Selective White Phosphorus Activation and Functionalization with Inorganic Grignard Reagents
Gilch, Franziska; Brossette, Jan; Westermair, Franz F.; Silva, Wagner; Balázs, Gábor; Gschwind, Ruth M.; Zipse, Hendrik; Wolf, Robert; Chemical Science  (2026) –; doi:10.1039/D6SC01229A

data_1577036
_publ_section_title
;
 Selective White Phosphorus Activation and Functionalization with
 Inorganic Grignard Reagents
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D6SC01229A
_journal_year                    2026
_chemical_formula_moiety         'C82 H112 Fe2 Mg2 N4 O4, 0.5(C7 H8)'
_chemical_formula_sum            'C85.5 H116 Fe2 Mg2 N4 O4'
_chemical_formula_weight         1424.14
_chemical_name_systematic        DippBDIMgFp*
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2026-02-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-09 deposited with the CCDC.	2026-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2799(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.76217(5)
_cell_length_b                   20.24982(7)
_cell_length_c                   21.68721(6)
_cell_measurement_reflns_used    296966
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.1340
_cell_measurement_theta_min      2.3110
_cell_volume                     8239.54(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 42.92a 64-bit (release 29-05-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (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      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_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     32.00  60.00   0.50    0.30    --   62.92-151.00  17.00   56
  2  \w     31.00  56.00   0.50    0.30    --   62.92-123.00 178.00   50
  3  \w    -75.00 -50.00   0.50    0.30    --  -63.82 151.00  61.00   50
  4  \w    -69.00 -23.00   0.50    0.30    --  -63.82 123.00-100.00   92
  5  \w   -101.00 -76.00   0.50    0.30    --  -63.82-151.00  17.00   50
  6  \w    -98.00 -65.00   0.50    0.30    --  -73.68 123.00-100.00   66
  7  \w   -118.00 -69.00   0.50    0.30    --  -73.68 151.00  61.00   98
  8  \w   -110.00 -75.00   0.50    0.30    --  -73.68-151.00  17.00   70
  9  \w     64.00  89.00   0.50    0.30    --   75.56 151.00  61.00   50
 10  \w     54.00  79.00   0.50    0.30    --   75.56-151.00  17.00   50
 11  \w     48.00  74.00   0.50    0.30    --   75.87-123.00 178.00   52
 12  \w     64.00  89.00   0.50    0.30    --   75.87 151.00  61.00   50
 13  \w     88.00 114.00   0.50    0.30    --   75.87-151.00  17.00   52
 14  \w    -93.00 -68.00   0.50    0.30    --  -76.65 123.00-100.00   50
 15  \w   -121.00 -96.00   0.50    0.30    --  -76.65 151.00  61.00   50
 16  \w   -107.00 -81.00   0.50    0.30    --  -76.65-151.00  17.00   52
 17  \w     -3.00  22.00   0.50    0.30    --   -6.00  78.00 -58.40   50
 18  \w    -19.00   6.00   0.50    0.30    --   -6.00 103.00-139.66   50
 19  \w      0.00  25.00   0.50    0.30    --   10.00  98.00  26.35   50
 20  \w     13.00  38.00   0.50    0.30    --   18.00  91.00  44.86   50
 21  \w     14.00  39.00   0.50    0.30    --   18.00  88.00 -93.67   50
 22  \w     14.00  39.00   0.50    0.30    --   18.00  88.00 -25.52   50
 23  \w     16.00  41.00   0.50    0.30    --   18.00  85.00-135.60   50
 24  \w    -46.00 -15.00   0.50    0.30    --  -22.00 129.00 140.21   62
 25  \w     17.00  42.00   0.50    0.30    --   22.00  90.00  77.85   50
