#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:56:30 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289501 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/48/7714876.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714876
loop_
_publ_author_name
'Besmer, Manuel Luca'
'Schwitter, Flurina'
'Battistin, Federica'
'Braband, Henrik'
'Fox, Thomas'
'Spingler, Bernhard'
'Alberto, Roger'
_publ_section_title
;
 Induced fac-mer rearrangements in
 {M(CO)₃}⁺ complexes (M = Re, 99(m)Tc) by
 a PNP ligand.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1434
_journal_page_last               1438
_journal_paper_doi               10.1039/d3dt03992g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H43 N O3 P2 Tc, 0.6(F6 P), 0.4(Cl)'
_chemical_formula_sum            'C26 H43 Cl0.4 F3.6 N O3 P2.6 Tc'
_chemical_formula_weight         678.71
_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     dual
_audit_creation_date             2023-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-11-13 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                106.0060(10)
_cell_angle_beta                 103.6810(10)
_cell_angle_gamma                92.6590(10)
_cell_formula_units_Z            2
_cell_length_a                   8.38590(10)
_cell_length_b                   12.89050(10)
_cell_length_c                   15.67840(10)
_cell_measurement_reflns_used    48946
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      78.8830
_cell_measurement_theta_min      2.9870
_cell_volume                     1571.54(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      159.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  13.00   0.50    0.80    --  -52.03  62.00 -19.00  136
  2  ω   -119.00 -39.00   0.50    0.80    --  -52.03 -62.00-157.00  160
  3  ω     47.00  99.00   0.50    0.80    --   52.03  62.00 -19.00  104
  4  ω     -2.00  52.00   0.50    0.80    --   52.03 -62.00-157.00  108
  5  ω    -83.00 -58.00   0.50    3.20    --  -86.25  62.00 -19.00   50
  6  ω   -114.00 -89.00   0.50    3.20    --  -86.25 -62.00-157.00   50
  7  ω     40.00  71.00   0.50    3.20    --  107.75 -62.00-157.00   62
  8  ω    110.00 169.00   0.50    3.20    --  107.75  62.00 -19.00  118
  9  ω    -58.00 -13.00   0.50    0.80    --  -52.03 125.00 -30.00   90
 10  ω   -124.00 -98.00   0.50    0.80    --  -52.03 -57.00  30.00   52
 11  ω   -125.00 -95.00   0.50    0.80    --  -52.03 -57.00  60.00   60
 12  ω   -123.00 -94.00   0.50    0.80    --  -52.03 -57.00 120.00   58
 13  ω   -124.00 -94.00   0.50    0.80    --  -52.03 -57.00 -60.00   60
 14  ω     59.00  84.00   0.50    0.80    --   52.03 -99.00  30.00   50
 15  ω     44.00  98.00   0.50    0.80    --   52.03-125.00-120.00  108
 16  ω   -135.00-109.00   0.50    3.20    --  -86.25 -61.00 -60.00   52
 17  ω     72.00 106.00   0.50    3.20    --  107.75 -94.00 120.00   68
 18  ω     65.00  91.00   0.50    3.20    --  107.75 -77.00 120.00   52
 19  ω     95.00 161.00   0.50    3.20    --  107.75  45.00 -60.00  132
 20  ω    114.00 176.00   0.50    3.20    --  107.75  77.00  30.00  124
 21  ω     38.00  69.00   0.50    3.20    --  107.75 -94.00   0.00   62
 22  ω     75.00 106.00   0.50    3.20    --  107.75 -94.00   0.00   62
 23  ω     35.00 109.00   0.50    3.20    --  107.75-111.00   0.00  148
 24  ω     80.00 106.00   0.50    3.20    --  107.75-111.00-150.00   52
 25  ω     74.00 109.00   0.50    3.20    --  107.75-111.00 120.00   70
 26  ω     39.00  75.00   0.50    3.20    --  107.75-111.00-150.00   72
 27  ω    133.00 171.00   0.50    3.20    --  107.75  61.00 -90.00   76
 28  ω     76.00 109.00   0.50    3.20    --  107.75-111.00-180.00   66
 29  ω     93.00 135.00   0.50    3.20    --  107.75  61.00 -60.00   84
 30  ω    146.00 178.00   0.50    3.20    --  107.75  61.00 -60.00   64
 31  ω     45.00  71.00   0.50    3.20    --  107.75 -30.00-180.00   52
 32  ω    101.00 126.00   0.50    3.20    --  107.75 -77.00 120.00   50
 33  ω     38.00  89.00   0.50    3.20    --  107.75 -61.00-180.00  102
 34  ω     73.00  99.00   0.50    3.20    --  107.75 178.00  30.00   52
