Di- and tetranuclear transition metal complexes of a tetrakisguanidino-substituted phenazine dye by stepwise coordination.
Lorenz, Roxana; Kaifer, Elisabeth; Wadepohl, Hubert; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11016–11029; doi:10.1039/c8dt02176g

data_7047006
_publ_section_title
;
 Di- and tetranuclear transition metal complexes of a
 tetrakisguanidino-substituted phenazine dye by stepwise coordination.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11016
_journal_page_last               11029
_journal_paper_doi               10.1039/c8dt02176g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(Br), 2(C H2 Cl2), C46 H66 N14'
_chemical_formula_sum            'C48 H70 Br2 Cl4 N14'
_chemical_formula_weight         1144.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_rl2
_audit_creation_date             2016-04-01
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7601(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.13680(10)
_cell_length_b                   13.78213(10)
_cell_length_c                   11.10358(6)
_cell_measurement_reflns_used    70873
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6450
_cell_measurement_theta_min      4.0560
_cell_volume                     2706.95(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -69.00  21.00   1.00    2.00    --    0.00 -57.00 -90.00   90
  2  \w    -30.00  70.00   1.00    2.00    --    0.00  77.00-120.00  100
  3  \w    -30.00  70.00   1.00    2.00    --    0.00  77.00   0.00  100
  4  \w    -56.00  42.00   1.00    2.00    --   14.00 -74.00-132.08   98
  5  \w    -40.00   3.00   1.00    2.00    --   14.00 119.00  21.05   43
  6  \w    -31.00   4.00   1.00    2.00    --   22.00 118.00  99.05   35
  7  \w    -46.00 -14.00   1.00    2.00    --   26.00 148.00 -33.53   32
  8  \w    -17.00  12.00   1.00    4.00    --   30.00 108.00-172.83   29
  9  \w     -1.00  27.00   1.00    4.00    --   38.00  93.00  27.34   28
 10  \w      5.00  33.00   1.00    4.00    --   42.00  89.00 166.73   28
 11  \w      6.00  33.00   1.00    4.00    --   42.00  88.00  14.63   27
 12  \w      6.00  33.00   1.00    4.00    --   42.00  88.00 -34.04   27
 13  \w      7.00  35.00   1.00    4.00    --   42.00  86.00-131.63   28
 14  \w     12.00  38.00   1.00    4.00    --   46.00  84.00-106.24   26
 15  \w     13.00  40.00   1.00    4.00    --   46.00  83.00 121.82   27
 16  \w     13.00  45.00   1.00    4.00    --   46.00  82.00 102.96   32
 17  \w     14.00  46.00   1.00    4.00    --   46.00  81.00-178.50   32
 18  \w     23.00  49.00   1.00    4.00    --   54.00  78.00 -37.25   26
 19  \w     23.00 111.00   1.00    4.00    --   54.00-125.00 -90.00   88
 20  \w     23.00  49.00   1.00    4.00    --   54.00  78.00  17.09   26
 21  \w     23.00  49.00   1.00    4.00    --   54.00  78.00 -78.21   26
 22  \w     24.00 124.00   1.00    4.00    --   54.00  77.00  30.00  100
 23  \w     24.00 124.00   1.00    4.00    --   54.00  77.00-120.00  100
 24  \w    -18.00  80.00   1.00    4.00    --   54.00 -38.00  90.00   98
 25  \w     24.00 124.00   1.00    4.00    --   54.00  77.00  60.00  100
 26  \w     23.00  49.00   1.00    4.00    --   54.00  78.00  47.80   26
 27  \w     24.00 124.00   1.00    4.00    --   54.00  77.00-150.00  100
 28  \w     23.00  49.00   1.00    4.00    --   54.00  78.00-103.47   26
 29  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
 30  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 -60.00  100
 31  \w     23.00  49.00   1.00    4.00    --   54.00  78.00 -14.31   26
 32  \w     23.00 111.00   1.00    4.00    --   54.00-125.00   0.00   88
 33  \w      1.00  96.00   1.00    4.00    --   54.00 -99.00  60.00   95