 26  \w     25.00  50.00   0.50    0.30    --   22.00  77.00-152.80   50
 27  \w     17.00  42.00   0.50    0.30    --   22.00  90.00 131.74   50
 28  \w     26.00  51.00   0.50    0.30    --   22.00  76.00  53.73   50
 29  \w     26.00  51.00   0.50    0.30    --   22.00  76.00  30.71   50
 30  \w     29.00  54.00   0.50    0.30    --   26.00  77.00 -81.61   50
 31  \w     31.00  56.00   0.50    0.30    --   26.00  75.00 158.71   50
 32  \w     31.00  56.00   0.50    0.30    --   26.00  74.00  71.95   50
 33  \w     29.00  54.00   0.50    0.30    --   26.00  77.00 -68.77   50
 34  \w     29.00  54.00   0.50    0.30    --   26.00  77.00 129.67   50
 35  \w     35.00  60.00   0.50    0.30    --   30.00  75.00 135.33   50
 36  \w     35.00  60.00   0.50    0.30    --   30.00  75.00  75.52   50
 37  \w    -61.00 -35.00   0.50    0.30    --  -30.00 -73.00 -93.29   52
 38  \w     35.00  60.00   0.50    0.30    --   30.00  75.00-110.74   50
 39  \w     37.00  62.00   0.50    0.30    --   30.00  70.00  60.84   50
 40  \w     36.00  61.00   0.50    0.30    --   30.00  73.00  -9.90   50
 41  \w    -63.00 -38.00   0.50    0.30    --  -34.00 -76.00 154.34   50
 42  \w     39.00  64.00   0.50    0.30    --   34.00  75.00-150.67   50
 43  \w     39.00  64.00   0.50    0.30    --   34.00  74.00-126.34   50
 44  \w     39.00  64.00   0.50    0.30    --   34.00  74.00   1.45   50
 45  \w     37.00  62.00   0.50    0.30    --   34.00  77.00 113.63   50
 46  \w     39.00  64.00   0.50    0.30    --   34.00  74.00 155.60   50
 47  \w     37.00  62.00   0.50    0.30    --   34.00  77.00-175.77   50
 48  \w     37.00  62.00   0.50    0.30    --   34.00  77.00  14.10   50
 49  \w     39.00  64.00   0.50    0.30    --   34.00  75.00  99.55   50
 50  \w     47.00  72.00   0.50    0.30    --   38.00  65.00-120.52   50
 51  \w     45.00  70.00   0.50    0.30    --   38.00  70.00   0.94   50
 52  \w     41.00  66.00   0.50    0.30    --   38.00  77.00 -87.00   50
 53  \w     45.00  70.00   0.50    0.30    --   38.00  70.00 139.34   50
 54  \w     42.00  67.00   0.50    0.30    --   38.00  76.00  45.99   50
 55  \w     44.00  69.00   0.50    0.30    --   38.00  73.00  75.82   50
 56  \w     44.00  69.00   0.50    0.30    --   38.00  72.00 119.99   50
 57  \w     42.00  67.00   0.50    0.30    --   38.00  76.00 -55.45   50
 58  \w     41.00  66.00   0.50    0.30    --   38.00  77.00 -45.98   50
 59  \w     42.00  67.00   0.50    0.30    --   38.00  76.00 168.43   50
 60  \w     49.00  74.00   0.50    0.30    --   42.00  71.00  66.74   50
 61  \w     48.00  73.00   0.50    0.30    --   42.00  73.00 -83.58   50
 62  \w     48.00  73.00   0.50    0.30    --   42.00  73.00-168.08   50
 63  \w    -75.00 -50.00   0.50    0.30    --  -42.00 -65.00 163.05   50
 64  \w     49.00  74.00   0.50    0.30    --   42.00  71.00   7.07   50
 65  \w     50.00  75.00   0.50    0.30    --   42.00  68.00 154.59   50
 66  \w     47.00  72.00   0.50    0.30    --   42.00  74.00-114.72   50
 67  \w     53.00  78.00   0.50    0.30    --   46.00  71.00 116.26   50
 68  \w     53.00  78.00   0.50    0.30    --   46.00  71.00  22.16   50
 69  \w     54.00  79.00   0.50    0.30    --   46.00  67.00 179.25   50
 70  \w     53.00  78.00   0.50    0.30    --   46.00  71.00-107.68   50
 71  \w     55.00  80.00   0.50    0.30    --   46.00  64.00 171.54   50
 72  \w     53.00  78.00   0.50    0.30    --   46.00  70.00 -62.39   50
