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_1570096
_publ_section_title
;
 Single-crystal quality data from polycrystalline samples: finding the
 needle in the haystack.
;
_journal_coeditor_code           LT5060
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252523008163
_journal_volume                  10
_journal_year                    2023
_chemical_formula_moiety         '3(C6 F6), 4(C4 H5 N)'
_chemical_formula_sum            'C34 H20 F18 N4'
_chemical_formula_weight         826.54
_chemical_name_systematic        Hexafluorobenzene:pyrrole
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.284(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6847(3)
_cell_length_b                   5.8648(2)
_cell_length_c                   23.2236(5)
_cell_measurement_reflns_used    14714
_cell_measurement_temperature    150
_cell_measurement_theta_max      74.6860
_cell_measurement_theta_min      3.8400
_cell_volume                     1724.84(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (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 0.993
_diffrn_measured_fraction_theta_max 0.961
_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     55.00  80.00   0.50    2.00    --   49.53-145.00 111.00   50
  2  \w     55.00  81.00   0.50    2.00    --   49.53-126.00 -81.00   52
  3  \w     99.00 149.00   0.50    2.00    --  102.51 126.00  -4.00  100
  4  \w     75.00 103.00   0.50    2.00    --  102.51-126.00 -81.00   56
  5  \w     61.00  86.00   0.50    2.00    --  102.51-145.00 111.00   50
  6  \w    113.00 138.00   0.50    2.00    --  102.51 145.00 163.00   50
  7  \w    -58.00 -30.00   0.50    2.00    --   14.00 159.00  30.61   56
  8  \w    -17.00  12.00   0.50    2.00    --   18.00 100.00-102.84   58
  9  \w    -18.00   7.00   0.50    2.00    --   18.00 102.00 151.38   50
 10  \w      1.00  27.00   0.50    2.00    --   34.00  97.00  75.03   52
 11  \w      2.00  28.00   0.50    2.00    --   34.00  97.00 -15.96   52
 12  \w      2.00  32.00   0.50    2.00    --   34.00  94.00-157.31   60
 13  \w     90.00 124.00   0.50    2.00    --   49.53  19.00  90.00   68
 14  \w     31.00  57.00   0.50    2.00    --   49.53  77.00  60.00   52
 15  \w     81.00 106.00   0.50    2.00    --   49.53  77.00-120.00   50
 16  \w     28.00  55.00   0.50    2.00    --   49.53  77.00 -30.00   54
 17  \w     25.00  57.00   0.50    2.00    --   49.53 -38.00  30.00   64
 18  \w     14.00  74.00   0.50    2.00    --   49.53  19.00  90.00  120
 19  \w     31.00  57.00   0.50    2.00    --   49.53  77.00-180.00   52
 20  \w     78.00 105.00   0.50    2.00    --   49.53  77.00-180.00   54
 21  \w     28.00  63.00   0.50    2.00    --   49.53  77.00 120.00   70
 22  \w     38.00  97.00   0.50    2.00    --   49.53-125.00-180.00  118
 23  \w      5.00  42.00   0.50    2.00    --   49.53 -57.00 -60.00   74
 24  \w     19.00  80.00   0.50    2.00    --   49.53 -99.00 -30.00  122
 25  \w     29.00  55.00   0.50    2.00    --   49.53  77.00-120.00   52
 26  \w     74.00 100.00   0.50    2.00    --   54.00  76.00 -74.97   52
 27  \w     33.00  59.00   0.50    2.00    --   54.00  76.00 -74.97   52
 28  \w     38.00  64.00   0.50    2.00    --   58.00  74.00-155.17   52
 29  \w     39.00  66.00   0.50    2.00    --   58.00  72.00 156.98   54
 30  \w     40.00  65.00   0.50    2.00    --   62.00  77.00   2.93   50
 31  \w     94.00 120.00   0.50    2.00    --   62.00  77.00   2.93   52
 32  \w     57.00  83.00   0.50    2.00    --   62.00  64.00-129.90   52
 33  \w     51.00  76.00   0.50    2.00    --   66.00  58.00 -86.02   50
 34  \w     44.00  72.00   0.50    2.00    --   66.00  77.00  -7.72   56
 35  \w     45.00  70.00   0.50    2.00    --   66.00  75.00  51.32   50
 36  \w     45.00  76.00   0.50    2.00    --   66.00  76.00  34.84   62
 37  \w     51.00  76.00   0.50    2.00    --   66.00  65.00 -74.67   50
 38  \w     46.00  75.00   0.50    2.00    --   66.00  73.00 -17.48   58
 39  \w     89.00 115.00   0.50    2.00    --   66.00  77.00  -7.72   52
 40  \w     45.00  71.00   0.50    2.00    --   66.00  76.00  63.11   52
 41  \w     99.00 127.00   0.50    2.00    --   70.00  77.00 -50.38   56
 42  \w     48.00  74.00   0.50    2.00    --   70.00  77.00 -50.38   52
 43  \w     91.00 134.00   0.50    2.00    --   70.00  77.00  97.58   86
 44  \w     48.00  81.00   0.50    2.00    --   70.00  77.00  97.58   66
 45  \w     51.00  77.00   0.50    2.00    --   70.00  72.00  13.28   52
 46  \w     59.00  92.00   0.50    2.00    --   74.00  57.00 141.25   66
 47  \w    118.00 144.00   0.50    2.00    --   74.00  50.00-107.93   52
