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_1570099
_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, 2(C4 H5)'
_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           '-I 1'
_space_group_name_H-M_alt        'I -1'
_atom_sites_solution_hydrogens   mixed
_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                106.811(5)
_cell_angle_beta                 80.111(4)
_cell_angle_gamma                97.168(4)
_cell_formula_units_Z            4
_cell_length_a                   10.2296(5)
_cell_length_b                   8.7819(5)
_cell_length_c                   14.6776(7)
_cell_measurement_reflns_used    5497
_cell_measurement_temperature    120
_cell_measurement_theta_max      72.3460
_cell_measurement_theta_min      4.9890
_cell_volume                     1239.51(12)
_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      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_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  87.00 170.66   25
  2  \w      9.00  34.00   1.00    1.00    --   42.00  78.00  96.55   25
  3  \w    -85.00  -7.00   1.00    1.00    --  -42.37 125.00  90.00   78
  4  \w    -99.00 -18.00   1.00    1.00    --  -42.37 -38.00 -30.00   81
  5  \w    -67.00  17.00   1.00    1.00    --  -42.37  38.00 -30.00   84
  6  \w     28.00  90.00   1.00    1.00    --   42.37-125.00  90.00   62
  7  \w     26.00  63.00   1.00    1.00    --   42.37  38.00  60.00   37
  8  \w     12.00  37.00   1.00    1.00    --   46.00  82.00  31.81   25
  9  \w     13.00  39.00   1.00    1.00    --   46.00  79.00 -69.03   26
 10  \w     14.00  42.00   1.00    1.00    --   46.00  79.00-142.31   28
 11  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 -22.21   25
 12  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 -98.11   25
 13  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 138.30   25
 14  \w     24.00  53.00   1.00    1.00    --   54.00  71.00 -41.21   29
 15  \w     25.00  65.00   1.00    1.00    --   54.00  71.00 160.21   40
 16  \w     82.00 127.00   1.00    1.00    --   54.00  71.00 160.21   45
 17  \w     36.00  63.00   1.00    1.00    --   54.00  70.00  82.65   27
 18  \w     85.00 132.00   1.00    1.00    --   58.00  71.00-159.37   47
 19  \w     27.00  53.00   1.00    1.00    --   58.00  70.00 119.34   26
 20  \w     27.00  65.00   1.00    1.00    --   58.00  71.00-159.37   38
 21  \w    117.00 143.00   1.00    1.00    --   70.00  70.00 -31.15   26
 22  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 -31.15   26
 23  \w     42.00  84.00   1.00    1.00    --   70.00  66.00  38.33   42
 24  \w     41.00  68.00   1.00    1.00    --   70.00  69.00-142.24   27
 25  \w    108.00 137.00   1.00    1.00    --   70.00  70.00 -96.69   29
 26  \w     39.00 102.00   1.00    1.00    --   70.00  70.00 -96.69   63
 27  \w     47.00  82.00   1.00    1.00    --   78.00  70.00 -31.25   35
 28  \w     61.00  92.00   1.00    1.00    --   82.00  46.00 146.11   31
 29  \w     52.00  79.00   1.00    1.00    --   82.00  64.00  -6.71   27
 30  \w     56.00  83.00   1.00    1.00    --   86.00  64.00  95.39   27
 31  \w     77.00 104.00   1.00    1.00    --  103.86  61.00 -90.00   27
 32  \w     25.00 104.00   1.00    1.00    --  103.86 -95.00 -30.00   79
 33  \w     76.00 174.00   1.00    1.00    --  103.86  61.00-180.00   98
 34  \w     75.00 148.00   1.00    1.00    --  103.86  61.00  30.00   73
 35  \w    130.00 164.00   1.00    1.00    --  103.86  61.00 -30.00   34
 36  \w    119.00 173.00   1.00    1.00    --  103.86 125.00 150.00   54
 37  \w     75.00 126.00   1.00    1.00    --  103.86  61.00 -30.00   51
 38  \w     26.00  84.00   1.00    1.00    --  103.86 -95.00 -90.00   58
 39  \w     24.00 106.00   1.00    1.00    --  103.86 -95.00  90.00   82
 40  \w     77.00 152.00   1.00    1.00    --  103.86  61.00 -60.00   75
 41  \w     75.00 111.00   1.00    1.00    --  103.86  61.00-150.00   36
 42  \w     55.00 109.00   1.00    1.00    --  103.86-108.00-135.20   54
 43  \w    143.00 170.00   1.00    1.00    --  103.86  60.00 140.18   27
 44  \w     75.00 112.00   1.00    1.00    --  103.86  61.00   0.00   37
 45  \w     78.00 105.00   1.00    1.00    --  103.86  45.00-180.00   27
 46  \w    105.00 170.00   1.00    1.00    --  103.86  77.00 120.00   65
 47  \w     75.00 103.00   1.00    1.00    --  103.86  60.00 140.18   28
 48  \w     81.00 174.00   1.00    1.00    --  103.86  61.00-120.00   93
 49  \w     32.00 129.00   1.00    1.00    --  103.86 -45.00  90.00   97
 50  \w     79.00 149.00   1.00    1.00    --  103.86  61.00  90.00   70
 51  \w     75.00 175.00   1.00    1.00    --  103.86  61.00  60.00  100
;
_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      -0.1003467105
_diffrn_orient_matrix_UB_12      0.1259240932
_diffrn_orient_matrix_UB_13      0.0504297572
_diffrn_orient_matrix_UB_21      0.1150541530
_diffrn_orient_matrix_UB_22      0.1321248765
_diffrn_orient_matrix_UB_23      0.0104932333
_diffrn_orient_matrix_UB_31      -0.0145455365
_diffrn_orient_matrix_UB_32      0.0219938929
_diffrn_orient_matrix_UB_33      -0.0980783227
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9202
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         5.050
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08346
_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    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_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          0.955
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.365
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2405
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1271P)^2^+1.1285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2042
_reflns_number_total             2405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5060.cif
_cod_data_source_block           exp_3166
_cod_database_code               1570099
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 F5 H C8 H10'
_chemical_oxdiff_usercomment
'Phase II in 0.3mm capillary 1:1 molar ratio grown at about 240-250K'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.391
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{F3, H3}
{F5, H5}
{F6, H6}
3. Restrained distances
 C2-H2
 0.9 with sigma of 0.001
 H2-C1 \\sim H2-C3
 with sigma of 0.001
 F2-C1 \\sim F2-C3
 with sigma of 0.001
 H2-C6 \\sim H2-C4
 with sigma of 0.001
 F2-C6 \\sim F2-C4
 with sigma of 0.001
4. Restrained planarity
 F2, H2, C1, C2, C3
 with sigma of 0.001
5. Others
 1*[Sof(F2)+Sof(H2)]+3*[Sof(F3)+Sof(F5)+Sof(F6)+Sof(H3)+Sof(H5)+Sof(H6)]=3
 with esd of 0.001
 Sof(H2)=1-FVAR(1)
 Sof(F2)=FVAR(1)
 Sof(H3)=Sof(H5)=Sof(H6)=1-FVAR(2)
 Sof(F3)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              97012
_shelx_hkl_checksum              66028
_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 12.243
_oxdiff_exptl_absorpt_empirical_full_min 0.353