 34  \w     30.00 128.00   1.00    4.00    --   58.00  74.00  91.35   98
 35  \w     28.00 128.00   1.00    4.00    --   58.00  77.00-154.75  100
 36  \w     28.00 128.00   1.00    4.00    --   58.00  77.00 131.14  100
 37  \w     29.00 128.00   1.00    4.00    --   58.00  75.00 116.47   99
 38  \w     30.00 127.00   1.00    4.00    --   58.00  73.00  34.07   97
 39  \w     28.00 128.00   1.00    4.00    --   58.00  77.00-177.31  100
 40  \w     30.00 127.00   1.00    4.00    --   58.00  73.00-115.59   97
 41  \w     29.00 128.00   1.00    4.00    --   58.00  75.00-136.02   99
 42  \w     28.00 128.00   1.00    4.00    --   58.00  77.00 149.26  100
 43  \w     29.00 128.00   1.00    4.00    --   58.00  75.00 -22.90   99
 44  \w     29.00 128.00   1.00    4.00    --   58.00  75.00 103.68   99
 45  \w     32.00 132.00   1.00    4.00    --   62.00  77.00  33.98  100
 46  \w     33.00 132.00   1.00    4.00    --   62.00  76.00 145.57   99
 47  \w     41.00 131.00   1.00    4.00    --   62.00  57.00 -43.81   90
 48  \w     34.00 132.00   1.00    4.00    --   62.00  74.00 -17.62   98
 49  \w     38.00 135.00   1.00    4.00    --   66.00  73.00-161.26   97
 50  \w     44.00 136.00   1.00    4.00    --   66.00  50.00 133.93   92
 51  \w     44.00 134.00   1.00    4.00    --   66.00  62.00 -96.87   90
 52  \w     42.00 134.00   1.00    4.00    --   66.00  67.00 -18.77   92
 53  \w     37.00 136.00   1.00    4.00    --   66.00  76.00 160.06   99
 54  \w     45.00 135.00   1.00    4.00    --   66.00  56.00 -35.27   90
 55  \w     49.00 139.00   1.00    4.00    --   70.00  58.00 144.19   90
 56  \w     49.00 139.00   1.00    4.00    --   70.00  56.00 -98.04   90
 57  \w     40.00 140.00   1.00    4.00    --   70.00  77.00 -18.57  100
 58  \w     53.00 143.00   1.00    4.00    --   74.00  58.00  90.04   90
 59  \w     51.00 145.00   1.00    4.00    --   74.00  48.00 -12.22   94
 60  \w     51.00 142.00   1.00    4.00    --   74.00  66.00 137.21   91
 61  \w     50.00 142.00   1.00    4.00    --   74.00  67.00  26.95   92
 62  \w     57.00 147.00   1.00    4.00    --   78.00  55.00-123.70   90
 63  \w     55.00 145.00   1.00    4.00    --   78.00  64.00   3.81   90
 64  \w     55.00 145.00   1.00    4.00    --   78.00  64.00-114.43   90
 65  \w     57.00 148.00   1.00    4.00    --   78.00  52.00  59.88   91
 66  \w     57.00 148.00   1.00    4.00    --   78.00  53.00-160.93   91
 67  \w     54.00 152.00   1.00    8.00    --   82.00  74.00 -44.00   98
 68  \w     52.00 152.00   1.00    8.00    --   82.00  77.00-110.20  100
 69  \w     59.00 149.00   1.00    8.00    --   82.00  64.00 -79.41   90
 70  \w     55.00 151.00   1.00    8.00    --   82.00  72.00  60.68   96
 71  \w     63.00 157.00   1.00    8.00    --   86.00  48.00  97.55   94
 72  \w     64.00 154.00   1.00    8.00    --   86.00  63.00 158.19   90
 73  \w     64.00 156.00   1.00    8.00    --   86.00  50.00 -47.62   92
 74  \w     63.00 153.00   1.00    8.00    --   86.00  64.00-171.36   90
 75  \w     63.00 159.00   1.00    8.00    --   90.00  72.00-125.66   96
 76  \w     63.00 159.00   1.00    8.00    --   90.00  71.00 120.10   96
 77  \w     66.00 158.00   1.00    8.00    --   90.00  68.00 -10.49   92
 78  \w     61.00 160.00   1.00    8.00    --   90.00  75.00  52.58   99
 79  \w     69.00 166.00   1.00    8.00    --   94.00  41.00 -48.53   97
 80  \w     77.00 167.00   1.00    8.00    --   98.00  56.00  17.89   90
 81  \w     36.00 116.00   1.00    8.00    --  108.00-111.00-180.00   80
 82  \w     82.00 178.00   1.00    8.00    --  108.00  38.00  90.00   96
 83  \w     78.00 178.00   1.00    8.00    --  108.00  77.00  98.63  100
 84  \w     82.00 178.00   1.00    8.00    --  108.00  38.00-150.00   96