 73  \w     55.00  80.00   0.50    0.30    --   46.00  62.00-127.66   50
 74  \w     52.00  77.00   0.50    0.30    --   46.00  73.00-124.99   50
 75  \w     53.00  78.00   0.50    0.30    --   46.00  70.00 125.63   50
 76  \w    -83.00 -57.00   0.50    0.30    --  -50.00 -70.00-122.94   52
 77  \w    -84.00 -59.00   0.50    0.30    --  -50.00 -64.00  21.22   50
 78  \w     57.00  82.00   0.50    0.30    --   50.00  70.00-102.84   50
 79  \w     57.00  82.00   0.50    0.30    --   50.00  70.00 139.89   50
 80  \w     56.00  81.00   0.50    0.30    --   50.00  73.00 -21.36   50
 81  \w     57.00  82.00   0.50    0.30    --   50.00  70.00 -50.51   50
 82  \w     58.00  83.00   0.50    0.30    --   50.00  69.00   5.86   50
 83  \w     58.00  83.00   0.50    0.30    --   50.00  69.00 -77.52   50
 84  \w     53.00  78.00   0.50    0.30    --   50.00  77.00  74.76   50
 85  \w     61.00  86.00   0.50    0.30    --   54.00  71.00 -37.31   50
 86  \w    -87.00 -61.00   0.50    0.30    --  -54.00 -72.00-137.37   52
 87  \w    -85.00 -59.00   0.50    0.30    --  -54.00 -73.00 -37.52   52
 88  \w     61.00  86.00   0.50    0.30    --   54.00  70.00 -44.21   50
 89  \w    -84.00 -59.00   0.50    0.30    --  -54.00 -73.00-173.18   50
 90  \w     63.00  88.00   0.50    0.30    --   54.00  62.00 -65.90   50
 91  \w     63.00  88.00   0.50    0.30    --   54.00  63.00 -57.52   50
 92  \w    -87.00 -61.00   0.50    0.30    --  -54.00 -69.00  68.17   52
 93  \w     61.00  86.00   0.50    0.30    --   54.00  70.00-126.64   50
 94  \w    -90.00 -64.00   0.50    0.30    --  -58.00 -72.00 -39.27   52
 95  \w     66.00  91.00   0.50    0.30    --   58.00  69.00-121.90   50
 96  \w     64.00  89.00   0.50    0.30    --   58.00  72.00-149.84   50
 97  \w     65.00  90.00   0.50    0.30    --   58.00  71.00  24.22   50
 98  \w     65.00  90.00   0.50    0.30    --   58.00  71.00 174.98   50
 99  \w     67.00  92.00   0.50    0.30    --   58.00  62.00 -50.99   50
100  \w     65.00  90.00   0.50    0.30    --   58.00  71.00 -39.36   50
101  \w     65.00  90.00   0.50    0.30    --   58.00  71.00 103.76   50
102  \w     65.00  90.00   0.50    0.30    --   58.00  70.00 117.33   50
103  \w    -88.00 -62.00   0.50    0.30    --  -58.00 -77.00  32.26   52
104  \w     66.00  91.00   0.50    0.30    --   58.00  69.00  60.30   50
105  \w     67.00  92.00   0.50    0.30    --   58.00  62.00 -89.36   50
106  \w     64.00  89.00   0.50    0.30    --   58.00  73.00 155.35   50
107  \w     67.00  92.00   0.50    0.30    --   58.00  64.00 147.41   50
108  \w     65.00  90.00   0.50    0.30    --   58.00  70.00   8.97   50
109  \w     68.00  93.00   0.50    0.30    --   62.00  73.00  25.20   50
110  \w     70.00  95.00   0.50    0.30    --   62.00  69.00 -57.50   50
111  \w     71.00  96.00   0.50    0.30    --   62.00  61.00 -68.87   50
112  \w     69.00  94.00   0.50    0.30    --   62.00  71.00  71.60   50
113  \w     69.00  94.00   0.50    0.30    --   62.00  71.00  57.79   50
114  \w     69.00  94.00   0.50    0.30    --   62.00  70.00-178.69   50
115  \w     69.00  94.00   0.50    0.30    --   62.00  71.00  11.02   50
116  \w     69.00  94.00   0.50    0.30    --   62.00  71.00  80.31   50
117  \w     69.00  94.00   0.50    0.30    --   62.00  71.00 123.51   50
118  \w     26.00  95.00   0.50    0.30    --   62.92   0.00 150.00  138
119  \w     28.00  54.00   0.50    0.30    --   62.92 -95.00-150.00   52