 35  ω    104.00 155.00   0.50    3.20    --  107.75 111.00  30.00  102
 36  ω     84.00 119.00   0.50    3.20    --  107.75 -45.00  60.00   70
 37  ω     31.00  56.00   0.50    3.20    --  107.75 -94.00-120.00   50
 38  ω     78.00 103.00   0.50    3.20    --  107.75 -94.00-120.00   50
 39  ω     61.00 118.00   0.50    3.20    --  107.75 -30.00  30.00  114
 40  ω     46.00  75.00   0.50    3.20    --  107.75-111.00 -60.00   58
 41  ω    128.00 176.00   0.50    3.20    --  107.75  55.00-100.61   96
 42  ω     95.00 120.00   0.50    3.20    --  107.75 -61.00 -30.00   50
 43  ω     83.00 109.00   0.50    3.20    --  107.75-111.00  90.00   52
 44  ω     53.00  78.00   0.50    3.20    --  107.75 -61.00 -30.00   50
 45  ω     84.00 109.00   0.50    3.20    --  107.75-111.00 -60.00   50
 46  ω     64.00 106.00   0.50    3.20    --  107.75-111.00 -30.00   84
 47  ω     32.00 118.00   0.50    3.20    --  107.75 -45.00   0.00  172
 48  ω     35.00  85.00   0.50    3.20    --  107.75 -77.00   0.00  100
 49  ω    146.00 178.00   0.50    3.20    --  107.75  30.00 150.00   64
 50  ω    140.00 172.00   0.50    3.20    --  107.75 111.00-120.00   64
 51  ω    130.00 173.00   0.50    3.20    --  107.75  15.00-180.00   86
 52  ω     64.00 138.00   0.50    3.20    --  107.75 178.00-180.00  148
 53  ω     94.00 144.00   0.50    3.20    --  107.75  48.00  32.35  100
 54  ω     36.00  67.00   0.50    3.20    --  107.75-111.00  90.00   62
 55  ω    101.00 173.00   0.50    3.20    --  107.75  77.00   0.00  144
 56  ω     95.00 120.00   0.50    3.20    --  107.75 -30.00-180.00   50
 57  ω     64.00  94.00   0.50    3.20    --  107.75 -15.00 -90.00   60
 58  ω     41.00  67.00   0.50    3.20    --  107.75-111.00-120.00   52
 59  ω     84.00 109.00   0.50    3.20    --  107.75-111.00-120.00   50
 60  ω     61.00  88.00   0.50    3.20    --  107.75   0.00 -30.00   54
 61  ω    140.00 166.00   0.50    3.20    --  107.75   0.00 -30.00   52
 62  ω     75.00 106.00   0.50    3.20    --  107.75 -94.00-180.00   62
 63  ω     56.00  82.00   0.50    3.20    --  107.75 -94.00-150.00   52
 64  ω    145.00 170.00   0.50    3.20    --  107.75  15.00  60.00   50
 65  ω     93.00 119.00   0.50    3.20    --  107.75 178.00 -90.00   52
 66  ω     64.00 108.00   0.50    3.20    --  107.75-111.00  60.00   88
 67  ω     91.00 116.00   0.50    3.20    --  107.75 -58.00 100.69   50
 68  ω     72.00  98.00   0.50    3.20    --  107.75 -50.00 -66.08   52
 69  ω     34.00  60.00   0.50    3.20    --  107.75 -38.00   9.15   52
 70  ω     71.00  99.00   0.50    3.20    --  107.75 -38.00   9.15   56
 71  ω     82.00 123.00   0.50    3.20    --  107.75 -77.00-150.00   82
 72  ω     52.00  78.00   0.50    3.20    --  107.75 -77.00 -90.00   52
 73  ω     91.00 129.00   0.50    3.20    --  107.75 -77.00 -90.00   76
 74  ω     97.00 122.00   0.50    3.20    --  107.75 -86.00 151.16   50
 75  ω     33.00  84.00   0.50    3.20    --  107.75 -86.00-109.06  102
 76  ω    103.00 129.00   0.50    3.20    --  107.75 -86.00-109.06   52
 77  ω     63.00 115.00   0.50    3.20    --  107.75 178.00-120.00  104
 78  ω   -121.00 -72.00   0.50    3.20    --  -86.25 -62.00-157.00   98
 79  ω    -70.00 -45.00   0.50    0.80    --   10.00 173.00  41.45   50
 80  ω    -32.00  -7.00   0.50    0.80    --  -26.00 -71.00 135.44   50
 81  ω    -31.00  -6.00   0.50    0.80    --  -26.00 -72.00 -34.07   50
 82  ω      6.00  31.00   0.50    0.80    --   26.00  71.00   8.66   50
 83  ω    -37.00 -12.00   0.50    0.80    --  -30.00 -67.00 172.77   50
 84  ω     13.00  38.00   0.50    0.80    --   30.00  63.00  79.74   50
 85  ω    -44.00 -19.00   0.50    0.80    --  -34.00 -63.00 113.42   50
 86  ω    -50.00 -25.00   0.50    0.80    --  -38.00 -60.00 121.58   50
 87  ω     22.00  47.00   0.50    0.80    --   38.00  61.00 103.64   50
 88  ω     23.00  48.00   0.50    0.80    --   38.00  59.00 142.22   50
 89  ω     22.00  47.00   0.50    0.80    --   38.00  60.00-143.98   50
 90  ω     22.00  47.00   0.50    0.80    --   38.00  60.00-166.13   50
