A general method for cultivating single crystals from melt microdroplets.
Ou, Xiao; Li, Xizhen; Rong, Haowei; Yu, Lian; Lu, Ming; Chemical communications (Cambridge, England) 56 (2020) 9950–9953; doi:10.1039/d0cc03157g

data_7126902
_publ_section_title
;
 A general method for cultivating single crystals from melt microdroplets.
;
_journal_issue                   69
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9950
_journal_page_last               9953
_journal_paper_doi               10.1039/d0cc03157g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C22 H17 Cl N2'
_chemical_formula_sum            'C22 H17 Cl N2'
_chemical_formula_weight         344.82
_chemical_melting_point          421
_chemical_name_common            Clotrimazole
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-01 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                113.566(2)
_cell_angle_beta                 97.7510(10)
_cell_angle_gamma                96.7670(10)
_cell_formula_units_Z            2
_cell_length_a                   8.68460(10)
_cell_length_b                   10.3809(2)
_cell_length_c                   10.5107(2)
_cell_measurement_reflns_used    18475
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9070
_cell_measurement_theta_min      4.6390
_cell_volume                     845.09(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_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    -26.00  61.00   0.50    0.05    --   46.37 -45.00 -99.00  174
  2  \w     31.00 122.00   0.50    0.05    --   46.37  19.00-180.00  182
  3  \w     56.00 122.00   0.50    0.05    --  105.44 -61.00 -90.00  132
  4  \w     91.00 178.00   0.50    0.05    --  105.44  45.00  51.00  174
  5  \w     89.00 176.00   0.50    0.05    --  105.44  61.00-120.00  174
  6  \w     42.00 137.00   0.50    0.05    --   64.00  73.00 -35.52  190
  7  \w     32.00 119.00   0.50    0.05    --   46.37  45.00  51.00  174
  8  \w     36.00 132.00   0.50    0.05    --   60.00  78.00 135.16  192
  9  \w     38.00 132.00   0.50    0.05    --   60.00  72.00  62.85  188
 10  \w     38.00 132.00   0.50    0.05    --   60.00  72.00  30.22  188
 11  \w     39.00 137.00   0.50    0.05    --   64.00  79.00 -27.19  196
 12  \w     33.00 120.00   0.50    0.05    --  105.44 -45.00 -99.00  174
 13  \w     43.00  69.00   0.50    0.05    --  105.44 -94.00-180.00   52
 14  \w     33.00 109.00   0.50    0.05    --  105.44-125.00 -60.00  152
 15  \w     40.00 100.00   0.50    0.05    --  105.44 -94.00  90.00  120
 16  \w     91.00 117.00   0.50    0.05    --  105.44-125.00  90.00   52
 17  \w     49.00 108.00   0.50    0.05    --  105.44 -94.00 120.00  118
 18  \w     15.00  95.00   0.50    0.05    --   46.37-125.00 150.00  160
 19  \w    -40.00 -11.00   0.50    0.05    --  -40.00 -88.00-119.25   58
 20  \w    -70.00 -44.00   0.50    0.05    --  -68.00 -78.00-153.38   52
 21  \w    -72.00 -46.00   0.50    0.05    --  -68.00 -73.00-179.37   52
 22  \w    -80.00 -54.00   0.50    0.05    --  -80.00 -82.00-110.24   52
 23  \w    -81.00 -55.00   0.50    0.05    --  -76.00 -74.00 -70.22   52
 24  \w    -72.00 -46.00   0.50    0.05    --  -72.00 -82.00  -6.71   52