120  \w     62.00 100.00   0.50    0.30    --   62.92   0.00 -90.00   76
121  \w     26.00  69.00   0.50    0.30    --   62.92 -95.00   0.00   86
122  \w     27.00  52.00   0.50    0.30    --   62.92   0.00 -90.00   50
123  \w    -87.00 -22.00   0.50    0.30    --  -63.82 125.00  30.00  130
124  \w    -73.00 -22.00   0.50    0.30    --  -63.82 125.00   0.00  102
125  \w    -86.00 -25.00   0.50    0.30    --  -63.82 125.00-150.00  122
126  \w    -55.00 -22.00   0.50    0.30    --  -63.82 125.00 -30.00   66
127  \w    -90.00 -61.00   0.50    0.30    --  -63.82 125.00 -30.00   58
128  \w     72.00  97.00   0.50    0.30    --   66.00  72.00  63.11   50
129  \w    -96.00 -70.00   0.50    0.30    --  -66.00 -75.00  24.20   52
130  \w     71.00  96.00   0.50    0.30    --   66.00  74.00-153.04   50
131  \w     75.00 105.00   0.50    0.30    --   70.00  75.00 -29.37   60
132  \w     75.00 100.00   0.50    0.30    --   70.00  75.00 146.30   50
133  \w   -104.00 -78.00   0.50    0.30    --  -70.00 -65.00-122.34   52
134  \w   -102.00 -76.00   0.50    0.30    --  -70.00 -72.00 145.64   52
135  \w   -101.00 -75.00   0.50    0.30    --  -70.00 -73.00  12.14   52
136  \w   -101.00 -75.00   0.50    0.30    --  -70.00 -73.00 112.84   52
137  \w   -106.00 -79.00   0.50    0.30    --  -70.00 -65.00 -24.41   54
138  \w    -99.00 -74.00   0.50    0.30    --  -70.00 -75.00 124.99   50
139  \w   -101.00 -75.00   0.50    0.30    --  -70.00 -74.00  88.19   52
140  \w   -101.00 -75.00   0.50    0.30    --  -70.00 -74.00   1.69   52
141  \w   -100.00 -74.00   0.50    0.30    --  -70.00 -75.00 -35.53   52
142  \w   -109.00 -37.00   0.50    0.30    --  -73.68   0.00 -60.00  144
143  \w   -120.00 -94.00   0.50    0.30    --  -74.00 -40.00-108.13   52
144  \w   -105.00 -79.00   0.50    0.30    --  -74.00 -73.00-134.50   52
145  \w   -111.00 -79.00   0.50    0.30    --  -74.00 -73.00-178.56   64
146  \w   -105.00 -79.00   0.50    0.30    --  -74.00 -76.00 -39.89   52
147  \w   -114.00 -83.00   0.50    0.30    --  -74.00 -64.00-109.46   62
148  \w   -110.00 -78.00   0.50    0.30    --  -74.00 -75.00  -1.37   64
149  \w   -105.00 -79.00   0.50    0.30    --  -74.00 -74.00-139.99   52
150  \w   -107.00 -81.00   0.50    0.30    --  -74.00 -72.00 -73.28   52
151  \w   -113.00 -82.00   0.50    0.30    --  -74.00 -65.00-133.72   62
152  \w    -76.00 -50.00   0.50    0.30    --  -74.00 145.00 125.37   52
153  \w   -114.00 -80.00   0.50    0.30    --  -74.00 145.00 125.37   68
154  \w     48.00 102.00   0.50    0.30    --   75.56-125.00  30.00  108
155  \w   -106.00 -80.00   0.50    0.30    --  -78.00 -78.00  51.69   52
156  \w   -106.00 -80.00   0.50    0.30    --  -78.00 -78.00  42.68   52
157  \w   -108.00 -82.00   0.50    0.30    --  -78.25 -80.00  15.85   52
158  \w   -105.00 -79.00   0.50    0.30    --  -78.25 -84.00 101.72   52
159  \w    -63.00 -38.00   0.50    0.30    --  -78.25 115.00 -41.57   50
160  \w    -98.00 -70.00   0.50    0.30    --  -78.25 115.00 -41.57   56
161  \w    -61.00 -36.00   0.50    0.30    --  -78.25  56.00 143.87   50
162  \w   -105.00 -80.00   0.50    0.30    --  -78.25 -80.00  63.20   50
163  \w   -106.00 -80.00   0.50    0.30    --  -78.25 -79.00-176.27   52
164  \w   -109.00 -83.00   0.50    0.30    --  -78.25 -76.00  32.99   52
165  \w   -111.00 -81.00   0.50    0.30    --  -78.25 -77.00 -10.51   60
166  \w   -110.00 -84.00   0.50    0.30    --  -78.25 -77.00 -73.78   52