 91  ω    -95.00 -41.00   0.50    0.80    --  -42.00 157.00 -50.77  108
 92  ω    -64.00 -37.00   0.50    0.80    --  -52.03 -56.00-132.99   54
 93  ω     54.00  79.00   0.50    0.80    --   52.03  19.00   0.00   50
 94  ω    -78.00 -45.00   0.50    0.80    --  -58.00 -54.00  39.36   66
 95  ω    -80.00 -46.00   0.50    0.80    --  -58.00 -56.00 -46.22   68
 96  ω    -78.00 -43.00   0.50    0.80    --  -58.00 -56.00 -68.60   70
 97  ω    -81.00 -43.00   0.50    0.80    --  -58.00 -56.00 -98.80   76
 98  ω     43.00  85.00   0.50    0.80    --   58.00  56.00-137.40   84
 99  ω     46.00  72.00   0.50    0.80    --   58.00  55.00  77.86   52
100  ω    -74.00 -48.00   0.50    0.80    --  -62.00 -54.00 110.73   52
101  ω    -76.00 -51.00   0.50    0.80    --  -66.00 -55.00  43.45   50
102  ω   -137.00-112.00   0.50    0.80    --  -66.00 -55.00  43.45   50
103  ω    -77.00 -51.00   0.50    0.80    --  -66.00 -55.00  87.72   52
104  ω    -78.00 -52.00   0.50    0.80    --  -66.00 -54.00 -13.48   52
105  ω    -82.00 -56.00   0.50    0.80    --  -70.00 -53.00  15.46   52
106  ω    -80.00 -55.00   0.50    0.80    --  -70.00 -56.00 -25.70   50
107  ω    -87.00 -61.00   0.50    0.80    --  -74.00 -50.00-148.23   52
108  ω    -84.00 -59.00   0.50    0.80    --  -74.00 -56.00 143.67   50
109  ω    -86.00 -60.00   0.50    0.80    --  -74.00 -52.00  82.64   52
110  ω    -93.00 -64.00   0.50    0.80    --  -78.00 -56.00  80.70   58
111  ω    -90.00 -64.00   0.50    0.80    --  -78.00 -56.00-159.02   52
112  ω    -89.00 -64.00   0.50    0.80    --  -78.00 -53.00   8.14   50
113  ω   -134.00-108.00   0.50    0.80    --  -78.00 -53.00   8.14   52
114  ω    -91.00 -65.00   0.50    0.80    --  -78.00 -56.00 -27.39   52
115  ω    -92.00 -66.00   0.50    0.80    --  -78.00 -50.00  47.41   52
116  ω   -101.00 -75.00   0.50    3.20    --  -86.25 -51.00 169.16   52
117  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -55.00-103.98   50
118  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -55.00 -47.25   50
119  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -52.00 -69.54   50
120  ω    -98.00 -72.00   0.50    3.20    --  -86.25 -54.00 -78.62   52
121  ω    -98.00 -72.00   0.50    3.20    --  -86.25 -53.00-118.44   52
122  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -55.00 133.08   50
123  ω    -98.00 -72.00   0.50    3.20    --  -86.25 -55.00 119.78   52
124  ω   -102.00 -77.00   0.50    3.20    --  -86.25 -56.00   7.02   50
125  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -52.00  42.35   50
126  ω   -100.00 -74.00   0.50    3.20    --  -86.25 -55.00 155.92   52
127  ω    -99.00 -73.00   0.50    3.20    --  -86.25 -55.00-135.76   52
128  ω   -102.00 -76.00   0.50    3.20    --  -86.25 -55.00 -86.11   52
129  ω   -102.00 -77.00   0.50    3.20    --  -86.25 -56.00  -4.42   50
130  ω   -138.00-112.00   0.50    3.20    --  -86.25 -56.00  -4.42   52
131  ω    -97.00 -72.00   0.50    3.20    --  -86.25 -55.00  93.79   50
132  ω    122.00 148.00   0.50    3.20    --  107.75  77.00  90.00   52
133  ω    150.00 177.00   0.50    3.20    --  107.75  61.00-180.00   54
134  ω     93.00 126.00   0.50    3.20    --  107.75  61.00 120.00   66
135  ω     92.00 117.00   0.50    3.20    --  107.75  61.00-180.00   50
136  ω     93.00 127.00   0.50    3.20    --  107.75  61.00   0.00   68
137  ω     92.00 118.00   0.50    3.20    --  107.75  61.00 -30.00   52
138  ω     86.00 113.00   0.50    3.20    --  107.75 -45.00 -90.00   54
139  ω     48.00  74.00   0.50    3.20    --  107.75 -45.00 -90.00   52
140  ω    153.00 178.00   0.50    3.20    --  107.75  61.00 150.00   50
141  ω     99.00 124.00   0.50    3.20    --  107.75  45.00  60.00   50
142  ω     92.00 128.00   0.50    3.20    --  107.75  61.00 150.00   72
143  ω    125.00 153.00   0.50    3.20    --  107.75  45.00 120.00   56
144  ω    126.00 171.00   0.50    3.20    --  107.75  61.00-150.00   90
145  ω    148.00 173.00   0.50    3.20    --  107.75  45.00-180.00   50
146  ω    104.00 143.00   0.50    3.20    --  107.75  45.00 150.00   78