 85  \w     86.00 176.00   1.00    8.00    --  108.00  62.00 158.73   90
 86  \w     85.00 175.00   1.00    8.00    --  108.00  64.00 150.00   90
 87  \w     85.00 175.00   1.00    8.00    --  108.00  64.00  30.00   90
 88  \w     85.00 175.00   1.00    8.00    --  108.00  64.00   0.00   90
 89  \w     80.00 178.00   1.00    8.00    --  108.00  74.00  85.78   98
 90  \w     85.00 175.00   1.00    8.00    --  108.00  64.00 -90.00   90
 91  \w     85.00 175.00   1.00    8.00    --  108.00  64.00  60.00   90
 92  \w     85.00 175.00   1.00    8.00    --  108.00  64.00-120.00   90
 93  \w     36.00 116.00   1.00    8.00    --  108.00-111.00   0.00   80
 94  \w     85.00 175.00   1.00    8.00    --  108.00  64.00 -60.00   90
 95  \w     85.00 175.00   1.00    8.00    --  108.00  64.00-180.00   90
 96  \w     78.00 178.00   1.00    8.00    --  108.00  77.00 150.00  100
 97  \w     78.00 178.00   1.00    8.00    --  108.00  77.00-150.00  100
 98  \w     78.00 178.00   1.00    8.00    --  108.00  77.00 -30.00  100
 99  \w     78.00 178.00   1.00    8.00    --  108.00  77.00  30.00  100
100  \w     78.00 178.00   1.00    8.00    --  108.00  77.00 -90.00  100
101  \w     78.00 178.00   1.00    8.00    --  108.00  77.00  60.00  100
102  \w     82.00 178.00   1.00    8.00    --  108.00  38.00 120.00   96
103  \w     78.00 178.00   1.00    8.00    --  108.00  77.00-120.00  100
104  \w     37.00 125.00   1.00    8.00    --  108.00-132.00 -46.00   88
105  \w     87.00 178.00   1.00    8.00    --  108.00 137.00-160.00   91
106  \w     78.00 178.00   1.00    8.00    --  108.00  77.00 120.00  100
107  \w     78.00 178.00   1.00    8.00    --  108.00  77.00   0.00  100
108  \w     78.00 178.00   1.00    8.00    --  108.00  77.00-180.00  100
109  \w     82.00 178.00   1.00    8.00    --  108.00  38.00 -90.00   96
110  \w     82.00 178.00   1.00    8.00    --  108.00  38.00  60.00   96
111  \w     78.00 178.00   1.00    8.00    --  108.00  77.00 -60.00  100
112  \w     41.00 131.00   1.00    8.00    --  108.00 -64.00 -30.00   90
113  \w     85.00 175.00   1.00    8.00    --  108.00  64.00 -30.00   90
114  \w     85.00 175.00   1.00    8.00    --  108.00  64.00-150.00   90
115  \w    100.00 178.00   1.00    8.00    --  108.00 111.00-120.00   78
116  \w     78.00 178.00   1.00    8.00    --  108.00  77.00  90.00  100
117  \w     41.00 131.00   1.00    8.00    --  108.00 -64.00 150.00   90
118  \w     36.00 146.00   1.00    8.00    --  108.00 -92.00 -60.00  110
119  \f    120.00 240.00   1.00    2.00   0.00   0.00 -40.00    --   120
120  \f    120.00 240.00   1.00    2.00   0.00   0.00  40.00    --   120
121  \f      0.00 120.00   1.00    2.00   0.00   0.00 -60.00    --   120
122  \f      0.00 120.00   1.00    2.00   0.00   0.00  60.00    --   120
123  \f      0.00 120.00   1.00    2.00   0.00   0.00  40.00    --   120
124  \f    120.00 240.00   1.00    2.00   0.00   0.00  60.00    --   120
125  \f      0.00 120.00   1.00    2.00   0.00   0.00 -40.00    --   120
126  \f    120.00 240.00   1.00    2.00   0.00   0.00 -60.00    --   120
127  \f    120.00 240.00   1.00    4.00  54.00  54.00  40.00    --   120
128  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 -60.00  100
129  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
130  \f    120.00 240.00   1.00    4.00  54.00  54.00 -40.00    --   120
131  \w     24.00 124.00   1.00    4.00    --   54.00  77.00  30.00  100
132  \f    120.00 240.00   1.00    4.00  54.00  54.00 -60.00    --   120
133  \f      0.00 120.00   1.00    4.00  54.00  54.00  60.00    --   120
134  \f      0.00 120.00   1.00    4.00  54.00  54.00 -60.00    --   120
135  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00  30.00  100