167  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -81.00-107.24   50
168  \w   -109.00 -81.00   0.50    0.30    --  -78.25 -78.00 133.53   56
169  \w    -88.00 -39.00   0.50    0.30    --  -78.25 122.00  57.54   98
170  \w   -107.00 -80.00   0.50    0.30    --  -78.25 -79.00 111.09   54
171  \w   -106.00 -81.00   0.50    0.30    --  -78.25 -77.00-171.17   50
172  \w   -110.00 -80.00   0.50    0.30    --  -78.25 -81.00  27.44   60
173  \w   -105.00 -80.00   0.50    0.30    --  -78.25 -79.00 171.33   50
174  \w   -106.00 -81.00   0.50    0.30    --  -78.25 -78.00 147.37   50
175  \w    -62.00 -36.00   0.50    0.30    --  -78.25  60.00-143.05   52
176  \w   -115.00 -85.00   0.50    0.30    --  -78.25 -70.00-169.71   60
177  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -82.00 -88.07   50
178  \w   -113.00 -82.00   0.50    0.30    --  -78.25 -78.00 -47.95   62
179  \w   -105.00 -79.00   0.50    0.30    --  -78.25 -81.00 126.09   52
180  \w   -106.00 -80.00   0.50    0.30    --  -78.25 -79.00-135.27   52
181  \w    -62.00 -36.00   0.50    0.30    --  -78.25 124.00 172.85   52
182  \w    -77.00 -43.00   0.50    0.30    --  -78.25  88.00-161.82   68
183  \w    -92.00 -66.00   0.50    0.30    --  -78.25 124.00 172.85   52
184  \w   -109.00 -41.00   0.50    0.30    --  -78.25 130.00-179.59  136
185  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -86.00   7.91   50
186  \w    -66.00 -41.00   0.50    0.30    --  -78.25 123.00 103.44   50
187  \w    -99.00 -73.00   0.50    0.30    --  -78.25 123.00 103.44   52
188  \w   -112.00 -82.00   0.50    0.30    --  -78.25 -77.00 154.62   60
189  \w   -112.00 -43.00   0.50    0.30    --  -78.25 135.00 -39.86  138
190  \w   -110.00 -79.00   0.50    0.30    --  -78.25 -87.00 -27.54   62
191  \w   -109.00 -81.00   0.50    0.30    --  -78.25 -78.00 -56.32   56
192  \w   -105.00 -79.00   0.50    0.30    --  -78.25 -84.00-109.03   52
193  \w    -78.00 -37.00   0.50    0.30    --  -78.25 117.00  46.36   82
194  \w   -106.00 -80.00   0.50    0.30    --  -78.25 -79.00-149.96   52
195  \w   -106.00 -79.00   0.50    0.30    --  -78.25 -81.00-101.24   54
196  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -81.00   3.88   50
197  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -82.00 -78.66   50
198  \w   -113.00 -79.00   0.50    0.30    --  -78.25 -83.00 105.67   68
199  \w   -105.00 -80.00   0.50    0.30    --  -78.25 -80.00 -63.24   50
200  \w    -67.00 -42.00   0.50    0.30    --  -78.25  89.00  18.44   50
201  \w   -106.00 -81.00   0.50    0.30    --  -78.25 -78.00 118.59   50
202  \w    -84.00 -37.00   0.50    0.30    --  -78.25 127.00-138.35   94
203  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -90.00  56.95   50
204  \w   -112.00 -79.00   0.50    0.30    --  -78.25 -83.00 -12.15   66
205  \w   -104.00 -79.00   0.50    0.30    --  -78.25 -84.00  75.12   50
206  \w   -113.00 -81.00   0.50    0.30    --  -78.25 -78.00  87.42   64
207  \w   -105.00 -80.00   0.50    0.30    --  -78.25 -79.00  80.95   50
208  \w    -66.00 -41.00   0.50    0.30    --  -78.25 101.00 116.53   50
209  \w     40.00  98.00   0.50    0.30    --   79.75-112.00-137.49  116
210  \w     40.00  77.00   0.50    0.30    --   79.75  -4.00  32.40   74
211  \w     67.00 126.00   0.50    0.30    --   79.75  23.00 163.75  118
212  \w     88.00 113.00   0.50    0.30    --   79.75   5.00   4.84   50
213  \w     45.00  78.00   0.50    0.30    --   79.75   5.00   4.84   66
