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_7126912
_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         'C19 H16 Cl N O4'
_chemical_formula_sum            'C19 H16 Cl N O4'
_chemical_formula_weight         357.78
_chemical_melting_point          436
_chemical_name_common            Indomethacin
_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             2019-12-26
_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                69.959(2)
_cell_angle_beta                 87.1970(10)
_cell_angle_gamma                69.501(2)
_cell_formula_units_Z            2
_cell_length_a                   9.21730(10)
_cell_length_b                   9.6060(2)
_cell_length_c                   10.8436(2)
_cell_measurement_reflns_used    16583
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      76.2890
_cell_measurement_theta_min      5.1300
_cell_volume                     842.09(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      99.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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   -121.00 -31.00   0.50    0.08    --  -46.37 -20.00 132.00  180
  2  \w    -61.00  30.00   0.50    0.08    --  -46.37  20.00 -60.00  182
  3  \w     31.00 122.00   0.50    0.08    --   46.37  20.00 -60.00  182
  4  \w    -29.00  62.00   0.50    0.08    --   46.37 -20.00 132.00  182
  5  \w   -115.00 -24.00   0.50    0.32    -- -100.00  20.00 -60.00  182
  6  \w   -175.00 -85.00   0.50    0.32    -- -100.00 -20.00 132.00  180
  7  \w     92.00 178.00   0.50    0.32    --  107.00  20.00 -60.00  172
  8  \w     31.00 122.00   0.50    0.32    --  107.00 -20.00 132.00  182
  9  \w     10.00 109.00   0.50    0.08    --   36.00  83.00 156.30  198
 10  \w     17.00  45.00   0.50    0.08    --   44.00  84.00 -37.85   56
 11  \w     16.00  45.00   0.50    0.08    --   44.00  86.00-124.53   58
 12  \w   -120.00 -32.00   0.50    0.08    --  -46.37 -38.00  60.00  176
 13  \w   -118.00 -30.00   0.50    0.08    --  -46.37 -57.00 150.00  176
 14  \w   -118.00 -23.00   0.50    0.08    --  -46.37 -77.00  90.00  190
 15  \w   -118.00 -23.00   0.50    0.08    --  -46.37 -77.00-180.00  190
 16  \w   -119.00 -32.00   0.50    0.08    --  -46.37 -43.00 -69.45  174
 17  \w   -120.00 -32.00   0.50    0.08    --  -46.37 -38.00  90.00  176
 18  \w   -118.00 -30.00   0.50    0.08    --  -46.37 -57.00   0.00  176
 19  \w     23.00 118.00   0.50    0.08    --   46.37  77.00-120.00  190
 20  \w    -25.00  63.00   0.50    0.08    --   46.37 -57.00   0.00  176
 21  \w     15.00  95.00   0.50    0.08    --   46.37-125.00 -90.00  160
 22  \w     19.00  45.00   0.50    0.08    --   48.00  89.00  43.04   52
 23  \w     19.00  45.00   0.50    0.08    --   48.00  88.00 -32.39   52
 24  \w     28.00 125.00   0.50    0.08    --   52.00  77.00 140.18  194
 25  \w   -128.00 -30.00   0.50    0.08    --  -56.00 -81.00 -47.86  196
 26  \w     33.00 129.00   0.50    0.08    --   56.00  75.00 158.90  192
 27  \w     32.00 129.00   0.50    0.08    --   56.00  78.00-114.31  194
 28  \w     32.00  57.00   0.50    0.08    --   56.00  79.00  81.85   50
 29  \w   -137.00 -85.00   0.50    0.08    --  -64.00 -72.00 -82.00  104
 30  \w    -75.00 -39.00   0.50    0.08    --  -64.00 -80.00  -8.77   72
 31  \w    -68.00 -42.00   0.50    0.08    --  -64.00 -73.00 170.54   52
 32  \w    -66.00 -40.00   0.50    0.08    --  -64.00 -76.00 -99.88   52
 33  \w    -63.00 -37.00   0.50    0.08    --  -64.00 -83.00  28.47   52
 34  \w    -75.00 -42.00   0.50    0.08    --  -64.00 -72.00 -82.00   66
 35  \w   -130.00-104.00   0.50    0.08    --  -64.00 -83.00  28.47   52