 48  \w     63.00  89.00   0.50    2.00    --   74.00  50.00-107.93   52
 49  \w     57.00  87.00   0.50    2.00    --   78.00  76.00 -50.70   60
 50  \w     58.00  84.00   0.50    2.00    --   78.00  74.00  58.73   52
 51  \w     58.00  84.00   0.50    2.00    --   78.00  74.00-169.59   52
 52  \w    108.00 155.00   0.50    2.00    --   86.00  59.00 -87.83   94
 53  \w     71.00  98.00   0.50    2.00    --   86.00  59.00 -87.83   54
 54  \w    124.00 156.00   0.50    2.00    --   90.00  72.00 151.49   64
 55  \w     71.00 117.00   0.50    2.00    --   90.00  72.00 151.49   92
 56  \w     74.00 154.00   0.50    2.00    --   90.00  72.00   6.67  160
 57  \w     74.00 160.00   0.50    2.00    --   90.00  62.00-158.53  172
 58  \w     78.00 162.00   0.50    2.00    --   94.00  63.00  51.05  168
 59  \w     82.00 162.00   0.50    2.00    --  102.51  77.00 -30.00  160
 60  \w    137.00 170.00   0.50    2.00    --  102.51  57.00-180.00   66
 61  \w     87.00 128.00   0.50    2.00    --  102.51  57.00-180.00   82
 62  \w     44.00 117.00   0.50    2.00    --  102.51 -57.00  60.00  146
 63  \w     81.00 166.00   0.50    2.00    --  102.51  77.00 120.00  170
 64  \w     81.00 148.00   0.50    2.00    --  102.51  77.00-120.00  134
 65  \w    140.00 166.00   0.50    2.00    --  102.51  77.00  60.00   52
 66  \w    132.00 161.00   0.50    2.00    --  102.51  77.00  90.00   58
 67  \w     81.00 127.00   0.50    2.00    --  102.51  77.00  90.00   92
 68  \w    139.00 166.00   0.50    2.00    --  102.51  77.00-150.00   54
 69  \w     81.00 117.00   0.50    2.00    --  102.51  77.00-150.00   72
 70  \w     81.00 122.00   0.50    2.00    --  102.51  77.00  60.00   82
 71  \w     53.00 103.00   0.50    2.00    --  102.51 -99.00 -30.00  100
 72  \w    131.00 157.00   0.50    2.00    --  102.51  77.00 -90.00   52
 73  \w     83.00 109.00   0.50    2.00    --  102.51  77.00 -90.00   52
 74  \w     89.00 115.00   0.50    2.00    --  102.51  57.00 -30.00   52
 75  \w     97.00 129.00   0.50    2.00    --  107.66 -76.00  -0.90   64
 76  \w     44.00  84.00   0.50    2.00    --  107.66 -76.00  -0.90   80
 77  \w     77.00 103.00   0.50    2.00    --  107.66 -34.00 -92.80   52
 78  \w     33.00  59.00   0.50    2.00    --  107.66 -34.00 -92.80   52
 79  \w     89.00 173.00   0.50    2.00    --  107.66  71.00 -56.89  168
 80  \w     74.00 103.00   0.50    2.00    --  107.66 -89.00 130.87   58
 81  \w     38.00 123.00   0.50    2.00    --  107.66 -62.00 176.81  170
 82  \w     96.00 124.00   0.50    2.00    --  107.66 -82.00  38.83   56
 83  \w     58.00  92.00   0.50    2.00    --  107.66 -82.00  38.83   68
 84  \w     81.00 107.00   0.50    2.00    --  107.66 -75.00-123.78   52
;
_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      0.0765306000
_diffrn_orient_matrix_UB_12      -0.0257062000
_diffrn_orient_matrix_UB_13      -0.0487968000
_diffrn_orient_matrix_UB_21      0.0941685000
_diffrn_orient_matrix_UB_22      -0.0026046000
_diffrn_orient_matrix_UB_23      0.0449236000
_diffrn_orient_matrix_UB_31      -0.0084097000
_diffrn_orient_matrix_UB_32      -0.2613423000
_diffrn_orient_matrix_UB_33      0.0043194000
_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  0.1005
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34525
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.093
_diffrn_reflns_theta_min         3.813
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_preparation
'Prepared from 1:1 molar ratio (1/100 mole scale)'
_exptl_crystal_recrystallization_method 'Grown in situ'
_exptl_crystal_size_max          0.943
_exptl_crystal_size_mid          0.436
_exptl_crystal_size_min          0.415
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0839P)^2^+0.7781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2925
_reflns_number_total             3554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5060.cif
_cod_data_source_block           exp_197
_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 (57 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 (39 times).

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               1570096
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         '(C6F6)3 (C4H4N)4'
_chemical_oxdiff_usercomment     'Grown from 1:1 molar mixture (1/100 mole)'
_shelx_estimated_absorpt_t_max   0.580
_shelx_estimated_absorpt_t_min   0.337
_olex2_refinement_description
;
;
_shelx_res_checksum              9921
_shelx_hkl_checksum              37828
_olex2_exptl_crystal_mounting_method '0.4um 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 7.576
_oxdiff_exptl_absorpt_empirical_full_min 0.375