 25  \w    -72.00 -46.00   0.50    0.05    --  -72.00 -82.00  52.19   52
 26  \w    -79.00 -53.00   0.50    0.05    --  -72.00 -69.00  83.58   52
 27  \w    -71.00 -46.00   0.50    0.05    --  -68.00 -72.00 152.90   50
 28  \w    -76.00 -50.00   0.50    0.05    --  -76.00 -83.00 170.22   52
 29  \w    -92.00 -66.00   0.50    0.05    --  -84.00 -62.00 178.51   52
 30  \w    -90.00 -64.00   0.50    0.05    --  -84.00 -71.00 146.75   52
 31  \w   -101.00 -67.00   0.50    0.05    --  -88.00 -73.00 136.06   68
 32  \w   -110.00 -84.00   0.50    0.05    --  -72.00 -69.00  83.58   52
 33  \w    -89.00 -64.00   0.50    0.05    --  -80.00 -56.00  56.57   50
 34  \w    -87.00 -61.00   0.50    0.05    --  -80.00 -73.00  49.44   52
 35  \w    -89.00 -63.00   0.50    0.05    --  -84.00 -69.00  29.48   52
 36  \w    -94.00 -68.00   0.50    0.05    --  -84.00 -59.00 -34.15   52
 37  \w    -95.00 -69.00   0.50    0.05    --  -92.00 -75.00 -24.67   52
 38  \w   -102.00 -49.00   0.50    0.05    --  -68.00 -68.00  43.90  106
 39  \w   -101.00 -70.00   0.50    0.05    --  -88.00 -62.00  74.62   62
 40  \w   -110.00 -69.00   0.50    0.05    --  -84.00 -55.00 147.89   82
 41  \w   -112.00 -69.00   0.50    0.05    --  -92.00 -74.00 108.20   86
 42  \w   -103.00 -75.00   0.50    0.05    --  -92.00 -64.00  22.60   56
 43  \w   -109.00 -70.00   0.50    0.05    --  -88.00 -63.00   6.32   78
 44  \w   -102.00 -68.00   0.50    0.05    --  -92.00 -80.00 -81.02   68
 45  \w   -102.00 -54.00   0.50    0.05    --  -72.00 -63.00-121.25   96
 46  \w    -88.00 -62.00   0.50    0.05    --  -80.00 -63.00-160.28   52
 47  \w    -93.00 -67.00   0.50    0.05    --  -84.00 -62.00-163.33   52
 48  \w   -100.00 -72.00   0.50    0.05    --  -96.00 -77.00 -94.02   56
 49  \w   -116.00 -73.00   0.50    0.05    --  -96.00 -76.00 -57.39   86
 50  \w   -112.00 -77.00   0.50    0.05    -- -100.00 -74.00-105.72   70
 51  \w   -115.00 -76.00   0.50    0.05    -- -100.00 -77.00 -30.00   78
 52  \w   -119.00 -32.00   0.50    0.05    --  -46.37 -45.00 -99.00  174
 53  \w     22.00 121.00   0.50    0.05    --   48.00  82.00  18.71  198
 54  \w     27.00 125.00   0.50    0.05    --   52.00  81.00 -65.16  196
 55  \w     30.00 125.00   0.50    0.05    --   52.00  74.00-100.25  190
 56  \w     34.00 129.00   0.50    0.05    --   56.00  73.00  84.13  190
 57  \w     34.00 129.00   0.50    0.05    --   56.00  73.00 -66.98  190
 58  \w     36.00 132.00   0.50    0.05    --   60.00  77.00 -55.80  192
 59  \w     28.00 125.00   0.50    0.05    --   52.00  78.00-155.43  194
 60  \w    -12.00  36.00   0.50    0.05    --   20.00  94.00 115.25   96
 61  \w     11.00  45.00   0.50    0.05    --   40.00  88.00 161.30   68
 62  \w     28.00 125.00   0.50    0.05    --   52.00  78.00 114.41  194
 63  \w    -57.00 -30.00   0.50    0.05    --   16.00 163.00 -87.26   54
 64  \w    -61.00  26.00   0.50    0.05    --  -46.37  45.00  51.00  174
 65  \w    -95.00 -70.00   0.50    0.05    -- -100.00  45.00  51.00   50
 66  \w   -122.00 -31.00   0.50    0.05    --  -46.37 -19.00 120.00  182
 67  \w   -120.00 -32.00   0.50    0.05    --  -46.37 -38.00 -30.00  176
 68  \w   -113.00 -35.00   0.50    0.05    -- -100.00  30.00-120.00  156