214  \w     37.00 110.00   0.50    0.30    --   79.75-129.00-141.90  146
215  \w     39.00  64.00   0.50    0.30    --   79.75 -59.00 -83.08   50
216  \w     51.00 111.00   0.50    0.30    --   79.75-131.00 -53.32  120
217  \w     52.00  79.00   0.50    0.30    --   79.75  -4.00 -29.58   54
218  \w     45.00  70.00   0.50    0.30    --   79.75 -81.00 -18.14   50
219  \w     42.00 123.00   0.50    0.30    --   79.75-149.00  -7.34  162
220  \w     89.00 114.00   0.50    0.30    --   79.75  78.00  70.53   50
221  \w     40.00  65.00   0.50    0.30    --   79.75  -4.00  77.00   50
222  \w     66.00 118.00   0.50    0.30    --   79.75  23.00 -64.47  104
223  \w     40.00  67.00   0.50    0.30    --   79.75-111.00 -14.08   54
224  \w     99.00 124.00   0.50    0.30    --   79.75  11.00 -76.11   50
225  \w     49.00  78.00   0.50    0.30    --   79.75  11.00 -76.11   58
226  \w     48.00 107.00   0.50    0.30    --   79.75   7.00 123.50  118
227  \w     40.00  70.00   0.50    0.30    --   79.75  -4.00 -46.07   60
228  \w     93.00 123.00   0.50    0.30    --   79.75  47.00 -69.92   60
229  \w     91.00 116.00   0.50    0.30    --   79.75  49.00 154.01   50
230  \w     43.00 111.00   0.50    0.30    --   79.75-131.00  13.11  136
231  \w     90.00 115.00   0.50    0.30    --   79.75  78.00 159.74   50
232  \w     98.00 126.00   0.50    0.30    --   79.75  42.00-139.50   56
233  \w     40.00  99.00   0.50    0.30    --   79.75-116.00  85.52  118
234  \w     39.00 106.00   0.50    0.30    --   79.75-123.00 115.14  134
235  \w     91.00 123.00   0.50    0.30    --   79.75  45.00  70.73   64
236  \w     42.00  88.00   0.50    0.30    --   79.75  -3.00 110.49   92
237  \w     83.00 116.00   0.50    0.30    --   79.75  -2.00-131.13   66
238  \w     48.00  80.00   0.50    0.30    --   79.75  -2.00-131.13   64
239  \w     74.00 111.00   0.50    0.30    --   79.75-136.00 176.00   74
240  \w     47.00  78.00   0.50    0.30    --   79.75  -4.00-179.67   62
241  \w    100.00 127.00   0.50    0.30    --   79.75  36.00-177.89   54
242  \w     46.00  71.00   0.50    0.30    --   79.75-136.00 176.00   50
243  \w     55.00 125.00   0.50    0.30    --   79.75  15.00  21.78  140
244  \w     40.00  93.00   0.50    0.30    --   79.75-113.00  32.17  106
245  \w     65.00 126.00   0.50    0.30    --   79.75  22.00  66.38  122
246  \w     52.00 101.00   0.50    0.30    --   79.75   9.00-108.36   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517761000
_diffrn_orient_matrix_UB_12      -0.0014261000
_diffrn_orient_matrix_UB_13      -0.0548866000
_diffrn_orient_matrix_UB_21      -0.0632663000
_diffrn_orient_matrix_UB_22      -0.0102690000
_diffrn_orient_matrix_UB_23      -0.0445041000
_diffrn_orient_matrix_UB_31      -0.0076177000
_diffrn_orient_matrix_UB_32      0.0753910000
_diffrn_orient_matrix_UB_33      -0.0071130000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0072
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            512297
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.256
_diffrn_reflns_theta_min         2.986
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.344
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.36a (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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             3060
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/n-hexane'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         16896
