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_1570098
_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 H1 F5, C8 H10'
_chemical_formula_sum            'C14 H11 F5'
_chemical_formula_weight         274.23
_chemical_name_systematic        p-xylene:pentafluorobenzene
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                108.087(7)
_cell_angle_beta                 93.949(6)
_cell_angle_gamma                98.796(6)
_cell_formula_units_Z            1
_cell_length_a                   6.3499(4)
_cell_length_b                   7.2178(5)
_cell_length_c                   7.3804(5)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    160
_cell_measurement_theta_max      71.9300
_cell_measurement_theta_min      7.5150
_cell_volume                     315.32(4)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.969
_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      2.00  27.00   1.00    1.00    --   38.00  88.00 -13.49   25
  2  \w      4.00  29.00   1.00    1.00    --   38.00  83.00-112.20   25
  3  \w    -21.00  31.00   1.00    1.00    --  -42.37  38.00-180.00   52
  4  \w    -62.00 -21.00   1.00    1.00    --  -42.37 -38.00   0.00   41
  5  \w   -102.00 -68.00   1.00    1.00    --  -42.37 -38.00   0.00   34
  6  \w    -59.00 -23.00   1.00    1.00    --  -42.37  38.00-180.00   36
  7  \w     28.00  86.00   1.00    1.00    --   42.37-125.00 -30.00   58
  8  \w      9.00  67.00   1.00    1.00    --   42.37 -38.00 -30.00   58
  9  \w     13.00  38.00   1.00    1.00    --   46.00  79.00  89.18   25
 10  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 -99.72   25
 11  \w     94.00 125.00   1.00    1.00    --   54.00  71.00 134.56   31
 12  \w     78.00 127.00   1.00    1.00    --   54.00  64.00  87.94   49
 13  \w     97.00 123.00   1.00    1.00    --   54.00  71.00  26.48   26
 14  \w     26.00  67.00   1.00    1.00    --   54.00  71.00  26.48   41
 15  \w     24.00  74.00   1.00    1.00    --   54.00  71.00 134.56   50
 16  \w     28.00  60.00   1.00    1.00    --   54.00  64.00  87.94   32
 17  \w     28.00  63.00   1.00    1.00    --   58.00  71.00-136.54   35
 18  \w     36.00  61.00   1.00    1.00    --   66.00  70.00 167.18   25
 19  \w     40.00  65.00   1.00    1.00    --   70.00  69.00 -96.67   25
 20  \w     43.00  78.00   1.00    1.00    --   70.00  61.00  -6.66   35
 21  \w     46.00  71.00   1.00    1.50    --   74.00  67.00 -55.22   25
 22  \w     54.00  80.00   1.00    1.50    --   78.00  69.00  29.02   26
 23  \w     55.00  81.00   1.00    1.50    --   82.00  59.00 -77.65   26
 24  \w     55.00  89.00   1.00    1.50    --   82.00  58.00-174.80   34
 25  \w     66.00  93.00   1.00    1.50    --   82.00  45.00 137.96   27
 26  \w     63.00  90.00   1.00    1.50    --   90.00  66.00 -44.19   27
 27  \w     79.00 125.00   1.00    1.50    --  103.86  61.00 150.00   46
 28  \w    101.00 127.00   1.00    1.50    --  103.86 -77.00-150.00   26
 29  \w     34.00  88.00   1.00    1.50    --  103.86 -77.00-150.00   54
 30  \w     45.00 110.00   1.00    1.50    --  103.86-125.00 120.00   65
 31  \w     79.00 104.00   1.00    1.50    --  103.86  45.00  60.00   25
 32  \w    123.00 176.00   1.00    1.50    --  103.86  45.00  30.00   53
 33  \w    116.00 175.00   1.00    1.50    --  103.86  77.00 -60.00   59
 34  \w    135.00 174.00   1.00    1.50    --  103.86  61.00 -30.00   39
 35  \w     84.00 109.00   1.00    1.50    --  103.86  45.00  30.00   25
 36  \w     82.00 111.00   1.00    1.50    --  103.86  61.00 -30.00   29
 37  \w     29.00  96.00   1.00    1.50    --  103.86 -77.00 120.00   67
 38  \w     76.00 101.00   1.00    1.50    --  103.86  61.00-150.00   25
 39  \w     24.00  81.00   1.00    1.50    --  103.86 -95.00  30.00   57
 40  \w    124.00 175.00   1.00    1.50    --  103.86  61.00-180.00   51
