Single-crystal quality data from polycrystalline samples: finding the needle in the haystack.
Bear, Joseph Charles; Terzoudis, Nikitas; Cockcroft, Jeremy Karl; IUCrJ 10 (2023) –; doi:10.1107/S2052252523008163

data_1570097
_publ_section_title
;
 Single-crystal quality data from polycrystalline samples: finding the
 needle in the haystack.
;
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252523008163
_journal_volume                  10
_journal_year                    2023
_chemical_formula_moiety         'C6 F6, C5 H5 N'
_chemical_formula_sum            'C11 H5 F6 N'
_chemical_formula_weight         265.16
_chemical_name_systematic        pyridine:hexafluorobenzene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.85770(10)
_cell_length_b                   10.4534(2)
_cell_length_c                   17.3482(3)
_cell_measurement_reflns_used    14128
_cell_measurement_temperature    150
_cell_measurement_theta_max      79.3690
_cell_measurement_theta_min      4.9320
_cell_volume                     1062.28(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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     38.00  63.00   0.50    0.75    --   49.53-118.00 -17.00   50
  2  \w     60.00  94.00   0.50    0.75    --   49.53-161.00-169.00   68
  3  \w    112.00 137.00   0.50    0.75    --  106.27 118.00  68.00   50
  4  \w     90.00 115.00   0.50    0.75    --  106.27 161.00-139.00   50
  5  \w     94.00 119.00   0.50    0.75    --  106.27-161.00-169.00   50
  6  \w     50.00  75.00   0.50    0.75    --  106.27-118.00 -17.00   50
  7  \w    -52.00 -17.00   0.50    0.75    --    2.00 132.00-128.34   70
  8  \w    -16.00  16.00   0.50    0.75    --   18.00  99.00  20.11   64
  9  \w      6.00  31.00   0.50    0.75    --   38.00  94.00-121.28   50
 10  \w     27.00  58.00   0.50    0.75    --   49.53 -38.00-120.00   62
 11  \w     43.00  75.00   0.50    0.75    --   49.53 -99.00-150.00   64
 12  \w     28.00  53.00   0.50    0.75    --   49.53  77.00 120.00   50
 13  \w     23.00  67.00   0.50    0.75    --   49.53 -77.00 -30.00   88
 14  \w     28.00  57.00   0.50    0.75    --   49.53  77.00   0.00   58
 15  \w     29.00  56.00   0.50    0.75    --   49.53  77.00 150.00   54
 16  \w     31.00  65.00   0.50    0.75    --   49.53  77.00  60.00   68
 17  \w     28.00  58.00   0.50    0.75    --   49.53  77.00-120.00   60
 18  \w     54.00  99.00   0.50    0.75    --   49.53-125.00-180.00   90
 19  \w     20.00  64.00   0.50    0.75    --   49.53 -77.00-120.00   88
 20  \w     34.00  60.00   0.50    0.75    --   54.00  76.00 -54.51   52
 21  \w     35.00  61.00   0.50    0.75    --   54.00  71.00-170.08   52
 22  \w     39.00  65.00   0.50    0.75    --   58.00  72.00 -84.88   52
 23  \w     49.00  77.00   0.50    0.75    --   62.00  64.00 -36.87   56
 24  \w     46.00  75.00   0.50    0.75    --   62.00  61.00-107.17   58
 25  \w     43.00  81.00   0.50    0.75    --   62.00  75.00-173.57   76
 26  \w     41.00  73.00   0.50    0.75    --   62.00  75.00  75.30   64
 27  \w    105.00 130.00   0.50    0.75    --   62.00  64.00 -36.87   50
 28  \w     98.00 127.00   0.50    0.75    --   62.00  75.00-173.57   58
 29  \w     99.00 137.00   0.50    0.75    --   66.00  53.00 -59.06   76
 30  \w     45.00  70.00   0.50    0.75    --   66.00  76.00  18.29   50
 31  \w     46.00  72.00   0.50    0.75    --   66.00  76.00  35.22   52
 32  \w    106.00 131.00   0.50    0.75    --   66.00  75.00 115.15   50
 33  \w     45.00  70.00   0.50    0.75    --   66.00  75.00 -10.28   50
 34  \w     45.00  70.00   0.50    0.75    --   66.00  76.00  63.75   50
 35  \w     45.00  71.00   0.50    0.75    --   66.00  75.00 115.15   52
 36  \w     55.00  83.00   0.50    0.75    --   66.00  53.00 -59.06   56
 37  \w     92.00 118.00   0.50    0.75    --   74.00  69.00 -11.03   52
 38  \w     56.00  82.00   0.50    0.75    --   74.00  69.00 -11.03   52
 39  \w     62.00 135.00   0.50    0.75    --   78.00  62.00 148.49  146
 40  \w     99.00 152.00   0.50    0.75    --   86.00  73.00-126.31  106
 41  \w     67.00  99.00   0.50    0.75    --   86.00  71.00  95.44   64
 42  \w     66.00  93.00   0.50    0.75    --   86.00  73.00-126.31   54
 43  \w     73.00 158.00   0.50    0.75    --   90.00  65.00   4.43  170
 44  \w    120.00 159.00   0.50    0.75    --   94.00  69.00  49.94   78
 45  \w     76.00 106.00   0.50    0.75    --   94.00  69.00  49.94   60
 46  \w     86.00 131.00   0.50    0.75    --  106.27  77.00  30.00   90
 47  \w     84.00 170.00   0.50    0.75    --  106.27  77.00 120.00  172
 48  \w     84.00 166.00   0.50    0.75    --  106.27  77.00-120.00  164
 49  \w     56.00  88.00   0.50    0.75    --  106.27 -77.00 -60.00   64
 50  \w    125.00 170.00   0.50    0.75    --  106.27  77.00 150.00   90