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0453P)^2^+2.8603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16306
_reflns_number_total             16896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc01229a2.cif
_cod_data_source_block           fg110_neu_p21-n
_cod_original_formula_sum        'C85.50 H116 Fe2 Mg2 N4 O4'
_cod_database_code               1577036
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C82H112Fe2Mg2N4O4
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.424
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C13-C14
 1.51 with sigma of 0.02
 C14-C15 = C14-C19 = C16-C17
 1.39 with sigma of 0.02
 C15-C16 = C17-C18 = C18-C19
 1.38 with sigma of 0.02
 C13-C15 = C13-C19
 2.52 with sigma of 0.04
 C14-C16
 2.42 with sigma of 0.04
 C14-C18
 2.41 with sigma of 0.04
 C15-C17
 2.39 with sigma of 0.04
 C16-C18 = C17-C19
 2.4 with sigma of 0.04
 C14-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C18 \\sim C18-C19 \\sim C19-C14
 with sigma of 0.02
 C14-C18 \\sim C14-C16 \\sim C19-C17 \\sim C15-C19 \\sim C16-C18 \\sim C15-C17
 with sigma of 0.04
 C13-C19 \\sim C13-C15
 with sigma of 0.04
 C00K-C01J \\sim C00K-C21
 with sigma of 0.02
 C01J-C12 \\sim C21-C1A
 with sigma of 0.02
 C01J-C20 \\sim C21-C9A
 with sigma of 0.02
 C00K-C12 \\sim C00K-C1A
 with sigma of 0.04
 C00K-C20 \\sim C00K-C9A
 with sigma of 0.04
 C12-C20 \\sim C1A-C9A
 with sigma of 0.04
 C01P-C02I \\sim C01P-C11
 with sigma of 0.02
 C01P-C02K \\sim C01P-C02L
 with sigma of 0.02
3. Restrained planarity
 C13, C14, C15, C16, C17, C18, C19
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C21)=Sof(H21)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C01J)=Sof(H01N)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(H01S)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C02L)=Sof(H16)=Sof(H24)=
 Sof(H25)=1-FVAR(2)
 Sof(H01R)=Sof(C02I)=Sof(H13)=Sof(HX)=Sof(HY)=Sof(C02K)=Sof(H15)=Sof(H22)=
 Sof(H23)=FVAR(2)
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) C15(0.5) H15A(0.5)
 C16(0.5) H16A(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5)
7.a Ternary CH refined with riding coordinates:
 C00S(H00S), C00W(H00W), C014(H014), C01J(H01N), C01N(H01Q), C01P(H01R),
 C01P(H01S), C01S(H01X), C01T(H01Y), C21(H21)
7.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C6(H6), C00Y(H00Y), C9(H9), C013(H013), C016(H016), C01A(H01D),
 C01L(H01O), C01M(H01P), C01R(H01W), C01U(H01Z), C01W(H1), C01X(H2), C022(H022),
  C15(H15A), C16(H16A), C17(H17), C18(H18), C19(H19)
7.c Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C01D(H01E,H01F,H01G), C01G(H01H,H01I,H01J), C01H(H01K,
 H01L,H01M), C01Q(H01T,H01U,H01V), C01V(H01,H,HA), C01Y(H3,HB,HC), C01Z(H4,HD,
 HE), C020(H02A,H02B,H02C), C021(H02D,H02E,H02F), C023(H02G,H02H,H02I),
 C024(H02J,H02K,H02L), C025(H02M,H02N,H02O), C026(H02P,H02Q,H02R), C027(H02S,
 H02T,H02U), C028(H02V,H02W,H02X), C029(H02Y,HF,HG), C02A(H02Z,HH,HI), C02B(H02,
 HJ,HK), C02C(H5,HL,HM), C02D(H7,HN,HO), C02E(H8,HP,HQ), C02F(H10,HR,HS),
 C02G(H11,HT,HU), C02H(H12,HV,HW), C02I(H13,HX,HY), C02J(H14,HZ,H20), C02K(H15,
 H22,H23), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C),
 C9A(H9AA,H9AB,H9AC), C1A(H1AA,H1AB,H1AC), C11(H11A,H11B,H11C), C02L(H16,H24,
 H25)
;
_shelx_res_checksum              87317
_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 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.777