 69  \w   -118.00 -23.00   0.50    0.05    --  -46.37 -77.00 -30.00  190
 70  \w   -118.00 -23.00   0.50    0.05    --  -46.37 -77.00  30.00  190
 71  \w   -129.00-103.00   0.50    0.05    --  -68.00 -72.00 152.90   52
 72  \w   -132.00 -35.00   0.50    0.05    --  -60.00 -80.00 118.86  194
 73  \w   -123.00 -76.00   0.50    0.05    -- -100.00 -78.00  23.23   94
 74  \w   -121.00 -79.00   0.50    0.05    -- -100.00 -70.00 -10.91   84
 75  \w   -130.00-104.00   0.50    0.05    --  -72.00 -63.00-121.25   52
 76  \w   -132.00 -78.00   0.50    0.05    --  -96.00 -61.00-163.26  108
 77  \w   -113.00 -80.00   0.50    0.05    -- -100.00 -71.00-178.01   66
 78  \w   -150.00-122.00   0.50    0.05    --  -96.00 -76.00 -57.39   56
 79  \w   -160.00-115.00   0.50    0.05    --  -88.00 -63.00   6.32   90
 80  \w   -154.00-128.00   0.50    0.05    --  -88.00 -62.00  74.62   52
 81  \w   -157.00-107.00   0.50    0.05    --  -88.00 -73.00 136.06  100
 82  \w   -155.00-120.00   0.50    0.05    --  -92.00 -74.00 108.20   70
 83  \w   -168.00 -77.00   0.50    0.05    -- -100.00 -76.00  77.69  182
 84  \w   -172.00 -85.00   0.50    0.05    -- -100.00 -45.00 -99.00  174
 85  \w   -164.00-111.00   0.50    0.05    --  -92.00 -75.00 -24.67  106
 86  \w   -166.00-123.00   0.50    0.05    -- -100.00 -74.00-105.72   86
 87  \w   -163.00-136.00   0.50    0.05    --  -96.00 -61.00-163.26   54
 88  \w   -157.00 -82.00   0.50    0.05    -- -100.00 -61.00-180.00  150
 89  \w   -111.00 -62.00   0.50    0.05    -- -100.00  61.00-120.00   98
 90  \w   -116.00 -34.00   0.50    0.05    -- -100.00 125.00-180.00  164
 91  \w   -113.00 -27.00   0.50    0.05    -- -100.00 125.00   0.00  172
 92  \w   -171.00 -77.00   0.50    0.05    -- -100.00 -77.00 150.00  188
 93  \w   -165.00-139.00   0.50    0.05    -- -100.00 -70.00 -10.91   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0573559000
_diffrn_orient_matrix_UB_12      -0.1390594000
_diffrn_orient_matrix_UB_13      -0.0830793000
_diffrn_orient_matrix_UB_21      0.1700120000
_diffrn_orient_matrix_UB_22      0.0850595000
_diffrn_orient_matrix_UB_23      0.0372617000
_diffrn_orient_matrix_UB_31      0.0323303000
_diffrn_orient_matrix_UB_32      -0.0247636000
_diffrn_orient_matrix_UB_33      0.1354408000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30455
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.050
_diffrn_reflns_theta_min         4.684
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0288P)^2^+0.9166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3152
_reflns_number_total             3349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Clotrimazole-100k-HWRong
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '421K' was changed to '421'
-- the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126896--7126915.cif.
;
_cod_database_code               7126902
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C),
 C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I),
 C00J(H00J), C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P)
;
_shelx_res_checksum              95345
_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 1.773
_oxdiff_exptl_absorpt_empirical_full_min 0.627