 51  \w    123.00 168.00   0.50    0.75    --  106.27  77.00  90.00   90
 52  \w     84.00 116.00   0.50    0.75    --  106.27  77.00 150.00   64
 53  \w    144.00 175.00   0.50    0.75    --  106.27  61.00 -30.00   62
 54  \w     87.00 119.00   0.50    0.75    --  106.27  77.00  90.00   64
 55  \w     84.00 136.00   0.50    0.75    --  106.27  77.00 -30.00  104
 56  \w    125.00 163.00   0.50    0.75    --  106.27  77.00 -90.00   76
 57  \w     91.00 133.00   0.50    0.75    --  106.27  61.00-180.00   84
 58  \w     92.00 121.00   0.50    0.75    --  106.27  61.00 -30.00   58
 59  \w     46.00 103.00   0.50    0.75    --  106.27 -94.00-150.00  114
 60  \w     84.00 114.00   0.50    0.75    --  106.27  77.00 -90.00   60
 61  \w    135.00 164.00   0.50    0.75    --  106.27  77.00  60.00   58
 62  \w    103.00 128.00   0.50    0.75    --  106.27 -77.00 -60.00   50
 63  \w     92.00 124.00   0.50    0.75    --  106.27  61.00-150.00   64
 64  \w    147.00 174.00   0.50    0.75    --  106.27  61.00-150.00   54
 65  \w     45.00 105.00   0.50    0.75    --  106.27 -94.00  90.00  120
 66  \w    123.00 169.00   0.50    0.75    --  106.27  77.00 -60.00   92
 67  \w     84.00 132.00   0.50    0.75    --  106.27  77.00  60.00   96
 68  \w     84.00 120.00   0.50    0.75    --  106.27  77.00 -60.00   72
 69  \w    128.00 167.00   0.50    0.75    --  106.27  77.00-180.00   78
 70  \w     84.00 138.00   0.50    0.75    --  106.27  77.00-150.00  108
 71  \w     84.00 110.00   0.50    0.75    --  106.27  77.00-180.00   52
 72  \w    130.00 160.00   0.50    0.75    --  106.27  77.00   0.00   60
 73  \w     84.00 110.00   0.50    0.75    --  106.27  77.00   0.00   52
 74  \w     41.00 104.00   0.50    0.75    --  106.27-125.00 -60.00  126
 75  \w    127.00 152.00   0.50    0.75    --  106.27  61.00 150.00   50
 76  \w     95.00 121.00   0.50    0.75    --  106.27  61.00 150.00   52
 77  \w     62.00 102.00   0.50    0.75    --  106.27 -94.00  60.00   80
 78  \w     91.00 120.00   0.50    0.75    --  106.27  61.00 -60.00   58
 79  \w    139.00 165.00   0.50    0.75    --  110.75  53.00  28.65   52
 80  \w     98.00 123.00   0.50    0.75    --  110.75  53.00  28.65   50
 81  \w     38.00 120.00   0.50    0.75    --  110.75 -45.00 -55.84  164
 82  \w     69.00 107.00   0.50    0.75    --  110.75-101.00  12.36   76
 83  \w     47.00 112.00   0.50    0.75    --  110.75 -42.00  45.72  130
 84  \w     52.00 105.00   0.50    0.75    --  110.75 -89.00 173.54  106
 85  \w     80.00 108.00   0.50    0.75    --  110.75 -45.00-166.19   56
 86  \w     42.00  68.00   0.50    0.75    --  110.75 -45.00-166.19   52
 87  \w     83.00 109.00   0.50    0.75    --  110.75-117.00 -16.52   52
 88  \w     50.00  75.00   0.50    0.75    --  110.75-117.00 -16.52   50
 89  \w    104.00 132.00   0.50    0.75    --  110.75 -82.00  73.33   56
 90  \w     57.00  84.00   0.50    0.75    --  110.75 -82.00  73.33   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0337089000
_diffrn_orient_matrix_UB_12      -0.0636674000
_diffrn_orient_matrix_UB_13      0.0792773000
_diffrn_orient_matrix_UB_21      -0.0167936000
_diffrn_orient_matrix_UB_22      0.1329531000
_diffrn_orient_matrix_UB_23      0.0379478000
_diffrn_orient_matrix_UB_31      -0.2601874000
_diffrn_orient_matrix_UB_32      -0.0002962000
_diffrn_orient_matrix_UB_33      -0.0127543000
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.570
_diffrn_reflns_theta_min         4.939
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_preparation
'1:1 molar ratio of C6F6 and C5H5N (fresh bottle)'
_exptl_crystal_recrystallization_method
'Grown from the melt within the capillary at about 230K'
_exptl_crystal_size_max          0.862
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 726 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_coef       0.0048(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                1952
_reflns_number_total             2275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5060.cif
_cod_data_source_block           exp_299
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (34 times).

data item '_geom_bond_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (23 times).

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               1570097
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 F6 N C5 H5'
_chemical_oxdiff_usercomment
'0.2mm capillary - 1:1 molar ratio - sample slightly yellow (on bench 1 week)'
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.346
_olex2_refinement_description
;
;
_shelx_res_checksum              1513
_shelx_hkl_checksum              65511
_olex2_exptl_crystal_mounting_method '0.2mm X-ray capillary'
_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 5.813
_oxdiff_exptl_absorpt_empirical_full_min 0.591