 41  \w     75.00 121.00   1.00    1.50    --  103.86  61.00-180.00   46
 42  \w     37.00 112.00   1.00    1.50    --  103.86-125.00 -30.00   75
 43  \w     76.00 175.00   1.00    1.50    --  103.86  61.00  90.00   99
 44  \w     76.00 118.00   1.00    1.50    --  103.86  61.00 -60.00   42
 45  \w     79.00 122.00   1.00    1.50    --  103.86  61.00 120.00   43
 46  \w    138.00 174.00   1.00    1.50    --  103.86  61.00 120.00   36
 47  \w     78.00 112.00   1.00    1.50    --  103.86  61.00   0.00   34
 48  \w     80.00 176.00   1.00    1.50    --  103.86  56.00-127.19   96
 49  \w    124.00 153.00   1.00    1.50    --  103.86  61.00 -90.00   29
 50  \w     78.00 116.00   1.00    1.50    --  103.86  61.00 -90.00   38
 51  \w    126.00 158.00   1.00    1.50    --  103.86  61.00  60.00   32
 52  \w     77.00 104.00   1.00    1.50    --  103.86  61.00  60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0252619000
_diffrn_orient_matrix_UB_12      0.2249305000
_diffrn_orient_matrix_UB_13      0.1020849000
_diffrn_orient_matrix_UB_21      0.2460027000
_diffrn_orient_matrix_UB_22      0.0180699000
_diffrn_orient_matrix_UB_23      0.0228858000
_diffrn_orient_matrix_UB_31      0.0073248000
_diffrn_orient_matrix_UB_32      0.0354768000
_diffrn_orient_matrix_UB_33      -0.1949978000
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3974
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.033
_diffrn_reflns_theta_min         7.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (Rigaku Oxford Diffraction, 2022)
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    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             140
_exptl_crystal_preparation
'0.3mm capillary 1:1 molar ratio grown at about 240-250K'
_exptl_crystal_recrystallization_method
'0.3mm capillary 1:1 molar ratio grown at about 240-250K'
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.09(2)
_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   1.156
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1201
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0959P)^2^+0.0787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1018
_reflns_number_total             1201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5060.cif
_cod_data_source_block           exp_3163
_cod_database_code               1570098
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 F5 H C8 H10'
_chemical_oxdiff_usercomment
'0.3mm capillary 1:1 molar ratio grown at about 240-250K'
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Shared sites
{F1, H1}
{F2, H2}
{F3, H3}
3. Restrained distances
 C6-H7A \\sim C6-H7B \\sim C6-H7C \\sim C6-H7D \\sim C6-H7E \\sim C6-H7F
 with sigma of 0.02
 C7-H7A \\sim C7-H7B \\sim C7-H7C \\sim C7-H7D \\sim C7-H7E \\sim C7-H7F
 with sigma of 0.02
 H7A-H7E \\sim H7A-H7F \\sim H7B-H7D \\sim H7B-H7F \\sim H7C-H7D \\sim H7C-H7E
 with sigma of 0.02
 H7A-H7B \\sim H7A-H7C \\sim H7B-H7C \\sim H7D-H7E \\sim H7D-H7F \\sim H7E-H7F
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(H1)
Uanis(F2) = Uanis(H2)
Uanis(F3) = Uanis(H3)
Uiso(H7A) = Uiso(H7B) = Uiso(H7C) = Uiso(H7D) = Uiso(H7E) = Uiso(H7F)
5. Others
 1*[Sof(F1)+Sof(H1)]+1*[Sof(F3)+Sof(H3)]+1*[Sof(F2)+Sof(H2)]=2.5 with esd of
 0.0005
 Sof(H1)=1-FVAR(1)
 Sof(F1)=FVAR(1)
 Sof(H3)=1-FVAR(2)
 Sof(F3)=FVAR(2)
 Sof(H2)=1-FVAR(3)
 Sof(F2)=FVAR(3)
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H7D(0.5) H7E(0.5) H7F(0.5)
;
_shelx_res_checksum              15864
_shelx_hkl_checksum              40586
_olex2_date_sample_data_collection 2022-03-31
_olex2_exptl_crystal_mounting_method
'0.3mm capillary 1:1 molar ratio grown at about 240-250K'
_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 5.088
_oxdiff_exptl_absorpt_empirical_full_min 0.311