147  ω     97.00 123.00   0.50    3.20    --  107.75  45.00 120.00   52
148  ω     92.00 118.00   0.50    3.20    --  107.75  61.00-150.00   52
149  ω     98.00 148.00   0.50    3.20    --  107.75  61.00  30.00  100
150  ω    138.00 164.00   0.50    3.20    --  107.75  61.00  60.00   52
151  ω     95.00 127.00   0.50    3.20    --  107.75  45.00-180.00   64
152  ω    142.00 167.00   0.50    3.20    --  107.75  45.00 -30.00   50
153  ω     92.00 125.00   0.50    3.20    --  107.75  61.00  60.00   66
154  ω     95.00 126.00   0.50    3.20    --  107.75  45.00 -30.00   62
155  ω     92.00 137.00   0.50    3.20    --  107.75  61.00-164.07   90
156  ω     94.00 145.00   0.50    3.20    --  107.75  61.00-120.00  102
157  ω     94.00 129.00   0.50    3.20    --  107.75  61.00  90.00   70
158  ω     97.00 130.00   0.50    3.20    --  107.75  45.00   0.00   66
159  ω    116.00 142.00   0.50    3.20    --  107.75 111.00  60.00   52
160  ω     92.00 122.00   0.50    3.20    --  107.75  61.00 -90.00   60
161  ω    134.00 167.00   0.50    3.20    --  107.75  45.00  90.00   66
162  ω     95.00 121.00   0.50    3.20    --  107.75  45.00  90.00   52
163  ω    104.00 143.00   0.50    3.20    --  107.75  45.00-120.00   78
164  ω    132.00 159.00   0.50    3.20    --  107.75  61.00 120.00   54
165  ω    129.00 172.00   0.50    3.20    --  107.75  61.00 -30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1808975000
_diffrn_orient_matrix_UB_12      -0.0134336000
_diffrn_orient_matrix_UB_13      -0.0017416000
_diffrn_orient_matrix_UB_21      0.0573311000
_diffrn_orient_matrix_UB_22      0.1089349000
_diffrn_orient_matrix_UB_23      0.0763192000
_diffrn_orient_matrix_UB_31      0.0160070000
_diffrn_orient_matrix_UB_32      -0.0602923000
_diffrn_orient_matrix_UB_33      0.0733306000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.239
_diffrn_reflns_theta_min         3.036
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.705
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.831
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6773
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1177P)²+4.4406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6637
_reflns_number_total             6773
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03992g2.cif
_cod_data_source_block           mlb-fs1-013_tc_auto
_cod_depositor_comments
'Adding full bibliography for 7714872--7714877.cif.'
_cod_original_formula_sum        'C26 H43 Cl0.40 F3.60 N O3 P2.60 Tc'
_cod_database_code               7714876
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H43 F6 N1 O3 P3 Tc1'
_chemical_oxdiff_usercomment     Pilatus
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.524
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.07
_olex2_refinement_description
;
1. Restrained distances
 P3-F4 \\sim P3-F1
 with sigma of 0.005
2. Rigid body (RIGU) restrains
 P3, F2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: P3(0.6) F1(0.6) F2(0.6) F3(0.6) F4(0.6) F5(0.6) F6(0.6) Cl1(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C)
;
_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 3.575
_oxdiff_exptl_absorpt_empirical_full_min 0.404
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.50760(3) 0.80385(2) 0.29938(2) 0.02461(13) Uani 1 1 d . . . . .
P1 P 0.37994(13) 0.90824(8) 0.19708(7) 0.0279(2) Uani 1 1 d . . . . .
P2 P 0.66873(12) 0.67013(8) 0.35358(7) 0.0253(2) Uani 1 1 d . . . . .
O1 O 0.1904(5) 0.6369(4) 0.2198(4) 0.0673(14) Uani 1 1 d . . . . .
O2 O 0.3717(6) 0.8979(4) 0.4658(3) 0.0634(12) Uani 1 1 d . . . . .
O3 O 0.8166(5) 0.9773(3) 0.3798(3) 0.0498(9) Uani 1 1 d . . . . .
N1 N 0.5924(4) 0.7261(3) 0.1765(2) 0.0256(7) Uani 1 1 d . . . . .
C1 C 0.3679(6) 0.8028(4) 0.0884(3) 0.0359(9) Uani 1 1 d . . . . .
H1A H 0.264823 0.752810 0.071814 0.043 Uiso 1 1 calc R U . . .
H1B H 0.362397 0.837808 0.039086 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5139(5) 0.7375(4) 0.0934(3) 0.0306(8) Uani 1 1 d . . . . .
C3 C 0.5641(6) 0.6881(4) 0.0150(3) 0.0390(10) Uani 1 1 d . . . . .
H3 H 0.510388 0.697952 -0.042296 0.047 Uiso 1 1 calc R U . . .