 36  \w    -68.00 -43.00   0.50    0.08    --  -68.00 -79.00-129.84   50
 37  \w    -74.00 -48.00   0.50    0.08    --  -68.00 -71.00 -22.78   52
 38  \w    -75.00 -49.00   0.50    0.08    --  -68.00 -69.00  70.07   52
 39  \w   -137.00-112.00   0.50    0.08    --  -68.00 -79.00-129.84   50
 40  \w    -76.00 -50.00   0.50    0.08    --  -72.00 -74.00  19.08   52
 41  \w    -74.00 -48.00   0.50    0.08    --  -72.00 -76.00 123.50   52
 42  \w    -82.00 -56.00   0.50    0.32    --  -76.00 -68.00 137.73   52
 43  \w    -81.00 -55.00   0.50    0.32    --  -76.00 -73.00 179.30   52
 44  \w    -90.00 -58.00   0.50    0.32    --  -80.00 -73.00 -35.79   64
 45  \w    -86.00 -53.00   0.50    0.32    --  -80.00 -83.00  85.12   66
 46  \w    -79.00 -54.00   0.50    0.32    --  -80.00 -81.00-120.75   50
 47  \w    -83.00 -57.00   0.50    0.32    --  -80.00 -75.00  -0.20   52
 48  \w    -93.00 -58.00   0.50    0.32    --  -80.00 -74.00 -98.63   70
 49  \w    -93.00 -61.00   0.50    0.32    --  -84.00 -74.00 -57.57   64
 50  \w   -149.00-123.00   0.50    0.32    --  -84.00 -73.00 -68.34   52
 51  \w    -90.00 -64.00   0.50    0.32    --  -84.00 -73.00 -68.34   52
 52  \w    -90.00 -64.00   0.50    0.32    --  -84.00 -72.00 113.53   52
 53  \w    -94.00 -69.00   0.50    0.32    --  -88.00 -65.00-154.95   50
 54  \w    -96.00 -70.00   0.50    0.32    --  -88.00 -64.00  32.23   52
 55  \w   -106.00 -72.00   0.50    0.32    --  -88.00 -59.00  14.32   68
 56  \w    -87.00 -61.00   0.50    0.32    --  -88.00 -83.00-167.79   52
 57  \w    -94.00 -68.00   0.50    0.32    --  -88.00 -72.00 136.97   52
 58  \w    -97.00 -71.00   0.50    0.32    --  -88.00 -63.00 -92.95   52
 59  \w    -91.00 -66.00   0.50    0.32    --  -88.00 -73.00-118.91   50
 60  \w    -97.00 -69.00   0.50    0.32    --  -92.00 -75.00-128.38   56
 61  \w   -161.00-135.00   0.50    0.32    --  -92.00 -75.00-128.38   52
 62  \w   -168.00 -72.00   0.50    0.32    --  -96.00 -76.00  16.07  192
 63  \w   -113.00 -62.00   0.50    0.32    -- -100.00  45.00 120.00  102
 64  \w   -102.00 -76.00   0.50    0.32    -- -100.00 -78.00  -2.85   52
 65  \w   -102.00 -76.00   0.50    0.32    -- -100.00 -77.00-180.00   52
 66  \w    -63.00 -28.00   0.50    0.32    -- -100.00 125.00 -60.00   70
 67  \w   -161.00 -80.00   0.50    0.32    -- -100.00 -70.00   2.19  162
 68  \w   -116.00 -91.00   0.50    0.32    -- -100.00 125.00 -60.00   50
 69  \w   -105.00 -80.00   0.50    0.32    -- -100.00 -68.00 121.02   50
 70  \w   -173.00-111.00   0.50    0.32    -- -100.00 -68.00 121.02  124
 71  \w   -114.00 -76.00   0.50    0.32    -- -100.00 -78.00-105.25   76
 72  \w   -113.00 -78.00   0.50    0.32    -- -100.00 -72.00 -60.04   70
 73  \w   -155.00-130.00   0.50    0.32    -- -100.00 -78.00-105.25   50
 74  \w   -151.00 -82.00   0.50    0.32    -- -100.00 -63.00 -93.70  138
 75  \w   -118.00 -80.00   0.50    0.32    -- -100.00 -67.00 -26.20   76
 76  \w     75.00 107.00   0.50    0.32    --  100.00  83.00  53.46   64
 77  \w   -172.00-126.00   0.50    0.32    -- -100.00 -67.00 -26.20   92
 78  \w   -136.00 -82.00   0.50    0.32    -- -100.00 -75.00 -39.79  108
 79  \w   -119.00 -76.00   0.50    0.32    -- -100.00 -76.00  37.89   86
 80  \w   -149.00-123.00   0.50    0.32    -- -100.00 -72.00 -60.04   52
 81  \w   -173.00-147.00   0.50    0.32    -- -100.00 -76.00  37.89   52
 82  \w   -137.00 -77.00   0.50    0.32    -- -100.00 -76.00-145.30  120
 83  \w   -121.00 -85.00   0.50    0.32    -- -100.00 -56.00 164.91   72
 84  \w   -104.00 -78.00   0.50    0.32    -- -100.00 -77.00  81.86   52
