositor_comments
'Adding full bibliography for 1571710--1571717.cif.'
_cod_database_code               1571717
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 H100 N10 Ni3'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-C27 = C55-C57A = C55-C58 = C56A-C55 = C60-C59 = C62-C59 = C60A-C59 = C61A-
 C59
 1.52 with sigma of 0.02
 C29A-C30A = C61A-C60A = C109-C108 = C108-C110 = C109-C110 = C122-C123 = C225-
 C224 = C114-C112 = C113-C114 = C112-C113 = C122-C124 = C124-C123
 2.5 with sigma of 0.02
 C108-C107 = C110-C107 = C109-C107 = C121-C122 = C121-C123 = C126-C125 = C235-
 C233 = C225-C223 = C224-C223 = C112-C111 = C114-C111 = C121-C124
 1.52 with sigma of 0.02
 Cl1_$1-C240
 2.6 with sigma of 0.02
 H22R-H216
 2 with sigma of 0.02
 C111-C113
 1.528 with sigma of 0.001
 C105-C113
 2.424 with sigma of 0.001
 H12G-H116
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C111, C113
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C57) \\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C58A)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C46A) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C48A)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C61A) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C60A) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C29A)
\\sim Ueq, Uanis(C177) \\sim Ueq, Uanis(C168) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C109) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C125) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C137) \\sim Ueq,
Uanis(C135) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C138) \\sim Ueq,
Uanis(C234) \\sim Ueq, Uanis(C233) \\sim Ueq, Uanis(C235) \\sim Ueq,
Uanis(C236) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C220) \\sim Ueq, Uanis(C219) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C226) \\sim Ueq, Uanis(C225) \\sim Ueq, Uanis(C223) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.006
5. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C60)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=
 Sof(C62)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(2)
 Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61A)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(2)
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C57A)=Sof(H57D)=Sof(H57E)=
 Sof(H57F)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(3)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(3)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(4)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(4)
 Fixed Sof: H14(0.35) H20(0.15) H88(0.7) H94(0.95) H180(0.65) H194(0.7)
 Cl1(0.35) Cl2(0.15) Cl3(0.3) Cl4(0.05) Cl5(0.35) Cl6(0.3)
6.a Me refined with riding coordinates:
 C109(H10D,H10E,H10F), C112(H11D,H11E,H11F), C114(H11J,H11K,H11L), C123(H12D,
 H12E,H12F), C124(H12G,H12H,H12I), C127(H12M,H12N,H12O), C128(H12P,H12Q,H12R),
 C235(H23D,H23E,H23F), C30(H30A,H30B,H30C), C28A(H28D,H28E,H28F), C30A(H30D,
 H30E,H30F), C58A(H58D,H58E,H58F)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C20(H20), C22(H22), C24(H24),
 C26(H26), C36(H36), C38(H38), C40(H40), C50(H50), C52(H52), C54(H54), C64(H64),
  C68(H68), C74(H74), C76(H76), C83(H83), C84(H84), C88(H88), C94(H94),
 C98(H98), C99(H99), C102(H102), C104(H104), C106(H106), C116(H116), C118(H118),
  C120(H120), C130(H130), C132(H132), C134(H134), C144(H144), C148(H148),
 C153(H153), C157(H157), C163(H163), C165(H165), C172(H172), C174(H174),
 C180(H180), C184(H184), C185(H185), C189(H189), C190(H190), C194(H194),
 C200(H200), C202(H202), C204(H204), C214(H214), C216(H216), C218(H218),
 C228(H228), C230(H230), C232(H232)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C78(H78A,H78B,H78C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C108(H10A,H10B,H10C), C110(H11A,H11B,H11C),
 C113(H11G,H11H,H11I), C122(H12A,H12B,H12C), C126(H12J,H12K,H12L), C136(H13A,
 H13B,H13C), C137(H13D,H13E,H13F), C138(H13G,H13H,H13I), C140(H14A,H14B,H14C),
 C141(H14D,H14E,H14F), C142(H14G,H14H,H14I), C167(H16A,H16B,H16C), C168(H16D,
 H16E,H16F), C169(H16G,H16H,H16I), C176(H17A,H17B,H17C), C177(H17D,H17E,H17F),
 C178(H17G,H17H,H17I), C206(H20A,H20B,H20C), C207(H20D,H20E,H20F), C208(H20G,
 H20H,H20I), C210(H21A,H21B,H21C), C211(H21D,H21E,H21F), C212(H21G,H21H,H21I),
 C220(H22A,H22B,H22C), C221(H22D,H22E,H22F), C222(H22G,H22H,H22I), C224(H22J,
 H22K,H22L), C225(H22M,H22N,H22O), C226(H22P,H22Q,H22R), C234(H23A,H23B,H23C),
 C236(H23G,H23H,H23I), C238(H23J,H23K,H23L), C239(H23M,H23N,H23O), C240(H24A,
 H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C60A(H60A,H60B,H60C), C61A(H61A,H61B,H61C),
 C62A(H62A,H62B,H62C), C29A(H29D,H29E,H29F), C46A(H46D,H46E,H46F), C47A(H47D,
 H47E,H47F), C48A(H48D,H48E,H48F), C56A(H56D,H56E,H56F), C57A(H57D,H57E,H57F),
 C60(H60D,H60E,H60F), C61(H61D,H61E,H61F), C62(H62D,H62E,H62F)
;
_shelx_res_checksum              80266
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.270