C4 C 0.6918(6) 0.6246(4) 0.0205(3) 0.0393(10) Uani 1 1 d . . . . .
H4 H 0.728064 0.591641 -0.032606 0.047 Uiso 1 1 calc R U . . .
C5 C 0.7666(6) 0.6095(4) 0.1041(3) 0.0337(9) Uani 1 1 d . . . . .
H5 H 0.851392 0.563323 0.108546 0.040 Uiso 1 1 calc R U . . .
C6 C 0.7164(5) 0.6624(3) 0.1813(3) 0.0274(8) Uani 1 1 d . . . . .
C7 C 0.8042(5) 0.6536(4) 0.2746(3) 0.0302(8) Uani 1 1 d . . . . .
H7A H 0.900972 0.710044 0.302118 0.036 Uiso 1 1 calc R U . . .
H7B H 0.845325 0.581747 0.267004 0.036 Uiso 1 1 calc R U . . .
C8 C 0.5566(6) 0.5296(3) 0.3275(3) 0.0339(9) Uani 1 1 d . . . . .
C9 C 0.4119(7) 0.5390(4) 0.3727(4) 0.0441(11) Uani 1 1 d . . . . .
H9A H 0.454167 0.549380 0.438712 0.066 Uiso 1 1 calc R U . . .
H9B H 0.334085 0.472383 0.344999 0.066 Uiso 1 1 calc R U . . .
H9C H 0.355137 0.601293 0.363239 0.066 Uiso 1 1 calc R U . . .
C10 C 0.4946(7) 0.4838(4) 0.2222(3) 0.0403(10) Uani 1 1 d . . . . .
H10A H 0.437846 0.538032 0.197337 0.060 Uiso 1 1 calc R U . . .
H10B H 0.417634 0.417689 0.206250 0.060 Uiso 1 1 calc R U . . .
H10C H 0.588760 0.466548 0.196087 0.060 Uiso 1 1 calc R U . . .
C11 C 0.6629(8) 0.4465(4) 0.3598(4) 0.0465(12) Uani 1 1 d . . . . .
H11A H 0.759631 0.442138 0.334554 0.070 Uiso 1 1 calc R U . . .
H11B H 0.597304 0.374975 0.338223 0.070 Uiso 1 1 calc R U . . .
H11C H 0.699487 0.469523 0.427024 0.070 Uiso 1 1 calc R U . . .
C12 C 0.8201(6) 0.7064(4) 0.4710(3) 0.0366(10) Uani 1 1 d . . . . .
C13 C 0.7280(8) 0.6924(5) 0.5413(3) 0.0487(13) Uani 1 1 d . . . . .
H13A H 0.633036 0.733980 0.537756 0.073 Uiso 1 1 calc R U . . .
H13B H 0.802732 0.718875 0.603203 0.073 Uiso 1 1 calc R U . . .
H13C H 0.689369 0.615255 0.528024 0.073 Uiso 1 1 calc R U . . .
C14 C 0.9676(7) 0.6398(5) 0.4729(4) 0.0511(13) Uani 1 1 d . . . . .
H14A H 0.927015 0.562230 0.446987 0.077 Uiso 1 1 calc R U . . .
H14B H 1.033198 0.654162 0.536516 0.077 Uiso 1 1 calc R U . . .
H14C H 1.036726 0.660636 0.436492 0.077 Uiso 1 1 calc R U . . .
C15 C 0.8922(7) 0.8260(4) 0.5008(4) 0.0444(11) Uani 1 1 d . . . . .
H15A H 0.967189 0.844492 0.562578 0.067 Uiso 1 1 calc R U . . .
H15B H 0.802310 0.871880 0.501401 0.067 Uiso 1 1 calc R U . . .
H15C H 0.953283 0.838064 0.457629 0.067 Uiso 1 1 calc R U . . .
C16 C 0.1600(6) 0.9396(4) 0.1894(3) 0.0362(9) Uani 1 1 d . . . . .
C17 C 0.0623(6) 0.8507(5) 0.2101(5) 0.0542(14) Uani 1 1 d . . . . .
H17A H 0.056556 0.781265 0.163146 0.081 Uiso 1 1 calc R U . . .
H17B H -0.049723 0.869324 0.209741 0.081 Uiso 1 1 calc R U . . .
H17C H 0.117554 0.844342 0.270641 0.081 Uiso 1 1 calc R U . . .
C18 C 0.0685(7) 0.9452(6) 0.0939(4) 0.0537(15) Uani 1 1 d . . . . .
H18A H 0.122735 1.005354 0.080160 0.081 Uiso 1 1 calc R U . . .
H18B H -0.046453 0.957022 0.092873 0.081 Uiso 1 1 calc R U . . .
H18C H 0.070793 0.876714 0.047623 0.081 Uiso 1 1 calc R U . . .
C19 C 0.1615(7) 1.0470(4) 0.2625(4) 0.0439(11) Uani 1 1 d . . . . .
H19A H 0.236918 1.047565 0.320939 0.066 Uiso 1 1 calc R U . . .