 85  \w   -162.00 -81.00   0.50    0.32    -- -100.00 -72.00 104.40  162
 86  \w   -151.00 -85.00   0.50    0.32    -- -100.00 -45.00 120.00  132
 87  \w   -136.00 -99.00   0.50    0.32    -- -100.00 -61.00-150.00   74
 88  \w   -172.00 -76.00   0.50    0.32    -- -100.00 -76.00  72.77  192
 89  \w     75.00 108.00   0.50    0.32    --  107.00 -94.00 150.00   66
 90  \w     83.00 151.00   0.50    0.32    --  107.00  77.00 120.00  136
 91  \w    146.00 172.00   0.50    0.32    --  107.00  30.00  30.00   52
 92  \w    118.00 144.00   0.50    0.32    --  107.00  30.00  30.00   52
 93  \w     43.00  69.00   0.50    0.32    --  107.00 -94.00 150.00   52
 94  \w     56.00  87.00   0.50    0.32    --  107.00 -61.00 -30.00   62
 95  \w     76.00 108.00   0.50    0.32    --  107.00 -94.00-150.00   64
 96  \w     39.00 122.00   0.50    0.32    --  107.00 -45.00 120.00  166
 97  \w    132.00 176.00   0.50    0.32    --  107.00  61.00 150.00   88
 98  \w     90.00 123.00   0.50    0.32    --  107.00  61.00 150.00   66
 99  \w    148.00 173.00   0.50    0.32    --  107.00  61.00 -30.00   50
100  \w     91.00 118.00   0.50    0.32    --  107.00  61.00 -30.00   54
101  \w     91.00 176.00   0.50    0.32    --  107.00  61.00-120.00  170
102  \w     78.00 117.00   0.50    0.32    --  107.00-125.00 120.00   78
103  \w     35.00 107.00   0.50    0.32    --  107.00 -94.00  90.00  144
104  \w     34.00  81.00   0.50    0.32    --  107.00 -94.00 120.00   94
105  \w     79.00 114.00   0.50    0.32    --  107.00-125.00  90.00   70
106  \w     35.00  73.00   0.50    0.32    --  107.00-125.00  90.00   76
107  \w     35.00  97.00   0.50    0.32    --  107.00-125.00   0.00  124
108  \w     83.00 116.00   0.50    0.32    --  107.00-125.00-150.00   66
109  \w     36.00 121.00   0.50    0.32    --  107.00 -45.00-120.00  170
110  \w     85.00 111.00   0.50    0.32    --  107.00-125.00 -30.00   52
111  \w     38.00  63.00   0.50    0.32    --  107.00-125.00 -30.00   50
112  \w     72.00 122.00   0.50    0.32    --  107.00 -77.00-150.00  100
113  \w     35.00  69.00   0.50    0.32    --  107.00 -77.00-150.00   68
;
_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      0.1763409000
_diffrn_orient_matrix_UB_12      -0.0568038000
_diffrn_orient_matrix_UB_13      0.0336848000
_diffrn_orient_matrix_UB_21      -0.0213160000
_diffrn_orient_matrix_UB_22      0.1556335000
_diffrn_orient_matrix_UB_23      0.0225340000
_diffrn_orient_matrix_UB_31      -0.0223292000
_diffrn_orient_matrix_UB_32      -0.0768516000
_diffrn_orient_matrix_UB_33      0.1462114000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32458
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.808
_diffrn_reflns_theta_min         4.354
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72826
_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    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0364P)^2^+0.4237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3165
_reflns_number_total             3473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Indomethacin-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '436K' was changed to '436'
-- 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               7126912
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K), C00M(H00M),
 C00N(H00N)
2.c Idealised Me refined as rotating group:
 C00O(H00C,H00D,H00F), C00P(H00I,H00L,H00O)
2.d Idealised tetrahedral OH refined as rotating group:
 O005(H005)
;
_shelx_res_checksum              61160
_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 1.545
_oxdiff_exptl_absorpt_empirical_full_min 0.728