136  \f    240.00 360.00   1.00    4.00  54.00  54.00  60.00    --   120
137  \f      0.00 120.00   1.00    4.00  54.00  54.00  40.00    --   120
138  \w     24.00 124.00   1.00    4.00    --   54.00  77.00-180.00  100
139  \w     24.00 124.00   1.00    4.00    --   54.00  77.00-150.00  100
140  \w     24.00 124.00   1.00    4.00    --   54.00  77.00-120.00  100
141  \f    240.00 360.00   1.00    4.00  54.00  54.00 -60.00    --   120
142  \f    240.00 360.00   1.00    4.00  54.00  54.00  40.00    --   120
143  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 -30.00  100
144  \w     24.00 124.00   1.00    4.00    --   54.00  77.00   0.00  100
145  \f      0.00 120.00   1.00    4.00  54.00  54.00 -40.00    --   120
146  \w     24.00 124.00   1.00    4.00    --   54.00  77.00  60.00  100
147  \w     24.00 124.00   1.00    4.00    --   54.00  77.00  90.00  100
148  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 120.00  100
149  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00-120.00  100
150  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00-150.00  100
151  \f    240.00 360.00   1.00    4.00  54.00  54.00 -40.00    --   120
152  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00-180.00  100
153  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -90.00  100
154  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -60.00  100
155  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -30.00  100
156  \w    -16.00  84.00   1.00    4.00    --   54.00 -77.00   0.00  100
157  \w     24.00 124.00   1.00    4.00    --   54.00  77.00 150.00  100
158  \w    -16.00  75.00   1.00    4.00    --   54.00 -77.00  60.00   91
159  \f    120.00 240.00   1.00    4.00  54.00  54.00  60.00    --   120
160  \f      0.00 270.00   1.00    0.50   0.00   0.00   0.00    --   270
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0850964000
_diffrn_orient_matrix_UB_12      -0.0015814000
_diffrn_orient_matrix_UB_13      -0.0601525000
_diffrn_orient_matrix_UB_21      0.0184627000
_diffrn_orient_matrix_UB_22      0.0028751000
_diffrn_orient_matrix_UB_23      -0.1288886000
_diffrn_orient_matrix_UB_31      0.0016625000
_diffrn_orient_matrix_UB_32      -0.1117310000
_diffrn_orient_matrix_UB_33      -0.0024336000
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            160921
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.828
_diffrn_reflns_theta_min         4.066
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0417
_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/[\s^2^(Fo^2^)+(0.0519P)^2^+4.8954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4965
_reflns_number_total             5194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02176g2.cif
_cod_data_source_block           hi_rl2
_cod_depositor_comments
'Adding full bibliography for 7047000--7047008.cif.'
_cod_database_code               7047006
_audit_block_refno               2688
_audit_block_usercomment         'rl129, irregular, red'
_chemical_oxdiff_formula         'C48 H70 Br2 Cl4 N14'
_chemical_oxdiff_usercomment     'rl129, irregular, red'
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.685
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2017/1
_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.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.848
_shelx_res_checksum              2355
_cell_oxdiff_length_a            18.13636(12)
_cell_oxdiff_length_b            13.78219(12)
_cell_oxdiff_length_c            11.10352(9)
_cell_oxdiff_angle_alpha         89.9844(7)
_cell_oxdiff_angle_beta          102.7537(6)
_cell_oxdiff_angle_gamma         90.0143(6)
_cell_oxdiff_volume              2706.95(4)
_cell_oxdiff_measurement_reflns_used 70873