H19B H 0.049770 1.054501 0.270519 0.066 Uiso 1 1 calc R U . . .
H19C H 0.198854 1.107715 0.242910 0.066 Uiso 1 1 calc R U . . .
C20 C 0.5066(6) 1.0304(4) 0.1909(4) 0.0379(10) Uani 1 1 d . . . . .
C21 C 0.6624(6) 0.9890(4) 0.1643(4) 0.0408(11) Uani 1 1 d . . . . .
H21A H 0.714865 0.948536 0.205650 0.061 Uiso 1 1 calc R U . . .
H21B H 0.739957 1.051021 0.169281 0.061 Uiso 1 1 calc R U . . .
H21C H 0.631638 0.941236 0.100869 0.061 Uiso 1 1 calc R U . . .
C22 C 0.5556(7) 1.1193(4) 0.2845(4) 0.0484(12) Uani 1 1 d . . . . .
H22A H 0.465650 1.164650 0.289865 0.073 Uiso 1 1 calc R U . . .
H22B H 0.656042 1.164642 0.288879 0.073 Uiso 1 1 calc R U . . .
H22C H 0.576059 1.085271 0.334111 0.073 Uiso 1 1 calc R U . . .
C23 C 0.4211(8) 1.0809(5) 0.1162(5) 0.0545(15) Uani 1 1 d . . . . .
H23A H 0.377417 1.023335 0.057997 0.082 Uiso 1 1 calc R U . . .
H23B H 0.501293 1.132980 0.108462 0.082 Uiso 1 1 calc R U . . .
H23C H 0.330139 1.118353 0.134673 0.082 Uiso 1 1 calc R U . . .
C24 C 0.3042(6) 0.6971(4) 0.2481(4) 0.0388(10) Uani 1 1 d . . . . .
C25 C 0.4258(6) 0.8647(4) 0.4045(3) 0.0390(10) Uani 1 1 d . . . . .
C26 C 0.7064(6) 0.9137(4) 0.3514(3) 0.0331(9) Uani 1 1 d . . . . .
P3 P 0.0330(2) 0.68815(16) -0.17540(16) 0.0224(4) Uani 0.6 1 d D . P A 1
F1 F 0.0626(7) 0.7277(5) -0.2608(3) 0.0509(12) Uani 0.6 1 d D . P A 1
F2 F -0.0032(7) 0.5686(4) -0.2403(4) 0.0551(15) Uani 0.6 1 d . . P A 1
F3 F 0.2230(6) 0.6703(6) -0.1483(4) 0.0602(16) Uani 0.6 1 d . . P A 1
F4 F 0.0209(9) 0.6566(6) -0.0835(5) 0.081(2) Uani 0.6 1 d D . P A 1
F5 F 0.0892(7) 0.8123(4) -0.1137(3) 0.0502(13) Uani 0.6 1 d . . P A 1
F6 F -0.1533(5) 0.7120(4) -0.1976(4) 0.0518(14) Uani 0.6 1 d . . P A 1
Cl1 Cl 0.0214(3) 0.6783(2) -0.1510(2) 0.0152(7) Uiso 0.4 1 d . . P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc 0.0057 3.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 1 7 0.0383
0 5 -9 0.0302
-3 -2 10 0.0466
-3 7 -2 0.0190
3 -7 2 0.0209
0 -5 9 0.0433
-3 -4 -4 0.0735
3 7 -3 0.0569
0 -4 -7 0.0691
-3 4 7 0.0346
4 -3 -7 0.0468
-5 5 1 0.0282
5 -4 2 0.0285
-5 -2 5 0.0412
1 6 3 0.0343
-2 7 2 0.0244
-3 7 0 0.0170
-3 6 -5 0.0230
2 -3 8 0.0374
0 2 8 0.0353
-5 -2 4 0.0454
-2 -7 6 0.0393
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Tc1 P1 159.76(4) . . ?
N1 Tc1 P1 80.02(9) . . ?
N1 Tc1 P2 79.75(9) . . ?
C24 Tc1 P1 88.34(14) . . ?
C24 Tc1 P2 91.48(14) . . ?
C24 Tc1 N1 88.85(18) . . ?
C25 Tc1 P1 100.76(16) . . ?
C25 Tc1 P2 99.46(15) . . ?
C25 Tc1 N1 176.98(17) . . ?
C25 Tc1 C24 88.2(2) . . ?
C25 Tc1 C26 90.6(2) . . ?
C26 Tc1 P1 90.68(13) . . ?
C26 Tc1 P2 89.90(13) . . ?
C26 Tc1 N1 92.29(16) . . ?
C26 Tc1 C24 178.35(18) . . ?
C1 P1 Tc1 96.51(14) . . ?
C1 P1 C16 104.6(2) . . ?
C1 P1 C20 104.6(2) . . ?
C16 P1 Tc1 120.24(15) . . ?
C16 P1 C20 108.7(2) . . ?
C20 P1 Tc1 119.00(16) . . ?
C7 P2 Tc1 97.39(13) . . ?
C7 P2 C8 104.9(2) . . ?
C7 P2 C12 103.3(2) . . ?
C8 P2 Tc1 116.81(15) . . ?
C8 P2 C12 108.9(2) . . ?
C12 P2 Tc1 122.14(15) . . ?
C2 N1 Tc1 119.8(3) . . ?
C6 N1 Tc1 121.0(3) . . ?
C6 N1 C2 119.1(4) . . ?
P1 C1 H1A 109.0 . . ?
P1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 P1 113.0(3) . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N1 C2 C1 118.3(4) . . ?
N1 C2 C3 120.7(4) . . ?
C3 C2 C1 121.0(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.3(4) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(4) . . ?
C6 C5 H5 120.4 . . ?
N1 C6 C5 121.7(4) . . ?
N1 C6 C7 118.0(4) . . ?
C5 C6 C7 120.2(4) . . ?
P2 C7 H7A 109.1 . . ?
P2 C7 H7B 109.1 . . ?
C6 C7 P2 112.5(3) . . ?
C6 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 P2 108.9(3) . . ?
C9 C8 C10 111.2(4) . . ?
C9 C8 C11 107.9(4) . . ?
C10 C8 P2 107.1(3) . . ?
C10 C8 C11 106.2(4) . . ?
C11 C8 P2 115.5(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 P2 109.1(3) . . ?
C13 C12 C14 110.9(4) . . ?
C14 C12 P2 112.9(4) . . ?
C15 C12 P2 110.2(3) . . ?
C15 C12 C13 107.0(4) . . ?
C15 C12 C14 106.5(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P1 109.6(3) . . ?
C17 C16 C18 107.1(5) . . ?
C17 C16 C19 107.8(4) . . ?
C18 C16 P1 113.1(3) . . ?
C19 C16 P1 108.9(3) . . ?
C19 C16 C18 110.3(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 P1 106.4(3) . . ?
C21 C20 C22 110.0(4) . . ?
C21 C20 C23 106.1(4) . . ?
C22 C20 P1 111.0(3) . . ?
C23 C20 P1 114.2(4) . . ?
C23 C20 C22 108.9(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O1 C24 Tc1 179.5(5) . . ?
O2 C25 Tc1 177.3(5) . . ?
O3 C26 Tc1 178.4(4) . . ?
F1 P3 F4 174.0(4) . . ?
F2 P3 F1 88.6(3) . . ?
F2 P3 F3 88.2(3) . . ?
F2 P3 F4 95.5(4) . . ?
F2 P3 F5 173.1(4) . . ?
F2 P3 F6 95.0(3) . . ?
F3 P3 F1 89.8(3) . . ?
F3 P3 F4 86.1(4) . . ?
F3 P3 F5 86.8(3) . . ?
F5 P3 F1 86.6(3) . . ?
F5 P3 F4 88.9(3) . . ?
F6 P3 F1 90.9(3) . . ?
F6 P3 F3 176.8(3) . . ?
F6 P3 F4 93.0(4) . . ?
F6 P3 F5 90.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 P1 2.4578(10) . ?
Tc1 P2 2.4495(10) . ?
Tc1 N1 2.206(3) . ?
Tc1 C24 1.993(5) . ?
Tc1 C25 1.917(5) . ?
Tc1 C26 1.988(5) . ?
P1 C1 1.841(5) . ?
P1 C16 1.890(5) . ?
P1 C20 1.896(5) . ?
P2 C7 1.847(4) . ?
P2 C8 1.893(4) . ?
P2 C12 1.893(4) . ?
O1 C24 1.118(6) . ?
O2 C25 1.144(6) . ?
O3 C26 1.122(6) . ?
N1 C2 1.365(5) . ?
N1 C6 1.356(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.517(6) . ?
C2 C3 1.389(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(6) . ?
C6 C7 1.512(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.538(7) . ?
C8 C10 1.539(6) . ?
C8 C11 1.541(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.532(7) . ?
C12 C14 1.537(7) . ?
C12 C15 1.530(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.527(7) . ?
C16 C18 1.536(7) . ?
C16 C19 1.532(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.538(6) . ?
C20 C22 1.542(8) . ?
C20 C23 1.542(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
P3 F1 1.623(5) . ?
P3 F2 1.565(5) . ?
P3 F3 1.593(5) . ?
P3 F4 1.625(6) . ?
P3 F5 1.607(5) . ?
P3 F6 1.582(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tc1 P1 C1 C2 -35.7(4) . . . . ?
Tc1 P1 C16 C17 -28.6(4) . . . . ?
Tc1 P1 C16 C18 -148.0(4) . . . . ?
Tc1 P1 C16 C19 89.0(3) . . . . ?
Tc1 P1 C20 C21 56.3(4) . . . . ?
Tc1 P1 C20 C22 -63.4(4) . . . . ?
Tc1 P1 C20 C23 173.0(3) . . . . ?
Tc1 P2 C7 C6 -34.7(3) . . . . ?
Tc1 P2 C8 C9 -60.3(3) . . . . ?
Tc1 P2 C8 C10 60.1(4) . . . . ?
Tc1 P2 C8 C11 178.1(3) . . . . ?
Tc1 P2 C12 C13 87.6(4) . . . . ?
Tc1 P2 C12 C14 -148.6(3) . . . . ?
Tc1 P2 C12 C15 -29.7(4) . . . . ?
Tc1 N1 C2 C1 -0.8(5) . . . . ?
Tc1 N1 C2 C3 -179.2(4) . . . . ?
Tc1 N1 C6 C5 177.3(3) . . . . ?
Tc1 N1 C6 C7 -4.9(5) . . . . ?
P1 C1 C2 N1 28.1(5) . . . . ?
P1 C1 C2 C3 -153.6(4) . . . . ?
N1 C2 C3 C4 1.5(7) . . . . ?
N1 C6 C7 P2 29.6(5) . . . . ?
C1 P1 C16 C17 78.1(4) . . . . ?
C1 P1 C16 C18 -41.3(5) . . . . ?
C1 P1 C16 C19 -164.3(3) . . . . ?
C1 P1 C20 C21 -49.9(4) . . . . ?
C1 P1 C20 C22 -169.5(3) . . . . ?
C1 P1 C20 C23 66.8(4) . . . . ?
C1 C2 C3 C4 -176.7(5) . . . . ?
C2 N1 C6 C5 0.6(6) . . . . ?
C2 N1 C6 C7 178.4(4) . . . . ?
C2 C3 C4 C5 1.2(8) . . . . ?
C3 C4 C5 C6 -2.9(7) . . . . ?
C4 C5 C6 N1 2.0(7) . . . . ?
C4 C5 C6 C7 -175.7(4) . . . . ?
C5 C6 C7 P2 -152.6(4) . . . . ?
C6 N1 C2 C1 175.9(4) . . . . ?
C6 N1 C2 C3 -2.4(6) . . . . ?
C7 P2 C8 C9 -166.8(3) . . . . ?
C7 P2 C8 C10 -46.4(4) . . . . ?
C7 P2 C8 C11 71.6(4) . . . . ?
C7 P2 C12 C13 -164.7(4) . . . . ?
C7 P2 C12 C14 -40.9(4) . . . . ?
C7 P2 C12 C15 78.1(4) . . . . ?
C8 P2 C7 C6 85.6(3) . . . . ?
C8 P2 C12 C13 -53.6(4) . . . . ?
C8 P2 C12 C14 70.2(4) . . . . ?
C8 P2 C12 C15 -170.8(4) . . . . ?
C12 P2 C7 C6 -160.3(3) . . . . ?
C12 P2 C8 C9 83.2(4) . . . . ?
C12 P2 C8 C10 -156.4(3) . . . . ?
C12 P2 C8 C11 -38.4(4) . . . . ?
C16 P1 C1 C2 -159.3(3) . . . . ?
C16 P1 C20 C21 -161.1(3) . . . . ?
C16 P1 C20 C22 79.2(4) . . . . ?
C16 P1 C20 C23 -44.4(4) . . . . ?
C20 P1 C1 C2 86.5(4) . . . . ?
C20 P1 C16 C17 -170.7(4) . . . . ?
C20 P1 C16 C18 69.9(5) . . . . ?
C20 P1 C16 C19 -53.0(4) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.6061 0.6160 6.8116 0.4513 0.7364 0.5041
-0.3348 4.9577 -9.1796 -0.1112 -0.1797 -0.9774
-3.0109 -2.1106 9.5625 -0.5330 0.3273 0.7803
-3.3084 6.8237 -1.7552 -0.6871 0.4197 -0.5931
3.1743 -6.9252 2.1912 0.6634 -0.4052 0.6290
0.4770 -4.7157 9.2074 0.1336 0.2163 0.9671
-3.1731 -3.5871 -3.6157 -0.5195 -0.8486 -0.0997
2.8802 6.8204 -2.6321 0.4340 0.7072 -0.5581
0.0775 -3.5421 -7.3569 0.0744 -0.9429 -0.3247
-2.6720 3.5199 7.3380 -0.5434 0.7903 0.2831
3.5889 -3.3439 -6.6941 0.7058 -0.6694 -0.2318
-4.5547 4.9003 0.5471 -0.8907 0.3144 -0.3282
4.5218 -4.1815 2.2883 0.8702 -0.0216 0.4923
-4.9996 -2.4665 5.1407 -0.8802 -0.1630 0.4457
1.1969 6.0243 3.4385 0.1296 0.9873 -0.0919
-1.8953 7.4059 1.5980 -0.4451 0.8201 -0.3597
-3.4035 6.7252 0.0610 -0.7061 0.5421 -0.4555
-2.8694 6.3098 -4.9675 -0.5952 0.1437 -0.7906
2.3151 -3.1985 7.8689 0.4481 0.3848 0.8069
0.3762 2.3831 8.0136 0.0221 0.8928 0.4500
-5.1466 -2.3272 3.6583 -0.9061 -0.2694 0.3262
-2.0394 -7.3044 5.9180 -0.2811 -0.4610 0.8417
